# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2267 data_gab9952b #Compound 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; mu-sulphatotetrakis(triphenylphosphine)disilver(I) dihydrate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H64 Ag2 O6 P4 S' _chemical_formula_weight 1396.91 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4953(4) _cell_length_b 13.3274(4) _cell_length_c 21.7824(6) _cell_angle_alpha 91.1910(10) _cell_angle_beta 95.3060(10) _cell_angle_gamma 118.2300(10) _cell_volume 3173.64(16) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description Colourless _exptl_crystal_colour Plate _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.6707 _exptl_absorpt_correction_T_max 0.8558 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30713 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 27.03 _reflns_number_total 13366 _reflns_number_gt 11528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+12.5289P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13366 _refine_ls_number_parameters 772 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.49546(3) 0.66553(3) 0.639834(15) 0.02844(9) Uani 1 d . . . Ag2 Ag 0.66520(3) 0.64234(3) 0.855135(16) 0.03041(9) Uani 1 d . . . S S 0.52041(10) 0.48416(9) 0.73834(5) 0.0296(2) Uani 1 d . . . P1 P 0.27831(10) 0.59243(10) 0.59422(5) 0.0266(2) Uani 1 d . . . P2 P 0.67635(10) 0.82821(9) 0.61193(5) 0.0251(2) Uani 1 d . . . P3 P 0.80157(10) 0.57616(10) 0.90697(5) 0.0272(2) Uani 1 d . . . P4 P 0.64122(10) 0.80758(10) 0.88426(5) 0.0269(2) Uani 1 d . . . O1 O 0.4529(4) 0.5040(4) 0.6852(2) 0.0693(14) Uani 1 d . . . O2 O 0.5228(4) 0.3777(3) 0.72319(18) 0.0477(9) Uani 1 d . . . O3 O 0.4627(4) 0.4765(3) 0.79490(19) 0.0569(11) Uani 1 d . . . O4 O 0.6476(3) 0.5805(3) 0.74895(15) 0.0398(8) Uani 1 d . . . C1 C 0.1584(4) 0.4631(4) 0.6221(2) 0.0306(9) Uani 1 d . . . C2 C 0.0578(4) 0.3828(4) 0.5827(2) 0.0350(10) Uani 1 d . . . H2B H 0.0524 0.3930 0.5397 0.042 Uiso 1 calc R . . C3 C -0.0347(4) 0.2877(4) 0.6060(3) 0.0423(12) Uani 1 d . . . H3B H -0.1026 0.2330 0.5790 0.051 Uiso 1 calc R . . C4 C -0.0270(5) 0.2735(4) 0.6692(3) 0.0449(13) Uani 1 d . . . H4A H -0.0916 0.2110 0.6856 0.054 Uiso 1 calc R . . C5 C 0.0750(6) 0.3507(5) 0.7080(3) 0.0571(16) Uani 1 d . . . H5A H 0.0816 0.3395 0.7509 0.069 Uiso 1 calc R . . C6 C 0.1680(5) 0.4444(4) 0.6844(2) 0.0443(12) Uani 1 d . . . H6A H 0.2385 0.4960 0.7110 0.053 Uiso 1 calc R . . C7 C 0.2194(4) 0.6950(4) 0.59449(19) 0.0272(9) Uani 1 d . . . C8 C 0.3035(4) 0.8111(4) 0.5957(2) 0.0314(9) Uani 1 d . . . H8A H 0.3886 0.8347 0.5991 0.038 Uiso 1 calc R . . C9 C 0.2631(5) 0.8929(4) 0.5920(2) 0.0366(10) Uani 1 d . . . H9A H 0.3207 0.9716 0.5924 0.044 Uiso 1 calc R . . C10 C 0.1398(5) 0.8591(4) 0.5877(2) 0.0409(11) Uani 1 d . . . H10A H 0.1126 0.9145 0.5846 0.049 Uiso 1 calc R . . C11 C 0.0553(5) 0.7442(5) 0.5879(3) 0.0468(13) Uani 1 d . . . H11A H -0.0295 0.7214 0.5856 0.056 Uiso 1 calc R . . C12 C 0.0948(4) 0.6624(4) 0.5914(2) 0.0380(11) Uani 1 d . . . H12A H 0.0367 0.5840 0.5918 0.046 Uiso 1 calc R . . C13 C 0.2690(4) 0.5554(4) 0.5118(2) 0.0267(9) Uani 1 d . . . C14 C 0.2168(4) 0.5936(4) 0.4645(2) 0.0327(10) Uani 1 d . . . H14A H 0.1792 0.6382 0.4746 0.039 Uiso 1 calc R . . C15 C 0.2196(5) 0.5670(4) 0.4034(2) 0.0387(11) Uani 1 d . . . H15A H 0.1829 0.5933 0.3721 0.046 Uiso 1 calc R . . C16 C 0.2742(5) 0.5033(4) 0.3865(2) 0.0424(12) Uani 1 d . . . H16A H 0.2766 0.4866 0.3442 0.051 Uiso 1 calc R . . C17 C 0.3259(5) 0.4641(4) 0.4333(3) 0.0462(13) Uani 1 d . . . H17A H 0.3626 0.4189 0.4226 0.055 Uiso 1 calc R . . C18 C 0.3246(5) 0.4898(4) 0.4950(3) 0.0398(11) Uani 1 d . . . H18A H 0.3613 0.4632 0.5262 0.048 Uiso 1 calc R . . C19 C 0.6533(4) 0.9541(4) 0.6143(2) 0.0269(9) Uani 1 d . . . C20 C 0.6272(4) 0.9870(4) 0.6697(2) 0.0360(10) Uani 1 d . . . H20A H 0.6268 0.9471 0.7054 0.043 Uiso 1 calc R . . C21 C 0.6016(5) 1.0780(4) 0.6734(2) 0.0402(11) Uani 1 d . . . H21A H 0.5850 1.1003 0.7115 0.048 Uiso 1 calc R . . C22 C 0.6004(5) 1.1358(4) 0.6216(3) 0.0402(11) Uani 1 d . . . H22A H 0.5822 1.1973 0.6242 0.048 Uiso 1 calc R . . C23 C 0.6256(5) 1.1040(4) 0.5660(2) 0.0406(11) Uani 1 d . . . H23A H 0.6243 1.1435 0.5303 0.049 Uiso 1 calc R . . C24 C 0.6531(4) 1.0138(4) 0.5622(2) 0.0354(10) Uani 1 d . . . H24A H 0.6717 0.9931 0.5242 0.043 Uiso 1 calc R . . C25 C 0.7021(4) 0.8097(4) 0.5319(2) 0.0277(9) Uani 1 d . . . C26 C 0.5999(4) 0.7523(4) 0.4873(2) 0.0337(10) Uani 1 d . . . H26A H 0.5203 0.7281 0.4988 0.040 Uiso 1 calc R . . C27 C 0.6134(5) 0.7303(4) 0.4262(2) 0.0379(11) Uani 1 d . . . H27A H 0.5436 0.6923 0.3964 0.046 Uiso 1 calc R . . C28 C 0.7295(5) 0.7644(4) 0.4096(2) 0.0404(11) Uani 1 d . . . H28A H 0.7395 0.7489 0.3683 0.048 Uiso 1 calc R . . C29 C 0.8311(5) 0.8212(5) 0.4531(2) 0.0426(12) Uani 1 d . . . H29A H 0.9104 0.8446 0.4414 0.051 Uiso 1 calc R . . C30 C 0.8183(4) 0.8446(4) 0.5141(2) 0.0362(10) Uani 1 d . . . H30A H 0.8887 0.8842 0.5434 0.043 Uiso 1 calc R . . C31 C 0.8249(4) 0.8748(4) 0.65751(19) 0.0264(9) Uani 1 d . . . C32 C 0.8415(4) 0.7962(4) 0.6933(2) 0.0346(10) Uani 1 d . . . H32A H 0.7760 0.7213 0.6950 0.041 Uiso 1 calc R . . C33 C 0.9559(5) 0.8293(5) 0.7263(2) 0.0425(12) Uani 1 d . . . H33A H 0.9676 0.7761 0.7505 0.051 Uiso 1 calc R . . C34 C 1.0511(5) 0.9368(5) 0.7246(2) 0.0457(13) Uani 1 d . . . H34A H 1.1280 0.9576 0.7474 0.055 Uiso 1 calc R . . C35 C 1.0355(4) 1.0162(5) 0.6892(2) 0.0409(12) Uani 1 d . . . H35A H 1.1013 1.0912 0.6881 0.049 Uiso 1 calc R . . C36 C 0.9225(4) 0.9844(4) 0.6556(2) 0.0330(10) Uani 1 d . . . H36A H 0.9117 1.0379 0.6312 0.040 Uiso 1 calc R . . C37 C 0.7850(4) 0.5555(4) 0.9892(2) 0.0282(9) Uani 1 d . . . C38 C 0.8822(4) 0.5917(4) 1.0354(2) 0.0339(10) Uani 1 d . . . H38A H 0.9636 0.6283 1.0249 0.041 Uiso 1 calc R . . C39 C 0.8624(5) 0.5751(4) 1.0969(2) 0.0392(11) Uani 1 d . . . H39A H 0.9300 0.6007 1.1281 0.047 Uiso 1 calc R . . C40 C 0.7441(5) 0.5213(4) 1.1131(2) 0.0401(11) Uani 1 d . . . H40A H 0.7306 0.5102 1.1552 0.048 Uiso 1 calc R . . C41 C 0.6464(5) 0.4842(5) 1.0677(3) 0.0444(12) Uani 1 d . . . H41A H 0.5655 0.4477 1.0788 0.053 Uiso 1 calc R . . C42 C 0.6649(4) 0.4998(4) 1.0052(2) 0.0386(11) Uani 1 d . . . H42A H 0.5970 0.4729 0.9741 0.046 Uiso 1 calc R . . C43 C 0.9626(4) 0.6830(4) 0.9054(2) 0.0294(9) Uani 1 d . . . C44 C 0.9915(5) 0.7966(4) 0.8971(2) 0.0364(10) Uani 1 d . . . H44A H 0.9278 0.8165 0.8912 0.044 Uiso 1 calc R . . C45 C 1.1129(5) 0.8809(4) 0.8974(2) 0.0434(12) Uani 1 d . . . H45A H 1.1315 0.9578 0.8918 0.052 Uiso 1 calc R . . C46 C 1.2065(5) 0.8522(5) 0.9060(3) 0.0482(13) Uani 1 d . . . H46A H 1.2892 0.9097 0.9069 0.058 Uiso 1 calc R . . C47 C 1.1791(5) 0.7394(5) 0.9133(3) 0.0511(14) Uani 1 d . . . H47A H 1.2428 0.7195 0.9182 0.061 Uiso 1 calc R . . C48 C 1.0578(4) 0.6558(4) 0.9132(2) 0.0395(11) Uani 1 d . . . H48A H 1.0396 0.5790 0.9186 0.047 Uiso 1 calc R . . C49 C 0.7943(4) 0.4442(4) 0.8757(2) 0.0288(9) Uani 1 d . . . C50 C 0.7798(5) 0.4252(4) 0.8114(2) 0.0396(11) Uani 1 d . . . H50A H 0.7716 0.4788 0.7859 0.048 Uiso 1 calc R . . C51 C 0.7773(6) 0.3287(5) 0.7845(3) 0.0514(14) Uani 1 d . . . H51A H 0.7679 0.3166 0.7407 0.062 Uiso 1 calc R . . C52 C 0.7884(5) 0.2503(5) 0.8212(3) 0.0484(13) Uani 1 d . . . H52A H 0.7873 0.1847 0.8026 0.058 Uiso 1 calc R . . C53 C 0.8010(4) 0.2666(4) 0.8845(3) 0.0400(11) Uani 1 d . . . H53A H 0.8083 0.2122 0.9095 0.048 Uiso 1 calc R . . C54 C 0.8029(4) 0.3633(4) 0.9122(2) 0.0348(10) Uani 1 d . . . H54A H 0.8102 0.3737 0.9560 0.042 Uiso 1 calc R . . C55 C 0.5322(4) 0.8343(4) 0.8351(2) 0.0297(9) Uani 1 d . . . C56 C 0.5367(5) 0.9413(4) 0.8357(2) 0.0363(10) Uani 1 d . . . H56A H 0.6009 1.0042 0.8605 0.044 Uiso 1 calc R . . C57 C 0.4471(5) 0.9556(5) 0.8000(2) 0.0426(12) Uani 1 d . . . H57A H 0.4497 1.0281 0.8006 0.051 Uiso 1 calc R . . C58 C 0.3539(5) 0.8637(6) 0.7634(3) 0.0508(14) Uani 1 d . . . H58A H 0.2927 0.8738 0.7394 0.061 Uiso 1 calc R . . C59 C 0.3490(5) 0.7586(5) 0.7616(2) 0.0479(13) Uani 1 d . . . H59A H 0.2848 0.6966 0.7363 0.057 Uiso 1 calc R . . C60 C 0.4385(4) 0.7422(4) 0.7971(2) 0.0368(11) Uani 1 d . . . H60A H 0.4359 0.6698 0.7954 0.044 Uiso 1 calc R . . C61 C 0.5979(4) 0.8072(4) 0.9623(2) 0.0301(9) Uani 1 d . . . C62 C 0.5176(5) 0.8464(4) 0.9784(2) 0.0382(11) Uani 1 d . . . H62A H 0.4829 0.8759 0.9479 0.046 Uiso 1 calc R . . C63 C 0.4885(5) 0.8423(5) 1.0385(3) 0.0487(13) Uani 1 d . . . H63A H 0.4348 0.8702 1.0492 0.058 Uiso 1 calc R . . C64 C 0.5372(6) 0.7980(5) 1.0832(3) 0.0543(15) Uani 1 d . . . H64A H 0.5158 0.7942 1.1241 0.065 Uiso 1 calc R . . C65 C 0.6165(6) 0.7594(5) 1.0680(3) 0.0517(14) Uani 1 d . . . H65A H 0.6511 0.7302 1.0988 0.062 Uiso 1 calc R . . C66 C 0.6462(5) 0.7629(5) 