# 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_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Ag2 Cl3 N5 O10' _chemical_formula_weight 796.54 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9576(4) _cell_length_b 12.0044(4) _cell_length_c 12.1220(4) _cell_angle_alpha 65.317(2) _cell_angle_beta 70.029(2) _cell_angle_gamma 76.155(2) _cell_volume 1352.96(8) _cell_formula_units_Z 2 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 9964 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.81 _exptl_crystal_description plate _exptl_crystal_colour color-less _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4974 _exptl_absorpt_correction_T_max 0.7143 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 114(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25396 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4793 _reflns_number_gt 3951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0457P)^2^+0.4148P] 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 4793 _refine_ls_number_parameters 350 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Ag1 Ag 0.48940(3) 0.28725(2) 0.71799(3) 0.02744(10) Uani 1 1 d . . . Ag2 Ag 0.09483(3) 0.77083(3) 0.81160(3) 0.03352(11) Uani 1 1 d . . . O9 O -0.0284(4) 0.6480(3) 0.7958(4) 0.0538(9) Uani 1 1 d D . . H9A H -0.076(4) 0.705(3) 0.756(5) 0.065 Uiso 1 1 d D . . H9B H -0.003(9) 0.603(7) 0.752(7) 0.16(4) Uiso 1 1 d D . . C1 C 0.3415(3) 0.5357(3) 0.5579(3) 0.0168(7) Uani 1 1 d . . . Cl1 Cl 0.35274(9) 0.44352(7) 0.47606(8) 0.0226(2) Uani 1 1 d . . . N1 N 0.3362(3) 0.6553(2) 0.4917(3) 0.0187(6) Uani 1 1 d . . . C2 C 0.3225(3) 0.7234(3) 0.5629(3) 0.0195(8) Uani 1 1 d . . . N2 N 0.3119(3) 0.6761(2) 0.6874(3) 0.0195(6) Uani 1 1 d . . . N4 N 0.3169(3) 0.8469(2) 0.5051(3) 0.0199(6) Uani 1 1 d . . . C4 C 0.3150(4) 0.9226(3) 0.5728(4) 0.0279(9) Uani 1 1 d . . . H4A H 0.3593 0.9966 0.5124 0.033 Uiso 1 1 calc R . . H4B H 0.3652 0.8754 0.6356 0.033 Uiso 1 1 calc R . . C5 C 0.1805(5) 0.9631(3) 0.6392(4) 0.0355(10) Uani 1 1 d . . . H5 H 0.1737 1.0031 0.6945 0.043 Uiso 1 1 calc R . . C6 C 0.0687(5) 0.9482(4) 0.6279(4) 0.0423(12) Uani 1 1 d . . . H6A H 0.0708 0.9087 0.5737 0.051 Uiso 1 1 calc R . . H6B H -0.0127 0.9771 0.6741 0.051 Uiso 1 1 calc R . . C7 C 0.3120(4) 0.9080(3) 0.3734(3) 0.0240(8) Uani 1 1 d . . . H7A H 0.2639 0.9914 0.3614 0.029 Uiso 1 1 calc R . . H7B H 0.2624 0.8607 0.3565 0.029 Uiso 1 1 calc R . . C8 C 0.4438(4) 0.9198(3) 0.2791(3) 0.0233(8) Uani 1 1 d . . . H8 H 0.4461 0.9550 0.1923 0.028 Uiso 1 1 calc R . . C9 C 0.5584(4) 0.8849(3) 0.3071(4) 0.0262(9) Uani 1 1 d . . . H9C H 0.5605 0.8493 0.3928 0.031 Uiso 1 1 calc R . . H9D H 0.6378 0.8958 0.2413 0.031 Uiso 1 1 calc R . . C3 C 0.3242(3) 0.5519(3) 0.7404(3) 0.0173(7) Uani 1 1 d . . . N3 N 0.3418(3) 0.4748(2) 0.6780(3) 0.0183(6) Uani 1 1 d . . . N5 N 0.3185(3) 0.5010(2) 0.8636(3) 0.0218(7) Uani 1 1 d . . . C10 C 0.3077(4) 0.3689(3) 0.9359(3) 0.0250(8) Uani 1 1 d . . . H10A H 0.2538 0.3411 0.9034 0.030 Uiso 1 1 calc R . . H10B H 0.2614 0.3571 1.0252 0.030 Uiso 1 1 calc R . . C11 C 0.4359(4) 0.2896(3) 0.9307(3) 0.0272(9) Uani 1 1 d . . . H11 H 0.4334 0.2032 0.9740 0.033 Uiso 1 1 calc R . . C12 C 0.5532(4) 0.3291(3) 0.8708(4) 0.0287(9) Uani 1 1 d . . . H12A H 0.5605 0.4148 0.8261 0.034 Uiso 1 1 calc R . . H12B H 0.6297 0.2716 0.8726 0.034 Uiso 1 1 calc R . . C13 C 0.3214(4) 0.5770(3) 0.9309(3) 0.0274(9) Uani 1 1 d . . . H13A H 0.3789 0.6422 0.8723 0.033 Uiso 1 1 calc R . . H13B H 0.3610 0.5246 1.0010 0.033 Uiso 1 1 calc R . . C14 C 0.1910(4) 0.6370(4) 0.9838(3) 0.0330(10) Uani 1 1 d . . . H14 H 0.1183 0.5907 1.0227 0.040 Uiso 1 1 calc R . . C15 C 0.1728(5) 0.7531(4) 0.9785(4) 0.0463(12) Uani 1 1 d . . . H15A H 0.2442 0.8009 0.9400 0.056 Uiso 1 1 calc R . . H15B H 0.0883 0.7878 1.0133 0.056 Uiso 1 1 calc R . . Cl3 Cl 0.65582(10) 0.74190(8) -0.29632(9) 0.0298(2) Uani 1 1 d . . . O5 O 0.7726(4) 0.7855(3) -0.3155(5) 0.0976(18) Uani 1 1 d . . . O6 O 0.6604(4) 0.6119(2) -0.2280(3) 0.0488(9) Uani 1 1 d . . . O7 O 0.5514(5) 0.8034(3) -0.2266(4) 0.0818(14) Uani 1 1 d . . . O8 O 0.6319(4) 0.7713(3) -0.4126(3) 0.0658(11) Uani 1 1 d . . . Cl2 Cl 0.20009(10) 1.02408(8) 0.05853(9) 0.0312(2) Uani 1 1 d . . . O1 O 0.1641(4) 1.1280(3) 0.0951(4) 0.0859(16) Uani 1 1 d . . . O2 O 0.1516(4) 1.0416(4) -0.0439(4) 0.0791(13) Uani 1 1 d . . . O3 O 0.3392(3) 1.0044(3) 0.0167(3) 0.0544(9) Uani 1 1 d . . . O4 O 0.1532(4) 0.9177(3) 0.1641(3) 0.0564(9) Uani 1 1 d . . . C16 C -0.0988(7) 0.4029(7) 0.6610(7) 0.091(2) Uani 1 1 d . . . H16A H -0.1409 0.4844 0.6619 0.137 Uiso 1 1 calc R . . H16B H -0.1571 0.3403 0.7217 0.137 Uiso 1 1 calc R . . H16C H -0.0803 0.4023 0.5762 0.137 Uiso 1 1 calc R . . C17 C 0.0230(5) 0.3754(4) 0.6956(5) 0.0479(12) Uani 1 1 d . . . O10 O 0.0543(4) 0.4461(4) 0.7297(5) 0.0824(14) Uani 1 1 d . . . C18 C 0.1010(5) 0.2585(5) 0.6991(6) 0.0649(16) Uani 1 1 d . . . H18A H 0.1801 0.2527 0.7226 0.097 Uiso 1 1 calc R . . H18B H 0.1255 0.2531 0.6157 0.097 Uiso 1 1 calc R . . H18C H 0.0501 0.1907 0.7615 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0417(2) 0.01808(15) 0.02064(16) -0.00788(11) -0.00956(13) 0.00292(12) Ag2 0.0340(2) 0.03491(18) 0.03033(18) -0.01583(14) -0.00772(14) 0.00401(14) O9 0.044(2) 0.047(2) 0.080(3) -0.029(2) -0.0268(19) 0.0036(17) C1 0.0151(18) 0.0192(17) 0.0195(18) -0.0102(14) -0.0056(14) -0.0008(14) Cl1 0.0309(5) 0.0195(4) 0.0225(4) -0.0100(3) -0.0102(4) -0.0034(4) N1 0.0229(17) 0.0147(14) 0.0189(15) -0.0066(12) -0.0059(12) -0.0017(12) C2 0.0164(19) 0.0188(17) 0.0197(18) -0.0053(15) -0.0040(14) 0.0000(14) N2 0.0233(17) 0.0156(14) 0.0179(15) -0.0052(12) -0.0052(12) -0.0016(12) N4 0.0260(18) 0.0138(14) 0.0187(15) -0.0058(12) -0.0071(12) 0.0008(12) C4 0.038(2) 0.0175(17) 0.028(2) -0.0086(16) -0.0100(17) -0.0011(17) C5 0.052(3) 0.0194(19) 0.028(2) -0.0109(17) -0.0084(19) 0.0082(19) C6 0.040(3) 0.042(2) 0.029(2) -0.011(2) -0.008(2) 0.017(2) C7 0.035(2) 0.0132(16) 0.0209(19) -0.0017(14) -0.0127(16) 0.0014(15) C8 0.035(2) 0.0117(16) 0.0210(19) -0.0048(14) -0.0099(16) 0.0017(15) C9 0.032(2) 0.0217(18) 0.026(2) -0.0100(16) -0.0057(17) -0.0056(17) C3 0.0159(19) 0.0192(17) 0.0171(17) -0.0068(14) -0.0038(14) -0.0031(14) N3 0.0208(16) 0.0158(14) 0.0186(15) -0.0065(12) -0.0049(12) -0.0029(12) N5 0.0321(19) 0.0146(14) 0.0150(15) -0.0042(12) -0.0050(13) -0.0006(13) C10 0.035(2) 0.0186(17) 0.0145(18) -0.0024(14) -0.0016(15) -0.0062(16) C11 0.045(3) 0.0184(17) 0.0186(19) -0.0048(15) -0.0126(17) -0.0026(17) C12 0.037(3) 0.0243(19) 0.029(2) -0.0089(17) -0.0206(18) 0.0040(18) C13 0.041(3) 0.0239(18) 0.0190(19) -0.0076(15) -0.0115(17) -0.0026(17) C14 0.045(3) 0.035(2) 0.0188(19) -0.0133(17) -0.0072(17) -0.0010(19) C15 0.070(4) 0.038(2) 0.032(2) -0.020(2) -0.019(2) 0.009(2) Cl3 0.0483(6) 0.0187(4) 0.0274(5) -0.0057(4) -0.0181(4) -0.0063(4) O5 0.078(3) 0.0347(19) 0.188(5) -0.003(2) -0.092(3) -0.0111(19) O6 0.081(3) 0.0186(14) 0.0419(18) -0.0002(13) -0.0233(17) -0.0078(15) O7 0.113(4) 0.054(2) 0.069(3) -0.039(2) 0.004(2) -0.004(2) O8 0.131(4) 0.0406(18) 0.0396(19) -0.0071(16) -0.045(2) -0.016(2) Cl2 0.0295(6) 0.0278(5) 0.0336(5) -0.0094(4) -0.0064(4) -0.0056(4) O1 0.079(3) 0.049(2) 0.108(3) -0.053(2) 0.046(2) -0.033(2) O2 0.074(3) 0.098(3) 0.064(3) -0.006(2) -0.042(2) -0.019(2) O3 0.036(2) 0.066(2) 0.058(2) -0.0284(18) -0.0051(16) -0.0023(17) O4 0.075(3) 0.0430(18) 0.0425(19) -0.0069(15) -0.0004(17) -0.0310(18) C16 0.075(5) 0.099(5) 0.106(6) -0.036(4) -0.052(4) 0.015(4) C17 0.027(3) 0.046(3) 0.061(3) -0.017(2) -0.002(2) -0.007(2) O10 0.051(3) 0.078(3) 0.139(4) -0.075(3) -0.002(2) -0.016(2) C18 0.047(3) 0.044(3) 0.090(4) -0.022(3) -0.008(3) -0.004(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 C8 2.406(3) 2_666 ? Ag1 C9 2.406(4) 2_666 ? Ag1 N3 2.409(3) . ? Ag1 C12 2.449(4) . ? Ag1 C11 2.452(4) . ? Ag1 N1 2.537(3) 2_666 ? Ag2 O9 2.323(4) . ? Ag2 C15 2.367(4) . ? Ag2 C6 2.399(4) . ? Ag2 C14 2.438(4) . ? Ag2 C5 2.499(4) . ? Ag2 N2 2.628(3) . ? O9 H9A 0.840(10) . ? O9 H9B 0.844(10) . ? C1 N1 1.319(4) . ? C1 N3 1.330(4) . ? C1 Cl1 1.729(3) . ? N1 C2 1.370(4) . ? N1 Ag1 2.537(3) 2_666 ? C2 N2 1.345(4) . ? C2 N4 1.345(4) . ? N2 C3 1.348(4) . ? N4 C4 1.450(5) . ? N4 C7 1.467(4) . ? C4 C5 1.493(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.338(6) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.498(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.337(5) . ? C8 Ag1 2.406(3) 2_666 ? C8 H8 0.9500 . ? C9 Ag1 2.406(4) 2_666 ? C9 H9C 0.9500 . ? C9 H9D 0.9500 . ? C3 N5 1.342(4) . ? C3 N3 1.365(4) . ? N5 C13 1.466(5) . ? N5 C10 1.468(4) . ? C10 C11 1.494(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.330(6) . ? C11 H11 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.496(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.337(6) . ? C14 H14 0.9500 . ? C15 H15A 0.9500 . ? C15 H15B 0.9500 . ? Cl3 O8 1.404(3) . ? Cl3 O5 1.407(4) . ? Cl3 O7 1.423(4) . ? Cl3 O6 1.427(3) . ? Cl2 O1 1.420(3) . ? Cl2 O4 1.425(3) . ? Cl2 O3 1.427(3) . ? Cl2 O2 1.431(4) . ? C16 C17 1.456(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O10 1.240(6) . ? C17 C18 1.450(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Ag1 C9 32.27(13) 2_666 2_666 ? C8 Ag1 N3 150.53(12) 2_666 . ? C9 Ag1 N3 118.36(11) 2_666 . ? C8 Ag1 C12 114.50(13) 2_666 . ? C9 Ag1 C12 138.92(12) 2_666 . ? N3 Ag1 C12 92.08(11) . . ? C8 Ag1 C11 110.79(12) 2_666 . ? C9 Ag1 C11 119.21(13) 2_666 . ? N3 Ag1 C11 84.88(11) . . ? C12 Ag1 C11 31.49(13) . . ? C8 Ag1 N1 84.20(11) 2_666 2_666 ? C9 Ag1 N1 93.03(11) 2_666 2_666 ? N3 Ag1 N1 99.29(9) . 2_666 ? C12 Ag1 N1 109.53(12) . 2_666 ? C11 Ag1 N1 140.97(12) . 2_666 ? O9 Ag2 C15 131.97(15) . . ? O9 Ag2 C6 96.86(16) . . ? C15 Ag2 C6 129.39(16) . . ? O9 Ag2 C14 105.31(14) . . ? C15 Ag2 C14 32.28(14) . . ? C6 Ag2 C14 156.90(17) . . ? O9 Ag2 C5 125.14(14) . . ? C15 Ag2 C5 102.89(16) . . ? C6 Ag2 C5 31.63(15) . . ? C14 Ag2 C5 125.42(16) . . ? O9 Ag2 N2 91.49(12) . . ? C15 Ag2 N2 96.94(14) . . ? C6 Ag2 N2 93.65(12) . . ? C14 Ag2 N2 79.55(11) . . ? C5 Ag2 N2 79.71(11) . . ? Ag2 O9 H9A 98(4) . . ? Ag2 O9 H9B 127(7) . . ? H9A O9 H9B 101(7) . . ? N1 C1 N3 129.6(3) . . ? N1 C1 Cl1 115.5(2) . . ? N3 C1 Cl1 114.9(2) . . ? C1 N1 C2 112.6(3) . . ? C1 N1 Ag1 113.5(2) . 2_666 ? C2 N1 Ag1 115.4(2) . 2_666 ? N2 C2 N4 117.3(3) . . ? N2 C2 N1 124.8(3) . . ? N4 C2 N1 117.9(3) . . ? C2 N2 C3 115.4(3) . . ? C2 N2 Ag2 111.0(2) . . ? C3 N2 Ag2 110.7(2) . . ? C2 N4 C4 120.3(3) . . ? C2 N4 C7 121.2(3) . . ? C4 N4 C7 118.5(3) . . ? N4 C4 C5 113.5(3) . . ? N4 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N4 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 125.9(4) . . ? C6 C5 Ag2 70.1(2) . . ? C4 C5 Ag2 105.3(2) . . ? C6 C5 H5 117.0 . . ? C4 C5 H5 117.0 . . ? Ag2 C5 H5 94.8 . . ? C5 C6 Ag2 78.3(2) . . ? C5 C6 H6A 120.0 . . ? Ag2 C6 H6A 100.0 . . ? C5 C6 H6B 120.0 . . ? Ag2 C6 H6B 91.7 . . ? H6A C6 H6B 120.0 . . ? N4 C7 C8 113.9(3) . . ? N4 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N4 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 125.4(3) . . ? C9 C8 Ag1 73.9(2) . 2_666 ? C7 C8 Ag1 102.0(2) . 2_666 ? C9 C8 H8 117.3 . . ? C7 C8 H8 117.3 . . ? Ag1 C8 H8 94.4 2_666 . ? C8 C9 Ag1 73.9(2) . 2_666 ? C8 C9 H9C 120.0 . . ? Ag1 C9 H9C 100.9 2_666 . ? C8 C9 H9D 120.0 . . ? Ag1 C9 H9D 95.1 2_666 . ? H9C C9 H9D 120.0 . . ? N5 C3 N2 117.2(3) . . ? N5 C3 N3 118.1(3) . . ? N2 C3 N3 124.8(3) . . ? C1 N3 C3 112.6(3) . . ? C1 N3 Ag1 115.1(2) . . ? C3 N3 Ag1 121.2(2) . . ? C3 N5 C13 120.6(3) . . ? C3 N5 C10 121.6(3) . . ? C13 N5 C10 117.8(3) . . ? N5 C10 C11 114.2(3) . . ? N5 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? N5 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C10 125.9(3) . . ? C12 C11 Ag1 74.2(2) . . ? C10 C11 Ag1 100.2(2) . . ? C12 C11 H11 117.0 . . ? C10 C11 H11 117.0 . . ? Ag1 C11 H11 96.1 . . ? C11 C12 Ag1 74.4(2) . . ? C11 C12 H12A 120.0 . . ? Ag1 C12 H12A 98.8 . . ? C11 C12 H12B 120.0 . . ? Ag1 C12 H12B 96.7 . . ? H12A C12 H12B 120.0 . . ? N5 C13 C14 115.0(3) . . ? N5 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? N5 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C13 122.6(4) . . ? C15 C14 Ag2 71.0(2) . . ? C13 C14 Ag2 108.9(2) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? Ag2 C14 H14 90.1 . . ? C14 C15 Ag2 76.8(3) . . ? C14 C15 H15A 120.0 . . ? Ag2 C15 H15A 105.8 . . ? C14 C15 H15B 120.0 . . ? Ag2 C15 H15B 87.5 . . ? H15A C15 H15B 120.0 . . ? O8 Cl3 O5 110.3(3) . . ? O8 Cl3 O7 107.7(3) . . ? O5 Cl3 O7 108.0(3) . . ? O8 Cl3 O6 110.07(19) . . ? O5 Cl3 O6 111.2(2) . . ? O7 Cl3 O6 109.5(2) . . ? O1 Cl2 O4 109.5(2) . . ? O1 Cl2 O3 108.8(2) . . ? O4 Cl2 O3 109.2(2) . . ? O1 Cl2 O2 112.5(3) . . ? O4 Cl2 O2 109.7(2) . . ? O3 Cl2 O2 107.1(2) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O10 C17 C18 120.9(5) . . ? O10 C17 C16 120.8(5) . . ? C18 C17 C16 118.1(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.203 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 940158' ####################################################################### # # 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_complex5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H20 Ag2 Cl F6 N5 O6 S2' _chemical_formula_sum 'C17 H20 Ag2 Cl F6 N5 O6 S2' _chemical_formula_weight 819.