# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_cpag2h _database_code_depnum_ccdc_archive 'CCDC 781516' #TrackingRef 'cpag2h.cif' _audit_creation_date 2010-06-16T16:01:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C75 H62 Ag4 N8 O P4 S4' _chemical_formula_moiety 'C75 H62 Ag4 N8 O P4 S4' _chemical_formula_weight 1774.93 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.930(5) _cell_length_b 18.450(5) _cell_length_c 23.853(5) _cell_angle_alpha 90 _cell_angle_beta 105.522(5) _cell_angle_gamma 90 _cell_volume 7179(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8901 _cell_measurement_theta_min 2.4246 _cell_measurement_theta_max 31.4661 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.76845 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.0286175187 _diffrn_orient_matrix_ub_12 0.0102964685 _diffrn_orient_matrix_ub_13 -0.0264010097 _diffrn_orient_matrix_ub_21 0.0296828773 _diffrn_orient_matrix_ub_22 0.0234633394 _diffrn_orient_matrix_ub_23 -0.0064252871 _diffrn_orient_matrix_ub_31 0.0138889477 _diffrn_orient_matrix_ub_32 -0.0287129223 _diffrn_orient_matrix_ub_33 -0.0146972095 _diffrn_reflns_av_R_equivalents 0.1442 _diffrn_reflns_av_unetI/netI 0.1946 _diffrn_reflns_number 78695 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 14093 _reflns_number_gt 5973 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. The assignments of the N atoms of the py groups were made on the basis of possible close contacts, the location of the hyrdogen atoms and refinement. Geometries of two Ph rings were restrined to ideal values. ADPs of 7 Ph and py rings were restrined to resaonable values. ; _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^)+(0.0790P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 14093 _refine_ls_number_parameters 866 _refine_ls_number_restraints 279 _refine_ls_R_factor_all 0.1429 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1733 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 0.87 _refine_ls_restrained_S_all 0.867 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.138 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.209 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' P P 0.1023 0.0942 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.81174(4) 0.34910(4) 0.23900(3) 0.0305(2) Uani 1 1 d . . . Ag2 Ag 0.87128(4) 0.48474(4) 0.15427(3) 0.0293(2) Uani 1 1 d . . . Ag3 Ag 1.12797(4) 0.44936(4) 0.36128(3) 0.0321(2) Uani 1 1 d . . . Ag4 Ag 1.15024(5) 0.31912(4) 0.25135(4) 0.0407(2) Uani 1 1 d . . . P1 P 0.67195(15) 0.31022(14) 0.21508(11) 0.0267(6) Uani 1 1 d . . . C131 C 0.6338(6) 0.2711(5) 0.2732(4) 0.030(2) Uani 1 1 d . . . N132 N 0.6581(5) 0.3124(5) 0.3229(3) 0.038(2) Uani 1 1 d . . . C133 C 0.6322(7) 0.2915(6) 0.3682(5) 0.050(3) Uani 1 1 d . . . H133 H 0.6481 0.3195 0.4028 0.06 Uiso 1 1 calc R . . C134 C 0.5827(7) 0.2302(6) 0.3677(5) 0.044(3) Uani 1 1 d . . . H134 H 0.5653 0.2173 0.401 0.053 Uiso 1 1 calc R . . C135 C 0.5600(6) 0.1896(6) 0.3178(4) 0.039(3) Uani 1 1 d . . . H135 H 0.5273 0.1475 0.3166 0.047 Uiso 1 1 calc R . . C136 C 0.5846(6) 0.2098(5) 0.2695(4) 0.033(2) Uani 1 1 d . . . H136 H 0.5685 0.1825 0.2345 0.04 Uiso 1 1 calc R . . C111 C 0.6505(5) 0.2419(4) 0.1585(3) 0.026(2) Uani 1 1 d DU . . C116 C 0.6795(6) 0.1724(4) 0.1711(4) 0.033(2) Uani 1 1 d DU . . H116 H 0.7084 0.1613 0.2101 0.04 Uiso 1 1 calc R . . C115 C 0.6686(6) 0.1182(5) 0.1301(4) 0.037(3) Uani 1 1 d D . . H115 H 0.6872 0.0703 0.1407 0.045 Uiso 1 1 calc R . . C114 C 0.6300(6) 0.1356(5) 0.0731(4) 0.044(3) Uani 1 1 d D . . H114 H 0.6212 0.0994 0.0438 0.053 Uiso 1 1 calc R . . C113 C 0.6041(7) 0.2063(5) 0.0589(4) 0.050(3) Uani 1 1 d D . . H113 H 0.5797 0.2186 0.0194 0.06 Uiso 1 1 calc R . . C112 C 0.6130(7) 0.2590(5) 0.1011(4) 0.042(3) Uani 1 1 d D . . H112 H 0.5936 0.3068 0.0908 0.051 Uiso 1 1 calc R . . C121 C 0.5975(6) 0.3817(5) 0.1862(4) 0.028(2) Uani 1 1 d . . . C122 C 0.5150(7) 0.3739(5) 0.1847(5) 0.047(3) Uani 1 1 d . . . H122 H 0.4973 0.3314 0.2003 0.057 Uiso 1 1 calc R . . C123 C 0.4585(7) 0.4275(6) 0.1607(5) 0.051(3) Uani 1 1 d . . . H123 H 0.4025 0.4215 0.16 0.062 Uiso 1 1 calc R . . C124 C 0.4832(7) 0.4890(6) 0.1380(4) 0.046(3) Uani 1 1 d . . . H124 H 0.4445 0.5254 0.1209 0.055 Uiso 1 1 calc R . . C125 C 0.5638(7) 0.4975(6) 0.1402(5) 0.044(3) Uani 1 1 d . . . H125 H 0.5813 0.5405 0.1251 0.053 Uiso 1 1 calc R . . C126 C 0.6206(6) 0.4444(5) 0.1641(4) 0.035(3) Uani 1 1 d . . . H126 H 0.6766 0.4516 0.1653 0.041 Uiso 1 1 calc R . . P2 P 0.79069(16) 0.53428(13) 0.06383(10) 0.0275(6) Uani 1 1 d . . . C211 C 0.8545(5) 0.5686(5) 0.0181(4) 0.033(2) Uani 1 1 d DU . . C212 C 0.9387(5) 0.5711(6) 0.0411(4) 0.048(3) Uani 1 1 d DU . . H212 H 0.9626 0.5537 0.0794 0.057 Uiso 1 1 calc R . . C213 C 0.9880(7) 0.5990(7) 0.0087(4) 0.063(3) Uani 1 1 d DU . . H213 H 1.0453 0.6038 0.0254 0.076 Uiso 1 1 calc R . . C214 C 0.9533(6) 0.6196(6) -0.0478(4) 0.053(3) Uani 1 1 d DU . . H214 H 0.9869 0.6362 -0.0713 0.064 Uiso 1 1 calc R . . C215 C 0.8691(6) 0.6162(6) -0.0705(4) 0.051(3) Uani 1 1 d DU . . H215 H 0.8454 0.6309 -0.1096 0.062 Uiso 1 1 calc R . . C216 C 0.8194(6) 0.5919(5) -0.0375(3) 0.031(2) Uani 1 1 d DU . . H216 H 0.7615 0.5913 -0.053 0.037 Uiso 1 1 calc R . . C231 C 0.7204(6) 0.6075(5) 0.0672(4) 0.034(2) Uani 1 1 d U . . N232 N 0.6624(6) 0.6312(5) 0.0163(4) 0.059(2) Uani 1 1 d U . . C233 C 0.6088(7) 0.6862(6) 0.0212(5) 0.049(2) Uani 1 1 d U . . H233 H 0.5689 0.7026 -0.0124 0.059 Uiso 1 1 calc R . . C234 C 0.6128(7) 0.7169(5) 0.0740(5) 0.043(2) Uani 1 1 d U . . H234 H 0.576 0.7551 0.076 0.052 Uiso 1 1 calc R . . C235 C 0.6684(6) 0.6946(5) 0.1245(5) 0.037(2) Uani 1 1 d U . . H235 H 0.6702 0.7165 0.1609 0.044 Uiso 1 1 calc R . . C236 C 0.7220(6) 0.6388(5) 0.1205(4) 0.032(2) Uani 1 1 d U . . H236 H 0.7603 0.6218 0.1548 0.039 Uiso 1 1 calc R . . C221 C 0.7248(6) 0.4653(5) 0.0189(4) 0.034(3) Uani 1 1 d . . . C226 C 0.6439(7) 0.4586(6) 0.0187(4) 0.042(3) Uani 1 1 d . . . H226 H 0.621 0.4928 0.0397 0.05 Uiso 1 1 calc R . . C225 C 0.5955(8) 0.4038(7) -0.0108(5) 0.061(4) Uani 1 1 d . . . H225 H 0.54 0.3995 -0.0099 0.073 Uiso 1 1 calc R . . C224 C 0.6281(9) 0.3560(7) -0.0415(5) 0.059(4) Uani 1 1 d . . . H224 H 0.5943 0.3191 -0.0633 0.071 Uiso 1 1 calc R . . C223 C 0.7079(9) 0.3596(6) -0.0417(5) 0.049(3) Uani 1 1 d . . . H223 H 0.7302 0.3242 -0.062 0.059 Uiso 1 1 calc R . . C222 C 0.7570(7) 0.4152(6) -0.0121(4) 0.042(3) Uani 1 1 d . . . H222 H 0.8125 0.4189 -0.0132 0.051 Uiso 1 1 calc R . . P3 P 1.22686(15) 0.49848(14) 0.44484(10) 0.0279(6) Uani 1 1 d . . . C331 C 1.1812(5) 0.5375(5) 0.4992(4) 0.023(2) Uani 1 1 d U . . C336 C 1.0969(6) 0.5519(5) 0.4842(4) 0.030(2) Uani 1 1 d U . . H336 H 1.0636 0.5438 0.4459 0.036 Uiso 1 1 calc R . . C335 C 1.0635(7) 0.5788(5) 0.5277(5) 0.045(3) Uani 1 1 d . . . H335 H 1.0065 0.5894 0.5184 0.054 Uiso 1 1 calc R . . C334 C 1.1101(7) 0.5900(6) 0.5827(5) 0.041(3) Uani 1 1 d . . . H334 H 1.0857 0.6068 0.6118 0.049 Uiso 1 1 calc R . . C333 C 1.1905(8) 0.5773(5) 0.5957(4) 0.041(3) Uani 1 1 d . . . H333 H 1.2232 0.5877 0.6339 0.049 Uiso 1 1 calc R . . N332 N 1.2280(6) 0.5495(5) 0.5551(4) 0.051(3) Uani 1 1 d . . . C321 C 1.2917(5) 0.5711(5) 0.4288(4) 0.032(2) Uani 1 1 d U . . C322 C 1.3187(6) 0.5632(7) 0.3803(4) 0.049(3) Uani 1 1 d U . . H322 H 1.3074 0.5206 0.3572 0.058 Uiso 1 1 calc R . . C323 C 1.3654(7) 0.6221(8) 0.3655(5) 0.063(3) Uani 1 1 d U . . H323 H 1.3858 0.6185 0.3322 0.075 Uiso 1 1 calc R . . C324 C 1.3803(7) 0.6830(7) 0.3991(6) 0.060(3) Uani 1 1 d U . . H324 H 1.4092 0.7225 0.3885 0.072 Uiso 1 1 calc R . . C325 C 1.3535(7) 0.6867(7) 0.4481(6) 0.067(3) Uani 1 1 d U . . H325 H 1.3661 0.7281 0.4725 0.08 Uiso 1 1 calc R . . C326 C 1.3091(6) 0.6318(6) 0.4621(5) 0.044(3) Uani 1 1 d U . . H326 H 1.2897 0.6359 0.4959 0.053 Uiso 1 1 calc R . . C311 C 1.2992(6) 0.4337(5) 0.4896(4) 0.027(2) Uani 1 1 d U . . C316 C 1.2756(6) 0.3647(5) 0.4959(4) 0.033(2) Uani 1 1 d U . . H316 H 1.2234 0.3491 0.473 0.039 Uiso 1 1 calc R . . C315 C 1.3233(6) 0.3161(6) 0.5339(4) 0.038(3) Uani 1 1 d . . . H315 H 1.3051 0.268 0.5372 0.046 Uiso 1 1 calc R . . C314 C 1.3992(6) 0.3398(5) 0.5672(4) 0.035(3) Uani 1 1 d . . . H314 H 1.4332 0.3083 0.595 0.042 Uiso 1 1 calc R . . C313 C 1.4251(6) 0.4094(6) 0.5598(4) 0.039(3) Uani 1 1 d U . . H313 H 1.478 0.4247 0.5815 0.046 Uiso 1 1 calc R . . C312 C 1.3759(6) 0.4566(5) 0.5219(4) 0.024(2) Uani 1 1 d . . . H312 H 1.394 0.5045 0.5178 0.029 Uiso 1 1 calc R . . P4 P 1.27683(16) 0.25416(14) 0.27523(12) 0.0345(7) Uani 1 1 d . . . C411 C 1.3194(5) 0.2332(5) 0.2149(4) 0.028(2) Uani 1 1 d U . . C412 C 1.3066(6) 0.2823(5) 0.1707(4) 0.031(2) Uani 1 1 d U . . H412 H 1.277 0.3255 0.1724 0.037 Uiso 1 1 calc R . . C413 C 1.3359(7) 0.2696(6) 0.1248(5) 0.049(3) Uani 1 1 d U . . H413 H 1.3257 0.3042 0.0942 0.059 Uiso 1 1 calc R . . C414 C 1.3798(6) 0.2089(5) 0.1201(5) 0.040(2) Uani 1 1 d U . . H414 H 1.4005 0.2018 0.0872 0.049 Uiso 1 1 calc R . . C415 C 1.3935(6) 0.1586(5) 0.1638(4) 0.033(2) Uani 1 1 d U . . H415 H 1.4228 0.1155 0.1609 0.039 Uiso 1 1 calc R . . C416 C 1.3652(6) 0.1701(5) 0.2118(5) 0.037(2) Uani 1 1 d U . . H416 H 1.3763 0.1358 0.2427 0.045 Uiso 1 1 calc R . . C431 C 1.2687(5) 0.1659(5) 0.3076(4) 0.030(2) Uani 1 1 d . . . C436 C 1.1924(6) 0.1339(5) 0.2932(4) 0.026(2) Uani 1 1 d . . . H436 H 1.1466 0.1601 0.2706 0.032 Uiso 1 1 calc R . . C435 C 1.1818(6) 0.0647(5) 0.3111(4) 0.031(2) Uani 1 1 d . . . H435 H 1.1293 0.0425 0.2995 0.037 Uiso 1 1 calc R . . C434 C 1.2475(6) 0.0275(6) 0.3460(4) 0.034(3) Uani 1 1 d . . . H434 H 1.2405 -0.0204 0.3586 0.041 Uiso 1 1 calc R . . C433 C 1.3220(6) 0.0596(5) 0.3622(4) 0.033(2) Uani 1 1 d . . . H433 H 1.3662 0.0342 0.3874 0.039 Uiso 1 1 calc R . . N432 N 1.3362(5) 0.1290(5) 0.3431(4) 0.050(3) Uani 1 1 d . . . C421 C 1.3589(6) 0.3033(5) 0.3268(5) 0.037(2) Uani 1 1 d U . . C422 C 1.3778(7) 0.2930(6) 0.3845(5) 0.047(3) Uani 1 1 d U . . H422 H 1.3516 0.2554 0.3999 0.057 Uiso 1 1 calc R . . C423 C 1.4361(8) 0.3374(7) 0.4224(6) 0.065(3) Uani 1 1 d U . . H423 H 1.4508 0.3284 0.4631 0.078 Uiso 1 1 calc R . . C424 C 1.4704(9) 0.3917(7) 0.4009(7) 0.077(4) Uani 1 1 d U . . H424 H 1.5103 0.4214 0.4263 0.093 Uiso 1 1 calc R . . C425 C 1.4486(8) 0.4052(7) 0.3423(7) 0.078(4) Uani 1 1 d U . . H425 H 1.4722 0.4452 0.3276 0.094 Uiso 1 1 calc R . . C426 C 1.3921(7) 0.3610(6) 0.3035(6) 0.056(3) Uani 1 1 d U . . H426 H 1.377 0.3702 0.2628 0.067 Uiso 1 1 calc R . . N1 N 0.9279(5) 0.3144(4) 0.3002(3) 0.0263(19) Uani 1 1 d . . . C1 C 0.9968(6) 0.3114(5) 0.3222(4) 0.024(2) Uani 1 1 d . . . S1 S 1.09722(15) 0.30807(13) 0.35524(11) 0.0310(6) Uani 1 1 d . . . N2 N 1.0099(5) 0.4976(4) 0.1878(3) 0.0285(19) Uani 1 1 d . . . C2 C 1.0714(6) 0.4816(5) 0.2173(4) 0.021(2) Uani 1 1 d . . . S2 S 1.16433(15) 0.46051(13) 0.26034(10) 0.0296(6) Uani 1 1 d . . . N3 N 0.9954(5) 0.4915(4) 0.3287(3) 0.0259(18) Uani 1 1 d . . . C3 C 0.9307(6) 0.4923(5) 0.2977(4) 0.024(2) Uani 1 1 d . . . S3 S 0.83507(14) 0.49341(13) 0.25347(10) 0.0251(6) Uani 1 1 d . . . N4 N 1.0272(5) 0.3078(4) 0.1890(3) 0.031(2) Uani 1 1 d . . . C4 C 0.9592(6) 0.3218(5) 0.1689(4) 0.025(2) Uani 1 1 d . . . S4 S 0.86184(15) 0.33885(13) 0.13910(10) 0.0281(6) Uani 1 1 d . . . C11 C 0.6315(6) 0.5249(6) 0.3100(5) 0.045(3) Uani 1 1 d . . . H11A H 0.6629 0.5388 0.3493 0.067 Uiso 1 1 calc R . . H11B H 0.6681 0.5229 0.2844 0.067 Uiso 1 1 calc R . . H11C H 0.6066 0.4772 0.3112 0.067 Uiso 1 1 calc R . . C12 C 0.5658(7) 0.5795(6) 0.2872(4) 0.038(3) Uani 1 1 d . . . O12 O 0.4948(5) 0.5659(4) 0.2865(3) 0.055(2) Uani 1 1 d . . . C13 C 0.5897(8) 0.6478(6) 0.2651(5) 0.060(3) Uani 1 1 d . . . H13A H 0.5413 0.6788 0.2515 0.09 Uiso 1 1 calc R . . H13B H 0.6134 0.6377 0.2326 0.09 Uiso 1 1 calc R . . H13C H 0.6303 0.6726 0.2962 0.09 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 0.0174(4) 0.0393(5) 0.0321(5) -0.0014(4) 0.0019(3) -0.0042(3) Ag2 0.0242(4) 0.0360(5) 0.0240(4) 0.0038(3) -0.0003(3) 0.0031(3) Ag3 0.0221(4) 0.0428(5) 0.0249(4) -0.0027(4) -0.0048(3) 0.0005(4) Ag4 0.0236(5) 0.0395(5) 0.0597(6) 0.0070(4) 0.0122(4) 0.0086(4) P1 0.0158(14) 0.0311(16) 0.0298(15) -0.0010(12) 0.0003(12) -0.0035(11) C131 0.025(6) 0.028(6) 0.034(6) -0.006(5) 0.005(5) 0.002(5) N132 0.039(6) 0.052(6) 0.023(5) 0.001(4) 0.007(4) -0.001(4) C133 0.043(8) 0.059(9) 0.044(8) -0.019(6) 0.002(6) 0.007(6) C134 0.046(8) 0.046(8) 0.045(8) 0.005(6) 0.019(6) 0.011(6) C135 0.020(6) 0.052(7) 0.041(7) 0.004(6) 0.002(5) -0.005(5) C136 0.023(6) 0.046(7) 0.030(6) -0.002(5) 0.006(5) -0.003(5) C111 0.024(5) 0.030(5) 0.021(5) 0.011(4) 0.001(4) 0.005(4) C116 0.040(6) 0.037(6) 0.018(5) 0.012(5) 0.000(5) 0.006(5) C115 0.031(6) 0.051(7) 0.028(6) 0.005(5) 0.002(5) 0.010(5) C114 0.041(7) 0.034(7) 0.058(8) -0.007(6) 0.015(6) 0.004(5) C113 0.058(8) 0.052(8) 0.030(7) -0.006(6) -0.008(6) 0.010(6) C112 0.064(8) 0.013(6) 0.045(7) 0.003(5) 0.006(6) 0.015(5) C121 0.017(6) 0.034(6) 0.029(6) -0.011(5) -0.001(5) 0.001(4) C122 0.044(8) 0.028(7) 0.071(9) 0.015(6) 0.020(7) -0.001(5) C123 0.029(7) 0.036(7) 0.092(10) 0.013(7) 0.021(7) 0.015(5) C124 0.043(8) 0.045(8) 0.050(7) 0.022(6) 0.013(6) 0.025(6) C125 0.048(8) 0.034(7) 0.048(7) 0.009(5) 0.008(6) -0.002(6) C126 0.026(6) 0.028(6) 0.051(7) 0.006(5) 0.012(5) 0.001(5) P2 0.0296(15) 0.0300(16) 0.0216(14) 0.0016(11) 0.0045(12) 0.0057(12) C211 0.041(5) 0.030(6) 0.029(5) 0.000(4) 0.012(4) 0.009(5) C212 0.033(5) 0.072(7) 0.040(6) 0.019(5) 0.012(4) 0.007(5) C213 0.040(6) 0.098(8) 0.058(7) 0.025(6) 0.023(5) 0.003(6) C214 0.065(6) 0.062(7) 0.044(6) 0.008(5) 0.035(6) 0.007(6) C215 0.075(7) 0.044(6) 0.034(6) 0.007(5) 0.012(5) -0.005(6) C216 0.037(5) 0.027(5) 0.023(5) 0.001(4) -0.001(4) -0.001(4) C231 0.025(5) 0.041(5) 0.040(5) 0.007(4) 0.016(4) 0.014(4) N232 0.056(5) 0.067(5) 0.053(5) 0.015(4) 0.011(4) 0.026(4) C233 0.047(5) 0.049(6) 0.051(5) 0.017(5) 0.012(5) 0.020(4) C234 0.041(5) 0.035(5) 0.059(5) 0.007(4) 0.022(5) 0.009(4) C235 0.035(5) 0.032(5) 0.050(5) -0.007(4) 0.022(4) 0.000(4) C236 0.026(5) 0.028(5) 0.045(5) -0.001(4) 0.015(4) -0.002(4) C221 0.038(7) 0.044(7) 0.014(5) 0.010(5) -0.005(5) 0.011(5) C226 0.041(7) 0.049(8) 0.035(7) 0.002(5) 0.009(6) -0.010(6) C225 0.058(9) 0.072(10) 0.054(8) -0.002(7) 0.016(7) -0.019(8) C224 0.081(11) 0.056(9) 0.039(8) -0.004(6) 0.011(7) -0.023(8) C223 0.096(11) 0.020(7) 0.038(7) -0.005(5) 0.029(7) 0.009(7) C222 0.053(8) 0.040(7) 0.043(7) -0.006(6) 0.027(6) 0.004(6) P3 0.0183(14) 0.0391(17) 0.0229(14) -0.0016(12) 0.0000(11) -0.0007(12) C331 0.017(5) 0.030(5) 0.020(5) -0.001(4) -0.002(4) -0.009(4) C336 0.030(5) 0.033(6) 0.024(5) -0.008(4) 0.004(5) -0.001(5) C335 0.032(7) 0.039(7) 0.074(9) -0.001(6) 0.031(7) 0.008(5) C334 0.042(8) 0.047(7) 0.038(7) -0.003(6) 0.022(6) -0.004(6) C333 0.068(9) 0.046(7) 0.011(5) 0.001(5) 0.015(6) 0.000(6) N332 0.046(6) 0.063(7) 0.037(6) 0.009(5) -0.004(5) 0.005(5) C321 0.011(5) 0.050(6) 0.028(5) 0.011(4) -0.003(4) 0.011(4) C322 0.024(6) 0.088(7) 0.029(6) -0.003(5) -0.002(5) -0.007(5) C323 0.030(6) 0.114(9) 0.046(7) 0.027(6) 0.013(6) -0.001(6) C324 0.033(6) 0.072(7) 0.072(8) 0.045(6) 0.006(6) 0.002(6) C325 0.048(7) 0.057(7) 0.102(8) 0.004(6) 0.033(7) -0.009(6) C326 0.041(6) 0.036(6) 0.065(7) 0.007(5) 0.033(5) 0.008(5) C311 0.021(5) 0.041(6) 0.015(5) 0.001(4) 0.000(4) 0.002(4) C316 0.019(5) 0.043(6) 0.033(6) 0.005(5) 0.001(5) -0.004(5) C315 0.032(7) 0.038(7) 0.040(7) 0.015(5) 0.001(5) 0.006(5) C314 0.036(7) 0.035(7) 0.029(6) 0.009(5) -0.001(5) 0.010(5) C313 0.028(5) 0.044(6) 0.032(5) 0.004(5) -0.012(4) 0.003(5) C312 0.029(6) 0.017(5) 0.023(5) 0.002(4) -0.001(5) 0.006(4) P4 0.0205(15) 0.0348(17) 0.0493(18) 0.0049(13) 0.0114(14) 0.0040(12) C411 0.011(5) 0.033(5) 0.037(5) -0.004(4) 0.003(4) 0.002(4) C412 0.025(5) 0.026(5) 0.042(6) 0.006(4) 0.009(5) 0.011(4) C413 0.052(7) 0.048(6) 0.039(6) 0.002(5) 0.000(5) 0.007(5) C414 0.042(6) 0.037(6) 0.045(6) -0.004(4) 0.016(5) -0.007(5) C415 0.026(5) 0.029(5) 0.042(6) -0.004(4) 0.006(5) -0.003(4) C416 0.037(6) 0.026(5) 0.053(6) 0.010(5) 0.020(5) 0.003(4) C431 0.007(5) 0.052(7) 0.031(6) -0.004(5) 0.004(4) -0.001(5) C436 0.032(6) 0.030(6) 0.018(5) -0.005(4) 0.008(5) 0.007(5) C435 0.023(6) 0.038(7) 0.032(6) 0.000(5) 0.006(5) -0.002(5) C434 0.028(6) 0.043(7) 0.032(6) 0.002(5) 0.007(5) -0.016(5) C433 0.026(6) 0.035(7) 0.037(6) 0.014(5) 0.008(5) -0.001(5) N432 0.037(6) 0.064(7) 0.040(6) -0.002(5) -0.004(5) 0.013(5) C421 0.024(5) 0.037(6) 0.058(6) -0.003(5) 0.022(5) 0.005(4) C422 0.041(7) 0.055(7) 0.054(6) -0.014(5) 0.027(5) -0.008(5) C423 0.061(8) 0.067(8) 0.076(7) -0.034(6) 0.036(6) -0.012(6) C424 0.068(8) 0.061(8) 0.109(8) -0.038(7) 0.034(7) -0.017(6) C425 0.062(8) 0.053(7) 0.126(9) -0.004(7) 0.035(8) -0.024(6) C426 0.041(7) 0.039(7) 0.087(7) 0.015(5) 0.016(6) -0.003(5) N1 0.011(5) 0.039(5) 0.024(5) -0.001(4) -0.003(4) 0.000(4) C1 0.036(7) 0.020(5) 0.022(5) 0.000(4) 0.016(5) 0.001(5) S1 0.0200(14) 0.0353(16) 0.0323(15) 0.0063(12) -0.0024(12) 0.0036(11) N2 0.015(5) 0.041(5) 0.024(5) 0.004(4) -0.005(4) -0.003(4) C2 0.019(6) 0.023(5) 0.020(5) 0.001(4) 0.006(5) -0.001(4) S2 0.0231(14) 0.0379(16) 0.0263(14) 0.0036(11) 0.0039(12) -0.0001(11) N3 0.017(5) 0.031(5) 0.024(5) -0.002(4) -0.003(4) -0.003(4) C3 0.033(6) 0.018(5) 0.027(6) -0.002(4) 0.016(5) -0.001(4) S3 0.0180(13) 0.0297(15) 0.0243(13) -0.0005(11) -0.0002(11) -0.0004(10) N4 0.032(6) 0.029(5) 0.036(5) -0.005(4) 0.014(5) 0.002(4) C4 0.029(6) 0.027(6) 0.021(5) -0.005(4) 0.011(5) 0.003(5) S4 0.0257(14) 0.0286(15) 0.0262(14) -0.0022(11) 0.0006(11) -0.0012(11) C11 0.029(6) 0.050(8) 0.050(7) -0.006(6) 0.002(6) 0.002(5) C12 0.044(8) 0.043(7) 0.029(6) -0.005(5) 0.012(6) 0.001(6) O12 0.038(5) 0.069(6) 0.051(5) 0.014(4) -0.004(4) -0.003(4) C13 0.070(9) 0.038(7) 0.070(9) 0.014(6) 0.014(7) -0.005(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.207(8) . ? Ag1 P1 2.391(3) . ? Ag1 S3 2.700(3) . ? Ag1 S4 2.742(3) . ? Ag2 N2 2.280(8) . ? Ag2 P2 2.403(3) . ? Ag2 S3 2.603(2) . ? Ag2 S4 2.715(3) . ? Ag3 N3 2.305(8) . ? Ag3 P3 2.411(3) . ? Ag3 S2 2.648(2) . ? Ag3 S1 2.655(3) . ? Ag4 N4 2.222(9) . ? Ag4 P4 2.387(3) . ? Ag4 S2 2.623(3) . ? Ag4 S1 2.860(3) . ? P1 C111 1.811(9) . ? P1 C121 1.827(10) . ? P1 C131 1.828(10) . ? C131 N132 1.376(11) . ? C131 C136 1.394(12) . ? N132 C133 1.326(13) . ? C133 C134 1.406(14) . ? C133 H133 0.95 . ? C134 C135 1.370(14) . ? C134 H134 0.95 . ? C135 C136 1.377(13) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C111 C116 1.376(8) . ? C111 C112 1.383(8) . ? C116 C115 1.377(8) . ? C116 H116 0.95 . ? C115 C114 1.378(8) . ? C115 H115 0.95 . ? C114 C113 1.389(8) . ? C114 H114 0.95 . ? C113 C112 1.378(8) . ? C113 H113 0.95 . ? C112 H112 0.95 . ? C121 C126 1.372(12) . ? C121 C122 1.395(13) . ? C122 C123 1.388(13) . ? C122 H122 0.95 . ? C123 C124 1.370(14) . ? C123 H123 0.95 . ? C124 C125 1.360(14) . ? C124 H124 0.95 . ? C125 C126 1.385(13) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? P2 C231 1.816(9) . ? P2 C221 1.836(10) . ? P2 C211 1.841(9) . ? C211 C216 1.370(8) . ? C211 C212 1.385(8) . ? C212 C213 1.380(8) . ? C212 H212 0.95 . ? C213 C214 1.372(8) . ? C213 H213 0.95 . ? C214 C215 1.384(8) . ? C214 H214 0.95 . ? C215 C216 1.372(8) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C231 C236 1.389(12) . ? C231 N232 1.412(13) . ? N232 C233 1.387(13) . ? C233 C234 1.366(14) . ? C233 H233 0.95 . ? C234 C235 1.379(14) . ? C234 H234 0.95 . ? C235 C236 1.392(12) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? C221 C226 1.374(13) . ? C221 C222 1.383(13) . ? C226 C225 1.372(14) . ? C226 H226 0.95 . ? C225 C224 1.354(16) . ? C225 H225 0.95 . ? C224 C223 1.354(16) . ? C224 H224 0.95 . ? C223 C222 1.389(15) . ? C223 H223 0.95 . ? C222 H222 0.95 . ? P3 C331 1.826(9) . ? P3 C321 1.835(10) . ? P3 C311 1.836(9) . ? C331 N332 1.375(11) . ? C331 C336 1.401(12) . ? C336 C335 1.398(13) . ? C336 H336 0.95 . ? C335 C334 1.353(14) . ? C335 H335 0.95 . ? C334 C333 1.333(14) . ? C334 H334 0.95 . ? C333 N332 1.390(12) . ? C333 H333 0.95 . ? C321 C322 1.361(13) . ? C321 C326 1.360(13) . ? C322 C323 1.442(15) . ? C322 H322 0.95 . ? C323 C324 1.365(17) . ? C323 H323 0.95 . ? C324 C325 1.362(16) . ? C324 H324 0.95 . ? C325 C326 1.356(14) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C311 C316 1.355(12) . ? C311 C312 1.386(12) . ? C316 C315 1.373(13) . ? C316 H316 0.95 . ? C315 C314 1.389(13) . ? C315 H315 0.95 . ? C314 C313 1.383(13) . ? C314 H314 0.95 . ? C313 C312 1.366(12) . ? C313 H313 0.95 . ? C312 H312 0.95 . ? P4 C411 1.814(9) . ? P4 C431 1.822(10) . ? P4 C421 1.831(11) . ? C411 C412 1.364(12) . ? C411 C416 1.413(12) . ? C412 C413 1.338(13) . ? C412 H412 0.95 . ? C413 C414 1.364(13) . ? C413 H413 0.95 . ? C414 C415 1.369(13) . ? C414 H414 0.95 . ? C415 C416 1.370(12) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C431 C436 1.378(12) . ? C431 N432 1.403(12) . ? C436 C435 1.374(12) . ? C436 H436 0.95 . ? C435 C434 1.381(13) . ? C435 H435 0.95 . ? C434 C433 1.352(12) . ? C434 H434 0.95 . ? C433 N432 1.402(12) . ? C433 H433 0.95 . ? C421 C422 1.339(14) . ? C421 C426 1.387(13) . ? C422 C423 1.409(15) . ? C422 H422 0.95 . ? C423 C424 1.329(16) . ? C423 H423 0.95 . ? C424 C425 1.370(18) . ? C424 H424 0.95 . ? C425 C426 1.400(17) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? N1 C1 1.146(11) . ? C1 S1 1.672(11) . ? N2 C2 1.129(10) . ? C2 S2 1.678(10) . ? N3 C3 1.146(11) . ? C3 S3 1.679(11) . ? N4 C4 1.152(11) . ? C4 S4 1.642(10) . ? C11 C12 1.491(14) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 O12 1.224(12) . ? C12 C13 1.464(14) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 P1 136.1(2) . . ? N1 Ag1 S3 97.3(2) . . ? P1 Ag1 S3 115.34(8) . . ? N1 Ag1 S4 97.27(19) . . ? P1 Ag1 S4 106.77(8) . . ? S3 Ag1 S4 96.34(7) . . ? N2 Ag2 P2 123.99(19) . . ? N2 Ag2 S3 98.37(19) . . ? P2 Ag2 S3 125.26(8) . . ? N2 Ag2 S4 99.7(2) . . ? P2 Ag2 S4 104.97(8) . . ? S3 Ag2 S4 99.34(7) . . ? N3 Ag3 P3 123.39(19) . . ? N3 Ag3 S2 96.29(19) . . ? P3 Ag3 S2 116.34(8) . . ? N3 Ag3 S1 98.83(19) . . ? P3 Ag3 S1 119.79(8) . . ? S2 Ag3 S1 96.71(8) . . ? N4 Ag4 P4 137.1(2) . . ? N4 Ag4 S2 101.4(2) . . ? P4 Ag4 S2 115.06(9) . . ? N4 Ag4 S1 96.8(2) . . ? P4 Ag4 S1 103.14(9) . . ? S2 Ag4 S1 92.45(7) . . ? C111 P1 C121 104.0(4) . . ? C111 P1 C131 104.5(4) . . ? C121 P1 C131 102.8(4) . . ? C111 P1 Ag1 112.0(3) . . ? C121 P1 Ag1 114.4(3) . . ? C131 P1 Ag1 117.7(3) . . ? N132 C131 C136 122.7(9) . . ? N132 C131 P1 110.5(7) . . ? C136 C131 P1 126.8(7) . . ? C133 N132 C131 116.9(9) . . ? N132 C133 C134 123.5(10) . . ? N132 C133 H133 118.2 . . ? C134 C133 H133 118.2 . . ? C135 C134 C133 118.4(10) . . ? C135 C134 H134 120.8 . . ? C133 C134 H134 120.8 . . ? C134 C135 C136 120.0(10) . . ? C134 C135 H135 120 . . ? C136 C135 H135 120 . . ? C135 C136 C131 118.4(9) . . ? C135 C136 H136 120.8 . . ? C131 C136 H136 120.8 . . ? C116 C111 C112 118.2(8) . . ? C116 C111 P1 119.8(6) . . ? C112 C111 P1 121.7(6) . . ? C111 C116 C115 123.3(9) . . ? C111 C116 H116 118.4 . . ? C115 C116 H116 118.4 . . ? C116 C115 C114 118.0(9) . . ? C116 C115 H115 121 . . ? C114 C115 H115 121 . . ? C115 C114 C113 119.7(9) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C112 C113 C114 121.2(9) . . ? C112 C113 H113 119.4 . . ? C114 C113 H113 119.4 . . ? C113 C112 C111 119.5(8) . . ? C113 C112 H112 120.2 . . ? C111 C112 H112 120.2 . . ? C126 C121 C122 117.6(9) . . ? C126 C121 P1 121.0(7) . . ? C122 C121 P1 121.4(8) . . ? C123 C122 C121 120.8(9) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C124 C123 C122 120.2(10) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C125 C124 C123 119.3(10) . . ? C125 C124 H124 120.3 . . ? C123 C124 H124 120.3 . . ? C124 C125 C126 120.9(10) . . ? C124 C125 H125 119.6 . . ? C126 C125 H125 119.6 . . ? C121 C126 C125 121.1(9) . . ? C121 C126 H126 119.4 . . ? C125 C126 H126 119.4 . . ? C231 P2 C221 103.8(5) . . ? C231 P2 C211 105.4(4) . . ? C221 P2 C211 104.7(4) . . ? C231 P2 Ag2 117.6(3) . . ? C221 P2 Ag2 111.7(3) . . ? C211 P2 Ag2 112.4(3) . . ? C216 C211 C212 120.5(9) . . ? C216 C211 P2 120.7(7) . . ? C212 C211 P2 118.8(6) . . ? C213 C212 C211 120.2(9) . . ? C213 C212 H212 119.9 . . ? C211 C212 H212 119.9 . . ? C214 C213 C212 119.3(10) . . ? C214 C213 H213 120.3 . . ? C212 C213 H213 120.3 . . ? C213 C214 C215 119.8(10) . . ? C213 C214 H214 120.1 . . ? C215 C214 H214 120.1 . . ? C216 C215 C214 121.0(10) . . ? C216 C215 H215 119.5 . . ? C214 C215 H215 119.5 . . ? C211 C216 C215 119.0(9) . . ? C211 C216 H216 120.5 . . ? C215 C216 H216 120.5 . . ? C236 C231 N232 119.8(9) . . ? C236 C231 P2 119.8(8) . . ? N232 C231 P2 120.3(7) . . ? C233 N232 C231 118.3(9) . . ? C234 C233 N232 120.6(10) . . ? C234 C233 H233 119.7 . . ? N232 C233 H233 119.7 . . ? C233 C234 C235 122.4(10) . . ? C233 C234 H234 118.8 . . ? C235 C234 H234 118.8 . . ? C234 C235 C236 117.8(10) . . ? C234 C235 H235 121.1 . . ? C236 C235 H235 121.1 . . ? C235 C236 C231 121.1(10) . . ? C235 C236 H236 119.4 . . ? C231 C236 H236 119.4 . . ? C226 C221 C222 118.3(10) . . ? C226 C221 P2 120.8(8) . . ? C222 C221 P2 120.7(8) . . ? C225 C226 C221 121.7(11) . . ? C225 C226 H226 119.2 . . ? C221 C226 H226 119.2 . . ? C224 C225 C226 118.9(12) . . ? C224 C225 H225 120.5 . . ? C226 C225 H225 120.5 . . ? C223 C224 C225 121.5(12) . . ? C223 C224 H224 119.3 . . ? C225 C224 H224 119.3 . . ? C224 C223 C222 119.7(10) . . ? C224 C223 H223 120.2 . . ? C222 C223 H223 120.2 . . ? C221 C222 C223 119.9(11) . . ? C221 C222 H222 120 . . ? C223 C222 H222 120 . . ? C331 P3 C321 104.5(4) . . ? C331 P3 C311 100.8(4) . . ? C321 P3 C311 104.7(4) . . ? C331 P3 Ag3 113.8(3) . . ? C321 P3 Ag3 115.1(3) . . ? C311 P3 Ag3 116.3(3) . . ? N332 C331 C336 120.0(8) . . ? N332 C331 P3 120.6(7) . . ? C336 C331 P3 119.4(7) . . ? C335 C336 C331 117.7(9) . . ? C335 C336 H336 121.1 . . ? C331 C336 H336 121.1 . . ? C334 C335 C336 121.7(10) . . ? C334 C335 H335 119.1 . . ? C336 C335 H335 119.1 . . ? C333 C334 C335 119.6(10) . . ? C333 C334 H334 120.2 . . ? C335 C334 H334 120.2 . . ? C334 C333 N332 122.0(10) . . ? C334 C333 H333 119 . . ? N332 C333 H333 119 . . ? C331 N332 C333 118.9(9) . . ? C322 C321 C326 121.0(10) . . ? C322 C321 P3 117.0(8) . . ? C326 C321 P3 121.9(8) . . ? C321 C322 C323 117.3(11) . . ? C321 C322 H322 121.4 . . ? C323 C322 H322 121.4 . . ? C324 C323 C322 120.2(11) . . ? C324 C323 H323 119.9 . . ? C322 C323 H323 119.9 . . ? C325 C324 C323 119.6(12) . . ? C325 C324 H324 120.2 . . ? C323 C324 H324 120.2 . . ? C326 C325 C324 120.5(13) . . ? C326 C325 H325 119.7 . . ? C324 C325 H325 119.7 . . ? C325 C326 C321 121.2(11) . . ? C325 C326 H326 119.4 . . ? C321 C326 H326 119.4 . . ? C316 C311 C312 119.0(9) . . ? C316 C311 P3 120.4(7) . . ? C312 C311 P3 120.3(7) . . ? C311 C316 C315 123.2(10) . . ? C311 C316 H316 118.4 . . ? C315 C316 H316 118.4 . . ? C316 C315 C314 117.6(10) . . ? C316 C315 H315 121.2 . . ? C314 C315 H315 121.2 . . ? C313 C314 C315 119.7(9) . . ? C313 C314 H314 120.2 . . ? C315 C314 H314 120.2 . . ? C312 C313 C314 121.2(9) . . ? C312 C313 H313 119.4 . . ? C314 C313 H313 119.4 . . ? C313 C312 C311 119.3(9) . . ? C313 C312 H312 120.4 . . ? C311 C312 H312 120.4 . . ? C411 P4 C431 103.7(4) . . ? C411 P4 C421 104.3(4) . . ? C431 P4 C421 106.7(5) . . ? C411 P4 Ag4 116.1(3) . . ? C431 P4 Ag4 112.6(3) . . ? C421 P4 Ag4 112.5(3) . . ? C412 C411 C416 118.8(9) . . ? C412 C411 P4 117.3(7) . . ? C416 C411 P4 123.9(7) . . ? C413 C412 C411 120.1(9) . . ? C413 C412 H412 120 . . ? C411 C412 H412 120 . . ? C412 C413 C414 122.6(10) . . ? C412 C413 H413 118.7 . . ? C414 C413 H413 118.7 . . ? C413 C414 C415 118.7(10) . . ? C413 C414 H414 120.7 . . ? C415 C414 H414 120.7 . . ? C414 C415 C416 120.4(9) . . ? C414 C415 H415 119.8 . . ? C416 C415 H415 119.8 . . ? C415 C416 C411 119.4(9) . . ? C415 C416 H416 120.3 . . ? C411 C416 H416 120.3 . . ? C436 C431 N432 120.0(9) . . ? C436 C431 P4 116.7(7) . . ? N432 C431 P4 123.2(7) . . ? C435 C436 C431 120.9(9) . . ? C435 C436 H436 119.6 . . ? C431 C436 H436 119.6 . . ? C436 C435 C434 119.9(9) . . ? C436 C435 H435 120.1 . . ? C434 C435 H435 120.1 . . ? C433 C434 C435 119.6(9) . . ? C433 C434 H434 120.2 . . ? C435 C434 H434 120.2 . . ? C434 C433 N432 122.4(9) . . ? C434 C433 H433 118.8 . . ? N432 C433 H433 118.8 . . ? C431 N432 C433 117.2(9) . . ? C422 C421 C426 120.6(11) . . ? C422 C421 P4 123.3(8) . . ? C426 C421 P4 115.3(9) . . ? C421 C422 C423 120.7(11) . . ? C421 C422 H422 119.7 . . ? C423 C422 H422 119.7 . . ? C424 C423 C422 119.7(14) . . ? C424 C423 H423 120.2 . . ? C422 C423 H423 120.2 . . ? C423 C424 C425 120.2(14) . . ? C423 C424 H424 119.9 . . ? C425 C424 H424 119.9 . . ? C424 C425 C426 121.2(13) . . ? C424 C425 H425 119.4 . . ? C426 C425 H425 119.4 . . ? C421 C426 C425 117.4(12) . . ? C421 C426 H426 121.3 . . ? C425 C426 H426 121.3 . . ? C1 N1 Ag1 159.4(7) . . ? N1 C1 S1 179.0(9) . . ? C1 S1 Ag3 98.6(3) . . ? C1 S1 Ag4 96.0(3) . . ? Ag3 S1 Ag4 82.80(7) . . ? C2 N2 Ag2 152.0(7) . . ? N2 C2 S2 177.9(9) . . ? C2 S2 Ag4 97.5(3) . . ? C2 S2 Ag3 99.6(3) . . ? Ag4 S2 Ag3 87.65(7) . . ? C3 N3 Ag3 153.9(7) . . ? N3 C3 S3 178.7(8) . . ? C3 S3 Ag2 98.5(3) . . ? C3 S3 Ag1 98.7(3) . . ? Ag2 S3 Ag1 83.41(7) . . ? C4 N4 Ag4 155.6(7) . . ? N4 C4 S4 177.9(9) . . ? C4 S4 Ag2 96.7(3) . . ? C4 S4 Ag1 98.4(3) . . ? Ag2 S4 Ag1 80.60(7) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O12 C12 C13 122.4(10) . . ? O12 C12 C11 120.1(10) . . ? C13 C12 C11 117.5(10) . . ? 