# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_1 _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H72 Cu4 N4 S4, 2(C H2 Cl2)' _chemical_formula_sum 'C44 H76 Cl4 Cu4 N4 S4' _chemical_formula_weight 1185.28 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.315(2) _cell_length_b 24.927(7) _cell_length_c 11.256(2) _cell_angle_alpha 90 _cell_angle_beta 104.654(10) _cell_angle_gamma 90 _cell_volume 2800.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5711 _cell_measurement_theta_min 9.55 _cell_measurement_theta_max 33.17 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_F_000 1232 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.352 _exptl_crystal_size_mid 0.333 _exptl_crystal_size_min 0.198 _exptl_absorpt_coefficient_mu 1.871 _shelx_estimated_absorpt_T_min 0.559 _shelx_estimated_absorpt_T_max 0.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6156 _exptl_absorpt_correction_T_max 0.7476 _exptl_absorpt_process_details SAD-ABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 118869 _diffrn_reflns_av_unetI/netI 0.0306 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.899 _diffrn_reflns_theta_max 38.724 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 15872 _reflns_number_gt 11922 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _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-2012 (Sheldrick, 2012)' _computing_molecular_graphics ? _computing_publication_material cif2tables.py _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+0.6367P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 15872 _refine_ls_number_parameters 331 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.036 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.96845(2) 0.09074(2) 0.07511(2) 0.01691(3) Uani 1 1 d . . . . . Cu2 Cu 0.90123(2) -0.01781(2) 0.08173(2) 0.02044(3) Uani 1 1 d . . . . . S1 S 0.96380(2) 0.03564(2) 0.23654(2) 0.02032(4) Uani 1 1 d . . . . . S2 S 1.17942(2) 0.07520(2) 0.06094(2) 0.02179(5) Uani 1 1 d . . . . . N1 N 0.79728(10) 0.18772(4) 0.01653(8) 0.02440(17) Uani 1 1 d . . . . . N2 N 0.73615(8) 0.12527(3) -0.12094(8) 0.01880(14) Uani 1 1 d . . . . . C1 C 0.81485(11) 0.04689(4) 0.29846(9) 0.02355(18) Uani 1 1 d . . . . . C2 C 0.79439(14) -0.00278(6) 0.37115(12) 0.0348(3) Uani 1 1 d . . . . . H2A H 0.7192 0.0033 0.4081 0.052 Uiso 1 1 calc R U . . . H2B H 0.8760 -0.0097 0.4360 0.052 Uiso 1 1 calc R U . . . H2C H 0.7749 -0.0338 0.3159 0.052 Uiso 1 1 calc R U . . . C3 C 0.84870(15) 0.09488(6) 0.38539(13) 0.0373(3) Uani 1 1 d . . . . . H3A H 0.7726 0.1027 0.4199 0.056 Uiso 1 1 calc R U . . . H3B H 0.8676 0.1262 0.3400 0.056 Uiso 1 1 calc R U . . . H3C H 0.9276 0.0865 0.4520 0.056 Uiso 1 1 calc R U . . . C4 C 0.68941(11) 0.05823(6) 0.19667(11) 0.0312(2) Uani 1 1 d . . . . . H4A H 0.6132 0.0638 0.2326 0.047 Uiso 1 1 calc R U . . . H4B H 0.6709 0.0277 0.1401 0.047 Uiso 1 1 calc R U . . . H4C H 0.7033 0.0905 0.1518 0.047 Uiso 1 1 calc R U . . . C5A C 1.24601(12) 0.12967(5) -0.01876(11) 0.0318(2) Uani 0.729(3) 1 d . U P A 1 C6A C 1.2906(3) 0.17252(9) 0.0718(2) 0.0516(7) Uani 0.729(3) 1 d . U P A 1 H6A1 H 1.3288 0.2020 0.0340 0.077 Uiso 0.729(3) 1 calc R U P A 1 H6A2 H 1.3588 0.1584 0.1420 0.077 Uiso 0.729(3) 1 calc R U P A 1 H6A3 H 1.2140 0.1858 0.1000 0.077 Uiso 0.729(3) 1 calc R U P A 1 C7A C 1.1472(2) 0.14605(11) -0.1333(2) 0.0311(4) Uani 0.729(3) 1 d . U P A 1 H7A1 H 1.0649 0.1585 -0.1136 0.047 Uiso 0.729(3) 1 calc R U P A 1 H7A2 H 1.1265 0.1153 -0.1893 0.047 Uiso 0.729(3) 1 calc R U P A 1 H7A3 H 1.1848 0.1751 -0.1728 0.047 Uiso 0.729(3) 1 calc R U P A 1 C8A C 1.37191(17) 0.10361(9) -0.0520(2) 0.0397(5) Uani 0.729(3) 1 d . U P A 1 H8A1 H 1.4181 0.1308 -0.0889 0.060 Uiso 0.729(3) 1 calc R U P A 1 H8A2 H 1.3426 0.0742 -0.1104 0.060 Uiso 0.729(3) 1 calc R U P A 1 H8A3 H 1.4332 0.0896 0.0228 0.060 Uiso 0.729(3) 1 calc R U P A 1 C5B C 1.24601(12) 0.12967(5) -0.01876(11) 0.0318(2) Uani 0.271(3) 1 d . U P A 2 C6B C 1.1924(7) 0.1895(2) 0.0338(8) 0.056(2) Uani 0.271(3) 1 d . U P A 2 H6B1 H 1.2231 0.1909 0.1236 0.084 Uiso 0.271(3) 1 calc R U P A 2 H6B2 H 1.0943 0.1912 0.0090 0.084 Uiso 0.271(3) 1 calc R U P A 2 H6B3 H 1.2296 0.2199 -0.0016 0.084 Uiso 0.271(3) 1 calc R U P A 2 C7B C 1.1874(11) 0.1356(4) -0.1574(7) 0.064(3) Uani 0.271(3) 1 d . U P A 2 H7B1 H 1.2193 0.1691 -0.1855 0.097 Uiso 0.271(3) 1 calc R U P A 2 H7B2 H 1.0893 0.1362 -0.1754 0.097 Uiso 0.271(3) 1 calc R U P A 2 H7B3 H 1.2159 0.1052 -0.1999 0.097 Uiso 0.271(3) 1 calc R U P A 2 C8B C 1.3909(5) 0.1371(2) 0.0180(6) 0.0426(14) Uani 0.271(3) 1 d . U P A 2 H8B1 H 1.4348 0.1061 -0.0089 0.064 Uiso 0.271(3) 1 calc R U P A 2 H8B2 H 1.4206 0.1403 0.1075 0.064 Uiso 0.271(3) 1 calc R U P A 2 H8B3 H 1.4147 0.1698 -0.0201 0.064 Uiso 0.271(3) 1 calc R U P A 2 C9 C 0.82963(9) 0.13767(4) -0.01530(9) 0.01838(16) Uani 1 1 d . . . . . C10 C 0.68237(12) 0.20659(5) -0.06653(10) 0.0286(2) Uani 1 1 d . . . . . C11 C 0.60819(18) 0.25381(6) -0.07157(13) 0.0490(4) Uani 1 1 d . . . . . H11A H 0.6331 0.2809 -0.0106 0.059 Uiso 1 1 calc R U . . . C12 C 0.4967(2) 0.25934(7) -0.16949(16) 0.0594(5) Uani 1 1 d . . . . . H12A H 0.4438 0.2909 -0.1754 0.071 Uiso 1 1 calc R U . . . C13 C 0.45988(16) 0.22001(7) -0.25949(15) 0.0504(4) Uani 1 1 d . . . . . H13A H 0.3828 0.2255 -0.3253 0.061 Uiso 1 1 calc R U . . . C14 C 0.53289(12) 0.17304(5) -0.25548(12) 0.0342(3) Uani 1 1 d . . . . . H14A H 0.5085 0.1464 -0.3175 0.041 Uiso 1 1 calc R U . . . C15 C 0.64409(10) 0.16689(4) -0.15561(10) 0.02391(19) Uani 1 1 d . . . . . C16 C 0.88244(18) 0.21696(5) 0.12180(11) 0.0420(3) Uani 1 1 d . . . . . H16A H 0.9554 0.1919 0.1637 0.050 Uiso 1 1 calc R U . . . C17 C 0.9498(3) 0.26503(7) 0.07832(17) 0.0772(8) Uani 1 1 d . . . . . H17A H 0.9934 0.2535 0.0148 0.116 Uiso 1 1 calc R U . . . H17B H 1.0170 0.2802 0.1478 0.116 Uiso 1 1 calc R U . . . H17C H 0.8822 0.2923 0.0444 0.116 Uiso 1 1 calc R U . . . C18 C 0.8045(3) 0.23190(9) 0.21524(14) 0.0827(9) Uani 1 1 d . . . . . H18A H 0.7517 0.2010 0.2295 0.124 Uiso 1 1 calc R U . . . H18B H 0.7443 0.2620 0.1837 0.124 Uiso 1 1 calc R U . . . H18C H 0.8672 0.2424 0.2926 0.124 Uiso 1 1 calc R U . . . C19 C 0.73830(10) 0.07431(4) -0.18661(10) 0.02283(18) Uani 1 1 d . . . . . H19A H 0.8137 0.0525 -0.1360 0.027 Uiso 1 1 calc R U . . . C20 C 0.76941(13) 0.08383(5) -0.30980(11) 0.0306(2) Uani 1 1 d . . . . . H20A H 0.8515 0.1052 -0.2978 0.046 Uiso 1 1 calc R U . . . H20B H 0.6949 0.1032 -0.3642 0.046 Uiso 1 1 calc R U . . . H20C H 0.7819 0.0493 -0.3470 0.046 Uiso 1 1 calc R U . . . C21 C 0.61026(12) 0.04212(5) -0.19656(13) 0.0336(3) Uani 1 1 d . . . . . H21A H 0.5943 0.0381 -0.1148 0.050 Uiso 1 1 calc R U . . . H21B H 0.6198 0.0066 -0.2307 0.050 Uiso 1 1 calc R U . . . H21C H 0.5345 0.0610 -0.2505 0.050 Uiso 1 1 calc R U . . . C1S C 0.26187(14) 0.10048(6) 0.39125(12) 0.0393(3) Uani 0.523(16) 1 d . . P B 3 H1S1 H 0.2109 0.0743 0.4276 0.047 Uiso 0.523(16) 1 calc R U P B 3 H1S2 H 0.2377 0.0943 0.3014 0.047 Uiso 0.523(16) 1 calc R U P B 3 Cl1S Cl 0.4309(4) 0.08665(19) 0.4470(4) 0.0560(7) Uani 0.523(16) 1 d . . P B 3 Cl2S Cl 0.2074(4) 0.16597(12) 0.4186(4) 0.0582(6) Uani 0.523(16) 1 d . . P B 3 C2S C 0.26187(14) 0.10048(6) 0.39125(12) 0.0393(3) Uani 0.477(16) 1 d . . P B 4 H2S1 H 0.2257 0.1033 0.3012 0.047 Uiso 0.477(16) 1 calc R U P B 4 H2S2 H 0.2219 0.0685 0.4203 0.047 Uiso 0.477(16) 1 calc R U P B 4 Cl3S Cl 0.2216(3) 0.1573(3) 0.4617(10) 0.0828(14) Uani 0.477(16) 1 d . . P B 4 Cl4S Cl 0.4402(4) 0.0938(2) 0.4276(5) 0.0474(7) Uani 0.477(16) 1 d . . P B 4 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 Cu1 0.01655(5) 0.01744(5) 0.01612(5) -0.00136(4) 0.00298(4) 0.00012(4) Cu2 0.01791(5) 0.02281(6) 0.02011(6) -0.00003(4) 0.00391(4) 0.00101(4) S1 0.01819(9) 0.02365(11) 0.01759(10) 0.00250(8) 0.00168(8) -0.00057(8) S2 0.01752(10) 0.02912(12) 0.01854(10) -0.00162(9) 0.00420(8) 0.00235(8) N1 0.0364(5) 0.0218(4) 0.0174(4) 0.0012(3) 0.0113(3) 0.0089(3) N2 0.0161(3) 0.0192(3) 0.0211(4) 0.0028(3) 0.0047(3) 0.0028(3) C1 0.0254(4) 0.0289(5) 0.0178(4) 0.0019(3) 0.0081(3) -0.0022(4) C2 0.0380(6) 0.0388(6) 0.0293(6) 0.0096(5) 0.0113(5) -0.0073(5) C3 0.0458(7) 0.0387(7) 0.0316(6) -0.0091(5) 0.0173(6) -0.0056(5) C4 0.0221(5) 0.0473(7) 0.0259(5) 0.0066(5) 0.0093(4) 0.0044(4) C5A 0.0244(5) 0.0443(7) 0.0269(5) -0.0023(5) 0.0066(4) -0.0135(5) C6A 0.0704(17) 0.0402(11) 0.0478(12) -0.0185(9) 0.0219(11) -0.0288(11) C7A 0.0310(9) 0.0313(9) 0.0334(10) 0.0101(8) 0.0125(7) -0.0015(7) C8A 0.0217(7) 0.0545(12) 0.0457(11) 0.0018(9) 0.0137(7) -0.0058(7) C5B 0.0244(5) 0.0443(7) 0.0269(5) -0.0023(5) 0.0066(4) -0.0135(5) C6B 0.047(3) 0.022(2) 0.114(6) -0.010(3) 0.046(4) -0.012(2) C7B 0.093(7) 0.054(5) 0.033(3) 0.016(3) -0.007(3) -0.042(5) C8B 0.0245(19) 0.055(3) 0.053(3) 0.012(3) 0.0180(19) -0.0012(19) C9 0.0202(4) 0.0201(4) 0.0170(4) 0.0012(3) 0.0088(3) 0.0021(3) C10 0.0388(6) 0.0281(5) 0.0226(5) 0.0067(4) 0.0146(4) 0.0163(4) C11 0.0739(11) 0.0427(8) 0.0327(6) 0.0051(5) 0.0178(7) 0.0381(7) C12 0.0728(11) 0.0573(10) 0.0483(9) 0.0112(7) 0.0155(8) 0.0489(9) C13 0.0434(8) 0.0559(9) 0.0487(9) 0.0149(7) 0.0056(7) 0.0306(7) C14 0.0264(5) 0.0369(6) 0.0365(6) 0.0112(5) 0.0028(5) 0.0102(4) C15 0.0220(4) 0.0250(5) 0.0264(5) 0.0074(4) 0.0093(4) 0.0075(4) C16 0.0776(10) 0.0274(6) 0.0161(5) -0.0048(4) 0.0031(5) 0.0146(6) C17 0.134(2) 0.0303(7) 0.0433(9) -0.0040(6) -0.0214(11) -0.0243(10) C18 0.142(2) 0.0844(14) 0.0212(6) -0.0026(7) 0.0188(9) 0.0755(14) C19 0.0202(4) 0.0199(4) 0.0250(5) -0.0007(3) -0.0005(3) 0.0020(3) C20 0.0300(5) 0.0348(6) 0.0250(5) -0.0042(4) 0.0032(4) 0.0064(4) C21 0.0264(5) 0.0271(5) 0.0409(7) 0.0041(5) -0.0032(5) -0.0050(4) C1S 0.0373(7) 0.0489(8) 0.0274(6) -0.0008(5) 0.0002(5) -0.0163(6) Cl1S 0.0404(8) 0.0818(13) 0.0414(10) -0.0070(8) 0.0022(6) -0.0165(7) Cl2S 0.0429(8) 0.0643(8) 0.0678(12) -0.0162(9) 0.0148(7) -0.0084(6) C2S 0.0373(7) 0.0489(8) 0.0274(6) -0.0008(5) 0.0002(5) -0.0163(6) Cl3S 0.0480(7) 0.0850(19) 0.109(3) -0.050(2) 0.0079(14) -0.0018(9) Cl4S 0.0314(6) 0.0617(11) 0.0456(13) -0.0154(9) 0.0032(6) -0.0038(7) _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 Cu1 C9 1.9280(10) . ? Cu1 S2 2.2554(6) . ? Cu1 S1 2.2878(5) . ? Cu1 Cu2 2.7990(8) . ? Cu2 S2 2.1543(5) 3_755 ? Cu2 S1 2.1586(5) . ? S1 C1 1.8619(11) . ? S2 C5A 1.8526(13) . ? S2 Cu2 2.1544(5) 3_755 ? N1 C9 1.3627(13) . ? N1 C10 1.3927(15) . ? N1 C16 1.4765(16) . ? N2 C9 1.3634(13) . ? N2 C15 1.3939(13) . ? N2 C19 1.4728(14) . ? C1 C4 1.5221(16) . ? C1 C2 1.5278(16) . ? C1 C3 1.5289(17) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5A C6A 1.468(2) . ? C5A C7A 1.485(3) . ? C5A C8A 1.579(2) . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C10 C15 1.3928(17) . ? C10 C11 1.3972(16) . ? C11 C12 1.384(2) . ? C11 H11A 0.9500 . ? C12 C13 1.392(3) . ? C12 H12A 0.9500 . ? C13 C14 1.3868(19) . ? C13 H13A 0.9500 . ? C14 C15 1.3966(16) . ? C14 H14A 0.9500 . ? C16 C18 1.523(2) . ? C16 C17 1.526(3) . ? C16 H16A 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.5189(17) . ? C19 C21 1.5250(16) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C1S Cl1S 1.731(4) . ? C1S Cl2S 1.779(4) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Cu1 S2 131.91(3) . . ? C9 Cu1 S1 128.42(3) . . ? S2 Cu1 S1 99.643(14) . . ? C9 Cu1 Cu2 116.40(3) . . ? S2 Cu1 Cu2 94.924(12) . . ? S1 Cu1 Cu2 48.961(11) . . ? S2 Cu2 S1 172.678(11) 3_755 . ? S2 Cu2 Cu1 132.344(14) 3_755 . ? S1 Cu2 Cu1 53.073(13) . . ? C1 S1 Cu2 106.77(4) . . ? C1 S1 Cu1 113.08(4) . . ? Cu2 S1 Cu1 77.97(2) . . ? C5A S2 Cu2 104.26(4) . 3_755 ? C5A S2 Cu1 113.01(4) . . ? Cu2 S2 Cu1 88.234(15) 3_755 . ? C9 N1 C10 110.87(9) . . ? C9 N1 C16 121.83(9) . . ? C10 N1 C16 127.19(10) . . ? C9 N2 C15 110.92(9) . . ? C9 N2 C19 122.41(8) . . ? C15 N2 C19 126.67(9) . . ? C4 C1 C2 110.33(10) . . ? C4 C1 C3 110.45(11) . . ? C2 C1 C3 109.36(10) . . ? C4 C1 S1 111.79(7) . . ? C2 C1 S1 108.50(8) . . ? C3 C1 S1 106.31(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6A C5A C7A 115.40(18) . . ? C6A C5A C8A 109.37(15) . . ? C7A C5A C8A 109.44(13) . . ? C6A C5A S2 106.64(11) . . ? C7A C5A S2 111.40(12) . . ? C8A C5A S2 103.94(11) . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5A C7A H7A1 109.5 . . ? C5A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C5A C8A H8A1 109.5 . . ? C5A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C5A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? N1 C9 N2 105.69(8) . . ? N1 C9 Cu1 127.98(8) . . ? N2 C9 Cu1 126.15(7) . . ? N1 C10 C15 106.35(9) . . ? N1 C10 C11 132.54(12) . . ? C15 C10 C11 121.11(12) . . ? C12 C11 C10 116.90(14) . . ? C12 C11 H11A 121.5 . . ? C10 C11 H11A 121.5 . . ? C11 C12 C13 121.90(13) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C14 C13 C12 121.67(14) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C15 116.58(13) . . ? C13 C14 H14A 121.7 . . ? C15 C14 H14A 121.7 . . ? C10 C15 N2 106.15(9) . . ? C10 C15 C14 121.81(10) . . ? N2 C15 C14 132.04(11) . . ? N1 C16 C18 111.35(16) . . ? N1 C16 C17 110.90(11) . . ? C18 C16 C17 113.08(16) . . ? N1 C16 H16A 107.1 . . ? C18 C16 H16A 107.1 . . ? C17 C16 H16A 107.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C20 110.90(9) . . ? N2 C19 C21 111.59(9) . . ? C20 C19 C21 113.22(10) . . ? N2 C19 H19A 106.9 . . ? C20 C19 H19A 106.9 . . ? C21 C19 H19A 106.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Cl1S C1S Cl2S 116.9(2) . . ? Cl1S C1S H1S1 108.1 . . ? Cl2S C1S H1S1 108.1 . . ? Cl1S C1S H1S2 108.1 . . ? Cl2S C1S H1S2 108.1 . . ? H1S1 C1S H1S2 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu2 S1 C1 C4 -45.46(9) . . . . ? Cu1 S1 C1 C4 38.32(9) . . . . ? Cu2 S1 C1 C2 76.43(8) . . . . ? Cu1 S1 C1 C2 160.21(7) . . . . ? Cu2 S1 C1 C3 -166.05(7) . . . . ? Cu1 S1 C1 C3 -82.27(8) . . . . ? Cu2 S2 C5A C6A 174.58(14) 3_755 . . . ? Cu1 S2 C5A C6A 80.37(14) . . . . ? Cu2 S2 C5A C7A 47.85(13) 3_755 . . . ? Cu1 S2 C5A C7A -46.36(13) . . . . ? Cu2 S2 C5A C8A -69.90(10) 3_755 . . . ? Cu1 S2 C5A C8A -164.11(9) . . . . ? C10 N1 C9 N2 1.36(11) . . . . ? C16 N1 C9 N2 -175.07(10) . . . . ? C10 N1 C9 Cu1 -173.91(8) . . . . ? C16 N1 C9 Cu1 9.65(15) . . . . ? C15 N2 C9 N1 -0.57(11) . . . . ? C19 N2 C9 N1 178.68(9) . . . . ? C15 N2 C9 Cu1 174.82(7) . . . . ? C19 N2 C9 Cu1 -5.93(13) . . . . ? C9 N1 C10 C15 -1.63(12) . . . . ? C16 N1 C10 C15 174.57(12) . . . . ? C9 N1 C10 C11 177.59(14) . . . . ? C16 N1 C10 C11 -6.2(2) . . . . ? N1 C10 C11 C12 -179.87(15) . . . . ? C15 C10 C11 C12 -0.7(2) . . . . ? C10 C11 C12 C13 -0.3(3) . . . . ? C11 C12 C13 C14 0.2(3) . . . . ? C12 C13 C14 C15 0.9(2) . . . . ? N1 C10 C15 N2 1.20(12) . . . . ? C11 C10 C15 N2 -178.12(12) . . . . ? N1 C10 C15 C14 -178.73(11) . . . . ? C11 C10 C15 C14 1.95(19) . . . . ? C9 N2 C15 C10 -0.41(12) . . . . ? C19 N2 C15 C10 -179.62(10) . . . . ? C9 N2 C15 C14 179.51(12) . . . . ? C19 N2 C15 C14 0.30(19) . . . . ? C13 C14 C15 C10 -1.96(19) . . . . ? C13 C14 C15 N2 178.13(13) . . . . ? C9 N1 C16 C18 -122.12(13) . . . . ? C10 N1 C16 C18 62.07(17) . . . . ? C9 N1 C16 C17 111.03(15) . . . . ? C10 N1 C16 C17 -64.8(2) . . . . ? C9 N2 C19 C20 -112.62(10) . . . . ? C15 N2 C19 C20 66.51(13) . . . . ? C9 N2 C19 C21 120.15(10) . . . . ? C15 N2 C19 C21 -60.72(13) . . . . ? _refine_diff_density_max 0.851 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.069 _shelxl_version_number 2012-9 _database_code_depnum_ccdc_archive 'CCDC 960478' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H76 Cu4 N4 S4, 2(C H2 Cl2)' _chemical_formula_sum 'C40 H80 Cl4 Cu4 N4 S4' _chemical_formula_weight 1141.28 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' 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' Cu Cu 0.3201 1.2651 '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 10.363(2) _cell_length_b 23.568(6) _cell_length_c 11.579(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.670(4) _cell_angle_gamma 90.00 _cell_volume 2709.