# Supplementary Material (ESI) data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'ProfD Martin Albrecht' _publ_contact_author_email MARTIN.ALBRECHT@UNIFR.CH _publ_section_title ; Palladation of diimidazolium salts at the C4 position: access to remarkably electron-rich palladium(II) centers ; loop_ _publ_author_name 'Martin Albrecht' 'Marion Heckenrot' 'Evelyne Kluser' 'Antonia Neels' # end Validation Reply Form ########################################### data_7 _database_code_depnum_ccdc_archive 'CCDC 603584' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40.50 H66.50 N8 O8.25 Pd2' _chemical_formula_weight 1010.32 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1967(10) _cell_length_b 13.7943(11) _cell_length_c 16.4100(12) _cell_angle_alpha 68.202(8) _cell_angle_beta 69.115(9) _cell_angle_gamma 86.363(9) _cell_volume 2583.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.75 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1047 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_process_details 'MULABS, (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' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20450 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.92 _reflns_number_total 9375 _reflns_number_gt 6348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1039P)^2^+0.0000P] 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 9375 _refine_ls_number_parameters 529 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1574 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.995 _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 -0.0175(4) 0.0753(4) 0.1855(4) 0.0397(13) Uani 1 1 d . . . C2 C -0.0324(5) 0.0833(5) 0.2691(5) 0.0452(15) Uani 1 1 d . . . H2A H 0.0101 0.0532 0.3070 0.054 Uiso 1 1 calc R . . C3 C -0.1598(5) 0.1710(5) 0.2218(5) 0.0496(16) Uani 1 1 d . . . C4 C -0.1190(4) 0.1378(5) 0.0753(4) 0.0449(15) Uani 1 1 d . . . H4A H -0.1697 0.1922 0.0615 0.054 Uiso 1 1 calc R . . H4B H -0.1534 0.0697 0.0873 0.054 Uiso 1 1 calc R . . C5 C -0.0037(5) 0.2242(5) -0.0938(5) 0.0432(15) Uani 1 1 d . . . C6 C 0.1484(5) 0.1493(5) -0.0891(5) 0.0472(15) Uani 1 1 d . . . H6A H 0.2213 0.1311 -0.1093 0.057 Uiso 1 1 calc R . . C7 C 0.0766(4) 0.1126(5) 0.0005(4) 0.0384(13) Uani 1 1 d . . . C8 C -0.1595(6) 0.1690(7) 0.3753(5) 0.065(2) Uani 1 1 d . . . H8A H -0.2268 0.2071 0.3768 0.078 Uiso 1 1 calc R . . C9 C -0.0746(9) 0.2386(9) 0.3695(8) 0.112(4) Uani 1 1 d . . . H9A H -0.0059 0.2051 0.3605 0.168 Uiso 1 1 calc R . . H9B H -0.0966 0.2518 0.4279 0.168 Uiso 1 1 calc R . . H9C H -0.0650 0.3051 0.3163 0.168 Uiso 1 1 calc R . . C10 C -0.1868(12) 0.0691(10) 0.4629(7) 0.129(5) Uani 1 1 d . . . H10A H -0.2210 0.0864 0.5190 0.194 Uiso 1 1 calc R . . H10B H -0.1200 0.0350 0.4654 0.194 Uiso 1 1 calc R . . H10C H -0.2371 0.0216 0.4607 0.194 Uiso 1 1 calc R . . C11 C -0.2531(6) 0.2358(7) 0.2170(7) 0.078(2) Uani 1 1 d . . . H11A H -0.2432 0.2984 0.2290 0.116 Uiso 1 1 calc R . . H11B H -0.3206 0.1950 0.2645 0.116 Uiso 1 1 calc R . . H11C H -0.2572 0.2569 0.1543 0.116 Uiso 1 1 calc R . . C12 C -0.0839(6) 0.2895(5) -0.1302(5) 0.0551(17) Uani 1 1 d . . . H12C H -0.0494 0.3598 -0.1725 0.083 Uiso 1 1 calc R . . H12B H -0.1462 0.2944 -0.0774 0.083 Uiso 1 1 calc R . . H12A H -0.1087 0.2572 -0.1646 0.083 Uiso 1 1 calc R . . C13 C 0.1507(6) 0.2728(7) -0.2500(5) 0.0648(19) Uani 1 1 d . . . H13A H 0.1029 0.3280 -0.2715 0.078 Uiso 1 1 calc R . . C14 C 0.1606(9) 0.2014(10) -0.2971(7) 0.122(5) Uani 1 1 d . . . H14A H 0.2165 0.1537 -0.2855 0.183 Uiso 1 1 calc R . . H14B H 0.1812 0.2410 -0.3649 0.183 Uiso 1 1 calc R . . H14C H 0.0908 0.1609 -0.2732 0.183 Uiso 1 1 calc R . . C15 C 0.2585(9) 0.3250(9) -0.2752(7) 0.109(4) Uani 1 1 d . . . H15A H 0.2889 0.3646 -0.3432 0.164 Uiso 1 1 calc R . . H15B H 0.3076 0.2720 -0.2570 0.164 Uiso 1 1 calc R . . H15C H 0.2501 0.3729 -0.2420 0.164 Uiso 1 1 calc R . . C16 C 0.2488(4) 0.1758(4) 0.1930(4) 0.0382(13) Uani 1 1 d . . . C17 C 0.2473(5) 0.1771(5) 0.2755(5) 0.0475(15) Uani 1 1 d . . . H17A H 0.2639 0.1212 0.3230 0.057 Uiso 1 1 calc R . . C18 C 0.2005(5) 0.3335(5) 0.2014(5) 0.0485(16) Uani 1 1 d . . . C19 C 0.2111(5) 0.3086(5) 0.0560(5) 0.0487(16) Uani 1 1 d . . . H19A H 0.2020 0.3847 0.0323 0.058 Uiso 1 1 calc R . . H19B H 0.1470 0.2708 0.0602 0.058 Uiso 1 1 calc R . . C20 C 0.3713(5) 0.3505(5) -0.0954(5) 0.0460(15) Uani 1 1 d . . . C21 C 0.4377(5) 0.1947(5) -0.0632(5) 0.0426(14) Uani 1 1 d . . . H21A H 0.4835 0.1405 -0.0715 0.051 Uiso 1 1 calc R . . C22 C 0.3503(4) 0.1850(4) 0.0163(4) 0.0375(13) Uani 1 1 d . . . C23 C 0.2140(8) 0.3115(7) 0.3553(6) 0.081(3) Uani 1 1 d . . . H23A H 0.1623 0.3677 0.3559 0.097 Uiso 1 1 calc R . . C24 C 0.1721(9) 0.2243(9) 0.4487(7) 0.102(3) Uani 1 1 d . . . H24A H 0.1641 0.2509 0.4982 0.153 Uiso 1 1 calc R . . H24B H 0.2234 0.1697 0.4512 0.153 Uiso 1 1 calc R . . H24C H 0.1013 0.1950 0.4581 0.153 Uiso 1 1 calc R . . C25 C 0.3244(12) 0.3595(12) 0.3302(10) 0.164(7) Uani 1 1 d . . . H25A H 0.3797 0.3171 0.3046 0.247 Uiso 1 1 calc R . . H25B H 0.3321 0.3623 0.3866 0.247 Uiso 1 1 calc R . . H25C H 0.3340 0.4306 0.2830 0.247 Uiso 1 1 calc R . . C26 C 0.1643(6) 0.4426(5) 0.1748(6) 0.064(2) Uani 1 1 d . . . H26A H 0.2234 0.4905 0.1215 0.095 Uiso 1 1 calc R . . H26B H 0.1454 0.4645 0.2285 0.095 Uiso 1 1 calc R . . H26C H 0.1005 0.4439 0.1572 0.095 Uiso 1 1 calc R . . C27 C 0.3555(7) 0.4611(5) -0.1440(6) 0.065(2) Uani 1 1 d . . . H27C H 0.4006 0.4839 -0.2110 0.098 Uiso 1 1 calc R . . H27B H 0.3768 0.5047 -0.1164 0.098 Uiso 1 1 calc R . . H27A H 0.2788 0.4681 -0.1370 0.098 Uiso 1 1 calc R . . C28 C 0.5433(7) 0.3361(7) -0.2201(5) 0.068(2) Uani 1 1 d . . . H28A H 0.5289 0.4066 -0.2597 0.082 Uiso 1 1 calc R . . C29 C 0.6467(7) 0.3454(9) -0.2012(7) 0.097(3) Uani 1 1 d . . . H29A H 0.7075 0.3759 -0.2611 0.146 Uiso 1 1 calc R . . H29B H 0.6629 0.2757 -0.1652 0.146 Uiso 1 1 calc R . . H29C H 0.6361 0.3905 -0.1652 0.146 Uiso 1 1 calc R . . C30 C 0.5574(7) 0.2611(8) -0.2719(7) 0.088(3) Uani 1 1 d . . . H30A H 0.5717 0.1920 -0.2333 0.132 Uiso 1 1 calc R . . H30B H 0.6187 0.2883 -0.3319 0.132 Uiso 1 1 calc R . . H30C H 0.4908 0.2550 -0.2838 0.132 Uiso 1 1 calc R . . C31 C 0.1598(5) -0.1199(5) 0.2829(4) 0.0429(14) Uani 1 1 d . . . C32 C 0.1370(7) -0.2194(5) 0.3707(5) 0.0637(19) Uani 1 1 d . . . H32C H 0.2008 -0.2312 0.3895 0.096 Uiso 1 1 calc R . . H32B H 0.1214 -0.2792 0.3572 0.096 Uiso 1 1 calc R . . H32A H 0.0742 -0.2119 0.4219 0.096 Uiso 1 1 calc R . . C33 C 0.3134(4) -0.0584(4) 0.0200(4) 0.0371(13) Uani 1 1 d . . . C34 C 0.3853(5) -0.0961(6) -0.0529(5) 0.0570(18) Uani 1 1 d . . . H34A H 0.3656 -0.0674 -0.1090 0.086 Uiso 1 1 calc R . . H34B H 0.3768 -0.1728 -0.0286 0.086 Uiso 1 1 calc R . . H34C H 0.4611 -0.0730 -0.0692 0.086 Uiso 1 1 calc R . . O5 O -0.3040(4) 0.3474(4) 0.0222(4) 0.0732(15) Uani 1 1 d . . . O6 O -0.4074(4) 0.4724(5) -0.0201(5) 0.0888(19) Uani 1 1 d . . . C35 C -0.3949(5) 0.3815(5) 0.0332(5) 0.0560(18) Uani 1 1 d D . . C36 C -0.4930(5) 0.3180(6) 0.1114(6) 0.070(2) Uani 1 1 d D . . H37A H -0.5224 0.2717 0.0908 0.105 Uiso 1 1 calc R . . H37B H -0.5481 0.3648 0.1294 0.105 Uiso 1 1 calc R . . H37C H -0.4730 0.2759 0.1656 0.105 Uiso 1 1 calc R . . O7 O -0.0321(16) 0.5082(14) -0.4273(13) 0.145(4) Uiso 0.50 1 d PD . . O8 O 0.0532(16) 0.5124(14) -0.3363(14) 0.145(4) Uiso 0.50 1 d PD . . C37 C 0.054(2) 0.5096(14) -0.4116(19) 0.145(4) Uiso 0.50 1 d PD . . C38 C 0.162(2) 0.504(2) -0.4843(19) 0.145(4) Uiso 0.50 1 d PD . . H40A H 0.1923 0.4379 -0.4591 0.217 Uiso 0.50 1 calc PR . . H40B H 0.2124 0.5627 -0.4995 0.217 Uiso 0.50 1 calc PR . . H40C H 0.1506 0.5084 -0.5414 0.217 Uiso 0.50 1 calc PR . . O9 O 0.3451(19) 0.0268(16) -0.2589(16) 0.159(4) Uiso 0.50 1 d PD . . O10 O 0.5329(19) 0.0102(16) -0.3271(16) 0.159(4) Uiso 0.50 1 d PD . . C39 C 0.432(3) 0.0308(15) -0.327(2) 0.159(4) Uiso 0.50 1 d PD . . C40 C 0.404(3) 0.050(2) -0.412(2) 0.159(4) Uiso 0.50 1 d PD . . H43C H 0.3268 0.0270 -0.3926 0.238 Uiso 0.50 1 calc PR . . H43B H 0.4491 0.0099 -0.4486 0.238 Uiso 0.50 1 calc PR . . H43A H 0.4163 0.1246 -0.4518 0.238 Uiso 0.50 1 calc PR . . N1 N -0.1198(4) 0.1424(4) 0.2897(4) 0.0501(13) Uani 1 1 d . . . N2 N -0.0988(4) 0.1328(4) 0.1568(4) 0.0413(12) Uani 1 1 d . . . N3 N -0.0176(4) 0.1623(4) -0.0048(4) 0.0394(11) Uani 1 1 d . . . N4 N 0.0985(4) 0.2176(4) -0.1468(4) 0.0453(12) Uani 1 1 d . . . N5 N 0.2170(5) 0.2757(4) 0.2788(4) 0.0558(15) Uani 1 1 d . . . N6 N 0.2199(4) 0.2758(4) 0.1477(4) 0.0397(11) Uani 1 1 d . . . N7 N 0.3098(4) 0.2855(4) -0.0076(4) 0.0398(11) Uani 1 1 d . . . N8 N 0.4498(4) 0.2948(4) -0.1297(4) 0.0475(12) Uani 1 1 d . . . O1 O 0.1032(3) -0.1119(3) 0.2331(3) 0.0471(10) Uani 1 1 d . . . O2 O 0.2320(3) -0.0530(3) 0.2665(3) 0.0459(10) Uani 1 1 d . . . O3 O 0.2151(3) -0.0514(3) 0.0265(3) 0.0425(10) Uani 1 1 d . . . O4 O 0.3539(3) -0.0348(3) 0.0692(3) 0.0394(9) Uani 1 1 d . . . Pd1 Pd 0.09474(3) 0.00979(3) 0.11276(3) 0.03502(14) Uani 1 1 d . . . Pd2 Pd 0.28952(3) 0.07059(3) 0.13604(3) 0.03538(14) Uani 1 1 d . . . C44 C -0.024(2) 0.4006(18) 0.1042(16) 0.112(3) Uiso 0.50 1 d PD . . H44C H -0.0961 0.3987 0.1514 0.168 Uiso 0.50 1 calc PR . . H44B H 0.0241 0.4560 0.0979 0.168 Uiso 0.50 1 calc PR . . H44A H 0.0062 0.3329 0.1239 0.168 Uiso 0.50 1 calc PR . . C45 C -0.0347(17) 0.4206(19) 0.0194(14) 0.112(3) Uiso 0.50 1 d PD . . H45A H -0.0690 0.4876 0.0032 0.134 Uiso 0.50 1 calc PR . . H45B H -0.0869 0.3653 0.0290 0.134 Uiso 0.50 1 calc PR . . C46 C 0.0592(18) 0.4272(17) -0.0611(14) 0.112(3) Uiso 0.50 1 d PD . . H46A H 0.1205 0.4225 -0.0387 0.134 Uiso 0.50 1 calc PR . . H46B H 0.0534 0.3597 -0.0681 0.134 Uiso 0.50 1 calc PR . . C47 C 0.099(2) 0.4963(17) -0.1501(15) 0.112(3) Uiso 0.50 1 d PD . . H47B H 0.0306 0.5313 -0.1466 0.134 Uiso 0.50 1 calc PR . . H47A H 0.1416 0.5408 -0.1364 0.134 Uiso 0.50 1 calc PR . . C48 C 0.1435(19) 0.5414(17) -0.2390(14) 0.112(3) Uiso 0.50 1 d PD . . H48A H 0.1279 0.4981 -0.2694 0.168 Uiso 0.50 1 calc PR . . H48B H 0.2223 0.5512 -0.2563 0.168 Uiso 0.50 1 calc PR . . H48C H 0.1144 0.6098 -0.2596 0.168 Uiso 0.50 1 calc PR . . O11 O 0.421(2) 0.633(2) -0.419(2) 0.096(7) Uiso 0.25 1 d P . . 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 0.030(3) 0.046(3) 0.047(4) -0.021(3) -0.016(3) 0.005(2) C2 0.036(3) 0.062(4) 0.049(4) -0.029(3) -0.020(3) 0.011(3) C3 0.036(3) 0.068(4) 0.052(5) -0.034(4) -0.015(3) 0.014(3) C4 0.029(3) 0.069(4) 0.051(4) -0.034(4) -0.020(3) 0.015(3) C5 0.047(3) 0.045(3) 0.052(5) -0.026(3) -0.029(3) 0.015(3) C6 0.031(3) 0.062(4) 0.054(5) -0.026(4) -0.018(3) 0.013(3) C7 0.029(3) 0.051(3) 0.047(4) -0.029(3) -0.017(3) 0.009(2) C8 0.055(4) 0.093(6) 0.050(5) -0.044(5) -0.008(3) 0.012(4) C9 0.112(8) 0.147(10) 0.095(8) -0.087(8) -0.009(6) -0.022(7) C10 0.179(13) 0.128(9) 0.044(7) -0.027(7) 0.000(7) -0.010(9) C11 0.054(4) 0.114(7) 0.085(7) -0.064(6) -0.026(4) 0.041(4) C12 0.055(4) 0.059(4) 0.061(5) -0.022(4) -0.035(4) 0.021(3) C13 0.053(4) 0.084(5) 0.047(5) -0.012(4) -0.019(3) 0.001(4) C14 0.116(8) 0.188(12) 0.051(6) -0.054(7) 0.007(5) -0.080(8) C15 0.116(8) 0.125(8) 0.068(7) -0.010(6) -0.028(6) -0.063(7) C16 0.031(3) 0.038(3) 0.049(4) -0.020(3) -0.014(3) 0.003(2) C17 0.054(4) 0.042(3) 0.052(4) -0.026(3) -0.017(3) 0.008(3) C18 0.038(3) 0.043(3) 0.062(5) -0.029(4) -0.008(3) 0.009(3) C19 0.036(3) 0.050(3) 0.066(5) -0.023(3) -0.024(3) 0.012(3) C20 0.052(4) 0.040(3) 0.050(5) -0.015(3) -0.024(3) 0.003(3) C21 0.041(3) 0.043(3) 0.050(4) -0.022(3) -0.018(3) 0.008(2) C22 0.032(3) 0.040(3) 0.049(4) -0.022(3) -0.020(3) 0.008(2) C23 0.124(8) 0.070(5) 0.065(6) -0.047(5) -0.030(5) 0.018(5) C24 0.117(8) 0.136(9) 0.080(8) -0.064(8) -0.043(6) 0.019(7) C25 0.194(14) 0.202(14) 0.133(12) -0.115(12) -0.028(10) -0.073(12) C26 0.064(4) 0.040(3) 0.079(6) -0.029(4) -0.011(4) 0.011(3) C27 0.082(5) 0.049(4) 0.067(6) -0.023(4) -0.031(4) 0.010(4) C28 0.071(5) 0.075(5) 0.043(5) -0.016(4) -0.007(4) -0.001(4) C29 0.070(6) 0.131(8) 0.070(7) -0.036(6) 0.003(5) -0.047(6) C30 0.065(5) 0.139(8) 0.073(7) -0.063(6) -0.015(4) 0.008(5) C31 0.051(4) 0.043(3) 0.032(4) -0.017(3) -0.012(3) 0.017(3) C32 0.074(5) 0.056(4) 0.043(5) -0.009(4) -0.010(4) 0.003(4) C33 0.034(3) 0.041(3) 0.045(4) -0.022(3) -0.018(3) 0.012(2) C34 0.040(3) 0.081(5) 0.073(5) -0.051(4) -0.024(3) 0.021(3) O5 0.045(3) 0.074(3) 0.096(5) -0.030(3) -0.025(3) 0.024(2) O6 0.055(3) 0.091(4) 0.087(5) -0.013(4) -0.013(3) 0.032(3) C35 0.044(4) 0.063(4) 0.075(6) -0.040(4) -0.025(4) 0.023(3) C36 0.038(4) 0.058(4) 0.113(7) -0.040(5) -0.019(4) 0.010(3) N1 0.043(3) 0.071(3) 0.044(4) -0.035(3) -0.011(2) 0.009(2) N2 0.031(2) 0.058(3) 0.047(3) -0.031(3) -0.017(2) 0.012(2) N3 0.034(2) 0.050(3) 0.046(4) -0.026(3) -0.019(2) 0.012(2) N4 0.045(3) 0.052(3) 0.039(3) -0.015(3) -0.019(2) 0.008(2) N5 0.066(4) 0.047(3) 0.058(4) -0.032(3) -0.014(3) 0.007(3) N6 0.029(2) 0.039(2) 0.052(3) -0.023(3) -0.009(2) 0.0038(19) N7 0.036(2) 0.039(2) 0.052(4) -0.023(3) -0.019(2) 0.008(2) N8 0.052(3) 0.049(3) 0.039(3) -0.016(3) -0.014(2) 0.005(2) O1 0.048(2) 0.045(2) 0.046(3) -0.011(2) -0.019(2) -0.0006(19) O2 0.052(2) 0.044(2) 0.051(3) -0.021(2) -0.027(2) 0.0047(19) O3 0.034(2) 0.057(2) 0.051(3) -0.032(2) -0.0210(19) 0.0128(18) O4 0.035(2) 0.042(2) 0.054(3) -0.027(2) -0.0231(19) 0.0120(16) Pd1 0.0270(2) 0.0446(3) 0.0420(3) -0.0228(2) -0.01613(19) 0.00812(17) Pd2 0.0309(2) 0.0371(2) 0.0476(3) -0.0223(2) -0.0186(2) 0.00671(17) _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 C2 1.359(8) . ? C1 N2 1.405(7) . ? C1 Pd1 1.951(5) . ? C2 N1 1.384(7) . ? C2 H2A 0.9500 . ? C3 N1 1.320(8) . ? C3 N2 1.347(7) . ? C3 C11 1.483(9) . ? C4 N2 1.432(7) . ? C4 N3 1.451(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N4 1.338(8) . ? C5 N3 1.341(8) . ? C5 C12 1.489(8) . ? C6 C7 1.353(9) . ? C6 N4 1.385(8) . ? C6 H6A 0.9500 . ? C7 N3 1.396(7) . ? C7 Pd1 1.947(6) . ? C8 C9 1.476(12) . ? C8 N1 1.488(8) . ? C8 C10 1.522(14) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C13 C14 1.436(12) . ? C13 N4 1.484(9) . ? C13 C15 1.484(11) . ? C13 H13A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.354(8) . ? C16 N6 1.405(7) . ? C16 Pd2 1.955(5) . ? C17 N5 1.407(7) . ? C17 H17A 0.9500 . ? C18 N5 1.312(9) . ? C18 N6 1.345(7) . ? C18 C26 1.501(9) . ? C19 N6 1.448(8) . ? C19 N7 1.454(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N8 1.336(8) . ? C20 N7 1.355(8) . ? C20 C27 1.478(9) . ? C21 C22 1.366(8) . ? C21 N8 1.381(8) . ? C21 H21A 0.9500 . ? C22 N7 1.419(7) . ? C22 Pd2 1.932(6) . ? C23 C24 1.487(13) . ? C23 C25 1.490(15) . ? C23 N5 1.498(9) . ? C23 H23A 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27C 0.9800 . ? C27 H27B 0.9800 . ? C27 H27A 0.9800 . ? C28 N8 1.485(9) . ? C28 C29 1.527(12) . ? C28 C30 1.530(11) . ? C28 H28A 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 O2 1.255(7) . ? C31 O1 1.264(7) . ? C31 C32 1.525(9) . ? C32 H32C 0.9800 . ? C32 H32B 0.9800 . ? C32 H32A 0.9800 . ? C33 O4 1.253(6) . ? C33 O3 1.264(6) . ? C33 C34 1.480(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O5 C35 1.236(7) . ? O6 C35 1.276(9) . ? C35 C36 1.488(9) . ? C36 H37A 0.9800 . ? C36 H37B 0.9800 . ? C36 H37C 0.9800 . ? O7 C37 1.25(3) . ? O8 C37 1.25(3) . ? C37 C38 1.515(10) . ? C38 H40A 0.9800 . ? C38 H40B 0.9800 . ? C38 H40C 0.9800 . ? O9 C39 1.28(3) . ? O10 C39 1.34(3) . ? C39 C40 1.501(18) . ? C40 H43C 0.9800 . ? C40 H43B 0.9800 . ? C40 H43A 0.9800 . ? O1 Pd1 2.098(4) . ? O2 Pd2 2.089(4) . ? O3 Pd1 2.087(4) . ? O4 Pd2 2.098(3) . ? Pd1 Pd2 2.9441(6) . ? C44 C45 1.369(17) . ? C44 C47 1.91(3) 2_565 ? C44 H44C 0.9800 . ? C44 H44B 0.9800 . ? C44 H44A 0.9800 . ? C45 C46 1.432(17) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.341(15) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.273(15) . ? C47 C44 1.91(3) 2_565 ? C47 H47B 0.9900 . ? C47 H47A 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? 