data_complex-2a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 I4 N6 Pd2, 0.5(C H2 Cl2)' _chemical_formula_sum 'C22.50 H27 Cl I4 N6 Pd2' _chemical_formula_weight 1137.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.6395(8) _cell_length_b 13.1766(10) _cell_length_c 13.3346(9) _cell_angle_alpha 71.430(5) _cell_angle_beta 66.276(5) _cell_angle_gamma 70.827(6) _cell_volume 1726.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23718 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 29.53 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1050 _exptl_absorpt_coefficient_mu 4.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2380 _exptl_absorpt_correction_T_max 0.4747 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16880 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6105 _reflns_number_gt 5157 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997), MERCURY (Macrea 2006), PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Iodine I3 in one of the binuclear compexes is disordered over two positions (occupancies 0.7/0.3 for atoms I3A/I3B). The methyl groups of the ethyl subsituents are disordered over two positions in each molecule (occupancies 0.7/0.3 for atoms C10A/C10B and C22A/C22B). Various restraints were applied, they included The two phenyl rings (C3-C8 Molecule A and C14-C19 Molecule B) were fitted to regular hexagons Equal anisotropic displacement parameters: EADP C22B C22A EADP C11B C11A EADP C16 C17 C15 EADP C7 C8 C6 Restrained C-C distances for the disordred ethyl groups: DFIX 1.50 .02 C10 C11A C10 C11B C21 C22A C21 C22B Anti bump restrictions: DFIX -3.2 .02 C22B C7 C22B C8 DFIX -2.8 .02 H22D C7 Upper 2\q limit of the data set to 50.1\% OMIT 0 50.1 Refections with large Delta(F^2^)/esd were omitted OMIT 2 0 0 OMIT 0 1 0 OMIT -2 2 1 The SQUEEZE routine in PLATON was used to deal with the disordered solvent: (the potential voids were calculated to contain 115 electrons for a volume of 338.6 \%A^3^). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.9776P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00136(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6105 _refine_ls_number_parameters 275 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I3A I Uani 0.60802(15) 0.06286(12) 0.02297(15) 0.700 0.0532(4) . . I4 I Uani 0.33278(4) -0.22216(3) 0.28235(3) 1.000 0.0372(1) . . Pd2 Pd Uani 0.47638(4) -0.08926(4) 0.14561(3) 1.000 0.0424(2) . . I3B I Uani 0.6475(4) 0.0231(3) 0.0021(4) 0.300 0.0696(14) . . N4 N Uani 0.5198(5) -0.0573(4) 0.3372(4) 1.000 0.0468(17) . . N5 N Uani 0.5891(6) -0.0945(5) 0.4054(4) 1.000 0.0537(17) . . N6 N Uani 0.6686(5) -0.1857(5) 0.3743(4) 1.000 0.0493(17) . . C12 C Uani 0.5540(5) -0.1197(5) 0.2618(4) 1.000 0.0403(17) . . C13 C Uani 0.6535(6) -0.2069(5) 0.2868(5) 1.000 0.0438(19) . . C14 C Uani 0.7284(4) -0.3003(3) 0.2347(3) 1.000 0.0470(19) . G C15 C Uani 0.7721(4) -0.2827(3) 0.1184(3) 1.000 0.0677(16) . G C16 C Uani 0.8395(4) -0.3711(4) 0.0662(2) 1.000 0.0677(16) . G C17 C Uani 0.8631(4) -0.4770(4) 0.1303(4) 1.000 0.0677(16) . G C18 C Uani 0.8193(4) -0.4946(3) 0.2466(3) 1.000 0.068(3) . G C19 C Uani 0.7520(4) -0.4063(3) 0.2988(2) 1.000 0.057(2) . G C20 C Uani 0.7653(8) -0.2466(7) 0.4310(7) 1.000 0.074(3) . . C21 C Uani 0.4164(7) 0.0427(5) 0.3530(6) 1.000 0.056(2) . . C22A C Uani 0.2881(10) 0.0178(8) 0.4354(10) 0.700 0.070(4) . . C22B C Uani 0.501(2) 0.1064(13) 0.2737(19) 0.300 0.070(4) . . I1 I Uani 0.07735(3) 0.61062(3) 0.47294(3) 1.000 0.0354(1) . . I2 I Uani 0.17084(4) 0.31644(3) 0.24869(3) 1.000 0.0440(1) . . Pd1 Pd Uani 0.11985(3) 0.46367(3) 0.36057(3) 1.000 0.0301(1) . . N1 N Uani 0.2423(4) 0.6039(4) 0.1457(3) 1.000 0.0367(14) . . N2 N Uani 0.3495(4) 0.6328(4) 0.0701(3) 1.000 0.0377(14) . . N3 N Uani 0.4384(4) 0.5713(3) 0.1155(3) 1.000 0.0304(12) . . C1 C Uani 0.2606(5) 0.5247(4) 0.2359(4) 1.000 0.0323(16) . . C2 C Uani 0.3913(5) 0.5024(4) 0.2150(4) 1.000 0.0309(14) . . C3 C Uani 0.4726(4) 0.4254(3) 0.2799(3) 1.000 0.0363(17) . G C4 C Uani 0.4599(4) 0.4418(3) 0.3821(3) 1.000 0.0468(19) . G C5 C Uani 0.5371(4) 0.3682(4) 0.4436(3) 1.000 0.053(2) . G C6 C Uani 0.6269(5) 0.2783(4) 0.4028(4) 1.000 0.0926(17) . G C7 C Uani 0.6396(5) 0.2619(4) 0.3006(4) 1.000 0.0926(17) . G C8 C Uani 0.5624(5) 0.3355(4) 0.2391(3) 1.000 0.0926(17) . G C9 C Uani 0.5684(5) 0.5911(5) 0.0589(5) 1.000 0.0482(19) . . C10 C Uani 0.1180(6) 0.6574(6) 0.1250(6) 1.000 0.061(2) . . C11A C Uani 0.1257(10) 0.7372(9) 0.0177(8) 0.700 0.066(3) . . C11B C Uani 0.077(2) 0.7719(14) 0.128(2) 0.300 0.066(3) . . H16 H Uiso 0.86930 -0.35910 -0.01330 1.000 0.0810 calc R H17 H Uiso 0.90910 -0.53740 0.09460 1.000 0.0810 calc R H15 H Uiso 0.75600 -0.21030 0.07460 1.000 0.0810 calc R H19 H Uiso 0.72210 -0.41830 0.37830 1.000 0.0680 calc R H20A H Uiso 0.80080 -0.19440 0.44150 1.000 0.1110 calc R H18 H Uiso 0.83550 -0.56700 0.29040 1.000 0.0820 calc R H20C H Uiso 0.72420 -0.29030 0.50420 1.000 0.1110 calc R H21A H Uiso 0.40570 0.08350 0.27970 0.700 0.0680 calc . H21B H Uiso 0.44180 0.09050 0.38070 0.700 0.0680 calc . H22A H Uiso 0.28910 0.00040 0.51220 0.700 0.1050 calc . H22B H Uiso 0.27450 -0.04520 0.42110 0.700 0.1050 calc . H22C H Uiso 0.21810 0.08210 0.42580 0.700 0.1050 calc . H20B H Uiso 0.83500 -0.29560 0.38480 1.000 0.1110 calc R H21C H Uiso 0.35540 0.05310 0.31410 0.300 0.0680 . . H21D H Uiso 0.36850 0.04380 0.43320 0.300 0.0680 . . H22D H Uiso 0.57760 0.08970 0.29460 0.300 0.1050 calc . H22E H Uiso 0.45810 0.18450 0.27050 0.300 0.1050 calc . H22F H Uiso 0.52590 0.08990 0.20000 0.300 0.1050 calc . H5 H Uiso 0.52840 0.37940 0.51350 1.000 0.0640 calc R H6 H Uiso 0.67970 0.22810 0.44480 1.000 0.1110 calc R H4 H Uiso 0.39850 0.50320 0.41000 1.000 0.0560 calc R H8 H Uiso 0.57110 0.32430 0.16920 1.000 0.1110 calc R H9A H Uiso 0.56860 0.65300 -0.00570 1.000 0.0730 calc R H7 H Uiso 0.70100 0.20050 0.27270 1.000 0.1110 calc R H9C H Uiso 0.59520 0.60840 0.11130 1.000 0.0730 calc R H10A H Uiso 0.07930 0.59940 0.12810 0.700 0.0730 calc . H10B H Uiso 0.05890 0.69540 0.18660 0.700 0.0730 calc . H11A H Uiso 0.04360 0.75620 0.00430 0.700 0.1000 calc . H11B H Uiso 0.19520 0.70490 -0.04320 0.700 0.1000 calc . H11C H Uiso 0.14360 0.80380 0.02060 0.700 0.1000 calc . H9B H Uiso 0.62860 0.52500 0.03340 1.000 0.0730 calc R H10C H Uiso 0.08810 0.59610 0.12860 0.300 0.0730 . . H10D H Uiso 0.09430 0.69560 0.18660 0.300 0.0730 . . H11D H Uiso 0.14880 0.80750 0.08230 0.300 0.1000 calc . H11E H Uiso 0.04710 0.78000 0.20520 0.300 0.1000 calc . H11F H Uiso 0.00570 0.80660 0.09710 0.300 0.1000 calc . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I3A 0.0606(8) 0.0742(8) 0.0371(6) 0.0294(5) -0.0349(6) -0.0475(6) I4 0.0469(2) 0.0373(2) 0.0256(2) 0.0058(1) -0.0111(2) -0.0206(2) Pd2 0.0449(3) 0.0576(3) 0.0282(2) 0.0220(2) -0.0246(2) -0.0307(2) I3B 0.065(2) 0.103(3) 0.051(2) 0.0447(17) -0.0436(17) -0.0606(18) N4 0.054(3) 0.050(3) 0.038(3) 0.007(2) -0.031(2) -0.010(2) N5 0.062(3) 0.061(3) 0.043(3) -0.004(2) -0.036(3) -0.004(3) N6 0.050(3) 0.068(3) 0.032(3) 0.003(2) -0.030(2) -0.009(3) C12 0.038(3) 0.052(3) 0.027(3) 0.011(2) -0.016(2) -0.018(3) C13 0.042(3) 0.060(4) 0.028(3) 0.007(3) -0.021(2) -0.014(3) C14 0.030(3) 0.076(4) 0.031(3) -0.001(3) -0.016(2) -0.010(3) C15 0.037(2) 0.123(4) 0.049(2) -0.028(2) -0.0172(17) -0.013(2) C16 0.037(2) 0.123(4) 0.049(2) -0.028(2) -0.0172(17) -0.013(2) C17 0.037(2) 0.123(4) 0.049(2) -0.028(2) -0.0172(17) -0.013(2) C18 0.037(4) 0.095(6) 0.059(4) -0.025(4) -0.010(3) 0.003(3) C19 0.041(3) 0.081(5) 0.036(3) -0.022(3) -0.010(3) 0.006(3) C20 0.075(5) 0.088(5) 0.068(5) -0.016(4) -0.057(4) 0.011(4) C21 0.071(5) 0.048(3) 0.058(4) 0.000(3) -0.043(4) -0.008(3) C22A 0.067(6) 0.046(5) 0.096(8) -0.011(5) -0.043(6) 0.004(4) C22B 0.067(6) 0.046(5) 0.096(8) -0.011(5) -0.043(6) 0.004(4) I1 0.0303(2) 0.0426(2) 0.0267(2) 0.0029(1) -0.0034(1) -0.0178(1) I2 0.0449(2) 0.0426(2) 0.0382(2) -0.0037(2) -0.0110(2) -0.0106(2) Pd1 0.0248(2) 0.0348(2) 0.0214(2) 0.0062(2) -0.0048(2) -0.0108(2) N1 0.034(2) 0.047(3) 0.026(2) 0.0031(19) -0.0115(19) -0.014(2) N2 0.035(2) 0.052(3) 0.022(2) 0.0061(19) -0.0083(19) -0.020(2) N3 0.024(2) 0.042(2) 0.021(2) -0.0033(17) -0.0018(17) -0.0131(18) C1 0.034(3) 0.036(3) 0.024(2) 0.003(2) -0.007(2) -0.017(2) C2 0.028(2) 0.042(3) 0.017(2) -0.003(2) -0.003(2) -0.010(2) C3 0.033(3) 0.043(3) 0.028(3) -0.001(2) -0.011(2) -0.008(2) C4 0.052(4) 0.048(3) 0.040(3) -0.012(3) -0.023(3) 0.001(3) C5 0.060(4) 0.060(4) 0.042(3) -0.008(3) -0.029(3) -0.005(3) C6 0.089(3) 0.096(3) 0.070(3) -0.029(3) -0.047(3) 0.044(3) C7 0.089(3) 0.096(3) 0.070(3) -0.029(3) -0.047(3) 0.044(3) C8 0.089(3) 0.096(3) 0.070(3) -0.029(3) -0.047(3) 0.044(3) C9 0.030(3) 0.066(4) 0.040(3) -0.004(3) -0.001(2) -0.021(3) C10 0.040(3) 0.072(4) 0.059(4) 0.024(3) -0.028(3) -0.021(3) C11A 0.055(6) 0.073(6) 0.063(6) 0.008(5) -0.032(5) -0.011(5) C11B 0.055(6) 0.073(6) 0.063(6) 0.008(5) -0.032(5) -0.011(5) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I3A Pd2 2.6369(19) . . yes I3A Pd2 2.6821(19) . 2_655 yes I3B Pd2 2.662(5) . 2_655 yes I3B Pd2 2.624(5) . . yes I4 Pd2 2.5732(7) . . yes I1 Pd1 2.6733(6) . 2_566 yes I1 Pd1 2.6195(6) . . yes I2 Pd1 2.5916(6) . . yes Pd2 C12 1.967(6) . . yes Pd1 C1 1.979(6) . . yes N4 C12 1.355(8) . . yes N4 C21 1.470(9) . . yes N4 N5 1.328(9) . . yes N5 N6 1.323(9) . . yes N6 C20 1.479(12) . . yes N6 C13 1.369(9) . . yes N1 C1 1.357(7) . . yes N1 N2 1.332(6) . . yes N1 C10 1.481(10) . . yes N2 N3 1.317(7) . . yes N3 C2 1.364(6) . . yes N3 C9 1.464(8) . . yes C12 C13 1.402(9) . . no C13 C14 1.453(7) . . no C14 C15 1.3897 . . no C14 C19 1.3905 . . no C15 C16 1.3905 . . no C16 C17 1.3895 . . no C17 C18 1.3896 . . no C18 C19 1.3893 . . no C21 C22B 1.39(2) . . no C21 C22A 1.522(15) . . no C15 H15 0.9500 . . no C16 H16 0.9500 . . no C17 H17 0.9500 . . no C18 H18 0.9500 . . no C19 H19 0.9500 . . no C20 H20B 0.9800 . . no C20 H20A 0.9800 . . no C20 H20C 0.9800 . . no C21 H21B 0.9900 . . no C21 H21A 0.9900 . . no C21 H21D 0.9900 . . no C21 H21C 0.9900 . . no C22A H22C 0.9800 . . no C22A H22B 0.9800 . . no C22A H22A 0.9800 . . no C22B H22D 0.9800 . . no C22B H22E 0.9800 . . no C22B H22F 0.9800 . . no C1 C2 1.377(9) . . no C2 C3 1.464(7) . . no C3 C4 1.3893 . . no C3 C8 1.3897 . . no C4 C5 1.3909 . . no C5 C6 1.3897 . . no C6 C7 1.3893 . . no C7 C8 1.3909 . . no C10 C11A 1.470(12) . . no C10 C11B 1.43(2) . . no C4 H4 0.9500 . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7 0.9500 . . no C8 H8 0.9500 . . no C9 H9A 0.9800 . . no C9 H9B 0.9800 . . no C9 H9C 0.9800 . . no C10 H10A 0.9900 . . no C10 H10B 0.9900 . . no C10 H10C 0.9600 . . no C10 H10D 1.0000 . . no C11A H11A 0.9800 . . no C11A H11B 0.9800 . . no C11A H11C 0.9800 . . no C11B H10D 1.0700 . . no C11B H11D 0.9800 . . no C11B H11E 0.9700 . . no C11B H11F 0.9900 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd2 I3A Pd2 90.33(6) . . 2_655 yes Pd2 I3B Pd2 91.06(16) . . 2_655 yes Pd1 I1 Pd1 92.80(2) . . 2_566 yes I3A Pd2 I3A 89.67(6) . . 2_655 yes I3A Pd2 I4 173.01(4) . . . yes I3A Pd2 C12 90.02(18) . . . yes I3A Pd2 I4 93.70(4) 2_655 . . yes I3B Pd2 I4 94.07(11) 2_655 . . yes I3B Pd2 C12 90.7(2) . . . yes I3B Pd2 I3B 88.94(15) . . 2_655 yes I3A Pd2 C12 174.05(18) 2_655 . . yes I3B Pd2 I4 172.46(9) . . . yes I4 Pd2 C12 87.26(17) . . . yes I3B Pd2 C12 172.3(2) 2_655 . . yes I1 Pd1 I1 87.20(2) . . 2_566 yes I2 Pd1 C1 86.98(15) . . . yes I1 Pd1 I2 94.16(2) 2_566 . . yes I1 Pd1 C1 177.55(16) 2_566 . . yes I1 Pd1 C1 91.73(15) . . . yes I1 Pd1 I2 177.88(2) . . . yes N5 N4 C12 114.1(5) . . . yes C12 N4 C21 128.3(6) . . . yes N5 N4 C21 117.6(5) . . . yes N4 N5 N6 103.6(5) . . . yes N5 N6 C13 113.4(6) . . . yes C13 N6 C20 128.6(6) . . . yes N5 N6 C20 117.9(6) . . . yes C1 N1 C10 126.4(5) . . . yes N2 N1 C10 119.2(5) . . . yes N2 N1 C1 114.4(5) . . . yes N1 N2 N3 102.8(4) . . . yes N2 N3 C9 117.3(4) . . . yes C2 N3 C9 129.3(5) . . . yes N2 N3 C2 113.3(5) . . . yes Pd2 C12 N4 125.8(5) . . . yes N4 C12 C13 104.4(5) . . . yes Pd2 C12 C13 129.8(5) . . . yes N6 C13 C14 125.4(6) . . . yes N6 C13 C12 104.5(5) . . . yes C12 C13 C14 130.1(6) . . . no C13 C14 C19 121.4(4) . . . no C13 C14 C15 118.6(4) . . . no C15 C14 C19 119.98 . . . no C14 C15 C16 119.98 . . . no C15 C16 C17 120.01 . . . no C16 C17 C18 120.01 . . . no C17 C18 C19 120.01 . . . no C14 C19 C18 120.02 . . . no N4 C21 C22A 112.6(6) . . . yes N4 C21 C22B 90.0(9) . . . yes C16 C15 H15 120.00 . . . no C14 C15 H15 120.00 . . . no C15 C16 H16 120.00 . . . no C17 C16 H16 120.00 . . . no C18 C17 H17 120.00 . . . no C16 C17 H17 120.00 . . . no C17 C18 H18 120.00 . . . no C19 C18 H18 120.00 . . . no C14 C19 H19 120.00 . . . no C18 C19 H19 120.00 . . . no N6 C20 H20C 109.00 . . . no H20A C20 H20B 109.00 . . . no N6 C20 H20A 110.00 . . . no N6 C20 H20B 109.00 . . . no H20B C20 H20C 109.00 . . . no H20A C20 H20C 109.00 . . . no H21A C21 H21B 108.00 . . . no C22A C21 H21B 109.00 . . . no N4 C21 H21A 109.00 . . . no N4 C21 H21B 109.00 . . . no N4 C21 H21C 112.00 . . . no N4 C21 H21D 112.00 . . . no C22A C21 H21A 109.00 . . . no H21C C21 H21D 110.00 . . . no C22B C21 H21C 102.00 . . . no C22B C21 H21D 129.00 . . . no H22A C22A H22B 110.00 . . . no C21 C22A H22A 109.00 . . . no C21 C22A H22B 109.00 . . . no C21 C22A H22C 109.00 . . . no H22A C22A H22C 110.00 . . . no H22B C22A H22C 109.00 . . . no H22E C22B H22F 109.00 . . . no C21 C22B H22D 109.00 . . . no C21 C22B H22E 109.00 . . . no C21 C22B H22F 109.00 . . . no H22D C22B H22E 110.00 . . . no H22D C22B H22F 110.00 . . . no Pd1 C1 N1 123.6(5) . . . yes Pd1 C1 C2 132.6(4) . . . yes N1 C1 C2 103.8(5) . . . yes N3 C2 C1 105.7(5) . . . yes N3 C2 C3 123.0(5) . . . yes C1 C2 C3 131.3(5) . . . no C2 C3 C4 120.2(4) . . . no C2 C3 C8 119.8(4) . . . no C4 C3 C8 120.03 . . . no C3 C4 C5 119.98 . . . no C4 C5 C6 119.99 . . . no C5 C6 C7 120.03 . . . no C6 C7 C8 119.98 . . . no C3 C8 C7 119.99 . . . no N1 C10 C11A 115.5(7) . . . yes N1 C10 C11B 112.8(12) . . . yes C3 C4 H4 120.00 . . . no C5 C4 H4 120.00 . . . no C4 C5 H5 120.00 . . . no C6 C5 H5 120.00 . . . no C5 C6 H6 120.00 . . . no C7 C6 H6 120.00 . . . no C6 C7 H7 120.00 . . . no C8 C7 H7 120.00 . . . no C3 C8 H8 120.00 . . . no C7 C8 H8 120.00 . . . no N3 C9 H9A 110.00 . . . no N3 C9 H9B 109.00 . . . no N3 C9 H9C 109.00 . . . no H9A C9 H9B 110.00 . . . no H9A C9 H9C 109.00 . . . no H9B C9 H9C 109.00 . . . no N1 C10 H10A 108.00 . . . no N1 C10 H10B 108.00 . . . no N1 C10 H10C 103.00 . . . no C11A C10 H10A 108.00 . . . no C11A C10 H10B 108.00 . . . no H10A C10 H10B 107.00 . . . no C11B C10 H10C 143.00 . . . no H10C C10 H10D 127.00 . . . no C10 C11A H11A 109.00 . . . no C10 C11A H11B 109.00 . . . no C10 C11A H11C 109.00 . . . no H11A C11A H11B 110.00 . . . no H11A C11A H11C 110.00 . . . no H11B C11A H11C 109.00 . . . no C10 C11B H11D 110.00 . . . no C10 C11B H11E 110.00 . . . no C10 C11B H11F 109.00 . . . no H10D C11B H11D 118.00 . . . no H10D C11B H11F 131.00 . . . no H11D C11B H11E 110.00 . . . no H11D C11B H11F 109.00 . . . no H11E C11B H11F 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd2 I3A Pd2 C12 174.06(18) 2_655 . . . no Pd2 I3A Pd2 I3A 0.00(6) 2_655 . . 2_655 no Pd2 I3A Pd2 I3A 0.00(4) . . 2_655 2_655 no Pd2 I3A Pd2 I4 -173.87(4) . . 2_655 2_655 no Pd1 I1 Pd1 C1 177.79(17) 2_566 . . . no Pd1 I1 Pd1 I1 0.00(3) 2_566 . . 2_566 no Pd1 I1 Pd1 I1 0.00(3) . . 2_566 2_566 no Pd1 I1 Pd1 I2 -178.37(2) . . 2_566 2_566 no I3A Pd2 C12 C13 -102.9(6) . . . . no I4 Pd2 C12 N4 -96.4(5) . . . . no I3A Pd2 C12 N4 77.2(5) . . . . no I4 Pd2 C12 C13 83.6(6) . . . . no I1 Pd1 C1 N1 -91.1(4) . . . . no I1 Pd1 C1 C2 89.8(5) . . . . no I2 Pd1 C1 C2 -88.5(5) . . . . no I2 Pd1 C1 N1 90.6(4) . . . . no C12 N4 C21 C22A 89.3(9) . . . . no C12 N4 N5 N6 -1.6(7) . . . . no C21 N4 N5 N6 177.4(6) . . . . no N5 N4 C12 Pd2 -178.6(5) . . . . no N5 N4 C12 C13 1.5(7) . . . . no C21 N4 C12 Pd2 2.6(9) . . . . no C21 N4 C12 C13 -177.4(6) . . . . no N5 N4 C21 C22A -89.5(9) . . . . no N4 N5 N6 C20 177.3(6) . . . . no N4 N5 N6 C13 1.0(8) . . . . no N5 N6 C13 C12 -0.2(8) . . . . no N5 N6 C13 C14 179.3(6) . . . . no C20 N6 C13 C14 3.5(11) . . . . no C20 N6 C13 C12 -176.0(7) . . . . no C1 N1 C10 C11A -177.1(7) . . . . no C1 N1 N2 N3 -1.4(6) . . . . no C10 N1 N2 N3 179.3(5) . . . . no N2 N1 C1 Pd1 -179.1(4) . . . . no N2 N1 C1 C2 0.3(6) . . . . no C10 N1 C1 Pd1 0.2(8) . . . . no C10 N1 C1 C2 179.5(5) . . . . no N2 N1 C10 C11A 2.1(9) . . . . no N1 N2 N3 C2 2.0(6) . . . . no N1 N2 N3 C9 -173.6(4) . . . . no N2 N3 C2 C1 -1.9(6) . . . . no N2 N3 C2 C3 179.2(4) . . . . no C9 N3 C2 C1 173.0(5) . . . . no C9 N3 C2 C3 -5.9(8) . . . . no Pd2 C12 C13 C14 -0.1(11) . . . . no N4 C12 C13 N6 -0.7(7) . . . . no Pd2 C12 C13 N6 179.4(5) . . . . no N4 C12 C13 C14 179.9(6) . . . . no C12 C13 C14 C19 -134.6(7) . . . . no C12 C13 C14 C15 42.7(10) . . . . no N6 C13 C14 C15 -136.6(6) . . . . no N6 C13 C14 C19 46.1(9) . . . . no C13 C14 C15 C16 -177.4(5) . . . . no C19 C14 C15 C16 -0.04 . . . . no C13 C14 C19 C18 177.3(5) . . . . no C15 C14 C19 C18 0.02 . . . . no C14 C15 C16 C17 0.02 . . . . no C15 C16 C17 C18 0.03 . . . . no C16 C17 C18 C19 -0.06 . . . . no C17 C18 C19 C14 0.03 . . . . no Pd1 C1 C2 N3 -179.8(4) . . . . no Pd1 C1 C2 C3 -1.0(9) . . . . no N1 C1 C2 N3 0.9(5) . . . . no N1 C1 C2 C3 179.7(5) . . . . no N3 C2 C3 C4 111.2(5) . . . . no N3 C2 C3 C8 -69.0(7) . . . . no C1 C2 C3 C4 -67.4(8) . . . . no C1 C2 C3 C8 112.4(6) . . . . no C2 C3 C4 C5 179.8(5) . . . . no C8 C3 C4 C5 -0.02 . . . . no C2 C3 C8 C7 -179.8(5) . . . . no C4 C3 C8 C7 0.00 . . . . no C3 C4 C5 C6 0.03 . . . . no C4 C5 C6 C7 0.00 . . . . no C5 C6 C7 C8 0.00 . . . . no C6 C7 C8 C3 -0.02 . . . . no _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.844 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.132 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.002 0.000 339 115 ' ' _platon_squeeze_details ; N: Total Potential Solvent Accessible Void Vol . 