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2759 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 32.45 _exptl_crystal_description 'tetragonal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5941 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details SAD-ABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 126773 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 33.20 _reflns_number_total 10352 _reflns_number_gt 8564 _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 ? _computing_publication_material cif2tables.py _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^)+(0.0353P)^2^+1.1636P] 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 10352 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Cu1 Cu 1.098521(16) 0.022221(7) -0.076183(15) 0.01824(4) Uani 1 1 d . . . Cu2 Cu 0.961066(15) 0.094104(7) 0.072516(14) 0.01614(4) Uani 1 1 d . . . S1 S 1.17682(3) 0.080537(14) 0.07045(3) 0.01702(6) Uani 1 1 d . . . S2 S 0.96297(3) 0.034059(14) 0.22929(3) 0.01729(6) Uani 1 1 d . . . N1 N 0.71932(10) 0.12963(4) -0.12197(10) 0.01522(19) Uani 1 1 d . . . N2 N 0.78512(11) 0.19594(5) 0.00879(10) 0.0175(2) Uani 1 1 d . . . C1 C 1.24746(13) 0.14130(6) 0.00672(13) 0.0220(3) Uani 1 1 d . . . C2 C 1.37644(16) 0.12117(9) -0.01811(18) 0.0417(4) Uani 1 1 d . . . H2A H 1.4203 0.1533 -0.0452 0.063 Uiso 1 1 calc R . . H2B H 1.3548 0.0919 -0.0809 0.063 Uiso 1 1 calc R . . H2C H 1.4372 0.1053 0.0558 0.063 Uiso 1 1 calc R . . C3 C 1.2789(2) 0.18744(8) 0.10349(16) 0.0401(4) Uani 1 1 d . . . H3A H 1.3143 0.2210 0.0730 0.060 Uiso 1 1 calc R . . H3B H 1.3462 0.1733 0.1756 0.060 Uiso 1 1 calc R . . H3C H 1.1964 0.1976 0.1239 0.060 Uiso 1 1 calc R . . C4 C 1.14884(16) 0.16333(7) -0.10785(14) 0.0274(3) Uani 1 1 d . . . H4A H 1.1874 0.1966 -0.1366 0.041 Uiso 1 1 calc R . . H4B H 1.0645 0.1741 -0.0914 0.041 Uiso 1 1 calc R . . H4C H 1.1309 0.1336 -0.1696 0.041 Uiso 1 1 calc R . . C5 C 0.81448(13) 0.04199(6) 0.28744(13) 0.0207(2) Uani 1 1 d . . . C6 C 0.68738(14) 0.05573(7) 0.18734(14) 0.0282(3) Uani 1 1 d . . . H6A H 0.6120 0.0607 0.2217 0.042 Uiso 1 1 calc R . . H6B H 0.6673 0.0246 0.1289 0.042 Uiso 1 1 calc R . . H6C H 0.7008 0.0908 0.1469 0.042 Uiso 1 1 calc R . . C7 C 0.84734(18) 0.09024(8) 0.37948(16) 0.0348(4) Uani 1 1 d . . . H7A H 0.7727 0.0951 0.4148 0.052 Uiso 1 1 calc R . . H7B H 0.8607 0.1255 0.3394 0.052 Uiso 1 1 calc R . . H7C H 0.9298 0.0811 0.4433 0.052 Uiso 1 1 calc R . . C8 C 0.79630(17) -0.01328(8) 0.35039(16) 0.0336(4) Uani 1 1 d . . . H8A H 0.7223 -0.0089 0.3866 0.050 Uiso 1 1 calc R . . H8B H 0.8796 -0.0221 0.4135 0.050 Uiso 1 1 calc R . . H8C H 0.7754 -0.0442 0.2913 0.050 Uiso 1 1 calc R . . C9 C 0.81722(12) 0.14288(5) -0.01952(11) 0.0156(2) Uani 1 1 d . . . C10 C 0.62599(12) 0.17354(5) -0.15734(12) 0.0175(2) Uani 1 1 d . . . C11 C 0.66716(13) 0.21542(6) -0.07470(12) 0.0186(2) Uani 1 1 d . . . C12 C 0.72307(13) 0.07531(5) -0.18440(12) 0.0183(2) Uani 1 1 d . . . H12A H 0.7964 0.0523 -0.1294 0.022 Uiso 1 1 calc R . . C13 C 0.59377(14) 0.04132(6) -0.20305(15) 0.0261(3) Uani 1 1 d . . . H13A H 0.5678 0.0409 -0.1281 0.039 Uiso 1 1 calc R . . H13B H 0.6084 0.0023 -0.2258 0.039 Uiso 1 1 calc R . . H13C H 0.5218 0.0588 -0.2672 0.039 Uiso 1 1 calc R . . C14 C 0.76349(15) 0.08403(6) -0.29956(14) 0.0254(3) Uani 1 1 d . . . H14A H 0.8465 0.1065 -0.2817 0.038 Uiso 1 1 calc R . . H14B H 0.6914 0.1041 -0.3589 0.038 Uiso 1 1 calc R . . H14C H 0.7786 0.0471 -0.3322 0.038 Uiso 1 1 calc R . . C15 C 0.50534(14) 0.17251(6) -0.26573(13) 0.0235(3) Uani 1 1 d . . . H15A H 0.4667 0.2107 -0.2806 0.035 Uiso 1 1 calc R . . H15B H 0.4380 0.1463 -0.2515 0.035 Uiso 1 1 calc R . . H15C H 0.5323 0.1598 -0.3361 0.035 Uiso 1 1 calc R . . C16 C 0.60145(16) 0.27135(7) -0.06961(14) 0.0287(3) Uani 1 1 d . . . H16A H 0.5296 0.2774 -0.1448 0.043 Uiso 1 1 calc R . . H16B H 0.6685 0.3017 -0.0593 0.043 Uiso 1 1 calc R . . H16C H 0.5631 0.2717 -0.0015 0.043 Uiso 1 1 calc R . . C17 C 0.87366(14) 0.22587(6) 0.11361(12) 0.0221(3) Uani 1 1 d . . . H17A H 0.9449 0.1982 0.1556 0.027 Uiso 1 1 calc R . . C18 C 0.80007(18) 0.24309(7) 0.20392(14) 0.0322(3) Uani 1 1 d . . . H18A H 0.7469 0.2110 0.2187 0.048 Uiso 1 1 calc R . . H18B H 0.7401 0.2751 0.1717 0.048 Uiso 1 1 calc R . . H18C H 0.8657 0.2544 0.2797 0.048 Uiso 1 1 calc R . . C19 C 0.94578(16) 0.27538(7) 0.07496(14) 0.0287(3) Uani 1 1 d . . . H19A H 0.9859 0.2627 0.0123 0.043 Uiso 1 1 calc R . . H19B H 1.0168 0.2894 0.1446 0.043 Uiso 1 1 calc R . . H19C H 0.8811 0.3059 0.0431 0.043 Uiso 1 1 calc R . . C1S C 1.73707(17) -0.10038(7) 0.60712(15) 0.0317(3) Uani 0.47(2) 1 d P A 1 H1S1 H 1.7821 -0.0913 0.6927 0.038 Uiso 0.47(2) 1 calc PR A 1 H1S2 H 1.7719 -0.0742 0.5562 0.038 Uiso 0.47(2) 1 calc PR A 1 Cl1S Cl 1.5583(6) -0.0915(3) 0.5759(7) 0.0367(7) Uani 0.47(2) 1 d P A 1 Cl2S Cl 1.7735(6) -0.1740(2) 0.5755(6) 0.0480(7) Uani 0.47(2) 1 d P A 1 C2S C 1.73707(17) -0.10038(7) 0.60712(15) 0.0317(3) Uani 0.53(2) 1 d P A 2 H2S1 H 1.7913 -0.0703 0.5837 0.038 Uiso 0.53(2) 1 calc PR A 2 H2S2 H 1.7641 -0.1023 0.6963 0.038 Uiso 0.53(2) 1 calc PR A 2 Cl3S Cl 1.5681(6) -0.0822(3) 0.5556(5) 0.0412(7) Uani 0.53(2) 1 d P A 2 Cl4S Cl 1.7715(5) -0.1631(4) 0.5522(9) 0.0641(13) Uani 0.53(2) 1 d P 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 Cu1 0.01736(7) 0.01736(8) 0.01902(8) 0.00075(6) 0.00366(6) -0.00024(5) Cu2 0.01426(7) 0.01687(7) 0.01562(8) 0.00067(5) 0.00161(5) -0.00083(5) S1 0.01590(13) 0.01852(14) 0.01655(14) 0.00217(11) 0.00454(11) 0.00040(10) S2 0.01479(12) 0.01902(14) 0.01681(14) 0.00245(11) 0.00254(10) -0.00044(10) N1 0.0151(4) 0.0150(4) 0.0152(5) 0.0007(4) 0.0038(4) 0.0002(3) N2 0.0197(5) 0.0182(5) 0.0147(5) -0.0008(4) 0.0052(4) -0.0001(4) C1 0.0194(5) 0.0245(6) 0.0208(6) 0.0035(5) 0.0038(5) -0.0061(5) C2 0.0206(7) 0.0611(12) 0.0473(11) 0.0154(9) 0.0160(7) -0.0013(7) C3 0.0547(11) 0.0306(8) 0.0291(8) -0.0024(7) 0.0025(8) -0.0212(8) C4 0.0302(7) 0.0260(7) 0.0233(7) 0.0073(6) 0.0032(6) -0.0046(5) C5 0.0188(5) 0.0241(6) 0.0200(6) 0.0032(5) 0.0069(5) 0.0000(5) C6 0.0177(6) 0.0387(8) 0.0290(7) 0.0087(6) 0.0079(5) 0.0017(5) C7 0.0359(8) 0.0388(9) 0.0326(9) -0.0091(7) 0.0146(7) -0.0004(7) C8 0.0296(7) 0.0390(9) 0.0340(8) 0.0169(7) 0.0122(6) -0.0021(6) C9 0.0158(5) 0.0171(5) 0.0142(5) 0.0013(4) 0.0047(4) -0.0016(4) C10 0.0175(5) 0.0184(5) 0.0170(6) 0.0027(4) 0.0055(4) 0.0024(4) C11 0.0216(6) 0.0192(6) 0.0162(6) 0.0016(5) 0.0073(5) 0.0030(4) C12 0.0178(5) 0.0153(5) 0.0198(6) -0.0017(4) 0.0022(4) 0.0009(4) C13 0.0209(6) 0.0197(6) 0.0343(8) -0.0021(6) 0.0026(5) -0.0028(5) C14 0.0269(6) 0.0270(7) 0.0228(7) -0.0033(5) 0.0079(5) 0.0045(5) C15 0.0209(6) 0.0258(7) 0.0203(6) 0.0019(5) 0.0004(5) 0.0059(5) C16 0.0344(8) 0.0232(7) 0.0282(8) -0.0013(6) 0.0083(6) 0.0103(6) C17 0.0273(6) 0.0215(6) 0.0166(6) -0.0034(5) 0.0049(5) -0.0013(5) C18 0.0426(9) 0.0351(8) 0.0209(7) -0.0044(6) 0.0123(6) 0.0016(7) C19 0.0322(7) 0.0259(7) 0.0269(7) -0.0033(6) 0.0067(6) -0.0080(6) C1S 0.0323(8) 0.0387(9) 0.0213(7) -0.0020(6) 0.0029(6) -0.0119(6) Cl1S 0.0297(8) 0.0385(13) 0.0377(18) -0.0118(10) 0.0028(9) -0.0042(7) Cl2S 0.0489(13) 0.0402(12) 0.0572(15) -0.0080(9) 0.0188(14) 0.0067(8) C2S 0.0323(8) 0.0387(9) 0.0213(7) -0.0020(6) 0.0029(6) -0.0119(6) Cl3S 0.0366(9) 0.0489(17) 0.0345(12) -0.0110(10) 0.0043(7) -0.0021(10) Cl4S 0.0442(10) 0.059(2) 0.074(2) -0.0265(18) -0.0057(12) 0.0145(13) _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 Cu1 S1 2.1539(5) . ? Cu1 S2 2.1587(5) 3_755 ? Cu1 Cu2 2.8131(7) 3_755 ? Cu1 Cu2 3.0447(5) . ? Cu2 C9 1.9410(13) . ? Cu2 S1 2.2655(6) . ? Cu2 S2 2.2973(6) . ? Cu2 Cu1 2.8133(7) 3_755 ? S1 C1 1.8551(14) . ? S2 C5 1.8575(14) . ? S2 Cu1 2.1588(5) 3_755 ? N1 C9 1.3577(16) . ? N1 C10 1.3953(16) . ? N1 C12 1.4762(17) . ? N2 C9 1.3581(17) . ? N2 C11 1.4007(17) . ? N2 C17 1.4743(17) . ? C1 C4 1.515(2) . ? C1 C2 1.521(2) . ? C1 C3 1.528(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.519(2) . ? C5 C7 1.529(2) . ? C5 C8 1.531(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C11 1.3557(19) . ? C10 C15 1.4961(18) . ? C11 C16 1.4925(19) . ? C12 C14 1.522(2) . ? C12 C13 1.5224(19) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.516(2) . ? C17 C19 1.521(2) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C1S Cl1S 1.795(6) . ? C1S Cl2S 1.834(6) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu1 S2 174.313(14) . 3_755 ? S1 Cu1 Cu2 130.136(16) . 3_755 ? S2 Cu1 Cu2 53.078(15) 3_755 3_755 ? S1 Cu1 Cu2 47.996(16) . . ? S2 Cu1 Cu2 136.928(16) 3_755 . ? Cu2 Cu1 Cu2 113.164(13) 3_755 . ? C9 Cu2 S1 133.05(4) . . ? C9 Cu2 S2 129.03(4) . . ? S1 Cu2 S2 97.853(13) . . ? C9 Cu2 Cu1 116.62(4) . 3_755 ? S1 Cu2 Cu1 94.828(12) . 3_755 ? S2 Cu2 Cu1 48.696(13) . 3_755 ? C9 Cu2 Cu1 115.42(4) . . ? S1 Cu2 Cu1 44.950(10) . . ? S2 Cu2 Cu1 101.81(2) . . ? Cu1 Cu2 Cu1 66.834(13) 3_755 . ? C1 S1 Cu1 106.35(5) . . ? C1 S1 Cu2 113.48(5) . . ? Cu1 S1 Cu2 87.054(15) . . ? C5 S2 Cu1 106.23(5) . 3_755 ? C5 S2 Cu2 113.84(5) . . ? Cu1 S2 Cu2 78.23(2) 3_755 . ? C9 N1 C10 111.55(11) . . ? C9 N1 C12 120.61(10) . . ? C10 N1 C12 127.79(11) . . ? C9 N2 C11 111.16(11) . . ? C9 N2 C17 120.11(11) . . ? C11 N2 C17 128.69(11) . . ? C4 C1 C2 110.48(13) . . ? C4 C1 C3 110.28(13) . . ? C2 C1 C3 110.27(14) . . ? C4 C1 S1 111.63(9) . . ? C2 C1 S1 107.62(11) . . ? C3 C1 S1 106.45(10) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 110.15(13) . . ? C6 C5 C8 110.28(12) . . ? C7 C5 C8 109.53(14) . . ? C6 C5 S2 111.84(10) . . ? C7 C5 S2 106.59(10) . . ? C8 C5 S2 108.35(10) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 N2 104.43(10) . . ? N1 C9 Cu2 127.39(9) . . ? N2 C9 Cu2 127.98(9) . . ? C11 C10 N1 106.35(11) . . ? C11 C10 C15 128.46(12) . . ? N1 C10 C15 125.19(12) . . ? C10 C11 N2 106.50(11) . . ? C10 C11 C16 128.03(12) . . ? N2 C11 C16 125.46(12) . . ? N1 C12 C14 111.38(11) . . ? N1 C12 C13 112.34(11) . . ? C14 C12 C13 113.52(12) . . ? N1 C12 H12A 106.3 . . ? C14 C12 H12A 106.3 . . ? C13 C12 H12A 106.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C18 112.25(12) . . ? N2 C17 C19 111.54(12) . . ? C18 C17 C19 112.62(13) . . ? N2 C17 H17A 106.7 . . ? C18 C17 H17A 106.7 . . ? C19 C17 H17A 106.7 . . ? 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 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Cl1S C1S Cl2S 109.2(3) . . ? Cl1S C1S H1S1 109.8 . . ? Cl2S C1S H1S1 109.8 . . ? Cl1S C1S H1S2 109.8 . . ? Cl2S C1S H1S2 109.8 . . ? H1S1 C1S H1S2 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 Cu1 Cu2 C9 126.42(4) . . . . ? S2 Cu1 Cu2 C9 -49.59(4) 3_755 . . . ? Cu2 Cu1 Cu2 C9 -109.65(4) 3_755 . . . ? S2 Cu1 Cu2 S1 -176.01(2) 3_755 . . . ? Cu2 Cu1 Cu2 S1 123.933(17) 3_755 . . . ? S1 Cu1 Cu2 S2 -89.315(19) . . . . ? S2 Cu1 Cu2 S2 94.68(2) 3_755 . . . ? Cu2 Cu1 Cu2 S2 34.618(12) 3_755 . . . ? S1 Cu1 Cu2 Cu1 -123.932(17) . . . 3_755 ? S2 Cu1 Cu2 Cu1 60.059(18) 3_755 . . 3_755 ? Cu2 Cu1 Cu2 Cu1 0.0 3_755 . . 3_755 ? S2 Cu1 S1 C1 37.71(16) 3_755 . . . ? Cu2 Cu1 S1 C1 160.21(5) 3_755 . . . ? Cu2 Cu1 S1 C1 -113.62(5) . . . . ? S2 Cu1 S1 Cu2 151.33(14) 3_755 . . . ? Cu2 Cu1 S1 Cu2 -86.165(15) 3_755 . . . ? C9 Cu2 S1 C1 22.55(7) . . . . ? S2 Cu2 S1 C1 -154.56(5) . . . . ? Cu1 Cu2 S1 C1 156.51(5) 3_755 . . . ? Cu1 Cu2 S1 C1 106.56(5) . . . . ? C9 Cu2 S1 Cu1 -84.01(6) . . . . ? S2 Cu2 S1 Cu1 98.88(2) . . . . ? Cu1 Cu2 S1 Cu1 49.953(16) 3_755 . . . ? C9 Cu2 S2 C5 -9.53(7) . . . . ? S1 Cu2 S2 C5 167.75(5) . . . . ? Cu1 Cu2 S2 C5 -102.71(5) 3_755 . . . ? Cu1 Cu2 S2 C5 -146.76(5) . . . . ? C9 Cu2 S2 Cu1 93.18(5) . . . 3_755 ? S1 Cu2 S2 Cu1 -89.537(15) . . . 3_755 ? Cu1 Cu2 S2 Cu1 -44.047(16) . . . 3_755 ? Cu1 S1 C1 C4 49.25(11) . . . . ? Cu2 S1 C1 C4 -44.71(12) . . . . ? Cu1 S1 C1 C2 -72.14(11) . . . . ? Cu2 S1 C1 C2 -166.10(10) . . . . ? Cu1 S1 C1 C3 169.64(10) . . . . ? Cu2 S1 C1 C3 75.68(11) . . . . ? Cu1 S2 C5 C6 -48.82(11) 3_755 . . . ? Cu2 S2 C5 C6 35.22(12) . . . . ? Cu1 S2 C5 C7 -169.27(9) 3_755 . . . ? Cu2 S2 C5 C7 -85.22(11) . . . . ? Cu1 S2 C5 C8 72.93(11) 3_755 . . . ? Cu2 S2 C5 C8 156.98(9) . . . . ? C10 N1 C9 N2 -0.50(13) . . . . ? C12 N1 C9 N2 177.22(10) . . . . ? C10 N1 C9 Cu2 174.71(9) . . . . ? C12 N1 C9 Cu2 -7.57(17) . . . . ? C11 N2 C9 N1 0.64(13) . . . . ? C17 N2 C9 N1 -177.25(11) . . . . ? C11 N2 C9 Cu2 -174.53(9) . . . . ? C17 N2 C9 Cu2 7.58(17) . . . . ? S1 Cu2 C9 N1 93.58(11) . . . . ? S2 Cu2 C9 N1 -90.11(11) . . . . ? Cu1 Cu2 C9 N1 -33.08(12) 3_755 . . . ? Cu1 Cu2 C9 N1 42.50(12) . . . . ? S1 Cu2 C9 N2 -92.31(11) . . . . ? S2 Cu2 C9 N2 84.00(12) . . . . ? Cu1 Cu2 C9 N2 141.04(10) 3_755 . . . ? Cu1 Cu2 C9 N2 -143.38(10) . . . . ? C9 N1 C10 C11 0.17(14) . . . . ? C12 N1 C10 C11 -177.34(12) . . . . ? C9 N1 C10 C15 -179.59(12) . . . . ? C12 N1 C10 C15 2.9(2) . . . . ? N1 C10 C11 N2 0.22(14) . . . . ? C15 C10 C11 N2 179.98(13) . . . . ? N1 C10 C11 C16 -178.91(13) . . . . ? C15 C10 C11 C16 0.8(2) . . . . ? C9 N2 C11 C10 -0.56(14) . . . . ? C17 N2 C11 C10 177.11(12) . . . . ? C9 N2 C11 C16 178.60(13) . . . . ? C17 N2 C11 C16 -3.7(2) . . . . ? C9 N1 C12 C14 -106.25(13) . . . . ? C10 N1 C12 C14 71.06(16) . . . . ? C9 N1 C12 C13 125.12(13) . . . . ? C10 N1 C12 C13 -57.56(17) . . . . ? C9 N2 C17 C18 -122.46(14) . . . . ? C11 N2 C17 C18 60.06(18) . . . . ? C9 N2 C17 C19 110.08(14) . . . . ? C11 N2 C17 C19 -67.41(17) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 33.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.536 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.073 _database_code_depnum_ccdc_archive 'CCDC 960479' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H78 Cu4 P2 S4' _chemical_formula_sum 'C34 H78 Cu4 P2 S4' _chemical_formula_weight 931.30 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.468(3) _cell_length_b 10.869(4) _cell_length_c 12.157(5) _cell_angle_alpha 68.774(14) _cell_angle_beta 78.351(10) _cell_angle_gamma 82.542(12) _cell_volume 1139.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7723 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 30.51 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_F_000 492 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.206 _exptl_crystal_size_mid 0.158 _exptl_crystal_size_min 0.151 _exptl_absorpt_coefficient_mu 2.115 _shelx_estimated_absorpt_T_min 0.670 _shelx_estimated_absorpt_T_max 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6746 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25671 _diffrn_reflns_av_unetI/netI 0.0519 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.791 _diffrn_reflns_theta_max 35.905 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.818 _diffrn_measured_fraction_theta_full 0.955 _diffrn_reflns_Laue_measured_fraction_max 0.818 _diffrn_reflns_Laue_measured_fraction_full 0.955 _diffrn_reflns_point_group_measured_fraction_max 0.818 _diffrn_reflns_point_group_measured_fraction_full 0.955 _reflns_number_total 8769 _reflns_number_gt 6239 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material cif2tables.py _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8769 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.55970(2) 0.44945(2) 0.88316(2) 0.02265(6) Uani 1 1 d . . . . . Cu2 Cu 0.59075(2) 0.71765(2) 0.88244(2) 0.01972(6) Uani 1 1 d . . . . . S1 S 0.40137(4) 0.30656(4) 0.92332(4) 0.01996(9) Uani 1 1 d . . . . . S2 S 0.74021(4) 0.57546(4) 0.81423(4) 0.02053(9) Uani 1 1 d . . . . . P1 P 0.44040(4) 0.89577(4) 0.81910(4) 0.01849(9) Uani 1 1 d . . . . . C1 C 0.23553(17) 0.39746(17) 0.86685(15) 0.0216(3) Uani 1 1 d . . . . . C2 C 0.2418(2) 0.3886(2) 0.74309(17) 0.0363(5) Uani 1 1 d . . . . . H2A H 0.1527 0.4301 0.7124 0.054 Uiso 1 1 calc R U . . . H2B H 0.2519 0.2955 0.7493 0.054 Uiso 1 1 calc R U . . . H2C H 0.3249 0.4345 0.6883 0.054 Uiso 1 1 calc R U . . . C3 C 0.2270(2) 0.54186(18) 0.85693(17) 0.0294(4) Uani 1 1 d . . . . . H3A H 0.1376 0.5862 0.8283 0.044 Uiso 1 1 calc R U . . . H3B H 0.3103 0.5853 0.8004 0.044 Uiso 1 1 calc R U . . . H3C H 0.2274 0.5470 0.9357 0.044 Uiso 1 1 calc R U . . . C4 C 0.10602(19) 0.3287(2) 0.95264(18) 0.0322(4) Uani 1 1 d . . . . . H4A H 0.0169 0.3739 0.9241 0.048 Uiso 1 1 calc R U . . . H4B H 0.1058 0.3313 1.0324 0.048 Uiso 1 1 calc R U . . . H4C H 0.1118 0.2365 0.9568 0.048 Uiso 1 1 calc R U . . . C5 C 0.76845(18) 0.60798(17) 0.65032(15) 0.0225(3) Uani 1 1 d . . . . . C6 C 0.8082(2) 0.4757(2) 0.63186(18) 0.0377(5) Uani 1 1 d . . . . . H6A H 0.8268 0.4898 0.5460 0.056 Uiso 1 1 calc R U . . . H6B H 0.7283 0.4175 0.6715 0.056 Uiso 1 1 calc R U . . . H6C H 0.8952 0.4345 0.6662 0.056 Uiso 1 1 calc R U . . . C7 C 0.8931(2) 0.6982(2) 0.59247(18) 0.0353(4) Uani 1 1 d . . . . . H7A H 0.9145 0.7134 0.5064 0.053 Uiso 1 1 calc R U . . . H7B H 0.9787 0.6565 0.6287 0.053 Uiso 1 1 calc R U . . . H7C H 0.8662 0.7829 0.6050 0.053 Uiso 1 1 calc R U . . . C8 C 0.6341(2) 0.6733(2) 0.59795(16) 0.0338(4) Uani 1 1 d . . . . . H8A H 0.6528 0.6901 0.5116 0.051 Uiso 1 1 calc R U . . . H8B H 0.6085 0.7572 0.6122 0.051 Uiso 1 1 calc R U . . . H8C H 0.5542 0.6149 0.6361 0.051 Uiso 1 1 calc R U . . . C9 C 0.30604(17) 0.89214(17) 0.73088(15) 0.0218(3) Uani 1 1 d . . . . . H9A H 0.3587 0.8794 0.6563 0.026 Uiso 1 1 calc R U . . . H9B H 0.2499 0.8133 0.7766 0.026 Uiso 1 1 calc R U . . . C10 C 0.19885(19) 1.01173(18) 0.69606(17) 0.0276(4) Uani 1 1 d . . . . . H10A H 0.1653 1.0419 0.7652 0.033 Uiso 1 1 calc R U . . . H10B H 0.2484 1.0848 0.6299 0.033 Uiso 1 1 calc R U . . . C11 C 0.0690(2) 0.9809(2) 0.65706(18) 0.0354(5) Uani 1 1 d . . . . . H11A H 0.0012 1.0589 0.6393 0.053 Uiso 1 1 calc R U . . . H11B H 0.0211 0.9070 0.7215 0.053 Uiso 1 1 calc R U . . . H11C H 0.1011 0.9568 0.5852 0.053 Uiso 1 1 calc R U . . . C12 C 0.52671(18) 1.05224(18) 0.73632(15) 0.0233(3) Uani 1 1 d . . . . . H12A H 0.4498 1.1243 0.7209 0.028 Uiso 1 1 calc R U . . . H12B H 0.5849 1.0681 0.7885 0.028 Uiso 1 1 calc R U . . . C13 C 0.6234(2) 1.06235(19) 0.61814(16) 0.0314(4) Uani 1 1 d . . . . . H13A H 0.5662 1.0494 0.5638 0.038 Uiso 1 1 calc R U . . . H13B H 0.7014 0.9911 0.6320 0.038 Uiso 1 1 calc R U . . . C14 C 0.6903(2) 1.19585(19) 0.55855(17) 0.0323(4) Uani 1 1 d . . . . . H14A H 0.7474 1.2006 0.4805 0.048 Uiso 1 1 calc R U . . . H14B H 