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 C2 C1 N2 104.2(5) . . ? C2 C1 Pd1 130.1(4) . . ? N2 C1 Pd1 125.6(4) . . ? C1 C2 N1 108.8(5) . . ? C1 C2 H2A 125.6 . . ? N1 C2 H2A 125.6 . . ? N1 C3 N2 107.5(5) . . ? N1 C3 C11 126.1(6) . . ? N2 C3 C11 126.3(6) . . ? N2 C4 N3 110.0(4) . . ? N2 C4 H4A 109.7 . . ? N3 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? N3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? N4 C5 N3 107.1(5) . . ? N4 C5 C12 124.8(6) . . ? N3 C5 C12 128.1(6) . . ? C7 C6 N4 109.1(5) . . ? C7 C6 H6A 125.4 . . ? N4 C6 H6A 125.4 . . ? C6 C7 N3 104.4(5) . . ? C6 C7 Pd1 129.1(4) . . ? N3 C7 Pd1 126.5(4) . . ? C9 C8 N1 108.4(6) . . ? C9 C8 C10 111.8(9) . . ? N1 C8 C10 109.8(7) . . ? C9 C8 H8A 108.9 . . ? N1 C8 H8A 108.9 . . ? C10 C8 H8A 108.9 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12C 109.5 . . ? C5 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C5 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C14 C13 N4 110.5(7) . . ? C14 C13 C15 110.7(8) . . ? N4 C13 C15 111.2(6) . . ? C14 C13 H13A 108.1 . . ? N4 C13 H13A 108.1 . . ? C15 C13 H13A 108.1 . . ? 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 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N6 104.2(5) . . ? C17 C16 Pd2 132.0(5) . . ? N6 C16 Pd2 123.7(4) . . ? C16 C17 N5 108.2(6) . . ? C16 C17 H17A 125.9 . . ? N5 C17 H17A 125.9 . . ? N5 C18 N6 107.1(5) . . ? N5 C18 C26 128.4(6) . . ? N6 C18 C26 124.5(7) . . ? N6 C19 N7 108.4(5) . . ? N6 C19 H19A 110.0 . . ? N7 C19 H19A 110.0 . . ? N6 C19 H19B 110.0 . . ? N7 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? N8 C20 N7 106.4(5) . . ? N8 C20 C27 126.4(6) . . ? N7 C20 C27 127.2(6) . . ? C22 C21 N8 110.1(5) . . ? C22 C21 H21A 124.9 . . ? N8 C21 H21A 124.9 . . ? C21 C22 N7 102.7(5) . . ? C21 C22 Pd2 132.4(4) . . ? N7 C22 Pd2 124.9(4) . . ? C24 C23 C25 114.8(10) . . ? C24 C23 N5 110.7(7) . . ? C25 C23 N5 107.9(8) . . ? C24 C23 H23A 107.7 . . ? C25 C23 H23A 107.7 . . ? N5 C23 H23A 107.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27C 109.5 . . ? C20 C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? C20 C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? N8 C28 C29 109.7(6) . . ? N8 C28 C30 109.2(6) . . ? C29 C28 C30 109.6(7) . . ? N8 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C30 C28 H28A 109.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O2 C31 O1 125.7(6) . . ? O2 C31 C32 117.8(6) . . ? O1 C31 C32 116.5(6) . . ? C31 C32 H32C 109.5 . . ? C31 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? C31 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? O4 C33 O3 125.1(5) . . ? O4 C33 C34 118.4(5) . . ? O3 C33 C34 116.5(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O5 C35 O6 121.5(7) . . ? O5 C35 C36 120.5(7) . . ? O6 C35 C36 118.0(6) . . ? C35 C36 H37A 109.5 . . ? C35 C36 H37B 109.5 . . ? H37A C36 H37B 109.5 . . ? C35 C36 H37C 109.5 . . ? H37A C36 H37C 109.5 . . ? H37B C36 H37C 109.5 . . ? O8 C37 O7 122(2) . . ? O8 C37 C38 119(3) . . ? O7 C37 C38 120(3) . . ? C37 C38 H40A 109.5 . . ? C37 C38 H40B 109.5 . . ? H40A C38 H40B 109.5 . . ? C37 C38 H40C 109.5 . . ? H40A C38 H40C 109.5 . . ? H40B C38 H40C 109.5 . . ? O9 C39 O10 129(3) . . ? O9 C39 C40 109(3) . . ? O10 C39 C40 122(3) . . ? C39 C40 H43C 109.5 . . ? C39 C40 H43B 109.5 . . ? H43C C40 H43B 109.5 . . ? C39 C40 H43A 109.5 . . ? H43C C40 H43A 109.5 . . ? H43B C40 H43A 109.5 . . ? C3 N1 C2 109.3(5) . . ? C3 N1 C8 126.5(6) . . ? C2 N1 C8 124.2(6) . . ? C3 N2 C1 110.2(5) . . ? C3 N2 C4 126.3(5) . . ? C1 N2 C4 123.2(5) . . ? C5 N3 C7 110.9(5) . . ? C5 N3 C4 126.2(5) . . ? C7 N3 C4 122.6(5) . . ? C5 N4 C6 108.5(5) . . ? C5 N4 C13 126.4(6) . . ? C6 N4 C13 125.1(5) . . ? C18 N5 C17 109.5(5) . . ? C18 N5 C23 125.5(6) . . ? C17 N5 C23 124.8(7) . . ? C18 N6 C16 111.0(5) . . ? C18 N6 C19 126.0(5) . . ? C16 N6 C19 123.0(4) . . ? C20 N7 C22 111.5(5) . . ? C20 N7 C19 127.0(5) . . ? C22 N7 C19 121.5(5) . . ? C20 N8 C21 109.3(5) . . ? C20 N8 C28 125.9(6) . . ? C21 N8 C28 124.5(6) . . ? C31 O1 Pd1 131.9(4) . . ? C31 O2 Pd2 120.1(4) . . ? C33 O3 Pd1 126.9(3) . . ? C33 O4 Pd2 124.0(3) . . ? C7 Pd1 C1 87.4(2) . . ? C7 Pd1 O3 88.62(19) . . ? C1 Pd1 O3 176.0(2) . . ? C7 Pd1 O1 173.94(18) . . ? C1 Pd1 O1 93.3(2) . . ? O3 Pd1 O1 90.68(17) . . ? C7 Pd1 Pd2 110.45(16) . . ? C1 Pd1 Pd2 101.39(15) . . ? O3 Pd1 Pd2 79.32(10) . . ? O1 Pd1 Pd2 75.30(11) . . ? C22 Pd2 C16 87.4(2) . . ? C22 Pd2 O2 176.84(18) . . ? C16 Pd2 O2 92.5(2) . . ? C22 Pd2 O4 89.12(19) . . ? C16 Pd2 O4 172.67(18) . . ? O2 Pd2 O4 90.68(16) . . ? C22 Pd2 Pd1 98.65(15) . . ? C16 Pd2 Pd1 107.00(15) . . ? O2 Pd2 Pd1 84.41(11) . . ? O4 Pd2 Pd1 79.89(10) . . ? C45 C44 C47 106.8(18) . 2_565 ? C45 C44 H44C 109.5 . . ? C47 C44 H44C 47.3 2_565 . ? C45 C44 H44B 109.5 . . ? C47 C44 H44B 66.2 2_565 . ? H44C C44 H44B 109.5 . . ? C45 C44 H44A 109.5 . . ? C47 C44 H44A 142.4 2_565 . ? H44C C44 H44A 109.5 . . ? H44B C44 H44A 109.5 . . ? C44 C45 C46 120(2) . . ? C44 C45 H45A 107.3 . . ? C46 C45 H45A 107.3 . . ? C44 C45 H45B 107.3 . . ? C46 C45 H45B 107.3 . . ? H45A C45 H45B 106.9 . . ? C47 C46 C45 134(2) . . ? C47 C46 H46A 103.7 . . ? C45 C46 H46A 103.7 . . ? C47 C46 H46B 103.7 . . ? C45 C46 H46B 103.7 . . ? H46A C46 H46B 105.3 . . ? C48 C47 C46 166(2) . . ? C48 C47 C44 106.8(19) . 2_565 ? C46 C47 C44 87.2(16) . 2_565 ? C48 C47 H47B 94.4 . . ? C46 C47 H47B 94.4 . . ? C44 C47 H47B 41.8 2_565 . ? C48 C47 H47A 94.4 . . ? C46 C47 H47A 94.4 . . ? C44 C47 H47A 62.7 2_565 . ? H47B C47 H47A 103.2 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? 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 N2 C1 C2 N1 0.5(7) . . . . ? Pd1 C1 C2 N1 176.4(4) . . . . ? N4 C6 C7 N3 -0.9(6) . . . . ? N4 C6 C7 Pd1 176.9(4) . . . . ? N6 C16 C17 N5 0.6(6) . . . . ? Pd2 C16 C17 N5 176.5(4) . . . . ? N8 C21 C22 N7 0.9(6) . . . . ? N8 C21 C22 Pd2 -178.0(4) . . . . ? N2 C3 N1 C2 -0.9(7) . . . . ? C11 C3 N1 C2 -179.5(7) . . . . ? N2 C3 N1 C8 178.5(6) . . . . ? C11 C3 N1 C8 -0.1(12) . . . . ? C1 C2 N1 C3 0.2(7) . . . . ? C1 C2 N1 C8 -179.2(6) . . . . ? C9 C8 N1 C3 -113.1(9) . . . . ? C10 C8 N1 C3 124.5(9) . . . . ? C9 C8 N1 C2 66.2(10) . . . . ? C10 C8 N1 C2 -56.2(10) . . . . ? N1 C3 N2 C1 1.3(7) . . . . ? C11 C3 N2 C1 179.9(7) . . . . ? N1 C3 N2 C4 174.4(6) . . . . ? C11 C3 N2 C4 -7.1(11) . . . . ? C2 C1 N2 C3 -1.1(7) . . . . ? Pd1 C1 N2 C3 -177.2(4) . . . . ? C2 C1 N2 C4 -174.4(5) . . . . ? Pd1 C1 N2 C4 9.5(8) . . . . ? N3 C4 N2 C3 138.8(6) . . . . ? N3 C4 N2 C1 -49.0(8) . . . . ? N4 C5 N3 C7 -1.2(6) . . . . ? C12 C5 N3 C7 179.0(5) . . . . ? N4 C5 N3 C4 -173.9(5) . . . . ? C12 C5 N3 C4 6.3(9) . . . . ? C6 C7 N3 C5 1.3(6) . . . . ? Pd1 C7 N3 C5 -176.6(4) . . . . ? C6 C7 N3 C4 174.3(5) . . . . ? Pd1 C7 N3 C4 -3.6(7) . . . . ? N2 C4 N3 C5 -142.3(5) . . . . ? N2 C4 N3 C7 45.8(7) . . . . ? N3 C5 N4 C6 0.6(6) . . . . ? C12 C5 N4 C6 -179.6(5) . . . . ? N3 C5 N4 C13 -180.0(6) . . . . ? C12 C5 N4 C13 -0.2(9) . . . . ? C7 C6 N4 C5 0.2(7) . . . . ? C7 C6 N4 C13 -179.2(6) . . . . ? C14 C13 N4 C5 -105.4(9) . . . . ? C15 C13 N4 C5 131.2(8) . . . . ? C14 C13 N4 C6 73.9(9) . . . . ? C15 C13 N4 C6 -49.5(10) . . . . ? N6 C18 N5 C17 -0.5(7) . . . . ? C26 C18 N5 C17 178.3(6) . . . . ? N6 C18 N5 C23 174.5(7) . . . . ? C26 C18 N5 C23 -6.7(11) . . . . ? C16 C17 N5 C18 -0.1(7) . . . . ? C16 C17 N5 C23 -175.1(7) . . . . ? C24 C23 N5 C18 146.8(8) . . . . ? C25 C23 N5 C18 -86.8(11) . . . . ? C24 C23 N5 C17 -38.9(11) . . . . ? C25 C23 N5 C17 87.4(11) . . . . ? N5 C18 N6 C16 0.9(7) . . . . ? C26 C18 N6 C16 -178.0(6) . . . . ? N5 C18 N6 C19 179.8(5) . . . . ? C26 C18 N6 C19 1.0(9) . . . . ? C17 C16 N6 C18 -0.9(6) . . . . ? Pd2 C16 N6 C18 -177.2(4) . . . . ? C17 C16 N6 C19 -179.9(5) . . . . ? Pd2 C16 N6 C19 3.8(7) . . . . ? N7 C19 N6 C18 130.9(6) . . . . ? N7 C19 N6 C16 -50.3(7) . . . . ? N8 C20 N7 C22 0.7(6) . . . . ? C27 C20 N7 C22 -179.1(6) . . . . ? N8 C20 N7 C19 -176.4(5) . . . . ? C27 C20 N7 C19 3.8(9) . . . . ? C21 C22 N7 C20 -1.0(6) . . . . ? Pd2 C22 N7 C20 178.0(4) . . . . ? C21 C22 N7 C19 176.3(5) . . . . ? Pd2 C22 N7 C19 -4.7(7) . . . . ? N6 C19 N7 C20 -132.6(6) . . . . ? N6 C19 N7 C22 50.6(6) . . . . ? N7 C20 N8 C21 -0.1(6) . . . . ? C27 C20 N8 C21 179.7(6) . . . . ? N7 C20 N8 C28 -173.6(6) . . . . ? C27 C20 N8 C28 6.3(10) . . . . ? C22 C21 N8 C20 -0.5(7) . . . . ? C22 C21 N8 C28 173.0(6) . . . . ? C29 C28 N8 C20 105.1(8) . . . . ? C30 C28 N8 C20 -134.7(7) . . . . ? C29 C28 N8 C21 -67.3(9) . . . . ? C30 C28 N8 C21 52.8(9) . . . . ? O2 C31 O1 Pd1 -4.0(9) . . . . ? C32 C31 O1 Pd1 175.6(4) . . . . ? O1 C31 O2 Pd2 -12.4(8) . . . . ? C32 C31 O2 Pd2 168.0(4) . . . . ? O4 C33 O3 Pd1 4.4(9) . . . . ? C34 C33 O3 Pd1 -174.6(4) . . . . ? O3 C33 O4 Pd2 -23.8(8) . . . . ? C34 C33 O4 Pd2 155.2(5) . . . . ? C6 C7 Pd1 C1 155.2(5) . . . . ? N3 C7 Pd1 C1 -27.4(4) . . . . ? C6 C7 Pd1 O3 -24.0(5) . . . . ? N3 C7 Pd1 O3 153.3(4) . . . . ? C6 C7 Pd1 O1 -107.4(18) . . . . ? N3 C7 Pd1 O1 69.9(19) . . . . ? C6 C7 Pd1 Pd2 54.0(5) . . . . ? N3 C7 Pd1 Pd2 -128.6(4) . . . . ? C2 C1 Pd1 C7 -150.4(6) . . . . ? N2 C1 Pd1 C7 24.7(5) . . . . ? C2 C1 Pd1 O3 -140(2) . . . . ? N2 C1 Pd1 O3 35(3) . . . . ? C2 C1 Pd1 O1 35.6(6) . . . . ? N2 C1 Pd1 O1 -149.3(5) . . . . ? C2 C1 Pd1 Pd2 -40.1(6) . . . . ? N2 C1 Pd1 Pd2 135.0(4) . . . . ? C33 O3 Pd1 C7 120.6(5) . . . . ? C33 O3 Pd1 C1 110(2) . . . . ? C33 O3 Pd1 O1 -65.4(5) . . . . ? C33 O3 Pd1 Pd2 9.5(5) . . . . ? C31 O1 Pd1 C7 174.0(17) . . . . ? C31 O1 Pd1 C1 -89.0(5) . . . . ? C31 O1 Pd1 O3 90.7(5) . . . . ? C31 O1 Pd1 Pd2 11.9(5) . . . . ? C21 C22 Pd2 C16 146.8(6) . . . . ? N7 C22 Pd2 C16 -31.9(4) . . . . ? C21 C22 Pd2 O2 60(3) . . . . ? N7 C22 Pd2 O2 -119(3) . . . . ? C21 C22 Pd2 O4 -26.8(5) . . . . ? N7 C22 Pd2 O4 154.6(4) . . . . ? C21 C22 Pd2 Pd1 -106.4(5) . . . . ? N7 C22 Pd2 Pd1 74.9(4) . . . . ? C17 C16 Pd2 C22 -142.9(6) . . . . ? N6 C16 Pd2 C22 32.3(4) . . . . ? C17 C16 Pd2 O2 33.9(6) . . . . ? N6 C16 Pd2 O2 -150.8(4) . . . . ? C17 C16 Pd2 O4 -81.6(18) . . . . ? N6 C16 Pd2 O4 93.7(16) . . . . ? C17 C16 Pd2 Pd1 118.8(5) . . . . ? N6 C16 Pd2 Pd1 -65.9(4) . . . . ? C31 O2 Pd2 C22 -151(3) . . . . ? C31 O2 Pd2 C16 122.0(4) . . . . ? C31 O2 Pd2 O4 -64.6(4) . . . . ? C31 O2 Pd2 Pd1 15.1(4) . . . . ? C33 O4 Pd2 C22 -76.6(5) . . . . ? C33 O4 Pd2 C16 -137.9(16) . . . . ? C33 O4 Pd2 O2 106.5(5) . . . . ? C33 O4 Pd2 Pd1 22.3(5) . . . . ? C7 Pd1 Pd2 C22 -9.2(2) . . . . ? C1 Pd1 Pd2 C22 -100.7(2) . . . . ? O3 Pd1 Pd2 C22 75.2(2) . . . . ? O1 Pd1 Pd2 C22 168.78(19) . . . . ? C7 Pd1 Pd2 C16 80.6(2) . . . . ? C1 Pd1 Pd2 C16 -10.8(3) . . . . ? O3 Pd1 Pd2 C16 165.1(2) . . . . ? O1 Pd1 Pd2 C16 -101.4(2) . . . . ? C7 Pd1 Pd2 O2 171.53(19) . . . . ? C1 Pd1 Pd2 O2 80.0(2) . . . . ? O3 Pd1 Pd2 O2 -104.00(16) . . . . ? O1 Pd1 Pd2 O2 -10.45(16) . . . . ? C7 Pd1 Pd2 O4 -96.8(2) . . . . ? C1 Pd1 Pd2 O4 171.7(2) . . . . ? O3 Pd1 Pd2 O4 -12.31(17) . . . . ? O1 Pd1 Pd2 O4 81.24(17) . . . . ? C47 C44 C45 C46 130(2) 2_565 . . . ? C44 C45 C46 C47 -131(3) . . . . ? C45 C46 C47 C48 -143(10) . . . . ? C45 C46 C47 C44 26(3) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.107 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.138 # start Validation Reply Form _vrf_PLAT029_7 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: For a triclinic system, max. 93% of the data are accessible with the STOE IPDS-I. Nevertheless, with a parameter / observed reflection ratio of 1:12, the structure has been refined with good precisions on bond distances and angles. ; _vrf_PLAT411_7 ; PROBLEM: Short Inter H...H Contact H19A .. H46A .. 1.78 Ang. RESPONSE: Hydrogens are part of partially occupied solvent molecules in the structure. ; _vrf_PLAT413_7 ; PROBLEM: Short Inter XH3 .. XHn H9C .. H48C .. 1.48 Ang. RESPONSE: Hydrogens are part of partially occupied solvent molecules in the structure. ; _vrf_PLAT430_7 ; PROBLEM: Short Inter D...A Contact O6 .. O6 .. 2.44 Ang. RESPONSE: Hydrogens are part of partially occupied solvent molecules in the structure. ; _vrf_PLAT432_7 ; PROBLEM: Short Inter X...Y Contact O8 .. C48 .. 2.45 Ang. RESPONSE: Hydrogens are part of partially occupied solvent molecules in the structure. ; _vrf_PLAT773_7 ; PROBLEM: Suspect C-C Bond in CIF: C44 -- C47 .. 1.91 Ang. RESPONSE: Hydrogens are part of partially occupied solvent molecules in the structure. ; # Attachment 'B812405A_2a_2c_2d_7_11.CIF' data_2a _database_code_depnum_ccdc_archive 'CCDC 695648' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H17.50 I2 N4.50 Pd' _chemical_formula_weight 585.01 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 orthorhombic _symmetry_space_group_name_H-M 'P b a m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' _cell_length_a 13.7424(13) _cell_length_b 18.4993(17) _cell_length_c 6.9570(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1768.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18042 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 25.49 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 4.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.458 _exptl_absorpt_correction_T_max 0.582 _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 20143 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.26 _reflns_number_total 1725 _reflns_number_gt 1554 _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^)+(0.0537P)^2^+8.9510P] 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 calc _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1725 _refine_ls_number_parameters 157 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.247 _refine_ls_restrained_S_all 1.247 _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 0.3257(13) -0.4291(10) -0.357(3) 0.039(4) Uani 0.50 1 d P . . C2 C 0.3632(15) -0.4962(9) -0.316(3) 0.044(4) Uani 0.50 1 d P . . H2A H 0.3907 -0.5119 -0.1982 0.053 Uiso 0.50 1 calc PR . . C3 C 0.3085(15) -0.5023(9) -0.619(2) 0.044(4) Uani 0.50 1 d P . . C4 C 0.2566(11) -0.3753(9) -0.658(2) 0.042(3) Uani 0.50 1 d P . . H4A H 0.3083 -0.3389 -0.6790 0.050 Uiso 0.50 1 calc PR . . H4B H 0.2332 -0.3921 -0.7853 0.050 Uiso 0.50 1 calc PR . . C5 C 0.0878(12) -0.3305(10) -0.622(3) 0.041(4) Uani 0.50 1 d P . . C6 C 0.0983(11) -0.2925(10) -0.316(3) 0.039(4) Uani 0.50 1 d P . . H6A H 0.0780 -0.2732 -0.1961 0.046 Uiso 0.50 1 calc PR . . C7 C 0.1861(12) -0.3213(10) -0.360(3) 0.035(4) Uani 0.50 1 d P . . C8 C 0.3800(12) -0.6173(6) -0.5000 0.062(4) Uani 1 2 d S . . H8A H 0.4356 -0.6244 -0.4137 0.093 Uiso 0.50 1 calc PR . . H8B H 0.3981 -0.6320 -0.6306 0.093 Uiso 0.50 1 calc PR . . H8C H 0.3251 -0.6467 -0.4557 0.093 Uiso 0.50 1 calc PR . . C9 C 0.2860(13) -0.5283(9) -0.811(3) 0.054(4) Uani 0.50 1 d P . . H9A H 0.2184 -0.5451 -0.8153 0.080 Uiso 0.50 1 calc PR . . H9B H 0.3297 -0.5683 -0.8441 0.080 Uiso 0.50 1 calc PR . . H9C H 0.2947 -0.4889 -0.9038 0.080 Uiso 0.50 1 calc PR . . C10 C 0.0510(12) -0.3461(10) -0.816(2) 0.050(4) Uani 0.50 1 d P . . H10A H 0.0241 -0.3951 -0.8188 0.075 Uiso 0.50 1 calc PR . . H10B H 0.1043 -0.3422 -0.9084 0.075 Uiso 0.50 1 calc PR . . H10C H -0.0001 -0.3112 -0.8486 0.075 Uiso 0.50 1 calc PR . . C11 C -0.0625(9) -0.2741(8) -0.5000 0.062(4) Uani 1 2 d S . . H11A H -0.0809 -0.2586 -0.6298 0.094 Uiso 0.50 1 calc PR . . H11B H -0.0703 -0.2335 -0.4106 0.094 Uiso 0.50 1 calc PR . . H11C H -0.1044 -0.3142 -0.4597 0.094 Uiso 0.50 1 calc PR . . C12 C 0.007(2) -0.523(2) -0.562(4) 0.050(5) Uiso 0.25 1 d PD . . C13 C 0.080(2) -0.5267(19) -0.721(4) 0.050(5) Uiso 0.25 1 d PD . . H13A H 0.0464 -0.5278 -0.8454 0.076 Uiso 0.25 1 calc PR . . H13B H 0.1194 -0.5706 -0.7068 0.076 Uiso 0.25 1 calc PR . . H13C H 0.1226 -0.4842 -0.7158 0.076 Uiso 0.25 1 calc PR . . I1 I 0.46585(5) -0.36844(4) 0.0000 0.0447(2) Uani 1 2 d S . . I2 I 0.27319(5) -0.21857(4) 0.0000 0.0433(2) Uani 1 2 d S . . N1 N 0.3519(8) -0.5405(5) -0.5000 0.054(3) Uani 1 2 d S . . N2 N 0.2952(10) -0.4368(7) -0.5475(18) 0.034(5) Uani 0.50 1 d P . . N3 N 0.1768(9) -0.3437(8) -0.5501(17) 0.029(4) Uani 0.50 1 d P . . N4 N 0.0392(7) -0.2978(6) -0.5000 0.049(2) Uani 1 2 d S . . N5 N -0.0241(18) -0.520(2) -0.400(4) 0.050(5) Uiso 0.25 1 d PD . . Pd1 Pd 0.30651(8) -0.33959(6) -0.20193(16) 0.0340(3) Uani 0.50 1 d P . . 