338.6 Ang^3 N: Electron Count / Cell = 115 Equated to one half molecule of Dichloromethane per molecule of complex. ; #################################################END data_complex-2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H26 I4 N6 Pd2' _chemical_formula_sum 'C14 H26 I4 N6 Pd2' _chemical_formula_weight 998.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 7.6739(15) _cell_length_b 14.442(2) _cell_length_c 11.515(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.469(17) _cell_angle_gamma 90.00 _cell_volume 1275.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3519 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 23.34 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 6.264 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.028 _exptl_absorpt_correction_T_max 0.410 _exptl_absorpt_process_details 'DELrefABS in PLATON; Spek, 2009' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9417 _diffrn_reflns_av_R_equivalents 0.2046 _diffrn_reflns_av_sigmaI/netI 0.1569 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.21 _reflns_number_total 2254 _reflns_number_gt 903 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1249P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2254 _refine_ls_number_parameters 70 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1487 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.2486 _refine_ls_wR_factor_gt 0.2110 _refine_ls_goodness_of_fit_ref 0.837 _refine_ls_restrained_S_all 0.837 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I1 I Uani 0.9105(2) 0.11642(10) 0.47644(16) 1.000 0.0893(6) . . I2 I Uani 0.8792(3) -0.18318(11) 0.22739(17) 1.000 0.1064(8) . . Pd1 Pd Uani 0.9025(3) -0.03439(11) 0.35216(18) 1.000 0.0834(7) . . N1 N Uani 0.592(3) 0.0325(13) 0.205(2) 1.000 0.103(5) . . N2 N Uani 0.541(4) 0.0791(14) 0.112(2) 1.000 0.103(5) . . N3 N Uani 0.681(4) 0.1037(13) 0.069(2) 1.000 0.103(5) . . C1 C Uani 0.768(4) 0.0287(16) 0.227(3) 1.000 0.103(5) . . C2 C Uani 0.825(4) 0.0795(17) 0.135(3) 1.000 0.103(5) . . C3 C Uani 1.008(5) 0.103(2) 0.101(3) 1.000 0.125(7) . . C4 C Uani 1.064(5) 0.199(2) 0.135(3) 1.000 0.125(7) . . C5 C Uani 0.655(5) 0.157(2) -0.037(3) 1.000 0.125(7) . . C6 C Uani 0.452(5) 0.004(2) 0.299(3) 1.000 0.125(7) . . C8 C Uani 0.397(4) 0.077(2) 0.374(3) 1.000 0.125(7) . . H3A H Uiso 1.09010 0.05780 0.13930 1.000 0.1880 calc R H3B H Uiso 1.01550 0.09520 0.01640 1.000 0.1880 calc R H4A H Uiso 1.06090 0.20570 0.21920 1.000 0.1880 calc R H4B H Uiso 0.98400 0.24340 0.09680 1.000 0.1880 calc R H4C H Uiso 1.18250 0.20950 0.10990 1.000 0.1880 calc R H5A H Uiso 0.53040 0.15960 -0.05810 1.000 0.1880 calc R H5B H Uiso 0.71720 0.12690 -0.09940 1.000 0.1880 calc R H5C H Uiso 0.70050 0.21950 -0.02430 1.000 0.1880 calc R H6A H Uiso 0.34780 -0.02200 0.25710 1.000 0.1880 calc R H6B H Uiso 0.50360 -0.04640 0.34820 1.000 0.1880 calc R H8A H Uiso 0.31120 0.05240 0.42670 1.000 0.1880 calc R H8B H Uiso 0.34390 0.12660 0.32670 1.000 0.1880 calc R H8C H Uiso 0.49790 0.10090 0.41920 1.000 0.1880 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0937(13) 0.0742(8) 0.0996(12) -0.0010(8) -0.0007(9) 0.0041(8) I2 0.1418(19) 0.0779(9) 0.0992(13) -0.0049(8) 0.0029(12) 0.0052(10) Pd1 0.0835(14) 0.0740(9) 0.0927(13) 0.0002(8) 0.0057(10) 0.0015(8) N1 0.109(10) 0.079(5) 0.121(10) 0.000(5) -0.002(8) 0.012(6) N2 0.109(10) 0.079(5) 0.121(10) 0.000(5) -0.002(8) 0.012(6) N3 0.109(10) 0.079(5) 0.121(10) 0.000(5) -0.002(8) 0.012(6) C1 0.109(10) 0.079(5) 0.121(10) 0.000(5) -0.002(8) 0.012(6) C2 0.109(10) 0.079(5) 0.121(10) 0.000(5) -0.002(8) 0.012(6) C3 0.117(12) 0.112(9) 0.148(14) 0.014(8) 0.031(10) -0.008(8) C4 0.117(12) 0.112(9) 0.148(14) 0.014(8) 0.031(10) -0.008(8) C5 0.117(12) 0.112(9) 0.148(14) 0.014(8) 0.031(10) -0.008(8) C6 0.117(12) 0.112(9) 0.148(14) 0.014(8) 0.031(10) -0.008(8) C8 0.117(12) 0.112(9) 0.148(14) 0.014(8) 0.031(10) -0.008(8) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd1 2.605(2) . . yes I1 Pd1 2.667(3) . 3_756 yes I2 Pd1 2.587(3) . . yes Pd1 C1 1.96(3) . . yes N1 N2 1.31(3) . . yes N1 C1 1.37(4) . . yes N1 C6 1.61(4) . . yes N2 N3 1.25(4) . . yes N3 C2 1.36(4) . . yes N3 C5 1.45(4) . . yes C1 C2 1.38(4) . . no C2 C3 1.51(5) . . no C3 C4 1.50(4) . . no C6 C8 1.44(4) . . no C3 H3A 1.0000 . . no C3 H3B 0.9800 . . no C4 H4A 0.9800 . . no C4 H4B 0.9800 . . no C4 H4C 0.9800 . . no C5 H5A 0.9800 . . no C5 H5B 0.9800 . . no C5 H5C 0.9800 . . no C6 H6A 0.9900 . . no C6 H6B 0.9900 . . no C8 H8A 0.9800 . . no C8 H8B 0.9800 . . no C8 H8C 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd1 I1 Pd1 91.97(8) . . 3_756 yes I1 Pd1 I2 177.36(12) . . . yes I1 Pd1 C1 90.8(8) . . . yes I1 Pd1 I1 88.03(8) . . 3_756 yes I2 Pd1 C1 87.5(8) . . . yes I1 Pd1 I2 93.68(8) 3_756 . . yes I1 Pd1 C1 178.6(9) 3_756 . . yes N2 N1 C1 116(2) . . . yes N2 N1 C6 120(2) . . . yes C1 N1 C6 123(2) . . . yes N1 N2 N3 104(3) . . . yes N2 N3 C2 113(2) . . . yes N2 N3 C5 113(3) . . . yes C2 N3 C5 133(3) . . . yes Pd1 C1 N1 130(2) . . . yes Pd1 C1 C2 130(2) . . . yes N1 C1 C2 100(3) . . . yes N3 C2 C1 107(3) . . . yes N3 C2 C3 123(3) . . . yes C1 C2 C3 130(3) . . . no C2 C3 C4 114(3) . . . no N1 C6 C8 116(2) . . . yes C2 C3 H3A 108.00 . . . no C2 C3 H3B 109.00 . . . no C4 C3 H3A 109.00 . . . no C4 C3 H3B 110.00 . . . no H3A C3 H3B 107.00 . . . no C3 C4 H4A 109.00 . . . no C3 C4 H4B 109.00 . . . no C3 C4 H4C 109.00 . . . no H4A C4 H4B 110.00 . . . no H4A C4 H4C 110.00 . . . no H4B C4 H4C 110.00 . . . no N3 C5 H5A 109.00 . . . no N3 C5 H5B 109.00 . . . no N3 C5 H5C 109.00 . . . no H5A C5 H5B 110.00 . . . no H5A C5 H5C 110.00 . . . no H5B C5 H5C 110.00 . . . no N1 C6 H6A 109.00 . . . no N1 C6 H6B 108.00 . . . no C8 C6 H6A 109.00 . . . no C8 C6 H6B 108.00 . . . no H6A C6 H6B 107.00 . . . no C6 C8 H8A 109.00 . . . no C6 C8 H8B 109.00 . . . no C6 C8 H8C 109.00 . . . no H8A C8 H8B 110.00 . . . no H8A C8 H8C 110.00 . . . no H8B C8 H8C 110.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 I1 Pd1 C1 -179.2(9) 3_756 . . . no Pd1 I1 Pd1 I1 0.00(8) 3_756 . . 3_756 no Pd1 I1 Pd1 I1 0.00(8) 3_756 3_756 . . no Pd1 I1 Pd1 I2 -177.99(9) 3_756 3_756 . . no I1 Pd1 C1 N1 -94(2) . . . . no I2 Pd1 C1 C2 -95(3) . . . . no I1 Pd1 C1 C2 88(3) . . . . no I2 Pd1 C1 N1 84(2) . . . . no C1 N1 N2 N3 2(3) . . . . no C6 N1 N2 N3 169(2) . . . . no N2 N1 C1 Pd1 -178.5(19) . . . . no N2 N1 C1 C2 0(3) . . . . no C6 N1 C1 Pd1 16(4) . . . . no C6 N1 C1 C2 -166(2) . . . . no N2 N1 C6 C8 -76(3) . . . . no C1 N1 C6 C8 89(3) . . . . no N1 N2 N3 C2 -4(3) . . . . no N1 N2 N3 C5 180(2) . . . . no N2 N3 C2 C1 4(3) . . . . no N2 N3 C2 C3 -179(2) . . . . no C5 N3 C2 C1 179(3) . . . . no C5 N3 C2 C3 -4(4) . . . . no Pd1 C1 C2 N3 176(2) . . . . no Pd1 C1 C2 C3 0(5) . . . . no N1 C1 C2 N3 -2(3) . . . . no N1 C1 C2 C3 -179(3) . . . . no N3 C2 C3 C4 83(4) . . . . no C1 C2 C3 C4 -101(4) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag I1 C1 3.28(3) . . no I1 I2 3.833(3) . 3_756 no I1 I1 3.664(2) . 3_756 no I1 C5 3.78(3) . 4_555 no I2 I1 3.833(3) . 3_756 no I2 C1 3.18(2) . . no I1 H8A 3.2000 . 3_656 no I1 H5C 3.2500 . 4_555 no I1 H8A 3.2800 . 1_655 no I1 H8C 3.2100 . . no I2 H3B 3.2200 . 3_755 no C1 I1 3.28(3) . . no C1 I2 3.18(2) . . no C5 I1 3.78(3) . 4_454 no C5 H3B 2.9500 . . no H3B C5 2.9500 . . no H3B I2 3.2200 . 3_755 no H4B H5C 2.5600 . . no H5B H6A 2.4000 . 3_655 no H5C H4B 2.5600 . . no H5C I1 3.2500 . 4_454 no H6A H5B 2.4000 . 3_655 no H8A I1 3.2800 . 1_455 no H8A I1 3.2000 . 3_656 no H8C I1 3.2100 . . no _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.068 _refine_diff_density_min -1.472 _refine_diff_density_rms 0.292 #################################################END data_complex-2c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H42 I4 N6 Pd2' _chemical_formula_sum 'C22 H42 I4 N6 Pd2' _chemical_formula_weight 1111.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.2840(8) _cell_length_b 9.6916(9) _cell_length_c 11.8468(11) _cell_angle_alpha 71.804(11) _cell_angle_beta 80.644(11) _cell_angle_gamma 69.299(11) _cell_volume 843.77(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6731 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 4.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.205 _exptl_absorpt_correction_T_max 0.384 _exptl_absorpt_process_details 'MULscanABS in PLATON; Spek, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6731 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 26.03 _reflns_number_total 3090 _reflns_number_gt 2307 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3090 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I1 I Uani -0.02227(5) 0.35505(4) 0.37418(3) 1.000 0.0421(1) . . I2 I Uani 0.08497(4) 0.65907(3) -0.06135(3) 1.000 0.0338(1) . . Pd1 Pd Uani 0.02959(5) 0.50436(4) 0.15613(3) 1.000 0.0270(1) . . N1 N Uani 0.1125(5) 0.8234(4) 0.2827(4) 1.000 0.0348(14) . . N2 N Uani 0.2779(5) 0.7496(4) 0.2590(4) 1.000 0.0385(14) . . N3 N Uani 0.2681(5) 0.6389(4) 0.2201(4) 1.000 0.0330(14) . . C1 C Uani 0.1038(6) 0.6396(5) 0.2155(5) 1.000 0.0318(16) . . C2 C Uani 0.0033(6) 0.7618(5) 0.2584(5) 1.000 0.0315(16) . . C3 C Uani -0.1878(6) 0.8262(5) 0.2726(5) 1.000 0.0394(18) . . C4 C Uani -0.2643(7) 0.9587(6) 0.1630(5) 1.000 0.0399(18) . . C5 C Uani -0.4587(7) 1.0279(6) 0.1746(6) 1.000 0.0452(19) . . C6 C Uani -0.5281(8) 1.1653(6) 0.0702(6) 1.000 0.057(2) . . C7 C Uani 0.0761(8) 0.9566(6) 0.3280(5) 1.000 0.043(2) . . C8 C Uani 0.4326(6) 0.5299(6) 0.1887(5) 1.000 0.0382(19) . . C9 C Uani 0.4679(6) 0.3737(5) 0.2794(5) 1.000 0.0391(19) . . C10 C Uani 0.4729(7) 0.3728(7) 0.4046(6) 1.000 0.049(2) . . C11 C Uani 0.5309(10) 0.2116(8) 0.4864(7) 1.000 0.074(3) . . H3A H Uiso -0.21950 0.86440 0.34420 1.000 0.0590 calc R H3B H Uiso -0.23860 0.74390 0.28490 1.000 0.0590 calc R H4A H Uiso -0.21190 1.04010 0.15050 1.000 0.0600 calc R H4B H Uiso -0.23240 0.91980 0.09170 1.000 0.0600 calc R H5A H Uiso -0.49180 1.06000 0.24900 1.000 0.0680 calc R H5B H Uiso -0.51200 0.94910 0.18030 1.000 0.0680 calc R H6A H Uiso -0.49700 1.13380 -0.00350 1.000 0.0850 calc R H6B H Uiso -0.47790 1.24470 0.06550 1.000 0.0850 calc R H6C H Uiso -0.65420 1.20610 0.08110 1.000 0.0850 calc R H7A H Uiso 0.12070 1.03340 0.26950 1.000 0.0660 calc R H7B H Uiso 0.13220 0.92420 0.40290 1.000 0.0660 calc R H7C H Uiso -0.04910 1.00110 0.34180 1.000 0.0660 calc R H8A H Uiso 0.52830 0.57020 0.18510 1.000 0.0570 calc R H8B H Uiso 0.42750 0.51940 0.10900 1.000 0.0570 calc R H9A H Uiso 0.37750 0.33050 0.27600 1.000 0.0580 calc R H9B H Uiso 0.58020 0.30480 0.25600 1.000 0.0580 calc R H10A H Uiso 0.35630 0.42930 0.43280 1.000 0.0730 calc R H10B H Uiso 0.55300 0.42670 0.40760 1.000 0.0730 calc R H11A H Uiso 0.64680 0.15560 0.45930 1.000 0.1110 calc R H11B H Uiso 0.45000 0.15870 0.48550 1.000 0.1110 calc R H11C H Uiso 0.53350 0.21600 0.56760 1.000 0.1110 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0628(2) 0.0385(2) 0.0271(2) -0.0045(2) 0.0031(2) -0.0253(2) I2 0.0473(2) 0.0312(2) 0.0270(2) -0.0041(1) -0.0007(1) -0.0215(1) Pd1 0.0341(2) 0.0218(2) 0.0248(2) -0.0059(1) 0.0007(2) -0.0103(1) N1 0.046(2) 0.0252(19) 0.032(3) -0.0074(17) -0.007(2) -0.0084(18) N2 0.038(2) 0.031(2) 0.047(3) -0.0108(19) -0.007(2) -0.0097(18) N3 0.036(2) 0.0268(19) 0.036(3) -0.0102(17) -0.0039(19) -0.0079(16) C1 0.045(3) 0.024(2) 0.027(3) -0.0051(19) -0.003(2) -0.013(2) C2 0.041(3) 0.024(2) 0.024(3) -0.0015(19) -0.003(2) -0.008(2) C3 0.040(3) 0.031(2) 0.041(4) -0.009(2) 0.002(2) -0.007(2) C4 0.037(3) 0.034(2) 0.044(4) -0.010(2) -0.001(2) -0.007(2) C5 0.038(3) 0.039(3) 0.056(4) -0.015(3) -0.002(3) -0.008(2) C6 0.055(4) 0.043(3) 0.062(5) -0.013(3) -0.019(3) 0.001(3) C7 0.062(4) 0.032(3) 0.038(4) -0.013(2) -0.006(3) -0.013(2) C8 0.034(3) 0.038(3) 0.040(4) -0.013(2) 0.001(2) -0.008(2) C9 0.029(3) 0.035(3) 0.047(4) -0.014(2) 0.001(2) -0.002(2) C10 0.040(3) 0.062(4) 0.036(4) -0.011(3) -0.002(3) -0.007(3) C11 0.063(4) 0.081(5) 0.046(5) 0.004(4) -0.003(3) -0.004(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd1 2.5876(5) . . yes I2 Pd1 2.6050(5) . . yes I2 Pd1 2.6814(6) . 2_565 yes Pd1 C1 1.969(5) . . yes N1 N2 1.332(6) . . yes N1 C2 1.353(7) . . yes N1 C7 1.466(7) . . yes N2 N3 1.324(6) . . yes N3 C1 1.369(7) . . yes N3 C8 1.475(7) . . yes C1 C2 1.377(7) . . no C2 C3 1.485(7) . . no C3 C4 1.545(8) . . no C4 C5 1.511(9) . . no C5 C6 1.515(9) . . no C8 C9 1.518(8) . . no C9 C10 1.488(9) . . no C10 C11 1.512(10) . . no C3 H3A 0.9900 . . no C3 H3B 0.9900 . . no C4 H4A 0.9900 . . no C4 H4B 0.9900 . . no C5 H5A 0.9900 . . no C5 H5B 0.9900 . . no C6 H6A 0.9800 . . no C6 H6B 0.9800 . . no C6 H6C 0.9800 . . no C7 H7A 0.9800 . . no C7 H7B 0.9800 . . no C7 H7C 0.9800 . . no C8 H8A 0.9900 . . no C8 H8B 0.9900 . . no C9 H9A 0.9900 . . no C9 H9B 0.9900 . . no C10 H10A 0.9900 . . no C10 H10B 0.9900 . . no C11 H11A 0.9800 . . no C11 H11B 0.9800 . . no C11 H11C 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd1 I2 Pd1 93.16(2) . . 2_565 yes I1 Pd1 I2 178.49(2) . . . yes I1 Pd1 C1 88.98(16) . . . yes I1 Pd1 I2 94.67(2) . . 2_565 yes I2 Pd1 C1 89.52(16) . . . yes I2 Pd1 I2 86.84(2) . . 2_565 yes I2 Pd1 C1 175.24(15) 2_565 . . yes N2 N1 C2 112.8(4) . . . yes N2 N1 C7 117.0(4) . . . yes C2 N1 C7 130.3(5) . . . yes N1 N2 N3 102.6(4) . . . yes N2 N3 C1 115.0(4) . . . yes N2 N3 C8 117.0(4) . . . yes C1 N3 C8 128.0(4) . . . yes Pd1 C1 N3 128.5(4) . . . yes Pd1 C1 C2 128.7(4) . . . yes N3 C1 C2 102.8(4) . . . yes N1 C2 C1 106.9(5) . . . yes N1 C2 C3 123.5(4) . . . yes C1 C2 C3 129.6(5) . . . no C2 C3 C4 112.0(5) . . . no C3 C4 C5 113.5(5) . . . no C4 C5 C6 112.2(5) . . . no N3 C8 C9 111.0(4) . . . yes C8 C9 C10 115.4(5) . . . no C9 C10 C11 112.0(5) . . . no C2 C3 H3A 109.00 . . . no C2 C3 H3B 109.00 . . . no C4 C3 H3A 109.00 . . . no C4 C3 H3B 109.00 . . . no H3A C3 H3B 108.00 . . . no C3 C4 H4A 109.00 . . . no C3 C4 H4B 109.00 . . . no C5 C4 H4A 109.00 . . . no C5 C4 H4B 109.00 . . . no H4A C4 H4B 108.00 . . . no C4 C5 H5A 109.00 . . . no C4 C5 H5B 109.00 . . . no C6 C5 H5A 109.00 . . . no C6 C5 H5B 109.00 . . . no H5A C5 H5B 108.00 . . . no C5 C6 H6A 109.00 . . . no C5 C6 H6B 109.00 . . . no C5 C6 H6C 109.00 . . . no H6A C6 H6B 109.00 . . . no H6A C6 H6C 109.00 . . . no H6B C6 H6C 110.00 . . . no N1 C7 H7A 109.00 . . . no N1 C7 H7B 109.00 . . . no N1 C7 H7C 109.00 . . . no H7A C7 H7B 110.00 . . . no H7A C7 H7C 110.00 . . . no H7B C7 H7C 109.00 . . . no N3 C8 H8A 109.00 . . . no N3 C8 H8B 109.00 . . . no C9 C8 H8A 109.00 . . . no C9 C8 H8B 109.00 . . . no H8A C8 H8B 108.00 . . . no C8 C9 H9A 108.00 . . . no C8 C9 H9B 108.00 . . . no C10 C9 H9A 108.00 . . . no C10 C9 H9B 108.00 . . . no H9A C9 H9B 107.00 . . . no C9 C10 H10A 109.00 . . . no C9 C10 H10B 109.00 . . . no C11 C10 H10A 109.00 . . . no C11 C10 H10B 109.00 . . . no H10A C10 H10B 108.00 . . . no C10 C11 H11A 109.00 . . . no C10 C11 H11B 110.00 . . . no C10 C11 H11C 109.00 . . . no H11A C11 H11B 110.00 . . . no H11A C11 H11C 109.00 . . . no H11B C11 H11C 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 I2 Pd1 C1 -176.94(15) 2_565 . . . no Pd1 I2 Pd1 I2 0.00(5) 2_565 . . 2_565 no Pd1 I2 Pd1 I1 179.97(4) . . 2_565 2_565 no Pd1 I2 Pd1 I2 0.02(9) . . 2_565 2_565 no I1 Pd1 C1 N3 103.2(5) . . . . no I1 Pd1 C1 C2 -79.6(5) . . . . no I2 Pd1 C1 N3 -76.7(5) . . . . no I2 Pd1 C1 C2 100.5(5) . . . . no C2 N1 N2 N3 -0.6(6) . . . . no C7 N1 N2 N3 -179.6(4) . . . . no N2 N1 C2 C1 -0.2(6) . . . . no N2 N1 C2 C3 -177.6(5) . . . . no C7 N1 C2 C1 178.7(5) . . . . no C7 N1 C2 C3 1.3(9) . . . . no N1 N2 N3 C1 1.2(6) . . . . no N1 N2 N3 C8 -178.1(4) . . . . no N2 N3 C1 Pd1 176.5(4) . . . . no N2 N3 C1 C2 -1.3(6) . . . . no C8 N3 C1 Pd1 -4.3(8) . . . . no C8 N3 C1 C2 177.9(5) . . . . no N2 N3 C8 C9 108.6(5) . . . . no C1 N3 C8 C9 -70.6(7) . . . . no Pd1 C1 C2 N1 -177.0(4) . . . . no Pd1 C1 C2 C3 0.2(9) . . . . no N3 C1 C2 N1 0.8(6) . . . . no N3 C1 C2 C3 178.0(5) . . . . no N1 C2 C3 C4 83.6(6) . . . . no C1 C2 C3 C4 -93.2(7) . . . . no C2 C3 C4 C5 -179.6(5) . . . . no C3 C4 C5 C6 175.5(5) . . . . no N3 C8 C9 C10 -57.1(6) . . . . no C8 C9 C10 C11 -172.7(5) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag I1 C1 3.223(5) . . no I1 C2 3.819(5) . . no I1 C7 3.850(6) . 1_545 no I1 I2 3.8751(6) . 2_565 no I2 C1 3.252(6) . . no I2 I2 3.6340(6) . 2_565 no I2 I1 3.8751(6) . 2_565 no I1 H10B 3.3200 . 1_455 no I1 H9A 3.2800 . . no I2 H8B 3.3800 . . no I2 H4A 3.2600 . 2_575 no I2 H6C 3.3600 . 2_475 no I2 H7A 3.3200 . 2_575 no I2 H9B 3.3500 . 2_665 no Pd1 C6 4.198(6) . 1_645 no Pd1 C9 3.773(5) . . no Pd1 H3B 3.1800 . . no Pd1 H6C 3.3900 . 1_645 no Pd1 H8B 3.3000 . . no Pd1 H9A 3.0900 . . no N2 C10 3.424(8) . . no N2 H5B 2.8900 . 1_655 no N2 H11C 2.9300 . 2_666 no N3 H10A 2.7100 . . no C1 I1 3.223(5) . . no C1 I2 3.252(6) . . no C6 Pd1 4.198(6) . 1_465 no C7 I1 3.850(6) . 1_565 no C9 Pd1 3.773(5) . . no C10 N2 3.424(8) . . no C1 H9A 3.0000 . . no C3 H7C 2.7200 . . no C5 H6A 3.0500 . 2_475 no C7 H3A 2.8500 . . no C9 H5A 3.0700 . 1_645 no C9 H6B 3.0700 . 1_645 no C11 H7B 2.9600 . 2_666 no H3A C7 2.8500 . . no H3A H5A 2.5300 . . no H3A H7C 2.2400 . . no H3A H11B 2.5600 . 