0.7531 1.2060 0.6093 0.048 Uiso 1 1 calc R U . . . H14C H 0.6135 1.2668 0.5476 0.048 Uiso 1 1 calc R U . . . C15 C 0.32970(17) 0.93731(17) 0.94499(14) 0.0215(3) Uani 1 1 d . . . . . H15A H 0.3936 0.9367 1.0004 0.026 Uiso 1 1 calc R U . . . H15B H 0.2857 1.0283 0.9138 0.026 Uiso 1 1 calc R U . . . C16 C 0.21053(18) 0.84486(18) 1.01471(15) 0.0254(4) Uani 1 1 d . . . . . H16A H 0.2526 0.7526 1.0398 0.031 Uiso 1 1 calc R U . . . H16B H 0.1403 0.8523 0.9620 0.031 Uiso 1 1 calc R U . . . C17 C 0.1320(2) 0.8752(2) 1.12477(17) 0.0361(5) Uani 1 1 d . . . . . H17A H 0.0538 0.8153 1.1654 0.054 Uiso 1 1 calc R U . . . H17B H 0.0914 0.9669 1.1006 0.054 Uiso 1 1 calc R U . . . H17C H 0.2000 0.8631 1.1794 0.054 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01839(11) 0.02505(12) 0.02250(11) -0.00599(10) -0.00399(8) -0.00004(8) Cu2 0.01653(10) 0.02127(11) 0.02086(10) -0.00763(9) -0.00359(7) 0.00225(8) S1 0.0186(2) 0.0204(2) 0.02107(19) -0.00801(17) -0.00491(14) 0.00314(15) S2 0.0178(2) 0.0219(2) 0.0225(2) -0.00877(18) -0.00532(14) 0.00306(15) P1 0.0170(2) 0.0196(2) 0.01871(19) -0.00759(18) -0.00327(15) 0.00268(16) C1 0.0205(8) 0.0223(9) 0.0237(8) -0.0087(8) -0.0091(6) 0.0041(7) C2 0.0397(12) 0.0444(13) 0.0304(10) -0.0189(10) -0.0172(8) 0.0133(9) C3 0.0279(10) 0.0219(9) 0.0382(11) -0.0098(9) -0.0116(8) 0.0065(7) C4 0.0190(9) 0.0326(11) 0.0444(12) -0.0109(10) -0.0072(8) -0.0035(8) C5 0.0219(8) 0.0231(9) 0.0222(8) -0.0095(8) -0.0011(6) 0.0007(7) C6 0.0481(13) 0.0340(12) 0.0338(11) -0.0202(10) -0.0001(9) 0.0020(9) C7 0.0284(10) 0.0359(12) 0.0350(11) -0.0067(10) 0.0014(8) -0.0056(8) C8 0.0294(10) 0.0478(13) 0.0234(9) -0.0116(10) -0.0076(7) 0.0034(9) C9 0.0221(8) 0.0227(9) 0.0226(8) -0.0102(7) -0.0072(6) 0.0039(7) C10 0.0250(9) 0.0250(10) 0.0309(10) -0.0067(8) -0.0099(7) 0.0047(7) C11 0.0270(10) 0.0445(13) 0.0379(11) -0.0170(11) -0.0137(8) 0.0076(9) C12 0.0215(8) 0.0247(9) 0.0245(8) -0.0110(8) -0.0006(6) -0.0019(7) C13 0.0386(11) 0.0284(10) 0.0267(9) -0.0126(9) 0.0061(8) -0.0092(8) C14 0.0334(11) 0.0312(11) 0.0322(10) -0.0117(9) 0.0009(8) -0.0092(8) C15 0.0208(8) 0.0233(9) 0.0219(8) -0.0106(7) -0.0035(6) 0.0016(7) C16 0.0209(9) 0.0262(9) 0.0263(9) -0.0085(8) 0.0004(6) 0.0004(7) C17 0.0307(11) 0.0497(14) 0.0279(10) -0.0161(10) 0.0038(8) -0.0073(9) _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 Cu1 S1 2.1580(8) . ? Cu1 S2 2.1673(8) . ? Cu1 Cu2 2.9551(10) 2_667 ? Cu1 Cu2 2.9643(11) . ? Cu2 S2 2.2282(7) . ? Cu2 P1 2.2394(8) . ? Cu2 S1 2.2951(10) 2_667 ? Cu2 Cu1 2.9551(10) 2_667 ? S1 C1 1.8586(17) . ? S1 Cu2 2.2951(10) 2_667 ? S2 C5 1.8619(18) . ? P1 C12 1.8336(19) . ? P1 C9 1.8343(16) . ? P1 C15 1.8369(16) . ? C1 C4 1.519(3) . ? C1 C3 1.523(2) . ? C1 C2 1.531(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.514(2) . ? C5 C7 1.521(3) . ? C5 C6 1.523(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.527(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.518(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.515(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.524(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.514(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.519(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 S1 Cu1 S2 167.928(18) . . ? S1 Cu1 Cu2 50.44(2) . 2_667 ? S2 Cu1 Cu2 138.239(18) . 2_667 ? S1 Cu1 Cu2 142.088(19) . . ? S2 Cu1 Cu2 48.468(18) . . ? Cu2 Cu1 Cu2 111.16(2) 2_667 . ? S2 Cu2 P1 140.65(3) . . ? S2 Cu2 S1 114.11(2) . 2_667 ? P1 Cu2 S1 104.98(2) . 2_667 ? S2 Cu2 Cu1 104.21(3) . 2_667 ? P1 Cu2 Cu1 105.78(3) . 2_667 ? S1 Cu2 Cu1 46.47(2) 2_667 2_667 ? S2 Cu2 Cu1 46.73(2) . . ? P1 Cu2 Cu1 126.03(2) . . ? S1 Cu2 Cu1 106.09(2) 2_667 . ? Cu1 Cu2 Cu1 68.84(2) 2_667 . ? C1 S1 Cu1 107.74(6) . . ? C1 S1 Cu2 114.72(5) . 2_667 ? Cu1 S1 Cu2 83.09(2) . 2_667 ? C5 S2 Cu1 103.01(6) . . ? C5 S2 Cu2 117.11(6) . . ? Cu1 S2 Cu2 84.80(3) . . ? C12 P1 C9 105.11(8) . . ? C12 P1 C15 99.73(8) . . ? C9 P1 C15 103.01(8) . . ? C12 P1 Cu2 115.66(7) . . ? C9 P1 Cu2 119.35(6) . . ? C15 P1 Cu2 111.54(6) . . ? C4 C1 C3 110.32(14) . . ? C4 C1 C2 110.25(15) . . ? C3 C1 C2 109.79(16) . . ? C4 C1 S1 107.82(13) . . ? C3 C1 S1 111.71(11) . . ? C2 C1 S1 106.87(11) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 109.99(17) . . ? C8 C5 C6 110.36(15) . . ? C7 C5 C6 110.23(15) . . ? C8 C5 S2 111.43(11) . . ? C7 C5 S2 107.27(12) . . ? C6 C5 S2 107.49(13) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 117.98(12) . . ? C10 C9 H9A 107.8 . . ? P1 C9 H9A 107.8 . . ? C10 C9 H9B 107.8 . . ? P1 C9 H9B 107.8 . . ? H9A C9 H9B 107.1 . . ? C11 C10 C9 112.28(15) . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 P1 116.68(12) . . ? C13 C12 H12A 108.1 . . ? P1 C12 H12A 108.1 . . ? C13 C12 H12B 108.1 . . ? P1 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? C12 C13 C14 111.88(15) . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13B 109.2 . . ? C14 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 P1 114.43(11) . . ? C16 C15 H15A 108.7 . . ? P1 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? P1 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C15 C16 C17 112.29(14) . . ? C15 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? C15 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 S1 C1 C4 -145.18(10) . . . . ? Cu2 S1 C1 C4 -54.71(12) 2_667 . . . ? Cu1 S1 C1 C3 -23.80(13) . . . . ? Cu2 S1 C1 C3 66.67(14) 2_667 . . . ? Cu1 S1 C1 C2 96.31(13) . . . . ? Cu2 S1 C1 C2 -173.22(11) 2_667 . . . ? Cu1 S2 C5 C8 58.80(14) . . . . ? Cu2 S2 C5 C8 -31.99(15) . . . . ? Cu1 S2 C5 C7 179.24(11) . . . . ? Cu2 S2 C5 C7 88.44(13) . . . . ? Cu1 S2 C5 C6 -62.23(13) . . . . ? Cu2 S2 C5 C6 -153.02(11) . . . . ? C12 P1 C9 C10 -52.12(15) . . . . ? C15 P1 C9 C10 51.89(15) . . . . ? Cu2 P1 C9 C10 176.10(11) . . . . ? P1 C9 C10 C11 -162.99(13) . . . . ? C9 P1 C12 C13 -69.94(16) . . . . ? C15 P1 C12 C13 -176.37(14) . . . . ? Cu2 P1 C12 C13 63.92(15) . . . . ? P1 C12 C13 C14 -179.29(14) . . . . ? C12 P1 C15 C16 163.47(13) . . . . ? C9 P1 C15 C16 55.35(15) . . . . ? Cu2 P1 C15 C16 -73.85(13) . . . . ? P1 C15 C16 C17 174.34(13) . . . . ? _refine_diff_density_max 0.511 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.091 _shelxl_version_number 2013-3 _database_code_depnum_ccdc_archive 'CCDC 960480' ####################################################################### # # 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_4 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H78 Cu4 P2 S4' _chemical_formula_sum 'C34 H78 Cu4 P2 S4' _chemical_formula_weight 931.30 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2300(14) _cell_length_b 13.023(2) _cell_length_c 18.533(3) _cell_angle_alpha 90 _cell_angle_beta 114.317(4) _cell_angle_gamma 90 _cell_volume 2250.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4623 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 35.65 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_F_000 984 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.612 _exptl_crystal_size_mid 0.233 _exptl_crystal_size_min 0.223 _exptl_absorpt_coefficient_mu 2.143 _shelx_estimated_absorpt_T_min 0.354 _shelx_estimated_absorpt_T_max 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.302997 _exptl_absorpt_correction_T_max 0.441125 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19802 _diffrn_reflns_av_unetI/netI 0.0361 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.294 _diffrn_reflns_theta_max 39.361 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.935 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.935 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 19802 _reflns_number_gt 16387 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection APEX2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution XS _computing_structure_refinement SHELXL-2013 _computing_molecular_graphics Mercury _computing_publication_material cif2tables.py _refine_special_details ; Refined as a 2-component twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.2815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 19802 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0592 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.003 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.62360(2) 0.09074(2) 0.55527(2) 0.01730(3) Uani 1 1 d . . . . . Cu2 Cu 0.37901(2) 0.15925(2) 0.40728(2) 0.01398(3) Uani 1 1 d . . . . . S1 S 0.61138(3) 0.19902(2) 0.46420(2) 0.01523(5) Uani 1 1 d . . . . . S2 S 0.33658(3) 0.00335(2) 0.34224(2) 0.01598(5) Uani 1 1 d . . . . . P1 P 0.16366(3) 0.23355(2) 0.37406(2) 0.01329(5) Uani 1 1 d . . . . . C1 C 0.65902(12) 0.32434(9) 0.51656(7) 0.0173(2) Uani 1 1 d . . . . . C2 C 0.81571(13) 0.31849(11) 0.57509(8) 0.0250(2) Uani 1 1 d . . . . . H2A H 0.8755 0.3035 0.5465 0.038 Uiso 1 1 calc R U . . . H2B H 0.8275 0.2639 0.6137 0.038 Uiso 1 1 calc R U . . . H2C H 0.8449 0.3843 0.6027 0.038 Uiso 1 1 calc R U . . . C3 C 0.56467(15) 0.34794(11) 0.56011(9) 0.0290(3) Uani 1 1 d . . . . . H3A H 0.5901 0.4155 0.5854 0.043 Uiso 1 1 calc R U . . . H3B H 0.5795 0.2954 0.6006 0.043 Uiso 1 1 calc R U . . . H3C H 0.4638 0.3481 0.5224 0.043 Uiso 1 1 calc R U . . . C4 C 0.64087(15) 0.40601(10) 0.45455(9) 0.0286(3) Uani 1 1 d . . . . . H4A H 0.5399 0.4095 0.4171 0.043 Uiso 1 1 calc R U . . . H4B H 0.7000 0.3884 0.4260 0.043 Uiso 1 1 calc R U . . . H4C H 0.6710 0.4728 0.4805 0.043 Uiso 1 1 calc R U . . . C5 C 0.47548(11) -0.03206(8) 0.30575(7) 0.01632(19) Uani 1 1 d . . . . . C6 C 0.43018(14) -0.13430(10) 0.26202(8) 0.0241(2) Uani 1 1 d . . . . . H6A H 0.3328 -0.1281 0.2204 0.036 Uiso 1 1 calc R U . . . H6B H 0.4320 -0.1880 0.2995 0.036 Uiso 1 1 calc R U . . . H6C H 0.4966 -0.1524 0.2382 0.036 Uiso 1 1 calc R U . . . C7 C 0.47623(13) 0.05187(10) 0.24855(8) 0.0226(2) Uani 1 1 d . . . . . H7A H 0.5048 0.1172 0.2770 0.034 Uiso 1 1 calc R U . . . H7B H 0.3800 0.0586 0.2060 0.034 Uiso 1 1 calc R U . . . H7C H 0.5444 0.0337 0.2259 0.034 Uiso 1 1 calc R U . . . C8 C 0.62313(12) -0.04250(10) 0.37357(7) 0.0216(2) Uani 1 1 d . . . . . H8A H 0.6921 -0.0656 0.3528 0.032 Uiso 1 1 calc R U . . . H8B H 0.6189 -0.0928 0.4119 0.032 Uiso 1 1 calc R U . . . H8C H 0.6534 0.0242 0.3997 0.032 Uiso 1 1 calc R U . . . C9 C 0.02117(11) 0.13429(9) 0.34944(7) 0.0176(2) Uani 1 1 d . . . . . H9 H 0.0310 0.0910 0.3074 0.021 Uiso 1 1 calc R U . . . C10 C -0.13490(12) 0.17083(10) 0.31398(9) 0.0286(3) Uani 1 1 d . . . . . H10A H -0.1983 0.1129 0.2886 0.043 Uiso 1 1 calc R U . . . H10B H -0.1473 0.2244 0.2746 0.043 Uiso 1 1 calc R U . . . H10C H -0.1591 0.1986 0.3561 0.043 Uiso 1 1 calc R U . . . C11 C 0.04875(14) 0.06126(11) 0.41883(9) 0.0281(3) Uani 1 1 d . . . . . H11A H 0.0247 0.0957 0.4588 0.042 Uiso 1 1 calc R U . . . H11B H 0.1502 0.0414 0.4424 0.042 Uiso 1 1 calc R U . . . H11C H -0.0109 -0.0002 0.3998 0.042 Uiso 1 1 calc R U . . . C12 C 0.11637(11) 0.30196(9) 0.27866(7) 0.01711(19) Uani 1 1 d . . . . . H12 H 0.0110 0.3163 0.2548 0.021 Uiso 1 1 calc R U . . . C13 C 0.19709(15) 0.40394(10) 0.29076(8) 0.0260(2) Uani 1 1 d . . . . . H13A H 0.3000 0.3919 0.3208 0.039 Uiso 1 1 calc R U . . . H13B H 0.1627 0.4514 0.3201 0.039 Uiso 1 1 calc R U . . . H13C H 0.1803 0.4337 0.2391 0.039 Uiso 1 1 calc R U . . . C14 C 0.15192(13) 0.23517(11) 0.22112(7) 0.0230(2) Uani 1 1 d . . . . . H14A H 0.1192 0.2697 0.1697 0.035 Uiso 1 1 calc R U . . . H14B H 0.1035 0.1687 0.2147 0.035 Uiso 1 1 calc R U . . . H14C H 0.2558 0.2244 0.2422 0.035 Uiso 1 1 calc R U . . . C15 C 0.13899(12) 0.33415(9) 0.43823(7) 0.0182(2) Uani 1 1 d . . . . . H15 H 0.2143 0.3867 0.4447 0.022 Uiso 1 1 calc R U . . . C16 C -0.00334(14) 0.39355(10) 0.40525(9) 0.0269(3) Uani 1 1 d . . . . . H16A H -0.0792 0.3506 0.4087 0.040 Uiso 1 1 calc R U . . . H16B H -0.0283 0.4116 0.3498 0.040 Uiso 1 1 calc R U . . . H16C H 0.0067 0.4563 0.4362 0.040 Uiso 1 1 calc R U . . . C17 C 0.17363(15) 0.29513(11) 0.52199(8) 0.0264(3) Uani 1 1 d . . . . . H17A H 0.1858 0.3537 0.5574 0.040 Uiso 1 1 calc R U . . . H17B H 0.2624 0.2549 0.5409 0.040 Uiso 1 1 calc R U . . . H17C H 0.0949 0.2518 0.5214 0.040 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01765(6) 0.01609(6) 0.01982(7) -0.00052(5) 0.00937(5) 0.00063(5) Cu2 0.01141(5) 0.01646(6) 0.01352(6) -0.00043(5) 0.00459(4) 0.00062(4) S1 0.01224(10) 0.01623(12) 0.01673(12) -0.00223(9) 0.00546(9) 0.00056(8) S2 0.01419(10) 0.01508(11) 0.01893(13) -0.00136(9) 0.00706(9) -0.00002(9) P1 0.01075(10) 0.01484(12) 0.01407(12) -0.00123(9) 0.00490(9) 0.00012(8) C1 0.0140(4) 0.0178(5) 0.0176(5) -0.0031(4) 0.0039(4) -0.0009(3) C2 0.0167(5) 0.0263(6) 0.0244(6) -0.0044(5) 0.0007(4) -0.0015(4) C3 0.0258(6) 0.0291(7) 0.0358(7) -0.0143(6) 0.0166(5) -0.0031(5) C4 0.0317(6) 0.0188(6) 0.0280(7) 0.0016(5) 0.0048(5) -0.0010(5) C5 0.0163(4) 0.0164(5) 0.0171(5) -0.0021(4) 0.0077(4) 0.0002(3) C6 0.0290(6) 0.0201(6) 0.0258(6) -0.0077(5) 0.0140(5) -0.0041(4) C7 0.0239(5) 0.0224(6) 0.0245(6) 0.0028(5) 0.0130(5) 0.0008(4) C8 0.0173(4) 0.0258(6) 0.0209(6) -0.0027(4) 0.0070(4) 0.0051(4) C9 0.0134(4) 0.0168(5) 0.0220(5) -0.0009(4) 0.0067(4) -0.0008(3) C10 0.0136(4) 0.0227(6) 0.0449(8) 0.0000(5) 0.0073(5) -0.0018(4) C11 0.0265(6) 0.0249(6) 0.0319(7) 0.0056(5) 0.0110(5) -0.0050(5) C12 0.0135(4) 0.0206(5) 0.0160(5) 0.0017(4) 0.0048(4) 0.0010(4) C13 0.0304(6) 0.0223(6) 0.0267(7) 0.0029(5) 0.0133(5) -0.0048(5) C14 0.0236(5) 0.0298(6) 0.0146(5) -0.0008(4) 0.0068(4) 0.0015(4) C15 0.0167(4) 0.0194(5) 0.0191(5) -0.0034(4) 0.0079(4) 0.0010(4) C16 0.0233(5) 0.0262(6) 0.0304(7) -0.0069(5) 0.0103(5) 0.0075(4) C17 0.0313(6) 0.0303(7) 0.0202(6) -0.0029(5) 0.0132(5) 0.0017(5) _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 Cu1 S2 2.1535(4) 3_656 ? Cu1 S1 2.1633(4) . ? Cu1 Cu2 2.9879(4) . ? Cu2 S1 2.2287(4) . ? Cu2 P1 2.2476(4) . ? Cu2 S2 2.3093(4) . ? S1 C1 1.8584(12) . ? S2 C5 1.8656(11) . ? S2 Cu1 2.1536(4) 3_656 ? P1 C15 1.8552(12) . ? P1 C12 1.8572(12) . ? P1 C9 1.8591(11) . ? C1 C4 1.5201(18) . ? C1 C3 1.5228(17) . ? C1 C2 1.5231(16) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.5220(16) . ? C5 C7 1.5249(17) . ? C5 C6 1.5281(16) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.5294(18) . ? C9 C10 1.5308(16) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.5309(17) . ? C12 C14 1.5313(17) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.5299(18) . ? C15 C16 1.5359(16) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 S2 Cu1 S1 171.214(13) 3_656 . ? S2 Cu1 Cu2 139.665(11) 3_656 . ? S1 Cu1 Cu2 48.057(10) . . ? S1 Cu2 P1 139.797(14) . . ? S1 Cu2 S2 112.704(11) . . ? P1 Cu2 S2 106.449(13) . . ? S1 Cu2 Cu1 46.218(10) . . ? P1 Cu2 Cu1 137.381(11) . . ? S2 Cu2 Cu1 97.063(12) . . ? C1 S1 Cu1 104.27(4) . . ? C1 S1 Cu2 116.78(4) . . ? Cu1 S1 Cu2 85.725(12) . . ? C5 S2 Cu1 106.46(4) . 3_656 ? C5 S2 Cu2 113.52(4) . . ? Cu1 S2 Cu2 96.504(16) 3_656 . ? C15 P1 C12 102.74(5) . . ? C15 P1 C9 110.39(5) . . ? C12 P1 C9 103.26(5) . . ? C15 P1 Cu2 120.34(4) . . ? C12 P1 Cu2 108.00(4) . . ? C9 P1 Cu2 110.42(4) . . ? C4 C1 C3 110.65(11) . . ? C4 C1 C2 109.79(10) . . ? C3 C1 C2 110.09(11) . . ? C4 C1 S1 107.19(8) . . ? C3 C1 S1 111.52(8) . . ? C2 C1 S1 107.50(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 C7 110.54(10) . . ? C8 C5 C6 109.95(10) . . ? C7 C5 C6 110.07(10) . . ? C8 C5 S2 111.58(8) . . ? C7 C5 S2 107.30(8) . . ? C6 C5 S2 107.32(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C10 110.67(10) . . ? C11 C9 P1 111.81(8) . . ? C10 C9 P1 117.58(8) . . ? C11 C9 H9 105.2 . . ? C10 C9 H9 105.2 . . ? P1 C9 H9 105.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 109.04(10) . . ? C13 C12 P1 111.31(8) . . ? C14 C12 P1 110.30(8) . . ? C13 C12 H12 108.7 . . ? C14 C12 H12 108.7 . . ? P1 C12 H12 108.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 110.89(10) . . ? C17 C15 P1 112.34(9) . . ? C16 C15 P1 117.22(8) . . ? C17 C15 H15 105.1 . . ? C16 C15 H15 105.1 . . ? P1 C15 H15 105.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 S1 C1 C4 -175.50(7) . . . . ? Cu2 S1 C1 C4 -83.08(8) . . . . ? Cu1 S1 C1 C3 -54.24(9) . . . . ? Cu2 S1 C1 C3 38.18(10) . . . . ? Cu1 S1 C1 C2 66.53(9) . . . . ? Cu2 S1 C1 C2 158.95(7) . . . . ? Cu1 S2 C5 C8 -43.55(9) 3_656 . . . ? Cu2 S2 C5 C8 61.37(9) . . . . ? Cu1 S2 C5 C7 -164.77(7) 3_656 . . . ? Cu2 S2 C5 C7 -59.85(8) . . . . ? Cu1 S2 C5 C6 76.96(8) 3_656 . . . ? Cu2 S2 C5 C6 -178.12(7) . . . . ? C15 P1 C9 C11 -76.54(10) . . . . ? C12 P1 C9 C11 174.22(9) . . . . ? Cu2 P1 C9 C11 58.98(9) . . . . ? C15 P1 C9 C10 53.10(11) . . . . ? C12 P1 C9 C10 -56.13(11) . . . . ? Cu2 P1 C9 C10 -171.38(9) . . . . ? C15 P1 C12 C13 50.40(9) . . . . ? C9 P1 C12 C13 165.26(8) . . . . ? Cu2 P1 C12 C13 -77.77(8) . . . . ? C15 P1 C12 C14 171.58(8) . . . . ? C9 P1 C12 C14 -73.56(9) . . . . ? Cu2 P1 C12 C14 43.41(8) . . . . ? C12 P1 C15 C17 -179.53(8) . . . . ? C9 P1 C15 C17 70.89(10) . . . . ? Cu2 P1 C15 C17 -59.57(9) . . . . ? C12 P1 C15 C16 50.30(10) . . . . ? C9 P1 C15 C16 -59.27(11) . . . . ? Cu2 P1 C15 C16 170.26(8) . . . . ? _refine_diff_density_max 0.465 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.086 _shelxl_version_number 2013-3 _database_code_depnum_ccdc_archive 'CCDC 960481' ####################################################################### # # 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_5 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41.60 H70.80 Ag4 N4 S4, C42 H72 Ag4 N4 S4, 2(C7 H8), 0.4(C H3)' _chemical_formula_sum 'C98 H160 Ag8 N8 S8' _chemical_formula_weight 2569.