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 . . ? data_cpscn2 _database_code_depnum_ccdc_archive 'CCDC 781517' #TrackingRef 'cpscn2.cif' _audit_creation_date 2010-06-16T21:07:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C76 H132 Ag4 N4 P4 S4' _chemical_formula_moiety 'C76 H132 Ag4 N4 P4 S4' _chemical_formula_weight 1785.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7034(3) _cell_length_b 14.9825(3) _cell_length_c 26.2157(7) _cell_angle_alpha 90 _cell_angle_beta 99.792(3) _cell_angle_gamma 90 _cell_volume 4142.80(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12267 _cell_measurement_theta_min 3.2915 _cell_measurement_theta_max 32.5654 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.87897 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0000596209 _diffrn_orient_matrix_ub_12 -0.0213548242 _diffrn_orient_matrix_ub_13 -0.0241639669 _diffrn_orient_matrix_ub_21 -0.0648399368 _diffrn_orient_matrix_ub_22 -0.0112789785 _diffrn_orient_matrix_ub_23 -0.0012913046 _diffrn_orient_matrix_ub_31 -0.0179304748 _diffrn_orient_matrix_ub_32 0.0407551912 _diffrn_orient_matrix_ub_33 -0.0130035855 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_unetI/netI 0.1535 _diffrn_reflns_number 58819 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 32.65 _diffrn_reflns_theta_full 31.75 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.936 _reflns_number_total 14210 _reflns_number_gt 6603 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. One phenyl ring was found to be disordered over two sites C11n and C14n with occupancies set at 0.5 after trial refinement. Disordered atoms were refined with isotropic ADPs after refinement with anisotropic refinement, even with reasonable restraints, was not successful. ADP's for phenyl ring C21n were restrained to reasonable values. ; _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^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 14210 _refine_ls_number_parameters 408 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.098 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 0.784 _refine_ls_restrained_S_all 0.789 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.732 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 0.346171(18) 0.540693(12) 0.501065(6) 0.02731(5) Uani 1 1 d . . . Ag2 Ag 0.46652(2) 0.397949(13) 0.701870(6) 0.03358(6) Uani 1 1 d . A . P1 P 0.22880(6) 0.65936(4) 0.45364(2) 0.02419(14) Uani 1 1 d . . . C111 C 0.0740(5) 0.6849(3) 0.47428(17) 0.0166(11) Uiso 0.5 1 d P A 1 H111 H 0.0093 0.6437 0.4548 0.02 Uiso 0.5 1 calc PR A 1 C112 C 0.0242(7) 0.7793(5) 0.4647(3) 0.0228(7) Uiso 0.5 1 d P A 1 H11A H 0.0891 0.8212 0.4823 0.027 Uiso 0.5 1 calc PR A 1 H11B H 0.0134 0.7915 0.4271 0.027 Uiso 0.5 1 calc PR A 1 C113 C -0.0968(4) 0.7984(3) 0.48227(16) 0.0198(10) Uiso 0.5 1 d P A 1 H11C H -0.1652 0.7619 0.4622 0.024 Uiso 0.5 1 calc PR A 1 H11D H -0.1189 0.8621 0.4763 0.024 Uiso 0.5 1 calc PR A 1 C114 C -0.0849(5) 0.7767(3) 0.54040(16) 0.0224(10) Uiso 0.5 1 d P A 1 H11E H -0.0237 0.8183 0.5606 0.027 Uiso 0.5 1 calc PR A 1 H11F H -0.1681 0.7851 0.5514 0.027 Uiso 0.5 1 calc PR A 1 C115 C -0.0408(5) 0.6823(3) 0.55124(18) 0.0220(10) Uiso 0.5 1 d P A 1 H11G H -0.1065 0.6409 0.5337 0.026 Uiso 0.5 1 calc PR A 1 H11H H -0.0308 0.6711 0.5889 0.026 Uiso 0.5 1 calc PR A 1 C116 C 0.0840(4) 0.6626(3) 0.53321(14) 0.0139(9) Uiso 0.5 1 d P A 1 H11I H 0.1058 0.5988 0.5391 0.017 Uiso 0.5 1 calc PR A 1 H11J H 0.1523 0.6988 0.5535 0.017 Uiso 0.5 1 calc PR A 1 C141 C 0.1054(5) 0.7017(3) 0.4902(2) 0.0233(12) Uiso 0.5 1 d P A 2 H141 H 0.1522 0.7148 0.5258 0.028 Uiso 0.5 1 calc PR A 2 C142 C 0.0391(8) 0.7901(5) 0.4715(3) 0.0228(7) Uiso 0.5 1 d P A 2 H14A H -0.0065 0.7838 0.4355 0.027 Uiso 0.5 1 calc PR A 2 H14B H 0.1022 0.8386 0.4724 0.027 Uiso 0.5 1 calc PR A 2 C143 C -0.0575(5) 0.8122(3) 0.5091(2) 0.0344(12) Uiso 0.5 1 d P A 2 H14C H -0.0086 0.8297 0.5431 0.041 Uiso 0.5 1 calc PR A 2 H14D H -0.1091 0.8643 0.4951 0.041 Uiso 0.5 1 calc PR A 2 C144 C -0.1445(5) 0.7381(3) 0.51720(19) 0.0351(12) Uiso 0.5 1 d P A 2 H14E H -0.2036 0.7268 0.4845 0.042 Uiso 0.5 1 calc PR A 2 H14F H -0.1954 0.7563 0.5436 0.042 Uiso 0.5 1 calc PR A 2 C145 C -0.0739(5) 0.6528(3) 0.53451(18) 0.0281(12) Uiso 0.5 1 d P A 2 H14G H -0.1358 0.6042 0.5361 0.034 Uiso 0.5 1 calc PR A 2 H14H H -0.0248 0.6613 0.5697 0.034 Uiso 0.5 1 calc PR A 2 C146 C 0.0174(5) 0.6257(3) 0.49718(18) 0.0311(11) Uiso 0.5 1 d P A 2 H14I H 0.0677 0.5732 0.5113 0.037 Uiso 0.5 1 calc PR A 2 H14J H -0.0324 0.609 0.4632 0.037 Uiso 0.5 1 calc PR A 2 C121 C 0.1737(2) 0.62843(15) 0.38523(8) 0.0252(5) Uani 1 1 d . A . H121 H 0.2525 0.6177 0.3704 0.03 Uiso 1 1 calc R . . C122 C 0.0987(2) 0.69825(15) 0.35003(8) 0.0258(5) Uani 1 1 d . . . H12A H 0.1456 0.7555 0.353 0.031 Uiso 1 1 calc R A . H12B H 0.0156 0.7084 0.3609 0.031 Uiso 1 1 calc R . . C123 C 0.0783(2) 0.66606(16) 0.29375(8) 0.0313(6) Uani 1 1 d . A . H12C H 0.0271 0.7106 0.2714 0.038 Uiso 1 1 calc R . . H12D H 0.1613 0.6606 0.2822 0.038 Uiso 1 1 calc R . . C124 C 0.0110(2) 0.57651(15) 0.28800(8) 0.0282(6) Uani 1 1 d . . . H12E H 0.0039 0.5558 0.2518 0.034 Uiso 1 1 calc R A . H12F H -0.0759 0.5837 0.2957 0.034 Uiso 1 1 calc R . . C125 C 0.0818(2) 0.50612(16) 0.32439(8) 0.0305(6) Uani 1 1 d . A . H12G H 0.1647 0.4932 0.314 0.037 Uiso 1 1 calc R . . H12H H 0.032 0.4501 0.3216 0.037 Uiso 1 1 calc R . . C126 C 0.1030(2) 0.53924(15) 0.38055(8) 0.0260(5) Uani 1 1 d . . . H12I H 0.0202 0.5466 0.3921 0.031 Uiso 1 1 calc R A . H12J H 0.1528 0.4945 0.4033 0.031 Uiso 1 1 calc R . . C131 C 0.3205(2) 0.76232(15) 0.44971(8) 0.0231(5) Uani 1 1 d . A . H131 H 0.2633 0.8079 0.43 0.028 Uiso 1 1 calc R . . C132 C 0.3708(2) 0.79981(16) 0.50372(8) 0.0281(6) Uani 1 1 d . . . H13A H 0.2984 0.8138 0.5214 0.034 Uiso 1 1 calc R A . H13B H 0.4234 0.754 0.5244 0.034 Uiso 1 1 calc R . . C133 C 0.4494(2) 0.88343(16) 0.50109(9) 0.0341(6) Uani 1 1 d . A . H13C H 0.4825 0.9044 0.5366 0.041 Uiso 1 1 calc R . . H13D H 0.395 0.9311 0.483 0.041 Uiso 1 1 calc R . . C134 C 0.5597(3) 0.86582(18) 0.47261(10) 0.0427(7) Uani 1 1 d . . . H13E H 0.6185 0.8222 0.4923 0.051 Uiso 1 1 calc R A . H13F H 0.6069 0.922 0.4699 0.051 Uiso 1 1 calc R . . C135 C 0.5113(3) 0.82950(17) 0.41865(10) 0.0412(7) Uani 1 1 d . A . H13G H 0.5843 0.8158 0.4013 0.049 Uiso 1 1 calc R . . H13H H 0.4591 0.8756 0.398 0.049 Uiso 1 1 calc R . . C136 C 0.4322(2) 0.74526(15) 0.42071(9) 0.0294(6) Uani 1 1 d . . . H13I H 0.4866 0.6973 0.4384 0.035 Uiso 1 1 calc R A . H13J H 0.399 0.725 0.385 0.035 Uiso 1 1 calc R . . P2 P 0.55063(7) 0.36163(4) 0.78986(2) 0.02811(15) Uani 1 1 d . . . C211 C 0.6495(2) 0.45077(16) 0.82448(8) 0.0314(6) Uani 1 1 d U . . H211 H 0.5905 0.4993 0.8314 0.038 Uiso 1 1 calc R . . C212 C 0.7267(3) 0.42440(19) 0.87644(9) 0.0425(7) Uani 1 1 d U . . H21A H 0.7819 0.3733 0.8715 0.051 Uiso 1 1 calc R . . H21B H 0.6685 0.405 0.8999 0.051 Uiso 1 1 calc R . . C213 C 0.8081(3) 0.5008(2) 0.90149(10) 0.0561(8) Uani 1 1 d U . . H21C H 0.8611 0.4795 0.9339 0.067 Uiso 1 1 calc R . . H21D H 0.7526 0.5491 0.9106 0.067 Uiso 1 1 calc R . . C214 C 0.8940(3) 0.5380(2) 0.86531(11) 0.0600(8) Uani 1 1 d U . . H21E H 0.9428 0.5894 0.8821 0.072 Uiso 1 1 calc R . . H21F H 0.955 0.4915 0.8587 0.072 Uiso 1 1 calc R . . C215 C 0.8159(3) 0.5676(2) 0.81450(11) 0.0557(8) Uani 1 1 d U . . H21G H 0.873 0.5891 0.7911 0.067 Uiso 1 1 calc R . . H21H H 0.7601 0.6176 0.8208 0.067 Uiso 1 1 calc R . . C216 C 0.7352(3) 0.49065(17) 0.78870(9) 0.0405(6) Uani 1 1 d U . . H21I H 0.7915 0.4434 0.7791 0.049 Uiso 1 1 calc R . . H21J H 0.6817 0.5124 0.7565 0.049 Uiso 1 1 calc R . . C221 C 0.6571(3) 0.26340(16) 0.79213(8) 0.0325(6) Uani 1 1 d . . . H221 H 0.745 0.2878 0.7952 0.039 Uiso 1 1 calc R . . C222 C 0.6590(3) 0.20009(18) 0.83818(10) 0.0461(8) Uani 1 1 d . . . H22A H 0.5734 0.1747 0.8375 0.055 Uiso 1 1 calc R . . H22B H 0.6829 0.2336 0.8709 0.055 Uiso 1 1 calc R . . C223 C 0.7550(3) 0.12400(19) 0.83571(12) 0.0572(9) Uani 1 1 d . . . H22C H 0.8416 0.1493 0.8398 0.069 Uiso 1 1 calc R . . H22D H 0.7523 0.0821 0.8647 0.069 Uiso 1 1 calc R . . C224 C 0.7267(3) 0.07372(19) 0.78499(13) 0.0588(9) Uani 1 1 d . . . H22E H 0.6428 0.0445 0.7819 0.071 Uiso 1 1 calc R . . H22F H 0.7913 0.0267 0.7843 0.071 Uiso 1 1 calc R . . C225 C 0.7269(3) 0.13706(17) 0.73953(11) 0.0484(8) Uani 1 1 d . . . H22G H 0.8128 0.1626 0.7411 0.058 Uiso 1 1 calc R . . H22H H 0.7054 0.1035 0.7067 0.058 Uiso 1 1 calc R . . C226 C 0.6315(3) 0.21230(16) 0.74064(9) 0.0371(7) Uani 1 1 d . . . H22I H 0.5448 0.1871 0.7356 0.045 Uiso 1 1 calc R . . H22J H 0.6363 0.2541 0.7118 0.045 Uiso 1 1 calc R . . C231 C 0.4290(2) 0.33363(16) 0.82928(8) 0.0281(6) Uani 1 1 d . . . H231 H 0.4717 0.3073 0.8628 0.034 Uiso 1 1 calc R . . C232 C 0.3362(3) 0.26476(17) 0.80103(9) 0.0379(7) Uani 1 1 d . . . H23A H 0.2989 0.2883 0.7665 0.045 Uiso 1 1 calc R . . H23B H 0.383 0.2094 0.7958 0.045 Uiso 1 1 calc R . . C233 C 0.2301(2) 0.24266(17) 0.83104(9) 0.0380(7) Uani 1 1 d . . . H23C H 0.2664 0.2137 0.8642 0.046 Uiso 1 1 calc R . . H23D H 0.1704 0.2001 0.8108 0.046 Uiso 1 1 calc R . . C234 C 0.1586(3) 0.32665(19) 0.84184(11) 0.0465(7) Uani 1 1 d . . . H23E H 0.093 0.3112 0.8628 0.056 Uiso 1 1 calc R . . H23F H 0.1157 0.3527 0.8088 0.056 Uiso 1 1 calc R . . C235 C 0.2500(3) 0.39490(19) 0.87083(11) 0.0471(7) Uani 1 1 d . . . H23G H 0.203 0.4501 0.8762 0.057 Uiso 1 1 calc R . . H23H H 0.2869 0.3708 0.9053 0.057 Uiso 1 1 calc R . . C236 C 0.3564(3) 0.41702(17) 0.84075(9) 0.0376(6) Uani 1 1 d . . . H23I H 0.4159 0.4595 0.8611 0.045 Uiso 1 1 calc R . . H23J H 0.3199 0.4464 0.8077 0.045 Uiso 1 1 calc R . . S1 S 0.56985(6) 0.58797(4) 0.55882(2) 0.02636(14) Uani 1 1 d . . . C1 C 0.5551(2) 0.52977(15) 0.61146(9) 0.0266(5) Uani 1 1 d . A . N1 N 0.54568(19) 0.49048(14) 0.64861(7) 0.0337(5) Uani 1 1 d . . . S2 S 0.27522(6) 0.33432(4) 0.64414(2) 0.03252(15) Uani 1 1 d . . . C2 C 0.2836(2) 0.39818(16) 0.59311(8) 0.0290(6) Uani 1 1 d . A . N2 N 0.2882(2) 0.44192(14) 0.55726(7) 0.0353(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03231(11) 0.02826(10) 0.02135(9) 0.00628(7) 0.00456(7) 0.01008(9) Ag2 0.04668(13) 0.03555(11) 0.01949(9) 0.00705(8) 0.00842(8) 0.01726(10) P1 0.0245(4) 0.0264(3) 0.0229(3) 0.0064(2) 0.0077(3) 0.0078(3) C121 0.0197(13) 0.0309(14) 0.0256(12) 0.0072(10) 0.0057(10) 0.0038(11) C122 0.0244(14) 0.0251(13) 0.0267(12) 0.0079(10) 0.0011(10) 0.0018(11) C123 0.0309(15) 0.0395(15) 0.0216(12) 0.0116(10) -0.0004(10) -0.0014(12) C124 0.0289(15) 0.0307(14) 0.0237(12) 0.0024(10) 0.0013(10) 0.0033(12) C125 0.0358(16) 0.0265(14) 0.0297(13) 0.0016(10) 0.0067(11) 0.0081(12) C126 0.0322(15) 0.0223(13) 0.0241(11) 0.0061(9) 0.0062(10) 0.0057(12) C131 0.0249(14) 0.0246(13) 0.0210(11) 0.0053(9) 0.0072(10) 0.0085(11) C132 0.0232(14) 0.0361(15) 0.0262(12) 0.0026(10) 0.0079(10) 0.0040(12) C133 0.0342(16) 0.0344(16) 0.0372(14) -0.0038(11) 0.0157(12) 0.0033(13) C134 0.0407(18) 0.0316(16) 0.0617(18) -0.0116(13) 0.0254(14) -0.0069(14) C135 0.0482(19) 0.0316(15) 0.0526(16) 0.0003(12) 0.0336(14) -0.0028(14) C136 0.0330(15) 0.0260(14) 0.0332(13) 0.0017(10) 0.0174(11) 0.0001(12) P2 0.0414(4) 0.0242(3) 0.0199(3) 0.0055(2) 0.0085(3) 0.0108(3) C211 0.0393(15) 0.0342(14) 0.0230(11) 0.0004(10) 0.0115(10) 0.0071(12) C212 0.0436(16) 0.0592(17) 0.0252(12) -0.0023(11) 0.0076(11) 0.0127(14) C213 0.0510(18) 0.074(2) 0.0416(15) -0.0191(14) 0.0040(13) 0.0115(16) C214 0.0493(18) 0.070(2) 0.0633(18) -0.0288(15) 0.0176(15) -0.0048(17) C215 0.0597(19) 0.0536(18) 0.0611(17) -0.0194(14) 0.0309(15) -0.0095(16) C216 0.0507(17) 0.0374(15) 0.0380(13) -0.0042(11) 0.0200(12) -0.0034(13) C221 0.0408(17) 0.0295(14) 0.0310(13) 0.0117(10) 0.0166(12) 0.0108(12) C222 0.0501(19) 0.0432(18) 0.0503(16) 0.0261(13) 0.0241(14) 0.0233(15) C223 0.055(2) 0.0443(19) 0.079(2) 0.0398(17) 0.0311(18) 0.0225(17) C224 0.053(2) 0.0293(16) 0.103(3) 0.0142(17) 0.0365(19) 0.0152(16) C225 0.055(2) 0.0228(15) 0.074(2) -0.0027(14) 0.0315(16) 0.0009(15) C226 0.0465(18) 0.0237(14) 0.0461(15) 0.0004(11) 0.0218(13) 0.0065(13) C231 0.0308(15) 0.0315(14) 0.0224(12) 0.0064(10) 0.0053(10) 0.0115(12) C232 0.0488(18) 0.0311(15) 0.0336(14) 0.0062(11) 0.0065(12) 0.0048(14) C233 0.0338(16) 0.0399(16) 0.0381(14) 0.0075(12) -0.0006(12) 0.0011(14) C234 0.0298(17) 0.0528(19) 0.0540(17) 0.0040(14) -0.0012(13) 0.0038(15) C235 0.0277(16) 0.0494(19) 0.0664(19) -0.0138(15) 0.0143(14) 0.0030(15) C236 0.0367(17) 0.0381(16) 0.0371(14) -0.0039(12) 0.0032(12) 0.0062(14) S1 0.0301(4) 0.0284(3) 0.0207(3) 0.0034(2) 0.0047(2) 0.0070(3) C1 0.0232(14) 0.0320(14) 0.0243(12) -0.0014(10) 0.0036(10) 0.0098(12) N1 0.0286(13) 0.0498(14) 0.0229(10) 0.0063(10) 0.0046(9) 0.0054(11) S2 0.0409(4) 0.0342(4) 0.0245(3) 0.0080(3) 0.0116(3) 0.0057(3) C2 0.0308(15) 0.0322(14) 0.0242(12) -0.0007(11) 0.0055(10) 0.0068(12) N2 0.0395(14) 0.0403(13) 0.0263(11) 0.0077(9) 0.0058(9) 0.0078(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. Atom of one phenyl rings were disordered over two sets of sites C11n and C14n with occupancy factors set at 0.5 after trial refinement. These disordered atoms were refined with isotropic ADPs since anisotropic refinement was not successful even with restrained parameters. ADPs of ring C21n were restrained to realistic values. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.249(2) . ? Ag1 P1 2.3987(6) . ? Ag1 S1 2.7005(6) . ? Ag1 S1 2.7328(6) 3_666 ? Ag2 N1 2.234(2) . ? Ag2 P2 2.3918(6) . ? Ag2 S2 2.5174(7) . ? P1 C131 1.841(2) . ? P1 C121 1.849(2) . ? P1 C111 1.868(5) . ? P1 C141 1.870(5) . ? C111 C112 1.517(9) . ? C111 C116 1.566(6) . ? C111 H111 1 . ? C112 C113 1.474(9) . ? C112 H11A 0.99 . ? C112 H11B 0.99 . ? C113 C114 1.542(6) . ? C113 H11C 0.99 . ? C113 H11D 0.99 . ? C114 C115 1.503(6) . ? C114 H11E 0.99 . ? C114 H11F 0.99 . ? C115 C116 1.519(6) . ? C115 H11G 0.99 . ? C115 H11H 0.99 . ? C116 H11I 0.99 . ? C116 H11J 0.99 . ? C141 C146 1.509(7) . ? C141 C142 1.543(9) . ? C141 H141 1 . ? C142 C143 1.580(9) . ? C142 H14A 0.99 . ? C142 H14B 0.99 . ? C143 C144 1.487(7) . ? C143 H14C 0.99 . ? C143 H14D 0.99 . ? C144 C145 1.514(7) . ? C144 H14E 0.99 . ? C144 H14F 0.99 . ? C145 C146 1.550(7) . ? C145 H14G 0.99 . ? C145 H14H 0.99 . ? C146 H14I 0.99 . ? C146 H14J 0.99 . ? C121 C122 1.529(3) . ? C121 C126 1.530(3) . ? C121 H121 1 . ? C122 C123 1.532(3) . ? C122 H12A 0.99 . ? C122 H12B 0.99 . ? C123 C124 1.518(3) . ? C123 H12C 0.99 . ? C123 H12D 0.99 . ? C124 C125 1.533(3) . ? C124 H12E 0.99 . ? C124 H12F 0.99 . ? C125 C126 1.533(3) . ? C125 H12G 0.99 . ? C125 H12H 0.99 . ? C126 H12I 0.99 . ? C126 H12J 0.99 . ? C131 C132 1.533(3) . ? C131 C136 1.543(3) . ? C131 H131 1 . ? C132 C133 1.517(3) . ? C132 H13A 0.99 . ? C132 H13B 0.99 . ? C133 C134 1.524(3) . ? C133 H13C 0.99 . ? C133 H13D 0.99 . ? C134 C135 1.522(4) . ? C134 H13E 0.99 . ? C134 H13F 0.99 . ? C135 C136 1.526(3) . ? C135 H13G 0.99 . ? C135 H13H 0.99 . ? C136 H13I 0.99 . ? C136 H13J 0.99 . ? P2 C231 1.843(2) . ? P2 C211 1.844(3) . ? P2 C221 1.856(2) . ? C211 C212 1.520(3) . ? C211 C216 1.539(3) . ? C211 H211 1 . ? C212 C213 1.519(4) . ? C212 H21A 0.99 . ? C212 H21B 0.99 . ? C213 C214 1.533(4) . ? C213 H21C 0.99 . ? C213 H21D 0.99 . ? C214 C215 1.513(4) . ? C214 H21E 0.99 . ? C214 H21F 0.99 . ? C215 C216 1.528(4) . ? C215 H21G 0.99 . ? C215 H21H 0.99 . ? C216 H21I 0.99 . ? C216 H21J 0.99 . ? C221 C222 1.533(3) . ? C221 C226 1.535(3) . ? C221 H221 1 . ? C222 C223 1.543(4) . ? C222 H22A 0.99 . ? C222 H22B 0.99 . ? C223 C224 1.513(4) . ? C223 H22C 0.99 . ? C223 H22D 0.99 . ? C224 C225 1.524(4) . ? C224 H22E 0.99 . ? C224 H22F 0.99 . ? C225 C226 1.525(3) . ? C225 H22G 0.99 . ? C225 H22H 0.99 . ? C226 H22I 0.99 . ? C226 H22J 0.99 . ? C231 C236 1.528(3) . ? C231 C232 1.533(3) . ? C231 H231 1 . ? C232 C233 1.524(3) . ? C232 H23A 0.99 . ? C232 H23B 0.99 . ? C233 C234 1.524(4) . ? C233 H23C 0.99 . ? C233 H23D 0.99 . ? C234 C235 1.525(4) . ? C234 H23E 0.99 . ? C234 H23F 0.99 . ? C235 C236 1.528(4) . ? C235 H23G 0.99 . ? C235 H23H 0.99 . ? C236 H23I 0.99 . ? C236 H23J 0.99 . ? S1 C1 1.663(2) . ? S1 Ag1 2.7328(6) 3_666 ? C1 N1 1.157(3) . ? S2 C2 1.660(2) . ? C2 N2 1.153(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 P1 130.45(6) . . ? N2 Ag1 S1 97.03(6) . . ? P1 Ag1 S1 115.62(2) . . ? N2 Ag1 S1 93.81(5) . 3_666 ? P1 Ag1 S1 114.806(19) . 3_666 ? S1 Ag1 S1 99.220(17) . 3_666 ? N1 Ag2 P2 128.56(5) . . ? N1 Ag2 S2 102.44(5) . . ? P2 Ag2 S2 128.89(2) . . ? C131 P1 C121 103.94(10) . . ? C131 P1 C111 110.65(17) . . ? C121 P1 C111 100.37(17) . . ? C131 P1 C141 100.02(17) . . ? C121 P1 C141 116.48(19) . . ? C131 P1 Ag1 114.38(7) . . ? C121 P1 Ag1 111.68(7) . . ? C111 P1 Ag1 114.43(14) . . ? C141 P1 Ag1 109.83(15) . . ? C112 C111 C116 108.9(4) . . ? C112 C111 P1 116.5(4) . . ? C116 C111 P1 109.1(3) . . ? C112 C111 H111 107.3 . . ? C116 C111 H111 107.3 . . ? P1 C111 H111 107.3 . . ? C113 C112 C111 115.6(6) . . ? C113 C112 H11A 108.4 . . ? C111 C112 H11A 108.4 . . ? C113 C112 H11B 108.4 . . ? C111 C112 H11B 108.4 . . ? H11A C112 H11B 107.4 . . ? C112 C113 C114 109.8(4) . . ? C112 C113 H11C 109.7 . . ? C114 C113 H11C 109.7 . . ? C112 C113 H11D 109.7 . . ? C114 C113 H11D 109.7 . . ? H11C C113 H11D 108.2 . . ? C115 C114 C113 110.8(4) . . ? C115 C114 H11E 109.5 . . ? C113 C114 H11E 109.5 . . ? C115 C114 H11F 109.5 . . ? C113 C114 H11F 109.5 . . ? H11E C114 H11F 108.1 . . ? C114 C115 C116 112.8(4) . . ? C114 C115 H11G 109 . . ? C116 C115 H11G 109 . . ? C114 C115 H11H 109 . . ? C116 C115 H11H 109 . . ? H11G C115 H11H 107.8 . . ? C115 C116 C111 110.5(3) . . ? C115 C116 H11I 109.6 . . ? C111 C116 H11I 109.6 . . ? C115 C116 H11J 109.6 . . ? C111 C116 H11J 109.6 . . ? H11I C116 H11J 108.1 . . ? C146 C141 C142 115.0(5) . . ? C146 C141 P1 108.4(3) . . ? C142 C141 P1 117.1(4) . . ? C146 C141 H141 105 . . ? C142 C141 H141 105 . . ? P1 C141 H141 105 . . ? C141 C142 C143 107.2(6) . . ? C141 C142 H14A 110.3 . . ? C143 C142 H14A 110.3 . . ? C141 C142 H14B 110.3 . . ? C143 C142 H14B 110.3 . . ? H14A C142 H14B 108.5 . . ? C144 C143 C142 115.1(5) . . ? C144 C143 H14C 108.5 . . ? C142 C143 H14C 108.5 . . ? C144 C143 H14D 108.5 . . ? C142 C143 H14D 108.5 . . ? H14C C143 H14D 107.5 . . ? C143 C144 C145 112.3(4) . . ? C143 C144 H14E 109.1 . . ? C145 C144 H14E 109.1 . . ? C143 C144 H14F 109.1 . . ? C145 C144 H14F 109.1 . . ? H14E C144 H14F 107.9 . . ? C144 C145 C146 111.6(4) . . ? C144 C145 H14G 109.3 . . ? C146 C145 H14G 109.3 . . ? C144 C145 H14H 109.3 . . ? C146 C145 H14H 109.3 . . ? H14G C145 H14H 108 . . ? C141 C146 C145 110.6(4) . . ? C141 C146 H14I 109.5 . . ? C145 C146 H14I 109.5 . . ? C141 C146 H14J 109.5 . . ? C145 C146 H14J 109.5 . . ? H14I C146 H14J 108.1 . . ? C122 C121 C126 110.30(18) . . ? C122 C121 P1 117.51(16) . . ? C126 C121 P1 111.61(14) . . ? C122 C121 H121 105.5 . . ? C126 C121 H121 105.5 . . ? P1 C121 H121 105.5 . . ? C121 C122 C123 109.87(19) . . ? C121 C122 H12A 109.7 . . ? C123 C122 H12A 109.7 . . ? C121 C122 H12B 109.7 . . ? C123 C122 H12B 109.7 . . ? H12A C122 H12B 108.2 . . ? C124 C123 C122 111.19(18) . . ? C124 C123 H12C 109.4 . . ? C122 C123 H12C 109.4 . . ? C124 C123 H12D 109.4 . . ? C122 C123 H12D 109.4 . . ? H12C C123 H12D 108 . . ? C123 C124 C125 111.72(19) . . ? C123 C124 H12E 109.3 . . ? C125 C124 H12E 109.3 . . ? C123 C124 H12F 109.3 . . ? C125 C124 H12F 109.3 . . ? H12E C124 H12F 107.9 . . ? C124 C125 C126 110.58(18) . . ? C124 C125 H12G 109.5 . . ? C126 C125 H12G 109.5 . . ? C124 C125 H12H 109.5 . . ? C126 C125 H12H 109.5 . . ? H12G C125 H12H 108.1 . . ? C121 C126 C125 110.48(18) . . ? C121 C126 H12I 109.6 . . ? C125 C126 H12I 109.6 . . ? C121 C126 H12J 109.6 . . ? C125 C126 H12J 109.6 . . ? H12I C126 H12J 108.1 . . ? C132 C131 C136 109.65(19) . . ? C132 C131 P1 111.22(15) . . ? C136 C131 P1 110.73(15) . . ? C132 C131 H131 108.4 . . ? C136 C131 H131 108.4 . . ? P1 C131 H131 108.4 . . ? C133 C132 C131 111.76(19) . . ? C133 C132 H13A 109.3 . . ? C131 C132 H13A 109.3 . . ? C133 C132 H13B 109.3 . . ? C131 C132 H13B 109.3 . . ? H13A C132 H13B 107.9 . . ? C132 C133 C134 111.2(2) . . ? C132 C133 H13C 109.4 . . ? C134 C133 H13C 109.4 . . ? C132 C133 H13D 109.4 . . ? C134 C133 H13D 109.4 . . ? H13C C133 H13D 108 . . ? C133 C134 C135 110.4(2) . . ? C133 C134 H13E 109.6 . . ? C135 C134 H13E 109.6 . . ? C133 C134 H13F 109.6 . . ? C135 C134 H13F 109.6 . . ? H13E C134 H13F 108.1 . . ? C134 C135 C136 111.5(2) . . ? C134 C135 H13G 109.3 . . ? C136 C135 H13G 109.3 . . ? C134 C135 H13H 109.3 . . ? C136 C135 H13H 109.3 . . ? H13G C135 H13H 108 . . ? C135 C136 C131 111.20(19) . . ? C135 C136 H13I 109.4 . . ? C131 C136 H13I 109.4 . . ? C135 C136 H13J 109.4 . . ? C131 C136 H13J 109.4 . . ? H13I C136 H13J 108 . . ? C231 P2 C211 106.84(10) . . ? C231 P2 C221 106.86(11) . . ? C211 P2 C221 105.10(12) . . ? C231 P2 Ag2 114.00(8) . . ? C211 P2 Ag2 113.60(7) . . ? C221 P2 Ag2 109.86(7) . . ? C212 C211 C216 111.0(2) . . ? C212 C211 P2 115.57(18) . . ? C216 C211 P2 109.43(15) . . ? C212 C211 H211 106.8 . . ? C216 C211 H211 106.8 . . ? P2 C211 H211 106.8 . . ? C211 C212 C213 112.1(2) . . ? C211 C212 H21A 109.2 . . ? C213 C212 H21A 109.2 . . ? C211 C212 H21B 109.2 . . ? C213 C212 H21B 109.2 . . ? H21A C212 H21B 107.9 . . ? C212 C213 C214 111.5(2) . . ? C212 C213 H21C 109.3 . . ? C214 C213 H21C 109.3 . . ? C212 C213 H21D 109.3 . . ? C214 C213 H21D 109.3 . . ? H21C C213 H21D 108 . . ? C215 C214 C213 110.6(3) . . ? C215 C214 H21E 109.5 . . ? C213 C214 H21E 109.5 . . ? C215 C214 H21F 109.5 . . ? C213 C214 H21F 109.5 . . ? H21E C214 H21F 108.1 . . ? C214 C215 C216 110.8(3) . . ? C214 C215 H21G 109.5 . . ? C216 C215 H21G 109.5 . . ? C214 C215 H21H 109.5 . . ? C216 C215 H21H 109.5 . . ? H21G C215 H21H 108.1 . . ? C215 C216 C211 111.9(2) . . ? C215 C216 H21I 109.2 . . ? C211 C216 H21I 109.2 . . ? C215 C216 H21J 109.2 . . ? C211 C216 H21J 109.2 . . ? H21I C216 H21J 107.9 . . ? C222 C221 C226 111.1(2) . . ? C222 C221 P2 116.22(17) . . ? C226 C221 P2 110.49(16) . . ? C222 C221 H221 106.1 . . ? C226 C221 H221 106.1 . . ? P2 C221 H221 106.1 . . ? C221 C222 C223 110.1(2) . . ? C221 C222 H22A 109.6 . . ? C223 C222 H22A 109.6 . . ? C221 C222 H22B 109.6 . . ? C223 C222 H22B 109.6 . . ? H22A C222 H22B 108.2 . . ? C224 C223 C222 111.7(3) . . ? C224 C223 H22C 109.3 . . ? C222 C223 H22C 109.3 . . ? C224 C223 H22D 109.3 . . ? C222 C223 H22D 109.3 . . ? H22C C223 H22D 107.9 . . ? C223 C224 C225 110.5(2) . . ? C223 C224 H22E 109.5 . . ? C225 C224 H22E 109.5 . . ? C223 C224 H22F 109.5 . . ? C225 C224 H22F 109.5 . . ? H22E C224 H22F 108.1 . . ? C226 C225 C224 110.8(2) . . ? C226 C225 H22G 109.5 . . ? C224 C225 H22G 109.5 . . ? C226 C225 H22H 109.5 . . ? C224 C225 H22H 109.5 . . ? H22G C225 H22H 108.1 . . ? C225 C226 C221 111.4(2) . . ? C225 C226 H22I 109.3 . . ? C221 C226 H22I 109.3 . . ? C225 C226 H22J 109.3 . . ? C221 C226 H22J 109.3 . . ? H22I C226 H22J 108 . . ? C236 C231 C232 109.6(2) . . ? C236 C231 P2 110.84(17) . . ? C232 C231 P2 110.10(15) . . ? C236 C231 H231 108.7 . . ? C232 C231 H231 108.7 . . ? P2 C231 H231 108.7 . . ? C233 C232 C231 112.0(2) . . ? C233 C232 H23A 109.2 . . ? C231 C232 H23A 109.2 . . ? C233 C232 H23B 109.2 . . ? C231 C232 H23B 109.2 . . ? H23A C232 H23B 107.9 . . ? C232 C233 C234 111.0(2) . . ? C232 C233 H23C 109.4 . . ? C234 C233 H23C 109.4 . . ? C232 C233 H23D 109.4 . . ? C234 C233 H23D 109.4 . . ? H23C C233 H23D 108 . . ? C233 C234 C235 110.3(2) . . ? C233 C234 H23E 109.6 . . ? C235 C234 H23E 109.6 . . ? C233 C234 H23F 109.6 . . ? C235 C234 H23F 109.6 . . ? H23E C234 H23F 108.1 . . ? C236 C235 C234 111.0(2) . . ? C236 C235 H23G 109.4 . . ? C234 C235 H23G 109.4 . . ? C236 C235 H23H 109.4 . . ? C234 C235 H23H 109.4 . . ? H23G C235 H23H 108 . . ? C235 C236 C231 111.9(2) . . ? C235 C236 H23I 109.2 . . ? C231 C236 H23I 109.2 . . ? C235 C236 H23J 109.2 . . ? C231 C236 H23J 109.2 . . ? H23I C236 H23J 107.9 . . ? C1 S1 Ag1 97.33(9) . . ? C1 S1 Ag1 101.17(8) . 