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 41.519(6) _cell_length_b 41.519(6) _cell_length_c 9.1478(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13657(4) _cell_formula_units_Z 18 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 6323 _cell_measurement_theta_min 3.6848 _cell_measurement_theta_max 73.4614 _exptl_crystal_description block _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7236 _exptl_absorpt_coefficient_mu 1.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.29076 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 114(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13776 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5354 _reflns_number_gt 4740 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+74.6638P] 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 5354 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Ag2 Ag 0.303776(10) 0.115423(11) -0.11467(4) 0.03042(16) Uani 1 1 d . . . Ag1 Ag 0.459474(10) 0.133304(10) -0.39494(4) 0.02673(15) Uani 1 1 d . . . C1 C 0.34624(13) 0.13932(12) -0.4228(5) 0.0233(9) Uani 1 1 d . . . N1 N 0.37381(11) 0.16658(11) -0.4956(5) 0.0252(8) Uani 1 1 d . . . C2 C 0.40805(13) 0.17554(12) -0.4420(5) 0.0233(9) Uani 1 1 d . . . N2 N 0.41344(11) 0.15844(11) -0.3268(4) 0.0253(8) Uani 1 1 d . . . C3 C 0.38300(14) 0.13310(13) -0.2582(5) 0.0246(9) Uani 1 1 d . . . N3 N 0.34737(11) 0.12183(11) -0.3031(4) 0.0236(8) Uani 1 1 d . . . Cl1 Cl 0.30227(3) 0.12491(3) -0.49268(13) 0.0269(3) Uani 1 1 d . . . N4 N 0.38775(11) 0.11773(11) -0.1373(5) 0.0253(8) Uani 1 1 d . . . C4 C 0.42475(14) 0.13433(14) -0.0691(6) 0.0295(10) Uani 1 1 d . . . H4A H 0.4216 0.1303 0.0357 0.035 Uiso 1 1 calc R . . H4B H 0.4377 0.1610 -0.0859 0.035 Uiso 1 1 calc R . . C5 C 0.44841(15) 0.11928(15) -0.1238(6) 0.0310(11) Uani 1 1 d . . . H5 H 0.4736 0.1326 -0.1015 0.037 Uiso 1 1 calc R . . C6 C 0.43622(16) 0.08823(15) -0.2022(6) 0.0343(11) Uani 1 1 d . . . H6A H 0.4112 0.0742 -0.2267 0.041 Uiso 1 1 calc R . . H6B H 0.4528 0.0806 -0.2324 0.041 Uiso 1 1 calc R . . C7 C 0.35677(14) 0.08495(13) -0.0665(5) 0.0269(10) Uani 1 1 d . . . H7A H 0.3665 0.0707 -0.0188 0.032 Uiso 1 1 calc R . . H7B H 0.3394 0.0693 -0.1411 0.032 Uiso 1 1 calc R . . C8 C 0.33620(15) 0.09481(15) 0.0451(6) 0.0312(11) Uani 1 1 d . . . H8 H 0.3147 0.0754 0.0855 0.037 Uiso 1 1 calc R . . C9 C 0.34670(16) 0.12975(16) 0.0908(6) 0.0337(11) Uani 1 1 d . . . H9A H 0.3681 0.1499 0.0529 0.040 Uiso 1 1 calc R . . H9B H 0.3325 0.1336 0.1600 0.040 Uiso 1 1 calc R . . N5 N 0.43841(12) 0.20328(12) -0.5062(5) 0.0278(9) Uani 1 1 d . . . C10 C 0.47461(14) 0.21808(14) -0.4351(6) 0.0330(11) Uani 1 1 d . . . H10A H 0.4709 0.2155 -0.3301 0.040 Uiso 1 1 calc R . . H10B H 0.4894 0.2444 -0.4568 0.040 Uiso 1 1 calc R . . C11 C 0.49592(14) 0.19921(14) -0.4814(7) 0.0348(12) Uani 1 1 d . . . H11 H 0.5165 0.2037 -0.4253 0.042 Uiso 1 1 calc R . . C12 C 0.48787(15) 0.17663(15) -0.5957(6) 0.0349(12) Uani 1 1 d . . . H12A H 0.4676 0.1714 -0.6547 0.042 Uiso 1 1 calc R . . H12B H 0.5025 0.1661 -0.6167 0.042 Uiso 1 1 calc R . . C13 C 0.43608(15) 0.22055(15) -0.6420(6) 0.0325(11) Uani 1 1 d . . . H13A H 0.4167 0.2017 -0.7029 0.039 Uiso 1 1 calc R . . H13B H 0.4594 0.2302 -0.6942 0.039 Uiso 1 1 calc R . . C14 C 0.42782(14) 0.25180(14) -0.6180(6) 0.0313(11) Uani 1 1 d . . . H14 H 0.4237 0.2623 -0.7005 0.038 Uiso 1 1 calc R . . C15 C 0.42604(15) 0.26549(15) -0.4883(7) 0.0366(12) Uani 1 1 d . . . H15A H 0.4300 0.2558 -0.4032 0.044 Uiso 1 1 calc R . . H15B H 0.4208 0.2848 -0.4831 0.044 Uiso 1 1 calc R . . S1 S 0.40122(3) 0.08136(3) -0.65932(13) 0.0261(3) Uani 1 1 d . . . O1 O 0.40118(11) 0.11612(11) -0.6620(5) 0.0419(9) Uani 1 1 d . . . O2 O 0.40023(11) 0.06485(12) -0.7988(4) 0.0379(9) Uani 1 1 d . . . O3 O 0.42787(10) 0.08078(10) -0.5571(4) 0.0317(8) Uani 1 1 d . . . C16 C 0.35644(15) 0.04906(15) -0.5773(6) 0.0307(10) Uani 1 1 d . . . F1 F 0.35521(10) 0.05842(10) -0.4370(4) 0.0429(8) Uani 1 1 d . . . F2 F 0.32874(9) 0.04964(10) -0.6488(4) 0.0425(8) Uani 1 1 d . . . F3 F 0.34992(9) 0.01446(8) -0.5776(4) 0.0375(7) Uani 1 1 d . . . S2 S 0.54529(4) 0.13290(6) -0.29924(18) 0.0494(4) Uani 1 1 d . . . O4 O 0.52325(14) 0.13509(16) -0.4148(5) 0.0533(12) Uani 1 1 d . . . O5 O 0.53427(17) 0.1363(3) -0.1555(6) 0.113(3) Uani 1 1 d . . . O6 O 0.55198(17) 0.10209(19) -0.3145(10) 0.093(2) Uani 1 1 d . . . C17 C 0.5900(2) 0.1731(2) -0.3285(8) 0.0622(19) Uani 1 1 d . . . F4 F 0.5878(3) 0.2042(2) -0.3239(11) 0.131(3) Uani 1 1 d . . . F5 F 0.60417(16) 0.1726(2) -0.4555(6) 0.107(2) Uani 1 1 d . . . F6 F 0.61458(14) 0.17681(19) -0.2263(6) 0.0929(19) 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 Ag2 0.0261(2) 0.0338(2) 0.0381(3) 0.01376(15) 0.00654(14) 0.02007(17) Ag1 0.0261(2) 0.0247(2) 0.0343(2) -0.00210(14) -0.00217(13) 0.01642(16) C1 0.023(2) 0.020(2) 0.030(2) -0.0029(18) -0.0010(18) 0.0141(19) N1 0.026(2) 0.0219(19) 0.032(2) 0.0010(16) 0.0032(16) 0.0149(17) C2 0.028(2) 0.019(2) 0.028(2) 0.0012(17) 0.0024(18) 0.0162(19) N2 0.026(2) 0.0221(19) 0.032(2) 0.0021(16) 0.0006(16) 0.0155(17) C3 0.031(2) 0.017(2) 0.032(2) 0.0004(17) 0.0003(19) 0.0164(19) N3 0.026(2) 0.0215(19) 0.029(2) 0.0010(15) 0.0013(16) 0.0161(16) Cl1 0.0246(6) 0.0239(5) 0.0334(6) 0.0013(4) -0.0019(4) 0.0132(5) N4 0.024(2) 0.0206(19) 0.033(2) 0.0045(16) -0.0001(16) 0.0121(16) C4 0.030(2) 0.026(2) 0.032(3) 0.0029(19) -0.003(2) 0.014(2) C5 0.030(3) 0.032(3) 0.034(3) 0.005(2) -0.004(2) 0.018(2) C6 0.037(3) 0.030(3) 0.043(3) 0.004(2) 0.001(2) 0.023(2) C7 0.029(2) 0.024(2) 0.031(2) 0.0052(19) 0.0015(19) 0.016(2) C8 0.032(3) 0.034(3) 0.030(2) 0.009(2) 0.000(2) 0.019(2) C9 0.038(3) 0.036(3) 0.030(3) 0.002(2) 0.000(2) 0.021(2) N5 0.026(2) 0.026(2) 0.036(2) 0.0077(17) 0.0050(17) 0.0167(17) C10 0.028(3) 0.025(2) 0.044(3) 0.001(2) 0.000(2) 0.012(2) C11 0.020(2) 0.028(3) 0.054(3) 0.005(2) -0.001(2) 0.011(2) C12 0.031(3) 0.030(3) 0.048(3) 0.008(2) 0.006(2) 0.019(2) C13 0.031(3) 0.034(3) 0.037(3) 0.013(2) 0.011(2) 0.020(2) C14 0.025(2) 0.029(3) 0.041(3) 0.012(2) 0.006(2) 0.014(2) C15 0.035(3) 0.024(2) 0.053(3) 0.004(2) -0.002(2) 0.017(2) S1 0.0219(6) 0.0268(6) 0.0307(6) -0.0001(4) -0.0023(4) 0.0131(5) O1 0.032(2) 0.0287(19) 0.066(3) 0.0036(18) -0.0055(18) 0.0161(17) O2 0.0317(19) 0.047(2) 0.0333(19) -0.0006(16) 0.0022(15) 0.0184(18) O3 0.0292(18) 0.0340(19) 0.0357(19) -0.0047(15) -0.0070(15) 0.0188(16) C16 0.031(3) 0.032(3) 0.032(3) -0.003(2) 0.000(2) 0.018(2) F1 0.0467(19) 0.050(2) 0.0353(17) -0.0070(14) 0.0074(14) 0.0268(16) F2 0.0233(15) 0.0473(19) 0.057(2) 0.0069(16) -0.0015(14) 0.0178(14) F3 0.0399(17) 0.0263(15) 0.0439(18) 0.0002(13) 0.0020(14) 0.0147(13) S2 0.0377(8) 0.0788(12) 0.0423(8) 0.0089(7) -0.0016(6) 0.0371(8) O4 0.058(3) 0.083(4) 0.042(2) -0.005(2) -0.009(2) 0.053(3) O5 0.049(3) 0.237(10) 0.043(3) 0.009(4) 0.000(2) 0.063(5) O6 0.053(3) 0.076(4) 0.156(7) 0.045(4) -0.003(4) 0.037(3) C17 0.069(5) 0.057(4) 0.049(4) 0.000(3) -0.001(3) 0.022(4) F4 0.142(7) 0.070(4) 0.176(8) -0.020(4) -0.027(6) 0.048(4) F5 0.072(3) 0.125(5) 0.059(3) -0.007(3) 0.012(3) -0.001(3) F6 0.050(3) 0.120(5) 0.071(3) 0.005(3) -0.008(2) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag2 C14 2.412(5) 13_554 ? Ag2 C8 2.415(5) . ? Ag2 N3 2.416(4) . ? Ag2 C15 2.436(6) 13_554 ? Ag2 N1 2.446(4) 13_554 ? Ag2 C9 2.450(5) . ? Ag1 C6 2.395(5) . ? Ag1 O3 2.412(4) . ? Ag1 C12 2.425(5) . ? Ag1 C11 2.502(5) . ? Ag1 C5 2.537(5) . ? C1 N1 1.319(6) . ? C1 N3 1.328(6) . ? C1 Cl1 1.734(5) . ? N1 C2 1.368(6) . ? N1 Ag2 2.446(4) 13_554 ? C2 N5 1.345(7) . ? C2 N2 1.350(6) . ? N2 C3 1.330(7) . ? C3 N4 1.340(6) . ? C3 N3 1.373(6) . ? N4 C4 1.472(6) . ? N4 C7 1.475(6) . ? C4 C5 1.490(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.335(8) . ? C5 H5 0.9300 . ? C6 H6A 0.9300 . ? C6 H6B 0.9300 . ? C7 C8 1.513(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.355(8) . ? C8 H8 0.9300 . ? C9 H9A 0.9300 . ? C9 H9B 0.9300 . ? N5 C13 1.462(7) . ? N5 C10 1.461(7) . ? C10 C11 1.507(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.331(9) . ? C11 H11 0.9300 . ? C12 H12A 0.9300 . ? C12 H12B 0.9300 . ? C13 C14 1.514(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.333(8) . ? C14 Ag2 2.412(5) 13_554 ? C14 H14 0.9300 . ? C15 Ag2 2.436(6) 13_554 ? C15 H15A 0.9300 . ? C15 H15B 0.9300 . ? S1 O2 1.439(4) . ? S1 O1 1.444(4) . ? S1 O3 1.458(4) . ? S1 C16 1.824(5) . ? C16 F3 1.322(6) . ? C16 F2 1.334(6) . ? C16 F1 1.350(6) . ? S2 O5 1.422(7) . ? S2 O4 1.430(5) . ? S2 O6 1.445(7) . ? S2 C17 1.791(8) . ? C17 F5 1.307(10) . ? C17 F6 1.336(10) . ? C17 F4 1.339(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Ag2 C8 107.47(18) 13_554 . ? C14 Ag2 N3 143.13(17) 13_554 . ? C8 Ag2 N3 87.21(15) . . ? C14 Ag2 C15 31.9(2) 13_554 13_554 ? C8 Ag2 C15 114.95(18) . 13_554 ? N3 Ag2 C15 111.22(17) . 13_554 ? C14 Ag2 N1 85.47(15) 13_554 13_554 ? C8 Ag2 N1 144.64(17) . 13_554 ? N3 Ag2 N1 102.05(13) . 13_554 ? C15 Ag2 N1 93.60(16) 13_554 13_554 ? C14 Ag2 C9 114.50(19) 13_554 . ? C8 Ag2 C9 32.34(19) . . ? N3 Ag2 C9 96.13(16) . . ? C15 Ag2 C9 137.52(19) 13_554 . ? N1 Ag2 C9 112.31(16) 13_554 . ? C6 Ag1 O3 85.50(17) . . ? C6 Ag1 C12 173.66(18) . . ? O3 Ag1 C12 92.74(17) . . ? C6 Ag1 C11 151.0(2) . . ? O3 Ag1 C11 123.55(17) . . ? C12 Ag1 C11 31.3(2) . . ? C6 Ag1 C5 31.23(18) . . ? O3 Ag1 C5 116.08(15) . . ? C12 Ag1 C5 151.18(19) . . ? C11 Ag1 C5 120.07(19) . . ? N1 C1 N3 129.3(4) . . ? N1 C1 Cl1 115.0(4) . . ? N3 C1 Cl1 115.7(4) . . ? C1 N1 C2 113.0(4) . . ? C1 N1 Ag2 113.3(3) . 13_554 ? C2 N1 Ag2 117.3(3) . 13_554 ? N5 C2 N2 117.4(4) . . ? N5 C2 N1 118.6(4) . . ? N2 C2 N1 124.0(4) . . ? C3 N2 C2 116.3(4) . . ? N2 C3 N4 117.3(4) . . ? N2 C3 N3 124.4(4) . . ? N4 C3 N3 118.4(4) . . ? C1 N3 C3 112.8(4) . . ? C1 N3 Ag2 114.8(3) . . ? C3 N3 Ag2 116.4(3) . . ? C3 N4 C4 119.7(4) . . ? C3 N4 C7 122.3(4) . . ? C4 N4 C7 118.1(4) . . ? N4 C4 C5 114.4(4) . . ? N4 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? N4 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C6 C5 C4 125.1(5) . . ? C6 C5 Ag1 68.5(3) . . ? C4 C5 Ag1 108.3(3) . . ? C6 C5 H5 117.5 . . ? C4 C5 H5 117.5 . . ? Ag1 C5 H5 93.3 . . ? C5 C6 Ag1 80.3(3) . . ? C5 C6 H6A 120.0 . . ? Ag1 C6 H6A 101.6 . . ? C5 C6 H6B 120.0 . . ? Ag1 C6 H6B 88.2 . . ? H6A C6 H6B 120.0 . . ? N4 C7 C8 113.4(4) . . ? N4 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N4 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 125.1(5) . . ? C9 C8 Ag2 75.2(3) . . ? C7 C8 Ag2 100.2(3) . . ? C9 C8 H8 117.5 . . ? C7 C8 H8 117.5 . . ? Ag2 C8 H8 94.8 . . ? C8 C9 Ag2 72.4(3) . . ? C8 C9 H9A 120.0 . . ? Ag2 C9 H9A 100.6 . . ? C8 C9 H9B 120.0 . . ? Ag2 C9 H9B 96.8 . . ? H9A C9 H9B 120.0 . . ? C2 N5 C13 121.8(4) . . ? C2 N5 C10 119.5(4) . . ? C13 N5 C10 118.6(4) . . ? N5 C10 C11 113.8(4) . . ? N5 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N5 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 125.5(5) . . ? C12 C11 Ag1 71.1(3) . . ? C10 C11 Ag1 106.8(3) . . ? C12 C11 H11 117.2 . . ? C10 C11 H11 117.2 . . ? Ag1 C11 H11 92.2 . . ? C11 C12 Ag1 77.6(3) . . ? C11 C12 H12A 120.0 . . ? Ag1 C12 H12A 102.6 . . ? C11 C12 H12B 120.0 . . ? Ag1 C12 H12B 89.8 . . ? H12A C12 H12B 120.0 . . ? N5 C13 C14 113.3(4) . . ? N5 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? N5 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C13 125.4(5) . . ? C15 C14 Ag2 75.0(3) . 13_554 ? C13 C14 Ag2 101.7(3) . 13_554 ? C15 C14 H14 117.3 . . ? C13 C14 H14 117.3 . . ? Ag2 C14 H14 93.5 13_554 . ? C14 C15 Ag2 73.0(3) . 