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.990(3) _cell_length_b 12.648(4) _cell_length_c 23.429(9) _cell_angle_alpha 78.597(13) _cell_angle_beta 78.069(9) _cell_angle_gamma 80.553(12) _cell_volume 2815.7(17) _cell_formula_units_Z 1 _cell_measurement_temperature 111(2) _cell_measurement_reflns_used 9986 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.74 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_F_000 1308 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.138 _exptl_crystal_size_mid 0.083 _exptl_crystal_size_min 0.076 _exptl_absorpt_coefficient_mu 1.553 _shelx_estimated_absorpt_T_min 0.814 _shelx_estimated_absorpt_T_max 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6816 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 111(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52327 _diffrn_reflns_av_unetI/netI 0.0519 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.656 _diffrn_reflns_theta_max 28.287 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 13901 _reflns_number_gt 9692 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection APEX2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution XS _computing_structure_refinement SHELXL-2013 _computing_molecular_graphics Mercury _computing_publication_material cif2tables.py _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+3.5701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 13901 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.49940(4) 1.19762(3) -0.08030(2) 0.04644(11) Uani 1 1 d . . . . . Ag2 Ag 0.55722(5) 0.91826(4) -0.04687(2) 0.03999(12) Uani 0.8 1 d . . P A 1 Ag2A Ag 0.6412(2) 0.91596(15) -0.07227(10) 0.0433(5) Uani 0.2 1 d . . P B 2 S1 S 0.40576(14) 1.03870(11) -0.10276(7) 0.0382(3) Uani 0.8 1 d . . P A 1 S1A S 0.5912(6) 1.0613(5) -0.1483(3) 0.0436(15) Uani 0.2 1 d . . P B 2 C1 C 0.4684(6) 1.0247(4) -0.1791(2) 0.0518(13) Uani 1 1 d . . . . . C2 C 0.3985(6) 1.1215(5) -0.2169(3) 0.0697(18) Uani 1 1 d . . . . . H2A H 0.4370 1.1203 -0.2588 0.105 Uiso 1 1 calc R U . . . H2B H 0.4142 1.1891 -0.2064 0.105 Uiso 1 1 calc R U . . . H2C H 0.2991 1.1174 -0.2099 0.105 Uiso 1 1 calc R U . . . C3 C 0.4450(8) 0.9182(6) -0.1917(4) 0.091(2) Uani 1 1 d . . . . . H3A H 0.3457 0.9150 -0.1860 0.137 Uiso 1 1 calc R U . . . H3B H 0.4866 0.8585 -0.1647 0.137 Uiso 1 1 calc R U . . . H3C H 0.4874 0.9115 -0.2327 0.137 Uiso 1 1 calc R U . . . C4 C 0.6326(6) 1.0234(6) -0.1958(3) 0.0510(16) Uani 0.8 1 d . . P A 1 H4A H 0.6769 0.9639 -0.1695 0.077 Uiso 0.8 1 calc R U P A 1 H4B H 0.6568 1.0928 -0.1911 0.077 Uiso 0.8 1 calc R U P A 1 H4C H 0.6645 1.0125 -0.2369 0.077 Uiso 0.8 1 calc R U P A 1 C4A C 0.326(3) 1.000(2) -0.1161(11) 0.052(7) Uani 0.2 1 d . . P A 2 H4A1 H 0.2445 0.9902 -0.1307 0.078 Uiso 0.2 1 calc R U P A 2 H4A2 H 0.3046 1.0619 -0.0951 0.078 Uiso 0.2 1 calc R U P A 2 H4A3 H 0.3539 0.9339 -0.0891 0.078 Uiso 0.2 1 calc R U P A 2 S2 S 0.28910(13) 1.22096(11) -0.00090(7) 0.0529(4) Uani 1 1 d . . . . . C5 C 0.2849(7) 1.3422(5) 0.0314(3) 0.0624(15) Uani 1 1 d . . . . . C6 C 0.4270(11) 1.3589(6) 0.0357(4) 0.124(3) Uani 1 1 d . . . . . H6A H 0.4671 1.2964 0.0616 0.187 Uiso 1 1 calc R U . . . H6B H 0.4223 1.4251 0.0522 0.187 Uiso 1 1 calc R U . . . H6C H 0.4847 1.3661 -0.0038 0.187 Uiso 1 1 calc R U . . . C7 C 0.2283(15) 1.4356(7) -0.0068(6) 0.205(7) Uani 1 1 d . . . . . H7A H 0.2866 1.4423 -0.0462 0.307 Uiso 1 1 calc R U . . . H7B H 0.2253 1.5014 0.0098 0.307 Uiso 1 1 calc R U . . . H7C H 0.1348 1.4265 -0.0100 0.307 Uiso 1 1 calc R U . . . C8 C 0.2122(16) 1.3185(11) 0.0937(5) 0.237(8) Uani 1 1 d . . . . . H8A H 0.2612 1.2536 0.1145 0.356 Uiso 1 1 calc R U . . . H8B H 0.1178 1.3057 0.0943 0.356 Uiso 1 1 calc R U . . . H8C H 0.2097 1.3806 0.1133 0.356 Uiso 1 1 calc R U . . . C9 C 0.6753(5) 1.2825(4) -0.1064(2) 0.0419(11) Uani 1 1 d . . . . . N1 N 0.7933(4) 1.2523(3) -0.08344(17) 0.0360(8) Uani 1 1 d . . . . . C10 C 0.8931(5) 1.3196(4) -0.1119(2) 0.0390(11) Uani 1 1 d . . . . . C11 C 1.0293(5) 1.3189(4) -0.1066(2) 0.0468(12) Uani 1 1 d . . . . . H11 H 1.0711 1.2656 -0.0787 0.056 Uiso 1 1 calc R U . . . C12 C 1.1018(6) 1.3976(4) -0.1432(3) 0.0583(15) Uani 1 1 d . . . . . H12 H 1.1944 1.4001 -0.1399 0.070 Uiso 1 1 calc R U . . . C13 C 1.0403(8) 1.4740(5) -0.1851(3) 0.0695(19) Uani 1 1 d . . . . . H13 H 1.0930 1.5268 -0.2102 0.083 Uiso 1 1 calc R U . . . C14 C 0.9065(7) 1.4751(4) -0.1910(2) 0.0611(17) Uani 1 1 d . . . . . H14 H 0.8655 1.5279 -0.2193 0.073 Uiso 1 1 calc R U . . . C15 C 0.8335(6) 1.3961(4) -0.1539(2) 0.0449(12) Uani 1 1 d . . . . . C16 C 0.8084(5) 1.1578(4) -0.0359(2) 0.0415(11) Uani 1 1 d . . . . . H16 H 0.7151 1.1333 -0.0222 0.050 Uiso 1 1 calc R U . . . C17 C 0.9025(5) 1.0641(4) -0.0602(2) 0.0493(13) Uani 1 1 d . . . . . H17A H 0.8686 1.0480 -0.0935 0.074 Uiso 1 1 calc R U . . . H17B H 0.9038 0.9997 -0.0290 0.074 Uiso 1 1 calc R U . . . H17C H 0.9962 1.0838 -0.0737 0.074 Uiso 1 1 calc R U . . . C18 C 0.8468(5) 1.1889(4) 0.0174(2) 0.0533(13) Uani 1 1 d . . . . . H18A H 0.9434 1.2024 0.0081 0.080 Uiso 1 1 calc R U . . . H18B H 0.8344 1.1295 0.0511 0.080 Uiso 1 1 calc R U . . . H18C H 0.7874 1.2549 0.0273 0.080 Uiso 1 1 calc R U . . . N2A N 0.7001(4) 1.3716(3) -0.14891(18) 0.0483(11) Uani 0.54(2) 1 d . . P C 1 C19A C 0.5839(19) 1.4130(14) -0.1858(7) 0.048(4) Uani 0.54(2) 1 d . . P C 1 H19A H 0.5412 1.3445 -0.1696 0.058 Uiso 0.54(2) 1 calc R U P C 1 C20A C 0.4804(14) 1.4663(19) -0.1634(6) 0.082(7) Uani 0.54(2) 1 d . . P C 1 H20A H 0.4247 1.5001 -0.1937 0.123 Uiso 0.54(2) 1 calc R U P C 1 H20B H 0.5067 1.5230 -0.1464 0.123 Uiso 0.54(2) 1 calc R U P C 1 H20C H 0.4264 1.4186 -0.1321 0.123 Uiso 0.54(2) 1 calc R U P C 1 C21A C 0.6373(6) 1.3752(4) -0.2442(2) 0.0514(13) Uani 0.54(2) 1 d . . P C 1 H21A H 0.5852 1.4185 -0.2739 0.077 Uiso 0.54(2) 1 calc R U P C 1 H21B H 0.6264 1.2983 -0.2400 0.077 Uiso 0.54(2) 1 calc R U P C 1 H21C H 0.7352 1.3843 -0.2568 0.077 Uiso 0.54(2) 1 calc R U P C 1 N2B N 0.7001(4) 1.3716(3) -0.14891(18) 0.0483(11) Uani 0.46(2) 1 d . . P C 2 C19B C 0.6331(18) 1.4423(15) -0.1946(7) 0.042(4) Uani 0.46(2) 1 d . . P C 2 H19B H 0.7100 1.4860 -0.2143 0.050 Uiso 0.46(2) 1 calc R U P C 2 C20B C 0.5330(18) 1.5246(14) -0.1823(9) 0.065(5) Uani 0.46(2) 1 d . . P C 2 H20D H 0.5142 1.5254 -0.1396 0.097 Uiso 0.46(2) 1 calc R U P C 2 H20E H 0.4489 1.5142 -0.1947 0.097 Uiso 0.46(2) 1 calc R U P C 2 H20F H 0.5633 1.5938 -0.2036 0.097 Uiso 0.46(2) 1 calc R U P C 2 C21B C 0.6373(6) 1.3752(4) -0.2442(2) 0.0514(13) Uani 0.46(2) 1 d . . P C 2 H21D H 0.5429 1.3684 -0.2474 0.077 Uiso 0.46(2) 1 calc R U P C 2 H21E H 0.6877 1.3027 -0.2345 0.077 Uiso 0.46(2) 1 calc R U P C 2 H21F H 0.6839 1.4125 -0.2821 0.077 Uiso 0.46(2) 1 calc R U P C 2 Ag3 Ag 0.37096(3) 1.54236(3) 0.45807(2) 0.03101(9) Uani 1 1 d . . . . . Ag4 Ag 0.46342(3) 1.28094(3) 0.52319(2) 0.03239(9) Uani 1 1 d . . . . . S3 S 0.42458(10) 1.37457(9) 0.42245(5) 0.0317(2) Uani 1 1 d . . . . . C22 C 0.2527(4) 1.3468(3) 0.4140(2) 0.0333(10) Uani 1 1 d . . . . . C23 C 0.1403(4) 1.3815(4) 0.4633(2) 0.0416(11) Uani 1 1 d . . . . . H23A H 0.0522 1.3623 0.4590 0.062 Uiso 1 1 calc R U . . . H23B H 0.1327 1.4604 0.4613 0.062 Uiso 1 1 calc R U . . . H23C H 0.1631 1.3444 0.5016 0.062 Uiso 1 1 calc R U . . . C24 C 0.2610(5) 1.2252(4) 0.4152(3) 0.0504(13) Uani 1 1 d . . . . . H24A H 0.1709 1.2080 0.4121 0.076 Uiso 1 1 calc R U . . . H24B H 0.2872 1.1854 0.4524 0.076 Uiso 1 1 calc R U . . . H24C H 0.3302 1.2040 0.3818 0.076 Uiso 1 1 calc R U . . . C25 C 0.2245(5) 1.4082(4) 0.3542(2) 0.0422(11) Uani 1 1 d . . . . . H25A H 0.3010 1.3879 0.3230 0.063 Uiso 1 1 calc R U . . . H25B H 0.2158 1.4866 0.3539 0.063 Uiso 1 1 calc R U . . . H25C H 0.1387 1.3898 0.3469 0.063 Uiso 1 1 calc R U . . . S4 S 0.71634(10) 1.28402(9) 0.51524(5) 0.0321(2) Uani 1 1 d . . . . . C26 C 0.7758(4) 1.2051(4) 0.5833(2) 0.0339(10) Uani 1 1 d . . . . . C27 C 0.6620(5) 1.2084(5) 0.6384(2) 0.0605(15) Uani 1 1 d . . . . . H27A H 0.6964 1.1640 0.6729 0.091 Uiso 1 1 calc R U . . . H27B H 0.5817 1.1796 0.6323 0.091 Uiso 1 1 calc R U . . . H27C H 0.6353 1.2837 0.6451 0.091 Uiso 1 1 calc R U . . . C28 C 0.8963(6) 1.2510(5) 0.5938(3) 0.0644(17) Uani 1 1 d . . . . . H28A H 0.9252 1.2107 0.6304 0.097 Uiso 1 1 calc R U . . . H28B H 0.8693 1.3279 0.5973 0.097 Uiso 1 1 calc R U . . . H28C H 0.9729 1.2445 0.5605 0.097 Uiso 1 1 calc R U . . . C29 C 0.8145(7) 1.0867(5) 0.5757(3) 0.0700(18) Uani 1 1 d . . . . . H29A H 0.8863 1.0814 0.5405 0.105 Uiso 1 1 calc R U . . . H29B H 0.7329 1.0578 0.5710 0.105 Uiso 1 1 calc R U . . . H29C H 0.8491 1.0445 0.6107 0.105 Uiso 1 1 calc R U . . . C30 C 0.3159(4) 1.2207(3) 0.59828(19) 0.0300(9) Uani 1 1 d . . . . . N3 N 0.2419(3) 1.2825(3) 0.63785(15) 0.0282(8) Uani 1 1 d . . . . . C31 C 0.1553(4) 1.2215(3) 0.68268(18) 0.0260(9) Uani 1 1 d . . . . . C32 C 0.0610(4) 1.2466(3) 0.7316(2) 0.0322(10) Uani 1 1 d . . . . . H32 H 0.0452 1.3178 0.7410 0.039 Uiso 1 1 calc R U . . . C33 C -0.0094(4) 1.1648(4) 0.7665(2) 0.0378(10) Uani 1 1 d . . . . . H33 H -0.0757 1.1803 0.8001 0.045 Uiso 1 1 calc R U . . . C34 C 0.0148(5) 1.0598(4) 0.7532(2) 0.0414(11) Uani 1 1 d . . . . . H34 H -0.0349 1.0050 0.7783 0.050 Uiso 1 1 calc R U . . . C35 C 0.1087(4) 1.0338(3) 0.7050(2) 0.0335(10) Uani 1 1 d . . . . . H35 H 0.1256 0.9622 0.6961 0.040 Uiso 1 1 calc R U . . . C36 C 0.1782(4) 1.1166(3) 0.66953(19) 0.0275(9) Uani 1 1 d . . . . . N4 N 0.2767(3) 1.1206(3) 0.61750(16) 0.0298(8) Uani 1 1 d . . . . . C37 C 0.2594(4) 1.3974(3) 0.6335(2) 0.0354(10) Uani 1 1 d . . . . . H37 H 0.3287 1.4157 0.5968 0.042 Uiso 1 1 calc R U . . . C38 C 0.3210(4) 1.4131(3) 0.6846(2) 0.0348(10) Uani 1 1 d . . . . . H38A H 0.2555 1.3976 0.7217 0.052 Uiso 1 1 calc R U . . . H38B H 0.3405 1.4883 0.6787 0.052 Uiso 1 1 calc R U . . . H38C H 0.4069 1.3634 0.6866 0.052 Uiso 1 1 calc R U . . . C39 C 0.1289(5) 1.4707(4) 0.6251(2) 0.0467(12) Uani 1 1 d . . . . . H39A H 0.0920 1.4518 0.5933 0.070 Uiso 1 1 calc R U . . . H39B H 0.1480 1.5464 0.6145 0.070 Uiso 1 1 calc R U . . . H39C H 0.0612 1.4620 0.6620 0.070 Uiso 1 1 calc R U . . . C40 C 0.3355(5) 1.0281(4) 0.5860(3) 0.0514(14) Uani 1 1 d . . . . . H40 H 0.4003 1.0587 0.5503 0.062 Uiso 1 1 calc R U . . . C41 C 0.4219(6) 0.9472(5) 0.6215(3) 0.0742(19) Uani 1 1 d . . . . . H41A H 0.4997 0.9800 0.6270 0.111 Uiso 1 1 calc R U . . . H41B H 0.4570 0.8851 0.6010 0.111 Uiso 1 1 calc R U . . . H41C H 0.3669 0.9224 0.6602 0.111 Uiso 1 1 calc R U . . . C42 C 0.2225(6) 0.9914(4) 0.5622(2) 0.0544(14) Uani 1 1 d . . . . . H42A H 0.1542 0.9617 0.5953 0.082 Uiso 1 1 calc R U . . . H42B H 0.2636 0.9351 0.5381 0.082 Uiso 1 1 calc R U . . . H42C H 0.1775 1.0536 0.5378 0.082 Uiso 1 1 calc R U . . . C1S C 0.1326(16) 0.7474(6) 0.7722(3) 0.119(5) Uani 1 1 d . . . . . C2S C 0.2556(8) 0.7202(4) 0.7218(4) 0.077(2) Uani 1 1 d . . . . . H2S H 0.3485 0.7013 0.7275 0.092 Uiso 1 1 calc R U . . . C3S C 0.2163(5) 0.7263(4) 0.6695(3) 0.0538(14) Uani 1 1 d . . . . . H3S H 0.2835 0.7115 0.6359 0.065 Uiso 1 1 calc R U . . . C4S C 0.0831(6) 0.7532(4) 0.6643(3) 0.0615(16) Uani 1 1 d . . . . . H4S H 0.0611 0.7563 0.6264 0.074 Uiso 1 1 calc R U . . . C5S C -0.0201(9) 0.7757(6) 0.7074(4) 0.089(2) Uani 1 1 d . . . . . H5S H -0.1121 0.7947 0.7005 0.106 Uiso 1 1 calc R U . . . C6S C 0.0072(8) 0.7714(5) 0.7561(5) 0.080(2) Uani 1 1 d . . . . . H6S H -0.0688 0.7865 0.7865 0.096 Uiso 1 1 calc R U . . . C7S C 0.1739(16) 0.7390(9) 0.8219(9) 0.245(9) Uani 1 1 d . . . . . H7S1 H 0.2744 0.7203 0.8160 0.367 Uiso 1 1 calc R U . . . H7S2 H 0.1304 0.6819 0.8510 0.367 Uiso 1 1 calc R U . . . H7S3 H 0.1483 0.8084 0.8364 0.367 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0450(2) 0.0436(2) 0.0553(3) -0.01288(19) -0.02467(18) 0.00659(16) Ag2 0.0366(3) 0.0335(2) 0.0497(3) 0.0035(2) -0.0118(2) -0.01164(19) Ag2A 0.0415(11) 0.0346(10) 0.0584(14) -0.0012(9) -0.0227(10) -0.0091(8) S1 0.0399(7) 0.0327(7) 0.0445(9) -0.0030(7) -0.0120(6) -0.0104(6) S1A 0.030(3) 0.039(3) 0.061(5) 0.000(3) -0.011(3) -0.006(2) C1 0.072(3) 0.046(3) 0.046(3) 0.003(2) -0.029(3) -0.022(3) C2 0.063(4) 0.089(5) 0.059(4) 0.021(3) -0.037(3) -0.022(3) C3 0.110(6) 0.084(5) 0.101(6) -0.048(5) -0.036(5) -0.014(4) C4 0.048(4) 0.058(4) 0.042(4) 0.000(3) -0.009(3) -0.003(3) C4A 0.056(15) 0.056(16) 0.046(16) 0.017(13) -0.014(12) -0.036(13) S2 0.0405(6) 0.0423(7) 0.0740(10) 0.0054(7) -0.0192(6) -0.0075(5) C5 0.079(4) 0.058(4) 0.043(4) -0.008(3) 0.001(3) -0.004(3) C6 0.183(10) 0.078(6) 0.137(8) -0.054(6) -0.048(7) -0.021(6) C7 0.377(19) 0.055(5) 0.214(13) -0.059(7) -0.182(13) 0.088(8) C8 0.324(19) 0.202(13) 0.128(10) -0.065(10) 0.142(12) -0.054(12) C9 0.042(2) 0.047(3) 0.037(3) -0.013(2) -0.016(2) 0.013(2) N1 0.0364(19) 0.033(2) 0.036(2) -0.0004(17) -0.0106(16) 0.0015(15) C10 0.049(3) 0.031(2) 0.037(3) -0.010(2) -0.010(2) 0.004(2) C11 0.054(3) 0.042(3) 0.046(3) -0.012(2) -0.007(2) -0.007(2) C12 0.070(4) 0.043(3) 0.064(4) -0.023(3) 0.004(3) -0.017(3) C13 0.108(5) 0.034(3) 0.061(4) -0.029(3) 0.028(4) -0.024(3) C14 0.110(5) 0.024(3) 0.035(3) -0.003(2) 0.007(3) 0.003(3) C15 0.071(3) 0.028(2) 0.032(3) -0.010(2) -0.008(2) 0.009(2) C16 0.040(2) 0.045(3) 0.033(3) 0.011(2) -0.010(2) -0.004(2) C17 0.060(3) 0.034(3) 0.051(3) 0.003(2) -0.018(3) 0.002(2) C18 0.056(3) 0.057(3) 0.043(3) -0.002(3) -0.016(2) 0.002(3) N2A 0.065(3) 0.044(2) 0.031(2) -0.007(2) -0.019(2) 0.021(2) C19A 0.042(9) 0.048(8) 0.054(9) 0.003(6) -0.025(7) 0.005(6) C20A 0.044(7) 0.111(15) 0.058(9) 0.030(8) -0.009(6) 0.029(8) C21A 0.066(3) 0.048(3) 0.048(3) 0.000(3) -0.025(3) -0.018(2) N2B 0.065(3) 0.044(2) 0.031(2) -0.007(2) -0.019(2) 0.021(2) C19B 0.031(8) 0.046(9) 0.043(8) 0.007(6) -0.007(6) -0.010(6) C20B 0.060(9) 0.048(9) 0.073(13) 0.002(8) -0.015(8) 0.018(7) C21B 0.066(3) 0.048(3) 0.048(3) 0.000(3) -0.025(3) -0.018(2) Ag3 0.02426(15) 0.03620(19) 0.0342(2) -0.00617(15) -0.00652(13) -0.00685(12) Ag4 0.02549(16) 0.03835(19) 0.0367(2) -0.00915(15) -0.01085(13) -0.00372(13) S3 0.0228(5) 0.0364(6) 0.0348(6) -0.0045(5) -0.0042(4) -0.0035(4) C22 0.032(2) 0.034(2) 0.036(3) 0.001(2) -0.0157(18) -0.0092(18) C23 0.026(2) 0.057(3) 0.042(3) 0.003(2) -0.0119(19) -0.010(2) C24 0.056(3) 0.031(3) 0.071(4) -0.001(2) -0.036(3) -0.004(2) C25 0.049(3) 0.041(3) 0.039(3) -0.002(2) -0.019(2) -0.004(2) S4 0.0248(5) 0.0419(6) 0.0328(6) -0.0109(5) -0.0083(4) -0.0036(4) C26 0.029(2) 0.036(2) 0.041(3) -0.010(2) -0.0149(18) -0.0020(17) C27 0.044(3) 0.092(4) 0.041(3) 0.002(3) -0.016(2) -0.001(3) C28 0.061(3) 0.076(4) 0.067(4) 0.010(3) -0.039(3) -0.034(3) C29 0.098(5) 0.050(4) 0.073(4) -0.014(3) -0.046(4) 0.004(3) C30 0.0239(19) 0.034(2) 0.036(3) -0.009(2) -0.0136(17) 0.0006(16) N3 0.0301(17) 0.0228(17) 0.035(2) -0.0039(16) -0.0148(15) -0.0041(13) C31 0.0255(18) 0.022(2) 0.034(2) -0.0081(18) -0.0123(17) -0.0007(15) C32 0.035(2) 0.025(2) 0.041(3) -0.013(2) -0.0124(19) 0.0013(17) C33 0.037(2) 0.040(3) 0.037(3) -0.013(2) -0.0034(19) -0.0037(19) C34 0.044(3) 0.033(2) 0.051(3) -0.007(2) -0.008(2) -0.014(2) C35 0.033(2) 0.023(2) 0.048(3) -0.013(2) -0.011(2) -0.0018(16) C36 0.0253(19) 0.027(2) 0.035(3) -0.0115(19) -0.0130(17) -0.0004(15) N4 0.0270(16) 0.0282(19) 0.038(2) -0.0130(16) -0.0121(15) 0.0015(14) C37 0.041(2) 0.026(2) 0.042(3) -0.006(2) -0.014(2) -0.0063(18) C38 0.032(2) 0.034(2) 0.044(3) -0.010(2) -0.0108(19) -0.0093(18) C39 0.052(3) 0.029(2) 0.065(4) -0.010(2) -0.024(3) -0.002(2) C40 0.053(3) 0.050(3) 0.057(4) -0.032(3) -0.020(3) 0.020(2) C41 0.058(3) 0.049(4) 0.113(6) -0.019(4) -0.016(4) 0.007(3) C42 0.083(4) 0.039(3) 0.051(3) -0.018(3) -0.025(3) -0.008(3) C1S 0.294(15) 0.046(4) 0.050(5) 0.029(3) -0.091(7) -0.090(7) C2S 0.098(5) 0.032(3) 0.105(6) 0.011(3) -0.037(5) -0.026(3) C3S 0.054(3) 0.026(3) 0.082(5) -0.012(3) -0.007(3) -0.009(2) C4S 0.057(3) 0.035(3) 0.096(5) -0.022(3) -0.006(3) -0.012(2) C5S 0.115(7) 0.052(4) 0.106(7) -0.015(5) -0.012(6) -0.038(4) C6S 0.082(5) 0.042(4) 0.109(7) -0.018(4) 0.018(5) -0.027(3) C7S 0.260(16) 0.087(8) 0.43(3) 0.013(12) -0.173(19) -0.087(9) _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 2.129(5) . ? Ag1 S1A 2.513(7) . ? Ag1 S2 2.5218(16) . ? Ag1 S1 2.5361(16) . ? Ag1 Ag2 3.0322(12) 2_675 ? Ag2 S1 2.3661(16) . ? Ag2 S2 2.3987(15) 2_675 ? Ag2 Ag1 3.0322(12) 2_675 ? Ag2 Ag2 3.2230(14) 2_675 ? Ag2A S2 2.312(2) 2_675 ? Ag2A S1A 2.361(7) . ? S1 C1 1.802(6) . ? S1A C1 1.711(7) . ? C1 C3 1.499(8) . ? C1 C2 1.522(7) . ? C1 C4 1.604(8) . ? C1 C4A 1.84(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? S2 C5 1.830(6) . ? S2 Ag2A 2.312(2) 2_675 ? S2 Ag2 2.3988(15) 2_675 ? C5 C7 1.445(10) . ? C5 C8 1.485(11) . ? C5 C6 1.496(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.363(5) . ? C9 N2A 1.366(6) . ? N1 C10 1.394(6) . ? N1 C16 1.475(6) . ? C10 C11 1.390(7) . ? C10 C15 1.392(6) . ? C11 C12 1.375(7) . ? C11 H11 0.9500 . ? C12 C13 1.398(9) . ? C12 H12 0.9500 . ? C13 C14 1.369(9) . ? C13 H13 0.9500 . ? C14 C15 1.385(7) . ? C14 H14 0.9500 . ? C15 N2A 1.394(7) . ? C16 C17 1.515(7) . ? C16 C18 1.517(7) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N2A C19A 1.551(14) . ? C19A C20A 1.22(2) . ? C19A C21A 1.503(16) . ? C19A H19A 1.0000 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C19B C20B 1.35(2) . ? C19B H19B 1.0000 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? Ag3 S3 2.3726(14) . ? Ag3 S4 2.3798(13) 2_686 ? Ag3 Ag4 3.1349(9) 2_686 ? Ag4 C30 2.148(4) . ? Ag4 S3 2.4991(14) . ? Ag4 S4 2.5010(13) . ? Ag4 Ag3 3.1349(9) 2_686 ? S3 C22 1.865(4) . ? C22 C23 1.514(6) . ? C22 C25 1.519(6) . ? C22 C24 1.521(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? S4 C26 1.860(5) . ? S4 Ag3 2.3798(14) 2_686 ? C26 C28 1.501(6) . ? C26 C29 1.521(7) . ? C26 C27 1.535(7) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N4 1.350(5) . ? C30 N3 1.353(5) . ? N3 C31 1.404(5) . ? N3 C37 1.473(5) . ? C31 C32 1.379(6) . ? C31 C36 1.393(5) . ? C32 C33 1.378(6) . ? C32 H32 0.9500 . ? C33 C34 1.395(6) . ? C33 H33 0.9500 . ? C34 C35 1.368(6) . ? C34 H34 0.9500 . ? C35 C36 1.387(6) . ? C35 H35 0.9500 . ? C36 N4 1.398(5) . ? N4 C40 1.480(5) . ? C37 C39 1.495(6) . ? C37 C38 1.514(6) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.468(7) . ? C40 C42 1.529(7) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C1S C7S 1.294(16) . ? C1S C6S 1.353(13) . ? C1S C2S 1.564(14) . ? C2S C3S 1.346(9) . ? C2S H2S 0.9500 . ? C3S C4S 1.343(7) . ? C3S H3S 0.9500 . ? C4S C5S 1.323(9) . ? C4S H4S 0.9500 . ? C5S C6S 1.215(11) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 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 C9 Ag1 S1A 94.55(18) . . ? C9 Ag1 S2 130.66(13) . . ? S1A Ag1 S2 134.52(13) . . ? C9 Ag1 S1 140.52(13) . . ? S2 Ag1 S1 88.75(5) . . ? C9 Ag1 Ag2 117.20(13) . 