1.0082(2) 0.0407(11) Uani 1 d . . . H66A H 0.7002 0.7349 0.9982 0.049 Uiso 1 calc R . . C67 C 0.7864(4) 0.9402(4) 0.8865(2) 0.0288(9) Uani 1 d . . . C68 C 0.8356(5) 0.9750(4) 0.8312(2) 0.0400(11) Uani 1 d . . . H68A H 0.7905 0.9338 0.7933 0.048 Uiso 1 calc R . . C69 C 0.9509(5) 1.0700(5) 0.8310(3) 0.0473(13) Uani 1 d . . . H69A H 0.9826 1.0941 0.7928 0.057 Uiso 1 calc R . . C70 C 1.0189(5) 1.1293(4) 0.8857(3) 0.0442(12) Uani 1 d . . . H70A H 1.0983 1.1924 0.8855 0.053 Uiso 1 calc R . . C71 C 0.9703(5) 1.0958(5) 0.9409(3) 0.0482(13) Uani 1 d . . . H71A H 1.0161 1.1368 0.9787 0.058 Uiso 1 calc R . . C72 C 0.8546(5) 1.0023(4) 0.9415(2) 0.0383(11) Uani 1 d . . . H72A H 0.8219 0.9806 0.9796 0.046 Uiso 1 calc R . . O5 C 0.3796(5) 0.1509(4) 0.7341(3) 0.0407(12) Uani 1 d D . . H5B H 0.438(4) 0.202(4) 0.753(2) 0.049 Uiso 1 d D . . O6 C 0.2474(4) 0.2600(4) 0.7916(2) 0.0326(10) Uani 1 d D . . H6B H 0.272(5) 0.220(4) 0.780(2) 0.039 Uiso 1 d 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 0.02497(16) 0.02833(17) 0.03042(17) 0.00336(13) 0.00229(13) 0.01153(13) Ag2 0.03412(18) 0.03082(18) 0.03022(18) -0.00236(13) -0.00195(14) 0.01986(15) S 0.0323(6) 0.0255(5) 0.0278(5) 0.0043(4) 0.0019(4) 0.0115(4) P1 0.0216(5) 0.0275(6) 0.0300(6) 0.0048(4) 0.0009(4) 0.0115(4) P2 0.0233(5) 0.0253(5) 0.0255(5) 0.0017(4) 0.0032(4) 0.0106(4) P3 0.0286(5) 0.0282(6) 0.0279(6) 0.0002(4) -0.0002(4) 0.0168(5) P4 0.0309(6) 0.0268(6) 0.0262(5) -0.0003(4) 0.0010(4) 0.0168(5) O1 0.055(2) 0.049(2) 0.082(3) 0.026(2) -0.027(2) 0.011(2) O2 0.054(2) 0.038(2) 0.054(2) -0.0021(17) 0.0116(18) 0.0228(18) O3 0.057(2) 0.039(2) 0.060(3) -0.0072(18) 0.033(2) 0.0071(18) O4 0.0361(18) 0.0378(19) 0.0317(18) 0.0005(14) 0.0039(14) 0.0065(15) C1 0.026(2) 0.027(2) 0.040(3) 0.0082(19) 0.0060(19) 0.0132(18) C2 0.030(2) 0.033(2) 0.042(3) 0.008(2) 0.002(2) 0.014(2) C3 0.025(2) 0.032(3) 0.065(4) 0.007(2) 0.004(2) 0.010(2) C4 0.038(3) 0.034(3) 0.065(4) 0.017(2) 0.022(3) 0.015(2) C5 0.068(4) 0.051(3) 0.044(3) 0.016(3) 0.020(3) 0.018(3) C6 0.047(3) 0.037(3) 0.038(3) 0.008(2) 0.006(2) 0.010(2) C7 0.030(2) 0.029(2) 0.025(2) 0.0032(17) 0.0034(17) 0.0157(18) C8 0.028(2) 0.032(2) 0.033(2) 0.0031(19) 0.0024(18) 0.0134(19) C9 0.044(3) 0.029(2) 0.036(3) 0.0027(19) 0.004(2) 0.017(2) C10 0.052(3) 0.041(3) 0.041(3) -0.001(2) 0.004(2) 0.032(3) C11 0.034(3) 0.049(3) 0.064(4) 0.003(3) 0.008(2) 0.025(2) C12 0.028(2) 0.034(3) 0.050(3) -0.003(2) 0.006(2) 0.013(2) C13 0.0211(19) 0.023(2) 0.033(2) 0.0022(17) 0.0047(17) 0.0077(16) C14 0.031(2) 0.034(2) 0.036(2) 0.0025(19) 0.0043(19) 0.018(2) C15 0.042(3) 0.039(3) 0.036(3) 0.005(2) 0.008(2) 0.020(2) C16 0.043(3) 0.035(3) 0.042(3) -0.004(2) 0.014(2) 0.012(2) C17 0.052(3) 0.034(3) 0.061(4) 0.003(2) 0.024(3) 0.024(2) C18 0.040(3) 0.033(3) 0.055(3) 0.009(2) 0.011(2) 0.023(2) C19 0.0210(19) 0.025(2) 0.033(2) 0.0012(17) 0.0011(17) 0.0100(17) C20 0.041(3) 0.037(3) 0.031(2) 0.005(2) 0.006(2) 0.019(2) C21 0.044(3) 0.036(3) 0.043(3) -0.001(2) 0.010(2) 0.020(2) C22 0.038(3) 0.030(2) 0.055(3) 0.002(2) 0.007(2) 0.018(2) C23 0.048(3) 0.034(3) 0.043(3) 0.014(2) 0.008(2) 0.022(2) C24 0.040(3) 0.036(3) 0.031(2) 0.008(2) 0.010(2) 0.018(2) C25 0.032(2) 0.026(2) 0.025(2) 0.0016(17) 0.0055(17) 0.0134(18) C26 0.031(2) 0.037(3) 0.032(2) 0.0025(19) 0.0028(19) 0.015(2) C27 0.045(3) 0.036(3) 0.030(2) -0.001(2) 0.000(2) 0.018(2) C28 0.056(3) 0.040(3) 0.028(2) 0.004(2) 0.013(2) 0.025(2) C29 0.043(3) 0.052(3) 0.041(3) 0.006(2) 0.019(2) 0.026(3) C30 0.031(2) 0.042(3) 0.033(2) -0.001(2) 0.0052(19) 0.016(2) C31 0.026(2) 0.028(2) 0.024(2) 0.0007(16) 0.0025(16) 0.0124(18) C32 0.040(3) 0.034(2) 0.029(2) 0.0040(19) 0.0038(19) 0.018(2) C33 0.048(3) 0.055(3) 0.034(3) 0.005(2) 0.001(2) 0.033(3) C34 0.035(3) 0.062(4) 0.038(3) -0.004(2) -0.006(2) 0.024(3) C35 0.026(2) 0.046(3) 0.039(3) -0.005(2) -0.001(2) 0.009(2) C36 0.033(2) 0.030(2) 0.035(2) 0.0025(19) 0.0042(19) 0.014(2) C37 0.033(2) 0.021(2) 0.033(2) 0.0027(17) 0.0054(18) 0.0152(18) C38 0.030(2) 0.036(3) 0.035(2) 0.001(2) 0.0042(19) 0.015(2) C39 0.045(3) 0.042(3) 0.029(2) 0.000(2) 0.002(2) 0.020(2) C40 0.055(3) 0.036(3) 0.034(3) 0.009(2) 0.018(2) 0.023(2) C41 0.037(3) 0.043(3) 0.050(3) 0.011(2) 0.018(2) 0.013(2) C42 0.031(2) 0.039(3) 0.039(3) 0.005(2) 0.006(2) 0.011(2) C43 0.032(2) 0.032(2) 0.024(2) 0.0015(17) 0.0049(17) 0.0154(19) C44 0.041(3) 0.035(3) 0.036(3) 0.003(2) 0.004(2) 0.020(2) C45 0.046(3) 0.033(3) 0.044(3) 0.006(2) 0.008(2) 0.013(2) C46 0.035(3) 0.049(3) 0.048(3) 0.002(3) 0.010(2) 0.010(2) C47 0.037(3) 0.057(4) 0.063(4) 0.004(3) 0.011(3) 0.024(3) C48 0.036(3) 0.038(3) 0.051(3) 0.006(2) 0.008(2) 0.022(2) C49 0.026(2) 0.029(2) 0.034(2) 0.0008(18) 0.0010(18) 0.0156(18) C50 0.055(3) 0.036(3) 0.034(3) -0.003(2) -0.002(2) 0.028(2) C51 0.073(4) 0.050(3) 0.039(3) -0.006(2) 0.000(3) 0.038(3) C52 0.050(3) 0.038(3) 0.062(4) -0.009(3) 0.002(3) 0.027(3) C53 0.035(3) 0.030(2) 0.057(3) 0.005(2) -0.001(2) 0.018(2) C54 0.035(2) 0.033(2) 0.038(3) 0.002(2) 0.001(2) 0.019(2) C55 0.038(2) 0.030(2) 0.029(2) 0.0053(18) 0.0069(19) 0.022(2) C56 0.046(3) 0.036(3) 0.035(2) 0.006(2) 0.009(2) 0.024(2) C57 0.060(3) 0.052(3) 0.036(3) 0.014(2) 0.015(2) 0.041(3) C58 0.055(3) 0.078(4) 0.040(3) 0.012(3) 0.005(3) 0.049(3) C59 0.044(3) 0.064(4) 0.037(3) -0.001(3) -0.007(2) 0.030(3) C60 0.041(3) 0.040(3) 0.032(2) 0.001(2) -0.002(2) 0.022(2) C61 0.032(2) 0.029(2) 0.027(2) 0.0001(17) 0.0016(18) 0.0130(19) C62 0.039(3) 0.039(3) 0.041(3) 0.003(2) 0.010(2) 0.020(2) C63 0.053(3) 0.052(3) 0.046(3) 0.001(3) 0.022(3) 0.026(3) C64 0.063(4) 0.057(4) 0.035(3) -0.001(3) 0.016(3) 0.021(3) C65 0.065(4) 0.056(4) 0.034(3) 0.004(2) 0.000(3) 0.029(3) C66 0.043(3) 0.049(3) 0.035(3) 0.007(2) 0.002(2) 0.026(2) C67 0.031(2) 0.027(2) 0.032(2) 0.0039(18) 0.0059(18) 0.0169(19) C68 0.048(3) 0.043(3) 0.031(2) 0.001(2) 0.008(2) 0.023(2) C69 0.054(3) 0.042(3) 0.054(3) 0.010(3) 0.026(3) 0.025(3) C70 0.039(3) 0.034(3) 0.062(4) 0.005(2) 0.013(3) 0.017(2) C71 0.046(3) 0.038(3) 0.047(3) -0.002(2) 0.002(2) 0.010(2) C72 0.041(3) 0.035(3) 0.034(3) 0.002(2) 0.009(2) 0.013(2) O5 0.044(3) 0.022(2) 0.057(3) 0.013(2) 0.009(2) 0.015(2) O6 0.024(2) 0.029(2) 0.038(3) 0.0066(19) 0.0106(19) 0.0063(18) _geom_special_details ; ? ; 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 O1 2.235(4) . y Ag1 P2 2.4190(11) . y Ag1 P1 2.5018(11) . y Ag2 O4 2.394(3) . y Ag2 P4 2.4380(11) . y Ag2 P3 2.4625(11) . y Ag2 O3 2.643(4) . y S O2 1.464(4) . y S O3 1.466(4) . y S O1 1.472(4) . y S O4 1.489(3) . y P1 C13 1.831(5) . y P1 C1 1.831(4) . y P1 C7 1.834(4) . y P2 C19 1.833(4) . y P2 C31 1.833(4) . y P2 C25 1.835(4) . y P3 C49 1.830(5) . y P3 C37 1.833(5) . y P3 C43 1.839(5) . y P4 C55 1.826(4) . y P4 C61 1.830(5) . y P4 C67 1.834(5) . y C1 C6 1.388(7) . ? C1 C2 1.397(7) . ? C2 C3 1.397(7) . ? C3 C4 1.394(8) . ? C4 C5 1.386(8) . ? C5 C6 1.393(7) . ? C7 C8 1.398(6) . ? C7 C12 1.399(6) . ? C8 C9 1.403(6) . ? C9 C10 1.378(7) . ? C10 C11 1.390(8) . ? C11 C12 1.394(7) . ? C13 C14 1.398(6) . ? C13 C18 1.411(6) . ? C14 C15 1.377(7) . ? C15 C16 1.381(7) . ? C16 C17 1.397(8) . ? C17 C18 1.384(8) . ? C19 C20 1.394(6) . ? C19 C24 1.399(6) . ? C20 C21 1.395(7) . ? C21 C22 1.380(7) . ? C22 C23 1.388(7) . ? C23 C24 1.401(7) . ? C25 C30 1.396(6) . ? C25 C26 1.405(6) . ? C26 C27 1.398(7) . ? C27 C28 1.388(7) . ? C28 C29 1.386(8) . ? C29 C30 1.398(7) . ? C31 C36 1.397(6) . ? C31 C32 1.399(6) . ? C32 C33 1.398(7) . ? C33 C34 1.367(8) . ? C34 C35 1.397(8) . ? C35 C36 1.392(7) . ? C37 C38 1.386(6) . ? C37 C42 1.407(6) . ? C38 C39 1.388(7) . ? C39 C40 1.388(7) . ? C40 C41 1.377(8) . ? C41 C42 1.405(7) . ? C43 C48 1.396(6) . ? C43 C44 1.400(7) . ? C44 C45 1.396(7) . ? C45 C46 1.391(8) . ? C46 C47 1.391(8) . ? C47 C48 1.393(7) . ? C49 C54 1.391(6) . ? C49 C50 1.398(7) . ? C50 C51 1.389(7) . ? C51 C52 1.378(8) . ? C52 C53 1.376(8) . ? C53 C54 1.400(7) . ? C55 C56 1.401(6) . ? C55 C60 1.407(7) . ? C56 C57 1.394(7) . ? C57 C58 1.388(8) . ? C58 C59 1.373(8) . ? C59 C60 1.405(7) . ? C61 C62 1.398(7) . ? C61 C66 1.401(6) . ? C62 C63 1.388(7) . ? C63 C64 1.386(9) . ? C64 C65 1.376(9) . ? C65 C66 1.382(7) . ? C67 C68 1.391(6) . ? C67 C72 1.395(7) . ? C68 C69 1.398(8) . ? C69 C70 1.382(8) . ? C70 C71 1.383(8) . ? C71 C72 1.393(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 O1 Ag1 P2 136.65(12) . . y O1 Ag1 P1 92.81(11) . . y P2 Ag1 P1 128.04(4) . . y O4 Ag2 P4 121.36(9) . . y O4 Ag2 P3 102.97(9) . . y P4 Ag2 P3 128.60(4) . . y O4 Ag2 O3 56.42(11) . . y P4 Ag2 O3 112.04(10) . . y P3 Ag2 O3 113.73(10) . . y O2 S O3 110.6(2) . . y O2 S O1 107.4(3) . . y O3 S O1 111.4(3) . . y O2 S O4 109.8(2) . . y O3 S O4 108.0(2) . . y O1 S O4 109.7(2) . . y C13 P1 C1 104.0(2) . . y C13 P1 C7 103.20(19) . . y C1 P1 C7 