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(9) 0.048(9) 0.027(10) -0.011(8) 0.002(7) -0.003(7) C2 0.059(11) 0.036(8) 0.037(9) -0.004(7) -0.010(8) 0.012(8) C3 0.059(11) 0.043(10) 0.030(10) -0.010(8) -0.008(8) 0.006(9) C4 0.046(8) 0.044(8) 0.035(8) 0.009(7) 0.002(7) 0.000(7) C5 0.038(9) 0.040(10) 0.045(11) -0.002(8) -0.010(8) 0.000(8) C6 0.037(8) 0.039(9) 0.040(9) -0.001(8) -0.004(7) 0.009(7) C7 0.046(9) 0.036(9) 0.023(10) -0.002(7) 0.001(7) 0.003(7) C8 0.089(10) 0.035(6) 0.063(9) 0.000 0.000 0.020(7) C9 0.066(11) 0.049(10) 0.046(10) -0.016(8) -0.005(9) 0.018(8) C10 0.046(9) 0.068(11) 0.036(8) 0.007(8) 0.002(7) 0.009(8) C11 0.041(7) 0.079(10) 0.068(9) 0.000 0.000 0.013(6) I1 0.0380(4) 0.0497(4) 0.0462(4) 0.000 0.000 0.0067(3) I2 0.0477(4) 0.0374(4) 0.0448(4) 0.000 0.000 0.0051(3) N1 0.061(6) 0.037(5) 0.064(7) 0.000 0.000 0.008(5) N2 0.039(6) 0.033(6) 0.030(16) 0.007(6) -0.002(6) 0.005(5) N3 0.033(6) 0.035(6) 0.019(13) -0.001(5) -0.002(5) 0.009(5) N4 0.036(5) 0.046(5) 0.064(7) 0.000 0.000 0.002(4) Pd1 0.0356(6) 0.0332(6) 0.0333(6) -0.0032(5) -0.0018(5) 0.0034(4) _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 N2 0.798(17) 6_554 ? C1 C2 1.37(3) . ? C1 C4 1.38(2) 6_554 ? C1 C3 1.39(3) 6_554 ? C1 N2 1.40(3) . ? C1 Pd1 1.994(17) . ? C2 N1 1.525(18) . ? C2 H2A 0.9500 . ? C3 C2 0.88(2) 6_554 ? C3 N1 1.239(17) . ? C3 N2 1.32(2) . ? C3 C1 1.39(3) 6_554 ? C3 C9 1.46(2) . ? C3 C3 1.65(3) 6_554 ? C3 N2 1.68(2) 6_554 ? C4 N3 1.45(2) . ? C4 N2 1.47(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 0.837(19) 6_554 ? C5 N4 1.236(18) . ? C5 N3 1.34(2) . ? C5 C7 1.37(2) 6_554 ? C5 C10 1.47(2) . ? C5 C5 1.70(4) 6_554 ? C5 N3 1.73(2) 6_554 ? C6 C7 1.35(2) . ? C6 N4 1.519(18) . ? C6 H6A 0.9500 . ? C7 N3 0.764(15) 6_554 ? C7 C5 1.37(2) 6_554 ? C7 N3 1.39(2) . ? C7 C4 1.40(2) 6_554 ? C7 Pd1 2.014(17) . ? C8 N1 1.473(15) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N4 1.466(15) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N5 0.50(4) 6_554 ? C12 C12 0.86(5) 6_554 ? C12 N5 0.86(3) 5_544 ? C12 C12 0.86(7) 2_545 ? C12 N5 1.206(5) . ? C12 C12 1.22(6) 5_544 ? C12 N5 1.39(2) 2_545 ? C12 C13 1.502(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? I1 Pd1 2.6558(12) . ? I1 Pd1 2.6558(12) 6 ? I2 Pd1 2.6825(12) . ? I2 Pd1 2.6825(12) 6 ? N1 C3 1.239(17) 6_554 ? N1 C2 1.525(18) 6_554 ? N2 N2 0.66(3) 6_554 ? N2 C1 0.798(17) 6_554 ? N2 C3 1.68(2) 6_554 ? N2 C2 1.73(2) 6_554 ? N2 C4 1.90(2) 6_554 ? N2 Pd1 2.509(14) 6_554 ? N3 N3 0.70(2) 6_554 ? N3 C7 0.764(15) 6_554 ? N3 C6 1.71(2) 6_554 ? N3 C5 1.73(2) 6_554 ? N3 C4 1.91(2) 6_554 ? N3 Pd1 2.482(13) 6_554 ? N4 C5 1.236(18) 6_554 ? N4 C6 1.519(18) 6_554 ? N5 C12 0.50(4) 6_554 ? N5 C12 0.86(3) 5_544 ? N5 N5 0.98(6) 2_545 ? N5 C12 1.39(2) 2_545 ? N5 N5 1.40(5) 6_554 ? N5 C13 1.43(5) 5_544 ? N5 C13 1.67(4) 6_554 ? N5 N5 1.71(5) 5_544 ? Pd1 C4 1.362(16) 6_554 ? Pd1 N3 2.482(13) 6_554 ? Pd1 N2 2.509(14) 6_554 ? Pd1 Pd1 2.810(2) 6 ? 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 N2 C1 C2 102(2) 6_554 . ? N2 C1 C4 80(2) 6_554 6_554 ? C2 C1 C4 153.4(18) . 6_554 ? N2 C1 C3 68.6(19) 6_554 6_554 ? C2 C1 C3 37.3(10) . 6_554 ? C4 C1 C3 126.7(18) 6_554 6_554 ? N2 C1 N2 15.2(9) 6_554 . ? C2 C1 N2 102.4(15) . . ? C4 C1 N2 86.6(15) 6_554 . ? C3 C1 N2 74.6(13) 6_554 . ? N2 C1 C1 33.7(17) 6_554 6_554 ? C2 C1 C1 101.9(11) . 6_554 ? C4 C1 C1 94.4(11) 6_554 6_554 ? C3 C1 C1 83.0(11) 6_554 6_554 ? N2 C1 C1 18.5(10) . 6_554 ? N2 C1 Pd1 122(2) 6_554 . ? C2 C1 Pd1 133.5(15) . . ? C4 C1 Pd1 43.0(8) 6_554 . ? C3 C1 Pd1 148.8(14) 6_554 . ? N2 C1 Pd1 124.0(14) . . ? C1 C1 Pd1 122.8(6) 6_554 . ? C1 C2 N1 106.0(15) . . ? C1 C2 H2A 127.0 . . ? N1 C2 H2A 127.0 . . ? C2 C3 N1 90.2(19) 6_554 . ? C2 C3 N2 101(2) 6_554 . ? N1 C3 N2 109.9(13) . . ? C2 C3 C1 71(2) 6_554 6_554 ? N1 C3 C1 123.9(15) . 6_554 ? N2 C3 C1 34.2(8) . 6_554 ? C2 C3 C9 75.7(18) 6_554 . ? N1 C3 C9 121.8(15) . . ? N2 C3 C9 128.1(15) . . ? C1 C3 C9 104.3(16) 6_554 . ? C2 C3 C3 120.7(16) 6_554 6_554 ? N1 C3 C3 48.2(9) . 6_554 ? N2 C3 C3 68.0(10) . 6_554 ? C1 C3 C3 97.0(11) 6_554 6_554 ? C9 C3 C3 156.9(11) . 6_554 ? C2 C3 N2 111(2) 6_554 6_554 ? N1 C3 N2 90.3(11) . 6_554 ? N2 C3 N2 21.3(9) . 6_554 ? C1 C3 N2 53.0(11) 6_554 6_554 ? C9 C3 N2 147.7(15) . 6_554 ? C3 C3 N2 46.7(8) 6_554 6_554 ? N3 C4 N2 108.2(13) . . ? N3 C4 H4A 110.1 . . ? N2 C4 H4A 110.1 . . ? N3 C4 H4B 110.1 . . ? N2 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C6 C5 N4 92.2(19) 6_554 . ? C6 C5 N3 101(2) 6_554 . ? N4 C5 N3 109.0(14) . . ? C6 C5 C7 71(2) 6_554 6_554 ? N4 C5 C7 122.5(15) . 6_554 ? N3 C5 C7 32.7(8) . 6_554 ? C6 C5 C10 76(2) 6_554 . ? N4 C5 C10 122.6(14) . . ? N3 C5 C10 128.3(15) . . ? C7 C5 C10 106.2(16) 6_554 . ? C6 C5 C5 121.1(17) 6_554 6_554 ? N4 C5 C5 46.7(9) . 6_554 ? N3 C5 C5 68.2(10) . 6_554 ? C7 C5 C5 95.4(11) 6_554 6_554 ? C10 C5 C5 156.6(10) . 6_554 ? C6 C5 N3 111(2) 6_554 6_554 ? N4 C5 N3 88.7(11) . 6_554 ? N3 C5 N3 22.0(8) . 6_554 ? C7 C5 N3 52.0(11) 6_554 6_554 ? C10 C5 N3 148.4(15) . 6_554 ? C5 C5 N3 46.2(7) 6_554 6_554 ? C7 C6 N4 105.2(15) . . ? C7 C6 H6A 127.4 . . ? N4 C6 H6A 127.4 . . ? N3 C7 C6 104(2) 6_554 . ? N3 C7 C5 72(2) 6_554 6_554 ? C6 C7 C5 35.8(9) . 6_554 ? N3 C7 N3 16.5(10) 6_554 . ? C6 C7 N3 104.4(16) . . ? C5 C7 N3 77.5(14) 6_554 . ? N3 C7 C4 78.5(19) 6_554 6_554 ? C6 C7 C4 151.6(18) . 6_554 ? C5 C7 C4 127.2(18) 6_554 6_554 ? N3 C7 C4 86.3(13) . 6_554 ? N3 C7 C7 34.6(19) 6_554 6_554 ? C6 C7 C7 103.0(11) . 6_554 ? C5 C7 C7 84.6(11) 6_554 6_554 ? N3 C7 C7 18.1(10) . 6_554 ? C4 C7 C7 95.1(10) 6_554 6_554 ? N3 C7 Pd1 120(2) 6_554 . ? C6 C7 Pd1 132.6(15) . . ? C5 C7 Pd1 147.4(14) 6_554 . ? N3 C7 Pd1 122.9(13) . . ? C4 C7 Pd1 42.4(8) 6_554 . ? C7 C7 Pd1 123.0(5) 6_554 . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C12 122(5) 6_554 6_554 ? N5 C12 N5 88(8) 6_554 5_544 ? C12 C12 N5 108(3) 6_554 5_544 ? N5 C12 C12 73(7) 6_554 2_545 ? C12 C12 C12 90.000(10) 6_554 2_545 ? N5 C12 C12 34(3) 5_544 2_545 ? N5 C12 N5 101(6) 6_554 . ? C12 C12 N5 21(2) 6_554 . ? N5 C12 N5 110(4) 5_544 . ? C12 C12 N5 83(3) 2_545 . ? N5 C12 C12 100(7) 6_554 5_544 ? C12 C12 C12 45(3) 6_554 5_544 ? N5 C12 C12 68(4) 5_544 5_544 ? C12 C12 C12 45(3) 2_545 5_544 ? N5 C12 C12 41.7(18) . 5_544 ? N5 C12 N5 121(7) 6_554 2_545 ? C12 C12 N5 36.0(11) 6_554 2_545 ? N5 C12 N5 72(4) 5_544 2_545 ? C12 C12 N5 59.1(15) 2_545 2_545 ? N5 C12 N5 44(3) . 2_545 ? C12 C12 N5 21(2) 5_544 2_545 ? N5 C12 C13 100(6) 6_554 . ? C12 C12 C13 137.6(19) 6_554 . ? N5 C12 C13 68(3) 5_544 . ? C12 C12 C13 101(4) 2_545 . ? N5 C12 C13 158(3) . . ? C12 C12 C13 131(5) 5_544 . ? N5 C12 C13 121(3) 2_545 . ? N5 C12 C13 25(7) 6_554 2_545 ? C12 C12 C13 126.4(12) 6_554 2_545 ? N5 C12 C13 63(3) 5_544 2_545 ? C12 C12 C13 52(2) 2_545 2_545 ? N5 C12 C13 108(3) . 2_545 ? C12 C12 C13 89(3) 5_544 2_545 ? N5 C12 C13 108(2) 2_545 2_545 ? C13 C12 C13 91(3) . 2_545 ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Pd1 I1 Pd1 63.87(5) . 6 ? Pd1 I2 Pd1 63.16(5) . 6 ? C3 N1 C3 83.5(18) 6_554 . ? C3 N1 C8 132.6(9) 6_554 . ? C3 N1 C8 132.6(9) . . ? C3 N1 C2 35.4(9) 6_554 . ? C3 N1 C2 107.5(12) . . ? C8 N1 C2 119.4(8) . . ? C3 N1 C2 107.5(12) 6_554 6_554 ? C3 N1 C2 35.4(9) . 6_554 ? C8 N1 C2 119.4(8) . 6_554 ? C2 N1 C2 113.7(14) . 6_554 ? N2 N2 C1 146.3(18) 6_554 6_554 ? N2 N2 C3 112.0(10) 6_554 . ? C1 N2 C3 77(2) 6_554 . ? N2 N2 C1 18.5(10) 6_554 . ? C1 N2 C1 128(3) 6_554 . ? C3 N2 C1 114.0(15) . . ? N2 N2 C4 121.6(8) 6_554 . ? C1 N2 C4 67.4(18) 6_554 . ? C3 N2 C4 124.2(13) . . ? C1 N2 C4 121.7(15) . . ? N2 N2 C3 46.7(8) 6_554 6_554 ? C1 N2 C3 130(2) 6_554 6_554 ? C3 N2 C3 65.3(15) . 6_554 ? C1 N2 C3 52.4(11) . 6_554 ? C4 N2 C3 162.5(14) . 6_554 ? N2 N2 C2 123.3(7) 6_554 6_554 ? C1 N2 C2 51.2(18) 6_554 6_554 ? C3 N2 C2 30.2(10) . 6_554 ? C1 N2 C2 115.0(13) . 6_554 ? C4 N2 C2 113.6(12) . 6_554 ? C3 N2 C2 81.9(10) 6_554 6_554 ? N2 N2 C4 41.2(6) 6_554 6_554 ? C1 N2 C4 132(2) 6_554 6_554 ? C3 N2 C4 150.2(15) . 6_554 ? C1 N2 C4 46.3(10) . 6_554 ? C4 N2 C4 80.3(13) . 6_554 ? C3 N2 C4 86.8(10) 6_554 6_554 ? C2 N2 C4 160.7(10) 6_554 6_554 ? N2 N2 Pd1 134.0(3) 6_554 6_554 ? C1 N2 Pd1 42.4(16) 6_554 6_554 ? C3 N2 Pd1 112.8(11) . 6_554 ? C1 N2 Pd1 124.6(12) . 6_554 ? C4 N2 Pd1 26.5(7) . 6_554 ? C3 N2 Pd1 170.2(11) 6_554 6_554 ? C2 N2 Pd1 92.4(8) 6_554 6_554 ? C4 N2 Pd1 96.4(7) 6_554 6_554 ? N3 N3 C7 145.4(19) 6_554 6_554 ? N3 N3 C5 111.8(10) 6_554 . ? C7 N3 C5 75(2) 6_554 . ? N3 N3 C7 18.1(10) 6_554 . ? C7 N3 C7 127(3) 6_554 . ? C5 N3 C7 112.5(15) . . ? N3 N3 C4 121.2(8) 6_554 . ? C7 N3 C4 70.5(18) 6_554 . ? C5 N3 C4 124.6(13) . . ? C7 N3 C4 122.9(14) . . ? N3 N3 C6 123.0(7) 6_554 6_554 ? C7 N3 C6 50.0(18) 6_554 6_554 ? C5 N3 C6 28.7(9) . 6_554 ? C7 N3 C6 114.2(13) . 6_554 ? C4 N3 C6 114.6(11) . 6_554 ? N3 N3 C5 46.2(7) 6_554 6_554 ? C7 N3 C5 128(2) 6_554 6_554 ? C5 N3 C5 65.6(16) . 6_554 ? C7 N3 C5 50.6(10) . 6_554 ? C4 N3 C5 161.8(13) . 6_554 ? C6 N3 C5 81.5(10) 6_554 6_554 ? N3 N3 C4 40.6(6) 6_554 6_554 ? C7 N3 C4 134(2) 6_554 6_554 ? C5 N3 C4 149.4(14) . 6_554 ? C7 N3 C4 46.9(9) . 6_554 ? C4 N3 C4 80.6(12) . 6_554 ? C6 N3 C4 160.9(10) 6_554 6_554 ? C5 N3 C4 85.7(9) 6_554 6_554 ? N3 N3 Pd1 134.0(3) 6_554 6_554 ? C7 N3 Pd1 44.8(17) 6_554 6_554 ? C5 N3 Pd1 112.9(11) . 6_554 ? C7 N3 Pd1 125.8(12) . 6_554 ? C4 N3 Pd1 27.2(7) . 6_554 ? C6 N3 Pd1 93.3(8) 6_554 6_554 ? C5 N3 Pd1 170.1(10) 6_554 6_554 ? C4 N3 Pd1 97.1(7) 6_554 6_554 ? C5 N4 C5 86.6(19) 6_554 . ? C5 N4 C11 131.4(9) 6_554 . ? C5 N4 C11 131.4(9) . . ? C5 N4 C6 33.4(8) 6_554 . ? C5 N4 C6 108.7(12) . . ? C11 N4 C6 119.4(8) . . ? C5 N4 C6 108.7(12) 6_554 6_554 ? C5 N4 C6 33.4(8) . 6_554 ? C11 N4 C6 119.4(8) . 6_554 ? C6 N4 C6 114.9(14) . 6_554 ? C12 N5 C12 73(8) 6_554 5_544 ? C12 N5 N5 61(6) 6_554 2_545 ? C12 N5 N5 31(3) 5_544 2_545 ? C12 N5 C12 37(5) 6_554 . ? C12 N5 C12 70(4) 5_544 . ? N5 N5 C12 78(3) 2_545 . ? C12 N5 C12 59(7) 6_554 2_545 ? C12 N5 C12 36(3) 5_544 2_545 ? N5 N5 C12 57.9(13) 2_545 2_545 ? C12 N5 C12 38(3) . 2_545 ? C12 N5 N5 58(5) 6_554 6_554 ? C12 N5 N5 72(3) 5_544 6_554 ? N5 N5 N5 90.000(4) 2_545 6_554 ? C12 N5 N5 21(2) . 6_554 ? C12 N5 N5 36.0(11) 2_545 6_554 ? C12 N5 C13 147(9) 6_554 5_544 ? C12 N5 C13 78(3) 5_544 5_544 ? N5 N5 C13 85(4) 2_545 5_544 ? C12 N5 C13 140(4) . 5_544 ? C12 N5 C13 103(3) 2_545 5_544 ? N5 N5 C13 126.2(19) 6_554 5_544 ? C12 N5 C13 63(4) 6_554 6_554 ? C12 N5 C13 89(3) 5_544 6_554 ? N5 N5 C13 59(3) 2_545 6_554 ? C12 N5 C13 100(2) . 6_554 ? C12 N5 C13 108(2) 2_545 6_554 ? N5 N5 C13 120.3(15) 6_554 6_554 ? C13 N5 C13 102(3) 5_544 6_554 ? C12 N5 N5 45(5) 6_554 5_544 ? C12 N5 N5 42(3) 5_544 5_544 ? N5 N5 N5 55(2) 2_545 5_544 ? C12 N5 N5 28.4(18) . 5_544 ? C12 N5 N5 14.7(17) 2_545 5_544 ? N5 N5 N5 35(2) 6_554 5_544 ? C13 N5 N5 116(4) 5_544 5_544 ? C13 N5 N5 96(2) 6_554 5_544 ? C4 Pd1 C1 43.6(8) 6_554 . ? C4 Pd1 C7 43.8(8) 6_554 . ? C1 Pd1 C7 87.3(8) . . ? C4 Pd1 N3 29.1(7) 6_554 6_554 ? C1 Pd1 N3 72.1(7) . 6_554 ? C7 Pd1 N3 15.5(5) . 6_554 ? C4 Pd1 N2 28.9(7) 6_554 6_554 ? C1 Pd1 N2 15.6(6) . 6_554 ? C7 Pd1 N2 72.0(6) . 6_554 ? N3 Pd1 N2 56.7(4) 6_554 6_554 ? C4 Pd1 I1 134.1(6) 6_554 . ? C1 Pd1 I1 90.6(6) . . ? C7 Pd1 I1 177.9(5) . . ? N3 Pd1 I1 162.5(3) 6_554 . ? N2 Pd1 I1 105.9(3) 6_554 . ? C4 Pd1 I2 133.9(6) 6_554 . ? C1 Pd1 I2 177.5(6) . . ? C7 Pd1 I2 90.3(5) . . ? N3 Pd1 I2 105.5(3) 6_554 . ? N2 Pd1 I2 162.0(3) 6_554 . ? I1 Pd1 I2 91.81(4) . . ? C4 Pd1 Pd1 135.6(7) 6_554 6 ? C1 Pd1 Pd1 122.8(6) . 6 ? C7 Pd1 Pd1 123.0(5) . 6 ? N3 Pd1 Pd1 134.0(3) 6_554 6 ? N2 Pd1 Pd1 134.0(3) 6_554 6 ? I1 Pd1 Pd1 58.06(3) . 6 ? I2 Pd1 Pd1 58.42(3) . 6 ? 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 N2 C1 C2 N1 16(2) 6_554 . . . ? C4 C1 C2 N1 108(4) 6_554 . . . ? C3 C1 C2 N1 43.1(14) 6_554 . . . ? N2 C1 C2 N1 0.7(18) . . . . ? C1 C1 C2 N1 -18.2(13) 6_554 . . . ? Pd1 C1 C2 N1 177.5(13) . . . . ? N4 C6 C7 N3 -19(3) . . . 6_554 ? N4 C6 C7 C5 -44.5(16) . . . 6_554 ? N4 C6 C7 N3 -2.1(18) . . . . ? N4 C6 C7 C4 -112(4) . . . 6_554 ? N4 C6 C7 C7 16.5(12) . . . 6_554 ? N4 C6 C7 Pd1 -177.5(12) . . . . ? C2 C3 N1 C3 132.9(15) 6_554 . . 6_554 ? N2 C3 N1 C3 31(2) . . . 6_554 ? C1 C3 N1 C3 66(3) 6_554 . . 6_554 ? C9 C3 N1 C3 -153.8(13) . . . 6_554 ? N2 C3 N1 C3 22.4(17) 6_554 . . 6_554 ? C2 C3 N1 C8 -82(2) 6_554 . . . ? N2 C3 N1 C8 176.2(14) . . . . ? C1 C3 N1 C8 -148.6(17) 6_554 . . . ? C9 C3 N1 C8 -9(3) . . . . ? C3 C3 N1 C8 145(2) 6_554 . . . ? N2 C3 N1 C8 167.5(13) 6_554 . . . ? C2 C3 N1 C2 106(2) 6_554 . . . ? N2 C3 N1 C2 5(2) . . . . ? C1 C3 N1 C2 40(3) 6_554 . . . ? C9 C3 N1 C2 179.8(16) . . . . ? C3 C3 N1 C2 -26.4(9) 6_554 . . . ? N2 C3 N1 C2 -4.1(17) 6_554 . . . ? N2 C3 N1 C2 -102(2) . . . 6_554 ? C1 C3 N1 C2 -67(2) 6_554 . . 6_554 ? C9 C3 N1 C2 73(2) . . . 6_554 ? C3 C3 N1 C2 -132.9(15) 6_554 . . 6_554 ? N2 C3 N1 C2 -111(2) 6_554 . . 6_554 ? C1 C2 N1 C3 -53.1(18) . . . 6_554 ? C1 C2 N1 C3 -3(2) . . . . ? C1 C2 N1 C8 -176.2(14) . . . . ? C1 C2 N1 C2 34(2) . . . 6_554 ? C2 C3 N2 N2 -118.8(17) 6_554 . . 6_554 ? N1 C3 N2 N2 -24(2) . . . 6_554 ? C1 C3 N2 N2 -146.0(18) 6_554 . . 6_554 ? C9 C3 N2 N2 160.7(18) . . . 6_554 ? C3 C3 N2 N2 0.000(10) 6_554 . . 6_554 ? C2 C3 N2 C1 27(2) 6_554 . . 6_554 ? N1 C3 N2 C1 122(2) . . . 6_554 ? C9 C3 N2 C1 -53(3) . . . 6_554 ? C3 C3 N2 C1 146.0(18) 6_554 . . 6_554 ? N2 C3 N2 C1 146.0(18) 6_554 . . 6_554 ? C2 C3 N2 C1 -99(2) 6_554 . . . ? N1 C3 N2 C1 -5(2) . . . . ? C1 C3 N2 C1 -126(3) 6_554 . . . ? C9 C3 N2 C1 -179(2) . . . . ? C3 C3 N2 C1 20.0(11) 6_554 . . . ? N2 C3 N2 C1 20.0(11) 6_554 . . . ? C2 C3 N2 C4 78(2) 6_554 . . . ? N1 C3 N2 C4 172.4(15) . . . . ? C1 C3 N2 C4 50.9(19) 6_554 . . . ? C9 C3 N2 C4 -2(3) . . . . ? C3 C3 N2 C4 -163.1(19) 6_554 . . . ? N2 C3 N2 C4 -163.1(19) 6_554 . . . ? C2 C3 N2 C3 -118.8(17) 6_554 . . 6_554 ? N1 C3 N2 C3 -24(2) . . . 6_554 ? C1 C3 N2 C3 -146.0(18) 6_554 . . 6_554 ? C9 C3 N2 C3 160.7(18) . . . 6_554 ? N2 C3 N2 C3 0.000(16) 6_554 . . 6_554 ? N1 C3 N2 C2 94(2) . . . 6_554 ? C1 C3 N2 C2 -27(2) 6_554 . . 6_554 ? C9 C3 N2 C2 -80(3) . . . 6_554 ? C3 C3 N2 C2 118.8(17) 6_554 . . 6_554 ? N2 C3 N2 C2 118.8(17) 6_554 . . 6_554 ? C2 C3 N2 C4 -141(3) 6_554 . . 6_554 ? N1 C3 N2 C4 -47(4) . . . 6_554 ? C1 C3 N2 C4 -168(3) 6_554 . . 6_554 ? C9 C3 N2 C4 139(2) . . . 6_554 ? C3 C3 N2 C4 -22(2) 6_554 . . 6_554 ? N2 C3 N2 C4 -22(2) 6_554 . . 6_554 ? C2 C3 N2 Pd1 51(2) 6_554 . . 6_554 ? N1 C3 N2 Pd1 145.0(13) . . . 6_554 ? C1 C3 N2 Pd1 23.5(15) 6_554 . . 6_554 ? C9 C3 N2 Pd1 -30(3) . . . 6_554 ? C3 C3 N2 Pd1 169.5(11) 6_554 . . 6_554 ? N2 C3 N2 Pd1 169.5(11) 6_554 . . 6_554 ? C2 C1 N2 N2 90(3) . . . 6_554 ? C4 C1 N2 N2 -65(3) 6_554 . . 6_554 ? C3 C1 N2 N2 65(3) 6_554 . . 6_554 ? C1 C1 N2 N2 180.00(3) 6_554 . . 6_554 ? Pd1 C1 N2 N2 -88(3) . . . 6_554 ? N2 C1 N2 C1 180.00(3) 6_554 . . 6_554 ? C2 C1 N2 C1 -90(3) . . . 6_554 ? C4 C1 N2 C1 115(3) 6_554 . . 6_554 ? C3 C1 N2 C1 -115(3) 6_554 . . 6_554 ? Pd1 C1 N2 C1 92(3) . . . 6_554 ? N2 C1 N2 C3 -88(3) 6_554 . . . ? C2 C1 N2 C3 2(2) . . . . ? C4 C1 N2 C3 -152.6(17) 6_554 . . . ? C3 C1 N2 C3 -23.0(14) 6_554 . . . ? C1 C1 N2 C3 92(3) 6_554 . . . ? Pd1 C1 N2 C3 -175.2(14) . . . . ? N2 C1 N2 C4 95(3) 6_554 . . . ? C2 C1 N2 C4 -175.0(15) . . . . ? C4 C1 N2 C4 30.3(17) 6_554 . . . ? C3 C1 N2 C4 159.9(17) 6_554 . . . ? C1 C1 N2 C4 -85(3) 6_554 . . . ? Pd1 C1 N2 C4 8(2) . . . . ? N2 C1 N2 C3 -65(3) 6_554 . . 6_554 ? C2 C1 N2 C3 25.1(12) . . . 6_554 ? C4 C1 N2 C3 -129.6(16) 6_554 . . 6_554 ? C1 C1 N2 C3 115(3) 6_554 . . 6_554 ? Pd1 C1 N2 C3 -152.1(18) . . . 6_554 ? N2 C1 N2 C2 -121(3) 6_554 . . 6_554 ? C2 C1 N2 C2 -31.1(17) . . . 6_554 ? C4 C1 N2 C2 174.2(14) 6_554 . . 6_554 ? C3 C1 N2 C2 -56.2(14) 6_554 . . 6_554 ? C1 C1 N2 C2 59(3) 6_554 . . 6_554 ? Pd1 C1 N2 C2 151.6(12) . . . 6_554 ? N2 C1 N2 C4 65(3) 6_554 . . 6_554 ? C2 C1 N2 C4 155(2) . . . 6_554 ? C3 C1 N2 C4 129.6(16) 6_554 . . 6_554 ? C1 C1 N2 C4 -115(3) 6_554 . . 6_554 ? Pd1 C1 N2 C4 -22.5(10) . . . 6_554 ? N2 C1 N2 Pd1 127(3) 6_554 . . 6_554 ? C2 C1 N2 Pd1 -143.3(12) . . . 6_554 ? C4 C1 N2 Pd1 62.0(15) 6_554 . . 6_554 ? C3 C1 N2 Pd1 -168.4(13) 6_554 . . 6_554 ? C1 C1 N2 Pd1 -53(3) 6_554 . . 6_554 ? Pd1 C1 N2 Pd1 39(2) . . . 6_554 ? N3 C4 N2 N2 -32.7(14) . . . 6_554 ? N3 C4 N2 C1 -176(2) . . . 6_554 ? N3 C4 N2 C3 128.8(18) . . . . ? N3 C4 N2 C1 -54(2) . . . . ? N3 C4 N2 C3 10(5) . . . 6_554 ? N3 C4 N2 C2 161.2(12) . . . 6_554 ? N3 C4 N2 C4 -32.7(14) . . . 6_554 ? N3 C4 N2 Pd1 -159(2) . . . 6_554 ? C6 C5 N3 N3 119.3(18) 6_554 . . 6_554 ? N4 C5 N3 N3 23.2(18) . . . 6_554 ? C7 C5 N3 N3 144(2) 6_554 . . 