# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistyr 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address "Jorge L. Sague'" ;University of Geneva Department of Inorganic, Analytical and Applied Chemistry 30, Quai Ernest-Ansermet 1211 Geneva 4 Switzerland ; 'Katharina Fromm' ;University of Basel Department of Chemistry Klingelbergstrasse 80 CH-4056. Basel Switzerland ; 'Markus Meuwly' '' _publ_contact_author_name 'Dr Jorge L Sague' _publ_contact_author_email JORGE.SAGUE@CHIAM.UNIGE.CH _publ_section_title ; Counterion effect on the formation of coordination polymer networks between AgNO3 and L (2,2'-oxybis(ethane-2,1-diyl) diisonicotinate). Part 2. ; _publ_contact_author_address ;University of Fribourg Chemistry Department Rue du Musee 9 CH-1700. Fribourg Switzerland ; _publ_contact_author_phone '+41 26 300 87 36' # Attachment 'CCDC_678543.cif' data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 678543' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common L6AgNO3.H2O _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Ag2 N6 O20' _chemical_formula_weight 1044.44 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.668(3) _cell_length_b 7.3268(15) _cell_length_c 20.232(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.86(3) _cell_angle_gamma 90.00 _cell_volume 2018.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 386(2) _cell_measurement_reflns_used 12538 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 27.04 _exptl_crystal_description 'Rod-like crystal' _exptl_crystal_colour colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.058 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Solvent used: Ethanol Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): Frames collected: 180 Seconds exposure per frame: 60 Degrees rotation per frame: 1 Crystal-Detector distance (mm): 160 ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube,12x0.4 mm long-fine focus' _diffrn_source_type 'STOE IPDS II' _diffrn_radiation_monochromator 'plane graphite' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_reflns_number 12538 _diffrn_reflns_av_R_equivalents 0.0844 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.04 _reflns_number_total 4277 _reflns_number_gt 3432 _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 'SHELXL97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97, SCHAKAL and PLATON (Spek, 2003)' _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^)+(0.0401P)^2^+2.4315P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4277 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.03413(2) 0.29258(5) 0.025709(16) 0.04919(13) Uani 1 1 d . . . N1 N -0.0901(2) 0.3321(4) 0.08606(16) 0.0387(6) Uani 1 1 d . . . C1 C -0.1834(3) 0.3041(5) 0.06398(19) 0.0421(8) Uani 1 1 d . . . H1 H -0.1971 0.2632 0.0207 0.050 Uiso 1 1 calc R . . C2 C -0.2617(2) 0.3333(5) 0.10268(18) 0.0394(8) Uani 1 1 d . . . H2 H -0.3261 0.3144 0.0854 0.047 Uiso 1 1 calc R . . C3 C -0.2412(2) 0.3905(5) 0.16695(17) 0.0353(7) Uani 1 1 d . . . C4 C -0.1448(3) 0.4163(6) 0.1906(2) 0.0475(9) Uani 1 1 d . . . H4 H -0.1290 0.4526 0.2343 0.057 Uiso 1 1 calc R . . C5 C -0.0720(3) 0.3874(6) 0.1487(2) 0.0478(9) Uani 1 1 d . . . H5 H -0.0071 0.4075 0.1648 0.057 Uiso 1 1 calc R . . C6 C -0.3212(3) 0.4277(6) 0.2120(2) 0.0452(9) Uani 1 1 d . . . O1 O -0.3070(2) 0.4404(7) 0.27042(17) 0.0778(12) Uani 1 1 d . . . O2 O -0.40735(17) 0.4467(4) 0.17783(15) 0.0522(7) Uani 1 1 d . . . C7 C -0.4939(3) 0.4701(7) 0.2149(3) 0.0614(12) Uani 1 1 d . A . H7A H -0.4763 0.5406 0.2547 0.074 Uiso 1 1 calc R . . H7B H -0.5438 0.5371 0.1880 0.074 Uiso 1 1 calc R . . C8 C -0.5330(4) 0.2947(8) 0.2330(3) 0.0782(18) Uani 1 1 d . . . H8A H -0.5938 0.3122 0.2537 0.094 Uiso 0.727(9) 1 calc PR A 1 H8B H -0.4866 0.2335 0.2644 0.094 Uiso 0.727(9) 1 calc PR A 1 H8C H -0.5258 0.2963 0.2811 0.094 Uiso 0.273(9) 1 calc PR A 2 H8D H -0.6030 0.3067 0.2211 0.094 Uiso 0.273(9) 1 calc PR A 2 O3A O -0.5515(3) 0.1816(6) 0.1721(2) 0.0547(15) Uani 0.727(9) 1 d P A 1 O3B O -0.5155(6) 0.1326(13) 0.2189(5) 0.035(3) Uani 0.273(9) 1 d P A 