104.8(2) . . y C13 P1 Ag1 107.61(14) . . y C1 P1 Ag1 119.13(15) . . y C7 P1 Ag1 116.35(15) . . y C19 P2 C31 104.6(2) . . y C19 P2 C25 105.0(2) . . y C31 P2 C25 105.0(2) . . y C19 P2 Ag1 109.07(14) . . y C31 P2 Ag1 120.19(14) . . y C25 P2 Ag1 111.75(14) . . y C49 P3 C37 104.4(2) . . y C49 P3 C43 103.5(2) . . y C37 P3 C43 104.7(2) . . y C49 P3 Ag2 118.52(14) . . y C37 P3 Ag2 113.87(14) . . y C43 P3 Ag2 110.51(15) . . y C55 P4 C61 104.7(2) . . y C55 P4 C67 104.5(2) . . y C61 P4 C67 103.7(2) . . y C55 P4 Ag2 117.80(15) . . y C61 P4 Ag2 113.67(15) . . y C67 P4 Ag2 111.13(14) . . y S O1 Ag1 129.6(2) . . y S O3 Ag2 92.79(18) . . y S O4 Ag2 102.63(17) . . y C6 C1 C2 119.1(4) . . ? C6 C1 P1 118.9(4) . . ? C2 C1 P1 122.0(4) . . ? C1 C2 C3 120.5(5) . . ? C4 C3 C2 119.6(5) . . ? C5 C4 C3 119.9(5) . . ? C4 C5 C6 120.1(5) . . ? C1 C6 C5 120.6(5) . . ? C8 C7 C12 118.8(4) . . ? C8 C7 P1 117.9(3) . . ? C12 C7 P1 123.2(4) . . ? C7 C8 C9 120.4(4) . . ? C10 C9 C8 120.0(5) . . ? C9 C10 C11 120.2(5) . . ? C10 C11 C12 120.1(5) . . ? C11 C12 C7 120.4(5) . . ? C14 C13 C18 118.1(4) . . ? C14 C13 P1 124.2(3) . . ? C18 C13 P1 117.5(4) . . ? C15 C14 C13 120.6(4) . . ? C14 C15 C16 121.8(5) . . ? C15 C16 C17 118.1(5) . . ? C18 C17 C16 121.2(5) . . ? C17 C18 C13 120.1(5) . . ? C20 C19 C24 118.8(4) . . ? C20 C19 P2 118.1(3) . . ? C24 C19 P2 123.0(3) . . ? C19 C20 C21 120.7(4) . . ? C22 C21 C20 120.2(5) . . ? C21 C22 C23 120.0(5) . . ? C22 C23 C24 120.1(5) . . ? C19 C24 C23 120.2(4) . . ? C30 C25 C26 118.6(4) . . ? C30 C25 P2 122.8(3) . . ? C26 C25 P2 118.5(3) . . ? C27 C26 C25 121.2(4) . . ? C28 C27 C26 119.4(5) . . ? C29 C28 C27 120.0(4) . . ? C28 C29 C30 120.8(5) . . ? C25 C30 C29 120.0(5) . . ? C36 C31 C32 119.4(4) . . ? C36 C31 P2 121.9(3) . . ? C32 C31 P2 118.6(3) . . ? C33 C32 C31 119.1(5) . . ? C34 C33 C32 121.3(5) . . ? C33 C34 C35 120.1(5) . . ? C36 C35 C34 119.4(5) . . ? C35 C36 C31 120.7(5) . . ? C38 C37 C42 119.1(4) . . ? C38 C37 P3 124.3(3) . . ? C42 C37 P3 116.6(4) . . ? C37 C38 C39 120.9(4) . . ? C40 C39 C38 120.2(5) . . ? C41 C40 C39 119.6(5) . . ? C40 C41 C42 120.9(5) . . ? C41 C42 C37 119.2(5) . . ? C48 C43 C44 118.5(4) . . ? C48 C43 P3 122.6(4) . . ? C44 C43 P3 118.9(4) . . ? C45 C44 C43 120.8(5) . . ? C46 C45 C44 119.8(5) . . ? C45 C46 C47 120.1(5) . . ? C46 C47 C48 119.8(5) . . ? C47 C48 C43 121.1(5) . . ? C54 C49 C50 118.9(4) . . ? C54 C49 P3 123.8(4) . . ? C50 C49 P3 117.3(3) . . ? C51 C50 C49 120.5(5) . . ? C52 C51 C50 120.0(5) . . ? C53 C52 C51 120.3(5) . . ? C52 C53 C54 120.2(5) . . ? C49 C54 C53 120.1(5) . . ? C56 C55 C60 119.6(4) . . ? C56 C55 P4 122.3(4) . . ? C60 C55 P4 118.1(3) . . ? C57 C56 C55 120.0(5) . . ? C58 C57 C56 119.9(5) . . ? C59 C58 C57 120.9(5) . . ? C58 C59 C60 120.3(5) . . ? C59 C60 C55 119.3(5) . . ? C62 C61 C66 118.2(4) . . ? C62 C61 P4 123.7(4) . . ? C66 C61 P4 118.0(4) . . ? C63 C62 C61 120.3(5) . . ? C64 C63 C62 120.5(5) . . ? C65 C64 C63 119.8(5) . . ? C64 C65 C66 120.3(5) . . ? C65 C66 C61 120.9(5) . . ? C68 C67 C72 118.5(4) . . ? C68 C67 P4 118.2(4) . . ? C72 C67 P4 123.1(4) . . ? C67 C68 C69 120.5(5) . . ? C70 C69 C68 120.5(5) . . ? C69 C70 C71 119.3(5) . . ? C70 C71 C72 120.5(5) . . ? C71 C72 C67 120.6(5) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.043 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.094 #===END data_gab9964 #Compound 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; mu-selenatotetra(triphenylphosphine)disilver(I) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H64 Ag2 O6 P4 Se' _chemical_formula_weight 1443.81 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' 'O' 'O' 0.0106 0.0060 '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.46450(10) _cell_length_b 13.264 _cell_length_c 21.85890(10) _cell_angle_alpha 91.5060(10) _cell_angle_beta 95.2500(10) _cell_angle_gamma 117.95 _cell_volume 3169.14(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.5301 _exptl_absorpt_correction_T_max 0.7745 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30330 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.05 _reflns_number_total 13379 _reflns_number_gt 11996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+1.3760P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13379 _refine_ls_number_parameters 774 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.009 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.497111(11) 0.668611(11) 0.639383(6) 0.02778(4) Uani 1 d . . . Ag2 Ag 0.666931(12) 0.641888(11) 0.856438(6) 0.02982(4) Uani 1 d . . . Se Se 0.523300(16) 0.476488(14) 0.738011(8) 0.02745(4) Uani 1 d . . . P1 P 0.27962(4) 0.59553(4) 0.59462(2) 0.02647(9) Uani 1 d . . . P2 P 0.67693(4) 0.83208(4) 0.61282(2) 0.02427(9) Uani 1 d . . . P3 P 0.80479(4) 0.57691(4) 0.90789(2) 0.02657(9) Uani 1 d . . . P4 P 0.64097(4) 0.80659(4) 0.88517(2) 0.02673(9) Uani 1 d . . . O1 O 0.44855(15) 0.50188(13) 0.67999(8) 0.0605(5) Uani 1 d . . . O2 O 0.52653(14) 0.35830(12) 0.71978(7) 0.0433(3) Uani 1 d . . . O3 O 0.46080(14) 0.47047(13) 0.80155(7) 0.0508(4) Uani 1 d . . . O4 O 0.66356(12) 0.58387(11) 0.75093(6) 0.0362(3) Uani 1 d . . . C1 C 0.16015(15) 0.46653(15) 0.62244(9) 0.0289(4) Uani 1 d . . . C2 C 0.06025(17) 0.38569(16) 0.58343(10) 0.0364(4) Uani 1 d . . . H2B H 0.0544 0.3949 0.5405 0.044 Uiso 1 calc R . . C3 C -0.03112(18) 0.29131(17) 0.60702(11) 0.0431(5) Uani 1 d . . . H3B H -0.0989 0.2361 0.5801 0.052 Uiso 1 calc R . . C4 C -0.0238(2) 0.27762(18) 0.66936(12) 0.0462(5) Uani 1 d . . . H4A H -0.0883 0.2152 0.6856 0.055 Uiso 1 calc R . . C5 C 0.0775(2) 0.3548(2) 0.70814(11) 0.0551(6) Uani 1 d . . . H5A H 0.0840 0.3438 0.7508 0.066 Uiso 1 calc R . . C6 C 0.1702(2) 0.44889(19) 0.68470(10) 0.0450(5) Uani 1 d . . . H6A H 0.2405 0.5011 0.7113 0.054 Uiso 1 calc R . . C7 C 0.22091(15) 0.69881(15) 0.59454(8) 0.0263(3) Uani 1 d . . . C8 C 0.30473(17) 0.81467(16) 0.59536(8) 0.0317(4) Uani 1 d . . . H8A H 0.3898 0.8380 0.5988 0.038 Uiso 1 calc R . . C9 C 0.26475(19) 0.89629(17) 0.59111(9) 0.0377(4) Uani 1 d . . . H9A H 0.3225 0.9750 0.5913 0.045 Uiso 1 calc R . . C10 C 0.1415(2) 0.86333(18) 0.58660(10) 0.0417(5) Uani 1 d . . . H10A H 0.1143 0.9192 0.5835 0.050 Uiso 1 calc R . . C11 C 0.05729(19) 0.74849(19) 0.58664(11) 0.0469(5) Uani 1 d . . . H11A H -0.0276 0.7259 0.5839 0.056 Uiso 1 calc R . . C12 C 0.09643(17) 0.66686(17) 0.59070(10) 0.0376(4) Uani 1 d . . . H12A H 0.0382 0.5884 0.5909 0.045 Uiso 1 calc R . . C13 C 0.27017(15) 0.55630(14) 0.51277(8) 0.0272(3) Uani 1 d . . . C14 C 0.21564(17) 0.59272(16) 0.46608(9) 0.0316(4) Uani 1 d . . . H14A H 0.1781 0.6378 0.4765 0.038 Uiso 1 calc R . . C15 C 0.21559(19) 0.56370(17) 0.40434(9) 0.0383(4) Uani 1 d . . . H15A H 0.1778 0.5886 0.3729 0.046 Uiso 1 calc R . . C16 C 0.27071(19) 0.49851(17) 0.38879(10) 0.0423(5) Uani 1 d . . . H16A H 0.2712 0.4789 0.3467 0.051 Uiso 1 calc R . . C17 C 0.3248(2) 0.46228(18) 0.43484(11) 0.0464(5) Uani 1 d . . . H17A H 0.3622 0.4172 0.4241 0.056 Uiso 1 calc R . . C18 C 0.32573(19) 0.49049(17) 0.49641(10) 0.0396(4) Uani 1 d . . . H18A H 0.3639 0.4653 0.5275 0.048 Uiso 1 calc R . . C19 C 0.65437(15) 0.95877(14) 0.61550(8) 0.0263(3) Uani 1 d . . . C20 C 0.62891(18) 0.99207(16) 0.67134(9) 0.0338(4) Uani 1 d . . . H20A H 0.6284 0.9517 0.7067 0.041 Uiso 1 calc R . . C21 C 0.60437(19) 1.08368(17) 0.67540(10) 0.0394(4) Uani 1 d . . . H21A H 0.5884 1.1064 0.7136 0.047 Uiso 1 calc R . . C22 C 0.60311(18) 1.14194(17) 0.62416(10) 0.0401(5) Uani 1 d . . . H22A H 0.5865 1.2048 0.6271 0.048 Uiso 1 calc R . . C23 C 0.6261(2) 1.10855(17) 0.56860(10) 0.0417(5) Uani 1 d . . . H23A H 0.6240 1.1478 0.5332 0.050 Uiso 1 calc R . . C24 C 0.65232(18) 1.01764(16) 0.56421(9) 0.0346(4) Uani 1 d . . . H24A H 0.6689 0.9958 0.5259 0.041 Uiso 1 calc R . . C25 C 0.70223(15) 0.81302(14) 0.53303(8) 0.0263(3) Uani 1 d . . . C26 C 0.60041(17) 0.75608(16) 0.48883(8) 0.0326(4) Uani 1 d . . . H26A H 0.5209 0.7326 0.5003 0.039 Uiso 1 calc R . . C27 C 0.61388(19) 0.73336(17) 0.42840(9) 0.0375(4) Uani 1 d . . . H27A H 0.5439 0.6951 0.3988 0.045 Uiso 1 calc R . . C28 C 0.7293(2) 0.76647(18) 0.41143(9) 0.0401(4) Uani 1 d . . . H28A H 0.7388 0.7499 0.3703 0.048 Uiso 1 calc R . . C29 C 0.8314(2) 0.82411(19) 0.45477(10) 0.0420(5) Uani 1 d . . . H29A H 0.9107 0.8477 0.4430 0.050 Uiso 1 calc R . . C30 C 0.81846(17) 0.84750(17) 0.51517(9) 0.0343(4) Uani 1 d . . . H30A H 0.8889 0.8871 0.5444 0.041 Uiso 1 calc R . . C31 C 0.82495(15) 0.87818(15) 0.65762(8) 0.0256(3) Uani 1 d . . . C32 C 0.84225(17) 0.79952(16) 0.69280(8) 0.0319(4) Uani 1 d . . . H32A H 0.7767 0.7246 0.6944 0.038 Uiso 1 calc R . . C33 C 0.95598(19) 0.83140(19) 0.72555(9) 0.0409(5) Uani 1 d . . . H33A H 0.9677 0.7779 0.7495 0.049 Uiso 1 calc R . . C34 C 1.05206(18) 0.9401(2) 0.72352(10) 0.0417(5) Uani 1 d . . . H34A H 1.1295 0.9609 0.7458 0.050 Uiso 1 calc R . . C35 C 1.03552(17) 1.01894(18) 0.68892(9) 0.0381(4) Uani 1 d . . . H35A H 1.1014 1.0938 0.6877 0.046 Uiso 1 calc R . . C36 C 0.92248(16) 0.98820(15) 0.65599(8) 0.0314(4) Uani 1 d . . . H36A H 0.9114 1.0422 0.6322 0.038 Uiso 1 calc R . . C37 C 0.78703(16) 0.55576(14) 0.98935(8) 0.0278(3) Uani 1 d . . . C38 C 0.88435(17) 0.59308(16) 1.03578(9) 0.0329(4) Uani 1 d . . . H38A H 0.9658 0.6306 1.0255 0.040 Uiso 1 calc R . . C39 C 0.86394(19) 0.57615(18) 1.09703(9) 0.0387(4) Uani 1 d . . . H39A H 0.9313 0.6016 1.1283 0.046 Uiso 1 calc R . . C40 C 0.7462(2) 0.52254(17) 1.11258(10) 0.0404(5) Uani 1 d . . . H40A H 0.7323 0.5117 1.1545 0.048 Uiso 1 calc R . . C41 C 0.6483(2) 0.48456(19) 1.06689(11) 0.0452(5) Uani 1 d . . . H41A H 0.5671 0.4472 1.0775 0.054 Uiso 1 calc R . . C42 C 0.66813(18) 0.50071(18) 1.00567(10) 0.0405(5) Uani 1 d . . . H42A H 0.6004 0.4742 0.9746 0.049 Uiso 1 calc R . . C43 C 0.96447(16) 0.68383(15) 0.90612(8) 0.0282(4) Uani 1 d . . . C44 C 0.99261(18) 0.79647(16) 0.89653(9) 0.0353(4) Uani 1 d . . . H44A H 0.9286 0.8163 0.8900 0.042 Uiso 1 calc R . . C45 C 1.1135(2) 0.88041(18) 0.89644(10) 0.0436(5) Uani 1 d . . . H45A H 1.1316 0.9572 0.8904 0.052 Uiso 1 calc R . . C46 C 1.2067(2) 0.8523(2) 0.90511(11) 0.0476(5) Uani 1 d . . . H46A H 1.2891 0.9097 0.9050 0.057 Uiso 1 calc R . . C47 C 1.1803(2) 0.7403(2) 0.91401(12) 0.0491(5) Uani 1 d . . . H47A H 1.2448 0.7209 0.9199 0.059 Uiso 1 calc R . . C48 C 1.06035(18) 0.65663(18) 0.91435(10) 0.0399(4) Uani 1 d . . . H48A H 1.0429 0.5800 0.9202 0.048 Uiso 1 calc R . . C49 C 0.79854(16) 0.44504(15) 0.87668(8) 0.0288(4) Uani 1 d . . . C50 C 0.7902(2) 0.42868(18) 0.81306(9) 0.0401(5) Uani 1 d . . . H50A H 0.7859 0.4841 0.7878 0.048 Uiso 1 calc R . . C51 C 0.7880(2) 0.3313(2) 0.78616(11) 0.0501(6) Uani 1 d . . . H51A H 0.7832 0.3209 0.7426 0.060 Uiso 1 calc R . . C52 C 0.7929(2) 0.24969(18) 0.82264(11) 0.0453(5) Uani 1 d . . . H52A H 0.7914 0.1833 0.8042 0.054 Uiso 1 calc R . . C53 C 0.79988(18) 0.26450(17) 0.88564(11) 0.0409(5) Uani 1 d . . . H53A H 0.8032 0.2082 0.9106 0.049 Uiso 1 calc R . . C54 C 0.80212(17) 0.36163(16) 0.91310(9) 0.0343(4) Uani 1 d . . . H54A H 0.8061 0.3710 0.9566 0.041 Uiso 1 calc R . . C55 C 0.53296(16) 0.83384(16) 0.83584(8) 0.0292(4) Uani 1 d . . . C56 C 0.53825(19) 0.94164(17) 0.83630(9) 0.0354(4) Uani 1 d . . . H56A H 0.6026 1.0044 0.8612 0.043 Uiso 1 calc R . . C57 C 0.4498(2) 0.9572(2) 0.80056(10) 0.0426(5) Uani 1 d . . . H57A H 0.4531 1.0303 0.8014 0.051 Uiso 1 calc R . . C58 C 0.3574(2) 0.8666(2) 0.76392(10) 0.0492(6) Uani 1 d . . . H58A H 0.2970 0.8774 0.7396 0.059 Uiso 1 calc R . . C59 C 0.3519(2) 0.7596(2) 0.76237(10) 0.0487(5) Uani 1 d . . . H59A H 0.2878 0.6976 0.7369 0.058 Uiso 1 calc R . . C60 C 0.43973(18) 0.74265(17) 0.79796(9) 0.0368(4) Uani 1 d . . . H60A H 0.4363 0.6695 0.7965 0.044 Uiso 1 calc R . . C61 C 0.59669(16) 0.80583(15) 0.96281(8) 0.0295(4) Uani 1 d . . . C62 C 0.51782(18) 0.84728(17) 0.97876(10) 0.0380(4) Uani 1 d . . . H62A H 0.4847 0.8786 0.9486 0.046 Uiso 1 calc R . . C63 C 0.4878(2) 0.8427(2) 1.03849(11) 0.0497(5) Uani 1 d . . . H63A H 0.4340 0.8709 1.0490 0.060 Uiso 1 calc R . . C64 C 0.5354(2) 0.7975(2) 1.08291(11) 0.0531(6) Uani 1 d . . . H64A H 0.5135 0.7938 1.1236 0.064 Uiso 1 calc R . . C65 C 0.6147(2) 0.7577(2) 1.06785(10) 0.0512(6) Uani 1 d . . . H65A H 0.6492 0.7282 1.0984 0.061 Uiso 1 calc R . . C66 C 0.6442(2) 0.76085(19) 1.00795(9) 0.0408(5) Uani 1 d . . . H66A H 0.6976 0.7319 0.9976 0.049 Uiso 1 calc R . . C67 C 0.78589(16) 0.93862(15) 0.88775(8) 0.0284(4) Uani 1 d . . . C68 C 0.8365(2) 0.97310(18) 0.83269(9) 0.0397(4) Uani 1 d . . . H68A H 0.7921 0.9317 0.7948 0.048 Uiso 1 calc R . . C69 C 0.9508(2) 1.06716(19) 0.83294(11) 0.0460(5) Uani 1 d . . . H69A H 0.9836 1.0905 0.7951 0.055 Uiso 1 calc R . . C70 C 1.0174(2) 1.12715(18) 0.88766(11) 0.0444(5) Uani 1 d . . . H70A H 1.0963 1.1908 0.8877 0.053 Uiso 1 calc R . . C71 C 0.9684(2) 1.09397(18) 0.94228(11) 0.0469(5) Uani 1 d . . . H71A H 1.0140 1.1351 0.9801 0.056 Uiso 1 calc R . . C72 C 0.85309(18) 1.00121(17) 0.94265(9) 0.0371(4) Uani 1 d . . . H72A H 0.8198 0.9802 0.9805 0.045 Uiso 1 calc R . . O5 O 0.36658(19) 0.13942(16) 0.73382(11) 0.0727(6) Uani 1 d . . . H5 H 0.3215 0.1401 0.7600 0.087 Uiso 1 calc R . . H5B H 0.433(3) 0.218(3) 0.7312(15) 0.087 Uiso 1 d . . . O6 O 0.24270(17) 0.25499(17) 0.79291(9) 0.0651(5) Uani 1 d . . . H6 H 0.2570 0.2033 0.7791 0.078 Uiso 1 calc R . . H6B H 0.328(3) 0.342(3) 0.7941(13) 0.078 Uiso 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 0.02419(6) 0.02668(7) 0.02980(7) 0.00257(5) 0.00229(5) 0.00997(5) Ag2 0.03479(7) 0.02977(7) 0.02852(7) -0.00400(5) -0.00227(5) 0.01961(6) Se 0.03059(9) 0.02240(8) 0.02579(9) 0.00230(6) 0.00132(7) 0.00992(7) P1 0.0216(2) 0.0261(2) 0.0309(2) 0.00464(17) 0.00181(17) 0.01071(18) P2 0.0234(2) 0.0235(2) 0.0243(2) 0.00082(16) 0.00305(16) 0.00983(17) P3 0.0289(2) 0.0267(2) 0.0268(2) 0.00008(17) 0.00077(17) 0.01586(19) P4 0.0312(2) 0.0263(2) 0.0256(2) -0.00145(17) 0.00059(17) 0.01671(19) O1 0.0522(9) 0.0388(8) 0.0716(12) 0.0174(8) -0.0251(8) 0.0109(7) O2 0.0509(9) 0.0313(7) 0.0470(9) -0.0035(6) 0.0054(7) 0.0193(7) O3 0.0503(9) 0.0420(8) 0.0489(9) -0.0049(7) 0.0257(7) 0.0095(7) O4 0.0337(7) 0.0318(7) 0.0297(7) 0.0003(5) 0.0041(5) 0.0043(6) C1 0.0252(8) 0.0252(8) 0.0382(10) 0.0066(7) 0.0057(7) 0.0128(7) C2 0.0310(9) 0.0319(10) 0.0439(11) 0.0064(8) 0.0005(8) 0.0134(8) C3 0.0279(9) 0.0281(10) 0.0685(15) 0.0051(9) 0.0043(9) 0.0095(8) C4 0.0443(12) 0.0303(10) 0.0678(15) 0.0160(10) 0.0267(11) 0.0167(9) C5 0.0659(16) 0.0459(13) 0.0439(13) 0.0140(10) 0.0190(11) 0.0158(12) C6 0.0460(12) 0.0397(11) 0.0374(11) 0.0048(9) 0.0060(9) 0.0102(10) C7 0.0273(8) 0.0297(9) 0.0229(8) 0.0007(7) 0.0020(6) 0.0144(7) C8 0.0283(9) 0.0306(9) 0.0329(10) 0.0023(7) 0.0017(7) 0.0115(8) C9 0.0457(11) 0.0295(9) 0.0365(11) 0.0025(8) 0.0051(8) 0.0165(9) C10 0.0515(12) 0.0404(11) 0.0457(12) 0.0017(9) 0.0096(9) 0.0315(10) C11 0.0341(10) 0.0481(12) 0.0663(15) 0.0007(11) 0.0095(10) 0.0253(10) C12 0.0285(9) 0.0331(10) 0.0515(12) 0.0004(9) 0.0075(8) 0.0146(8) C13 0.0232(8) 0.0228(8) 0.0341(9) 0.0028(7) 0.0063(7) 0.0091(7) C14 0.0322(9) 0.0332(9) 0.0330(10) 0.0026(7) 0.0065(7) 0.0179(8) C15 0.0426(11) 0.0380(10) 0.0330(10) 0.0037(8) 0.0079(8) 0.0173(9) C16 0.0459(12) 0.0321(10) 0.0421(12) -0.0021(8) 0.0197(9) 0.0106(9) C17 0.0526(13) 0.0351(11) 0.0608(14) 0.0008(10) 0.0220(11) 0.0261(10) C18 0.0413(11) 0.0325(10) 0.0524(12) 0.0055(9) 0.0107(9) 0.0225(9) C19 0.0228(8) 0.0251(8) 0.0285(9) 0.0009(7) 0.0033(6) 0.0094(7) C20 0.0399(10) 0.0352(10) 0.0283(9) 0.0034(7) 0.0063(8) 0.0188(9) C21 0.0427(11) 0.0361(10) 0.0412(11) -0.0036(8) 0.0102(9) 0.0197(9) C22 0.0384(10) 0.0289(9) 0.0566(13) 0.0041(9) 0.0087(9) 0.0183(9) C23 0.0488(12) 0.0356(10) 0.0437(12) 0.0125(9) 0.0074(9) 0.0216(10) C24 0.0412(10) 0.0332(10) 0.0305(9) 0.0058(7) 0.0087(8) 0.0176(8) C25 0.0283(8) 0.0255(8) 0.0257(8) 0.0012(7) 0.0040(7) 0.0131(7) C26 0.0312(9) 0.0344(10) 0.0306(9) -0.0002(7) 0.0025(7) 0.0145(8) C27 0.0447(11) 0.0367(10) 0.0283(10) -0.0017(8) -0.0024(8) 0.0182(9) C28 0.0561(13) 0.0408(11) 0.0263(10) 0.0017(8) 0.0103(9) 0.0246(10) C29 0.0419(11) 0.0503(12) 0.0375(11) 0.0031(9) 0.0153(9) 0.0231(10) C30 0.0299(9) 0.0382(10) 0.0332(10) -0.0004(8) 0.0044(7) 0.0150(8) C31 0.0250(8) 0.0276(8) 0.0229(8) 0.0001(6) 0.0030(6) 0.0113(7) C32 0.0350(9) 0.0303(9) 0.0294(9) 0.0037(7) 0.0044(7) 0.0143(8) C33 0.0462(11) 0.0487(12) 0.0351(11) 0.0053(9) 0.0000(9) 0.0291(10) C34 0.0308(10) 0.0558(13) 0.0365(11) -0.0054(9) -0.0041(8) 0.0206(10) C35 0.0275(9) 0.0375(10) 0.0376(11) -0.0040(8) 0.0021(8) 0.0064(8) C36 0.0317(9) 0.0277(9) 0.0313(9) 0.0026(7) 0.0033(7) 0.0113(8) C37 0.0308(9) 0.0241(8) 0.0302(9) 0.0008(7) 0.0049(7) 0.0143(7) C38 0.0301(9) 0.0362(10) 0.0320(10) 0.0017(8) 0.0046(7) 0.0151(8) C39 0.0440(11) 0.0415(11) 0.0295(10) 0.0007(8) 0.0015(8) 0.0198(9) C40 0.0535(12) 0.0351(10) 0.0336(10) 0.0067(8) 0.0163(9) 0.0197(10) C41 0.0375(11) 0.0434(12) 0.0504(13) 0.0101(10) 0.0186(9) 0.0130(9) C42 0.0312(10) 0.0426(11) 0.0433(12) 0.0049(9) 0.0051(8) 0.0135(9) C43 0.0317(9) 0.0304(9) 0.0231(8) 0.0013(7) 0.0047(7) 0.0149(8) C44 0.0413(10) 0.0341(10) 0.0350(10) 0.0039(8) 0.0066(8) 0.0210(9) C45 0.0488(12) 0.0329(10) 0.0453(12) 0.0062(9) 0.0112(10) 0.0151(9) C46 0.0358(11) 0.0470(12) 0.0489(13) 0.0033(10) 0.0141(9) 0.0089(10) C47 0.0337(11) 0.0521(13) 0.0632(15) 0.0051(11) 0.0090(10) 0.0210(10) C48 0.0349(10) 0.0365(10) 0.0518(12) 0.0052(9) 0.0059(9) 0.0195(9) C49 0.0262(8) 0.0265(8) 0.0348(10) -0.0010(7) -0.0005(7) 0.0143(7) C50 