2_675 ? S2 Ag1 Ag2 50.15(4) . 2_675 ? S1 Ag1 Ag2 84.23(4) . 2_675 ? S1 Ag2 S2 172.14(6) . 2_675 ? S1 Ag2 Ag1 129.44(5) . 2_675 ? S2 Ag2 Ag1 53.81(4) 2_675 2_675 ? S1 Ag2 Ag2 82.82(5) . 2_675 ? S2 Ag2 Ag2 104.70(5) 2_675 2_675 ? Ag1 Ag2 Ag2 66.71(3) 2_675 2_675 ? S2 Ag2A S1A 174.47(16) 2_675 . ? C1 S1 Ag2 106.67(19) . . ? C1 S1 Ag1 109.69(16) . . ? Ag2 S1 Ag1 89.16(5) . . ? C1 S1A Ag2A 106.4(3) . . ? C1 S1A Ag1 114.1(3) . . ? Ag2A S1A Ag1 95.0(3) . . ? C3 C1 C2 112.3(5) . . ? C3 C1 C4 104.0(5) . . ? C2 C1 C4 109.8(4) . . ? C3 C1 S1A 132.8(5) . . ? C2 C1 S1A 111.9(4) . . ? C3 C1 S1 112.3(4) . . ? C2 C1 S1 107.4(4) . . ? C4 C1 S1 111.1(4) . . ? C3 C1 C4A 84.0(9) . . ? C2 C1 C4A 100.1(9) . . ? S1A C1 C4A 103.6(9) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C4A H4A1 109.5 . . ? C1 C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C1 C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C5 S2 Ag2A 101.5(2) . 2_675 ? C5 S2 Ag2 106.1(2) . 2_675 ? C5 S2 Ag1 111.4(2) . . ? Ag2A S2 Ag1 98.21(8) 2_675 . ? Ag2 S2 Ag1 76.04(5) 2_675 . ? C7 C5 C8 117.9(9) . . ? C7 C5 C6 108.2(8) . . ? C8 C5 C6 104.9(9) . . ? C7 C5 S2 108.4(5) . . ? C8 C5 S2 106.4(6) . . ? C6 C5 S2 111.0(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 N2A 105.4(4) . . ? N1 C9 Ag1 124.3(4) . . ? N2A C9 Ag1 130.3(3) . . ? C9 N1 C10 111.0(4) . . ? C9 N1 C16 122.2(4) . . ? C10 N1 C16 126.7(4) . . ? C11 C10 C15 120.8(5) . . ? C11 C10 N1 132.8(4) . . ? C15 C10 N1 106.4(4) . . ? C12 C11 C10 117.9(5) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? C11 C12 C13 120.5(6) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 122.1(5) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 117.3(6) . . ? C13 C14 H14 121.4 . . ? C15 C14 H14 121.4 . . ? C14 C15 C10 121.3(5) . . ? C14 C15 N2A 132.6(5) . . ? C10 C15 N2A 106.1(4) . . ? N1 C16 C17 110.5(4) . . ? N1 C16 C18 111.8(4) . . ? C17 C16 C18 114.9(4) . . ? N1 C16 H16 106.3 . . ? C17 C16 H16 106.3 . . ? C18 C16 H16 106.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C9 N2A C15 111.1(4) . . ? C9 N2A C19A 114.2(9) . . ? C15 N2A C19A 134.1(9) . . ? C20A C19A C21A 136.7(13) . . ? C20A C19A N2A 117.8(13) . . ? C21A C19A N2A 105.5(10) . . ? C20A C19A H19A 90.5 . . ? C21A C19A H19A 90.5 . . ? N2A C19A H19A 90.5 . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19A C21A H21A 109.5 . . ? C19A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C19A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20B C19B H19B 98.9 . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? S3 Ag3 S4 169.84(4) . 2_686 ? S3 Ag3 Ag4 136.47(3) . 2_686 ? S4 Ag3 Ag4 51.76(3) 2_686 2_686 ? C30 Ag4 S3 128.95(11) . . ? C30 Ag4 S4 129.12(11) . . ? S3 Ag4 S4 101.87(4) . . ? C30 Ag4 Ag3 115.87(11) . 2_686 ? S3 Ag4 Ag3 94.65(3) . 2_686 ? S4 Ag4 Ag3 48.36(3) . 2_686 ? C22 S3 Ag3 102.73(14) . . ? C22 S3 Ag4 107.21(14) . . ? Ag3 S3 Ag4 89.15(4) . . ? C23 C22 C25 110.7(4) . . ? C23 C22 C24 109.8(4) . . ? C25 C22 C24 109.5(4) . . ? C23 C22 S3 111.2(3) . . ? C25 C22 S3 107.7(3) . . ? C24 C22 S3 107.8(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 S4 Ag3 103.00(14) . 2_686 ? C26 S4 Ag4 110.30(14) . . ? Ag3 S4 Ag4 79.88(3) 2_686 . ? C28 C26 C29 111.2(4) . . ? C28 C26 C27 108.1(4) . . ? C29 C26 C27 107.1(4) . . ? C28 C26 S4 109.9(3) . . ? C29 C26 S4 108.5(3) . . ? C27 C26 S4 112.1(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C30 N3 105.5(4) . . ? N4 C30 Ag4 130.9(3) . . ? N3 C30 Ag4 123.6(3) . . ? C30 N3 C31 111.2(3) . . ? C30 N3 C37 122.1(4) . . ? C31 N3 C37 126.6(3) . . ? C32 C31 C36 120.6(4) . . ? C32 C31 N3 133.4(4) . . ? C36 C31 N3 106.0(3) . . ? C33 C32 C31 117.8(4) . . ? C33 C32 H32 121.1 . . ? C31 C32 H32 121.1 . . ? C32 C33 C34 121.3(4) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 121.4(4) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C34 C35 C36 117.2(4) . . ? C34 C35 H35 121.4 . . ? C36 C35 H35 121.4 . . ? C35 C36 C31 121.7(4) . . ? C35 C36 N4 132.8(4) . . ? C31 C36 N4 105.5(3) . . ? C30 N4 C36 111.9(3) . . ? C30 N4 C40 122.3(4) . . ? C36 N4 C40 125.8(4) . . ? N3 C37 C39 111.3(3) . . ? N3 C37 C38 110.9(3) . . ? C39 C37 C38 114.5(4) . . ? N3 C37 H37 106.5 . . ? C39 C37 H37 106.5 . . ? C38 C37 H37 106.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 N4 110.3(4) . . ? C41 C40 C42 119.2(5) . . ? N4 C40 C42 109.8(4) . . ? C41 C40 H40 105.5 . . ? N4 C40 H40 105.5 . . ? C42 C40 H40 105.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C7S C1S C6S 133.4(15) . . ? C7S C1S C2S 111.3(14) . . ? C6S C1S C2S 115.2(6) . . ? C3S C2S C1S 113.1(7) . . ? C3S C2S H2S 123.4 . . ? C1S C2S H2S 123.4 . . ? C4S C3S C2S 120.7(7) . . ? C4S C3S H3S 119.7 . . ? C2S C3S H3S 119.7 . . ? C5S C4S C3S 125.6(8) . . ? C5S C4S H4S 117.2 . . ? C3S C4S H4S 117.2 . . ? C6S C5S C4S 117.6(9) . . ? C6S C5S H5S 121.2 . . ? C4S C5S H5S 121.2 . . ? C5S C6S C1S 127.8(9) . . ? C5S C6S H6S 116.1 . . ? C1S C6S H6S 116.1 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag2A S1A C1 C3 -37.0(8) . . . . ? Ag1 S1A C1 C3 -140.4(6) . . . . ? Ag2A S1A C1 C2 164.5(4) . . . . ? Ag1 S1A C1 C2 61.1(6) . . . . ? Ag2A S1A C1 C4 -99.1(5) . . . . ? Ag1 S1A C1 C4 157.5(6) . . . . ? Ag2A S1A C1 S1 63.8(3) . . . . ? Ag1 S1A C1 S1 -39.6(3) . . . . ? Ag2A S1A C1 C4A 57.6(10) . . . . ? Ag1 S1A C1 C4A -45.8(10) . . . . ? Ag2 S1 C1 C3 71.3(4) . . . . ? Ag1 S1 C1 C3 166.6(4) . . . . ? Ag2 S1 C1 C2 -164.7(3) . . . . ? Ag1 S1 C1 C2 -69.5(4) . . . . ? Ag2 S1 C1 C4 -44.7(4) . . . . ? Ag1 S1 C1 C4 50.5(4) . . . . ? Ag2 S1 C1 S1A -57.5(3) . . . . ? Ag1 S1 C1 S1A 37.7(3) . . . . ? Ag2 S1 C1 C4A 112.1(15) . . . . ? Ag1 S1 C1 C4A -152.7(15) . . . . ? Ag2A S2 C5 C7 -174.0(7) 2_675 . . . ? Ag2 S2 C5 C7 163.3(7) 2_675 . . . ? Ag1 S2 C5 C7 82.3(8) . . . . ? Ag2A S2 C5 C8 -46.3(8) 2_675 . . . ? Ag2 S2 C5 C8 -69.0(8) 2_675 . . . ? Ag1 S2 C5 C8 -149.9(8) . . . . ? Ag2A S2 C5 C6 67.3(5) 2_675 . . . ? Ag2 S2 C5 C6 44.6(6) 2_675 . . . ? Ag1 S2 C5 C6 -36.3(6) . . . . ? N2A C9 N1 C10 -1.4(5) . . . . ? Ag1 C9 N1 C10 176.2(3) . . . . ? N2A C9 N1 C16 -179.7(4) . . . . ? Ag1 C9 N1 C16 -2.1(6) . . . . ? C9 N1 C10 C11 -176.4(5) . . . . ? C16 N1 C10 C11 1.8(8) . . . . ? C9 N1 C10 C15 0.9(5) . . . . ? C16 N1 C10 C15 179.1(4) . . . . ? C15 C10 C11 C12 1.6(7) . . . . ? N1 C10 C11 C12 178.6(5) . . . . ? C10 C11 C12 C13 -1.5(7) . . . . ? C11 C12 C13 C14 1.1(8) . . . . ? C12 C13 C14 C15 -0.7(8) . . . . ? C13 C14 C15 C10 0.8(7) . . . . ? C13 C14 C15 N2A -177.9(5) . . . . ? C11 C10 C15 C14 -1.3(7) . . . . ? N1 C10 C15 C14 -179.0(4) . . . . ? C11 C10 C15 N2A 177.7(4) . . . . ? N1 C10 C15 N2A 0.0(5) . . . . ? C9 N1 C16 C17 106.5(5) . . . . ? C10 N1 C16 C17 -71.5(6) . . . . ? C9 N1 C16 C18 -124.1(5) . . . . ? C10 N1 C16 C18 57.9(6) . . . . ? N1 C9 N2A C15 1.4(5) . . . . ? Ag1 C9 N2A C15 -176.0(3) . . . . ? N1 C9 N2A C19A 173.9(7) . . . . ? Ag1 C9 N2A C19A -3.5(8) . . . . ? C14 C15 N2A C9 177.9(5) . . . . ? C10 C15 N2A C9 -0.9(5) . . . . ? C14 C15 N2A C19A 7.5(11) . . . . ? C10 C15 N2A C19A -171.4(9) . . . . ? C9 N2A C19A C20A 78.1(15) . . . . ? C15 N2A C19A C20A -111.7(14) . . . . ? C9 N2A C19A C21A -103.5(12) . . . . ? C15 N2A C19A C21A 66.8(15) . . . . ? Ag3 S3 C22 C23 -37.5(3) . . . . ? Ag4 S3 C22 C23 55.6(3) . . . . ? Ag3 S3 C22 C25 84.0(3) . . . . ? Ag4 S3 C22 C25 177.0(3) . . . . ? Ag3 S3 C22 C24 -158.0(3) . . . . ? Ag4 S3 C22 C24 -64.9(3) . . . . ? Ag3 S4 C26 C28 -66.8(4) 2_686 . . . ? Ag4 S4 C26 C28 -150.6(3) . . . . ? Ag3 S4 C26 C29 171.5(3) 2_686 . . . ? Ag4 S4 C26 C29 87.6(4) . . . . ? Ag3 S4 C26 C27 53.4(4) 2_686 . . . ? Ag4 S4 C26 C27 -30.5(4) . . . . ? N4 C30 N3 C31 0.1(4) . . . . ? Ag4 C30 N3 C31 -179.1(3) . . . . ? N4 C30 N3 C37 177.6(3) . . . . ? Ag4 C30 N3 C37 -1.6(5) . . . . ? C30 N3 C31 C32 -179.2(4) . . . . ? C37 N3 C31 C32 3.5(7) . . . . ? C30 N3 C31 C36 0.1(4) . . . . ? C37 N3 C31 C36 -177.3(3) . . . . ? C36 C31 C32 C33 -0.3(6) . . . . ? N3 C31 C32 C33 178.8(4) . . . . ? C31 C32 C33 C34 0.8(6) . . . . ? C32 C33 C34 C35 -0.4(7) . . . . ? C33 C34 C35 C36 -0.4(7) . . . . ? C34 C35 C36 C31 0.9(6) . . . . ? C34 C35 C36 N4 -178.7(4) . . . . ? C32 C31 C36 C35 -0.6(6) . . . . ? N3 C31 C36 C35 -179.9(4) . . . . ? C32 C31 C36 N4 179.1(4) . . . . ? N3 C31 C36 N4 -0.2(4) . . . . ? N3 C30 N4 C36 -0.3(4) . . . . ? Ag4 C30 N4 C36 178.9(3) . . . . ? N3 C30 N4 C40 -179.6(3) . . . . ? Ag4 C30 N4 C40 -0.4(6) . . . . ? C35 C36 N4 C30 180.0(4) . . . . ? C31 C36 N4 C30 0.3(4) . . . . ? C35 C36 N4 C40 -0.7(7) . . . . ? C31 C36 N4 C40 179.6(4) . . . . ? C30 N3 C37 C39 118.2(4) . . . . ? C31 N3 C37 C39 -64.7(5) . . . . ? C30 N3 C37 C38 -113.0(4) . . . . ? C31 N3 C37 C38 64.0(5) . . . . ? C30 N4 C40 C41 111.1(5) . . . . ? C36 N4 C40 C41 -68.1(6) . . . . ? C30 N4 C40 C42 -115.5(5) . . . . ? C36 N4 C40 C42 65.2(6) . . . . ? C7S C1S C2S C3S 178.9(7) . . . . ? C6S C1S C2S C3S 0.8(7) . . . . ? C1S C2S C3S C4S -0.2(7) . . . . ? C2S C3S C4S C5S 0.0(9) . . . . ? C3S C4S C5S C6S -0.4(10) . . . . ? C4S C5S C6S C1S 1.1(11) . . . . ? C7S C1S C6S C5S -179.0(9) . . . . ? C2S C1S C6S C5S -1.3(10) . . . . ? _refine_diff_density_max 1.728 _refine_diff_density_min -1.243 _refine_diff_density_rms 0.121 _shelxl_version_number 2013-3 _database_code_depnum_ccdc_archive 'CCDC 960482' ####################################################################### # # 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_6 _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H54 Ag5 S6, C22 H40 Ag N4, 0.34(C4 H8 O)' _chemical_formula_sum 'C47.38 H96.75 Ag6 N4 O0.34 S6' _chemical_formula_weight 1567.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_H-M_alt 'C 2' _space_group_name_Hall 'C 2y' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 29.293(11) _cell_length_b 12.976(5) _cell_length_c 19.198(8) _cell_angle_alpha 90 _cell_angle_beta 98.423(7) _cell_angle_gamma 90 _cell_volume 7219(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9974 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 21.98 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_F_000 3159 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.115 _exptl_absorpt_coefficient_mu 1.798 _shelx_estimated_absorpt_T_min 0.704 _shelx_estimated_absorpt_T_max 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6796 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 101010 _diffrn_reflns_av_unetI/netI 0.0579 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.720 _diffrn_reflns_theta_max 28.849 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 18753 _reflns_number_gt 14020 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.914 _reflns_Friedel_fraction_max 0.987 _reflns_Friedel_fraction_full 0.999 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. These statistics refer to single and composite reflections containing twin component 1 only. ; _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution XS _computing_structure_refinement SHELXL-2012 _computing_molecular_graphics Mercury _computing_publication_material cif2tables.py _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+0.7571P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00124(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.31(5) _chemical_absolute_configuration ? _refine_ls_number_reflns 18753 _refine_ls_number_parameters 638 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1648 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.16760(3) 0.45467(7) 0.21420(4) 0.0407(2) Uani 1 1 d . . . . . Ag2 Ag 0.25990(3) 0.43121(7) 0.13718(5) 0.0441(2) Uani 1 1 d . . . . . Ag3 Ag 0.22720(3) 0.65945(7) 0.26715(5) 0.0442(2) Uani 1 1 d . . . . . Ag4 Ag 0.24091(3) 0.36139(7) 0.33640(5) 0.0432(2) Uani 1 1 d . . . . . Ag5 Ag 0.31801(3) 0.51366(7) 0.28078(4) 0.0401(2) Uani 1 1 d . . . . . S1 S 0.18121(10) 0.4015(2) 0.09377(15) 0.0406(6) Uani 1 1 d . . . . . S2 S 0.14716(11) 0.6383(2) 0.23090(14) 0.0402(6) Uani 1 1 d . . . . . S3 S 0.16224(10) 0.3192(2) 0.30384(14) 0.0400(6) Uani 1 1 d . . . . . S4 S 0.34007(10) 0.4600(2) 0.16659(14) 0.0391(6) Uani 1 1 d . . . . . S5 S 0.30539(11) 0.6987(2) 0.30606(15) 0.0423(6) Uani 1 1 d . . . . . S6 S 0.31944(10) 0.3918(2) 0.38031(14) 0.0404(6) Uani 1 1 d . . . . . C1 C 0.1652(4) 0.5109(10) 0.0312(6) 0.041(2) Uani 1 1 d . . . . . C2 C 0.1742(5) 0.4790(11) -0.0406(7) 0.060(4) Uani 1 1 d . . . . . H2A H 0.1638 0.5336 -0.0746 0.089 Uiso 1 1 calc R U . . . H2B H 0.1574 0.4153 -0.0545 0.089 Uiso 1 1 calc R U . . . H2C H 0.2074 0.4675 -0.0397 0.089 Uiso 1 1 calc R U . . . C3 C 0.1141(5) 0.5271(11) 0.0299(7) 0.055(3) Uani 1 1 d . . . . . H3A H 0.1087 0.5630 0.0728 0.082 Uiso 1 1 calc R U . . . H3B H 0.0984 0.4602 0.0272 0.082 Uiso 1 1 calc R U . . . H3C H 0.1019 0.5686 -0.0113 0.082 Uiso 1 1 calc R U . . . C4 C 0.1917(4) 0.6079(9) 0.0558(6) 0.045(3) Uani 1 1 d . . . . . H4A H 0.2248 0.5930 0.0634 0.067 Uiso 1 1 calc R U . . . H4B H 0.1822 0.6317 0.0999 0.067 Uiso 1 1 calc R U . . . H4C H 0.1851 0.6617 0.0199 0.067 Uiso 1 1 calc R U . . . C5 C 0.1210(4) 0.6567(9) 0.3131(6) 0.040(2) Uani 1 1 d . . . . . C6 C 0.0746(5) 0.6107(15) 0.3008(8) 0.065(4) Uani 1 1 d . . . . . H6A H 0.0594 0.6209 0.3425 0.098 Uiso 1 1 calc R U . . . H6B H 0.0771 0.5368 0.2916 0.098 Uiso 1 1 calc R U . . . H6C H 0.0563 0.6439 0.2600 0.098 Uiso 1 1 calc R U . . . C7 C 0.1481(4) 0.6022(11) 0.3772(6) 0.048(3) Uani 1 1 d . . . . . H7A H 0.1300 0.6036 0.4163 0.071 Uiso 1 1 calc R U . . . H7B H 0.1775 0.6377 0.3911 0.071 Uiso 1 1 calc R U . . . H7C H 0.1539 0.5306 0.3650 0.071 Uiso 1 1 calc R U . . . C8 C 0.1192(5) 0.7718(11) 0.3269(7) 0.058(3) Uani 1 1 d . . . . . H8A H 0.0983 0.8048 0.2889 0.087 Uiso 1 1 calc R U . . . H8B H 0.1502 0.8011 0.3289 0.087 Uiso 1 1 calc R U . . . H8C H 0.1080 0.7836 0.3719 0.087 Uiso 1 1 calc R U . . . C9 C 0.1631(4) 0.1903(9) 0.2625(6) 0.041(2) Uani 1 1 d . . . . . C10 C 0.1630(7) 0.1105(13) 0.3201(8) 0.075(5) Uani 1 1 d . . . . . H10A H 0.1686 0.0421 0.3014 0.113 Uiso 1 1 calc R U . . . H10B H 0.1330 0.1111 0.3370 0.113 Uiso 1 1 calc R U . . . H10C H 0.1874 0.1268 0.3592 0.113 Uiso 1 1 calc R U . . . C11 C 0.1186(5) 0.1807(12) 0.2081(8) 0.061(4) Uani 1 1 d . . . . . H11A H 0.1182 0.1135 0.1847 0.091 Uiso 1 1 calc R U . . . H11B H 0.1180 0.2356 0.1730 0.091 Uiso 1 1 calc R U . . . H11C H 0.0915 0.1869 0.2324 0.091 Uiso 1 1 calc R U . . . C12 C 0.2043(5) 0.1754(11) 0.2231(7) 0.053(3) Uani 1 1 d . . . . . H12A H 0.2329 0.1886 0.2551 0.079 Uiso 1 1 calc R U . . . H12B H 0.2019 0.2237 0.1834 0.079 Uiso 1 1 calc R U . . . H12C H 0.2044 0.1046 0.2054 0.079 Uiso 1 1 calc R U . . . C13 C 0.3663(4) 0.3271(9) 0.1696(6) 0.044(3) Uani 1 1 d . . . . . C14 C 0.3377(6) 0.2501(11) 0.2039(10) 0.070(4) Uani 1 1 d . . . . . H14A H 0.3063 0.2478 0.1777 0.105 Uiso 1 1 calc R U . . . H14B H 0.3363 0.2711 0.2526 0.105 Uiso 1 1 calc R U . . . H14C H 0.3518 0.1817 0.2035 0.105 Uiso 1 1 calc R U . . . C15 C 0.3671(9) 0.2938(15) 0.0956(8) 0.102(8) Uani 1 1 d . . . . . H15A