13_554 ? C14 C15 H15A 120.0 . . ? Ag2 C15 H15A 101.6 13_554 . ? C14 C15 H15B 120.0 . . ? Ag2 C15 H15B 95.2 13_554 . ? H15A C15 H15B 120.0 . . ? O2 S1 O1 116.6(3) . . ? O2 S1 O3 113.7(2) . . ? O1 S1 O3 114.0(2) . . ? O2 S1 C16 103.8(2) . . ? O1 S1 C16 103.4(2) . . ? O3 S1 C16 103.1(2) . . ? S1 O3 Ag1 117.0(2) . . ? F3 C16 F2 108.0(4) . . ? F3 C16 F1 107.4(4) . . ? F2 C16 F1 107.7(4) . . ? F3 C16 S1 112.2(4) . . ? F2 C16 S1 110.9(4) . . ? F1 C16 S1 110.5(4) . . ? O5 S2 O4 115.5(3) . . ? O5 S2 O6 112.9(5) . . ? O4 S2 O6 113.4(4) . . ? O5 S2 C17 106.3(4) . . ? O4 S2 C17 103.2(4) . . ? O6 S2 C17 104.1(4) . . ? F5 C17 F6 107.4(8) . . ? F5 C17 F4 107.1(8) . . ? F6 C17 F4 106.5(7) . . ? F5 C17 S2 112.4(6) . . ? F6 C17 S2 112.2(6) . . ? F4 C17 S2 110.9(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.927 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.165 _database_code_depnum_ccdc_archive 'CCDC 940159' ####################################################################### # # 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_3sw37 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H31 Ag2 F6 N5 O6 S2' _chemical_formula_sum 'C24 H31 Ag2 F6 N5 O6 S2' _chemical_formula_weight 879.40 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' 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 12.4040(4) _cell_length_b 22.1684(8) _cell_length_c 23.4044(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.655(2) _cell_angle_gamma 90.00 _cell_volume 6378.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 112(2) _cell_measurement_reflns_used 9805 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 25.69 _exptl_crystal_description block _exptl_crystal_colour gold _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 1.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5635 _exptl_absorpt_correction_T_max 0.6106 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 112(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 127348 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.72 _reflns_number_total 12139 _reflns_number_gt 9382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0581P)^2^+29.3231P] 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 12139 _refine_ls_number_parameters 816 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Ag1 Ag 0.51251(3) 0.499729(19) 0.317035(18) 0.03662(12) Uani 1 1 d . . . Ag2 Ag 0.54746(4) 0.72107(2) 0.34978(2) 0.04693(13) Uani 1 1 d . . . Ag3 Ag -0.03195(3) 0.495740(18) 0.143001(18) 0.03427(11) Uani 1 1 d . . . Ag4 Ag -0.00188(3) 0.718266(18) 0.205910(17) 0.03180(11) Uani 1 1 d . . . N1 N 0.7035(3) 0.66042(18) 0.32582(19) 0.0301(9) Uani 1 1 d . . . N2 N 0.6843(3) 0.55414(18) 0.30880(18) 0.0297(9) Uani 1 1 d . . . N3 N 0.7827(4) 0.4854(2) 0.3679(2) 0.0421(12) Uani 1 1 d . . . N4 N 0.8131(4) 0.6976(2) 0.40526(19) 0.0357(10) Uani 1 1 d . . . N5 N 0.5989(3) 0.62292(19) 0.24410(18) 0.0299(9) Uani 1 1 d . . . N6 N 0.1484(3) 0.54928(18) 0.16770(18) 0.0271(9) Uani 1 1 d . . . N7 N 0.1732(3) 0.65205(18) 0.20083(18) 0.0272(9) Uani 1 1 d . . . N8 N 0.1076(3) 0.57902(19) 0.25682(18) 0.0299(9) Uani 1 1 d . . . N9 N 0.1985(4) 0.5194(2) 0.0810(2) 0.0352(10) Uani 1 1 d . . . N10 N 0.2436(3) 0.72485(19) 0.1464(2) 0.0352(10) Uani 1 1 d . . . C1 C 0.7594(4) 0.5445(2) 0.3555(2) 0.0341(12) Uani 1 1 d . . . C2 C 0.8110(4) 0.5905(2) 0.3883(2) 0.0341(12) Uani 1 1 d . . . H2A H 0.8671 0.5829 0.4193 0.041 Uiso 1 1 calc R . . C3 C 0.7754(4) 0.6488(2) 0.3731(2) 0.0300(11) Uani 1 1 d . . . C4 C 0.6649(4) 0.6121(2) 0.2944(2) 0.0267(10) Uani 1 1 d . . . C5 C 0.7372(5) 0.4380(3) 0.3297(3) 0.0485(16) Uani 1 1 d . . . H5A H 0.7892 0.4039 0.3320 0.058 Uiso 1 1 calc R . . H5B H 0.7281 0.4532 0.2896 0.058 Uiso 1 1 calc R . . C6 C 0.6286(5) 0.4150(3) 0.3434(3) 0.0504(17) Uani 1 1 d . . . H6A H 0.5900 0.3876 0.3169 0.060 Uiso 1 1 calc R . . C7 C 0.5835(6) 0.4302(3) 0.3892(3) 0.061(2) Uani 1 1 d . . . H7A H 0.6196 0.4575 0.4166 0.073 Uiso 1 1 calc R . . H7B H 0.5149 0.4138 0.3948 0.073 Uiso 1 1 calc R . . C8 C 0.8580(5) 0.4678(3) 0.4187(3) 0.0575(19) Uani 1 1 d . . . H8A H 0.8372 0.4275 0.4318 0.069 Uiso 1 1 calc R . . H8B H 0.8520 0.4969 0.4502 0.069 Uiso 1 1 calc R . . C9 C 0.9745(6) 0.4658(4) 0.4066(4) 0.081(3) Uani 1 1 d . . . H9A H 0.9783 0.4507 0.3689 0.097 Uiso 1 1 calc R . . C10 C 1.0532(9) 0.4763(10) 0.4276(4) 0.226(12) Uani 1 1 d . . . H10A H 1.0620 0.4919 0.4657 0.271 Uiso 1 1 calc R . . H10B H 1.1149 0.4700 0.4083 0.271 Uiso 1 1 calc R . . C11 C 0.7878(5) 0.7585(3) 0.3857(3) 0.0438(14) Uani 1 1 d . . . H11A H 0.7801 0.7594 0.3431 0.053 Uiso 1 1 calc R . . H11B H 0.8491 0.7852 0.4004 0.053 Uiso 1 1 calc R . . C12 C 0.6847(6) 0.7827(3) 0.4051(3) 0.0584(18) Uani 1 1 d . . . H12A H 0.6593 0.8209 0.3908 0.070 Uiso 1 1 calc R . . C13 C 0.6262(6) 0.7538(4) 0.4414(3) 0.074(2) Uani 1 1 d . . . H13A H 0.6491 0.7155 0.4566 0.089 Uiso 1 1 calc R . . H13B H 0.5620 0.7719 0.4517 0.089 Uiso 1 1 calc R . . C14 C 0.8843(5) 0.6909(3) 0.4609(2) 0.0420(14) Uani 1 1 d . . . H14A H 0.8643 0.6536 0.4802 0.050 Uiso 1 1 calc R . . H14B H 0.8723 0.7255 0.4861 0.050 Uiso 1 1 calc R . . C15 C 1.0016(5) 0.6882(3) 0.4536(3) 0.0480(15) Uani 1 1 d . . . H15A H 1.0267 0.6529 0.4364 0.058 Uiso 1 1 calc R . . C16 C 1.0731(6) 0.7310(4) 0.4692(3) 0.066(2) Uani 1 1 d . . . H16A H 1.0510 0.7669 0.4865 0.079 Uiso 1 1 calc R . . H16B H 1.1468 0.7260 0.4631 0.079 Uiso 1 1 calc R . . C17 C 0.5842(4) 0.6848(2) 0.2226(2) 0.0364(12) Uani 1 1 d . . . H17A H 0.5683 0.6836 0.1800 0.044 Uiso 1 1 calc R . . H17B H 0.6534 0.7070 0.2326 0.044 Uiso 1 1 calc R . . C18 C 0.4951(5) 0.7193(3) 0.2457(3) 0.0420(13) Uani 1 1 d . . . H18A H 0.4291 0.6989 0.2496 0.050 Uiso 1 1 calc R . . C19 C 0.5048(6) 0.7767(3) 0.2608(3) 0.0583(18) Uani 1 1 d . . . H19A H 0.5701 0.7978 0.2572 0.070 Uiso 1 1 calc R . . H19B H 0.4463 0.7968 0.2752 0.070 Uiso 1 1 calc R . . C20 C 0.5509(4) 0.5733(3) 0.2083(2) 0.0343(12) Uani 1 1 d . . . H20A H 0.6060 0.5411 0.2081 0.041 Uiso 1 1 calc R . . H20B H 0.5331 0.5881 0.1683 0.041 Uiso 1 1 calc R . . C21 C 0.4491(4) 0.5461(3) 0.2271(2) 0.0365(12) Uani 1 1 d . . . H21A H 0.4007 0.5719 0.2438 0.044 Uiso 1 1 calc R . . C22 C 0.4242(5) 0.4877(3) 0.2212(3) 0.0469(15) Uani 1 1 d . . . H22A H 0.4713 0.4610 0.2046 0.056 Uiso 1 1 calc R . . H22B H 0.3594 0.4728 0.2337 0.056 Uiso 1 1 calc R . . C23 C 0.3496(11) 0.6041(8) 0.4495(5) 0.128(5) Uani 1 1 d . . . C24 C 0.1923(4) 0.5642(2) 0.1194(2) 0.0298(11) Uani 1 1 d . . . C25 C 0.2298(4) 0.6222(2) 0.1109(2) 0.0324(11) Uani 1 1 d . . . H25A H 0.2642 0.6318 0.0781 0.039 Uiso 1 1 calc R . . C26 C 0.2151(4) 0.6658(2) 0.1519(2) 0.0281(11) Uani 1 1 d . . . C27 C 0.1452(4) 0.5941(2) 0.2066(2) 0.0265(10) Uani 1 1 d . . . C28 C 0.1110(5) 0.6243(3) 0.3033(2) 0.0369(12) Uani 1 1 d . . . H28A H 0.1786 0.6481 0.3039 0.044 Uiso 1 1 calc R . . H28B H 0.1152 0.6027 0.3406 0.044 Uiso 1 1 calc R . . C29 C 0.0162(5) 0.6673(3) 0.2990(2) 0.0402(13) Uani 1 1 d . . . H29A H -0.0554 0.6521 0.2888 0.048 Uiso 1 1 calc R . . C30 C 0.0304(6) 0.7264(3) 0.3090(2) 0.0453(15) Uani 1 1 d . . . H30A H 0.1016 0.7422 0.3192 0.054 Uiso 1 1 calc R . . H30B H -0.0308 0.7526 0.3060 0.054 Uiso 1 1 calc R . . C31 C 0.0860(4) 0.5160(2) 0.2695(2) 0.0350(12) Uani 1 1 d . . . H31A H 0.0996 0.5100 0.3117 0.042 Uiso 1 1 calc R . . H31B H 0.1381 0.4903 0.2519 0.042 Uiso 1 1 calc R . . C32 C -0.0275(4) 0.4953(2) 0.2480(2) 0.0360(12) Uani 1 1 d . . . H32A H -0.0423 0.4534 0.2504 0.043 Uiso 1 1 calc R . . C33 C -0.1098(4) 0.5310(3) 0.2257(3) 0.0396(13) Uani 1 1 d . . . H33A H -0.0985 0.5731 0.2225 0.047 Uiso 1 1 calc R . . H33B H -0.1793 0.5141 0.2131 0.047 Uiso 1 1 calc R . . C34 C 0.2278(5) 0.5318(3) 0.0230(3) 0.0427(13) Uani 1 1 d . . . H34A H 0.1974 0.5716 0.0100 0.051 Uiso 1 1 calc R . . H34B H 0.1929 0.5010 -0.0040 0.051 Uiso 1 1 calc R . . C35 C 0.3470(5) 0.5321(3) 0.0193(3) 0.0520(16) Uani 1 1 d . . . H35A H 0.3692 0.5395 -0.0173 0.062 Uiso 1 1 calc R . . C36 C 0.4224(5) 0.5232(4) 0.0622(3) 0.061(2) Uani 1 1 d . . . H36A H 0.4036 0.5157 0.0996 0.073 Uiso 1 1 calc R . . H36B H 0.4967 0.5241 0.0563 0.073 Uiso 1 1 calc R . . C37 C 0.1825(4) 0.4562(2) 0.0955(3) 0.0367(12) Uani 1 1 d . . . H37A H 0.2064 0.4507 0.1373 0.044 Uiso 1 1 calc R . . H37B H 0.2299 0.4310 0.0745 0.044 Uiso 1 1 calc R . . C38 C 0.0681(4) 0.4338(2) 0.0821(3) 0.0376(12) Uani 1 1 d . . . H38A H 0.0259 0.4467 0.0473 0.045 Uiso 1 1 calc R . . C39 C 0.0233(5) 0.3967(2) 0.1166(3) 0.0450(14) Uani 1 1 d . . . H39A H 0.0641 0.3833 0.1516 0.054 Uiso 1 1 calc R . . H39B H -0.0496 0.3835 0.1065 0.054 Uiso 1 1 calc R . . C40 C 0.2787(4) 0.7477(3) 0.0932(3) 0.0418(14) Uani 1 1 d . . . H40A H 0.2556 0.7903 0.0878 0.050 Uiso 1 1 calc R . . H40B H 0.2421 0.7243 0.0602 0.050 Uiso 1 1 calc R . . C41 C 0.3991(5) 0.7439(4) 0.0932(3) 0.0546(18) Uani 1 1 d . . . H41A H 0.4428 0.7623 0.1250 0.066 Uiso 1 1 calc R . . C42 C 0.4464(7) 0.7208(6) 0.0582(4) 0.104(4) Uani 1 1 d . . . H42A H 0.4070 0.7017 0.0255 0.125 Uiso 1 1 calc R . . H42B H 0.5237 0.7212 0.0628 0.125 Uiso 1 1 calc R . . C43 C 0.2262(4) 0.7689(2) 0.1900(3) 0.0363(12) Uani 1 1 d . . . H43A H 0.2828 0.8006 0.1910 0.044 Uiso 1 1 calc R . . H43B H 0.2350 0.7489 0.2281 0.044 Uiso 1 1 calc R . . C44 C 0.1158(4) 0.7983(2) 0.1799(3) 0.0351(12) Uani 1 1 d . . . H44A H 0.0977 0.8258 0.2083 0.042 Uiso 1 1 calc R . . C45 C 0.0415(5) 0.7886(2) 0.1341(3) 0.0387(13) Uani 1 1 d . . . H45A H 0.0567 0.7615 0.1048 0.046 Uiso 1 1 calc R . . H45B H -0.0265 0.8089 0.1307 0.046 Uiso 1 1 calc R . . C46 C -0.2552(5) 0.6352(3) 0.0735(3) 0.0466(15) Uani 1 1 d . . . C47 C 0.3218(7) 0.8405(4) 0.3926(4) 0.069(2) Uani 1 1 d . . . C48 C -0.2788(5) 0.8569(3) 0.1540(4) 0.0581(18) Uani 1 1 d . . . S1 S 0.4109(2) 0.60124(10) 0.38649(12) 0.0808(7) Uani 1 1 d . . . S2 S -0.10804(11) 0.63040(6) 0.08164(6) 0.0327(3) Uani 1 1 d . . . S3 S 0.27730(16) 0.89396(10) 0.33695(9) 0.0426(8) Uani 0.798(8) 1 d P A 1 S3' S 0.2929(10) 0.8592(7) 0.3217(5) 0.073(4) Uiso 0.202(8) 1 d P A 2 S4 S -0.19359(12) 0.83973(7) 0.22132(7) 0.0437(4) Uani 1 1 d . . . O1 O 0.5041(9) 0.5897(5) 0.4078(5) 0.206(6) Uani 1 1 d . . . O2 O 0.3452(8) 0.5542(3) 0.3538(4) 0.136(3) Uani 1 1 d . . . O3 O 0.3959(7) 0.6591(3) 0.3647(3) 0.112(2) Uani 1 1 d . . . O4 O -0.0779(4) 0.6729(2) 0.0406(2) 0.0621(13) Uani 1 1 d . . . O5 O -0.0784(4) 0.64563(18) 0.14163(18) 0.0469(10) Uani 1 1 d . . . O6 O -0.0880(3) 0.56791(17) 0.06914(16) 0.0388(9) Uani 1 1 d . . . O7 O 0.3653(5) 0.8951(3) 0.3029(3) 0.0905(19) Uani 1 1 d . . . O8 O 0.1808(4) 0.8671(3) 0.3070(2) 0.0707(15) Uani 1 1 d . . . O9 O 0.2614(6) 0.9465(2) 0.3710(3) 0.091(2) Uani 1 1 d . . . O10 O -0.2545(4) 0.8628(3) 0.2645(2) 0.0724(15) Uani 1 1 d . . . O11 O -0.1865(3) 0.77476(18) 0.2200(2) 0.0512(11) Uani 1 1 d . . . O12 O -0.0939(3) 0.87041(19) 0.2157(2) 0.0573(13) Uani 1 1 d . . . F1 F 0.4012(13) 0.6354(4) 0.4898(3) 0.262(8) Uani 1 1 d . . . F2 F 0.3652(9) 0.5420(5) 0.4743(3) 0.177(4) Uani 1 1 d . . . F3 F 0.2510(6) 0.6111(5) 0.4410(4) 0.170(4) Uani 1 1 d . . . F4 F -0.2953(3) 0.5984(3) 0.1097(2) 0.0848(15) Uani 1 1 d . . . F5 F -0.2856(4) 0.6910(2) 0.0834(2) 0.0880(16) Uani 1 1 d . . . F6 F -0.2993(3) 0.6203(2) 0.02054(18) 0.0683(12) Uani 1 1 d . . . F7 F 0.3301(5) 0.7846(2) 0.3695(3) 0.117(2) Uani 1 1 d . A . F8 F 0.4190(4) 0.8568(3) 0.4211(2) 0.1024(19) Uani 1 1 d . A . F9 F 0.2531(4) 0.8382(3) 0.4308(2) 0.0998(18) Uani 1 1 d . A . F10 F -0.2942(4) 0.9163(2) 0.1481(2) 0.0869(15) Uani 1 1 d . . . F11 F -0.2333(4) 0.8382(2) 0.1086(2) 0.0821(14) Uani 1 1 d . . . F12 F -0.3758(3) 0.8312(2) 0.1509(2) 0.0824(15) 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 0.0377(2) 0.0339(2) 0.0375(2) 0.00188(18) 0.00219(17) -0.00388(17) Ag2 0.0446(3) 0.0531(3) 0.0450(3) -0.0043(2) 0.0128(2) 0.0079(2) Ag3 0.0307(2) 0.0283(2) 0.0441(2) -0.00186(17) 0.00604(17) 0.00149(16) Ag4 0.0295(2) 0.0283(2) 0.0378(2) -0.00471(17) 0.00522(16) 0.00128(15) N1 0.028(2) 0.025(2) 0.037(2) -0.0016(18) 0.0034(18) -0.0024(17) N2 0.029(2) 0.025(2) 0.034(2) -0.0002(18) -0.0002(18) -0.0036(17) N3 0.038(3) 0.033(3) 0.051(3) 0.006(2) -0.010(2) -0.002(2) N4 0.039(2) 0.031(2) 0.036(2) -0.0082(19) 0.001(2) -0.0077(19) N5 0.029(2) 0.031(2) 0.029(2) 0.0026(18) -0.0007(17) -0.0003(17) N6 0.0219(19) 0.022(2) 0.039(2) 0.0005(18) 0.0083(17) 0.0038(16) N7 0.023(2) 0.024(2) 0.035(2) 0.0013(17) 0.0058(17) 0.0010(16) N8 0.032(2) 0.025(2) 0.033(2) 0.0018(18) 0.0055(18) -0.0008(17) N9 0.033(2) 0.031(2) 0.045(3) -0.003(2) 0.015(2) 0.0010(18) N10 0.028(2) 0.026(2) 0.053(3) 0.008(2) 0.011(2) 0.0006(18) C1 0.029(3) 0.033(3) 0.040(3) 0.004(2) 0.001(2) -0.001(2) C2 0.033(3) 0.037(3) 0.030(3) 0.003(2) -0.003(2) -0.005(2) C3 0.026(2) 0.034(3) 0.029(3) -0.003(2) 0.004(2) -0.007(2) C4 0.022(2) 0.031(3) 0.028(2) -0.003(2) 0.0047(19) 0.0014(19) C5 0.046(3) 0.025(3) 0.071(4) 0.000(3) -0.006(3) 0.006(2) C6 0.054(4) 0.026(3) 0.065(4) 0.008(3) -0.015(3) -0.007(3) C7 0.059(4) 0.059(4) 0.058(4) 0.026(4) -0.015(4) -0.021(3) C8 0.046(4) 0.054(4) 0.065(4) 0.031(4) -0.015(3) -0.005(3) C9 0.040(4) 0.109(7) 0.087(6) 0.057(5) -0.019(4) -0.003(4) C10 0.061(6) 0.58(4) 0.035(5) -0.012(11) -0.008(4) 0.088(12) C11 0.051(4) 0.030(3) 0.049(3) -0.007(3) 0.002(3) -0.009(3) C12 0.069(5) 0.047(4) 0.057(4) -0.020(3) 0.003(4) 0.011(3) C13 0.061(5) 0.105(7) 0.057(5) -0.027(5) 0.014(4) 0.017(5) C14 0.043(3) 0.049(4) 0.033(3) -0.012(3) 0.001(2) -0.009(3) C15 0.044(3) 0.062(4) 0.036(3) -0.016(3) -0.004(3) -0.002(3) C16 