# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a #TrackingRef '4-bpy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 Ag2 Cd I2 N4 O9, 2(H2 O)' _chemical_formula_sum 'C36 H28 Ag2 Cd I2 N4 O11' _chemical_formula_weight 1274.58 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' Cd Cd -0.8075 1.2024 '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 'P 21/c' _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 14.0054(3) _cell_length_b 15.1789(3) _cell_length_c 18.5649(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.108(2) _cell_angle_gamma 90.00 _cell_volume 3936.51(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6098 _cell_measurement_theta_min 2.8765 _cell_measurement_theta_max 29.1779 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 3.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.538 _exptl_absorpt_correction_T_max 0.567 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15670 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6934 _reflns_number_gt 5487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0301P)^2^+1.0849P] 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 6923 _refine_ls_number_parameters 510 _refine_ls_number_restraints 1266 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Cd1 Cd -0.74346(3) -0.04280(2) 0.252378(19) 0.02783(10) Uani 1 1 d U . . I2 I -0.57809(3) -0.31975(3) -0.06827(2) 0.05323(13) Uani 1 1 d U . . I1 I -0.90607(3) -0.34651(3) 0.55240(2) 0.05470(14) Uani 1 1 d U . . Ag1 Ag -0.53527(3) 0.02630(3) 0.13609(2) 0.05094(15) Uani 1 1 d U . . Ag2 Ag 0.03203(4) 0.12059(3) 0.59933(2) 0.05841(17) Uani 1 1 d U . . O5 O -0.6126(3) -0.1671(2) 0.26432(19) 0.0437(9) Uani 1 1 d U . . O6 O -0.6574(2) -0.0993(2) 0.16241(18) 0.0363(8) Uani 1 1 d U . . C8 C -0.8544(4) -0.1908(3) 0.2884(3) 0.0338(11) Uani 1 1 d U . . C1 C -0.9367(4) -0.3321(3) 0.4403(3) 0.0320(11) Uani 1 1 d U . . C9 C -0.5667(3) -0.2313(3) 0.1556(3) 0.0272(10) Uani 1 1 d U . . C2 C -1.0104(4) -0.3808(3) 0.4046(3) 0.0356(11) Uani 1 1 d U . . H2 H -1.0463 -0.4198 0.4303 0.043 Uiso 1 1 calc R . . C16 C -0.6153(4) -0.1617(3) 0.1978(3) 0.0318(10) Uani 1 1 d U . . C32 C -0.2055(4) 0.0611(4) 0.3932(3) 0.0359(11) Uani 1 1 d U . . C31 C -0.4140(4) -0.0238(4) 0.2753(3) 0.0427(12) Uani 1 1 d U . . H31 H -0.4600 -0.0678 0.2767 0.051 Uiso 1 1 calc R . . C11 C -0.5438(4) -0.3051(3) 0.0435(3) 0.0325(11) Uani 1 1 d U . . C4 C -0.9771(3) -0.3106(3) 0.2933(3) 0.0322(10) Uani 1 1 d U . . H4 H -0.9898 -0.3042 0.2437 0.039 Uiso 1 1 calc R . . O2 O -0.8513(3) -0.1962(3) 0.2222(2) 0.0531(11) Uani 1 1 d U . . C28 C -0.2808(4) 0.1038(4) 0.2730(3) 0.0416(12) Uani 1 1 d U . . H28 H -0.2365 0.1492 0.2707 0.050 Uiso 1 1 calc R . . C14 C -0.4998(3) -0.2873(3) 0.1907(3) 0.0314(10) Uani 1 1 d U . . H14 H -0.4854 -0.2815 0.2401 0.038 Uiso 1 1 calc R . . C29 C -0.2780(4) 0.0493(4) 0.3324(3) 0.0348(11) Uani 1 1 d U . . N4 N -0.0675(3) 0.0875(3) 0.5083(2) 0.0420(11) Uani 1 1 d U . . C33 C -0.1138(4) 0.0918(4) 0.3825(3) 0.0454(12) Uani 1 1 d U . . H33 H -0.0967 0.1042 0.3360 0.054 Uiso 1 1 calc R . . N3 N -0.4156(3) 0.0283(3) 0.2175(2) 0.0392(10) Uani 1 1 d U . . O1 O -0.8185(3) -0.1286(2) 0.3261(2) 0.0457(9) Uani 1 1 d U . . C5 C -0.9055(3) -0.2601(3) 0.3287(3) 0.0304(11) Uani 1 1 d U . . C6 C -0.8847(4) -0.2723(3) 0.4028(3) 0.0324(11) Uani 1 1 d U . . H6 H -0.8358 -0.2402 0.4270 0.039 Uiso 1 1 calc R . . C3 C -1.0300(3) -0.3705(3) 0.3306(3) 0.0322(11) Uani 1 1 d U . . C36 C -0.2241(4) 0.0427(4) 0.4637(3) 0.0441(12) Uani 1 1 d U . . H36 H -0.2835 0.0205 0.4740 0.053 Uiso 1 1 calc R . . N1 N -0.6177(3) 0.0512(3) 0.0353(2) 0.0519(12) Uani 1 1 d U . . O1W O 0.1726(4) 0.1930(4) 0.5418(3) 0.1109(19) Uani 1 1 d U . . H1WA H 0.1769 0.1782 0.4980 0.166 Uiso 1 1 d R . . H1WB H 0.1688 0.2488 0.5415 0.166 Uiso 1 1 d R . . C10 C -0.5890(3) -0.2407(3) 0.0812(3) 0.0305(11) Uani 1 1 d U . . H10 H -0.6339 -0.2038 0.0574 0.037 Uiso 1 1 calc R . . C12 C -0.4763(4) -0.3607(3) 0.0791(3) 0.0365(11) Uani 1 1 d U . . H12 H -0.4462 -0.4039 0.0532 0.044 Uiso 1 1 calc R . . C30 C -0.3472(4) -0.0153(4) 0.3330(3) 0.0394(12) Uani 1 1 d U . . H30 H -0.3487 -0.0531 0.3723 0.047 Uiso 1 1 calc R . . C34 C -0.0483(4) 0.1039(4) 0.4408(3) 0.0483(13) Uani 1 1 d U . . H34 H 0.0123 0.1247 0.4323 0.058 Uiso 1 1 calc R . . C27 C -0.3493(4) 0.0908(4) 0.2167(3) 0.0418(12) Uani 1 1 d U . . H27 H -0.3492 0.1275 0.1766 0.050 Uiso 1 1 calc R . . O3 O -1.1162(3) -0.4231(3) 0.2249(2) 0.0600(12) Uani 1 1 d U . . C19 C -0.7322(4) 0.0902(4) -0.0910(3) 0.0472(12) Uani 1 1 d U . . C13 C -0.4540(4) -0.3519(3) 0.1526(3) 0.0329(11) Uani 1 1 d U . . C7 C -1.1076(4) -0.4248(4) 0.2916(3) 0.0382(12) Uani 1 1 d U . . C35 C -0.1547(4) 0.0569(4) 0.5188(3) 0.0493(13) Uani 1 1 d U . . H35 H -0.1694 0.0446 0.5658 0.059 Uiso 1 1 calc R . . C20 C -0.6466(4) 0.1301(4) -0.0746(3) 0.0599(14) Uani 1 1 d U . . H20 H -0.6240 0.1718 -0.1060 0.072 Uiso 1 1 calc R . . C21 C -0.5927(4) 0.1092(4) -0.0115(3) 0.0600(14) Uani 1 1 d U . . H21 H -0.5348 0.1384 -0.0019 0.072 Uiso 1 1 calc R . . C18 C -0.7576(5) 0.0285(5) -0.0417(4) 0.0730(15) Uani 1 1 d U . . H18 H -0.8150 -0.0019 -0.0497 0.088 Uiso 1 1 calc R . . C17 C -0.6989(5) 0.0111(5) 0.0196(3) 0.0709(15) Uani 1 1 d U . . H17 H -0.7183 -0.0316 0.0515 0.085 Uiso 1 1 calc R . . O7 O -0.3683(3) -0.4065(3) 0.2584(2) 0.0510(10) Uani 1 1 d U . . O4 O -1.1589(3) -0.4708(3) 0.3290(2) 0.0515(10) Uani 1 1 d U . . C15 C -0.3828(4) -0.4126(4) 0.1916(3) 0.0377(12) Uani 1 1 d U . . O8 O -0.3407(3) -0.4681(2) 0.1540(2) 0.0479(10) Uani 1 1 d U . . C22 C -0.7911(4) 0.1056(4) -0.1593(3) 0.0440(12) Uani 1 1 d U . . C26 C -0.7652(4) 0.1634(4) -0.2111(3) 0.0528(13) Uani 1 1 d U . . H26 H -0.7112 0.1986 -0.2022 0.063 Uiso 1 1 calc R . . C23 C -0.8738(4) 0.0612(5) -0.1769(3) 0.0617(14) Uani 1 1 d U . . H23 H -0.8973 0.0225 -0.1436 0.074 Uiso 1 1 calc R . . C25 C -0.8181(4) 0.1700(4) -0.2762(3) 0.0505(14) Uani 1 1 d U . . H25 H -0.7976 0.2093 -0.3102 0.061 Uiso 1 1 calc R . . C24 C -0.9231(4) 0.0719(5) -0.2426(3) 0.0600(15) Uani 1 1 d U . . H24 H -0.9795 0.0402 -0.2519 0.072 Uiso 1 1 calc R . . N2 N -0.8957(3) 0.1241(3) -0.2932(2) 0.0434(11) Uani 1 1 d U . . O3W O -0.7997(4) -0.8494(4) 0.4004(2) 0.0871(16) Uani 1 1 d . . . H3WA H -0.7642 -0.8944 0.4080 0.131 Uiso 1 1 d R . . H3WB H -0.7652 -0.8052 0.3916 0.131 Uiso 1 1 d R . . O2W O 0.2680(7) 0.3228(6) 0.6167(5) 0.109(2) Uani 0.643(7) 1 d PU A 1 H2WA H 0.2952 0.3455 0.6546 0.164 Uiso 0.643(7) 1 d PR A 1 H2WB H 0.2263 0.3583 0.5981 0.164 Uiso 0.643(7) 1 d PR A 1 O4W O 0.3399(12) 0.2668(11) 0.6359(9) 0.109(2) Uani 0.357(7) 1 d PU A 2 H4WA H 0.3734 0.2834 0.6734 0.164 Uiso 0.357(7) 1 d PR A 2 H4WB H 0.3757 0.2414 0.6071 0.164 Uiso 0.357(7) 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0291(2) 0.0274(2) 0.0268(2) -0.00039(17) 0.00085(15) -0.00151(18) I2 0.0639(3) 0.0644(3) 0.0298(2) -0.0131(2) -0.00797(18) 0.0057(2) I1 0.0725(3) 0.0580(3) 0.0324(2) 0.0111(2) -0.0053(2) -0.0003(2) Ag1 0.0444(3) 0.0725(3) 0.0330(3) 0.0089(2) -0.0176(2) -0.0076(3) Ag2 0.0659(3) 0.0640(3) 0.0404(3) -0.0147(3) -0.0303(2) 0.0158(3) O5 0.0497(19) 0.050(2) 0.0315(18) -0.0019(17) 0.0012(16) 0.0076(18) O6 0.0410(18) 0.0356(18) 0.0327(17) 0.0045(16) 0.0048(15) 0.0033(16) C8 0.033(2) 0.033(2) 0.035(2) 0.002(2) 0.002(2) -0.002(2) C1 0.037(2) 0.027(2) 0.031(2) 0.002(2) -0.003(2) -0.001(2) C9 0.026(2) 0.026(2) 0.029(2) 0.0023(19) -0.0011(18) -0.0014(19) C2 0.037(2) 0.029(2) 0.041(2) 0.005(2) 0.001(2) -0.003(2) C16 0.029(2) 0.037(2) 0.029(2) 0.000(2) -0.0022(19) -0.003(2) C32 0.037(2) 0.040(2) 0.030(2) -0.001(2) -0.0082(19) 0.001(2) C31 0.041(2) 0.051(3) 0.034(2) 0.002(2) -0.010(2) -0.004(2) C11 0.034(2) 0.034(2) 0.028(2) -0.004(2) -0.001(2) -0.001(2) C4 0.033(2) 0.030(2) 0.032(2) -0.003(2) -0.0018(19) 0.001(2) O2 0.062(3) 0.064(3) 0.033(2) 0.007(2) 0.0007(19) -0.017(2) C28 0.042(2) 0.047(3) 0.034(2) 0.004(2) -0.010(2) -0.004(2) C14 0.033(2) 0.032(2) 0.029(2) 0.005(2) -0.0010(19) 0.002(2) C29 0.035(2) 0.042(2) 0.026(2) -0.003(2) -0.0056(19) 0.002(2) N4 0.047(2) 0.045(2) 0.032(2) -0.008(2) -0.015(2) 0.003(2) C33 0.047(3) 0.055(3) 0.032(2) 0.002(2) -0.009(2) -0.005(2) N3 0.035(2) 0.052(2) 0.029(2) 0.000(2) -0.0079(18) -0.002(2) O1 0.058(2) 0.0384(19) 0.042(2) -0.0063(18) 0.0121(18) -0.0154(19) C5 0.033(2) 0.024(2) 0.034(2) -0.003(2) 0.001(2) 0.001(2) C6 0.033(2) 0.026(2) 0.038(2) -0.003(2) -0.003(2) -0.004(2) C3 0.028(2) 0.025(2) 0.042(2) 0.000(2) -0.004(2) -0.002(2) C36 0.046(3) 0.052(3) 0.033(2) -0.006(2) -0.007(2) -0.002(2) N1 0.048(2) 0.067(3) 0.037(2) 0.017(2) -0.015(2) -0.023(2) O1W 0.138(4) 0.133(5) 0.066(3) -0.028(3) 0.030(3) -0.049(4) C10 0.031(2) 0.031(2) 0.028(2) 0.001(2) -0.0037(19) 0.002(2) C12 0.038(2) 0.033(2) 0.039(2) 0.000(2) 0.002(2) 0.005(2) C30 0.044(2) 0.042(2) 0.031(2) 0.006(2) -0.008(2) -0.005(2) C34 0.048(3) 0.058(3) 0.037(3) -0.005(2) -0.013(2) -0.004(3) C27 0.042(3) 0.053(3) 0.030(2) 0.010(2) -0.007(2) 0.000(2) O3 0.055(3) 0.065(3) 0.056(3) -0.005(2) -0.018(2) -0.015(2) C19 0.042(2) 0.063(3) 0.034(2) 0.017(2) -0.012(2) -0.019(2) C13 0.030(2) 0.032(2) 0.036(2) 0.006(2) -0.002(2) 0.001(2) C7 0.035(3) 0.029(2) 0.048(3) 0.000(3) -0.010(2) -0.002(2) C35 0.057(3) 0.058(3) 0.031(2) -0.008(2) -0.011(2) 0.002(3) C20 0.054(3) 0.078(3) 0.044(3) 0.029(3) -0.021(2) -0.033(3) C21 0.051(3) 0.081(3) 0.045(3) 0.022(3) -0.019(2) -0.031(3) C18 0.061(3) 0.096(3) 0.057(3) 0.033(3) -0.025(3) -0.033(3) C17 0.066(3) 0.090(3) 0.054(3) 0.035(3) -0.023(2) -0.032(3) O7 0.043(2) 0.057(2) 0.051(2) 0.017(2) -0.0077(18) 0.011(2) O4 0.048(2) 0.043(2) 0.061(2) 