2 C9 C -0.5883(3) 0.0146(8) 0.1830(3) 0.0718(14) Uani 1 1 d . . . H9A H -0.6545 0.0259 0.1965 0.086 Uiso 0.727(9) 1 calc PR A 1 H9B H -0.5483 -0.0458 0.2184 0.086 Uiso 0.727(9) 1 calc PR A 1 H9C H -0.6049 -0.0732 0.2162 0.086 Uiso 0.273(9) 1 calc PR A 2 H9D H -0.6456 0.0923 0.1756 0.086 Uiso 0.273(9) 1 calc PR A 2 C10 C -0.5894(3) -0.0877(7) 0.1255(3) 0.0625(13) Uani 1 1 d . A . H10A H -0.6231 -0.0209 0.0890 0.075 Uiso 1 1 calc R . . H10B H -0.6244 -0.2011 0.1310 0.075 Uiso 1 1 calc R . . O4 O -0.48899(18) -0.1268(5) 0.11066(16) 0.0541(7) Uani 1 1 d . . . O5 O -0.5468(2) -0.2484(7) 0.0153(2) 0.0869(13) Uani 1 1 d . . . C11 C -0.4795(3) -0.2050(6) 0.0532(2) 0.0473(9) Uani 1 1 d . A . N2 N -0.1821(2) -0.2745(4) 0.00640(15) 0.0399(7) Uani 1 1 d . . . C12 C -0.2021(2) -0.1910(5) 0.06209(19) 0.0401(8) Uani 1 1 d . . . H12 H -0.1499 -0.1466 0.0900 0.048 Uiso 1 1 calc R . . C13 C -0.2965(3) -0.1667(5) 0.08063(19) 0.0402(8) Uani 1 1 d . A . H13 H -0.3071 -0.1081 0.1202 0.048 Uiso 1 1 calc R . . C14 C -0.3737(2) -0.2305(5) 0.03979(18) 0.0372(7) Uani 1 1 d . . . C15 C -0.3542(3) -0.3212(6) -0.0177(2) 0.0498(10) Uani 1 1 d . A . H15 H -0.4050 -0.3691 -0.0460 0.060 Uiso 1 1 calc R . . C16 C -0.2578(3) -0.3389(6) -0.0320(2) 0.0505(10) Uani 1 1 d . . . H16 H -0.2451 -0.3994 -0.0708 0.061 Uiso 1 1 calc R A . N3 N -0.1001(2) 0.1561(5) -0.09768(17) 0.0451(7) Uani 1 1 d . . . O6 O -0.0930(3) 0.3208(5) -0.0865(2) 0.0736(10) Uani 1 1 d . . . O7 O -0.0321(3) 0.0545(6) -0.0792(3) 0.0931(14) Uani 1 1 d . . . O8 O -0.1750(2) 0.0933(6) -0.1267(2) 0.0808(11) Uani 1 1 d . . . O9 O -0.2634(2) 0.4333(6) -0.18703(18) 0.0568(8) Uani 1 1 d . . . H9E H -0.226(4) 0.362(9) -0.168(3) 0.073(18) Uiso 1 1 d . . . H9F H -0.227(4) 0.522(8) -0.189(3) 0.066(17) Uiso 1 1 d . . . O10 O -0.1626(3) -0.2388(5) -0.1980(2) 0.0599(8) Uani 1 1 d . . . H10E H -0.170(6) -0.157(13) -0.163(5) 0.14(3) Uiso 1 1 d . . . H10F H -0.193(5) -0.194(10) -0.223(3) 0.09(2) Uiso 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 Ag1 0.04049(17) 0.0544(2) 0.0555(2) -0.00548(15) 0.02063(13) 0.00169(13) N1 0.0348(14) 0.0388(16) 0.0433(16) 0.0027(13) 0.0077(12) 0.0031(12) C1 0.0404(17) 0.046(2) 0.0407(19) -0.0050(16) 0.0072(15) -0.0047(16) C2 0.0327(15) 0.0441(19) 0.0413(19) -0.0024(15) 0.0026(14) -0.0035(14) C3 0.0313(15) 0.0393(18) 0.0363(17) 0.0019(14) 0.0082(13) -0.0012(14) C4 0.0346(16) 0.066(3) 0.041(2) -0.0046(19) 0.0018(14) 0.0005(17) C5 0.0297(16) 0.069(3) 0.044(2) -0.0018(19) -0.0007(14) 0.0034(18) C6 0.0372(17) 0.051(2) 0.049(2) -0.0041(18) 0.0111(15) -0.0013(16) O1 0.0539(17) 0.134(4) 0.0472(18) -0.012(2) 0.0134(14) 0.009(2) O2 0.0292(12) 0.0679(19) 0.0611(18) -0.0050(15) 0.0123(12) 0.0021(12) C7 0.0366(19) 0.064(3) 0.087(3) -0.014(3) 0.024(2) 0.0012(19) C8 0.059(3) 0.067(3) 0.117(5) 0.009(3) 0.054(3) 0.015(2) O3A 0.059(2) 0.059(3) 0.049(3) 0.012(2) 0.026(2) 0.010(2) O3B 0.026(4) 0.048(5) 0.034(6) 0.011(4) 0.009(3) 0.013(4) C9 0.045(2) 0.091(4) 0.082(4) -0.002(3) 0.021(2) 0.004(3) C10 0.0366(19) 0.062(3) 0.092(4) 0.017(3) 0.026(2) 0.0096(19) O4 0.0314(12) 0.0680(19) 0.0647(18) -0.0022(16) 0.0147(12) 0.0022(13) O5 0.0375(15) 0.127(4) 0.094(3) -0.026(3) -0.0090(17) -0.0012(19) C11 0.0339(17) 0.051(2) 0.058(2) 0.0071(19) 0.0055(16) -0.0001(16) N2 0.0405(15) 0.0421(16) 0.0392(15) -0.0009(13) 0.0157(13) 0.0013(13) C12 0.0332(16) 0.044(2) 0.0436(19) -0.0067(16) 0.0056(14) -0.0025(15) C13 0.0364(16) 0.045(2) 0.0402(19) -0.0069(15) 0.0097(14) 0.0001(15) C14 0.0310(15) 0.0398(18) 0.0414(18) 0.0071(15) 0.0059(13) -0.0022(14) C15 0.046(2) 0.064(3) 0.039(2) -0.0086(18) 0.0013(16) -0.0064(19) C16 0.051(2) 0.064(3) 0.038(2) -0.0103(18) 0.0119(17) -0.0044(19) N3 0.0414(16) 0.0509(19) 0.0433(17) 0.0041(14) 0.0049(13) 0.0001(15) O6 0.098(3) 0.0456(19) 0.076(2) -0.0050(16) -0.004(2) 0.0022(18) O7 0.0578(19) 0.065(2) 0.151(4) 0.030(3) -0.023(2) 0.0052(18) O8 0.0471(17) 0.085(3) 0.107(3) -0.023(2) -0.0116(18) -0.0043(18) O9 0.0510(17) 0.0568(19) 0.062(2) 0.0056(16) 0.0008(15) 0.0030(17) O10 0.0562(18) 0.0507(19) 0.072(2) 0.0002(17) -0.0010(17) 