3_666 ? Ag1 S1 Ag1 80.780(17) . 3_666 ? N1 C1 S1 178.8(2) . . ? C1 N1 Ag2 159.79(19) . . ? C2 S2 Ag2 96.67(9) . . ? N2 C2 S2 179.1(3) . . ? C2 N2 Ag1 164.2(2) . . ? data_n22cr _database_code_depnum_ccdc_archive 'CCDC 781519' #TrackingRef 'web_deposit_cif_file_0_BrianSkelton_1330156946.n22cr.cif' _audit_creation_date 2007-03-25T10:23:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C70 H56 Ag2 N6 P4 S2' _chemical_formula_moiety 'C70 H56 Ag2 N6 P4 S2' _chemical_formula_weight 1384.95 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a' _symmetry_space_group_name_Hall -P_2a_2ac loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 22.9000(5) _cell_length_b 11.7896(2) _cell_length_c 22.6981(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6128.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23538 _cell_measurement_theta_min 2.8388 _cell_measurement_theta_max 31.8589 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.90704 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.036001667 _diffrn_orient_matrix_ub_12 -0.023347163 _diffrn_orient_matrix_ub_13 -0.0087999844 _diffrn_orient_matrix_ub_21 0.0089389336 _diffrn_orient_matrix_ub_22 0.0077041247 _diffrn_orient_matrix_ub_23 -0.0295840973 _diffrn_orient_matrix_ub_31 0.047320939 _diffrn_orient_matrix_ub_32 -0.0192350657 _diffrn_orient_matrix_ub_33 -0.0011402182 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_unetI/netI 0.0625 _diffrn_reflns_number 80170 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 31.95 _diffrn_reflns_theta_full 31 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 10144 _reflns_number_gt 5633 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. The SCN ligands were modelled as being disordered end to end about the crystallographic 2-fold axis. The C and N atoms of these were refined with isotropic ADPs after anisotropic refinement was unsuccessful even with reasonable restraints. Geometries were restrained to ideal values. ; _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^)+(0.0751P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10144 _refine_ls_number_parameters 385 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.53 _refine_diff_density_min -0.95 _refine_diff_density_rms 0.1 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 0.657945(11) 0.660805(19) 0.546529(10) 0.03467(9) Uani 1 1 d . . . P1 P 0.60590(3) 0.70376(7) 0.63816(3) 0.02988(18) Uani 1 1 d . A . C111 C 0.62313(16) 0.8362(3) 0.67588(15) 0.0410(8) Uani 1 1 d . . . C112 C 0.59835(19) 0.8636(3) 0.73029(15) 0.0532(10) Uani 1 1 d . A . H112 H 0.5755 0.8088 0.7505 0.064 Uiso 1 1 calc R . . C113 C 0.6065(2) 0.9679(4) 0.75472(19) 0.0737(14) Uani 1 1 d . . . H113 H 0.5893 0.9862 0.7916 0.088 Uiso 1 1 calc R A . C114 C 0.6403(3) 1.0469(4) 0.7252(2) 0.0757(15) Uani 1 1 d . A . H114 H 0.6451 1.1204 0.7417 0.091 Uiso 1 1 calc R . . C115 C 0.6674(2) 1.0219(4) 0.6720(2) 0.0708(14) Uani 1 1 d . . . H115 H 0.6919 1.0758 0.653 0.085 Uiso 1 1 calc R A . C116 C 0.65767(16) 0.9146(3) 0.64704(18) 0.0497(9) Uani 1 1 d . A . H116 H 0.6749 0.8959 0.6102 0.06 Uiso 1 1 calc R . . C121 C 0.52758(14) 0.7163(3) 0.62649(13) 0.0369(7) Uani 1 1 d . . . C122 C 0.50040(16) 0.6216(3) 0.60962(19) 0.0540(10) Uani 1 1 d . A . H122 H 0.521 0.5517 0.6091 0.065 Uiso 1 1 calc R . . C123 C 0.4443(2) 0.6245(5) 0.5935(2) 0.0837(16) Uani 1 1 d . . . H123 H 0.4255 0.5559 0.5824 0.1 Uiso 1 1 calc R A . C124 C 0.41325(19) 0.7230(5) 0.59234(18) 0.0656(13) Uani 1 1 d . A . H124 H 0.3737 0.7234 0.5796 0.079 Uiso 1 1 calc R . . C125 C 0.43972(19) 0.8209(4) 0.60975(18) 0.0637(12) Uani 1 1 d . . . H125 H 0.4185 0.8901 0.6103 0.076 Uiso 1 1 calc R A . C126 C 0.49856(18) 0.8189(3) 0.62678(16) 0.0533(10) Uani 1 1 d . A . H126 H 0.518 0.8865 0.6383 0.064 Uiso 1 1 calc R . . C131 C 0.61399(13) 0.5921(3) 0.69329(13) 0.0308(6) Uani 1 1 d . . . N132 N 0.57270(15) 0.5730(3) 0.73553(14) 0.0621(9) Uani 1 1 d . A . C133 C 0.58150(17) 0.4838(4) 0.77450(16) 0.0544(10) Uani 1 1 d . . . H133 H 0.553 0.4694 0.804 0.065 Uiso 1 1 calc R A . C134 C 0.63007(16) 0.4158(3) 0.77180(14) 0.0450(8) Uani 1 1 d . A . H134 H 0.6351 0.3554 0.799 0.054 Uiso 1 1 calc R . . C135 C 0.67082(15) 0.4362(3) 0.72953(15) 0.0411(8) Uani 1 1 d . . . H135 H 0.705 0.3906 0.7276 0.049 Uiso 1 1 calc R A . C136 C 0.66293(13) 0.5229(3) 0.68926(13) 0.0318(6) Uani 1 1 d . A . H136 H 0.6909 0.5351 0.659 0.038 Uiso 1 1 calc R . . P2 P 0.63897(4) 0.77197(7) 0.45771(3) 0.03009(18) Uani 1 1 d . A . C211 C 0.69574(13) 0.7645(3) 0.40209(13) 0.0307(6) Uani 1 1 d . . . C212 C 0.72927(12) 0.6664(2) 0.40148(13) 0.0282(6) Uani 1 1 d . A . H212 H 0.7231 0.6093 0.4304 0.034 Uiso 1 1 calc R . . C213 C 0.77169(14) 0.6519(3) 0.35873(14) 0.0348(7) Uani 1 1 d . . . H213 H 0.7942 0.5843 0.3584 0.042 Uiso 1 1 calc R A . C214 C 0.78174(14) 0.7331(3) 0.31707(13) 0.0381(7) Uani 1 1 d . A . H214 H 0.8108 0.7222 0.2878 0.046 Uiso 1 1 calc R . . C215 C 0.74875(17) 0.8317(3) 0.31823(17) 0.0557(10) Uani 1 1 d . . . H215 H 0.7559 0.8894 0.2899 0.067 Uiso 1 1 calc R A . C216 C 0.70582(16) 0.8468(3) 0.35991(16) 0.0485(9) Uani 1 1 d . A . H216 H 0.683 0.9141 0.3597 0.058 Uiso 1 1 calc R . . C221 C 0.57059(14) 0.7483(3) 0.41778(15) 0.0372(7) Uani 1 1 d . . . C222 C 0.52889(18) 0.6732(3) 0.4428(2) 0.0597(12) Uani 1 1 d . A . H222 H 0.5366 0.6342 0.4787 0.072 Uiso 1 1 calc R . . C223 C 0.4776(2) 0.6590(4) 0.4138(4) 0.095(2) Uani 1 1 d . . . H223 H 0.4491 0.6088 0.4295 0.114 Uiso 1 1 calc R A . C224 C 0.46581(19) 0.7150(5) 0.3625(3) 0.0862(19) Uani 1 1 d . A . H224 H 0.4297 0.7037 0.3427 0.103 Uiso 1 1 calc R . . C225 C 0.5072(2) 0.7886(5) 0.33973(18) 0.0736(14) Uani 1 1 d . . . H225 H 0.4993 0.8284 0.3042 0.088 Uiso 1 1 calc R A . C226 C 0.55910(15) 0.8043(3) 0.36775(14) 0.0429(8) Uani 1 1 d . A . H226 H 0.5872 0.8551 0.3518 0.052 Uiso 1 1 calc R . . C231 C 0.63199(13) 0.9196(2) 0.47989(13) 0.0300(6) Uani 1 1 d . . . N232 N 0.67857(14) 0.9907(3) 0.47714(17) 0.0594(9) Uani 1 1 d . A . C233 C 0.67428(15) 1.0962(3) 0.50318(19) 0.0492(9) Uani 1 1 d . . . H233 H 0.7067 1.1463 0.5015 0.059 Uiso 1 1 calc R A . C234 C 0.62452(16) 1.1305(3) 0.53135(15) 0.0395(8) Uani 1 1 d . A . H234 H 0.6227 1.2032 0.5493 0.047 Uiso 1 1 calc R . . C235 C 0.57735(15) 1.0590(3) 0.53346(14) 0.0383(7) Uani 1 1 d . . . H235 H 0.5424 1.0824 0.5525 0.046 Uiso 1 1 calc R A . C236 C 0.58075(14) 0.9524(3) 0.50780(13) 0.0346(7) Uani 1 1 d . A . H236 H 0.5483 0.9023 0.5093 0.041 Uiso 1 1 calc R . . S1 S 0.65465(11) 0.45285(19) 0.51356(10) 0.0429(6) Uani 0.5 1 d PD A 1 C1 C 0.7086(3) 0.3829(6) 0.5517(3) 0.0341(17) Uiso 0.5 1 d PD A 1 N1 N 0.7277(5) 0.3138(9) 0.5896(5) 0.0210(12) Uiso 0.5 1 d PD A 1 S2 S 0.73800(16) 0.3150(4) 0.5863(2) 0.0614(12) Uani 0.5 1 d PD . -1 C2 C 0.6933(3) 0.4025(5) 0.5502(3) 0.0234(13) Uiso 0.5 1 d PD A -1 N2 N 0.6608(3) 0.4650(6) 0.5295(3) 0.0210(12) Uiso 0.5 1 d PD A -1 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 0.04369(17) 0.03144(13) 0.02889(13) 0.00850(9) 0.01132(10) 0.01063(10) P1 0.0304(4) 0.0355(4) 0.0237(4) 0.0015(3) 0.0025(3) 0.0069(3) C111 0.048(2) 0.0398(17) 0.0355(17) -0.0027(14) -0.0139(15) 0.0111(15) C112 0.081(3) 0.052(2) 0.0267(16) -0.0043(15) -0.0114(18) 0.014(2) C113 0.117(4) 0.062(3) 0.042(2) -0.015(2) -0.030(3) 0.017(3) C114 0.118(4) 0.054(3) 0.056(3) -0.020(2) -0.047(3) 0.013(3) C115 0.085(3) 0.045(2) 0.082(3) 0.003(2) -0.039(3) -0.006(2) C116 0.056(2) 0.0404(18) 0.052(2) -0.0014(17) -0.0124(18) -0.0012(17) C121 0.0331(17) 0.057(2) 0.0208(14) 0.0088(13) 0.0077(12) 0.0074(15) C122 0.033(2) 0.048(2) 0.081(3) 0.010(2) -0.0120(19) -0.0008(16) C123 0.050(3) 0.086(3) 0.114(4) 0.038(3) -0.013(3) -0.008(3) C124 0.040(2) 0.104(4) 0.053(2) 0.036(3) 0.0096(19) 0.003(2) C125 0.055(3) 0.089(3) 0.048(2) 0.005(2) -0.001(2) 0.039(2) C126 0.050(2) 0.070(2) 0.040(2) 0.0002(18) -0.0004(17) 0.0233(19) C131 0.0264(15) 0.0402(16) 0.0258(14) 0.0035(12) 0.0018(12) 0.0022(12) N132 0.066(2) 0.083(2) 0.0376(16) 0.0072(17) 0.0141(16) 0.0128(18) C133 0.048(2) 0.080(3) 0.0352(18) 0.0213(18) 0.0153(17) 0.004(2) C134 0.046(2) 0.062(2) 0.0272(16) 0.0169(16) -0.0054(15) -0.0090(18) C135 0.0353(18) 0.0485(19) 0.0394(18) 0.0106(15) -0.0083(15) 0.0034(14) C136 0.0286(16) 0.0412(16) 0.0256(14) 0.0070(12) 0.0025(12) -0.0002(12) P2 0.0304(4) 0.0301(4) 0.0298(4) 0.0081(3) 0.0063(3) 0.0083(3) C211 0.0241(15) 0.0417(16) 0.0262(14) 0.0080(12) -0.0001(11) 0.0047(12) C212 0.0264(15) 0.0292(14) 0.0290(14) 0.0000(11) 0.0024(12) -0.0013(11) C213 0.0280(16) 0.0397(16) 0.0368(16) -0.0087(13) 0.0074(13) -0.0013(13) C214 0.0256(16) 0.061(2) 0.0280(15) 0.0014(15) 0.0056(13) -0.0004(15) C215 0.043(2) 0.077(3) 0.047(2) 0.0317(19) 0.0127(17) 0.0124(19) C216 0.0357(19) 0.058(2) 0.051(2) 0.0260(18) 0.0112(17) 0.0212(16) C221 0.0304(17) 0.0348(16) 0.0464(19) -0.0065(14) 0.0098(14) 0.0037(13) C222 0.038(2) 0.0365(19) 0.105(4) 0.0094(19) 0.007(2) -0.0024(15) C223 0.033(3) 0.055(3) 0.197(8) -0.017(3) 0.008(4) -0.008(2) C224 0.032(2) 0.100(4) 0.127(5) -0.075(4) -0.015(3) 0.008(3) C225 0.051(3) 0.133(4) 0.037(2) -0.025(3) -0.0108(19) 0.013(3) C226 0.0309(18) 0.070(2) 0.0278(16) -0.0003(16) -0.0011(14) 0.0040(16) C231 0.0213(14) 0.0316(14) 0.0371(16) 0.0079(13) 0.0010(13) 0.0043(12) N232 0.0458(19) 0.0443(17) 0.088(3) 0.0013(17) 0.0061(19) 0.0071(15) C233 0.0322(18) 0.0361(17) 0.079(3) -0.0063(18) 0.0105(19) -0.0014(14) C234 0.040(2) 0.0289(15) 0.0500(19) 0.0006(14) -0.0035(15) 0.0037(14) C235 0.0312(18) 0.0416(17) 0.0422(18) -0.0034(14) 0.0035(14) -0.0012(14) C236 0.0327(17) 0.0374(16) 0.0335(16) -0.0001(13) -0.0004(13) -0.0028(13) S1 0.0603(14) 0.0351(10) 0.0332(11) -0.0031(8) -0.0129(10) 0.0016(8) S2 0.037(2) 0.0624(14) 0.085(2) -0.0304(13) -0.0269(17) 0.0165(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.341(7) . ? Ag1 N1 2.811(11) 2_665 ? Ag1 P2 2.4435(8) . ? Ag1 P1 2.4500(8) . ? Ag1 S2 2.564(4) 2_665 ? Ag1 S1 2.565(2) . ? P1 C121 1.819(3) . ? P1 C111 1.824(3) . ? P1 C131 1.825(3) . ? C111 C116 1.382(5) . ? C111 C112 1.397(5) . ? C112 C113 1.362(5) . ? C112 H112 0.95 . ? C113 C114 1.384(7) . ? C113 H113 0.95 . ? C114 C115 1.390(7) . ? C114 H114 0.95 . ? C115 C116 1.403(5) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.335(5) . ? C121 C126 1.380(5) . ? C122 C123 1.337(6) . ? C122 H122 0.95 . ? C123 C124 1.361(7) . ? C123 H123 0.95 . ? C124 C125 1.363(6) . ? C124 H124 0.95 . ? C125 C126 1.402(6) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 N132 1.365(4) . ? C131 C136 1.389(4) . ? N132 C133 1.389(5) . ? C133 C134 1.373(5) . ? C133 H133 0.95 . ? C134 C135 1.360(5) . ? C134 H134 0.95 . ? C135 C136 1.383(4) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? P2 C211 1.814(3) . ? P2 C231 1.818(3) . ? P2 C221 1.831(3) . ? C211 C216 1.382(4) . ? C211 C212 1.388(4) . ? C212 C213 1.384(4) . ? C212 H212 0.95 . ? C213 C214 1.365(4) . ? C213 H213 0.95 . ? C214 C215 1.387(5) . ? C214 H214 0.95 . ? C215 C216 1.376(5) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.340(5) . ? C221 C222 1.421(5) . ? C222 C223 1.359(7) . ? C222 H222 0.95 . ? C223 C224 1.364(8) . ? C223 H223 0.95 . ? C224 C225 1.385(7) . ? C224 H224 0.95 . ? C225 C226 1.361(5) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C231 N232 1.358(4) . ? C231 C236 1.389(4) . ? N232 C233 1.381(5) . ? C233 C234 1.368(5) . ? C233 H233 0.95 . ? C234 C235 1.371(5) . ? C234 H234 0.95 . ? C235 C236 1.387(4) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? S1 C1 1.719(6) . ? C1 N1 1.263(8) . ? S2 C2 1.669(6) . ? S2 Ag1 2.564(4) 2_665 ? C2 N2 1.147(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 P2 113.44(15) . . ? N2 Ag1 P1 110.94(17) . . ? P2 Ag1 P1 120.20(3) . . ? N2 Ag1 S2 98.15(18) . 2_665 ? P2 Ag1 S2 113.34(12) . 2_665 ? P1 Ag1 S2 97.47(10) . 2_665 ? P2 Ag1 S1 105.47(5) . . ? P1 Ag1 S1 115.53(6) . . ? S2 Ag1 S1 103.68(12) 2_665 . ? P1 Ag1 N1 97.8(2) . 2_665 ? P2 Ag1 N1 113.3(2) . 2_665 ? S1 Ag1 N1 103.3(2) . 2_665 ? N2 Ag1 N1 97.8(3) . 2_665 ? C121 P1 C111 102.25(16) . . ? C121 P1 C131 104.97(14) . . ? C111 P1 C131 105.86(14) . . ? C121 P1 Ag1 111.88(10) . . ? C111 P1 Ag1 118.05(13) . . ? C131 P1 Ag1 112.56(10) . . ? C116 C111 C112 119.8(3) . . ? C116 C111 P1 118.3(3) . . ? C112 C111 P1 121.7(3) . . ? C113 C112 C111 120.9(4) . . ? C113 C112 H112 119.6 . . ? C111 C112 H112 119.6 . . ? C112 C113 C114 119.2(4) . . ? C112 C113 H113 120.4 . . ? C114 C113 H113 120.4 . . ? C113 C114 C115 121.8(4) . . ? C113 C114 H114 119.1 . . ? C115 C114 H114 119.1 . . ? C114 C115 C116 118.1(5) . . ? C114 C115 H115 121 . . ? C116 C115 H115 121 . . ? C111 C116 C115 120.2(4) . . ? C111 C116 H116 119.9 . . ? C115 C116 H116 119.9 . . ? C122 C121 C126 120.7(3) . . ? C122 C121 P1 115.7(3) . . ? C126 C121 P1 123.0(3) . . ? C121 C122 C123 120.3(4) . . ? C121 C122 H122 119.8 . . ? C123 C122 H122 119.8 . . ? C122 C123 C124 121.9(5) . . ? C122 C123 H123 119 . . ? C124 C123 H123 119 . . ? C123 C124 C125 119.0(4) . . ? C123 C124 H124 120.5 . . ? C125 C124 H124 120.5 . . ? C124 C125 C126 119.5(4) . . ? C124 C125 H125 120.2 . . ? C126 C125 H125 120.2 . . ? C121 C126 C125 118.5(4) . . ? C121 C126 H126 120.8 . . ? C125 C126 H126 120.8 . . ? N132 C131 C136 120.5(3) . . ? N132 C131 P1 122.0(2) . . ? C136 C131 P1 117.4(2) . . ? C131 N132 C133 118.2(3) . . ? C134 C133 N132 122.1(3) . . ? C134 C133 H133 118.9 . . ? N132 C133 H133 118.9 . . ? C135 C134 C133 118.9(3) . . ? C135 C134 H134 120.5 . . ? C133 C134 H134 120.5 . . ? C134 C135 C136 120.5(3) . . ? C134 C135 H135 119.8 . . ? C136 C135 H135 119.8 . . ? C135 C136 C131 119.7(3) . . ? C135 C136 H136 120.1 . . ? C131 C136 H136 120.1 . . ? C211 P2 C231 107.58(14) . . ? C211 P2 C221 105.13(14) . . ? C231 P2 C221 101.99(14) . . ? C211 P2 Ag1 114.88(10) . . ? C231 P2 Ag1 107.48(10) . . ? C221 P2 Ag1 118.61(11) . . ? C216 C211 C212 119.1(3) . . ? C216 C211 P2 124.6(2) . . ? C212 C211 P2 116.3(2) . . ? C213 C212 C211 119.9(3) . . ? C213 C212 H212 120.1 . . ? C211 C212 H212 120.1 . . ? C214 C213 C212 121.2(3) . . ? C214 C213 H213 119.4 . . ? C212 C213 H213 119.4 . . ? C213 C214 C215 118.9(3) . . ? C213 C214 H214 120.6 . . ? C215 C214 H214 120.6 . . ? C216 C215 C214 120.7(3) . . ? C216 C215 H215 119.6 . . ? C214 C215 H215 119.6 . . ? C215 C216 C211 120.3(3) . . ? C215 C216 H216 119.9 . . ? C211 C216 H216 119.9 . . ? C226 C221 C222 121.0(4) . . ? C226 C221 P2 120.8(3) . . ? C222 C221 P2 118.1(3) . . ? C223 C222 C221 117.6(5) . . ? C223 C222 H222 121.2 . . ? C221 C222 H222 121.2 . . ? C222 C223 C224 121.7(5) . . ? C222 C223 H223 119.1 . . ? C224 C223 H223 119.1 . . ? C223 C224 C225 119.1(4) . . ? C223 C224 H224 120.4 . . ? C225 C224 H224 120.4 . . ? C226 C225 C224 120.6(5) . . ? C226 C225 H225 119.7 . . ? C224 C225 H225 119.7 . . ? C221 C226 C225 120.0(4) . . ? C221 C226 H226 120 . . ? C225 C226 H226 120 . . ? N232 C231 C236 120.8(3) . . ? N232 C231 P2 120.6(2) . . ? C236 C231 P2 117.9(2) . . ? C231 N232 C233 118.7(3) . . ? C234 C233 N232 121.7(3) . . ? C234 C233 H233 119.1 . . ? N232 C233 H233 119.1 . . ? C233 C234 C235 119.4(3) . . ? C233 C234 H234 120.3 . . ? C235 C234 H234 120.3 . . ? C234 C235 C236 119.9(3) . . ? C234 C235 H235 120.1 . . ? C236 C235 H235 120.1 . . ? C235 C236 C231 119.5(3) . . ? C235 C236 H236 120.3 . . ? C231 C236 H236 120.3 . . ? C1 S1 Ag1 106.9(3) . . ? N1 C1 S1 154.3(8) . . ? C1 N1 Ag1 91.0(7) . 2_665 ? C2 S2 Ag1 109.2(3) . 2_665 ? N2 C2 S2 174.7(7) . . ? Ag1 N2 C2 125.7(6) . . ? #===END data_cmpnd01 _database_code_depnum_ccdc_archive 'CCDC 869208' #TrackingRef 'UWA120227.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H45 Ag N P3 S, C5 H5 N' _chemical_formula_sum 'C60 H50 Ag N2 P3 S' _chemical_formula_weight 1031.86 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' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3580(12) _cell_length_b 14.0634(13) _cell_length_c 14.2421(12) _cell_angle_alpha 88.369(2) _cell_angle_beta 78.086(2) _cell_angle_gamma 82.160(2) _cell_volume 2593.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 6455 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 29.1 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5027 _exptl_absorpt_correction_T_max 0.8944 _exptl_absorpt_process_details 'SADABS - Bruker area detector absorption corrections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13723 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 29.17 _reflns_number_total 11089 _reflns_number_gt 8683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL, v. 5.1' _computing_structure_refinement 'Bruker SHELXTL, v. 5.1' _computing_molecular_graphics 'XTAL: Ortep' _computing_publication_material 'Bruker SHELXTL, v. 5.1' _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^)+(0.0800P)^2^+1.1500P] 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 11089 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.59345(9) 0.23331(10) 0.25664(12) 0.1049(5) Uani 1 1 d . . . C C 0.4865(3) 0.2252(2) 0.2218(3) 0.0622(8) Uani 1 1 d . . . N N 0.4116(2) 0.2213(3) 0.1960(3) 0.0766(9) Uani 1 1 d . . . Ag Ag 0.239937(17) 0.201549(16) 0.205192(17) 0.05285(9) Uani 1 1 d . . . P1 P 0.23492(6) 0.02846(5) 0.26037(6) 0.04885(18) Uani 1 1 d . . . C111 C 0.2924(2) -0.0056(2) 0.3644(2) 0.0533(7) Uani 1 1 d . . . C112 C 0.2952(3) 0.0648(3) 0.4286(3) 0.0798(11) Uani 1 1 d . . . H112 H 0.2671 0.1277 0.4191 0.096 Uiso 1 1 calc R . . C113 C 0.3396(4) 0.0426(4) 0.5070(4) 0.1026(16) Uani 1 1 d . . . H113 H 0.3419 0.0909 0.5494 0.123 Uiso 1 1 calc R . . C114 C 0.3802(4) -0.0497(4) 0.5230(3) 0.0895(13) Uani 1 1 d . . . H114 H 0.4087 -0.0643 0.5768 0.107 Uiso 1 1 calc R . . C115 C 0.3786(3) -0.1199(3) 0.4598(3) 0.0807(11) Uani 1 1 d . . . H115 H 0.4073 -0.1825 0.4696 0.097 Uiso 1 1 calc R . . C116 C 0.3343(3) -0.0979(3) 0.3810(3) 0.0734(10) Uani 1 1 d . . . H116 H 0.3328 -0.1463 0.3384 0.088 Uiso 1 1 calc R . . C121 C 0.3052(2) -0.0617(2) 0.1724(2) 0.0493(6) Uani 1 1 d . . . C122 C 0.4015(2) -0.0465(3) 0.1208(3) 0.0651(9) Uani 1 1 d . . . H122 H 0.4284 0.0091 0.1309 0.078 Uiso 1 1 calc R . . C123 C 0.4577(3) -0.1132(3) 0.0549(3) 0.0769(11) Uani 1 1 d . . . H123 H 0.5227 -0.1025 0.0212 0.092 Uiso 1 1 calc R . . C124 C 0.4194(3) -0.1949(3) 0.0381(3) 0.0761(11) Uani 1 1 d . . . H124 H 0.4573 -0.2387 -0.0078 0.091 Uiso 1 1 calc R . . C125 C 0.3243(3) -0.2120(3) 0.0896(3) 0.0762(10) Uani 1 1 d . . . H125 H 0.2984 -0.2681 0.0796 0.091 Uiso 1 1 calc R . . C126 C 0.2673(3) -0.1449(2) 0.1568(3) 0.0647(9) Uani 1 1 d . . . H126 H 0.2030 -0.1564 0.1914 0.078 Uiso 1 1 calc R . . C131 C 0.1060(2) -0.0086(2) 0.2889(2) 0.0532(7) Uani 1 1 d . . . C132 C 0.0414(3) 0.0180(3) 0.2258(3) 0.0639(8) Uani 1 1 d . . . H132 H 0.0635 0.0559 0.1730 0.077 Uiso 1 1 calc R . . C133 C -0.0562(3) -0.0110(3) 0.2399(4) 0.0801(11) Uani 1 1 d . . . H133 H -0.0985 0.0065 0.1963 0.096 Uiso 1 1 calc R . . C134 C -0.0891(3) -0.0652(4) 0.3183(4) 0.0941(14) Uani 1 1 d . . . H134 H -0.1541 -0.0850 0.3280 0.113 Uiso 1 1 calc R . . C135 C -0.0272(4) -0.0906(4) 0.3827(4) 0.1054(16) Uani 1 1 d . . . H135 H -0.0509 -0.1268 0.4364 0.126 Uiso 1 1 calc R . . C136 C 0.0707(3) -0.0630(3) 0.3688(3) 0.0775(11) Uani 1 1 d . . . H136 H 0.1125 -0.0808 0.4128 0.093 Uiso 1 1 calc R . . P2 P 0.14028(6) 0.33089(6) 0.32803(6) 0.05330(19) Uani 1 1 d . . . C211 C 0.1369(3) 0.4577(2) 0.2940(3) 0.0592(8) Uani 1 1 d . . . C212 C 0.1103(3) 0.4854(3) 0.2075(3) 0.0762(10) Uani 1 1 d . . . H212 H 0.1002 0.4390 0.1664 0.091 Uiso 1 1 calc R . . C213 C 0.0983(4) 0.5815(3) 0.1812(4) 0.0912(13) Uani 1 1 d . . . H213 H 0.0783 0.5995 0.1238 0.109 Uiso 1 1 calc R . . C214 C 0.1160(4) 0.6494(3) 0.2404(4) 0.0968(15) Uani 1 1 d . . . H214 H 0.1084 0.7138 0.2228 0.116 Uiso 1 1 calc R . . C215 C 0.1451(4) 0.6231(3) 0.3257(4) 0.1001(16) Uani 1 1 d . . . H215 H 0.1574 0.6697 0.3655 0.120 Uiso 1 1 calc R . . C216 C 0.1562(3) 0.5272(3) 0.3526(3) 0.0815(11) Uani 1 1 d . . . H216 H 0.1766 0.5095 0.4099 0.098 Uiso 1 1 calc R . . C221 C 0.1868(3) 0.3268(2) 0.4396(3) 0.0594(8) Uani 1 1 d . . . C222 C 0.2929(3) 0.3168(3) 0.4345(3) 0.0819(12) Uani 1 1 d . . . H222 H 0.3379 0.3102 0.3751 0.098 Uiso 1 1 calc R . . C223 C 0.3320(4) 0.3164(4) 0.5174(4) 0.0934(14) Uani 1 1 d . . . H223 H 0.4030 0.3117 0.5131 0.112 Uiso 1 1 calc R . . C224 C 0.2671(5) 0.3230(3) 0.6055(4) 0.0957(15) Uani 1 1 d . . . H224 H 0.2936 0.3218 0.6610 0.115 Uiso 1 1 calc R . . C225 C 0.1624(4) 0.3314(4) 0.6114(3) 0.0919(13) Uani 1 1 d . . . H225 H 0.1181 0.3358 0.6713 0.110 Uiso 1 1 calc R . . C226 C 0.1223(3) 0.3334(3) 0.5299(3) 0.0734(10) Uani 1 1 d . . . H226 H 0.0512 0.3392 0.5352 0.088 Uiso 1 1 calc R . . C231 C 0.0028(2) 0.3206(2) 0.3662(2) 0.0556(7) Uani 1 1 d . . . C232 C -0.0269(3) 0.2299(3) 0.3805(3) 0.0673(9) Uani 1 1 d . . . H232 H 0.0235 0.1766 0.3729 0.081 Uiso 1 1 calc R . . C233 C -0.1301(3) 0.2167(3) 0.4060(3) 0.0802(11) Uani 1 1 d . . . H233 H -0.1486 0.1553 0.4165 0.096 Uiso 1 1 calc R . . C234 C -0.2044(3) 0.2951(4) 0.4156(4) 0.0898(13) Uani 1 1 d . . . H234 H -0.2738 0.2870 0.4312 0.108 Uiso 1 1 calc R . . C235 C -0.1767(3) 0.3856(4) 0.4023(4) 0.0932(14) Uani 1 1 d . . . H235 H -0.2276 0.4385 0.4101 0.112 Uiso 1 1 calc R . . C236 C -0.0740(3) 0.3993(3) 0.3773(3) 0.0752(10) Uani 1 1 d . . . H236 H -0.0563 0.4611 0.3680 0.090 Uiso 1 1 calc R . . P3 P 0.20226(6) 0.23474(6) 0.03848(6) 0.05171(19) Uani 1 1 d . . . C311 C 0.2219(3) 0.3553(2) -0.0042(3) 0.0625(8) Uani 1 1 d . . . C312 C 0.3039(3) 0.3937(3) 0.0180(3) 0.0781(11) Uani 1 1 d . . . H312 H 0.3446 0.3597 0.0566 0.094 Uiso 1 1 calc R . . C313 C 0.3252(4) 0.4830(3) -0.0173(5) 0.1109(18) Uani 1 1 d . . . H313 H 0.3811 0.5081 -0.0030 0.133 Uiso 1 1 calc R . . C314 C 0.2655(5) 0.5347(4) -0.0728(5) 0.125(2) Uani 1 1 d . . . H314 H 0.2811 0.5942 -0.0970 0.150 Uiso 1 1 calc R . . C315 C 0.1836(5) 0.4986(4) -0.0923(5) 0.125(2) Uani 1 1 d . . . H315 H 0.1413 0.5351 -0.1280 0.150 Uiso 1 1 calc R . . C316 C 0.1610(4) 0.4084(3) -0.0603(4) 0.0937(14) Uani 1 1 d . . . H316 H 0.1057 0.3836 -0.0764 0.112 Uiso 1 1 calc R . . C321 C 0.2694(2) 0.1607(2) -0.0641(2) 0.0536(7) Uani 1 1 d . . . C322 C 0.2736(3) 0.0616(2) -0.0550(3) 0.0655(9) Uani 1 1 d . . . H322 H 0.2422 0.0354 0.0024 0.079 Uiso 1 1 calc R . . C323 C 0.3236(4) 0.0019(3) -0.1298(3) 0.0801(11) Uani 1 1 d . . . H323 H 0.3246 -0.0642 -0.1231 0.096 Uiso 1 1 calc R . . C324 C 0.3719(4) 0.0396(3) -0.2145(3) 0.0851(12) Uani 1 1 d . . . H324 H 0.4055 -0.0011 -0.2649 0.102 Uiso 1 1 calc R . . C325 C 0.3706(4) 0.1365(3) -0.2249(3) 0.0860(12) Uani 1 1 d . . . H325 H 0.4044 0.1617 -0.2819 0.103 Uiso 1 1 calc R . . C326 C 0.3188(3) 0.1977(3) -0.1500(3) 0.0723(10) Uani 1 1 d . . . H326 H 0.3173 0.2638 -0.1576 0.087 Uiso 1 1 calc R . . C331 C 0.0666(2) 0.2255(2) 0.0398(2) 0.0545(7) Uani 1 1 d . . . C332 C -0.0059(3) 0.2544(3) 0.1220(3) 0.0649(8) Uani 1 1 d . . . H332 H 0.0152 0.2823 0.1718 0.078 Uiso 1 1 calc R . . C333 C -0.1084(3) 0.2428(3) 0.1317(3) 0.0749(10) Uani 1 1 d . . . H333 H -0.1557 0.2628 0.1874 0.090 Uiso 1 1 calc R . . C334 C -0.1398(3) 0.2018(3) 0.0593(4) 0.0872(13) Uani 1 1 d . . . H334 H -0.2087 0.1935 0.0653 0.105 Uiso 1 1 calc R . . C335 C -0.0691(4) 0.1727(4) -0.0229(4) 0.1035(17) Uani 1 1 d . . . H335 H -0.0906 0.1440 -0.0720 0.124 Uiso 1 1 calc R . . C336 C 0.0328(3) 0.1854(4) -0.0335(3) 0.0863(13) Uani 1 1 d . . . H336 H 0.0791 0.1669 -0.0903 0.104 Uiso 1 1 calc R . . N1 N 0.5059(6) 0.6469(5) 0.3230(6) 0.143(4) Uiso 0.50 1 d PG A 1 C2 C 0.5311(5) 0.5579(5) 0.3564(6) 0.160(6) Uiso 0.50 1 d PG A 1 H2 H 0.5695 0.5492 0.4043 0.192 Uiso 0.50 1 calc PR A 1 C3 C 0.5006(5) 0.4814(4) 0.3203(6) 0.139(6) Uiso 0.50 1 d PG A 1 H3 H 0.5180 0.4201 0.3433 0.167 Uiso 0.50 1 calc PR A 1 C4 C 0.4448(6) 0.4940(4) 0.2508(5) 0.103(3) Uiso 0.50 1 d PG A 1 H4 H 0.4238 0.4413 0.2259 0.123 Uiso 0.50 1 calc PR A 1 C5 C 0.4196(7) 0.5830(5) 0.2174(5) 0.108(3) Uiso 0.50 1 d PG A 1 H5 H 0.3812 0.5917 0.1695 0.129 Uiso 0.50 1 calc PR A 1 C6 C 0.4501(8) 0.6595(5) 0.2535(5) 0.34(2) Uiso 0.50 1 d PG A 1 H6 H 0.4327 0.7208 0.2305 0.411 Uiso 0.50 1 calc PR A 1 N1' N 0.4305(6) 0.6549(5) 0.3651(5) 0.131(3) Uiso 0.50 1 d PG A 2 C2' C 0.4442(6) 0.5676(6) 0.4062(4) 0.129(4) Uiso 0.50 1 d PG A 2 H2' H 0.4270 0.5614 0.4725 0.155 Uiso 0.50 1 calc PR A 2 C3' C 0.4829(6) 0.4894(4) 0.3508(5) 0.162(7) Uiso 0.50 1 d PG A 2 H3' H 0.4923 0.4293 0.3791 0.195 Uiso 0.50 1 calc PR A 2 C4' C 0.5080(5) 0.4984(4) 0.2544(5) 0.184(7) Uiso 0.50 1 d PG A 2 H4' H 0.5346 0.4446 0.2164 0.221 Uiso 0.50 1 calc PR A 2 C5' C 0.4943(6) 0.5857(5) 0.2134(4) 0.226(10) Uiso 0.50 1 d PG A 2 H5' H 0.5110 0.5910 0.1469 0.271 Uiso 0.50 1 calc PR A 2 C6' C 0.4588(8) 0.6614(7) 0.2640(7) 0.090(3) Uiso 0.50 1 d PG A 2 H6' H 0.4517 0.7209 0.2341 0.108 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S 0.0712(6) 0.0975(8) 0.1573(13) -0.0393(8) -0.0521(7) 0.0017(6) C 0.0531(17) 0.0584(18) 0.074(2) -0.0122(16) -0.0086(15) -0.0085(14) N 0.0542(16) 0.093(2) 0.084(2) -0.0108(18) -0.0153(15) -0.0128(15) Ag 0.05094(13) 0.04980(13) 0.06082(18) -0.00068(10) -0.01751(10) -0.00786(9) P1 0.0493(4) 0.0447(4) 0.0554(5) 0.0027(3) -0.0154(3) -0.0099(3) C111 0.0513(16) 0.0557(16) 0.0557(19) 0.0019(13) -0.0156(13) -0.0101(13) C112 0.093(3) 0.072(2) 0.080(3) -0.017(2) -0.037(2) 0.004(2) C113 0.121(4) 0.108(4) 0.088(4) -0.030(3) -0.051(3) 0.004(3) C114 0.086(3) 0.124(4) 0.065(3) 0.005(3) -0.034(2) -0.011(3) C115 0.083(3) 0.081(3) 0.084(3) 0.021(2) -0.035(2) -0.008(2) C116 0.093(3) 0.062(2) 0.074(3) 0.0035(17) -0.038(2) -0.0073(19) C121 0.0480(14) 0.0532(15) 0.0496(17) 0.0060(13) -0.0161(12) -0.0083(12) C122 0.0502(17) 0.065(2) 0.079(2) 0.0114(17) -0.0105(15) -0.0104(15) C123 0.0549(19) 0.085(3) 0.080(3) 0.016(2) 0.0014(17) 0.0021(18) C124 0.070(2) 0.088(3) 