0.004(2) -0.0104(19) -0.020(2) C15 0.030(2) 0.034(2) 0.049(3) 0.009(2) -0.002(2) -0.001(2) O8 0.043(2) 0.036(2) 0.064(2) 0.0014(19) -0.0094(19) 0.0104(18) C22 0.040(2) 0.060(3) 0.031(2) 0.012(2) -0.011(2) -0.016(2) C26 0.045(3) 0.071(3) 0.039(3) 0.014(3) -0.018(2) -0.023(3) C23 0.056(3) 0.083(3) 0.043(3) 0.022(3) -0.016(2) -0.027(3) C25 0.048(3) 0.065(3) 0.037(3) 0.013(3) -0.010(2) -0.013(3) C24 0.048(3) 0.079(3) 0.050(3) 0.013(3) -0.019(2) -0.027(3) N2 0.040(2) 0.053(3) 0.035(2) 0.004(2) -0.014(2) -0.001(2) O3W 0.102(4) 0.108(4) 0.053(3) -0.019(3) 0.015(3) -0.007(3) O2W 0.110(3) 0.109(3) 0.109(3) -0.0010(14) 0.0083(14) -0.0027(14) O4W 0.110(3) 0.109(3) 0.109(3) -0.0010(14) 0.0083(14) -0.0027(14) _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 Cd1 O1 2.208(4) . ? Cd1 O4 2.247(4) 2_355 ? Cd1 O6 2.295(3) . ? Cd1 O8 2.324(4) 2_455 ? Cd1 O7 2.610(4) 2_455 ? Cd1 O5 2.628(4) . ? I2 C11 2.109(5) . ? I1 C1 2.106(5) . ? Ag1 N1 2.160(4) . ? Ag1 N3 2.175(4) . ? Ag2 N4 2.171(4) . ? Ag2 N2 2.173(4) 1_656 ? Ag2 O1W 2.553(5) . ? O5 C16 1.236(6) . ? O6 C16 1.273(6) . ? C8 O2 1.235(6) . ? C8 O1 1.258(6) . ? C8 C5 1.501(7) . ? C1 C6 1.382(7) . ? C1 C2 1.397(7) . ? C9 C14 1.393(6) . ? C9 C10 1.401(6) . ? C9 C16 1.505(7) . ? C2 C3 1.390(7) . ? C2 H2 0.9300 . ? C32 C36 1.381(7) . ? C32 C33 1.394(7) . ? C32 C29 1.474(6) . ? C31 N3 1.331(7) . ? C31 C30 1.378(7) . ? C31 H31 0.9300 . ? C11 C10 1.382(7) . ? C11 C12 1.397(7) . ? C4 C3 1.389(7) . ? C4 C5 1.390(7) . ? C4 H4 0.9300 . ? C28 C29 1.378(7) . ? C28 C27 1.381(7) . ? C28 H28 0.9300 . ? C14 C13 1.392(7) . ? C14 H14 0.9300 . ? C29 C30 1.378(7) . ? N4 C34 1.324(7) . ? N4 C35 1.333(7) . ? C33 C34 1.380(7) . ? C33 H33 0.9300 . ? N3 C27 1.328(7) . ? C5 C6 1.399(7) . ? C6 H6 0.9300 . ? C3 C7 1.508(7) . ? C36 C35 1.376(7) . ? C36 H36 0.9300 . ? N1 C21 1.301(7) . ? N1 C17 1.305(7) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? C10 H10 0.9300 . ? C12 C13 1.385(7) . ? C12 H12 0.9300 . ? C30 H30 0.9300 . ? C34 H34 0.9300 . ? C27 H27 0.9300 . ? O3 C7 1.236(6) . ? C19 C20 1.359(7) . ? C19 C18 1.374(8) . ? C19 C22 1.480(7) . ? C13 C15 1.504(7) . ? C7 O4 1.248(6) . ? C35 H35 0.9300 . ? C20 C21 1.385(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C18 C17 1.382(8) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? O7 C15 1.245(6) . ? O7 Cd1 2.610(4) 2_445 ? O4 Cd1 2.247(4) 2_345 ? C15 O8 1.267(6) . ? O8 Cd1 2.324(4) 2_445 ? C22 C23 1.360(7) . ? C22 C26 1.371(7) . ? C26 C25 1.375(7) . ? C26 H26 0.9300 . ? C23 C24 1.368(7) . ? C23 H23 0.9300 . ? C25 N2 1.310(7) . ? C25 H25 0.9300 . ? C24 N2 1.306(7) . ? C24 H24 0.9300 . ? N2 Ag2 2.173(4) 1_454 ? O3W H3WA 0.8499 . ? O3W H3WB 0.8500 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8500 . ? O4W H2WA 1.4036 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? 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 O1 Cd1 O4 114.15(15) . 2_355 ? O1 Cd1 O6 121.92(13) . . ? O4 Cd1 O6 91.08(14) 2_355 . ? O1 Cd1 O8 93.58(14) . 2_455 ? O4 Cd1 O8 121.15(14) 2_355 2_455 ? O6 Cd1 O8 117.49(13) . 2_455 ? O1 Cd1 O7 146.00(13) . 2_455 ? O4 Cd1 O7 84.43(13) 2_355 2_455 ? O6 Cd1 O7 83.75(12) . 2_455 ? O8 Cd1 O7 52.84(13) 2_455 2_455 ? O1 Cd1 O5 83.38(13) . . ? O4 Cd1 O5 142.45(13) 2_355 . ? O6 Cd1 O5 52.68(11) . . ? O8 Cd1 O5 88.48(12) 2_455 . ? O7 Cd1 O5 99.01(12) 2_455 . ? N1 Ag1 N3 159.49(18) . . ? N4 Ag2 N2 162.06(19) . 1_656 ? N4 Ag2 O1W 104.21(18) . . ? N2 Ag2 O1W 92.94(18) 1_656 . ? C16 O5 Cd1 84.1(3) . . ? C16 O6 Cd1 98.7(3) . . ? O2 C8 O1 124.2(5) . . ? O2 C8 C5 120.0(5) . . ? O1 C8 C5 115.8(5) . . ? C6 C1 C2 120.5(5) . . ? C6 C1 I1 119.2(4) . . ? C2 C1 I1 120.3(4) . . ? C14 C9 C10 119.6(5) . . ? C14 C9 C16 120.0(4) . . ? C10 C9 C16 120.4(4) . . ? C3 C2 C1 119.7(5) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? O5 C16 O6 123.0(5) . . ? O5 C16 C9 119.4(5) . . ? O6 C16 C9 117.6(4) . . ? C36 C32 C33 116.2(5) . . ? C36 C32 C29 122.3(5) . . ? C33 C32 C29 121.5(5) . . ? N3 C31 C30 122.9(5) . . ? N3 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C10 C11 C12 120.5(5) . . ? C10 C11 I2 119.5(4) . . ? C12 C11 I2 120.0(4) . . ? C3 C4 C5 121.2(5) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C29 C28 C27 119.9(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C13 C14 C9 120.8(5) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? C30 C29 C28 117.0(5) . . ? C30 C29 C32 121.8(5) . . ? C28 C29 C32 121.2(5) . . ? C34 N4 C35 117.0(5) . . ? C34 N4 Ag2 122.0(4) . . ? C35 N4 Ag2 120.7(4) . . ? C34 C33 C32 119.9(6) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C27 N3 C31 117.5(4) . . ? C27 N3 Ag1 120.4(3) . . ? C31 N3 Ag1 121.3(4) . . ? C8 O1 Cd1 106.7(3) . . ? C4 C5 C6 118.9(5) . . ? C4 C5 C8 120.3(5) . . ? C6 C5 C8 120.7(4) . . ? C1 C6 C5 120.2(5) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C4 C3 C2 119.5(5) . . ? C4 C3 C7 120.7(5) . . ? C2 C3 C7 119.8(5) . . ? C35 C36 C32 120.1(6) . . ? C35 C36 H36 120.0 . . ? C32 C36 H36 120.0 . . ? C21 N1 C17 116.0(5) . . ? C21 N1 Ag1 123.0(4) . . ? C17 N1 Ag1 121.0(4) . . ? Ag2 O1W H1WA 113.4 . . ? Ag2 O1W H1WB 112.6 . . ? H1WA O1W H1WB 105.4 . . ? C11 C10 C9 119.5(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C13 C12 C11 120.3(5) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C31 C30 C29 119.9(5) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? N4 C34 C33 123.3(6) . . ? N4 C34 H34 118.3 . . ? C33 C34 H34 118.4 . . ? N3 C27 C28 122.8(5) . . ? N3 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C20 C19 C18 114.9(5) . . ? C20 C19 C22 123.3(5) . . ? C18 C19 C22 121.6(5) . . ? C12 C13 C14 119.3(5) . . ? C12 C13 C15 120.7(5) . . ? C14 C13 C15 120.0(5) . . ? O3 C7 O4 123.4(5) . . ? O3 C7 C3 119.0(5) . . ? O4 C7 C3 117.6(5) . . ? N4 C35 C36 123.5(6) . . ? N4 C35 H35 118.2 . . ? C36 C35 H35 118.2 . . ? C19 C20 C21 120.4(6) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? N1 C21 C20 124.3(6) . . ? N1 C21 H21 117.8 . . ? C20 C21 H21 117.8 . . ? C19 C18 C17 120.9(6) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? N1 C17 C18 123.5(6) . . ? N1 C17 H17 118.3 . . ? C18 C17 H17 118.3 . . ? C15 O7 Cd1 85.5(3) . 2_445 ? C7 O4 Cd1 104.2(3) . 2_345 ? O7 C15 O8 123.3(5) . . ? O7 C15 C13 119.3(5) . . ? O8 C15 C13 117.4(5) . . ? C15 O8 Cd1 98.2(3) . 2_445 ? C23 C22 C26 114.3(5) . . ? C23 C22 C19 122.7(5) . . ? C26 C22 C19 122.9(5) . . ? C22 C26 C25 120.7(5) . . ? C22 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C22 C23 C24 121.5(6) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? N2 C25 C26 124.0(6) . . ? N2 C25 H25 118.0 . . ? C26 C25 H25 118.0 . . ? N2 C24 C23 123.9(6) . . ? N2 C24 H24 118.1 . . ? C23 C24 H24 118.1 . . ? C24 N2 C25 115.5(5) . . ? C24 N2 Ag2 120.2(4) . 1_454 ? C25 N2 Ag2 123.9(4) . 1_454 ? H3WA O3W H3WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? H2WA O4W H4WA 76.9 . . ? H2WA O4W H4WB 146.6 . . ? H4WA O4W H4WB 109.6 . . ? 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 O1 Cd1 O5 C16 132.3(3) . . . . ? O4 Cd1 O5 C16 10.6(4) 2_355 . . . ? O6 Cd1 O5 C16 -7.0(3) . . . . ? O8 Cd1 O5 C16 -133.9(3) 2_455 . . . ? O7 Cd1 O5 C16 -82.0(3) 2_455 . . . ? O1 Cd1 O6 C16 -42.9(3) . . . . ? O4 Cd1 O6 C16 -162.5(3) 2_355 . . . ? O8 Cd1 O6 C16 71.1(3) 2_455 . . . ? O7 Cd1 O6 C16 113.2(3) 2_455 . . . ? O5 Cd1 O6 C16 6.8(3) . . . . ? C6 C1 C2 C3 1.6(8) . . . . ? I1 C1 C2 C3 179.9(4) . . . . ? Cd1 O5 C16 O6 12.0(5) . . . . ? Cd1 O5 C16 C9 -168.1(4) . . . . ? Cd1 O6 C16 O5 -13.9(5) . . . . ? Cd1 O6 C16 C9 166.3(4) . . . . ? C14 C9 C16 O5 -16.5(7) . . . . ? C10 C9 C16 O5 163.1(5) . . . . ? C14 C9 C16 O6 163.4(4) . . . . ? C10 C9 C16 O6 -17.1(7) . . . . ? C10 C9 C14 C13 0.6(7) . . . . ? C16 C9 C14 C13 -179.8(4) . . . . ? C27 C28 C29 C30 -1.5(8) . . . . ? C27 C28 C29 C32 179.8(5) . . . . ? C36 C32 C29 C30 -31.4(8) . . . . ? C33 C32 C29 C30 148.6(6) . . . . ? C36 C32 C29 C28 147.2(6) . . . . ? C33 C32 C29 C28 -32.8(8) . . . . ? N2 Ag2 N4 C34 -161.4(5) 1_656 . . . ? O1W Ag2 N4 C34 1.1(5) . . . . ? N2 Ag2 N4 C35 24.8(8) 1_656 . . . ? O1W Ag2 N4 C35 -172.6(4) . . . . ? C36 C32 C33 C34 -1.4(8) . . . . ? C29 C32 C33 C34 178.6(5) . . . . ? C30 C31 N3 C27 -0.3(8) . . . . ? C30 C31 N3 Ag1 -169.9(4) . . . . ? N1 Ag1 N3 C27 22.8(8) . . . . ? N1 Ag1 N3 C31 -167.8(5) . . . . ? O2 C8 O1 Cd1 -4.4(6) . . . . ? C5 C8 O1 Cd1 177.2(3) . . . . ? O4 Cd1 O1 C8 68.1(4) 2_355 . . . ? O6 Cd1 O1 C8 -39.5(4) . . . . ? O8 Cd1 O1 C8 -165.3(3) 2_455 . . . ? O7 Cd1 O1 C8 -173.5(3) 2_455 . . . ? O5 Cd1 O1 C8 -77.2(3) . . . . ? C3 C4 C5 C6 2.1(7) . . . . ? C3 C4 C5 C8 -175.2(5) . . . . ? O2 C8 C5 C4 -23.7(7) . . . . ? O1 C8 C5 C4 154.8(5) . . . . ? O2 C8 C5 C6 159.0(5) . . . . ? O1 C8 C5 C6 -22.5(7) . . . . ? C2 C1 C6 C5 -0.1(8) . . . . ? I1 C1 C6 C5 -178.4(4) . . . . ? C4 C5 C6 C1 -1.8(7) . . . . ? C8 C5 C6 C1 175.6(5) . . . . ? C5 C4 C3 C2 -0.6(8) . . . . ? C5 C4 C3 C7 179.9(5) . . . . ? C1 C2 C3 C4 -1.3(8) . . . . ? C1 C2 C3 C7 178.2(5) . . . . ? C33 C32 C36 C35 1.7(8) . . . . ? C29 C32 C36 C35 -178.4(5) . . . . ? N3 Ag1 N1 C21 -13.6(9) . . . . ? N3 Ag1 N1 C17 169.7(5) . . . . ? C12 C11 C10 C9 0.0(8) . . . . ? I2 C11 C10 C9 179.6(4) . . . . ? C14 C9 C10 C11 -0.3(7) . . . . ? C16 C9 C10 C11 -179.8(5) . . . . ? C10 C11 C12 C13 0.1(8) . . . . ? I2 C11 C12 C13 -179.5(4) . . . . ? N3 C31 C30 C29 0.0(9) . . . . ? C28 C29 C30 C31 0.9(8) . . . . ? C32 C29 C30 C31 179.6(5) . . . . ? C35 N4 C34 C33 0.7(9) . . . . ? Ag2 N4 C34 C33 -173.3(4) . . . . ? C32 C33 C34 N4 0.2(9) . . . . ? C31 N3 C27 C28 -0.4(8) . . . . ? Ag1 N3 C27 C28 169.4(4) . . . . ? C29 C28 C27 N3 1.3(9) . . . . ? C11 C12 C13 C14 0.3(8) . . . . ? C11 C12 C13 C15 178.8(5) . . . . ? C9 C14 C13 C12 -0.6(8) . . . . ? C9 C14 C13 C15 -179.1(5) . . . . ? C4 C3 C7 O3 8.4(8) . . . . ? C2 C3 C7 O3 -171.1(5) . . . . ? C4 C3 C7 O4 -172.9(5) . . . . ? C2 C3 C7 O4 7.6(8) . . . . ? C34 N4 C35 C36 -0.4(9) . . . . ? Ag2 N4 C35 C36 173.6(4) . . . . ? C32 C36 C35 N4 -0.8(9) . . . . ? C18 C19 C20 C21 -1.3(10) . . . . ? C22 C19 C20 C21 -176.5(6) . . . . ? C17 N1 C21 C20 0.6(11) . . . . ? Ag1 N1 C21 C20 -176.3(6) . . . . ? C19 C20 C21 N1 0.7(12) . . . . ? C20 C19 C18 C17 0.7(11) . . . . ? C22 C19 C18 C17 176.0(7) . . . . ? C21 N1 C17 C18 -1.2(11) . . . . ? Ag1 N1 C17 C18 175.7(6) . . . . ? C19 C18 C17 N1 0.6(13) . . . . ? O3 C7 O4 Cd1 1.3(7) . . . 