0.0065(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.181(3) 3 ? Ag1 N1 2.193(3) . ? Ag1 Ag1 3.3206(9) 3_565 ? N1 C1 1.331(5) . ? N1 C5 1.333(5) . ? C1 C2 1.394(5) . ? C1 H1 0.9300 . ? C2 C3 1.372(5) . ? C2 H2 0.9300 . ? C3 C4 1.377(5) . ? C3 C6 1.506(5) . ? C4 C5 1.378(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 O1 1.186(5) . ? C6 O2 1.321(5) . ? O2 C7 1.463(4) . ? C7 C8 1.450(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O3B 1.250(11) . ? C8 O3A 1.487(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? O3A C9 1.349(7) . ? O3B C9 1.464(11) . ? C9 C10 1.384(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C10 O4 1.458(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O4 C11 1.312(5) . ? O5 C11 1.189(5) . ? C11 C14 1.506(5) . ? N2 C16 1.327(5) . ? N2 C12 1.330(5) . ? N2 Ag1 2.181(3) 3 ? C12 C13 1.385(5) . ? C12 H12 0.9300 . ? C13 C14 1.366(5) . ? C13 H13 0.9300 . ? C14 C15 1.384(5) . ? C15 C16 1.379(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? N3 O7 1.225(5) . ? N3 O8 1.226(5) . ? N3 O6 1.230(5) . ? O9 H9E 0.81(6) . ? O9 H9F 0.82(6) . ? O10 H10E 0.94(10) . ? O10 H10F 0.71(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 N2 Ag1 N1 162.86(12) 3 . ? N2 Ag1 Ag1 101.86(9) 3 3_565 ? N1 Ag1 Ag1 80.99(8) . 3_565 ? C1 N1 C5 117.5(3) . . ? C1 N1 Ag1 123.9(3) . . ? C5 N1 Ag1 118.6(2) . . ? N1 C1 C2 123.1(4) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 C6 121.9(3) . . ? C4 C3 C6 119.2(3) . . ? C3 C4 C5 119.0(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 123.1(3) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? O1 C6 O2 125.2(4) . . ? O1 C6 C3 123.5(4) . . ? O2 C6 C3 111.3(3) . . ? C6 O2 C7 117.9(4) . . ? C8 C7 O2 110.9(4) . . ? C8 C7 H7A 109.5 . . ? O2 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? O3B C8 C7 134.6(5) . . ? O3B C8 O3A 45.9(5) . . ? C7 C8 O3A 109.0(5) . . ? O3B C8 H8A 114.3 . . ? C7 C8 H8A 109.9 . . ? O3A C8 H8A 109.9 . . ? O3B C8 H8B 65.3 . . ? C7 C8 H8B 109.9 . . ? O3A C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? O3B C8 H8C 103.5 . . ? C7 C8 H8C 103.5 . . ? O3A C8 H8C 146.4 . . ? H8A C8 H8C 65.4 . . ? H8B C8 H8C 48.8 . . ? O3B C8 H8D 103.5 . . ? C7 C8 H8D 103.5 . . ? O3A C8 H8D 75.6 . . ? H8A C8 H8D 40.0 . . ? H8B C8 H8D 141.4 . . ? H8C C8 H8D 105.3 . . ? C9 O3A C8 114.2(4) . . ? C8 O3B C9 122.6(7) . . ? O3A C9 C10 109.4(5) . . ? O3A C9 O3B 45.4(4) . . ? C10 C9 O3B 134.1(5) . . ? O3A C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? O3B C9 H9A 114.9 . . ? O3A C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? O3B C9 H9B 65.5 . . ? H9A C9 H9B 108.2 . . ? O3A C9 H9C 145.8 . . ? C10 C9 H9C 103.7 . . ? O3B C9 H9C 103.7 . . ? H9A C9 H9C 65.5 . . ? H9B C9 H9C 48.5 . . ? O3A C9 H9D 75.5 . . ? C10 C9 H9D 103.7 . . ? O3B C9 H9D 103.7 . . ? H9A C9 H9D 40.0 . . ? H9B C9 H9D 141.3 . . ? H9C C9 H9D 105.3 . . ? C9 C10 O4 109.7(4) . . ? C9 C10 H10A 109.7 . . ? O4 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? O4 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C11 O4 C10 115.7(4) . . ? O5 C11 O4 124.0(4) . . ? O5 C11 C14 123.5(4) . . ? O4 C11 C14 112.5(3) . . ? C16 N2 C12 117.0(3) . . ? C16 N2 Ag1 120.0(2) . 3 ? C12 N2 Ag1 122.8(3) . 3 ? N2 C12 C13 123.4(3) . . ? N2 C12 H12 118.3 . . ? C13 C12 H12 118.3 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 118.6(3) . . ? C13 C14 C11 123.6(4) . . ? C15 C14 C11 117.8(4) . . ? C16 C15 C14 118.5(4) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? N2 C16 C15 123.7(4) . . ? N2 C16 H16 118.2 . . ? C15 C16 H16 118.2 . . ? O7 N3 O8 120.0(4) . . ? O7 N3 O6 119.6(4) . . ? O8 N3 O6 120.4(4) . . ? H9E O9 H9F 100(5) . . ? H10E O10 H10F 98(7) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.477 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.076 _chemical_compound_source 'L6 and AgNO3 in Water/THF' _exptl_crystal_recrystallization_method 'Solvent diffusion' # Attachment 'CCDC_678545.cif' data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 678544' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common L6AgNO3 _chemical_melting_point 194 _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Ag2 N6 O16' _chemical_formula_weight 972.38 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9203(14) _cell_length_b 12.156(2) _cell_length_c 12.332(3) _cell_angle_alpha 63.18(3) _cell_angle_beta 87.13(3) _cell_angle_gamma 79.87(3) _cell_volume 910.