0.0538(12) 0.0377(11) 0.0356(11) -0.0010(8) 0.0013(9) 0.0282(10) C51 0.0707(16) 0.0477(13) 0.0401(12) -0.0090(10) 0.0025(11) 0.0361(12) C52 0.0457(12) 0.0343(10) 0.0593(14) -0.0093(10) 0.0008(10) 0.0235(10) C53 0.0366(10) 0.0292(10) 0.0584(13) 0.0047(9) -0.0006(9) 0.0179(9) C54 0.0352(10) 0.0309(9) 0.0374(10) 0.0022(8) 0.0001(8) 0.0167(8) C55 0.0339(9) 0.0332(9) 0.0258(9) 0.0021(7) 0.0033(7) 0.0203(8) C56 0.0436(11) 0.0356(10) 0.0337(10) 0.0032(8) 0.0074(8) 0.0237(9) C57 0.0587(13) 0.0520(13) 0.0379(11) 0.0126(9) 0.0141(10) 0.0414(11) C58 0.0560(13) 0.0777(17) 0.0355(11) 0.0112(11) 0.0045(10) 0.0493(13) C59 0.0489(12) 0.0615(14) 0.0375(12) -0.0061(10) -0.0091(9) 0.0306(12) C60 0.0415(11) 0.0378(10) 0.0328(10) -0.0019(8) -0.0020(8) 0.0215(9) C61 0.0298(9) 0.0266(8) 0.0287(9) -0.0021(7) 0.0033(7) 0.0107(7) C62 0.0397(11) 0.0382(10) 0.0389(11) 0.0022(8) 0.0091(8) 0.0199(9) C63 0.0540(13) 0.0510(13) 0.0493(13) 0.0006(10) 0.0211(11) 0.0268(11) C64 0.0645(15) 0.0551(14) 0.0336(12) 0.0002(10) 0.0155(10) 0.0218(12) C65 0.0604(14) 0.0634(15) 0.0304(11) 0.0053(10) 0.0011(10) 0.0304(13) C66 0.0443(11) 0.0491(12) 0.0337(10) 0.0038(9) 0.0035(8) 0.0260(10) C67 0.0322(9) 0.0271(8) 0.0310(9) 0.0001(7) 0.0052(7) 0.0181(8) C68 0.0487(12) 0.0417(11) 0.0319(10) -0.0001(8) 0.0095(9) 0.0234(10) C69 0.0520(13) 0.0442(12) 0.0508(13) 0.0108(10) 0.0254(10) 0.0264(11) C70 0.0385(11) 0.0333(10) 0.0624(14) 0.0070(10) 0.0153(10) 0.0159(9) C71 0.0430(12) 0.0382(11) 0.0469(13) -0.0045(9) 0.0002(10) 0.0101(10) C72 0.0414(11) 0.0353(10) 0.0298(10) 0.0007(8) 0.0057(8) 0.0141(9) O5 0.0670(13) 0.0458(10) 0.1083(18) 0.0240(11) 0.0214(11) 0.0265(9) O6 0.0522(10) 0.0598(11) 0.0696(13) 0.0055(10) 0.0136(9) 0.0140(9) _geom_special_details ; ? ; 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 O1 2.2342(15) . ? Ag1 P2 2.4105(5) . ? Ag1 P1 2.4994(4) . ? Ag2 O4 2.4025(13) . ? Ag2 P4 2.4289(4) . ? Ag2 P3 2.4590(4) . ? Ag2 O3 2.6507(16) . ? Se O2 1.6271(13) . ? Se O3 1.6394(14) . ? Se O1 1.6403(15) . ? Se O4 1.6489(13) . ? P1 C13 1.8279(18) . ? P1 C1 1.8294(18) . ? P1 C7 1.8309(17) . ? P2 C31 1.8213(17) . ? P2 C19 1.8296(17) . ? P2 C25 1.8323(17) . ? P3 C49 1.8250(18) . ? P3 C37 1.8272(18) . ? P3 C43 1.8289(19) . ? P4 C55 1.8212(18) . ? P4 C67 1.8285(19) . ? P4 C61 1.8308(18) . ? C1 C2 1.390(3) . ? C1 C6 1.391(3) . ? C2 C3 1.391(3) . ? C3 C4 1.380(3) . ? C4 C5 1.381(3) . ? C5 C6 1.395(3) . ? C7 C8 1.394(2) . ? C7 C12 1.397(2) . ? C8 C9 1.390(3) . ? C9 C10 1.379(3) . ? C10 C11 1.387(3) . ? C11 C12 1.382(3) . ? C13 C14 1.394(3) . ? C13 C18 1.402(2) . ? C14 C15 1.394(3) . ? C15 C16 1.385(3) . ? C16 C17 1.380(3) . ? C17 C18 1.385(3) . ? C19 C24 1.388(3) . ? C19 C20 1.400(2) . ? C20 C21 1.388(3) . ? C21 C22 1.381(3) . ? C22 C23 1.381(3) . ? C23 C24 1.393(3) . ? C25 C30 1.397(2) . ? C25 C26 1.398(2) . ? C26 C27 1.390(3) . ? C27 C28 1.384(3) . ? C28 C29 1.389(3) . ? C29 C30 1.389(3) . ? C31 C32 1.396(2) . ? C31 C36 1.399(2) . ? C32 C33 1.392(3) . ? C33 C34 1.382(3) . ? C34 C35 1.386(3) . ? C35 C36 1.389(3) . ? C37 C38 1.390(3) . ? C37 C42 1.397(3) . ? C38 C39 1.390(3) . ? C39 C40 1.379(3) . ? C40 C41 1.383(3) . ? C41 C42 1.387(3) . ? C43 C44 1.392(3) . ? C43 C48 1.400(3) . ? C44 C45 1.392(3) . ? C45 C46 1.376(3) . ? C46 C47 1.387(3) . ? C47 C48 1.384(3) . ? C49 C50 1.389(3) . ? C49 C54 1.395(3) . ? C50 C51 1.393(3) . ? C51 C52 1.381(3) . ? C52 C53 1.375(3) . ? C53 C54 1.394(3) . ? C55 C60 1.397(3) . ? C55 C56 1.400(3) . ? C56 C57 1.390(3) . ? C57 C58 1.377(3) . ? C58 C59 1.387(3) . ? C59 C60 1.393(3) . ? C61 C66 1.392(3) . ? C61 C62 1.396(3) . ? C62 C63 1.386(3) . ? C63 C64 1.383(3) . ? C64 C65 1.380(3) . ? C65 C66 1.389(3) . ? C67 C72 1.394(3) . ? C67 C68 1.397(3) . ? C68 C69 1.385(3) . ? C69 C70 1.379(3) . ? C70 C71 1.379(3) . ? C71 C72 1.387(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 O1 Ag1 P2 138.40(5) . . ? O1 Ag1 P1 90.38(4) . . ? P2 Ag1 P1 128.353(16) . . ? O4 Ag2 P4 122.21(4) . . ? O4 Ag2 P3 100.36(4) . . ? P4 Ag2 P3 128.755(16) . . ? O4 Ag2 O3 62.46(4) . . ? P4 Ag2 O3 111.74(4) . . ? P3 Ag2 O3 112.73(4) . . ? O2 Se O3 112.20(8) . . ? O2 Se O1 108.10(8) . . ? O3 Se O1 110.95(10) . . ? O2 Se O4 110.24(7) . . ? O3 Se O4 106.14(7) . . ? O1 Se O4 109.19(7) . . ? C13 P1 C1 103.65(8) . . ? C13 P1 C7 103.51(8) . . ? C1 P1 C7 105.02(8) . . ? C13 P1 Ag1 107.14(6) . . ? C1 P1 Ag1 119.31(6) . . ? C7 P1 Ag1 116.41(6) . . ? C31 P2 C19 104.52(8) . . ? C31 P2 C25 104.79(8) . . ? C19 P2 C25 104.98(8) . . ? C31 P2 Ag1 120.46(6) . . ? C19 P2 Ag1 109.82(6) . . ? C25 P2 Ag1 111.05(6) . . ? C49 P3 C37 104.29(8) . . ? C49 P3 C43 103.48(8) . . ? C37 P3 C43 105.45(8) . . ? C49 P3 Ag2 118.41(6) . . ? C37 P3 Ag2 113.51(6) . . ? C43 P3 Ag2 110.49(6) . . ? C55 P4 C67 104.36(8) . . ? C55 P4 C61 105.04(8) . . ? C67 P4 C61 104.06(8) . . ? C55 P4 Ag2 118.09(6) . . ? C67 P4 Ag2 110.54(5) . . ? C61 P4 Ag2 113.47(6) . . ? Se O1 Ag1 127.94(8) . . ? Se O3 Ag2 91.17(6) . . ? Se O4 Ag2 100.18(6) . . ? C2 C1 C6 119.13(18) . . ? C2 C1 P1 122.19(15) . . ? C6 C1 P1 118.68(15) . . ? C1 C2 C3 120.2(2) . . ? C4 C3 C2 120.3(2) . . ? C3 C4 C5 119.95(19) . . ? C4 C5 C6 120.1(2) . . ? C1 C6 C5 120.2(2) . . ? C8 C7 C12 118.67(16) . . ? C8 C7 P1 117.99(13) . . ? C12 C7 P1 123.26(14) . . ? C9 C8 C7 120.49(17) . . ? C10 C9 C8 120.17(19) . . ? C9 C10 C11 119.91(18) . . ? C12 C11 C10 120.21(19) . . ? C11 C12 C7 120.53(19) . . ? C14 C13 C18 118.72(17) . . ? C14 C13 P1 123.37(13) . . ? C18 C13 P1 117.84(15) . . ? C15 C14 C13 120.70(17) . . ? C16 C15 C14 120.0(2) . . ? C17 C16 C15 119.50(19) . . ? C16 C17 C18 121.18(18) . . ? C17 C18 C13 119.89(19) . . ? C24 C19 C20 118.78(16) . . ? C24 C19 P2 123.36(13) . . ? C20 C19 P2 117.68(13) . . ? C21 C20 C19 120.40(18) . . ? C22 C21 C20 120.31(18) . . ? C21 C22 C23 119.74(18) . . ? C22 C23 C24 120.39(19) . . ? C19 C24 C23 120.36(18) . . ? C30 C25 C26 118.62(16) . . ? C30 C25 P2 122.80(14) . . ? C26 C25 P2 118.49(13) . . ? C27 C26 C25 120.95(18) . . ? C28 C27 C26 119.94(18) . . ? C27 C28 C29 119.69(18) . . ? C28 C29 C30 120.59(19) . . ? C29 C30 C25 120.20(18) . . ? C32 C31 C36 119.31(16) . . ? C32 C31 P2 118.64(13) . . ? C36 C31 P2 122.00(13) . . ? C33 C32 C31 119.70(18) . . ? C34 C33 C32 120.64(19) . . ? C33 C34 C35 120.03(18) . . ? C34 C35 C36 119.90(19) . . ? C35 C36 C31 120.40(17) . . ? C38 C37 C42 118.46(17) . . ? C38 C37 P3 123.94(14) . . ? C42 C37 P3 117.59(14) . . ? C37 C38 C39 120.80(18) . . ? C40 C39 C38 120.19(19) . . ? C39 C40 C41 119.72(19) . . ? C40 C41 C42 120.35(19) . . ? C41 C42 C37 120.49(19) . . ? C44 C43 C48 118.41(18) . . ? C44 C43 P3 119.32(14) . . ? C48 C43 P3 122.27(14) . . ? C45 C44 C43 120.71(18) . . ? C46 C45 C44 120.1(2) . . ? C45 C46 C47 120.1(2) . . ? C48 C47 C46 120.0(2) . . ? C47 C48 C43 120.69(19) . . ? C50 C49 C54 119.15(17) . . ? C50 C49 P3 117.21(14) . . ? C54 C49 P3 123.63(14) . . ? C49 C50 C51 120.28(19) . . ? C52 C51 C50 120.1(2) . . ? C53 C52 C51 120.03(19) . . ? C52 C53 C54 120.36(19) . . ? C53 C54 C49 120.02(19) . . ? C60 C55 C56 119.41(17) . . ? C60 C55 P4 118.41(14) . . ? C56 C55 P4 122.14(14) . . ? C57 C56 C55 120.31(19) . . ? C58 C57 C56 119.90(19) . . ? C57 C58 C59 120.43(19) . . ? C58 C59 C60 120.3(2) . . ? C59 C60 C55 119.58(19) . . ? C66 C61 C62 118.70(18) . . ? C66 C61 P4 117.76(14) . . ? C62 C61 P4 123.54(15) . . ? C63 C62 C61 120.0(2) . . ? C64 C63 C62 120.7(2) . . ? C65 C64 C63 119.7(2) . . ? C64 C65 C66 119.9(2) . . ? C65 C66 C61 120.9(2) . . ? C72 C67 C68 118.40(18) . . ? C72 C67 P4 122.92(15) . . ? C68 C67 P4 118.46(14) . . ? C69 C68 C67 120.57(19) . . ? C70 C69 C68 120.5(2) . . ? C71 C70 C69 119.5(2) . . ? C70 C71 C72 120.7(2) . . ? C71 C72 C67 120.37(19) . . ? 