2_345 ? C3 C7 O4 Cd1 -177.4(4) . . . 2_345 ? Cd1 O7 C15 O8 -3.8(5) 2_445 . . . ? Cd1 O7 C15 C13 176.0(4) 2_445 . . . ? C12 C13 C15 O7 -175.8(5) . . . . ? C14 C13 C15 O7 2.7(8) . . . . ? C12 C13 C15 O8 4.0(7) . . . . ? C14 C13 C15 O8 -177.6(5) . . . . ? O7 C15 O8 Cd1 4.3(6) . . . 2_445 ? C13 C15 O8 Cd1 -175.5(4) . . . 2_445 ? C20 C19 C22 C23 175.8(7) . . . . ? C18 C19 C22 C23 0.9(11) . . . . ? C20 C19 C22 C26 -1.6(11) . . . . ? C18 C19 C22 C26 -176.6(7) . . . . ? C23 C22 C26 C25 -3.2(10) . . . . ? C19 C22 C26 C25 174.4(6) . . . . ? C26 C22 C23 C24 2.6(10) . . . . ? C19 C22 C23 C24 -175.1(7) . . . . ? C22 C26 C25 N2 0.9(11) . . . . ? C22 C23 C24 N2 0.4(12) . . . . ? C23 C24 N2 C25 -2.8(10) . . . . ? C23 C24 N2 Ag2 170.6(6) . . . 1_454 ? C26 C25 N2 C24 2.1(9) . . . . ? C26 C25 N2 Ag2 -171.0(5) . . . 1_454 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.922 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.105 _database_code_depnum_ccdc_archive 'CCDC 918615' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '5-phen.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H22 Ag2 Cd I2 N4 O8, H2 O' _chemical_formula_sum 'C40 H24 Ag2 Cd I2 N4 O9' _chemical_formula_weight 1286.58 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' Cd Cd -0.8075 1.2024 '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 'P 21/c' _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 15.7940(5) _cell_length_b 13.4071(6) _cell_length_c 17.8147(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.021(3) _cell_angle_gamma 90.00 _cell_volume 3767.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4734 _cell_measurement_theta_min 2.9788 _cell_measurement_theta_max 29.1599 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 3.292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.506 _exptl_absorpt_correction_T_max 0.535 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14285 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6627 _reflns_number_gt 5375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0223P)^2^+125.4739P] 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 6616 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 C17 C 1.2851(8) 0.3308(10) -0.2997(6) 0.048(3) Uani 1 1 d . . . H17 H 1.2529 0.2864 -0.3294 0.058 Uiso 1 1 calc R . . C18 C 1.3338(10) 0.3989(11) -0.3330(8) 0.070(4) Uani 1 1 d . . . H18 H 1.3352 0.3995 -0.3851 0.084 Uiso 1 1 calc R . . C19 C 1.3799(9) 0.4654(10) -0.2931(8) 0.061(4) Uani 1 1 d . . . H19 H 1.4133 0.5114 -0.3170 0.073 Uiso 1 1 calc R . . C20 C 1.3774(7) 0.4652(9) -0.2130(7) 0.048(3) Uani 1 1 d . . . C21 C 1.3273(6) 0.3910(8) -0.1833(5) 0.031(2) Uani 1 1 d . . . C25 C 1.3245(6) 0.3849(8) -0.1016(6) 0.037(3) Uani 1 1 d . . . C22 C 1.4236(8) 0.5329(10) -0.1663(9) 0.063(4) Uani 1 1 d . . . H22 H 1.4586 0.5798 -0.1874 0.075 Uiso 1 1 calc R . . C23 C 1.4178(9) 0.5302(10) -0.0929(8) 0.060(4) Uani 1 1 d . . . H23 H 1.4459 0.5783 -0.0634 0.072 Uiso 1 1 calc R . . C24 C 1.3697(7) 0.4561(8) -0.0577(7) 0.042(3) Uani 1 1 d . . . C26 C 1.3668(8) 0.4455(11) 0.0227(8) 0.068(4) Uani 1 1 d . . . H26 H 1.3940 0.4917 0.0545 0.081 Uiso 1 1 calc R . . C27 C 1.3247(8) 0.3685(11) 0.0512(7) 0.055(4) Uani 1 1 d . . . H27 H 1.3246 0.3591 0.1029 0.066 Uiso 1 1 calc R . . C28 C 1.2814(8) 0.3035(10) 0.0029(7) 0.054(4) Uani 1 1 d . . . H28 H 1.2515 0.2518 0.0241 0.065 Uiso 1 1 calc R . . N1 N 1.2824(6) 0.3259(7) -0.2235(5) 0.038(2) Uani 1 1 d . . . N2 N 1.2794(5) 0.3090(7) -0.0713(5) 0.040(2) Uani 1 1 d . . . Ag1 Ag 1.20464(6) 0.20767(8) -0.15078(5) 0.0522(3) Uani 1 1 d . . . I2 I 0.45598(5) -0.16865(6) -0.07529(4) 0.0464(2) Uani 1 1 d . . . C13 C 0.4746(6) -0.2011(8) 0.0411(5) 0.029(2) Uani 1 1 d . . . I1 I 1.04104(5) 0.16028(7) -0.06043(4) 0.0511(2) Uani 1 1 d . . . Cd1 Cd 0.74651(4) 0.01316(5) 0.26068(4) 0.02392(16) Uani 1 1 d . . . Ag2 Ag 0.70157(6) 0.23038(8) 0.13086(6) 0.0592(3) Uani 1 1 d . . . N3 N 0.7885(6) 0.3285(8) 0.0636(5) 0.045(3) Uani 1 1 d . . . N4 N 0.7735(5) 0.3417(7) 0.2160(5) 0.040(2) Uani 1 1 d . . . C36 C 0.8711(7) 0.4823(9) 0.2213(7) 0.049(3) Uani 1 1 d . . . C37 C 0.8240(6) 0.4091(7) 0.1805(6) 0.030(2) Uani 1 1 d . . . C32 C 0.8789(7) 0.4729(9) 0.0628(7) 0.047(3) Uani 1 1 d . . . C33 C 0.8305(6) 0.4034(8) 0.1015(6) 0.036(3) Uani 1 1 d . . . C29 C 0.8000(8) 0.3205(12) -0.0113(7) 0.062(4) Uani 1 1 d . . . H29 H 0.7731 0.2681 -0.0370 0.075 Uiso 1 1 calc R . . O2 O 0.8714(4) 0.1245(6) 0.2678(4) 0.041(2) Uani 1 1 d . . . O1 O 0.8074(4) 0.0923(6) 0.1584(4) 0.0400(19) Uani 1 1 d . . . O6 O 0.6200(4) -0.1073(5) 0.2711(4) 0.0390(19) Uani 1 1 d . . . O5 O 0.6783(4) -0.0723(5) 0.1639(4) 0.0375(19) Uani 1 1 d . . . C9 C 0.6206(6) -0.1142(7) 0.2007(5) 0.028(2) Uani 1 1 d . . . C1 C 0.8678(7) 0.1311(8) 0.2002(6) 0.035(3) Uani 1 1 d . . . C3 C 0.9384(6) 0.1815(8) 0.1592(6) 0.030(2) Uani 1 1 d . . . C4 C 0.9911(6) 0.2490(7) 0.1982(5) 0.026(2) Uani 1 1 d . . . H4 H 0.9822 0.2635 0.2482 0.031 Uiso 1 1 calc R . . C12 C 0.5393(7) -0.1521(8) 0.0792(6) 0.039(3) Uani 1 1 d . . . H12 H 0.5738 -0.1082 0.0544 0.046 Uiso 1 1 calc R . . C11 C 0.5525(5) -0.1694(7) 0.1563(5) 0.027(2) Uani 1 1 d . . . C40 C 0.7743(8) 0.3412(10) 0.2895(7) 0.052(3) Uani 1 1 d . . . H40 H 0.7444 0.2919 0.3135 0.062 Uiso 1 1 calc R . . C16 C 0.4986(6) -0.2338(7) 0.1918(5) 0.027(2) Uani 1 1 d . . . H16 H 0.5056 -0.2430 0.2435 0.032 Uiso 1 1 calc R . . C15 C 0.4353(6) -0.2841(7) 0.1523(5) 0.030(2) Uani 1 1 d . . . C35 C 0.9187(9) 0.5517(11) 0.1821(10) 0.075(5) Uani 1 1 d . . . H35 H 0.9489 0.6007 0.2092 0.090 Uiso 1 1 calc R . . C31 C 0.8834(9) 0.4616(13) -0.0139(8) 0.080(5) Uani 1 1 d . . . H31 H 0.9118 0.5095 -0.0408 0.096 Uiso 1 1 calc R . . C39 C 0.8191(11) 0.4131(12) 0.3333(8) 0.075(5) Uani 1 1 d . . . H39 H 0.8160 0.4142 0.3853 0.091 Uiso 1 1 calc R . . C30 C 0.8476(9) 0.3829(13) -0.0510(8) 0.074(5) Uani 1 1 d . . . H30 H 0.8555 0.3722 -0.1018 0.088 Uiso 1 1 calc R . . C34 C 0.9221(10) 0.5498(10) 0.1084(11) 0.082(5) Uani 1 1 d . . . H34 H 0.9528 0.5988 0.0848 0.099 Uiso 1 1 calc R . . C38 C 0.8666(9) 0.4802(11) 0.2981(8) 0.066(4) Uani 1 1 d . . . H38 H 0.8974 0.5269 0.3268 0.079 Uiso 1 1 calc R . . C10 C 0.3772(6) -0.3519(7) 0.1935(6) 0.030(2) Uani 1 1 d . . . C14 C 0.4232(6) -0.2683(8) 0.0754(6) 0.031(2) Uani 1 1 d . . . H14 H 0.3811 -0.3025 0.0475 0.038 Uiso 1 1 calc R . . C2 C 1.1165(6) 0.3658(7) 0.2061(6) 0.028(2) Uani 1 1 d . . . C8 C 0.9504(7) 0.1598(8) 0.0869(6) 0.036(3) Uani 1 1 d . . . H8 H 0.9131 0.1178 0.0599 0.043 Uiso 1 1 calc R . . C6 C 1.0709(6) 0.2704(7) 0.0878(5) 0.029(2) Uani 1 1 d . . . H6 H 1.1141 0.3009 0.0626 0.034 Uiso 1 1 calc R . . C5 C 1.0566(6) 0.2945(7) 0.1632(6) 0.029(2) Uani 1 1 d . . . O4 O 1.1081(4) 0.3776(5) 0.2748(4) 0.0364(18) Uani 1 1 d . . . O3 O 1.1729(4) 0.4072(5) 0.1688(4) 0.0340(18) Uani 1 1 d . . . O7 O 0.3207(4) -0.3973(5) 0.1530(4) 0.0317(17) Uani 1 1 d . . . O8 O 0.3850(5) -0.3612(6) 0.2617(4) 0.041(2) Uani 1 1 d . . . C7 C 1.0198(6) 0.2013(8) 0.0533(6) 0.036(3) Uani 1 1 d . . . O1W O 0.7395(10) 0.9946(15) 0.0180(7) 0.157(7) Uani 1 1 d . . . H1WA H 0.7398 0.9344 0.0328 0.188 Uiso 1 1 d R . . H1WB H 0.7772 1.0274 0.0433 0.235 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C17 0.059(7) 0.054(7) 0.032(6) 0.000(6) 0.005(5) 0.013(6) C18 0.095(10) 0.074(10) 0.044(7) 0.008(7) 0.023(7) 0.020(9) C19 0.073(9) 0.041(7) 0.070(9) 0.020(7) 0.014(7) -0.002(7) C20 0.049(7) 0.038(6) 0.057(7) -0.001(6) 0.010(6) 0.002(5) C21 0.034(5) 0.032(5) 0.029(5) -0.003(4) 0.006(4) 0.002(4) C25 0.027(5) 0.039(6) 0.047(6) -0.008(5) 0.012(4) -0.001(5) C22 0.049(7) 0.041(7) 0.098(11) 0.008(8) 0.002(7) -0.004(6) C23 0.067(8) 0.044(7) 0.069(9) -0.016(7) 0.000(7) -0.002(7) C24 0.035(5) 0.035(6) 0.055(7) -0.013(5) -0.016(5) 0.008(5) C26 0.054(8) 0.085(10) 0.063(8) -0.048(8) -0.009(6) 0.009(7) C27 0.061(7) 0.077(9) 0.027(6) -0.015(6) 0.010(5) 0.001(7) C28 0.064(8) 0.063(8) 0.038(6) -0.009(6) 0.011(6) -0.006(7) N1 0.042(5) 0.041(5) 0.032(5) -0.005(4) 0.004(4) 0.003(4) N2 0.038(5) 0.050(6) 0.033(5) -0.011(4) 0.007(4) 0.002(4) Ag1 0.0500(5) 0.0564(6) 0.0503(5) -0.0155(5) 0.0037(4) -0.0166(5) I2 0.0508(4) 0.0615(5) 0.0264(3) 0.0089(3) -0.0026(3) -0.0264(4) C13 0.028(5) 0.044(6) 0.016(4) 0.005(4) -0.002(4) -0.007(4) I1 0.0577(4) 0.0630(5) 0.0337(4) -0.0131(4) 0.0132(3) -0.0230(4) Cd1 0.0233(3) 0.0270(3) 0.0215(3) -0.0010(3) 0.0017(3) -0.0005(3) Ag2 0.0476(5) 0.0551(6) 0.0733(7) 0.0011(5) -0.0123(5) -0.0165(5) N3 0.037(5) 0.053(6) 0.043(5) -0.001(5) -0.008(4) 0.003(5) N4 0.036(5) 0.044(5) 0.041(5) 0.006(5) 0.002(4) -0.005(4) C36 0.049(7) 0.041(6) 0.056(7) -0.005(6) 0.008(6) 0.007(6) C37 0.024(5) 0.027(5) 0.038(6) -0.001(4) -0.005(4) 0.005(4) C32 0.042(6) 0.037(6) 0.061(8) 0.018(6) -0.011(5) 0.009(5) C33 0.030(5) 0.032(6) 0.047(6) 0.010(5) -0.002(5) 0.008(4) C29 0.043(7) 0.104(12) 0.039(7) -0.008(7) -0.016(5) 0.010(7) O2 0.040(4) 0.055(5) 0.029(4) 0.007(4) 