H 0.3802 0.2243 0.0954 0.153 Uiso 1 1 calc R U . . . H15B H 0.3861 0.3417 0.0727 0.153 Uiso 1 1 calc R U . . . H15C H 0.3356 0.2933 0.0701 0.153 Uiso 1 1 calc R U . . . C16 C 0.4158(6) 0.3416(15) 0.2155(10) 0.080(5) Uani 1 1 d . . . . . H16A H 0.4331 0.2769 0.2161 0.120 Uiso 1 1 calc R U . . . H16B H 0.4121 0.3606 0.2638 0.120 Uiso 1 1 calc R U . . . H16C H 0.4327 0.3962 0.1948 0.120 Uiso 1 1 calc R U . . . C17 C 0.3238(5) 0.7804(10) 0.2354(7) 0.051(3) Uani 1 1 d . . . . . C18 C 0.3018(6) 0.7428(11) 0.1624(7) 0.065(4) Uani 1 1 d . . . . . H18A H 0.3139 0.7834 0.1261 0.097 Uiso 1 1 calc R U . . . H18B H 0.2682 0.7512 0.1575 0.097 Uiso 1 1 calc R U . . . H18C H 0.3093 0.6699 0.1570 0.097 Uiso 1 1 calc R U . . . C19 C 0.3057(8) 0.8891(12) 0.2440(9) 0.082(5) Uani 1 1 d . . . . . H19A H 0.3186 0.9159 0.2904 0.123 Uiso 1 1 calc R U . . . H19B H 0.2720 0.8875 0.2397 0.123 Uiso 1 1 calc R U . . . H19C H 0.3149 0.9338 0.2073 0.123 Uiso 1 1 calc R U . . . C20 C 0.3743(6) 0.7739(19) 0.2394(12) 0.100(7) Uani 1 1 d . . . . . H20A H 0.3835 0.8032 0.1965 0.150 Uiso 1 1 calc R U . . . H20B H 0.3839 0.7016 0.2439 0.150 Uiso 1 1 calc R U . . . H20C H 0.3890 0.8127 0.2804 0.150 Uiso 1 1 calc R U . . . C21 C 0.3176(4) 0.4649(11) 0.4639(5) 0.045(3) Uani 1 1 d . . . . . C22 C 0.2777(4) 0.5392(10) 0.4587(6) 0.047(3) Uani 1 1 d . . . . . H22A H 0.2486 0.5007 0.4524 0.071 Uiso 1 1 calc R U . . . H22B H 0.2786 0.5851 0.4184 0.071 Uiso 1 1 calc R U . . . H22C H 0.2801 0.5802 0.5020 0.071 Uiso 1 1 calc R U . . . C23 C 0.3132(5) 0.3876(15) 0.5216(7) 0.067(4) Uani 1 1 d . . . . . H23A H 0.3142 0.4237 0.5666 0.100 Uiso 1 1 calc R U . . . H23B H 0.3386 0.3381 0.5247 0.100 Uiso 1 1 calc R U . . . H23C H 0.2837 0.3509 0.5107 0.100 Uiso 1 1 calc R U . . . C24 C 0.3622(4) 0.5258(17) 0.4795(8) 0.075(5) Uani 1 1 d . . . . . H24A H 0.3603 0.5734 0.5186 0.112 Uiso 1 1 calc R U . . . H24B H 0.3671 0.5650 0.4376 0.112 Uiso 1 1 calc R U . . . H24C H 0.3881 0.4782 0.4923 0.112 Uiso 1 1 calc R U . . . Ag6 Ag 0.0000 0.49669(10) 0.5000 0.0393(3) Uani 1 2 d S T P . . N1 N 0.1011(3) 0.5628(7) 0.5590(5) 0.039(2) Uani 1 1 d . . . . . N2 N 0.1007(3) 0.4178(7) 0.5043(5) 0.038(2) Uani 1 1 d . . . . . C25 C 0.0731(4) 0.4935(10) 0.5217(6) 0.040(2) Uani 1 1 d . . . . . C26 C 0.1463(4) 0.5310(9) 0.5661(6) 0.041(2) Uani 1 1 d . . . . . C27 C 0.1464(4) 0.4373(9) 0.5325(5) 0.037(2) Uani 1 1 d . . . . . C28 C 0.0858(4) 0.6625(11) 0.5851(7) 0.050(3) Uani 1 1 d . . . . . H28 H 0.1139 0.6963 0.6111 0.060 Uiso 1 1 calc R U . . . C29 C 0.0535(6) 0.6428(13) 0.6385(8) 0.069(4) Uani 1 1 d . . . . . H29A H 0.0485 0.7071 0.6630 0.103 Uiso 1 1 calc R U . . . H29B H 0.0672 0.5914 0.6727 0.103 Uiso 1 1 calc R U . . . H29C H 0.0239 0.6170 0.6143 0.103 Uiso 1 1 calc R U . . . C30 C 0.0684(5) 0.7316(10) 0.5259(8) 0.053(3) Uani 1 1 d . . . . . H30A H 0.0945 0.7617 0.5065 0.080 Uiso 1 1 calc R U . . . H30B H 0.0499 0.7867 0.5427 0.080 Uiso 1 1 calc R U . . . H30C H 0.0492 0.6920 0.4891 0.080 Uiso 1 1 calc R U . . . C31 C 0.1850(4) 0.5918(11) 0.6038(7) 0.051(3) Uani 1 1 d . . . . . H31A H 0.1848 0.6611 0.5833 0.077 Uiso 1 1 calc R U . . . H31B H 0.2143 0.5577 0.5992 0.077 Uiso 1 1 calc R U . . . H31C H 0.1816 0.5970 0.6537 0.077 Uiso 1 1 calc R U . . . C32 C 0.1853(4) 0.3636(12) 0.5254(7) 0.052(3) Uani 1 1 d . . . . . H32A H 0.1820 0.3018 0.5537 0.077 Uiso 1 1 calc R U . . . H32B H 0.2149 0.3970 0.5422 0.077 Uiso 1 1 calc R U . . . H32C H 0.1842 0.3441 0.4759 0.077 Uiso 1 1 calc R U . . . C33 C 0.0867(4) 0.3225(10) 0.4685(6) 0.043(3) Uani 1 1 d . . . . . H33 H 0.1155 0.2898 0.4564 0.051 Uiso 1 1 calc R U . . . C34 C 0.0562(4) 0.3391(12) 0.4015(6) 0.051(3) Uani 1 1 d . . . . . H34A H 0.0267 0.3674 0.4110 0.077 Uiso 1 1 calc R U . . . H34B H 0.0508 0.2733 0.3766 0.077 Uiso 1 1 calc R U . . . H34C H 0.0707 0.3876 0.3724 0.077 Uiso 1 1 calc R U . . . C35 C 0.0673(5) 0.2485(10) 0.5192(8) 0.057(3) Uani 1 1 d . . . . . H35A H 0.0903 0.2381 0.5612 0.086 Uiso 1 1 calc R U . . . H35B H 0.0601 0.1822 0.4958 0.086 Uiso 1 1 calc R U . . . H35C H 0.0392 0.2779 0.5331 0.086 Uiso 1 1 calc R U . . . Ag7 Ag 0.5000 0.50578(11) 0.0000 0.0395(3) Uani 1 2 d S T P . . N3 N 0.3972(3) 0.5688(8) -0.0065(5) 0.0369(19) Uani 1 1 d . . . . . N4 N 0.4035(3) 0.4424(8) -0.0758(4) 0.0373(19) Uani 1 1 d . . . . . C36 C 0.4274(3) 0.5041(10) -0.0307(5) 0.038(2) Uani 1 1 d . . . . . C37 C 0.3526(4) 0.5455(9) -0.0385(6) 0.040(2) Uani 1 1 d . . . . . C38 C 0.3567(4) 0.4645(9) -0.0807(6) 0.039(2) Uani 1 1 d . . . . . C39 C 0.4081(4) 0.6554(12) 0.0428(7) 0.050(3) Uani 1 1 d . . . . . H39 H 0.3783 0.6786 0.0573 0.061 Uiso 1 1 calc R U . . . C40 C 0.4403(5) 0.6213(12) 0.1116(7) 0.055(3) Uani 1 1 d . . . . . H40A H 0.4301 0.5543 0.1272 0.083 Uiso 1 1 calc R U . . . H40B H 0.4387 0.6726 0.1487 0.083 Uiso 1 1 calc R U . . . H40C H 0.4722 0.6158 0.1020 0.083 Uiso 1 1 calc R U . . . C41 C 0.4268(5) 0.7445(11) 0.0062(8) 0.062(4) Uani 1 1 d . . . . . H41A H 0.4485 0.7191 -0.0241 0.093 Uiso 1 1 calc R U . . . H41B H 0.4427 0.7921 0.0412 0.093 Uiso 1 1 calc R U . . . H41C H 0.4013 0.7805 -0.0226 0.093 Uiso 1 1 calc R U . . . C42 C 0.3106(4) 0.6031(11) -0.0227(7) 0.047(3) Uani 1 1 d . . . . . H42A H 0.2839 0.5841 -0.0572 0.071 Uiso 1 1 calc R U . . . H42B H 0.3161 0.6774 -0.0252 0.071 Uiso 1 1 calc R U . . . H42C H 0.3046 0.5851 0.0247 0.071 Uiso 1 1 calc R U . . . C43 C 0.3201(4) 0.4050(11) -0.1274(8) 0.056(3) Uani 1 1 d . . . . . H43A H 0.2895 0.4268 -0.1181 0.084 Uiso 1 1 calc R U . . . H43B H 0.3240 0.3311 -0.1177 0.084 Uiso 1 1 calc R U . . . H43C H 0.3228 0.4183 -0.1769 0.084 Uiso 1 1 calc R U . . . C44 C 0.4218(4) 0.3582(10) -0.1164(6) 0.048(3) Uani 1 1 d . . . . . H44 H 0.3959 0.3321 -0.1518 0.057 Uiso 1 1 calc R U . . . C45 C 0.4600(5) 0.4032(15) -0.1577(8) 0.072(5) Uani 1 1 d . . . . . H45A H 0.4616 0.4782 -0.1516 0.107 Uiso 1 1 calc R U . . . H45B H 0.4522 0.3868 -0.2078 0.107 Uiso 1 1 calc R U . . . H45C H 0.4899 0.3728 -0.1392 0.107 Uiso 1 1 calc R U . . . C46 C 0.4396(9) 0.2731(14) -0.0731(11) 0.096(7) Uani 1 1 d . . . . . H46A H 0.4625 0.2982 -0.0345 0.144 Uiso 1 1 calc R U . . . H46B H 0.4542 0.2237 -0.1015 0.144 Uiso 1 1 calc R U . . . H46C H 0.4143 0.2393 -0.0538 0.144 Uiso 1 1 calc R U . . . O1S O 0.0356(5) 0.0190(18) 0.3507(11) 0.052(6) Uani 0.344(15) 1 d D U P . . C1S C 0.0143(7) -0.059(2) 0.388(2) 0.071(12) Uani 0.344(15) 1 d D U P . . H1S1 H 0.0316 -0.0680 0.4355 0.085 Uiso 0.344(15) 1 calc R U P . . H1S2 H 0.0141 -0.1254 0.3623 0.085 Uiso 0.344(15) 1 calc R U P . . C2S C -0.0329(7) -0.025(3) 0.3915(17) 0.060(10) Uani 0.344(15) 1 d D U P . . H2S1 H -0.0355 0.0017 0.4390 0.072 Uiso 0.344(15) 1 calc R U P . . H2S2 H -0.0549 -0.0831 0.3809 0.072 Uiso 0.344(15) 1 calc R U P . . C3S C -0.0427(7) 0.059(2) 0.3367(16) 0.058(8) Uani 0.344(15) 1 d D U P . . H3S1 H -0.0699 0.0412 0.3019 0.069 Uiso 0.344(15) 1 calc R U P . . H3S2 H -0.0485 0.1254 0.3591 0.069 Uiso 0.344(15) 1 calc R U P . . C4S C -0.0011(8) 0.065(2) 0.3029(12) 0.054(7) Uani 0.344(15) 1 d D U P . . H4S1 H -0.0056 0.0270 0.2576 0.065 Uiso 0.344(15) 1 calc R U P . . H4S2 H 0.0063 0.1376 0.2936 0.065 Uiso 0.344(15) 1 calc R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0464(4) 0.0375(4) 0.0380(4) -0.0013(3) 0.0050(3) -0.0009(4) Ag2 0.0455(5) 0.0438(5) 0.0423(4) 0.0008(4) 0.0042(3) 0.0029(4) Ag3 0.0512(5) 0.0420(5) 0.0417(5) 0.0010(4) 0.0146(4) -0.0030(4) Ag4 0.0485(5) 0.0416(5) 0.0375(4) -0.0010(4) -0.0010(3) -0.0073(4) Ag5 0.0472(4) 0.0390(5) 0.0346(4) -0.0005(3) 0.0080(3) -0.0004(4) S1 0.0468(15) 0.0346(14) 0.0402(14) -0.0026(11) 0.0053(11) -0.0002(11) S2 0.0549(16) 0.0347(14) 0.0311(13) 0.0011(10) 0.0072(11) -0.0001(12) S3 0.0443(14) 0.0436(15) 0.0326(13) -0.0020(11) 0.0068(11) -0.0055(12) S4 0.0474(14) 0.0370(14) 0.0339(13) 0.0009(11) 0.0089(11) 0.0005(12) S5 0.0550(16) 0.0366(14) 0.0374(14) -0.0006(11) 0.0135(12) -0.0030(12) S6 0.0463(15) 0.0387(15) 0.0351(13) 0.0024(11) 0.0022(11) -0.0012(12) C1 0.049(6) 0.038(6) 0.035(5) -0.002(5) 0.007(4) -0.001(5) C2 0.082(9) 0.051(8) 0.044(7) -0.008(6) 0.003(6) -0.007(7) C3 0.056(7) 0.051(8) 0.055(7) 0.003(6) -0.005(6) 0.010(6) C4 0.054(7) 0.036(6) 0.045(6) 0.003(5) 0.008(5) 0.000(5) C5 0.047(6) 0.040(6) 0.034(5) -0.004(5) 0.007(4) 0.002(5) C6 0.051(8) 0.092(12) 0.051(8) -0.002(8) 0.000(6) -0.005(8) C7 0.058(7) 0.054(7) 0.033(6) 0.000(5) 0.013(5) 0.019(6) C8 0.074(9) 0.058(8) 0.041(6) -0.008(6) 0.005(6) 0.019(7) C9 0.049(6) 0.040(6) 0.034(5) 0.007(4) 0.003(5) -0.007(5) C10 0.112(13) 0.050(8) 0.062(9) 0.022(7) 0.002(9) -0.021(9) C11 0.063(8) 0.056(9) 0.060(8) -0.007(7) -0.001(6) -0.018(7) C12 0.060(8) 0.049(7) 0.051(7) -0.009(6) 0.011(6) -0.001(6) C13 0.055(7) 0.039(6) 0.038(6) 0.000(5) 0.005(5) 0.006(5) C14 0.070(10) 0.036(7) 0.110(13) 0.015(8) 0.035(9) 0.005(7) C15 0.19(2) 0.066(11) 0.048(9) 0.002(8) 0.025(12) 0.051(13) C16 0.070(10) 0.076(11) 0.088(12) 0.022(10) -0.005(8) 0.024(9) C17 0.064(8) 0.042(7) 0.051(7) 0.005(5) 0.016(6) -0.010(6) C18 0.118(14) 0.040(7) 0.042(7) 0.001(5) 0.031(8) -0.004(8) C19 0.145(17) 0.036(7) 0.066(10) 0.002(7) 0.021(10) -0.014(9) C20 0.073(12) 0.114(17) 0.122(17) 0.044(14) 0.044(11) -0.010(11) C21 0.044(6) 0.065(8) 0.025(5) 0.001(5) 0.000(4) -0.001(6) C22 0.056(7) 0.054(7) 0.032(5) -0.007(5) 0.009(5) -0.007(6) C23 0.055(8) 0.108(13) 0.036(6) 0.015(7) 0.003(5) 0.023(8) C24 0.041(6) 0.129(17) 0.055(8) -0.031(9) 0.006(6) -0.014(8) Ag6 0.0346(5) 0.0355(6) 0.0477(6) 0.000 0.0059(4) 0.000 N1 0.034(4) 0.033(5) 0.048(5) -0.003(4) 0.004(4) -0.003(4) N2 0.031(4) 0.036(5) 0.046(5) 0.006(4) 0.005(4) 0.003(4) C25 0.034(5) 0.042(6) 0.046(6) -0.007(5) 0.010(4) -0.005(5) C26 0.040(5) 0.045(7) 0.036(5) 0.007(5) 0.000(4) 0.007(5) C27 0.035(5) 0.039(6) 0.036(5) 0.008(4) 0.005(4) -0.003(4) C28 0.043(6) 0.047(7) 0.058(7) -0.017(6) 0.005(5) -0.003(6) C29 0.083(10) 0.070(10) 0.062(9) -0.019(8) 0.038(8) -0.005(8) C30 0.057(8) 0.033(6) 0.070(9) -0.003(6) 0.014(6) 0.001(6) C31 0.037(6) 0.049(7) 0.064(8) 0.001(6) -0.001(5) 0.002(5) C32 0.038(6) 0.067(9) 0.052(7) 0.011(6) 0.013(5) 0.011(6) C33 0.037(6) 0.041(6) 0.052(7) -0.006(5) 0.013(5) 0.004(5) C34 0.049(7) 0.061(8) 0.043(6) -0.010(6) 0.005(5) -0.003(6) C35 0.058(8) 0.033(6) 0.080(10) -0.001(6) 0.005(7) -0.003(6) Ag7 0.0328(5) 0.0445(6) 0.0412(6) 0.000 0.0051(4) 0.000 N3 0.031(4) 0.042(5) 0.037(5) 0.000(4) 0.006(4) -0.004(4) N4 0.037(4) 0.038(5) 0.037(4) -0.006(4) 0.003(3) 0.000(4) C36 0.031(4) 0.047(6) 0.037(5) -0.008(5) 0.007(4) -0.003(5) C37 0.037(5) 0.041(6) 0.040(6) 0.000(5) 0.004(4) -0.007(5) C38 0.031(5) 0.043(6) 0.041(6) 0.006(5) -0.001(4) -0.011(4) C39 0.035(6) 0.063(8) 0.052(7) -0.022(6) 0.004(5) 0.002(6) C40 0.067(8) 0.059(8) 0.040(6) -0.011(6) 0.010(6) -0.012(7) C41 0.063(8) 0.038(7) 0.076(10) -0.001(7) -0.016(7) -0.003(6) C42 0.040(6) 0.052(7) 0.049(7) 0.004(6) 0.003(5) -0.002(5) C43 0.045(7) 0.042(7) 0.076(9) -0.011(6) -0.008(6) -0.008(5) C44 0.050(7) 0.046(7) 0.047(6) -0.018(6) 0.005(5) 0.002(6) C45 0.070(9) 0.090(12) 0.062(9) -0.021(8) 0.033(7) 0.007(8) C46 0.15(2) 0.047(9) 0.089(13) -0.007(9) 0.013(13) 0.021(11) O1S 0.045(10) 0.057(14) 0.053(12) -0.011(10) 0.010(8) -0.001(8) C1S 0.022(11) 0.076(18) 0.12(3) 0.04(2) 0.018(12) 0.016(11) C2S 0.016(10) 0.09(2) 0.079(18) 0.003(16) 0.004(10) 0.011(11) C3S 0.048(12) 0.062(17) 0.058(16) -0.024(12) -0.008(10) 0.017(11) C4S 0.062(13) 0.046(15) 0.051(13) -0.017(11) -0.002(10) 0.008(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S3 2.481(3) . ? Ag1 S2 2.489(3) . ? Ag1 S1 2.500(3) . ? Ag1 Ag4 3.1787(15) . ? Ag1 Ag3 3.2591(16) . ? Ag1 Ag2 3.2804(16) . ? Ag2 S4 2.363(3) . ? Ag2 S1 2.365(3) . ? Ag2 Ag5 3.2044(15) . ? Ag3 S5 2.358(3) . ? Ag3 S2 2.362(3) . ? Ag3 Ag5 3.2433(16) . ? Ag4 S3 2.362(3) . ? Ag4 S6 2.365(3) . ? Ag4 Ag5 3.2942(15) . ? Ag5 S4 2.475(3) . ? Ag5 S6 2.475(3) . ? Ag5 S5 2.488(3) . ? S1 C1 1.874(12) . ? S2 C5 1.867(11) . ? S3 C9 1.854(13) . ? S4 C13 1.884(12) . ? S5 C17 1.862(13) . ? S6 C21 1.872(12) . ? C1 C2 1.500(17) . ? C1 C3 1.508(17) . ? C1 C4 1.517(17) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.473(18) . ? C5 C8 1.518(19) . ? C5 C7 1.535(16) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.514(17) . ? C9 C12 1.527(18) . ? C9 C11 1.551(17) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.489(19) . ? C13 C14 1.515(19) . ? C13 C16 1.59(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.47(2) . ? C17 C19 1.52(2) . ? C17 C18 1.534(19) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.506(18) . ? C21 C23 1.514(19) . ? C21 C24 1.520(19) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Ag6 C25 2.122(10) . ? Ag6 C25 2.122(10) 2_556 ? N1 C25 1.348(15) . ? N1 C26 1.374(14) . ? N1 C28 1.481(16) . ? N2 C25 1.346(15) . ? N2 C27 1.391(13) . ? N2 C33 1.443(15) . ? C26 C27 1.377(17) . ? C26 C31 1.481(17) . ? C27 C32 1.508(17) . ? C28 C30 1.477(19) . ? C28 C29 1.515(18) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.472(17) . ? C33 C35 1.535(19) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? Ag7 C36 2.122(10) 2_655 ? Ag7 C36 2.122(10) . ? N3 C36 1.351(14) . ? N3 C37 1.392(14) . ? N3 C39 1.474(16) . ? N4 C36 1.306(14) . ? N4 C38 1.389(14) . ? N4 C44 1.487(15) . ? C37 C38 1.343(17) . ? C37 C42 1.508(17) . ? C38 C43 1.508(16) . ? C39 C41 1.50(2) . ? C39 C40 1.570(19) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.43(2) . ? C44 C45 1.57(2) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? O1S C1S 1.429(7) . ? O1S C4S 1.435(7) . ? C1S C2S 1.464(7) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S C3S 1.513(7) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.465(7) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ag1 S2 123.23(10) . . ? S3 Ag1 S1 118.73(10) . . ? S2 Ag1 S1 117.22(10) . . ? S3 Ag1 Ag4 47.37(7) . . ? S2 Ag1 Ag4 114.75(7) . . ? S1 Ag1 Ag4 113.29(8) . . ? S3 Ag1 Ag3 116.53(8) . . ? S2 Ag1 Ag3 46.16(8) . . ? S1 Ag1 Ag3 111.28(8) . . ? Ag4 Ag1 Ag3 78.88(4) . . ? S3 Ag1 Ag2 112.78(8) . . ? S2 Ag1 Ag2 112.12(8) . . ? S1 Ag1 Ag2 45.89(7) . . ? Ag4 Ag1 Ag2 77.59(4) . . ? Ag3 Ag1 Ag2 77.12(3) . . ? S4 Ag2 S1 173.24(10) . . ? S4 Ag2 Ag5 50.03(7) . . ? S1 Ag2 Ag5 136.48(8) . . ? S4 Ag2 Ag1 137.17(8) . . ? S1 Ag2 Ag1 49.38(8) . . ? Ag5 Ag2 Ag1 87.14(4) . . ? S5 Ag3 S2 173.97(11) . . ? S5 Ag3 Ag5 49.72(8) . . ? S2 Ag3 Ag5 136.31(8) . . ? S5 Ag3 Ag1 136.55(8) . . ? S2 Ag3 Ag1 49.47(7) . . ? Ag5 Ag3 Ag1 86.86(4) . . ? S3 Ag4 S6 173.55(11) . . ? S3 Ag4 Ag1 50.61(8) . . ? S6 Ag4 Ag1 135.74(8) . . ? S3 Ag4 Ag5 137.89(8) . . ? S6 Ag4 Ag5 48.54(7) . . ? Ag1 Ag4 Ag5 87.33(4) . . ? S4 Ag5 S6 121.81(11) . . ? S4 Ag5 S5 120.65(10) . . ? S6 Ag5 S5 116.87(10) . . ? S4 Ag5 Ag2 47.04(7) . . ? S6 Ag5 Ag2 113.44(8) . . ? S5 Ag5 Ag2 114.50(8) . . ? S4 Ag5 Ag3 114.21(7) . . ? S6 Ag5 Ag3 110.84(8) . . ? S5 Ag5 Ag3 46.31(8) . . ? Ag2 Ag5 Ag3 78.42(3) . . ? S4 Ag5 Ag4 113.50(8) . . ? S6 Ag5 Ag4 45.71(7) . . ? S5 Ag5 Ag4 112.78(8) . . ? Ag2 Ag5 Ag4 77.04(4) . . ? Ag3 Ag5 Ag4 77.46(4) . . ? C1 S1 Ag2 104.0(4) . . ? C1 S1 Ag1 108.9(4) . . ? Ag2 S1 Ag1 84.73(10) . . ? C5 S2 Ag3 104.4(4) . . ? C5 S2 Ag1 111.6(4) . . ? Ag3 S2 Ag1 84.38(10) . . ? C9 S3 Ag4 104.4(4) . . ? C9 S3 Ag1 109.7(4) . . ? Ag4 S3 Ag1 82.01(10) . . ? C13 S4 Ag2 104.4(4) . . ? C13 S4 Ag5 112.8(4) . . ? Ag2 S4 Ag5 82.92(9) . . ? C17 S5 Ag3 105.3(5) . . ? C17 S5 Ag5 109.9(5) . . ? Ag3 S5 Ag5 83.96(10) . . ? C21 S6 Ag4 104.0(4) . . ? C21 S6 Ag5 109.8(4) . . ? Ag4 S6 Ag5 85.75(9) . . ? C2 C1 C3 109.3(11) . . ? C2 C1 C4 111.3(10) . . ? C3 C1 C4 110.5(10) . . ? C2 C1 S1 108.6(9) . . ? C3 C1 S1 105.7(8) . . ? C4 C1 S1 111.2(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C8 111.8(12) . . ? C6 C5 C7 107.3(11) . . ? C8 C5 C7 109.9(10) . . ? C6 C5 S2 107.2(9) . . ? C8 C5 S2 107.6(9) . . ? C7 C5 S2 113.0(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C12 111.2(12) . . ? C10 C9 C11 110.2(11) . . ? C12 C9 C11 107.6(11) . . ? C10 C9 S3 107.6(9) . . ? C12 C9 S3 112.8(8) . . ? C11 C9 S3 107.3(9) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 108.1(14) . . ? C15 C13 C16 114.8(15) . . ? C14 C13 C16 110.8(12) . . ? C15 C13 S4 107.5(10) . . ? C14 C13 S4 111.6(9) . . ? C16 C13 S4 104.1(9) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C19 114.2(15) . . ? C20 C17 C18 108.2(14) . . ? C19 C17 C18 106.7(13) . . ? C20 C17 S5 109.0(11) . . ? C19 C17 S5 107.8(10) . . ? C18 C17 S5 111.0(9) . . ? 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 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 108.9(10) . . ? C22 C21 C24 108.5(13) . . ? C23 C21 C24 111.4(11) . . ? C22 C21 S6 112.7(7) . . ? C23 C21 S6 107.9(10) . . ? C24 C21 S6 107.4(9) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 Ag6 C25 177.8(7) . 2_556 ? C25 N1 C26 110.8(10) . . ? C25 N1 C28 124.9(9) . . ? C26 N1 C28 124.3(10) . . ? C25 N2 C27 110.4(9) . . ? C25 N2 C33 127.1(9) . . ? C27 N2 C33 122.1(9) . . ? N2 C25 N1 106.2(9) . . ? N2 C25 Ag6 126.3(8) . . ? N1 C25 Ag6 127.5(8) . . ? N1 C26 C27 106.7(10) . . ? N1 C26 C31 123.2(11) . . ? C27 C26 C31 130.1(11) . . ? C26 C27 N2 105.9(10) . . ? C26 C27 C32 131.0(11) . . ? N2 C27 C32 123.0(11) . . ? C30 C28 N1 110.9(10) . . ? C30 C28 C29 116.4(12) . . ? N1 C28 C29 109.3(12) . . ? C30 C28 H28 106.5 . . ? N1 C28 H28 106.5 . . ? C29 C28 H28 106.