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 O5 H5 O6 0.84 2.30 2.980(3) 138.6 . O5 H5B O2 0.99(3) 1.71(3) 2.689(2) 170(3) . O6 H6B O3 1.14(3) 1.72(3) 2.862(2) 176(2) . _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.05 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.418 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.048 #===END data_gab9963 #Compound 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H33 Ag O5 P2 S' _chemical_formula_weight 747.49 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.58420(10) _cell_length_b 13.26680(10) _cell_length_c 24.3057(3) _cell_angle_alpha 92.9180(10) _cell_angle_beta 103.5360(10) _cell_angle_gamma 118.0230(10) _cell_volume 3420.90(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8088 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.7708 _exptl_absorpt_correction_T_max 0.9049 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32305 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 27.07 _reflns_number_total 14368 _reflns_number_gt 12199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+3.9827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14368 _refine_ls_number_parameters 829 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 2.145 _refine_ls_shift/su_mean 0.018 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.627060(19) 0.603946(17) 0.867034(9) 0.03348(6) Uani 1 d . . . P1 P 0.60556(6) 0.77306(6) 0.88920(3) 0.03080(14) Uani 1 d . . . P2 P 0.78474(6) 0.55286(6) 0.91308(3) 0.03125(14) Uani 1 d . . . S1 S 0.35294(8) 0.33800(7) 0.79366(3) 0.0500(2) Uani 1 d . . . O1 O 0.4325(2) 0.4221(2) 0.84539(10) 0.0692(8) Uani 1 d . . . O2 O 0.2389(2) 0.2446(2) 0.79970(11) 0.0725(8) Uani 1 d . . . O3 O 0.3141(3) 0.4004(2) 0.74820(12) 0.0732(8) Uani 1 d . . . H3B H 0.393(4) 0.473(4) 0.7413(19) 0.088 Uiso 1 d . . . O4 O 0.4226(3) 0.2933(3) 0.76928(15) 0.0872(10) Uani 1 d . . . C1 C 0.5991(2) 0.8004(2) 0.96268(12) 0.0344(6) Uani 1 d . . . C2 C 0.6655(3) 0.7681(3) 1.00601(13) 0.0430(7) Uani 1 d . . . H2B H 0.7148 0.7367 0.9970 0.052 Uiso 1 calc R . . C3 C 0.6598(3) 0.7817(3) 1.06205(14) 0.0519(8) Uani 1 d . . . H3B H 0.7056 0.7602 1.0913 0.062 Uiso 1 calc R . . C4 C 0.5878(3) 0.8263(3) 1.07553(15) 0.0545(9) Uani 1 d . . . H4B H 0.5832 0.8347 1.1138 0.065 Uiso 1 calc R . . C5 C 0.5229(3) 0.8585(3) 1.03319(15) 0.0531(8) Uani 1 d . . . H5A H 0.4741 0.8901 1.0426 0.064 Uiso 1 calc R . . C6 C 0.5274(3) 0.8455(3) 0.97691(14) 0.0444(7) Uani 1 d . . . H6A H 0.4814 0.8676 0.9481 0.053 Uiso 1 calc R . . C7 C 0.7466(2) 0.9006(2) 0.88383(12) 0.0332(6) Uani 1 d . . . C8 C 0.7697(3) 0.9041(3) 0.83042(14) 0.0446(7) Uani 1 d . . . H8A H 0.7098 0.8448 0.7982 0.053 Uiso 1 calc R . . C9 C 0.8794(3) 0.9935(3) 0.82393(17) 0.0558(9) Uani 1 d . . . H9A H 0.8937 0.9958 0.7872 0.067 Uiso 1 calc R . . C10 C 0.9676(3) 1.0790(3) 0.8703(2) 0.0620(10) Uani 1 d . . . H10A H 1.0427 1.1401 0.8657 0.074 Uiso 1 calc R . . C11 C 0.9468(3) 1.0757(3) 0.92365(18) 0.0579(9) Uani 1 d . . . H11A H 1.0084 1.1338 0.9559 0.070 Uiso 1 calc R . . C12 C 0.8357(3) 0.9873(2) 0.93034(14) 0.0445(7) Uani 1 d . . . H12A H 0.8209 0.9865 0.9669 0.053 Uiso 1 calc R . . C13 C 0.4753(3) 0.7822(2) 0.84290(12) 0.0359(6) Uani 1 d . . . C14 C 0.4750(3) 0.8876(3) 0.84036(14) 0.0442(7) Uani 1 d . . . H14A H 0.5459 0.9580 0.8628 0.053 Uiso 1 calc R . . C15 C 0.3724(4) 0.8897(4) 0.80546(16) 0.0596(9) Uani 1 d . . . H15A H 0.3722 0.9611 0.8045 0.072 Uiso 1 calc R . . C16 C 0.2706(4) 0.7883(5) 0.77205(19) 0.0769(13) Uani 1 d . . . H16A H 0.2004 0.7900 0.7479 0.092 Uiso 1 calc R . . C17 C 0.2701(3) 0.6844(4) 0.77350(18) 0.0719(12) Uani 1 d . . . H17A H 0.1998 0.6150 0.7500 0.086 Uiso 1 calc R . . C18 C 0.3721(3) 0.6802(3) 0.80923(14) 0.0497(8) Uani 1 d . . . H18A H 0.3708 0.6082 0.8104 0.060 Uiso 1 calc R . . C19 C 0.7901(2) 0.5542(2) 0.98878(12) 0.0323(5) Uani 1 d . . . C20 C 0.6753(3) 0.4982(2) 1.00162(14) 0.0430(7) Uani 1 d . . . H20A H 0.5985 0.4597 0.9713 0.052 Uiso 1 calc R . . C21 C 0.6733(3) 0.4986(3) 1.05825(15) 0.0514(8) Uani 1 d . . . H21A H 0.5952 0.4596 1.0666 0.062 Uiso 1 calc R . . C22 C 0.7849(3) 0.5559(3) 1.10296(14) 0.0482(7) Uani 1 d . . . H22A H 0.7830 0.5570 1.1418 0.058 Uiso 1 calc R . . C23 C 0.8986(3) 0.6112(3) 1.09080(13) 0.0438(7) Uani 1 d . . . H23A H 0.9751 0.6499 1.1213 0.053 Uiso 1 calc R . . C24 C 0.9014(3) 0.6102(2) 1.03382(12) 0.0361(6) Uani 1 d . . . H24A H 0.9799 0.6480 1.0257 0.043 Uiso 1 calc R . . C25 C 0.7689(2) 0.4127(2) 0.88912(12) 0.0343(6) Uani 1 d . . . C26 C 0.7644(3) 0.3339(2) 0.92540(13) 0.0395(6) Uani 1 d . . . H26A H 0.7705 0.3526 0.9647 0.047 Uiso 1 calc R . . C27 C 0.7512(3) 0.2275(2) 0.90436(15) 0.0453(7) Uani 1 d . . . H27A H 0.7480 0.1740 0.9294 0.054 Uiso 1 calc R . . C28 C 0.7426(3) 0.1996(3) 0.84769(15) 0.0497(8) Uani 1 d . . . H28A H 0.7325 0.1266 0.8334 0.060 Uiso 1 calc R . . C29 C 0.7487(4) 0.2778(3) 0.81164(15) 0.0597(9) Uani 1 d . . . H29A H 0.7448 0.2591 0.7727 0.072 Uiso 1 calc R . . C30 C 0.7604(3) 0.3833(3) 0.83157(14) 0.0505(8) Uani 1 d . . . H30A H 0.7627 0.4358 0.8061 0.061 Uiso 1 calc R . . C31 C 0.9445(2) 0.6593(2) 0.91402(11) 0.0324(5) Uani 1 d . . . C32 C 1.0379(3) 0.6308(3) 0.91590(15) 0.0448(7) Uani 1 d . . . H32A H 1.0193 0.5526 0.9162 0.054 Uiso 1 calc R . . C33 C 1.1584(3) 0.7151(3) 0.91730(16) 0.0535(8) Uani 1 d . . . H33A H 1.2213 0.6942 0.9182 0.064 Uiso 1 calc R . . C34 C 1.1872(3) 0.8292(3) 0.91733(15) 0.0523(8) Uani 1 d . . . H34A H 1.2698 0.8872 0.9188 0.063 Uiso 1 calc R . . C35 C 1.0942(3) 0.8583(3) 0.91521(18) 0.0602(10) Uani 1 d . . . H35A H 1.1133 0.9366 0.9152 0.072 Uiso 1 calc R . . C36 C 0.9735(3) 0.7741(3) 0.91307(16) 0.0497(8) Uani 1 d . . . H36A H 0.9101 0.7948 0.9109 0.060 Uiso 1 calc R . . Ag2 Ag 0.79490(2) 0.721628(18) 0.632591(9) 0.03658(6) Uani 1 d . . . P3 P 0.73685(6) 0.86229(6) 0.59724(3) 0.03097(14) Uani 1 d . . . P4 P 0.88978(7) 0.62439(6) 0.59278(3) 0.03676(16) Uani 1 d . . . S2 S 0.62632(9) 0.55316(7) 0.72549(3) 0.04769(19) Uani 1 d . . . O5 O 0.6325(2) 0.5882(2) 0.67066(9) 0.0486(5) Uani 1 d . . . O6 O 0.5782(3) 0.4221(2) 0.71486(10) 0.0540(6) Uani 1 d . . . H6B H 0.533(4) 0.394(4) 0.7311(18) 0.065 Uiso 1 d . . . O7 O 0.5345(3) 0.5706(2) 0.74637(13) 0.0774(9) Uani 1 d . . . O8 O 0.7471(3) 0.6108(2) 0.76946(11) 0.0847(10) Uani 1 d . . . O9 O 0.9198(4) 0.8007(3) 0.73360(12) 0.1095(14) Uani 1 d D . . H9B H 0.871(4) 0.757(4) 0.7545(19) 0.131 Uiso 1 d D . . H9C H 1.003(3) 0.842(5) 0.7658(19) 0.131 Uiso 1 d D . . C37 C 0.8808(3) 0.9918(2) 0.59693(11) 0.0329(5) Uani 1 d . . . C38 C 0.9751(3) 1.0458(3) 0.64934(14) 0.0525(8) Uani 1 d . . . H38A H 0.9598 1.0181 0.6835 0.063 Uiso 1 calc R . . C39 C 1.0904(3) 1.1393(3) 0.65194(16) 0.0607(10) Uani 1 d . . . H39A H 1.1532 1.1766 0.6880 0.073 Uiso 1 calc R . . C40 C 1.1149(3) 1.1790(3) 0.60246(17) 0.0547(9) Uani 1 d . . . H40A H 1.1949 1.2423 0.6042 0.066 Uiso 1 calc R . . C41 C 1.0234(3) 1.1264(3) 0.55097(16) 0.0553(9) Uani 1 d . . . H41A H 1.0401 1.1539 0.5169 0.066 Uiso 1 calc R . . C42 C 0.9059(3) 1.0331(3) 0.54760(13) 0.0430(7) Uani 1 d . . . H42A H 0.8429 0.9979 0.5115 0.052 Uiso 1 calc R . . C43 C 0.6316(2) 0.8208(2) 0.52397(11) 0.0330(6) Uani 1 d . . . C44 C 0.6402(3) 0.7489(2) 0.48316(12) 0.0391(6) Uani 1 d . . . H44A H 0.7019 0.7258 0.4937 0.047 Uiso 1 calc R . . C45 C 0.5593(3) 0.7112(3) 0.42743(13) 0.0469(7) Uani 1 d . . . H45A H 0.5669 0.6637 0.3998 0.056 Uiso 1 calc R . . C46 C 0.4676(3) 0.7427(3) 0.41222(13) 0.0499(8) Uani 1 d . . . H46A H 0.4114 0.7158 0.3743 0.060 Uiso 1 calc R . . C47 C 0.4577(3) 0.8130(3) 0.45214(14) 0.0528(8) Uani 1 d . . . H47A H 0.3944 0.8342 0.4416 0.063 Uiso 1 calc R . . C48 C 0.5402(3) 0.8531(3) 0.50797(13) 0.0438(7) Uani 1 d . . . H48A H 0.5338 0.9026 0.5351 0.053 Uiso 1 calc R . . C49 C 0.6684(3) 0.9160(2) 0.64070(11) 0.0337(6) Uani 1 d . . . C50 C 0.6864(3) 1.0290(3) 0.64401(12) 0.0432(7) Uani 1 d . . . H50A H 0.7382 1.0812 0.6239 0.052 Uiso 1 calc R . . C51 C 0.6292(3) 1.0646(3) 0.67636(13) 0.0501(8) Uani 1 d . . . H51A H 0.6420 1.1414 0.6785 0.060 Uiso 1 calc R . . C52 C 0.5534(3) 0.9893(3) 0.70556(13) 0.0504(8) Uani 1 d . . . H52A H 0.5140 1.0142 0.7277 0.061 Uiso 1 calc R . . C53 C 0.5348(3) 0.8774(3) 0.70258(13) 0.0482(7) Uani 1 d . . . H53A H 0.4819 0.8253 0.7224 0.058 Uiso 1 calc R . . C54 C 0.5930(3) 0.8407(3) 0.67089(12) 0.0382(6) Uani 1 d . . . H54A H 0.5815 0.7645 0.6697 0.046 Uiso 1 calc R . . C55 C 0.9007(3) 0.5070(2) 0.62494(14) 0.0419(7) Uani 1 d . . . C56 C 0.8949(3) 0.4126(3) 0.59350(17) 0.0497(8) Uani 1 d . . . H56A H 0.8789 0.4046 0.5529 0.060 Uiso 1 calc R . . C57 C 0.9123(3) 0.3304(3) 0.62144(19) 0.0594(10) Uani 1 d . . . H57A H 0.9089 0.2666 0.5999 0.071 Uiso 1 calc R . . C58 C 0.9346(4) 0.3411(3) 0.6804(2) 0.0672(11) Uani 1 d . . . H58A H 0.9478 0.2853 0.6993 0.081 Uiso 1 calc R . . C59 C 0.9378(4) 0.4325(3) 0.71198(18) 0.0646(10) Uani 1 d . . . H59A H 0.9519 0.4391 0.7525 0.077 Uiso 1 calc R . . C60 C 0.9201(3) 0.5153(3) 0.68400(16) 0.0526(8) Uani 1 d . . . H60A H 0.9215 0.5778 0.7056 0.063 Uiso 1 calc R . . C61 C 0.8037(3) 0.5602(2) 0.51706(13) 0.0375(6) Uani 1 d . . . C62 C 0.8589(3) 0.5806(3) 0.47252(14) 0.0438(7) Uani 1 d . . . H62A H 0.9479 0.6258 0.4813 0.053 Uiso 1 calc R . . C63 C 0.7857(3) 0.5358(3) 0.41529(15) 0.0487(7) Uani 1 d . . . H63A H 0.8248 0.5509 0.3853 0.058 Uiso 1 calc R . . C64 C 0.6564(3) 0.4695(3) 0.40200(15) 0.0495(8) Uani 1 d . . . H64A H 0.6063 0.4388 0.3630 0.059 Uiso 1 calc R . . C65 C 0.6001(3) 0.4480(3) 0.44577(16) 0.0526(8) Uani 1 d . . . H65A H 0.5112 0.4021 0.4367 0.063 Uiso 1 calc R . . C66 C 0.6723(3) 0.4927(3) 0.50278(15) 0.0466(7) Uani 1 d . . . H66A H 0.6325 0.4774 0.5325 0.056 Uiso 1 calc R . . C67 C 1.0504(3) 0.7260(2) 