6_554 ? C10 C5 N3 N3 -160.6(17) . . . 6_554 ? C5 C5 N3 N3 0.000(3) 6_554 . . 6_554 ? C6 C5 N3 C7 -25(3) 6_554 . . 6_554 ? N4 C5 N3 C7 -121(2) . . . 6_554 ? C10 C5 N3 C7 55(3) . . . 6_554 ? C5 C5 N3 C7 -144(2) 6_554 . . 6_554 ? N3 C5 N3 C7 -144(2) 6_554 . . 6_554 ? C6 C5 N3 C7 100(2) 6_554 . . . ? N4 C5 N3 C7 4(2) . . . . ? C7 C5 N3 C7 125(3) 6_554 . . . ? C10 C5 N3 C7 179.8(19) . . . . ? C5 C5 N3 C7 -19.6(11) 6_554 . . . ? N3 C5 N3 C7 -19.6(11) 6_554 . . . ? C6 C5 N3 C4 -78(2) 6_554 . . . ? N4 C5 N3 C4 -174.2(15) . . . . ? C7 C5 N3 C4 -53(2) 6_554 . . . ? C10 C5 N3 C4 2(3) . . . . ? C5 C5 N3 C4 162.6(19) 6_554 . . . ? N3 C5 N3 C4 162.6(19) 6_554 . . . ? N4 C5 N3 C6 -96(2) . . . 6_554 ? C7 C5 N3 C6 25(3) 6_554 . . 6_554 ? C10 C5 N3 C6 80(3) . . . 6_554 ? C5 C5 N3 C6 -119.3(18) 6_554 . . 6_554 ? N3 C5 N3 C6 -119.3(18) 6_554 . . 6_554 ? C6 C5 N3 C5 119.3(18) 6_554 . . 6_554 ? N4 C5 N3 C5 23.2(18) . . . 6_554 ? C7 C5 N3 C5 144(2) 6_554 . . 6_554 ? C10 C5 N3 C5 -160.6(17) . . . 6_554 ? N3 C5 N3 C5 0.000(6) 6_554 . . 6_554 ? C6 C5 N3 C4 141(3) 6_554 . . 6_554 ? N4 C5 N3 C4 45(3) . . . 6_554 ? C7 C5 N3 C4 166(4) 6_554 . . 6_554 ? C10 C5 N3 C4 -139(2) . . . 6_554 ? C5 C5 N3 C4 22(2) 6_554 . . 6_554 ? N3 C5 N3 C4 22(2) 6_554 . . 6_554 ? C6 C5 N3 Pd1 -50(2) 6_554 . . 6_554 ? N4 C5 N3 Pd1 -146.1(13) . . . 6_554 ? C7 C5 N3 Pd1 -25.0(16) 6_554 . . 6_554 ? C10 C5 N3 Pd1 30(2) . . . 6_554 ? C5 C5 N3 Pd1 -169.3(11) 6_554 . . 6_554 ? N3 C5 N3 Pd1 -169.3(11) 6_554 . . 6_554 ? C6 C7 N3 N3 -92(3) . . . 6_554 ? C5 C7 N3 N3 -68(3) 6_554 . . 6_554 ? C4 C7 N3 N3 61(3) 6_554 . . 6_554 ? C7 C7 N3 N3 180.00(3) 6_554 . . 6_554 ? Pd1 C7 N3 N3 84(3) . . . 6_554 ? N3 C7 N3 C7 180.00(3) 6_554 . . 6_554 ? C6 C7 N3 C7 88(3) . . . 6_554 ? C5 C7 N3 C7 112(3) 6_554 . . 6_554 ? C4 C7 N3 C7 -119(3) 6_554 . . 6_554 ? Pd1 C7 N3 C7 -96(3) . . . 6_554 ? N3 C7 N3 C5 92(3) 6_554 . . . ? C6 C7 N3 C5 -1(2) . . . . ? C5 C7 N3 C5 23.3(14) 6_554 . . . ? C4 C7 N3 C5 152.7(16) 6_554 . . . ? C7 C7 N3 C5 -88(3) 6_554 . . . ? Pd1 C7 N3 C5 175.4(14) . . . . ? N3 C7 N3 C4 -91(3) 6_554 . . . ? C6 C7 N3 C4 177.3(15) . . . . ? C5 C7 N3 C4 -158.9(17) 6_554 . . . ? C4 C7 N3 C4 -29.4(17) 6_554 . . . ? C7 C7 N3 C4 89(3) 6_554 . . . ? Pd1 C7 N3 C4 -7(2) . . . . ? N3 C7 N3 C6 123(3) 6_554 . . 6_554 ? C6 C7 N3 C6 30.7(17) . . . 6_554 ? C5 C7 N3 C6 54.6(14) 6_554 . . 6_554 ? C4 C7 N3 C6 -176.0(13) 6_554 . . 6_554 ? C7 C7 N3 C6 -57(3) 6_554 . . 6_554 ? Pd1 C7 N3 C6 -153.4(11) . . . 6_554 ? N3 C7 N3 C5 68(3) 6_554 . . 6_554 ? C6 C7 N3 C5 -23.9(11) . . . 6_554 ? C4 C7 N3 C5 129.4(16) 6_554 . . 6_554 ? C7 C7 N3 C5 -112(3) 6_554 . . 6_554 ? Pd1 C7 N3 C5 152.1(19) . . . 6_554 ? N3 C7 N3 C4 -61(3) 6_554 . . 6_554 ? C6 C7 N3 C4 -153.3(19) . . . 6_554 ? C5 C7 N3 C4 -129.4(16) 6_554 . . 6_554 ? C7 C7 N3 C4 119(3) 6_554 . . 6_554 ? Pd1 C7 N3 C4 22.7(10) . . . 6_554 ? N3 C7 N3 Pd1 -123(3) 6_554 . . 6_554 ? C6 C7 N3 Pd1 144.4(12) . . . 6_554 ? C5 C7 N3 Pd1 168.3(12) 6_554 . . 6_554 ? C4 C7 N3 Pd1 -62.3(15) 6_554 . . 6_554 ? C7 C7 N3 Pd1 57(3) 6_554 . . 6_554 ? Pd1 C7 N3 Pd1 -40(2) . . . 6_554 ? N2 C4 N3 N3 32.6(15) . . . 6_554 ? N2 C4 N3 C7 176(2) . . . 6_554 ? N2 C4 N3 C5 -128.5(18) . . . . ? N2 C4 N3 C7 54(2) . . . . ? N2 C4 N3 C6 -159.6(12) . . . 6_554 ? N2 C4 N3 C5 -9(5) . . . 6_554 ? N2 C4 N3 C4 32.6(15) . . . 6_554 ? N2 C4 N3 Pd1 159(2) . . . 6_554 ? C6 C5 N4 C5 -132.4(16) 6_554 . . 6_554 ? N3 C5 N4 C5 -30(2) . . . 6_554 ? C7 C5 N4 C5 -63(3) 6_554 . . 6_554 ? C10 C5 N4 C5 153.4(12) . . . 6_554 ? N3 C5 N4 C5 -21.7(16) 6_554 . . 6_554 ? C6 C5 N4 C11 81(2) 6_554 . . . ? N3 C5 N4 C11 -176.4(13) . . . . ? C7 C5 N4 C11 150.4(17) 6_554 . . . ? C10 C5 N4 C11 7(3) . . . . ? C5 C5 N4 C11 -146(2) 6_554 . . . ? N3 C5 N4 C11 -167.9(13) 6_554 . . . ? C6 C5 N4 C6 -107(2) 6_554 . . . ? N3 C5 N4 C6 -5(2) . . . . ? C7 C5 N4 C6 -38(3) 6_554 . . . ? C10 C5 N4 C6 178.8(15) . . . . ? C5 C5 N4 C6 25.4(8) 6_554 . . . ? N3 C5 N4 C6 3.7(16) 6_554 . . . ? N3 C5 N4 C6 102(2) . . . 6_554 ? C7 C5 N4 C6 69(2) 6_554 . . 6_554 ? C10 C5 N4 C6 -74(2) . . . 6_554 ? C5 C5 N4 C6 132.4(16) 6_554 . . 6_554 ? N3 C5 N4 C6 111(2) 6_554 . . 6_554 ? C7 C6 N4 C5 55.5(19) . . . 6_554 ? C7 C6 N4 C5 4(2) . . . . ? C7 C6 N4 C11 177.2(13) . . . . ? C7 C6 N4 C6 -31(2) . . . 6_554 ? N5 C12 N5 C12 180.00(2) 6_554 . . 6_554 ? N5 C12 N5 C12 -88(9) 5_544 . . 6_554 ? C12 C12 N5 C12 -109(8) 2_545 . . 6_554 ? C12 C12 N5 C12 -88(9) 5_544 . . 6_554 ? N5 C12 N5 C12 -57(7) 2_545 . . 6_554 ? C13 C12 N5 C12 -7(21) . . . 6_554 ? C13 C12 N5 C12 -155(7) 2_545 . . 6_554 ? N5 C12 N5 C12 -92(9) 6_554 . . 5_544 ? C12 C12 N5 C12 88(9) 6_554 . . 5_544 ? N5 C12 N5 C12 0.000(7) 5_544 . . 5_544 ? C12 C12 N5 C12 -21(2) 2_545 . . 5_544 ? N5 C12 N5 C12 31(3) 2_545 . . 5_544 ? C13 C12 N5 C12 81(14) . . . 5_544 ? C13 C12 N5 C12 -67(3) 2_545 . . 5_544 ? N5 C12 N5 N5 -123(7) 6_554 . . 2_545 ? C12 C12 N5 N5 57(7) 6_554 . . 2_545 ? N5 C12 N5 N5 -31(3) 5_544 . . 2_545 ? C12 C12 N5 N5 -52(4) 2_545 . . 2_545 ? C12 C12 N5 N5 -31(3) 5_544 . . 2_545 ? C13 C12 N5 N5 50(15) . . . 2_545 ? C13 C12 N5 N5 -98(3) 2_545 . . 2_545 ? N5 C12 N5 C12 -71(8) 6_554 . . 2_545 ? C12 C12 N5 C12 109(8) 6_554 . . 2_545 ? N5 C12 N5 C12 21(2) 5_544 . . 2_545 ? C12 C12 N5 C12 21(2) 5_544 . . 2_545 ? N5 C12 N5 C12 52(4) 2_545 . . 2_545 ? C13 C12 N5 C12 102(15) . . . 2_545 ? C13 C12 N5 C12 -46(3) 2_545 . . 2_545 ? C12 C12 N5 N5 180.000(18) 6_554 . . 6_554 ? N5 C12 N5 N5 92(9) 5_544 . . 6_554 ? C12 C12 N5 N5 71(8) 2_545 . . 6_554 ? C12 C12 N5 N5 92(9) 5_544 . . 6_554 ? N5 C12 N5 N5 123(7) 2_545 . . 6_554 ? C13 C12 N5 N5 173(21) . . . 6_554 ? C13 C12 N5 N5 25(7) 2_545 . . 6_554 ? N5 C12 N5 C13 -55(13) 6_554 . . 5_544 ? C12 C12 N5 C13 125(13) 6_554 . . 5_544 ? N5 C12 N5 C13 37(6) 5_544 . . 5_544 ? C12 C12 N5 C13 16(8) 2_545 . . 5_544 ? C12 C12 N5 C13 37(6) 5_544 . . 5_544 ? N5 C12 N5 C13 68(6) 2_545 . . 5_544 ? C13 C12 N5 C13 118(10) . . . 5_544 ? C13 C12 N5 C13 -30(7) 2_545 . . 5_544 ? N5 C12 N5 C13 -178(7) 6_554 . . 6_554 ? C12 C12 N5 C13 2(7) 6_554 . . 6_554 ? N5 C12 N5 C13 -86(4) 5_544 . . 6_554 ? C12 C12 N5 C13 -107(4) 2_545 . . 6_554 ? C12 C12 N5 C13 -86(4) 5_544 . . 6_554 ? N5 C12 N5 C13 -55(3) 2_545 . . 6_554 ? C13 C12 N5 C13 -5(14) . . . 6_554 ? C13 C12 N5 C13 -153.0(15) 2_545 . . 6_554 ? N5 C12 N5 N5 -92(9) 6_554 . . 5_544 ? C12 C12 N5 N5 88(9) 6_554 . . 5_544 ? C12 C12 N5 N5 -21(2) 2_545 . . 5_544 ? C12 C12 N5 N5 0.000(13) 5_544 . . 5_544 ? N5 C12 N5 N5 31(3) 2_545 . . 5_544 ? C13 C12 N5 N5 81(14) . . . 5_544 ? C13 C12 N5 N5 -67(3) 2_545 . . 5_544 ? N2 C1 Pd1 C4 16(2) 6_554 . . 6_554 ? C2 C1 Pd1 C4 -142(3) . . . 6_554 ? C3 C1 Pd1 C4 -85(3) 6_554 . . 6_554 ? N2 C1 Pd1 C4 34.1(15) . . . 6_554 ? C1 C1 Pd1 C4 56.2(12) 6_554 . . 6_554 ? N2 C1 Pd1 C7 12(2) 6_554 . . . ? C2 C1 Pd1 C7 -147(2) . . . . ? C4 C1 Pd1 C7 -4.4(13) 6_554 . . . ? C3 C1 Pd1 C7 -90(3) 6_554 . . . ? N2 C1 Pd1 C7 29.7(16) . . . . ? C1 C1 Pd1 C7 51.8(6) 6_554 . . . ? N2 C1 Pd1 N3 9(2) 6_554 . . 6_554 ? C2 C1 Pd1 N3 -150(2) . . . 6_554 ? C4 C1 Pd1 N3 -7.6(12) 6_554 . . 6_554 ? C3 C1 Pd1 N3 -93(3) 6_554 . . 6_554 ? N2 C1 Pd1 N3 26.5(14) . . . 6_554 ? C1 C1 Pd1 N3 48.6(4) 6_554 . . 6_554 ? C2 C1 Pd1 N2 -158(4) . . . 6_554 ? C4 C1 Pd1 N2 -16(2) 6_554 . . 6_554 ? C3 C1 Pd1 N2 -102(4) 6_554 . . 6_554 ? N2 C1 Pd1 N2 18.0(12) . . . 6_554 ? C1 C1 Pd1 N2 40(2) 6_554 . . 6_554 ? N2 C1 Pd1 I1 -169(2) 6_554 . . . ? C2 C1 Pd1 I1 33.1(19) . . . . ? C4 C1 Pd1 I1 175.3(12) 6_554 . . . ? C3 C1 Pd1 I1 90(3) 6_554 . . . ? N2 C1 Pd1 I1 -150.6(15) . . . . ? C1 C1 Pd1 I1 -128.5(3) 6_554 . . . ? N2 C1 Pd1 I2 21(15) 6_554 . . . ? C2 C1 Pd1 I2 -137(12) . . . . ? C4 C1 Pd1 I2 5(13) 6_554 . . . ? C3 C1 Pd1 I2 -80(14) 6_554 . . . ? N2 C1 Pd1 I2 39(14) . . . . ? C1 C1 Pd1 I2 61(13) 6_554 . . . ? N2 C1 Pd1 Pd1 140(2) 6_554 . . 6 ? C2 C1 Pd1 Pd1 -18(2) . . . 6 ? C4 C1 Pd1 Pd1 123.8(12) 6_554 . . 6 ? C3 C1 Pd1 Pd1 38(3) 6_554 . . 6 ? N2 C1 Pd1 Pd1 157.9(13) . . . 6 ? C1 C1 Pd1 Pd1 180.000(5) 6_554 . . 6 ? N3 C7 Pd1 C4 -16(2) 6_554 . . 6_554 ? C6 C7 Pd1 C4 140(2) . . . 6_554 ? C5 C7 Pd1 C4 87(3) 6_554 . . 6_554 ? N3 C7 Pd1 C4 -34.7(14) . . . 6_554 ? C7 C7 Pd1 C4 -56.4(11) 6_554 . . 6_554 ? N3 C7 Pd1 C1 -11(2) 6_554 . . . ? C6 C7 Pd1 C1 144.3(19) . . . . ? C5 C7 Pd1 C1 92(3) 6_554 . . . ? N3 C7 Pd1 C1 -30.3(15) . . . . ? C4 C7 Pd1 C1 4.4(13) 6_554 . . . ? C7 C7 Pd1 C1 -52.0(6) 6_554 . . . ? C6 C7 Pd1 N3 156(4) . . . 6_554 ? C5 C7 Pd1 N3 103(4) 6_554 . . 6_554 ? N3 C7 Pd1 N3 -19.0(12) . . . 6_554 ? C4 C7 Pd1 N3 16(2) 6_554 . . 6_554 ? C7 C7 Pd1 N3 -41(2) 6_554 . . 6_554 ? N3 C7 Pd1 N2 -8(2) 6_554 . . 6_554 ? C6 C7 Pd1 N2 148(2) . . . 6_554 ? C5 C7 Pd1 N2 95(3) 6_554 . . 6_554 ? N3 C7 Pd1 N2 -27.0(13) . . . 6_554 ? C4 C7 Pd1 N2 7.7(11) 6_554 . . 6_554 ? C7 C7 Pd1 N2 -48.7(4) 6_554 . . 6_554 ? N3 C7 Pd1 I1 -20(16) 6_554 . . . ? C6 C7 Pd1 I1 136(13) . . . . ? C5 C7 Pd1 I1 84(14) 6_554 . . . ? N3 C7 Pd1 I1 -38(15) . . . . ? C4 C7 Pd1 I1 -4(14) 6_554 . . . ? C7 C7 Pd1 I1 -60(14) 6_554 . . . ? N3 C7 Pd1 I2 169(2) 6_554 . . . ? C6 C7 Pd1 I2 -35.3(18) . . . . ? C5 C7 Pd1 I2 -88(3) 6_554 . . . ? N3 C7 Pd1 I2 150.1(14) . . . . ? C4 C7 Pd1 I2 -175.2(12) 6_554 . . . ? C7 C7 Pd1 I2 128.4(3) 6_554 . . . ? N3 C7 Pd1 Pd1 -139(2) 6_554 . . 6 ? C6 C7 Pd1 Pd1 16(2) . . . 6 ? C5 C7 Pd1 Pd1 -36(3) 6_554 . . 6 ? N3 C7 Pd1 Pd1 -158.3(12) . . . 6 ? C4 C7 Pd1 Pd1 -123.6(11) 6_554 . . 6 ? C7 C7 Pd1 Pd1 180.000(2) 6_554 . . 6 ? Pd1 I1 Pd1 C4 -124.6(10) 6 . . 6_554 ? Pd1 I1 Pd1 C1 -129.2(5) 6 . . . ? Pd1 I1 Pd1 C7 -121(14) 6 . . . ? Pd1 I1 Pd1 N3 -138.3(10) 6 . . 6_554 ? Pd1 I1 Pd1 N2 -132.3(3) 6 . . 6_554 ? Pd1 I1 Pd1 I2 50.43(4) 6 . . . ? Pd1 I2 Pd1 C4 124.9(10) 6 . . 6_554 ? Pd1 I2 Pd1 C1 120(13) 6 . . . ? Pd1 I2 Pd1 C7 129.5(5) 6 . . . ? Pd1 I2 Pd1 N3 132.6(3) 6 . . 6_554 ? Pd1 I2 Pd1 N2 138.5(9) 6 . . 6_554 ? Pd1 I2 Pd1 I1 -50.16(4) 6 . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.693 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.165 ############################################### data_2c _database_code_depnum_ccdc_archive 'CCDC 695649' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 I2 N4 Pd' _chemical_formula_weight 772.77 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' N N 0.0061 0.0033 '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' 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_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8664(11) _cell_length_b 12.3939(15) _cell_length_c 12.8016(13) _cell_angle_alpha 66.710(8) _cell_angle_beta 83.725(9) _cell_angle_gamma 78.530(9) _cell_volume 1408.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13671 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 25.55 _exptl_crystal_description block _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 2.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.619 _exptl_absorpt_correction_T_max 0.678 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 15991 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.14 _reflns_number_total 5004 _reflns_number_gt 3974 _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^)+(0.0341P)^2^+0.0000P] 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 5004 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.001 _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 1.0530(4) 0.6738(3) 0.2256(3) 0.0319(8) Uani 1 1 d . . . C2 C 1.0993(4) 0.7194(4) 0.1156(3) 0.0353(9) Uani 1 1 d . . . H2A H 1.0439 0.7645 0.0536 0.042 Uiso 1 1 calc R . . C3 C 1.2876(4) 0.6235(3) 0.2145(3) 0.0329(8) Uani 1 1 d . . . C4 C 1.1748(4) 0.5500(3) 0.4070(3) 0.0376(9) Uani 1 1 d . . . H4A H 1.1282 0.4821 0.4280 0.045 Uiso 1 1 calc R . . H4B H 1.2690 0.5212 0.4326 0.045 Uiso 1 1 calc R . . C5 C 1.1515(4) 0.6527(3) 0.5418(3) 0.0336(8) Uani 1 1 d . . . C6 C 0.9403(4) 0.7571(3) 0.4973(3) 0.0346(8) Uani 1 1 d . . . H6A H 0.8584 0.8089 0.4987 0.042 Uiso 1 1 calc R . . C7 C 0.9687(4) 0.6954(3) 0.4281(3) 0.0326(8) Uani 1 1 d . . . C8 C 1.3267(4) 0.7313(4) 0.0072(3) 0.0340(8) Uani 1 1 d . . . C9 C 1.3767(4) 0.8355(4) -0.0171(4) 0.0386(9) Uani 1 1 d . . . C10 C 1.4511(4) 0.8797(4) -0.1199(4) 0.0457(10) Uani 1 1 d . . . H10A H 1.4860 0.9497 -0.1385 0.055 Uiso 1 1 calc R . . C11 C 1.4743(4) 0.8215(4) -0.1950(4) 0.0455(10) Uani 1 1 d . . . C12 C 1.4229(4) 0.7177(4) -0.1659(4) 0.0455(10) Uani 1 1 d . . . H12A H 1.4395 0.6779 -0.2155 0.055 Uiso 1 1 calc R . . C13 C 1.3470(4) 0.6700(4) -0.0651(3) 0.0400(9) Uani 1 1 d . . . C14 C 1.3543(5) 0.8995(4) 0.0641(4) 0.0528(11) Uani 1 1 d . . . H14A H 1.4271 0.8674 0.1176 0.079 Uiso 1 1 calc R . . H14B H 1.2668 0.8888 0.1042 0.079 Uiso 1 1 calc R . . H14C H 1.3548 0.9830 0.0219 0.079 Uiso 1 1 calc R . . C15 C 1.5533(6) 0.8724(5) -0.3059(4) 0.0680(15) Uani 1 1 d . . . H15A H 1.6452 0.8759 -0.2909 0.102 Uiso 1 1 calc R . . H15B H 1.5070 0.9513 -0.3494 0.102 Uiso 1 1 calc R . . H15C H 1.5579 0.8226 -0.3480 0.102 Uiso 1 1 calc R . . C16 C 1.2882(5) 0.5585(4) -0.0363(4) 0.0562(12) Uani 1 1 d . . . H16A H 1.1906 0.5736 -0.0199 0.084 Uiso 1 1 calc R . . H16B H 1.3326 0.4964 0.0290 0.084 Uiso 1 1 calc R . . H16C H 1.3036 0.5341 -0.0997 0.084 Uiso 1 1 calc R . . C17 C 1.4312(4) 0.5705(4) 0.2469(4) 0.0450(10) Uani 1 1 d . . . H17A H 1.4612 0.6081 0.2910 0.067 Uiso 1 1 calc R . . H17B H 1.4896 0.5819 0.1796 0.067 Uiso 1 1 calc R . . H17C H 1.4368 0.4867 0.2914 0.067 Uiso 1 1 calc R . . C18 C 1.2851(4) 0.5999(4) 0.5983(4) 0.0429(10) Uani 1 1 d . . . H18A H 1.3594 0.6228 0.5436 0.064 Uiso 1 1 calc R . . H18B H 1.2939 0.5146 0.6303 0.064 Uiso 1 1 calc R . . H18C H 1.2889 0.6279 0.6578 0.064 Uiso 1 1 calc R . . C19 C 1.0593(4) 0.7881(3) 0.6433(3) 0.0347(8) Uani 1 1 d . . . C20 C 0.9817(4) 0.7550(4) 0.7441(3) 0.0395(9) Uani 1 1 d . . . C21 C 0.9773(4) 0.8212(4) 0.8111(3) 0.0435(10) Uani 1 1 d . . . H21A H 0.9232 0.8025 0.8780 0.052 Uiso 1 1 calc R . . C22 C 1.0510(4) 0.9138(3) 0.7809(3) 0.0402(9) Uani 1 1 d . . . C23 C 1.1320(4) 0.9403(3) 0.6811(4) 0.0411(10) Uani 1 1 d . . . H23A H 1.1851 0.9999 0.6621 0.049 Uiso 1 1 calc R . . C24 C 1.1362(4) 0.8809(4) 0.6090(3) 0.0381(9) Uani 1 1 d . . . C25 C 0.9060(5) 0.6505(4) 0.7822(4) 0.0558(12) Uani 1 1 d . . . H25A H 0.9719 0.5781 0.7974 0.084 Uiso 1 1 calc R . . H25B H 0.8466 0.6604 0.7233 0.084 Uiso 1 1 calc R . . H25C H 0.8515 0.6464 0.8501 0.084 Uiso 1 1 calc R . . C26 C 1.0409(5) 0.9882(4) 0.8506(4) 0.0562(12) Uani 1 1 d . . . H26A H 1.1305 0.9806 0.8780 0.084 Uiso 1 1 calc R . . H26B H 0.9772 0.9615 0.9139 0.084 Uiso 1 1 calc R . . H26C H 1.0086 1.0702 0.8043 0.084 Uiso 1 1 calc R . . C27 C 1.2176(5) 0.9168(4) 0.4979(4) 0.0507(11) Uani 1 1 d . . . H27C H 1.2550 0.9868 0.4863 0.076 Uiso 1 1 calc R . . H27A H 1.1581 0.9336 0.4369 0.076 Uiso 1 1 calc R . . H27B H 1.2919 0.8530 0.4996 0.076 Uiso 1 1 calc R . . N1 N 1.2428(3) 0.6881(3) 0.1101(3) 0.0323(7) Uani 1 1 d . . . N2 N 1.1749(3) 0.6147(3) 0.2846(3) 0.0311(7) Uani 1 1 d . . . N3 N 1.1030(3) 0.6311(3) 0.4590(3) 0.0332(7) Uani 1 1 d . . . N4 N 1.0523(3) 0.7312(3) 0.5659(3) 0.0340(7) Uani 1 1 d . . . I1 I 0.75005(3) 0.71346(3) 0.11705(2) 0.04592(9) Uani 1 1 d . . . I2 I 0.62159(3) 0.74523(3) 0.40173(2) 0.04484(9) Uani 1 1 d . . . Pd1 Pd 0.86799(3) 0.69846(3) 0.29992(2) 0.03109(8) 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 0.036(2) 0.0294(19) 0.029(2) -0.0093(16) -0.0005(16) -0.0076(15) C2 0.0332(19) 0.039(2) 0.033(2) -0.0105(18) 0.0008(16) -0.0127(16) C3 0.0331(19) 0.034(2) 0.035(2) -0.0166(17) 0.0047(16) -0.0103(16) C4 0.042(2) 0.032(2) 0.034(2) -0.0092(17) 0.0009(17) -0.0026(17) C5 0.037(2) 0.035(2) 0.029(2) -0.0112(17) 0.0046(16) -0.0103(16) C6 0.038(2) 0.034(2) 0.029(2) -0.0102(17) -0.0023(16) -0.0054(16) C7 0.0355(19) 0.034(2) 0.0231(19) -0.0063(16) 0.0029(15) -0.0066(16) C8 0.0309(19) 0.041(2) 0.029(2) -0.0108(17) 0.0031(15) -0.0113(16) C9 0.036(2) 0.041(2) 0.042(2) -0.0170(19) 0.0040(17) -0.0149(17) C10 0.045(2) 0.047(3) 0.046(3) -0.014(2) 0.0065(19) -0.022(2) C11 0.036(2) 0.054(3) 0.041(2) -0.012(2) 0.0102(18) -0.0143(19) C12 0.051(2) 0.050(3) 0.037(2) -0.020(2) 0.0076(19) -0.011(2) C13 0.043(2) 0.042(2) 0.037(2) -0.0176(19) 0.0039(18) -0.0101(18) C14 0.055(3) 0.057(3) 0.058(3) -0.030(2) 