0.008(3) -0.009(4) O1 0.031(4) 0.048(4) 0.042(4) -0.005(4) 0.006(3) -0.011(3) O6 0.041(4) 0.041(4) 0.034(4) -0.004(3) -0.006(3) -0.008(3) O5 0.029(4) 0.037(4) 0.046(4) -0.008(4) 0.005(3) -0.009(3) C9 0.023(5) 0.031(5) 0.029(5) 0.006(4) -0.001(4) -0.006(4) C1 0.040(6) 0.027(5) 0.039(6) 0.011(5) 0.000(5) -0.004(5) C3 0.020(4) 0.035(5) 0.036(5) 0.005(5) 0.004(4) 0.007(4) C4 0.028(5) 0.030(5) 0.019(5) -0.001(4) 0.001(4) 0.004(4) C12 0.051(6) 0.034(6) 0.032(6) 0.000(5) 0.005(5) -0.020(5) C11 0.015(4) 0.034(5) 0.032(5) -0.005(4) -0.002(4) 0.002(4) C40 0.056(7) 0.057(8) 0.042(7) 0.002(6) -0.005(6) -0.006(6) C16 0.036(5) 0.027(5) 0.016(4) -0.004(4) -0.001(4) 0.002(4) C15 0.041(5) 0.029(5) 0.022(5) -0.002(4) 0.008(4) -0.004(4) C35 0.052(8) 0.053(8) 0.119(13) -0.023(9) 0.001(8) -0.020(7) C31 0.059(8) 0.112(12) 0.068(9) 0.062(9) 0.004(7) 0.021(8) C39 0.112(12) 0.081(11) 0.034(7) -0.003(7) 0.006(8) 0.014(10) C30 0.072(9) 0.114(13) 0.033(7) 0.016(8) -0.016(6) 0.011(9) C34 0.080(10) 0.036(7) 0.134(14) 0.013(9) 0.046(10) -0.011(7) C38 0.067(8) 0.058(8) 0.070(9) -0.023(8) -0.024(7) 0.012(7) C10 0.030(5) 0.020(5) 0.040(6) -0.003(4) 0.012(4) -0.008(4) C14 0.030(5) 0.033(5) 0.031(5) -0.001(5) 0.001(4) -0.005(4) C2 0.028(5) 0.021(5) 0.035(5) 0.002(4) 0.003(4) 0.006(4) C8 0.042(6) 0.036(6) 0.028(5) -0.007(5) 0.004(4) -0.017(5) C6 0.023(5) 0.033(5) 0.030(5) 0.011(4) 0.000(4) 0.002(4) C5 0.027(5) 0.023(5) 0.037(5) 0.005(4) 0.000(4) 0.006(4) O4 0.040(4) 0.037(4) 0.032(4) -0.001(3) -0.001(3) 0.000(3) O3 0.032(4) 0.040(4) 0.031(4) -0.002(3) 0.001(3) -0.012(3) O7 0.025(3) 0.040(4) 0.030(4) 0.010(3) -0.001(3) -0.015(3) O8 0.061(5) 0.047(4) 0.017(3) 0.007(3) 0.012(3) -0.006(4) C7 0.035(5) 0.038(6) 0.036(6) -0.008(5) 0.011(4) -0.001(5) O1W 0.151(13) 0.25(2) 0.070(9) -0.033(11) 0.003(8) 0.008(14) _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 C17 C18 1.351(19) . ? C17 N1 1.362(14) . ? C18 C19 1.33(2) . ? C19 C20 1.429(18) . ? C20 C21 1.393(15) . ? C20 C22 1.410(18) . ? C21 N1 1.314(13) . ? C21 C25 1.461(14) . ? C25 N2 1.369(14) . ? C25 C24 1.404(15) . ? C22 C23 1.31(2) . ? C23 C24 1.417(18) . ? C24 C26 1.442(18) . ? C26 C27 1.342(19) . ? C27 C28 1.380(17) . ? C28 N2 1.322(14) . ? N1 Ag1 2.422(9) . ? N2 Ag1 2.252(9) . ? Ag1 O4 2.275(7) 4_565 ? Ag1 I1 3.1795(12) . ? I2 C13 2.123(9) . ? I2 Ag2 2.7564(12) 3_655 ? C13 C12 1.365(14) . ? C13 C14 1.377(14) . ? I1 C7 2.143(10) . ? Cd1 O3 2.247(7) 2_745 ? Cd1 O7 2.259(6) 2_655 ? Cd1 O5 2.292(7) . ? Cd1 O1 2.357(7) . ? Cd1 O2 2.472(7) . ? Cd1 O6 2.584(7) . ? Ag2 N3 2.286(10) . ? Ag2 N4 2.373(9) . ? Ag2 O1 2.525(8) . ? Ag2 I2 2.7564(12) 3_655 ? N3 C29 1.360(15) . ? N3 C33 1.362(14) . ? N4 C40 1.309(15) . ? N4 C37 1.382(13) . ? C36 C38 1.374(19) . ? C36 C35 1.404(19) . ? C36 C37 1.410(15) . ? C37 C33 1.419(15) . ? C32 C31 1.379(19) . ? C32 C33 1.408(16) . ? C32 C34 1.46(2) . ? C29 C30 1.35(2) . ? O2 C1 1.207(12) . ? O1 C1 1.287(12) . ? O6 C9 1.257(12) . ? O5 C9 1.281(11) . ? C9 C11 1.498(13) . ? C1 C3 1.523(14) . ? C3 C8 1.344(14) . ? C3 C4 1.390(13) . ? C4 C5 1.377(13) . ? C12 C11 1.398(14) . ? C11 C16 1.387(13) . ? C40 C39 1.408(19) . ? C16 C15 1.369(13) . ? C15 C14 1.390(13) . ? C15 C10 1.510(13) . ? C35 C34 1.32(2) . ? C31 C30 1.35(2) . ? C39 C38 1.35(2) . ? C10 O8 1.221(12) . ? C10 O7 1.273(11) . ? C2 O4 1.248(12) . ? C2 O3 1.268(11) . ? C2 C5 1.522(13) . ? C8 C7 1.393(14) . ? C6 C7 1.354(14) . ? C6 C5 1.412(14) . ? O4 Ag1 2.275(7) 4_566 ? O3 Cd1 2.247(7) 2_755 ? O7 Cd1 2.259(6) 2_645 ? 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 C18 C17 N1 121.2(12) . . ? C19 C18 C17 121.7(13) . . ? C18 C19 C20 119.3(13) . . ? C21 C20 C22 121.5(12) . . ? C21 C20 C19 115.3(11) . . ? C22 C20 C19 123.2(12) . . ? N1 C21 C20 124.6(10) . . ? N1 C21 C25 117.6(9) . . ? C20 C21 C25 117.8(10) . . ? N2 C25 C24 123.1(10) . . ? N2 C25 C21 118.5(9) . . ? C24 C25 C21 118.4(10) . . ? C23 C22 C20 120.5(13) . . ? C22 C23 C24 121.8(12) . . ? C25 C24 C23 119.9(11) . . ? C25 C24 C26 116.3(11) . . ? C23 C24 C26 123.7(11) . . ? C27 C26 C24 119.6(12) . . ? C26 C27 C28 119.2(12) . . ? N2 C28 C27 124.9(12) . . ? C21 N1 C17 117.9(10) . . ? C21 N1 Ag1 114.7(7) . . ? C17 N1 Ag1 127.5(8) . . ? C28 N2 C25 116.7(10) . . ? C28 N2 Ag1 125.4(8) . . ? C25 N2 Ag1 117.9(7) . . ? N2 Ag1 O4 169.4(3) . 4_565 ? N2 Ag1 N1 71.2(3) . . ? O4 Ag1 N1 111.1(3) 4_565 . ? N2 Ag1 I1 102.4(2) . . ? O4 Ag1 I1 69.95(18) 4_565 . ? N1 Ag1 I1 148.2(2) . . ? C13 I2 Ag2 111.4(3) . 3_655 ? C12 C13 C14 122.4(9) . . ? C12 C13 I2 116.7(7) . . ? C14 C13 I2 120.9(7) . . ? C7 I1 Ag1 126.8(3) . . ? O3 Cd1 O7 103.2(2) 2_745 2_655 ? O3 Cd1 O5 109.6(3) 2_745 . ? O7 Cd1 O5 124.0(2) 2_655 . ? O3 Cd1 O1 118.3(2) 2_745 . ? O7 Cd1 O1 120.8(3) 2_655 . ? O5 Cd1 O1 80.7(2) . . ? O3 Cd1 O2 85.7(3) 2_745 . ? O7 Cd1 O2 92.7(2) 2_655 . ? O5 Cd1 O2 133.1(2) . . ? O1 Cd1 O2 53.9(2) . . ? O3 Cd1 O6 89.0(2) 2_745 . ? O7 Cd1 O6 83.7(2) 2_655 . ? O5 Cd1 O6 53.6(2) . . ? O1 Cd1 O6 133.3(2) . . ? O2 Cd1 O6 172.8(2) . . ? N3 Ag2 N4 72.1(3) . . ? N3 Ag2 O1 96.5(3) . . ? N4 Ag2 O1 92.7(3) . . ? N3 Ag2 I2 122.7(2) . 3_655 ? N4 Ag2 I2 144.2(2) . 3_655 ? O1 Ag2 I2 115.20(16) . 3_655 ? C29 N3 C33 117.2(11) . . ? C29 N3 Ag2 125.7(9) . . ? C33 N3 Ag2 117.1(7) . . ? C40 N4 C37 119.0(10) . . ? C40 N4 Ag2 128.0(8) . . ? C37 N4 Ag2 112.8(7) . . ? C38 C36 C35 124.5(13) . . ? C38 C36 C37 116.4(12) . . ? C35 C36 C37 119.1(12) . . ? N4 C37 C36 121.4(10) . . ? N4 C37 C33 119.5(9) . . ? C36 C37 C33 119.1(10) . . ? C31 C32 C33 118.1(12) . . ? C31 C32 C34 125.5(13) . . ? C33 C32 C34 116.4(12) . . ? N3 C33 C32 120.5(11) . . ? N3 C33 C37 118.2(10) . . ? C32 C33 C37 121.3(10) . . ? C30 C29 N3 125.0(14) . . ? C1 O2 Cd1 89.8(6) . . ? C1 O1 Cd1 93.2(6) . . ? C1 O1 Ag2 106.2(6) . . ? Cd1 O1 Ag2 100.8(3) . . ? C9 O6 Cd1 85.9(6) . . ? C9 O5 Cd1 98.8(6) . . ? O6 C9 O5 121.5(9) . . ? O6 C9 C11 121.3(8) . . ? O5 C9 C11 117.2(8) . . ? O2 C1 O1 122.8(10) . . ? O2 C1 C3 120.9(9) . . ? O1 C1 C3 116.2(9) . . ? C8 C3 C4 120.6(9) . . ? C8 C3 C1 120.4(9) . . ? C4 C3 C1 119.0(9) . . ? C5 C4 C3 120.4(9) . . ? C13 C12 C11 118.6(9) . . ? C16 C11 C12 119.2(8) . . ? C16 C11 C9 120.5(8) . . ? C12 C11 C9 120.2(9) . . ? N4 C40 C39 122.1(12) . . ? C15 C16 C11 121.4(9) . . ? C16 C15 C14 119.3(9) . . ? C16 C15 C10 119.5(8) . . ? C14 C15 C10 121.1(9) . . ? C34 C35 C36 122.2(13) . . ? C30 C31 C32 121.8(14) . . ? C38 C39 C40 118.3(13) . . ? C29 C30 C31 117.2(13) . . ? C35 C34 C32 121.8(13) . . ? C39 C38 C36 122.5(13) . . ? O8 C10 O7 123.1(9) . . ? O8 C10 C15 120.9(9) . . ? O7 C10 C15 116.0(9) . . ? C13 C14 C15 119.0(9) . . ? O4 C2 O3 125.0(9) . . ? O4 C2 C5 118.5(9) . . ? O3 C2 C5 116.5(9) . . ? C3 C8 C7 118.6(9) . . ? C7 C6 C5 117.8(9) . . ? C4 C5 C6 119.4(9) . . ? C4 C5 C2 120.8(9) . . ? C6 C5 C2 119.7(9) . . ? C2 O4 Ag1 114.0(6) . 4_566 ? C2 O3 Cd1 112.1(6) . 2_755 ? C10 O7 Cd1 102.0(6) . 2_645 ? C6 C7 C8 122.9(10) . . ? C6 C7 I1 119.0(7) . . ? C8 C7 I1 118.0(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.157 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.197 _database_code_depnum_ccdc_archive 'CCDC 918616' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef '2-bbi.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H10 Ag2 I N O4' _chemical_formula_sum 'C14 H10 Ag2 I N O4 ' _chemical_formula_weight 598.87 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' 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 'C 2/c' _symmetry_space_group_name_Hall '-c 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.0990(17) _cell_length_b 8.7015(3) _cell_length_c 15.0839(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.468(8) _cell_angle_gamma 90.00 _cell_volume 3066.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2596 _cell_measurement_theta_min 3.0111 _cell_measurement_theta_max 29.1672 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240.0 _exptl_absorpt_coefficient_mu 4.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.416 _exptl_absorpt_correction_T_max 0.438 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6301 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2702 _reflns_number_gt 2285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0379P)^2^+16.5156P] 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 2697 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 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 Ag1 Ag 0.35625(3) 0.66314(9) 0.22528(5) 0.0742(3) Uani 1 1 d . . . Ag2 Ag 0.48973(2) 1.51210(6) 0.08909(4) 0.04878(19) Uani 1 1 d . . . O3 O 0.4469(2) 1.2927(5) 0.0250(3) 0.0437(11) Uani 1 1 d . . . N1 N 0.2991(3) 0.5935(7) 0.2849(4) 0.0446(14) Uani 1 1 d . . . C9 C 0.3114(3) 0.5809(8) 0.3792(5) 0.0411(16) Uani 1 1 d . . . H9 H 0.3476 0.5986 0.4305 0.049 Uiso 1 1 calc R . . C10 C 0.2666(2) 0.5402(6) 0.3933(4) 0.0231(12) Uani 1 1 d . . . C6 C 0.4138(2) 0.9870(6) 0.0075(4) 0.0285(13) Uani 1 1 d . . . H6 H 0.4120 1.0447 0.0580 0.034 Uiso 1 1 calc R . . C5 C 0.4272(2) 1.0588(7) -0.0612(4) 0.0283(13) Uani 1 1 d . . . C8 C 0.4443(2) 1.2246(7) -0.0493(5) 0.0323(14) Uani 1 1 d . . . C11 C 0.2216(3) 0.5258(9) 0.3021(5) 0.0522(19) Uani 1 1 d . . . H11 H 0.1844 0.4988 0.2884 0.063 Uiso 1 1 calc R . . C12 C 0.2411(3) 0.5580(10) 0.2355(5) 0.056(2) Uani 1 1 d . . . H12 H 0.2193 0.5567 0.1672 0.068 Uiso 1 1 calc R . . C1 C 0.4029(3) 0.8309(7) 0.0026(4) 0.0289(13) Uani 1 1 d . . . C2 C 0.4036(2) 0.7456(7) -0.0752(4) 0.0294(13) Uani 1 1 d . . . H2 H 0.3961 0.6407 -0.0798 0.035 Uiso 1 1 calc R . . C14 C 0.2366(3) 0.6758(8) 0.5056(5) 0.0451(17) Uani 1 1 d . . . H14A H 0.1962 0.6764 0.4594 0.054 Uiso 1 1 calc R . . H14B