0.59312(12) 0.0382(6) Uani 1 d . . . C68 C 1.0908(3) 0.8444(3) 0.60121(14) 0.0453(7) Uani 1 d . . . H68A H 1.0372 0.8712 0.6093 0.054 Uiso 1 calc R . . C69 C 1.2092(3) 0.9237(3) 0.59746(17) 0.0576(9) Uani 1 d . . . H69A H 1.2359 1.0044 0.6030 0.069 Uiso 1 calc R . . C71 C 1.2501(3) 0.7695(3) 0.57850(18) 0.0601(9) Uani 1 d . . . H71A H 1.3049 0.7438 0.5708 0.072 Uiso 1 calc R . . C70 C 1.2877(3) 0.8862(3) 0.58578(17) 0.0588(9) Uani 1 d . . . H70A H 1.3679 0.9407 0.5827 0.071 Uiso 1 calc R . . C72 C 1.1324(3) 0.6894(3) 0.58235(16) 0.0517(8) Uani 1 d . . . H72A H 1.1074 0.6092 0.5776 0.062 Uiso 1 calc R . . O10 O 1.1474(5) 0.9956(4) 0.7811(2) 0.1346(16) Uani 1 d D . . H10B H 1.190(7) 1.004(6) 0.752(3) 0.161 Uiso 1 d D . . H10C H 1.136(7) 1.060(4) 0.781(3) 0.161 Uiso 1 d 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 0.03356(11) 0.02967(10) 0.03263(11) 0.00009(8) 0.00422(8) 0.01513(8) P1 0.0296(3) 0.0291(3) 0.0319(3) 0.0030(3) 0.0079(3) 0.0139(3) P2 0.0303(3) 0.0254(3) 0.0357(4) 0.0044(3) 0.0082(3) 0.0128(3) S1 0.0499(4) 0.0377(4) 0.0364(4) -0.0001(3) 0.0157(3) 0.0009(3) O1 0.0561(15) 0.0553(14) 0.0404(13) -0.0045(11) 0.0129(11) -0.0140(11) O2 0.0597(15) 0.0502(14) 0.0578(15) -0.0026(11) 0.0207(13) -0.0119(12) O3 0.0569(16) 0.0589(16) 0.0652(17) 0.0107(13) 0.0015(13) 0.0062(13) O4 0.116(3) 0.0763(19) 0.097(2) 0.0322(17) 0.071(2) 0.0500(19) C1 0.0320(13) 0.0295(13) 0.0356(14) 0.0023(11) 0.0101(11) 0.0108(11) C2 0.0430(16) 0.0440(16) 0.0385(16) 0.0035(12) 0.0093(13) 0.0205(14) C3 0.056(2) 0.0517(19) 0.0370(16) 0.0079(14) 0.0085(14) 0.0208(16) C4 0.062(2) 0.0495(18) 0.0409(17) 0.0004(14) 0.0229(16) 0.0161(16) C5 0.060(2) 0.0538(19) 0.054(2) 0.0059(15) 0.0287(17) 0.0290(17) C6 0.0476(17) 0.0453(16) 0.0460(17) 0.0073(13) 0.0196(14) 0.0250(14) C7 0.0295(13) 0.0301(13) 0.0418(15) 0.0048(11) 0.0097(11) 0.0167(11) C8 0.0409(16) 0.0416(16) 0.0499(18) 0.0078(13) 0.0174(14) 0.0176(13) C9 0.055(2) 0.054(2) 0.071(2) 0.0203(18) 0.0350(18) 0.0283(17) C10 0.0425(18) 0.0413(18) 0.105(3) 0.0178(19) 0.033(2) 0.0172(15) C11 0.0409(17) 0.0353(16) 0.080(3) 0.0001(16) 0.0073(17) 0.0108(14) C12 0.0409(16) 0.0328(14) 0.0537(18) 0.0014(13) 0.0114(14) 0.0152(13) C13 0.0306(13) 0.0440(15) 0.0342(14) 0.0081(12) 0.0113(11) 0.0185(12) C14 0.0461(17) 0.0553(18) 0.0450(17) 0.0167(14) 0.0207(14) 0.0318(15) C15 0.062(2) 0.085(3) 0.061(2) 0.029(2) 0.0269(19) 0.055(2) C16 0.054(2) 0.119(4) 0.073(3) 0.031(3) 0.013(2) 0.057(3) C17 0.0346(18) 0.086(3) 0.068(3) 0.006(2) -0.0003(17) 0.0170(19) C18 0.0361(16) 0.0535(19) 0.0505(19) 0.0081(15) 0.0094(14) 0.0169(14) C19 0.0343(13) 0.0244(12) 0.0376(14) 0.0043(10) 0.0121(11) 0.0137(11) C20 0.0334(14) 0.0359(15) 0.0497(17) 0.0045(13) 0.0135(13) 0.0093(12) C21 0.0462(18) 0.0448(17) 0.058(2) 0.0092(15) 0.0276(16) 0.0126(14) C22 0.061(2) 0.0418(16) 0.0434(17) 0.0095(13) 0.0228(15) 0.0238(15) C23 0.0474(17) 0.0410(16) 0.0385(16) 0.0052(12) 0.0084(13) 0.0206(14) C24 0.0322(14) 0.0349(14) 0.0385(15) 0.0059(11) 0.0087(11) 0.0154(11) C25 0.0296(13) 0.0270(12) 0.0405(15) 0.0025(11) 0.0058(11) 0.0119(11) C26 0.0421(15) 0.0322(14) 0.0452(16) 0.0063(12) 0.0154(13) 0.0181(12) C27 0.0447(17) 0.0323(14) 0.062(2) 0.0121(14) 0.0192(15) 0.0193(13) C28 0.0483(18) 0.0286(14) 0.065(2) -0.0032(14) 0.0164(16) 0.0151(13) C29 0.076(2) 0.0464(19) 0.0446(19) -0.0068(15) 0.0111(17) 0.0256(18) C30 0.068(2) 0.0377(16) 0.0382(16) 0.0027(13) 0.0055(15) 0.0254(16) C31 0.0341(13) 0.0296(13) 0.0331(13) 0.0071(10) 0.0115(11) 0.0147(11) C32 0.0400(16) 0.0382(15) 0.062(2) 0.0148(14) 0.0201(14) 0.0208(13) C33 0.0410(17) 0.0539(19) 0.073(2) 0.0167(17) 0.0253(16) 0.0252(15) C34 0.0397(17) 0.0465(18) 0.064(2) 0.0128(16) 0.0221(15) 0.0127(14) C35 0.051(2) 0.0330(16) 0.092(3) 0.0151(17) 0.0280(19) 0.0143(15) C36 0.0412(16) 0.0342(15) 0.076(2) 0.0119(15) 0.0208(16) 0.0188(13) Ag2 0.04167(12) 0.03583(11) 0.03832(12) 0.01108(9) 0.01769(9) 0.02087(9) P3 0.0354(3) 0.0276(3) 0.0279(3) 0.0049(3) 0.0107(3) 0.0134(3) P4 0.0338(4) 0.0320(3) 0.0475(4) 0.0087(3) 0.0171(3) 0.0162(3) S2 0.0663(5) 0.0402(4) 0.0307(4) 0.0109(3) 0.0206(3) 0.0186(4) O5 0.0431(12) 0.0591(13) 0.0325(11) 0.0181(10) 0.0138(9) 0.0147(10) O6 0.0704(17) 0.0394(12) 0.0468(13) 0.0056(10) 0.0267(12) 0.0189(12) O7 0.114(2) 0.0449(14) 0.097(2) 0.0251(14) 0.079(2) 0.0349(15) O8 0.103(2) 0.0540(15) 0.0372(13) 0.0093(11) -0.0118(14) 0.0065(15) O9 0.116(3) 0.076(2) 0.0416(16) 0.0012(14) -0.0042(16) -0.0129(19) C37 0.0346(14) 0.0284(12) 0.0328(13) 0.0042(10) 0.0086(11) 0.0140(11) C38 0.0520(19) 0.0447(17) 0.0363(16) 0.0057(13) 0.0048(14) 0.0086(15) C39 0.0486(19) 0.0435(18) 0.056(2) -0.0003(15) -0.0068(16) 0.0070(15) C40 0.0376(16) 0.0349(16) 0.077(2) 0.0064(16) 0.0165(16) 0.0073(13) C41 0.056(2) 0.0436(18) 0.057(2) 0.0128(15) 0.0273(17) 0.0124(15) C42 0.0435(16) 0.0397(15) 0.0348(15) 0.0068(12) 0.0119(13) 0.0119(13) C43 0.0319(13) 0.0299(13) 0.0306(13) 0.0049(10) 0.0098(11) 0.0098(11) C44 0.0386(15) 0.0394(15) 0.0347(14) 0.0002(12) 0.0085(12) 0.0175(12) C45 0.0524(18) 0.0450(17) 0.0344(15) -0.0011(13) 0.0113(13) 0.0187(15) C46 0.0511(18) 0.0472(17) 0.0348(16) 0.0013(13) -0.0012(14) 0.0185(15) C47 0.0514(19) 0.058(2) 0.0457(18) 0.0055(15) 0.0015(15) 0.0305(16) C48 0.0477(17) 0.0427(16) 0.0403(16) 0.0017(13) 0.0090(13) 0.0243(14) C49 0.0398(14) 0.0332(13) 0.0270(13) 0.0032(10) 0.0086(11) 0.0181(12) C50 0.0597(19) 0.0367(15) 0.0348(15) 0.0063(12) 0.0159(14) 0.0244(14) C51 0.076(2) 0.0452(17) 0.0376(16) 0.0016(13) 0.0142(16) 0.0386(17) C52 0.064(2) 0.066(2) 0.0354(16) 0.0035(14) 0.0163(15) 0.0432(18) C53 0.0533(19) 0.060(2) 0.0398(16) 0.0136(14) 0.0220(14) 0.0306(16) C54 0.0428(15) 0.0382(15) 0.0335(14) 0.0062(11) 0.0126(12) 0.0193(13) C55 0.0341(14) 0.0348(14) 0.0593(19) 0.0149(13) 0.0199(14) 0.0157(12) C56 0.0478(18) 0.0366(15) 0.072(2) 0.0161(15) 0.0319(16) 0.0195(14) C57 0.060(2) 0.0390(17) 0.094(3) 0.0252(18) 0.041(2) 0.0265(16) C58 0.059(2) 0.047(2) 0.103(3) 0.039(2) 0.029(2) 0.0275(18) C59 0.064(2) 0.054(2) 0.066(2) 0.0247(18) 0.0154(19) 0.0225(18) C60 0.0530(19) 0.0422(17) 0.060(2) 0.0133(15) 0.0169(16) 0.0208(15) C61 0.0331(14) 0.0285(13) 0.0517(17) 0.0064(12) 0.0138(12) 0.0153(11) C62 0.0328(14) 0.0392(15) 0.0546(18) 0.0037(13) 0.0156(13) 0.0134(12) C63 0.0482(18) 0.0485(18) 0.0500(18) 0.0053(14) 0.0179(15) 0.0232(15) C64 0.0449(17) 0.0366(16) 0.055(2) 0.0016(14) 0.0057(15) 0.0159(14) C65 0.0319(15) 0.0379(16) 0.070(2) 0.0058(15) 0.0079(15) 0.0070(13) C66 0.0355(15) 0.0386(16) 0.062(2) 0.0126(14) 0.0206(14) 0.0123(13) C67 0.0325(14) 0.0374(14) 0.0397(15) 0.0073(12) 0.0079(12) 0.0147(12) C68 0.0407(16) 0.0375(15) 0.0504(18) 0.0062(13) 0.0091(14) 0.0158(13) C69 0.0447(18) 0.0368(17) 0.071(2) 0.0095(16) 0.0078(17) 0.0090(14) C71 0.0362(17) 0.060(2) 0.086(3) 0.0207(19) 0.0231(17) 0.0222(16) C70 0.0309(16) 0.056(2) 0.070(2) 0.0181(18) 0.0104(15) 0.0079(15) C72 0.0360(16) 0.0425(17) 0.077(2) 0.0109(16) 0.0195(16) 0.0183(14) O10 0.114(4) 0.115(3) 0.170(5) 0.017(3) 0.009(3) 0.069(3) _geom_special_details ; ? ; 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 O1 2.410(2) . y Ag1 P1 2.4316(7) . y Ag1 P2 2.4394(7) . y P1 C13 1.819(3) . y P1 C7 1.827(3) . y P1 C1 1.833(3) . y P2 C25 1.823(3) . y P2 C19 1.824(3) . y P2 C31 1.829(3) . y S1 O1 1.431(2) . y S1 O2 1.436(2) . y S1 O4 1.472(3) . y S1 O3 1.538(3) . y C1 C6 1.387(4) . ? C1 C2 1.400(4) . ? C2 C3 1.388(4) . ? C3 C4 1.378(5) . ? C4 C5 1.374(5) . ? C5 C6 1.388(4) . ? C7 C12 1.386(4) . ? C7 C8 1.394(4) . ? C8 C9 1.386(4) . ? C9 C10 1.375(5) . ? C10 C11 1.380(6) . ? C11 C12 1.393(5) . ? C13 C18 1.388(4) . ? C13 C14 1.404(4) . ? C14 C15 1.382(5) . ? C15 C16 1.375(6) . ? C16 C17 1.377(6) . ? C17 C18 1.399(5) . ? C19 C24 1.391(4) . ? C19 C20 1.402(4) . ? C20 C21 1.382(4) . ? C21 C22 1.389(5) . ? C22 C23 1.381(5) . ? C23 C24 1.393(4) . ? C25 C26 1.391(4) . ? C25 C30 1.398(4) . ? C26 C27 1.396(4) . ? C27 C28 1.374(5) . ? C28 C29 1.378(5) . ? C29 C30 1.386(5) . ? C31 C32 1.387(4) . ? C31 C36 1.392(4) . ? C32 C33 1.389(4) . ? C33 C34 1.382(5) . ? C34 C35 1.385(5) . ? C35 C36 1.386(4) . ? Ag2 O5 2.412(2) . y Ag2 P4 2.4265(8) . y Ag2 P3 2.4300(7) . y Ag2 O9 2.446(3) . y P3 C49 1.814(3) . ?y P3 C37 1.821(3) . y P3 C43 1.828(3) . y P4 C61 1.824(3) . y P4 C55 1.824(3) . y P4 C67 1.825(3) . y S2 O5 1.441(2) . y S2 O8 1.450(3) . y S2 O7 1.470(3) . y S2 O6 1.532(2) . y C37 C42 1.386(4) . ? C37 C38 1.394(4) . ? C38 C39 1.381(5) . ? C39 C40 1.380(5) . ? C40 C41 1.364(5) . ? C41 C42 1.392(4) . ? C43 C48 1.387(4) . ? C43 C44 1.399(4) . ? C44 C45 1.389(4) . ? C45 C46 1.383(5) . ? C46 C47 1.378(5) . ? C47 C48 1.397(4) . ? C49 C54 1.396(4) . ? C49 C50 1.401(4) . ? C50 C51 1.381(4) . ? C51 C52 1.380(5) . ? C52 C53 1.386(5) . ? C53 C54 