2_566 no H3B Pd1 3.1800 . . no H4A H6B 2.4900 . . no H4A I2 3.2600 . 2_575 no H4B H6A 2.5500 . . no H5A C9 3.0700 . 1_465 no H5A H3A 2.5300 . . no H5A H9A 2.5600 . 1_465 no H5B N2 2.8900 . 1_455 no H5B H6A 2.4500 . 2_475 no H6A H4B 2.5500 . . no H6A C5 3.0500 . 2_475 no H6A H5B 2.4500 . 2_475 no H6A H6A 2.5900 . 2_475 no H6B C9 3.0700 . 1_465 no H6B H4A 2.4900 . . no H6C Pd1 3.3900 . 1_465 no H6C I2 3.3600 . 2_475 no H7A I2 3.3200 . 2_575 no H7B C11 2.9600 . 2_666 no H7B H11A 2.4100 . 2_666 no H7C C3 2.7200 . . no H7C H3A 2.2400 . . no H8A H10B 2.5700 . . no H8B I2 3.3800 . . no H8B Pd1 3.3000 . . no H9A I1 3.2800 . . no H9A Pd1 3.0900 . . no H9A C1 3.0000 . . no H9A H5A 2.5600 . 1_645 no H9A H11B 2.5500 . . no H9B H11A 2.4300 . . no H9B I2 3.3500 . 2_665 no H10A N3 2.7100 . . no H10B I1 3.3200 . 1_655 no H10B H8A 2.5700 . . no H11A H9B 2.4300 . . no H11A H7B 2.4100 . 2_666 no H11B H9A 2.5500 . . no H11B H3A 2.5600 . 2_566 no H11C N2 2.9300 . 2_666 no _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.215 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.168 # start Validation Reply Form _vrf_PLAT029_complex-2c ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: ...The Stoe IPDS1 one circle machine for the triclinic system can measure only ca. 93% of the Ewald sphere. ; # end Validation Reply Form #################################################END data_complex-2d _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H34 I4 N6 Pd2, C H2 Cl2' _chemical_formula_sum 'C27 H36 Cl2 I4 N6 Pd2' _chemical_formula_weight 1235.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 8.7187(5) _cell_length_b 15.5227(7) _cell_length_c 14.8293(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.836(5) _cell_angle_gamma 90.00 _cell_volume 1992.70(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24356 _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 26.09 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 4.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details 'MULscanABS in PLATON; Spek, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25123 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.71 _reflns_number_total 3747 _reflns_number_gt 3089 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+1.7730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3747 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I1 I Uani 0.55330(5) 0.10351(2) 0.55064(2) 1.000 0.0324(1) . . I2 I Uani 0.21707(5) 0.01665(3) 0.25028(3) 1.000 0.0382(1) . . Pd1 Pd Uani 0.38198(5) 0.05922(3) 0.40174(3) 1.000 0.0264(1) . . N1 N Uani 0.2427(6) 0.2344(3) 0.4179(3) 1.000 0.0336(16) . . N2 N Uani 0.2321(7) 0.3153(3) 0.3858(4) 1.000 0.0399(16) . . N3 N Uani 0.3215(7) 0.3142(3) 0.3198(4) 1.000 0.0374(16) . . C1 C Uani 0.3350(7) 0.1812(4) 0.3733(4) 1.000 0.0308(17) . . C2 C Uani 0.3858(7) 0.2350(4) 0.3086(4) 1.000 0.0353(17) . . C3 C Uani 0.4861(8) 0.2178(4) 0.2358(4) 1.000 0.0387(19) . . C4 C Uani 0.6566(8) 0.2459(5) 0.2574(5) 1.000 0.045(2) . . C5 C Uani 0.7467(9) 0.1971(5) 0.3355(5) 1.000 0.048(2) . . C6 C Uani 0.7642(10) 0.1014(5) 0.3159(6) 1.000 0.060(3) . . C7 C Uani 0.3387(10) 0.3939(4) 0.2709(5) 1.000 0.052(3) . . C8 C Uani 0.1600(7) 0.2153(4) 0.4938(4) 1.000 0.0324(17) . . C9 C Uani 0.1510(8) 0.2774(4) 0.5607(5) 1.000 0.042(2) . . C10 C Uani 0.0709(8) 0.2589(5) 0.6329(5) 1.000 0.045(2) . . C11 C Uani -0.0004(8) 0.1788(5) 0.6377(5) 1.000 0.046(2) . . C12 C Uani 0.0101(8) 0.1184(4) 0.5711(5) 1.000 0.0416(19) . . C13 C Uani 0.0892(8) 0.1355(4) 0.4979(5) 1.000 0.040(2) . . Cl1 Cl Uani 0.5702(5) 0.1304(3) 0.0072(3) 0.500 0.0682(17) . . Cl2 Cl Uani 0.8441(6) 0.0320(3) 0.0535(4) 0.500 0.0816(17) . . C14 C Uani 0.7610(19) 0.1150(9) -0.0083(9) 0.500 0.050(5) . . H3A H Uiso 0.44130 0.24770 0.17990 1.000 0.0580 calc R H3B H Uiso 0.48370 0.15520 0.22280 1.000 0.0580 calc R H4A H Uiso 0.70890 0.23790 0.20230 1.000 0.0680 calc R H4B H Uiso 0.65950 0.30810 0.27220 1.000 0.0680 calc R H5A H Uiso 0.69340 0.20360 0.39040 1.000 0.0720 calc R H5B H Uiso 0.85070 0.22300 0.34860 1.000 0.0720 calc R H6A H Uiso 0.81820 0.09430 0.26210 1.000 0.0900 calc R H6B H Uiso 0.66180 0.07480 0.30490 1.000 0.0900 calc R H6C H Uiso 0.82390 0.07370 0.36810 1.000 0.0900 calc R H7A H Uiso 0.23740 0.41300 0.24220 1.000 0.0780 calc R H7B H Uiso 0.38290 0.43820 0.31340 1.000 0.0780 calc R H7C H Uiso 0.40750 0.38450 0.22420 1.000 0.0780 calc R H9 H Uiso 0.19940 0.33180 0.55650 1.000 0.0620 calc R H10 H Uiso 0.06430 0.30050 0.67930 1.000 0.0680 calc R H11 H Uiso -0.05650 0.16610 0.68720 1.000 0.0690 calc R H12 H Uiso -0.03780 0.06380 0.57560 1.000 0.0620 calc R H13 H Uiso 0.09510 0.09380 0.45150 1.000 0.0600 calc R H14A H Uiso 0.76790 0.10400 -0.07340 0.500 0.0600 calc . H14B H Uiso 0.81940 0.16840 0.00890 0.500 0.0600 calc . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0441(2) 0.0216(2) 0.0303(2) -0.0003(1) 0.0002(2) 0.0029(2) I2 0.0476(3) 0.0304(2) 0.0344(2) 0.0012(2) -0.0037(2) -0.0011(2) Pd1 0.0319(2) 0.0204(2) 0.0270(2) 0.0024(2) 0.0046(2) 0.0020(2) N1 0.038(3) 0.023(2) 0.040(3) 0.003(2) 0.005(2) 0.002(2) N2 0.044(3) 0.024(2) 0.053(3) 0.006(2) 0.011(3) 0.004(2) N3 0.046(3) 0.025(2) 0.042(3) 0.008(2) 0.008(2) 0.003(2) C1 0.032(3) 0.026(3) 0.034(3) 0.002(2) 0.002(2) 0.002(2) C2 0.041(3) 0.028(3) 0.037(3) 0.008(3) 0.005(3) 0.001(3) C3 0.045(4) 0.034(3) 0.038(3) 0.005(3) 0.009(3) -0.001(3) C4 0.050(4) 0.039(4) 0.048(4) 0.003(3) 0.012(3) -0.002(3) C5 0.048(4) 0.043(4) 0.052(4) -0.001(3) 0.004(3) -0.002(3) C6 0.057(5) 0.043(4) 0.081(6) 0.001(4) 0.010(4) 0.007(4) C7 0.069(5) 0.026(3) 0.062(5) 0.018(3) 0.016(4) 0.001(3) C8 0.030(3) 0.028(3) 0.040(3) 0.004(2) 0.007(3) 0.002(2) C9 0.045(4) 0.030(3) 0.051(4) -0.004(3) 0.010(3) -0.003(3) C10 0.050(4) 0.040(4) 0.048(4) -0.010(3) 0.014(3) -0.001(3) C11 0.042(4) 0.045(4) 0.054(4) 0.002(3) 0.017(3) 0.002(3) C12 0.038(3) 0.031(3) 0.058(4) -0.002(3) 0.015(3) -0.003(3) C13 0.042(4) 0.029(3) 0.051(4) -0.007(3) 0.011(3) 0.000(3) Cl1 0.064(3) 0.073(3) 0.066(3) 0.003(2) 0.001(2) 0.018(2) Cl2 0.082(3) 0.077(3) 0.087(3) 0.038(3) 0.015(3) 0.035(3) C14 0.076(10) 0.040(7) 0.029(6) 0.008(6) -0.011(7) -0.003(7) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd1 2.6066(6) . . yes I1 Pd1 2.6651(6) . 3_656 yes I2 Pd1 2.6038(6) . . yes Pd1 C1 1.972(6) . . yes Cl1 C14 1.723(17) . . yes Cl2 C14 1.693(15) . . yes N1 C8 1.438(8) . . yes N1 N2 1.342(7) . . yes N1 C1 1.376(8) . . yes N2 N3 1.322(8) . . yes N3 C2 1.370(8) . . yes N3 C7 1.451(8) . . yes C1 C2 1.384(9) . . no C2 C3 1.492(9) . . no C3 C4 1.546(10) . . no C4 C5 1.522(11) . . no C5 C6 1.525(11) . . no C8 C9 1.392(9) . . no C8 C13 1.389(9) . . no C9 C10 1.376(10) . . no C10 C11 1.396(11) . . no C11 C12 1.373(10) . . no C12 C13 1.379(10) . . no C3 H3B 0.9900 . . no C3 H3A 0.9900 . . no C4 H4B 0.9900 . . no C4 H4A 0.9900 . . no C5 H5B 0.9900 . . no C5 H5A 0.9900 . . no C6 H6A 0.9800 . . no C6 H6B 0.9800 . . no C6 H6C 0.9800 . . no C7 H7A 0.9800 . . no C7 H7C 0.9800 . . no C7 H7B 0.9800 . . no C9 H9 0.9500 . . no C10 H10 0.9500 . . no C11 H11 0.9500 . . no C12 H12 0.9500 . . no C13 H13 0.9500 . . no C14 H14A 0.9900 . . no C14 H14B 0.9900 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd1 I1 Pd1 93.23(2) . . 3_656 yes I1 Pd1 I2 178.33(2) . . . yes I1 Pd1 C1 90.65(17) . . . yes I1 Pd1 I1 86.77(2) . . 3_656 yes I2 Pd1 C1 88.85(17) . . . yes I1 Pd1 I2 93.77(2) 3_656 . . yes I1 Pd1 C1 177.01(17) 3_656 . . yes N2 N1 C1 114.2(5) . . . yes N2 N1 C8 116.8(5) . . . yes C1 N1 C8 129.0(5) . . . yes N1 N2 N3 103.2(5) . . . yes N2 N3 C2 112.8(5) . . . yes N2 N3 C7 117.7(5) . . . yes C2 N3 C7 129.6(6) . . . yes Pd1 C1 N1 126.3(4) . . . yes Pd1 C1 C2 130.7(5) . . . yes N1 C1 C2 103.0(5) . . . yes N3 C2 C1 106.8(5) . . . yes N3 C2 C3 122.1(5) . . . yes C1 C2 C3 131.1(6) . . . no C2 C3 C4 115.6(5) . . . no C3 C4 C5 114.5(6) . . . no C4 C5 C6 113.2(6) . . . no N1 C8 C9 119.4(5) . . . yes N1 C8 C13 119.0(5) . . . yes C9 C8 C13 121.6(6) . . . no C8 C9 C10 119.1(6) . . . no C9 C10 C11 119.7(7) . . . no C10 C11 C12 120.2(7) . . . no C11 C12 C13 121.1(6) . . . no C8 C13 C12 118.2(6) . . . no C2 C3 H3A 108.00 . . . no C2 C3 H3B 108.00 . . . no C4 C3 H3A 108.00 . . . no C4 C3 H3B 108.00 . . . no H3A C3 H3B 107.00 . . . no C3 C4 H4A 109.00 . . . no C3 C4 H4B 109.00 . . . no C5 C4 H4A 109.00 . . . no C5 C4 H4B 109.00 . . . no H4A C4 H4B 108.00 . . . no C4 C5 H5A 109.00 . . . no C4 C5 H5B 109.00 . . . no C6 C5 H5A 109.00 . . . no C6 C5 H5B 109.00 . . . no H5A C5 H5B 108.00 . . . no C5 C6 H6A 109.00 . . . no C5 C6 H6B 109.00 . . . no C5 C6 H6C 109.00 . . . no H6A C6 H6B 109.00 . . . no H6A C6 H6C 109.00 . . . no H6B C6 H6C 110.00 . . . no N3 C7 H7A 109.00 . . . no N3 C7 H7B 109.00 . . . no N3 C7 H7C 110.00 . . . no H7A C7 H7B 109.00 . . . no H7A C7 H7C 110.00 . . . no H7B C7 H7C 109.00 . . . no C8 C9 H9 120.00 . . . no C10 C9 H9 120.00 . . . no C9 C10 H10 120.00 . . . no C11 C10 H10 120.00 . . . no C10 C11 H11 120.00 . . . no C12 C11 H11 120.00 . . . no C11 C12 H12 119.00 . . . no C13 C12 H12 119.00 . . . no C8 C13 H13 121.00 . . . no C12 C13 H13 121.00 . . . no Cl1 C14 Cl2 113.0(9) . . . yes Cl1 C14 H14A 109.00 . . . no Cl1 C14 H14B 109.00 . . . no Cl2 C14 H14A 109.00 . . . no Cl2 C14 H14B 109.00 . . . no H14A C14 H14B 108.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 I1 Pd1 C1 178.48(18) 3_656 . . . no Pd1 I1 Pd1 I1 0.00(5) 3_656 . . 3_656 no Pd1 I1 Pd1 I1 0.03(11) . . 3_656 3_656 no Pd1 I1 Pd1 I2 -178.42(2) . . 3_656 3_656 no I1 Pd1 C1 N1 -70.9(5) . . . . no I1 Pd1 C1 C2 107.1(6) . . . . no I2 Pd1 C1 N1 110.7(5) . . . . no I2 Pd1 C1 C2 -71.4(6) . . . . no C1 N1 N2 N3 -0.8(7) . . . . no C8 N1 N2 N3 178.2(5) . . . . no N2 N1 C1 Pd1 178.9(4) . . . . no N2 N1 C1 C2 0.4(7) . . . . no C8 N1 C1 Pd1 0.0(9) . . . . no C8 N1 C1 C2 -178.5(6) . . . . no N2 N1 C8 C9 -36.7(8) . . . . no N2 N1 C8 C13 142.5(6) . . . . no C1 N1 C8 C9 142.2(6) . . . . no C1 N1 C8 C13 -38.7(9) . . . . no N1 N2 N3 C2 0.9(7) . . . . no N1 N2 N3 C7 -178.8(6) . . . . no N2 N3 C2 C1 -0.7(7) . . . . no N2 N3 C2 C3 177.7(6) . . . . no C7 N3 C2 C1 178.9(7) . . . . no C7 N3 C2 C3 -2.7(11) . . . . no Pd1 C1 C2 N3 -178.2(5) . . . . no Pd1 C1 C2 C3 3.6(11) . . . . no N1 C1 C2 N3 0.2(6) . . . . no N1 C1 C2 C3 -178.0(6) . . . . no N3 C2 C3 C4 81.7(8) . . . . no C1 C2 C3 C4 -100.4(8) . . . . no C2 C3 C4 C5 65.1(8) . . . . no C3 C4 C5 C6 64.4(8) . . . . no N1 C8 C9 C10 179.6(6) . . . . no C13 C8 C9 C10 0.5(10) . . . . no N1 C8 C13 C12 -179.9(6) . . . . no C9 C8 C13 C12 -0.7(10) . . . . no C8 C9 C10 C11 -0.3(10) . . . . no C9 C10 C11 C12 0.5(11) . . . . no C10 C11 C12 C13 -0.7(11) . . . . no C11 C12 C13 C8 0.8(10) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag I1 C1 3.287(6) . . no I1 C8 3.846(6) . . no I1 C4 3.875(8) . 4_555 no I1 I1 3.6213(5) . 3_656 no I1 I2 3.8465(6) . 3_656 no I2 C2 3.755(6) . . no I2 C1 3.235(6) . . no I2 I1 3.8465(6) . 3_656 no I1 H3A 3.2300 . 4_555 no I1 H7C 3.0100 . 4_555 no I1 H5A 3.2000 . . no I2 H3B 3.2300 . . no I2 H11 3.3400 . 3_556 no I2 H14A 3.2400 . 3_655 no I2 H10 3.2600 . 4_554 no Pd1 C13 3.289(7) . . no Pd1 H6B 2.9800 . . no Pd1 H13 2.7400 . . no Cl1 N3 3.425(7) . 4_554 no Cl1 N2 3.373(7) . 4_554 no N2 Cl1 3.373(7) . 4_555 no N3 Cl1 3.425(7) . 4_555 no N2 H9 2.5900 . . no C1 I1 3.287(6) . . no C1 I2 3.235(6) . . no C2 C10 3.554(9) . 4_554 no C4 I1 3.875(8) . 4_554 no C6 C7 3.544(10) . 2_645 no C7 C11 3.539(11) . 4_554 no C7 C6 3.544(10) . 2_655 no C8 I1 3.846(6) . . no C10 C2 3.554(9) . 4_555 no C11 C7 3.539(11) . 4_555 no C13 Pd1 3.289(7) . . no C1 H13 2.8500 . . no C2 H5A 2.8500 . . no C3 H7C 2.6800 . . no C3 H6B 2.8200 . . no C4 H7C 3.0600 . . no C6 H7A 3.0500 . 2_645 no C6 H3B 2.7900 . . no C7 H4B 3.1000 . . no C7 H3A 2.8400 . . no C7 H6B 3.0200 . 2_655 no C9 H3A 2.9400 . 4_555 no C9 H14B 3.0200 . 4_455 no C10 H14B 2.9200 . 4_455 no C11 H7A 2.8200 . 4_555 no C11 H4A 3.1000 . 4_455 no C12 H7A 3.0700 . 4_555 no C13 H6C 2.9900 . 1_455 no H3A I1 3.2300 . 4_554 no H3A C9 2.9400 . 4_554 no H3A C7 2.8400 . . no H3A H7C 2.2500 . . no H3B H6B 2.2400 . . no H3B I2 3.2300 . . no H3B C6 2.7900 . . no H4A H11 2.5600 . 4_654 no H4A C11 3.1000 . 4_654 no H4A H6A 2.5400 . . no H4B H7C 2.5200 . . no H4B C7 3.1000 . . no H5A I1 3.2000 . . no H5A C2 2.8500 . . no H6A H4A 2.5400 . . no H6B Pd1 2.9800 . . no H6B C7 3.0200 . 2_645 no H6B C3 2.8200 . . no H6B H3B 2.2400 . . no H6C C13 2.9900 . 1_655 no H6C H13 2.5500 . 1_655 no H7A C11 2.8200 . 4_554 no H7A C6 3.0500 . 2_655 no H7A C12 3.0700 . 4_554 no H7C H3A 2.2500 . . no H7C H4B 2.5200 . . no H7C C4 3.0600 . . no H7C C3 2.6800 . . no H7C I1 3.0100 . 4_554 no H9 N2 2.5900 . . no H10 I2 3.2600 . 4_555 no H11 H4A 2.5600 . 4_455 no H11 I2 3.3400 . 3_556 no H12 H13 2.5200 . 3_556 no H13 Pd1 2.7400 . . no H13 H12 2.5200 . 3_556 no H13 C1 2.8500 . . no H13 H6C 2.5500 . 1_455 no H14A I2 3.2400 . 3_655 no H14B C9 3.0200 . 4_654 no H14B C10 2.9200 . 4_654 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C7 H7C I1 0.9800 3.0100 3.953(8) 162.00 4_554 yes _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.373 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.161 #################################################END data_complex-2e _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H34 I4 N6 Pd2, 2(C H2 Cl2)' _chemical_formula_sum 'C28 H38 Cl4 I4 N6 Pd2' _chemical_formula_weight 1320.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.9204(14) _cell_length_b 10.5994(13) _cell_length_c 10.5337(14) _cell_angle_alpha 91.475(11) _cell_angle_beta 94.257(11) _cell_angle_gamma 112.019(10) _cell_volume 1022.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7261 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 25.55 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 4.188 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.308 _exptl_absorpt_correction_T_max 0.576 _exptl_absorpt_process_details 'DELrefABS in PLATON; Spek, 2009' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7810 _diffrn_reflns_av_R_equivalents 0.1113 _diffrn_reflns_av_sigmaI/netI 0.1079 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.19 _reflns_number_total 3523 _reflns_number_gt 2254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1962P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3523 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2832 _refine_ls_wR_factor_gt 0.2291 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I1 I Uani 0.21642(11) 0.40105(10) 0.16849(10) 1.000 0.0574(4) . . I2 I Uani 0.39011(11) 0.31775(9) 0.47119(10) 1.000 0.0538(4) . . Pd1 Pd Uani 0.40937(11) 0.54027(9) 0.35073(10) 1.000 0.0463(4) . . N1 N Uani 0.5156(12) 0.7617(11) 0.1716(11) 1.000 0.047(3) . . N2 N Uani 0.5184(13) 0.8817(11) 0.1344(12) 1.000 0.053(4) . . N3 N Uani 0.4343(12) 0.9117(11) 0.2145(11) 1.000 0.045(4) . . C1 C Uani 0.4250(15) 0.7091(13) 0.2665(15) 1.000 0.051(5) . . C2 C Uani 0.3759(15) 0.8101(12) 0.2946(15) 1.000 0.048(4) . . C3 C Uani 0.4115(16) 1.0382(13) 0.1940(17) 1.000 0.058(5) . . C4 C Uani 0.2744(15) 0.8134(14) 0.3892(15) 1.000 0.054(5) . . C5 C Uani 0.2947(17) 0.9277(15) 0.4661(15) 1.000 0.057(5) . . C6 C Uani 0.194(2) 0.9265(19) 0.5490(19) 1.000 0.077(7) . . C7 C Uani 0.0695(19) 0.8117(16) 0.5615(19) 1.000 0.073(7) . . C8 C Uani 0.051(2) 0.6962(17) 0.4838(18) 1.000 0.072(6) . . C9 C Uani 0.1503(17) 0.6970(15) 0.3967(15) 1.000 0.056(5) . . C10 C Uani 0.6051(15) 0.6994(15) 0.1122(14) 1.000 0.051(5) . . C11 C Uani 0.7646(15) 0.7551(15) 0.1642(15) 1.000 0.055(5) . . C12 C Uani 0.8504(17) 0.8975(15) 0.1386(14) 1.000 0.057(5) . . C13 C Uani 1.0054(16) 0.9426(16) 0.1977(19) 1.000 0.067(6) . . Cl8 Cl Uani 0.6891(7) 0.3952(5) 0.2331(8) 1.000 0.112(3) . . Cl9 Cl Uani 0.7884(6) 0.2318(7) 0.0675(7) 1.000 0.107(2) . . C14 C Uani 0.826(2) 0.3896(18) 0.145(2) 1.000 0.087(8) . . H3A H Uiso 0.47460 1.10920 0.25710 1.000 0.0870 calc R H3B H Uiso 0.30910 1.02330 0.20300 1.000 0.0870 calc R H3C H Uiso 0.43550 1.06680 0.10800 1.000 0.0870 calc R H5 H Uiso 0.37920 1.00790 0.46150 1.000 0.0850 calc R H6 H Uiso 0.20980 1.00710 0.59960 1.000 0.1160 calc R H7 H Uiso 0.00080 0.81150 0.61970 1.000 0.1100 calc R H8 H Uiso -0.03210 0.61500 0.49050 1.000 0.1080 calc R H9 H Uiso 0.13320 0.61830 0.34290 1.000 0.0840 calc R H10A H Uiso 0.59960 0.71240 0.01950 1.000 0.0770 calc R H10B H Uiso 0.56340 0.60010 0.12360 1.000 0.0770 calc R H11A H Uiso 0.76920 0.74690 0.25760 1.000 0.0820 calc R H11B H Uiso 0.81180 0.69670 0.12790 1.000 0.0820 calc R H12A H Uiso 0.80410 0.95740 0.17330 1.000 0.0860 calc R H12B H Uiso 0.85090 0.90670 0.04530 1.000 0.0860 calc R H13A H Uiso 1.05420 0.88880 0.15800 1.000 0.1010 calc R H13B H Uiso 1.00510 0.92910 0.28940 1.000 0.1010 calc R H13C H Uiso 1.05760 1.03940 0.18430 1.000 0.1010 calc R H14A H Uiso 0.91670 0.41420 0.20180 1.000 0.1050 calc R H14B H Uiso 0.84270 0.45890 0.08020 1.000 0.1050 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0588(7) 0.0474(6) 0.0624(7) -0.0052(5) 0.0106(5) 0.0156(5) I2 0.0671(7) 0.0312(6) 0.0604(7) 0.0027(4) 0.0079(5) 0.0150(5) Pd1 0.0529(7) 0.0321(7) 0.0554(8) 0.0022(5) 0.0140(5) 0.0161(5) N1 0.054(6) 0.041(6) 0.048(6) -0.011(5) 0.008(5) 0.020(5) N2 0.067(7) 0.042(6) 0.056(7) 0.006(6) 0.015(6) 0.026(6) N3 0.048(6) 0.034(6) 0.054(7) -0.002(5) 0.009(5) 0.016(5) C1 0.056(8) 0.031(7) 0.064(9) 0.008(7) 0.018(7) 0.012(6) C2 0.057(8) 0.023(6) 0.065(9) -0.007(6) 0.008(7) 0.016(6) C3 0.065(9) 0.036(7) 0.088(11) 0.021(8) 0.043(8) 0.027(7) C4 0.054(8) 0.045(8) 0.068(9) 0.007(7) 0.017(7) 0.023(7) C5 0.070(9) 0.044(8) 0.061(9) -0.010(7) 0.024(8) 0.025(7) C6 0.100(13) 0.069(11) 0.077(12) -0.011(10) 0.026(11) 0.046(11) C7 0.078(11) 0.046(9) 0.104(14) 0.011(9) 0.057(11) 0.025(9) C8 0.085(11) 0.051(9) 0.080(12) -0.003(9) 0.033(10) 0.020(9) C9 0.072(9) 0.044(8) 0.057(9) 0.007(7) 0.036(8) 0.021(7) C10 0.064(8) 0.049(8) 0.050(8) 0.002(7) 0.023(7) 0.028(7) C11 0.050(8) 0.051(8) 0.065(9) 0.007(7) 0.027(7) 0.017(7) C12 0.070(9) 0.054(9) 0.045(8) 0.009(7) 0.019(7) 0.018(8) C13 0.049(8) 0.049(9) 0.096(13) -0.001(9) 0.008(8) 0.011(7) Cl8 0.098(4) 0.063(3) 0.183(7) 0.019(4) 0.063(4) 0.030(3) Cl9 0.089(3) 0.099(4) 0.126(5) -0.038(4) -0.012(3) 0.036(3) C14 0.082(12) 0.058(11) 0.132(18) 0.034(12) 0.047(12) 0.029(10) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd1 2.5918(15) . . yes I2 Pd1 2.6574(14) . . yes I2 Pd1 2.6070(15) . 