0.043(4) 0.093(6) 0.061(4) -0.023(4) 0.003(3) -0.006(4) C17 0.037(3) 0.036(3) 0.036(3) 0.008(2) 0.004(2) 0.001(2) C18 0.033(3) 0.040(3) 0.050(3) 0.010(3) -0.002(2) 0.007(2) C19 0.055(4) 0.052(4) 0.065(5) 0.003(3) 0.002(3) 0.015(3) C20 0.032(3) 0.043(3) 0.028(3) -0.002(2) 0.000(2) -0.004(2) C21 0.027(3) 0.044(3) 0.037(3) 0.000(2) -0.004(2) 0.000(2) C22 0.040(3) 0.053(4) 0.045(3) 0.000(3) -0.003(3) -0.012(3) C23 0.098(9) 0.208(16) 0.084(8) -0.026(9) 0.038(7) -0.037(10) C24 0.021(2) 0.030(3) 0.039(3) -0.001(2) 0.007(2) 0.0048(19) C25 0.030(3) 0.031(3) 0.040(3) 0.005(2) 0.020(2) 0.003(2) C26 0.016(2) 0.027(3) 0.041(3) 0.002(2) 0.004(2) 0.0044(18) C27 0.015(2) 0.027(3) 0.038(3) 0.002(2) 0.0037(19) 0.0029(18) C28 0.043(3) 0.037(3) 0.031(3) 0.002(2) 0.004(2) 0.002(2) C29 0.044(3) 0.045(3) 0.034(3) -0.005(3) 0.011(2) -0.002(3) C30 0.058(4) 0.044(4) 0.033(3) -0.008(3) 0.004(3) 0.015(3) C31 0.038(3) 0.028(3) 0.040(3) 0.009(2) 0.010(2) 0.001(2) C32 0.038(3) 0.029(3) 0.042(3) 0.004(2) 0.010(2) -0.004(2) C33 0.031(3) 0.038(3) 0.052(3) -0.002(3) 0.013(2) -0.002(2) C34 0.046(3) 0.043(3) 0.041(3) -0.007(3) 0.012(3) 0.000(3) C35 0.055(4) 0.057(4) 0.050(4) -0.011(3) 0.029(3) -0.004(3) C36 0.037(3) 0.089(5) 0.060(4) -0.028(4) 0.023(3) 0.000(3) C37 0.033(3) 0.030(3) 0.049(3) -0.005(2) 0.011(2) 0.004(2) C38 0.037(3) 0.032(3) 0.043(3) -0.008(2) 0.005(2) 0.004(2) C39 0.043(3) 0.028(3) 0.065(4) -0.006(3) 0.012(3) 0.003(2) C40 0.034(3) 0.036(3) 0.055(4) 0.016(3) 0.006(3) 0.001(2) C41 0.035(3) 0.084(5) 0.044(4) 0.029(4) 0.004(3) -0.006(3) C42 0.057(5) 0.201(13) 0.056(5) 0.024(6) 0.015(4) 0.034(6) C43 0.029(3) 0.026(3) 0.053(3) 0.000(2) 0.001(2) -0.003(2) C44 0.032(3) 0.021(3) 0.053(3) -0.001(2) 0.009(2) 0.000(2) C45 0.038(3) 0.032(3) 0.048(3) 0.005(2) 0.010(3) 0.006(2) C46 0.038(3) 0.053(4) 0.047(4) -0.005(3) 0.002(3) 0.013(3) C47 0.063(5) 0.074(5) 0.074(5) 0.010(4) 0.020(4) 0.023(4) C48 0.039(3) 0.055(4) 0.079(5) 0.012(4) 0.004(3) 0.008(3) S1 0.0819(15) 0.0616(13) 0.1090(18) 0.0201(13) 0.0497(14) 0.0184(11) S2 0.0342(7) 0.0269(7) 0.0370(7) 0.0008(5) 0.0047(5) -0.0007(5) S3 0.0496(12) 0.0359(14) 0.0400(11) -0.0018(9) -0.0022(8) 0.0096(8) S4 0.0323(7) 0.0362(8) 0.0623(10) -0.0088(7) 0.0051(7) 0.0057(6) O1 0.175(9) 0.180(10) 0.221(11) 0.126(9) -0.124(9) -0.067(8) O2 0.226(10) 0.058(4) 0.127(7) -0.034(4) 0.038(6) -0.019(5) O3 0.151(7) 0.065(4) 0.121(6) 0.022(4) 0.020(5) -0.035(4) O4 0.077(3) 0.048(3) 0.066(3) 0.014(2) 0.025(3) -0.010(2) O5 0.060(3) 0.033(2) 0.043(2) -0.0065(18) -0.010(2) 0.0007(19) O6 0.043(2) 0.031(2) 0.041(2) -0.0036(17) 0.0008(17) 0.0084(16) O7 0.079(4) 0.094(5) 0.102(5) 0.032(4) 0.025(3) 0.010(3) O8 0.058(3) 0.088(4) 0.060(3) -0.023(3) -0.013(2) 0.006(3) O9 0.126(5) 0.049(3) 0.090(4) -0.013(3) -0.010(4) 0.026(3) O10 0.069(3) 0.079(4) 0.072(3) -0.014(3) 0.020(3) 0.021(3) O11 0.036(2) 0.036(2) 0.081(3) 0.000(2) 0.006(2) 0.0030(17) O12 0.037(2) 0.037(2) 0.097(4) -0.019(2) 0.004(2) -0.0017(18) F1 0.56(2) 0.152(8) 0.055(4) -0.027(4) -0.039(8) -0.034(11) F2 0.255(11) 0.187(9) 0.094(5) 0.056(6) 0.046(6) -0.023(8) F3 0.095(5) 0.270(11) 0.159(7) -0.048(7) 0.068(5) 0.021(6) F4 0.049(2) 0.126(4) 0.085(3) 0.021(3) 0.027(2) -0.013(3) F5 0.075(3) 0.083(3) 0.101(4) -0.028(3) -0.009(3) 0.049(3) F6 0.057(2) 0.079(3) 0.061(2) -0.007(2) -0.021(2) 0.016(2) F7 0.110(4) 0.042(3) 0.211(7) 0.007(3) 0.058(5) 0.026(3) F8 0.070(3) 0.149(5) 0.081(3) 0.014(3) -0.019(3) 0.033(3) F9 0.096(4) 0.137(5) 0.074(3) 0.028(3) 0.039(3) 0.038(3) F10 0.071(3) 0.065(3) 0.123(4) 0.033(3) 0.007(3) 0.023(2) F11 0.071(3) 0.107(4) 0.065(3) -0.001(3) 0.000(2) 0.007(3) F12 0.033(2) 0.100(4) 0.108(4) 0.020(3) -0.012(2) -0.008(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 C7 2.368(6) . ? Ag1 C22 2.376(6) . ? Ag1 C21 2.381(5) . ? Ag1 C6 2.397(6) . ? Ag1 N2 2.478(4) . ? Ag2 C13 2.349(7) . ? Ag2 O3 2.390(7) . ? Ag2 C19 2.418(7) . ? Ag2 C12 2.420(7) . ? Ag2 C18 2.436(6) . ? Ag2 N1 2.482(4) . ? Ag3 O6 2.390(4) . ? Ag3 C39 2.405(5) . ? Ag3 C33 2.405(6) . ? Ag3 C38 2.436(5) . ? Ag3 C32 2.450(6) . ? Ag3 N6 2.530(4) . ? Ag4 O5 2.319(4) . ? Ag4 C30 2.400(6) . ? Ag4 C45 2.407(6) . ? Ag4 C44 2.427(5) . ? Ag4 C29 2.437(6) . ? Ag4 N7 2.637(4) . ? N1 C3 1.351(6) . ? N1 C4 1.351(6) . ? N2 C4 1.342(6) . ? N2 C1 1.356(7) . ? N3 C1 1.364(7) . ? N3 C5 1.446(8) . ? N3 C8 1.463(7) . ? N4 C3 1.363(6) . ? N4 C11 1.447(7) . ? N4 C14 1.480(7) . ? N5 C4 1.362(6) . ? N5 C20 1.460(7) . ? N5 C17 1.464(7) . ? N6 C27 1.353(6) . ? N6 C24 1.360(7) . ? N7 C27 1.341(6) . ? N7 C26 1.354(7) . ? N8 C27 1.362(7) . ? N8 C31 1.460(6) . ? N8 C28 1.476(7) . ? N9 C24 1.349(7) . ? N9 C37 1.461(7) . ? N9 C34 1.477(7) . ? N10 C26 1.367(6) . ? N10 C43 1.450(7) . ? N10 C40 1.462(7) . ? C1 C2 1.381(7) . ? C2 C3 1.397(8) . ? C2 H2A 0.9500 . ? C5 C6 1.514(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.318(10) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C7 H7B 0.9500 . ? C8 C9 1.509(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.058(13) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C10 H10B 0.9500 . ? C11 C12 1.511(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.349(11) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C13 H13B 0.9500 . ? C14 C15 1.488(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.316(9) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C16 H16B 0.9500 . ? C17 C18 1.502(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.322(9) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C19 H19B 0.9500 . ? C20 C21 1.516(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.334(8) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C22 H22B 0.9500 . ? C23 F3 1.222(14) . ? C23 F1 1.272(14) . ? C23 F2 1.496(18) . ? C23 S1 1.749(11) . ? C24 C25 1.391(7) . ? C25 C26 1.390(7) . ? C25 H25A 0.9500 . ? C28 C29 1.507(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.339(8) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C30 H30B 0.9500 . ? C31 C32 1.503(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.340(8) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C33 H33B 0.9500 . ? C34 C35 1.492(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.292(10) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C36 H36B 0.9500 . ? C37 C38 1.496(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.327(8) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C39 H39B 0.9500 . ? C40 C41 1.495(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.187(11) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C42 H42B 0.9500 . ? C43 C44 1.507(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.336(8) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C45 H45B 0.9500 . ? C46 F4 1.321(8) . ? C46 F5 1.323(7) . ? C46 F6 1.327(7) . ? C46 S2 1.813(6) . ? C47 F9 1.316(9) . ? C47 F8 1.348(10) . ? C47 F7 1.361(10) . ? C47 S3' 1.701(14) . ? C47 S3 1.792(8) . ? C48 F12 1.324(8) . ? C48 F10 1.335(8) . ? C48 F11 1.335(9) . ? C48 S4 1.817(7) . ? S1 O1 1.224(9) . ? S1 O3 1.384(7) . ? S1 O2 1.472(8) . ? S2 O4 1.430(5) . ? S2 O5 1.443(4) . ? S2 O6 1.444(4) . ? S3 O8 1.434(5) . ? S3 O7 1.434(7) . ? S3 O9 1.439(6) . ? S3' O7 1.318(13) . ? S3' O8 1.398(13) . ? S3' F7 2.015(15) . ? S4 O12 1.432(5) . ? S4 O10 1.435(5) . ? S4 O11 1.443(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Ag1 C22 132.9(2) . . ? C7 Ag1 C21 163.6(3) . . ? C22 Ag1 C21 32.6(2) . . ? C7 Ag1 C6 32.1(3) . . ? C22 Ag1 C6 109.9(2) . . ? C21 Ag1 C6 133.0(2) . . ? C7 Ag1 N2 97.5(2) . . ? C22 Ag1 N2 105.93(18) . . ? C21 Ag1 N2 84.67(16) . . ? C6 Ag1 N2 84.74(18) . . ? C13 Ag2 O3 106.5(3) . . ? C13 Ag2 C19 130.2(3) . . ? O3 Ag2 C19 109.4(3) . . ? C13 Ag2 C12 32.8(3) . . ? O3 Ag2 C12 139.2(3) . . ? C19 Ag2 C12 103.4(3) . . ? C13 Ag2 C18 160.1(3) . . ? O3 Ag2 C18 91.5(2) . . ? C19 Ag2 C18 31.6(2) . . ? C12 Ag2 C18 128.3(2) . . ? C13 Ag2 N1 97.6(2) . . ? O3 Ag2 N1 112.0(2) . . ? C19 Ag2 N1 99.7(2) . . ? C12 Ag2 N1 84.97(19) . . ? C18 Ag2 N1 82.94(17) . . ? O6 Ag3 C39 119.41(19) . . ? O6 Ag3 C33 104.80(17) . . ? C39 Ag3 C33 131.4(2) . . ? O6 Ag3 C38 94.34(17) . . ? C39 Ag3 C38 31.8(2) . . ? C33 Ag3 C38 160.9(2) . . ? O6 Ag3 C32 133.91(16) . . ? C39 Ag3 C32 106.5(2) . . ? C33 Ag3 C32 32.03(19) . . ? C38 Ag3 C32 129.78(19) . . ? O6 Ag3 N6 90.82(13) . . ? C39 Ag3 N6 102.32(17) . . ? C33 Ag3 N6 95.80(17) . . ? C38 Ag3 N6 83.93(16) . . ? C32 Ag3 N6 82.64(16) . . ? O5 Ag4 C30 134.73(19) . . ? O5 Ag4 C45 96.15(18) . . ? C30 Ag4 C45 129.1(2) . . ? O5 Ag4 C44 123.60(18) . . ? C30 Ag4 C44 99.9(2) . . ? C45 Ag4 C44 32.09(19) . . ? O5 Ag4 C29 103.83(18) . . ? C30 Ag4 C29 32.1(2) . . ? C45 Ag4 C29 157.3(2) . . ? C44 Ag4 C29 125.2(2) . . ? O5 Ag4 N7 81.52(14) . . ? C30 Ag4 N7 93.40(17) . . ? C45 Ag4 N7 93.86(16) . . ? C44 Ag4 N7 82.50(15) . . ? C29 Ag4 N7 78.69(16) . . ? C3 N1 C4 116.3(4) . . ? C3 N1 Ag2 111.6(3) . . ? C4 N1 Ag2 108.8(3) . . ? C4 N2 C1 115.8(4) . . ? C4 N2 Ag1 111.0(3) . . ? C1 N2 Ag1 111.5(3) . . ? C1 N3 C5 120.9(5) . . ? C1 N3 C8 121.5(5) . . ? C5 N3 C8 117.5(5) . . ? C3 N4 C11 121.4(5) . . ? C3 N4 C14 121.8(5) . . ? C11 N4 C14 116.8(4) . . ? C4 N5 C20 121.0(4) . . ? C4 N5 C17 119.7(4) . . ? C20 N5 C17 119.1(4) . . ? C27 N6 C24 115.6(4) . . ? C27 N6 Ag3 113.3(3) . . ? C24 N6 Ag3 111.4(3) . . ? C27 N7 C26 115.7(4) . . ? C27 N7 Ag4 107.6(3) . . ? C26 N7 Ag4 109.0(3) . . ? C27 N8 C31 120.2(4) . . ? C27 N8 C28 119.3(4) . . ? C31 N8 C28 119.3(4) . . ? C24 N9 C37 121.9(5) . . ? C24 N9 C34 121.2(5) . . ? C37 N9 C34 116.8(4) . . ? C26 N10 C43 121.0(5) . . ? C26 N10 C40 121.5(5) . . ? C43 N10 C40 117.0(4) . . ? N2 C1 N3 115.2(5) . . ? N2 C1 C2 123.4(5) . . ? N3 C1 C2 121.4(5) . . ? C1 C2 C3 115.8(5) . . ? C1 C2 H2A 122.1 . . ? C3 C2 H2A 122.1 . . ? N1 C3 N4 116.2(5) . . ? N1 C3 C2 122.4(5) . . ? N4 C3 C2 121.4(5) . . ? N2 C4 N1 125.7(4) . . ? N2 C4 N5 117.0(4) . . ? N1 C4 N5 117.4(4) . . ? N3 C5 C6 113.5(6) . . ? N3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C5 124.9(6) . . ? C7 C6 Ag1 72.7(4) . . ? C5 C6 Ag1 101.7(4) . . ? C7 C6 H6A 117.5 . . ? C5 C6 H6A 117.5 . . ? Ag1 C6 H6A 95.8 . . ? C6 C7 Ag1 75.2(4) . . ? C6 C7 H7A 120.0 . . ? Ag1 C7 H7A 99.4 . . ? C6 C7 H7B 120.0 . . ? Ag1 C7 H7B 95.3 . . ? H7A C7 H7B 120.0 . . ? N3 C8 C9 112.3(6) . . ? N3 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N3 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C8 138.9(12) . . ? C10 C9 H9A 110.6 . . ? C8 C9 H9A 110.6 . . ? C9 C10 H10A 120.0 . . ? C9 C10 H10B 120.0 . . ? H10A C10 H10B 120.0 . . ? N4 C11 C12 113.1(5) . . ? N4 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N4 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C11 124.7(7) . . ? C13 C12 Ag2 70.7(4) . . ? C11 C12 Ag2 101.6(4) . . ? C13 C12 H12A 117.7 . . ? C11 C12 H12A 117.7 . . ? Ag2 C12 H12A 97.9 . . ? C12 C13 Ag2 76.4(4) . . ? C12 C13 H13A 120.0 . . ? Ag2 C13 H13A 97.6 . . ? C12 C13 H13B 120.0 . . ? Ag2 C13 H13B 95.8 . . ? H13A C13 H13B 120.0 . . ? N4 C14 C15 112.4(5) . . ? N4 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N4 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 124.8(6) . . ? C16 C15 H15A 117.6 . . ? C14 C15 H15A 117.6 . . ? C15 C16 H16A 120.0 . . ? C15 C16 H16B 120.0 . . ? H16A C16 H16B 120.0 . . ? N5 C17 C18 114.7(5) . . ? N5 C17 H17A 108.6 . . ? C18 C17 H17A 108.6 . . ? N5 C17 H17B 108.6 . . ? C18 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C19 C18 C17 122.7(6) . . ? C19 C18 Ag2 73.4(4) . . ? C17 C18 Ag2 104.9(3) . . ? C19 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? Ag2 C18 H18A 91.7 . . ? C18 C19 Ag2 75.0(4) . . ? C18 C19 H19A 120.0 . . ? Ag2 C19 H19A 103.7 . . ? C18 C19 H19B 120.0 . . ? Ag2 C19 H19B 91.3 . . ? H19A C19 H19B 120.0 . . ? N5 C20 C21 115.2(4) . . ? N5 C20 H20A 108.5 . . ? C21 C20 H20A 108.5 . . ? N5 C20 H20B 108.5 . . ? C21 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C22 C21 C20 123.2(6) . . ? C22 C21 Ag1 73.5(3) . . ? C20 C21 Ag1 103.8(3) . . ? C22 C21 H21A 118.4 . . ? C20 C21 H21A 118.4 . . ? Ag1 C21 H21A 92.8 . . ? C21 C22 Ag1 73.9(3) . . ? C21 C22 H22A 120.0 . . ? Ag1 C22 H22A 103.0 . . ? C21 C22 H22B 120.0 . . ? Ag1 C22 H22B 93.0 . . ? H22A C22 H22B 120.0 . . ? F3 C23 F1 116.5(15) . . ? F3 C23 F2 104.8(12) . . ? F1 C23 F2 100.9(12) . . ? F3 C23 S1 113.8(10) . . ? F1 C23 S1 114.4(10) . . ? F2 C23 S1 104.2(10) . . ? N9 C24 N6 116.1(5) . . ? N9 C24 C25 122.4(5) . . ? N6 C24 C25 121.5(5) . . ? C26 C25 C24 117.8(5) . . ? C26 C25 H25A 121.1 . . ? C24 C25 H25A 121.1 . . ? N7 C26 N10 115.3(5) . . ? N7 C26 C25 121.9(5) . . ? N10 C26 C25 122.7(5) . . ? N7 C27 N6 127.2(5) . . ? N7 C27 N8 116.5(4) . . ? N6 C27 N8 116.3(4) . . ? N8 C28 C29 115.8(4) . . ? N8 C28 H28A 108.3 . . ? C29 C28 H28A 108.3 . . ? N8 C28 H28B 108.3 . . ? C29 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? C30 