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 C34 112.6(11) . . ? N2 C33 C35 109.9(10) . . ? C34 C33 C35 114.3(11) . . ? N2 C33 H33 106.5 . . ? C34 C33 H33 106.5 . . ? C35 C33 H33 106.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C36 Ag7 C36 178.8(7) 2_655 . ? C36 N3 C37 109.4(9) . . ? C36 N3 C39 127.0(9) . . ? C37 N3 C39 123.5(9) . . ? C36 N4 C38 110.2(9) . . ? C36 N4 C44 126.8(9) . . ? C38 N4 C44 123.0(9) . . ? N4 C36 N3 107.1(9) . . ? N4 C36 Ag7 127.5(8) . . ? N3 C36 Ag7 125.4(8) . . ? C38 C37 N3 106.0(10) . . ? C38 C37 C42 131.1(11) . . ? N3 C37 C42 122.9(10) . . ? C37 C38 N4 107.2(9) . . ? C37 C38 C43 129.8(11) . . ? N4 C38 C43 122.9(11) . . ? N3 C39 C41 110.3(11) . . ? N3 C39 C40 111.9(11) . . ? C41 C39 C40 113.4(11) . . ? N3 C39 H39 106.9 . . ? C41 C39 H39 106.9 . . ? C40 C39 H39 106.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 N4 113.0(12) . . ? C46 C44 C45 110.6(15) . . ? N4 C44 C45 109.1(11) . . ? C46 C44 H44 108.0 . . ? N4 C44 H44 108.0 . . ? C45 C44 H44 108.0 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C1S O1S C4S 105.6(10) . . ? O1S C1S C2S 107.4(6) . . ? O1S C1S H1S1 110.2 . . ? C2S C1S H1S1 110.2 . . ? O1S C1S H1S2 110.2 . . ? C2S C1S H1S2 110.2 . . ? H1S1 C1S H1S2 108.5 . . ? C1S C2S C3S 105.3(5) . . ? C1S C2S H2S1 110.7 . . ? C3S C2S H2S1 110.7 . . ? C1S C2S H2S2 110.7 . . ? C3S C2S H2S2 110.7 . . ? H2S1 C2S H2S2 108.8 . . ? C4S C3S C2S 105.1(5) . . ? C4S C3S H3S1 110.7 . . ? C2S C3S H3S1 110.7 . . ? C4S C3S H3S2 110.7 . . ? C2S C3S H3S2 110.7 . . ? H3S1 C3S H3S2 108.8 . . ? O1S C4S C3S 106.8(6) . . ? O1S C4S H4S1 110.4 . . ? C3S C4S H4S1 110.4 . . ? O1S C4S H4S2 110.4 . . ? C3S C4S H4S2 110.4 . . ? H4S1 C4S H4S2 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag2 S1 C1 C2 89.9(9) . . . . ? Ag1 S1 C1 C2 179.0(8) . . . . ? Ag2 S1 C1 C3 -152.9(7) . . . . ? Ag1 S1 C1 C3 -63.7(8) . . . . ? Ag2 S1 C1 C4 -32.9(8) . . . . ? Ag1 S1 C1 C4 56.2(8) . . . . ? Ag3 S2 C5 C6 -161.0(9) . . . . ? Ag1 S2 C5 C6 -71.4(10) . . . . ? Ag3 S2 C5 C8 78.6(9) . . . . ? Ag1 S2 C5 C8 168.2(7) . . . . ? Ag3 S2 C5 C7 -42.9(9) . . . . ? Ag1 S2 C5 C7 46.7(10) . . . . ? Ag4 S3 C9 C10 89.7(10) . . . . ? Ag1 S3 C9 C10 176.2(9) . . . . ? Ag4 S3 C9 C12 -33.3(9) . . . . ? Ag1 S3 C9 C12 53.2(9) . . . . ? Ag4 S3 C9 C11 -151.7(8) . . . . ? Ag1 S3 C9 C11 -65.1(9) . . . . ? Ag2 S4 C13 C15 77.9(13) . . . . ? Ag5 S4 C13 C15 166.2(12) . . . . ? Ag2 S4 C13 C14 -40.4(11) . . . . ? Ag5 S4 C13 C14 47.9(11) . . . . ? Ag2 S4 C13 C16 -159.9(9) . . . . ? Ag5 S4 C13 C16 -71.6(10) . . . . ? Ag3 S5 C17 C20 -157.1(13) . . . . ? Ag5 S5 C17 C20 -68.0(14) . . . . ? Ag3 S5 C17 C19 78.5(11) . . . . ? Ag5 S5 C17 C19 167.5(10) . . . . ? Ag3 S5 C17 C18 -38.0(11) . . . . ? Ag5 S5 C17 C18 51.0(11) . . . . ? Ag4 S6 C21 C22 -37.0(10) . . . . ? Ag5 S6 C21 C22 53.4(10) . . . . ? Ag4 S6 C21 C23 83.3(8) . . . . ? Ag5 S6 C21 C23 173.8(7) . . . . ? Ag4 S6 C21 C24 -156.5(10) . . . . ? Ag5 S6 C21 C24 -66.0(11) . . . . ? C27 N2 C25 N1 1.9(13) . . . . ? C33 N2 C25 N1 175.3(10) . . . . ? C27 N2 C25 Ag6 -174.6(8) . . . . ? C33 N2 C25 Ag6 -1.2(17) . . . . ? C26 N1 C25 N2 -0.7(13) . . . . ? C28 N1 C25 N2 175.8(11) . . . . ? C26 N1 C25 Ag6 175.7(8) . . . . ? C28 N1 C25 Ag6 -7.8(17) . . . . ? C25 N1 C26 C27 -0.7(13) . . . . ? C28 N1 C26 C27 -177.2(11) . . . . ? C25 N1 C26 C31 179.3(11) . . . . ? C28 N1 C26 C31 2.7(18) . . . . ? N1 C26 C27 N2 1.7(12) . . . . ? C31 C26 C27 N2 -178.2(12) . . . . ? N1 C26 C27 C32 -177.0(11) . . . . ? C31 C26 C27 C32 3(2) . . . . ? C25 N2 C27 C26 -2.3(12) . . . . ? C33 N2 C27 C26 -176.1(10) . . . . ? C25 N2 C27 C32 176.6(10) . . . . ? C33 N2 C27 C32 2.8(16) . . . . ? C25 N1 C28 C30 -65.2(15) . . . . ? C26 N1 C28 C30 110.9(13) . . . . ? C25 N1 C28 C29 64.5(16) . . . . ? C26 N1 C28 C29 -119.4(13) . . . . ? C25 N2 C33 C34 54.0(16) . . . . ? C27 N2 C33 C34 -133.3(11) . . . . ? C25 N2 C33 C35 -74.7(14) . . . . ? C27 N2 C33 C35 98.0(12) . . . . ? C38 N4 C36 N3 -1.3(13) . . . . ? C44 N4 C36 N3 179.8(11) . . . . ? C38 N4 C36 Ag7 179.0(8) . . . . ? C44 N4 C36 Ag7 0.1(17) . . . . ? C37 N3 C36 N4 -0.1(13) . . . . ? C39 N3 C36 N4 -176.8(11) . . . . ? C37 N3 C36 Ag7 179.6(8) . . . . ? C39 N3 C36 Ag7 2.9(17) . . . . ? C36 N3 C37 C38 1.5(13) . . . . ? C39 N3 C37 C38 178.3(11) . . . . ? C36 N3 C37 C42 179.5(11) . . . . ? C39 N3 C37 C42 -3.6(17) . . . . ? N3 C37 C38 N4 -2.2(12) . . . . ? C42 C37 C38 N4 180.0(12) . . . . ? N3 C37 C38 C43 178.8(12) . . . . ? C42 C37 C38 C43 1(2) . . . . ? C36 N4 C38 C37 2.3(13) . . . . ? C44 N4 C38 C37 -178.8(11) . . . . ? C36 N4 C38 C43 -178.7(11) . . . . ? C44 N4 C38 C43 0.3(18) . . . . ? C36 N3 C39 C41 75.1(15) . . . . ? C37 N3 C39 C41 -101.2(13) . . . . ? C36 N3 C39 C40 -52.2(16) . . . . ? C37 N3 C39 C40 131.5(11) . . . . ? C36 N4 C44 C46 69.3(18) . . . . ? C38 N4 C44 C46 -109.5(15) . . . . ? C36 N4 C44 C45 -54.2(16) . . . . ? C38 N4 C44 C45 127.0(12) . . . . ? C4S O1S C1S C2S -30(3) . . . . ? O1S C1S C2S C3S 17(4) . . . . ? C1S C2S C3S C4S 2(3) . . . . ? C1S O1S C4S C3S 31(3) . . . . ? C2S C3S C4S O1S -20(3) . . . . ? _refine_diff_density_max 1.909 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.204 _shelxl_version_number 2012-9 _database_code_depnum_ccdc_archive 'CCDC 960483' ####################################################################### # # 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_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H78 Ag4 P2 S4' _chemical_formula_sum 'C34 H78 Ag4 P2 S4' _chemical_formula_weight 1108.62 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' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.538(4) _cell_length_b 10.919(3) _cell_length_c 12.288(4) _cell_angle_alpha 69.848(19) _cell_angle_beta 78.879(13) _cell_angle_gamma 83.194(9) _cell_volume 1177.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 34.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.905 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5359 _exptl_absorpt_correction_T_max 0.6870 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 26384 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 35.58 _reflns_number_total 8855 _reflns_number_gt 7744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution XS _computing_structure_refinement XL _computing_molecular_graphics SCHAKAL99 _computing_publication_material cif2tables.py _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^)+(0.0122P)^2^+0.5354P] 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 8855 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0396 _refine_ls_wR_factor_gt 0.0374 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.570840(10) 0.445995(9) 0.869548(8) 0.01744(2) Uani 1 1 d . . . Ag2 Ag 0.601183(9) 0.727312(9) 0.870520(8) 0.01634(2) Uani 1 1 d . . . S1 S 0.77102(3) 0.57772(3) 0.79522(3) 0.01582(5) Uani 1 1 d . . . S2 S 0.61092(3) 0.70059(3) 1.08251(3) 0.01526(5) Uani 1 1 d . . . P1 P 0.43179(3) 0.91110(3) 0.81167(3) 0.01425(6) Uani 1 1 d . . . C15 C 0.32706(13) 0.94760(13) 0.93970(11) 0.0183(2) Uani 1 1 d . . . H15A H 0.3931 0.9493 0.9922 0.022 Uiso 1 1 calc R . . H15B H 0.2792 1.0358 0.9128 0.022 Uiso 1 1 calc R . . C16 C 0.21419(14) 0.84978(13) 1.00962(11) 0.0207(2) Uani 1 1 d . . . H16A H 0.1384 0.8586 0.9621 0.025 Uiso 1 1 calc R . . H16B H 0.2588 0.7600 1.0259 0.025 Uiso 1 1 calc R . . C17 C 0.14717(18) 0.87037(19) 1.12501(13) 0.0363(4) Uani 1 1 d . . . H17A H 0.0717 0.8090 1.1653 0.054 Uiso 1 1 calc R . . H17B H 0.1059 0.9601 1.1095 0.054 Uiso 1 1 calc R . . H17C H 0.2206 0.8553 1.1747 0.054 Uiso 1 1 calc R . . C12 C 0.29649(13) 0.89816(12) 0.72944(11) 0.0169(2) Uani 1 1 d . . . H12A H 0.3468 0.8862 0.6551 0.020 Uiso 1 1 calc R . . H12B H 0.2452 0.8179 0.7754 0.020 Uiso 1 1 calc R . . C13 C 0.18474(14) 1.01214(13) 0.69910(12) 0.0221(3) Uani 1 1 d . . . H13A H 0.1497 1.0396 0.7689 0.027 Uiso 1 1 calc R . . H13B H 0.2302 1.0872 0.6357 0.027 Uiso 1 1 calc R . . C14 C 0.05822(16) 0.97574(16) 0.65953(14) 0.0292(3) Uani 1 1 d . . . H14A H -0.0127 1.0498 0.6445 0.044 Uiso 1 1 calc R . . H14B H 0.0145 0.9000 0.7213 0.044 Uiso 1 1 calc R . . H14C H 0.0915 0.9540 0.5874 0.044 Uiso 1 1 calc R . . C9 C 0.51208(14) 1.06764(12) 0.72798(11) 0.0185(2) Uani 1 1 d . . . H9A H 0.4341 1.1359 0.7088 0.022 Uiso 1 1 calc R . . H9B H 0.5660 1.0904 0.7789 0.022 Uiso 1 1 calc R . . C10 C 0.61192(16) 1.07103(14) 0.61475(12) 0.0257(3) Uani 1 1 d . . . H10A H 0.5570 1.0566 0.5600 0.031 Uiso 1 1 calc R . . H10B H 0.6868 0.9993 0.6320 0.031 Uiso 1 1 calc R . . C11 C 0.68268(16) 1.20065(14) 0.55623(12) 0.0259(3) Uani 1 1 d . . . H11A H 0.7415 1.2013 0.4813 0.039 Uiso 1 1 calc R . . H11B H 0.7433 1.2120 0.6077 0.039 Uiso 1 1 calc R . . H11C H 0.6088 1.2722 0.5420 0.039 Uiso 1 1 calc R . . C1 C 0.78453(13) 0.61336(12) 0.63466(11) 0.0174(2) Uani 1 1 d . . . C4 C 0.90784(15) 0.70300(14) 0.57490(13) 0.0258(3) Uani 1 1 d . . . H4A H 0.9227 0.7197 0.4900 0.039 Uiso 1 1 calc R . . H4B H 0.9952 0.6610 0.6058 0.039 Uiso 1 1 calc R . . H4C H 0.8849 0.7859 0.5905 0.039 Uiso 1 1 calc R . . C3 C 0.64666(15) 0.67901(15) 0.59082(12) 0.0255(3) Uani 1 1 d . . . H3A H 0.6581 0.6970 0.5059 0.038 Uiso 1 1 calc R . . H3B H 0.6251 0.7612 0.6078 0.038 Uiso 1 1 calc R . . H3C H 0.5680 0.6211 0.6306 0.038 Uiso 1 1 calc R . . C2 C 0.81756(17) 0.48456(14) 0.60983(13) 0.0273(3) Uani 1 1 d . . . H2A H 0.8301 0.5015 0.5250 0.041 Uiso 1 1 calc R . . H2B H 0.7382 0.4274 0.6494 0.041 Uiso 1 1 calc R . . H2C H 0.9056 0.4420 0.6392 0.041 Uiso 1 1 calc R . . C5 C 0.77372(13) 0.60384(12) 1.13254(11) 0.0172(2) Uani 1 1 d . . . C8 C 0.77385(18) 0.60330(17) 1.25701(13) 0.0332(3) Uani 1 1 d . . . H8A H 0.8600 0.5544 1.2855 0.050 Uiso 1 1 calc R . . H8B H 0.6887 0.5618 1.3090 0.050 Uiso 1 1 calc R . . H8C H 0.7729 0.6934 1.2564 0.050 Uiso 1 1 calc R . . C7 C 0.90262(15) 0.67215(15) 1.04990(14) 0.0279(3) Uani 1 1 d . . . H7A H 0.9906 0.6272 1.0778 0.042 Uiso 1 1 calc R . . H7B H 0.8976 0.7631 1.0479 0.042 Uiso 1 1 calc R . . H7C H 0.9027 0.6702 0.9707 0.042 Uiso 1 1 calc R . . C6 C 0.77696(16) 0.46417(13) 1.13257(14) 0.0265(3) Uani 1 1 d . . . H6A H 0.8646 0.4166 1.1590 0.040 Uiso 1 1 calc R . . H6B H 0.7749 0.4650 1.0529 0.040 Uiso 1 1 calc R . . H6C H 0.6935 0.4210 1.1858 0.040 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 0.01486(4) 0.01779(4) 0.01779(4) -0.00354(3) -0.00265(3) -0.00076(3) Ag2 0.01410(4) 0.01700(4) 0.01797(4) -0.00611(3) -0.00338(3) 0.00117(3) S1 0.01367(13) 0.01761(13) 0.01666(13) -0.00609(11) -0.00427(10) 0.00160(10) S2 0.01532(13) 0.01396(12) 0.01681(13) -0.00589(10) -0.00321(10) 0.00150(10) P1 0.01379(14) 0.01465(13) 0.01487(13) -0.00590(11) -0.00274(10) 0.00079(10) C15 0.0156(6) 0.0215(6) 0.0200(6) -0.0103(5) -0.0006(4) -0.0028(4) C16 0.0187(6) 0.0200(6) 0.0206(6) -0.0046(5) -0.0006(5) -0.0009(5) C17 0.0303(8) 0.0558(11) 0.0234(7) -0.0152(7) 0.0056(6) -0.0147(7) C12 0.0185(6) 0.0158(5) 0.0191(5) -0.0077(4) -0.0061(4) 0.0001(4) C13 0.0209(6) 0.0190(6) 0.0259(6) -0.0045(5) -0.0100(5) 0.0022(5) C14 0.0221(7) 0.0347(8) 0.0328(7) -0.0098(6) -0.0127(6) 0.0000(6) C9 0.0175(6) 0.0182(5) 0.0212(6) -0.0089(5) -0.0010(4) -0.0026(4) C10 0.0302(7) 0.0256(6) 0.0229(6) -0.0124(5) 0.0054(5) -0.0103(5) C11 0.0270(7) 0.0272(7) 0.0238(6) -0.0083(5) 0.0015(5) -0.0120(5) C1 0.0175(6) 0.0180(5) 0.0162(5) -0.0060(4) -0.0006(4) -0.0010(4) C4 0.0228(7) 0.0248(6) 0.0255(7) -0.0041(5) 0.0004(5) -0.0048(5) C3 0.0205(6) 0.0357(7) 0.0191(6) -0.0068(5) -0.0067(5) 0.0018(5) C2 0.0350(8) 0.0246(6) 0.0249(7) -0.0137(6) -0.0004(6) -0.0018(6) C5 0.0171(6) 0.0167(5) 0.0186(5) -0.0065(4) -0.0052(4) 0.0020(4) C8 0.0370(9) 0.0424(9) 0.0247(7) -0.0156(6) -0.0160(6) 0.0121(7) C7 0.0156(6) 0.0288(7) 0.0365(8) -0.0067(6) -0.0046(5) -0.0023(5) C6 0.0242(7) 0.0172(6) 0.0387(8) -0.0089(6) -0.0106(6) 0.0052(5) _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 S2 2.3512(8) 2_667 ? Ag1 S1 2.3710(8) . ? Ag1 Ag2 3.1235(10) . ? Ag1 Ag2 3.3204(10) 2_667 ? Ag2 P1 2.4172(7) . ? Ag2 S1 2.4463(7) . ? Ag2 S2 2.5383(8) . ? Ag2 Ag1 3.3204(10) 2_667 ? S1 C1 1.8563(14) . ? S2 C5 1.8540(14) . ? S2 Ag1 2.3512(8) 2_667 ? P1 C12 1.8306(13) . ? P1 C9 1.8333(14) . ? P1 C15 1.8340(13) . ? C15 C16 1.5236(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.519(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C12 C13 1.5307(17) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.524(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C9 C10 1.5186(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.5210(19) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C1 C3 1.5222(19) . ? C1 C2 1.5244(19) . ? C1 C4 1.5248(19) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C5 C7 1.521(2) . ? C5 C6 1.5216(19) . ? C5 C8 1.5277(19) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 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 S2 Ag1 S1 169.999(12) 2_667 . ? S2 Ag1 Ag2 137.924(15) 2_667 . ? S1 Ag1 Ag2 50.639(15) . . ? S2 Ag1 Ag2 49.645(17) 2_667 2_667 ? S1 Ag1 Ag2 137.845(14) . 2_667 ? Ag2 Ag1 Ag2 108.93(2) . 2_667 ? P1 Ag2 S1 142.611(18) . . ? P1 Ag2 S2 104.08(2) . . ? S1 Ag2 S2 113.07(2) . . ? P1 Ag2 Ag1 125.34(2) . . ? S1 Ag2 Ag1 48.54(2) . . ? S2 Ag2 Ag1 105.26(2) . . ? P1 Ag2 Ag1 101.29(3) . 2_667 ? S1 Ag2 Ag1 107.72(2) . 2_667 ? S2 Ag2 Ag1 44.900(18) . 2_667 ? Ag1 Ag2 Ag1 71.07(2) . 2_667 ? C1 S1 Ag1 101.38(4) . . ? C1 S1 Ag2 113.29(4) . . ? Ag1 S1 Ag2 80.83(3) . . ? C5 S2 Ag1 107.34(5) . 2_667 ? C5 S2 Ag2 112.10(4) . . ? Ag1 S2 Ag2 85.45(2) 2_667 . ? C12 P1 C9 105.61(6) . . ? C12 P1 C15 104.02(6) . . ? C9 P1 C15 101.18(6) . . ? C12 P1 Ag2 118.10(5) . . ? C9 P1 Ag2 114.93(5) . . ? C15 P1 Ag2 111.15(5) . . ? C16 C15 P1 113.72(9) . . ? C16 C15 H15A 108.8 . . ? P1 C15 H15A 108.8 . . ? C16 C15 H15B 108.8 . . ? P1 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 111.90(12) . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C12 P1 117.40(9) . . ? C13 C12 H12A 108.0 . . ? P1 C12 H12A 108.0 . . ? C13 C12 H12B 108.0 . . ? P1 C12 H12B 108.0 . . ? H12A C12 H12B 107.2 . . ? C14 C13 C12 112.02(12) . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C9 P1 115.37(9) . . ? C10 C9 H9A 108.4 . . ? P1 C9 H9A 108.4 . . ? C10 C9 H9B 108.4 . . ? P1 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? C9 C10 C11 111.80(12) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 C1 C2 109.69(12) . . ? C3 C1 C4 110.19(11) . . ? C2 C1 C4 110.19(11) . . ? C3 C1 S1 111.82(9) . . ? C2 C1 S1 108.03(9) . . ? C4 C1 S1 106.86(9) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C7 C5 C6 110.00(11) . . ? C7 C5 C8 110.12(12) . . ? C6 C5 C8 109.74(12) . . ? C7 C5 S2 107.53(9) . . ? C6 C5 S2 111.97(9) . . ? C8 C5 S2 107.41(9) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ag1 Ag2 P1 -40.52(3) 2_667 . . . ? S1 Ag1 Ag2 P1 132.32(3) . . . . ? Ag2 Ag1 Ag2 P1 -90.60(3) 2_667 . . . ? S2 Ag1 Ag2 S1 -172.834(16) 2_667 . . . ? Ag2 Ag1 Ag2 S1 137.082(14) 2_667 . . . ? S2 Ag1 Ag2 S2 79.65(2) 2_667 . . . ? S1 Ag1 Ag2 S2 -107.51(2) . . . . ? Ag2 Ag1 Ag2 S2 29.570(16) 2_667 . . . ? S2 Ag1 Ag2 Ag1 50.084(16) 2_667 . . 2_667 ? S1 Ag1 Ag2 Ag1 -137.082(14) . . . 2_667 ? Ag2 Ag1 Ag2 Ag1 0.0 2_667 . . 2_667 ? S2 Ag1 S1 C1 39.14(8) 2_667 . . . ? Ag2 Ag1 S1 C1 -112.09(4) . . . . ? Ag2 Ag1 S1 C1 174.23(4) 2_667 . . . ? S2 Ag1 S1 Ag2 151.22(6) 2_667 . . . ? Ag2 Ag1 S1 Ag2 -73.69(2) 2_667 . . . ? P1 Ag2 S1 C1 1.91(5) . . . . ? S2 Ag2 S1 C1 -171.17(5) . . . . ? Ag1 Ag2 S1 C1 98.51(5) . . . . ? Ag1 Ag2 S1 C1 141.06(5) 2_667 . . . ? P1 Ag2 S1 Ag1 -96.60(3) . . . . ? S2 Ag2 S1 Ag1 90.31(2) . . . . ? Ag1 Ag2 S1 Ag1 42.547(15) 2_667 . . . ? P1 Ag2 S2 C5 -161.16(4) . . . . ? S1 Ag2 S2 C5 14.51(5) . . . . ? Ag1 Ag2 S2 C5 65.48(5) . . . . ? Ag1 Ag2 S2 C5 106.88(5) 2_667 . . . ? P1 Ag2 S2 Ag1 91.96(3) . . . 2_667 ? S1 Ag2 S2 Ag1 -92.36(3) . . . 2_667 ? Ag1 Ag2 S2 Ag1 -41.400(16) . . . 