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 386(2) _cell_measurement_reflns_used 13141 _cell_measurement_theta_min 3.35 _cell_measurement_theta_max 26.87 _exptl_crystal_description 'Rod-like crystal' _exptl_crystal_colour Colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 1.158 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube,12x0.4 mm long-fine focus' _diffrn_source_type 'STOE IPDS II' _diffrn_radiation_monochromator 'plane graphite' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_reflns_number 4389 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 26.87 _reflns_number_total 3074 _reflns_number_gt 2870 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXL97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97, SCHAKAL and PLATON (Spek, 2003)' _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^)+(0.0432P)^2^+0.7474P] 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 3074 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.24274(4) 0.48242(2) 0.037879(19) 0.05434(15) Uani 1 1 d . . . N1 N 0.2674(4) 0.4230(2) 0.2334(2) 0.0400(5) Uani 1 1 d . . . C1 C 0.2576(4) 0.3059(3) 0.3175(3) 0.0379(5) Uani 1 1 d . . . H1 H 0.2519 0.2455 0.2917 0.045 Uiso 1 1 calc R . . C2 C 0.2558(4) 0.2714(2) 0.4403(2) 0.0370(5) Uani 1 1 d . . . H2 H 0.2485 0.1894 0.4960 0.044 Uiso 1 1 calc R . . C3 C 0.2648(4) 0.3605(3) 0.4797(3) 0.0377(5) Uani 1 1 d . . . C4 C 0.2794(6) 0.4804(3) 0.3936(3) 0.0532(8) Uani 1 1 d . . . H4 H 0.2881 0.5421 0.4172 0.064 Uiso 1 1 calc R . . C5 C 0.2810(6) 0.5075(3) 0.2728(3) 0.0520(8) Uani 1 1 d . . . H5 H 0.2920 0.5884 0.2157 0.062 Uiso 1 1 calc R . . C6 C 0.2586(5) 0.3311(3) 0.6110(3) 0.0472(7) Uani 1 1 d . . . O1 O 0.2565(8) 0.4087(3) 0.6456(3) 0.0992(14) Uani 1 1 d . . . O2 O 0.2542(4) 0.2121(2) 0.68272(19) 0.0491(5) Uani 1 1 d . . . C7 C 0.2255(6) 0.1736(4) 0.8119(3) 0.0578(8) Uani 1 1 d . A . H7A H 0.3197 0.0990 0.8593 0.069 Uiso 1 1 calc R . . H7B H 0.2475 0.2393 0.8315 0.069 Uiso 1 1 calc R . . C8 C 0.0307(8) 0.1487(6) 0.8424(4) 0.0840(15) Uani 1 1 d . . . H8A H 0.0252 0.1092 0.9304 0.101 Uiso 0.681(8) 1 calc PR A 1 H8B H -0.0572 0.2287 0.8126 0.101 Uiso 0.681(8) 1 calc PR A 1 H8C H 0.0406 0.0592 0.8720 0.101 Uiso 0.319(8) 1 calc PR A 2 H8D H -0.0002 0.1648 0.9121 0.101 Uiso 0.319(8) 1 calc PR A 2 O3A O -0.0405(5) 0.0796(3) 0.8037(3) 0.0529(11) Uani 0.681(8) 1 d P A 1 O3B O -0.1145(10) 0.1954(5) 0.7767(6) 0.040(2) Uani 0.319(8) 1 d P A 2 C9 C -0.2556(7) 0.1018(6) 0.7994(4) 0.0782(14) Uani 1 1 d . . . H9A H -0.3099 0.1904 0.7643 0.094 Uiso 0.681(8) 1 calc PR A 1 H9B H -0.3083 0.0589 0.8792 0.094 Uiso 0.681(8) 1 calc PR A 1 H9C H -0.2149 0.0317 0.8779 0.094 Uiso 0.319(8) 1 calc PR A 2 H9D H -0.3837 0.1425 0.8101 0.094 Uiso 0.319(8) 1 calc PR A 2 C10 C -0.2894(6) 0.0469(3) 0.7195(3) 0.0592(8) Uani 1 1 d . A . H10A H -0.1954 -0.0294 0.7397 0.071 Uiso 1 1 calc R . . H10B H -0.4205 0.0264 0.7299 0.071 Uiso 1 1 calc R . . O4 O -0.2677(4) 0.1369(2) 0.59456(19) 0.0498(5) Uani 1 1 d . . . O5 O -0.2434(7) -0.0128(2) 0.5373(2) 0.0911(14) Uani 1 1 d . . . C11 C -0.2474(5) 0.0946(3) 0.5129(3) 0.0438(6) Uani 1 1 d . A . N2 N -0.2012(4) 0.3734(2) 0.1496(2) 0.0397(5) Uani 1 1 d . . . C16 C -0.1870(5) 0.2515(3) 0.1770(3) 0.0447(6) Uani 1 1 d . . . H16 H -0.1667 0.2283 0.1145 0.054 Uiso 1 1 calc R . . C15 C -0.2013(5) 0.1604(3) 0.2930(3) 0.0430(6) Uani 1 1 d . A . H15 H -0.1924 0.0774 0.3082 0.052 Uiso 1 1 calc R . . C14 C -0.2293(4) 0.1932(2) 0.3876(2) 0.0341(5) Uani 1 1 d . . . C13 C -0.2398(4) 0.3182(2) 0.3605(2) 0.0349(5) Uani 1 1 d . A . H13 H -0.2556 0.3433 0.4218 0.042 Uiso 1 1 calc R . . C12 C -0.2265(4) 0.4041(2) 0.2417(3) 0.0375(5) Uani 1 1 d . . . H12 H -0.2354 0.4877 0.2242 0.045 Uiso 1 1 calc R A . N3 N 0.4273(5) 0.2415(3) 0.0263(2) 0.0486(6) Uani 1 