H 0.2396 0.6712 0.5720 0.054 Uiso 1 1 calc R . . C4 C 0.4280(2) 0.9735(7) -0.1389(4) 0.0309(14) Uani 1 1 d . . . H4 H 0.4369 1.0202 -0.1859 0.037 Uiso 1 1 calc R . . C13 C 0.2641(3) 0.5323(9) 0.4875(5) 0.0466(18) Uani 1 1 d . . . H13A H 0.3026 0.5212 0.5406 0.056 Uiso 1 1 calc R . . H13B H 0.2423 0.4426 0.4882 0.056 Uiso 1 1 calc R . . O2 O 0.4031(2) 0.6115(6) 0.0966(3) 0.0476(12) Uani 1 1 d . . . C3 C 0.4155(3) 0.8180(7) -0.1450(4) 0.0302(13) Uani 1 1 d . . . O4 O 0.4552(2) 1.2839(5) -0.1154(3) 0.0495(13) Uani 1 1 d . . . C7 C 0.3911(3) 0.7501(8) 0.0806(4) 0.0354(14) Uani 1 1 d . . . O1 O 0.3686(2) 0.8296(6) 0.1241(4) 0.0531(13) Uani 1 1 d . . . I1 I 0.41650(2) 0.68486(5) -0.26131(3) 0.04251(16) 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 0.0972(6) 0.0919(6) 0.0528(4) -0.0121(3) 0.0508(4) -0.0392(4) Ag2 0.0537(4) 0.0293(3) 0.0684(4) -0.0044(2) 0.0318(3) -0.0087(2) O3 0.057(3) 0.023(2) 0.055(3) -0.008(2) 0.028(3) -0.008(2) N1 0.053(4) 0.051(4) 0.038(3) 0.005(3) 0.027(3) 0.008(3) C9 0.037(4) 0.043(4) 0.042(4) -0.001(3) 0.017(3) 0.007(3) C10 0.018(3) 0.028(3) 0.026(3) 0.000(2) 0.012(2) 0.001(2) C6 0.033(3) 0.023(3) 0.031(3) -0.002(2) 0.015(3) 0.001(3) C5 0.028(3) 0.022(3) 0.032(3) 0.002(2) 0.011(3) 0.000(2) C8 0.026(3) 0.027(3) 0.036(3) 0.002(3) 0.007(3) 0.001(3) C11 0.039(4) 0.062(5) 0.056(5) -0.011(4) 0.021(4) -0.005(4) C12 0.045(4) 0.078(6) 0.036(4) -0.008(4) 0.009(4) 0.006(4) C1 0.029(3) 0.026(3) 0.034(3) -0.001(2) 0.016(3) -0.001(3) C2 0.034(3) 0.026(3) 0.029(3) 0.002(3) 0.015(3) 0.001(3) C14 0.047(4) 0.049(4) 0.051(4) 0.009(3) 0.033(4) 0.005(3) C4 0.030(3) 0.034(4) 0.030(3) 0.003(3) 0.015(3) 0.000(3) C13 0.048(4) 0.054(5) 0.045(4) 0.012(3) 0.027(3) 0.002(3) O2 0.063(3) 0.039(3) 0.056(3) 0.011(2) 0.040(3) -0.001(2) C3 0.035(3) 0.031(3) 0.026(3) -0.003(2) 0.014(3) 0.001(3) O4 0.064(3) 0.032(3) 0.044(3) 0.006(2) 0.016(3) -0.016(2) C7 0.041(4) 0.038(4) 0.031(3) 0.000(3) 0.020(3) -0.005(3) O1 0.076(4) 0.051(3) 0.059(3) 0.002(2) 0.053(3) 0.006(3) I1 0.0532(3) 0.0488(3) 0.0285(2) -0.00333(18) 0.0209(2) 0.0072(2) _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 N1 2.145(6) . ? Ag1 O1 2.229(5) . ? Ag2 O4 2.206(4) 5_685 ? Ag2 O3 2.206(4) . ? Ag2 O2 2.470(5) 1_565 ? Ag2 Ag2 2.9731(12) 5_685 ? Ag2 I1 3.1636(8) 5_675 ? O3 C8 1.243(7) . ? N1 C9 1.316(8) . ? N1 C12 1.390(9) . ? C9 C10 1.325(8) . ? C10 C11 1.359(9) . ? C10 C13 1.453(8) . ? C6 C1 1.383(8) . ? C6 C5 1.382(8) . ? C5 C4 1.397(8) . ? C5 C8 1.497(8) . ? C8 O4 1.263(8) . ? C11 C12 1.342(11) . ? C1 C2 1.395(8) . ? C1 C7 1.515(8) . ? C2 C3 1.376(8) . ? C14 C14 1.513(13) 7_566 ? C14 C13 1.525(9) . ? C4 C3 1.385(8) . ? O2 C7 1.242(8) . ? O2 Ag2 2.470(5) 1_545 ? C3 I1 2.113(6) . ? O4 Ag2 2.206(4) 5_685 ? C7 O1 1.264(8) . ? I1 Ag2 3.1636(8) 5_675 ? 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 Ag1 O1 144.1(2) . . ? O4 Ag2 O3 159.67(19) 5_685 . ? O4 Ag2 O2 104.26(18) 5_685 1_565 ? O3 Ag2 O2 91.58(17) . 1_565 ? O4 Ag2 Ag2 81.61(13) 5_685 5_685 ? O3 Ag2 Ag2 78.64(13) . 5_685 ? O2 Ag2 Ag2 127.14(11) 1_565 5_685 ? O4 Ag2 I1 94.85(12) 5_685 5_675 ? O3 Ag2 I1 86.93(12) . 5_675 ? O2 Ag2 I1 122.75(11) 1_565 5_675 ? Ag2 Ag2 I1 108.59(3) 5_685 5_675 ? C8 O3 Ag2 128.4(4) . . ? C9 N1 C12 104.1(6) . . ? C9 N1 Ag1 126.6(5) . . ? C12 N1 Ag1 129.2(5) . . ? N1 C9 C10 112.8(6) . . ? C9 C10 C11 106.7(6) . . ? C9 C10 C13 126.6(6) . . ? C11 C10 C13 126.2(6) . . ? C1 C6 C5 121.3(6) . . ? C6 C5 C4 119.5(5) . . ? C6 C5 C8 120.5(5) . . ? C4 C5 C8 119.8(5) . . ? O3 C8 O4 125.2(6) . . ? O3 C8 C5 117.4(6) . . ? O4 C8 C5 117.4(6) . . ? C12 C11 C10 107.1(6) . . ? C11 C12 N1 109.3(6) . . ? C6 C1 C2 119.2(5) . . ? C6 C1 C7 121.5(5) . . ? C2 C1 C7 119.3(5) . . ? C3 C2 C1 119.5(6) . . ? C14 C14 C13 113.6(7) 7_566 . ? C3 C4 C5 118.8(6) . . ? C10 C13 C14 111.5(6) . . ? C7 O2 Ag2 119.2(4) . 1_545 ? C2 C3 C4 121.6(5) . . ? C2 C3 I1 118.4(4) . . ? C4 C3 I1 120.0(4) . . ? C8 O4 Ag2 123.0(4) . 5_685 ? O2 C7 O1 124.5(6) . . ? O2 C7 C1 118.7(6) . . ? O1 C7 C1 116.8(6) . . ? C7 O1 Ag1 104.0(4) . . ? C3 I1 Ag2 84.64(16) . 5_675 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.402 _refine_diff_density_min -1.365 _refine_diff_density_rms 0.130 _database_code_depnum_ccdc_archive 'CCDC 917684' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '1-bpa.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H15 Ag2 I N2 O4' _chemical_formula_sum 'C20 H15 Ag2 I N2 O4' _chemical_formula_weight 689.98 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2367(9) _cell_length_b 9.3456(8) _cell_length_c 13.4445(11) _cell_angle_alpha 88.897(7) _cell_angle_beta 71.282(8) _cell_angle_gamma 67.893(8) _cell_volume 1011.53(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2314 _cell_measurement_theta_min 3.0083 _cell_measurement_theta_max 29.2026 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 3.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.485 _exptl_absorpt_correction_T_max 0.515 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7642 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3565 _reflns_number_gt 2849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0258P)^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 3565 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 I1 I 0.17000(4) 0.23489(5) 0.48570(3) 0.04929(13) Uani 1 1 d . . . Ag1 Ag 0.98768(4) 0.11390(5) -0.07403(3) 0.03997(13) Uani 1 1 d . . . Ag2 Ag 1.19365(5) 0.27902(5) -0.01515(3) 0.05036(15) Uani 1 1 d . . . N1 N 1.0286(5) 0.2399(5) 0.1320(3) 0.0378(10) Uani 1 1 d . . . N2 N 1.3864(5) 0.2536(5) -0.1666(3) 0.0387(10) Uani 1 1 d . . . C2 C 1.4593(6) 0.2286(7) -0.3538(4) 0.0456(14) Uani 1 1 d . . . H2 H 1.4318 0.2125 -0.4122 0.055 Uiso 1 1 calc R . . C3 C 1.6067(6) 0.2472(6) -0.3688(4) 0.0414(13) Uani 1 1 d . . . C7 C 1.0758(6) 0.1252(6) 0.1907(4) 0.0428(13) Uani 1 1 d . . . H7 H 1.1841 0.0511 0.1660 0.051 Uiso 1 1 calc R . . C4 C 1.6409(6) 0.2648(7) -0.2790(4) 0.0456(14) Uani 1 1 d . . . H4 H 1.7393 0.2751 -0.2845 0.055 Uiso 1 1 calc R . . C10 C 0.7620(6) 0.3415(6) 0.2661(4) 0.0448(14) Uani 1 1 d . . . H10 H 0.6558 0.4195 0.2900 0.054 Uiso 1 1 calc R . . C11 C 0.8742(6) 0.3444(6) 0.1700(4) 0.0411(13) Uani 1 1 d . . . H11 H 0.8395 0.4240 0.1298 0.049 Uiso 1 1 calc R . . C1 C 1.3543(6) 0.2334(6) -0.2547(4) 0.0395(13) Uani 1 1 d . . . H1 H 1.2557 0.2222 -0.2478 0.047 Uiso 1 1 calc R . . C9 C 0.8073(7) 0.2236(6) 0.3262(4) 0.0411(13) Uani 1 1 d . . . C5 C 1.5315(6) 0.2673(6) -0.1809(4) 0.0423(13) Uani 1 1 d . . . H5 H 1.5590 0.2790 -0.1217 0.051 Uiso 1 1 calc R . . O1 O 0.7148(4) 0.1818(4) 0.0091(3) 0.0471(10) Uani 1 1 d . . . C12 C 0.6863(7) 0.2136(8) 0.4297(4) 0.0542(16) Uani 1 1 d . . . H12A H 0.5756 0.2865 0.4358 0.065 Uiso 1 1 calc R . . H1B H 0.6860 0.1099 0.4297 0.065 Uiso 1 1 calc R . . C8 C 0.9685(7) 0.1135(7) 0.2871(4) 0.0459(14) Uani 1 1 d . . . H8 H 1.0049 0.0318 0.3254 0.055 Uiso 1 1 calc R . . C19 C 0.3818(5) 0.3583(5) 0.1296(4) 0.0277(11) Uani 1 1 d . . . H19 H 0.4219 0.3811 0.0610 0.033 Uiso 1 1 calc R . . C14 C 0.4836(6) 0.2351(5) 0.1661(4) 0.0298(11) Uani 1 1 d . . . C13 C 0.6639(6) 0.1422(6) 0.0987(4) 0.0319(11) Uani 1 1 d . . . C6 C 1.7256(8) 0.2476(9) -0.4770(4) 0.069(2) Uani 1 1 d . . . H6B H 1.7320 0.3489 -0.4802 0.082 Uiso 1 1 calc R . . H6A H 1.8351 0.1719 -0.4830 0.082 Uiso 1 1 calc R . . O2 O 0.7477(4) 0.0369(4) 0.1414(3) 0.0433(9) Uani 1 1 d . . . C17 C 0.1628(5) 0.4138(5) 0.2952(4) 0.0325(11) Uani 1 1 d . . . H17 H 0.0566 0.4754 0.3399 0.039 Uiso 1 1 calc R . . C18 C 0.2203(5) 0.4488(5) 0.1936(4) 0.0260(10) Uani 1 1 d . . . C20 C 0.1109(5) 0.5890(6) 0.1553(4) 0.0304(11) Uani 1 1 d . . . C15 C 0.4228(6) 0.1967(6) 0.2669(4) 0.0332(12) Uani 1 1 d . . . H15 H 0.4886 0.1114 0.2912 0.040 Uiso 1 1 calc R . . C16 C 0.2624(6) 0.2875(6) 0.3306(4) 0.0325(11) Uani 1 1 d . . . O4 O 0.0383(4) 0.7123(4) 0.2153(3) 0.0429(9) Uani 1 1 d . . . O3 O 0.1002(4) 0.5675(4) 0.0662(3) 0.0460(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 I1 0.0358(2) 0.0711(3) 0.0298(2) 0.01599(19) -0.00611(16) -0.01365(19) Ag1 0.0235(2) 0.0406(2) 0.0389(3) 0.01046(19) -0.00227(18) -0.00168(18) Ag2 0.0517(3) 0.0657(3) 0.0231(2) -0.0002(2) 0.00823(19) -0.0287(2) N1 0.046(3) 0.040(3) 0.019(2) 0.003(2) -0.001(2) -0.018(2) N2 0.032(2) 0.046(3) 0.025(2) 0.000(2) 0.0007(19) -0.010(2) C2 0.039(3) 0.084(4) 0.019(3) 0.005(3) -0.006(2) -0.032(3) C3 0.035(3) 0.063(4) 0.021(3) 0.002(3) 0.001(2) -0.022(3) C7 0.042(3) 0.043(3) 0.030(3) -0.001(3) -0.004(3) -0.008(3) C4 0.032(3) 0.075(4) 0.028(3) -0.006(3) -0.003(2) -0.024(3) C10 0.038(3) 0.043(3) 0.036(3) -0.001(3) 0.002(3) -0.009(3) C11 0.049(3) 0.037(3) 0.022(3) 0.005(2) 0.000(2) -0.011(3) C1 0.028(3) 0.057(4) 0.030(3) 0.004(3) -0.002(2) -0.018(3) C9 0.048(3) 0.049(3) 0.024(3) 0.005(3) -0.004(2) -0.023(3) C5 0.037(3) 0.057(4) 0.029(3) 0.001(3) -0.009(2) -0.017(3) O1 0.0202(19) 0.066(3) 0.032(2) 0.0049(19) 0.0034(16) -0.0016(18) C12 0.059(4) 0.075(4) 0.021(3) 0.009(3) -0.004(3) -0.027(3) C8 0.056(4) 0.050(4) 0.026(3) 0.015(3) -0.011(3) -0.018(3) C19 0.023(3) 0.032(3) 0.019(3) 0.002(2) -0.001(2) -0.006(2) C14 0.029(3) 0.030(3) 0.022(3) 0.000(2) -0.001(2) -0.010(2) C13 0.023(3) 0.031(3) 0.032(3) -0.002(2) -0.002(2) -0.005(2) C6 0.058(4) 0.131(7) 0.025(3) 0.008(4) 0.000(3) -0.057(4) O2 0.0216(18) 0.037(2) 0.049(2) 0.0072(18) 0.0004(17) 0.0022(16) C17 0.015(2) 0.033(3) 0.032(3) -0.004(2) -0.002(2) 0.005(2) C18 0.022(2) 0.026(2) 0.026(3) 0.000(2) -0.007(2) -0.006(2) C20 0.018(2) 0.035(3) 0.032(3) 0.007(2) -0.007(2) -0.006(2) C15 0.025(3) 0.033(3) 0.035(3) 0.010(2) -0.011(2) -0.003(2) C16 0.028(3) 0.040(3) 0.021(3) 0.004(2) -0.004(2) -0.009(2) O4 0.035(2) 0.033(2) 0.049(2) 0.0001(19) -0.0144(18) 0.0003(17) O3 0.051(2) 0.041(2) 0.037(2) 0.0078(18) -0.0184(19) -0.0045(18) _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 I1 C16 2.110(5) . ? Ag1 O2 2.194(3) 2_755 ? Ag1 O1 2.241(3) . ? Ag1 O4 2.486(3) 2_665 ? Ag1 Ag1 2.8827(8) 2_755 ? Ag1 Ag2 3.1386(6) . ? Ag2 N2 2.179(4) . ? Ag2 N1 2.197(4) . ? N1 C11 1.323(6) . ? N1 C7 1.341(6) . ? N2 C1 1.343(6) . ? N2 C5 1.346(6) . ? C2 C1 1.363(7) . ? C2 C3 1.387(6) . ? C2 H2 0.9300 . ? C3 C4 1.369(7) . ? C3 C6 1.517(7) . ? C7 C8 1.388(7) . ? C7 H7 0.9300 . ? C4 C5 1.375(7) . ? C4 H4 0.9300 . ? C10 C9 1.371(7) . ? C10 C11 1.379(7) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C1 H1 0.9300 . ? C9 C8 1.385(7) . ? C9 C12 1.507(7) . ? C5 H5 0.9300 . ? O1 C13 1.249(6) . ? C12 C6 1.484(8) 1_456 ? C12 H12A 0.9700 . ? C12 H1B 0.9700 . ? C8 H8 0.9300 . ? C19 C14 1.382(6) . ? C19 C18 1.391(6) . ? C19 H19 0.9300 . ? C14 C15 1.388(6) . ? C14 C13 1.524(6) . ? C13 O2 1.260(6) . ? C6 C12 1.484(8) 1_654 ? C6 H6B 0.9700 . ? C6 H6A 0.9700 . ? O2 Ag1 2.194(3) 2_755 ? C17 C18 1.379(6) . ? C17 C16 1.382(6) . ? C17 H17 0.9300 . ? C18 C20 1.521(6) . ? C20 O4 1.240(6) . ? C20 O3 1.258(6) . ? C15 C16 1.384(6) . ? C15 H15 0.9300 . ? O4 Ag1 2.486(3) 2_665 ? 