0.012(2) -0.025(2) C15 0.070(3) 0.079(4) 0.050(3) -0.017(3) 0.027(3) -0.032(3) C16 0.071(3) 0.054(3) 0.058(3) -0.033(2) 0.015(2) -0.028(2) C17 0.039(2) 0.053(3) 0.043(2) -0.019(2) -0.0015(18) -0.0083(19) C18 0.046(2) 0.043(2) 0.038(2) -0.0118(19) -0.0038(18) -0.0081(19) C19 0.042(2) 0.035(2) 0.029(2) -0.0139(17) -0.0001(16) -0.0076(16) C20 0.048(2) 0.041(2) 0.030(2) -0.0113(18) 0.0036(17) -0.0159(18) C21 0.055(2) 0.046(2) 0.030(2) -0.0126(19) 0.0061(18) -0.015(2) C22 0.054(2) 0.032(2) 0.035(2) -0.0125(18) -0.0065(19) -0.0054(18) C23 0.044(2) 0.031(2) 0.045(2) -0.0095(19) -0.0034(19) -0.0106(17) C24 0.042(2) 0.038(2) 0.032(2) -0.0085(18) 0.0020(17) -0.0128(17) C25 0.072(3) 0.056(3) 0.045(3) -0.019(2) 0.016(2) -0.033(2) C26 0.077(3) 0.047(3) 0.048(3) -0.022(2) -0.006(2) -0.009(2) C27 0.054(3) 0.049(3) 0.047(3) -0.013(2) 0.015(2) -0.024(2) N1 0.0324(16) 0.0371(18) 0.0274(17) -0.0120(14) 0.0061(13) -0.0105(13) N2 0.0360(16) 0.0301(16) 0.0269(16) -0.0103(13) 0.0044(13) -0.0090(13) N3 0.0389(17) 0.0328(17) 0.0259(16) -0.0094(14) 0.0014(13) -0.0070(13) N4 0.0407(18) 0.0354(18) 0.0271(17) -0.0120(14) 0.0020(14) -0.0110(14) I1 0.04128(15) 0.06419(19) 0.03712(16) -0.01969(14) 0.00192(11) -0.02093(13) I2 0.03697(14) 0.05171(18) 0.04390(17) -0.01943(13) 0.00552(11) -0.00463(12) Pd1 0.03172(15) 0.03305(16) 0.02795(16) -0.01041(12) 0.00302(11) -0.00926(12) _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 C2 1.358(5) . ? C1 N2 1.401(5) . ? C1 Pd1 1.990(4) . ? C2 N1 1.393(5) . ? C2 H2A 0.9300 . ? C3 N1 1.328(5) . ? C3 N2 1.344(5) . ? C3 C17 1.468(5) . ? C4 N3 1.448(5) . ? C4 N2 1.451(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N4 1.338(5) . ? C5 N3 1.347(5) . ? C5 C18 1.476(5) . ? C6 C7 1.358(5) . ? C6 N4 1.394(5) . ? C6 H6A 0.9300 . ? C7 N3 1.411(5) . ? C7 Pd1 1.994(4) . ? C8 C9 1.382(5) . ? C8 C13 1.388(6) . ? C8 N1 1.445(5) . ? C9 C10 1.396(6) . ? C9 C14 1.513(6) . ? C10 C11 1.390(6) . ? C10 H10A 0.9300 . ? C11 C12 1.375(6) . ? C11 C15 1.505(6) . ? C12 C13 1.392(6) . ? C12 H12A 0.9300 . ? C13 C16 1.501(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.381(5) . ? C19 C24 1.402(5) . ? C19 N4 1.440(5) . ? C20 C21 1.394(6) . ? C20 C25 1.510(6) . ? C21 C22 1.384(6) . ? C21 H21A 0.9300 . ? C22 C23 1.388(6) . ? C22 C26 1.500(6) . ? C23 C24 1.383(6) . ? C23 H23A 0.9300 . ? C24 C27 1.502(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? I1 Pd1 2.6522(5) . ? I2 Pd1 2.6998(5) . ? 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 C2 C1 N2 103.0(3) . . ? C2 C1 Pd1 132.0(3) . . ? N2 C1 Pd1 124.3(3) . . ? C1 C2 N1 109.5(3) . . ? C1 C2 H2A 125.3 . . ? N1 C2 H2A 125.3 . . ? N1 C3 N2 106.3(3) . . ? N1 C3 C17 127.0(3) . . ? N2 C3 C17 126.7(4) . . ? N3 C4 N2 107.8(3) . . ? N3 C4 H4A 110.2 . . ? N2 C4 H4A 110.2 . . ? N3 C4 H4B 110.2 . . ? N2 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? N4 C5 N3 106.1(3) . . ? N4 C5 C18 125.9(3) . . ? N3 C5 C18 128.0(4) . . ? C7 C6 N4 109.7(3) . . ? C7 C6 H6A 125.1 . . ? N4 C6 H6A 125.1 . . ? C6 C7 N3 103.0(3) . . ? C6 C7 Pd1 132.4(3) . . ? N3 C7 Pd1 124.3(3) . . ? C9 C8 C13 123.3(4) . . ? C9 C8 N1 118.0(3) . . ? C13 C8 N1 118.6(3) . . ? C8 C9 C10 117.3(4) . . ? C8 C9 C14 122.1(4) . . ? C10 C9 C14 120.6(4) . . ? C11 C10 C9 121.5(4) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C12 C11 C10 118.6(4) . . ? C12 C11 C15 121.2(4) . . ? C10 C11 C15 120.2(4) . . ? C11 C12 C13 122.4(4) . . ? C11 C12 H12A 118.8 . . ? C13 C12 H12A 118.8 . . ? C8 C13 C12 116.9(4) . . ? C8 C13 C16 121.5(4) . . ? C12 C13 C16 121.7(4) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C3 C17 H17A 109.5 . . ? C3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C5 C18 H18A 109.5 . . ? C5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 123.0(4) . . ? C20 C19 N4 118.5(3) . . ? C24 C19 N4 118.3(3) . . ? C19 C20 C21 117.3(4) . . ? C19 C20 C25 122.0(4) . . ? C21 C20 C25 120.7(4) . . ? C22 C21 C20 121.9(4) . . ? C22 C21 H21A 119.0 . . ? C20 C21 H21A 119.0 . . ? C21 C22 C23 118.5(4) . . ? C21 C22 C26 121.7(4) . . ? C23 C22 C26 119.8(4) . . ? C24 C23 C22 122.2(4) . . ? C24 C23 H23A 118.9 . . ? C22 C23 H23A 118.9 . . ? C23 C24 C19 117.0(4) . . ? C23 C24 C27 121.0(4) . . ? C19 C24 C27 122.0(4) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27C 109.5 . . ? C24 C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C3 N1 C2 109.0(3) . . ? C3 N1 C8 126.9(3) . . ? C2 N1 C8 123.8(3) . . ? C3 N2 C1 112.1(3) . . ? C3 N2 C4 125.4(3) . . ? C1 N2 C4 122.4(3) . . ? C5 N3 C7 112.1(3) . . ? C5 N3 C4 125.7(3) . . ? C7 N3 C4 122.1(3) . . ? C5 N4 C6 109.0(3) . . ? C5 N4 C19 127.1(3) . . ? C6 N4 C19 123.8(3) . . ? C1 Pd1 C7 86.68(15) . . ? C1 Pd1 I1 89.44(10) . . ? C7 Pd1 I1 174.95(10) . . ? C1 Pd1 I2 176.09(11) . . ? C7 Pd1 I2 91.11(11) . . ? I1 Pd1 I2 92.585(15) . . ? 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 N2 C1 C2 N1 0.2(4) . . . . ? Pd1 C1 C2 N1 170.9(3) . . . . ? N4 C6 C7 N3 0.2(4) . . . . ? N4 C6 C7 Pd1 -173.4(3) . . . . ? C13 C8 C9 C10 0.0(6) . . . . ? N1 C8 C9 C10 -176.6(3) . . . . ? C13 C8 C9 C14 -179.3(4) . . . . ? N1 C8 C9 C14 4.2(6) . . . . ? C8 C9 C10 C11 0.0(6) . . . . ? C14 C9 C10 C11 179.2(4) . . . . ? C9 C10 C11 C12 -0.4(6) . . . . ? C9 C10 C11 C15 179.1(4) . . . . ? C10 C11 C12 C13 1.0(7) . . . . ? C15 C11 C12 C13 -178.6(4) . . . . ? C9 C8 C13 C12 0.5(6) . . . . ? N1 C8 C13 C12 177.0(3) . . . . ? C9 C8 C13 C16 -178.7(4) . . . . ? N1 C8 C13 C16 -2.2(6) . . . . ? C11 C12 C13 C8 -1.0(6) . . . . ? C11 C12 C13 C16 178.2(4) . . . . ? C24 C19 C20 C21 2.4(6) . . . . ? N4 C19 C20 C21 -172.5(4) . . . . ? C24 C19 C20 C25 -176.6(4) . . . . ? N4 C19 C20 C25 8.4(6) . . . . ? C19 C20 C21 C22 -2.2(6) . . . . ? C25 C20 C21 C22 176.9(4) . . . . ? C20 C21 C22 C23 -0.4(6) . . . . ? C20 C21 C22 C26 177.2(4) . . . . ? C21 C22 C23 C24 3.0(6) . . . . ? C26 C22 C23 C24 -174.7(4) . . . . ? C22 C23 C24 C19 -2.8(6) . . . . ? C22 C23 C24 C27 176.0(4) . . . . ? C20 C19 C24 C23 0.0(6) . . . . ? N4 C19 C24 C23 174.9(3) . . . . ? C20 C19 C24 C27 -178.8(4) . . . . ? N4 C19 C24 C27 -3.9(6) . . . . ? N2 C3 N1 C2 -0.3(4) . . . . ? C17 C3 N1 C2 178.7(4) . . . . ? N2 C3 N1 C8 173.6(3) . . . . ? C17 C3 N1 C8 -7.4(6) . . . . ? C1 C2 N1 C3 0.1(4) . . . . ? C1 C2 N1 C8 -174.1(3) . . . . ? C9 C8 N1 C3 -83.0(5) . . . . ? C13 C8 N1 C3 100.3(5) . . . . ? C9 C8 N1 C2 90.1(4) . . . . ? C13 C8 N1 C2 -86.6(5) . . . . ? N1 C3 N2 C1 0.4(4) . . . . ? C17 C3 N2 C1 -178.6(4) . . . . ? N1 C3 N2 C4 179.0(3) . . . . ? C17 C3 N2 C4 0.0(6) . . . . ? C2 C1 N2 C3 -0.3(4) . . . . ? Pd1 C1 N2 C3 -172.1(3) . . . . ? C2 C1 N2 C4 -179.0(3) . . . . ? Pd1 C1 N2 C4 9.3(5) . . . . ? N3 C4 N2 C3 126.6(4) . . . . ? N3 C4 N2 C1 -54.9(4) . . . . ? N4 C5 N3 C7 -0.6(4) . . . . ? C18 C5 N3 C7 178.1(4) . . . . ? N4 C5 N3 C4 -179.1(3) . . . . ? C18 C5 N3 C4 -0.4(6) . . . . ? C6 C7 N3 C5 0.3(4) . . . . ? Pd1 C7 N3 C5 174.5(3) . . . . ? C6 C7 N3 C4 178.8(3) . . . . ? Pd1 C7 N3 C4 -6.9(5) . . . . ? N2 C4 N3 C5 -128.2(4) . . . . ? N2 C4 N3 C7 53.4(4) . . . . ? N3 C5 N4 C6 0.7(4) . . . . ? C18 C5 N4 C6 -178.1(4) . . . . ? N3 C5 N4 C19 -175.3(3) . . . . ? C18 C5 N4 C19 6.0(6) . . . . ? C7 C6 N4 C5 -0.5(4) . . . . ? C7 C6 N4 C19 175.6(3) . . . . ? C20 C19 N4 C5 -109.3(4) . . . . ? C24 C19 N4 C5 75.5(5) . . . . ? C20 C19 N4 C6 75.3(5) . . . . ? C24 C19 N4 C6 -99.9(4) . . . . ? C2 C1 Pd1 C7 -140.8(4) . . . . ? N2 C1 Pd1 C7 28.3(3) . . . . ? C2 C1 Pd1 I1 36.0(4) . . . . ? N2 C1 Pd1 I1 -154.9(3) . . . . ? C2 C1 Pd1 I2 -85.2(16) . . . . ? N2 C1 Pd1 I2 83.9(16) . . . . ? C6 C7 Pd1 C1 143.0(4) . . . . ? N3 C7 Pd1 C1 -29.4(3) . . . . ? C6 C7 Pd1 I1 103.3(12) . . . . ? N3 C7 Pd1 I1 -69.1(14) . . . . ? C6 C7 Pd1 I2 -33.8(4) . . . . ? N3 C7 Pd1 I2 153.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.777 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.082 ################################################ data_2d _database_code_depnum_ccdc_archive 'CCDC 695650' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28.25 H35 I2 N4 Pd' _chemical_formula_weight 790.80 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' 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' I I -0.4742 1.8119 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8204(15) _cell_length_b 15.0692(17) _cell_length_c 16.8311(19) _cell_angle_alpha 94.572(13) _cell_angle_beta 107.296(13) _cell_angle_gamma 104.040(13) _cell_volume 2971.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2137 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.75 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1538 _exptl_absorpt_coefficient_mu 2.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.437 _exptl_absorpt_correction_T_max 0.476 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23096 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.1389 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.15 _reflns_number_total 10901 _reflns_number_gt 4822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON03 (Spek, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Two butyl groups of the ligand in one of the two Pd-complex molecules are disordered. The involved carbon atoms are refined with occupancies of 0.5 and their thermal values to be equal. In the structure, a strongly disordered pentane molecule is co-crystallised. It was not possible to find a reasonable model defining the disorder. The SQUEEZE instruction in PLATON03 was used to calculate the potential solvent accessible area in the unit cell; 201/%A^3^ were calculated containing about 32 electrons. Therefore, one pentane molecule (1 x 42 electrons) per unit cell were included in all further calculations. 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^)+(0.0637P)^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 10901 _refine_ls_number_parameters 552 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 0.748 _refine_ls_restrained_S_all 0.749 _refine_ls_shift/su_max 0.001 _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 1.0071(9) 1.2039(6) 0.4330(6) 0.048(2) Uani 1 1 d . . . C2 C 1.0460(9) 1.2834(7) 0.4030(7) 0.053(3) Uani 1 1 d . . . H2A H 1.0085 1.2995 0.3516 0.063 Uiso 1 1 calc R . . C3 C 1.1791(11) 1.2925(10) 0.5246(10) 0.0972(17) Uani 1 1 d . . . C4 C 1.0905(9) 1.1465(6) 0.5660(6) 0.050(2) Uani 1 1 d . . . H4A H 1.0948 1.0874 0.5403 0.060 Uiso 1 1 calc R . . H4B H 1.1551 1.1693 0.6184 0.060 Uiso 1 1 calc R . . C7 C 0.8805(9) 1.1089(5) 0.5197(6) 0.047(2) Uani 1 1 d . . . C6 C 0.8053(9) 1.1091(6) 0.5626(6) 0.049(2) Uani 1 1 d . . . H6A H 0.7260 1.0955 0.5380 0.059 Uiso 1 1 calc R . . C5 C 0.9733(10) 1.1475(6) 0.6596(6) 0.049(3) Uani 1 1 d . . . C8 C 1.2129(16) 1.4256(11) 0.4487(13) 0.143(4) Uani 1 1 d D . . H8A H 1.1713 1.4713 0.4536 0.172 Uiso 0.50 1 calc PR A 1 H8B H 1.2859 1.4456 0.4947 0.172 Uiso 0.50 1 calc PR A 1 H8C H 1.2587 1.4593 0.5048 0.172 Uiso 0.50 1 d PR A 2 H8D H 1.1603 1.4602 0.4237 0.172 Uiso 0.50 1 d PR A 2 C9 C 1.235(3) 1.425(3) 0.3692(18) 0.143(4) Uani 0.50 1 d PD B 1 H9A H 1.2645 1.4888 0.3610 0.172 Uiso 0.50 1 calc PR B 1 H9B H 1.1639 1.3957 0.3225 0.172 Uiso 0.50 1 calc PR B 1 C9A C 1.297(3) 1.425(3) 0.402(2) 0.143(4) Uani 0.50 1 d PD B 2 H9A1 H 1.3292 1.4868 0.3909 0.172 Uiso 0.50 1 calc PR B 2 H9A2 H 1.3596 1.4011 0.4330 0.172 Uiso 0.50 1 calc PR B 2 C10 C 1.322(3) 1.370(2) 0.3716(17) 0.143(4) Uani 0.50 1 d PD B 1 H10A H 1.3994 1.4076 0.4047 0.172 Uiso 0.50 1 calc PR B 1 H10B H 1.3034 1.3128 0.3940 0.172 Uiso 0.50 1 calc PR B 1 C10A C 1.226(3) 1.361(2) 0.322(2) 0.143(4) Uani 0.50 1 d PD B 2 H10C H 1.1889 1.3012 0.3335 0.172 Uiso 0.50 1 calc PR B 2 H10D H 1.1683 1.3878 0.2888 0.172 Uiso 0.50 1 calc PR B 2 C11 C 1.3071(16) 1.3521(11) 0.2787(12) 0.143(4) Uani 1 1 d D . . H11C H 1.3578 1.3166 0.2703 0.215 Uiso 0.50 1 calc PR B 1 H11B H 1.3250 1.4106 0.2586 0.215 Uiso 0.50 1 calc PR B 1 H11A H 1.2290 1.3174 0.2477 0.215 Uiso 0.50 1 calc PR B 1 H11D H 1.3382 1.3033 0.2994 0.215 Uiso 0.50 1 d PR B 2 H11E H 1.3669 1.4091 0.2930 0.215 Uiso 0.50 1 d PR B 2 H11F H 1.2725 1.3370 0.2185 0.215 Uiso 0.50 1 d PR B 2 C12 C 1.2828(11) 1.3265(9) 0.5990(9) 0.0972(17) Uani 1 1 d . . . C13 C 1.3712(10) 1.2884(9) 0.6071(9) 0.0972(17) Uani 1 1 d . . . H13A H 1.3646 1.2390 0.5664 0.117 Uiso 1 1 calc R . . C14 C 1.4700(11) 1.3219(9) 0.6748(9) 0.0972(17) Uani 1 1 d . . . H14A H 1.5314 1.2968 0.6791 0.117 Uiso 1 1 calc R . . C15 C 1.4787(11) 1.3894(9) 0.7339(9) 0.0972(17) Uani 1 1 d . . . H15A H 1.5476 1.4140 0.7786 0.117 Uiso 1 1 calc R . . C16 C 1.3894(10) 1.4231(9) 0.7303(9) 0.0972(17) Uani 1 1 d . . . H16A H 1.3951 1.4676 0.7750 0.117 Uiso 1 1 calc R . . C17 C 1.2897(11) 1.3937(9) 0.6627(9) 0.0972(17) Uani 1 1 d . . . H17A H 1.2285 1.4187 0.6600 0.117 Uiso 1 1 calc R . . C18 C 1.0659(10) 1.1768(7) 0.7398(6) 0.058(3) Uani 1 1 d . . . C19 C 1.1317(11) 1.1184(8) 0.7687(8) 0.076(3) Uani 1 1 d . . . H19A H 1.1153 1.0597 0.7366 0.091 Uiso 1 1 calc R . . C20 C 1.2197(15) 1.1442(13) 0.8426(10) 0.112(5) Uani 1 1 d . . . H20A H 1.2603 1.1017 0.8623 0.135 Uiso 1 1 calc R . . C21 C 1.2491(17) 1.2271(16) 0.8871(11) 0.141(7) Uani 1 1 d . . . H21A H 1.3172 1.2474 0.9329 0.169 Uiso 1 1 calc R . . C22 C 1.1771(16) 1.2858(12) 0.8654(9) 0.121(6) Uani 1 1 d . . . H22A H 1.1902 1.3411 0.9015 0.145 Uiso 1 1 calc R . . C23 C 1.0867(12) 1.2603(8) 0.7897(7) 0.080(4) Uani 1 1 d . . . H23A H 1.0404 1.2997 0.7729 0.096 Uiso 1 1 calc R . . C24 C 0.8079(13) 1.1314(8) 0.7115(9) 0.102(3) Uani 1 1 d D . . H24A H 0.7372 1.1482 0.6872 0.123 Uiso 0.50 1 calc PR C 1 H24B H 0.8567 1.1806 0.7589 0.123 Uiso 0.50 1 calc PR C 1 H24C H 0.7658 1.1773 0.7056 0.123 Uiso 0.50 1 d PR C 2 H24D H 0.8644 1.1467 0.7674 0.123 Uiso 0.50 1 d PR C 2 C25A C 0.7263(18) 1.0331(13) 0.7009(18) 0.102(3) Uani 0.50 1 d PD D 2 H25A H 0.6755 1.0331 0.7344 0.123 Uiso 0.50 1 calc PR D 2 H25B H 0.6806 1.0095 0.6416 0.123 Uiso 0.50 1 calc PR D 2 C25 C 0.779(3) 1.0455(11) 0.7462(16) 0.102(3) Uani 0.50 1 d PD D 1 H25C H 0.8397 1.0556 0.8006 0.123 Uiso 0.50 1 calc PR D 1 H25D H 0.7104 1.0466 0.7598 0.123 Uiso 0.50 1 calc PR D 1 C26A C 0.8093(17) 0.9762(11) 0.7341(11) 0.102(3) Uani 0.50 1 d PD D 2 H26A H 0.8821 1.0189 0.7699 0.123 Uiso 0.50 1 calc PR D 2 H26B H 0.7796 0.9358 0.7699 0.123 Uiso 0.50 1 calc PR D 2 C26 C 0.7595(17) 0.9484(11) 0.7109(11) 0.102(3) Uani 0.50 1 d PRD D 1 H26C H 0.7595 0.9143 0.7574 0.123 Uiso 0.50 1 d PR D 1 H26D H 0.6834 0.9263 0.6701 0.123 Uiso 0.50 1 d PR D 1 C27 C 0.8310(12) 0.9183(8) 0.6693(9) 0.102(3) Uani 1 1 d D . . H27A H 0.7844 0.8822 0.6145 0.154 Uiso 0.50 1 calc PR D 1 H27B H 0.8717 0.8805 0.7032 0.154 Uiso 0.50 1 calc PR D 1 H27C H 0.8851 0.9721 0.6624 0.154 Uiso 0.50 1 calc PR D 1 H27D H 0.8148 0.9424 0.6173 0.154 Uiso 0.50 1 d PR D 2 H27E H 0.7854 0.8553 0.6601 0.154 Uiso 0.50 1 d PR D 2 H27F H 0.9101 0.9206 0.6896 0.154 Uiso 0.50 1 d PR D 2 C28 C 0.8478(8) 1.4173(6) 0.2801(5) 0.044(2) Uani 1 1 d . . . C29 C 0.8341(8) 1.3844(6) 0.3508(6) 0.043(2) Uani 1 1 d . . . H29A H 0.8885 1.4039 0.4050 0.052 Uiso 1 1 calc R . . C30 C 0.6763(8) 1.3102(6) 0.2517(6) 0.042(2) Uani 1 1 d . . . C31 C 0.7236(8) 1.3760(6) 0.1313(5) 0.046(2) Uani 1 1 d . . . H31A H 0.7218 1.4389 0.1215 0.055 Uiso 1 1 calc R . . H31B H 0.6503 1.3328 0.0972 0.055 Uiso 1 1 calc R . . C32 C 0.9283(9) 1.4021(6) 0.1492(6) 0.052(3) Uani 1 1 d . . . C33 C 0.9837(9) 1.3659(7) 0.1052(7) 0.063(3) Uani 1 1 d . . . H33A H 1.0632 1.3835 0.1179 0.075 Uiso 1 1 calc R . . C34 C 0.8064(10) 1.2924(6) 0.0414(6) 0.053(3) Uani 1 1 d . . . C35 C 0.6928(8) 1.2709(6) 0.3949(6) 0.049(2) Uani 1 1 d . . . H35A H 0.7585 1.2615 0.4377 0.058 Uiso 1 1 calc R . . H35B H 0.6418 1.2097 0.3664 0.058 Uiso 1 1 calc R . . C36 C 0.6324(10) 1.3201(7) 0.4375(7) 0.069(3) Uani 1 1 d . . . H36A H 0.5629 1.3243 0.3954 0.082 Uiso 1 1 calc R . . H36B H 0.6807 1.3834 0.4616 0.082 Uiso 1 1 calc R . . C37 C 0.6011(12) 1.2738(8) 0.5065(8) 0.092(5) Uani 1 1 d . . . H37A H 0.6702 1.2672 0.5474 0.111 Uiso 1 1 calc R . . H37B H 0.5697 1.3139 0.5360 0.111 Uiso 1 1 calc R . . C38 C 0.5186(13) 1.1828(9) 0.4760(10) 0.110(5) Uani 1 1 d . . . H38C H 0.4917 1.1617 0.5212 0.165 Uiso 1 1 calc R . . H38B H 0.5544 1.1392 0.4572 0.165 Uiso 1 1 