2_667 ? S1 Ag2 P1 C12 51.24(5) . . . . ? S2 Ag2 P1 C12 -135.32(5) . . . . ? Ag1 Ag2 P1 C12 -14.62(5) . . . . ? Ag1 Ag2 P1 C12 -89.32(5) 2_667 . . . ? S1 Ag2 P1 C9 -74.54(5) . . . . ? S2 Ag2 P1 C9 98.90(5) . . . . ? Ag1 Ag2 P1 C9 -140.41(5) . . . . ? Ag1 Ag2 P1 C9 144.90(5) 2_667 . . . ? S1 Ag2 P1 C15 171.31(4) . . . . ? S2 Ag2 P1 C15 -15.25(5) . . . . ? Ag1 Ag2 P1 C15 105.44(5) . . . . ? Ag1 Ag2 P1 C15 30.75(5) 2_667 . . . ? C12 P1 C15 C16 54.15(10) . . . . ? C9 P1 C15 C16 163.54(9) . . . . ? Ag2 P1 C15 C16 -73.96(10) . . . . ? P1 C15 C16 C17 170.59(10) . . . . ? C9 P1 C12 C13 -53.27(11) . . . . ? C15 P1 C12 C13 52.83(11) . . . . ? Ag2 P1 C12 C13 176.53(8) . . . . ? P1 C12 C13 C14 -165.40(10) . . . . ? C12 P1 C9 C10 -73.52(11) . . . . ? C15 P1 C9 C10 178.33(10) . . . . ? Ag2 P1 C9 C10 58.49(11) . . . . ? P1 C9 C10 C11 -175.44(10) . . . . ? Ag1 S1 C1 C3 57.32(10) . . . . ? Ag2 S1 C1 C3 -27.49(11) . . . . ? Ag1 S1 C1 C2 -63.48(9) . . . . ? Ag2 S1 C1 C2 -148.29(8) . . . . ? Ag1 S1 C1 C4 177.97(8) . . . . ? Ag2 S1 C1 C4 93.16(9) . . . . ? Ag1 S2 C5 C7 149.29(8) 2_667 . . . ? Ag2 S2 C5 C7 57.16(10) . . . . ? Ag1 S2 C5 C6 28.34(10) 2_667 . . . ? Ag2 S2 C5 C6 -63.79(10) . . . . ? Ag1 S2 C5 C8 -92.21(10) 2_667 . . . ? Ag2 S2 C5 C8 175.66(9) . . . . ? _diffrn_measured_fraction_theta_max 0.819 _diffrn_reflns_theta_full 30.95 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.470 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.079 _database_code_depnum_ccdc_archive 'CCDC 960484' ####################################################################### # # 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_8 _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H96 Ag6 P2 S6' _chemical_formula_sum 'C42 H96 Ag6 P2 S6' _chemical_formula_weight 1502.70 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' P P 0.1023 0.0942 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 52 _space_group_name_H-M_alt 'P n n a' _space_group_name_Hall '-P 2a 2bc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 24.641(9) _cell_length_b 15.066(5) _cell_length_c 16.081(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5970(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9456 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 25.67 _exptl_crystal_description 'tetragonal prism' _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_F_000 3024 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.066 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_min 0.039 _exptl_absorpt_coefficient_mu 2.219 _shelx_estimated_absorpt_T_min 0.867 _shelx_estimated_absorpt_T_max 0.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6102 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details SAD-ABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 83082 _diffrn_reflns_av_unetI/netI 0.0467 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.704 _diffrn_reflns_theta_max 25.712 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 5693 _reflns_number_gt 3844 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _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-2012 (Sheldrick, 2012)' _computing_molecular_graphics ? _computing_publication_material cif2tables.py _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+11.7184P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5693 _refine_ls_number_parameters 320 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1056 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.023 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.59455(2) 0.14173(3) 0.16917(3) 0.04655(15) Uani 1 1 d . . . . . Ag2 Ag 0.60630(2) 0.33611(3) 0.13741(3) 0.04034(14) Uani 1 1 d . . . . . Ag3 Ag 0.45370(2) 0.35611(3) 0.24088(3) 0.03706(14) Uani 1 1 d . . . . . S1 S 0.57342(6) 0.04274(9) 0.28238(11) 0.0412(4) Uani 1 1 d . . . . . S2A S 0.64055(7) 0.21569(12) 0.05488(10) 0.0476(4) Uani 0.834(8) 1 d . . P A 1 C5A C 0.7156(3) 0.2061(5) 0.0630(4) 0.0520(17) Uani 0.834(8) 1 d . . P A 1 C6A C 0.7399(4) 0.2641(7) -0.0013(7) 0.087(4) Uani 0.834(8) 1 d . . P A 1 H6A1 H 0.7303 0.3261 0.0102 0.131 Uiso 0.834(8) 1 calc R U P A 1 H6A2 H 0.7260 0.2472 -0.0561 0.131 Uiso 0.834(8) 1 calc R U P A 1 H6A3 H 0.7795 0.2575 -0.0005 0.131 Uiso 0.834(8) 1 calc R U P A 1 C7A C 0.7296(4) 0.1085(6) 0.0459(6) 0.072(3) Uani 0.834(8) 1 d . . P A 1 H7A1 H 0.7158 0.0914 -0.0090 0.108 Uiso 0.834(8) 1 calc R U P A 1 H7A2 H 0.7130 0.0709 0.0886 0.108 Uiso 0.834(8) 1 calc R U P A 1 H7A3 H 0.7691 0.1007 0.0471 0.108 Uiso 0.834(8) 1 calc R U P A 1 C8A C 0.7333(3) 0.2302(6) 0.1506(6) 0.067(3) Uani 0.834(8) 1 d . . P A 1 H8A1 H 0.7729 0.2261 0.1547 0.100 Uiso 0.834(8) 1 calc R U P A 1 H8A2 H 0.7167 0.1890 0.1903 0.100 Uiso 0.834(8) 1 calc R U P A 1 H8A3 H 0.7217 0.2909 0.1634 0.100 Uiso 0.834(8) 1 calc R U P A 1 S2B S 0.64055(7) 0.21569(12) 0.05488(10) 0.0476(4) Uani 0.166(8) 1 d . U P A 2 C5B C 0.7156(3) 0.2061(5) 0.0630(4) 0.0520(17) Uani 0.166(8) 1 d . U P A 2 C6B C 0.7373(15) 0.181(3) -0.028(2) 0.053(7) Uani 0.166(8) 1 d . U P A 2 H6B1 H 0.7770 0.1850 -0.0285 0.079 Uiso 0.166(8) 1 calc R U P A 2 H6B2 H 0.7219 0.2216 -0.0686 0.079 Uiso 0.166(8) 1 calc R U P A 2 H6B3 H 0.7264 0.1198 -0.0410 0.079 Uiso 0.166(8) 1 calc R U P A 2 C7B C 0.7355(16) 0.147(3) 0.122(3) 0.055(7) Uani 0.166(8) 1 d . U P A 2 H7B1 H 0.7202 0.0881 0.1124 0.082 Uiso 0.166(8) 1 calc R U P A 2 H7B2 H 0.7252 0.1676 0.1779 0.082 Uiso 0.166(8) 1 calc R U P A 2 H7B3 H 0.7752 0.1444 0.1181 0.082 Uiso 0.166(8) 1 calc R U P A 2 C8B C 0.7427(14) 0.306(3) 0.079(3) 0.045(7) Uani 0.166(8) 1 d . U P A 2 H8B1 H 0.7220 0.3368 0.1225 0.068 Uiso 0.166(8) 1 calc R U P A 2 H8B2 H 0.7414 0.3403 0.0276 0.068 Uiso 0.166(8) 1 calc R U P A 2 H8B3 H 0.7805 0.2991 0.0972 0.068 Uiso 0.166(8) 1 calc R U P A 2 S3 S 0.49670(6) 0.23550(9) 0.14643(9) 0.0335(3) Uani 1 1 d . . . . . P1A P 0.39194(6) 0.47587(10) 0.22102(10) 0.0386(4) Uani 0.708(15) 1 d . . P B 3 C19A C 0.3977(5) 0.5373(12) 0.1255(9) 0.074(4) Uani 0.708(15) 1 d . . P B 3 H19A H 0.4199 0.5868 0.1491 0.089 Uiso 0.708(15) 1 calc R U P B 3 C20A C 0.3560(4) 0.5907(8) 0.0958(7) 0.064(4) Uani 0.708(15) 1 d . . P B 3 H20A H 0.3696 0.6278 0.0503 0.096 Uiso 0.708(15) 1 calc R U P B 3 H20B H 0.3426 0.6287 0.1408 0.096 Uiso 0.708(15) 1 calc R U P B 3 H20C H 0.3263 0.5533 0.0753 0.096 Uiso 0.708(15) 1 calc R U P B 3 C21A C 0.4399(4) 0.5051(5) 0.0659(5) 0.076(2) Uani 0.708(15) 1 d . . P B 3 H21A H 0.4473 0.5514 0.0245 0.114 Uiso 0.708(15) 1 calc R U P B 3 H21B H 0.4268 0.4515 0.0378 0.114 Uiso 0.708(15) 1 calc R U P B 3 H21C H 0.4734 0.4914 0.0963 0.114 Uiso 0.708(15) 1 calc R U P B 3 P1B P 0.39194(6) 0.47587(10) 0.22102(10) 0.0386(4) Uani 0.292(15) 1 d . U P B 4 C19B C 0.3892(13) 0.490(2) 0.0991(19) 0.057(6) Uani 0.292(15) 1 d . U P B 4 H19B H 0.3894 0.4249 0.0872 0.068 Uiso 0.292(15) 1 calc R U P B 4 C20B C 0.3384(10) 0.507(2) 0.0529(15) 0.074(9) Uani 0.292(15) 1 d . U P B 4 H20D H 0.3374 0.5698 0.0357 0.111 Uiso 0.292(15) 1 calc R U P B 4 H20E H 0.3072 0.4946 0.0887 0.111 Uiso 0.292(15) 1 calc R U P B 4 H20F H 0.3370 0.4692 0.0035 0.111 Uiso 0.292(15) 1 calc R U P B 4 C21B C 0.4399(4) 0.5051(5) 0.0659(5) 0.076(2) Uani 0.292(15) 1 d . U P B 4 H21D H 0.4528 0.4512 0.0382 0.114 Uiso 0.292(15) 1 calc R U P B 4 H21E H 0.4652 0.5213 0.1105 0.114 Uiso 0.292(15) 1 calc R U P B 4 H21F H 0.4379 0.5536 0.0254 0.114 Uiso 0.292(15) 1 calc R U P B 4 C1 C 0.6231(2) -0.0504(4) 0.2794(5) 0.0516(19) Uani 1 1 d . . . . . C2 C 0.6801(3) -0.0179(4) 0.2842(5) 0.067(2) Uani 1 1 d . . . . . H2A H 0.6860 0.0115 0.3378 0.101 Uiso 1 1 calc R U . . . H2B H 0.6867 0.0245 0.2390 0.101 Uiso 1 1 calc R U . . . H2C H 0.7051 -0.0681 0.2788 0.101 Uiso 1 1 calc R U . . . C3 C 0.6157(3) -0.0967(6) 0.1941(7) 0.097(3) Uani 1 1 d . . . . . H3A H 0.6423 -0.1446 0.1885 0.146 Uiso 1 1 calc R U . . . H3B H 0.6210 -0.0534 0.1494 0.146 Uiso 1 1 calc R U . . . H3C H 0.5790 -0.1214 0.1904 0.146 Uiso 1 1 calc R U . . . C4 C 0.6089(4) -0.1114(6) 0.3476(7) 0.119(4) Uani 1 1 d . . . . . H4A H 0.6303 -0.1659 0.3426 0.179 Uiso 1 1 calc R U . . . H4B H 0.5701 -0.1259 0.3445 0.179 Uiso 1 1 calc R U . . . H4C H 0.6166 -0.0829 0.4011 0.179 Uiso 1 1 calc R U . . . C9 C 0.4705(3) 0.2075(4) 0.0411(4) 0.0410(15) Uani 1 1 d . . . . . C10 C 0.4097(3) 0.2237(5) 0.0384(4) 0.0532(17) Uani 1 1 d . . . . . H10A H 0.3961 0.2113 -0.0177 0.080 Uiso 1 1 calc R U . . . H10B H 0.4021 0.2857 0.0527 0.080 Uiso 1 1 calc R U . . . H10C H 0.3916 0.1845 0.0784 0.080 Uiso 1 1 calc R U . . . C11 C 0.4831(3) 0.1104(4) 0.0238(4) 0.065(2) Uani 1 1 d . . . . . H11A H 0.4669 0.0734 0.0674 0.097 Uiso 1 1 calc R U . . . H11B H 0.5225 0.1017 0.0232 0.097 Uiso 1 1 calc R U . . . H11C H 0.4679 0.0936 -0.0303 0.097 Uiso 1 1 calc R U . . . C12 C 0.4990(3) 0.2669(4) -0.0223(4) 0.0458(16) Uani 1 1 d . . . . . H12A H 0.4844 0.2551 -0.0779 0.069 Uiso 1 1 calc R U . . . H12B H 0.5380 0.2545 -0.0217 0.069 Uiso 1 1 calc R U . . . H12C H 0.4929 0.3293 -0.0079 0.069 Uiso 1 1 calc R U . . . C13 C 0.4000(3) 0.5665(6) 0.2979(8) 0.116(4) Uani 1 1 d . . . . . H13 H 0.3965 0.5359 0.3528 0.139 Uiso 1 1 calc R U . B 3 C14 C 0.4543(4) 0.6019(7) 0.2987(9) 0.154(6) Uani 1 1 d . . . . . H14A H 0.4603 0.6372 0.2484 0.230 Uiso 1 1 calc R U . . . H14B H 0.4805 0.5529 0.3005 0.230 Uiso 1 1 calc R U . . . H14C H 0.4591 0.6396 0.3479 0.230 Uiso 1 1 calc R U . . . C15 C 0.3580(4) 0.6378(8) 0.3013(10) 0.177(7) Uani 1 1 d . . . . . H15A H 0.3665 0.6788 0.3468 0.266 Uiso 1 1 calc R U . . . H15B H 0.3223 0.6112 0.3108 0.266 Uiso 1 1 calc R U . . . H15C H 0.3578 0.6703 0.2485 0.266 Uiso 1 1 calc R U . . . C16 C 0.3200(2) 0.4443(5) 0.2345(4) 0.0501(17) Uani 1 1 d . . . . . H16 H 0.2969 0.4977 0.2242 0.060 Uiso 1 1 calc R U . B 3 C17 C 0.3091(4) 0.4112(9) 0.3201(7) 0.150(6) Uani 1 1 d . . . . . H17A H 0.2703 0.3987 0.3261 0.225 Uiso 1 1 calc R U . . . H17B H 0.3199 0.4563 0.3606 0.225 Uiso 1 1 calc R U . . . H17C H 0.3299 0.3567 0.3297 0.225 Uiso 1 1 calc R U . . . C18 C 0.3044(4) 0.3731(6) 0.1730(8) 0.121(4) Uani 1 1 d . . . . . H18A H 0.3237 0.3180 0.1865 0.182 Uiso 1 1 calc R U . . . H18B H 0.3142 0.3922 0.1167 0.182 Uiso 1 1 calc R U . . . H18C H 0.2652 0.3628 0.1758 0.182 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0549(3) 0.0375(3) 0.0473(3) -0.0027(2) -0.0019(2) -0.0023(2) Ag2 0.0430(3) 0.0375(3) 0.0405(3) 0.0079(2) 0.0037(2) 0.0086(2) Ag3 0.0313(2) 0.0301(2) 0.0497(3) -0.0007(2) 0.0009(2) 0.00480(18) S1 0.0300(8) 0.0267(7) 0.0668(11) 0.0017(7) 0.0002(7) 0.0008(6) S2A 0.0414(9) 0.0606(10) 0.0408(10) -0.0031(8) 0.0035(7) 0.0098(8) C5A 0.040(4) 0.061(4) 0.055(4) 0.002(3) 0.006(3) 0.012(3) C6A 0.051(6) 0.091(8) 0.119(10) 0.051(8) 0.033(6) 0.019(5) C7A 0.071(6) 0.067(6) 0.077(7) 0.004(5) 0.015(5) 0.023(5) C8A 0.041(5) 0.081(7) 0.078(7) -0.006(5) -0.007(5) 0.006(4) S2B 0.0414(9) 0.0606(10) 0.0408(10) -0.0031(8) 0.0035(7) 0.0098(8) C5B 0.040(4) 0.061(4) 0.055(4) 0.002(3) 0.006(3) 0.012(3) C6B 0.034(13) 0.068(16) 0.056(9) -0.003(8) 0.002(8) 0.012(11) C7B 0.049(14) 0.059(12) 0.057(11) 0.001(9) -0.004(9) 0.012(10) C8B 0.031(13) 0.060(9) 0.043(16) 0.000(8) 0.008(11) 0.011(7) S3 0.0392(8) 0.0254(7) 0.0359(9) -0.0024(6) 0.0001(6) 0.0031(6) P1A 0.0310(8) 0.0383(9) 0.0466(10) -0.0010(7) 0.0040(7) 0.0077(7) C19A 0.069(8) 0.092(11) 0.061(9) 0.029(8) 0.030(7) 0.035(8) C20A 0.073(8) 0.073(8) 0.046(7) 0.027(6) -0.004(6) 0.025(6) C21A 0.083(5) 0.070(5) 0.075(5) 0.016(4) 0.037(4) 0.025(4) P1B 0.0310(8) 0.0383(9) 0.0466(10) -0.0010(7) 0.0040(7) 0.0077(7) C19B 0.066(8) 0.061(18) 0.042(8) 0.013(8) 0.013(6) 0.027(7) C20B 0.067(9) 0.11(3) 0.044(11) 0.012(12) 0.012(8) 0.031(10) C21B 0.083(5) 0.070(5) 0.075(5) 0.016(4) 0.037(4) 0.025(4) C1 0.029(3) 0.028(3) 0.097(6) 0.011(4) 0.009(3) 0.006(3) C2 0.037(4) 0.047(4) 0.118(7) 0.009(4) -0.005(4) 0.008(3) C3 0.067(6) 0.064(5) 0.162(9) -0.053(6) -0.009(6) 0.023(4) C4 0.080(6) 0.078(6) 0.198(12) 0.083(7) 0.055(7) 0.035(5) C9 0.057(4) 0.029(3) 0.037(4) -0.003(3) -0.012(3) 0.007(3) C10 0.042(4) 0.067(4) 0.050(4) 0.007(4) -0.011(3) -0.003(3) C11 0.114(6) 0.028(3) 0.053(5) -0.009(3) -0.026(4) 0.011(4) C12 0.057(4) 0.045(4) 0.036(4) 0.005(3) 0.001(3) 0.012(3) C13 0.061(6) 0.072(6) 0.213(12) -0.082(7) -0.035(7) 0.030(5) C14 0.066(7) 0.094(8) 0.301(17) -0.124(10) -0.016(8) 0.001(6) C15 0.085(8) 0.137(10) 0.310(19) -0.137(12) -0.024(10) 0.046(7) C16 0.031(3) 0.068(5) 0.052(4) 0.009(4) -0.001(3) 0.012(3) C17 0.061(6) 0.255(15) 0.134(10) 0.116(10) 0.041(6) 0.037(8) C18 0.061(6) 0.067(6) 0.236(14) -0.048(7) -0.013(7) -0.005(5) _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 S1 2.4103(17) . ? Ag1 S2A 2.4299(18) . ? Ag1 S3 2.8183(17) . ? Ag1 Ag2 2.9869(12) . ? Ag1 Ag2 3.1416(12) 3 ? Ag2 S1 2.3774(17) 3 ? Ag2 S2A 2.4011(18) . ? Ag2 Ag1 3.1415(12) 3 ? Ag3 P1A 2.3819(16) . ? Ag3 S3 2.5123(16) 3 ? Ag3 S3 2.5946(15) . ? Ag3 Ag3 3.2108(14) 3 ? S1 C1 1.864(6) . ? S1 Ag2 2.3775(17) 3 ? S2A C5A 1.860(7) . ? C5A C6A 1.480(11) . ? C5A C8A 1.518(11) . ? C5A C7A 1.537(11) . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? S3 C9 1.861(6) . ? S3 Ag3 2.5123(16) 3 ? P1A C19A 1.798(12) . ? P1A C16 1.848(6) . ? P1A C13 1.852(8) . ? C19A C20A 1.390(14) . ? C19A C21A 1.496(14) . ? C19A H19A 1.0000 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C19B C20B 1.48(4) . ? C19B H19B 1.0000 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C1 C4 1.473(10) . ? C1 C2 1.489(8) . ? C1 C3 1.550(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C9 C10 1.518(8) . ? C9 C11 1.521(8) . ? C9 C12 1.528(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.442(12) . ? C13 C15 1.491(11) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.488(10) . ? C16 C18 1.509(11) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 S1 Ag1 S2A 162.90(6) . . ? S1 Ag1 S3 102.91(5) . . ? S2A Ag1 S3 94.08(5) . . ? S1 Ag1 Ag2 139.19(4) . . ? S2A Ag1 Ag2 51.38(4) . . ? S3 Ag1 Ag2 64.49(3) . . ? S1 Ag1 Ag2 48.54(4) . 3 ? S2A Ag1 Ag2 131.08(5) . 3 ? S3 Ag1 Ag2 98.87(3) . 3 ? Ag2 Ag1 Ag2 93.221(19) . 3 ? S1 Ag2 S2A 178.91(6) 3 . ? S1 Ag2 Ag1 128.82(5) 3 . ? S2A Ag2 Ag1 52.25(5) . . ? S1 Ag2 Ag1 49.45(4) 3 3 ? S2A Ag2 Ag1 131.29(4) . 3 ? Ag1 Ag2 Ag1 85.750(19) . 3 ? P1A Ag3 S3 141.48(5) . 3 ? P1A Ag3 S3 135.48(6) . . ? S3 Ag3 S3 82.26(6) 3 . ? P1A Ag3 Ag3 140.05(4) . 3 ? S3 Ag3 Ag3 52.20(3) 3 3 ? S3 Ag3 Ag3 49.91(4) . 3 ? C1 S1 Ag2 111.6(2) . 3 ? C1 S1 Ag1 107.8(2) . . ? Ag2 S1 Ag1 82.01(5) 3 . ? C5A S2A Ag2 111.7(2) . . ? C5A S2A Ag1 112.0(2) . . ? Ag2 S2A Ag1 76.38(5) . . ? C6A C5A C8A 113.0(8) . . ? C6A C5A C7A 110.4(7) . . ? C8A C5A C7A 109.3(6) . . ? C6A C5A S2A 107.9(5) . . ? C8A C5A S2A 109.4(5) . . ? C7A C5A S2A 106.6(5) . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5A C7A H7A1 109.5 . . ? C5A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C5A C8A H8A1 109.5 . . ? C5A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C5A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C9 S3 Ag3 112.7(2) . 3 ? C9 S3 Ag3 123.32(19) . . ? Ag3 S3 Ag3 77.89(5) 3 . ? C9 S3 Ag1 107.57(19) . . ? Ag3 S3 Ag1 89.53(5) 3 . ? Ag3 S3 Ag1 128.64(6) . . ? C19A P1A C16 107.9(5) . . ? C19A P1A C13 100.5(8) . . ? C16 P1A C13 102.4(4) . . ? C19A P1A Ag3 117.0(4) . . ? C16 P1A Ag3 113.7(2) . . ? C13 P1A Ag3 113.6(3) . . ? C20A C19A C21A 118.8(10) . . ? C20A C19A P1A 122.3(8) . . ? C21A C19A P1A 115.8(8) . . ? C20A C19A H19A 95.9 . . ? C21A C19A H19A 95.9 . . ? P1A C19A H19A 95.9 . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19A C21A H21A 109.5 . . ? C19A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C19A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20B C19B H19B 94.8 . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C4 C1 C2 113.1(7) . . ? C4 C1 C3 110.5(7) . . ? C2 C1 C3 107.8(6) . . ? C4 C1 S1 107.1(5) . . ? C2 C1 S1 111.7(4) . . ? C3 C1 S1 106.5(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C9 C11 110.5(5) . . ? C10 C9 C12 110.0(5) . . ? C11 C9 C12 110.3(5) . . ? C10 C9 S3 109.4(4) . . ? C11 C9 S3 108.3(4) . . ? C12 C9 S3 108.3(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 112.1(9) . . ? C14 C13 P1A 112.2(7) . . ? C15 C13 P1A 118.8(7) . . ? C14 C13 H13 103.9 . . ? C15 C13 H13 103.9 . . ? P1A C13 H13 103.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 108.8(9) . . ? C17 C16 P1A 111.6(5) . . ? C18 C16 P1A 110.5(5) . . ? C17 C16 H16 108.6 . . ? C18 C16 H16 108.6 . . ? P1A C16 H16 108.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag2 S2A C5A C6A -88.0(7) . . . . ? Ag1 S2A C5A C6A -171.5(6) . . . . ? Ag2 S2A C5A C8A 35.4(6) . . . . ? Ag1 S2A C5A C8A -48.2(6) . . . . ? Ag2 S2A C5A C7A 153.4(5) . . . . ? Ag1 S2A C5A C7A 69.9(5) . . . . ? C16 P1A C19A C20A 31.8(16) . . . . ? C13 P1A C19A C20A -75.0(15) . . . . ? Ag3 P1A C19A C20A 161.5(11) . . . . ? C16 P1A C19A C21A -127.8(11) . . . . ? C13 P1A C19A C21A 125.4(12) . . . . ? Ag3 P1A C19A C21A 1.9(15) . . . . ? Ag2 S1 C1 C4 93.1(6) 3 . . . ? Ag1 S1 C1 C4 -178.6(6) . . . . ? Ag2 S1 C1 C2 -31.3(6) 3 . . . ? Ag1 S1 C1 C2 57.0(6) . . . . ? Ag2 S1 C1 C3 -148.7(5) 3 . . . ? Ag1 S1 C1 C3 -60.4(5) . . . . ? Ag3 S3 C9 C10 60.0(4) 3 . . . ? Ag3 S3 C9 C10 -30.2(5) . . . . ? Ag1 S3 C9 C10 157.0(4) . . . . ? Ag3 S3 C9 C11 -60.5(5) 3 . . . ? Ag3 S3 C9 C11 -150.7(4) . . . . ? Ag1 S3 C9 C11 36.5(5) . . . . ? Ag3 S3 C9 C12 179.8(3) 3 . . . ? Ag3 S3 C9 C12 89.7(4) . . . . ? Ag1 S3 C9 C12 -83.1(4) . . . . ? C19A P1A C13 C14 -69.1(11) . . . . ? C16 P1A C13 C14 179.7(9) . . . . ? Ag3 P1A C13 C14 56.7(11) . . . . ? C19A P1A C13 C15 64.4(12) . . . . ? C16 P1A C13 C15 -46.8(12) . . . . ? Ag3 P1A C13 C15 -169.8(10) . . . . ? C19A P1A C16 C17 -167.3(9) . . . . ? C13 P1A C16 C17 -61.8(8) . . . . ? Ag3 P1A C16 C17 61.2(7) . . . . ? C19A P1A C16 C18 71.6(9) . . . . ? C13 P1A C16 C18 177.0(7) . . . . ? Ag3 P1A C16 C18 -60.0(6) . . . . ? _refine_diff_density_max 0.850 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.125 _shelxl_version_number 2012-9 _database_code_depnum_ccdc_archive 'CCDC 960485'