0.061(2) -0.0058(19) -0.0072(17) 0.016(2) C125 0.071(2) 0.071(2) 0.086(3) -0.025(2) -0.0146(19) -0.0071(18) C126 0.0548(17) 0.0623(19) 0.076(2) -0.0129(17) -0.0072(15) -0.0128(15) C131 0.0498(15) 0.0475(15) 0.062(2) -0.0039(13) -0.0104(13) -0.0062(12) C132 0.0585(18) 0.0616(19) 0.075(2) 0.0021(16) -0.0204(16) -0.0093(15) C133 0.060(2) 0.080(3) 0.107(3) -0.010(2) -0.031(2) -0.0084(19) C134 0.060(2) 0.109(3) 0.118(4) -0.001(3) -0.015(2) -0.035(2) C135 0.084(3) 0.131(4) 0.105(4) 0.030(3) -0.006(3) -0.052(3) C136 0.069(2) 0.091(3) 0.075(3) 0.017(2) -0.0154(18) -0.025(2) P2 0.0527(4) 0.0465(4) 0.0594(5) -0.0098(3) -0.0084(3) -0.0046(3) C211 0.0559(17) 0.0512(16) 0.066(2) -0.0089(14) -0.0017(15) -0.0070(13) C212 0.088(3) 0.060(2) 0.080(3) -0.0021(18) -0.017(2) -0.0081(19) C213 0.096(3) 0.072(3) 0.101(3) 0.016(2) -0.014(3) -0.007(2) C214 0.100(3) 0.057(2) 0.129(4) 0.014(3) -0.007(3) -0.024(2) C215 0.117(4) 0.059(2) 0.128(5) -0.012(3) -0.019(3) -0.034(2) C216 0.094(3) 0.060(2) 0.092(3) -0.0082(19) -0.012(2) -0.025(2) C221 0.0632(19) 0.0487(16) 0.066(2) -0.0119(14) -0.0134(15) -0.0025(14) C222 0.066(2) 0.097(3) 0.084(3) -0.024(2) -0.0155(19) -0.010(2) C223 0.086(3) 0.105(3) 0.098(4) -0.012(3) -0.044(3) -0.002(3) C224 0.130(4) 0.086(3) 0.081(3) -0.004(2) -0.052(3) -0.001(3) C225 0.111(4) 0.096(3) 0.065(3) 0.002(2) -0.017(2) -0.003(3) C226 0.077(2) 0.073(2) 0.068(3) -0.0019(18) -0.0121(19) -0.0034(19) C231 0.0533(16) 0.0538(16) 0.059(2) -0.0081(14) -0.0085(13) -0.0077(13) C232 0.069(2) 0.0544(18) 0.075(2) -0.0067(16) -0.0044(17) -0.0100(15) C233 0.079(3) 0.072(2) 0.088(3) -0.004(2) -0.004(2) -0.028(2) C234 0.065(2) 0.107(3) 0.099(3) 0.002(3) -0.009(2) -0.029(2) C235 0.058(2) 0.088(3) 0.127(4) -0.004(3) -0.008(2) 0.001(2) C236 0.0591(19) 0.0577(19) 0.104(3) -0.0071(19) -0.0058(19) -0.0048(16) P3 0.0547(4) 0.0476(4) 0.0562(5) 0.0012(3) -0.0203(3) -0.0054(3) C311 0.0638(19) 0.0481(16) 0.074(2) 0.0004(15) -0.0123(16) -0.0038(14) C312 0.066(2) 0.059(2) 0.111(3) 0.000(2) -0.018(2) -0.0116(17) C313 0.089(3) 0.072(3) 0.170(6) 0.003(3) -0.014(3) -0.026(2) C314 0.114(4) 0.064(3) 0.190(6) 0.039(3) -0.019(4) -0.017(3) C315 0.139(5) 0.068(3) 0.173(6) 0.043(3) -0.055(5) -0.006(3) C316 0.099(3) 0.065(2) 0.125(4) 0.024(2) -0.046(3) -0.008(2) C321 0.0582(17) 0.0519(16) 0.0537(19) 0.0007(13) -0.0216(13) -0.0026(13) C322 0.076(2) 0.0547(18) 0.068(2) 0.0021(16) -0.0208(17) -0.0078(16) C323 0.102(3) 0.055(2) 0.088(3) -0.0108(19) -0.035(2) 0.000(2) C324 0.109(3) 0.080(3) 0.067(3) -0.019(2) -0.030(2) 0.009(2) C325 0.112(3) 0.085(3) 0.054(2) -0.003(2) -0.011(2) 0.005(2) C326 0.091(3) 0.062(2) 0.061(2) 0.0063(17) -0.0174(19) -0.0013(18) C331 0.0569(17) 0.0529(16) 0.058(2) 0.0017(14) -0.0234(14) -0.0056(13) C332 0.0625(19) 0.065(2) 0.071(2) -0.0063(16) -0.0235(16) -0.0047(15) C333 0.059(2) 0.077(2) 0.088(3) 0.005(2) -0.0166(18) -0.0032(17) C334 0.059(2) 0.087(3) 0.123(4) 0.001(3) -0.032(2) -0.016(2) C335 0.080(3) 0.131(4) 0.114(4) -0.040(3) -0.043(3) -0.020(3) C336 0.071(2) 0.118(4) 0.076(3) -0.024(2) -0.028(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S C 1.625(4) . ? C N 1.144(4) . ? N Ag 2.323(3) . ? Ag P1 2.5419(8) . ? Ag P3 2.5445(9) . ? Ag P2 2.5885(8) . ? P1 C121 1.827(3) . ? P1 C111 1.829(3) . ? P1 C131 1.829(3) . ? C111 C116 1.376(5) . ? C111 C112 1.376(5) . ? C112 C113 1.377(6) . ? C112 H112 0.9300 . ? C113 C114 1.370(7) . ? C113 H113 0.9300 . ? C114 C115 1.359(7) . ? C114 H114 0.9300 . ? C115 C116 1.383(5) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C121 C126 1.379(4) . ? C121 C122 1.385(4) . ? C122 C123 1.376(6) . ? C122 H122 0.9300 . ? C123 C124 1.365(6) . ? C123 H123 0.9300 . ? C124 C125 1.378(6) . ? C124 H124 0.9300 . ? C125 C126 1.393(5) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C132 1.380(5) . ? C131 C136 1.388(5) . ? C132 C133 1.392(5) . ? C132 H132 0.9300 . ? C133 C134 1.365(7) . ? C133 H133 0.9300 . ? C134 C135 1.366(7) . ? C134 H134 0.9300 . ? C135 C136 1.389(6) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? P2 C221 1.818(4) . ? P2 C231 1.829(3) . ? P2 C211 1.832(3) . ? C211 C212 1.382(6) . ? C211 C216 1.387(5) . ? C212 C213 1.389(6) . ? C212 H212 0.9300 . ? C213 C214 1.367(7) . ? C213 H213 0.9300 . ? C214 C215 1.377(8) . ? C214 H214 0.9300 . ? C215 C216 1.389(6) . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? C221 C226 1.390(5) . ? C221 C222 1.393(5) . ? C222 C223 1.386(6) . ? C222 H222 0.9300 . ? C223 C224 1.368(7) . ? C223 H223 0.9300 . ? C224 C225 1.372(7) . ? C224 H224 0.9300 . ? C225 C226 1.374(6) . ? C225 H225 0.9300 . ? C226 H226 0.9300 . ? C231 C232 1.384(5) . ? C231 C236 1.392(5) . ? C232 C233 1.388(5) . ? C232 H232 0.9300 . ? C233 C234 1.368(6) . ? C233 H233 0.9300 . ? C234 C235 1.371(7) . ? C234 H234 0.9300 . ? C235 C236 1.382(6) . ? C235 H235 0.9300 . ? C236 H236 0.9300 . ? P3 C311 1.820(3) . ? P3 C321 1.821(3) . ? P3 C331 1.831(3) . ? C311 C312 1.380(5) . ? C311 C316 1.388(5) . ? C312 C313 1.383(6) . ? C312 H312 0.9300 . ? C313 C314 1.363(8) . ? C313 H313 0.9300 . ? C314 C315 1.347(8) . ? C314 H314 0.9300 . ? C315 C316 1.388(6) . ? C315 H315 0.9300 . ? C316 H316 0.9300 . ? C321 C326 1.388(5) . ? C321 C322 1.390(5) . ? C322 C323 1.375(6) . ? C322 H322 0.9300 . ? C323 C324 1.373(6) . ? C323 H323 0.9300 . ? C324 C325 1.365(6) . ? C324 H324 0.9300 . ? C325 C326 1.394(6) . ? C325 H325 0.9300 . ? C326 H326 0.9300 . ? C331 C336 1.383(5) . ? C331 C332 1.387(5) . ? C332 C333 1.379(5) . ? C332 H332 0.9300 . ? C333 C334 1.360(6) . ? C333 H333 0.9300 . ? C334 C335 1.377(7) . ? C334 H334 0.9300 . ? C335 C336 1.373(6) . ? C335 H335 0.9300 . ? C336 H336 0.9300 . ? N1 C2 1.351(3) . ? N1 C6 1.351(3) . ? C2 C3 1.351(3) . ? C2 H2 0.9300 . ? C3 C4 1.351(3) . ? C3 H3 0.9300 . ? C4 C5 1.351(3) . ? C4 H4 0.9300 . ? C5 C6 1.351(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N1' C2' 1.351(3) . ? N1' C6' 1.415(13) . ? C2' C3' 1.351(3) . ? C2' H2' 0.9300 . ? C3' C4' 1.351(3) . ? C3' H3' 0.9300 . ? C4' C5' 1.351(3) . ? C4' H4' 0.9300 . ? C5' C6' 1.281(12) . ? C5' H5' 0.9300 . ? C6' H6' 0.9300 . ? 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 N C S 178.5(4) . . ? C N Ag 158.2(3) . . ? N Ag P1 102.77(9) . . ? N Ag P3 106.90(9) . . ? P1 Ag P3 114.47(3) . . ? N Ag P2 103.33(9) . . ? P1 Ag P2 115.75(3) . . ? P3 Ag P2 112.06(3) . . ? C121 P1 C111 101.58(14) . . ? C121 P1 C131 102.21(14) . . ? C111 P1 C131 105.63(15) . . ? C121 P1 Ag 115.06(10) . . ? C111 P1 Ag 115.74(10) . . ? C131 P1 Ag 114.86(10) . . ? C116 C111 C112 118.3(3) . . ? C116 C111 P1 123.2(3) . . ? C112 C111 P1 118.4(3) . . ? C111 C112 C113 120.3(4) . . ? C111 C112 H112 119.8 . . ? C113 C112 H112 119.8 . . ? C114 C113 C112 120.7(4) . . ? C114 C113 H113 119.6 . . ? C112 C113 H113 119.6 . . ? C115 C114 C113 119.6(4) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C114 C115 C116 119.8(4) . . ? C114 C115 H115 120.1 . . ? C116 C115 H115 120.1 . . ? C111 C116 C115 121.2(4) . . ? C111 C116 H116 119.4 . . ? C115 C116 H116 119.4 . . ? C126 C121 C122 118.7(3) . . ? C126 C121 P1 122.8(2) . . ? C122 C121 P1 118.5(3) . . ? C123 C122 C121 120.4(4) . . ? C123 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C124 C123 C122 120.9(3) . . ? C124 C123 H123 119.6 . . ? C122 C123 H123 119.6 . . ? C123 C124 C125 119.6(4) . . ? C123 C124 H124 120.2 . . ? C125 C124 H124 120.2 . . ? C124 C125 C126 119.7(4) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? C121 C126 C125 120.6(3) . . ? C121 C126 H126 119.7 . . ? C125 C126 H126 119.7 . . ? C132 C131 C136 118.6(3) . . ? C132 C131 P1 117.4(3) . . ? C136 C131 P1 123.9(3) . . ? C131 C132 C133 121.1(4) . . ? C131 C132 H132 119.4 . . ? C133 C132 H132 119.4 . . ? C134 C133 C132 119.4(4) . . ? C134 C133 H133 120.3 . . ? C132 C133 H133 120.3 . . ? C133 C134 C135 120.5(4) . . ? C133 C134 H134 119.8 . . ? C135 C134 H134 119.8 . . ? C134 C135 C136 120.6(4) . . ? C134 C135 H135 119.7 . . ? C136 C135 H135 119.7 . . ? C131 C136 C135 119.8(4) . . ? C131 C136 H136 120.1 . . ? C135 C136 H136 120.1 . . ? C221 P2 C231 104.06(16) . . ? C221 P2 C211 102.93(16) . . ? C231 P2 C211 101.65(15) . . ? C221 P2 Ag 113.54(11) . . ? C231 P2 Ag 113.80(11) . . ? C211 P2 Ag 119.02(11) . . ? C212 C211 C216 118.8(3) . . ? C212 C211 P2 118.3(3) . . ? C216 C211 P2 122.8(3) . . ? C211 C212 C213 121.0(4) . . ? C211 C212 H212 119.5 . . ? C213 C212 H212 119.5 . . ? C214 C213 C212 119.6(5) . . ? C214 C213 H213 120.2 . . ? C212 C213 H213 120.2 . . ? C213 C214 C215 120.4(4) . . ? C213 C214 H214 119.8 . . ? C215 C214 H214 119.8 . . ? C214 C215 C216 120.2(4) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C211 C216 C215 120.0(5) . . ? C211 C216 H216 120.0 . . ? C215 C216 H216 120.0 . . ? C226 C221 C222 117.9(4) . . ? C226 C221 P2 123.7(3) . . ? C222 C221 P2 118.3(3) . . ? C223 C222 C221 120.5(4) . . ? C223 C222 H222 119.8 . . ? C221 C222 H222 119.8 . . ? C224 C223 C222 120.5(5) . . ? C224 C223 H223 119.8 . . ? C222 C223 H223 119.8 . . ? C223 C224 C225 119.5(4) . . ? C223 C224 H224 120.2 . . ? C225 C224 H224 120.2 . . ? C224 C225 C226 120.7(5) . . ? C224 C225 H225 119.6 . . ? C226 C225 H225 119.6 . . ? C225 C226 C221 120.8(4) . . ? C225 C226 H226 119.6 . . ? C221 C226 H226 119.6 . . ? C232 C231 C236 118.2(3) . . ? C232 C231 P2 118.5(3) . . ? C236 C231 P2 123.2(3) . . ? C231 C232 C233 121.6(4) . . ? C231 C232 H232 119.2 . . ? C233 C232 H232 119.2 . . ? C234 C233 C232 119.3(4) . . ? C234 C233 H233 120.4 . . ? C232 C233 H233 120.4 . . ? C233 C234 C235 120.1(4) . . ? C233 C234 H234 119.9 . . ? C235 C234 H234 119.9 . . ? C234 C235 C236 120.9(4) . . ? C234 C235 H235 119.5 . . ? C236 C235 H235 119.5 . . ? C235 C236 C231 119.9(4) . . ? C235 C236 H236 120.0 . . ? C231 C236 H236 120.0 . . ? C311 P3 C321 102.49(16) . . ? C311 P3 C331 105.68(15) . . ? C321 P3 C331 102.50(15) . . ? C311 P3 Ag 113.07(13) . . ? C321 P3 Ag 121.53(10) . . ? C331 P3 Ag 110.03(11) . . ? C312 C311 C316 119.0(4) . . ? C312 C311 P3 117.8(3) . . ? C316 C311 P3 123.2(3) . . ? C311 C312 C313 119.7(4) . . ? C311 C312 H312 120.1 . . ? C313 C312 H312 120.1 . . ? C314 C313 C312 121.1(5) . . ? C314 C313 H313 119.4 . . ? C312 C313 H313 119.4 . . ? C315 C314 C313 119.3(5) . . ? C315 C314 H314 120.3 . . ? C313 C314 H314 120.3 . . ? C314 C315 C316 121.4(5) . . ? C314 C315 H315 119.3 . . ? C316 C315 H315 119.3 . . ? C315 C316 C311 119.4(5) . . ? C315 C316 H316 120.3 . . ? C311 C316 H316 120.3 . . ? C326 C321 C322 118.3(3) . . ? C326 C321 P3 123.5(3) . . ? C322 C321 P3 118.2(3) . . ? C323 C322 C321 120.9(4) . . ? C323 C322 H322 119.5 . . ? C321 C322 H322 119.5 . . ? C324 C323 C322 120.2(4) . . ? C324 C323 H323 119.9 . . ? C322 C323 H323 119.9 . . ? C325 C324 C323 120.2(4) . . ? C325 C324 H324 119.9 . . ? C323 C324 H324 119.9 . . ? C324 C325 C326 120.0(4) . . ? C324 C325 H325 120.0 . . ? C326 C325 H325 120.0 . . ? C321 C326 C325 120.4(4) . . ? C321 C326 H326 119.8 . . ? C325 C326 H326 119.8 . . ? C336 C331 C332 117.9(3) . . ? C336 C331 P3 123.9(3) . . ? C332 C331 P3 118.1(2) . . ? C333 C332 C331 121.7(4) . . ? C333 C332 H332 119.2 . . ? C331 C332 H332 119.2 . . ? C334 C333 C332 119.5(4) . . ? C334 C333 H333 120.2 . . ? C332 C333 H333 120.2 . . ? C333 C334 C335 119.7(4) . . ? C333 C334 H334 120.2 . . ? C335 C334 H334 120.2 . . ? C336 C335 C334 121.0(4) . . ? C336 C335 H335 119.5 . . ? C334 C335 H335 119.5 . . ? C335 C336 C331 120.2(4) . . ? C335 C336 H336 119.9 . . ? C331 C336 H336 119.9 . . ? C2 N1 C6 120.0 . . ? N1 C2 C3 120.0 . . ? N1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 N1 120.0 . . ? C5 C6 H6 120.0 . . ? N1 C6 H6 120.0 . . ? C2' N1' C6' 118.2(5) . . ? N1' C2' C3' 120.0 . . ? N1' C2' H2' 120.0 . . ? C3' C2' H2' 120.0 . . ? C4' C3' C2' 120.0 . . ? C4' C3' H3' 120.0 . . ? C2' C3' H3' 120.0 . . ? C5' C4' C3' 120.0 . . ? C5' C4' H4' 120.0 . . ? C3' C4' H4' 120.0 . . ? C6' C5' C4' 121.5(6) . . ? C6' C5' H5' 119.3 . . ? C4' C5' H5' 119.3 . . ? C5' C6' N1' 120.4(9) . . ? C5' C6' H6' 119.8 . . ? N1' C6' H6' 119.8 . . ? 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 S C N Ag -138(14) . . . . ? C N Ag P1 -62.7(9) . . . . ? C N Ag P3 176.4(8) . . . . ? C N Ag P2 58.1(9) . . . . ? N Ag P1 C121 -68.45(14) . . . . ? P3 Ag P1 C121 47.06(11) . . . . ? P2 Ag P1 C121 179.72(10) . . . . ? N Ag P1 C111 49.68(15) . . . . ? P3 Ag P1 C111 165.19(12) . . . . ? P2 Ag P1 C111 -62.15(12) . . . . ? N Ag P1 C131 173.26(15) . . . . ? P3 Ag P1 C131 -71.23(12) . . . . ? P2 Ag P1 C131 61.43(12) . . . . ? C121 P1 C111 C116 -27.4(3) . . . . ? C131 P1 C111 C116 78.9(3) . . . . ? Ag P1 C111 C116 -152.8(3) . . . . ? C121 P1 C111 C112 151.6(3) . . . . ? C131 P1 C111 C112 -102.1(3) . . . . ? Ag P1 C111 C112 26.2(3) . . . . ? C116 C111 C112 C113 0.3(7) . . . . ? P1 C111 C112 C113 -178.7(4) . . . . ? C111 C112 C113 C114 -0.9(8) . . . . ? C112 C113 C114 C115 1.4(8) . . . . ? C113 C114 C115 C116 -1.3(8) . . . . ? C112 C111 C116 C115 -0.2(6) . . . . ? P1 C111 C116 C115 178.8(3) . . . . ? C114 C115 C116 C111 0.7(7) . . . . ? C111 P1 C121 C126 95.8(3) . . . . ? C131 P1 C121 C126 -13.2(3) . . . . ? Ag P1 C121 C126 -138.3(3) . . . . ? C111 P1 C121 C122 -82.8(3) . . . . ? C131 P1 C121 C122 168.2(3) . . . . ? Ag P1 C121 C122 43.0(3) . . . . ? C126 C121 C122 C123 0.4(5) . . . . ? P1 C121 C122 C123 179.1(3) . . . . ? C121 C122 C123 C124 0.7(6) . . . . ? C122 C123 C124 C125 -1.6(6) . . . . ? C123 C124 C125 C126 1.3(6) . . . . ? C122 C121 C126 C125 -0.7(5) . . . . ? P1 C121 C126 C125 -179.3(3) . . . . ? C124 C125 C126 C121 -0.2(6) . . . . ? C121 P1 C131 C132 -80.7(3) . . . . ? C111 P1 C131 C132 173.4(3) . . . . ? Ag P1 C131 C132 44.6(3) . . . . ? C121 P1 C131 C136 98.0(3) . . . . ? C111 P1 C131 C136 -7.9(4) . . . . ? Ag P1 C131 C136 -136.7(3) . . . . ? C136 C131 C132 C133 -1.7(5) . . . . ? P1 C131 C132 C133 177.0(3) . . . . ? C131 C132 C133 C134 1.1(6) . . . . ? C132 C133 C134 C135 0.3(8) . . . . ? C133 C134 C135 C136 -1.0(9) . . . . ? C132 C131 C136 C135 1.0(6) . . . . ? P1 C131 C136 C135 -177.7(4) . . . . ? C134 C135 C136 C131 0.3(8) . . . . ? N Ag P2 C221 -51.55(16) . . . . ? P1 Ag P2 C221 59.96(13) . . . . ? P3 Ag P2 C221 -166.28(12) . . . . ? N Ag P2 C231 -170.35(15) . . . . ? P1 Ag P2 C231 -58.84(13) . . . . ? P3 Ag P2 C231 74.92(13) . . . . ? N Ag P2 C211 69.84(16) . . . . ? P1 Ag P2 C211 -178.65(13) . . . . ? P3 Ag P2 C211 -44.89(14) . . . . ? C221 P2 C211 C212 176.2(3) . . . . ? C231 P2 C211 C212 -76.3(3) . . . . ? Ag P2 C211 C212 49.6(3) . . . . ? C221 P2 C211 C216 -6.2(3) . . . . ? C231 P2 C211 C216 101.3(3) . . . . ? Ag P2 C211 C216 -132.8(3) . . . . ? C216 C211 C212 C213 -2.9(6) . . . . ? P2 C211 C212 C213 174.8(3) . . . . ? C211 C212 C213 C214 1.9(7) . . . . ? C212 C213 C214 C215 -0.3(8) . . . . ? C213 C214 C215 C216 -0.3(8) . . . . ? C212 C211 C216 C215 2.3(6) . . . . ? P2 C211 C216 C215 -175.3(4) . . . . ? C214 C215 C216 C211 -0.7(7) . . . . ? C231 P2 C221 C226 -10.8(3) . . . . ? C211 P2 C221 C226 94.9(3) . . . . ? Ag P2 C221 C226 -135.1(3) . . . . ? C231 P2 C221 C222 169.3(3) . . . . ? C211 P2 C221 C222 -84.9(3) . . . . ? Ag P2 C221 C222 45.1(3) . . . . ? C226 C221 C222 C223 -2.0(6) . . . . ? P2 C221 C222 C223 177.9(4) . . . . ? C221 C222 C223 C224 2.0(7) . . . . ? C222 C223 C224 C225 -0.9(8) . . . . ? C223 C224 C225 C226 -0.1(8) . . . . ? C224 C225 C226 C221 0.1(7) . . . . ? C222 C221 C226 C225 0.9(6) . . . . ? P2 C221 C226 C225 -178.9(3) . . . . ? C221 P2 C231 C232 -85.3(3) . . . . ? C211 P2 C231 C232 168.0(3) . . . . ? Ag P2 C231 C232 38.8(3) . . . . ? C221 P2 C231 C236 97.7(3) . . . . ? C211 P2 C231 C236 -9.0(4) . . . . ? Ag P2 C231 C236 -138.2(3) . . . . ? C236 C231 C232 C233 -0.4(6) . . . . ? P2 C231 C232 C233 -177.6(3) . . . . ? C231 C232 C233 C234 1.1(7) . . . . ? C232 C233 C234 C235 -1.5(7) . . . . ? C233 C234 C235 C236 1.2(8) . . . . ? C234 C235 C236 C231 -0.5(8) . . . . ? C232 C231 C236 C235 0.1(6) . . . . ? P2 C231 C236 C235 177.1(4) . . . . ? N Ag P3 C311 -59.87(16) . . . . ? P1 Ag P3 C311 -172.96(12) . . . . ? P2 Ag P3 C311 52.66(13) . . . . ? N Ag P3 C321 62.62(16) . . . . ? P1 Ag P3 C321 -50.47(13) . . . . ? P2 Ag P3 C321 175.14(12) . . . . ? N Ag P3 C331 -177.77(14) . . . . ? P1 Ag P3 C331 69.14(11) . . . . ? P2 Ag P3 C331 -65.25(11) . . . . ? C321 P3 C311 C312 -94.8(3) . . . . ? C331 P3 C311 C312 158.2(3) . . . . ? Ag P3 C311 C312 37.7(3) . . . . ? C321 P3 C311 C316 82.8(4) . . . . ? C331 P3 C311 C316 -24.2(4) . . . . ? Ag P3 C311 C316 -144.6(4) . . . . ? C316 C311 C312 C313 -1.3(7) . . . . ? P3 C311 C312 C313 176.5(4) . . . . ? C311 C312 C313 C314 1.0(8) . . . . ? C312 C313 C314 C315 0.9(10) . . . . ? C313 C314 C315 C316 -2.6(11) . . . . ? C314 C315 C316 C311 2.3(10) . . . . ? C312 C311 C316 C315 -0.3(8) . . . . ? P3 C311 C316 C315 -177.9(4) . . . . ? C311 P3 C321 C326 -0.9(3) . . . . ? C331 P3 C321 C326 108.5(3) . . . . ? Ag P3 C321 C326 -128.3(3) . . . . ? C311 P3 C321 C322 177.4(3) . . . . ? C331 P3 C321 C322 -73.1(3) . . . . ? Ag P3 C321 C322 50.1(3) . . . . ? C326 C321 C322 C323 -1.3(5) . . . . ? P3 C321 C322 C323 -179.7(3) . . . . ? C321 C322 C323 C324 1.2(6) . . . . ? C322 C323 C324 C325 0.0(7) . . . . ? C323 C324 C325 C326 -1.1(7) . . . . ? C322 C321 C326 C325 0.3(6) . . . . ? P3 C321 C326 C325 178.6(3) . . . . ? C324 C325 C326 C321 0.9(7) . . . . ? C311 P3 C331 C336 96.5(4) . . . . ? C321 P3 C331 C336 -10.5(4) . . . . ? Ag P3 C331 C336 -141.1(3) . . . . ? C311 P3 C331 C332 -88.2(3) . . . . ? C321 P3 C331 C332 164.8(3) . . . . ? Ag P3 C331 C332 34.2(3) . . . . ? C336 C331 C332 C333 0.8(6) . . . . ? P3 C331 C332 C333 -174.8(3) . . . . ? C331 C332 C333 C334 0.1(6) . . . . ? C332 C333 C334 C335 -0.2(7) . . . . ? C333 C334 C335 C336 -0.8(8) . . . . ? C334 C335 C336 C331 1.8(8) . . . . ? C332 C331 C336 C335 -1.8(7) . . . . ? P3 C331 C336 C335 173.6(4) . . . . ? C6 N1 C2 C3 0.0 . . . . ? N1 C2 C3 C4 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 N1 0.0 . . . . ? C2 N1 C6 C5 0.0 . . . . ? C6' N1' C2' C3' -0.7(6) . . . . ? N1' C2' C3' C4' 0.0 . . . . ? C2' C3' C4' C5' 0.0 . . . . ? C3' C4' C5' C6' 0.8(7) . . . . ? C4' C5' C6' N1' -1.5(14) . . . . ? C2' N1' C6' C5' 1.5(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C223 H223 N1 0.93 2.95 3.539(8) 122.4 2_666 C224 H224 N1 0.93 2.83 3.474(9) 127.5 2_666 C115 H115 N1' 0.93 2.71 3.40(4) 132.0 1_545 _diffrn_measured_fraction_theta_max 0.791 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.943 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.069 data_cmpnd02 _database_code_depnum_ccdc_archive 'CCDC 869209' #TrackingRef 'UWA120227.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H45 Ag N P3 S, C2 H8 N2' _chemical_formula_sum 'C57 H53 Ag N3 P3 S' _chemical_formula_weight 1012.86 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' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.276(7) _cell_length_b 13.780(10) _cell_length_c 14.313(3) _cell_angle_alpha 89.17(5) _cell_angle_beta 79.22(3) _cell_angle_gamma 80.40(6) _cell_volume 2536(2) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 8.0 _cell_measurement_theta_max 12.0 _exptl_crystal_description colorless _exptl_crystal_colour plate _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'XTAL: ABSCOR' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8766 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 24.99 _reflns_number_total 8766 _reflns_number_gt 5486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 control software' _computing_cell_refinement 'Enraf-Nonius CAD4 control software' _computing_data_reduction 'XTAL: ABSCOR, ADDREF, SORTRF' _computing_structure_solution 'Bruker SHELXTL, v. 5.1' _computing_structure_refinement 'Bruker SHELXTL, v. 5.1' _computing_molecular_graphics XTAL _computing_publication_material 'Bruker SHELXTL, v. 5.1' _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^)+(0.0930P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8766 _refine_ls_number_parameters 570 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1672 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.58888(15) 0.25989(17) 0.25609(18) 0.1014(7) Uani 1 1 d . . . C C 0.4837(5) 0.2355(4) 0.2210(4) 0.0627(15) Uani 1 1 d . . . N N 0.4119(4) 0.2172(4) 0.1980(4) 0.0746(15) Uani 1 1 d . . . Ag Ag 0.24340(3) 0.19457(3) 0.20359(3) 0.04794(15) Uani 1 1 d . . . P1 P 0.24515(11) 0.01760(10) 0.25728(10) 0.0490(3) Uani 1 1 d . . . C111 C 0.3034(4) -0.0168(4) 0.3614(4) 0.0483(12) Uani 1 1 d . . . C112 C 0.3014(5) 0.0539(5) 0.4292(5) 0.0776(19) Uani 1 1 d . . . H112 H 0.2716 0.1186 0.4206 0.093 Uiso 1 1 calc R . . C113 C 0.3427(6) 0.0301(6) 0.5090(5) 0.096(2) Uani 1 1 d . . . H113 H 0.3410 0.0788 0.5539 0.115 Uiso 1 1 calc R . . C114 C 0.3867(6) -0.0655(6) 0.5231(5) 0.086(2) Uani 1 1 d . . . H114 H 0.4147 -0.0816 0.5773 0.103 Uiso 1 1 calc R . . C115 C 0.3887(5) -0.1358(5) 0.4573(5) 0.0752(18) Uani 1 1 d . . . H115 H 0.4183 -0.2005 0.4664 0.090 Uiso 1 1 calc R . . C116 C 0.3471(5) -0.1123(4) 0.3769(4) 0.0674(16) Uani 1 1 d . . . H116 H 0.3485 -0.1615 0.3325 0.081 Uiso 1 1 calc R . . C121 C 0.3141(4) -0.0771(4) 0.1702(3) 0.0465(12) Uani 1 1 d . . . C122 C 0.4038(5) -0.0609(5) 0.1110(5) 0.0692(17) Uani 1 1 d . . . H122 H 0.4275 -0.0015 0.1152 0.083 Uiso 1 1 calc R . . C123 C 0.4591(5) -0.1319(6) 0.0452(5) 0.083(2) Uani 1 1 d . . . H123 H 0.5204 -0.1207 0.0064 0.100 Uiso 1 1 calc R . . C124 C 0.4238(5) -0.2188(6) 0.0371(5) 0.079(2) Uani 1 1 d . . . H124 H 0.4606 -0.2660 -0.0080 0.094 Uiso 1 1 calc R . . C125 C 0.3357(5) -0.2359(5) 0.0944(5) 0.0749(18) Uani 1 1 d . . . H125 H 0.3120 -0.2950 0.0889 0.090 Uiso 1 1 calc R . . C126 C 0.2803(5) -0.1655(4) 0.1617(4) 0.0625(15) Uani 1 1 d . . . H126 H 0.2200 -0.1780 0.2013 0.075 Uiso 1 1 calc R . . C131 C 0.1151(4) -0.0153(4) 0.2864(4) 0.0511(12) Uani 1 1 d . . . C132 C 0.0486(5) 0.0105(4) 0.2218(4) 0.0618(15) Uani 1 1 d . . . H132 H 0.0712 0.0441 0.1671 0.074 Uiso 1 1 calc R . . C133 C -0.0494(5) -0.0131(5) 0.2380(5) 0.0742(18) Uani 1 1 d . . . H133 H -0.0928 0.0040 0.1942 0.089 Uiso 1 1 calc R . . C134 C -0.0829(6) -0.0616(5) 0.3184(6) 0.087(2) Uani 1 1 d . . . H134 H -0.1492 -0.0782 0.3288 0.104 Uiso 1 1 calc R . . C135 C -0.0206(6) -0.0860(6) 0.3837(5) 0.088(2) Uani 1 1 d . . . H135 H -0.0453 -0.1180 0.4388 0.106 Uiso 1 1 calc R . . C136 C 0.0789(5) -0.0638(5) 0.3692(5) 0.0700(17) Uani 1 1 d . . . H136 H 0.1211 -0.0809 0.4139 0.084 Uiso 1 1 calc R . . P2 P 0.14058(11) 0.32759(10) 0.32793(10) 0.0505(3) Uani 1 1 d . . . C211 C 0.1334(4) 0.4568(4) 0.2959(4) 0.0532(13) Uani 1 1 d . . . C212 C 0.1098(5) 0.4854(4) 0.2079(4) 0.0673(16) Uani 1 1 d . . . H212 H 0.1037 0.4378 0.1649 0.081 Uiso 1 1 calc R . . C213 C 0.0953(5) 0.5824(5) 0.1835(6) 0.0811(19) Uani 1 1 d . . . H213 H 0.0781 0.5997 0.1247 0.097 Uiso 1 1 calc R . . C214 C 0.1058(5) 0.6550(5) 0.2447(6) 0.085(2) Uani 1 1 d . . . H214 H 0.0954 0.7209 0.2280 0.102 Uiso 1 1 calc R . . C215 C 0.1323(6) 0.6275(5) 0.3318(6) 0.084(2) Uani 1 1 d . . . H215 H 0.1405 0.6753 0.3737 0.100 Uiso 1 1 calc R . . C216 C 0.1465(5) 0.5298(4) 0.3567(5) 0.0667(16) Uani 1 1 d . . . H216 H 0.1651 0.5124 0.4149 0.080 Uiso 1 1 calc R . . C221 C 0.1903(4) 0.3238(4) 0.4383(4) 0.0521(13) Uani 1 1 d . . . C222 C 0.2968(5) 0.3229(5) 0.4318(5) 0.0714(17) Uani 1 1 d . . . H222 H 0.3395 0.3231 0.3724 0.086 Uiso 1 1 calc R . . C223 C 0.3385(6) 0.3218(5) 0.5125(6) 0.084(2) Uani 1 1 d . . . H223 H 0.4095 0.3213 0.5076 0.101 Uiso 1 1 calc R . . C224 C 0.2764(7) 0.3213(5) 0.6004(5) 0.085(2) Uani 1 1 d . . . H224 H 0.3053 0.3214 0.6548 0.102 Uiso 1 1 calc R . . C225 C 0.1716(6) 0.3208(5) 0.6086(5) 0.083(2) Uani 1 1 d . . . H225 H 0.1300 0.3190 0.6683 0.100 Uiso 1 1 calc R . . C226 C 0.1288(5) 0.3228(5) 0.5285(4) 0.0652(15) Uani 1 1 d . . . H226 H 0.0577 0.3235 0.5344 0.078 Uiso 1 1 calc R . . C231 C 0.0026(4) 0.3196(4) 0.3657(4) 0.0519(13) Uani 1 1 d . . . C232 C -0.0248(5) 0.2272(4) 0.3807(4) 0.0591(14) Uani 1 1 d . . . H232 H 0.0270 0.1719 0.3737 0.071 Uiso 1 1 calc R . . C233 C -0.1276(5) 0.2156(5) 0.4058(5) 0.0747(18) Uani 1 1 d . . . H233 H -0.1446 0.1531 0.4173 0.090 Uiso 1 1 calc R . . C234 C -0.2057(5) 0.2975(6) 0.4139(5) 0.0789(19) Uani 1 1 d . . . H234 H -0.2752 0.2901 0.4285 0.095 Uiso 1 1 calc R . . C235 C -0.1792(5) 0.3887(5) 0.4001(5) 0.0754(18) Uani 1 1 d . . . H235 H -0.2311 0.4439 0.4068 0.090 Uiso 1 1 calc R . . C236 C -0.0761(4) 0.4002(4) 0.3761(5) 0.0650(15) Uani 1 1 d . . . H236 H -0.0595 0.4631 0.3669 0.078 Uiso 1 1 calc R . . P3 P 0.20108(11) 0.22822(10) 0.03882(10) 0.0492(3) Uani 1 1 d . . . C311 C 0.2188(4) 0.3510(4) -0.0023(4) 0.0557(13) Uani 1 1 d . . . C312 C 0.3015(5) 0.3879(4) 0.0215(5) 0.0695(17) Uani 1 1 d . . . H312 H 0.3413 0.3531 0.0618 0.083 Uiso 1 1 calc R . . C313 C 0.3249(6) 0.4766(5) -0.0148(6) 0.094(2) Uani 1 1 d . . . H313 H 0.3825 0.4996 -0.0010 0.113 Uiso 1 1 calc R . . C314 C 0.2650(7) 0.5303(6) -0.0703(7) 0.109(3) Uani 1 1 d . . . H314 H 0.2806 0.5906 -0.0933 0.131 Uiso 1 1 calc R . . C315 C 0.1814(8) 0.4955(6) -0.0923(7) 0.117(3) Uani 1 1 d . . . H315 H 0.1403 0.5322 -0.1306 0.141 Uiso 1 1 calc R . . C316 C 0.1576(6) 0.4060(5) -0.0580(6) 0.090(2) Uani 1 1 d . . . H316 H 0.1002 0.3831 -0.0726 0.108 Uiso 1 1 calc R . . C321 C 0.2692(4) 0.1512(4) -0.0646(4) 0.0522(13) Uani 1 1 d . . . C322 C 0.2737(5) 0.0503(4) -0.0582(4) 0.0657(16) Uani 1 1 d . . . H322 H 0.2422 0.0236 -0.0025 0.079 Uiso 1 1 calc R . . C323 C 0.3249(6) -0.0111(5) -0.1340(5) 0.082(2) Uani 1 1 d . . . H323 H 0.3259 -0.0787 -0.1296 0.098 Uiso 1 1 calc R . . C324 C 0.3733(6) 0.0265(5) -0.2146(5) 0.085(2) Uani 1 1 d . . . H324 H 0.4086 -0.0153 -0.2649 0.102 Uiso 1 1 calc R . . C325 C 0.3704(6) 0.1252(6) -0.2221(5) 0.090(2) Uani 1 1 d . . . H325 H 0.4045 0.1507 -0.2773 0.108 Uiso 1 1 calc R . . C326 C 0.3179(6) 0.1870(5) -0.1493(4) 0.0746(18) Uani 1 1 d . . . H326 H 0.3146 0.2546 -0.1565 0.089 Uiso 1 1 calc R . . C331 C 0.0650(4) 0.2228(4) 0.0398(4) 0.0499(12) Uani 1 1 d . . . C332 C -0.0066(4) 0.2476(4) 0.1234(4) 0.0599(14) Uani 1 1 d . . . H332 H 0.0163 0.2697 0.1756 0.072 Uiso 1 1 calc R . . C333 C -0.1096(5) 0.2408(5) 0.1318(5) 0.0676(16) Uani 1 1 d . . . H333 H -0.1557 0.2598 0.1883 0.081 Uiso 1 1 calc R . . C334 C -0.1446(5) 0.2058(5) 0.0565(5) 0.0751(18) Uani 1 1 d . . . H334 H -0.2143 0.2002 0.0619 0.090 Uiso 1 1 calc R . . C335 C -0.0763(6) 0.1795(5) -0.0260(6) 0.085(2) Uani 1 