1 d . . . O6 O 0.2639(5) 0.2490(3) 0.0711(3) 0.0787(9) Uani 1 1 d . . . O7 O 0.4927(5) 0.3395(3) -0.0352(3) 0.0710(7) Uani 1 1 d . . . O8 O 0.5227(6) 0.1392(3) 0.0438(3) 0.0803(9) 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 Ag1 0.0698(2) 0.05279(19) 0.02711(16) -0.00824(11) 0.00238(11) -0.00545(12) N1 0.0457(12) 0.0387(11) 0.0301(11) -0.0106(9) 0.0022(10) -0.0078(10) C1 0.0447(13) 0.0378(12) 0.0319(13) -0.0148(11) 0.0002(11) -0.0113(11) C2 0.0451(14) 0.0338(12) 0.0308(12) -0.0114(10) -0.0002(11) -0.0121(11) C3 0.0437(13) 0.0391(12) 0.0334(13) -0.0178(11) 0.0035(11) -0.0111(11) C4 0.083(2) 0.0369(13) 0.0442(16) -0.0201(13) 0.0110(16) -0.0193(15) C5 0.079(2) 0.0346(13) 0.0395(15) -0.0125(12) 0.0111(16) -0.0159(14) C6 0.0621(18) 0.0503(15) 0.0364(15) -0.0224(13) 0.0056(14) -0.0199(15) O1 0.206(5) 0.0638(16) 0.0516(15) -0.0391(14) 0.016(2) -0.047(2) O2 0.0673(14) 0.0531(11) 0.0304(10) -0.0183(9) 0.0061(10) -0.0215(11) C7 0.072(2) 0.071(2) 0.0282(14) -0.0163(14) -0.0005(15) -0.0228(19) C8 0.085(3) 0.136(4) 0.0390(19) -0.037(3) 0.016(2) -0.049(3) O3A 0.055(2) 0.056(2) 0.049(2) -0.0260(16) 0.0035(16) -0.0082(16) O3B 0.046(4) 0.032(3) 0.032(3) -0.008(2) -0.001(3) -0.002(2) C9 0.064(2) 0.134(4) 0.0354(17) -0.031(2) 0.0101(18) -0.038(3) C10 0.062(2) 0.0599(18) 0.0310(15) -0.0037(14) 0.0076(15) 0.0001(16) O4 0.0691(14) 0.0445(10) 0.0274(10) -0.0099(8) 0.0041(10) -0.0073(10) O5 0.181(4) 0.0354(12) 0.0513(16) -0.0121(12) 0.019(2) -0.0305(19) C11 0.0524(15) 0.0367(13) 0.0365(14) -0.0119(12) 0.0008(13) -0.0062(12) N2 0.0492(12) 0.0380(11) 0.0261(10) -0.0109(9) -0.0006(10) -0.0030(10) C16 0.0603(17) 0.0404(13) 0.0348(14) -0.0210(12) -0.0018(13) 0.0003(13) C15 0.0574(16) 0.0335(12) 0.0399(14) -0.0193(11) -0.0012(13) -0.0035(12) C14 0.0373(12) 0.0311(11) 0.0306(12) -0.0117(10) -0.0015(11) -0.0034(10) C13 0.0418(13) 0.0339(11) 0.0308(12) -0.0167(10) -0.0011(11) -0.0039(10) C12 0.0466(14) 0.0319(11) 0.0318(13) -0.0129(10) -0.0015(11) -0.0047(10) N3 0.0663(16) 0.0487(13) 0.0305(11) -0.0181(11) -0.0001(12) -0.0075(13) O6 0.082(2) 0.0728(17) 0.085(2) -0.0381(17) 0.0314(18) -0.0230(15) O7 0.0726(17) 0.0590(14) 0.0590(16) -0.0056(12) 0.0071(15) -0.0173(13) O8 0.111(2) 0.0564(15) 0.0718(19) -0.0344(15) -0.0009(19) 0.0065(16) _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 Ag1 N2 2.175(3) 2_565 ? Ag1 N1 2.189(2) . ? N1 C5 1.338(4) . ? N1 C1 1.342(4) . ? C1 C2 1.378(4) . ? C1 H1 0.9300 . ? C2 C3 1.383(3) . ? C2 H2 0.9300 . ? C3 C4 1.380(4) . ? C3 C6 1.493(4) . ? C4 C5 1.373(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 O1 1.195(4) . ? C6 O2 1.317(4) . ? O2 C7 1.458(4) . ? C7 C8 1.429(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O3B 1.206(9) . ? C8 O3A 1.307(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? O3A C9 1.464(6) . ? O3B C9 1.549(8) . ? C9 C10 1.464(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C10 O4 1.451(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O4 C11 1.313(4) . ? O5 C11 1.195(4) . ? C11 C14 1.484(4) . ? N2 C12 1.342(4) . ? N2 C16 1.349(4) . ? N2 Ag1 2.175(3) 2_565 ? C16 C15 1.370(4) . ? C16 H16 0.9300 . ? C15 C14 1.389(4) . ? C15 H15 0.9300 . ? C14 C13 1.390(3) . ? C13 C12 1.373(4) . ? C13 H13 0.9300 . ? C12 H12 0.9300 . ? N3 O8 1.230(4) . ? N3 O6 1.240(4) . ? N3 O7 1.241(4) . ? 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 Ag1 N1 151.76(9) 2_565 . ? C5 N1 C1 117.5(2) . . ? C5 N1 Ag1 119.42(18) . . ? C1 N1 Ag1 122.95(18) . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 119.1(2) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 118.3(2) . . ? C4 C3 C6 119.5(2) . . ? C2 C3 C6 122.2(2) . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 123.0(3) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? O1 C6 O2 124.5(3) . . ? O1 C6 C3 122.8(3) . . ? O2 C6 C3 112.7(2) . . ? C6 O2 C7 118.2(2) . . ? C8 C7 O2 110.3(3) . . ? C8 C7 H7A 109.6 . . ? O2 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? O2 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? O3B C8 O3A 62.3(4) . . ? O3B C8 C7 127.1(5) . . ? O3A C8 C7 119.2(4) . . ? O3B C8 H8A 122.7 . . ? O3A C8 H8A 107.5 . . ? C7 C8 H8A 107.5 . . ? O3B C8 H8B 45.4 . . ? O3A C8 H8B 107.5 . . ? C7 C8 H8B 107.5 . . ? H8A C8 H8B 107.0 . . ? O3B C8 H8C 105.5 . . ? O3A C8 H8C 46.3 . . ? C7 C8 H8C 105.5 . . ? H8A C8 H8C 70.8 . . ? H8B C8 H8C 145.7 . . ? O3B C8 H8D 105.5 . . ? O3A C8 H8D 131.4 . . ? C7 C8 H8D 105.5 . . ? H8A C8 H8D 36.2 . . ? H8B C8 H8D 73.5 . . ? H8C C8 H8D 106.1 . . ? C8 O3A C9 112.3(4) . . ? C8 O3B C9 112.8(5) . . ? O3A C9 C10 99.5(4) . . ? O3A C9 O3B 51.1(3) . . ? C10 C9 O3B 126.2(4) . . ? O3A C9 H9A 111.9 . . ? C10 C9 H9A 111.9 . . ? O3B C9 H9A 61.7 . . ? O3A C9 H9B 111.9 . . ? C10 C9 H9B 111.9 . . ? O3B C9 H9B 120.5 . . ? H9A C9 H9B 109.6 . . ? O3A C9 H9C 73.7 . . ? C10 C9 H9C 105.8 . . ? O3B C9 H9C 105.8 . . ? H9A C9 H9C 140.0 . . ? H9B C9 H9C 40.7 . . ? O3A C9 H9D 153.5 . . ? C10 C9 H9D 105.8 . . ? O3B C9 H9D 105.8 . . ? H9A C9 H9D 50.9 . . ? H9B C9 H9D 65.7 . . ? H9C C9 H9D 106.2 . . ? O4 C10 C9 108.6(3) . . ? O4 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O4 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.3 . . ? C11 O4 C10 117.0(3) . . ? O5 C11 O4 123.3(3) . . ? O5 C11 C14 123.4(3) . . ? O4 C11 C14 113.4(2) . . ? C12 N2 C16 117.4(3) . . ? C12 N2 Ag1 120.50(18) . 2_565 ? C16 N2 Ag1 120.87(19) . 2_565 ? N2 C16 C15 122.8(3) . . ? N2 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C16 C15 C14 119.3(2) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C14 C13 118.2(3) . . ? C15 C14 C11 119.2(2) . . ? C13 C14 C11 122.6(2) . . ? C12 C13 C14 118.9(2) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? N2 C12 C13 123.3(2) . . ? N2 C12 H12 118.4 . . ? C13 C12 H12 118.4 . . ? O8 N3 O6 120.7(3) . . ? O8 N3 O7 121.0(3) . . ? O6 N3 O7 118.3(3) . . ? _diffrn_measured_fraction_theta_max 0.782 _diffrn_reflns_theta_full 26.87 _diffrn_measured_fraction_theta_full 0.782 _refine_diff_density_max 0.421 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.045 _chemical_compound_source 'L6 and AgNO3 in THF/Water' _exptl_crystal_recrystallization_method 'Solvent diffusion' # Attachment 'CCDC_678544.cif' data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 678545' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common L6AgNO3 _chemical_melting_point 210 _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Ag2 N6 O16' _chemical_formula_weight 972.38 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' Ag Ag -0.8971 1.1015 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6811(13) _cell_length_b 12.263(3) _cell_length_c 22.585(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.74(3) _cell_angle_gamma 90.00 _cell_volume 1844.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 386(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 27.15 _exptl_crystal_description 'Rod-like crystal' _exptl_crystal_colour Colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 1.144 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed X-ray tube,12x0.4 mm long-fine focus' _diffrn_source_type 'STOE IPDS II' _diffrn_radiation_monochromator 'plane graphite' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_reflns_number 13141 _diffrn_reflns_av_R_equivalents 0.2612 _diffrn_reflns_av_sigmaI/netI 0.2127 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.15 _reflns_number_total 3804 _reflns_number_gt 1360 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXL97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97, SCHAKAL and PLATON (Spek, 2003)' _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^)+(0.0581P)^2^+11.1621P] 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 3804 _refine_ls_number_parameters 239 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2719 _refine_ls_R_factor_gt 0.1237 _refine_ls_wR_factor_ref 0.2764 _refine_ls_wR_factor_gt 0.2162 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.004 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.2453(3) 0.51040(13) 0.00742(5) 0.0780(6) Uani 1 1 d . . . N1 N -0.1427(16) 0.5534(8) 0.0990(3) 0.056(4) Uani 1 1 d G . . C1 C -0.1022(17) 0.4739(7) 0.1422(4) 0.056(5) Uani 1 