C29 C28 121.7(6) . . ? C30 C29 Ag4 72.4(3) . . ? C28 C29 Ag4 109.4(4) . . ? C30 C29 H29A 119.1 . . ? C28 C29 H29A 119.1 . . ? Ag4 C29 H29A 88.2 . . ? C29 C30 Ag4 75.4(3) . . ? C29 C30 H30A 120.0 . . ? Ag4 C30 H30A 107.7 . . ? C29 C30 H30B 120.0 . . ? Ag4 C30 H30B 86.9 . . ? H30A C30 H30B 120.0 . . ? N8 C31 C32 114.4(4) . . ? N8 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? N8 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C33 C32 C31 125.5(5) . . ? C33 C32 Ag3 72.1(3) . . ? C31 C32 Ag3 103.2(3) . . ? C33 C32 H32A 117.3 . . ? C31 C32 H32A 117.3 . . ? Ag3 C32 H32A 94.9 . . ? C32 C33 Ag3 75.8(3) . . ? C32 C33 H33A 120.0 . . ? Ag3 C33 H33A 100.2 . . ? C32 C33 H33B 120.0 . . ? Ag3 C33 H33B 93.9 . . ? H33A C33 H33B 120.0 . . ? N9 C34 C35 114.8(5) . . ? N9 C34 H34A 108.6 . . ? C35 C34 H34A 108.6 . . ? N9 C34 H34B 108.6 . . ? C35 C34 H34B 108.6 . . ? H34A C34 H34B 107.5 . . ? C36 C35 C34 125.2(6) . . ? C36 C35 H35A 117.4 . . ? C34 C35 H35A 117.4 . . ? C35 C36 H36A 120.0 . . ? C35 C36 H36B 120.0 . . ? H36A C36 H36B 120.0 . . ? N9 C37 C38 115.1(5) . . ? N9 C37 H37A 108.5 . . ? C38 C37 H37A 108.5 . . ? N9 C37 H37B 108.5 . . ? C38 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? C39 C38 C37 122.7(6) . . ? C39 C38 Ag3 72.8(3) . . ? C37 C38 Ag3 103.4(3) . . ? C39 C38 H38A 118.7 . . ? C37 C38 H38A 118.7 . . ? Ag3 C38 H38A 93.8 . . ? C38 C39 Ag3 75.4(3) . . ? C38 C39 H39A 120.0 . . ? Ag3 C39 H39A 101.7 . . ? C38 C39 H39B 120.0 . . ? Ag3 C39 H39B 92.9 . . ? H39A C39 H39B 120.0 . . ? N10 C40 C41 113.0(5) . . ? N10 C40 H40A 109.0 . . ? C41 C40 H40A 109.0 . . ? N10 C40 H40B 109.0 . . ? C41 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C42 C41 C40 127.5(8) . . ? C42 C41 H41A 116.2 . . ? C40 C41 H41A 116.2 . . ? C41 C42 H42A 120.0 . . ? C41 C42 H42B 120.0 . . ? H42A C42 H42B 120.0 . . ? N10 C43 C44 113.5(4) . . ? N10 C43 H43A 108.9 . . ? C44 C43 H43A 108.9 . . ? N10 C43 H43B 108.9 . . ? C44 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C45 C44 C43 124.9(5) . . ? C45 C44 Ag4 73.1(3) . . ? C43 C44 Ag4 102.1(3) . . ? C45 C44 H44A 117.6 . . ? C43 C44 H44A 117.6 . . ? Ag4 C44 H44A 95.0 . . ? C44 C45 Ag4 74.8(3) . . ? C44 C45 H45A 120.0 . . ? Ag4 C45 H45A 100.2 . . ? C44 C45 H45B 120.0 . . ? Ag4 C45 H45B 94.9 . . ? H45A C45 H45B 120.0 . . ? F4 C46 F5 108.9(6) . . ? F4 C46 F6 107.6(6) . . ? F5 C46 F6 107.8(5) . . ? F4 C46 S2 110.9(4) . . ? F5 C46 S2 110.0(5) . . ? F6 C46 S2 111.6(4) . . ? F9 C47 F8 106.9(7) . . ? F9 C47 F7 109.0(7) . . ? F8 C47 F7 109.3(6) . . ? F9 C47 S3' 126.9(7) . . ? F8 C47 S3' 118.4(7) . . ? F7 C47 S3' 81.5(8) . . ? F9 C47 S3 110.8(5) . . ? F8 C47 S3 110.6(6) . . ? F7 C47 S3 110.2(6) . . ? S3' C47 S3 29.0(6) . . ? F12 C48 F10 107.6(5) . . ? F12 C48 F11 107.5(7) . . ? F10 C48 F11 107.1(6) . . ? F12 C48 S4 112.1(5) . . ? F10 C48 S4 110.8(6) . . ? F11 C48 S4 111.5(4) . . ? O1 S1 O3 114.7(6) . . ? O1 S1 O2 119.4(7) . . ? O3 S1 O2 115.3(5) . . ? O1 S1 C23 99.0(9) . . ? O3 S1 C23 103.0(7) . . ? O2 S1 C23 101.0(6) . . ? O4 S2 O5 116.3(3) . . ? O4 S2 O6 115.4(3) . . ? O5 S2 O6 113.1(2) . . ? O4 S2 C46 103.9(3) . . ? O5 S2 C46 102.2(3) . . ? O6 S2 C46 103.5(3) . . ? O8 S3 O7 112.6(4) . . ? O8 S3 O9 116.1(4) . . ? O7 S3 O9 117.6(4) . . ? O8 S3 C47 103.7(4) . . ? O7 S3 C47 103.4(4) . . ? O9 S3 C47 100.7(4) . . ? O7 S3' O8 122.8(11) . . ? O7 S3' C47 114.1(9) . . ? O8 S3' C47 110.2(9) . . ? O7 S3' F7 124.4(9) . . ? O8 S3' F7 112.7(8) . . ? C47 S3' F7 41.9(5) . . ? O12 S4 O10 115.9(3) . . ? O12 S4 O11 114.6(3) . . ? O10 S4 O11 114.2(3) . . ? O12 S4 C48 103.3(3) . . ? O10 S4 C48 103.7(3) . . ? O11 S4 C48 102.7(3) . . ? S1 O3 Ag2 121.1(5) . . ? S2 O5 Ag4 145.4(3) . . ? S2 O6 Ag3 122.5(2) . . ? S3' O7 S3 37.0(7) . . ? S3' O8 S3 36.2(7) . . ? C47 F7 S3' 56.6(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.72 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.409 _refine_diff_density_min -1.799 _refine_diff_density_rms 0.117 # start Validation Reply Form _vrf_PLAT241_3sw37 ; PROBLEM: Check High Ueq as Compared to Neighbors for O2 RESPONSE: There is evidence for additional (unmodelled) disorder of this triflate anion. Attempts to include this did not improve the model. ; _vrf_PLAT213_3sw37 ; PROBLEM: Atom C10 has ADP max/min Ratio ..... 4.5 prola RESPONSE: This atom (on a non-coordinated allyl arm) appears to also be slightly disordered but attempts to model this led to additional complications. ; _vrf_PLAT220_3sw37 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 8.4 Ratio RESPONSE: See above; there is additional unmodelled disorder. ; _vrf_PLAT242_3sw37 ; PROBLEM: Check Low Ueq as Compared to Neighbors for S1 RESPONSE: See above; the sulfur atoms of the triflate anions are not involved in the disorder. ; _database_code_depnum_ccdc_archive 'CCDC 940160' ####################################################################### # # 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_test _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H60 Ag4 Cl4 N12 O16' _chemical_formula_sum 'C42 H60 Ag4 Cl4 N12 O16' _chemical_formula_weight 1562.30 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.4069(2) _cell_length_b 13.8557(4) _cell_length_c 37.5419(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5413.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 117(2) _cell_measurement_reflns_used 9768 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.90 _exptl_crystal_description plate _exptl_crystal_colour 'Color less' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.702 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.800309 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 117(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 103327 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.05 _reflns_number_total 9594 _reflns_number_gt 8844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0515P)^2^+0.9463P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 9594 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.60622(3) 0.79493(3) 0.159483(11) 0.02074(10) Uani 1 1 d . . . Ag3 Ag 0.10775(3) 0.23883(3) 0.157754(10) 0.02048(10) Uani 1 1 d . . . Ag2 Ag 0.07739(4) 0.75790(3) 0.068113(12) 0.02827(12) Uani 1 1 d . . . Ag4 Ag -0.41120(5) 0.29018(4) 0.055516(19) 0.0589(2) Uani 1 1 d . . . Cl1 Cl 0.00209(12) 0.80144(12) 0.16754(4) 0.0294(3) Uani 1 1 d . . . O1 O -0.0222(6) 0.7062(5) 0.1784(3) 0.132(4) Uani 1 1 d . . . O2 O 0.0454(6) 0.8044(8) 0.13233(15) 0.125(4) Uani 1 1 d . . . O3 O 0.0975(5) 0.8418(4) 0.18961(13) 0.0570(14) Uani 1 1 d . . . O4 O -0.1129(4) 0.8561(4) 0.16922(15) 0.0533(14) Uani 1 1 d . . . Cl3 Cl 0.49421(11) 0.23796(11) 0.17143(4) 0.0263(3) Uani 1 1 d . . . O9 O 0.5967(4) 0.1898(4) 0.18933(13) 0.0508(13) Uani 1 1 d . . . O10 O 0.5313(5) 0.2630(5) 0.13669(13) 0.0657(17) Uani 1 1 d . . . O11 O 0.4608(4) 0.3239(4) 0.19085(14) 0.0497(13) Uani 1 1 d . . . O12 O 0.3843(4) 0.1764(4) 0.17051(14) 0.0483(13) Uani 1 1 d . . . N12 N -0.1286(4) 0.1966(3) 0.09584(11) 0.0186(10) Uani 1 1 d . . . C37 C -0.1436(5) 0.1902(4) 0.05715(15) 0.0249(13) Uani 1 1 d . . . H37A H -0.0769 0.1464 0.0475 0.030 Uiso 1 1 calc R . . H37B H -0.1296 0.2548 0.0466 0.030 Uiso 1 1 calc R . . C38 C -0.2744(5) 0.1537(4) 0.04593(17) 0.0287(14) Uani 1 1 d . . . H38A H -0.2905 0.1492 0.0211 0.034 Uiso 1 1 calc R . . C39 C -0.3679(6) 0.1276(4) 0.0674(2) 0.0376(16) Uani 1 1 d . . . H39A H -0.3562 0.1308 0.0925 0.045 Uiso 1 1 calc R . . H39B H -0.4471 0.1055 0.0579 0.045 Uiso 1 1 calc R . . C40 C -0.0944(5) 0.1090(4) 0.11490(14) 0.0219(12) Uani 1 1 d . . . H40A H -0.1259 0.0528 0.1012 0.026 Uiso 1 1 calc R . . H40B H -0.1392 0.1089 0.1382 0.026 Uiso 1 1 calc R . . C41 C 0.0483(5) 0.0969(4) 0.12137(16) 0.0215(12) Uani 1 1 d . . . H41A H 0.1059 0.1144 0.1028 0.026 Uiso 1 1 calc R . . C42 C 0.0969(5) 0.0635(4) 0.15128(15) 0.0262(13) Uani 1 1 d . . . H42A H 0.0415 0.0455 0.1703 0.031 Uiso 1 1 calc R . . H42B H 0.1873 0.0574 0.1539 0.031 Uiso 1 1 calc R . . N11 N -0.1312(4) 0.3676(3) 0.20066(12) 0.0211(10) Uani 1 1 d . . . C31 C -0.1548(5) 0.4570(4) 0.22033(16) 0.0249(13) Uani 1 1 d . . . H31A H -0.1379 0.5125 0.2044 0.030 Uiso 1 1 calc R . . H31B H -0.0933 0.4609 0.2404 0.030 Uiso 1 1 calc R . . C32 C -0.2889(5) 0.4654(4) 0.23471(15) 0.0216(12) Uani 1 1 d . . . H32A H -0.3578 0.4459 0.2197 0.026 Uiso 1 1 calc R . . C33 C -0.3171(7) 0.4975(5) 0.26627(17) 0.0348(16) Uani 1 1 d . . . H33A H -0.2506 0.5175 0.2819 0.042 Uiso 1 1 calc R . . H33B H -0.4043 0.5009 0.2737 0.042 Uiso 1 1 calc R . . C34 C -0.0942(5) 0.2809(4) 0.22056(14) 0.0257(13) Uani 1 1 d . . . H34A H -0.1383 0.2244 0.2099 0.031 Uiso 1 1 calc R . . H34B H -0.1248 0.2874 0.2454 0.031 Uiso 1 1 calc R . . C35 C 0.0481(5) 0.2616(5) 0.22105(14) 0.0274(14) Uani 1 1 d . . . H35A H 0.0753 0.1992 0.2284 0.033 Uiso 1 1 calc R . . C36 C 0.1381(5) 0.3241(5) 0.21213(15) 0.0285(14) Uani 1 1 d . . . H36A H 0.1150 0.3872 0.2046 0.034 Uiso 1 1 calc R . . H36B H 0.2261 0.3059 0.2132 0.034 Uiso 1 1 calc R . . C22 C -0.1615(4) 0.3623(4) 0.16564(15) 0.0190(12) Uani 1 1 d . . . N7 N -0.1232(4) 0.2811(3) 0.14822(11) 0.0191(10) Uani 1 1 d . . . C23 C -0.1583(4) 0.2782(4) 0.11389(14) 0.0172(11) Uani 1 1 d . . . N8 N -0.2203(4) 0.3489(3) 0.09590(12) 0.0182(10) Uani 1 1 d . . . C24 C -0.2499(4) 0.4256(4) 0.11682(14) 0.0164(11) Uani 1 1 d . . . N9 N -0.2234(4) 0.4364(3) 0.15139(11) 0.0159(10) Uani 1 1 d . . . C1 C 0.3390(4) 0.6710(4) 0.16623(14) 0.0190(12) Uani 1 1 d . . . N1 N 0.2767(4) 0.5959(3) 0.15143(12) 0.0212(11) Uani 1 1 d . . . C2 C 0.2466(5) 0.6094(4) 0.11708(15) 0.0204(12) Uani 1 1 d . . . N2 N 0.2750(4) 0.6879(3) 0.09752(12) 0.0173(10) Uani 1 1 d . . . C3 C 0.3389(4) 0.7570(4) 0.11547(14) 0.0193(12) Uani 1 1 d . . . N3 N 0.3772(4) 0.7511(3) 0.14984(11) 0.0185(9) Uani 1 1 d . . . N4 N 0.3694(4) 0.8391(3) 0.09774(12) 0.0222(10) Uani 1 1 d . . . C4 C 0.3517(5) 0.8494(4) 0.05963(15) 0.0265(14) Uani 1 1 d . . . H4A H 0.3666 0.7861 0.0481 0.032 Uiso 1 1 calc R . . H4B H 0.4164 0.8953 0.0503 0.032 Uiso 1 1 calc R . . C5 C 0.2161(6) 0.8857(5) 0.04982(18) 0.0359(16) Uani 1 1 d . . . H5A H 0.1753 0.9301 0.0654 0.043 Uiso 1 1 calc R . . C6 C 0.1540(7) 0.8585(6) 0.0210(2) 0.051(2) Uani 1 1 d . . . H6A H 0.1926 0.8142 0.0049 0.061 Uiso 1 1 calc R . . H6B H 0.0706 0.8832 0.0162 0.061 Uiso 1 1 calc R . . C7 C 0.4060(5) 0.9261(4) 0.11778(15) 0.0219(12) Uani 1 1 d . . . H7A H 0.3633 0.9245 0.1413 0.026 Uiso 1 1 calc R . . H7B H 0.3738 0.9836 0.1049 0.026 Uiso 1 1 calc R . . C8 C 0.5471(5) 0.9368(4) 0.12325(15) 0.0201(12) Uani 1 1 d . . . H8A H 0.6033 0.9192 0.1044 0.024 Uiso 1 1 calc R . . C9 C 0.5984(6) 0.9703(4) 0.15365(15) 0.0255(13) Uani 1 1 d . . . H9A H 0.5442 0.9883 0.1729 0.031 Uiso 1 1 calc R . . H9B H 0.6890 0.9759 0.1559 0.031 Uiso 1 1 calc R . . N5 N 0.3710(4) 0.6614(3) 0.20151(12) 0.0217(10) Uani 1 1 d . . . C10 C 0.4083(5) 0.7480(4) 0.22170(14) 0.0270(12) Uani 1 1 d . . . H10A H 0.3775 0.7410 0.2465 0.032 Uiso 1 1 calc R . . H10B H 0.3642 0.8046 0.2112 0.032 Uiso 1 1 calc R . . C11 C 0.5508(5) 0.7680(5) 0.22247(15) 0.0292(14) Uani 1 1 d . . . H11A H 0.5774 0.8300 0.2304 0.035 Uiso 1 1 calc R . . C12 C 0.6404(6) 0.7073(5) 0.21313(15) 0.0335(15) Uani 1 1 d . . . H12A H 0.6179 0.6446 0.2050 0.040 Uiso 1 1 calc R . . H12B H 0.7282 0.7258 0.2144 0.040 Uiso 1 1 calc R . . C13 C 0.3459(5) 0.5720(4) 0.22076(15) 0.0225(13) Uani 1 1 d . . . H13A H 0.4058 0.5673 0.2412 0.027 Uiso 1 1 calc R . . H13B H 0.3628 0.5166 0.2048 0.027 Uiso 1 1 calc R . . C14 C 0.2097(5) 0.5658(4) 0.23431(15) 0.0233(13) Uani 1 1 d . . . H14A H 0.1417 0.5864 0.2192 0.028 Uiso 1 1 calc R . . C15 C 0.1819(6) 0.5333(5) 0.26596(18) 0.0380(17) Uani 1 1 d . . . H15A H 0.2486 0.5123 0.2814 0.046 Uiso 1 1 calc R . . H15B H 0.0949 0.5304 0.2736 0.046 Uiso 1 1 calc R . . N6 N 0.1790(4) 0.5387(3) 0.10108(12) 0.0189(10) Uani 1 1 d . . . C16 C 0.1591(6) 0.5383(5) 0.06293(16) 0.0290(14) Uani 1 1 d . . . H16A H 0.1547 0.4703 0.0549 0.035 Uiso 1 1 calc R . . H16B H 0.2353 0.5677 0.0515 0.035 Uiso 1 1 calc R . . C17 C 0.0422(6) 0.5894(5) 0.0496(2) 0.0402(17) Uani 1 1 d . . . H17A H 0.0343 0.6011 0.0247 0.048 Uiso 1 1 calc R . . C18 C -0.0464(6) 0.6177(5) 0.0700(2) 0.0445(18) Uani 1 1 d . . . H18A H -0.0403 0.6067 0.0949 0.053 Uiso 1 1 calc R . . H18B H -0.1192 0.6500 0.0604 0.053 Uiso 1 1 calc R . . C19 C 0.1206(5) 0.4596(4) 0.12169(17) 0.0249(13) Uani 1 1 d . . . H19A H 0.0413 0.4375 0.1096 0.030 Uiso 1 1 calc R . . H19B H 0.0966 0.4834 0.1457 0.030 Uiso 1 1 calc R . . C20 C 0.2117(5) 0.3772(4) 0.12525(15) 0.0213(12) Uani 1 1 d . . . H20A H 0.2752 0.3803 0.1434 0.026 Uiso 1 1 calc R . . C21 C 0.2093(5) 0.3000(4) 0.10457(15) 0.0245(13) Uani 1 1 d . . . H21A H 0.1469 0.2949 0.0862 0.029 