1 d . . . H335 H -0.0999 0.1558 -0.0770 0.102 Uiso 1 1 calc R . . C336 C 0.0279(5) 0.1875(5) -0.0352(5) 0.0754(18) Uani 1 1 d . . . H336 H 0.0733 0.1691 -0.0922 0.090 Uiso 1 1 calc R . . N1 N 0.5329(15) 0.4988(14) 0.3789(12) 0.329(9) Uiso 1 1 d D . . H11 H 0.5466 0.4437 0.3425 0.494 Uiso 1 1 d . . . H12 H 0.5852 0.5335 0.3633 0.494 Uiso 1 1 d . . . C1 C 0.4343(12) 0.5594(13) 0.3630(9) 0.283(10) Uiso 1 1 d D B . H1A H 0.3774 0.5227 0.3800 0.340 Uiso 1 1 calc R . . H1B H 0.4188 0.6188 0.4023 0.340 Uiso 1 1 calc R . . C2 C 0.4464(13) 0.5847(10) 0.2637(11) 0.253(8) Uiso 1 1 d D . . H2A H 0.5166 0.5972 0.2413 0.303 Uiso 0.50 1 calc PR A 1 H2B H 0.3986 0.6446 0.2568 0.303 Uiso 0.50 1 calc PR A 1 H2C H 0.3851 0.6240 0.2483 0.303 Uiso 0.50 1 d PR A 2 H2D H 0.4623 0.5251 0.2260 0.303 Uiso 0.50 1 d PR A 2 N2A N 0.4264(14) 0.5060(12) 0.2049(10) 0.137(6) Uiso 0.50 1 d PD B 1 H21A H 0.3717 0.4802 0.2359 0.206 Uiso 0.50 1 d P C 1 H22A H 0.4829 0.4586 0.1934 0.206 Uiso 0.50 1 d P D 1 N2B N 0.5275(16) 0.6468(16) 0.2420(14) 0.196(9) Uiso 0.50 1 d PD B 2 H21B H 0.5216 0.6890 0.2909 0.295 Uiso 0.50 1 d P E 2 H22B H 0.5905 0.6086 0.2329 0.295 Uiso 0.50 1 d P F 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 S 0.0702(12) 0.1001(15) 0.1414(19) -0.0371(14) -0.0350(12) -0.0154(10) C 0.059(4) 0.060(4) 0.065(4) -0.011(3) -0.001(3) -0.008(3) N 0.049(3) 0.096(4) 0.082(4) -0.018(3) -0.010(3) -0.023(3) Ag 0.0509(3) 0.0441(2) 0.0523(3) 0.00227(17) -0.01582(18) -0.01097(17) P1 0.0546(8) 0.0440(7) 0.0526(8) 0.0055(6) -0.0159(6) -0.0139(6) C111 0.053(3) 0.046(3) 0.051(3) 0.005(2) -0.018(2) -0.011(2) C112 0.088(5) 0.062(4) 0.087(5) -0.012(3) -0.036(4) -0.003(3) C113 0.113(6) 0.114(6) 0.069(5) -0.024(4) -0.050(4) -0.002(5) C114 0.086(5) 0.115(6) 0.063(4) 0.010(4) -0.036(4) -0.010(4) C115 0.089(5) 0.076(4) 0.068(4) 0.020(3) -0.036(4) -0.012(4) C116 0.092(5) 0.056(4) 0.061(4) 0.001(3) -0.031(3) -0.012(3) C121 0.043(3) 0.054(3) 0.046(3) 0.009(2) -0.015(2) -0.011(2) C122 0.061(4) 0.071(4) 0.076(4) 0.020(3) -0.012(3) -0.014(3) C123 0.057(4) 0.102(6) 0.080(5) 0.015(4) -0.002(3) 0.004(4) C124 0.070(4) 0.095(5) 0.057(4) -0.012(4) -0.006(3) 0.018(4) C125 0.070(4) 0.075(4) 0.078(4) -0.016(3) -0.010(4) -0.011(3) C126 0.060(4) 0.064(4) 0.065(4) -0.016(3) -0.008(3) -0.018(3) C131 0.054(3) 0.042(3) 0.058(3) -0.002(2) -0.011(3) -0.009(2) C132 0.063(4) 0.061(4) 0.062(4) 0.001(3) -0.017(3) -0.008(3) C133 0.065(4) 0.069(4) 0.093(5) -0.006(4) -0.026(4) -0.011(3) C134 0.065(4) 0.082(5) 0.116(6) -0.008(4) -0.007(4) -0.028(4) C135 0.071(5) 0.106(6) 0.088(5) 0.030(4) 0.000(4) -0.038(4) C136 0.069(4) 0.073(4) 0.070(4) 0.016(3) -0.011(3) -0.019(3) P2 0.0533(8) 0.0453(8) 0.0516(8) -0.0071(6) -0.0076(6) -0.0063(6) C211 0.050(3) 0.044(3) 0.063(3) -0.009(2) -0.002(3) -0.007(2) C212 0.081(4) 0.057(4) 0.065(4) 0.003(3) -0.016(3) -0.011(3) C213 0.081(5) 0.066(4) 0.095(5) 0.018(4) -0.016(4) -0.008(4) C214 0.072(4) 0.050(4) 0.133(7) 0.018(4) -0.014(4) -0.019(3) C215 0.084(5) 0.059(4) 0.112(6) -0.006(4) -0.012(4) -0.030(4) C216 0.069(4) 0.057(4) 0.075(4) -0.005(3) -0.008(3) -0.021(3) C221 0.058(3) 0.045(3) 0.055(3) -0.005(2) -0.016(3) -0.005(2) C222 0.057(4) 0.081(4) 0.077(4) -0.010(3) -0.019(3) -0.004(3) C223 0.068(4) 0.089(5) 0.097(6) -0.009(4) -0.035(4) 0.004(4) C224 0.113(6) 0.078(5) 0.075(5) 0.004(4) -0.047(5) -0.009(4) C225 0.104(6) 0.091(5) 0.058(4) 0.002(3) -0.025(4) -0.014(4) C226 0.066(4) 0.074(4) 0.056(3) 0.001(3) -0.011(3) -0.013(3) C231 0.055(3) 0.051(3) 0.049(3) -0.009(2) -0.011(2) -0.005(2) C232 0.062(4) 0.051(3) 0.062(3) -0.005(3) -0.004(3) -0.010(3) C233 0.083(5) 0.074(4) 0.070(4) -0.006(3) 0.000(3) -0.035(4) C234 0.064(4) 0.094(5) 0.082(5) -0.004(4) -0.012(3) -0.025(4) C235 0.050(4) 0.076(5) 0.093(5) -0.003(4) -0.005(3) 0.001(3) C236 0.055(4) 0.051(3) 0.088(4) -0.002(3) -0.011(3) -0.007(3) P3 0.0557(8) 0.0455(7) 0.0491(8) 0.0031(6) -0.0169(6) -0.0083(6) C311 0.058(3) 0.042(3) 0.067(4) 0.003(3) -0.011(3) -0.007(2) C312 0.063(4) 0.050(3) 0.095(5) 0.003(3) -0.015(3) -0.009(3) C313 0.083(5) 0.065(5) 0.136(7) 0.017(5) -0.018(5) -0.027(4) C314 0.115(7) 0.056(4) 0.161(9) 0.027(5) -0.028(6) -0.029(4) C315 0.127(7) 0.072(5) 0.167(9) 0.051(6) -0.066(7) -0.018(5) C316 0.098(5) 0.061(4) 0.120(6) 0.025(4) -0.047(5) -0.013(4) C321 0.054(3) 0.051(3) 0.053(3) 0.011(2) -0.021(2) -0.003(2) C322 0.082(4) 0.055(4) 0.060(4) 0.004(3) -0.015(3) -0.009(3) C323 0.105(6) 0.065(4) 0.071(4) -0.011(3) -0.011(4) -0.006(4) C324 0.104(6) 0.079(5) 0.062(4) -0.024(4) -0.018(4) 0.016(4) C325 0.117(6) 0.089(5) 0.046(4) -0.003(3) 0.011(4) 0.002(4) C326 0.101(5) 0.063(4) 0.058(4) 0.007(3) -0.010(3) -0.014(4) C331 0.059(3) 0.044(3) 0.051(3) 0.010(2) -0.020(3) -0.012(2) C332 0.059(4) 0.065(4) 0.058(3) -0.004(3) -0.018(3) -0.005(3) C333 0.057(4) 0.078(4) 0.067(4) 0.009(3) -0.015(3) -0.004(3) C334 0.064(4) 0.075(4) 0.093(5) 0.012(4) -0.021(4) -0.022(3) C335 0.077(5) 0.092(5) 0.100(6) -0.011(4) -0.043(4) -0.026(4) C336 0.069(4) 0.104(5) 0.059(4) -0.012(3) -0.022(3) -0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S C 1.655(7) . ? C N 1.132(7) . ? N Ag 2.296(5) . ? Ag P3 2.5434(15) . ? Ag P1 2.544(2) . ? Ag P2 2.596(2) . ? P1 C121 1.822(6) . ? P1 C111 1.826(5) . ? P1 C131 1.830(5) . ? C111 C112 1.377(8) . ? C111 C116 1.380(8) . ? C112 C113 1.370(9) . ? C112 H112 0.9300 . ? C113 C114 1.377(10) . ? C113 H113 0.9300 . ? C114 C115 1.355(10) . ? C114 H114 0.9300 . ? C115 C116 1.378(8) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C121 C122 1.376(8) . ? C121 C126 1.380(7) . ? C122 C123 1.382(10) . ? C122 H122 0.9300 . ? C123 C124 1.370(10) . ? C123 H123 0.9300 . ? C124 C125 1.352(9) . ? C124 H124 0.9300 . ? C125 C126 1.391(8) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C132 1.397(8) . ? C131 C136 1.397(8) . ? C132 C133 1.370(8) . ? C132 H132 0.9300 . ? C133 C134 1.362(10) . ? C133 H133 0.9300 . ? C134 C135 1.365(10) . ? C134 H134 0.9300 . ? C135 C136 1.382(9) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? P2 C221 1.820(5) . ? P2 C211 1.824(6) . ? P2 C231 1.831(6) . ? C211 C212 1.391(8) . ? C211 C216 1.392(8) . ? C212 C213 1.368(9) . ? C212 H212 0.9300 . ? C213 C214 1.381(10) . ? C213 H213 0.9300 . ? C214 C215 1.388(11) . ? C214 H214 0.9300 . ? C215 C216 1.379(9) . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? C221 C226 1.393(8) . ? C221 C222 1.398(8) . ? C222 C223 1.370(9) . ? C222 H222 0.9300 . ? C223 C224 1.370(10) . ? C223 H223 0.9300 . ? C224 C225 1.375(10) . ? C224 H224 0.9300 . ? C225 C226 1.369(9) . ? C225 H225 0.9300 . ? C226 H226 0.9300 . ? C231 C236 1.382(8) . ? C231 C232 1.384(8) . ? C232 C233 1.381(8) . ? C232 H232 0.9300 . ? C233 C234 1.389(10) . ? C233 H233 0.9300 . ? C234 C235 1.363(9) . ? C234 H234 0.9300 . ? C235 C236 1.383(8) . ? C235 H235 0.9300 . ? C236 H236 0.9300 . ? P3 C331 1.818(5) . ? P3 C311 1.822(6) . ? P3 C321 1.833(6) . ? C311 C316 1.375(8) . ? C311 C312 1.382(8) . ? C312 C313 1.381(9) . ? C312 H312 0.9300 . ? C313 C314 1.354(11) . ? C313 H313 0.9300 . ? C314 C315 1.370(11) . ? C314 H314 0.9300 . ? C315 C316 1.384(10) . ? C315 H315 0.9300 . ? C316 H316 0.9300 . ? C321 C322 1.384(8) . ? C321 C326 1.388(8) . ? C322 C323 1.384(9) . ? C322 H322 0.9300 . ? C323 C324 1.352(10) . ? C323 H323 0.9300 . ? C324 C325 1.358(10) . ? C324 H324 0.9300 . ? C325 C326 1.361(9) . ? C325 H325 0.9300 . ? C326 H326 0.9300 . ? C331 C336 1.388(7) . ? C331 C332 1.389(8) . ? C332 C333 1.368(8) . ? C332 H332 0.9300 . ? C333 C334 1.373(9) . ? C333 H333 0.9300 . ? C334 C335 1.360(10) . ? C334 H334 0.9300 . ? C335 C336 1.388(9) . ? C335 H335 0.9300 . ? C336 H336 0.9300 . ? N1 C1 1.485(9) . ? N1 H11 0.9000 . ? N1 H12 0.9000 . ? C1 C2 1.444(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2A 1.470(9) . ? C2 N2B 1.471(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9601 . ? C2 H2D 0.9600 . ? N2A H2D 0.6975 . ? N2A H21A 0.9000 . ? N2A H22A 0.9001 . ? N2B H21B 0.9001 . ? N2B H22B 0.9001 . ? 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 N C S 178.7(7) . . ? C N Ag 160.7(5) . . ? N Ag P3 107.62(15) . . ? N Ag P1 103.38(16) . . ? P3 Ag P1 114.94(6) . . ? N Ag P2 102.01(14) . . ? P3 Ag P2 112.18(6) . . ? P1 Ag P2 115.11(7) . . ? C121 P1 C111 102.4(2) . . ? C121 P1 C131 102.6(2) . . ? C111 P1 C131 104.8(2) . . ? C121 P1 Ag 115.92(17) . . ? C111 P1 Ag 116.35(17) . . ? C131 P1 Ag 113.04(18) . . ? C112 C111 C116 118.0(5) . . ? C112 C111 P1 119.5(4) . . ? C116 C111 P1 122.4(4) . . ? C113 C112 C111 121.0(6) . . ? C113 C112 H112 119.5 . . ? C111 C112 H112 119.5 . . ? C112 C113 C114 120.3(7) . . ? C112 C113 H113 119.8 . . ? C114 C113 H113 119.8 . . ? C115 C114 C113 119.4(6) . . ? C115 C114 H114 120.3 . . ? C113 C114 H114 120.3 . . ? C114 C115 C116 120.6(6) . . ? C114 C115 H115 119.7 . . ? C116 C115 H115 119.7 . . ? C115 C116 C111 120.8(6) . . ? C115 C116 H116 119.6 . . ? C111 C116 H116 119.6 . . ? C122 C121 C126 118.4(5) . . ? C122 C121 P1 119.1(4) . . ? C126 C121 P1 122.5(4) . . ? C121 C122 C123 120.6(6) . . ? C121 C122 H122 119.7 . . ? C123 C122 H122 119.7 . . ? C124 C123 C122 120.2(6) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C125 C124 C123 120.0(6) . . ? C125 C124 H124 120.0 . . ? C123 C124 H124 120.0 . . ? C124 C125 C126 120.2(7) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C121 C126 C125 120.5(6) . . ? C121 C126 H126 119.8 . . ? C125 C126 H126 119.8 . . ? C132 C131 C136 118.7(5) . . ? C132 C131 P1 117.5(4) . . ? C136 C131 P1 123.8(4) . . ? C133 C132 C131 120.8(6) . . ? C133 C132 H132 119.6 . . ? C131 C132 H132 119.6 . . ? C134 C133 C132 119.8(7) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C133 C134 C135 120.7(6) . . ? C133 C134 H134 119.6 . . ? C135 C134 H134 119.6 . . ? C134 C135 C136 120.9(7) . . ? C134 C135 H135 119.5 . . ? C136 C135 H135 119.5 . . ? C135 C136 C131 119.0(6) . . ? C135 C136 H136 120.5 . . ? C131 C136 H136 120.5 . . ? C221 P2 C211 102.6(3) . . ? C221 P2 C231 104.3(2) . . ? C211 P2 C231 101.2(3) . . ? C221 P2 Ag 113.52(18) . . ? C211 P2 Ag 118.55(18) . . ? C231 P2 Ag 114.71(17) . . ? C212 C211 C216 117.7(5) . . ? C212 C211 P2 118.8(4) . . ? C216 C211 P2 123.4(5) . . ? C213 C212 C211 121.2(6) . . ? C213 C212 H212 119.4 . . ? C211 C212 H212 119.4 . . ? C212 C213 C214 121.0(7) . . ? C212 C213 H213 119.5 . . ? C214 C213 H213 119.5 . . ? C213 C214 C215 118.5(6) . . ? C213 C214 H214 120.7 . . ? C215 C214 H214 120.7 . . ? C216 C215 C214 120.5(7) . . ? C216 C215 H215 119.8 . . ? C214 C215 H215 119.8 . . ? C215 C216 C211 121.0(6) . . ? C215 C216 H216 119.5 . . ? C211 C216 H216 119.5 . . ? C226 C221 C222 118.2(5) . . ? C226 C221 P2 124.2(4) . . ? C222 C221 P2 117.6(4) . . ? C223 C222 C221 120.3(6) . . ? C223 C222 H222 119.8 . . ? C221 C222 H222 119.8 . . ? C224 C223 C222 120.4(7) . . ? C224 C223 H223 119.8 . . ? C222 C223 H223 119.8 . . ? C223 C224 C225 120.4(6) . . ? C223 C224 H224 119.8 . . ? C225 C224 H224 119.8 . . ? C226 C225 C224 119.8(7) . . ? C226 C225 H225 120.1 . . ? C224 C225 H225 120.1 . . ? C225 C226 C221 120.9(6) . . ? C225 C226 H226 119.5 . . ? C221 C226 H226 119.5 . . ? C236 C231 C232 118.0(5) . . ? C236 C231 P2 123.7(4) . . ? C232 C231 P2 118.2(4) . . ? C233 C232 C231 121.2(6) . . ? C233 C232 H232 119.4 . . ? C231 C232 H232 119.4 . . ? C232 C233 C234 119.8(6) . . ? C232 C233 H233 120.1 . . ? C234 C233 H233 120.1 . . ? C235 C234 C233 119.3(6) . . ? C235 C234 H234 120.3 . . ? C233 C234 H234 120.3 . . ? C234 C235 C236 120.8(6) . . ? C234 C235 H235 119.6 . . ? C236 C235 H235 119.6 . . ? C231 C236 C235 120.9(6) . . ? C231 C236 H236 119.6 . . ? C235 C236 H236 119.6 . . ? C331 P3 C311 105.3(3) . . ? C331 P3 C321 103.2(2) . . ? C311 P3 C321 101.9(3) . . ? C331 P3 Ag 110.39(17) . . ? C311 P3 Ag 112.8(2) . . ? C321 P3 Ag 121.61(17) . . ? C316 C311 C312 119.2(6) . . ? C316 C311 P3 123.7(5) . . ? C312 C311 P3 117.1(4) . . ? C313 C312 C311 119.8(7) . . ? C313 C312 H312 120.1 . . ? C311 C312 H312 120.1 . . ? C314 C313 C312 120.9(7) . . ? C314 C313 H313 119.6 . . ? C312 C313 H313 119.6 . . ? C313 C314 C315 119.6(7) . . ? C313 C314 H314 120.2 . . ? C315 C314 H314 120.2 . . ? C314 C315 C316 120.4(8) . . ? C314 C315 H315 119.8 . . ? C316 C315 H315 119.8 . . ? C311 C316 C315 119.9(7) . . ? C311 C316 H316 120.0 . . ? C315 C316 H316 120.0 . . ? C322 C321 C326 117.3(6) . . ? C322 C321 P3 118.3(4) . . ? C326 C321 P3 124.5(5) . . ? C323 C322 C321 120.5(6) . . ? C323 C322 H322 119.7 . . ? C321 C322 H322 119.7 . . ? C324 C323 C322 120.4(7) . . ? C324 C323 H323 119.8 . . ? C322 C323 H323 119.8 . . ? C323 C324 C325 120.0(6) . . ? C323 C324 H324 120.0 . . ? C325 C324 H324 120.0 . . ? C324 C325 C326 120.4(7) . . ? C324 C325 H325 119.8 . . ? C326 C325 H325 119.8 . . ? C325 C326 C321 121.3(6) . . ? C325 C326 H326 119.3 . . ? C321 C326 H326 119.3 . . ? C336 C331 C332 116.7(5) . . ? C336 C331 P3 124.4(5) . . ? C332 C331 P3 118.6(4) . . ? C333 C332 C331 122.4(5) . . ? C333 C332 H332 118.8 . . ? C331 C332 H332 118.8 . . ? C332 C333 C334 119.8(6) . . ? C332 C333 H333 120.1 . . ? C334 C333 H333 120.1 . . ? C335 C334 C333 119.3(6) . . ? C335 C334 H334 120.4 . . ? C333 C334 H334 120.4 . . ? C334 C335 C336 121.1(6) . . ? C334 C335 H335 119.5 . . ? C336 C335 H335 119.5 . . ? C331 C336 C335 120.6(6) . . ? C331 C336 H336 119.7 . . ? C335 C336 H336 119.7 . . ? C1 N1 H11 109.5 . . ? C1 N1 H12 109.5 . . ? H11 N1 H12 109.5 . . ? C2 C1 N1 108.3(9) . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? N1 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? C1 C2 N2A 112.0(9) . . ? C1 C2 N2B 108.8(8) . . ? N2A C2 N2B 128.5(17) . . ? C1 C2 H2A 109.2 . . ? N2A C2 H2A 109.2 . . ? N2B C2 H2A 25.2 . . ? C1 C2 H2B 109.2 . . ? N2A C2 H2B 109.2 . . ? N2B C2 H2B 84.9 . . ? H2A C2 H2B 107.9 . . ? C1 C2 H2C 112.8 . . ? N2A C2 H2C 87.0 . . ? N2B C2 H2C 104.9 . . ? H2A C2 H2C 124.3 . . ? H2B C2 H2C 23.4 . . ? C1 C2 H2D 108.9 . . ? N2A C2 H2D 23.1 . . ? N2B C2 H2D 112.9 . . ? H2A C2 H2D 89.9 . . ? H2B C2 H2D 129.1 . . ? H2C C2 H2D 108.7 . . ? C2 N2A H2D 32.7 . . ? C2 N2A H21A 109.5 . . ? H2D N2A H21A 125.8 . . ? C2 N2A H22A 109.5 . . ? H2D N2A H22A 77.0 . . ? H21A N2A H22A 109.5 . . ? C2 N2B H21B 109.5 . . ? C2 N2B H22B 109.5 . . ? H21B N2B H22B 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 S C N Ag 73(28) . . . . ? C N Ag P3 150.0(17) . . . . ? C N Ag P1 -88.0(17) . . . . ? C N Ag P2 31.8(17) . . . . ? N Ag P1 C121 -71.1(2) . . . . ? P3 Ag P1 C121 45.90(19) . . . . ? P2 Ag P1 C121 178.56(17) . . . . ? N Ag P1 C111 49.4(2) . . . . ? P3 Ag P1 C111 166.4(2) . . . . ? P2 Ag P1 C111 -60.9(2) . . . . ? N Ag P1 C131 170.8(2) . . . . ? P3 Ag P1 C131 -72.2(2) . . . . ? P2 Ag P1 C131 60.5(2) . . . . ? C121 P1 C111 C112 155.9(5) . . . . ? C131 P1 C111 C112 -97.3(5) . . . . ? Ag P1 C111 C112 28.4(6) . . . . ? C121 P1 C111 C116 -26.2(5) . . . . ? C131 P1 C111 C116 80.7(5) . . . . ? Ag P1 C111 C116 -153.7(4) . . . . ? C116 C111 C112 C113 0.7(10) . . . . ? P1 C111 C112 C113 178.8(6) . . . . ? C111 C112 C113 C114 -0.3(12) . . . . ? C112 C113 C114 C115 0.0(13) . . . . ? C113 C114 C115 C116 -0.1(12) . . . . ? C114 C115 C116 C111 0.5(11) . . . . ? C112 C111 C116 C115 -0.8(10) . . . . ? P1 C111 C116 C115 -178.8(5) . . . . ? C111 P1 C121 C122 -90.8(5) . . . . ? C131 P1 C121 C122 160.6(4) . . . . ? Ag P1 C121 C122 36.9(5) . . . . ? C111 P1 C121 C126 88.6(5) . . . . ? C131 P1 C121 C126 -19.9(5) . . . . ? Ag P1 C121 C126 -143.6(4) . . . . ? C126 C121 C122 C123 -0.6(9) . . . . ? P1 C121 C122 C123 178.9(5) . . . . ? C121 C122 C123 C124 1.3(10) . . . . ? C122 C123 C124 C125 -1.1(11) . . . . ? C123 C124 C125 C126 0.2(11) . . . . ? C122 C121 C126 C125 -0.3(9) . . . . ? P1 C121 C126 C125 -179.8(5) . . . . ? C124 C125 C126 C121 0.5(10) . . . . ? C121 P1 C131 C132 -78.5(5) . . . . ? C111 P1 C131 C132 174.8(4) . . . . ? Ag P1 C131 C132 47.1(5) . . . . ? C121 P1 C131 C136 102.0(5) . . . . ? C111 P1 C131 C136 -4.7(6) . . . . ? Ag P1 C131 C136 -132.4(5) . . . . ? C136 C131 C132 C133 -1.5(9) . . . . ? P1 C131 C132 C133 179.0(5) . . . . ? C131 C132 C133 C134 0.5(10) . . . . ? C132 C133 C134 C135 0.8(11) . . . . ? C133 C134 C135 C136 -1.2(12) . . . . ? C134 C135 C136 C131 0.3(11) . . . . ? C132 C131 C136 C135 1.1(9) . . . . ? P1 C131 C136 C135 -179.4(5) . . . . ? N Ag P2 C221 -51.1(3) . . . . ? P3 Ag P2 C221 -166.0(2) . . . . ? P1 Ag P2 C221 60.0(2) . . . . ? N Ag P2 C211 69.5(3) . . . . ? P3 Ag P2 C211 -45.4(2) . . . . ? P1 Ag P2 C211 -179.4(2) . . . . ? N Ag P2 C231 -170.9(2) . . . . ? P3 Ag P2 C231 74.2(2) . . . . ? P1 Ag P2 C231 -59.7(2) . . . . ? C221 P2 C211 C212 172.4(5) . . . . ? C231 P2 C211 C212 -80.0(5) . . . . ? Ag P2 C211 C212 46.4(5) . . . . ? C221 P2 C211 C216 -10.2(5) . . . . ? C231 P2 C211 C216 97.4(5) . . . . ? Ag P2 C211 C216 -136.2(4) . . . . ? C216 C211 C212 C213 -2.8(9) . . . . ? P2 C211 C212 C213 174.7(5) . . . . ? C211 C212 C213 C214 1.3(10) . . . . ? C212 C213 C214 C215 0.5(11) . . . . ? C213 C214 C215 C216 -0.8(11) . . . . ? C214 C215 C216 C211 -0.8(10) . . . . ? C212 C211 C216 C215 2.6(9) . . . . ? P2 C211 C216 C215 -174.9(5) . . . . ? C211 P2 C221 C226 100.9(5) . . . . ? C231 P2 C221 C226 -4.4(5) . . . . ? Ag P2 C221 C226 -129.9(5) . . . . ? C211 P2 C221 C222 -78.4(5) . . . . ? C231 P2 C221 C222 176.4(5) . . . . ? Ag P2 C221 C222 50.8(5) . . . . ? C226 C221 C222 C223 -0.4(9) . . . . ? P2 C221 C222 C223 178.9(5) . . . . ? C221 C222 C223 C224 0.1(11) . . . . ? C222 C223 C224 C225 0.8(11) . . . . ? C223 C224 C225 C226 -1.4(11) . . . . ? C224 C225 C226 C221 1.1(10) . . . . ? C222 C221 C226 C225 -0.2(9) . . . . ? P2 C221 C226 C225 -179.4(5) . . . . ? C221 P2 C231 C236 98.6(5) . . . . ? C211 P2 C231 C236 -7.8(5) . . . . ? Ag P2 C231 C236 -136.7(4) . . . . ? C221 P2 C231 C232 -84.3(5) . . . . ? C211 P2 C231 C232 169.4(4) . . . . ? Ag P2 C231 C232 40.5(5) . . . . ? C236 C231 C232 C233 -0.3(9) . . . . ? P2 C231 C232 C233 -177.6(5) . . . . ? C231 C232 C233 C234 1.7(10) . . . . ? C232 C233 C234 C235 -2.3(10) . . . . ? C233 C234 C235 C236 1.5(11) . . . . ? C232 C231 C236 C235 -0.5(9) . . . . ? P2 C231 C236 C235 176.6(5) . . . . ? C234 C235 C236 C231 -0.1(10) . . . . ? N Ag P3 C331 -174.8(2) . . . . ? P1 Ag P3 C331 70.6(2) . . . . ? P2 Ag P3 C331 -63.4(2) . . . . ? N Ag P3 C311 -57.3(3) . . . . ? P1 Ag P3 C311 -171.9(2) . . . . ? P2 Ag P3 C311 54.1(2) . . . . ? N Ag P3 C321 64.1(3) . . . . ? P1 Ag P3 C321 -50.4(2) . . . . ? P2 Ag P3 C321 175.6(2) . . . . ? C331 P3 C311 C316 -25.2(7) . . . . ? C321 P3 C311 C316 82.3(6) . . . . ? Ag P3 C311 C316 -145.6(6) . . . . ? C331 P3 C311 C312 157.5(5) . . . . ? C321 P3 C311 C312 -95.0(5) . . . . ? Ag P3 C311 C312 37.1(5) . . . . ? C316 C311 C312 C313 -3.4(10) . . . . ? P3 C311 C312 C313 174.1(5) . . . . ? C311 C312 C313 C314 3.0(12) . . . . ? C312 C313 C314 C315 -1.4(14) . . . . ? C313 C314 C315 C316 0.2(16) . . . . ? C312 C311 C316 C315 2.3(12) . . . . ? P3 C311 C316 C315 -175.0(7) . . . . ? C314 C315 C316 C311 -0.7(15) . . . . ? C331 P3 C321 C322 -72.3(5) . . . . ? C311 P3 C321 C322 178.7(5) . . . . ? Ag P3 C321 C322 52.1(5) . . . . ? C331 P3 C321 C326 108.4(5) . . . . ? C311 P3 C321 C326 -0.6(6) . . . . ? Ag P3 C321 C326 -127.2(5) . . . . ? C326 C321 C322 C323 -0.2(9) . . . . ? P3 C321 C322 C323 -179.5(5) . . . . ? C321 C322 C323 C324 1.6(11) . . . . ? C322 C323 C324 C325 -1.1(12) . . . . ? C323 C324 C325 C326 -0.8(12) . . . . ? C324 C325 C326 C321 2.3(12) . . . . ? C322 C321 C326 C325 -1.7(10) . . . . ? P3 C321 C326 C325 177.5(6) . . . . ? C311 P3 C331 C336 92.9(5) . . . . ? C321 P3 C331 C336 -13.6(6) . . . . ? Ag P3 C331 C336 -145.1(5) . . . . ? C311 P3 C331 C332 -92.7(5) . . . . ? C321 P3 C331 C332 160.8(4) . . . . ? Ag P3 C331 C332 29.4(5) . . . . ? C336 C331 C332 C333 -1.8(9) . . . . ? P3 C331 C332 C333 -176.6(5) . . . . ? C331 C332 C333 C334 1.8(10) . . . . ? C332 C333 C334 C335 -0.8(10) . . . . ? C333 C334 C335 C336 -0.1(11) . . . . ? C332 C331 C336 C335 0.9(9) . . . . ? P3 C331 C336 C335 175.4(5) . . . . ? C334 C335 C336 C331 0.0(11) . . . . ? N1 C1 C2 N2A 83.6(18) . . . . ? N1 C1 C2 N2B -64(2) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.500 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.071 data_cmpnd03 _database_code_depnum_ccdc_archive 'CCDC 869210' #TrackingRef 'UWA120227.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H45 Ag As3 N S, 0.5(C6 H7 N)' _chemical_formula_sum 'C58 H48.50 Ag As3 N1.50 S' _chemical_formula_weight 1131.17 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2746(11) _cell_length_b 13.7113(11) _cell_length_c 14.2718(12) _cell_angle_alpha 85.260(1) _cell_angle_beta 88.870(1) _cell_angle_gamma 78.721(1) _cell_volume 2538.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 29.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 2.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.430 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details 'SADABS - Bruker area detector absorption corrections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28240 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 29.01 _reflns_number_total 12337 _reflns_number_gt 8739 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL, v. 5.1' _computing_structure_refinement 'Bruker SHELXTL, v. 5.1' _computing_molecular_graphics 'XTAL: Ortep' _computing_publication_material 'Bruker SHELXTL, v. 5.1' _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^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12337 _refine_ls_number_parameters 564 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.261768(16) 0.185521(18) 0.234562(16) 0.04539(8) Uani 1 1 d . . . N N 0.4148(2) 0.2340(3) 0.2255(3) 0.0804(11) Uani 1 1 d . . . C C 0.4741(3) 0.2741(3) 0.2000(3) 0.0762(12) Uani 1 1 d . . . S S 0.56635(13) 0.32849(15) 0.1577(2) 0.1814(11) Uani 1 1 d . . . As1 As 0.27335(2) 0.00183(2) 0.30786(2) 0.04397(9) Uani 1 1 d . . . C111 C 0.3312(2) -0.0322(2) 0.4328(2) 0.0450(7) Uani 1 1 d . . . C112 C 0.3373(3) 0.0466(3) 0.4868(3) 0.0575(9) Uani 1 1 d . . . H112 H 0.3119 0.1121 0.4638 0.069 Uiso 1 1 calc R . . C113 C 0.3818(3) 0.0263(3) 0.5756(3) 0.0696(10) Uani 1 1 d . . . H113 H 0.3860 0.0783 0.6123 0.083 Uiso 1 1 calc R . . C114 C 0.4191(3) -0.0696(3) 0.6088(3) 0.0689(11) Uani 1 1 d . . . H114 H 0.4497 -0.0827 0.6677 0.083 Uiso 1 1 calc R . . C115 C 0.4120(3) -0.1475(3) 0.5556(3) 0.0636(9) Uani 1 1 d . . . H115 H 0.4363 -0.2129 0.5795 0.076 Uiso 1 1 calc R . . C116 C 0.3692(2) -0.1290(3) 0.4682(2) 0.0554(8) Uani 1 1 d . . . H116 H 0.3657 -0.1818 0.4322 0.067 Uiso 1 1 calc R . . C121 C 0.3479(2) -0.1103(2) 0.2437(2) 0.0455(7) Uani 1 1 d . . . C122 C 0.4489(2) -0.1115(3) 0.2200(3) 0.0618(9) Uani 1 1 d . . . H122 H 0.4800 -0.0598 0.2354 0.074 Uiso 1 1 calc R . . C123 C 0.5052(3) -0.1897(4) 0.1729(3) 0.0764(12) Uani 1 1 d . . . H123 H 0.5742 -0.1911 0.1588 0.092 Uiso 1 1 calc R . . C124 C 0.4589(3) -0.2642(4) 0.1477(3) 0.0861(14) Uani 1 1 d . . . H124 H 0.4960 -0.3158 0.1153 0.103 Uiso 1 1 calc R . . C125 C 0.3583(3) -0.2631(3) 0.1699(4) 0.0946(16) Uani 1 1 d . . . H125 H 0.3267 -0.3138 0.1527 0.114 Uiso 1 1 calc R . . C126 C 0.3033(3) -0.1861(3) 0.2183(3) 0.0726(12) Uani 1 1 d . . . H126 H 0.2348 -0.1859 0.2337 0.087 Uiso 1 1 calc R . . C131 C 0.1383(2) -0.0332(2) 0.3220(2) 0.0457(7) Uani 1 1 d . . . C132 C 0.0709(2) -0.0065(3) 0.2469(2) 0.0562(8) Uani 1 1 d . . . H132 H 0.0917 0.0252 0.1918 0.067 Uiso 1 1 calc R . . C133 C -0.0269(3) -0.0268(3) 0.2536(3) 0.0698(11) Uani 1 1 d . . . H133 H -0.0714 -0.0098 0.2028 0.084 Uiso 1 1 calc R . . C134 C -0.0584(3) -0.0718(4) 0.3350(3) 0.0756(12) Uani 1 1 d . . . H134 H -0.1249 -0.0841 0.3396 0.091 Uiso 1 1 calc R . . C135 C 0.0062(3) -0.0985(4) 0.4086(3) 0.0783(12) Uani 1 1 d . . . H135 H -0.0156 -0.1306 0.4630 0.094 Uiso 1 1 calc R . . C136 C 0.1052(3) -0.0784(3) 0.4038(3) 0.0631(10) Uani 1 1 d . . . H136 H 0.1487 -0.0954 0.4554 0.076 Uiso 1 1 calc R . . As2 As 0.15437(2) 0.31921(2) 0.34036(2) 0.04339(9) Uani 1 1 d . . . C211 C 0.1464(2) 0.4585(2) 0.2940(2) 0.0481(8) Uani 1 1 d . . . C212 C 0.1499(3) 0.4808(3) 0.1979(3) 0.0675(10) Uani 1 1 d . . . H212 H 0.1619 0.4296 0.1578 0.081 Uiso 1 1 calc R . . C213 C 0.1357(4) 0.5786(4) 0.1615(4) 0.0918(15) Uani 1 1 d . . . H213 H 0.1382 0.5931 0.0967 0.110 Uiso 1 1 calc R . . C214 C 0.1186(3) 0.6522(4) 0.2175(4) 0.0861(15) Uani 1 1 d . . . H214 H 0.1069 0.7178 0.1914 0.103 Uiso 1 1 calc R . . C215 C 0.1176(3) 0.6335(3) 0.3147(4) 0.0815(14) Uani 1 1 d . . . H215 H 0.1079 0.6856 0.3537 0.098 Uiso 1 1 calc R . . C216 C 0.1313(3) 0.5356(3) 0.3520(3) 0.0614(9) Uani 1 1 d . . . H216 H 0.1303 0.5216 0.4169 0.074 Uiso 1 1 calc R . . C221 C 0.2022(2) 0.3191(2) 0.4688(2) 0.0466(7) Uani 1 1 d . . . C222 C 0.3053(3) 0.3188(3) 0.4824(3) 0.0633(10) Uani 1 1 d . . . H222 H 0.3489 0.3207 0.4308 0.076 Uiso 1 1 calc R . . C223 C 0.3436(3) 0.3159(3) 0.5716(3) 0.0763(12) Uani 1 1 d . . . H223 H 0.4131 0.3144 0.5803 0.092 Uiso 1 1 calc R . . C224 C 0.2781(3) 0.3150(3) 0.6486(3) 0.0747(11) Uani 1 1 d . . . H224 H 0.3035 0.3142 0.7090 0.090 Uiso 1 1 calc R . . C225 C 0.1762(3) 0.3155(3) 0.6356(3) 0.0702(11) Uani 1 1 d . . . H225 H 0.1328 0.3145 0.6875 0.084 Uiso 1 1 calc R . . C226 C 0.1371(3) 0.3175(3) 0.5464(2) 0.0567(9) Uani 1 1 d . . . H226 H 0.0677 0.3178 0.5382 0.068 Uiso 1 1 calc R . . C231 C 0.0091(2) 0.3168(2) 0.3584(2) 0.0441(7) Uani 1 1 d . . . C232 C -0.0230(3) 0.2273(3) 0.3492(3) 0.0636(10) Uani 1 1 d . . . H232 H 0.0249 0.1712 0.3351 0.076 Uiso 1 1 calc R . . C233 C -0.1244(3) 0.2211(3) 0.3607(3) 0.0793(13) Uani 1 1 d . . . H233 H -0.1444 0.1603 0.3561 0.095 Uiso 1 1 calc R . . C234 C -0.1960(3) 0.3028(3) 0.3789(3) 0.0727(11) Uani 1 1 d . . . H234 H -0.2649 0.2985 0.3850 0.087 Uiso 1 1 calc R . . C235 C -0.1660(2) 0.3917(3) 0.3880(3) 0.0695(11) Uani 1 1 d . . . H235 H -0.2150 0.4475 0.4007 0.083 Uiso 1 1 calc R . . C236 C -0.0640(2) 0.3995(3) 0.3786(3) 0.0602(9) Uani 1 1 d . . . H236 H -0.0444 0.4600 0.3858 0.072 Uiso 1 1 calc R . . As3 As 0.19138(2) 0.20740(2) 0.06064(2) 0.04489(9) Uani 1 1 d . . . C311 C 0.2057(3) 0.3275(3) -0.0163(2) 0.0535(8) Uani 1 1 d . . . C312 C 0.2951(3) 0.3631(3) -0.0078(3) 0.0671(10) Uani 1 1 d . . . H312 H 0.3433 0.3328 0.0374 0.080 Uiso 1 1 calc R . . C313 C 0.3134(4) 0.4428(3) -0.0656(4) 0.0910(16) Uani 1 1 d . . . H313 H 0.3733 0.4671 -0.0588 0.109 Uiso 1 1 calc R . . C314 C 0.2432(5) 0.4870(4) -0.1338(4) 