calc R . . H38A H 0.4548 1.1869 0.4293 0.165 Uiso 1 1 calc R . . C39 C 0.5605(8) 1.2531(6) 0.2050(6) 0.047(2) Uani 1 1 d . . . C40 C 0.5298(9) 1.1571(7) 0.2009(6) 0.059(3) Uani 1 1 d . . . H40A H 0.5820 1.1268 0.2300 0.070 Uiso 1 1 calc R . . C41 C 0.4199(11) 1.1080(8) 0.1524(8) 0.073(3) Uani 1 1 d . . . H41A H 0.3987 1.0430 0.1467 0.088 Uiso 1 1 calc R . . C42 C 0.3414(11) 1.1504(11) 0.1125(8) 0.092(4) Uani 1 1 d . . . H42A H 0.2659 1.1153 0.0834 0.111 Uiso 1 1 calc R . . C43 C 0.3734(10) 1.2458(11) 0.1150(8) 0.091(4) Uani 1 1 d . . . H43A H 0.3211 1.2752 0.0846 0.109 Uiso 1 1 calc R . . C44 C 0.4808(9) 1.2962(8) 0.1617(7) 0.064(3) Uani 1 1 d . . . H44A H 0.5018 1.3610 0.1650 0.077 Uiso 1 1 calc R . . C45 C 0.6956(8) 1.2286(6) -0.0166(6) 0.049(2) Uani 1 1 d . . . C46 C 0.6259(9) 1.1680(7) 0.0147(6) 0.056(3) Uani 1 1 d . . . H46A H 0.6478 1.1647 0.0727 0.068 Uiso 1 1 calc R . . C47 C 0.5242(9) 1.1121(7) -0.0389(7) 0.063(3) Uani 1 1 d . . . H47A H 0.4730 1.0748 -0.0169 0.076 Uiso 1 1 calc R . . C48 C 0.4956(10) 1.1099(8) -0.1248(7) 0.072(3) Uani 1 1 d . . . H48A H 0.4283 1.0679 -0.1616 0.087 Uiso 1 1 calc R . . C49 C 0.5648(11) 1.1681(8) -0.1548(7) 0.076(4) Uani 1 1 d . . . H49A H 0.5447 1.1675 -0.2134 0.091 Uiso 1 1 calc R . . C50 C 0.6651(9) 1.2292(7) -0.1023(6) 0.060(3) Uani 1 1 d . . . H50A H 0.7120 1.2707 -0.1247 0.072 Uiso 1 1 calc R . . C51 C 0.9386(10) 1.2457(7) -0.0240(7) 0.065(3) Uani 1 1 d . . . H51A H 0.9664 1.2870 -0.0599 0.079 Uiso 1 1 calc R . . H51B H 0.8707 1.1976 -0.0601 0.079 Uiso 1 1 calc R . . C52 C 1.0275(11) 1.2018(9) 0.0179(9) 0.090(4) Uani 1 1 d . . . H52A H 1.0463 1.1690 -0.0262 0.108 Uiso 1 1 calc R . . H52B H 1.0960 1.2514 0.0505 0.108 Uiso 1 1 calc R . . C53 C 1.0016(13) 1.1362(9) 0.0747(9) 0.094(4) Uani 1 1 d . . . H53A H 1.0677 1.1130 0.0976 0.113 Uiso 1 1 calc R . . H53B H 0.9901 1.1699 0.1222 0.113 Uiso 1 1 calc R . . C54 C 0.9013(14) 1.0570(10) 0.0346(10) 0.117(6) Uani 1 1 d . . . H54A H 0.9163 1.0177 -0.0068 0.176 Uiso 1 1 calc R . . H54B H 0.8368 1.0791 0.0070 0.176 Uiso 1 1 calc R . . H54C H 0.8844 1.0216 0.0772 0.176 Uiso 1 1 calc R . . N1 N 1.1472(7) 1.3349(6) 0.4594(6) 0.063(2) Uani 1 1 d . B . N2 N 1.0954(6) 1.2130(5) 0.5089(5) 0.047(2) Uani 1 1 d . . . N3 N 0.9869(7) 1.1334(5) 0.5839(5) 0.0460(19) Uani 1 1 d . . . N4 N 0.8644(8) 1.1323(5) 0.6477(5) 0.057(2) Uani 1 1 d . D . N5 N 0.7325(6) 1.3203(4) 0.3330(4) 0.0384(18) Uani 1 1 d . . . N6 N 0.7440(6) 1.3701(5) 0.2192(4) 0.0399(18) Uani 1 1 d . . . N7 N 0.8145(7) 1.3528(5) 0.1078(5) 0.0456(19) Uani 1 1 d . . . N8 N 0.9081(8) 1.2990(5) 0.0383(5) 0.060(2) Uani 1 1 d . . . Pd1 Pd 0.86119(6) 1.10683(5) 0.39777(4) 0.04397(19) Uani 1 1 d . . . Pd2 Pd 0.97505(6) 1.49597(5) 0.25295(5) 0.0454(2) Uani 1 1 d . . . I1 I 0.83058(7) 1.12805(5) 0.23691(4) 0.0622(2) Uani 1 1 d . . . I2 I 0.66226(6) 0.97916(4) 0.36162(4) 0.0608(2) Uani 1 1 d . . . I3 I 1.03388(6) 1.61247(4) 0.39611(4) 0.0553(2) Uani 1 1 d . . . I4 I 1.14558(7) 1.59245(5) 0.20575(6) 0.0769(3) 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 0.053(6) 0.039(5) 0.059(7) 0.008(5) 0.019(6) 0.026(5) C2 0.049(7) 0.056(6) 0.056(7) 0.008(5) 0.010(6) 0.029(5) C3 0.062(3) 0.096(4) 0.109(5) -0.026(3) -0.002(3) 0.030(3) C4 0.054(7) 0.048(5) 0.037(5) -0.002(4) -0.004(5) 0.021(5) C7 0.056(7) 0.029(5) 0.047(6) 0.000(4) 0.007(6) 0.010(4) C6 0.049(6) 0.045(5) 0.047(6) 0.002(4) 0.011(6) 0.007(4) C5 0.068(8) 0.034(5) 0.043(6) 0.002(4) 0.006(6) 0.023(5) C8 0.135(10) 0.108(7) 0.179(13) 0.035(8) 0.053(9) 0.015(7) C9 0.135(10) 0.108(7) 0.179(13) 0.035(8) 0.053(9) 0.015(7) C9A 0.135(10) 0.108(7) 0.179(13) 0.035(8) 0.053(9) 0.015(7) C10 0.135(10) 0.108(7) 0.179(13) 0.035(8) 0.053(9) 0.015(7) C10A 0.135(10) 0.108(7) 0.179(13) 0.035(8) 0.053(9) 0.015(7) C11 0.135(10) 0.108(7) 0.179(13) 0.035(8) 0.053(9) 0.015(7) C12 0.062(3) 0.096(4) 0.109(5) -0.026(3) -0.002(3) 0.030(3) C13 0.062(3) 0.096(4) 0.109(5) -0.026(3) -0.002(3) 0.030(3) C14 0.062(3) 0.096(4) 0.109(5) -0.026(3) -0.002(3) 0.030(3) C15 0.062(3) 0.096(4) 0.109(5) -0.026(3) -0.002(3) 0.030(3) C16 0.062(3) 0.096(4) 0.109(5) -0.026(3) -0.002(3) 0.030(3) C17 0.062(3) 0.096(4) 0.109(5) -0.026(3) -0.002(3) 0.030(3) C18 0.078(8) 0.058(6) 0.029(5) 0.003(5) -0.001(6) 0.028(6) C19 0.074(9) 0.084(8) 0.058(8) -0.001(6) -0.010(7) 0.042(7) C20 0.114(13) 0.139(14) 0.087(12) 0.022(10) 0.002(11) 0.080(11) C21 0.139(17) 0.170(19) 0.072(11) 0.010(12) -0.039(12) 0.064(15) C22 0.135(15) 0.127(13) 0.054(9) -0.034(9) -0.001(10) 0.008(11) C23 0.109(11) 0.063(7) 0.055(7) -0.001(6) 0.011(8) 0.026(7) C24 0.132(8) 0.076(5) 0.104(7) 0.015(5) 0.061(6) 0.009(5) C25A 0.132(8) 0.076(5) 0.104(7) 0.015(5) 0.061(6) 0.009(5) C25 0.132(8) 0.076(5) 0.104(7) 0.015(5) 0.061(6) 0.009(5) C26A 0.132(8) 0.076(5) 0.104(7) 0.015(5) 0.061(6) 0.009(5) C26 0.132(8) 0.076(5) 0.104(7) 0.015(5) 0.061(6) 0.009(5) C27 0.132(8) 0.076(5) 0.104(7) 0.015(5) 0.061(6) 0.009(5) C28 0.048(6) 0.043(5) 0.029(5) -0.006(4) -0.010(5) 0.019(4) C29 0.044(6) 0.046(5) 0.033(5) -0.001(4) -0.001(5) 0.020(5) C30 0.041(6) 0.040(5) 0.046(6) -0.003(4) 0.017(5) 0.013(4) C31 0.047(6) 0.047(5) 0.035(5) 0.005(4) 0.002(5) 0.012(4) C32 0.065(7) 0.054(6) 0.045(6) 0.011(5) 0.026(6) 0.019(5) C33 0.044(6) 0.069(7) 0.066(7) -0.001(6) 0.017(6) 0.005(5) C34 0.076(8) 0.049(6) 0.040(6) 0.003(4) 0.021(6) 0.025(5) C35 0.053(6) 0.044(5) 0.039(5) 0.003(4) 0.005(5) 0.010(5) C36 0.088(9) 0.053(6) 0.082(8) 0.012(5) 0.057(8) 0.016(6) C37 0.110(11) 0.074(8) 0.105(10) -0.009(7) 0.078(10) 0.003(8) C38 0.111(12) 0.100(11) 0.157(15) 0.026(10) 0.092(12) 0.037(9) C39 0.040(6) 0.051(6) 0.051(6) 0.008(5) 0.020(5) 0.007(5) C40 0.048(7) 0.067(7) 0.052(7) 0.000(5) 0.014(6) 0.007(5) C41 0.061(8) 0.078(8) 0.066(8) 0.005(6) 0.026(8) -0.012(7) C42 0.051(8) 0.117(12) 0.075(10) -0.004(8) 0.005(8) -0.012(8) C43 0.047(8) 0.120(12) 0.086(10) 0.020(8) -0.003(8) 0.016(8) C44 0.050(7) 0.068(7) 0.059(7) -0.001(6) 0.004(6) 0.012(6) C45 0.054(6) 0.048(5) 0.035(5) -0.005(4) 0.005(5) 0.012(5) C46 0.075(8) 0.061(6) 0.035(6) 0.012(5) 0.018(6) 0.022(6) C47 0.059(7) 0.068(7) 0.050(7) 0.004(5) 0.011(6) 0.004(6) C48 0.074(8) 0.065(7) 0.051(7) -0.012(6) 0.006(7) -0.002(6) C49 0.086(9) 0.087(8) 0.034(6) 0.000(6) 0.010(7) 0.002(7) C50 0.068(8) 0.061(6) 0.047(7) 0.016(5) 0.016(6) 0.011(6) C51 0.076(8) 0.073(7) 0.055(7) -0.010(5) 0.032(7) 0.029(6) C52 0.088(10) 0.075(8) 0.103(11) -0.020(8) 0.038(9) 0.021(7) C53 0.125(13) 0.067(8) 0.112(11) 0.007(8) 0.071(11) 0.026(8) C54 0.133(14) 0.109(12) 0.145(15) 0.008(10) 0.091(13) 0.046(11) N1 0.045(6) 0.054(5) 0.087(7) 0.011(5) 0.016(6) 0.015(4) N2 0.042(5) 0.035(4) 0.054(5) -0.004(4) 0.005(5) 0.010(4) N3 0.051(5) 0.038(4) 0.044(5) 0.002(3) 0.011(5) 0.010(4) N4 0.077(7) 0.051(5) 0.045(5) 0.006(4) 0.026(5) 0.017(5) N5 0.040(5) 0.041(4) 0.035(5) 0.001(3) 0.016(4) 0.009(4) N6 0.046(5) 0.042(4) 0.032(4) 0.004(3) 0.013(4) 0.014(4) N7 0.050(5) 0.045(4) 0.042(5) 0.003(3) 0.016(4) 0.012(4) N8 0.055(6) 0.063(5) 0.060(6) -0.012(4) 0.025(5) 0.013(4) Pd1 0.0509(5) 0.0396(4) 0.0356(4) 0.0011(3) 0.0057(4) 0.0143(3) Pd2 0.0452(5) 0.0395(4) 0.0449(4) 0.0011(3) 0.0102(4) 0.0074(3) I1 0.0749(5) 0.0720(5) 0.0418(4) 0.0093(3) 0.0146(4) 0.0300(4) I2 0.0623(5) 0.0507(4) 0.0485(4) -0.0023(3) 0.0011(4) 0.0029(3) I3 0.0608(4) 0.0440(3) 0.0467(4) -0.0041(3) 0.0025(4) 0.0112(3) I4 0.0774(6) 0.0534(4) 0.1032(7) 0.0098(4) 0.0465(5) 0.0044(4) _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 C2 1.376(13) . ? C1 N2 1.403(12) . ? C1 Pd1 1.966(10) . ? C2 N1 1.359(13) . ? C2 H2A 0.9400 . ? C3 N1 1.323(17) . ? C3 N2 1.348(15) . ? C3 C12 1.475(18) . ? C4 N3 1.419(12) . ? C4 N2 1.446(12) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C7 C6 1.366(12) . ? C7 N3 1.407(12) . ? C7 Pd1 1.990(9) . ? C6 N4 1.376(12) . ? C6 H6A 0.9400 . ? C5 N4 1.309(12) . ? C5 N3 1.343(11) . ? C5 C18 1.458(14) . ? C8 C9 1.445(18) . ? C8 N1 1.477(17) . ? C8 C9A 1.522(18) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? C9 C10 1.537(19) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9A C10A 1.474(19) . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C10 C11 1.511(18) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10A C11 1.460(18) . ? C10A H10C 0.9800 . ? C10A H10D 0.9800 . ? C11 H11C 0.9700 . ? C11 H11B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11D 0.9600 . ? C11 H11E 0.9600 . ? C11 H11F 0.9600 . ? C12 C13 1.368(16) . ? C12 C17 1.382(16) . ? C13 C14 1.377(16) . ? C13 H13A 0.9400 . ? C14 C15 1.324(16) . ? C14 H14A 0.9400 . ? C15 C16 1.348(16) . ? C15 H15A 0.9400 . ? C16 C17 1.380(17) . ? C16 H16A 0.9400 . ? C17 H17A 0.9400 . ? C18 C23 1.378(13) . ? C18 C19 1.380(14) . ? C19 C20 1.359(18) . ? C19 H19A 0.9400 . ? C20 C21 1.31(2) . ? C20 H20A 0.9400 . ? C21 C22 1.42(2) . ? C21 H21A 0.9400 . ? C22 C23 1.393(19) . ? C22 H22A 0.9400 . ? C23 H23A 0.9400 . ? C24 N4 1.462(14) . ? C24 C25 1.472(16) . ? C24 C25A 1.554(17) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9700 . ? C24 H24D 0.9700 . ? C25A C26A 1.531(18) . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H26D 1.5587 . ? C25 C26 1.466(16) . ? C25 H24D 1.5875 . ? C25 H25C 0.9800 . ? C25 H25D 0.9800 . ? C26A C27 1.474(12) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 1.1615 . ? C26 C27 1.437(12) . ? C26 H26C 0.9700 . ? C26 H26D 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C27 H27D 0.9600 . ? C27 H27E 0.9600 . ? C27 H27F 0.9600 . ? C28 C29 1.368(12) . ? C28 N6 1.393(11) . ? C28 Pd2 1.966(10) . ? C29 N5 1.353(11) . ? C29 H29A 0.9400 . ? C30 N5 1.320(11) . ? C30 N6 1.360(11) . ? C30 C39 1.463(13) . ? C31 N6 1.438(11) . ? C31 N7 1.443(11) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C33 1.337(13) . ? C32 N7 1.398(12) . ? C32 Pd2 1.995(9) . ? C33 N8 1.386(12) . ? C33 H33A 0.9400 . ? C34 N8 1.300(12) . ? C34 N7 1.346(11) . ? C34 C45 1.504(14) . ? C35 N5 1.468(11) . ? C35 C36 1.478(12) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 C37 1.505(15) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.458(16) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 H38C 0.9700 . ? C38 H38B 0.9700 . ? C38 H38A 0.9700 . ? C39 C40 1.395(13) . ? C39 C44 1.397(14) . ? C40 C41 1.383(15) . ? C40 H40A 0.9400 . ? C41 C42 1.361(18) . ? C41 H41A 0.9400 . ? C42 C43 1.389(18) . ? C42 H42A 0.9400 . ? C43 C44 1.358(15) . ? C43 H43A 0.9400 . ? C44 H44A 0.9400 . ? C45 C46 1.368(13) . ? C45 C50 1.380(13) . ? C46 C47 1.368(14) . ? C46 H46A 0.9400 . ? C47 C48 1.376(14) . ? C47 H47A 0.9400 . ? C48 C49 1.332(14) . ? C48 H48A 0.9400 . ? C49 C50 1.380(14) . ? C49 H49A 0.9400 . ? C50 H50A 0.9400 . ? C51 N8 1.469(11) . ? C51 C52 1.482(16) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C52 C53 1.477(17) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.465(18) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C54 H54C 0.9700 . ? Pd1 I2 2.6619(11) . ? Pd1 I1 2.6747(10) . ? Pd2 I3 2.6569(10) . ? Pd2 I4 2.6832(11) . ? 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 C2 C1 N2 101.9(8) . . ? C2 C1 Pd1 133.4(8) . . ? N2 C1 Pd1 124.1(7) . . ? N1 C2 C1 109.4(10) . . ? N1 C2 H2A 125.3 . . ? C1 C2 H2A 125.3 . . ? N1 C3 N2 105.1(11) . . ? N1 C3 C12 127.2(14) . . ? N2 C3 C12 127.7(15) . . ? N3 C4 N2 109.0(8) . . ? N3 C4 H4A 109.9 . . ? N2 C4 H4A 109.9 . . ? N3 C4 H4B 109.9 . . ? N2 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C6 C7 N3 103.6(8) . . ? C6 C7 Pd1 131.0(8) . . ? N3 C7 Pd1 123.8(7) . . ? C5 C6 N4 109.1(9) . . ? C5 C6 H6A 125.5 . . ? N4 C6 H6A 125.5 . . ? N4 C5 N3 108.1(9) . . ? N4 C5 C18 127.1(9) . . ? N3 C5 C18 124.8(10) . . ? C9 C8 N1 114(2) . . ? C9 C8 C9A 32.3(18) . . ? N1 C8 C9A 117.0(19) . . ? C9 C8 H8A 108.7 . . ? N1 C8 H8A 108.7 . . ? C9A C8 H8A 129.2 . . ? C9 C8 H8B 108.7 . . ? N1 C8 H8B 108.7 . . ? C9A C8 H8B 78.0 . . ? H8A C8 H8B 107.6 . . ? C9 C8 H8C 131.3 . . ? N1 C8 H8C 107.0 . . ? C9A C8 H8C 105.1 . . ? H8A C8 H8C 80.2 . . ? H8B C8 H8C 30.2 . . ? C9 C8 H8D 83.5 . . ? N1 C8 H8D 108.7 . . ? C9A C8 H8D 111.2 . . ? H8A C8 H8D 28.7 . . ? H8B C8 H8D 130.7 . . ? H8C C8 H8D 107.3 . . ? C8 C9 C10 108(2) . . ? C8 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? C8 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C10A C9A C8 103(2) . . ? C10A C9A H9A1 111.2 . . ? C8 C9A H9A1 111.2 . . ? C10A C9A H9A2 111.2 . . ? C8 C9A H9A2 111.2 . . ? H9A1 C9A H9A2 109.2 . . ? C11 C10 C9 100(2) . . ? C11 C10 H10A 111.7 . . ? C9 C10 H10A 111.7 . . ? C11 C10 H10B 111.7 . . ? C9 C10 H10B 111.7 . . ? H10A C10 H10B 109.5 . . ? C11 C10A C9A 104(2) . . ? C11 C10A H10C 110.9 . . ? C9A C10A H10C 110.9 . . ? C11 C10A H10D 110.9 . . ? C9A C10A H10D 110.9 . . ? H10C C10A H10D 109.0 . . ? C10A C11 C10 48.7(17) . . ? C10A C11 H11C 145.0 . . ? C10 C11 H11C 109.5 . . ? C10A C11 H11B 104.4 . . ? C10 C11 H11B 109.5 . . ? H11C C11 H11B 109.5 . . ? C10A C11 H11A 66.0 . . ? C10 C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? C10A C11 H11D 106.5 . . ? C10 C11 H11D 77.9 . . ? H11C C11 H11D 38.6 . . ? H11B C11 H11D 143.4 . . ? H11A C11 H11D 100.8 . . ? C10A C11 H11E 108.8 . . ? C10 C11 H11E 82.6 . . ? H11C C11 H11E 91.6 . . ? H11B C11 H11E 40.6 . . ? H11A C11 H11E 149.3 . . ? H11D C11 H11E 109.5 . . ? C10A C11 H11F 113.0 . . ? C10 C11 H11F 161.5 . . ? H11C C11 H11F 84.7 . . ? H11B C11 H11F 75.1 . . ? H11A C11 H11F 53.2 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? C13 C12 C17 119.4(13) . . ? C13 C12 C3 119.8(12) . . ? C17 C12 C3 120.7(11) . . ? C12 C13 C14 120.3(12) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C15 C14 C13 120.2(12) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 120.3(13) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C15 C16 C17 121.6(12) . . ? C15 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C16 C17 C12 117.8(12) . . ? C16 C17 H17A 121.1 . . ? C12 C17 H17A 121.1 . . ? C23 C18 C19 118.8(10) . . ? C23 C18 C7 121.4(10) . . ? C19 C18 C7 119.8(9) . . ? C20 C19 C18 121.2(12) . . ? C20 C19 H19A 119.4 . . ? C18 C19 H19A 119.4 . . ? C21 C20 C19 121.4(15) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C22 119.4(16) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 119.1(14) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C18 C23 C22 119.3(13) . . ? C18 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? N4 C24 C25 118.7(14) . . ? N4 C24 C25A 109.1(14) . . ? C25 C24 C25A 31.6(14) . . ? N4 C24 H24A 107.6 . . ? C25 C24 H24A 107.6 . . ? C25A C24 H24A 83.8 . . ? N4 C24 H24B 107.6 . . ? C25 C24 H24B 107.6 . . ? C25A C24 H24B 136.1 . . ? H24A C24 H24B 107.1 . . ? N4 C24 H24C 110.0 . . ? C25 C24 H24C 125.2 . . ? C25A C24 H24C 110.3 . . ? H24A C24 H24C 30.0 . . ? H24B C24 H24C 78.1 . . ? N4 C24 H24D 109.7 . . ? C25 C24 H24D 78.1 . . ? C25A C24 H24D 109.5 . . ? H24A C24 H24D 132.8 . . ? H24B C24 H24D 33.7 . . ? H24C C24 H24D 108.3 . . ? C26A C25A C24 102.3(14) . . ? C26A C25A H25A 111.3 . . ? C24 C25A H25A 111.3 . . ? C26A C25A H25B 111.3 . . ? C24 C25A H25B 111.3 . . ? H25A C25A H25B 109.2 . . ? C26A C25A H26D 62.6 . . ? C24 C25A H26D 153.7 . . ? H25A C25A H26D 94.7 . . ? H25B C25A H26D 61.0 . . ? C26 C25 C24 131.1(19) . . ? C26 C25 H24D 145.0 . . ? C24 C25 H24D 36.7 . . ? C26 C25 H25C 104.5 . . ? C24 C25 H25C 104.5 . . ? H24D C25 H25C 68.0 . . ? C26 C25 H25D 104.5 . . ? C24 C25 H25D 104.5 . . ? H24D C25 H25D 110.4 . . ? H25C C25 H25D 105.6 . . ? C27 C26A C25A 115.7(18) . . ? C27 C26A H26A 108.4 . . ? C25A C26A H26A 108.4 . . ? C27 C26A H26B 108.4 . . ? C25A C26A H26B 108.4 . . ? H26A C26A H26B 107.4 . . ? C27 C26A H26C 95.2 . . ? C25A C26A H26C 106.3 . . ? H26A C26A H26C 122.9 . . ? H26B C26A H26C 16.9 . . ? C27 C26 C25 123.0(19) . . ? C27 C26 H26C 107.3 . . ? C25 C26 H26C 105.5 . . ? C27 C26 H26D 104.8 . . ? C25 C26 H26D 108.7 . . ? H26C C26 H26D 106.6 . . ? C26 C27 C26A 26.1(2) . . ? C26 C27 H27A 109.5 . . ? C26A C27 H27A 134.3 . . ? C26 C27 H27B 109.5 . . ? C26A C27 H27B 101.4 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? C26A C27 H27C 90.1 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C27 H27D 104.2 . . ? C26A C27 H27D 110.2 . . ? H27A C27 H27D 54.8 . . ? H27B C27 H27D 146.2 . . ? H27C C27 H27D 60.0 . . ? C26 C27 H27E 90.5 . . ? C26A C27 H27E 111.0 . . ? H27A C27 H27E 55.2 . . ? H27B C27 H27E 68.2 . . ? H27C C27 H27E 158.9 . . ? H27D C27 H27E 109.5 . . ? C26 C27 H27F 131.3 . . ? C26A C27 H27F 107.2 . . ? H27A C27 H27F 118.5 . . ? H27B C27 H27F 47.4 . . ? H27C C27 H27F 62.6 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? C29 C28 N6 101.5(8) . . ? C29 C28 Pd2 135.0(7) . . ? N6 C28 Pd2 123.1(6) . . ? N5 C29 C28 111.4(8) . . ? N5 C29 H29A 124.3 . . ? C28 C29 H29A 124.3 . . ? N5 C30 N6 106.3(7) . . ? N5 C30 C39 128.2(8) . . ? N6 C30 C39 125.3(9) . . ? N6 C31 N7 108.1(7) . . ? N6 C31 H31A 110.1 . . ? N7 C31 H31A 110.1 . . ? N6 C31 H31B 110.1 . . ? N7 C31 H31B 110.1 . . ? H31A C31 H31B 108.4 . . ? C33 C32 N7 103.3(8) . . ? C33 C32 Pd2 134.8(8) . . ? N7 C32 Pd2 121.8(6) . . ? C32 C33 N8 110.7(9) . . ? C32 C33 H33A 124.6 . . ? N8 C33 H33A 124.6 . . ? N8 C34 N7 108.7(9) . . ? N8 C34 C45 127.8(8) . . ? N7 C34 C45 123.5(9) . . ? N5 C35 C36 113.7(8) . . ? N5 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? N5 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C35 C36 C37 113.6(9) . . ? C35 C36 H36A 108.8 . . ? C37 C36 H36A 108.8 . . ? C35 C36 H36B 108.8 . . ? C37 C36 H36B 108.8 . . ? H36A C36 H36B 107.7 . . ? C38 C37 C36 113.5(11) . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37B 108.9 . . ? C36 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C37 C38 H38C 109.5 . . ? C37 C38 H38B 109.5 . . ? H38C C38 H38B 109.5 . . ? C37 C38 H38A 109.5 . . ? H38C C38 H38A 109.5 . . ? H38B C38 H38A 109.5 . . ? C40 C39 C44 119.9(9) . . ? C40 C39 C30 121.3(9) . . ? C44 C39 C30 118.7(9) . . ? C41 C40 C39 117.5(11) . . ? C41 C40 H40A 121.2 . . ? C39 C40 H40A 121.2 . . ? C42 C41 C40 122.5(12) . . ? C42 C41 H41A 118.8 . . ? C40 C41 H41A 118.8 . . ? C41 C42 C43 119.6(12) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C44 C43 C42 119.5(13) . . ? C44 C43 H43A 120.2 . . ? C42 C43 H43A 120.2 . . ? C43 C44 C39 120.9(11) . . ? C43 C44 H44A 119.6 . . ? C39 C44 H44A 119.6 . . ? C46 C45 C50 119.6(9) . . ? C46 C45 C34 120.5(9) . . ? C50 C45 C34 119.9(9) . . ? C47 C46 C45 119.4(9) . . ? C47 C46 H46A 120.3 . . ? C45 C46 H46A 120.3 . . ? C46 C47 C48 121.0(10) . . ? C46 C47 H47A 119.5 . . ? C48 C47 H47A 119.5 . . ? C49 C48 C47 118.9(10) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C48 C49 C50 121.8(10) . . ? C48 C49 H49A 119.1 . . ? C50 C49 H49A 119.1 . . ? C49 C50 C45 119.0(10) . . ? C49 C50 H50A 120.5 . . ? C45 C50 H50A 120.5 . . ? N8 C51 C52 111.1(9) . . ? N8 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? N8 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C53 C52 C51 117.8(11) . . ? C53 C52 H52A 107.8 . . ? C51 C52 H52A 107.8 . . ? C53 C52 H52B 107.8 . . ? C51 C52 H52B 107.8 . . ? H52A C52 H52B 107.2 . . ? C54 C53 C52 114.4(14) . . ? C54 C53 H53A 108.7 . . ? C52 C53 H53A 108.7 . . ? C54 C53 H53B 108.7 . . ? C52 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C3 N1 C2 110.9(10) . . ? C3 N1 C8 124.7(13) . . ? C2 N1 C8 124.4(12) . . ? C3 N2 C1 112.7(10) . . ? C3 N2 C4 124.7(11) . . ? C1 N2 C4 122.5(7) . . ? C5 N3 C7 110.0(8) . . ? C5 N3 C4 127.7(9) . . ? C7 N3 C4 122.2(8) . . ? C5 N4 C6 109.2(8) . . ? C5 N4 C24 127.9(10) . . ? C6 N4 C24 122.7(10) . . ? C30 N5 C29 108.9(7) . . ? C30 N5 C35 126.3(7) . . ? C29 N5 C35 124.8(8) . . ? C30 N6 C28 111.8(7) . . ? C30 N6 C31 126.1(7) . . ? C28 N6 C31 121.4(7) . . ? C34 N7 C32 109.9(8) . . ? C34 N7 C31 128.2(8) . . ? C32 N7 C31 121.4(7) . . ? C34 N8 C33 107.3(8) . . ? C34 N8 C51 126.9(9) . . ? C33 N8 C51 125.8(9) . . ? C1 Pd1 C7 87.1(4) . . ? C1 Pd1 I2 175.6(3) . . ? C7 Pd1 I2 88.8(3) . . ? C1 Pd1 I1 90.0(3) . . ? C7 Pd1 I1 171.8(2) . . ? I2 Pd1 I1 93.83(4) . . ? C28 Pd2 C32 86.4(4) . . ? C28 Pd2 I3 90.8(2) . . ? C32 Pd2 I3 176.5(3) . . ? C28 Pd2 I4 175.4(2) . . ? C32 Pd2 I4 89.1(3) . . ? I3 Pd2 I4 93.75(3) . . ? 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 N2 C1 C2 N1 -1.9(9) . . . . ? Pd1 C1 C2 N1 169.2(7) . . . . ? N3 C7 C6 N4 -0.1(9) . . . . ? Pd1 C5 C6 N4 -166.2(6) . . . . ? N1 C8 C9 C10 -71(3) . . . . ? C9A C8 C9 C10 32(3) . . . . ? C9 C8 C9A C10A -39(3) . . . . ? N1 C8 C9A C10A 53(4) . . . . ? C8 C9 C10 C11 164(2) . . . . ? C8 C9A C10A C11 -175(2) . . . . ? C9A C10A C11 C10 29(3) . . . . ? C9 C10 C11 C10A -32(2) . . . . ? N1 C3 C12 C13 -105.8(17) . . . . ? N2 C3 C12 C13 76(2) . . . . ? N1 C3 C12 C17 77(2) . . . . ? N2 C3 C12 C17 -101.3(17) . . . . ? C17 C12 C13 C14 -5(2) . . . . ? C3 C12 C13 C14 177.6(15) . . . . ? C12 C13 C14 C15 2(2) . . . . ? C13 C14 C15 C16 3(2) . . . . ? C14 C15 C16 C17 -5(2) . . . . ? C15 C16 C17 C12 2(2) . . . . ? C13 C12 C17 C16 3(2) . . . . ? C3 C12 C17 C16 -179.5(15) . . . . ? N4 C5 C18 C23 -61.9(15) . . . . ? N3 C5 C18 C23 116.7(12) . . . . ? N4 C5 C18 C19 115.3(12) . . . . ? N3 C5 C18 C19 -66.2(14) . . . . ? C23 C18 C19 C20 -3.7(19) . . . . ? C5 C18 C19 C20 179.1(13) . . . . ? C18 C19 C20 C21 -4(3) . . . . ? C19 C20 C21 C22 10(3) . . . . ? C20 C21 C22 C23 -10(3) . . . . ? C19 C18 C23 C22 3.6(18) . . . . ? C5 C18 C23 C22 -179.2(12) . . . . ? C21 C22 C23 C18 3(2) . . . . ? N4 C24 C25A C26A 72.9(19) . . . . ? C25 C24 C25A C26A -41(2) . . . . ? N4 C24 C25 C26 -24(4) . . . . ? C25A C24 C25 C26 55(3) . . . . ? C24 C25A C26A C27 -101.4(19) . . . . ? C24 C25 C26 C27 45(5) . . . . ? C25 C26 C27 C26A 37(2) . . . . ? C25A C26A C27 C26 -57.9(14) . . . . ? N6 C28 C29 N5 2.2(9) . . . . ? Pd2 C28 C29 N5 -170.4(6) . . . . ? N7 C32 C33 N8 1.5(12) . . . . ? Pd2 C32 C33 N8 177.7(8) . . . . ? N5 C35 C36 C37 -174.7(9) . . . . ? C35 C36 C37 C38 -65.2(15) . . . . ? N5 C30 C39 C40 -61.2(13) . . . . ? N6 C30 C39 C40 124.7(10) . . . . ? N5 C30 C39 C44 120.9(11) . . . . ? N6 C30 C39 C44 -53.2(12) . . . . ? C44 C39 C40 C41 0.6(14) . . . . ? C30 C39 C40 C41 -177.2(9) . . . . ? C39 C40 C41 C42 -2.9(16) . . . . ? C40 C41 C42 C43 4.7(19) . . . . ? C41 C42 C43 C44 -4(2) . . . . ? C42 C43 C44 C39 2.1(18) . . . . ? C40 C39 C44 C43 -0.4(15) . . . . ? C30 C39 C44 C43 177.6(10) . . . . ? N8 C34 C45 C46 122.2(12) . . . . ? N7 C34 C45 C46 -56.8(14) . . . . ? N8 C34 C45 C50 -56.0(15) . . . . ? N7 C34 C45 C50 125.0(11) . . . . ? C50 C45 C46 C47 -3.4(15) . . . . ? C34 C45 C46 C47 178.4(9) . . . . ? C45 C46 C47 C48 6.1(16) . . . . ? C46 C47 C48 C49 -5.0(18) . . . . ? C47 C48 C49 C50 1.2(19) . . . . ? C48 C49 C50 C45 1.4(18) . . . . ? C46 C45 C50 C49 -0.3(16) . . . . ? C34 C45 C50 C49 177.9(10) . . . . ? N8 C51 C52 C53 59.5(14) . . . . ? C51 C52 C53 C54 58.3(15) . . . . ? N2 C3 N1 C2 -0.6(12) . . . . ? C12 C3 N1 C2 -179.2(11) . . . . ? N2 C3 N1 C8 179.9(11) . . . . ? C12 C3 N1 C8 1(2) . . . . ? C1 C2 N1 C3 1.6(12) . . . . ? C1 C2 N1 C8 -178.9(11) . . . . ? C9 C8 N1 C3 127(2) . . . . ? C9A C8 N1 C3 91(2) . . . . ? C9 C8 N1 C2 -53(2) . . . . ? C9A C8 N1 C2 -89(2) . . . . ? N1 C3 N2 C1 -0.7(12) . . . . ? C12 C3 N2 C1 178.0(11) . . . . ? N1 C3 N2 C4 -176.2(8) . . . . ? C12 C3 N2 C4 2.5(18) . . . . ? C2 C1 N2 C3 1.6(10) . . . . ? Pd1 C1 N2 C3 -170.6(7) . . . . ? C2 C1 N2 C4 177.2(8) . . . . ? Pd1 C1 N2 C4 5.0(11) . . . . ? N3 C4 N2 C3 123.0(10) . . . . ? N3 C4 N2 C1 -52.1(10) . . . . ? N4 C5 N3 C7 0.9(10) . . . . ? C18 C5 N3 C7 -177.9(8) . . . . ? N4 C5 N3 C4 176.4(8) . . . . ? C18 C5 N3 C4 -2.3(14) . . . . ? C6 C7 N3 C5 -0.4(9) . . . . ? Pd1 C7 N3 C5 166.9(6) . . . . ? C6 C7 N3 C4 -176.3(8) . . . . ? Pd1 C7 N3 C4 -9.0(11) . . . . ? N2 C4 N3 C5 -121.3(9) . . . . ? N2 C4 N3 C7 53.8(10) . . . . ? N3 C5 N4 C6 -0.9(10) . . . . ? C18 C5 N4 C6 177.8(9) . . . . ? N3 C5 N4 C24 174.4(9) . . . . ? C18 C5 N4 C24 -6.9(15) . . . . ? C7 C6 N4 C5 0.7(10) . . . . ? C7 C6 N4 C24 -175.0(9) . . . . ? C25 C24 N4 C5 -85(2) . . . . ? C25A C24 N4 C5 -117.7(14) . . . . ? C25 C24 N4 C6 90(2) . . . . ? C25A C24 N4 C6 57.1(16) . . . . ? N6 C30 N5 C29 -0.8(9) . . . . ? C39 C30 N5 C29 -175.8(8) . . . . ? N6 C30 N5 C35 179.1(7) . . . . ? C39 C30 N5 C35 4.1(14) . . . . ? C28 C29 N5 C30 -1.0(10) . . . . ? C28 C29 N5 C35 179.1(8) . . . . ? C36 C35 N5 C30 -91.7(10) . . . . ? C36 C35 N5 C29 88.2(11) . . . . ? N5 C30 N6 C28 2.2(9) . . . . ? C39 C30 N6 C28 177.4(8) . . . . ? N5 C30 N6 C31 172.6(7) . . . . ? C39 C30 N6 C31 -12.1(13) . . . . ? C29 C28 N6 C30 -2.7(9) . . . . ? Pd2 C28 N6 C30 171.1(6) . . . . ? C29 C28 N6 C31 -173.6(7) . . . . ? Pd2 C28 N6 C31 0.1(11) . . . . ? N7 C31 N6 C30 -116.7(9) . . . . ? N7 C31 N6 C28 52.9(10) . . . . ? N8 C34 N7 C32 0.9(11) . . . . ? C45 C34 N7 C32 -180.0(9) . . . . ? N8 C34 N7 C31 173.5(9) . . . . ? C45 C34 N7 C31 -7.4(15) . . . . ? C33 C32 N7 C34 -1.5(11) . . . . ? Pd2 C32 N7 C34 -178.3(7) . . . . ? C33 C32 N7 C31 -174.7(9) . . . . ? Pd2 C32 N7 C31 8.5(12) . . . . ? N6 C31 N7 C34 130.7(9) . . . . ? N6 C31 N7 C32 -57.5(10) . . . . ? N7 C34 N8 C33 0.0(12) . . . . ? C45 C34 N8 C33 -179.0(10) . . . . ? N7 C34 N8 C51 179.9(9) . . . . ? C45 C34 N8 C51 0.8(18) . . . . ? C32 C33 N8 C34 -1.0(13) . . . . ? C32 C33 N8 C51 179.1(10) . . . . ? C52 C51 N8 C34 -128.0(12) . . . . ? C52 C51 N8 C33 51.8(15) . . . . ? C2 C1 Pd1 C7 -139.5(9) . . . . ? N2 C1 Pd1 C7 30.0(7) . . . . ? C2 C1 Pd1 I2 -118(3) . . . . ? N2 C1 Pd1 I2 52(4) . . . . ? C2 C1 Pd1 I1 32.9(9) . . . . ? N2 C1 Pd1 I1 -157.7(7) . . . . ? C6 C7 Pd1 C1 135.1(8) . . . . ? N3 C7 Pd1 C1 -28.4(7) . . . . ? C6 C7 Pd1 I2 -43.2(8) . . . . ? N3 C7 Pd1 I2 153.2(6) . . . . ? C6 C7 Pd1 I1 66(2) . . . . ? N3 C7 Pd1 I1 -98(2) . . . . ? C29 C28 Pd2 C32 134.1(9) . . . . ? N6 C28 Pd2 C32 -37.2(7) . . . . ? C29 C28 Pd2 I3 -43.8(9) . . . . ? N6 C28 Pd2 I3 144.9(7) . . . . ? C29 C28 Pd2 I4 126(3) . . . . ? N6 C28 Pd2 I4 -45(4) . . . . ? C33 C32 Pd2 C28 -143.0(11) . . . . ? N7 C32 Pd2 C28 32.7(8) . . . . ? C33 C32 Pd2 I3 -107(5) . . . . ? N7 C32 Pd2 I3 69(5) . . . . ? C33 C32 Pd2 I4 36.4(11) . . . . ? N7 C32 Pd2 I4 -147.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 26.15 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.280 _refine_diff_density_min -1.423 _refine_diff_density_rms 0.146 # start Validation Reply Form _vrf_PLAT029_2d ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.92 RESPONSE: For a triclinic system, max. 93% of the data are accessible with the STOE IPDS-I. Nevertheless, with a parameter / observed reflection ratio of 1:9, the structure has been refined with good precisions on bond distances and angles. ; _vrf_PLAT770_2d ; PROBLEM: Suspect C-H Bond in CIF: C25A -H26D .. 1.56 Ang. RESPONSE: The atoms are in different parts of the disordered butyl substituents. ; # end Validation Reply Form ############################################ data_11 _database_code_depnum_ccdc_archive 'CCDC 695651' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H24.50 I3 N4.50 Pd' _chemical_formula_weight 754.99 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 13.9765(12) _cell_length_b 9.9155(6) _cell_length_c 33.885(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.039(10) _cell_angle_gamma 90.00 _cell_volume 4660.6(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.75 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 4.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.252 _exptl_absorpt_correction_T_max 0.296 _exptl_absorpt_process_details ? _exptl_special_details ; 'MULABS, (PLATON03, Speck, 2003)' ; _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 oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 31627 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.99 _reflns_number_total 9055 _reflns_number_gt 6590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0690P)^2^+0.0000P] 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 9055 _refine_ls_number_parameters 408 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.001 _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 0.7904(4) 0.6030(6) 0.05953(17) 0.0240(12) Uani 1 1 d . . . C2 C 0.6848(5) 0.5971(7) 0.0038(2) 0.0342(15) Uani 1 1 d . . . H2A H 0.6600 0.5906 -0.0235 0.041 Uiso 1 1 calc R . . C3 C 0.6336(4) 0.6119(7) 0.0340(2) 0.0327(15) Uani 1 1 d . . . H3A H 0.5653 0.6173 0.0324 0.039 Uiso 1 1 calc R . . C4 C 0.6737(4) 0.6404(7) 0.1082(2) 0.0325(14) Uani 1 1 d . . . H4B H 0.6088 0.6816 0.1067 0.039 Uiso 1 1 calc R . . H4A H 0.7206 0.7043 0.1223 0.039 Uiso 1 1 calc R . . C5 C 0.6190(4) 0.4021(7) 0.11884(19) 0.0312(14) Uani 1 1 d . . . H5A H 0.5740 0.3947 0.0956 0.037 Uiso 1 1 calc R . . C6 C 0.6403(6) 0.3062(9) 0.1464(2) 0.0475(19) Uani 1 1 d . . . H6A H 0.6134 0.2182 0.1464 0.057 Uiso 1 1 calc R . . C7 C 0.7296(5) 0.4862(9) 0.16481(19) 0.0434(19) Uani 1 1 d . . . C8 C 0.7980(6) 0.5778(12) 0.1879(3) 0.067(3) Uani 1 1 d . . . H8C H 0.7895 0.5720 0.2161 0.101 Uiso 1 1 calc R . . H8B H 0.7861 0.6705 0.1785 0.101 Uiso 1 1 calc R . . H8A H 0.8641 0.5518 0.1843 0.101 Uiso 1 1 calc R . . C9 C 0.8647(4) 0.5889(8) -0.00348(18) 0.0331(15) Uani 1 1 d . . . H9A H 0.9226 0.5613 0.0151 0.040 Uiso 1 1 calc R . . C10 C 0.8485(6) 0.4825(11) -0.0360(3) 0.062(3) Uani 1 1 d . . . H10A H 0.9030 0.4828 -0.0516 0.093 Uiso 1 1 calc R . . H10B H 0.7889 0.5027 -0.0534 0.093 Uiso 1 1 calc R . . H10C H 0.8432 0.3935 -0.0239 0.093 Uiso 1 1 calc R . . C11 C 0.8836(6) 0.7283(9) -0.0186(3) 0.053(2) Uani 1 1 d . . . H11C H 0.8918 0.7917 0.0037 0.080 Uiso 1 1 calc R . . H11B H 0.8290 0.7567 -0.0377 0.080 Uiso 1 1 calc R . . H11A H 0.9424 0.7271 -0.0317 0.080 Uiso 1 1 calc R . . C12 C 0.7558(6) 0.2811(9) 0.2098(2) 0.0564(12) Uani 1 1 d D . . H12A H 0.8057 0.3369 0.2260 0.068 Uiso 0.50 1 calc PR A 1 H12B H 0.7891 0.3509 0.2278 0.068 Uiso 0.50 1 d PR A 2 C13 C 0.8040(13) 0.1525(17) 0.1933(5) 0.0564(12) Uani 0.50 1 d PD B 1 H13A H 0.7539 0.0946 0.1794 0.085 Uiso 0.50 1 calc PR B 1 H13B H 0.8391 0.1026 0.2155 0.085 Uiso 0.50 1 calc PR B 1 H13C H 0.8488 0.1804 0.1748 0.085 Uiso 0.50 1 calc PR B 1 C13A C 0.8347(11) 0.197(2) 0.1985(5) 0.0564(12) Uani 0.50 1 d PD B 2 H13D H 0.8084 0.1285 0.1794 0.085 Uiso 0.50 1 calc PR B 2 H13E H 0.8679 0.1533 0.2222 0.085 Uiso 0.50 1 calc PR B 2 H13F H 0.8805 0.2541 0.1863 0.085 Uiso 0.50 1 calc PR B 2 C14 C 0.6881(14) 0.224(4) 0.2353(6) 0.0564(12) Uani 0.50 1 d PD B 1 H14A H 0.6504 0.2975 0.2453 0.085 Uiso 0.50 1 calc PR B 1 H14B H 0.7242 0.1770 0.2577 0.085 Uiso 0.50 1 calc PR B 1 H14C H 0.6446 0.1611 0.2198 0.085 Uiso 0.50 1 calc PR B 1 C14A C 0.6726(13) 0.230(4) 0.2305(6) 0.0564(12) Uani 0.50 1 d PD B 2 H14D H 0.6346 0.3071 0.2381 0.085 Uiso 0.50 1 calc PR B 2 H14E H 0.6978 0.1797 0.2544 0.085 Uiso 0.50 1 calc PR B 2 H14F H 0.6315 0.1712 0.2125 0.085 Uiso 0.50 1 calc PR B 2 C15 C 0.7112(4) 0.7566(7) 0.31858(16) 0.0253(13) Uani 1 1 d . . . C16 C 0.6992(5) 0.8647(7) 0.25976(18) 0.0333(15) Uani 1 1 d . . . H16A H 0.6748 0.8932 0.2337 0.040 Uiso 1 1 calc R . . C17 C 0.7816(5) 0.9054(7) 0.28064(18) 0.0322(15) Uani 1 1 d . . . H17A H 0.8269 0.9674 0.2723 0.039 Uiso 1 1 calc R . . C18 C 0.8672(4) 0.8525(7) 0.34897(17) 0.0281(14) Uani 1 1 d . . . H18A H 0.9268 0.8757 0.3374 0.034 Uiso 1 1 calc R . . H18B H 0.8781 0.7658 0.3633 0.034 Uiso 1 1 calc R . . C19 C 0.8228(5) 1.0893(7) 0.36693(19) 0.0324(15) Uani 1 1 d . . . H19A H 0.8160 1.1263 0.3409 0.039 Uiso 1 1 calc R . . C20 C 0.8108(6) 1.1560(8) 0.40040(19) 0.0445(19) Uani 1 1 d . . . H20A H 0.7932 1.2480 0.4027 0.053 Uiso 1 1 calc R . . C21 C 0.8511(5) 0.9431(7) 0.41660(18) 0.0307(14) Uani 1 1 d . . . C22 C 0.8743(6) 0.8172(8) 0.4388(2) 0.0446(18) Uani 1 1 d . . . H22C H 0.8633 0.8295 0.4665 0.067 Uiso 1 1 calc R . . H22B H 0.9421 0.7939 0.4376 0.067 Uiso 1 1 calc R . . H22A H 0.8330 0.7443 0.4269 0.067 Uiso 1 1 calc R . . C23 C 0.5627(5) 0.7060(7) 0.27139(19) 0.0340(15) Uani 1 1 d . . . H23A H 0.5497 0.6452 0.2937 0.041 Uiso 1 1 calc R . . C24 C 0.4834(5) 0.8132(9) 0.2660(2) 0.0465(19) Uani 1 1 d . . . H24A H 0.4205 0.7691 0.2604 0.070 Uiso 1 1 calc R . . H24B H 0.4939 0.8724 0.2438 0.070 Uiso 1 1 calc R . . H24C H 0.4850 0.8666 0.2904 0.070 Uiso 1 1 calc R . . C25 C 0.5672(6) 0.6208(8) 0.2347(2) 0.0450(18) Uani 1 1 d . . . H25C H 0.6212 0.5575 0.2395 0.067 Uiso 1 1 calc R . . H25B H 0.5764 0.6793 0.2122 0.067 Uiso 1 1 calc R . . H25A H 0.5068 0.5704 0.2288 0.067 Uiso 1 1 calc R . . C26 C 0.8240(5) 1.0979(8) 0.4736(2) 0.0545(12) Uani 1 1 d D . . H26A H 0.8645 1.0318 0.4906 0.065 Uiso 0.50 1 calc PR C 1 H26B H 0.8481 1.0185 