1 d G . . H1 H -0.1089 0.4005 0.1319 0.068 Uiso 1 1 calc R . . C2 C -0.0516(17) 0.5042(7) 0.2009(3) 0.057(4) Uani 1 1 d G . . H2 H -0.0245 0.4510 0.2298 0.068 Uiso 1 1 calc R . . C3 C -0.0416(17) 0.6139(8) 0.2163(3) 0.053(4) Uani 1 1 d G . . C4 C -0.0821(18) 0.6934(6) 0.1730(4) 0.056(5) Uani 1 1 d G . . H4 H -0.0754 0.7668 0.1834 0.067 Uiso 1 1 calc R . . C5 C -0.1326(17) 0.6631(8) 0.1144(4) 0.067(5) Uani 1 1 d G . . H5 H -0.1597 0.7163 0.0855 0.080 Uiso 1 1 calc R . . C6 C 0.005(3) 0.6507(16) 0.2808(7) 0.060(5) Uani 1 1 d . . . O1 O 0.033(2) 0.7419(11) 0.2921(5) 0.084(4) Uani 1 1 d . . . O2 O 0.016(2) 0.5648(10) 0.3168(4) 0.081(4) Uani 1 1 d . . . C7 C 0.079(5) 0.594(2) 0.3788(8) 0.123(11) Uani 1 1 d . A . H7A H 0.1764 0.6529 0.3799 0.147 Uiso 1 1 calc R . . H7B H -0.0363 0.6188 0.3988 0.147 Uiso 1 1 calc R . . C8 C 0.161(4) 0.504(3) 0.4065(8) 0.124(10) Uani 1 1 d . . . H8A H 0.2423 0.5307 0.4411 0.149 Uiso 0.69(3) 1 calc PR A 1 H8B H 0.0501 0.4647 0.4216 0.149 Uiso 0.69(3) 1 calc PR A 1 H8C H 0.1094 0.4355 0.3899 0.149 Uiso 0.31(3) 1 calc PR A 2 H8D H 0.1581 0.5048 0.4494 0.149 Uiso 0.31(3) 1 calc PR A 2 O3A O 0.275(3) 0.4270(19) 0.3824(7) 0.084(7) Uani 0.69(3) 1 d PU A 1 O3B O 0.380(8) 0.539(4) 0.3836(15) 0.086(15) Uani 0.31(3) 1 d PU A 2 C9 C 0.495(5) 0.453(2) 0.3928(9) 0.121(9) Uani 1 1 d U . . H9A H 0.5262 0.5243 0.3780 0.145 Uiso 0.69(3) 1 calc PR A 1 H9B H 0.5418 0.4473 0.4345 0.145 Uiso 0.69(3) 1 calc PR A 1 H9C H 0.4269 0.4122 0.4222 0.145 Uiso 0.31(3) 1 calc PR A 2 H9D H 0.6138 0.4825 0.4145 0.145 Uiso 0.31(3) 1 calc PR A 2 C10 C 0.574(4) 0.370(2) 0.3594(7) 0.098(7) Uani 1 1 d U A . H10A H 0.5098 0.3010 0.3673 0.118 Uiso 1 1 calc R . . H10B H 0.7169 0.3626 0.3701 0.118 Uiso 1 1 calc R . . O4 O 0.538(2) 0.3975(10) 0.2961(5) 0.086(5) Uani 1 1 d . . . O5 O 0.525(2) 0.2259(12) 0.2677(6) 0.092(5) Uani 1 1 d . . . C11 C 0.518(3) 0.3210(15) 0.2566(8) 0.056(5) Uani 1 1 d . A . N2 N 0.3617(18) 0.4379(9) 0.0815(3) 0.070(5) Uani 1 1 d G . . C12 C 0.3889(17) 0.5116(7) 0.1282(4) 0.052(4) Uani 1 1 d G . . H12 H 0.3749 0.5860 0.1209 0.063 Uiso 1 1 calc R . . C13 C 0.4368(17) 0.4742(7) 0.1857(3) 0.050(4) Uani 1 1 d G A . H13 H 0.4550 0.5236 0.2169 0.060 Uiso 1 1 calc R . . C14 C 0.4577(17) 0.3631(8) 0.1965(3) 0.050(4) Uani 1 1 d G . . C15 C 0.431(2) 0.2893(6) 0.1498(4) 0.072(6) Uani 1 1 d G A . H15 H 0.4445 0.2149 0.1570 0.086 Uiso 1 1 calc R . . C16 C 0.383(2) 0.3267(8) 0.0923(4) 0.078(6) Uani 1 1 d G . . H16 H 0.3644 0.2773 0.0610 0.094 Uiso 1 1 calc R A . N3 N -0.187(3) 0.2625(15) -0.0089(6) 0.084(7) Uani 1 1 d . . . O6 O -0.069(3) 0.3246(13) 0.0230(6) 0.100(5) Uani 1 1 d . . . O7 O -0.352(3) 0.3028(13) -0.0273(6) 0.104(6) Uani 1 1 d . . . O8 O -0.132(3) 0.1710(13) -0.0194(6) 0.123(7) 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 Ag1 0.0848(10) 0.1018(12) 0.0463(6) -0.0019(9) -0.0013(5) -0.0071(13) N1 0.042(10) 0.073(11) 0.057(7) 0.010(7) 0.019(6) 0.012(7) C1 0.031(10) 0.078(14) 0.062(8) -0.004(8) 0.013(7) 0.000(9) C2 0.039(10) 0.074(12) 0.058(7) 0.012(10) 0.009(6) -0.006(11) C3 0.043(12) 0.052(11) 0.065(9) -0.005(8) 0.012(8) -0.010(8) C4 0.059(13) 0.056(11) 0.051(8) 0.007(8) -0.002(8) 0.000(9) C5 0.047(13) 0.069(14) 0.085(12) 0.009(10) 0.012(9) -0.002(10) C6 0.075(14) 0.038(11) 0.063(9) 0.016(8) -0.010(9) -0.007(9) O1 0.124(14) 0.054(9) 0.071(7) -0.007(7) -0.011(7) 0.009(8) O2 0.116(13) 0.077(9) 0.048(6) -0.015(6) -0.010(6) 0.021(8) C7 0.20(3) 0.10(2) 0.058(11) -0.030(12) -0.041(15) 0.028(19) C8 0.17(3) 0.13(2) 0.067(11) -0.029(18) -0.016(14) 0.03(3) O3A 0.070(16) 0.114(17) 0.062(10) -0.003(11) -0.027(10) 0.027(12) O3B 0.09(3) 0.11(3) 0.049(18) 0.019(18) 0.00(2) 0.01(2) C9 0.15(2) 0.14(2) 0.066(12) 0.001(12) -0.012(13) 0.088(18) C10 0.121(19) 0.111(18) 0.060(10) 0.017(11) -0.011(11) 0.015(14) O4 0.137(14) 0.045(8) 0.072(7) 0.009(6) -0.019(8) 0.000(8) O5 0.121(15) 0.067(10) 0.088(9) 0.008(7) 0.004(9) 0.014(9) C11 0.055(13) 0.035(11) 0.080(11) 0.015(9) 0.009(9) 0.006(8) N2 0.070(13) 0.087(12) 0.051(7) 0.016(7) -0.003(7) -0.004(9) C12 0.059(11) 0.054(10) 0.043(6) 0.004(8) 0.004(6) 