Uiso 1 1 calc R . . H21B H 0.2699 0.2496 0.1081 0.029 Uiso 1 1 calc R . . N10 N -0.3177(4) 0.4983(3) 0.10130(12) 0.0173(10) Uani 1 1 d . . . C25 C -0.3316(5) 0.5046(4) 0.06271(15) 0.0203(12) Uani 1 1 d . . . H25A H -0.2580 0.4713 0.0514 0.024 Uiso 1 1 calc R . . H25B H -0.3281 0.5734 0.0556 0.024 Uiso 1 1 calc R . . C26 C -0.4547(5) 0.4611(4) 0.04890(17) 0.0250(13) Uani 1 1 d . . . H26A H -0.4683 0.4619 0.0239 0.030 Uiso 1 1 calc R . . C27 C -0.5445(5) 0.4222(4) 0.06883(17) 0.0283(14) Uani 1 1 d . . . H27A H -0.5344 0.4201 0.0940 0.034 Uiso 1 1 calc R . . H27B H -0.6196 0.3962 0.0581 0.034 Uiso 1 1 calc R . . C28 C -0.3784(5) 0.5730(4) 0.12258(15) 0.0204(12) Uani 1 1 d . . . H28A H -0.4009 0.5468 0.1463 0.025 Uiso 1 1 calc R . . H28B H -0.4586 0.5945 0.1108 0.025 Uiso 1 1 calc R . . C29 C -0.2883(5) 0.6574(4) 0.12680(15) 0.0234(13) Uani 1 1 d . . . H29A H -0.2244 0.6543 0.1448 0.028 Uiso 1 1 calc R . . C30 C -0.2939(6) 0.7371(4) 0.10633(14) 0.0270(13) Uani 1 1 d . . . H30A H -0.3569 0.7421 0.0881 0.032 Uiso 1 1 calc R . . H30B H -0.2348 0.7884 0.1101 0.032 Uiso 1 1 calc R . . Cl4 Cl -0.70416(13) 0.14384(11) 0.02697(4) 0.0264(3) Uani 1 1 d . . . O13 O -0.8364(4) 0.1512(4) 0.01671(16) 0.0566(15) Uani 1 1 d . . . O14 O -0.6474(4) 0.2386(3) 0.02546(11) 0.0368(11) Uani 1 1 d . . . O15 O -0.6952(4) 0.1067(3) 0.06221(11) 0.0364(10) Uani 1 1 d . . . O16 O -0.6388(5) 0.0806(4) 0.00306(12) 0.0509(14) Uani 1 1 d . . . Cl2 Cl -0.19957(13) 0.89176(11) 0.03202(4) 0.0271(3) Uani 1 1 d . . . O5 O -0.3334(4) 0.8919(4) 0.03737(14) 0.0489(13) Uani 1 1 d . . . O6 O -0.1637(5) 0.9705(4) 0.00988(14) 0.0555(15) Uani 1 1 d . . . O7 O -0.1362(5) 0.9011(4) 0.06528(12) 0.0523(14) Uani 1 1 d . . . O8 O -0.1602(5) 0.8026(5) 0.01652(16) 0.0731(19) 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 0.02277(19) 0.0188(2) 0.0206(2) 0.00221(17) -0.00304(18) -0.00249(17) Ag3 0.02017(18) 0.0200(2) 0.0213(2) -0.00177(17) -0.00009(17) 0.00139(16) Ag2 0.0223(2) 0.0267(2) 0.0358(3) 0.0057(2) -0.00680(18) -0.00293(18) Ag4 0.0361(3) 0.0278(3) 0.1129(5) -0.0260(3) -0.0369(3) 0.0109(2) Cl1 0.0236(6) 0.0345(9) 0.0302(9) -0.0063(7) -0.0054(6) 0.0015(6) O1 0.064(4) 0.040(4) 0.292(12) 0.041(6) -0.072(6) -0.011(3) O2 0.079(4) 0.264(11) 0.032(3) -0.054(5) -0.008(3) 0.068(6) O3 0.054(3) 0.064(4) 0.053(3) 0.002(3) -0.025(3) -0.022(3) O4 0.033(2) 0.049(3) 0.077(4) -0.016(3) 0.008(2) 0.008(2) Cl3 0.0206(6) 0.0328(9) 0.0255(7) 0.0019(6) 0.0001(5) 0.0010(6) O9 0.043(3) 0.048(3) 0.061(3) -0.005(3) -0.026(2) 0.015(2) O10 0.070(3) 0.096(5) 0.032(3) 0.010(3) 0.013(2) -0.017(3) O11 0.039(2) 0.043(3) 0.067(4) -0.021(3) 0.004(2) 0.006(2) O12 0.030(2) 0.042(3) 0.072(4) 0.008(3) -0.003(2) -0.015(2) N12 0.018(2) 0.019(3) 0.019(2) -0.006(2) -0.0009(18) 0.0032(18) C37 0.024(3) 0.027(3) 0.024(3) -0.005(3) -0.004(2) 0.002(2) C38 0.032(3) 0.022(4) 0.032(4) -0.008(3) -0.011(3) 0.007(3) C39 0.032(3) 0.024(3) 0.056(5) 0.007(3) -0.021(3) -0.007(3) C40 0.024(3) 0.016(3) 0.026(3) -0.003(2) -0.004(2) -0.004(2) C41 0.028(3) 0.007(3) 0.030(3) -0.004(2) -0.003(2) -0.001(2) C42 0.024(3) 0.024(3) 0.031(3) 0.001(2) -0.003(3) -0.001(3) N11 0.026(2) 0.023(3) 0.015(2) -0.004(2) -0.0017(19) 0.005(2) C31 0.021(3) 0.029(3) 0.024(3) -0.004(3) -0.004(2) -0.002(2) C32 0.027(3) 0.020(3) 0.018(3) 0.003(2) 0.002(2) 0.009(2) C33 0.044(4) 0.037(4) 0.024(4) -0.003(3) 0.006(3) 0.008(3) C34 0.028(3) 0.036(4) 0.013(3) 0.005(2) -0.001(2) 0.008(3) C35 0.030(3) 0.033(4) 0.019(3) -0.003(3) -0.003(2) 0.012(3) C36 0.027(3) 0.039(4) 0.019(3) -0.009(3) -0.004(2) 0.007(3) C22 0.012(2) 0.016(3) 0.028(3) 0.003(2) 0.005(2) 0.001(2) N7 0.017(2) 0.021(3) 0.019(2) -0.0032(19) -0.0014(17) 0.0015(19) C23 0.010(2) 0.018(3) 0.023(3) 0.002(2) 0.003(2) -0.001(2) N8 0.017(2) 0.019(3) 0.018(3) -0.006(2) 0.0003(18) -0.0020(19) C24 0.011(2) 0.020(3) 0.018(3) -0.003(2) 0.002(2) -0.006(2) N9 0.016(2) 0.022(3) 0.010(2) 0.0004(19) -0.0029(17) -0.0012(18) C1 0.014(2) 0.027(3) 0.016(3) 0.004(2) 0.002(2) 0.002(2) N1 0.021(2) 0.019(3) 0.024(3) 0.003(2) 0.0058(19) -0.0032(19) C2 0.016(2) 0.018(3) 0.028(3) 0.001(3) -0.002(2) 0.000(2) N2 0.015(2) 0.016(3) 0.021(3) 0.000(2) -0.0009(18) -0.0037(18) C3 0.012(2) 0.023(3) 0.023(3) 0.006(3) -0.002(2) 0.002(2) N3 0.0171(19) 0.020(3) 0.019(2) 0.006(2) -0.0048(16) -0.0017(18) N4 0.022(2) 0.023(3) 0.021(3) 0.008(2) -0.0054(19) -0.003(2) C4 0.027(3) 0.028(4) 0.024(3) 0.015(3) -0.007(2) -0.012(2) C5 0.043(4) 0.033(4) 0.032(4) 0.020(3) -0.019(3) -0.017(3) C6 0.044(4) 0.050(5) 0.058(5) 0.022(4) -0.011(4) -0.008(4) C7 0.022(3) 0.017(3) 0.027(3) 0.005(2) -0.003(2) 0.000(2) C8 0.021(3) 0.017(3) 0.022(3) 0.005(2) 0.001(2) -0.002(2) C9 0.032(3) 0.015(3) 0.029(3) 0.004(2) -0.001(3) -0.006(2) N5 0.021(2) 0.022(3) 0.022(3) 0.002(2) 0.0022(19) -0.004(2) C10 0.028(3) 0.035(3) 0.018(3) 0.003(3) 0.003(2) -0.001(3) C11 0.033(3) 0.036(4) 0.019(3) 0.003(3) -0.007(2) -0.009(3) C12 0.034(3) 0.041(4) 0.025(3) 0.011(3) -0.001(3) -0.002(3) C13 0.025(3) 0.023(3) 0.019(3) 0.007(3) -0.004(2) 0.002(2) C14 0.025(3) 0.022(3) 0.023(3) 0.005(3) -0.001(2) -0.003(2) C15 0.033(3) 0.049(5) 0.033(4) -0.004(3) 0.008(3) -0.011(3) N6 0.020(2) 0.014(2) 0.022(3) 0.002(2) 0.0013(19) -0.0039(19) C16 0.037(3) 0.024(3) 0.026(4) -0.006(3) -0.013(3) 0.003(3) C17 0.045(4) 0.029(4) 0.047(4) -0.009(3) -0.008(3) -0.001(3) C18 0.039(4) 0.036(4) 0.058(5) 0.008(4) -0.013(4) -0.011(3) C19 0.021(3) 0.018(3) 0.037(4) -0.002(3) 0.002(3) -0.004(2) C20 0.021(3) 0.016(3) 0.027(3) 0.001(3) 0.002(2) -0.002(2) C21 0.029(3) 0.022(3) 0.022(3) 0.008(3) 0.010(2) -0.004(3) N10 0.021(2) 0.015(2) 0.016(3) 0.0021(19) -0.0026(18) 0.0016(19) C25 0.026(3) 0.021(3) 0.014(3) 0.003(2) 0.000(2) -0.003(2) C26 0.023(3) 0.024(3) 0.028(3) -0.007(3) -0.011(2) 0.001(2) C27 0.026(3) 0.028(3) 0.032(4) -0.009(3) 0.002(3) 0.000(2) C28 0.023(3) 0.018(3) 0.020(3) -0.002(2) 0.000(2) -0.005(2) C29 0.023(3) 0.026(3) 0.021(3) -0.007(3) 0.000(2) 0.002(2) C30 0.044(3) 0.019(3) 0.018(3) -0.002(3) 0.000(2) -0.003(3) Cl4 0.0278(7) 0.0257(8) 0.0256(8) -0.0034(6) -0.0059(6) -0.0046(6) O13 0.029(2) 0.054(3) 0.087(4) 0.001(3) -0.021(3) -0.011(2) O14 0.052(2) 0.029(3) 0.030(2) 0.009(2) -0.0129(19) -0.015(2) O15 0.052(3) 0.028(2) 0.029(3) 0.006(2) 0.003(2) -0.001(2) O16 0.062(3) 0.056(3) 0.035(3) -0.025(3) 0.001(2) 0.010(3) Cl2 0.0273(7) 0.0310(9) 0.0231(8) -0.0009(6) 0.0007(6) -0.0006(6) O5 0.022(2) 0.064(4) 0.060(3) 0.008(3) 0.003(2) -0.005(2) O6 0.060(3) 0.064(4) 0.042(3) 0.021(3) 0.017(3) -0.001(3) O7 0.073(3) 0.061(3) 0.023(3) 0.009(2) -0.012(2) -0.034(3) O8 0.073(4) 0.064(4) 0.083(5) -0.039(4) 0.007(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C12 2.379(6) . ? Ag1 C30 2.389(5) 1_655 ? Ag1 C9 2.441(5) . ? Ag1 C11 2.462(6) . ? Ag1 C8 2.469(5) . ? Ag1 N3 2.486(4) . ? Ag1 C29 2.518(6) 1_655 ? Ag3 C36 2.380(6) . ? Ag3 C21 2.413(5) . ? Ag3 C42 2.444(6) . ? Ag3 C41 2.473(5) . ? Ag3 C35 2.476(5) . ? Ag3 N7 2.500(4) . ? Ag3 C20 2.517(5) . ? Ag2 C18 2.332(6) . ? Ag2 C5 2.386(6) . ? Ag2 C6 2.389(7) . ? Ag2 C17 2.464(7) . ? Ag2 O2 2.518(5) . ? Ag2 N2 2.527(4) . ? Ag4 C39 2.341(6) . ? Ag4 C27 2.350(5) . ? Ag4 C38 2.395(6) . ? Ag4 C26 2.424(6) . ? Ag4 N8 2.628(4) . ? Cl1 O2 1.397(6) . ? Cl1 O1 1.404(7) . ? Cl1 O3 1.409(5) . ? Cl1 O4 1.417(5) . ? Cl3 O10 1.404(5) . ? Cl3 O9 1.426(4) . ? Cl3 O12 1.427(4) . ? Cl3 O11 1.438(5) . ? N12 C23 1.354(7) . ? N12 C40 1.453(7) . ? N12 C37 1.464(7) . ? C37 C38 1.511(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.315(9) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C39 H39B 0.9500 . ? C40 C41 1.514(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.316(8) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C42 H42B 0.9500 . ? N11 C22 1.354(7) . ? N11 C31 1.462(7) . ? N11 C34 1.467(7) . ? C31 C32 1.501(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.299(8) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C33 H33B 0.9500 . ? C34 C35 1.505(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.319(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C36 H36B 0.9500 . ? C22 N9 1.325(7) . ? C22 N7 1.361(7) . ? N7 C23 1.340(7) . ? C23 N8 1.353(7) . ? N8 C24 1.356(7) . ? C24 N9 1.335(7) . ? C24 N10 1.361(7) . ? C1 N3 1.330(7) . ? C1 N1 1.346(7) . ? C1 N5 1.372(7) . ? N1 C2 1.340(7) . ? C2 N2 1.345(7) . ? C2 N6 1.347(7) . ? N2 C3 1.346(7) . ? C3 N3 1.353(6) . ? C3 N4 1.356(7) . ? N4 C4 1.449(7) . ? N4 C7 1.471(7) . ? C4 C5 1.543(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.316(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.490(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.342(8) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? N5 C13 1.458(7) . ? N5 C10 1.472(7) . ? C10 C11 1.508(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.304(8) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.508(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.304(8) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C15 H15B 0.9500 . ? N6 C16 1.447(7) . ? N6 C19 1.473(7) . ? C16 C17 1.494(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.262(9) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C19 C20 1.491(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.321(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C21 H21B 0.9500 . ? N10 C28 1.452(7) . ? N10 C25 1.458(7) . ? C25 C26 1.508(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.313(8) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C27 H27B 0.9500 . ? C28 C29 1.508(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.346(8) . ? C29 Ag1 2.518(6) 1_455 ? C29 H29A 0.9500 . ? C30 Ag1 2.389(5) 1_455 ? C30 H30A 0.9500 . ? C30 H30B 0.9500 . ? Cl4 O15 1.423(4) . ? Cl4 O16 1.427(5) . ? Cl4 O13 1.433(4) . ? Cl4 O14 1.441(4) . ? Cl2 O5 1.408(4) . ? Cl2 O7 1.418(4) . ? Cl2 O6 1.421(5) . ? Cl2 O8 1.425(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Ag1 C30 118.1(2) . 1_655 ? C12 Ag1 C9 126.1(2) . . ? C30 Ag1 C9 105.9(2) 1_655 . ? C12 Ag1 C11 31.2(2) . . ? C30 Ag1 C11 148.6(2) 1_655 . ? C9 Ag1 C11 103.2(2) . . ? C12 Ag1 C8 155.6(2) . . ? C30 Ag1 C8 85.14(19) 1_655 . ? C9 Ag1 C8 31.73(18) . . ? C11 Ag1 C8 126.3(2) . . ? C12 Ag1 N3 98.16(18) . . ? C30 Ag1 N3 102.34(17) 1_655 . ? C9 Ag1 N3 101.44(17) . . ? C11 Ag1 N3 83.01(15) . . ? C8 Ag1 N3 82.84(15) . . ? C12 Ag1 C29 87.8(2) . 1_655 ? C30 Ag1 C29 31.72(19) 1_655 1_655 ? C9 Ag1 C29 136.4(2) . 1_655 ? C11 Ag1 C29 117.1(2) . 1_655 ? C8 Ag1 C29 116.28(19) . 1_655 ? N3 Ag1 C29 99.33(16) . 1_655 ? C36 Ag3 C21 118.5(2) . . ? C36 Ag3 C42 125.8(2) . . ? C21 Ag3 C42 106.7(2) . . ? C36 Ag3 C41 154.4(2) . . ? C21 Ag3 C41 86.1(2) . . ? C42 Ag3 C41 31.04(18) . . ? C36 Ag3 C35 31.4(2) . . ? C21 Ag3 C35 149.2(2) . . ? C42 Ag3 C35 102.1(2) . . ? C41 Ag3 C35 124.6(2) . . ? C36 Ag3 N7 97.72(17) . . ? C21 Ag3 N7 102.73(17) . . ? C42 Ag3 N7 100.01(17) . . ? C41 Ag3 N7 82.32(16) . . ? C35 Ag3 N7 82.32(15) . . ? C36 Ag3 C20 88.9(2) . . ? C21 Ag3 C20 31.01(19) . . ? C42 Ag3 C20 136.78(19) . . ? C41 Ag3 C20 116.44(19) . . ? C35 Ag3 C20 118.4(2) . . ? N7 Ag3 C20 99.54(16) . . ? C18 Ag2 C5 164.0(3) . . ? C18 Ag2 C6 133.8(3) . . ? C5 Ag2 C6 32.0(2) . . ? C18 Ag2 C17 30.4(2) . . ? C5 Ag2 C17 135.4(3) . . ? C6 Ag2 C17 113.1(3) . . ? C18 Ag2 O2 96.4(3) . . ? C5 Ag2 O2 99.5(3) . . ? C6 Ag2 O2 127.1(3) . . ? C17 Ag2 O2 119.6(3) . . ? C18 Ag2 N2 96.7(2) . . ? C5 Ag2 N2 85.31(17) . . ? C6 Ag2 N2 106.0(2) . . ? C17 Ag2 N2 83.16(18) . . ? O2 Ag2 N2 77.73(18) . . ? C39 Ag4 C27 145.3(2) . . ? C39 Ag4 C38 32.2(2) . . ? C27 Ag4 C38 176.4(2) . . ? C39 Ag4 C26 174.8(2) . . ? C27 Ag4 C26 31.88(19) . . ? C38 Ag4 C26 150.1(2) . . ? C39 Ag4 N8 92.43(18) . . ? C27 Ag4 N8 94.73(18) . . ? C38 Ag4 N8 83.21(17) . . ? C26 Ag4 N8 84.12(16) . . ? O2 Cl1 O1 111.2(6) . . ? O2 Cl1 O3 108.5(4) . . ? O1 Cl1 O3 109.2(4) . . ? O2 Cl1 O4 107.4(4) . . ? O1 Cl1 O4 109.7(4) . . ? O3 Cl1 O4 110.9(3) . . ? Cl1 O2 Ag2 160.2(6) . . ? O10 Cl3 O9 110.3(3) . . ? O10 Cl3 O12 110.2(3) . . ? O9 Cl3 O12 109.4(3) . . ? O10 Cl3 O11 109.4(4) . . ? O9 Cl3 O11 109.2(3) . . ? O12 Cl3 O11 108.2(3) . . ? C23 N12 C40 120.5(4) . . ? C23 N12 C37 121.5(5) . . ? C40 N12 C37 117.6(4) . . ? N12 C37 C38 113.1(5) . . ? N12 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? N12 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C39 C38 C37 126.0(6) . . ? C39 C38 Ag4 71.6(4) . . ? C37 C38 Ag4 103.2(4) . . ? C39 C38 H38A 117.0 . . ? C37 C38 H38A 117.0 . . ? Ag4 C38 H38A 95.4 . . ? C38 C39 Ag4 76.2(4) . . ? C38 C39 H39A 120.0 . . ? Ag4 C39 H39A 99.7 . . ? C38 C39 H39B 120.0 . . ? Ag4 C39 H39B 94.1 . . ? H39A C39 H39B 120.0 . . ? N12 C40 C41 114.3(4) . . ? N12 C40 H40A 108.7 . . ? C41 C40 H40A 108.7 . . ? N12 C40 H40B 108.7 . . ? C41 C40 H40B 108.7 . . ? H40A C40 H40B 107.6 . . ? C42 C41 