0.107(2) Uani 1 1 d . . . H314 H 0.2569 0.5395 -0.1743 0.129 Uiso 1 1 calc R . . C315 C 0.1541(5) 0.4538(4) -0.1420(4) 0.1020(16) Uani 1 1 d . . . H315 H 0.1062 0.4841 -0.1874 0.122 Uiso 1 1 calc R . . C316 C 0.1351(3) 0.3750(3) -0.0825(3) 0.0788(12) Uani 1 1 d . . . H316 H 0.0733 0.3536 -0.0872 0.095 Uiso 1 1 calc R . . C321 C 0.2585(2) 0.1081(2) -0.0219(2) 0.0470(7) Uani 1 1 d . . . C322 C 0.3263(3) 0.0273(3) 0.0158(3) 0.0689(11) Uani 1 1 d . . . H322 H 0.3396 0.0214 0.0800 0.083 Uiso 1 1 calc R . . C323 C 0.3754(3) -0.0455(3) -0.0390(3) 0.0845(14) Uani 1 1 d . . . H323 H 0.4228 -0.0994 -0.0127 0.101 Uiso 1 1 calc R . . C324 C 0.3533(3) -0.0376(3) -0.1332(3) 0.0796(13) Uani 1 1 d . . . H324 H 0.3847 -0.0877 -0.1703 0.096 Uiso 1 1 calc R . . C325 C 0.2873(3) 0.0413(4) -0.1727(3) 0.0730(12) Uani 1 1 d . . . H325 H 0.2737 0.0462 -0.2368 0.088 Uiso 1 1 calc R . . C326 C 0.2397(2) 0.1153(3) -0.1175(2) 0.0618(10) Uani 1 1 d . . . H326 H 0.1946 0.1704 -0.1448 0.074 Uiso 1 1 calc R . . C331 C 0.0462(2) 0.2039(3) 0.0472(2) 0.0462(7) Uani 1 1 d . . . C332 C -0.0223(3) 0.2636(3) 0.1008(3) 0.0781(12) Uani 1 1 d . . . H332 H 0.0008 0.3062 0.1391 0.094 Uiso 1 1 calc R . . C333 C -0.1264(3) 0.2608(4) 0.0982(4) 0.0965(17) Uani 1 1 d . . . H333 H -0.1723 0.3032 0.1339 0.116 Uiso 1 1 calc R . . C334 C -0.1623(3) 0.1981(3) 0.0452(3) 0.0708(11) Uani 1 1 d . . . H334 H -0.2321 0.1967 0.0441 0.085 Uiso 1 1 calc R . . C335 C -0.0945(3) 0.1377(4) -0.0061(3) 0.0828(13) Uani 1 1 d . . . H335 H -0.1180 0.0937 -0.0426 0.099 Uiso 1 1 calc R . . C336 C 0.0097(3) 0.1395(3) -0.0056(3) 0.0712(11) Uani 1 1 d . . . H336 H 0.0550 0.0967 -0.0413 0.085 Uiso 1 1 calc R . . N1 N 0.4392(5) 0.5661(6) 0.5362(5) 0.101(6) Uiso 0.50 1 d PG A -1 C2 C 0.4758(5) 0.5170(6) 0.4628(5) 0.139(5) Uiso 0.50 1 d PG A -1 C3 C 0.5574(5) 0.4440(6) 0.4724(5) 0.117(9) Uiso 0.50 1 d PG A -1 H3 H 0.5831 0.4095 0.4209 0.140 Uiso 0.50 1 calc PR A -1 C4 C 0.6025(5) 0.4201(6) 0.5554(6) 0.097(3) Uiso 0.50 1 d PG A -1 H4 H 0.6598 0.3688 0.5621 0.116 Uiso 0.50 1 calc PR A -1 C5 C 0.5659(5) 0.4692(6) 0.6288(5) 0.20(2) Uiso 0.50 1 d PG A -1 H5 H 0.5975 0.4524 0.6870 0.234 Uiso 0.50 1 calc PR A -1 C6 C 0.4842(5) 0.5422(6) 0.6192(5) 0.107(3) Uiso 0.50 1 d PG A -1 H6 H 0.4586 0.5767 0.6707 0.129 Uiso 0.50 1 calc PR A -1 C7 C 0.4268(8) 0.5391(9) 0.3689(6) 0.144(15) Uiso 0.50 1 d PG A -1 H7A H 0.3689 0.5932 0.3714 0.216 Uiso 0.50 1 calc PR A -1 H7B H 0.4042 0.4810 0.3508 0.216 Uiso 0.50 1 calc PR A -1 H7C H 0.4757 0.5575 0.3236 0.216 Uiso 0.50 1 calc PR A -1 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 Ag 0.04908(13) 0.04493(14) 0.04412(14) -0.00593(11) -0.00044(10) -0.01292(10) N 0.0480(16) 0.087(3) 0.107(3) 0.013(2) -0.0018(17) -0.0248(17) C 0.055(2) 0.069(3) 0.104(3) 0.000(3) -0.008(2) -0.0103(19) S 0.1159(12) 0.1266(16) 0.318(3) -0.0159(18) 0.0689(16) -0.0715(12) As1 0.05109(17) 0.03775(17) 0.04469(18) -0.00056(14) -0.00631(14) -0.01318(13) C111 0.0473(15) 0.0408(17) 0.0479(18) -0.0005(15) -0.0041(13) -0.0122(13) C112 0.069(2) 0.049(2) 0.055(2) -0.0122(18) -0.0020(17) -0.0088(16) C113 0.092(3) 0.066(3) 0.050(2) -0.014(2) -0.009(2) -0.010(2) C114 0.074(2) 0.085(3) 0.044(2) -0.001(2) -0.0091(17) -0.009(2) C115 0.071(2) 0.053(2) 0.062(2) 0.012(2) -0.0113(18) -0.0083(17) C116 0.0651(19) 0.049(2) 0.053(2) -0.0022(17) -0.0112(16) -0.0139(16) C121 0.0496(16) 0.0422(18) 0.0453(17) -0.0015(15) -0.0061(13) -0.0103(13) C122 0.0512(18) 0.074(3) 0.063(2) -0.006(2) -0.0034(16) -0.0190(17) C123 0.0498(19) 0.094(3) 0.083(3) -0.009(3) 0.008(2) -0.007(2) C124 0.074(3) 0.078(3) 0.103(4) -0.031(3) 0.021(3) -0.001(2) C125 0.082(3) 0.074(3) 0.138(5) -0.050(3) 0.022(3) -0.024(2) C126 0.0549(19) 0.063(2) 0.107(3) -0.034(3) 0.018(2) -0.0176(17) C131 0.0480(16) 0.0371(17) 0.0533(19) -0.0071(15) -0.0020(14) -0.0100(13) C132 0.065(2) 0.058(2) 0.051(2) -0.0096(18) -0.0043(16) -0.0212(16) C133 0.064(2) 0.076(3) 0.073(3) -0.013(2) -0.0156(19) -0.0191(19) C134 0.053(2) 0.093(3) 0.088(3) -0.014(3) 0.005(2) -0.028(2) C135 0.068(2) 0.097(4) 0.075(3) 0.006(3) 0.005(2) -0.034(2) C136 0.0571(19) 0.071(3) 0.061(2) 0.005(2) -0.0060(17) -0.0171(18) As2 0.04614(16) 0.04075(18) 0.04304(18) -0.00944(15) 0.00342(13) -0.00568(13) C211 0.0417(15) 0.050(2) 0.0544(19) -0.0093(17) 0.0040(14) -0.0126(13) C212 0.079(2) 0.070(3) 0.056(2) 0.003(2) -0.0109(19) -0.023(2) C213 0.118(4) 0.085(4) 0.079(3) 0.028(3) -0.025(3) -0.047(3) C214 0.074(3) 0.059(3) 0.125(4) 0.032(3) -0.026(3) -0.026(2) C215 0.073(2) 0.042(2) 0.132(4) -0.014(3) 0.007(3) -0.0144(18) C216 0.068(2) 0.049(2) 0.069(2) -0.010(2) 0.0092(18) -0.0139(17) C221 0.0517(16) 0.0361(17) 0.0524(19) -0.0086(15) -0.0048(14) -0.0067(13) C222 0.0545(19) 0.071(3) 0.067(2) -0.014(2) -0.0023(17) -0.0134(17) C223 0.061(2) 0.082(3) 0.087(3) -0.008(3) -0.024(2) -0.016(2) C224 0.095(3) 0.067(3) 0.062(2) -0.011(2) -0.033(2) -0.009(2) C225 0.081(2) 0.083(3) 0.045(2) -0.006(2) -0.0050(18) -0.011(2) C226 0.0556(18) 0.064(2) 0.051(2) -0.0073(19) 0.0013(15) -0.0109(16) C231 0.0457(15) 0.0467(18) 0.0392(16) -0.0067(15) -0.0014(13) -0.0059(13) C232 0.063(2) 0.048(2) 0.082(3) -0.017(2) 0.0049(19) -0.0123(16) C233 0.072(2) 0.066(3) 0.109(4) -0.020(3) 0.011(2) -0.030(2) C234 0.0509(19) 0.081(3) 0.088(3) -0.003(3) 0.0020(19) -0.0180(19) C235 0.0480(18) 0.062(3) 0.094(3) -0.004(2) 0.0061(19) -0.0019(17) C236 0.0551(18) 0.045(2) 0.081(3) -0.010(2) 0.0055(18) -0.0092(15) As3 0.05368(18) 0.0469(2) 0.03550(16) -0.00453(15) -0.00411(13) -0.01242(14) C311 0.0656(19) 0.047(2) 0.0485(19) -0.0084(17) 0.0041(16) -0.0109(15) C312 0.068(2) 0.054(2) 0.082(3) -0.005(2) 0.010(2) -0.0174(18) C313 0.085(3) 0.054(3) 0.136(5) -0.009(3) 0.035(3) -0.021(2) C314 0.146(5) 0.053(3) 0.118(5) 0.009(3) 0.051(4) -0.020(3) C315 0.138(4) 0.065(3) 0.091(4) 0.028(3) -0.013(3) -0.005(3) C316 0.101(3) 0.070(3) 0.065(3) 0.017(2) -0.020(2) -0.025(2) C321 0.0530(16) 0.0491(19) 0.0413(17) -0.0071(15) -0.0001(14) -0.0146(14) C322 0.085(2) 0.064(3) 0.048(2) 0.003(2) 0.0059(19) 0.004(2) C323 0.109(3) 0.058(3) 0.073(3) 0.004(2) 0.017(2) 0.010(2) C324 0.085(3) 0.075(3) 0.086(3) -0.035(3) 0.031(3) -0.021(2) C325 0.059(2) 0.108(4) 0.057(2) -0.037(3) 0.0056(18) -0.017(2) C326 0.0525(18) 0.086(3) 0.0459(19) -0.014(2) -0.0061(15) -0.0069(17) C331 0.0507(16) 0.0477(18) 0.0394(16) 0.0018(15) -0.0040(13) -0.0091(13) C332 0.066(2) 0.076(3) 0.097(3) -0.042(3) 0.003(2) -0.0106(19) C333 0.062(2) 0.101(4) 0.127(4) -0.043(4) 0.022(3) -0.006(2) C334 0.055(2) 0.074(3) 0.083(3) 0.001(2) 0.001(2) -0.0146(19) C335 0.069(2) 0.094(4) 0.097(3) -0.029(3) -0.004(2) -0.035(2) C336 0.063(2) 0.083(3) 0.075(3) -0.032(2) 0.0081(19) -0.0220(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N 2.256(3) . ? Ag As1 2.6231(4) . ? Ag As3 2.6425(4) . ? Ag As2 2.6500(4) . ? N C 1.086(5) . ? C S 1.635(5) . ? As1 C111 1.940(3) . ? As1 C121 1.945(3) . ? As1 C131 1.948(3) . ? C111 C116 1.382(5) . ? C111 C112 1.394(5) . ? C112 C113 1.393(5) . ? C112 H112 0.9300 . ? C113 C114 1.360(6) . ? C113 H113 0.9300 . ? C114 C115 1.379(5) . ? C114 H114 0.9300 . ? C115 C116 1.365(5) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C121 C126 1.369(5) . ? C121 C122 1.374(4) . ? C122 C123 1.394(5) . ? C122 H122 0.9300 . ? C123 C124 1.367(6) . ? C123 H123 0.9300 . ? C124 C125 1.363(5) . ? C124 H124 0.9300 . ? C125 C126 1.387(5) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C136 1.382(5) . ? C131 C132 1.388(5) . ? C132 C133 1.379(5) . ? C132 H132 0.9300 . ? C133 C134 1.367(6) . ? C133 H133 0.9300 . ? C134 C135 1.350(6) . ? C134 H134 0.9300 . ? C135 C136 1.394(5) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? As2 C231 1.947(3) . ? As2 C211 1.952(3) . ? As2 C221 1.952(3) . ? C211 C216 1.378(4) . ? C211 C212 1.382(5) . ? C212 C213 1.377(6) . ? C212 H212 0.9300 . ? C213 C214 1.321(7) . ? C213 H213 0.9300 . ? C214 C215 1.390(7) . ? C214 H214 0.9300 . ? C215 C216 1.381(5) . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? C221 C222 1.385(4) . ? C221 C226 1.392(4) . ? C222 C223 1.374(5) . ? C222 H222 0.9300 . ? C223 C224 1.389(5) . ? C223 H223 0.9300 . ? C224 C225 1.367(5) . ? C224 H224 0.9300 . ? C225 C226 1.381(5) . ? C225 H225 0.9300 . ? C226 H226 0.9300 . ? C231 C236 1.387(4) . ? C231 C232 1.391(5) . ? C232 C233 1.371(5) . ? C232 H232 0.9300 . ? C233 C234 1.360(5) . ? C233 H233 0.9300 . ? C234 C235 1.370(6) . ? C234 H234 0.9300 . ? C235 C236 1.382(4) . ? C235 H235 0.9300 . ? C236 H236 0.9300 . ? As3 C311 1.942(4) . ? As3 C321 1.945(3) . ? As3 C331 1.951(3) . ? C311 C316 1.374(5) . ? C311 C312 1.380(5) . ? C312 C313 1.371(6) . ? C312 H312 0.9300 . ? C313 C314 1.378(7) . ? C313 H313 0.9300 . ? C314 C315 1.359(7) . ? C314 H314 0.9300 . ? C315 C316 1.377(6) . ? C315 H315 0.9300 . ? C316 H316 0.9300 . ? C321 C322 1.363(5) . ? C321 C326 1.383(4) . ? C322 C323 1.375(5) . ? C322 H322 0.9300 . ? C323 C324 1.373(6) . ? C323 H323 0.9300 . ? C324 C325 1.344(6) . ? C324 H324 0.9300 . ? C325 C326 1.382(5) . ? C325 H325 0.9300 . ? C326 H326 0.9300 . ? C331 C332 1.367(5) . ? C331 C336 1.367(5) . ? C332 C333 1.391(5) . ? C332 H332 0.9300 . ? C333 C334 1.349(6) . ? C333 H333 0.9300 . ? C334 C335 1.347(5) . ? C334 H334 0.9300 . ? C335 C336 1.389(5) . ? C335 H335 0.9300 . ? C336 H336 0.9300 . ? N1 C2 1.324(3) . ? N1 C6 1.324(3) . ? C2 C3 1.325(3) . ? C2 C7 1.484(3) . ? C3 C4 1.325(3) . ? C3 H3 0.9300 . ? C4 C5 1.324(3) . ? C4 H4 0.9300 . ? C5 C6 1.324(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 N Ag As1 113.41(10) . . ? N Ag As3 105.75(10) . . ? As1 Ag As3 111.237(13) . . ? N Ag As2 101.60(10) . . ? As1 Ag As2 112.671(13) . . ? As3 Ag As2 111.631(14) . . ? C N Ag 159.1(4) . . ? N C S 176.4(5) . . ? C111 As1 C121 99.86(13) . . ? C111 As1 C131 102.88(13) . . ? C121 As1 C131 101.08(12) . . ? C111 As1 Ag 117.82(9) . . ? C121 As1 Ag 120.76(10) . . ? C131 As1 Ag 111.74(10) . . ? C116 C111 C112 119.5(3) . . ? C116 C111 As1 123.3(2) . . ? C112 C111 As1 117.1(3) . . ? C113 C112 C111 119.3(4) . . ? C113 C112 H112 120.3 . . ? C111 C112 H112 120.3 . . ? C114 C113 C112 120.1(4) . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C113 C114 C115 120.5(4) . . ? C113 C114 H114 119.7 . . ? C115 C114 H114 119.7 . . ? C116 C115 C114 120.2(4) . . ? C116 C115 H115 119.9 . . ? C114 C115 H115 119.9 . . ? C115 C116 C111 120.3(3) . . ? C115 C116 H116 119.8 . . ? C111 C116 H116 119.8 . . ? C126 C121 C122 118.6(3) . . ? C126 C121 As1 123.0(2) . . ? C122 C121 As1 118.4(2) . . ? C121 C122 C123 120.5(4) . . ? C121 C122 H122 119.7 . . ? C123 C122 H122 119.7 . . ? C124 C123 C122 119.8(3) . . ? C124 C123 H123 120.1 . . ? C122 C123 H123 120.1 . . ? C125 C124 C123 120.1(4) . . ? C125 C124 H124 120.0 . . ? C123 C124 H124 120.0 . . ? C124 C125 C126 119.8(4) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? C121 C126 C125 121.1(3) . . ? C121 C126 H126 119.4 . . ? C125 C126 H126 119.4 . . ? C136 C131 C132 119.0(3) . . ? C136 C131 As1 123.3(3) . . ? C132 C131 As1 117.6(2) . . ? C133 C132 C131 120.3(3) . . ? C133 C132 H132 119.9 . . ? C131 C132 H132 119.9 . . ? C134 C133 C132 120.1(4) . . ? C134 C133 H133 120.0 . . ? C132 C133 H133 120.0 . . ? C135 C134 C133 120.4(3) . . ? C135 C134 H134 119.8 . . ? C133 C134 H134 119.8 . . ? C134 C135 C136 120.7(4) . . ? C134 C135 H135 119.7 . . ? C136 C135 H135 119.7 . . ? C131 C136 C135 119.5(4) . . ? C131 C136 H136 120.2 . . ? C135 C136 H136 120.2 . . ? C231 As2 C211 100.34(13) . . ? C231 As2 C221 102.58(12) . . ? C211 As2 C221 101.66(13) . . ? C231 As2 Ag 117.28(9) . . ? C211 As2 Ag 115.60(9) . . ? C221 As2 Ag 116.81(9) . . ? C216 C211 C212 118.8(4) . . ? C216 C211 As2 123.1(3) . . ? C212 C211 As2 118.0(3) . . ? C213 C212 C211 120.2(4) . . ? C213 C212 H212 119.9 . . ? C211 C212 H212 119.9 . . ? C214 C213 C212 120.6(5) . . ? C214 C213 H213 119.7 . . ? C212 C213 H213 119.7 . . ? C213 C214 C215 121.3(5) . . ? C213 C214 H214 119.3 . . ? C215 C214 H214 119.3 . . ? C216 C215 C214 118.4(4) . . ? C216 C215 H215 120.8 . . ? C214 C215 H215 120.8 . . ? C211 C216 C215 120.6(4) . . ? C211 C216 H216 119.7 . . ? C215 C216 H216 119.7 . . ? C222 C221 C226 119.4(3) . . ? C222 C221 As2 118.2(2) . . ? C226 C221 As2 122.4(2) . . ? C223 C222 C221 120.6(3) . . ? C223 C222 H222 119.7 . . ? C221 C222 H222 119.7 . . ? C222 C223 C224 119.7(3) . . ? C222 C223 H223 120.1 . . ? C224 C223 H223 120.1 . . ? C225 C224 C223 120.0(4) . . ? C225 C224 H224 120.0 . . ? C223 C224 H224 120.0 . . ? C224 C225 C226 120.7(4) . . ? C224 C225 H225 119.6 . . ? C226 C225 H225 119.6 . . ? C225 C226 C221 119.6(3) . . ? C225 C226 H226 120.2 . . ? C221 C226 H226 120.2 . . ? C236 C231 C232 118.5(3) . . ? C236 C231 As2 123.5(2) . . ? C232 C231 As2 118.0(2) . . ? C233 C232 C231 120.7(3) . . ? C233 C232 H232 119.7 . . ? C231 C232 H232 119.7 . . ? C234 C233 C232 120.6(4) . . ? C234 C233 H233 119.7 . . ? C232 C233 H233 119.7 . . ? C233 C234 C235 119.5(3) . . ? C233 C234 H234 120.2 . . ? C235 C234 H234 120.2 . . ? C234 C235 C236 121.0(3) . . ? C234 C235 H235 119.5 . . ? C236 C235 H235 119.5 . . ? C235 C236 C231 119.7(3) . . ? C235 C236 H236 120.2 . . ? C231 C236 H236 120.2 . . ? C311 As3 C321 99.18(13) . . ? C311 As3 C331 102.79(14) . . ? C321 As3 C331 102.99(13) . . ? C311 As3 Ag 117.87(11) . . ? C321 As3 Ag 115.49(10) . . ? C331 As3 Ag 116.03(9) . . ? C316 C311 C312 118.5(4) . . ? C316 C311 As3 123.8(3) . . ? C312 C311 As3 117.6(3) . . ? C313 C312 C311 120.3(4) . . ? C313 C312 H312 119.8 . . ? C311 C312 H312 119.8 . . ? C312 C313 C314 120.2(5) . . ? C312 C313 H313 119.9 . . ? C314 C313 H313 119.9 . . ? C315 C314 C313 120.1(5) . . ? C315 C314 H314 120.0 . . ? C313 C314 H314 120.0 . . ? C314 C315 C316 119.5(5) . . ? C314 C315 H315 120.2 . . ? C316 C315 H315 120.2 . . ? C311 C316 C315 121.3(4) . . ? C311 C316 H316 119.3 . . ? C315 C316 H316 119.3 . . ? C322 C321 C326 118.3(3) . . ? C322 C321 As3 118.8(2) . . ? C326 C321 As3 122.9(3) . . ? C321 C322 C323 121.3(4) . . ? C321 C322 H322 119.3 . . ? C323 C322 H322 119.3 . . ? C324 C323 C322 119.0(4) . . ? C324 C323 H323 120.5 . . ? C322 C323 H323 120.5 . . ? C325 C324 C323 121.1(4) . . ? C325 C324 H324 119.5 . . ? C323 C324 H324 119.5 . . ? C324 C325 C326 119.6(4) . . ? C324 C325 H325 120.2 . . ? C326 C325 H325 120.2 . . ? C325 C326 C321 120.7(4) . . ? C325 C326 H326 119.7 . . ? C321 C326 H326 119.7 . . ? C332 C331 C336 118.0(3) . . ? C332 C331 As3 117.3(3) . . ? C336 C331 As3 124.4(2) . . ? C331 C332 C333 120.3(4) . . ? C331 C332 H332 119.8 . . ? C333 C332 H332 119.8 . . ? C334 C333 C332 121.5(4) . . ? C334 C333 H333 119.3 . . ? C332 C333 H333 119.3 . . ? C335 C334 C333 118.2(4) . . ? C335 C334 H334 120.9 . . ? C333 C334 H334 120.9 . . ? C334 C335 C336 121.5(4) . . ? C334 C335 H335 119.2 . . ? C336 C335 H335 119.2 . . ? C331 C336 C335 120.4(3) . . ? C331 C336 H336 119.8 . . ? C335 C336 H336 119.8 . . ? C2 N1 C6 120.0 . . ? N1 C2 C3 120.0 . . ? N1 C2 C7 122.2 . . ? C3 C2 C7 117.8 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? N1 C6 C5 120.0 . . ? N1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 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 As1 Ag N C 151.8(11) . . . . ? As3 Ag N C 29.7(11) . . . . ? As2 Ag N C -87.0(11) . . . . ? Ag N C S -97(7) . . . . ? N Ag As1 C111 57.28(14) . . . . ? As3 Ag As1 C111 176.33(9) . . . . ? As2 Ag As1 C111 -57.45(10) . . . . ? N Ag As1 C121 -65.35(15) . . . . ? As3 Ag As1 C121 53.69(11) . . . . ? As2 Ag As1 C121 179.92(10) . . . . ? N Ag As1 C131 176.09(14) . . . . ? As3 Ag As1 C131 -64.87(10) . . . . ? As2 Ag As1 C131 61.35(10) . . . . ? C121 As1 C111 C116 -27.7(3) . . . . ? C131 As1 C111 C116 76.2(3) . . . . ? Ag As1 C111 C116 -160.4(2) . . . . ? C121 As1 C111 C112 149.9(2) . . . . ? C131 As1 C111 C112 -106.2(2) . . . . ? Ag As1 C111 C112 17.1(3) . . . . ? C116 C111 C112 C113 0.1(5) . . . . ? As1 C111 C112 C113 -177.6(3) . . . . ? C111 C112 C113 C114 0.2(5) . . . . ? C112 C113 C114 C115 -1.0(6) . . . . ? C113 C114 C115 C116 1.5(6) . . . . ? C114 C115 C116 C111 -1.1(5) . . . . ? C112 C111 C116 C115 0.4(5) . . . . ? As1 C111 C116 C115 177.9(2) . . . . ? C111 As1 C121 C126 106.9(4) . . . . ? C131 As1 C121 C126 1.6(4) . . . . ? Ag As1 C121 C126 -122.2(3) . . . . ? C111 As1 C121 C122 -75.5(3) . . . . ? C131 As1 C121 C122 179.1(3) . . . . ? Ag As1 C121 C122 55.4(3) . . . . ? C126 C121 C122 C123 -1.6(6) . . . . ? As1 C121 C122 C123 -179.2(3) . . . . ? C121 C122 C123 C124 2.0(7) . . . . ? C122 C123 C124 C125 -1.2(8) . . . . ? C123 C124 C125 C126 0.0(8) . . . . ? C122 C121 C126 C125 0.3(7) . . . . ? As1 C121 C126 C125 177.9(4) . . . . ? C124 C125 C126 C121 0.5(8) . . . . ? C111 As1 C131 C136 -4.5(3) . . . . ? C121 As1 C131 C136 98.4(3) . . . . ? Ag As1 C131 C136 -131.8(3) . . . . ? C111 As1 C131 C132 172.4(3) . . . . ? C121 As1 C131 C132 -84.7(3) . . . . ? Ag As1 C131 C132 45.0(3) . . . . ? C136 C131 C132 C133 -1.2(5) . . . . ? As1 C131 C132 C133 -178.2(3) . . . . ? C131 C132 C133 C134 1.1(6) . . . . ? C132 C133 C134 C135 -1.3(7) . . . . ? C133 C134 C135 C136 1.6(7) . . . . ? C132 C131 C136 C135 1.5(5) . . . . ? As1 C131 C136 C135 178.3(3) . . . . ? C134 C135 C136 C131 -1.7(7) . . . . ? N Ag As2 C231 173.97(14) . . . . ? As1 Ag As2 C231 -64.34(11) . . . . ? As3 Ag As2 C231 61.67(11) . . . . ? N Ag As2 C211 55.86(14) . . . . ? As1 Ag As2 C211 177.55(10) . . . . ? As3 Ag As2 C211 -56.43(10) . . . . ? N Ag As2 C221 -63.69(14) . . . . ? As1 Ag As2 C221 58.00(10) . . . . ? As3 Ag As2 C221 -175.99(10) . . . . ? C231 As2 C211 C216 79.1(3) . . . . ? C221 As2 C211 C216 -26.2(3) . . . . ? Ag As2 C211 C216 -153.7(2) . . . . ? C231 As2 C211 C212 -96.9(3) . . . . ? C221 As2 C211 C212 157.8(3) . . . . ? Ag As2 C211 C212 30.3(3) . . . . ? C216 C211 C212 C213 -1.8(5) . . . . ? As2 C211 C212 C213 174.4(3) . . . . ? C211 C212 C213 C214 0.0(7) . . . . ? C212 C213 C214 C215 2.1(7) . . . . ? C213 C214 C215 C216 -2.3(7) . . . . ? C212 C211 C216 C215 1.5(5) . . . . ? As2 C211 C216 C215 -174.5(3) . . . . ? C214 C215 C216 C211 0.5(6) . . . . ? C231 As2 C221 C222 178.9(3) . . . . ? C211 As2 C221 C222 -77.6(3) . . . . ? Ag As2 C221 C222 49.2(3) . . . . ? C231 As2 C221 C226 0.0(3) . . . . ? C211 As2 C221 C226 103.5(3) . . . . ? Ag As2 C221 C226 -129.7(3) . . . . ? C226 C221 C222 C223 0.8(6) . . . . ? As2 C221 C222 C223 -178.1(3) . . . . ? C221 C222 C223 C224 -1.3(6) . . . . ? C222 C223 C224 C225 1.1(7) . . . . ? C223 C224 C225 C226 -0.5(7) . . . . ? C224 C225 C226 C221 0.0(6) . . . . ? C222 C221 C226 C225 -0.2(5) . . . . ? As2 C221 C226 C225 178.7(3) . . . . ? C211 As2 C231 C236 -28.1(3) . . . . ? C221 As2 C231 C236 76.4(3) . . . . ? Ag As2 C231 C236 -154.2(3) . . . . ? C211 As2 C231 C232 150.9(3) . . . . ? C221 As2 C231 C232 -104.5(3) . . . . ? Ag As2 C231 C232 24.9(3) . . . . ? C236 C231 C232 C233 -0.6(6) . . . . ? As2 C231 C232 C233 -179.7(3) . . . . ? C231 C232 C233 C234 1.8(7) . . . . ? C232 C233 C234 C235 -1.6(7) . . . . ? C233 C234 C235 C236 0.3(7) . . . . ? C234 C235 C236 C231 0.9(7) . . . . ? C232 C231 C236 C235 -0.7(6) . . . . ? As2 C231 C236 C235 178.4(3) . . . . ? N Ag As3 C311 -42.80(14) . . . . ? As1 Ag As3 C311 -166.34(10) . . . . ? As2 Ag As3 C311 66.87(11) . . . . ? N Ag As3 C321 74.07(14) . . . . ? As1 Ag As3 C321 -49.46(10) . . . . ? As2 Ag As3 C321 -176.26(10) . . . . ? N Ag As3 C331 -165.27(15) . . . . ? As1 Ag As3 C331 71.19(11) . . . . ? As2 Ag As3 C331 -55.60(11) . . . . ? C321 As3 C311 C316 89.0(3) . . . . ? C331 As3 C311 C316 -16.7(4) . . . . ? Ag As3 C311 C316 -145.7(3) . . . . ? C321 As3 C311 C312 -86.8(3) . . . . ? C331 As3 C311 C312 167.6(3) . . . . ? Ag As3 C311 C312 38.6(3) . . . . ? C316 C311 C312 C313 -1.3(6) . . . . ? As3 C311 C312 C313 174.7(3) . . . . ? C311 C312 C313 C314 -1.1(6) . . . . ? C312 C313 C314 C315 2.2(8) . . . . ? C313 C314 C315 C316 -0.9(8) . . . . ? C312 C311 C316 C315 2.6(6) . . . . ? As3 C311 C316 C315 -173.1(3) . . . . ? C314 C315 C316 C311 -1.6(8) . . . . ? C311 As3 C321 C322 135.7(3) . . . . ? C331 As3 C321 C322 -118.8(3) . . . . ? Ag As3 C321 C322 8.7(3) . . . . ? C311 As3 C321 C326 -45.1(3) . . . . ? C331 As3 C321 C326 60.4(3) . . . . ? Ag As3 C321 C326 -172.1(2) . . . . ? C326 C321 C322 C323 0.2(6) . . . . ? As3 C321 C322 C323 179.5(3) . . . . ? C321 C322 C323 C324 -1.7(7) . . . . ? C322 C323 C324 C325 2.0(7) . . . . ? C323 C324 C325 C326 -0.8(7) . . . . ? C324 C325 C326 C321 -0.8(6) . . . . ? C322 C321 C326 C325 1.1(5) . . . . ? As3 C321 C326 C325 -178.2(3) . . . . ? C311 As3 C331 C332 -80.1(3) . . . . ? C321 As3 C331 C332 177.2(3) . . . . ? Ag As3 C331 C332 50.0(3) . . . . ? C311 As3 C331 C336 106.0(3) . . . . ? C321 As3 C331 C336 3.3(4) . . . . ? Ag As3 C331 C336 -123.9(3) . . . . ? C336 C331 C332 C333 -2.4(6) . . . . ? As3 C331 C332 C333 -176.7(4) . . . . ? C331 C332 C333 C334 1.7(8) . . . . ? C332 C333 C334 C335 -0.2(8) . . . . ? C333 C334 C335 C336 -0.4(7) . . . . ? C332 C331 C336 C335 1.8(6) . . . . ? As3 C331 C336 C335 175.6(3) . . . . ? C334 C335 C336 C331 -0.4(7) . . . . ? C6 N1 C2 C3 0.0 . . . . ? C6 N1 C2 C7 178.5 . . . . ? N1 C2 C3 C4 0.0 . . . . ? C7 C2 C3 C4 -178.6 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C2 N1 C6 C5 0.0 . . . . ? C4 C5 C6 N1 0.0 . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C234 H234 N1 0.93 2.94 3.613(7) 130.7 2_566 _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.706 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.096 data_cmpnd04 _database_code_depnum_ccdc_archive 'CCDC 869211' #TrackingRef 'UWA120227.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H42 Ag2 N2 P2 S2' _chemical_formula_sum 'C44 H42 Ag2 N2 P2 S2' _chemical_formula_weight 940.60 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' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.370(11) _cell_length_b 11.025(8) _cell_length_c 10.300(11) _cell_angle_alpha 111.52(8) _cell_angle_beta 98.98(8) _cell_angle_gamma 115.77(7) _cell_volume 1002.0(16) _cell_formula_units_Z 1 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 14 _cell_measurement_theta_max 16 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'XTAL: ABSCOR' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3388 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3388 _reflns_number_gt 2818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 control software' _computing_cell_refinement 'Enraf-Nonius CAD4 control software' _computing_data_reduction 'XTAL: ABSCOR, ADDREF, SORTRF' _computing_structure_solution 'Bruker SHELXTL, v. 5.1' _computing_structure_refinement 'Bruker SHELXTL, v. 5.1' _computing_molecular_graphics XTAL _computing_publication_material 'Bruker SHELXTL, v. 5.1' _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^)+(0.0300P)^2^+0.7000P] 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 3388 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.06495(3) 0.39904(3) 0.74956(3) 0.04870(11) Uani 1 1 d . . . S S -0.16719(11) 0.21634(12) 0.73131(12) 0.0683(3) Uani 1 1 d . . . C C -0.1610(3) 0.3214(4) 0.8983(4) 0.0452(8) Uani 1 1 d . . . N N -0.1602(3) 0.3901(4) 1.0137(4) 0.0601(8) Uani 1 1 d . . . P P 0.23273(8) 0.41783(9) 0.62709(9) 0.03356(18) Uani 1 1 d . . . C11 C 0.1674(3) 0.3483(3) 0.4243(3) 0.0348(7) Uani 1 1 d . . . C12 C 0.0565(3) 0.1958(4) 0.3251(4) 0.0443(8) Uani 1 1 d . . . C121 C -0.0074(4) 0.0804(4) 0.3778(5) 0.0640(11) Uani 1 1 d . . . H12A H -0.0817 -0.0171 0.2933 0.096 Uiso 1 1 calc R . . H12B H -0.0449 0.1166 0.4498 0.096 Uiso 1 1 calc R . . H12C H 0.0638 0.0681 0.4240 0.096 Uiso 1 1 calc R . . C13 C 0.0053(4) 0.1495(5) 0.1731(4) 0.0573(10) Uani 1 1 d . . . H13 H -0.0675 0.0479 0.1061 0.069 Uiso 1 1 calc R . . C14 C 0.0599(5) 0.2508(6) 0.1188(4) 0.0638(11) Uani 1 1 d . . . H14 H 0.0230 0.2176 0.0165 0.077 Uiso 1 1 calc R . . C15 C 0.1680(5) 0.3995(5) 0.2155(4) 0.0608(10) Uani 1 1 d . . . H15 H 0.2049 0.4680 0.1793 0.073 Uiso 1 1 calc R . . C16 C 0.2227(4) 0.4482(4) 0.3671(4) 0.0450(8) Uani 1 1 d . . . H16 H 0.2976 0.5493 0.4321 0.054 Uiso 1 1 calc R . . C21 C 0.3770(3) 0.6194(3) 0.7115(3) 0.0356(7) Uani 1 1 d . . . C22 C 0.3480(4) 0.7363(4) 0.7337(4) 0.0449(8) Uani 1 1 d . . . C221 C 0.2011(5) 0.7017(5) 0.6762(5) 0.0688(12) Uani 1 1 d . . . H22A H 0.2044 0.7966 0.7030 0.103 Uiso 1 1 calc R . . H22B H 0.1450 0.6481 0.7202 0.103 Uiso 1 1 calc R . . H22C H 0.1599 0.6384 0.5685 0.103 Uiso 1 1 calc R . . C23 C 0.4611(5) 0.8873(4) 0.8089(4) 0.0607(10) Uani 1 1 d . . . H23 H 0.4438 0.9657 0.8258 0.073 Uiso 1 1 calc R . . C24 C 0.5992(5) 0.9264(4) 0.8600(4) 0.0646(11) Uani 1 1 d . . . H24 H 0.6729 1.0294 0.9106 0.078 Uiso 1 1 calc R . . C25 C 0.6265(4) 0.8115(4) 0.8353(4) 0.0543(9) Uani 1 1 d . . . H25 H 0.7189 0.8361 0.8683 0.065 Uiso 1 1 calc R . . C26 C 0.5161(3) 0.6600(4) 0.7616(3) 0.0412(7) Uani 1 1 d . . . H26 H 0.5351 0.5827 0.7449 0.049 Uiso 1 1 calc R . . C31 C 0.3227(3) 0.3186(3) 0.6487(3) 0.0352(7) Uani 1 1 d . . . C32 C 0.3514(3) 0.3054(4) 0.7782(4) 0.0408(7) Uani 1 1 d . . . C321 C 0.3085(4) 0.3671(5) 0.9053(4) 0.0568(9) Uani 1 1 d . . . H32A H 0.2602 0.4139 0.8818 0.085 Uiso 1 1 calc R . . H32B H 0.3908 0.4428 0.9960 0.085 Uiso 1 1 calc R . . H32C H 0.2468 0.2841 0.9194 0.085 Uiso 1 1 calc R . . C33 C 0.4232(4) 0.2321(4) 0.7880(4) 0.0529(9) Uani 1 1 d . . . H33 H 0.4426 0.2222 0.8733 0.063 Uiso 1 1 calc R . . C34 C 0.4664(4) 0.1740(4) 0.6766(4) 0.0554(9) Uani 1 1 d . . . H34 H 0.5151 0.1267 0.6873 0.066 Uiso 1 1 calc R . . C35 C 0.4369(4) 0.1864(4) 0.5481(4) 0.0535(9) Uani 1 1 d . . . H35 H 0.4647 0.1462 0.4713 0.064 Uiso 1 1 calc R . . C36 C 0.3667(4) 0.2581(4) 0.5347(4) 0.0446(8) Uani 1 1 d . . . H36 H 0.3479 0.2669 0.4486 0.054 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 Ag 0.04634(16) 0.06632(19) 0.04834(18) 0.03296(14) 0.03023(13) 0.03329(14) S 0.0537(6) 0.0552(6) 0.0596(6) 0.0093(5) 0.0306(5) 0.0140(5) C 0.0333(17) 0.0428(18) 0.055(2) 0.0243(17) 0.0189(15) 0.0162(15) N 0.0577(19) 0.061(2) 0.056(2) 0.0248(17) 0.0315(16) 0.0275(16) P 0.0340(4) 0.0391(4) 0.0308(4) 0.0185(3) 0.0147(3) 0.0201(3) C11 0.0359(16) 0.0432(17) 0.0290(15) 0.0165(13) 0.0129(13) 0.0246(14) C12 0.0376(17) 0.0487(19) 0.0389(18) 0.0142(15) 0.0108(14) 0.0246(15) C121 0.056(2) 0.043(2) 0.060(2) 0.0170(18) 0.0154(19) 0.0109(18) C13 0.050(2) 0.067(2) 0.039(2) 0.0104(18) 0.0078(16) 0.0347(19) C14 0.078(3) 0.101(3) 0.034(2) 0.030(2) 0.020(2) 0.067(3) C15 0.086(3) 0.086(3) 0.051(2) 0.045(2) 0.039(2) 0.064(3) C16 0.057(2) 0.053(2) 0.0412(19) 0.0286(16) 0.0244(16) 0.0351(17) C21 0.0410(17) 0.0379(16) 0.0270(15) 0.0158(13) 0.0139(13) 0.0201(14) C22 0.064(2) 0.0462(19) 0.0414(19) 0.0240(15) 0.0305(17) 0.0362(18) C221 0.083(3) 0.083(3) 0.088(3) 0.052(3) 0.048(3) 0.067(3) C23 0.095(3) 0.045(2) 0.053(2) 0.0255(18) 0.039(2) 0.041(2) C24 0.075(3) 0.042(2) 0.048(2) 0.0175(17) 0.022(2) 0.012(2) C25 0.044(2) 0.052(2) 0.044(2) 0.0196(17) 0.0129(16) 0.0132(17) C26 0.0433(18) 0.0423(17) 0.0347(17) 0.0180(14) 0.0155(14) 0.0208(15) C31 0.0326(15) 0.0356(16) 0.0344(17) 0.0181(13) 0.0118(13) 0.0155(13) C32 0.0455(18) 0.0411(17) 0.0362(18) 0.0208(14) 0.0159(14) 0.0217(15) C321 0.071(2) 0.077(3) 0.041(2) 0.0336(19) 0.0246(18) 0.048(2) C33 0.060(2) 0.057(2) 0.056(2) 0.0349(19) 0.0204(18) 0.0373(19) C34 0.059(2) 0.057(2) 0.067(2) 0.035(2) 0.0243(19) 0.0388(19) C35 0.059(2) 0.057(2) 0.058(2) 0.0272(18) 0.0311(18) 0.0383(19) C36 0.0508(19) 0.053(2) 0.0390(18) 0.0241(16) 0.0201(15) 0.0325(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N 2.313(5) 2_567 ? Ag P 2.423(2) . ? Ag S 2.450(3) . ? S C 1.654(4) . ? C N 1.147(5) . ? N Ag 2.313(5) 2_567 ? P C11 1.829(4) . ? P C21 1.831(4) . ? P C31 1.836(3) . ? C11 C16 1.395(5) . ? C11 C12 1.398(5) . ? C12 C13 1.386(5) . ? C12 C121 1.506(5) . ? C121 H12A 0.9600 . ? C121 H12B 0.9600 . ? C121 H12C 0.9600 . ? C13 C14 1.382(6) . ? C13 H13 0.9300 . ? C14 C15 1.363(6) . ? C14 H14 0.9300 . ? C15 C16 1.380(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.389(5) . ? C21 C22 1.413(4) . ? C22 C23 1.381(6) . ? C22 C221 1.503(6) . ? C221 H22A 0.9600 . ? C221 H22B 0.9600 . ? C221 H22C 0.9600 . ? C23 C24 1.384(6) . ? C23 H23 0.9300 . ? C24 C25 1.378(6) . ? C24 H24 0.9300 . ? C25 C26 1.375(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C31 C32 1.399(5) . ? C31 C36 1.404(5) . ? C32 C33 1.391(5) . ? C32 C321 1.500(5) . ? C321 H32A 0.9600 . ? C321 H32B 0.9600 . ? C321 H32C 0.9600 . ? C33 C34 1.371(5) . ? C33 H33 0.9300 . ? C34 C35 1.384(5) . ? C34 H34 0.9300 . ? C35 C36 1.369(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? 