2_666 yes Pd1 C1 1.977(14) . . yes Cl8 C14 1.72(2) . . yes Cl9 C14 1.74(2) . . yes N1 C10 1.46(2) . . yes N1 N2 1.332(16) . . yes N1 C1 1.380(19) . . yes N2 N3 1.341(18) . . yes N3 C2 1.363(18) . . yes N3 C3 1.460(18) . . yes C1 C2 1.37(2) . . no C2 C4 1.48(2) . . no C4 C5 1.38(2) . . no C4 C9 1.39(2) . . no C5 C6 1.37(3) . . no C6 C7 1.39(3) . . no C7 C8 1.40(2) . . no C8 C9 1.39(3) . . no C10 C11 1.52(2) . . no C11 C12 1.47(2) . . no C12 C13 1.51(2) . . no C3 H3B 0.9800 . . no C3 H3A 0.9800 . . no C3 H3C 0.9800 . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7 0.9500 . . no C8 H8 0.9500 . . no C9 H9 0.9500 . . no C10 H10B 0.9900 . . no C10 H10A 0.9900 . . no C11 H11B 0.9900 . . no C11 H11A 0.9900 . . no C12 H12B 0.9900 . . no C12 H12A 0.9900 . . no C13 H13C 0.9800 . . no C13 H13A 0.9800 . . no C13 H13B 0.9800 . . no C14 H14A 0.9900 . . no C14 H14B 0.9900 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd1 I2 Pd1 91.83(4) . . 2_666 yes I1 Pd1 I2 92.52(4) . . . yes I1 Pd1 C1 89.0(4) . . . yes I1 Pd1 I2 178.14(6) . . 2_666 yes I2 Pd1 C1 178.2(4) . . . yes I2 Pd1 I2 88.17(5) . . 2_666 yes I2 Pd1 C1 90.3(4) 2_666 . . yes N2 N1 C1 114.4(12) . . . yes N2 N1 C10 119.2(12) . . . yes C1 N1 C10 126.4(11) . . . yes N1 N2 N3 102.8(11) . . . yes N2 N3 C2 112.2(11) . . . yes N2 N3 C3 115.8(11) . . . yes C2 N3 C3 131.8(13) . . . yes Pd1 C1 N1 123.8(11) . . . yes Pd1 C1 C2 132.3(12) . . . yes N1 C1 C2 103.1(12) . . . yes N3 C2 C1 107.4(13) . . . yes N3 C2 C4 123.8(12) . . . yes C1 C2 C4 128.8(13) . . . no C2 C4 C5 123.2(13) . . . no C2 C4 C9 117.8(13) . . . no C5 C4 C9 119.1(15) . . . no C4 C5 C6 120.7(15) . . . no C5 C6 C7 122.4(17) . . . no C6 C7 C8 116.4(18) . . . no C7 C8 C9 121.9(16) . . . no C4 C9 C8 119.6(14) . . . no N1 C10 C11 114.7(12) . . . yes C10 C11 C12 116.2(13) . . . no C11 C12 C13 111.4(13) . . . no N3 C3 H3A 109.00 . . . no N3 C3 H3B 109.00 . . . no N3 C3 H3C 109.00 . . . no H3A C3 H3B 110.00 . . . no H3A C3 H3C 110.00 . . . no H3B C3 H3C 109.00 . . . no C4 C5 H5 120.00 . . . no C6 C5 H5 120.00 . . . no C5 C6 H6 119.00 . . . no C7 C6 H6 119.00 . . . no C6 C7 H7 122.00 . . . no C8 C7 H7 122.00 . . . no C7 C8 H8 119.00 . . . no C9 C8 H8 119.00 . . . no C4 C9 H9 120.00 . . . no C8 C9 H9 120.00 . . . no N1 C10 H10A 109.00 . . . no N1 C10 H10B 109.00 . . . no C11 C10 H10A 109.00 . . . no C11 C10 H10B 109.00 . . . no H10A C10 H10B 108.00 . . . no C10 C11 H11A 108.00 . . . no C10 C11 H11B 108.00 . . . no C12 C11 H11A 108.00 . . . no C12 C11 H11B 108.00 . . . no H11A C11 H11B 107.00 . . . no C11 C12 H12A 109.00 . . . no C11 C12 H12B 109.00 . . . no C13 C12 H12A 109.00 . . . no C13 C12 H12B 109.00 . . . no H12A C12 H12B 108.00 . . . no C12 C13 H13A 110.00 . . . no C12 C13 H13B 109.00 . . . no C12 C13 H13C 109.00 . . . no H13A C13 H13B 110.00 . . . no H13A C13 H13C 110.00 . . . no H13B C13 H13C 109.00 . . . no Cl8 C14 Cl9 113.9(11) . . . yes Cl8 C14 H14A 109.00 . . . no Cl8 C14 H14B 109.00 . . . no Cl9 C14 H14A 109.00 . . . no Cl9 C14 H14B 109.00 . . . no H14A C14 H14B 108.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 I2 Pd1 I1 178.28(5) 2_666 . . . no Pd1 I2 Pd1 I2 -0.02(9) 2_666 . . 2_666 no Pd1 I2 Pd1 I2 0.00(5) . . 2_666 2_666 no Pd1 I2 Pd1 C1 -179.0(5) . . 2_666 2_666 no I1 Pd1 C1 N1 -85.9(12) . . . . no I1 Pd1 C1 C2 106.0(15) . . . . no I2 Pd1 C1 N1 92.4(12) 2_666 . . . no I2 Pd1 C1 C2 -75.8(15) 2_666 . . . no C1 N1 N2 N3 4.3(15) . . . . no C10 N1 N2 N3 -175.4(12) . . . . no N2 N1 C1 Pd1 -175.1(10) . . . . no N2 N1 C1 C2 -4.0(17) . . . . no C10 N1 C1 Pd1 5(2) . . . . no C10 N1 C1 C2 175.6(13) . . . . no N2 N1 C10 C11 80.5(16) . . . . no C1 N1 C10 C11 -99.1(17) . . . . no N1 N2 N3 C2 -2.8(15) . . . . no N1 N2 N3 C3 -177.8(12) . . . . no N2 N3 C2 C1 0.5(17) . . . . no N2 N3 C2 C4 -177.5(13) . . . . no C3 N3 C2 C1 174.5(15) . . . . no C3 N3 C2 C4 -4(2) . . . . no Pd1 C1 C2 N3 171.9(11) . . . . no Pd1 C1 C2 C4 -10(3) . . . . no N1 C1 C2 N3 1.9(16) . . . . no N1 C1 C2 C4 179.8(15) . . . . no N3 C2 C4 C5 -44(2) . . . . no N3 C2 C4 C9 133.8(16) . . . . no C1 C2 C4 C5 138.8(17) . . . . no C1 C2 C4 C9 -44(2) . . . . no C2 C4 C5 C6 177.6(16) . . . . no C9 C4 C5 C6 0(2) . . . . no C2 C4 C9 C8 -179.4(15) . . . . no C5 C4 C9 C8 -2(2) . . . . no C4 C5 C6 C7 1(3) . . . . no C5 C6 C7 C8 -1(3) . . . . no C6 C7 C8 C9 -1(3) . . . . no C7 C8 C9 C4 3(3) . . . . no N1 C10 C11 C12 -67.0(17) . . . . no C10 C11 C12 C13 178.4(14) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag I1 I2 3.7928(16) . . no I1 C1 3.233(13) . . no I1 C14 3.82(2) . 1_455 no I1 C10 3.878(15) . 2_665 no I2 Cl8 3.892(8) . . no I2 C5 3.878(15) . 1_545 no I2 I1 3.7928(16) . . no I2 I2 3.6627(14) . 2_666 no I2 C1 3.280(16) . 2_666 no I2 C2 3.872(15) . 2_666 no I1 H9 3.2900 . . no I1 H10B 3.3700 . . no I1 H14A 3.0700 . 1_455 no I1 H14B 3.1700 . 2_665 no I1 H10A 3.2800 . 2_665 no I1 H11B 3.2200 . 2_665 no I2 H5 3.2400 . 1_545 no I2 H11A 3.3300 . 2_666 no Pd1 H10B 2.8900 . . no Cl8 I2 3.892(8) . . no Cl9 N2 3.376(15) . 2_665 no Cl8 H3A 3.0100 . 1_545 no Cl8 H10B 3.0900 . . no N2 C12 3.23(2) . . no N2 Cl9 3.376(15) . 2_665 no N1 H12A 2.8300 . . no N2 H12A 2.6400 . . no N2 H3C 2.6600 . 2_675 no N3 H5 2.9300 . . no C1 I2 3.280(16) . 2_666 no C1 I1 3.233(13) . . no C3 C5 3.25(2) . . no C5 C3 3.25(2) . . no C5 I2 3.878(15) . 1_565 no C10 I1 3.878(15) . 2_665 no C12 N2 3.23(2) . . no C14 I1 3.82(2) . 1_655 no C1 H9 2.8700 . . no C3 H5 2.8700 . . no C4 H3B 2.9400 . . no C5 H5 3.0800 . 2_676 no C5 H3B 2.9700 . . no C12 H6 3.0900 . 2_676 no C13 H3B 2.8000 . 1_655 no H3A H5 2.5200 . . no H3A Cl8 3.0100 . 1_565 no H3B C5 2.9700 . . no H3B C4 2.9400 . . no H3B H13C 2.5600 . 1_455 no H3B C13 2.8000 . 1_455 no H3B H13A 2.3900 . 1_455 no H3C N2 2.6600 . 2_675 no H5 C3 2.8700 . . no H5 H3A 2.5200 . . no H5 C5 3.0800 . 2_676 no H5 N3 2.9300 . . no H5 I2 3.2400 . 1_565 no H5 H5 2.5400 . 2_676 no H6 C12 3.0900 . 2_676 no H6 H12A 2.4300 . 2_676 no H9 C1 2.8700 . . no H9 I1 3.2900 . . no H10A I1 3.2800 . 2_665 no H10A H12B 2.5600 . . no H10B I1 3.3700 . . no H10B Pd1 2.8900 . . no H10B Cl8 3.0900 . . no H11A I2 3.3300 . 2_666 no H11A H13B 2.4000 . . no H11B I1 3.2200 . 2_665 no H11B H13A 2.4900 . . no H12A N1 2.8300 . . no H12A H6 2.4300 . 2_676 no H12A N2 2.6400 . . no H12B H10A 2.5600 . . no H13A H11B 2.4900 . . no H13A H3B 2.3900 . 1_655 no H13B H11A 2.4000 . . no H13C H3B 2.5600 . 1_655 no H14A I1 3.0700 . 1_655 no H14B I1 3.1700 . 2_665 no _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.504 _refine_diff_density_min -2.569 _refine_diff_density_rms 0.356 #################################################END data_complex-trans3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 I2 N6 Pd' _chemical_formula_sum 'C22 H26 I2 N6 Pd' _chemical_formula_weight 734.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 9.6971(7) _cell_length_b 13.6009(12) _cell_length_c 9.4707(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.490(6) _cell_angle_gamma 90.00 _cell_volume 1203.71(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14119 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 26.15 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3014 _exptl_absorpt_correction_T_max 0.5997 _exptl_absorpt_process_details 'MULscanABS in PLATON; Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-2' _diffrn_measurement_method 'phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10308 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.65 _reflns_number_total 2268 _reflns_number_gt 2014 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area V1.35 (Stoe & Cie, 2006)' _computing_cell_refinement 'X-Area V1.35' _computing_data_reduction 'X-RED32 V1.31 (Stoe & Cie, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) & PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0048(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2268 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 #================================================================ # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I1 I Uani 0.66270(2) -0.13975(1) 0.64631(2) 1.000 0.0343(1) . . Pd1 Pd Uani 0.50000 0.00000 0.50000 1.000 0.0223(1) . . N1 N Uani 0.7014(3) 0.16189(19) 0.6399(3) 1.000 0.0279(7) . . N2 N Uani 0.8214(3) 0.21219(19) 0.6512(3) 1.000 0.0315(8) . . N3 N Uani 0.8721(3) 0.17435(18) 0.5473(3) 1.000 0.0283(7) . . C1 C Uani 0.6729(3) 0.0922(2) 0.5343(3) 1.000 0.0259(8) . . C2 C Uani 0.7866(3) 0.1008(2) 0.4710(3) 1.000 0.0252(8) . . C3 C Uani 0.8126(3) 0.0469(2) 0.3456(3) 1.000 0.0268(8) . . C4 C Uani 0.9459(3) 0.0385(2) 0.3173(3) 1.000 0.0323(9) . . C5 C Uani 0.9614(4) -0.0139(3) 0.1973(4) 1.000 0.0380(11) . . C6 C Uani 0.8461(4) -0.0606(3) 0.1048(4) 1.000 0.0428(11) . . C7 C Uani 0.7126(4) -0.0535(3) 0.1317(4) 1.000 0.0441(11) . . C8 C Uani 0.6954(4) 0.0001(2) 0.2500(4) 1.000 0.0355(10) . . C9 C Uani 1.0071(4) 0.2168(3) 0.5331(4) 1.000 0.0386(10) . . C10 C Uani 0.6154(4) 0.1884(2) 0.7401(4) 1.000 0.0360(10) . . C11 C Uani 0.6590(5) 0.1296(3) 0.8789(4) 1.000 0.0484(12) . . H4 H Uiso 1.02690 0.06910 0.38110 1.000 0.0390 calc R H5 H Uiso 1.05270 -0.01770 0.17840 1.000 0.0460 calc R H6 H Uiso 0.85790 -0.09730 0.02340 1.000 0.0510 calc R H7 H Uiso 0.63270 -0.08570 0.06850 1.000 0.0530 calc R H8 H Uiso 0.60330 0.00520 0.26670 1.000 0.0430 calc R H9A H Uiso 1.02720 0.27780 0.59010 1.000 0.0460 calc R H9B H Uiso 1.08510 0.16990 0.57000 1.000 0.0460 calc R H9C H Uiso 0.99900 0.23110 0.42980 1.000 0.0460 calc R H10A H Uiso 0.51300 0.17650 0.69160 1.000 0.0430 calc R H10B H Uiso 0.62760 0.25940 0.76380 1.000 0.0430 calc R H11A H Uiso 0.64010 0.05980 0.85630 1.000 0.0580 calc R H11B H Uiso 0.76140 0.13920 0.92470 1.000 0.0580 calc R H11C H Uiso 0.60420 0.15150 0.94620 1.000 0.0580 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0233(2) 0.0336(2) 0.0453(2) 0.0067(1) 0.0077(1) 0.0005(1) Pd1 0.0165(2) 0.0246(2) 0.0270(2) -0.0026(1) 0.0082(1) -0.0027(1) N1 0.0223(13) 0.0286(12) 0.0327(13) -0.0034(10) 0.0071(10) -0.0030(11) N2 0.0252(13) 0.0317(13) 0.0379(14) -0.0036(11) 0.0091(11) -0.0051(11) N3 0.0223(13) 0.0278(12) 0.0339(13) 0.0019(10) 0.0060(10) -0.0042(10) C1 0.0213(14) 0.0274(14) 0.0291(14) 0.0019(12) 0.0067(11) 0.0053(12) C2 0.0188(14) 0.0239(13) 0.0303(15) 0.0034(11) 0.0023(11) -0.0004(11) C3 0.0237(15) 0.0275(14) 0.0297(15) 0.0046(11) 0.0080(12) 0.0019(12) C4 0.0250(16) 0.0357(16) 0.0369(16) 0.0057(13) 0.0096(13) 0.0043(13) C5 0.0329(18) 0.0454(18) 0.0420(19) 0.0127(14) 0.0208(15) 0.0123(15) C6 0.050(2) 0.0470(19) 0.0375(17) -0.0019(15) 0.0222(16) 0.0095(17) C7 0.042(2) 0.051(2) 0.0396(19) -0.0131(16) 0.0115(15) -0.0029(17) C8 0.0280(17) 0.0422(19) 0.0387(18) -0.0057(13) 0.0133(14) -0.0049(13) C9 0.0276(17) 0.0429(18) 0.0479(18) 0.0001(15) 0.0146(14) -0.0138(15) C10 0.0317(17) 0.0385(17) 0.0407(17) -0.0142(14) 0.0149(14) -0.0064(14) C11 0.050(2) 0.058(2) 0.040(2) -0.0092(16) 0.0169(17) -0.0110(18) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd1 2.6181(3) . . yes Pd1 C1 2.049(3) . . yes Pd1 C1 2.049(3) . 3_656 yes N1 N2 1.329(4) . . yes N1 C1 1.352(4) . . yes N1 C10 1.466(5) . . yes N2 N3 1.317(4) . . yes N3 C2 1.375(4) . . yes N3 C9 1.469(5) . . yes C1 C2 1.394(4) . . no C2 C3 1.474(4) . . no C3 C4 1.393(4) . . no C3 C8 1.403(5) . . no C4 C5 1.383(5) . . no C5 C6 1.378(6) . . no C6 C7 1.388(6) . . no C7 C8 1.384(5) . . no C10 C11 1.500(5) . . no C4 H4 0.9500 . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7 0.9500 . . no C8 H8 0.9500 . . no C9 H9A 0.9800 . . no C9 H9B 0.9800 . . no C9 H9C 0.9800 . . no C10 H10A 0.9900 . . no C10 H10B 0.9900 . . no C11 H11A 0.9800 . . no C11 H11B 0.9800 . . no C11 H11C 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Pd1 C1 90.49(8) . . . yes I1 Pd1 I1 180.00 . . 3_656 yes I1 Pd1 C1 89.51(8) . . 3_656 yes I1 Pd1 C1 89.51(8) 3_656 . . yes C1 Pd1 C1 180.00 . . 3_656 yes I1 Pd1 C1 90.49(8) 3_656 . 3_656 yes N2 N1 C1 115.0(3) . . . yes N2 N1 C10 117.3(3) . . . yes C1 N1 C10 127.8(3) . . . yes N1 N2 N3 103.4(2) . . . yes N2 N3 C2 112.6(3) . . . yes N2 N3 C9 115.8(3) . . . yes C2 N3 C9 131.7(3) . . . yes Pd1 C1 N1 122.9(2) . . . yes Pd1 C1 C2 133.7(2) . . . yes N1 C1 C2 103.3(3) . . . yes N3 C2 C1 105.7(2) . . . yes N3 C2 C3 125.2(3) . . . yes C1 C2 C3 129.1(3) . . . no C2 C3 C4 124.3(3) . . . no C2 C3 C8 117.6(3) . . . no C4 C3 C8 118.2(3) . . . no C3 C4 C5 120.7(3) . . . no C4 C5 C6 120.8(4) . . . no C5 C6 C7 119.3(4) . . . no C6 C7 C8 120.4(4) . . . no C3 C8 C7 120.7(4) . . . no N1 C10 C11 111.1(3) . . . yes C3 C4 H4 120.00 . . . no C5 C4 H4 120.00 . . . no C4 C5 H5 120.00 . . . no C6 C5 H5 120.00 . . . no C5 C6 H6 120.00 . . . no C7 C6 H6 120.00 . . . no C6 C7 H7 120.00 . . . no C8 C7 H7 120.00 . . . no C3 C8 H8 120.00 . . . no C7 C8 H8 120.00 . . . no N3 C9 H9A 109.00 . . . no N3 C9 H9B 109.00 . . . no N3 C9 H9C 109.00 . . . no H9A C9 H9B 109.00 . . . no H9A C9 H9C 109.00 . . . no H9B C9 H9C 109.00 . . . no N1 C10 H10A 109.00 . . . no N1 C10 H10B 109.00 . . . no C11 C10 H10A 109.00 . . . no C11 C10 H10B 109.00 . . . no H10A C10 H10B 108.00 . . . no C10 C11 H11A 109.00 . . . no C10 C11 H11B 109.00 . . . no C10 C11 H11C 109.00 . . . no H11A C11 H11B 110.00 . . . no H11A C11 H11C 110.00 . . . no H11B C11 H11C 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I1 Pd1 C1 N1 -99.4(2) . . . . no I1 Pd1 C1 C2 77.9(3) . . . . no I1 Pd1 C1 N1 80.6(2) 3_656 . . . no I1 Pd1 C1 C2 -102.1(3) 3_656 . . . no C1 N1 N2 N3 0.8(3) . . . . no C10 N1 N2 N3 -178.5(3) . . . . no N2 N1 C1 Pd1 177.1(2) . . . . no N2 N1 C1 C2 -1.0(3) . . . . no C10 N1 C1 Pd1 -3.7(4) . . . . no C10 N1 C1 C2 178.2(3) . . . . no N2 N1 C10 C11 -90.2(3) . . . . no C1 N1 C10 C11 90.6(4) . . . . no N1 N2 N3 C2 -0.3(3) . . . . no N1 N2 N3 C9 179.8(3) . . . . no N2 N3 C2 C1 -0.3(3) . . . . no N2 N3 C2 C3 177.9(3) . . . . no C9 N3 C2 C1 179.6(3) . . . . no C9 N3 C2 C3 -2.2(5) . . . . no Pd1 C1 C2 N3 -177.0(2) . . . . no Pd1 C1 C2 C3 4.9(5) . . . . no N1 C1 C2 N3 0.7(3) . . . . no N1 C1 C2 C3 -177.4(3) . . . . no N3 C2 C3 C4 22.4(4) . . . . no N3 C2 C3 C8 -158.5(3) . . . . no C1 C2 C3 C4 -159.9(3) . . . . no C1 C2 C3 C8 19.3(4) . . . . no C2 C3 C4 C5 179.7(3) . . . . no C8 C3 C4 C5 0.6(4) . . . . no C2 C3 C8 C7 -178.7(3) . . . . no C4 C3 C8 C7 0.5(4) . . . . no C3 C4 C5 C6 -1.3(5) . . . . no C4 C5 C6 C7 1.0(6) . . . . no C5 C6 C7 C8 0.1(6) . . . . no C6 C7 C8 C3 -0.9(5) . . . . no _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.589 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.112 #################################################END data_complex_cis3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 I2 N6 Pd' _chemical_formula_sum 'C22 H26 I2 N6 Pd' _chemical_formula_weight 734.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 9.5874(7) _cell_length_b 13.4276(9) _cell_length_c 19.6702(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.350(8) _cell_angle_gamma 90.00 _cell_volume 2473.