C40 123.6(5) . . ? C42 C41 Ag3 73.3(3) . . ? C40 C41 Ag3 104.2(3) . . ? C42 C41 H41A 118.2 . . ? C40 C41 H41A 118.2 . . ? Ag3 C41 H41A 92.5 . . ? C41 C42 Ag3 75.7(3) . . ? C41 C42 H42A 120.0 . . ? Ag3 C42 H42A 102.4 . . ? C41 C42 H42B 120.0 . . ? Ag3 C42 H42B 91.8 . . ? H42A C42 H42B 120.0 . . ? C22 N11 C31 119.9(5) . . ? C22 N11 C34 120.7(5) . . ? C31 N11 C34 118.7(4) . . ? N11 C31 C32 113.8(5) . . ? N11 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? N11 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C33 C32 C31 124.4(6) . . ? C33 C32 H32A 117.8 . . ? C31 C32 H32A 117.8 . . ? C32 C33 H33A 120.0 . . ? C32 C33 H33B 120.0 . . ? H33A C33 H33B 120.0 . . ? N11 C34 C35 114.2(5) . . ? N11 C34 H34A 108.7 . . ? C35 C34 H34A 108.7 . . ? N11 C34 H34B 108.7 . . ? C35 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C36 C35 C34 125.4(6) . . ? C36 C35 Ag3 70.2(3) . . ? C34 C35 Ag3 104.9(3) . . ? C36 C35 H35A 117.3 . . ? C34 C35 H35A 117.3 . . ? Ag3 C35 H35A 95.0 . . ? C35 C36 Ag3 78.3(4) . . ? C35 C36 H36A 120.0 . . ? Ag3 C36 H36A 99.8 . . ? C35 C36 H36B 120.0 . . ? Ag3 C36 H36B 91.9 . . ? H36A C36 H36B 120.0 . . ? N9 C22 N11 117.6(5) . . ? N9 C22 N7 126.1(5) . . ? N11 C22 N7 116.4(5) . . ? C23 N7 C22 114.0(5) . . ? C23 N7 Ag3 113.1(3) . . ? C22 N7 Ag3 114.0(3) . . ? N7 C23 N8 126.1(5) . . ? N7 C23 N12 116.3(5) . . ? N8 C23 N12 117.6(5) . . ? C23 N8 C24 112.7(5) . . ? C23 N8 Ag4 115.1(3) . . ? C24 N8 Ag4 113.9(3) . . ? N9 C24 N8 127.1(5) . . ? N9 C24 N10 116.1(5) . . ? N8 C24 N10 116.7(5) . . ? C22 N9 C24 114.0(5) . . ? N3 C1 N1 126.7(5) . . ? N3 C1 N5 117.1(5) . . ? N1 C1 N5 116.1(5) . . ? C2 N1 C1 113.7(5) . . ? N1 C2 N2 126.0(5) . . ? N1 C2 N6 116.7(5) . . ? N2 C2 N6 117.3(5) . . ? C2 N2 C3 114.2(5) . . ? C2 N2 Ag2 111.7(3) . . ? C3 N2 Ag2 110.4(3) . . ? N2 C3 N3 125.5(5) . . ? N2 C3 N4 117.8(5) . . ? N3 C3 N4 116.7(5) . . ? C1 N3 C3 113.8(5) . . ? C1 N3 Ag1 115.0(3) . . ? C3 N3 Ag1 114.0(3) . . ? C3 N4 C4 122.5(5) . . ? C3 N4 C7 119.8(4) . . ? C4 N4 C7 117.2(4) . . ? N4 C4 C5 112.6(5) . . ? N4 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N4 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 123.5(7) . . ? C6 C5 Ag2 74.1(4) . . ? C4 C5 Ag2 104.0(4) . . ? C6 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? Ag2 C5 H5A 91.9 . . ? C5 C6 Ag2 73.9(4) . . ? C5 C6 H6A 120.0 . . ? Ag2 C6 H6A 103.5 . . ? C5 C6 H6B 120.0 . . ? Ag2 C6 H6B 92.5 . . ? H6A C6 H6B 120.0 . . ? N4 C7 C8 114.1(5) . . ? N4 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N4 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 122.9(5) . . ? C9 C8 Ag1 73.0(3) . . ? C7 C8 Ag1 104.0(3) . . ? C9 C8 H8A 118.5 . . ? C7 C8 H8A 118.5 . . ? Ag1 C8 H8A 93.0 . . ? C8 C9 Ag1 75.3(3) . . ? C8 C9 H9A 120.0 . . ? Ag1 C9 H9A 102.3 . . ? C8 C9 H9B 120.0 . . ? Ag1 C9 H9B 92.3 . . ? H9A C9 H9B 120.0 . . ? C1 N5 C13 121.2(5) . . ? C1 N5 C10 118.8(5) . . ? C13 N5 C10 119.0(4) . . ? N5 C10 C11 114.8(5) . . ? N5 C10 H10A 108.6 . . ? C11 C10 H10A 108.6 . . ? N5 C10 H10B 108.6 . . ? C11 C10 H10B 108.6 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C10 125.4(6) . . ? C12 C11 Ag1 70.9(3) . . ? C10 C11 Ag1 103.9(3) . . ? C12 C11 H11A 117.3 . . ? C10 C11 H11A 117.3 . . ? Ag1 C11 H11A 95.5 . . ? C11 C12 Ag1 78.0(4) . . ? C11 C12 H12A 120.0 . . ? Ag1 C12 H12A 99.1 . . ? C11 C12 H12B 120.0 . . ? Ag1 C12 H12B 92.9 . . ? H12A C12 H12B 120.0 . . ? N5 C13 C14 112.6(5) . . ? N5 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N5 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 122.4(5) . . ? C15 C14 H14A 118.8 . . ? C13 C14 H14A 118.8 . . ? C14 C15 H15A 120.0 . . ? C14 C15 H15B 120.0 . . ? H15A C15 H15B 120.0 . . ? C2 N6 C16 121.3(5) . . ? C2 N6 C19 121.5(5) . . ? C16 N6 C19 117.2(5) . . ? N6 C16 C17 116.6(5) . . ? N6 C16 H16A 108.1 . . ? C17 C16 H16A 108.1 . . ? N6 C16 H16B 108.1 . . ? C17 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C16 122.5(7) . . ? C18 C17 Ag2 69.1(4) . . ? C16 C17 Ag2 103.5(4) . . ? C18 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? Ag2 C17 H17A 97.4 . . ? C17 C18 Ag2 80.6(4) . . ? C17 C18 H18A 120.0 . . ? Ag2 C18 H18A 97.3 . . ? C17 C18 H18B 120.0 . . ? Ag2 C18 H18B 92.1 . . ? H18A C18 H18B 120.0 . . ? N6 C19 C20 110.7(4) . . ? N6 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? N6 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 123.7(5) . . ? C21 C20 Ag3 70.1(3) . . ? C19 C20 Ag3 110.7(3) . . ? C21 C20 H20A 118.1 . . ? C19 C20 H20A 118.1 . . ? Ag3 C20 H20A 89.2 . . ? C20 C21 Ag3 78.9(3) . . ? C20 C21 H21A 120.0 . . ? Ag3 C21 H21A 106.0 . . ? C20 C21 H21B 120.0 . . ? Ag3 C21 H21B 85.3 . . ? H21A C21 H21B 120.0 . . ? C24 N10 C28 121.2(5) . . ? C24 N10 C25 121.4(5) . . ? C28 N10 C25 117.4(4) . . ? N10 C25 C26 113.7(5) . . ? N10 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? N10 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 125.0(6) . . ? C27 C26 Ag4 70.9(4) . . ? C25 C26 Ag4 101.3(3) . . ? C27 C26 H26A 117.5 . . ? C25 C26 H26A 117.5 . . ? Ag4 C26 H26A 98.1 . . ? C26 C27 Ag4 77.2(3) . . ? C26 C27 H27A 120.0 . . ? Ag4 C27 H27A 97.0 . . ? C26 C27 H27B 120.0 . . ? Ag4 C27 H27B 95.8 . . ? H27A C27 H27B 120.0 . . ? N10 C28 C29 109.9(4) . . ? N10 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? N10 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C28 123.3(5) . . ? C30 C29 Ag1 68.8(3) . 1_455 ? C28 C29 Ag1 111.5(3) . 1_455 ? C30 C29 H29A 118.3 . . ? C28 C29 H29A 118.3 . . ? Ag1 C29 H29A 89.6 1_455 . ? C29 C30 Ag1 79.4(3) . 1_455 ? C29 C30 H30A 120.0 . . ? Ag1 C30 H30A 106.0 1_455 . ? C29 C30 H30B 120.0 . . ? Ag1 C30 H30B 84.7 1_455 . ? H30A C30 H30B 120.0 . . ? O15 Cl4 O16 109.3(3) . . ? O15 Cl4 O13 109.8(3) . . ? O16 Cl4 O13 109.4(3) . . ? O15 Cl4 O14 109.9(3) . . ? O16 Cl4 O14 109.9(3) . . ? O13 Cl4 O14 108.5(3) . . ? O5 Cl2 O7 109.6(3) . . ? O5 Cl2 O6 110.0(3) . . ? O7 Cl2 O6 108.8(3) . . ? O5 Cl2 O8 110.1(3) . . ? O7 Cl2 O8 107.7(4) . . ? O6 Cl2 O8 110.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.442 _refine_diff_density_min -2.750 _refine_diff_density_rms 0.107 # start Validation Reply Form _vrf_PLAT241_test ; PROBLEM: Check High Ueq as Compared to Neighbors for O2 RESPONSE: This weakly coordinated oxygen atom is bound to two much heavier atoms (Ag2 and Cl1) whose positions are more precisely defined and subject to less thermal motion. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 940161' ####################################################################### # # 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_test2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H30 Ag3 F9 N6 O9 S3' _chemical_formula_sum 'C24 H30 Ag3 F9 N6 O9 S3' _chemical_formula_weight 1137.33 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.8670(7) _cell_length_b 12.8111(5) _cell_length_c 18.0525(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.503(2) _cell_angle_gamma 90.00 _cell_volume 3662.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 26.67 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5231 _exptl_absorpt_correction_T_max 0.8807 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 114(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 68271 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6487 _reflns_number_gt 4726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0285P)^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 6487 _refine_ls_number_parameters 533 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.990 _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 Ag1 Ag 0.15045(2) 0.43744(2) 0.071948(18) 0.02550(10) Uani 1 1 d . . . Ag2 Ag 0.15051(2) 0.05616(2) 0.101192(18) 0.02521(10) Uani 1 1 d . . . Ag3 Ag 0.52112(2) 0.25285(2) 0.180688(18) 0.02281(9) Uani 1 1 d . . . C1 C 0.2218(3) 0.2589(3) 0.1842(2) 0.0164(9) Uani 1 1 d . . . N4 N 0.1505(2) 0.2627(2) 0.22019(17) 0.0167(8) Uani 1 1 d . . . C4 C 0.1124(3) 0.1671(3) 0.2475(2) 0.0236(10) Uani 1 1 d . . . H4A H 0.0795 0.1849 0.2906 0.028 Uiso 1 1 calc R . . H4B H 0.1582 0.1190 0.2651 0.028 Uiso 1 1 calc R . . C5 C 0.0560(3) 0.1115(3) 0.1916(2) 0.0241(10) Uani 1 1 d . . . H5A H 0.0223 0.1528 0.1576 0.029 Uiso 1 1 calc R . . C6 C 0.0491(3) 0.0075(3) 0.1854(3) 0.0351(12) Uani 1 1 d . . . H6A H 0.0817 -0.0366 0.2184 0.042 Uiso 1 1 calc R . . H6B H 0.0115 -0.0222 0.1482 0.042 Uiso 1 1 calc R . . C7 C 0.1091(3) 0.3633(3) 0.2334(2) 0.0226(10) Uani 1 1 d . . . H7A H 0.1533 0.4158 0.2468 0.027 Uiso 1 1 calc R . . H7B H 0.0739 0.3555 0.2765 0.027 Uiso 1 1 calc R . . C8 C 0.0547(3) 0.4041(3) 0.1691(2) 0.0236(10) Uani 1 1 d . . . H8A H 0.0223 0.3554 0.1396 0.028 Uiso 1 1 calc R . . C9 C 0.0491(3) 0.5055(3) 0.1508(2) 0.0342(12) Uani 1 1 d . . . H9A H 0.0807 0.5560 0.1793 0.041 Uiso 1 1 calc R . . H9B H 0.0134 0.5269 0.1094 0.041 Uiso 1 1 calc R . . N1 N 0.2551(2) 0.1640(2) 0.17224(16) 0.0152(7) Uani 1 1 d . . . S2 S 0.47016(8) 0.26487(7) 0.36804(6) 0.0248(3) Uani 1 1 d . . . O4 O 0.4828(2) 0.3124(2) 0.29700(16) 0.0382(9) Uani 1 1 d . . . O5 O 0.4811(2) 0.1540(2) 0.37073(17) 0.0396(9) Uani 1 1 d . . . O6 O 0.5086(2) 0.3213(2) 0.42987(16) 0.0384(9) Uani 1 1 d . . . C23 C 0.3575(3) 0.2819(3) 0.3784(2) 0.0328(12) Uani 1 1 d . . . F4 F 0.3128(2) 0.2290(3) 0.32791(17) 0.0735(11) Uani 1 1 d . . . F5 F 0.33576(18) 0.2493(2) 0.44427(15) 0.0451(7) Uani 1 1 d . . . F6 F 0.3347(2) 0.3811(2) 0.3723(2) 0.0752(11) Uani 1 1 d . . . S1 S 0.09141(8) 0.24136(9) -0.03372(6) 0.0306(3) Uani 1 1 d . . . O1 O 0.0988(2) 0.3499(2) -0.05292(19) 0.0549(11) Uani 1 1 d . . . O2 O 0.1245(2) 0.2220(2) 0.04138(16) 0.0382(9) Uani 1 1 d . . . O3 O 0.1136(3) 0.1667(3) -0.08754(19) 0.0637(12) Uani 1 1 d . . . C22 C -0.0211(4) 0.2235(4) -0.0271(3) 0.0511(15) Uani 1 1 d . . . F1 F -0.0525(2) 0.2948(3) 0.0173(2) 0.0888(13) Uani 1 1 d . . . F2 F -0.0378(2) 0.1300(3) 0.00047(19) 0.0771(11) Uani 1 1 d . . . F3 F -0.0632(2) 0.2310(2) -0.09186(19) 0.0770(12) Uani 1 1 d . . . C2 C 0.3297(3) 0.1656(3) 0.1416(2) 0.0151(9) Uani 1 1 d . . . N5 N 0.3666(2) 0.0734(2) 0.12615(18) 0.0178(8) Uani 1 1 d . . . C10 C 0.3302(3) -0.0253(3) 0.1488(2) 0.0237(11) Uani 1 1 d . . . H10A H 0.3042 -0.0151 0.1967 0.028 Uiso 1 1 calc R . . H10B H 0.3761 -0.0773 0.1567 0.028 Uiso 1 1 calc R . . C11 C 0.2648(3) -0.0678(3) 0.0932(3) 0.0298(11) Uani 1 1 d . . . H11A H 0.2349 -0.1282 0.1071 0.036 Uiso 1 1 calc R . . C12 C 0.2450(3) -0.0283(4) 0.0261(3) 0.0350(12) Uani 1 1 d . . . H12A H 0.2733 0.0321 0.0098 0.042 Uiso 1 1 calc R . . H12B H 0.2025 -0.0605 -0.0055 0.042 Uiso 1 1 calc R . . C13 C 0.4407(3) 0.0691(3) 0.0824(2) 0.0209(10) Uani 1 1 d . . . H13A H 0.4378 0.1273 0.0462 0.025 Uiso 1 1 calc R . . H13B H 0.4394 0.0030 0.0539 0.025 Uiso 1 1 calc R . . C14 C 0.5228(3) 0.0756(3) 0.1276(2) 0.0227(10) Uani 1 1 d . . . H14A H 0.5723 0.0851 0.1014 0.027 Uiso 1 1 calc R . . C15 C 0.5327(3) 0.0694(3) 0.2014(2) 0.0298(11) Uani 1 1 d . . . H15A H 0.4850 0.0600 0.2300 0.036 Uiso 1 1 calc R . . H15B H 0.5876 0.0744 0.2254 0.036 Uiso 1 1 calc R . . N2 N 0.3728(2) 0.2525(2) 0.12404(17) 0.0150(7) Uani 1 1 d . . . C3 C 0.3296(3) 0.3422(3) 0.1322(2) 0.0161(9) Uani 1 1 d . . . N6 N 0.3665(2) 0.4308(2) 0.11017(17) 0.0176(8) Uani 1 1 d . . . C16 C 0.3269(3) 0.5324(3) 0.1213(2) 0.0215(10) Uani 1 1 d . . . H16A H 0.3717 0.5861 0.1268 0.026 Uiso 1 1 calc R . . H16B H 0.2977 0.5303 0.1682 0.026 Uiso 1 1 calc R . . C17 C 0.2647(3) 0.5644(3) 0.0596(3) 0.0303(11) Uani 1 1 d . . . H17A H 0.2321 0.6251 0.0679 0.036 Uiso 1 1 calc R . . C18 C 0.2501(3) 0.5171(3) -0.0051(2) 0.0322(12) Uani 1 1 d . . . H18A H 0.2809 0.4561 -0.0163 0.039 Uiso 1 1 calc R . . H18B H 0.2090 0.5442 -0.0404 0.039 Uiso 1 1 calc R . . C19 C 0.4420(3) 0.4267(3) 0.0682(2) 0.0206(10) Uani 1 1 d . . . H19A H 0.4440 0.4907 0.0376 0.025 Uiso 1 1 calc R . . H19B H 0.4369 0.3665 0.0338 0.025 Uiso 1 1 calc R . . C20 C 0.5244(3) 0.4173(3) 0.1138(2) 0.0224(10) Uani 1 1 d . . . H20A H 0.5305 0.4536 0.1597 0.027 Uiso 1 1 calc R . . C21 C 0.5889(3) 0.3608(3) 0.0930(2) 0.0307(11) Uani 1 1 d . . . H21A H 0.5844 0.3238 0.0473 0.037 Uiso 1 1 calc R . . H21B H 0.6396 0.3574 0.1237 0.037 Uiso 1 1 calc R . . N3 N 0.2535(2) 0.3499(2) 0.16061(17) 0.0167(8) Uani 1 1 d . . . O7 O 0.2019(4) -0.2995(4) 0.2019(2) 0.1008(17) Uani 1 1 d U . . O8 O 0.2198(3) -0.1443(3) 0.2826(3) 0.0929(16) Uani 1 1 d U . . S3 S 0.1837(3) -0.2409(2) 0.26211(14) 0.0311(7) Uani 0.592(5) 1 d P A 1 O9 O 0.0945(4) -0.2298(4) 0.2607(4) 0.058(2) Uani 0.592(5) 1 d P A 1 S3' S 0.2327(4) -0.2412(3) 0.2585(2) 0.0373(11) Uani 0.408(5) 1 d P A 2 O9' O 0.3185(6) -0.2438(7) 0.2481(5) 0.063(3) Uani 0.408(5) 1 d P A 2 C24 C 0.2113(4) -0.3248(4) 0.3407(3) 0.0466(15) Uani 1 1 d . . . F7 F 0.2865(4) -0.3483(7) 0.3528(5) 0.078(2) Uani 0.592(5) 1 d PU A 1 F8 F 