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 O2 Ag1 O1 158.62(13) 2_755 . ? O2 Ag1 O4 99.81(12) 2_755 2_665 ? O1 Ag1 O4 96.43(12) . 2_665 ? O2 Ag1 Ag1 79.50(9) 2_755 2_755 ? O1 Ag1 Ag1 82.66(10) . 2_755 ? O4 Ag1 Ag1 172.94(8) 2_665 2_755 ? O2 Ag1 Ag2 71.47(9) 2_755 . ? O1 Ag1 Ag2 123.26(10) . . ? O4 Ag1 Ag2 87.67(8) 2_665 . ? Ag1 Ag1 Ag2 98.70(2) 2_755 . ? N2 Ag2 N1 165.43(15) . . ? N2 Ag2 Ag1 101.97(11) . . ? N1 Ag2 Ag1 71.65(10) . . ? C11 N1 C7 117.3(4) . . ? C11 N1 Ag2 117.5(3) . . ? C7 N1 Ag2 124.9(3) . . ? C1 N2 C5 116.2(4) . . ? C1 N2 Ag2 117.6(3) . . ? C5 N2 Ag2 126.0(3) . . ? C1 C2 C3 121.0(5) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 115.9(4) . . ? C4 C3 C6 120.9(4) . . ? C2 C3 C6 123.2(5) . . ? N1 C7 C8 122.2(5) . . ? N1 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C3 C4 C5 120.8(5) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C9 C10 C11 119.9(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? N1 C11 C10 123.5(5) . . ? N1 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N2 C1 C2 123.0(4) . . ? N2 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C10 C9 C8 117.0(5) . . ? C10 C9 C12 121.4(5) . . ? C8 C9 C12 121.6(5) . . ? N2 C5 C4 123.0(5) . . ? N2 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C13 O1 Ag1 120.0(3) . . ? C6 C12 C9 113.2(5) 1_456 . ? C6 C12 H12A 108.9 1_456 . ? C9 C12 H12A 108.9 . . ? C6 C12 H1B 108.9 1_456 . ? C9 C12 H1B 108.9 . . ? H12A C12 H1B 107.7 . . ? C9 C8 C7 120.0(5) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C14 C19 C18 121.2(4) . . ? C14 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C14 C15 119.8(4) . . ? C19 C14 C13 121.3(4) . . ? C15 C14 C13 118.9(4) . . ? O1 C13 O2 126.9(4) . . ? O1 C13 C14 117.0(4) . . ? O2 C13 C14 116.1(4) . . ? C12 C6 C3 117.2(4) 1_654 . ? C12 C6 H6B 108.0 1_654 . ? C3 C6 H6B 108.0 . . ? C12 C6 H6A 108.0 1_654 . ? C3 C6 H6A 108.0 . . ? H6B C6 H6A 107.2 . . ? C13 O2 Ag1 127.2(3) . 2_755 ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 118.7(4) . . ? C17 C18 C20 120.0(4) . . ? C19 C18 C20 121.2(4) . . ? O4 C20 O3 126.2(5) . . ? O4 C20 C18 117.2(4) . . ? O3 C20 C18 116.6(4) . . ? C16 C15 C14 118.9(4) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C17 C16 C15 121.2(4) . . ? C17 C16 I1 119.4(3) . . ? C15 C16 I1 119.4(4) . . ? C20 O4 Ag1 95.9(3) . 2_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.858 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 917683' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #TrackingRef '3-bix.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H34 Ag4 I2 N8 O8' _chemical_formula_sum 'C44 H34 Ag4 I2 N8 O8' _chemical_formula_weight 1488.07 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2576(4) _cell_length_b 12.6293(4) _cell_length_c 16.9504(5) _cell_angle_alpha 102.542(3) _cell_angle_beta 93.087(3) _cell_angle_gamma 106.942(3) _cell_volume 2232.56(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2314 _cell_measurement_theta_min 3.0083 _cell_measurement_theta_max 29.2026 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 3.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.519 _exptl_absorpt_correction_T_max 0.547 _exptl_absorpt_process_details 'SADABS(Bruker, 2009)' _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 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16596 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7851 _reflns_number_gt 6154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0583P)^2^+5.7621P] 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 7839 _refine_ls_number_parameters 592 _refine_ls_number_restraints 1574 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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 I1 I 1.67194(4) 1.55620(4) -0.09561(3) 0.04129(14) Uani 1 1 d U . . O4 O 1.4556(5) 1.0755(4) -0.3862(3) 0.0449(11) Uani 1 1 d U . . O3 O 1.5754(5) 1.2416(4) -0.4032(3) 0.0424(11) Uani 1 1 d U . . C8 C 1.5114(6) 1.1829(6) -0.3629(4) 0.0346(13) Uani 1 1 d U . . C5 C 1.4911(6) 1.2375(5) -0.2777(4) 0.0308(12) Uani 1 1 d U . . C4 C 1.5691(6) 1.3469(5) -0.2388(4) 0.0292(12) Uani 1 1 d U . . H4 H 1.6331 1.3856 -0.2643 0.035 Uiso 1 1 calc R . . C3 C 1.5496(6) 1.3964(5) -0.1616(4) 0.0294(12) Uani 1 1 d U . . C6 C 1.3955(6) 1.1813(6) -0.2397(4) 0.0343(12) Uani 1 1 d U . . H6 H 1.3455 1.1076 -0.2655 0.041 Uiso 1 1 calc R . . C2 C 1.4509(6) 1.3418(5) -0.1241(4) 0.0337(13) Uani 1 1 d U . . H2 H 1.4373 1.3777 -0.0730 0.040 Uiso 1 1 calc R . . C1 C 1.3730(6) 1.2336(5) -0.1632(4) 0.0332(12) Uani 1 1 d DU . . O1 O 1.2426(5) 1.2263(5) -0.0597(3) 0.0547(13) Uani 1 1 d U . . C7 C 1.2588(9) 1.1735(8) -0.1233(6) 0.0778(14) Uani 1 1 d DU . . O2 O 1.2126(6) 1.0742(5) -0.1492(4) 0.0778(14) Uani 1 1 d U . . Ag1 Ag 1.06520(5) 1.09606(5) -0.03610(3) 0.04427(16) Uani 1 1 d U . . I2 I 0.82135(5) 1.12717(4) 0.41398(3) 0.05136(16) Uani 1 1 d U . . Ag2 Ag 1.5000 1.0000 -0.5000 0.0482(2) Uani 1 2 d SU . . Ag5 Ag 0.0000 0.5000 1.0000 0.0530(2) Uani 1 2 d SU . . Ag3 Ag 0.79090(6) 1.23350(4) 0.59445(4) 0.04897(17) Uani 1 1 d U . . Ag4 Ag 0.98957(6) 1.25439(6) 0.73639(4) 0.0602(2) Uani 1 1 d U . . N8 N 0.1223(5) 0.5222(5) 0.9113(3) 0.0395(12) Uani 1 1 d U . . N7 N 0.2293(5) 0.6014(5) 0.8243(3) 0.0330(11) Uani 1 1 d U . . C42 C 0.2567(7) 0.5014(6) 0.8224(4) 0.0401(13) Uani 1 1 d U . . H42 H 0.3097 0.4722 0.7902 0.048 Uiso 1 1 calc R . . C44 C 0.1489(6) 0.6098(6) 0.8781(4) 0.0340(12) Uani 1 1 d U . . H44 H 0.1157 0.6699 0.8906 0.041 Uiso 1 1 calc R . . C43 C 0.1897(7) 0.4545(6) 0.8777(4) 0.0412(14) Uani 1 1 d U . . H43 H 0.1901 0.3866 0.8905 0.049 Uiso 1 1 calc R . . C35 C 0.5930(6) 0.9709(6) 0.9185(4) 0.0338(12) Uani 1 1 d U . . C39 C 0.4808(6) 0.7703(6) 0.8808(4) 0.0365(12) Uani 1 1 d U . . H39 H 0.4740 0.6968 0.8854 0.044 Uiso 1 1 calc R . . C36 C 0.5016(6) 0.9867(6) 0.8687(4) 0.0376(12) Uani 1 1 d U . . H36 H 0.5074 1.0602 0.8643 0.045 Uiso 1 1 calc R . . C40 C 0.5810(6) 0.8607(6) 0.9250(4) 0.0367(13) Uani 1 1 d U . . H40 H 0.6400 0.8475 0.9590 0.044 Uiso 1 1 calc R . . C37 C 0.4017(6) 0.8962(6) 0.8254(4) 0.0381(13) Uani 1 1 d U . . H37 H 0.3410 0.9093 0.7927 0.046 Uiso 1 1 calc R . . C38 C 0.3917(6) 0.7863(6) 0.8304(4) 0.0318(12) Uani 1 1 d U . . C41 C 0.2855(6) 0.6867(6) 0.7793(4) 0.0369(13) Uani 1 1 d U . . H41A H 0.2214 0.7154 0.7598 0.044 Uiso 1 1 calc R . . H41B H 0.3169 0.6503 0.7321 0.044 Uiso 1 1 calc R . . C34 C 0.7031(7) 1.0678(6) 0.9649(4) 0.0395(13) Uani 1 1 d U . . H34A H 0.6761 1.1088 1.0123 0.047 Uiso 1 1 calc R . . H34B H 0.7654 1.0370 0.9842 0.047 Uiso 1 1 calc R . . C33 C 0.8420(6) 1.1338(6) 0.8628(4) 0.0363(12) Uani 1 1 d U . . H33 H 0.8706 1.0709 0.8508 0.044 Uiso 1 1 calc R . . C32 C 0.7416(7) 1.2490(6) 0.9155(4) 0.0428(14) Uani 1 1 d U . . H32 H 0.6898 1.2814 0.9467 0.051 Uiso 1 1 calc R . . N6 N 0.7612(5) 1.1485(5) 0.9171(3) 0.0349(11) Uani 1 1 d U . . N5 N 0.8746(5) 1.2213(5) 0.8291(3) 0.0391(12) Uani 1 1 d U . . C31 C 0.8093(7) 1.2936(6) 0.8616(4) 0.0450(15) Uani 1 1 d U . . H31 H 0.8118 1.3618 0.8482 0.054 Uiso 1 1 calc R . . N2 N 0.7309(5) 0.9177(5) 0.6738(3) 0.0331(11) Uani 1 1 d U . . N1 N 0.7756(5) 1.0636(5) 0.6173(3) 0.0379(11) Uani 1 1 d U . . C18 C 0.8242(6) 0.9090(6) 0.6280(4) 0.0392(13) Uani 1 1 d U . . H18 H 0.8617 0.8516 0.6209 0.047 Uiso 1 1 calc R . . C17 C 0.8520(7) 0.9990(6) 0.5950(4) 0.0417(14) Uani 1 1 d U . . H17 H 0.9145 1.0152 0.5617 0.050 Uiso 1 1 calc R . . C19 C 0.7030(7) 1.0106(6) 0.6653(4) 0.0389(13) Uani 1 1 d U . . H19 H 0.6406 1.0351 0.6898 0.047 Uiso 1 1 calc R . . C9 C 1.0514(6) 1.4024(5) 0.3197(4) 0.0272(11) Uani 1 1 d U . . C14 C 0.9866(6) 1.3403(5) 0.3712(4) 0.0281(11) Uani 1 1 d U . . H14 H 0.9780 1.3771 0.4234 0.034 Uiso 1 1 calc R . . C13 C 0.9353(6) 1.2235(5) 0.3436(4) 0.0269(11) Uani 1 1 d U . . C10 C 1.0646(6) 1.3447(5) 0.2423(4) 0.0298(11) Uani 1 1 d U . . H10 H 1.1057 1.3859 0.2071 0.036 Uiso 1 1 calc R . . C12 C 0.9521(6) 1.1644(5) 0.2681(4) 0.0310(12) Uani 1 1 d U . . H12 H 0.9205 1.0852 0.2522 0.037 Uiso 1 1 calc R . . C11 C 1.0169(6) 1.2259(5) 0.2170(4) 0.0266(11) Uani 1 1 d U . . C16 C 1.0291(6) 1.1646(5) 0.1317(4) 0.0312(12) Uani 1 1 d U . . O8 O 1.0666(4) 1.0792(4) 0.1252(3) 0.0404(10) Uani 1 1 d U . . C21 C 0.5718(6) 0.7296(6) 0.6660(4) 0.0338(12) Uani 1 1 d U . . C23 C 0.3991(7) 