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 26.0 _exptl_crystal_description plate _exptl_crystal_colour pale_yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 3.268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3344 _exptl_absorpt_correction_T_max 0.6133 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'phi rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12387 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4790 _reflns_number_gt 3582 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'EXPOSE in IPDS-I (Stoe & Cie, 2000)' _computing_cell_refinement 'CELL in IPDS-I (Stoe & Cie, 2000)' _computing_data_reduction 'INTEGRATE in IPDS-I (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00085(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4790 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I1 I Uani 0.85360(4) 0.07962(2) 0.25131(2) 1.000 0.0332(1) . . I2 I Uani 0.76041(4) 0.20508(3) 0.41496(2) 1.000 0.0331(1) . . Pd1 Pd Uani 0.88475(4) 0.25718(3) 0.31153(2) 1.000 0.0226(1) . . N1 N Uani 0.8264(5) 0.4688(3) 0.3458(2) 1.000 0.0297(12) . . N2 N Uani 0.8781(5) 0.5531(3) 0.3776(3) 1.000 0.0339(14) . . N3 N Uani 1.0100(5) 0.5288(3) 0.4075(2) 1.000 0.0295(12) . . N4 N Uani 1.1117(4) 0.2865(3) 0.2298(2) 1.000 0.0257(12) . . N5 N Uani 1.1457(5) 0.3239(3) 0.1725(2) 1.000 0.0303(12) . . N6 N Uani 1.0267(5) 0.3661(3) 0.1397(2) 1.000 0.0304(12) . . C1 C Uani 0.9216(5) 0.3923(4) 0.3535(3) 1.000 0.0234(12) . . C2 C Uani 1.0435(5) 0.4335(4) 0.3954(3) 1.000 0.0268(17) . . C3 C Uani 1.1800(5) 0.3864(4) 0.4265(3) 1.000 0.0283(17) . . C4 C Uani 1.1773(6) 0.2918(4) 0.4551(3) 1.000 0.0352(17) . . C5 C Uani 1.3025(6) 0.2443(5) 0.4862(3) 1.000 0.0409(17) . . C6 C Uani 1.4314(6) 0.2899(5) 0.4885(3) 1.000 0.0419(19) . . C7 C Uani 1.4354(6) 0.3822(6) 0.4598(4) 1.000 0.050(2) . . C8 C Uani 1.3099(6) 0.4310(5) 0.4288(3) 1.000 0.0387(19) . . C9 C Uani 1.0989(7) 0.6078(5) 0.4464(3) 1.000 0.047(2) . . C10 C Uani 0.6763(6) 0.4677(5) 0.3076(3) 1.000 0.0422(19) . . C11 C Uani 0.5866(7) 0.5447(6) 0.3344(5) 1.000 0.060(3) . . C12 C Uani 0.9736(5) 0.3027(4) 0.2339(3) 1.000 0.0260(16) . . C13 C Uani 0.9186(5) 0.3561(4) 0.1746(3) 1.000 0.0270(17) . . C14 C Uani 0.7730(6) 0.3946(4) 0.1496(3) 1.000 0.0298(17) . . C15 C Uani 0.6582(6) 0.3328(4) 0.1531(3) 1.000 0.0338(17) . . C16 C Uani 0.5191(6) 0.3678(5) 0.1347(3) 1.000 0.0391(17) . . C17 C Uani 0.4935(7) 0.4654(5) 0.1126(3) 1.000 0.0462(19) . . C18 C Uani 0.6062(7) 0.5265(5) 0.1080(4) 1.000 0.050(2) . . C19 C Uani 0.7457(6) 0.4929(4) 0.1268(3) 1.000 0.0396(19) . . C20 C Uani 1.0308(7) 0.4193(5) 0.0755(3) 1.000 0.0412(19) . . C21 C Uani 1.2193(6) 0.2291(4) 0.2776(3) 1.000 0.0344(17) . . C22 C Uani 1.3663(7) 0.2714(6) 0.2846(4) 1.000 0.063(3) . . H4 H Uiso 1.08840 0.25950 0.45320 1.000 0.0420 calc R H5 H Uiso 1.29940 0.18000 0.50610 1.000 0.0490 calc R H6 H Uiso 1.51770 0.25740 0.50990 1.000 0.0510 calc R H7 H Uiso 1.52480 0.41340 0.46090 1.000 0.0600 calc R H8 H Uiso 1.31400 0.49530 0.40920 1.000 0.0460 calc R H9A H Uiso 1.16160 0.63540 0.41770 1.000 0.0560 calc R H9B H Uiso 1.03750 0.66070 0.45800 1.000 0.0560 calc R H9C H Uiso 1.15700 0.58010 0.48930 1.000 0.0560 calc R H10A H Uiso 0.63550 0.40080 0.31180 1.000 0.0510 calc R H10B H Uiso 0.67270 0.48020 0.25770 1.000 0.0510 calc R H11A H Uiso 0.62650 0.61110 0.33040 1.000 0.0720 calc R H11B H Uiso 0.58640 0.53090 0.38330 1.000 0.0720 calc R H11C H Uiso 0.48850 0.54210 0.30690 1.000 0.0720 calc R H15 H Uiso 0.67530 0.26580 0.16830 1.000 0.0410 calc R H16 H Uiso 0.44150 0.32500 0.13710 1.000 0.0470 calc R H17 H Uiso 0.39850 0.49000 0.10080 1.000 0.0560 calc R H18 H Uiso 0.58810 0.59280 0.09160 1.000 0.0590 calc R H19 H Uiso 0.82270 0.53640 0.12420 1.000 0.0470 calc R H20A H Uiso 1.05570 0.48920 0.08620 1.000 0.0490 calc R H20B H Uiso 1.10260 0.38890 0.05320 1.000 0.0490 calc R H20C H Uiso 0.93690 0.41560 0.04390 1.000 0.0490 calc R H21A H Uiso 1.21860 0.15960 0.26060 1.000 0.0420 calc R H21B H Uiso 1.19470 0.22770 0.32400 1.000 0.0420 calc R H22A H Uiso 1.36430 0.34290 0.29420 1.000 0.0760 calc R H22B H Uiso 1.39890 0.26070 0.24130 1.000 0.0760 calc R H22C H Uiso 1.43170 0.23820 0.32300 1.000 0.0760 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0410(2) 0.0197(2) 0.0364(2) -0.0041(1) 0.0028(2) -0.0020(1) I2 0.0306(2) 0.0336(2) 0.0350(2) -0.0013(2) 0.0072(1) -0.0061(1) Pd1 0.0217(2) 0.0182(2) 0.0259(2) -0.0011(1) 0.0003(2) -0.0011(1) N1 0.032(2) 0.023(2) 0.033(2) -0.0025(19) 0.0044(19) 0.0016(19) N2 0.034(2) 0.024(2) 0.043(3) -0.0101(19) 0.007(2) -0.0001(19) N3 0.033(2) 0.022(2) 0.032(2) -0.0078(18) 0.0036(19) -0.0050(18) N4 0.025(2) 0.018(2) 0.033(2) -0.0023(17) 0.0039(18) 0.0008(17) N5 0.028(2) 0.030(2) 0.032(2) -0.0012(19) 0.0045(19) -0.0008(19) N6 0.034(2) 0.029(2) 0.027(2) -0.0009(18) 0.0038(19) -0.0067(19) C1 0.026(2) 0.021(2) 0.023(2) -0.0026(19) 0.005(2) -0.001(2) C2 0.028(3) 0.024(3) 0.028(3) -0.003(2) 0.005(2) -0.003(2) C3 0.029(3) 0.033(3) 0.021(3) -0.004(2) 0.001(2) -0.003(2) C4 0.031(3) 0.035(3) 0.038(3) -0.001(2) 0.004(2) 0.001(2) C5 0.037(3) 0.045(3) 0.040(3) 0.009(3) 0.007(3) 0.006(3) C6 0.030(3) 0.058(4) 0.036(3) 0.007(3) 0.003(2) 0.012(3) C7 0.024(3) 0.070(5) 0.053(4) 0.005(4) 0.001(3) -0.007(3) C8 0.025(3) 0.049(4) 0.040(3) 0.002(3) 0.002(2) -0.007(2) C9 0.054(4) 0.034(3) 0.051(4) -0.022(3) 0.008(3) -0.012(3) C10 0.028(3) 0.042(3) 0.051(4) -0.007(3) -0.004(3) 0.003(3) C11 0.033(3) 0.058(4) 0.090(6) 0.007(4) 0.015(4) 0.013(3) C12 0.028(3) 0.019(2) 0.029(3) -0.003(2) 0.002(2) 0.001(2) C13 0.028(3) 0.023(3) 0.029(3) -0.007(2) 0.004(2) -0.003(2) C14 0.034(3) 0.027(3) 0.025(3) -0.004(2) -0.001(2) 0.001(2) C15 0.031(3) 0.028(3) 0.036(3) 0.003(2) -0.007(2) 0.001(2) C16 0.032(3) 0.042(3) 0.039(3) 0.000(3) -0.002(2) -0.004(3) C17 0.037(3) 0.043(3) 0.050(4) 0.002(3) -0.010(3) 0.009(3) C18 0.053(4) 0.032(3) 0.054(4) 0.006(3) -0.010(3) 0.011(3) C19 0.041(3) 0.026(3) 0.047(4) 0.003(2) -0.001(3) 0.000(2) C20 0.047(4) 0.041(3) 0.034(3) 0.005(3) 0.005(3) -0.006(3) C21 0.029(3) 0.034(3) 0.038(3) 0.006(2) 0.002(2) 0.007(2) C22 0.038(4) 0.085(6) 0.060(5) 0.018(4) -0.003(3) -0.002(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd1 2.6505(5) . . yes I2 Pd1 2.6622(6) . . yes Pd1 C1 1.993(5) . . yes Pd1 C12 1.997(5) . . yes N1 N2 1.336(6) . . yes N1 C1 1.361(7) . . yes N1 C10 1.474(7) . . yes N2 N3 1.317(7) . . yes N3 C2 1.353(7) . . yes N3 C9 1.469(8) . . yes N4 N5 1.336(6) . . yes N4 C12 1.361(6) . . yes N4 C21 1.459(7) . . yes N5 N6 1.313(6) . . yes N6 C13 1.367(7) . . yes N6 C20 1.459(7) . . yes C1 C2 1.393(8) . . no C2 C3 1.464(7) . . no C3 C4 1.392(8) . . no C3 C8 1.374(8) . . no C4 C5 1.381(8) . . no C5 C6 1.371(9) . . no C6 C7 1.366(10) . . no C7 C8 1.391(9) . . no C10 C11 1.510(10) . . no C12 C13 1.375(8) . . no C13 C14 1.471(8) . . no C14 C15 1.392(8) . . no C14 C19 1.401(8) . . no C15 C16 1.387(8) . . no C16 C17 1.386(9) . . no C17 C18 1.375(10) . . no C18 C19 1.385(9) . . no C21 C22 1.498(9) . . no C4 H4 0.9500 . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7 0.9500 . . no C8 H8 0.9500 . . no C9 H9A 0.9800 . . no C9 H9B 0.9800 . . no C9 H9C 0.9800 . . no C10 H10A 0.9900 . . no C10 H10B 0.9900 . . no C11 H11A 0.9800 . . no C11 H11B 0.9800 . . no C11 H11C 0.9800 . . no C15 H15 0.9500 . . no C16 H16 0.9500 . . no C17 H17 0.9500 . . no C18 H18 0.9500 . . no C19 H19 0.9500 . . no C20 H20A 0.9800 . . no C20 H20B 0.9800 . . no C20 H20C 0.9800 . . no C21 H21A 0.9900 . . no C21 H21B 0.9900 . . no C22 H22A 0.9800 . . no C22 H22B 0.9800 . . no C22 H22C 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I1 Pd1 I2 94.54(2) . . . yes I1 Pd1 C1 175.47(15) . . . yes I1 Pd1 C12 87.67(16) . . . yes I2 Pd1 C1 89.50(16) . . . yes I2 Pd1 C12 177.24(15) . . . yes C1 Pd1 C12 88.4(2) . . . yes N2 N1 C1 114.5(5) . . . yes N2 N1 C10 118.1(5) . . . yes C1 N1 C10 127.4(5) . . . yes N1 N2 N3 102.9(4) . . . yes N2 N3 C2 113.4(4) . . . yes N2 N3 C9 116.7(4) . . . yes C2 N3 C9 129.9(5) . . . yes N5 N4 C12 113.9(4) . . . yes N5 N4 C21 118.4(4) . . . yes C12 N4 C21 127.5(4) . . . yes N4 N5 N6 103.5(4) . . . yes N5 N6 C13 112.5(4) . . . yes N5 N6 C20 117.1(5) . . . yes C13 N6 C20 130.3(5) . . . yes Pd1 C1 N1 125.9(4) . . . yes Pd1 C1 C2 131.2(4) . . . yes N1 C1 C2 102.9(5) . . . yes N3 C2 C1 106.2(5) . . . yes N3 C2 C3 124.0(5) . . . yes C1 C2 C3 129.6(5) . . . no C2 C3 C4 118.1(5) . . . no C2 C3 C8 123.3(5) . . . no C4 C3 C8 118.7(5) . . . no C3 C4 C5 120.7(5) . . . no C4 C5 C6 120.0(6) . . . no C5 C6 C7 119.8(6) . . . no C6 C7 C8 120.7(6) . . . no C3 C8 C7 120.1(6) . . . no N1 C10 C11 112.5(5) . . . yes Pd1 C12 N4 125.2(4) . . . yes Pd1 C12 C13 131.3(4) . . . yes N4 C12 C13 103.6(4) . . . yes N6 C13 C12 106.4(4) . . . yes N6 C13 C14 124.4(5) . . . yes C12 C13 C14 129.2(5) . . . no C13 C14 C15 118.5(5) . . . no C13 C14 C19 122.5(5) . . . no C15 C14 C19 118.8(5) . . . no C14 C15 C16 120.8(5) . . . no C15 C16 C17 119.9(6) . . . no C16 C17 C18 119.7(6) . . . no C17 C18 C19 121.1(6) . . . no C14 C19 C18 119.8(5) . . . no N4 C21 C22 112.4(5) . . . yes C3 C4 H4 120.00 . . . no C5 C4 H4 120.00 . . . no C4 C5 H5 120.00 . . . no C6 C5 H5 120.00 . . . no C5 C6 H6 120.00 . . . no C7 C6 H6 120.00 . . . no C6 C7 H7 120.00 . . . no C8 C7 H7 120.00 . . . no C3 C8 H8 120.00 . . . no C7 C8 H8 120.00 . . . no N3 C9 H9A 109.00 . . . no N3 C9 H9B 110.00 . . . no N3 C9 H9C 110.00 . . . no H9A C9 H9B 109.00 . . . no H9A C9 H9C 109.00 . . . no H9B C9 H9C 110.00 . . . no N1 C10 H10A 109.00 . . . no N1 C10 H10B 109.00 . . . no C11 C10 H10A 109.00 . . . no C11 C10 H10B 109.00 . . . no H10A C10 H10B 108.00 . . . no C10 C11 H11A 109.00 . . . no C10 C11 H11B 110.00 . . . no C10 C11 H11C 110.00 . . . no H11A C11 H11B 109.00 . . . no H11A C11 H11C 109.00 . . . no H11B C11 H11C 109.00 . . . no C14 C15 H15 120.00 . . . no C16 C15 H15 120.00 . . . no C15 C16 H16 120.00 . . . no C17 C16 H16 120.00 . . . no C16 C17 H17 120.00 . . . no C18 C17 H17 120.00 . . . no C17 C18 H18 119.00 . . . no C19 C18 H18 119.00 . . . no C14 C19 H19 120.00 . . . no C18 C19 H19 120.00 . . . no N6 C20 H20A 109.00 . . . no N6 C20 H20B 110.00 . . . no N6 C20 H20C 109.00 . . . no H20A C20 H20B 109.00 . . . no H20A C20 H20C 109.00 . . . no H20B C20 H20C 109.00 . . . no N4 C21 H21A 109.00 . . . no N4 C21 H21B 109.00 . . . no C22 C21 H21A 109.00 . . . no C22 C21 H21B 109.00 . . . no H21A C21 H21B 108.00 . . . no C21 C22 H22A 109.00 . . . no C21 C22 H22B 109.00 . . . no C21 C22 H22C 109.00 . . . no H22A C22 H22B 110.00 . . . no H22A C22 H22C 109.00 . . . no H22B C22 H22C 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I2 Pd1 C1 N1 -82.1(5) . . . . no I2 Pd1 C1 C2 98.7(5) . . . . no C12 Pd1 C1 N1 96.1(5) . . . . no C12 Pd1 C1 C2 -83.0(6) . . . . no I1 Pd1 C12 N4 -80.9(4) . . . . no I1 Pd1 C12 C13 100.0(5) . . . . no C1 Pd1 C12 N4 96.9(5) . . . . no C1 Pd1 C12 C13 -82.2(6) . . . . no C1 N1 N2 N3 -1.0(6) . . . . no C10 N1 N2 N3 178.4(4) . . . . no N2 N1 C1 Pd1 -178.2(4) . . . . no N2 N1 C1 C2 1.1(6) . . . . no C10 N1 C1 Pd1 2.4(8) . . . . no C10 N1 C1 C2 -178.3(5) . . . . no N2 N1 C10 C11 -24.6(7) . . . . no C1 N1 C10 C11 154.8(6) . . . . no N1 N2 N3 C2 0.5(6) . . . . no N1 N2 N3 C9 178.7(4) . . . . no N2 N3 C2 C1 0.2(6) . . . . no N2 N3 C2 C3 -175.8(5) . . . . no C9 N3 C2 C1 -177.7(5) . . . . no C9 N3 C2 C3 6.3(9) . . . . no C12 N4 N5 N6 0.8(5) . . . . no C21 N4 N5 N6 177.0(4) . . . . no N5 N4 C12 Pd1 179.7(3) . . . . no N5 N4 C12 C13 -1.1(6) . . . . no C21 N4 C12 Pd1 3.9(7) . . . . no C21 N4 C12 C13 -176.9(5) . . . . no N5 N4 C21 C22 38.1(7) . . . . no C12 N4 C21 C22 -146.3(6) . . . . no N4 N5 N6 C13 -0.2(5) . . . . no N4 N5 N6 C20 176.9(4) . . . . no N5 N6 C13 C12 -0.5(6) . . . . no N5 N6 C13 C14 -179.0(5) . . . . no C20 N6 C13 C12 -177.0(5) . . . . no C20 N6 C13 C14 4.5(9) . . . . no Pd1 C1 C2 N3 178.6(4) . . . . no Pd1 C1 C2 C3 -5.8(9) . . . . no N1 C1 C2 N3 -0.7(6) . . . . no N1 C1 C2 C3 174.9(5) . . . . no N3 C2 C3 C4 133.5(6) . . . . no N3 C2 C3 C8 -46.5(8) . . . . no C1 C2 C3 C4 -41.5(9) . . . . no C1 C2 C3 C8 138.6(6) . . . . no C2 C3 C4 C5 -178.9(5) . . . . no C8 C3 C4 C5 1.1(9) . . . . no C2 C3 C8 C7 179.4(6) . . . . no C4 C3 C8 C7 -0.6(9) . . . . no C3 C4 C5 C6 -0.7(9) . . . . no C4 C5 C6 C7 -0.2(9) . . . . no C5 C6 C7 C8 0.6(10) . . . . no C6 C7 C8 C3 -0.3(10) . . . . no Pd1 C12 C13 N6 -179.9(4) . . . . no Pd1 C12 C13 C14 -1.5(9) . . . . no N4 C12 C13 N6 0.9(6) . . . . no N4 C12 C13 C14 179.3(5) . . . . no N6 C13 C14 C15 134.3(6) . . . . no N6 C13 C14 C19 -50.0(8) . . . . no C12 C13 C14 C15 -43.9(9) . . . . no C12 C13 C14 C19 131.8(6) . . . . no C13 C14 C15 C16 175.5(5) . . . . no C19 C14 C15 C16 -0.3(9) . . . . no C13 C14 C19 C18 -176.0(6) . . . . no C15 C14 C19 C18 -0.3(9) . . . . no C14 C15 C16 C17 -0.1(9) . . . . no C15 C16 C17 C18 1.0(9) . . . . no C16 C17 C18 C19 -1.7(10) . . . . no C17 C18 C19 C14 1.3(10) . . . . no _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.949 _refine_diff_density_min -1.653 _refine_diff_density_rms 0.160 #################################################END data_complex_cis3a_pentane _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H28 Cl2 I2 N6 Pd' _chemical_formula_weight 819.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7461(9) _cell_length_b 17.2912(9) _cell_length_c 14.1530(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.592(5) _cell_angle_gamma 90.00 _cell_volume 2879.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22444 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 25.58 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 2.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.369 _exptl_absorpt_correction_T_max 0.520 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28970 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.17 _reflns_number_total 5134 _reflns_number_gt 3814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5134 _refine_ls_number_parameters 318 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.912 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3687(5) 0.1461(3) 0.5150(4) 0.0321(13) Uani 1 1 d . . . C2 C 0.4667(5) 0.1893(3) 0.5372(4) 0.0337(13) Uani 1 1 d . . . C3 C 0.4843(5) 0.2591(3) 0.4852(5) 0.0369(13) Uani 1 1 d . . . C4 C 0.4487(6) 0.2591(4) 0.3795(5) 0.0444(15) Uani 1 1 d . . . H4A H 0.4164 0.2138 0.3414 0.053 Uiso 1 1 calc R . . C5 C 0.4605(6) 0.3259(5) 0.3295(6) 0.0553(19) Uani 1 1 d . . . H5A H 0.4372 0.3258 0.2572 0.066 Uiso 1 1 calc R . . C6 C 0.5060(6) 0.3925(4) 0.3841(6) 0.059(2) Uani 1 1 d . . . H6A H 0.5115 0.4384 0.3495 0.071 Uiso 1 1 calc R . . C7 C 0.5430(7) 0.3913(4) 0.4891(6) 0.060(2) Uani 1 1 d . . . H7A H 0.5760 0.4365 0.5271 0.072 Uiso 1 1 calc R . . C8 C 0.5330(6) 0.3255(4) 0.5400(5) 0.0459(16) Uani 1 1 d . . . H8A H 0.5594 0.3255 0.6125 0.055 Uiso 1 1 calc R . . C9 C 0.6683(6) 0.1765(4) 0.6703(5) 0.0497(16) Uani 1 1 d . . . H9A H 0.6740 0.2175 0.7198 0.075 Uiso 1 1 calc R . . H9B H 0.6985 0.1952 0.6205 0.075 Uiso 1 1 calc R . . H9C H 0.7121 0.1314 0.7063 0.075 Uiso 1 1 calc R . . C10 C 0.3402(6) 0.0183(3) 0.5935(5) 0.0457(16) Uani 1 1 d . . . H10A H 0.2585 0.0264 0.5518 0.055 Uiso 1 1 calc R . . H10B H 0.3491 0.0103 0.6654 0.055 Uiso 1 1 calc R . . C11 C 0.3820(8) -0.0527(4) 0.5553(6) 0.062(2) Uani 1 1 d . . . H11A H 0.3753 -0.0439 0.4848 0.093 Uiso 1 1 calc R . . H11B H 0.3359 -0.0975 0.5574 0.093 Uiso 1 1 calc R . . H11C H 0.4616 -0.0623 0.5991 0.093 Uiso 1 1 calc R . . C12 C 0.2010(5) 0.2368(3) 0.5264(5) 0.0330(13) Uani 1 1 d . . . C13 C 0.1881(5) 0.2227(3) 0.6180(4) 0.0311(12) Uani 1 1 d . . . C14 C 0.1723(5) 0.1483(3) 0.6624(5) 0.0337(13) Uani 1 1 d . . . C15 C 0.0816(5) 0.1015(3) 0.6066(5) 0.0413(14) Uani 1 1 d . . . H15A H 0.0288 0.1184 0.5419 0.050 Uiso 1 1 calc R . . C16 C 0.0671(6) 0.0303(4) 0.6444(5) 0.0488(17) Uani 1 1 d . . . H16A H 0.0044 -0.0015 0.6061 0.059 Uiso 1 1 calc R . . C17 C 0.1447(7) 0.0056(3) 0.7385(5) 0.0494(17) Uani 1 1 d . . . H17A H 0.1344 -0.0430 0.7650 0.059 Uiso 1 1 calc R . . C18 C 0.2369(6) 0.0510(3) 0.7941(5) 0.0485(17) Uani 1 1 d . . . H18A H 0.2908 0.0330 0.8577 0.058 Uiso 1 1 calc R . . C19 C 0.2509(6) 0.1235(3) 0.7564(5) 0.0431(15) Uani 1 1 d . . . H19A H 0.3135 0.1554 0.7947 0.052 Uiso 1 1 calc R . . C20 C 0.1815(6) 0.3104(4) 0.7600(5) 0.0480(17) Uani 1 1 d . . . H20A H 0.1540 0.3636 0.7577 0.072 Uiso 1 1 calc R . . H20B H 0.2557 0.3053 0.8163 0.072 Uiso 1 1 calc R . . H20C H 0.1274 0.2747 0.7707 0.072 Uiso 1 1 calc R . . C21 C 0.2245(6) 0.3628(3) 0.4468(5) 0.0487(17) Uani 1 1 d D . . H21A H 0.2719 0.3342 0.4172 0.058 Uiso 0.65 1 calc PR A 1 H21B H 0.1483 0.3695 0.3918 0.058 Uiso 0.65 1 calc PR A 1 H21C H 0.2207 0.3286 0.3895 0.058 Uiso 0.35 1 d PR A 2 H21D H 0.3007 0.3870 0.4738 0.058 Uiso 0.35 1 d PR A 2 C22 C 0.2729(12) 0.4372(6) 0.4770(10) 0.066(3) Uani 0.65 1 d PD B 1 H22A H 0.2265 0.4666 0.5057 0.099 Uiso 0.65 1 calc PR B 1 H22B H 0.2758 0.4645 0.4174 0.099 Uiso 0.65 1 calc PR B 1 H22C H 0.3501 0.4316 0.5288 0.099 Uiso 0.65 1 calc PR B 1 C22A C 0.1389(18) 0.4240(10) 0.4061(17) 0.066(3) Uani 0.35 1 d PD B 2 H22D H 0.1224 0.4471 0.4621 0.099 Uiso 0.35 1 calc PR B 2 H22E H 0.0692 0.4019 0.3555 0.099 Uiso 0.35 1 calc PR B 2 H22F H 0.1681 0.4640 0.3734 0.099 Uiso 0.35 1 calc PR B 2 I1 I -0.00363(3) 0.20500(2) 0.30549(3) 0.04123(13) Uani 1 1 d . . . I2 I 0.23142(4) 0.06453(2) 0.28629(3) 0.04761(14) Uani 1 1 d . . . N1 N 0.4062(5) 0.0878(3) 0.5863(4) 0.0372(12) Uani 1 1 d . . . N2 N 0.5133(5) 0.0913(3) 0.6482(4) 0.0404(12) Uani 1 1 d . . . N3 N 0.5494(4) 0.1546(3) 0.6172(4) 0.0369(11) Uani 1 1 d . . . N4 N 0.2124(4) 0.3155(2) 0.5272(4) 0.0344(11) Uani 1 1 d . B . N5 N 0.2068(4) 0.3502(3) 0.6085(4) 0.0358(11) Uani 1 1 d . . . N6 N 0.1922(4) 0.2922(2) 0.6635(4) 0.0332(11) Uani 1 1 d . B . Pd1 Pd 0.20888(4) 0.16522(2) 0.41963(3) 0.02983(12) Uani 1 1 d . . . C23 C 0.3277(16) 0.1531(9) 0.046(2) 0.0977(13) Uani 0.50 1 d PD C 1 H23A H 0.3171 0.1403 0.1102 0.117 Uiso 0.50 1 calc PR C 1 H23B H 0.2599 0.1351 -0.0122 0.117 Uiso 0.50 1 calc PR C 1 Cl1 Cl 0.3427(6) 0.2549(4) 0.0380(6) 0.0977(13) Uani 0.50 1 d PD C 1 Cl2 Cl 0.4489(5) 0.1070(4) 0.0450(5) 0.0977(13) Uani 0.50 1 d PD C 1 C23A C 0.3512(17) 0.1329(10) 0.084(2) 0.1159(16) Uani 0.50 1 d PD D 2 H23C H 0.3404 0.1380 0.1496 0.139 Uiso 0.50 1 calc PR D 2 H23D H 0.2786 0.1147 0.0316 0.139 Uiso 0.50 1 calc PR D 2 Cl1A Cl 0.3845(6) 0.2234(5) 0.0484(7) 0.1159(16) Uani 0.50 1 d PD D 2 Cl2A Cl 0.4554(6) 0.0648(4) 0.0987(6) 0.1159(16) Uani 0.50 1 d PD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(3) 0.029(3) 0.029(3) -0.004(2) 0.016(3) 0.006(2) C2 0.035(3) 0.034(3) 0.031(3) -0.006(2) 0.011(3) 0.003(2) C3 0.033(3) 0.039(3) 0.037(3) 0.007(3) 0.011(3) 0.005(3) C4 0.043(4) 0.054(4) 0.037(4) 0.005(3) 0.017(3) 0.002(3) C5 0.038(4) 0.087(5) 0.043(4) 0.023(4) 0.018(3) 0.006(4) C6 0.045(4) 0.061(4) 0.073(5) 0.031(4) 0.023(4) -0.001(4) C7 0.060(5) 0.043(4) 0.070(5) 0.012(4) 0.016(4) -0.016(3) C8 0.048(4) 0.046(4) 0.042(4) 0.003(3) 0.016(3) -0.004(3) C9 0.041(4) 0.053(4) 0.045(4) 0.002(3) 0.006(3) 0.006(3) C10 0.067(5) 0.029(3) 0.053(4) 0.008(3) 0.036(4) 0.005(3) C11 0.099(6) 0.032(3) 0.071(5) 0.007(3) 0.051(5) 