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 N Ag P 112.84(13) 2_567 . ? N Ag S 104.15(15) 2_567 . ? P Ag S 142.15(8) . . ? C S Ag 98.65(18) . . ? N C S 177.8(3) . . ? C N Ag 155.1(3) . 2_567 ? C11 P C21 105.42(19) . . ? C11 P C31 104.02(15) . . ? C21 P C31 103.71(16) . . ? C11 P Ag 117.42(14) . . ? C21 P Ag 110.13(13) . . ? C31 P Ag 114.87(12) . . ? C16 C11 C12 119.0(3) . . ? C16 C11 P 120.6(3) . . ? C12 C11 P 120.3(3) . . ? C13 C12 C11 118.6(4) . . ? C13 C12 C121 119.2(3) . . ? C11 C12 C121 122.2(3) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C13 C12 121.6(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C13 119.8(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 119.9(4) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 121.1(4) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? C26 C21 C22 119.3(3) . . ? C26 C21 P 120.2(3) . . ? C22 C21 P 120.4(3) . . ? C23 C22 C21 117.6(3) . . ? C23 C22 C221 119.7(3) . . ? C21 C22 C221 122.6(3) . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C22 C23 C24 122.5(4) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C25 C24 C23 119.4(4) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C26 C25 C24 119.5(4) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C21 121.6(3) . . ? C25 C26 H26 119.2 . . ? C21 C26 H26 119.2 . . ? C32 C31 C36 119.2(3) . . ? C32 C31 P 121.3(2) . . ? C36 C31 P 119.5(2) . . ? C33 C32 C31 117.9(3) . . ? C33 C32 C321 119.5(3) . . ? C31 C32 C321 122.6(3) . . ? C32 C321 H32A 109.5 . . ? C32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? C32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? C34 C33 C32 122.6(3) . . ? C34 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C33 C34 C35 119.4(3) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C31 121.3(3) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? 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 N Ag S C 0.51(16) 2_567 . . . ? P Ag S C 168.14(13) . . . . ? Ag S C N -163(9) . . . . ? S C N Ag 163(9) . . . 2_567 ? N Ag P C11 -141.48(17) 2_567 . . . ? S Ag P C11 51.55(17) . . . . ? N Ag P C21 -20.86(15) 2_567 . . . ? S Ag P C21 172.17(11) . . . . ? N Ag P C31 95.76(17) 2_567 . . . ? S Ag P C31 -71.21(16) . . . . ? C21 P C11 C16 -3.8(3) . . . . ? C31 P C11 C16 -112.6(3) . . . . ? Ag P C11 C16 119.2(2) . . . . ? C21 P C11 C12 179.3(2) . . . . ? C31 P C11 C12 70.5(3) . . . . ? Ag P C11 C12 -57.7(3) . . . . ? C16 C11 C12 C13 -0.1(5) . . . . ? P C11 C12 C13 176.8(3) . . . . ? C16 C11 C12 C121 179.1(3) . . . . ? P C11 C12 C121 -3.9(4) . . . . ? C11 C12 C13 C14 -0.9(5) . . . . ? C121 C12 C13 C14 179.8(3) . . . . ? C12 C13 C14 C15 0.9(6) . . . . ? C13 C14 C15 C16 0.1(6) . . . . ? C14 C15 C16 C11 -1.2(5) . . . . ? C12 C11 C16 C15 1.2(5) . . . . ? P C11 C16 C15 -175.8(3) . . . . ? C11 P C21 C26 -104.2(3) . . . . ? C31 P C21 C26 4.8(3) . . . . ? Ag P C21 C26 128.2(2) . . . . ? C11 P C21 C22 79.1(3) . . . . ? C31 P C21 C22 -171.8(2) . . . . ? Ag P C21 C22 -48.4(3) . . . . ? C26 C21 C22 C23 -1.8(5) . . . . ? P C21 C22 C23 174.9(3) . . . . ? C26 C21 C22 C221 176.9(3) . . . . ? P C21 C22 C221 -6.5(4) . . . . ? C21 C22 C23 C24 1.0(5) . . . . ? C221 C22 C23 C24 -177.7(4) . . . . ? C22 C23 C24 C25 0.2(6) . . . . ? C23 C24 C25 C26 -0.6(6) . . . . ? C24 C25 C26 C21 -0.2(5) . . . . ? C22 C21 C26 C25 1.5(5) . . . . ? P C21 C26 C25 -175.2(3) . . . . ? C11 P C31 C32 -161.2(3) . . . . ? C21 P C31 C32 88.7(3) . . . . ? Ag P C31 C32 -31.5(3) . . . . ? C11 P C31 C36 20.4(3) . . . . ? C21 P C31 C36 -89.7(3) . . . . ? Ag P C31 C36 150.1(2) . . . . ? C36 C31 C32 C33 0.1(5) . . . . ? P C31 C32 C33 -178.4(2) . . . . ? C36 C31 C32 C321 179.8(3) . . . . ? P C31 C32 C321 1.4(4) . . . . ? C31 C32 C33 C34 0.2(5) . . . . ? C321 C32 C33 C34 -179.5(4) . . . . ? C32 C33 C34 C35 -0.7(6) . . . . ? C33 C34 C35 C36 0.8(6) . . . . ? C34 C35 C36 C31 -0.5(5) . . . . ? C32 C31 C36 C35 0.1(5) . . . . ? P C31 C36 C35 178.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.421 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.058 data_cmpnd05 _database_code_depnum_ccdc_archive 'CCDC 869212' #TrackingRef 'UWA120227.cif' _audit_creation_method 'XTAL 3.7' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H132 Ag4 N4 P4 S4, 1.5(C2 H3 N)' _chemical_formula_sum 'C79 H136.50 Ag4 N5.50 P4 S4' _chemical_formula_weight 1847.04 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' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.432(5) _cell_length_b 14.422(5) _cell_length_c 11.203(1) _cell_angle_alpha 95.85(3) _cell_angle_beta 107.33(2) _cell_angle_gamma 94.05(3) _cell_volume 2201.8(11) _cell_formula_units_Z 1 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.0 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 961 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'XTAL: ABSCOR' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4942 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1195 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 22.55 _reflns_number_total 4942 _reflns_number_gt 2298 _reflns_threshold_expression >3sigma(F) _computing_data_collection 'Enraf-Nonius CAD4 control software' _computing_cell_refinement 'Enraf-Nonius CAD4 control software' _computing_data_reduction 'XTAL: ABSCOR, ADDREF, SORTRF' _computing_structure_solution 'XTAL: FOURR' _computing_structure_refinement 'XTAL: CRYLSQ' _computing_molecular_graphics 'XTAL: ORTEP' _computing_publication_material 'XTAL: BONDLA, CIFIO' _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(F)+0.04*F^2^]' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 2298 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.113 _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_ref 0.062 _refine_ls_wR_factor_gt 0.050 _refine_ls_goodness_of_fit_ref 1.605 _refine_ls_restrained_S_all 1.284 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 .45266(9) .48866(8) .14211(12) .0853(8) Uani ? ? 1.00000 ? ? Ag2 .66042(9) .17138(8) .12682(12) .0863(8) Uani ? ? 1.00000 ? ? S1 .4249(3) .3774(3) -.0868(4) .075(2) Uani ? ? 1.00000 ? ? C1 .4991(9) .2985(8) -.0362(12) .065(8) Uani ? ? 1.00000 ? ? N1 .5500(8) .2422(7) -.0036(10) .073(7) Uani ? ? 1.00000 ? ? S2 .7022(3) .2824(3) .3318(4) .099(3) Uani ? ? 1.00000 ? ? C2 .6269(10) .3590(9) .2829(11) .075(9) Uani ? ? 1.00000 ? ? N2 .5697(8) .4109(8) .2485(10) .095(8) Uani ? ? 1.00000 ? ? P1 .3142(3) .5442(3) .1912(4) .072(2) Uani ? ? 1.00000 ? ? C111 .2056(9) .5269(9) .0526(12) .073(9) Uani ? ? 1.00000 ? ? C112 .2197(11) .5774(10) -.0542(13) .092(10) Uani ? ? 1.00000 ? ? C113 .1341(11) .5592(12) -.1723(14) .121(12) Uani ? ? 1.00000 ? ? C114 .1058(12) .4561(13) -.2176(14) .130(13) Uani ? ? 1.00000 ? ? C115 .0894(12) .4058(12) -.1116(15) .119(12) Uani ? ? 1.00000 ? ? C116 .1767(11) .4239(10) .0072(13) .094(10) Uani ? ? 1.00000 ? ? C121 .2828(11) .4871(13) .3145(15) .128(13) Uani ? ? 1.00000 ? ? C122 .3478(12) .4494(14) .3998(16) .154(15) Uani ? ? 1.00000 ? ? C123 .3228(12) .3937(11) .4925(14) .116(12) Uani ? ? 1.00000 ? ? C124 .2279(14) .4020(13) .5100(18) .157(16) Uani ? ? 1.00000 ? ? C125 .1622(14) .4390(16) .426(2) .191(18) Uani ? ? 1.00000 ? ? C126 .1848(10) .4969(9) .3310(13) .085(10) Uani ? ? 1.00000 ? ? C131 .3373(10) .6712(10) .2441(13) .089(10) Uani ? ? 1.00000 ? ? C132 .2577(12) .7210(10) .2767(16) .117(12) Uani ? ? 1.00000 ? ? C133 .2813(13) .8283(11) .3032(17) .140(13) Uani ? ? 1.00000 ? ? C134 .3786(15) .8527(12) .4047(17) .150(15) Uani ? ? 1.00000 ? ? C135 .4595(14) .8095(13) .3727(18) .157(15) Uani ? ? 1.00000 ? ? C136 .4332(10) .7010(11) .3451(14) .102(11) Uani ? ? 1.00000 ? ? P2 .7432(3) .0354(3) .1114(4) .076(2) Uani ? ? 1.00000 ? ? C211 .8650(10) .0704(9) .1036(12) .081(9) Uani ? ? 1.00000 ? ? C212 .9299(13) .1166(16) .2156(19) .179(17) Uani ? ? 1.00000 ? ? C213 1.0331(14) .1470(16) .217(2) .199(18) Uani ? ? 1.00000 ? ? C214 1.0292(15) .2118(11) .124(2) .169(15) Uani ? ? 1.00000 ? ? C215 .9739(16) .1600(14) .002(2) .20(2) Uani ? ? 1.00000 ? ? C216 .8658(13) .1282(15) .0015(18) .168(16) Uani ? ? 1.00000 ? ? C221 .6808(11) -.0475(11) -.0255(16) .145(13) Uani ? ? 1.00000 ? ? C222 .6050(13) -.0318(13) -.1089(17) .185(15) Uani ? ? 1.00000 ? ? C223 .5542(12) -.0901(11) -.2254(15) .120(12) Uani ? ? 1.00000 ? ? C224 .6006(16) -.1726(15) -.2621(17) .195(17) Uani ? ? 1.00000 ? ? C225 .6780(17) -.1903(15) -.177(2) .25(2) Uani ? ? 1.00000 ? ? C226 .7348(11) -.1299(10) -.0606(15) .109(11) Uani ? ? 1.00000 ? ? C231 .7574(11) -.0326(10) .2418(15) .106(11) Uani ? ? 1.00000 ? ? C232A .812(2) -.112(2) .253(3) .106(11) Uiso ? ? .50000 ? ? C233A .814(3) -.164(3) .369(3) .146(15) Uiso ? ? .50000 ? ? C234 .7573(18) -.1190(17) .455(2) .230(11) Uiso ? ? 1.00000 ? ? C235A .703(3) -.061(2) .439(3) .135(14) Uiso ? ? .50000 ? ? C236A .692(2) -.018(2) .310(3) .123(13) Uiso ? ? .50000 ? ? C232B .676(2) -.105(2) .240(3) .129(13) Uiso ? ? .50000 ? ? C233B .706(3) -.167(3) .343(4) .161(16) Uiso ? ? .50000 ? ? C235B .833(2) -.033(2) .485(3) .122(12) Uiso ? ? .50000 ? ? C236B .793(2) .0267(19) .376(3) .083(9) Uiso ? ? .50000 ? ? N31 .950(2) .282(2) .528(3) .287(15) Uiso ? ? .75000 ? ? C31 .956(2) .214(2) .598(3) .238(16) Uiso ? ? .75000 ? ? C32 .963(3) .140(3) .651(4) .30(2) Uiso ? ? .75000 ? ? H111 .15488 .55308 .07818 .09860 Uiso ? ? 1.00000 ? ? H112a .27548 .55740 -.07339 .11440 Uiso ? ? 1.00000 ? ? H112e .23024 .64284 -.02650 .11440 Uiso ? ? 1.00000 ? ? H113a .08018 .58579 -.15579 .14760 Uiso ? ? 1.00000 ? ? H113e .15087 .58853 -.23633 .14760 Uiso ? ? 1.00000 ? ? H114a .15682 .43081 -.24340 .15610 Uiso ? ? 1.00000 ? ? H114e .04767 .44830 -.28662 .15610 Uiso ? ? 1.00000 ? ? H115a .03373 .42661 -.09261 .14430 Uiso ? ? 1.00000 ? ? H115e .07765 .34017 -.13937 .14430 Uiso ? ? 1.00000 ? ? H116a .23044 .39734 -.00991 .12060 Uiso ? ? 1.00000 ? ? H116e .16070 .39479 .07193 .12060 Uiso ? ? 1.00000 ? ? H121 .26040 .42825 .26085 .18600 Uiso ? ? 1.00000 ? ? H122a .39389 .49971 .44802 .21240 Uiso ? ? 1.00000 ? ? H122e .37818 .40898 .35408 .21240 Uiso ? ? 1.00000 ? ? H123a .32562 .32954 .46601 .15040 Uiso ? ? 1.00000 ? ? H123e .37105 .41255 .57189 .15040 Uiso ? ? 1.00000 ? ? H124a .23893 .43943 .58921 .21950 Uiso ? ? 1.00000 ? ? H124e .20125 .34068 .51405 .21950 Uiso ? ? 1.00000 ? ? H125a .11680 .38774 .37760 .26600 Uiso ? ? 1.00000 ? ? H125e .13092 .47794 .47203 .26600 Uiso ? ? 1.00000 ? ? H126a .18197 .56091 .35798 .10700 Uiso ? ? 1.00000 ? ? H126e .13640 .47820 .25167 .10700 Uiso ? ? 1.00000 ? ? H131 .33981 .69193 .16744 .11550 Uiso ? ? 1.00000 ? ? H132a .24816 .69892 .34971 .14810 Uiso ? ? 1.00000 ? ? H132e .19941 .70632 .20800 .14810 Uiso ? ? 1.00000 ? ? H133a .28446 .85244 .22843 .16780 Uiso ? ? 1.00000 ? ? H133e .23195 .85548 .33089 .16780 Uiso ? ? 1.00000 ? ? H134a .37328 .83148 .48015 .19440 Uiso ? ? 1.00000 ? ? H134e .39381 .91878 .41801 .19440 Uiso ? ? 1.00000 ? ? H135a .46867 .83277 .29994 .20040 Uiso ? ? 1.00000 ? ? H135e .51803 .82435 .44121 .20040 Uiso ? ? 1.00000 ? ? H136a .43034 .67858 .42063 .12250 Uiso ? ? 1.00000 ? ? H136e .48345 .67422 .31878 .12250 Uiso ? ? 1.00000 ? ? H211 .88699 .01156 .08512 .09880 Uiso ? ? 1.00000 ? ? H212a .90244 .17104 .23815 .21840 Uiso ? ? 1.00000 ? ? H212e .93442 .07548 .27820 .21840 Uiso ? ? 1.00000 ? ? H213a 1.06349 .09378 .19664 .23760 Uiso ? ? 1.00000 ? ? H213e 1.07012 .17727 .29880 .23760 Uiso ? ? 1.00000 ? ? H214a .99688 .26425 .14289 .21400 Uiso ? ? 1.00000 ? ? H214e 1.09303 .23285 .12502 .21400 Uiso ? ? 1.00000 ? ? H215a 1.00500 .10618 -.01395 .28580 Uiso ? ? 1.00000 ? ? H215e .97112 .19898 -.06233 .28580 Uiso ? ? 1.00000 ? ? H216a .83413 .18235 .01360 .22310 Uiso ? ? 1.00000 ? ? H216e .83102 .09250 -.07692 .22310 Uiso ? ? 1.00000 ? ? H221 .71889 -.00763 -.07749 .15880 Uiso ? ? 1.00000 ? ? H222a .61394 .02916 -.13401 .19640 Uiso ? ? 1.00000 ? ? H222e .56134 -.03124 -.06177 .19640 Uiso ? ? 1.00000 ? ? H223a .49281 -.11289 -.21913 .14260 Uiso ? ? 1.00000 ? ? H223e .54471 -.05196 -.29158 .14260 Uiso ? ? 1.00000 ? ? H224a .61709 -.16185 -.33567 .22200 Uiso ? ? 1.00000 ? ? H224e .55388 -.22575 -.28006 .22200 Uiso ? ? 1.00000 ? ? H225a .66028 -.24693 -.15138 .26400 Uiso ? ? 1.00000 ? ? H225e .72405 -.19995 -.22277 .26400 Uiso ? ? 1.00000 ? ? H226a .79735 -.11048 -.06654 .13930 Uiso ? ? 1.00000 ? ? H226e .74184 -.16534 .00791 .13930 Uiso ? ? 1.00000 ? ? H231A .80956 .00918 .29915 .07280 Uiso ? ? .50000 ? ? H232Aa .78338 -.15599 .17853 .13310 Uiso ? ? .50000 ? ? H232Ae .87703 -.09217 .25799 .13310 Uiso ? ? .50000 ? ? H233Aa .88018 -.16433 .41801 .18510 Uiso ? ? .50000 ? ? H233Ae .78554 -.22700 .33922 .18510 Uiso ? ? .50000 ? ? H234Aa .80796 -.09300 .53050 .14320 Uiso ? ? .50000 ? ? H234Ae .72144 -.17067 .47254 .14320 Uiso ? ? .50000 ? ? H235Aa .64101 -.08915 .43729 .16740 Uiso ? ? .50000 ? ? H235Ae .72606 -.01241 .50759 .16740 Uiso ? ? .50000 ? ? H236Aa .62900 -.04141 .25622 .15340 Uiso ? ? .50000 ? ? H236Ae .69479 .04804 .33163 .15340 Uiso ? ? .50000 ? ? H231B .80647 -.06749 .22647 .07280 Uiso ? ? .50000 ? ? H232Ba .62231 -.07324 .25270 .15950 Uiso ? ? .50000 ? ? H232Be .65429 -.14292 .16139 .15950 Uiso ? ? .50000 ? ? H233Ba .65023 -.19987 .35237 .20100 Uiso ? ? .50000 ? ? H233Be .74639 -.21053 .31962 .20100 Uiso ? ? .50000 ? ? H234Ba .70935 -.09912 .49171 .14320 Uiso ? ? .50000 ? ? H234Be .79183 -.16411 .50206 .14320 Uiso ? ? .50000 ? ? H235Ba .89520 -.05083 .48501 .15100 Uiso ? ? .50000 ? ? H235Be .83823 .00165 .56357 .15100 Uiso ? ? .50000 ? ? H236Ba .74046 .05692 .39010 .10070 Uiso ? ? .50000 ? ? H236Be .84424 .07314 .37711 .10070 Uiso ? ? .50000 ? ? H32a 1.02312 .11708 .65585 .43200 Uiso ? ? .75000 ? ? H32b .95674 .15293 .73305 .43200 Uiso ? ? .75000 ? ? H32c .91077 .09352 .60224 .43200 Uiso ? ? .75000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag1 .0843(9) .0885(10) .0997(10) .0390(8) .0431(8) .0233(8) Ag2 .0957(10) .0547(8) .1250(12) .0301(7) .0511(9) .0201(7) S1 .076(3) .071(3) .086(3) .021(2) .033(3) .012(2) C1 .085(11) .050(9) .078(11) .008(8) .050(9) .005(8) N1 .085(9) .062(8) .081(9) .018(7) .035(7) .015(7) S2 .120(4) .084(3) .088(3) .049(3) .015(3) .018(3) C2 .091(12) .082(11) .043(10) .007(9) .013(9) -.012(8) N2 .099(10) .090(10) .092(10) .042(8) .023(8) -.005(8) P1 .067(3) .085(3) .078(3) .027(2) .033(3) .023(3) C111 .080(11) .067(10) .091(12) .021(8) .051(9) .018(9) C112 .116(14) .089(12) .071(12) .009(10) .025(10) .020(9) C113 .097(14) .161(17) .099(14) .020(12) .006(11) .058(12) C114 .127(16) .167(18) .083(14) -.017(14) .029(12) -.005(12) C115 .113(15) .132(16) .103(14) -.029(12) .034(12) -.006(12) C116 .107(13) .092(12) .091(13) .002(10) .043(11) .008(10) C121 .101(14) .21(2) .130(15) .095(14) .075(12) .111(14) C122 .123(16) .25(2) .139(17) .090(16) .070(14) .141(17) C123 .154(17) .120(15) .088(13) .047(13) .036(12) .055(11) C124 .18(2) .157(19) .19(2) .050(16) .119(17) .096(16) C125 .148(19) .29(3) .21(2) .077(18) .110(17) .17(2) C126 .104(13) .079(11) .075(12) .022(10) .022(10) .030(9) C131 .104(13) .083(12) .093(13) .019(10) .053(11) -.000(10) C132 .130(16) .081(12) .147(16) .037(11) .048(13) .016(11) C133 .151(17) .085(13) .171(19) .043(12) .027(14) .009(12) C134 .23(2) .097(15) .145(18) .024(15) .085(17) .022(13) C135 .17(2) .132(17) .18(2) -.034(15) .087(16) -.006(15) C136 .070(11) .123(15) .101(13) .011(10) .024(10) -.031(11) P2 .076(3) .056(3) .097(4) .018(2) .027(3) .005(2) C211 .092(12) .070(11) .075(11) .008(9) .018(10) .006(9) C212 .095(15) .25(3) .18(2) -.054(16) .036(15) .066(19) C213 .119(17) .22(2) .23(3) -.023(17) -.001(17) .12(2) C214 .19(2) .071(13) .26(2) -.040(13) .108(19) -.032(14) C215 .21(2) .17(2) .30(3) .046(17) .18(2) .09(2) C216 .123(17) .24(2) .17(2) .037(16) .039(15) .136(18) C221 .091(14) .119(15) .164(18) .056(12) -.038(13) -.054(13) C222 .140(17) .18(2) .155(19) .092(15) -.050(15) -.106(16) C223 .128(15) .110(15) .107(15) .017(12) .015(12) .010(11) C224 .22(2) .21(2) .105(17) -.00(2) .003(16) -.067(16) C225 .24(3) .19(2) .21(2) .08(2) -.05(2) -.17(2) C226 .117(14) .093(13) .127(15) .040(11) .048(12) .008(11) C231 .137(15) .075(11) .145(15) .052(11) .085(13) .036(11) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter y(es) for value to be published Ag1 S1 . . 2.787(4) ? Ag1 N2 . . 2.207(11) ? Ag1 P1 . . 2.394(5) ? Ag1 S1 . '2 665' 2.767(4) ? Ag2 N1 . . 2.206(10) ? Ag2 S2 . . 2.547(4) ? Ag2 P2 . . 2.385(4) ? S1 C1 . . 1.645(13) ? C1 N1 . . 1.147(16) ? S2 C2 . . 1.626(14) ? C2 N2 . . 1.161(18) ? P1 C111 . . 1.829(12) ? P1 C121 . . 1.83(2) ? P1 C131 . . 1.841(14) ? C111 C112 . . 1.52(2) ? C111 C116 . . 1.507(18) ? C112 C113 . . 1.501(18) ? C113 C114 . . 1.51(2) ? C114 C115 . . 1.52(3) ? C115 C116 . . 1.520(19) ? C121 C122 . . 1.32(2) ? C121 C126 . . 1.49(2) ? C122 C123 . . 1.49(3) ? C123 C124 . . 1.45(3) ? C124 C125 . . 1.31(3) ? C125 C126 . . 1.51(3) ? C131 C132 . . 1.51(2) ? C131 C136 . . 1.505(17) ? C132 C133 . . 1.54(2) ? C133 C134 . . 1.51(2) ? C134 C135 . . 1.48(3) ? C135 C136 . . 1.56(2) ? P2 C211 . . 1.824(16) ? P2 C221 . . 1.801(15) ? P2 C231 . . 1.811(17) ? C211 C212 . . 1.39(2) ? C211 C216 . . 1.49(3) ? C212 C213 . . 1.52(3) ? C213 C214 . . 1.46(3) ? C214 C215 . . 1.46(3) ? C215 C216 . . 1.59(3) ? C221 C222 . . 1.26(2) ? C221 C226 . . 1.55(2) ? C222 C223 . . 1.44(2) ? C223 C224 . . 1.49(3) ? C224 C225 . . 1.30(3) ? C225 C226 . . 1.47(2) ? C231 C232A . . 1.43(4) ? C231 C236A . . 1.40(4) ? C231 C232B . . 1.51(4) ? C231 C236B . . 1.57(3) ? C232A C233A . . 1.56(5) ? C232A C232B . . 1.94(5) ? C233A C234 . . 1.56(5) ? C233A C233B . . 1.48(6) ? C234 C235A . . 1.17(4) ? C234 C233B . . 1.34(4) ? C234 C235B . . 1.54(4) ? C235A C236A . . 1.59(5) ? C235A C233B . . 1.79(5) ? C235A C235B . . 1.79(5) ? C236A C232B . . 1.37(5) ? C236A C236B . . 1.49(4) ? C232B C233B . . 1.51(5) ? C235B C236B . . 1.55(4) ? N31 C31 . . 1.31(5) ? C31 C32 . . 1.27(6) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter yes for value to be published S1 Ag1 N2 . . . 94.1(3) ? S1 Ag1 P1 . . . 119.26(12) ? S1 Ag1 S1 . . '2 665' 92.12(13) ? N2 Ag1 P1 . . . 131.1(4) ? N2 Ag1 S1 . . '2 665' 95.9(3) ? P1 Ag1 S1 . . '2 665' 115.67(14) ? N1 Ag2 S2 . . . 102.3(3) ? N1 Ag2 P2 . . . 136.2(3) ? S2 Ag2 P2 . . . 121.40(14) ? Ag1 S1 C1 . . . 99.0(5) ? Ag1 S1 Ag1 . . '2 665' 87.88(11) ? C1 S1 Ag1 . . '2 665' 101.9(5) ? S1 C1 N1 . . . 178.4(11) ? Ag2 N1 C1 . . . 157.8(9) ? Ag2 S2 C2 . . . 98.4(4) ? S2 C2 N2 . . . 176.8(13) ? Ag1 N2 C2 . . . 166.9(10) ? Ag1 P1 C111 . . . 111.4(5) ? Ag1 P1 C121 . . . 113.5(6) ? Ag1 P1 C131 . . . 110.1(5) ? C111 P1 C121 . . . 107.2(7) ? C111 P1 C131 . . . 106.5(6) ? C121 P1 C131 . . . 107.8(8) ? P1 C111 C112 . . . 112.5(9) ? P1 C111 C116 . . . 110.5(9) ? C112 C111 C116 . . . 109.9(11) ? C111 C112 C113 . . . 113.7(13) ? C112 C113 C114 . . . 112.5(13) ? C113 C114 C115 . . . 109.8(13) ? C114 C115 C116 . . . 112.2(13) ? C111 C116 C115 . . . 112.6(12) ? P1 C121 C122 . . . 122.1(14) ? P1 C121 C126 . . . 118.5(11) ? C122 C121 C126 . . . 118.7(17) ? C121 C122 C123 . . . 123.5(17) ? C122 C123 C124 . . . 116.9(15) ? C123 C124 C125 . . . 119(2) ? C124 C125 C126 . . . 124.2(19) ? C121 C126 C125 . . . 114.2(14) ? P1 C131 C132 . . . 118.7(10) ? P1 C131 C136 . . . 114.2(10) ? C132 C131 C136 . . . 109.7(12) ? C131 C132 C133 . . . 113.4(14) ? C132 C133 C134 . . . 109.3(13) ? C133 C134 C135 . . . 113.3(15) ? C134 C135 C136 . . . 108.9(15) ? C131 C136 C135 . . . 113.4(13) ? Ag2 P2 C211 . . . 109.3(5) ? Ag2 P2 C221 . . . 113.0(6) ? Ag2 P2 C231 . . . 114.5(6) ? C211 P2 C221 . . . 108.2(8) ? C211 P2 C231 . . . 107.5(7) ? C221 P2 C231 . . . 104.0(7) ? P2 C211 C212 . . . 114.9(13) ? P2 C211 C216 . . . 114.1(10) ? C212 C211 C216 . . . 108.0(14) ? C211 C212 C213 . . . 118.1(19) ? C212 C213 C214 . . . 108.9(17) ? C213 C214 C215 . . . 106.6(16) ? C214 C215 C216 . . . 110(2) ? C211 C216 C215 . . . 112.1(15) ? P2 C221 C222 . . . 123.1(14) ? P2 C221 C226 . . . 118.5(10) ? C222 C221 C226 . . . 116.6(15) ? C221 C222 C223 . . . 127.3(18) ? C222 C223 C224 . . . 118.0(15) ? C223 C224 C225 . . . 115.2(17) ? C224 C225 C226 . . . 128(2) ? C221 C226 C225 . . . 113.4(14) ? P2 C231 C232A . . . 122.0(18) ? P2 C231 C236A . . . 115.0(17) ? P2 C231 C232B . . . 119.6(15) ? P2 C231 C236B . . . 114.8(13) ? C232A C231 C236A . . . 121(2) ? C232A C231 C232B . . . 82(2) ? C232A C231 C236B . . . 105.5(17) ? C236A C231 C232B . . . 56(2) ? C236A C231 C236B . . . 60.0(17) ? C232B C231 C236B . . . 108(2) ? C231 C232A C233A . . . 115(3) ? C231 C232A C232B . . . 50.5(16) ? C233A C232A C232B . . . 84(2) ? C232A C233A C234 . . . 114(3) ? C232A C233A C233B . . . 93(3) ? C234 C233A C233B . . . 52(2) ? C233A C234 C235A . . . 131(3) ? C233A C234 C233B . . . 61(2) ? C233A C234 C235B . . . 87(2) ? C235A C234 C233B . . . 90(3) ? C235A C234 C235B . . . 82(3) ? C233B C234 C235B . . . 129(3) ? C234 C235A C236A . . . 113(3) ? C234 C235A C233B . . . 49(2) ? C234 C235A C235B . . . 58(2) ? C236A C235A C233B . . . 82(2) ? C236A C235A C235B . . . 90(3) ? C233B C235A C235B . . . 93(2) ? C231 C236A C235A . . . 122(3) ? C231 C236A C232B . . . 66(2) ? C231 C236A C236B . . . 66(2) ? C235A C236A C232B . . . 93(3) ? C235A C236A C236B . . . 84(2) ? C232B C236A C236B . . . 121(3) ? C231 C232B C232A . . . 47.1(15) ? C231 C232B C236A . . . 58(2) ? C231 C232B C233B . . . 112(2) ? C232A C232B C236A . . . 95(2) ? C232A C232B C233B . . . 78(2) ? C236A C232B C233B . . . 101(3) ? C233A C233B C234 . . . 67(2) ? C233A C233B C235A . . . 99(3) ? C233A C233B C232B . . . 104(3) ? C234 C233B C235A . . . 41.0(19) ? C234 C233B C232B . . . 113(3) ? C235A C233B C232B . . . 81(3) ? C234 C235B C235A . . . 40.4(17) ? C234 C235B C236B . . . 105(2) ? C235A C235B C236B . . . 76(2) ? C231 C236B C236A . . . 54.2(18) ? C231 C236B C235B . . . 114(2) ? C236A C236B C235B . . . 104(2) ? N31 C31 C32 . . . 171(4) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter yes for value to be published N2 Ag1 S1 C1 . . . . 5.6(6) ? N2 Ag1 S1 Ag1 . . . '2 665' -96.1(3) ? P1 Ag1 S1 C1 . . . . -137.1(5) ? P1 Ag1 S1 Ag1 . . . '2 665' 121.17(15) ? S1 Ag1 S1 C1 '2 665' . . . 101.8(5) ? S1 Ag1 S1 Ag1 '2 665' . . '2 665' -.00(12) ? S1 Ag1 N2 C2 . . . . -5(5) ? P1 Ag1 N2 C2 . . . . 131(5) ? S1 Ag1 N2 C2 '2 665' . . . -97(5) ? S1 Ag1 P1 C111 . . . . -12.7(5) ? S1 Ag1 P1 C121 . . . . 108.4(5) ? S1 Ag1 P1 C131 . . . . -130.7(5) ? N2 Ag1 P1 C111 . . . . -139.4(6) ? N2 Ag1 P1 C121 . . . . -18.3(6) ? N2 Ag1 P1 C131 . . . . 102.6(6) ? S1 Ag1 P1 C111 '2 665' . . . 95.7(5) ? S1 Ag1 P1 C121 '2 665' . . . -143.1(5) ? S1 Ag1 P1 C131 '2 665' . . . -22.2(5) ? S1 Ag1 S1 Ag1 . . '2 665' '2 665' .00(12) ? N2 Ag1 S1 Ag1 . . '2 665' '2 665' 94.4(3) ? P1 Ag1 S1 Ag1 . . '2 665' '2 665' -124.09(13) ? S2 Ag2 N1 C1 . . . . 0(3) ? P2 Ag2 N1 C1 . . . . -177(3) ? N1 Ag2 S2 C2 . . . . 1.8(6) ? P2 Ag2 S2 C2 . . . . 178.4(6) ? N1 Ag2 P2 C211 . . . . 100.0(6) ? N1 Ag2 P2 C221 . . . . -20.5(9) ? N1 Ag2 P2 C231 . . . . -139.3(7) ? S2 Ag2 P2 C211 . . . . -75.2(5) ? S2 Ag2 P2 C221 . . . . 164.3(7) ? S2 Ag2 P2 C231 . . . . 45.4(5) ? Ag1 S1 C1 N1 . . . . 169(48) ? Ag1 S1 C1 N1 '2 665' . . . -102(48) ? Ag1 S1 Ag1 S1 . . '2 665' '2 665' -.00(12) ? C1 S1 Ag1 S1 . . '2 665' '2 665' -98.7(5) ? S1 C1 N1 Ag2 . . . . -174(46) ? Ag2 S2 C2 N2 . . . . 79(21) ? S2 C2 N2 Ag1 . . . . -80(23) ? Ag1 P1 C111 C112 . . . . -59.5(10) ? Ag1 P1 C111 C116 . . . . 63.7(12) ? C121 P1 C111 C112 . . . . 175.7(11) ? C121 P1 C111 C116 . . . . -61.1(13) ? C131 P1 C111 C112 . . . . 60.6(12) ? C131 P1 C111 C116 . . . . -176.2(11) ? Ag1 P1 C121 C122 . . . . 25.2(17) ? Ag1 P1 C121 C126 . . . . -164.6(9) ? C111 P1 C121 C122 . . . . 148.7(15) ? C111 P1 C121 C126 . . . . -41.1(13) ? C131 P1 C121 C122 . . . . -97.0(16) ? C131 P1 C121 C126 . . . . 73.2(12) ? Ag1 P1 C131 C132 . . . . 178.4(10) ? Ag1 P1 C131 C136 . . . . -49.7(13) ? C111 P1 C131 C132 . . . . 57.4(13) ? C111 P1 C131 C136 . . . . -170.7(12) ? C121 P1 C131 C132 . . . . -57.3(13) ? C121 P1 C131 C136 . . . . 74.6(13) ? P1 C111 C112 C113 . . . . 176.2(11) ? C116 C111 C112 C113 . . . . 52.6(17) ? P1 C111 C116 C115 . . . . -177.5(12) ? C112 C111 C116 C115 . . . . -52.8(18) ? C111 C112 C113 C114 . . . . -54(2) ? C112 C113 C114 C115 . . . . 54(2) ? C113 C114 C115 C116 . . . . -54.3(19) ? C114 C115 C116 C111 . . . . 