0.1901(7) -0.2685(5) 0.4049(3) 0.084(3) Uani 0.592(5) 1 d P A 1 F9 F 0.1624(5) -0.4069(5) 0.3412(4) 0.068(3) Uani 0.592(5) 1 d P A 1 F7' F 0.1441(8) -0.3446(12) 0.3558(7) 0.091(4) Uani 0.408(5) 1 d PU A 2 F8' F 0.2477(8) -0.4265(6) 0.3166(6) 0.083(4) Uani 0.408(5) 1 d P A 2 F9' F 0.2631(9) -0.3034(9) 0.3944(5) 0.072(3) Uani 0.408(5) 1 d PU 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 Ag1 0.0203(2) 0.02987(19) 0.02630(18) 0.00273(15) 0.00100(15) 0.00114(15) Ag2 0.0221(2) 0.02826(19) 0.02541(18) -0.00348(15) 0.00309(15) -0.00545(15) Ag3 0.0232(2) 0.02177(17) 0.02352(18) 0.00100(14) 0.00193(14) 0.00105(15) C1 0.018(2) 0.017(2) 0.013(2) 0.0012(16) -0.0047(19) 0.0001(18) N4 0.016(2) 0.0175(18) 0.0172(18) 0.0005(14) 0.0051(16) 0.0005(15) C4 0.027(3) 0.026(2) 0.019(2) 0.0033(18) 0.012(2) -0.002(2) C5 0.019(3) 0.030(2) 0.024(2) 0.0052(19) 0.009(2) -0.002(2) C6 0.034(3) 0.035(3) 0.038(3) 0.000(2) 0.016(3) -0.009(2) C7 0.022(3) 0.026(2) 0.021(2) 0.0015(19) 0.009(2) 0.006(2) C8 0.017(3) 0.031(2) 0.024(2) -0.0023(19) 0.007(2) 0.0055(19) C9 0.034(3) 0.038(3) 0.032(3) 0.003(2) 0.012(2) 0.016(2) N1 0.014(2) 0.0169(17) 0.0152(17) -0.0016(14) 0.0019(15) -0.0015(14) S2 0.0342(7) 0.0174(6) 0.0235(6) -0.0009(4) 0.0075(5) 0.0005(5) O4 0.063(3) 0.0274(18) 0.0255(17) 0.0012(14) 0.0178(17) 0.0039(16) O5 0.054(3) 0.0159(16) 0.050(2) 0.0031(15) 0.0106(18) 0.0096(15) O6 0.041(2) 0.043(2) 0.0321(18) -0.0103(15) 0.0051(17) -0.0169(16) C23 0.039(3) 0.034(3) 0.025(3) 0.002(2) -0.005(2) 0.001(2) F4 0.050(2) 0.119(3) 0.048(2) -0.0175(19) -0.0224(18) -0.013(2) F5 0.0338(18) 0.067(2) 0.0351(16) 0.0142(14) 0.0066(14) -0.0066(15) F6 0.062(3) 0.054(2) 0.114(3) 0.0338(19) 0.039(2) 0.0340(17) S1 0.0380(8) 0.0322(6) 0.0203(6) 0.0017(5) -0.0078(6) -0.0015(6) O1 0.063(3) 0.040(2) 0.060(2) 0.0205(18) -0.010(2) -0.0105(19) O2 0.046(2) 0.046(2) 0.0214(16) 0.0067(14) -0.0138(16) 0.0001(16) O3 0.072(3) 0.076(3) 0.043(2) -0.032(2) 0.003(2) 0.001(2) C22 0.049(4) 0.050(4) 0.052(4) -0.003(3) -0.014(3) -0.013(3) F1 0.038(2) 0.112(3) 0.116(3) -0.049(3) -0.001(2) 0.006(2) F2 0.062(3) 0.081(2) 0.086(3) 0.017(2) -0.011(2) -0.038(2) F3 0.063(3) 0.087(3) 0.075(3) 0.0026(19) -0.048(2) -0.0089(19) C2 0.014(3) 0.017(2) 0.014(2) 0.0003(16) -0.0031(18) 0.0002(17) N5 0.018(2) 0.0117(17) 0.0246(19) 0.0008(14) 0.0082(16) -0.0013(15) C10 0.028(3) 0.011(2) 0.033(3) 0.0038(18) 0.008(2) 0.0007(18) C11 0.029(3) 0.019(2) 0.042(3) -0.008(2) 0.012(2) -0.007(2) C12 0.030(3) 0.040(3) 0.035(3) -0.019(2) 0.006(2) -0.007(2) C13 0.019(3) 0.021(2) 0.023(2) -0.0031(18) 0.0070(19) -0.0003(19) C14 0.021(3) 0.016(2) 0.033(3) -0.0021(19) 0.007(2) 0.0028(18) C15 0.032(3) 0.019(2) 0.038(3) 0.003(2) -0.001(2) 0.002(2) N2 0.0156(19) 0.0121(16) 0.0174(17) -0.0001(14) 0.0027(15) 0.0005(15) C3 0.016(3) 0.017(2) 0.015(2) -0.0001(16) -0.0018(18) -0.0015(18) N6 0.014(2) 0.0152(17) 0.0244(18) 0.0041(14) 0.0043(15) -0.0005(14) C16 0.022(3) 0.015(2) 0.028(2) 0.0011(18) 0.004(2) 0.0006(18) C17 0.024(3) 0.022(2) 0.045(3) 0.012(2) 0.003(2) -0.001(2) C18 0.023(3) 0.041(3) 0.032(3) 0.013(2) -0.002(2) 0.001(2) C19 0.019(3) 0.020(2) 0.024(2) 0.0040(18) 0.0058(19) -0.0004(19) C20 0.025(3) 0.018(2) 0.025(2) 0.0045(18) 0.007(2) -0.0049(19) C21 0.027(3) 0.029(2) 0.036(3) 0.012(2) 0.007(2) 0.000(2) N3 0.016(2) 0.0144(17) 0.0195(18) 0.0031(14) 0.0026(16) 0.0005(14) O7 0.136(5) 0.121(4) 0.047(3) -0.008(3) 0.013(3) -0.004(4) O8 0.120(4) 0.055(3) 0.102(4) 0.023(3) -0.017(3) -0.009(3) S3 0.0301(19) 0.0357(13) 0.0283(13) 0.0059(9) 0.0096(13) -0.0021(15) O9 0.042(5) 0.058(4) 0.075(5) 0.026(3) 0.006(4) 0.019(3) S3' 0.037(3) 0.041(2) 0.033(2) 0.0094(15) -0.005(2) 0.008(2) O9' 0.053(7) 0.087(8) 0.048(6) 0.039(5) -0.009(5) -0.019(6) C24 0.036(4) 0.055(4) 0.047(4) 0.016(3) -0.014(3) -0.018(3) F7 0.038(4) 0.103(6) 0.091(5) 0.029(4) -0.011(4) 0.014(4) F8 0.148(8) 0.076(5) 0.031(3) 0.004(3) 0.022(4) 0.027(5) F9 0.068(6) 0.038(4) 0.092(5) 0.029(4) -0.036(5) -0.029(4) F7' 0.049(6) 0.118(8) 0.107(8) 0.027(7) 0.022(6) -0.029(7) F8' 0.110(10) 0.028(5) 0.114(8) 0.017(5) 0.034(7) 0.003(5) F9' 0.094(8) 0.077(6) 0.041(5) 0.011(5) -0.020(6) -0.046(6) _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 C9 2.378(4) . ? Ag1 C18 2.397(4) . ? Ag1 C8 2.428(4) . ? Ag1 C17 2.455(4) . ? Ag1 N3 2.485(3) . ? Ag2 C12 2.346(4) . ? Ag2 C6 2.365(4) . ? Ag2 C5 2.390(4) . ? Ag2 O2 2.407(3) . ? Ag2 C11 2.421(4) . ? Ag2 N1 2.458(3) . ? Ag3 O4 2.349(3) . ? Ag3 C15 2.385(4) . ? Ag3 C21 2.406(4) . ? Ag3 C20 2.431(4) . ? Ag3 C14 2.465(4) . ? Ag3 N2 2.508(3) . ? C1 N4 1.340(5) . ? C1 N3 1.349(5) . ? C1 N1 1.348(4) . ? N4 C4 1.464(5) . ? N4 C7 1.473(5) . ? C4 C5 1.489(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.341(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.498(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.343(5) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? N1 C2 1.338(5) . ? S2 O5 1.431(3) . ? S2 O6 1.434(3) . ? S2 O4 1.444(3) . ? S2 C23 1.822(5) . ? C23 F4 1.309(5) . ? C23 F6 1.324(5) . ? C23 F5 1.326(5) . ? S1 O3 1.423(3) . ? S1 O1 1.439(3) . ? S1 O2 1.445(3) . ? S1 C22 1.811(6) . ? C22 F3 1.314(6) . ? C22 F2 1.330(6) . ? C22 F1 1.332(6) . ? C2 N2 1.354(5) . ? C2 N5 1.355(5) . ? N5 C13 1.458(5) . ? N5 C10 1.459(4) . ? C10 C11 1.501(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.334(6) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C12 H12B 0.9500 . ? C13 C14 1.496(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.334(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C15 H15B 0.9500 . ? N2 C3 1.350(5) . ? C3 N3 1.344(5) . ? C3 N6 1.348(5) . ? N6 C19 1.457(5) . ? N6 C16 1.464(5) . ? C16 C17 1.499(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.324(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C18 H18B 0.9500 . ? C19 C20 1.507(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.326(6) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C21 H21B 0.9500 . ? O7 S3' 1.334(6) . ? O7 S3 1.367(5) . ? O8 S3' 1.335(6) . ? O8 S3 1.405(5) . ? S3 O9 1.420(8) . ? S3 C24 1.813(6) . ? S3' O9' 1.387(12) . ? S3' C24 1.878(7) . ? C24 F7' 1.146(12) . ? C24 F7 1.237(8) . ? C24 F9' 1.261(10) . ? C24 F9 1.307(8) . ? C24 F8 1.423(9) . ? C24 F8' 1.500(10) . ? 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 C9 Ag1 C18 133.28(16) . . ? C9 Ag1 C8 32.43(13) . . ? C18 Ag1 C8 163.42(15) . . ? C9 Ag1 C17 109.94(16) . . ? C18 Ag1 C17 31.64(14) . . ? C8 Ag1 C17 132.84(15) . . ? C9 Ag1 N3 102.86(14) . . ? C18 Ag1 N3 97.71(13) . . ? C8 Ag1 N3 82.62(12) . . ? C17 Ag1 N3 84.08(13) . . ? C12 Ag2 C6 137.24(16) . . ? C12 Ag2 C5 168.81(15) . . ? C6 Ag2 C5 32.76(13) . . ? C12 Ag2 O2 104.22(14) . . ? C6 Ag2 O2 114.62(14) . . ? C5 Ag2 O2 86.96(13) . . ? C12 Ag2 C11 32.44(14) . . ? C6 Ag2 C11 114.01(16) . . ? C5 Ag2 C11 137.60(15) . . ? O2 Ag2 C11 131.34(13) . . ? C12 Ag2 N1 97.24(14) . . ? C6 Ag2 N1 106.06(14) . . ? C5 Ag2 N1 84.77(13) . . ? O2 Ag2 N1 80.21(10) . . ? C11 Ag2 N1 85.14(13) . . ? O4 Ag3 C15 101.61(13) . . ? O4 Ag3 C21 123.55(13) . . ? C15 Ag3 C21 129.53(15) . . ? O4 Ag3 C20 100.23(12) . . ? C15 Ag3 C20 158.16(14) . . ? C21 Ag3 C20 31.83(13) . . ? O4 Ag3 C14 130.98(12) . . ? C15 Ag3 C14 31.88(13) . . ? C21 Ag3 C14 104.95(14) . . ? C20 Ag3 C14 127.17(14) . . ? O4 Ag3 N2 94.42(11) . . ? C15 Ag3 N2 97.12(13) . . ? C21 Ag3 N2 100.30(13) . . ? C20 Ag3 N2 81.21(12) . . ? C14 Ag3 N2 82.65(12) . . ? N4 C1 N3 117.7(3) . . ? N4 C1 N1 117.4(3) . . ? N3 C1 N1 124.9(4) . . ? C1 N4 C4 120.8(3) . . ? C1 N4 C7 120.5(3) . . ? C4 N4 C7 118.7(3) . . ? N4 C4 C5 114.5(3) . . ? N4 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? N4 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C6 C5 C4 125.0(4) . . ? C6 C5 Ag2 72.6(2) . . ? C4 C5 Ag2 103.2(3) . . ? C6 C5 H5A 117.5 . . ? C4 C5 H5A 117.5 . . ? Ag2 C5 H5A 94.4 . . ? C5 C6 Ag2 74.6(2) . . ? C5 C6 H6A 120.0 . . ? Ag2 C6 H6A 101.1 . . ? C5 C6 H6B 120.0 . . ? Ag2 C6 H6B 94.1 . . ? H6A C6 H6B 120.0 . . ? N4 C7 C8 114.9(3) . . ? N4 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N4 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C9 C8 C7 123.7(4) . . ? C9 C8 Ag1 71.8(2) . . ? C7 C8 Ag1 105.3(3) . . ? C9 C8 H8A 118.2 . . ? C7 C8 H8A 118.2 . . ? Ag1 C8 H8A 92.9 . . ? C8 C9 Ag1 75.8(2) . . ? C8 C9 H9A 120.0 . . ? Ag1 C9 H9A 102.7 . . ? C8 C9 H9B 120.0 . . ? Ag1 C9 H9B 91.5 . . ? H9A C9 H9B 120.0 . . ? C2 N1 C1 114.6(3) . . ? C2 N1 Ag2 112.3(2) . . ? C1 N1 Ag2 109.4(2) . . ? O5 S2 O6 115.4(2) . . ? O5 S2 O4 115.14(18) . . ? O6 S2 O4 113.80(18) . . ? O5 S2 C23 103.5(2) . . ? O6 S2 C23 103.5(2) . . ? O4 S2 C23 103.3(2) . . ? S2 O4 Ag3 135.61(17) . . ? F4 C23 F6 107.8(4) . . ? F4 C23 F5 107.5(4) . . ? F6 C23 F5 106.9(4) . . ? F4 C23 S2 111.1(3) . . ? F6 C23 S2 111.8(3) . . ? F5 C23 S2 111.4(3) . . ? O3 S1 O1 117.2(2) . . ? O3 S1 O2 115.8(2) . . ? O1 S1 O2 111.2(2) . . ? O3 S1 C22 104.3(3) . . ? O1 S1 C22 103.5(2) . . ? O2 S1 C22 102.7(2) . . ? S1 O2 Ag2 127.93(18) . . ? F3 C22 F2 107.3(4) . . ? F3 C22 F1 107.3(5) . . ? F2 C22 F1 107.6(5) . . ? F3 C22 S1 112.4(4) . . ? F2 C22 S1 111.0(4) . . ? F1 C22 S1 111.1(4) . . ? N1 C2 N2 125.6(3) . . ? N1 C2 N5 118.4(3) . . ? N2 C2 N5 116.0(4) . . ? C2 N5 C13 121.2(3) . . ? C2 N5 C10 121.0(3) . . ? C13 N5 C10 117.7(3) . . ? N5 C10 C11 113.3(3) . . ? N5 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? N5 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 125.8(4) . . ? C12 C11 Ag2 70.7(3) . . ? C10 C11 Ag2 102.3(3) . . ? C12 C11 H11A 117.1 . . ? C10 C11 H11A 117.1 . . ? Ag2 C11 H11A 97.5 . . ? C11 C12 Ag2 76.9(3) . . ? C11 C12 H12A 120.0 . . ? Ag2 C12 H12A 97.7 . . ? C11 C12 H12B 120.0 . . ? Ag2 C12 H12B 95.3 . . ? H12A C12 H12B 120.0 . . ? N5 C13 C14 113.9(3) . . ? N5 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? N5 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C13 126.0(4) . . ? C15 C14 Ag3 70.8(2) . . ? C13 C14 Ag3 103.5(2) . . ? C15 C14 H14A 117.0 . . ? C13 C14 H14A 117.0 . . ? Ag3 C14 H14A 96.0 . . ? C14 C15 Ag3 77.4(2) . . ? C14 C15 H15A 120.0 . . ? Ag3 C15 H15A 98.9 . . ? C14 C15 H15B 120.0 . . ? Ag3 C15 H15B 93.7 . . ? H15A C15 H15B 120.0 . . ? C3 N2 C2 114.1(3) . . ? C3 N2 Ag3 115.1(2) . . ? C2 N2 Ag3 112.3(2) . . ? N3 C3 N6 117.9(3) . . ? N3 C3 N2 125.3(3) . . ? N6 C3 N2 116.9(4) . . ? C3 N6 C19 120.6(3) . . ? C3 N6 C16 120.6(3) . . ? C19 N6 C16 118.5(3) . . ? N6 C16 C17 114.3(3) . . ? N6 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? N6 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C16 126.9(4) . . ? C18 C17 Ag1 71.8(3) . . ? C16 C17 Ag1 102.0(3) . . ? C18 C17 H17A 116.5 . . ? C16 C17 H17A 116.5 . . ? Ag1 C17 H17A 96.7 . . ? C17 C18 Ag1 76.6(3) . . ? C17 C18 H18A 120.0 . . ? Ag1 C18 H18A 98.0 . . ? C17 C18 H18B 120.0 . . ? Ag1 C18 H18B 95.4 . . ? H18A C18 H18B 120.0 . . ? N6 C19 C20 115.6(3) . . ? N6 C19 H19A 108.4 . . ? C20 C19 H19A 108.4 . . ? N6 C19 H19B 108.4 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? C21 C20 C19 123.2(4) . . ? C21 C20 Ag3 73.1(2) . . ? C19 C20 Ag3 107.2(2) . . ? C21 C20 H20A 118.4 . . ? C19 C20 H20A 118.4 . . ? Ag3 C20 H20A 89.7 . . ? C20 C21 Ag3 75.1(2) . . ? C20 C21 H21A 120.0 . . ? Ag3 C21 H21A 105.7 . . ? C20 C21 H21B 120.0 . . ? Ag3 C21 H21B 89.2 . . ? H21A C21 H21B 120.0 . . ? C3 N3 C1 114.7(3) . . ? C3 N3 Ag1 111.0(2) . . ? C1 N3 Ag1 110.5(2) . . ? S3' O7 S3 33.7(2) . . ? S3' O8 S3 33.1(2) . . ? O7 S3 O8 126.1(4) . . ? O7 S3 O9 107.5(4) . . ? O8 S3 O9 107.9(4) . . ? O7 S3 C24 104.1(3) . . ? O8 S3 C24 104.0(3) . . ? O9 S3 C24 105.5(4) . . ? O7 S3' O8 135.6(5) . . ? O7 S3' O9' 101.5(6) . . ? O8 S3' O9' 103.7(6) . . ? O7 S3' C24 102.2(4) . . ? O8 S3' C24 103.6(4) . . ? O9' S3' C24 108.6(5) . . ? F7' C24 F7 143.7(9) . . ? F7' C24 F9' 116.0(11) . . ? F7 C24 F9' 48.8(7) . . ? F7' C24 F9 42.2(7) . . ? F7 C24 F9 111.7(7) . . ? F9' C24 F9 121.9(6) . . ? F7' C24 F8 69.4(9) . . ? F7 C24 F8 104.6(7) . . ? F9' C24 F8 55.9(7) . . ? F9 C24 F8 103.4(7) . . ? F7' C24 F8' 104.9(9) . . ? F7 C24 F8' 57.1(6) . . ? F9' C24 F8' 99.7(9) . . ? F9 C24 F8' 62.7(5) . . ? F8 C24 F8' 142.2(6) . . ? F7' C24 S3 97.6(8) . . ? F7 C24 S3 117.9(5) . . ? F9' C24 S3 126.0(6) . . ? F9 C24 S3 111.5(5) . . ? F8 C24 S3 106.2(5) . . ? F8' C24 S3 111.6(5) . . ? F7' C24 S3' 122.0(8) . . ? F7 C24 S3' 93.5(5) . . ? F9' C24 S3' 110.0(6) . . ? F9 C24 S3' 126.9(5) . . ? F8 C24 S3' 114.7(4) . . ? F8' C24 S3' 100.1(5) . . ? S3 C24 S3' 24.45(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.748 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.104 _vrf_PLAT241_test ; PROBLEM: Check High Ueq as Compared to Neighbors for O7 RESPONSE: This is a consequence of imperfect modelling of partial occupancy disordered triflate anions. ; _database_code_depnum_ccdc_archive 'CCDC 940162'