0.013(4) C12 0.028(3) 0.027(3) 0.041(3) 0.000(2) 0.011(3) 0.001(2) C13 0.034(3) 0.026(3) 0.033(3) -0.005(2) 0.012(3) 0.000(2) C14 0.040(3) 0.028(3) 0.041(3) 0.001(2) 0.025(3) 0.001(2) C15 0.041(4) 0.036(3) 0.046(4) -0.008(3) 0.016(3) -0.005(3) C16 0.059(5) 0.036(3) 0.057(4) -0.008(3) 0.029(4) -0.013(3) C17 0.078(5) 0.033(3) 0.048(4) 0.003(3) 0.035(4) -0.003(3) C18 0.071(5) 0.036(3) 0.043(4) 0.007(3) 0.028(4) 0.008(3) C19 0.056(4) 0.034(3) 0.044(4) -0.001(3) 0.024(3) -0.002(3) C20 0.066(5) 0.042(3) 0.051(4) -0.010(3) 0.039(4) -0.001(3) C21 0.068(5) 0.029(3) 0.055(4) 0.009(3) 0.032(4) 0.001(3) C22 0.098(9) 0.048(5) 0.062(7) -0.005(5) 0.040(6) -0.010(6) C22A 0.098(9) 0.048(5) 0.062(7) -0.005(5) 0.040(6) -0.010(6) I1 0.0344(2) 0.0392(2) 0.0472(3) -0.00332(17) 0.01264(19) 0.00062(16) I2 0.0588(3) 0.0412(2) 0.0395(2) -0.00777(18) 0.0152(2) 0.01379(19) N1 0.047(3) 0.031(2) 0.042(3) 0.003(2) 0.026(3) 0.007(2) N2 0.046(3) 0.036(3) 0.041(3) 0.005(2) 0.018(3) 0.011(2) N3 0.036(3) 0.037(3) 0.034(3) 0.002(2) 0.009(2) 0.007(2) N4 0.043(3) 0.027(2) 0.036(3) 0.000(2) 0.018(2) 0.001(2) N5 0.042(3) 0.028(2) 0.040(3) -0.003(2) 0.019(2) 0.001(2) N6 0.039(3) 0.029(2) 0.035(3) -0.004(2) 0.018(2) 0.000(2) Pd1 0.0340(3) 0.0238(2) 0.0330(2) -0.00170(17) 0.0144(2) 0.00062(17) C23 0.086(3) 0.109(3) 0.109(3) -0.014(3) 0.049(3) -0.008(2) Cl1 0.086(3) 0.109(3) 0.109(3) -0.014(3) 0.049(3) -0.008(2) Cl2 0.086(3) 0.109(3) 0.109(3) -0.014(3) 0.049(3) -0.008(2) C23A 0.084(3) 0.124(4) 0.130(4) 0.013(3) 0.030(3) -0.017(3) Cl1A 0.084(3) 0.124(4) 0.130(4) 0.013(3) 0.030(3) -0.017(3) Cl2A 0.084(3) 0.124(4) 0.130(4) 0.013(3) 0.030(3) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.375(7) . ? C1 C2 1.384(8) . ? C1 Pd1 1.992(6) . ? C2 N3 1.355(7) . ? C2 C3 1.475(8) . ? C3 C4 1.387(9) . ? C3 C8 1.390(9) . ? C4 C5 1.393(9) . ? C4 H4A 0.9500 . ? C5 C6 1.383(11) . ? C5 H5A 0.9500 . ? C6 C7 1.376(11) . ? C6 H6A 0.9500 . ? C7 C8 1.378(9) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 N3 1.459(8) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N1 1.492(8) . ? C10 C11 1.517(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N4 1.368(7) . ? C12 C13 1.388(8) . ? C12 Pd1 1.985(6) . ? C13 N6 1.354(7) . ? C13 C14 1.480(7) . ? C14 C15 1.384(8) . ? C14 C19 1.391(9) . ? C15 C16 1.382(9) . ? C15 H15A 0.9500 . ? C16 C17 1.387(10) . ? C16 H16A 0.9500 . ? C17 C18 1.380(10) . ? C17 H17A 0.9500 . ? C18 C19 1.400(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 N6 1.458(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.419(11) . ? C21 N4 1.458(8) . ? C21 C22A 1.469(16) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 H21C 0.9900 . ? C21 H21D 0.9900 . ? C22 H21D 0.9436 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? I1 Pd1 2.6567(6) . ? I2 Pd1 2.6630(6) . ? N1 N2 1.311(7) . ? N2 N3 1.325(7) . ? N4 N5 1.324(6) . ? N5 N6 1.326(6) . ? C23 Cl2 1.745(15) . ? C23 Cl1 1.779(16) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23A Cl2A 1.727(16) . ? C23A Cl1A 1.748(16) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 101.6(5) . . ? N1 C1 Pd1 126.5(4) . . ? C2 C1 Pd1 131.5(4) . . ? N3 C2 C1 107.2(5) . . ? N3 C2 C3 124.1(5) . . ? C1 C2 C3 128.7(5) . . ? C4 C3 C8 119.5(6) . . ? C4 C3 C2 119.3(6) . . ? C8 C3 C2 121.3(5) . . ? C3 C4 C5 119.6(7) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C6 C5 C4 120.7(7) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C7 C6 C5 119.2(6) . . ? C7 C6 H6A 120.4 . . ? C5 C6 H6A 120.4 . . ? C6 C7 C8 121.0(7) . . ? C6 C7 H7A 119.5 . . ? C8 C7 H7A 119.5 . . ? C7 C8 C3 120.1(6) . . ? C7 C8 H8A 120.0 . . ? C3 C8 H8A 120.0 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 110.1(5) . . ? N1 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N1 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C13 102.5(5) . . ? N4 C12 Pd1 126.1(4) . . ? C13 C12 Pd1 131.3(4) . . ? N6 C13 C12 107.0(5) . . ? N6 C13 C14 123.7(5) . . ? C12 C13 C14 129.2(5) . . ? C15 C14 C19 120.1(5) . . ? C15 C14 C13 119.1(6) . . ? C19 C14 C13 120.6(5) . . ? C16 C15 C14 120.5(6) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 120.6(6) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 119.8(6) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C14 C19 C18 119.3(6) . . ? C14 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? N6 C20 H20A 109.5 . . ? N6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N4 116.0(7) . . ? C22 C21 C22A 68.8(11) . . ? N4 C21 C22A 115.2(10) . . ? C22 C21 H21A 108.3 . . ? N4 C21 H21A 108.3 . . ? C22A C21 H21A 132.5 . . ? C22 C21 H21B 108.3 . . ? N4 C21 H21B 108.3 . . ? C22A C21 H21B 41.6 . . ? H21A C21 H21B 107.4 . . ? C22 C21 H21C 131.9 . . ? N4 C21 H21C 108.4 . . ? C22A C21 H21C 108.4 . . ? H21A C21 H21C 36.9 . . ? H21B C21 H21C 72.6 . . ? C22 C21 H21D 41.5 . . ? N4 C21 H21D 108.5 . . ? C22A C21 H21D 108.5 . . ? H21A C21 H21D 72.9 . . ? H21B C21 H21D 140.8 . . ? H21C C21 H21D 107.5 . . ? C21 C22 H21D 44.1 . . ? C21 C22 H22A 109.5 . . ? H21D C22 H22A 142.6 . . ? C21 C22 H22B 109.5 . . ? H21D C22 H22B 105.3 . . ? C21 C22 H22C 109.5 . . ? H21D C22 H22C 70.1 . . ? C21 C22A H22D 109.5 . . ? C21 C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C21 C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? N2 N1 C1 115.8(5) . . ? N2 N1 C10 117.5(5) . . ? C1 N1 C10 126.4(5) . . ? N1 N2 N3 102.9(5) . . ? N2 N3 C2 112.6(5) . . ? N2 N3 C9 117.9(5) . . ? C2 N3 C9 129.5(5) . . ? N5 N4 C12 114.7(5) . . ? N5 N4 C21 118.7(4) . . ? C12 N4 C21 126.5(5) . . ? N4 N5 N6 103.5(4) . . ? N5 N6 C13 112.3(5) . . ? N5 N6 C20 118.1(4) . . ? C13 N6 C20 129.6(5) . . ? C12 Pd1 C1 85.7(2) . . ? C12 Pd1 I1 87.92(17) . . ? C1 Pd1 I1 173.39(15) . . ? C12 Pd1 I2 176.08(17) . . ? C1 Pd1 I2 90.62(15) . . ? I1 Pd1 I2 95.781(19) . . ? Cl2 C23 Cl1 109.5(10) . . ? Cl2 C23 H23A 109.8 . . ? Cl1 C23 H23A 109.8 . . ? Cl2 C23 H23B 109.8 . . ? Cl1 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? Cl2A C23A Cl1A 112.6(11) . . ? Cl2A C23A H23C 109.1 . . ? Cl1A C23A H23C 109.1 . . ? Cl2A C23A H23D 109.1 . . ? Cl1A C23A H23D 109.1 . . ? H23C C23A H23D 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N3 -0.7(6) . . . . ? Pd1 C1 C2 N3 172.2(4) . . . . ? N1 C1 C2 C3 177.8(6) . . . . ? Pd1 C1 C2 C3 -9.2(9) . . . . ? N3 C2 C3 C4 129.0(6) . . . . ? C1 C2 C3 C4 -49.3(9) . . . . ? N3 C2 C3 C8 -52.8(8) . . . . ? C1 C2 C3 C8 128.9(7) . . . . ? C8 C3 C4 C5 -1.0(9) . . . . ? C2 C3 C4 C5 177.2(6) . . . . ? C3 C4 C5 C6 -0.9(10) . . . . ? C4 C5 C6 C7 2.2(11) . . . . ? C5 C6 C7 C8 -1.5(12) . . . . ? C6 C7 C8 C3 -0.4(11) . . . . ? C4 C3 C8 C7 1.6(10) . . . . ? C2 C3 C8 C7 -176.6(7) . . . . ? N4 C12 C13 N6 0.3(6) . . . . ? Pd1 C12 C13 N6 177.9(4) . . . . ? N4 C12 C13 C14 -179.8(6) . . . . ? Pd1 C12 C13 C14 -2.3(10) . . . . ? N6 C13 C14 C15 122.6(6) . . . . ? C12 C13 C14 C15 -57.3(9) . . . . ? N6 C13 C14 C19 -61.0(8) . . . . ? C12 C13 C14 C19 119.1(7) . . . . ? C19 C14 C15 C16 1.1(9) . . . . ? C13 C14 C15 C16 177.5(5) . . . . ? C14 C15 C16 C17 -0.5(10) . . . . ? C15 C16 C17 C18 -0.8(10) . . . . ? C16 C17 C18 C19 1.6(10) . . . . ? C15 C14 C19 C18 -0.3(9) . . . . ? C13 C14 C19 C18 -176.7(5) . . . . ? C17 C18 C19 C14 -1.0(10) . . . . ? C2 C1 N1 N2 0.5(6) . . . . ? Pd1 C1 N1 N2 -173.0(4) . . . . ? C2 C1 N1 C10 -173.6(5) . . . . ? Pd1 C1 N1 C10 13.0(8) . . . . ? C11 C10 N1 N2 -68.8(7) . . . . ? C11 C10 N1 C1 105.2(7) . . . . ? C1 N1 N2 N3 0.0(6) . . . . ? C10 N1 N2 N3 174.6(5) . . . . ? N1 N2 N3 C2 -0.5(6) . . . . ? N1 N2 N3 C9 -179.7(5) . . . . ? C1 C2 N3 N2 0.8(7) . . . . ? C3 C2 N3 N2 -177.9(5) . . . . ? C1 C2 N3 C9 180.0(6) . . . . ? C3 C2 N3 C9 1.3(10) . . . . ? C13 C12 N4 N5 -0.6(6) . . . . ? Pd1 C12 N4 N5 -178.3(4) . . . . ? C13 C12 N4 C21 -177.6(6) . . . . ? Pd1 C12 N4 C21 4.7(9) . . . . ? C22 C21 N4 N5 23.9(10) . . . . ? C22A C21 N4 N5 -53.6(12) . . . . ? C22 C21 N4 C12 -159.2(8) . . . . ? C22A C21 N4 C12 123.3(11) . . . . ? C12 N4 N5 N6 0.6(6) . . . . ? C21 N4 N5 N6 177.8(5) . . . . ? N4 N5 N6 C13 -0.3(6) . . . . ? N4 N5 N6 C20 -179.5(5) . . . . ? C12 C13 N6 N5 0.0(7) . . . . ? C14 C13 N6 N5 -179.9(5) . . . . ? C12 C13 N6 C20 179.0(6) . . . . ? C14 C13 N6 C20 -0.9(10) . . . . ? N4 C12 Pd1 C1 99.0(5) . . . . ? C13 C12 Pd1 C1 -78.0(6) . . . . ? N4 C12 Pd1 I1 -79.2(5) . . . . ? C13 C12 Pd1 I1 103.7(6) . . . . ? N4 C12 Pd1 I2 120(2) . . . . ? C13 C12 Pd1 I2 -57(3) . . . . ? N1 C1 Pd1 C12 93.3(5) . . . . ? C2 C1 Pd1 C12 -78.1(5) . . . . ? N1 C1 Pd1 I1 108.9(14) . . . . ? C2 C1 Pd1 I1 -62.5(17) . . . . ? N1 C1 Pd1 I2 -85.2(4) . . . . ? C2 C1 Pd1 I2 103.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.880 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.138 #################################################END data_complex-4a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 Cl2 N6 Pd' _chemical_formula_sum 'C22 H26 Cl2 N6 Pd' _chemical_formula_weight 551.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2661(2) _cell_length_b 8.8875(3) _cell_length_c 9.3445(3) _cell_angle_alpha 108.081(3) _cell_angle_beta 115.551(3) _cell_angle_gamma 91.735(2) _cell_volume 577.89(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9286 _cell_measurement_theta_min 5.6170 _cell_measurement_theta_max 76.5986 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2705 _exptl_crystal_size_mid 0.1736 _exptl_crystal_size_min 0.1662 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 8.776 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.215 _exptl_absorpt_correction_T_max 0.419 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8246 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 5.62 _diffrn_reflns_theta_max 76.80 _reflns_number_total 2401 _reflns_number_gt 2401 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+2.3112P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2401 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.5000 0.01083(17) Uani 1 2 d S . . Cl Cl 0.27856(11) 0.61269(11) 0.57094(10) 0.0153(2) Uani 1 1 d . . . N1 N 0.2040(4) 0.2780(4) 0.1590(4) 0.0145(6) Uani 1 1 d . . . N2 N 0.1008(5) 0.2475(4) -0.0065(4) 0.0186(7) Uani 1 1 d . . . N3 N 0.1549(4) 0.3779(4) -0.0268(4) 0.0162(6) Uani 1 1 d . . . C1 C 0.3209(5) 0.4227(4) 0.2476(4) 0.0123(7) Uani 1 1 d . . . C2 C 0.2882(5) 0.4881(5) 0.1215(5) 0.0136(7) Uani 1 1 d . . . C3 C 0.3822(5) 0.6425(5) 0.1416(5) 0.0147(7) Uani 1 1 d . . . C4 C 0.0690(6) 0.3798(6) -0.2003(5) 0.0232(9) Uani 1 1 d . . . H4A H 0.1468 0.3435 -0.2540 0.035 Uiso 1 1 calc R . . H4B H 0.0534 0.4897 -0.1962 0.035 Uiso 1 1 calc R . . H4C H -0.0506 0.3075 -0.2665 0.035 Uiso 1 1 calc R . . C5 C 0.1795(6) 0.1553(5) 0.2273(5) 0.0200(8) Uani 1 1 d . . . H5A H 0.2959 0.1619 0.3262 0.024 Uiso 1 1 calc R . . H5B H 0.1478 0.0468 0.1395 0.024 Uiso 1 1 calc R . . C6 C 0.0312(7) 0.1778(6) 0.2810(7) 0.0337(11) Uani 1 1 d . . . H6A H 0.0631 0.2845 0.3691 0.051 Uiso 1 1 calc R . . H6B H 0.0191 0.0945 0.3260 0.051 Uiso 1 1 calc R . . H6C H -0.0848 0.1689 0.1827 0.051 Uiso 1 1 calc R . . C7 C 0.4093(6) 0.6673(5) 0.0120(5) 0.0179(8) Uani 1 1 d . . . H7 H 0.3579 0.5854 -0.0976 0.021 Uiso 1 1 calc R . . C8 C 0.5111(6) 0.8115(5) 0.0437(6) 0.0214(8) Uani 1 1 d . . . H8 H 0.5280 0.8280 -0.0450 0.026 Uiso 1 1 calc R . . C9 C 0.5889(6) 0.9326(5) 0.2041(6) 0.0221(8) Uani 1 1 d . . . H9 H 0.6608 1.0300 0.2254 0.027 Uiso 1 1 calc R . . C10 C 0.5606(6) 0.9095(5) 0.3322(5) 0.0214(8) Uani 1 1 d . . . H10 H 0.6122 0.9918 0.4415 0.026 Uiso 1 1 calc R . . C11 C 0.4559(6) 0.7650(5) 0.3005(5) 0.0188(8) Uani 1 1 d . . . H11 H 0.4350 0.7506 0.3881 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0117(2) 0.0143(2) 0.0068(2) 0.00556(14) 0.00359(15) 0.00040(13) Cl 0.0146(4) 0.0253(5) 0.0038(4) 0.0042(3) 0.0027(3) 0.0114(3) N1 0.0122(14) 0.0175(15) 0.0104(14) 0.0051(12) 0.0024(12) 0.0000(12) N2 0.0172(16) 0.0224(17) 0.0139(16) 0.0074(13) 0.0049(13) 0.0013(13) N3 0.0156(15) 0.0207(16) 0.0127(15) 0.0072(13) 0.0060(13) 0.0039(12) C1 0.0116(16) 0.0168(17) 0.0080(16) 0.0044(13) 0.0042(13) 0.0020(13) C2 0.0146(16) 0.0191(18) 0.0083(16) 0.0056(14) 0.0057(14) 0.0044(14) C3 0.0169(17) 0.0175(18) 0.0144(17) 0.0106(15) 0.0079(14) 0.0057(14) C4 0.023(2) 0.033(2) 0.0105(18) 0.0094(16) 0.0046(16) 0.0064(17) C5 0.0204(19) 0.0181(18) 0.0196(19) 0.0099(16) 0.0058(16) -0.0002(15) C6 0.038(3) 0.035(3) 0.041(3) 0.021(2) 0.024(2) 0.004(2) C7 0.0220(19) 0.0210(19) 0.0168(18) 0.0103(15) 0.0115(16) 0.0095(15) C8 0.026(2) 0.026(2) 0.027(2) 0.0197(18) 0.0184(18) 0.0126(17) C9 0.025(2) 0.021(2) 0.030(2) 0.0163(18) 0.0166(18) 0.0056(16) C10 0.027(2) 0.0182(19) 0.020(2) 0.0085(16) 0.0110(17) 0.0024(16) C11 0.0235(19) 0.0194(19) 0.0165(18) 0.0088(15) 0.0105(16) 0.0019(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.037(3) . ? Pd1 C1 2.037(3) 2_666 ? Pd1 Cl 2.3534(8) 2_666 ? Pd1 Cl 2.3534(8) . ? N1 N2 1.334(4) . ? N1 C1 1.359(5) . ? N1 C5 1.472(5) . ? N2 N3 1.326(5) . ? N3 C2 1.367(5) . ? N3 C4 1.469(5) . ? C1 C2 1.399(5) . ? C2 C3 1.474(5) . ? C3 C11 1.392(6) . ? C3 C7 1.401(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.509(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.386(6) . ? C7 H7 0.9500 . ? C8 C9 1.394(6) . ? C8 H8 0.9500 . ? C9 C10 1.386(6) . ? C9 H9 0.9500 . ? C10 C11 1.400(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C1 180.00(15) . 2_666 ? C1 Pd1 Cl 88.81(10) . 2_666 ? C1 Pd1 Cl 91.19(10) 2_666 2_666 ? C1 Pd1 Cl 91.19(10) . . ? C1 Pd1 Cl 88.81(10) 2_666 . ? Cl Pd1 Cl 179.999(1) 2_666 . ? N2 N1 C1 115.4(3) . . ? N2 N1 C5 117.9(3) . . ? C1 N1 C5 126.8(3) . . ? N3 N2 N1 103.1(3) . . ? N2 N3 C2 112.5(3) . . ? N2 N3 C4 116.6(3) . . ? C2 N3 C4 130.8(3) . . ? N1 C1 C2 102.5(3) . . ? N1 C1 Pd1 124.3(3) . . ? C2 C1 Pd1 133.1(3) . . ? N3 C2 C1 106.5(3) . . ? N3 C2 C3 126.2(3) . . ? C1 C2 C3 127.3(3) . . ? C11 C3 C7 119.2(4) . . ? C11 C3 C2 117.7(3) . . ? C7 C3 C2 123.1(3) . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 111.7(4) . . ? N1 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N1 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C3 120.0(4) . . ? C8 C7 H7 120.0 . . ? C3 C7 H7 120.0 . . ? C7 C8 C9 120.9(4) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 119.4(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C3 C11 C10 120.5(4) . . ? C3 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 N2 N3 0.8(4) . . . . ? C5 N1 N2 N3 -179.9(3) . . . . ? N1 N2 N3 C2 -0.1(4) . . . . ? N1 N2 N3 C4 178.3(3) . . . . ? N2 N1 C1 C2 -1.0(4) . . . . ? C5 N1 C1 C2 179.7(4) . . . . ? N2 N1 C1 Pd1 -178.2(3) . . . . ? C5 N1 C1 Pd1 2.5(5) . . . . ? C1 Pd1 C1 N1 24(7) 2_666 . . . ? Cl Pd1 C1 N1 91.6(3) 2_666 . . . ? Cl Pd1 C1 N1 -88.4(3) . . . . ? C1 Pd1 C1 C2 -153(7) 2_666 . . . ? Cl Pd1 C1 C2 -84.7(4) 2_666 . . . ? Cl Pd1 C1 C2 95.3(4) . . . . ? N2 N3 C2 C1 -0.5(4) . . . . ? C4 N3 C2 C1 -178.6(4) . . . . ? N2 N3 C2 C3 177.6(3) . . . . ? C4 N3 C2 C3 -0.5(6) . . . . ? N1 C1 C2 N3 0.8(4) . . . . ? Pd1 C1 C2 N3 177.7(3) . . . . ? N1 C1 C2 C3 -177.2(4) . . . . ? Pd1 C1 C2 C3 -0.4(6) . . . . ? N3 C2 C3 C11 154.7(4) . . . . ? C1 C2 C3 C11 -27.5(6) . . . . ? N3 C2 C3 C7 -29.1(6) . . . . ? C1 C2 C3 C7 148.6(4) . . . . ? N2 N1 C5 C6 -87.8(4) . . . . ? C1 N1 C5 C6 91.5(5) . . . . ? C11 C3 C7 C8 1.1(6) . . . . ? C2 C3 C7 C8 -175.0(4) . . . . ? C3 C7 C8 C9 0.6(6) . . . . ? C7 C8 C9 C10 -1.4(6) . . . . ? C8 C9 C10 C11 0.6(6) . . . . ? C7 C3 C11 C10 -1.9(6) . . . . ? C2 C3 C11 C10 174.4(4) . . . . ? C9 C10 C11 C3 1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 75.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.716 _refine_diff_density_min -1.618 _refine_diff_density_rms 0.147 #################################################END data_complex-5e _audit_creation_date 2010-09-22T16:44:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _chemical_name_systematic ; ? ; _chemical_formula_sum 'C13 H16 I N3 Pd' _chemical_formula_weight 447.59 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4522(11) _cell_length_b 12.7285(11) _cell_length_c 15.3977(14) _cell_angle_alpha 73.253(7) _cell_angle_beta 66.849(7) _cell_angle_gamma 87.828(7) _cell_volume 2140.9(3) _cell_formula_units_Z 6 _cell_measurement_temperature 100 _cell_measurement_reflns_used 21680 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 26.15 _exptl_crystal_description 'lanceolate blocks' _exptl_crystal_colour 'grey' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 30 -3 8 0.1566 30 3 -1 0.1358 -4 12 30 0.164 -2 6 30 0.2162 -20 -5 -30 0.1573 -30 12 -4 0.1473 -30 2 1 0.2273 0 -30 -3 0.2793 _exptl_special_details ; ? ; _exptl_absorpt_coefficient_mu 3.449 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1822 _exptl_absorpt_correction_T_max 0.4718 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_reflns_av_unetI/netI 0.0105 _diffrn_reflns_number 7982 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.95 _diffrn_measured_fraction_theta_max 0.95 _reflns_number_total 7982 _reflns_number_gt 7154 _reflns_threshold_expression >2\s(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_special_details ; Samples of AP590 show twinning. Two domains were indexed and integrated using STOE X-Area. Structure solution and initial refinement was carried out on the basis of non-overlapping reflections, belonging to one domain only. The resulting model was further refined to convergence in SHELXL-97 with a HKLF5 dataset (featuring both domains including overlapping reflections). A free-format CIF using the LIST 6 command was written and imported in WinGX. Final HKLF4 refinement was carried out. This procedure allows to merge the reflections of the major component and to obtain averaged standard deviations. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1189P)^2^+10.9512P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 7982 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.117 _refine_diff_density_min -2.099 _refine_diff_density_rms 0.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I3 I 0.64261(6) 0.53398(5) 0.12163(5) 0.04805(18) Uani 1 1 d . . . I2 I 0.34462(6) 0.58491(5) 0.27294(5) 0.05062(19) Uani 1 1 d . . . Pd2 Pd 0.46423(6) 0.62979(5) 0.07949(5) 0.03658(18) Uani 1 1 d . . . Pd3 Pd 0.55073(6) 0.58482(5) 0.29128(4) 0.03508(17) Uani 1 1 d . . . N303 N 0.4306(6) 0.6765(6) 0.5524(5) 0.0355(14) Uani 1 1 d . . . N302 N 0.5464(7) 0.6870(6) 0.5211(5) 0.0391(15) Uani 1 1 d . . . N301 N 0.5822(6) 0.6568(5) 0.4377(5) 0.0357(14) Uani 1 1 d . . . C201 C 0.5418(7) 0.6643(6) -0.0684(7) 0.0377(17) Uani 1 1 d . . . N201 N 0.4744(6) 0.7210(5) -0.1136(5) 0.0347(14) Uani 1 1 d . . . N202 N 0.5224(7) 0.7494(6) -0.2114(5) 0.0408(15) Uani 1 1 d . . . C306 C 0.9174(8) 0.6190(7) 0.2530(7) 0.048(2) Uani 1 1 d . . . H306 H 0.9917 0.6071 0.2119 0.057 Uiso 1 1 calc R . . N203 N 0.6258(7) 0.7115(6) -0.2300(6) 0.0423(16) Uani 1 1 d . . . C305 C 0.8206(8) 0.5937(7) 0.2371(7) 0.0415(18) Uani 1 1 d . . . H305 H 0.8314 0.5674 0.1841 0.05 Uiso 1 1 calc R . . C211 C 0.7526(8) 0.6047(7) -0.1504(7) 0.045(2) Uani 1 1 d . . . H21A H 0.7842 0.5822 -0.2101 0.054 Uiso 1 1 calc R . . H21B H 0.7351 0.5389 -0.0945 0.054 Uiso 1 1 calc R . . C308 C 0.7929(8) 0.6786(7) 0.3918(7) 0.0405(18) Uani 1 1 d . . . H308 H 0.7829 0.7097 0.4419 0.049 Uiso 1 1 calc R . . C206 C 0.1544(8) 0.7976(8) 0.0629(8) 0.051(2) Uani 1 1 d . . . H206 H 0.0837 0.8154 0.1047 0.061 Uiso 1 1 calc R . . C207 C 0.1826(8) 0.8292(7) -0.0374(9) 0.051(2) Uani 1 1 d . . . H207 H 0.1316 0.8678 -0.0632 0.061 Uiso 1 1 calc R . . C212 C 0.8477(8) 0.6818(8) -0.1514(7) 0.0441(19) Uani 1 1 d . . . H21C H 0.8719 0.7438 -0.2111 0.053 Uiso 1 1 calc R . . H21D H 0.8142 0.7103 -0.0951 0.053 Uiso 1 1 calc R . . C208 C 0.2895(8) 0.8021(7) -0.1001(7) 0.0447(19) Uani 1 1 d . . . H208 H 0.3101 0.8214 -0.168 0.054 Uiso 1 1 calc R . . C301 C 0.4930(7) 0.6262(7) 0.4154(6) 0.0360(16) Uani 1 1 d . . . C204 C 0.3362(7) 0.7121(7) 0.0430(7) 0.0413(18) Uani 1 1 d . . . C304 C 0.7067(7) 0.6073(6) 0.2994(6) 0.0374(17) Uani 1 1 d . . . C311 C 0.2639(8) 0.6197(7) 0.5171(7) 0.0434(19) Uani 1 1 d . . . H31A H 0.2535 0.5617 0.4911 0.052 Uiso 1 1 calc R . . H31B H 0.2215 0.5944 0.5884 0.052 Uiso 1 1 calc R . . C312 C 0.2110(9) 0.7211(7) 0.4754(9) 0.052(2) Uani 1 1 d . . . H31C H 0.2649 0.7577 0.408 0.063 Uiso 1 1 calc R . . H31D H 0.2024 0.7716 0.5139 0.063 Uiso 1 1 calc R . . C205 C 0.2312(8) 0.7382(8) 0.1039(8) 0.050(2) Uani 1 1 d . . . H205 H 0.2103 0.7173 0.1719 0.06 Uiso 1 1 calc R . . C303 C 0.6988(7) 0.6488(6) 0.3776(6) 0.0348(16) Uani 1 1 d . . . C209 C 0.7065(9) 0.7282(8) -0.3332(7) 0.050(2) Uani 1 1 d . . . H20A H 0.722 0.6581 -0.3452 0.075 Uiso 1 1 calc R . . H20B H 0.7786 0.7664 -0.3459 0.075 Uiso 1 1 calc R . . H20C H 0.6717 0.771 -0.3762 0.075 Uiso 1 1 calc R . . C302 C 0.3935(8) 0.6392(7) 0.4931(6) 0.0371(17) Uani 1 1 d . . . C307 C 0.9047(8) 0.6618(8) 0.3298(7) 0.047(2) Uani 1 1 d . . . H307 H 0.9702 0.679 0.3397 0.057 Uiso 1 1 calc R . . C202 C 0.6435(8) 0.6558(7) -0.1442(7) 0.0416(18) Uani 1 1 d . . . C213 C 0.9535(9) 0.6227(10) -0.1472(9) 0.057(2) Uani 1 1 d . . . H21E H 0.9876 0.5958 -0.2043 0.068 Uiso 1 1 calc R . . H21F H 0.9284 0.5594 -0.0885 0.068 Uiso 1 1 calc R . . C203 C 0.3633(7) 0.7462(6) -0.0586(6) 0.0363(17) Uani 1 1 d . . . C214 C 1.0466(10) 0.6939(12) -0.1453(11) 0.076(4) Uani 1 1 d . . . H21G H 1.0753 0.7545 -0.2049 0.114 Uiso 1 1 calc R . . H21H H 1.1101 0.6508 -0.1404 0.114 Uiso 1 1 calc R . . H21I H 1.0135 0.7215 -0.0892 0.114 Uiso 1 1 calc R . . C313 C 0.0920(12) 0.6967(12) 0.4753(16) 0.107(7) Uani 1 1 d . . . H31E H 0.0623 0.7668 0.4542 0.129 Uiso 1 1 calc R . . H31F H 0.1053 0.6604 0.425 0.129 Uiso 1 1 calc R . . C309 C 0.3600(8) 0.7033(7) 0.6419(6) 0.0420(18) Uani 1 1 d . . . H30A H 0.4101 0.7234 0.6697 0.063 Uiso 1 1 calc R . . H30B H 0.3076 0.6405 0.6887 0.063 Uiso 1 1 calc R . . H30C H 0.3154 0.7639 0.6269 0.063 Uiso 1 1 calc R . . C314 C 0.0071(14) 0.6361(17) 0.558(2) 0.160(12) Uani 1 1 d . . . H31G H 0.0342 0.5663 0.5814 0.24 Uiso 1 1 calc R . . H31H H -0.0601 0.6247 0.545 0.24 Uiso 1 1 calc R . . H31I H -0.0139 0.6738 0.6075 0.24 Uiso 1 1 calc R . . I1 I 0.57790(5) 1.02326(5) 0.57263(4) 0.04208(17) Uani 1 1 d . . . Pd1 Pd 0.64817(5) 0.97832(5) 0.40164(4) 0.03308(17) Uani 1 1 d . . . N2 N 0.8779(6) 0.9064(6) 0.1557(5) 0.0397(15) Uani 1 1 d . . . N3 N 0.7830(7) 0.8809(6) 0.1439(6) 0.0445(17) Uani 1 1 d . . . C1 C 0.7108(7) 0.9351(6) 0.2782(6) 0.0336(16) Uani 1 1 d . . . C12 C 0.5176(8) 0.9759(6) 0.1609(6) 0.0382(17) Uani 1 1 d . . . H12A H 0.5071 1.031 0.1952 0.046 Uiso 1 1 calc R . . H12B H 0.5748 1.0071 0.0937 0.046 Uiso 1 1 calc R . . C9 C 0.8011(10) 0.8386(8) 0.0602(7) 0.053(2) Uani 1 1 d . . . H9A H 0.8818 0.8537 0.0148 0.079 Uiso 1 1 calc R . . H9B H 0.7524 0.8739 0.027 0.079 Uiso 1 1 calc R . . H9C H 0.7808 0.7605 0.0842 0.079 Uiso 1 1 calc R . . C11 C 0.5641(8) 0.8724(6) 0.2139(7) 0.0405(18) Uani 1 1 d . . . H11A H 0.5077 0.8433 0.2818 0.049 Uiso 1 1 calc R . . H11B H 0.5704 0.8162 0.1814 0.049 Uiso 1 1 calc R . . C13 C 0.4035(7) 0.9467(6) 0.1589(6) 0.0368(17) Uani 1 1 d . . . H13A H 0.3467 0.9147 0.2261 0.044 Uiso 1 1 calc R . . H13B H 0.4144 0.8917 0.1244 0.044 Uiso 1 1 calc R . . C2 C 0.6820(7) 0.8962(6) 0.2142(6) 0.0360(17) Uani 1 1 d . . . C14 C 0.3553(8) 1.0467(8) 0.1079(8) 0.052(2) Uani 1 1 d . . . H14A H 0.3396 1.0993 0.1442 0.078 Uiso 1 1 calc R . . H14B H 0.2842 1.0239 0.1055 0.078 Uiso 1 1 calc R . . H14C H 0.412 1.0797 0.0418 0.078 Uiso 1 1 calc R . . C3 C 0.8957(7) 0.9707(6) 0.2839(6) 0.0363(17) Uani 1 1 d . . . C8 C 1.0166(8) 0.9765(8) 0.2475(7) 0.046(2) Uani 1 1 d . . . H8 H 1.0608 0.9568 0.1908 0.055 Uiso 1 1 calc R . . C5 C 0.8786(8) 1.0282(7) 0.4212(7) 0.0435(19) Uani 1 1 d . . . H5 H 0.8347 1.0432 0.4803 0.052 Uiso 1 1 calc R . . C6 C 1.0011(9) 1.0402(9) 0.3829(8) 0.057(2) Uani 1 1 d . . . H6 H 1.0373 1.0674 0.4155 0.069 Uiso 1 1 calc R . . C7 C 1.0693(8) 1.0134(9) 0.2995(7) 0.053(2) Uani 1 1 d . . . H7 H 1.1506 1.0196 0.2775 0.063 Uiso 1 1 calc R . . N1 N 0.8301(6) 0.9372(5) 0.2371(5) 0.0350(14) Uani 1 1 d . . . C4 C 0.8224(7) 0.9938(7) 0.3703(6) 0.0372(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I3 0.0568(4) 0.0462(3) 0.0491(3) -0.0132(3) -0.0304(3) 0.0086(3) I2 0.0554(4) 0.0552(4) 0.0481(3) -0.0139(3) -0.0285(3) 0.0014(3) Pd2 0.0394(4) 0.0321(3) 0.0419(3) -0.0085(2) -0.0216(3) 0.0023(2) Pd3 0.0439(4) 0.0291(3) 0.0362(3) -0.0057(2) -0.0231(3) 0.0042(2) N303 0.037(4) 0.038(3) 0.035(3) -0.006(3) -0.022(3) 0.012(3) N302 0.053(4) 0.036(3) 0.042(4) -0.015(3) -0.032(3) 0.013(3) N301 0.049(4) 0.028(3) 0.034(3) -0.003(2) -0.027(3) 0.008(3) C201 0.035(4) 0.032(4) 0.053(5) -0.016(3) -0.023(4) 0.014(3) N201 0.037(4) 0.027(3) 0.046(4) -0.009(3) -0.024(3) 0.003(3) N202 0.045(4) 0.038(4) 0.040(4) -0.012(3) -0.017(3) 0.008(3) C306 0.037(5) 0.039(4) 0.060(6) -0.004(4) -0.020(4) 0.009(4) N203 0.044(4) 0.041(4) 0.046(4) -0.014(3) -0.021(3) 0.010(3) C305 0.042(5) 0.033(4) 0.042(4) -0.004(3) -0.014(4) 0.005(3) C211 0.048(5) 0.042(4) 0.051(5) -0.021(4) -0.021(4) 0.012(4) C308 0.041(5) 0.032(4) 0.048(5) -0.007(3) -0.020(4) -0.001(3) C206 0.031(4) 0.051(5) 0.070(6) -0.023(5) -0.017(4) 0.004(4) C207 0.034(5) 0.039(4) 0.086(7) -0.015(4) -0.033(5) 0.006(4) C212 0.037(4) 0.046(5) 0.058(5) -0.020(4) -0.025(4) 0.012(4) C208 0.044(5) 0.037(4) 0.052(5) -0.008(4) -0.022(4) -0.001(4) C301 0.036(4) 0.034(4) 0.038(4) -0.008(3) -0.017(3) 0.001(3) C204 0.032(4) 0.035(4) 0.055(5) -0.013(4) -0.016(4) 0.002(3) C304 0.042(4) 0.025(3) 0.044(4) 0.001(3) -0.025(4) 0.010(3) C311 0.037(4) 0.035(4) 0.049(5) 0.001(4) -0.018(4) -0.002(3) C312 0.045(5) 0.032(4) 0.087(7) -0.006(4) -0.041(5) 0.008(4) C205 0.042(5) 0.048(5) 0.059(6) -0.016(4) -0.021(4) 0.008(4) C303 0.036(4) 0.026(3) 0.043(4) -0.006(3) -0.021(3) 0.010(3) C209 0.049(5) 0.056(5) 0.044(5) -0.018(4) -0.015(4) 0.010(4) C302 0.044(5) 0.033(4) 0.039(4) -0.007(3) -0.025(4) 0.007(3) C307 0.036(5) 0.046(5) 0.054(5) -0.006(4) -0.017(4) 0.001(4) C202 0.044(5) 0.039(4) 0.050(5) -0.014(4) -0.028(4) 0.009(4) C213 0.047(6) 0.070(7) 0.070(7) -0.038(5) -0.031(5) 0.014(5) C203 0.032(4) 0.026(3) 0.047(4) -0.001(3) -0.018(3) 0.002(3) C214 0.044(6) 0.103(10) 0.100(10) -0.052(8) -0.034(6) 0.005(6) C313 0.050(7) 0.067(8) 0.195(19) 0.003(10) -0.069(10) 0.009(6) C309 0.047(5) 0.047(5) 0.032(4) -0.011(3) -0.017(4) 0.004(4) C314 0.051(9) 0.110(14) 0.26(3) 0.038(16) -0.065(14) -0.002(9) I1 0.0336(3) 0.0459(3) 0.0441(3) -0.0107(2) -0.0149(2) 0.0054(2) Pd1 0.0293(3) 0.0302(3) 0.0381(3) -0.0066(2) -0.0147(2) 0.0060(2) N2 0.036(4) 0.046(4) 0.042(4) -0.018(3) -0.018(3) 0.016(3) N3 0.051(4) 0.040(4) 0.044(4) -0.015(3) -0.020(3) 0.013(3) C1 0.030(4) 0.031(4) 0.037(4) -0.006(3) -0.014(3) 0.008(3) C12 0.040(4) 0.031(4) 0.044(4) -0.014(3) -0.016(4) 0.002(3) C9 0.069(7) 0.055(5) 0.052(5) -0.022(4) -0.039(5) 0.020(5) C11 0.048(5) 0.028(4) 0.049(5) -0.002(3) -0.029(4) 0.005(3) C13 0.031(4) 0.031(4) 0.045(4) -0.008(3) -0.015(3) 0.001(3) C2 0.037(4) 0.028(4) 0.046(4) -0.005(3) -0.024(4) 0.008(3) C14 0.030(4) 0.058(6) 0.057(5) -0.006(4) -0.014(4) 0.005(4) C3 0.030(4) 0.030(4) 0.044(4) -0.007(3) -0.014(3) 0.008(3) C8 0.034(4) 0.051(5) 0.047(5) -0.007(4) -0.014(4) 0.003(4) C5 0.033(4) 0.049(5) 0.055(5) -0.019(4) -0.021(4) 0.000(4) C6 0.046(6) 0.064(6) 0.066(6) -0.019(5) -0.027(5) 0.006(5) C7 0.027(4) 0.067(6) 0.053(5) -0.009(5) -0.011(4) -0.003(4) N1 0.037(4) 0.033(3) 0.042(4) -0.012(3) -0.024(3) 0.016(3) C4 0.025(4) 0.035(4) 0.040(4) -0.005(3) -0.006(3) 0.003(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I3 Pd3 2.6683(9) . ? I3 Pd2 2.7045(9) . ? I2 Pd2 2.6482(10) . ? I2 Pd3 2.6901(9) . ? Pd2 C201 2.010(9) . ? Pd2 C204 2.047(8) . ? Pd3 C301 1.979(8) . ? Pd3 C304 2.031(8) . ? N303 N302 1.327(10) . ? N303 C302 1.367(10) . ? N303 C309 1.444(11) . ? N302 N301 1.348(10) . ? N301 C301 1.384(10) . ? N301 C303 1.401(11) . ? C201 N201 1.354(10) . ? C201 C202 1.370(13) . ? N201 N202 1.324(10) . ? N201 C203 1.391(11) . ? N202 N203 1.309(10) . ? C306 C305 1.387(13) . ? C306 C307 1.392(15) . ? C306 H306 0.93 . ? N203 C202 1.405(11) . ? N203 C209 1.465(12) . ? C305 C304 1.403(12) . ? C305 H305 0.93 . ? C211 C202 1.465(12) . ? C211 C212 1.560(13) . ? C211 H21A 0.97 . ? C211 H21B 0.97 . ? C308 C303 1.359(12) . ? C308 C307 1.395(13) . ? C308 H308 0.93 . ? C206 C207 1.377(16) . ? C206 C205 1.425(14) . ? C206 H206 0.93 . ? C207 C208 1.403(14) . ? C207 H207 0.93 . ? C212 C213 1.505(13) . ? C212 H21C 0.97 . ? C212 H21D 0.97 . ? C208 C203 1.382(12) . ? C208 H208 0.93 . ? C301 C302 1.389(12) . ? C204 C205 1.372(13) . ? C204 C203 1.398(13) . ? C304 C303 1.417(12) . ? C311 C312 1.517(11) . ? C311 C302 1.520(12) . ? C311 H31A 0.97 . ? C311 H31B 0.97 . ? C312 C313 1.527(15) . ? C312 H31C 0.97 . ? C312 H31D 0.97 . ? C205 H205 0.93 . ? C209 H20A 0.96 . ? C209 H20B 0.96 . ? C209 H20C 0.96 . ? C307 H307 0.93 . ? C213 C214 1.513(15) . ? C213 H21E 0.97 . ? C213 H21F 0.97 . ? C214 H21G 0.96 . ? C214 H21H 0.96 . ? C214 H21I 0.96 . ? C313 C314 1.33(3) . ? C313 H31E 0.97 . ? C313 H31F 0.97 . ? C309 H30A 0.96 . ? C309 H30B 0.96 . ? C309 H30C 0.96 . ? C314 H31G 0.96 . ? C314 H31H 0.96 . ? C314 H31I 0.96 . ? I1 Pd1 2.6539(9) . ? I1 Pd1 2.6842(8) 2_676 ? Pd1 C1 1.983(8) . ? Pd1 C4 2.034(8) . ? Pd1 I1 2.6842(8) 2_676 ? N2 N1 1.325(10) . ? N2 N3 1.330(11) . ? N3 C2 1.350(12) . ? N3 C9 1.471(12) . ? C1 N1 1.365(10) . ? C1 C2 1.385(11) . ? C12 C13 1.497(11) . ? C12 C11 1.559(11) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C11 C2 1.511(11) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C13 C14 1.528(12) . ? C13 H13A 0.97 . ? C13 H13B 0.97 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C3 C8 1.381(12) . ? C3 C4 1.393(12) . ? C3 N1 1.426(11) . ? C8 C7 1.396(14) . ? C8 H8 0.93 . ? C5 C4 1.394(12) . ? C5 C6 1.399(14) . ? C5 H5 0.93 . ? C6 C7 1.363(15) . ? C6 H6 0.93 . ? C7 H7 0.93 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd3 I3 Pd2 87.33(3) . . ? Pd2 I2 Pd3 88.04(3) . . ? C201 Pd2 C204 80.7(3) . . ? C201 Pd2 I2 175.1(2) . . ? C204 Pd2 I2 94.9(3) . . ? C201 Pd2 I3 97.8(2) . . ? C204 Pd2 I3 176.1(2) . . ? I2 Pd2 I3 86.72(3) . . ? C301 Pd3 C304 81.1(3) . . ? C301 Pd3 I3 176.3(2) . . ? C304 Pd3 I3 95.3(3) . . ? C301 Pd3 I2 96.8(2) . . ? C304 Pd3 I2 172.3(2) . . ? I3 Pd3 I2 86.61(3) . . ? N302 N303 C302 113.3(7) . . ? N302 N303 C309 118.6(7) . . ? C302 N303 C309 128.1(7) . . ? N303 N302 N301 102.4(6) . . ? N302 N301 C301 115.0(7) . . ? N302 N301 C303 125.5(7) . . ? C301 N301 C303 119.3(7) . . ? N201 C201 C202 104.8(8) . . ? N201 C201 Pd2 112.2(6) . . ? C202 C201 Pd2 142.9(6) . . ? N202 N201 C201 115.1(7) . . ? N202 N201 C203 124.1(7) . . ? C201 N201 C203 120.9(7) . . ? N203 N202 N201 102.8(7) . . ? C305 C306 C307 120.9(9) . . ? C305 C306 H306 119.5 . . ? C307 C306 H306 119.5 . . ? N202 N203 C202 113.3(7) . . ? N202 N203 C209 118.8(7) . . ? C202 N203 C209 127.9(8) . . ? C306 C305 C304 121.2(9) . . ? C306 C305 H305 119.4 . . ? C304 C305 H305 119.4 . . ? C202 C211 C212 113.7(7) . . ? C202 C211 H21A 108.8 . . ? C212 C211 H21A 108.8 . . ? C202 C211 H21B 108.8 . . ? C212 C211 H21B 108.8 . . ? H21A C211 H21B 107.7 . . ? C303 C308 C307 118.9(9) . . ? C303 C308 H308 120.6 . . ? C307 C308 H308 120.6 . . ? C207 C206 C205 121.4(9) . . ? C207 C206 H206 119.3 . . ? C205 C206 H206 119.3 . . ? C206 C207 C208 118.9(8) . . ? C206 C207 H207 120.5 . . ? C208 C207 H207 120.5 . . ? C213 C212 C211 112.0(8) . . ? C213 C212 H21C 109.2 . . ? C211 C212 H21C 109.2 . . ? C213 C212 H21D 109.2 . . ? C211 C212 H21D 109.2 . . ? H21C C212 H21D 107.9 . . ? C203 C208 C207 118.5(9) . . ? C203 C208 H208 120.7 . . ? C207 C208 H208 120.7 . . ? N301 C301 C302 102.1(7) . . ? N301 C301 Pd3 113.2(6) . . ? C302 C301 Pd3 144.6(6) . . ? C205 C204 C203 117.5(8) . . ? C205 C204 Pd2 128.9(7) . . ? C203 C204 Pd2 113.6(6) . . ? C305 C304 C303 115.5(8) . . ? C305 C304 Pd3 130.2(7) . . ? C303 C304 Pd3 114.2(6) . . ? C312 C311 C302 113.7(7) . . ? C312 C311 H31A 108.8 . . ? C302 C311 H31A 108.8 . . ? C312 C311 H31B 108.8 . . ? C302 C311 H31B 108.8 . . ? H31A C311 H31B 107.7 . . ? C311 C312 C313 114.0(8) . . ? C311 C312 H31C 108.8 . . ? C313 C312 H31C 108.8 . . ? C311 C312 H31D 108.8 . . ? C313 C312 H31D 108.8 . . ? H31C C312 H31D 107.6 . . ? C204 C205 C206 119.9(10) . . ? C204 C205 H205 120 . . ? C206 C205 H205 120 . . ? C308 C303 N301 124.1(8) . . ? C308 C303 C304 124.1(8) . . ? N301 C303 C304 111.8(7) . . ? N203 C209 H20A 109.5 . . ? N203 C209 H20B 109.5 . . ? H20A C209 H20B 109.5 . . ? N203 C209 H20C 109.5 . . ? H20A C209 H20C 109.5 . . ? H20B C209 H20C 109.5 . . ? N303 C302 C301 107.2(7) . . ? N303 C302 C311 121.5(8) . . ? C301 C302 C311 131.3(8) . . ? C306 C307 C308 119.3(9) . . ? C306 C307 H307 120.4 . . ? C308 C307 H307 120.4 . . ? C201 C202 N203 104.1(7) . . ? C201 C202 C211 134.9(8) . . ? N203 C202 C211 121.1(8) . . ? C212 C213 C214 113.7(9) . . ? C212 C213 H21E 108.8 . . ? C214 C213 H21E 108.8 . . ? C212 C213 H21F 108.8 . . ? C214 C213 H21F 108.8 . . ? H21E C213 H21F 107.7 . . ? C208 C203 N201 123.7(8) . . ? C208 C203 C204 123.7(8) . . ? N201 C203 C204 112.6(7) . . ? C213 C214 H21G 109.5 . . ? C213 C214 H21H 109.5 . . ? H21G C214 H21H 109.5 . . ? C213 C214 H21I 109.5 . . ? H21G C214 H21I 109.5 . . ? H21H C214 H21I 109.5 . . ? C314 C313 C312 119.6(17) . . ? C314 C313 H31E 107.4 . . ? C312 C313 H31E 107.4 . . ? C314 C313 H31F 107.4 . . ? C312 C313 H31F 107.4 . . ? H31E C313 H31F 107 . . ? N303 C309 H30A 109.5 . . ? N303 C309 H30B 109.5 . . ? H30A C309 H30B 109.5 . . ? N303 C309 H30C 109.5 . . ? H30A C309 H30C 109.5 . . ? H30B C309 H30C 109.5 . . ? C313 C314 H31G 109.5 . . ? C313 C314 H31H 109.5 . . ? H31G C314 H31H 109.5 . . ? C313 C314 H31I 109.5 . . ? H31G C314 H31I 109.5 . . ? H31H C314 H31I 109.5 . . ? Pd1 I1 Pd1 93.50(3) . 2_676 ? C1 Pd1 C4 80.6(3) . . ? C1 Pd1 I1 174.5(2) . . ? C4 Pd1 I1 95.7(2) . . ? C1 Pd1 I1 97.6(2) . 2_676 ? C4 Pd1 I1 174.1(2) . 2_676 ? I1 Pd1 I1 86.50(3) . 2_676 ? N1 N2 N3 101.1(6) . . ? N2 N3 C2 113.3(7) . . ? N2 N3 C9 117.3(8) . . ? C2 N3 C9 129.4(8) . . ? N1 C1 C2 100.8(7) . . ? N1 C1 Pd1 113.9(6) . . ? C2 C1 Pd1 145.2(6) . . ? C13 C12 C11 111.0(7) . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C11 C12 113.3(7) . . ? C2 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C2 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C12 C13 C14 112.1(7) . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N3 C2 C1 107.6(7) . . ? N3 C2 C11 121.6(8) . . ? C1 C2 C11 130.7(8) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C3 C4 125.4(8) . . ? C8 C3 N1 123.1(8) . . ? C4 C3 N1 111.5(7) . . ? C3 C8 C7 117.0(9) . . ? C3 C8 H8 121.5 . . ? C7 C8 H8 121.5 . . ? C4 C5 C6 119.8(9) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 122.3(10) . . ? C7 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C6 C7 C8 119.6(9) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? N2 N1 C1 117.2(7) . . ? N2 N1 C3 123.9(7) . . ? C1 N1 C3 118.9(7) . . ? C3 C4 C5 115.8(7) . . ? C3 C4 Pd1 115.1(6) . . ? C5 C4 Pd1 129.0(6) . . ? #################################################END data_complex-5f _audit_creation_date 2010-09-22T15:58:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _chemical_name_systematic ; ? ; _chemical_formula_sum 'C15.67 H13.33 Cl1.33 I N3 Pd' _chemical_formula_weight 524.19 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.4702(14) _cell_length_b 20.6531(10) _cell_length_c 16.2193(10) _cell_angle_alpha 90 _cell_angle_beta 91.153(6) _cell_angle_gamma 90 _cell_volume 5181.1(6) _cell_formula_units_Z 12 _cell_measurement_temperature 100 _cell_measurement_reflns_used 19545 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 26.76 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 21 -30 -26 0.1396 -11 30 -13 0.0777 -22 28 30 0.164 3 -30 12 0.0777 22 30 -21 0.1245 -29 -30 -13 0.1819 20 30 13 0.1705 -3 -23 30 0.0977 _exptl_special_details ; ? ; _exptl_absorpt_coefficient_mu 3.067 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3984 _exptl_absorpt_correction_T_max 0.6435 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_reflns_av_R_equivalents 0.1104 _diffrn_reflns_av_unetI/netI 0.0981 _diffrn_reflns_number 35537 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.953 _reflns_number_total 9049 _reflns_number_gt 5522 _reflns_threshold_expression >2\s(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_special_details ; Crystals of AP607 contain volatile solvent and therefore cooling was necessary throughout the mounting procedure in order to afford a sufficiently diffracting specimen. During the refinement, not all solvent molecules could be resolved due to disorder and were thus removed by the SQUEEZE routine in PLATON. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 9049 _refine_ls_number_parameters 598 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.063 _refine_ls_wR_factor_ref 0.1574 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.633 _refine_diff_density_min -1.24 _refine_diff_density_rms 0.185 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4866(9) 0.0087(5) 1.2330(6) 0.038(3) Uani 1 1 d . . . C2 C 0.4129(10) 0.0058(5) 1.2789(6) 0.043(4) Uani 1 1 d . . . C3 C 0.6370(10) 0.0084(5) 1.2704(7) 0.045(3) Uani 1 1 d . . . C4 C 0.6448(10) 0.0108(6) 1.1844(8) 0.047(3) Uani 1 1 d . . . C5 C 0.7322(12) 0.0141(6) 1.1580(10) 0.060(4) Uani 1 1 d . . . H5 H 0.7439 0.0161 1.102 0.073 Uiso 1 1 calc R . . C6 C 0.8014(11) 0.0142(6) 1.2171(11) 0.062(4) Uani 1 1 d . . . H6 H 0.8581 0.0173 1.1996 0.074 Uiso 1 1 calc R . . C7 C 0.7846(15) 0.0098(7) 1.3008(11) 0.074(5) Uani 1 1 d . . . H7 H 0.8307 0.0078 1.3384 0.088 Uiso 1 1 calc R . . C8 C 0.7019(12) 0.0084(6) 1.3290(9) 0.056(4) Uani 1 1 d . . . H8 H 0.6904 0.0074 1.3851 0.067 Uiso 1 1 calc R . . C9 C 0.3862(15) 0.0064(8) 1.4322(8) 0.084(7) Uani 1 1 d . . . H9A H 0.3668 -0.0368 1.4441 0.127 Uiso 1 1 calc R . . H9B H 0.337 0.034 1.4229 0.127 Uiso 1 1 calc R . . H9C H 0.4199 0.0225 1.4781 0.127 Uiso 1 1 calc R . . C11 C 0.3186(10) 0.0090(7) 1.2521(7) 0.048(3) Uani 1 1 d . . . C12 C 0.2841(11) 0.0594(7) 1.2077(7) 0.050(4) Uani 1 1 d . . . H12 H 0.32 0.0935 1.1932 0.06 Uiso 1 1 calc R . . C13 C 0.2014(12) 0.0615(8) 1.1846(8) 0.061(4) Uani 1 1 d . . . H13 H 0.1809 0.0976 1.1559 0.073 Uiso 1 1 calc R . . C14 C 0.1434(13) 0.0105(7) 1.2023(10) 0.070(5) Uani 1 1 d . . . H14 H 0.0865 0.0099 1.1828 0.084 Uiso 1 1 calc R . . C15 C 0.1795(14) -0.0402(10) 1.2528(19) 0.124(11) Uani 1 1 d . . . H15 H 0.1429 -0.0731 1.2697 0.148 Uiso 1 1 calc R . . C16 C 0.2619(13) -0.0427(7) 1.2770(12) 0.075(6) Uani 1 1 d . . . H16 H 0.2827 -0.0769 1.309 0.09 Uiso 1 1 calc R . . C98 C 0.6410(11) 0.3612(8) 0.3737(10) 0.066(4) Uani 1 1 d . . . H98A H 0.6394 0.3143 0.3715 0.08 Uiso 1 1 calc R . . H98B H 0.6829 0.3761 0.3343 0.08 Uiso 1 1 calc R . . C99 C 0.4209(11) 0.3506(8) 0.5288(8) 0.063(4) Uani 1 1 d . . . H99A H 0.3881 0.3176 0.557 0.075 Uiso 1 1 calc R . . H99B H 0.4587 0.3292 0.4903 0.075 Uiso 1 1 calc R . . C201 C 0.4117(7) 0.1724(5) 0.6562(6) 0.026(2) Uani 1 1 d . . . C202 C 0.4510(8) 0.1789(5) 0.7327(6) 0.031(3) Uani 1 1 d . . . C203 C 0.2640(8) 0.1554(5) 0.6065(6) 0.032(3) Uani 1 1 d . . . C204 C 0.3027(8) 0.1594(6) 0.5299(7) 0.035(3) Uani 1 1 d . . . C205 C 0.2471(9) 0.1505(8) 0.4637(8) 0.057(4) Uani 1 1 d . . . H205 H 0.2685 0.1512 0.4105 0.068 Uiso 1 1 calc R . . C206 C 0.1586(11) 0.1405(10) 0.4752(10) 0.079(5) Uani 1 1 d . . . H206 H 0.1222 0.1358 0.4293 0.095 Uiso 1 1 calc R . . C207 C 0.1243(11) 0.1375(11) 0.5522(11) 0.083(6) Uani 1 1 d . . . H207 H 0.0653 0.1306 0.558 0.1 Uiso 1 1 calc R . . C208 C 0.1760(9) 0.1444(6) 0.6203(8) 0.046(3) Uani 1 1 d . . . H208 H 0.1543 0.1421 0.6733 0.055 Uiso 1 1 calc R . . C209 C 0.3873(9) 0.1711(6) 0.8770(6) 0.040(3) Uani 1 1 d . . . H20A H 0.3335 0.1867 0.8979 0.06 Uiso 1 1 calc R . . H20B H 0.4333 0.1992 0.895 0.06 Uiso 1 1 calc R . . H20C H 0.398 0.1281 0.8973 0.06 Uiso 1 1 calc R . . C211 C 0.5367(7) 0.1931(5) 0.7581(5) 0.025(2) Uani 1 1 d . . . C212 C 0.5784(9) 0.2508(6) 0.7343(7) 0.041(3) Uani 1 1 d . . . H212 H 0.5492 0.2791 0.699 0.049 Uiso 1 1 calc R . . C213 C 0.6587(10) 0.2664(7) 0.7609(7) 0.048(3) Uani 1 1 d . . . H213 H 0.6826 0.306 0.7466 0.058 Uiso 1 1 calc R . . C214 C 0.7071(9) 0.2222(6) 0.8109(6) 0.040(3) Uani 1 1 d . . . H214 H 0.7642 0.2308 0.8262 0.048 Uiso 1 1 calc R . . C215 C 0.6656(9) 0.1649(6) 0.8365(6) 0.039(3) Uani 1 1 d . . . H215 H 0.6947 0.1363 0.8716 0.047 Uiso 1 1 calc R . . C216 C 0.5835(8) 0.1511(6) 0.8105(6) 0.031(2) Uani 1 1 d . . . H216 H 0.5577 0.1129 0.8278 0.037 Uiso 1 1 calc R . . C301 C 0.6380(8) 0.1893(5) 0.2580(6) 0.029(2) Uani 1 1 d . . . C302 C 0.5987(7) 0.1973(5) 0.1819(6) 0.025(2) Uani 1 1 d . . . C303 C 0.7850(8) 0.1737(5) 0.3038(6) 0.028(2) Uani 1 1 d . . . C304 C 0.7469(8) 0.1750(5) 0.3806(7) 0.032(2) Uani 1 1 d . . . C305 C 0.8040(10) 0.1665(6) 0.4491(8) 0.051(3) Uani 1 1 d . . . H305 H 0.7826 0.1648 0.5022 0.061 Uiso 1 1 calc R . . C306 C 0.8936(10) 0.1605(8) 0.4360(9) 0.059(4) Uani 1 1 d . . . H306 H 0.9309 0.1568 0.4814 0.071 Uiso 1 1 calc R . . C307 C 0.9273(11) 0.1600(7) 0.3590(9) 0.056(4) Uani 1 1 d . . . H307 H 0.9864 0.1545 0.3527 0.068 Uiso 1 1 calc R . . C308 C 0.8755(9) 0.1675(6) 0.2917(8) 0.041(3) Uani 1 1 d . . . H308 H 0.8982 0.1685 0.2391 0.05 Uiso 1 1 calc R . . C309 C 0.6560(10) 0.1931(7) 0.0369(6) 0.051(4) Uani 1 1 d . . . H30A H 0.7095 0.2074 0.0141 0.076 Uiso 1 1 calc R . . H30B H 0.6106 0.2225 0.021 0.076 Uiso 1 1 calc R . . H30C H 0.6424 0.1506 0.0164 0.076 Uiso 1 1 calc R . . C311 C 0.5101(7) 0.2101(5) 0.1582(6) 0.026(2) Uani 1 1 d . . . C312 C 0.4621(7) 0.1696(5) 0.1051(5) 0.026(2) Uani 1 1 d . . . H312 H 0.4889 0.1335 0.0828 0.032 Uiso 1 1 calc R . . C313 C 0.3788(9) 0.1812(6) 0.0853(7) 0.039(3) Uani 1 1 d . . . H313 H 0.3486 0.1531 0.0503 0.046 Uiso 1 1 calc R . . C314 C 0.3378(9) 0.2355(7) 0.1175(7) 0.045(3) Uani 1 1 d . . . H314 H 0.2801 0.2441 0.1047 0.054 Uiso 1 1 calc R . . C315 C 0.3835(9) 0.2750(6) 0.1673(8) 0.045(3) Uani 1 1 d . . . H315 H 0.3556 0.3108 0.1891 0.054 Uiso 1 1 calc R . . C316 C 0.4682(9) 0.2659(5) 0.1880(7) 0.039(3) Uani 1 1 d . . . H316 H 0.4979 0.2957 0.2209 0.047 Uiso 1 1 calc R . . N1 N 0.5489(8) 0.0061(5) 1.2917(6) 0.043(3) Uani 1 1 d . . . N2 N 0.5215(11) 0.0046(5) 1.3689(6) 0.057(4) Uani 1 1 d . . . N3 N 0.4385(10) 0.0055(5) 1.3593(6) 0.052(3) Uani 1 1 d . . . N201 N 0.3251(6) 0.1623(4) 0.6718(5) 0.0240(19) Uani 1 1 d . . . N202 N 0.3067(7) 0.1612(4) 0.7524(5) 0.029(2) Uani 1 1 d . . . N203 N 0.3827(6) 0.1700(4) 0.7867(5) 0.027(2) Uani 1 1 d . . . N301 N 0.7236(6) 0.1815(4) 0.2404(5) 0.030(2) Uani 1 1 d . . . N302 N 0.7406(7) 0.1828(5) 0.1592(5) 0.037(2) Uani 1 1 d . . . N303 N 0.6641(6) 0.1911(4) 0.1266(5) 0.030(2) Uani 1 1 d . . . Cl96 Cl 0.3492(3) 0.4022(2) 0.4739(2) 0.0717(11) Uani 1 1 d . . . Cl97 Cl 0.4834(3) 0.3939(2) 0.6009(2) 0.0709(11) Uani 1 1 d . . . Cl98 Cl 0.5369(3) 0.3927(2) 0.3464(2) 0.0648(10) Uani 1 1 d . . . Cl99 Cl 0.6728(3) 0.3856(2) 0.4717(2) 0.0781(12) Uani 1 1 d . . . Pd1 Pd 0.53525(6) 0.00702(4) 1.11700(5) 0.0327(2) Uani 1 1 d . . . Pd2 Pd 0.43134(6) 0.17419(4) 0.53332(4) 0.0260(2) Uani 1 1 d . . . Pd3 Pd 0.61769(6) 0.18325(4) 0.38021(4) 0.0260(2) Uani 1 1 d . . . I1 I 0.61313(6) 0.00502(4) 0.97287(4) 0.0471(2) Uani 1 1 d . . . I2 I 0.44415(6) 0.18343(4) 0.37224(4) 0.0438(2) Uani 1 1 d . . . I3 I 0.60333(6) 0.18377(5) 0.54135(4) 0.0467(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.069(10) 0.022(6) 0.022(5) -0.002(4) -0.004(5) 0.005(5) C2 0.084(12) 0.033(6) 0.014(5) -0.001(4) 0.023(6) -0.003(6) C3 0.066(11) 0.023(6) 0.046(7) 0.001(5) -0.023(7) 0.010(6) C4 0.042(9) 0.026(6) 0.071(9) 0.009(6) -0.015(7) 0.008(5) C5 0.075(13) 0.029(7) 0.078(10) -0.004(6) -0.014(9) -0.006(7) C6 0.035(9) 0.043(8) 0.106(13) 0.011(8) -0.020(8) -0.010(6) C7 0.109(18) 0.040(8) 0.071(10) 0.002(7) -0.018(10) -0.007(9) C8 0.075(13) 0.037(7) 0.055(8) 0.008(6) -0.008(8) -0.004(7) C9 0.16(2) 0.071(10) 0.029(7) -0.007(7) 0.038(9) -0.008(11) C11 0.047(9) 0.060(8) 0.037(6) 0.002(6) 0.020(6) 0.011(7) C12 0.062(11) 0.055(8) 0.035(6) 0.000(6) 0.019(7) -0.005(7) C13 0.064(12) 0.077(10) 0.042(7) -0.012(7) 0.012(7) -0.006(8) C14 0.076(13) 0.056(10) 0.077(10) 0.009(8) 0.012(9) -0.008(9) C15 0.050(14) 0.066(12) 0.26(3) 0.007(15) 0.056(18) 0.005(10) C16 0.073(14) 0.049(9) 0.105(13) 0.011(8) 0.052(11) 0.003(8) C98 0.040(10) 0.078(11) 0.082(10) -0.021(9) 0.011(8) 0.007(8) C99 0.065(12) 0.074(10) 0.050(8) 0.013(7) 0.017(8) -0.003(8) C201 0.021(6) 0.035(6) 0.023(5) -0.007(4) -0.005(4) 0.001(4) C202 0.036(7) 0.029(6) 0.027(5) 0.009(4) 0.009(5) 0.002(5) C203 0.036(8) 0.038(6) 0.022(5) 0.002(4) -0.008(5) 0.001(5) C204 0.023(7) 0.042(7) 0.040(6) 0.009(5) -0.011(5) -0.001(5) C205 0.030(8) 0.103(11) 0.038(7) 0.016(7) -0.003(6) 0.003(8) C206 0.027(10) 0.141(16) 0.068(10) 0.035(10) -0.021(8) -0.004(10) C207 0.017(9) 0.154(18) 0.079(11) 0.038(11) -0.009(8) -0.010(10) C208 0.027(8) 0.055(8) 0.055(7) 0.013(6) -0.009(6) -0.003(6) C209 0.053(9) 0.043(7) 0.025(5) 0.003(5) 0.013(5) -0.009(6) C211 0.034(7) 0.030(6) 0.012(4) -0.004(4) 0.003(4) -0.005(5) C212 0.046(9) 0.050(7) 0.027(5) 0.005(5) 0.015(5) 0.000(6) C213 0.047(10) 0.065(9) 0.034(6) 0.000(6) 0.008(6) -0.015(7) C214 0.032(8) 0.064(8) 0.025(5) -0.018(5) -0.006(5) -0.014(6) C215 0.041(8) 0.061(8) 0.015(5) -0.008(5) -0.005(5) -0.005(6) C216 0.026(7) 0.041(6) 0.026(5) -0.003(5) -0.001(4) -0.003(5) C301 0.025(7) 0.030(6) 0.031(5) -0.010(4) -0.010(4) -0.005(5) C302 0.025(7) 0.028(5) 0.022(5) -0.009(4) 0.002(4) -0.003(4) C303 0.027(7) 0.021(5) 0.036(5) -0.007(4) -0.004(5) 0.001(4) C304 0.017(6) 0.036(6) 0.043(6) 0.005(5) -0.004(5) 0.007(5) C305 0.044(10) 0.056(8) 0.051(7) -0.012(6) -0.003(6) -0.012(6) C306 0.038(10) 0.085(11) 0.054(8) 0.001(7) -0.012(7) 0.009(8) C307 0.055(11) 0.059(9) 0.056(8) 0.000(7) 0.009(8) 0.011(7) C308 0.027(7) 0.042(7) 0.055(7) -0.010(5) 0.000(6) -0.001(5) C309 0.053(10) 0.089(10) 0.010(5) -0.007(5) 0.001(5) 0.003(7) C311 0.030(7) 0.027(5) 0.022(5) 0.006(4) 0.011(4) 0.003(4) C312 0.032(7) 0.035(6) 0.013(4) 0.006(4) 0.002(4) 0.000(5) C313 0.042(8) 0.046(7) 0.028(5) 0.006(5) -0.002(5) 0.002(6) C314 0.027(8) 0.071(9) 0.037(6) 0.020(6) -0.002(5) 0.000(6) C315 0.037(9) 0.046(7) 0.052(7) 0.011(6) 0.018(6) 0.022(6) C316 0.039(8) 0.036(6) 0.043(6) -0.005(5) 0.005(6) -0.001(5) N1 0.063(9) 0.031(5) 0.034(5) -0.008(4) -0.023(5) 0.011(5) N2 0.112(13) 0.034(6) 0.026(5) -0.007(4) -0.002(6) 0.017(7) N3 0.087(11) 0.050(7) 0.019(4) 0.006(4) 0.012(5) 0.021(7) N201 0.025(6) 0.029(5) 0.018(4) 0.000(3) 0.000(4) -0.002(4) N202 0.032(6) 0.037(5) 0.018(4) 0.005(3) 0.006(4) 0.004(4) N203 0.024(6) 0.042(5) 0.016(4) 0.003(3) 0.003(4) -0.003(4) N301 0.019(5) 0.034(5) 0.036(5) -0.002(4) 0.001(4) 0.003(4) N302 0.038(7) 0.045(6) 0.029(5) -0.011(4) 0.009(5) -0.005(5) N303 0.021(6) 0.054(6) 0.017(4) -0.009(4) 0.008(4) -0.006(4) Cl96 0.047(3) 0.100(3) 0.068(2) 0.013(2) -0.0013(19) 0.002(2) Cl97 0.044(2) 0.101(3) 0.068(2) 0.017(2) -0.0003(18) -0.004(2) Cl98 0.054(3) 0.075(3) 0.066(2) -0.0121(18) 0.0004(18) 0.0017(19) Cl99 0.060(3) 0.116(4) 0.058(2) -0.005(2) 0.006(2) 0.007(2) Pd1 0.0409(6) 0.0320(5) 0.0255(4) 0.0004(3) 0.0045(4) 0.0024(4) Pd2 0.0266(5) 0.0340(4) 0.0173(4) 0.0035(3) -0.0015(3) -0.0004(4) Pd3 0.0259(5) 0.0326(4) 0.0194(4) -0.0040(3) -0.0006(3) -0.0003(3) I1 0.0523(6) 0.0572(5) 0.0319(4) -0.0015(3) 0.0070(4) 0.0006(4) I2 0.0378(5) 0.0659(5) 0.0276(4) 0.0018(3) 0.0020(3) -0.0025(4) I3 0.0377(5) 0.0740(6) 0.0283(4) 0.0010(4) 0.0028(3) -0.0045(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(17) . ? C1 C2 1.375(18) . ? C1 Pd1 2.040(10) . ? C2 N3 1.356(16) . ? C2 C11 1.51(2) . ? C3 C8 1.37(2) . ? C3 C4 1.404(18) . ? C3 N1 1.413(19) . ? C4 C5 1.43(2) . ? C4 Pd1 2.000(14) . ? C5 C6 1.42(2) . ? C6 C7 1.39(2) . ? C7 C8 1.37(3) . ? C9 N3 1.447(16) . ? C11 C12 1.368(19) . ? C11 C16 1.44(2) . ? C12 C13 1.33(2) . ? C13 C14 1.42(2) . ? C14 C15 1.43(3) . ? C15 C16 1.33(3) . ? C98 Cl99 1.728(17) . ? C98 Cl98 1.784(17) . ? C99 Cl97 1.747(17) . ? C99 Cl96 1.766(17) . ? C201 C202 1.377(15) . ? C201 N201 1.385(14) . ? C201 Pd2 2.022(9) . ? C202 N203 1.398(13) . ? C202 C211 1.412(17) . ? C203 C204 1.393(15) . ? C203 C208 1.402(18) . ? C203 N201 1.413(15) . ? C204 C205 1.375(19) . ? C204 Pd2 2.013(12) . ? C205 C206 1.40(2) . ? C206 C207 1.37(2) . ? C207 C208 1.36(2) . ? C209 N203 1.465(13) . ? C211 C216 1.404(16) . ? C211 C212 1.412(15) . ? C212 C213 1.347(19) . ? C213 C214 1.42(2) . ? C214 C215 1.414(17) . ? C215 C216 1.360(17) . ? C301 N301 1.370(15) . ? C301 C302 1.375(15) . ? C301 Pd3 2.017(10) . ? C302 N303 1.372(12) . ? C302 C311 1.440(16) . ? C303 C304 1.389(14) . ? C303 N301 1.395(15) . ? C303 C308 1.422(17) . ? C304 C305 1.416(19) . ? C304 Pd3 2.007(12) . ? C305 C306 1.41(2) . ? C306 C307 1.363(18) . ? C307 C308 1.35(2) . ? C309 N303 1.460(13) . ? C311 C312 1.402(15) . ? C311 C316 1.412(15) . ? C312 C313 1.343(17) . ? C313 C314 1.396(18) . ? C314 C315 1.34(2) . ? C315 C316 1.359(19) . ? N1 N2 1.331(14) . ? N2 N3 1.291(18) . ? N201 N202 1.343(10) . ? N202 N203 1.304(13) . ? N301 N302 1.348(12) . ? N302 N303 1.297(14) . ? Pd1 I1 2.6518(11) . ? Pd1 I1 2.7056(14) 3_657 ? Pd2 I2 2.6309(10) . ? Pd2 I3 2.6685(13) . ? Pd3 I3 2.6275(10) . ? Pd3 I2 2.6853(13) . ? I1 Pd1 2.7056(14) 3_657 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 101.9(10) . . ? N1 C1 Pd1 112.3(10) . . ? C2 C1 Pd1 145.4(11) . . ? N3 C2 C1 107.0(14) . . ? N3 C2 C11 122.4(11) . . ? C1 C2 C11 130.3(10) . . ? C8 C3 C4 127.9(15) . . ? C8 C3 N1 121.9(12) . . ? C4 C3 N1 110.2(12) . . ? C3 C4 C5 113.6(14) . . ? C3 C4 Pd1 117.0(11) . . ? C5 C4 Pd1 129.4(11) . . ? C6 C5 C4 120.1(15) . . ? C7 C6 C5 120.4(16) . . ? C8 C7 C6 121.5(18) . . ? C7 C8 C3 116.4(15) . . ? C12 C11 C16 118.4(16) . . ? C12 C11 C2 123.2(13) . . ? C16 C11 C2 118.3(13) . . ? C13 C12 C11 122.6(14) . . ? C12 C13 C14 121.8(17) . . ? C13 C14 C15 114.8(19) . . ? C16 C15 C14 123.9(18) . . ? C15 C16 C11 118.3(18) . . ? Cl99 C98 Cl98 111.2(8) . . ? Cl97 C99 Cl96 111.2(9) . . ? C202 C201 N201 105.1(8) . . ? C202 C201 Pd2 144.5(9) . . ? N201 C201 Pd2 110.4(7) . . ? C201 C202 N203 103.2(11) . . ? C201 C202 C211 132.6(9) . . ? N203 C202 C211 124.2(10) . . ? C204 C203 C208 126.1(11) . . ? C204 C203 N201 111.8(10) . . ? C208 C203 N201 122.2(10) . . ? C205 C204 C203 114.5(11) . . ? C205 C204 Pd2 130.2(9) . . ? C203 C204 Pd2 115.2(8) . . ? C204 C205 C206 120.9(13) . . ? C207 C206 C205 121.8(14) . . ? C208 C207 C206 120.3(14) . . ? C207 C208 C203 116.4(13) . . ? C216 C211 C202 121.2(9) . . ? C216 C211 C212 117.0(11) . . ? C202 C211 C212 121.8(10) . . ? C213 C212 C211 122.6(12) . . ? C212 C213 C214 120.0(12) . . ? C215 C214 C213 117.9(12) . . ? C216 C215 C214 120.7(12) . . ? C215 C216 C211 121.7(11) . . ? N301 C301 C302 103.8(9) . . ? N301 C301 Pd3 111.6(8) . . ? C302 C301 Pd3 144.5(9) . . ? N303 C302 C301 104.8(10) . . ? N303 C302 C311 123.6(9) . . ? C301 C302 C311 131.5(9) . . ? C304 C303 N301 111.3(9) . . ? C304 C303 C308 124.2(10) . . ? N301 C303 C308 124.5(10) . . ? C303 C304 C305 115.6(11) . . ? C303 C304 Pd3 116.1(8) . . ? C305 C304 Pd3 128.1(9) . . ? C306 C305 C304 119.4(12) . . ? C307 C306 C305 122.3(14) . . ? C308 C307 C306 120.5(14) . . ? C307 C308 C303 118.0(12) . . ? C312 C311 C316 117.1(11) . . ? C312 C311 C302 122.9(9) . . ? C316 C311 C302 119.9(10) . . ? C313 C312 C311 122.4(11) . . ? C312 C313 C314 119.6(12) . . ? C315 C314 C313 118.5(13) . . ? C314 C315 C316 124.0(12) . . ? C315 C316 C311 118.3(12) . . ? N2 N1 C1 115.5(12) . . ? N2 N1 C3 123.9(11) . . ? C1 N1 C3 120.5(10) . . ? N3 N2 N1 102.8(10) . . ? N2 N3 C2 112.7(11) . . ? N2 N3 C9 118.3(13) . . ? C2 N3 C9 129.0(16) . . ? N202 N201 C201 113.9(9) . . ? N202 N201 C203 125.2(9) . . ? C201 N201 C203 120.8(8) . . ? N203 N202 N201 101.9(8) . . ? N202 N203 C202 115.9(8) . . ? N202 N203 C209 117.0(9) . . ? C202 N203 C209 127.1(11) . . ? N302 N301 C301 114.1(9) . . ? N302 N301 C303 125.4(9) . . ? C301 N301 C303 120.5(9) . . ? N303 N302 N301 101.9(8) . . ? N302 N303 C302 115.2(9) . . ? N302 N303 C309 118.0(9) . . ? C302 N303 C309 126.8(11) . . ? C4 Pd1 C1 79.6(6) . . ? C4 Pd1 I1 95.0(4) . . ? C1 Pd1 I1 174.6(4) . . ? C4 Pd1 I1 177.0(3) . 3_657 ? C1 Pd1 I1 100.0(4) . 3_657 ? I1 Pd1 I1 85.37(4) . 3_657 ? C204 Pd2 C201 81.8(5) . . ? C204 Pd2 I2 94.4(3) . . ? C201 Pd2 I2 174.7(3) . . ? C204 Pd2 I3 175.4(3) . . ? C201 Pd2 I3 97.0(3) . . ? I2 Pd2 I3 87.03(3) . . ? C304 Pd3 C301 80.4(5) . . ? C304 Pd3 I3 95.8(3) . . ? C301 Pd3 I3 174.4(3) . . ? C304 Pd3 I2 174.6(3) . . ? C301 Pd3 I2 97.4(3) . . ? I3 Pd3 I2 86.75(3) . . ? Pd1 I1 Pd1 94.63(4) . 3_657 ? Pd2 I2 Pd3 92.71(4) . . ? Pd3 I3 Pd2 93.17(4) . . ? # END of CIF