55(2) ? P1 C121 C122 C123 . . . . -173.2(13) ? C126 C121 C122 C123 . . . . 17(3) ? P1 C121 C126 C125 . . . . 173.9(11) ? C122 C121 C126 C125 . . . . -15(2) ? C121 C122 C123 C124 . . . . -16(2) ? C122 C123 C124 C125 . . . . 15(2) ? C123 C124 C125 C126 . . . . -17(3) ? C124 C125 C126 C121 . . . . 17(3) ? P1 C131 C132 C133 . . . . -172.7(11) ? C136 C131 C132 C133 . . . . 53.5(18) ? P1 C131 C136 C135 . . . . 170.4(13) ? C132 C131 C136 C135 . . . . -54(2) ? C131 C132 C133 C134 . . . . -55(2) ? C132 C133 C134 C135 . . . . 57(2) ? C133 C134 C135 C136 . . . . -57(2) ? C134 C135 C136 C131 . . . . 55(2) ? Ag2 P2 C211 C212 . . . . 70.9(14) ? Ag2 P2 C211 C216 . . . . -54.5(12) ? C221 P2 C211 C212 . . . . -165.6(14) ? C221 P2 C211 C216 . . . . 69.0(13) ? C231 P2 C211 C212 . . . . -53.9(15) ? C231 P2 C211 C216 . . . . -179.3(12) ? Ag2 P2 C221 C222 . . . . 5(2) ? Ag2 P2 C221 C226 . . . . 169.1(12) ? C211 P2 C221 C222 . . . . -116.4(19) ? C211 P2 C221 C226 . . . . 47.9(16) ? C231 P2 C221 C222 . . . . 129.6(19) ? C231 P2 C221 C226 . . . . -66.1(16) ? Ag2 P2 C231 C232A . . . . -175.2(15) ? Ag2 P2 C231 C236A . . . . 21.3(16) ? Ag2 P2 C231 C232B . . . . 85(2) ? Ag2 P2 C231 C236B . . . . -45.7(16) ? C211 P2 C231 C232A . . . . -53.5(17) ? C211 P2 C231 C236A . . . . 142.9(15) ? C211 P2 C231 C232B . . . . -153.6(19) ? C211 P2 C231 C236B . . . . 76.0(16) ? C221 P2 C231 C232A . . . . 61.0(17) ? C221 P2 C231 C236A . . . . -102.6(16) ? C221 P2 C231 C232B . . . . -39(2) ? C221 P2 C231 C236B . . . . -169.5(16) ? P2 C211 C212 C213 . . . . 179.3(15) ? C216 C211 C212 C213 . . . . -52(2) ? P2 C211 C216 C215 . . . . 177.9(12) ? C212 C211 C216 C215 . . . . 49(2) ? C211 C212 C213 C214 . . . . 60(2) ? C212 C213 C214 C215 . . . . -61(2) ? C213 C214 C215 C216 . . . . 62(2) ? C214 C215 C216 C211 . . . . -57(2) ? P2 C221 C222 C223 . . . . 175.2(16) ? C226 C221 C222 C223 . . . . 11(3) ? P2 C221 C226 C225 . . . . -177.5(15) ? C222 C221 C226 C225 . . . . -12(3) ? C221 C222 C223 C224 . . . . -8(3) ? C222 C223 C224 C225 . . . . 8(3) ? C223 C224 C225 C226 . . . . -12(4) ? C224 C225 C226 C221 . . . . 14(3) ? P2 C231 C232A C233A . . . . -178.2(17) ? P2 C231 C232A C232B . . . . -120.2(18) ? C236A C231 C232A C233A . . . . -16(3) ? C236A C231 C232A C232B . . . . 42(2) ? C232B C231 C232A C233A . . . . -58(2) ? C232B C231 C232A C232B . . . . .0(18) ? C236B C231 C232A C233A . . . . 48(3) ? C236B C231 C232A C232B . . . . 106(2) ? P2 C231 C236A C235A . . . . -171(2) ? P2 C231 C236A C232B . . . . 110(2) ? P2 C231 C236A C236B . . . . -105.4(17) ? C232A C231 C236A C235A . . . . 25(3) ? C232A C231 C236A C232B . . . . -54(2) ? C232A C231 C236A C236B . . . . 91(2) ? C232B C231 C236A C235A . . . . 79(3) ? C232B C231 C236A C232B . . . . 0(2) ? C232B C231 C236A C236B . . . . 145(3) ? C236B C231 C236A C235A . . . . -66(3) ? C236B C231 C236A C232B . . . . -145(3) ? C236B C231 C236A C236B . . . . .0(17) ? P2 C231 C232B C232A . . . . 123(2) ? P2 C231 C232B C236A . . . . -102(2) ? P2 C231 C232B C233B . . . . 169(2) ? C232A C231 C232B C232A . . . . -.0(17) ? C232A C231 C232B C236A . . . . 136(2) ? C232A C231 C232B C233B . . . . 47(3) ? C236A C231 C232B C232A . . . . -136(2) ? C236A C231 C232B C236A . . . . 0(2) ? C236A C231 C232B C233B . . . . -89(3) ? C236B C231 C232B C232A . . . . -104(2) ? C236B C231 C232B C236A . . . . 32(2) ? C236B C231 C232B C233B . . . . -57(3) ? P2 C231 C236B C236A . . . . 106(2) ? P2 C231 C236B C235B . . . . -163(2) ? C232A C231 C236B C236A . . . . -117(2) ? C232A C231 C236B C235B . . . . -26(3) ? C236A C231 C236B C236A . . . . 0(2) ? C236A C231 C236B C235B . . . . 91(3) ? C232B C231 C236B C236A . . . . -30(2) ? C232B C231 C236B C235B . . . . 61(3) ? C231 C232A C233A C234 . . . . -1(3) ? C231 C232A C233A C233B . . . . 48(3) ? C232B C232A C233A C234 . . . . -42(2) ? C232B C232A C233A C233B . . . . 7(2) ? C231 C232A C232B C231 . . . . .0(12) ? C231 C232A C232B C236A . . . . -36(2) ? C231 C232A C232B C233B . . . . -137(3) ? C233A C232A C232B C231 . . . . 129(2) ? C233A C232A C232B C236A . . . . 93(3) ? C233A C232A C232B C233B . . . . -7(2) ? C232A C233A C234 C235A . . . . 12(4) ? C232A C233A C234 C233B . . . . 73(3) ? C232A C233A C234 C235B . . . . -65(3) ? C233B C233A C234 C235A . . . . -62(4) ? C233B C233A C234 C233B . . . . 0(3) ? C233B C233A C234 C235B . . . . -138(3) ? C232A C233A C233B C234 . . . . -119(3) ? C232A C233A C233B C235A . . . . -93(3) ? C232A C233A C233B C232B . . . . -9(3) ? C234 C233A C233B C234 . . . . .0(17) ? C234 C233A C233B C235A . . . . 26(2) ? C234 C233A C233B C232B . . . . 109(3) ? C233A C234 C235A C236A . . . . -4(5) ? C233A C234 C235A C233B . . . . 50(3) ? C233A C234 C235A C235B . . . . -79(3) ? C233B C234 C235A C236A . . . . -54(3) ? C233B C234 C235A C233B . . . . 0(3) ? C233B C234 C235A C235B . . . . -129(3) ? C235B C234 C235A C236A . . . . 75(3) ? C235B C234 C235A C233B . . . . 129(3) ? C235B C234 C235A C235B . . . . .0(19) ? C233A C234 C233B C233A . . . . 0(2) ? C233A C234 C233B C235A . . . . -138(3) ? C233A C234 C233B C232B . . . . -96(4) ? C235A C234 C233B C233A . . . . 138(3) ? C235A C234 C233B C235A . . . . 0(3) ? C235A C234 C233B C232B . . . . 42(4) ? C235B C234 C233B C233A . . . . 59(4) ? C235B C234 C233B C235A . . . . -79(4) ? C235B C234 C233B C232B . . . . -37(5) ? C233A C234 C235B C235A . . . . 132(3) ? C233A C234 C235B C236B . . . . 86(3) ? C235A C234 C235B C235A . . . . 0(3) ? C235A C234 C235B C236B . . . . -47(3) ? C233B C234 C235B C235A . . . . 84(4) ? C233B C234 C235B C236B . . . . 37(5) ? C234 C235A C236A C231 . . . . -15(4) ? C234 C235A C236A C232B . . . . 49(3) ? C234 C235A C236A C236B . . . . -71(3) ? C233B C235A C236A C231 . . . . -53(3) ? C233B C235A C236A C232B . . . . 11(3) ? C233B C235A C236A C236B . . . . -110(2) ? C235B C235A C236A C231 . . . . 40(3) ? C235B C235A C236A C232B . . . . 104(3) ? C235B C235A C236A C236B . . . . -16(2) ? C234 C235A C233B C233A . . . . -38(3) ? C234 C235A C233B C234 . . . . 0(3) ? C234 C235A C233B C232B . . . . -141(4) ? C236A C235A C233B C233A . . . . 93(3) ? C236A C235A C233B C234 . . . . 131(4) ? C236A C235A C233B C232B . . . . -10(2) ? C235B C235A C233B C233A . . . . 3(3) ? C235B C235A C233B C234 . . . . 41(3) ? C235B C235A C233B C232B . . . . -100(3) ? C234 C235A C235B C234 . . . . 0(2) ? C234 C235A C235B C236B . . . . 134(3) ? C236A C235A C235B C234 . . . . -117(3) ? C236A C235A C235B C236B . . . . 16(2) ? C233B C235A C235B C234 . . . . -36(2) ? C233B C235A C235B C236B . . . . 98(2) ? C231 C236A C232B C231 . . . . -.0(9) ? C231 C236A C232B C232A . . . . 30.9(17) ? C231 C236A C232B C233B . . . . 110(3) ? C235A C236A C232B C231 . . . . -123(2) ? C235A C236A C232B C232A . . . . -92(2) ? C235A C236A C232B C233B . . . . -13(3) ? C236B C236A C232B C231 . . . . -38(3) ? C236B C236A C232B C232A . . . . -7(4) ? C236B C236A C232B C233B . . . . 72(4) ? C231 C236A C236B C231 . . . . .0(10) ? C231 C236A C236B C235B . . . . -109(2) ? C235A C236A C236B C231 . . . . 129(2) ? C235A C236A C236B C235B . . . . 20(3) ? C232B C236A C236B C231 . . . . 38(3) ? C232B C236A C236B C235B . . . . -71(4) ? C231 C232B C233B C233A . . . . -25(4) ? C231 C232B C233B C234 . . . . 45(5) ? C231 C232B C233B C235A . . . . 72(3) ? C232A C232B C233B C233A . . . . 8(2) ? C232A C232B C233B C234 . . . . 78(3) ? C232A C232B C233B C235A . . . . 105(2) ? C236A C232B C233B C233A . . . . -85(4) ? C236A C232B C233B C234 . . . . -14(4) ? C236A C232B C233B C235A . . . . 12(3) ? C234 C235B C236B C231 . . . . -46(3) ? C234 C235B C236B C236A . . . . 11(3) ? C235A C235B C236B C231 . . . . -75(2) ? C235A C235B C236B C236A . . . . -18(3) ? S1 Ag1 S1 Ag1 . '2 665' '2 665' . -.00(12) ? _diffrn_measured_fraction_theta_max 0.805 _diffrn_reflns_theta_full 22.55 _diffrn_measured_fraction_theta_full 0.805 _refine_diff_density_max 0.49 _refine_diff_density_min -0.34 _refine_diff_density_rms 0.06 data_cmpnd06 _database_code_depnum_ccdc_archive 'CCDC 869213' #TrackingRef 'UWA120227.cif' _audit_creation_date 2011-10-13T16:31:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C44 H42 Ag2 N2 P2 S2' _chemical_formula_moiety 'C44 H42 Ag2 N2 P2 S2' _chemical_formula_weight 940.6 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3067(4) _cell_length_b 11.2705(6) _cell_length_c 19.6439(10) _cell_angle_alpha 81.971(4) _cell_angle_beta 87.408(4) _cell_angle_gamma 78.200(4) _cell_volume 1996.86(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6100 _cell_measurement_theta_min 3.6925 _cell_measurement_theta_max 32.4974 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0317 0 0 1 0.0693 2 1 0 0.1284 2 1 2 0.1342 -1 0 -1 0.1 -1 -1 2 0.0786 0 1 0 0.0128 0 -1 0 0.0054 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.979 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0378984764 _diffrn_orient_matrix_ub_12 0.0384383976 _diffrn_orient_matrix_ub_13 -0.0280187204 _diffrn_orient_matrix_ub_21 0.067099668 _diffrn_orient_matrix_ub_22 0.0149442761 _diffrn_orient_matrix_ub_23 -0.0133300073 _diffrn_orient_matrix_ub_31 0.0111539715 _diffrn_orient_matrix_ub_32 -0.0500540419 _diffrn_orient_matrix_ub_33 -0.0191967985 _diffrn_measurement_device_type 'Oxford Diffraction Gemini diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_unetI/netI 0.1166 _diffrn_reflns_number 22081 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.7 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 11618 _reflns_number_gt 6372 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0225P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11618 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.807 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.83 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 0.32581(3) 0.15328(2) 0.335730(13) 0.01913(7) Uani 1 1 d . . . Ag2 Ag 0.68991(3) -0.15144(2) 0.167620(13) 0.01832(7) Uani 1 1 d . . . S1 S 0.25479(9) -0.04816(8) 0.31785(4) 0.01953(19) Uani 1 1 d . . . C1 C 0.3846(4) -0.0960(3) 0.26140(17) 0.0147(7) Uani 1 1 d . . . N1 N 0.4744(3) -0.1331(2) 0.22285(14) 0.0192(6) Uani 1 1 d . . . S2 S 0.78400(11) 0.02205(9) 0.20644(6) 0.0385(3) Uani 1 1 d . . . C2 C 0.6378(4) 0.0825(3) 0.24946(18) 0.0220(8) Uani 1 1 d . . . N2 N 0.5360(3) 0.1296(3) 0.27834(16) 0.0281(8) Uani 1 1 d . . . P1 P 0.18155(9) 0.29832(8) 0.40277(4) 0.01186(18) Uani 1 1 d . . . C111 C -0.0010(3) 0.2685(3) 0.42635(15) 0.0120(6) Uani 1 1 d . . . C112 C -0.0928(3) 0.2503(3) 0.37506(16) 0.0141(7) Uani 1 1 d . . . C113 C -0.2348(3) 0.2375(3) 0.39445(17) 0.0177(7) Uani 1 1 d . . . H113 H -0.2989 0.2266 0.3605 0.021 Uiso 1 1 calc R . . C114 C -0.2860(3) 0.2400(3) 0.46158(16) 0.0181(7) Uani 1 1 d . . . H114 H -0.3838 0.2312 0.4731 0.022 Uiso 1 1 calc R . . C115 C -0.1950(3) 0.2551(3) 0.51163(15) 0.0163(7) Uani 1 1 d . . . H115 H -0.2289 0.2551 0.558 0.02 Uiso 1 1 calc R . . C116 C -0.0534(3) 0.2705(3) 0.49393(15) 0.0141(6) Uani 1 1 d . . . H116 H 0.0088 0.2825 0.5283 0.017 Uiso 1 1 calc R . . C117 C -0.0430(3) 0.2470(3) 0.30143(15) 0.0191(7) Uani 1 1 d . . . H11A H 0.0344 0.1745 0.2982 0.029 Uiso 1 1 calc R . . H11B H -0.0047 0.3207 0.2846 0.029 Uiso 1 1 calc R . . H11C H -0.1262 0.2435 0.2734 0.029 Uiso 1 1 calc R . . C121 C 0.1413(3) 0.4597(3) 0.36434(14) 0.0125(6) Uani 1 1 d . . . C122 C 0.2511(3) 0.5148(3) 0.32887(15) 0.0155(7) Uani 1 1 d . . . C123 C 0.2136(4) 0.6377(3) 0.30117(15) 0.0177(7) Uani 1 1 d . . . H123 H 0.2872 0.6763 0.278 0.021 Uiso 1 1 calc R . . C124 C 0.0722(4) 0.7051(3) 0.30641(15) 0.0196(7) Uani 1 1 d . . . H124 H 0.0492 0.7881 0.286 0.024 Uiso 1 1 calc R . . C125 C -0.0349(4) 0.6514(3) 0.34135(16) 0.0189(7) Uani 1 1 d . . . H125 H -0.1318 0.6973 0.3456 0.023 Uiso 1 1 calc R . . C126 C -0.0001(3) 0.5297(3) 0.37032(15) 0.0156(7) Uani 1 1 d . . . H126 H -0.0739 0.4932 0.3947 0.019 Uiso 1 1 calc R . . C127 C 0.4060(3) 0.4462(3) 0.32045(16) 0.0203(7) Uani 1 1 d . . . H12A H 0.4675 0.5033 0.3 0.03 Uiso 1 1 calc R . . H12B H 0.4072 0.3836 0.2904 0.03 Uiso 1 1 calc R . . H12C H 0.4442 0.407 0.3655 0.03 Uiso 1 1 calc R . . C131 C 0.2723(3) 0.2989(3) 0.48381(14) 0.0116(6) Uani 1 1 d . . . C132 C 0.3216(3) 0.1891(3) 0.52714(16) 0.0145(7) Uani 1 1 d . . . C133 C 0.3993(3) 0.1926(3) 0.58577(15) 0.0159(7) Uani 1 1 d . . . H133 H 0.4319 0.1189 0.6156 0.019 Uiso 1 1 calc R . . C134 C 0.4298(3) 0.3002(3) 0.60134(15) 0.0178(7) Uani 1 1 d . . . H134 H 0.4839 0.3003 0.6412 0.021 Uiso 1 1 calc R . . C135 C 0.3808(3) 0.4085(3) 0.55847(15) 0.0170(7) Uani 1 1 d . . . H135 H 0.4017 0.483 0.5688 0.02 Uiso 1 1 calc R . . C136 C 0.3015(3) 0.4078(3) 0.50051(15) 0.0137(6) Uani 1 1 d . . . H136 H 0.2666 0.4824 0.4718 0.016 Uiso 1 1 calc R . . C137 C 0.2933(4) 0.0674(3) 0.51333(17) 0.0224(7) Uani 1 1 d . . . H13A H 0.1875 0.0732 0.5089 0.034 Uiso 1 1 calc R . . H13B H 0.3301 0.0043 0.5515 0.034 Uiso 1 1 calc R . . H13C H 0.3439 0.0458 0.4706 0.034 Uiso 1 1 calc R . . P2 P 0.81662(9) -0.29278(8) 0.09325(4) 0.01136(18) Uani 1 1 d . . . C211 C 1.0148(3) -0.3381(3) 0.10955(14) 0.0136(6) Uani 1 1 d . . . C212 C 1.1009(4) -0.2503(3) 0.10869(16) 0.0167(7) Uani 1 1 d . . . C213 C 1.2501(3) -0.2893(3) 0.12431(15) 0.0191(7) Uani 1 1 d . . . H213 H 1.3099 -0.2304 0.1244 0.023 Uiso 1 1 calc R . . C214 C 1.3115(4) -0.4124(3) 0.13960(15) 0.0235(8) Uani 1 1 d . . . H214 H 1.4131 -0.4371 0.1495 0.028 Uiso 1 1 calc R . . C215 C 1.2271(3) -0.4987(3) 0.14052(15) 0.0214(7) Uani 1 1 d . . . H215 H 1.2695 -0.583 0.1514 0.026 Uiso 1 1 calc R . . C216 C 1.0787(3) -0.4623(3) 0.12551(15) 0.0168(7) Uani 1 1 d . . . H216 H 1.02 -0.5222 0.1261 0.02 Uiso 1 1 calc R . . C217 C 1.0451(4) -0.1149(3) 0.08831(18) 0.0261(8) Uani 1 1 d . . . H21A H 0.9386 -0.0989 0.0821 0.039 Uiso 1 1 calc R . . H21B H 1.0929 -0.0878 0.0451 0.039 Uiso 1 1 calc R . . H21C H 1.0674 -0.07 0.1245 0.039 Uiso 1 1 calc R . . C221 C 0.7500(3) -0.4366(3) 0.10167(15) 0.0120(6) Uani 1 1 d . . . C222 C 0.7250(3) -0.4987(3) 0.16799(16) 0.0126(7) Uani 1 1 d . . . C223 C 0.6710(3) -0.6054(3) 0.17166(15) 0.0159(6) Uani 1 1 d . . . H223 H 0.6538 -0.6479 0.2155 0.019 Uiso 1 1 calc R . . C224 C 0.6412(3) -0.6518(3) 0.11321(16) 0.0179(7) Uani 1 1 d . . . H224 H 0.6048 -0.7253 0.1173 0.021 Uiso 1 1 calc R . . C225 C 0.6649(3) -0.5905(3) 0.04877(16) 0.0186(7) Uani 1 1 d . . . H225 H 0.6445 -0.6213 0.0084 0.022 Uiso 1 1 calc R . . C226 C 0.7183(3) -0.4844(3) 0.04400(15) 0.0143(6) Uani 1 1 d . . . H226 H 0.734 -0.4425 -0.0003 0.017 Uiso 1 1 calc R . . C227 C 0.7542(3) -0.4515(3) 0.23327(15) 0.0179(7) Uani 1 1 d . . . H22A H 0.6835 -0.3756 0.238 0.027 Uiso 1 1 calc R . . H22B H 0.8541 -0.4356 0.2314 0.027 Uiso 1 1 calc R . . H22C H 0.744 -0.5128 0.2728 0.027 Uiso 1 1 calc R . . C231 C 0.8058(3) -0.2379(3) 0.00054(14) 0.0135(6) Uani 1 1 d . . . C232 C 0.6701(4) -0.1804(3) -0.02903(16) 0.0150(7) Uani 1 1 d . . . C233 C 0.6685(4) -0.1388(3) -0.09946(15) 0.0198(7) Uani 1 1 d . . . H233 H 0.5777 -0.0999 -0.1202 0.024 Uiso 1 1 calc R . . C234 C 0.7940(4) -0.1523(3) -0.13980(16) 0.0218(7) Uani 1 1 d . . . H234 H 0.7895 -0.1225 -0.1875 0.026 Uiso 1 1 calc R . . C235 C 0.9272(4) -0.2097(3) -0.11027(16) 0.0207(7) Uani 1 1 d . . . H235 H 1.0145 -0.2196 -0.1377 0.025 Uiso 1 1 calc R . . C236 C 0.9326(3) -0.2526(3) -0.04047(15) 0.0169(7) Uani 1 1 d . . . H236 H 1.0238 -0.2925 -0.0204 0.02 Uiso 1 1 calc R . . C237 C 0.5280(3) -0.1658(3) 0.01221(16) 0.0199(7) Uani 1 1 d . . . H23A H 0.446 -0.129 -0.0184 0.03 Uiso 1 1 calc R . . H23B H 0.5318 -0.1129 0.0474 0.03 Uiso 1 1 calc R . . H23C H 0.5141 -0.2462 0.0344 0.03 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 0.01723(14) 0.02034(15) 0.02054(15) -0.00947(12) 0.00307(11) -0.00158(11) Ag2 0.01979(14) 0.01632(15) 0.01819(14) -0.00600(11) 0.00328(11) -0.00034(11) S1 0.0193(4) 0.0170(4) 0.0231(5) -0.0053(4) 0.0060(3) -0.0052(4) C1 0.0164(17) 0.0093(16) 0.0186(17) 0.0006(14) -0.0064(14) -0.0034(13) N1 0.0178(15) 0.0162(16) 0.0255(17) -0.0090(13) 0.0017(13) -0.0040(12) S2 0.0254(5) 0.0343(6) 0.0652(7) -0.0328(5) 0.0239(5) -0.0158(4) C2 0.0217(19) 0.021(2) 0.028(2) -0.0091(16) 0.0036(15) -0.0132(16) N2 0.0229(17) 0.0272(19) 0.039(2) -0.0181(16) 0.0109(15) -0.0099(14) P1 0.0108(4) 0.0131(5) 0.0127(4) -0.0043(4) 0.0008(3) -0.0031(3) C111 0.0107(15) 0.0088(15) 0.0159(16) -0.0014(12) 0.0000(12) -0.0005(12) C112 0.0137(16) 0.0082(16) 0.0204(17) -0.0042(13) -0.0007(13) -0.0007(13) C113 0.0155(16) 0.0107(16) 0.0281(19) -0.0059(14) -0.0065(14) -0.0018(13) C114 0.0124(15) 0.0124(16) 0.0306(19) -0.0037(14) 0.0054(13) -0.0062(13) C115 0.0189(17) 0.0128(16) 0.0162(16) 0.0006(13) 0.0060(13) -0.0037(13) C116 0.0169(16) 0.0132(16) 0.0126(15) -0.0030(12) -0.0003(12) -0.0030(13) C117 0.0176(17) 0.0201(18) 0.0201(17) -0.0078(14) -0.0042(13) -0.0005(14) C121 0.0147(15) 0.0156(16) 0.0082(14) -0.0036(12) -0.0014(11) -0.0041(13) C122 0.0178(17) 0.0218(19) 0.0092(16) -0.0091(14) 0.0000(13) -0.0049(14) C123 0.0257(18) 0.0199(18) 0.0103(15) -0.0044(13) 0.0009(13) -0.0096(14) C124 0.0300(19) 0.0134(17) 0.0160(16) -0.0022(13) -0.0067(14) -0.0041(14) C125 0.0184(17) 0.0172(17) 0.0209(17) -0.0074(14) -0.0065(13) 0.0017(14) C126 0.0183(16) 0.0169(17) 0.0130(15) -0.0063(13) 0.0008(12) -0.0040(13) C127 0.0168(17) 0.0243(18) 0.0204(17) -0.0048(14) 0.0066(13) -0.0058(14) C131 0.0083(14) 0.0165(16) 0.0103(14) -0.0042(12) 0.0015(11) -0.0019(12) C132 0.0097(15) 0.0165(19) 0.0181(18) -0.0074(15) 0.0032(13) -0.0015(14) C133 0.0133(16) 0.0149(17) 0.0175(16) 0.0019(13) -0.0006(12) -0.0009(13) C134 0.0152(16) 0.0237(18) 0.0147(16) -0.0032(14) -0.0026(12) -0.0030(14) C135 0.0160(16) 0.0177(17) 0.0187(17) -0.0054(14) 0.0012(13) -0.0050(13) C136 0.0099(15) 0.0139(16) 0.0156(16) 0.0004(13) -0.0007(12) 0.0001(12) C137 0.0263(19) 0.0142(17) 0.0256(19) 0.0003(14) -0.0074(15) -0.0022(14) P2 0.0106(4) 0.0121(5) 0.0113(4) -0.0029(4) 0.0009(3) -0.0015(3) C211 0.0096(14) 0.0192(17) 0.0101(15) -0.0019(13) 0.0012(11) 0.0008(13) C212 0.0169(17) 0.0220(19) 0.0120(16) -0.0048(14) 0.0016(13) -0.0049(14) C213 0.0140(16) 0.032(2) 0.0145(17) -0.0070(15) 0.0024(12) -0.0098(15) C214 0.0126(16) 0.043(2) 0.0148(17) -0.0075(15) -0.0011(13) -0.0018(16) C215 0.0168(17) 0.0278(19) 0.0162(17) -0.0037(14) -0.0001(13) 0.0037(15) C216 0.0155(16) 0.0212(18) 0.0150(16) -0.0057(13) 0.0006(12) -0.0046(14) C217 0.0241(19) 0.0215(19) 0.036(2) -0.0056(16) 0.0042(15) -0.0117(15) C221 0.0073(14) 0.0108(15) 0.0170(16) -0.0024(12) -0.0001(11) 0.0005(12) C222 0.0109(15) 0.0096(16) 0.0159(17) 0.0004(13) -0.0019(12) -0.0001(12) C223 0.0122(15) 0.0197(17) 0.0136(16) 0.0002(13) 0.0045(12) -0.0010(13) C224 0.0151(16) 0.0131(16) 0.0261(18) -0.0040(14) -0.0018(13) -0.0027(13) C225 0.0206(17) 0.0213(18) 0.0155(16) -0.0090(14) -0.0043(13) -0.0025(14) C226 0.0136(15) 0.0152(16) 0.0130(15) -0.0021(13) 0.0013(12) -0.0002(13) C227 0.0193(17) 0.0189(17) 0.0145(16) -0.0016(13) 0.0015(13) -0.0026(14) C231 0.0211(17) 0.0085(15) 0.0115(15) 0.0016(12) -0.0004(12) -0.0060(13) C232 0.0199(17) 0.0061(17) 0.0185(18) 0.0009(14) -0.0037(14) -0.0023(14) C233 0.0213(18) 0.0172(18) 0.0199(18) 0.0013(14) -0.0077(14) -0.0023(14) C234 0.031(2) 0.0196(18) 0.0154(17) -0.0004(14) -0.0018(14) -0.0082(15) C235 0.0252(18) 0.0170(17) 0.0193(17) -0.0021(14) 0.0094(14) -0.0054(14) C236 0.0196(17) 0.0138(16) 0.0172(16) -0.0021(13) -0.0011(13) -0.0031(13) C237 0.0153(16) 0.0206(18) 0.0222(17) -0.0007(14) -0.0049(13) -0.0002(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.200(3) . ? Ag1 P1 2.3986(9) . ? Ag1 S1 2.5637(9) . ? Ag2 N1 2.222(3) . ? Ag2 P2 2.4059(9) . ? Ag2 S2 2.5198(10) . ? S1 C1 1.661(4) . ? C1 N1 1.155(4) . ? S2 C2 1.645(4) . ? C2 N2 1.154(4) . ? P1 C111 1.825(3) . ? P1 C131 1.837(3) . ? P1 C121 1.839(3) . ? C111 C116 1.395(4) . ? C111 C112 1.412(4) . ? C112 C113 1.389(4) . ? C112 C117 1.502(4) . ? C113 C114 1.384(4) . ? C113 H113 0.95 . ? C114 C115 1.376(4) . ? C114 H114 0.95 . ? C115 C116 1.386(4) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C117 H11A 0.98 . ? C117 H11B 0.98 . ? C117 H11C 0.98 . ? C121 C126 1.398(4) . ? C121 C122 1.411(4) . ? C122 C123 1.395(4) . ? C122 C127 1.504(4) . ? C123 C124 1.386(4) . ? C123 H123 0.95 . ? C124 C125 1.379(4) . ? C124 H124 0.95 . ? C125 C126 1.388(4) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C127 H12A 0.98 . ? C127 H12B 0.98 . ? C127 H12C 0.98 . ? C131 C136 1.394(4) . ? C131 C132 1.406(4) . ? C132 C133 1.397(4) . ? C132 C137 1.510(4) . ? C133 C134 1.377(4) . ? C133 H133 0.95 . ? C134 C135 1.388(4) . ? C134 H134 0.95 . ? C135 C136 1.387(4) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C137 H13A 0.98 . ? C137 H13B 0.98 . ? C137 H13C 0.98 . ? P2 C221 1.835(3) . ? P2 C231 1.840(3) . ? P2 C211 1.840(3) . ? C211 C212 1.393(4) . ? C211 C216 1.403(4) . ? C212 C213 1.403(4) . ? C212 C217 1.511(4) . ? C213 C214 1.385(4) . ? C213 H213 0.95 . ? C214 C215 1.367(5) . ? C214 H214 0.95 . ? C215 C216 1.390(4) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C217 H21A 0.98 . ? C217 H21B 0.98 . ? C217 H21C 0.98 . ? C221 C226 1.388(4) . ? C221 C222 1.423(4) . ? C222 C223 1.387(4) . ? C222 C227 1.510(4) . ? C223 C224 1.387(4) . ? C223 H223 0.95 . ? C224 C225 1.386(4) . ? C224 H224 0.95 . ? C225 C226 1.375(4) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C227 H22A 0.98 . ? C227 H22B 0.98 . ? C227 H22C 0.98 . ? C231 C236 1.393(4) . ? C231 C232 1.407(4) . ? C232 C233 1.397(4) . ? C232 C237 1.511(4) . ? C233 C234 1.375(4) . ? C233 H233 0.95 . ? C234 C235 1.387(4) . ? C234 H234 0.95 . ? C235 C236 1.388(4) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? C237 H23A 0.98 . ? C237 H23B 0.98 . ? C237 H23C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 P1 138.33(8) . . ? N2 Ag1 S1 98.05(8) . . ? P1 Ag1 S1 123.57(3) . . ? N1 Ag2 P2 133.33(7) . . ? N1 Ag2 S2 100.27(7) . . ? P2 Ag2 S2 126.38(3) . . ? C1 S1 Ag1 99.71(11) . . ? N1 C1 S1 177.8(3) . . ? C1 N1 Ag2 156.4(3) . . ? C2 S2 Ag2 99.06(12) . . ? N2 C2 S2 177.2(4) . . ? C2 N2 Ag1 159.5(3) . . ? C111 P1 C131 106.25(13) . . ? C111 P1 C121 102.50(13) . . ? C131 P1 C121 104.49(13) . . ? C111 P1 Ag1 114.00(10) . . ? C131 P1 Ag1 110.91(10) . . ? C121 P1 Ag1 117.60(10) . . ? C116 C111 C112 119.8(3) . . ? C116 C111 P1 120.4(2) . . ? C112 C111 P1 119.7(2) . . ? C113 C112 C111 117.7(3) . . ? C113 C112 C117 119.9(3) . . ? C111 C112 C117 122.4(3) . . ? C114 C113 C112 122.1(3) . . ? C114 C113 H113 118.9 . . ? C112 C113 H113 118.9 . . ? C115 C114 C113 120.0(3) . . ? C115 C114 H114 120 . . ? C113 C114 H114 120 . . ? C114 C115 C116 119.5(3) . . ? C114 C115 H115 120.2 . . ? C116 C115 H115 120.2 . . ? C115 C116 C111 120.9(3) . . ? C115 C116 H116 119.5 . . ? C111 C116 H116 119.5 . . ? C112 C117 H11A 109.5 . . ? C112 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? C112 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? C126 C121 C122 119.1(3) . . ? C126 C121 P1 119.8(2) . . ? C122 C121 P1 121.1(2) . . ? C123 C122 C121 118.2(3) . . ? C123 C122 C127 119.3(3) . . ? C121 C122 C127 122.4(3) . . ? C124 C123 C122 121.9(3) . . ? C124 C123 H123 119 . . ? C122 C123 H123 119 . . ? C125 C124 C123 119.8(3) . . ? C125 C124 H124 120.1 . . ? C123 C124 H124 120.1 . . ? C124 C125 C126 119.5(3) . . ? C124 C125 H125 120.3 . . ? C126 C125 H125 120.3 . . ? C125 C126 C121 121.4(3) . . ? C125 C126 H126 119.3 . . ? C121 C126 H126 119.3 . . ? C122 C127 H12A 109.5 . . ? C122 C127 H12B 109.5 . . ? H12A C127 H12B 109.5 . . ? C122 C127 H12C 109.5 . . ? H12A C127 H12C 109.5 . . ? H12B C127 H12C 109.5 . . ? C136 C131 C132 119.4(3) . . ? C136 C131 P1 119.9(2) . . ? C132 C131 P1 120.6(2) . . ? C133 C132 C131 118.7(3) . . ? C133 C132 C137 118.5(3) . . ? C131 C132 C137 122.8(3) . . ? C134 C133 C132 121.6(3) . . ? C134 C133 H133 119.2 . . ? C132 C133 H133 119.2 . . ? C133 C134 C135 119.6(3) . . ? C133 C134 H134 120.2 . . ? C135 C134 H134 120.2 . . ? C136 C135 C134 119.9(3) . . ? C136 C135 H135 120 . . ? C134 C135 H135 120 . . ? C135 C136 C131 120.8(3) . . ? C135 C136 H136 119.6 . . ? C131 C136 H136 119.6 . . ? C132 C137 H13A 109.5 . . ? C132 C137 H13B 109.5 . . ? H13A C137 H13B 109.5 . . ? C132 C137 H13C 109.5 . . ? H13A C137 H13C 109.5 . . ? H13B C137 H13C 109.5 . . ? C221 P2 C231 103.88(13) . . ? C221 P2 C211 105.27(14) . . ? C231 P2 C211 104.30(14) . . ? C221 P2 Ag2 113.55(10) . . ? C231 P2 Ag2 115.80(10) . . ? C211 P2 Ag2 112.92(10) . . ? C212 C211 C216 119.6(3) . . ? C212 C211 P2 120.8(2) . . ? C216 C211 P2 119.5(2) . . ? C211 C212 C213 118.6(3) . . ? C211 C212 C217 123.9(3) . . ? C213 C212 C217 117.5(3) . . ? C214 C213 C212 121.0(3) . . ? C214 C213 H213 119.5 . . ? C212 C213 H213 119.5 . . ? C215 C214 C213 120.5(3) . . ? C215 C214 H214 119.8 . . ? C213 C214 H214 119.8 . . ? C214 C215 C216 119.7(3) . . ? C214 C215 H215 120.2 . . ? C216 C215 H215 120.2 . . ? C215 C216 C211 120.7(3) . . ? C215 C216 H216 119.7 . . ? C211 C216 H216 119.7 . . ? C212 C217 H21A 109.5 . . ? C212 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? C212 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C226 C221 C222 118.9(3) . . ? C226 C221 P2 120.9(2) . . ? C222 C221 P2 120.1(2) . . ? C223 C222 C221 117.9(3) . . ? C223 C222 C227 119.8(3) . . ? C221 C222 C227 122.2(3) . . ? C224 C223 C222 122.0(3) . . ? C224 C223 H223 119 . . ? C222 C223 H223 119 . . ? C225 C224 C223 119.8(3) . . ? C225 C224 H224 120.1 . . ? C223 C224 H224 120.1 . . ? C226 C225 C224 119.1(3) . . ? C226 C225 H225 120.4 . . ? C224 C225 H225 120.4 . . ? C225 C226 C221 122.2(3) . . ? C225 C226 H226 118.9 . . ? C221 C226 H226 118.9 . . ? C222 C227 H22A 109.5 . . ? C222 C227 H22B 109.5 . . ? H22A C227 H22B 109.5 . . ? C222 C227 H22C 109.5 . . ? H22A C227 H22C 109.5 . . ? H22B C227 H22C 109.5 . . ? C236 C231 C232 119.8(3) . . ? C236 C231 P2 119.9(2) . . ? C232 C231 P2 120.3(2) . . ? C233 C232 C231 117.9(3) . . ? C233 C232 C237 119.8(3) . . ? C231 C232 C237 122.3(3) . . ? C234 C233 C232 122.2(3) . . ? C234 C233 H233 118.9 . . ? C232 C233 H233 118.9 . . ? C233 C234 C235 119.5(3) . . ? C233 C234 H234 120.3 . . ? C235 C234 H234 120.3 . . ? C234 C235 C236 119.7(3) . . ? C234 C235 H235 120.1 . . ? C236 C235 H235 120.1 . . ? C235 C236 C231 120.8(3) . . ? C235 C236 H236 119.6 . . ? C231 C236 H236 119.6 . . ? C232 C237 H23A 109.5 . . ? C232 C237 H23B 109.5 . . ? H23A C237 H23B 109.5 . . ? C232 C237 H23C 109.5 . . ? H23A C237 H23C 109.5 . . ? H23B C237 H23C 109.5 . . ? #===END