0.4901 0.065 Uiso 0.50 1 d PR C 2 C27 C 0.7203(8) 1.0773(19) 0.4802(6) 0.0545(12) Uani 0.50 1 d PD D 1 H27A H 0.6789 1.1372 0.4625 0.082 Uiso 0.50 1 calc PR D 1 H27B H 0.7127 1.0981 0.5079 0.082 Uiso 0.50 1 calc PR D 1 H27C H 0.7018 0.9834 0.4745 0.082 Uiso 0.50 1 calc PR D 1 C27A C 0.7207(8) 1.119(2) 0.4803(6) 0.0545(12) Uani 0.50 1 d PD D 2 H27D H 0.6979 1.2057 0.4687 0.082 Uiso 0.50 1 calc PR D 2 H27E H 0.7159 1.1200 0.5089 0.082 Uiso 0.50 1 calc PR D 2 H27F H 0.6809 1.0461 0.4677 0.082 Uiso 0.50 1 calc PR D 2 C28 C 0.8588(13) 1.2378(12) 0.4851(4) 0.0545(12) Uani 0.50 1 d PD D 1 H28A H 0.9193 1.2555 0.4742 0.082 Uiso 0.50 1 calc PR D 1 H28B H 0.8696 1.2450 0.5142 0.082 Uiso 0.50 1 calc PR D 1 H28C H 0.8101 1.3038 0.4745 0.082 Uiso 0.50 1 calc PR D 1 C28A C 0.8937(10) 1.2120(13) 0.4839(2) 0.0545(12) Uani 0.50 1 d PD D 2 H28D H 0.9178 1.2447 0.4597 0.082 Uiso 0.50 1 calc PR D 2 H28E H 0.9479 1.1799 0.5027 0.082 Uiso 0.50 1 calc PR D 2 H28F H 0.8608 1.2855 0.4961 0.082 Uiso 0.50 1 calc PR D 2 C29 C 1.0043(4) 1.2052(6) 0.30939(16) 0.0441(18) Uani 1 1 d R . . C30 C 1.0580(4) 1.3131(6) 0.33111(16) 0.059(2) Uani 1 1 d R . . H30A H 1.1184 1.2770 0.3448 0.089 Uiso 1 1 d R . . H30B H 1.0193 1.3513 0.3507 0.089 Uiso 1 1 d R . . H30C H 1.0725 1.3836 0.3125 0.089 Uiso 1 1 d R . . N1 N 0.7817(3) 0.5928(6) 0.01951(15) 0.0292(12) Uani 1 1 d . . . N2 N 0.6979(3) 0.6177(6) 0.06824(15) 0.0284(12) Uani 1 1 d . . . N3 N 0.6750(4) 0.5150(6) 0.13058(15) 0.0329(13) Uani 1 1 d . . . N4 N 0.7098(5) 0.3611(8) 0.17485(18) 0.0564(12) Uani 1 1 d . B . N5 N 0.6558(4) 0.7738(6) 0.28283(14) 0.0287(12) Uani 1 1 d . . . N6 N 0.7875(3) 0.8381(5) 0.31721(14) 0.0271(11) Uani 1 1 d . . . N7 N 0.8465(4) 0.9579(6) 0.37688(14) 0.0296(12) Uani 1 1 d . . . N8 N 0.8295(5) 1.0630(8) 0.43102(17) 0.0545(12) Uani 1 1 d . D . N9 N 0.9640(5) 1.1210(9) 0.2926(2) 0.062(2) Uani 1 1 d . . . Pd1 Pd 0.90748(3) 0.59368(5) 0.098148(13) 0.02427(11) Uani 1 1 d . . . Pd2 Pd 0.68021(3) 0.63614(5) 0.361401(13) 0.02679(12) Uani 1 1 d . . . I1 I 0.89944(3) 0.85786(5) 0.103930(14) 0.03777(12) Uani 1 1 d . . . I2 I 1.06382(3) 0.57013(5) 0.151755(12) 0.03812(12) Uani 1 1 d . . . I3 I 0.89028(3) 0.33189(5) 0.090685(12) 0.03354(11) Uani 1 1 d . . . I4 I 0.78128(3) 0.45680(5) 0.327630(13) 0.03965(12) Uani 1 1 d . . . I5 I 0.62480(4) 0.46749(5) 0.416048(13) 0.04130(13) Uani 1 1 d . . . I6 I 0.59580(3) 0.84455(5) 0.389284(13) 0.03623(12) 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 0.024(3) 0.015(3) 0.033(3) 0.003(2) 0.006(2) -0.003(2) C2 0.030(3) 0.026(4) 0.044(4) 0.008(3) -0.008(3) -0.001(3) C3 0.015(3) 0.035(4) 0.047(4) 0.007(3) -0.005(3) -0.003(3) C4 0.022(3) 0.029(4) 0.048(4) -0.004(3) 0.010(3) -0.004(3) C5 0.031(3) 0.026(4) 0.034(3) -0.001(3) -0.006(3) -0.009(3) C6 0.053(4) 0.048(5) 0.040(4) 0.002(3) -0.003(3) -0.019(4) C7 0.035(4) 0.069(6) 0.026(3) -0.009(3) 0.006(3) -0.015(4) C8 0.052(5) 0.103(8) 0.047(5) -0.019(5) 0.006(4) -0.043(5) C9 0.026(3) 0.047(5) 0.026(3) 0.008(3) 0.003(2) 0.004(3) C10 0.057(5) 0.074(7) 0.059(5) -0.030(5) 0.021(4) -0.015(5) C11 0.042(4) 0.057(6) 0.064(5) 0.013(4) 0.021(4) -0.009(4) C12 0.063(3) 0.068(3) 0.035(2) 0.015(2) -0.0051(19) -0.008(2) C13 0.063(3) 0.068(3) 0.035(2) 0.015(2) -0.0051(19) -0.008(2) C13A 0.063(3) 0.068(3) 0.035(2) 0.015(2) -0.0051(19) -0.008(2) C14 0.063(3) 0.068(3) 0.035(2) 0.015(2) -0.0051(19) -0.008(2) C14A 0.063(3) 0.068(3) 0.035(2) 0.015(2) -0.0051(19) -0.008(2) C15 0.028(3) 0.026(4) 0.021(3) 0.002(2) 0.000(2) 0.009(3) C16 0.037(3) 0.036(4) 0.025(3) 0.008(3) -0.004(3) -0.001(3) C17 0.036(3) 0.032(4) 0.028(3) 0.010(3) 0.001(3) -0.005(3) C18 0.022(3) 0.035(4) 0.026(3) -0.001(3) -0.001(2) 0.002(3) C19 0.049(4) 0.018(4) 0.029(3) 0.005(3) 0.000(3) 0.003(3) C20 0.060(5) 0.042(5) 0.028(3) 0.000(3) -0.008(3) 0.009(4) C21 0.034(3) 0.026(4) 0.030(3) 0.004(3) -0.002(3) 0.002(3) C22 0.051(4) 0.052(5) 0.030(3) 0.006(3) 0.002(3) 0.008(4) C23 0.034(3) 0.035(4) 0.031(3) 0.007(3) -0.003(3) -0.012(3) C24 0.028(3) 0.057(5) 0.052(4) 0.015(4) -0.005(3) -0.005(3) C25 0.055(4) 0.038(5) 0.040(4) -0.002(3) 0.001(3) -0.021(4) C26 0.079(3) 0.055(3) 0.0280(18) -0.0068(19) -0.0005(19) 0.017(2) C27 0.079(3) 0.055(3) 0.0280(18) -0.0068(19) -0.0005(19) 0.017(2) C27A 0.079(3) 0.055(3) 0.0280(18) -0.0068(19) -0.0005(19) 0.017(2) C28 0.079(3) 0.055(3) 0.0280(18) -0.0068(19) -0.0005(19) 0.017(2) C28A 0.079(3) 0.055(3) 0.0280(18) -0.0068(19) -0.0005(19) 0.017(2) C29 0.035(4) 0.047(5) 0.052(4) -0.009(4) 0.008(3) -0.008(3) C30 0.056(5) 0.048(6) 0.071(6) -0.013(4) -0.002(4) -0.002(4) N1 0.021(2) 0.035(3) 0.030(3) 0.007(2) 0.000(2) 0.001(2) N2 0.019(2) 0.029(3) 0.038(3) 0.004(2) 0.003(2) 0.003(2) N3 0.026(3) 0.040(4) 0.033(3) -0.004(2) 0.007(2) 0.001(2) N4 0.063(3) 0.068(3) 0.035(2) 0.015(2) -0.0051(19) -0.008(2) N5 0.031(3) 0.029(3) 0.026(2) 0.003(2) 0.000(2) -0.004(2) N6 0.024(3) 0.029(3) 0.027(2) 0.004(2) -0.0028(19) -0.004(2) N7 0.028(3) 0.036(3) 0.023(2) 0.003(2) -0.002(2) -0.001(2) N8 0.079(3) 0.055(3) 0.0280(18) -0.0068(19) -0.0005(19) 0.017(2) N9 0.057(4) 0.066(6) 0.065(4) -0.017(4) 0.017(4) -0.021(4) Pd1 0.0188(2) 0.0291(3) 0.0245(2) 0.00058(18) 0.00095(16) 0.00122(18) Pd2 0.0287(2) 0.0278(3) 0.0228(2) 0.00430(19) -0.00084(17) -0.0011(2) I1 0.0238(2) 0.0291(3) 0.0594(3) 0.0009(2) 0.00096(18) -0.00056(17) I2 0.0404(2) 0.0392(3) 0.0316(2) 0.00264(18) -0.00780(17) -0.0005(2) I3 0.0320(2) 0.0295(3) 0.0377(2) -0.00322(18) -0.00122(16) 0.00301(17) I4 0.0458(3) 0.0327(3) 0.0417(2) 0.00429(19) 0.01044(19) 0.0061(2) I5 0.0547(3) 0.0381(3) 0.0318(2) 0.00871(19) 0.00811(19) 0.0001(2) I6 0.0357(2) 0.0349(3) 0.0386(2) -0.00079(19) 0.00642(17) 0.00086(19) _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 1.350(8) . ? C1 N2 1.368(8) . ? C1 Pd1 1.968(6) . ? C2 C3 1.328(10) . ? C2 N1 1.393(8) . ? C2 H2A 0.9500 . ? C3 N2 1.378(8) . ? C3 H3A 0.9500 . ? C4 N2 1.454(8) . ? C4 N3 1.455(9) . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 C6 1.340(10) . ? C5 N3 1.394(8) . ? C5 H5A 0.9500 . ? C6 N4 1.393(10) . ? C6 H6A 0.9500 . ? C7 N4 1.324(11) . ? C7 N3 1.339(9) . ? C7 C8 1.472(10) . ? C8 H8C 0.9800 . ? C8 H8B 0.9800 . ? C8 H8A 0.9800 . ? C9 N1 1.475(8) . ? C9 C11 1.509(11) . ? C9 C10 1.521(10) . ? C9 H9A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11C 0.9800 . ? C11 H11B 0.9800 . ? C11 H11A 0.9800 . ? C12 C13A 1.468(15) . ? C12 C14 1.469(16) . ? C12 N4 1.503(10) . ? C12 C14A 1.517(16) . ? C12 C13 1.575(16) . ? C12 H12A 1.0000 . ? C12 H12B 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C15 N6 1.343(8) . ? C15 N5 1.366(7) . ? C15 Pd2 1.968(6) . ? C16 C17 1.338(9) . ? C16 N5 1.381(8) . ? C16 H16A 0.9500 . ? C17 N6 1.401(8) . ? C17 H17A 0.9500 . ? C18 N6 1.458(7) . ? C18 N7 1.462(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.341(10) . ? C19 N7 1.377(9) . ? C19 H19A 0.9500 . ? C20 N8 1.389(10) . ? C20 H20A 0.9500 . ? C21 N8 1.334(9) . ? C21 N7 1.348(8) . ? C21 C22 1.472(10) . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C22 H22A 0.9800 . ? C23 N5 1.474(8) . ? C23 C25 1.509(10) . ? C23 C24 1.530(10) . ? C23 H23A 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25C 0.9800 . ? C25 H25B 0.9800 . ? C25 H25A 0.9800 . ? C26 N8 1.494(9) . ? C26 C27A 1.505(9) . ? C26 C28 1.505(9) . ? C26 C28A 1.506(7) . ? C26 C27 1.507(9) . ? C26 H26A 1.0000 . ? C26 H26B 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27A H27D 0.9800 . ? C27A H27E 0.9800 . ? C27A H27F 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29 N9 1.122(9) . ? C29 C30 1.4541 . ? C30 H30A 0.9799 . ? C30 H30B 0.9808 . ? C30 H30C 0.9795 . ? Pd1 I3 2.6162(7) . ? Pd1 I1 2.6302(7) . ? Pd1 I2 2.6751(7) . ? Pd2 I6 2.6131(7) . ? Pd2 I4 2.6199(7) . ? Pd2 I5 2.6789(7) . ? 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 N2 104.7(5) . . ? N1 C1 Pd1 129.0(4) . . ? N2 C1 Pd1 126.3(4) . . ? C3 C2 N1 107.5(6) . . ? C3 C2 H2A 126.2 . . ? N1 C2 H2A 126.2 . . ? C2 C3 N2 107.1(5) . . ? C2 C3 H3A 126.4 . . ? N2 C3 H3A 126.4 . . ? N2 C4 N3 111.3(5) . . ? N2 C4 H4B 109.4 . . ? N3 C4 H4B 109.4 . . ? N2 C4 H4A 109.4 . . ? N3 C4 H4A 109.4 . . ? H4B C4 H4A 108.0 . . ? C6 C5 N3 107.6(6) . . ? C6 C5 H5A 126.2 . . ? N3 C5 H5A 126.2 . . ? C5 C6 N4 106.3(7) . . ? C5 C6 H6A 126.8 . . ? N4 C6 H6A 126.8 . . ? N4 C7 N3 107.9(6) . . ? N4 C7 C8 125.8(8) . . ? N3 C7 C8 126.4(8) . . ? C7 C8 H8C 109.5 . . ? C7 C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? C7 C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? N1 C9 C11 109.7(6) . . ? N1 C9 C10 110.1(6) . . ? C11 C9 C10 113.9(7) . . ? N1 C9 H9A 107.6 . . ? C11 C9 H9A 107.6 . . ? C10 C9 H9A 107.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11C 109.5 . . ? C9 C11 H11B 109.5 . . ? H11C C11 H11B 109.5 . . ? C9 C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? C13A C12 C14 119.6(17) . . ? C13A C12 N4 110.9(9) . . ? C14 C12 N4 114.9(10) . . ? C13A C12 C14A 125.1(17) . . ? C14 C12 C14A 9.8(14) . . ? N4 C12 C14A 105.1(10) . . ? C13A C12 C13 23.5(9) . . ? C14 C12 C13 103.4(18) . . ? N4 C12 C13 108.0(8) . . ? C14A C12 C13 106.3(17) . . ? C13A C12 H12A 87.8 . . ? C14 C12 H12A 110.1 . . ? N4 C12 H12A 110.1 . . ? C14A C12 H12A 116.8 . . ? C13 C12 H12A 110.1 . . ? C13A C12 H12B 104.1 . . ? C14 C12 H12B 100.9 . . ? N4 C12 H12B 103.8 . . ? C14A C12 H12B 105.8 . . ? C13 C12 H12B 126.1 . . ? H12A C12 H12B 16.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? C12 C13A H13D 109.5 . . ? C12 C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C12 C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? C12 C14A H14D 109.5 . . ? C12 C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C12 C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? N6 C15 N5 105.1(5) . . ? N6 C15 Pd2 129.6(4) . . ? N5 C15 Pd2 125.3(5) . . ? C17 C16 N5 107.8(5) . . ? C17 C16 H16A 126.1 . . ? N5 C16 H16A 126.1 . . ? C16 C17 N6 106.1(6) . . ? C16 C17 H17A 126.9 . . ? N6 C17 H17A 126.9 . . ? N6 C18 N7 110.7(5) . . ? N6 C18 H18A 109.5 . . ? N7 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? N7 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 N7 108.1(6) . . ? C20 C19 H19A 125.9 . . ? N7 C19 H19A 125.9 . . ? C19 C20 N8 105.8(7) . . ? C19 C20 H20A 127.1 . . ? N8 C20 H20A 127.1 . . ? N8 C21 N7 106.5(6) . . ? N8 C21 C22 127.9(6) . . ? N7 C21 C22 125.6(6) . . ? C21 C22 H22C 109.5 . . ? C21 C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C21 C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? N5 C23 C25 110.3(6) . . ? N5 C23 C24 108.5(6) . . ? C25 C23 C24 113.1(6) . . ? N5 C23 H23A 108.2 . . ? C25 C23 H23A 108.2 . . ? C24 C23 H23A 108.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25C 109.5 . . ? C23 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C23 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? N8 C26 C27A 110.0(9) . . ? N8 C26 C28 114.3(8) . . ? C27A C26 C28 96.6(11) . . ? N8 C26 C28A 106.9(6) . . ? C27A C26 C28A 117.7(11) . . ? C28 C26 C28A 21.3(9) . . ? N8 C26 C27 106.0(9) . . ? C27A C26 C27 15.9(12) . . ? C28 C26 C27 111.8(11) . . ? C28A C26 C27 132.3(11) . . ? N8 C26 H26A 108.2 . . ? C27A C26 H26A 119.4 . . ? C28 C26 H26A 108.2 . . ? C28A C26 H26A 93.1 . . ? C27 C26 H26A 108.2 . . ? N8 C26 H26B 107.7 . . ? C27A C26 H26B 106.9 . . ? C28 C26 H26B 120.3 . . ? C28A C26 H26B 107.3 . . ? C27 C26 H26B 94.2 . . ? H26A C26 H26B 15.1 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? C26 C27A H27D 109.5 . . ? C26 C27A H27E 109.5 . . ? H27D C27A H27E 109.5 . . ? C26 C27A H27F 109.5 . . ? H27D C27A H27F 109.5 . . ? H27E C27A H27F 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? C26 C28A H28D 109.5 . . ? C26 C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C26 C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? N9 C29 C30 179.1(5) . . ? C29 C30 H30A 109.4 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.4 . . ? H30B C30 H30C 109.5 . . ? C1 N1 C2 110.1(5) . . ? C1 N1 C9 123.5(5) . . ? C2 N1 C9 126.2(5) . . ? C1 N2 C3 110.5(5) . . ? C1 N2 C4 123.5(5) . . ? C3 N2 C4 126.0(5) . . ? C7 N3 C5 108.4(6) . . ? C7 N3 C4 127.0(6) . . ? C5 N3 C4 124.5(5) . . ? C7 N4 C6 109.8(6) . . ? C7 N4 C12 127.9(7) . . ? C6 N4 C12 122.3(7) . . ? C15 N5 C16 110.1(5) . . ? C15 N5 C23 124.2(5) . . ? C16 N5 C23 125.7(5) . . ? C15 N6 C17 110.9(5) . . ? C15 N6 C18 124.9(5) . . ? C17 N6 C18 124.3(5) . . ? C21 N7 C19 109.2(6) . . ? C21 N7 C18 125.4(6) . . ? C19 N7 C18 125.4(5) . . ? C21 N8 C20 110.4(6) . . ? C21 N8 C26 126.9(6) . . ? C20 N8 C26 122.7(7) . . ? C1 Pd1 I3 85.59(18) . . ? C1 Pd1 I1 87.89(18) . . ? I3 Pd1 I1 172.33(2) . . ? C1 Pd1 I2 177.37(17) . . ? I3 Pd1 I2 92.11(2) . . ? I1 Pd1 I2 94.31(2) . . ? C15 Pd2 I6 86.37(17) . . ? C15 Pd2 I4 84.87(17) . . ? I6 Pd2 I4 170.48(3) . . ? C15 Pd2 I5 175.41(17) . . ? I6 Pd2 I5 93.56(2) . . ? I4 Pd2 I5 95.47(2) . . ? 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 C2 C3 N2 0.4(8) . . . . ? N3 C5 C6 N4 -0.2(9) . . . . ? N5 C16 C17 N6 -0.4(8) . . . . ? N7 C19 C20 N8 1.0(8) . . . . ? N2 C1 N1 C2 -1.8(7) . . . . ? Pd1 C1 N1 C2 176.5(5) . . . . ? N2 C1 N1 C9 173.7(6) . . . . ? Pd1 C1 N1 C9 -8.0(9) . . . . ? C3 C2 N1 C1 0.9(8) . . . . ? C3 C2 N1 C9 -174.5(6) . . . . ? C11 C9 N1 C1 -96.5(7) . . . . ? C10 C9 N1 C1 137.4(7) . . . . ? C11 C9 N1 C2 78.3(8) . . . . ? C10 C9 N1 C2 -47.8(9) . . . . ? N1 C1 N2 C3 2.1(7) . . . . ? Pd1 C1 N2 C3 -176.3(5) . . . . ? N1 C1 N2 C4 -176.2(6) . . . . ? Pd1 C1 N2 C4 5.5(9) . . . . ? C2 C3 N2 C1 -1.6(8) . . . . ? C2 C3 N2 C4 176.6(6) . . . . ? N3 C4 N2 C1 -80.3(7) . . . . ? N3 C4 N2 C3 101.7(7) . . . . ? N4 C7 N3 C5 -0.3(8) . . . . ? C8 C7 N3 C5 -178.9(7) . . . . ? N4 C7 N3 C4 -179.1(6) . . . . ? C8 C7 N3 C4 2.2(11) . . . . ? C6 C5 N3 C7 0.3(8) . . . . ? C6 C5 N3 C4 179.2(6) . . . . ? N2 C4 N3 C7 121.0(7) . . . . ? N2 C4 N3 C5 -57.7(8) . . . . ? N3 C7 N4 C6 0.1(9) . . . . ? C8 C7 N4 C6 178.8(8) . . . . ? N3 C7 N4 C12 176.9(7) . . . . ? C8 C7 N4 C12 -4.5(14) . . . . ? C5 C6 N4 C7 0.0(10) . . . . ? C5 C6 N4 C12 -176.9(7) . . . . ? C13A C12 N4 C7 -94.4(13) . . . . ? C14 C12 N4 C7 126.0(18) . . . . ? C14A C12 N4 C7 127.7(17) . . . . ? C13 C12 N4 C7 -119.1(11) . . . . ? C13A C12 N4 C6 81.9(12) . . . . ? C14 C12 N4 C6 -57.6(19) . . . . ? C14A C12 N4 C6 -55.9(18) . . . . ? C13 C12 N4 C6 57.2(12) . . . . ? N6 C15 N5 C16 0.6(7) . . . . ? Pd2 C15 N5 C16 -179.5(5) . . . . ? N6 C15 N5 C23 -178.5(6) . . . . ? Pd2 C15 N5 C23 1.4(9) . . . . ? C17 C16 N5 C15 -0.1(8) . . . . ? C17 C16 N5 C23 178.9(6) . . . . ? C25 C23 N5 C15 -120.0(7) . . . . ? C24 C23 N5 C15 115.5(7) . . . . ? C25 C23 N5 C16 61.0(9) . . . . ? C24 C23 N5 C16 -63.4(8) . . . . ? N5 C15 N6 C17 -0.9(7) . . . . ? Pd2 C15 N6 C17 179.3(5) . . . . ? N5 C15 N6 C18 -179.4(5) . . . . ? Pd2 C15 N6 C18 0.8(9) . . . . ? C16 C17 N6 C15 0.8(8) . . . . ? C16 C17 N6 C18 179.4(6) . . . . ? N7 C18 N6 C15 -88.8(7) . . . . ? N7 C18 N6 C17 92.8(7) . . . . ? N8 C21 N7 C19 0.7(8) . . . . ? C22 C21 N7 C19 179.9(7) . . . . ? N8 C21 N7 C18 178.4(6) . . . . ? C22 C21 N7 C18 -2.3(10) . . . . ? C20 C19 N7 C21 -1.1(8) . . . . ? C20 C19 N7 C18 -178.8(6) . . . . ? N6 C18 N7 C21 127.1(6) . . . . ? N6 C18 N7 C19 -55.5(8) . . . . ? N7 C21 N8 C20 0.0(9) . . . . ? C22 C21 N8 C20 -179.3(7) . . . . ? N7 C21 N8 C26 179.4(7) . . . . ? C22 C21 N8 C26 0.1(13) . . . . ? C19 C20 N8 C21 -0.6(9) . . . . ? C19 C20 N8 C26 179.9(7) . . . . ? C27A C26 N8 C21 -108.6(12) . . . . ? C28 C26 N8 C21 143.9(10) . . . . ? C28A C26 N8 C21 122.5(11) . . . . ? C27 C26 N8 C21 -92.4(12) . . . . ? C27A C26 N8 C20 70.7(12) . . . . ? C28 C26 N8 C20 -36.7(13) . . . . ? C28A C26 N8 C20 -58.1(12) . . . . ? C27 C26 N8 C20 86.9(11) . . . . ? N1 C1 Pd1 I3 -81.2(6) . . . . ? N2 C1 Pd1 I3 96.7(5) . . . . ? N1 C1 Pd1 I1 102.9(6) . . . . ? N2 C1 Pd1 I1 -79.2(5) . . . . ? N1 C1 Pd1 I2 -110(4) . . . . ? N2 C1 Pd1 I2 68(4) . . . . ? N6 C15 Pd2 I6 88.0(6) . . . . ? N5 C15 Pd2 I6 -91.8(5) . . . . ? N6 C15 Pd2 I4 -88.3(6) . . . . ? N5 C15 Pd2 I4 91.9(5) . . . . ? N6 C15 Pd2 I5 177.3(18) . . . . ? N5 C15 Pd2 I5 -3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.623 _refine_diff_density_min -1.861 _refine_diff_density_rms 0.205 ###################################################################END