0.6410(6) 0.5592(4) 0.0414(14) Uani 1 1 d U . . H23 H 0.3437 0.6479 0.5194 0.050 Uiso 1 1 calc R . . C24 C 0.3916(6) 0.5347(6) 0.5701(4) 0.0368(13) Uani 1 1 d U . . C22 C 0.4877(7) 0.7379(6) 0.6065(4) 0.0419(13) Uani 1 1 d U . . H22 H 0.4910 0.8091 0.5984 0.050 Uiso 1 1 calc R . . C25 C 0.4771(6) 0.5269(6) 0.6295(4) 0.0404(13) Uani 1 1 d U . . H25 H 0.4742 0.4558 0.6377 0.048 Uiso 1 1 calc R . . C26 C 0.5662(6) 0.6240(6) 0.6764(4) 0.0368(13) Uani 1 1 d U . . H26 H 0.6229 0.6173 0.7155 0.044 Uiso 1 1 calc R . . C20 C 0.6667(7) 0.8355(6) 0.7198(4) 0.0390(12) Uani 1 1 d U . . H20A H 0.6246 0.8727 0.7603 0.047 Uiso 1 1 calc R . . H20B H 0.7286 0.8130 0.7484 0.047 Uiso 1 1 calc R . . O7 O 1.0002(5) 1.2023(4) 0.0744(3) 0.0433(10) Uani 1 1 d U . . C15 C 1.1050(6) 1.5301(5) 0.3454(4) 0.0319(12) Uani 1 1 d U . . O5 O 1.1303(5) 1.5834(4) 0.2909(3) 0.0468(11) Uani 1 1 d U . . N3 N 0.2322(5) 0.3471(5) 0.5612(3) 0.0359(11) Uani 1 1 d U . . C27 C 0.2945(7) 0.4305(6) 0.5162(4) 0.0440(14) Uani 1 1 d U . . H27A H 0.2319 0.4546 0.4898 0.053 Uiso 1 1 calc R . . H27B H 0.3346 0.3940 0.4740 0.053 Uiso 1 1 calc R . . O6 O 1.1185(4) 1.5785(4) 0.4197(3) 0.0414(11) Uani 1 1 d U . . C30 C 0.1407(7) 0.3555(6) 0.6073(4) 0.0424(14) Uani 1 1 d U . . H30 H 0.1030 0.4127 0.6122 0.051 Uiso 1 1 calc R . . C28 C 0.2616(7) 0.2530(6) 0.5705(5) 0.0447(14) Uani 1 1 d U . . H28 H 0.3220 0.2249 0.5462 0.054 Uiso 1 1 calc R . . C29 C 0.1864(7) 0.2088(6) 0.6215(5) 0.0468(15) Uani 1 1 d U . . H29 H 0.1864 0.1435 0.6384 0.056 Uiso 1 1 calc R . . N4 N 0.1110(6) 0.2719(5) 0.6451(4) 0.0437(13) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0469(3) 0.0309(3) 0.0367(2) -0.00158(19) 0.0057(2) 0.0050(2) O4 0.052(2) 0.041(2) 0.032(2) -0.0065(19) 0.0188(19) 0.008(2) O3 0.047(2) 0.048(2) 0.028(2) 0.0066(19) 0.0137(19) 0.010(2) C8 0.037(3) 0.038(3) 0.027(2) 0.004(2) 0.008(2) 0.011(2) C5 0.035(3) 0.032(2) 0.026(2) 0.005(2) 0.008(2) 0.012(2) C4 0.035(2) 0.027(2) 0.026(2) 0.006(2) 0.009(2) 0.009(2) C3 0.038(3) 0.025(3) 0.024(2) 0.003(2) 0.006(2) 0.010(2) C6 0.039(2) 0.030(2) 0.031(2) 0.003(2) 0.011(2) 0.008(2) C2 0.041(3) 0.031(3) 0.028(2) 0.004(2) 0.011(2) 0.011(2) C1 0.039(3) 0.028(2) 0.032(2) 0.004(2) 0.010(2) 0.012(2) O1 0.060(3) 0.051(3) 0.042(2) 0.002(2) 0.023(2) 0.003(2) C7 0.079(3) 0.057(2) 0.066(2) -0.010(2) 0.026(2) -0.011(2) O2 0.079(3) 0.057(2) 0.066(2) -0.010(2) 0.026(2) -0.011(2) Ag1 0.0471(3) 0.0410(3) 0.0345(3) 0.0006(2) 0.0173(2) 0.0023(3) I2 0.0771(4) 0.0313(3) 0.0453(3) 0.0134(2) 0.0312(3) 0.0092(2) Ag2 0.0595(5) 0.0491(5) 0.0287(4) -0.0075(3) 0.0138(4) 0.0168(4) Ag5 0.0553(5) 0.0573(6) 0.0436(4) 0.0197(4) 0.0186(4) 0.0055(4) Ag3 0.0520(4) 0.0223(3) 0.0700(4) 0.0120(3) 0.0121(3) 0.0063(2) Ag4 0.0541(4) 0.0658(4) 0.0431(3) 0.0150(3) 0.0148(3) -0.0109(3) N8 0.043(3) 0.038(3) 0.037(2) 0.013(2) 0.010(2) 0.008(2) N7 0.033(2) 0.035(2) 0.034(2) 0.013(2) 0.008(2) 0.011(2) C42 0.040(3) 0.038(3) 0.044(3) 0.009(2) 0.006(2) 0.013(2) C44 0.036(3) 0.034(3) 0.037(2) 0.013(2) 0.006(2) 0.014(2) C43 0.046(3) 0.037(3) 0.042(3) 0.012(2) 0.008(3) 0.013(2) C35 0.033(2) 0.037(2) 0.032(2) 0.013(2) 0.008(2) 0.008(2) C39 0.038(2) 0.037(2) 0.037(2) 0.017(2) 0.004(2) 0.009(2) C36 0.040(2) 0.035(2) 0.040(2) 0.013(2) 0.002(2) 0.012(2) C40 0.035(3) 0.042(3) 0.036(2) 0.016(2) 0.002(2) 0.011(2) C37 0.037(3) 0.041(3) 0.039(3) 0.016(2) -0.001(2) 0.013(2) C38 0.033(2) 0.036(2) 0.030(2) 0.014(2) 0.008(2) 0.010(2) C41 0.038(3) 0.037(3) 0.037(2) 0.015(2) 0.007(2) 0.009(2) C34 0.043(3) 0.040(3) 0.034(2) 0.016(2) 0.004(2) 0.007(2) C33 0.038(2) 0.036(2) 0.035(2) 0.012(2) 0.005(2) 0.009(2) C32 0.042(3) 0.039(3) 0.044(3) 0.007(3) 0.004(3) 0.011(2) N6 0.037(2) 0.034(2) 0.033(2) 0.013(2) 0.005(2) 0.006(2) N5 0.040(2) 0.038(2) 0.037(2) 0.013(2) 0.007(2) 0.005(2) C31 0.048(3) 0.040(3) 0.044(3) 0.013(3) 0.001(3) 0.009(3) N2 0.034(2) 0.032(2) 0.034(2) 0.0123(19) 0.006(2) 0.0083(19) N1 0.043(2) 0.029(2) 0.043(2) 0.012(2) 0.010(2) 0.010(2) C18 0.039(3) 0.036(3) 0.045(3) 0.015(2) 0.006(2) 0.011(2) C17 0.038(3) 0.040(3) 0.044(3) 0.009(2) 0.014(2) 0.006(2) C19 0.038(2) 0.035(2) 0.042(2) 0.012(2) 0.009(2) 0.007(2) C9 0.031(2) 0.022(2) 0.032(2) 0.007(2) 0.004(2) 0.013(2) C14 0.035(2) 0.024(2) 0.027(2) 0.003(2) 0.006(2) 0.014(2) C13 0.036(2) 0.023(2) 0.026(2) 0.010(2) 0.006(2) 0.013(2) C10 0.034(2) 0.028(2) 0.028(2) 0.006(2) 0.006(2) 0.011(2) C12 0.039(2) 0.025(2) 0.031(2) 0.006(2) 0.006(2) 0.014(2) C11 0.032(2) 0.023(2) 0.028(2) 0.004(2) 0.008(2) 0.015(2) C16 0.036(3) 0.027(3) 0.029(2) 0.003(2) 0.010(2) 0.010(2) O8 0.049(2) 0.034(2) 0.038(2) -0.0001(19) 0.0070(19) 0.0180(19) C21 0.035(2) 0.035(2) 0.032(2) 0.016(2) 0.009(2) 0.007(2) C23 0.039(3) 0.042(3) 0.039(3) 0.015(2) 0.000(2) 0.004(2) C24 0.035(3) 0.039(3) 0.034(2) 0.014(2) 0.011(2) 0.004(2) C22 0.044(3) 0.037(3) 0.044(2) 0.017(2) 0.001(2) 0.006(2) C25 0.042(3) 0.037(3) 0.041(2) 0.018(2) 0.004(2) 0.004(2) C26 0.038(3) 0.036(3) 0.036(3) 0.016(2) 0.000(2) 0.006(2) C20 0.041(2) 0.038(2) 0.038(2) 0.0150(19) 0.005(2) 0.0068(19) O7 0.060(2) 0.042(2) 0.029(2) 0.0032(19) 0.0095(19) 0.022(2) C15 0.033(3) 0.024(2) 0.038(3) 0.003(2) 0.006(2) 0.011(2) O5 0.059(3) 0.025(2) 0.049(2) 0.006(2) 0.009(2) 0.003(2) N3 0.032(2) 0.036(2) 0.037(2) 0.012(2) 0.007(2) 0.003(2) C27 0.042(3) 0.042(3) 0.041(3) 0.014(2) 0.008(2) -0.001(2) O6 0.049(2) 0.027(2) 0.039(2) -0.0056(19) 0.000(2) 0.0087(19) C30 0.040(3) 0.040(3) 0.047(3) 0.013(2) 0.007(2) 0.010(2) C28 0.041(3) 0.041(3) 0.054(3) 0.012(3) 0.008(3) 0.013(2) C29 0.046(3) 0.038(3) 0.055(3) 0.015(3) 0.002(3) 0.009(3) N4 0.042(3) 0.041(3) 0.043(3) 0.014(2) 0.009(2) 0.001(2) _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 I1 C3 2.111(6) . ? O4 C8 1.278(8) . ? O4 Ag2 2.112(4) . ? O3 C8 1.224(8) . ? O3 Ag3 2.460(5) 1_654 ? C8 C5 1.519(8) . ? C5 C6 1.380(9) . ? C5 C4 1.396(9) . ? C4 C3 1.381(8) . ? C4 H4 0.9300 . ? C3 C2 1.390(9) . ? C6 C1 1.395(8) . ? C6 H6 0.9300 . ? C2 C1 1.385(9) . ? C2 H2 0.9300 . ? C1 C7 1.560(7) . ? O1 C7 1.191(9) . ? O1 Ag1 2.305(5) . ? C7 O2 1.180(10) . ? Ag1 O7 2.339(4) . ? Ag1 O8 2.403(5) 2_775 ? Ag1 Ag1 2.9912(11) 2_775 ? I2 C13 2.105(6) . ? I2 Ag3 3.1425(8) . ? Ag2 O4 2.112(4) 2_874 ? Ag5 N8 2.102(5) 2_567 ? Ag5 N8 2.102(5) . ? Ag3 N1 2.222(5) . ? Ag3 O6 2.365(5) 2_786 ? Ag3 O3 2.460(5) 1_456 ? Ag3 O5 2.565(5) 2_786 ? Ag3 Ag4 3.1082(10) . ? Ag4 N5 2.124(5) . ? Ag4 N4 2.125(6) 1_665 ? N8 C44 1.313(8) . ? N8 C43 1.358(9) . ? N7 C44 1.329(8) . ? N7 C42 1.379(9) . ? N7 C41 1.468(8) . ? C42 C43 1.362(10) . ? C42 H42 0.9300 . ? C44 H44 0.9300 . ? C43 H43 0.9300 . ? C35 C36 1.382(9) . ? C35 C40 1.388(9) . ? C35 C34 1.498(9) . ? C39 C38 1.369(9) . ? C39 C40 1.388(10) . ? C39 H39 0.9300 . ? C36 C37 1.381(10) . ? C36 H36 0.9300 . ? C40 H40 0.9300 . ? C37 C38 1.382(9) . ? C37 H37 0.9300 . ? C38 C41 1.517(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C34 N6 1.468(8) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C33 N5 1.320(8) . ? C33 N6 1.349(8) . ? C33 H33 0.9300 . ? C32 C31 1.335(10) . ? C32 N6 1.356(9) . ? C32 H32 0.9300 . ? N5 C31 1.376(9) . ? C31 H31 0.9300 . ? N2 C19 1.334(9) . ? N2 C18 1.355(8) . ? N2 C20 1.478(8) . ? N1 C19 1.329(8) . ? N1 C17 1.363(9) . ? C18 C17 1.338(10) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? C19 H19 0.9300 . ? C9 C10 1.393(8) . ? C9 C14 1.394(8) . ? C9 C15 1.501(9) . ? C14 C13 1.379(8) . ? C14 H14 0.9300 . ? C13 C12 1.388(8) . ? C10 C11 1.396(9) . ? C10 H10 0.9300 . ? C12 C11 1.384(9) . ? C12 H12 0.9300 . ? C11 C16 1.518(8) . ? C16 O7 1.239(8) . ? C16 O8 1.254(7) . ? O8 Ag1 2.403(5) 2_775 ? C21 C26 1.367(9) . ? C21 C22 1.387(10) . ? C21 C20 1.515(9) . ? C23 C24 1.373(10) . ? C23 C22 1.383(10) . ? C23 H23 0.9300 . ? C24 C25 1.394(10) . ? C24 C27 1.515(10) . ? C22 H22 0.9300 . ? C25 C26 1.384(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C15 O5 1.256(8) . ? C15 O6 1.254(8) . ? O5 Ag3 2.565(5) 2_786 ? N3 C30 1.341(8) . ? N3 C28 1.361(9) . ? N3 C27 1.470(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? O6 Ag3 2.365(5) 2_786 ? C30 N4 1.322(9) . ? C30 H30 0.9300 . ? C28 C29 1.337(10) . ? C28 H28 0.9300 . ? C29 N4 1.345(9) . ? C29 H29 0.9300 . ? N4 Ag4 2.125(6) 1_445 ? 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 C8 O4 Ag2 113.1(4) . . ? C8 O3 Ag3 115.1(4) . 1_654 ? O3 C8 O4 125.7(6) . . ? O3 C8 C5 120.0(6) . . ? O4 C8 C5 114.3(6) . . ? C6 C5 C4 120.2(5) . . ? C6 C5 C8 120.8(6) . . ? C4 C5 C8 119.0(5) . . ? C3 C4 C5 118.7(6) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C3 C2 121.3(6) . . ? C4 C3 I1 120.8(5) . . ? C2 C3 I1 117.9(4) . . ? C5 C6 C1 120.8(6) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C1 C2 C3 119.8(5) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C1 C6 119.1(6) . . ? C2 C1 C7 120.3(6) . . ? C6 C1 C7 120.6(6) . . ? C7 O1 Ag1 99.4(5) . . ? O2 C7 O1 124.6(8) . . ? O2 C7 C1 117.1(7) . . ? O1 C7 C1 116.4(7) . . ? O1 Ag1 O7 102.89(17) . . ? O1 Ag1 O8 129.49(16) . 2_775 ? O7 Ag1 O8 124.39(17) . 2_775 ? O1 Ag1 Ag1 152.38(16) . 2_775 ? O7 Ag1 Ag1 81.85(12) . 2_775 ? O8 Ag1 Ag1 61.09(11) 2_775 2_775 ? C13 I2 Ag3 122.22(16) . . ? O4 Ag2 O4 180.0(3) 2_874 . ? N8 Ag5 N8 180.000(2) 2_567 . ? N1 Ag3 O6 160.03(19) . 2_786 ? N1 Ag3 O3 103.08(19) . 1_456 ? O6 Ag3 O3 96.35(16) 2_786 1_456 ? N1 Ag3 O5 121.52(19) . 2_786 ? O6 Ag3 O5 53.00(15) 2_786 2_786 ? O3 Ag3 O5 90.39(16) 1_456 2_786 ? N1 Ag3 Ag4 69.06(15) . . ? O6 Ag3 Ag4 94.87(12) 2_786 . ? O3 Ag3 Ag4 130.15(10) 1_456 . ? O5 Ag3 Ag4 59.66(12) 2_786 . ? N1 Ag3 I2 86.43(14) . . ? O6 Ag3 I2 92.03(11) 2_786 . ? O3 Ag3 I2 107.86(10) 1_456 . ? O5 Ag3 I2 142.76(11) 2_786 . ? Ag4 Ag3 I2 120.09(2) . . ? N5 Ag4 N4 173.7(2) . 