0.005(10) C13 0.035(10) 0.052(11) 0.065(8) -0.005(7) 0.014(6) -0.005(8) C14 0.027(10) 0.064(12) 0.060(9) -0.003(8) 0.014(7) -0.010(8) C15 0.077(16) 0.076(14) 0.063(10) -0.008(10) 0.010(9) 0.004(11) C16 0.094(18) 0.078(16) 0.062(10) -0.014(10) 0.001(10) -0.016(12) N3 0.15(2) 0.059(11) 0.039(7) -0.011(7) -0.003(9) -0.043(12) O6 0.119(14) 0.109(12) 0.073(8) -0.010(8) 0.004(8) -0.024(10) O7 0.119(15) 0.119(13) 0.070(8) 0.004(8) -0.024(9) 0.005(11) O8 0.22(2) 0.070(10) 0.075(9) 0.002(8) -0.027(10) 0.011(11) _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 Ag1 N2 2.186(6) 3_565 ? Ag1 N1 2.189(6) . ? Ag1 O6 2.576(16) . ? Ag1 Ag1 3.332(3) 3_565 ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 C6 1.534(18) . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 O1 1.158(18) . ? C6 O2 1.328(19) . ? O2 C7 1.473(18) . ? C7 C8 1.37(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O3A 1.35(3) . ? C8 O3B 1.65(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? O3A C9 1.50(3) . ? O3B C9 1.32(5) . ? C9 C10 1.39(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C10 O4 1.469(19) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O4 C11 1.29(2) . ? O5 C11 1.192(18) . ? C11 C14 1.477(17) . ? N2 C12 1.3900 . ? N2 C16 1.3900 . ? N2 Ag1 2.186(6) 3_565 ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? N3 O8 1.21(2) . ? N3 O7 1.24(2) . ? N3 O6 1.277(19) . ? 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 Ag1 N1 149.0(4) 3_565 . ? N2 Ag1 O6 120.4(4) 3_565 . ? N1 Ag1 O6 88.9(4) . . ? N2 Ag1 Ag1 102.0(3) 3_565 3_565 ? N1 Ag1 Ag1 83.1(3) . 3_565 ? O6 Ag1 Ag1 60.2(4) . 3_565 ? C1 N1 C5 120.0 . . ? C1 N1 Ag1 121.5(5) . . ? C5 N1 Ag1 118.3(5) . . ? N1 C1 C2 120.0 . . ? N1 C1 H1 120.0 . . ? C2 C1 H1 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 C6 118.3(9) . . ? C2 C3 C6 121.6(9) . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 H5 120.0 . . ? N1 C5 H5 120.0 . . ? O1 C6 O2 129.2(16) . . ? O1 C6 C3 120.6(14) . . ? O2 C6 C3 110.2(15) . . ? C6 O2 C7 112.5(16) . . ? C8 C7 O2 108.0(17) . . ? C8 C7 H7A 110.1 . . ? O2 C7 H7A 110.1 . . ? C8 C7 H7B 110.1 . . ? O2 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? O3A C8 C7 127(2) . . ? O3A C8 O3B 61(2) . . ? C7 C8 O3B 89(3) . . ? O3A C8 H8A 105.6 . . ? C7 C8 H8A 105.6 . . ? O3B C8 H8A 73.4 . . ? O3A C8 H8B 105.6 . . ? C7 C8 H8B 105.6 . . ? O3B C8 H8B 165.0 . . ? H8A C8 H8B 106.1 . . ? O3A C8 H8C 55.8 . . ? C7 C8 H8C 113.9 . . ? O3B C8 H8C 113.9 . . ? H8A C8 H8C 139.8 . . ? H8B C8 H8C 56.6 . . ? O3A C8 H8D 118.1 . . ? C7 C8 H8D 113.9 . . ? O3B C8 H8D 113.9 . . ? H8A C8 H8D 41.4 . . ? H8B C8 H8D 64.8 . . ? H8C C8 H8D 111.1 . . ? C8 O3A C9 111(2) . . ? C9 O3B C8 105(3) . . ? O3B C9 C10 138(2) . . ? O3B C9 O3A 66(2) . . ? C10 C9 O3A 100(2) . . ? O3B C9 H9A 49.8 . . ? C10 C9 H9A 111.8 . . ? O3A C9 H9A 111.8 . . ? O3B C9 H9B 110.1 . . ? C10 C9 H9B 111.8 . . ? O3A C9 H9B 111.8 . . ? H9A C9 H9B 109.5 . . ? O3B C9 H9C 102.6 . . ? C10 C9 H9C 102.6 . . ? O3A C9 H9C 59.5 . . ? H9A C9 H9C 145.6 . . ? H9B C9 H9C 55.6 . . ? O3B C9 H9D 102.6 . . ? C10 C9 H9D 102.6 . . ? O3A C9 H9D 155.1 . . ? H9A C9 H9D 69.0 . . ? H9B C9 H9D 49.4 . . ? H9C C9 H9D 105.0 . . ? C9 C10 O4 108.7(18) . . ? C9 C10 H10A 110.0 . . ? O4 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? O4 C10 H10B 110.0 . . ? H10A C10 H10B 108.3 . . ? C11 O4 C10 120.2(15) . . ? O5 C11 O4 124.3(16) . . ? O5 C11 C14 122.5(17) . . ? O4 C11 C14 112.7(14) . . ? C12 N2 C16 120.0 . . ? C12 N2 Ag1 121.5(5) . 3_565 ? C16 N2 Ag1 118.0(5) . 3_565 ? N2 C12 C13 120.0 . . ? N2 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 C11 118.6(10) . . ? C13 C14 C11 121.4(10) . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 N2 120.0 . . ? C15 C16 H16 120.0 . . ? N2 C16 H16 120.0 . . ? O8 N3 O7 125.4(17) . . ? O8 N3 O6 118(2) . . ? O7 N3 O6 116.2(19) . . ? N3 O6 Ag1 101.2(14) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.471 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.113 _chemical_compound_source 'L6 and AgNO3 in THF/Water' _exptl_crystal_recrystallization_method 'Solvent diffusion'