1_665 ? N5 Ag4 Ag3 100.97(16) . . ? N4 Ag4 Ag3 82.38(17) 1_665 . ? C44 N8 C43 106.5(5) . . ? C44 N8 Ag5 124.5(5) . . ? C43 N8 Ag5 129.1(5) . . ? C44 N7 C42 107.5(6) . . ? C44 N7 C41 126.2(6) . . ? C42 N7 C41 126.1(5) . . ? C43 C42 N7 105.4(6) . . ? C43 C42 H42 127.3 . . ? N7 C42 H42 127.3 . . ? N8 C44 N7 111.2(6) . . ? N8 C44 H44 124.4 . . ? N7 C44 H44 124.4 . . ? C42 C43 N8 109.4(6) . . ? C42 C43 H43 125.3 . . ? N8 C43 H43 125.3 . . ? C36 C35 C40 118.0(6) . . ? C36 C35 C34 122.4(6) . . ? C40 C35 C34 119.6(6) . . ? C38 C39 C40 121.9(6) . . ? C38 C39 H39 119.1 . . ? C40 C39 H39 119.1 . . ? C37 C36 C35 121.7(6) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C35 C40 C39 119.8(6) . . ? C35 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C38 C37 C36 120.1(6) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39 C38 C37 118.5(6) . . ? C39 C38 C41 121.7(6) . . ? C37 C38 C41 119.8(6) . . ? N7 C41 C38 113.0(5) . . ? N7 C41 H41A 109.0 . . ? C38 C41 H41A 109.0 . . ? N7 C41 H41B 109.0 . . ? C38 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? N6 C34 C35 113.8(5) . . ? N6 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? N6 C34 H34B 108.8 . . ? C35 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? N5 C33 N6 110.5(6) . . ? N5 C33 H33 124.7 . . ? N6 C33 H33 124.7 . . ? C31 C32 N6 108.4(6) . . ? C31 C32 H32 125.8 . . ? N6 C32 H32 125.8 . . ? C33 N6 C32 106.4(6) . . ? C33 N6 C34 125.9(6) . . ? C32 N6 C34 127.6(6) . . ? C33 N5 C31 106.4(6) . . ? C33 N5 Ag4 131.9(5) . . ? C31 N5 Ag4 121.5(5) . . ? C32 C31 N5 108.2(7) . . ? C32 C31 H31 125.9 . . ? N5 C31 H31 125.9 . . ? C19 N2 C18 106.9(6) . . ? C19 N2 C20 126.6(6) . . ? C18 N2 C20 126.4(6) . . ? C19 N1 C17 104.6(6) . . ? C19 N1 Ag3 127.8(5) . . ? C17 N1 Ag3 127.0(4) . . ? C17 C18 N2 106.8(6) . . ? C17 C18 H18 126.6 . . ? N2 C18 H18 126.6 . . ? C18 C17 N1 110.2(6) . . ? C18 C17 H17 124.9 . . ? N1 C17 H17 124.9 . . ? N1 C19 N2 111.5(6) . . ? N1 C19 H19 124.3 . . ? N2 C19 H19 124.3 . . ? C10 C9 C14 119.2(6) . . ? C10 C9 C15 119.6(6) . . ? C14 C9 C15 121.3(5) . . ? C13 C14 C9 119.0(5) . . ? C13 C14 H14 120.5 . . ? C9 C14 H14 120.5 . . ? C14 C13 C12 122.4(6) . . ? C14 C13 I2 120.8(4) . . ? C12 C13 I2 116.8(4) . . ? C9 C10 C11 120.9(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C11 C12 C13 118.5(6) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 C16 119.8(5) . . ? C10 C11 C16 120.2(5) . . ? O7 C16 O8 125.4(6) . . ? O7 C16 C11 117.5(5) . . ? O8 C16 C11 117.1(6) . . ? C16 O8 Ag1 116.7(4) . 2_775 ? C26 C21 C22 118.8(6) . . ? C26 C21 C20 120.3(6) . . ? C22 C21 C20 120.9(6) . . ? C24 C23 C22 121.1(7) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 118.1(6) . . ? C23 C24 C27 119.5(6) . . ? C25 C24 C27 122.4(6) . . ? C23 C22 C21 120.5(7) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C26 C25 C24 120.6(6) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C21 C26 C25 120.8(7) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? N2 C20 C21 113.0(5) . . ? N2 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? N2 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C16 O7 Ag1 102.6(4) . . ? O5 C15 O6 123.2(6) . . ? O5 C15 C9 118.0(6) . . ? O6 C15 C9 118.8(6) . . ? C15 O5 Ag3 87.2(4) . 2_786 ? C30 N3 C28 106.5(6) . . ? C30 N3 C27 125.5(6) . . ? C28 N3 C27 127.8(6) . . ? N3 C27 C24 113.1(6) . . ? N3 C27 H27A 109.0 . . ? C24 C27 H27A 109.0 . . ? N3 C27 H27B 109.0 . . ? C24 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C15 O6 Ag3 96.5(4) . 2_786 ? N4 C30 N3 111.1(6) . . ? N4 C30 H30 124.4 . . ? N3 C30 H30 124.4 . . ? C29 C28 N3 106.4(6) . . ? C29 C28 H28 126.8 . . ? N3 C28 H28 126.8 . . ? C28 C29 N4 110.6(7) . . ? C28 C29 H29 124.7 . . ? N4 C29 H29 124.7 . . ? C30 N4 C29 105.3(6) . . ? C30 N4 Ag4 127.2(5) . 1_445 ? C29 N4 Ag4 126.9(5) . 1_445 ? 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 Ag3 O3 C8 O4 -80.5(8) 1_654 . . . ? Ag3 O3 C8 C5 100.5(6) 1_654 . . . ? Ag2 O4 C8 O3 6.5(9) . . . . ? Ag2 O4 C8 C5 -174.5(4) . . . . ? O3 C8 C5 C6 163.0(7) . . . . ? O4 C8 C5 C6 -16.1(9) . . . . ? O3 C8 C5 C4 -15.7(10) . . . . ? O4 C8 C5 C4 165.2(6) . . . . ? C6 C5 C4 C3 0.8(9) . . . . ? C8 C5 C4 C3 179.5(6) . . . . ? C5 C4 C3 C2 -3.0(10) . . . . ? C5 C4 C3 I1 175.5(5) . . . . ? C4 C5 C6 C1 1.9(10) . . . . ? C8 C5 C6 C1 -176.9(6) . . . . ? C4 C3 C2 C1 2.5(10) . . . . ? I1 C3 C2 C1 -176.0(5) . . . . ? C3 C2 C1 C6 0.2(10) . . . . ? C3 C2 C1 C7 -177.5(7) . . . . ? C5 C6 C1 C2 -2.3(10) . . . . ? C5 C6 C1 C7 175.4(8) . . . . ? Ag1 O1 C7 O2 -17.0(13) . . . . ? Ag1 O1 C7 C1 179.2(7) . . . . ? C2 C1 C7 O2 -163.8(9) . . . . ? C6 C1 C7 O2 18.6(14) . . . . ? C2 C1 C7 O1 1.3(14) . . . . ? C6 C1 C7 O1 -176.4(8) . . . . ? C7 O1 Ag1 O7 -169.4(7) . . . . ? C7 O1 Ag1 O8 -9.4(8) . . . 2_775 ? C7 O1 Ag1 Ag1 93.5(7) . . . 2_775 ? C13 I2 Ag3 N1 -146.2(2) . . . . ? C13 I2 Ag3 O6 13.9(2) . . . 2_786 ? C13 I2 Ag3 O3 111.2(2) . . . 1_456 ? C13 I2 Ag3 O5 -4.6(3) . . . 2_786 ? C13 I2 Ag3 Ag4 -82.9(2) . . . . ? N1 Ag3 Ag4 N5 -71.3(2) . . . . ? O6 Ag3 Ag4 N5 120.88(19) 2_786 . . . ? O3 Ag3 Ag4 N5 18.4(2) 1_456 . . . ? O5 Ag3 Ag4 N5 79.4(2) 2_786 . . . ? I2 Ag3 Ag4 N5 -143.93(16) . . . . ? N1 Ag3 Ag4 N4 103.3(2) . . . 1_665 ? O6 Ag3 Ag4 N4 -64.5(2) 2_786 . . 1_665 ? O3 Ag3 Ag4 N4 -167.1(2) 1_456 . . 1_665 ? O5 Ag3 Ag4 N4 -106.0(2) 2_786 . . 1_665 ? I2 Ag3 Ag4 N4 30.65(17) . . . 1_665 ? C44 N7 C42 C43 -0.6(8) . . . . ? C41 N7 C42 C43 175.5(6) . . . . ? C43 N8 C44 N7 0.5(8) . . . . ? Ag5 N8 C44 N7 179.7(4) . . . . ? C42 N7 C44 N8 0.1(8) . . . . ? C41 N7 C44 N8 -176.1(6) . . . . ? N7 C42 C43 N8 0.9(8) . . . . ? C44 N8 C43 C42 -0.9(8) . . . . ? Ag5 N8 C43 C42 180.0(5) . . . . ? C40 C35 C36 C37 -1.0(10) . . . . ? C34 C35 C36 C37 179.0(6) . . . . ? C36 C35 C40 C39 1.5(9) . . . . ? C34 C35 C40 C39 -178.6(6) . . . . ? C38 C39 C40 C35 -0.3(10) . . . . ? C35 C36 C37 C38 -0.6(10) . . . . ? C40 C39 C38 C37 -1.3(10) . . . . ? C40 C39 C38 C41 177.2(6) . . . . ? C36 C37 C38 C39 1.7(10) . . . . ? C36 C37 C38 C41 -176.8(6) . . . . ? C44 N7 C41 C38 77.8(8) . . . . ? C42 N7 C41 C38 -97.6(8) . . . . ? C39 C38 C41 N7 43.4(8) . . . . ? C37 C38 C41 N7 -138.1(6) . . . . ? C36 C35 C34 N6 -44.1(9) . . . . ? C40 C35 C34 N6 136.0(6) . . . . ? N5 C33 N6 C32 1.1(8) . . . . ? N5 C33 N6 C34 178.7(6) . . . . ? C31 C32 N6 C33 -0.1(8) . . . . ? C31 C32 N6 C34 -177.6(6) . . . . ? C35 C34 N6 C33 -80.0(8) . . . . ? C35 C34 N6 C32 97.0(8) . . . . ? N6 C33 N5 C31 -1.7(8) . . . . ? N6 C33 N5 Ag4 -176.8(4) . . . . ? Ag3 Ag4 N5 C33 109.7(6) . . . . ? Ag3 Ag4 N5 C31 -64.8(5) . . . . ? N6 C32 C31 N5 -0.9(8) . . . . ? C33 N5 C31 C32 1.6(8) . . . . ? Ag4 N5 C31 C32 177.3(5) . . . . ? O6 Ag3 N1 C19 130.7(6) 2_786 . . . ? O3 Ag3 N1 C19 -35.6(6) 1_456 . . . ? O5 Ag3 N1 C19 63.0(6) 2_786 . . . ? Ag4 Ag3 N1 C19 92.7(6) . . . . ? I2 Ag3 N1 C19 -143.1(6) . . . . ? O6 Ag3 N1 C17 -38.5(9) 2_786 . . . ? O3 Ag3 N1 C17 155.1(6) 1_456 . . . ? O5 Ag3 N1 C17 -106.2(6) 2_786 . . . ? Ag4 Ag3 N1 C17 -76.6(6) . . . . ? I2 Ag3 N1 C17 47.6(6) . . . . ? C19 N2 C18 C17 1.7(8) . . . . ? C20 N2 C18 C17 177.9(6) . . . . ? N2 C18 C17 N1 -1.6(8) . . . . ? C19 N1 C17 C18 0.9(8) . . . . ? Ag3 N1 C17 C18 172.1(5) . . . . ? C17 N1 C19 N2 0.3(8) . . . . ? Ag3 N1 C19 N2 -170.9(4) . . . . ? C18 N2 C19 N1 -1.2(8) . . . . ? C20 N2 C19 N1 -177.4(6) . . . . ? C10 C9 C14 C13 -1.1(9) . . . . ? C15 C9 C14 C13 177.8(6) . . . . ? C9 C14 C13 C12 3.9(10) . . . . ? C9 C14 C13 I2 -173.9(4) . . . . ? Ag3 I2 C13 C14 -8.9(6) . . . . ? Ag3 I2 C13 C12 173.2(4) . . . . ? C14 C9 C10 C11 -1.8(9) . . . . ? C15 C9 C10 C11 179.3(6) . . . . ? C14 C13 C12 C11 -3.6(10) . . . . ? I2 C13 C12 C11 174.2(5) . . . . ? C13 C12 C11 C10 0.6(9) . . . . ? C13 C12 C11 C16 -175.8(6) . . . . ? C9 C10 C11 C12 2.0(9) . . . . ? C9 C10 C11 C16 178.4(6) . . . . ? C12 C11 C16 O7 129.0(7) . . . . ? C10 C11 C16 O7 -47.4(9) . . . . ? C12 C11 C16 O8 -50.4(9) . . . . ? C10 C11 C16 O8 133.3(6) . . . . ? O7 C16 O8 Ag1 -54.7(8) . . . 2_775 ? C11 C16 O8 Ag1 124.6(5) . . . 2_775 ? C22 C23 C24 C25 -0.9(10) . . . . ? C22 C23 C24 C27 -179.1(6) . . . . ? C24 C23 C22 C21 0.3(11) . . . . ? C26 C21 C22 C23 0.7(10) . . . . ? C20 C21 C22 C23 -178.2(6) . . . . ? C23 C24 C25 C26 0.5(10) . . . . ? C27 C24 C25 C26 178.6(6) . . . . ? C22 C21 C26 C25 -1.1(10) . . . . ? C20 C21 C26 C25 177.8(6) . . . . ? C24 C25 C26 C21 0.5(10) . . . . ? C19 N2 C20 C21 98.5(8) . . . . ? C18 N2 C20 C21 -76.9(8) . . . . ? C26 C21 C20 N2 135.5(6) . . . . ? C22 C21 C20 N2 -45.7(9) . . . . ? O8 C16 O7 Ag1 -9.0(8) . . . . ? C11 C16 O7 Ag1 171.7(5) . . . . ? O1 Ag1 O7 C16 -106.0(4) . . . . ? O8 Ag1 O7 C16 92.7(4) 2_775 . . . ? Ag1 Ag1 O7 C16 46.3(4) 2_775 . . . ? C10 C9 C15 O5 18.6(9) . . . . ? C14 C9 C15 O5 -160.3(6) . . . . ? C10 C9 C15 O6 -163.8(6) . . . . ? C14 C9 C15 O6 17.3(9) . . . . ? O6 C15 O5 Ag3 3.8(7) . . . 2_786 ? C9 C15 O5 Ag3 -178.7(5) . . . 2_786 ? C30 N3 C27 C24 78.1(9) . . . . ? C28 N3 C27 C24 -95.6(8) . . . . ? C23 C24 C27 N3 -138.0(7) . . . . ? C25 C24 C27 N3 43.9(9) . . . . ? O5 C15 O6 Ag3 -4.2(7) . . . 2_786 ? C9 C15 O6 Ag3 178.4(5) . . . 2_786 ? C28 N3 C30 N4 0.0(8) . . . . ? C27 N3 C30 N4 -174.9(6) . . . . ? C30 N3 C28 C29 0.2(8) . . . . ? C27 N3 C28 C29 174.9(7) . . . . ? N3 C28 C29 N4 -0.3(9) . . . . ? N3 C30 N4 C29 -0.1(8) . . . . ? N3 C30 N4 Ag4 171.8(4) . . . 1_445 ? C28 C29 N4 C30 0.2(9) . . . . ? C28 C29 N4 Ag4 -171.7(5) . . . 1_445 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.110 _refine_diff_density_min -1.987 _refine_diff_density_rms 0.124 _database_code_depnum_ccdc_archive 'CCDC 917685'