1.388(4) . ? C55 C60 1.388(5) . ? C55 C56 1.396(4) . ? C56 C57 1.389(5) . ? C57 C58 1.380(6) . ? C58 C59 1.381(6) . ? C59 C60 1.397(5) . ? C61 C62 1.391(4) . ? C61 C66 1.401(4) . ? C62 C63 1.392(5) . ? C63 C64 1.381(4) . ? C64 C65 1.381(5) . ? C65 C66 1.385(5) . ? C67 C68 1.391(4) . ? C67 C72 1.397(4) . ? C68 C69 1.392(5) . ? C69 C70 1.371(5) . ? C71 C70 1.376(5) . ? C71 C72 1.389(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 P1 113.72(8) . . y O1 Ag1 P2 103.15(8) . . y P1 Ag1 P2 131.38(2) . . y C13 P1 C7 104.65(13) . . ? C13 P1 C1 105.21(13) . . ? C7 P1 C1 105.54(12) . . ? C13 P1 Ag1 118.58(10) . . ? C7 P1 Ag1 107.37(9) . . ? C1 P1 Ag1 114.38(9) . . ? C25 P2 C19 103.72(12) . . ? C25 P2 C31 104.47(12) . . ? C19 P2 C31 104.88(12) . . ? C25 P2 Ag1 121.01(9) . . ? C19 P2 Ag1 108.01(9) . . ? C31 P2 Ag1 113.29(9) . . ? O1 S1 O2 114.13(15) . . ? O1 S1 O4 111.1(2) . . ? O2 S1 O4 111.15(18) . . ? O1 S1 O3 107.89(17) . . ? O2 S1 O3 106.94(17) . . ? O4 S1 O3 105.12(18) . . ? S1 O1 Ag1 133.14(14) . . ? C6 C1 C2 118.7(3) . . ? C6 C1 P1 123.6(2) . . ? C2 C1 P1 117.6(2) . . ? C3 C2 C1 120.4(3) . . ? C4 C3 C2 120.3(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 121.0(3) . . ? C1 C6 C5 120.1(3) . . ? C12 C7 C8 118.9(3) . . ? C12 C7 P1 123.9(2) . . ? C8 C7 P1 117.0(2) . . ? C9 C8 C7 120.4(3) . . ? C10 C9 C8 120.4(3) . . ? C9 C10 C11 119.8(3) . . ? C10 C11 C12 120.2(3) . . ? C7 C12 C11 120.3(3) . . ? C18 C13 C14 119.3(3) . . ? C18 C13 P1 118.1(2) . . ? C14 C13 P1 122.7(2) . . ? C15 C14 C13 120.4(3) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C17 120.2(3) . . ? C16 C17 C18 120.7(4) . . ? C13 C18 C17 119.4(3) . . ? C24 C19 C20 119.0(3) . . ? C24 C19 P2 123.4(2) . . ? C20 C19 P2 117.6(2) . . ? C21 C20 C19 120.2(3) . . ? C20 C21 C22 120.4(3) . . ? C23 C22 C21 119.9(3) . . ? C22 C23 C24 120.1(3) . . ? C19 C24 C23 120.5(3) . . ? C26 C25 C30 118.8(3) . . ? C26 C25 P2 123.0(2) . . ? C30 C25 P2 118.3(2) . . ? C25 C26 C27 120.3(3) . . ? C28 C27 C26 120.4(3) . . ? C27 C28 C29 119.7(3) . . ? C28 C29 C30 120.7(3) . . ? C29 C30 C25 120.1(3) . . ? C32 C31 C36 118.7(3) . . ? C32 C31 P2 122.9(2) . . ? C36 C31 P2 118.4(2) . . ? C31 C32 C33 120.7(3) . . ? C34 C33 C32 120.3(3) . . ? C33 C34 C35 119.2(3) . . ? C34 C35 C36 120.6(3) . . ? C35 C36 C31 120.4(3) . . ? O5 Ag2 P4 110.46(6) . . y O5 Ag2 P3 108.28(6) . . y P4 Ag2 P3 130.48(3) . . y O5 Ag2 O9 84.92(10) . . y P4 Ag2 O9 105.70(13) . . y P3 Ag2 O9 107.32(11) . . y C49 P3 C37 103.95(13) . . ? C49 P3 C43 104.82(13) . . ? C37 P3 C43 105.44(12) . . ? C49 P3 Ag2 116.83(9) . . ? C37 P3 Ag2 107.47(9) . . ? C43 P3 Ag2 117.04(9) . . ? C61 P4 C55 104.88(14) . . ? C61 P4 C67 104.94(13) . . ? C55 P4 C67 104.74(13) . . ? C61 P4 Ag2 109.99(9) . . ? C55 P4 Ag2 119.20(10) . . ? C67 P4 Ag2 111.96(10) . . ? O5 S2 O8 113.40(15) . . ? O5 S2 O7 111.61(16) . . ? O8 S2 O7 109.5(2) . . ? O5 S2 O6 106.08(14) . . ? O8 S2 O6 108.86(17) . . ? O7 S2 O6 107.10(15) . . ? S2 O5 Ag2 136.00(13) . . ? C42 C37 C38 118.6(3) . . ? C42 C37 P3 124.1(2) . . ? C38 C37 P3 117.0(2) . . ? C39 C38 C37 120.5(3) . . ? C40 C39 C38 120.4(3) . . ? C41 C40 C39 119.5(3) . . ? C40 C41 C42 121.0(3) . . ? C37 C42 C41 120.0(3) . . ? C48 C43 C44 118.9(3) . . ? C48 C43 P3 122.9(2) . . ? C44 C43 P3 118.1(2) . . ? C45 C44 C43 120.6(3) . . ? C46 C45 C44 120.0(3) . . ? C47 C46 C45 120.0(3) . . ? C46 C47 C48 120.4(3) . . ? C43 C48 C47 120.2(3) . . ? C54 C49 C50 119.1(3) . . ? C54 C49 P3 118.4(2) . . ? C50 C49 P3 122.5(2) . . ? C51 C50 C49 120.3(3) . . ? C52 C51 C50 120.4(3) . . ? C51 C52 C53 119.9(3) . . ? C52 C53 C54 120.4(3) . . ? C53 C54 C49 119.9(3) . . ? C60 C55 C56 119.0(3) . . ? C60 C55 P4 117.7(2) . . ? C56 C55 P4 123.3(3) . . ? C57 C56 C55 120.2(4) . . ? C58 C57 C56 120.2(4) . . ? C57 C58 C59 120.3(3) . . ? C58 C59 C60 119.6(4) . . ? C55 C60 C59 120.7(3) . . ? C62 C61 C66 118.2(3) . . ? C62 C61 P4 124.3(2) . . ? C66 C61 P4 117.4(2) . . ? C61 C62 C63 120.9(3) . . ? C64 C63 C62 120.1(3) . . ? C65 C64 C63 119.7(3) . . ? C64 C65 C66 120.5(3) . . ? C65 C66 C61 120.6(3) . . ? C68 C67 C72 118.4(3) . . ? C68 C67 P4 118.9(2) . . ? C72 C67 P4 122.7(2) . . ? C67 C68 C69 120.5(3) . . ? C70 C69 C68 120.4(3) . . ? C70 C71 C72 120.2(3) . . ? C69 C70 C71 120.0(3) . . ? C71 C72 C67 120.5(3) . . ? 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 O9 H9C O10 1.02(2) 1.93(4) 2.722(6) 132(4) . O3 H3B O7 1.06(5) 1.61(5) 2.641(4) 162(4) . O6 H6B O4 0.74(4) 1.88(4) 2.608(4) 167(5) . O9 H9B O8 0.904(19) 1.95(3) 2.793(4) 154(5) . O10 H10C O2 0.928(19) 2.13(5) 2.910(5) 141(6) 1_665 _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.07 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 2.090 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.065 #===END data_gab9969 #Compound 4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H33 Ag O5 P2 Se' _chemical_formula_weight 794.39 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' 'O' 'O' 0.0106 0.0060 '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5358(2) _cell_length_b 13.2580(2) _cell_length_c 24.5566(2) _cell_angle_alpha 104.3870(10) _cell_angle_beta 91.6760(10) _cell_angle_gamma 117.4040(10) _cell_volume 3460.39(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7524 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.767 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.5240 _exptl_absorpt_correction_T_max 0.8028 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32862 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.87 _diffrn_reflns_theta_max 26.73 _reflns_number_total 14255 _reflns_number_gt 11986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+15.3110P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14255 _refine_ls_number_parameters 824 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 1.010 _refine_ls_shift/su_mean 0.011 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.26357(4) 0.74018(3) 0.133636(17) 0.03299(10) Uani 1 d . . . Se1 Se 0.05687(6) 0.53759(6) 0.20527(3) 0.05655(19) Uani 1 d . . . P1 P 0.37589(12) 0.64261(11) 0.08810(6) 0.0310(3) Uani 1 d . . . P2 P 0.21906(12) 0.88698(12) 0.11098(6) 0.0304(3) Uani 1 d . . . O1 O 0.0869(4) 0.5732(5) 0.14820(19) 0.0745(17) Uani 1 d . . . O2 O -0.0764(5) 0.4295(5) 0.1997(2) 0.0861(19) Uani 1 d . . . O3 O 0.1601(5) 0.5150(5) 0.2332(3) 0.100(2) Uani 1 d . . . O4 O 0.0653(5) 0.6576(5) 0.2535(2) 0.0823(17) Uani 1 d . . . H4 H 0.179(8) 0.759(8) 0.266(4) 0.099 Uiso 1 d . . . C1 C 0.3037(5) 0.5691(4) 0.0137(2) 0.0326(11) Uani 1 d . . . C2 C 0.1764(5) 0.4996(5) 0.0018(3) 0.0438(13) Uani 1 d . . . H2B H 0.1314 0.4914 0.0324 0.053 Uiso 1 calc R . . C3 C 0.1156(6) 0.4431(5) -0.0535(3) 0.0506(15) Uani 1 d . . . H3B H 0.0292 0.3967 -0.0609 0.061 Uiso 1 calc R . . C4 C 0.1809(6) 0.4540(5) -0.0984(3) 0.0480(14) Uani 1 d . . . H4B H 0.1393 0.4144 -0.1366 0.058 Uiso 1 calc R . . C5 C 0.3059(5) 0.5224(5) -0.0875(2) 0.0428(13) Uani 1 d . . . H5A H 0.3502 0.5307 -0.1183 0.051 Uiso 1 calc R . . C6 C 0.3673(5) 0.5790(5) -0.0320(2) 0.0364(12) Uani 1 d . . . H6A H 0.4536 0.6250 -0.0249 0.044 Uiso 1 calc R . . C7 C 0.5333(4) 0.7471(4) 0.0858(2) 0.0311(10) Uani 1 d . . . C8 C 0.6243(5) 0.7150(5) 0.0819(3) 0.0433(13) Uani 1 d . . . H8A H 0.6060 0.6366 0.0811 0.052 Uiso 1 calc R . . C9 C 0.7422(5) 0.7969(6) 0.0790(3) 0.0542(17) Uani 1 d . . . H9A H 0.8034 0.7735 0.0755 0.065 Uiso 1 calc R . . C10 C 0.7710(5) 0.9104(6) 0.0811(3) 0.0521(16) Uani 1 d . . . H10A H 0.8521 0.9662 0.0799 0.063 Uiso 1 calc R . . C11 C 0.6812(6) 0.9438(6) 0.0849(3) 0.0620(19) Uani 1 d . . . H11A H 0.7000 1.0219 0.0849 0.074 Uiso 1 calc R . . C12 C 0.5632(5) 0.8628(5) 0.0887(3) 0.0487(15) Uani 1 d . . . H12A H 0.5029 0.8872 0.0932 0.058 Uiso 1 calc R . . C13 C 0.3856(5) 0.5257(5) 0.1113(2) 0.0332(11) Uani 1 d . . . C14 C 0.3391(5) 0.4100(5) 0.0763(3) 0.0403(12) Uani 1 d . . . H14A H 0.3011 0.3890 0.0382 0.048 Uiso 1 calc R . . C15 C 0.3478(5) 0.3245(5) 0.0967(3) 0.0457(14) Uani 1 d . . . H15A H 0.3166 0.2457 0.0723 0.055 Uiso 1 calc R . . C16 C 0.4013(6) 0.3536(6) 0.1519(3) 0.0503(15) Uani 1 d . . . H16A H 0.4051 0.2946 0.1661 0.060 Uiso 1 calc R . . C17 C 0.4495(7) 0.4691(6) 0.1868(3) 0.0564(17) Uani 1 d . . . H17A H 0.4885 0.4898 0.2247 0.068 Uiso 1 calc R . . C18 C 0.4415(6) 0.5547(5) 0.1671(3) 0.0503(15) Uani 1 d . . . H18A H 0.4741 0.6336 0.1916 0.060 Uiso 1 calc R . . C19 C 0.1395(5) 0.8419(5) 0.0386(2) 0.0339(11) Uani 1 d . . . C20 C 0.0517(5) 0.8722(5) 0.0245(3) 0.0427(13) Uani 1 d . . . H20A H 0.0333 0.9219 0.0531 0.051 Uiso 1 calc R . . C21 C -0.0086(6) 0.8302(6) -0.0309(3) 0.0529(16) Uani 1 d . . . H21A H -0.0676 0.8521 -0.0401 0.063 Uiso 1 calc R . . C22 C 0.0161(6) 0.7562(6) -0.0734(3) 0.0509(15) Uani 1 d . . . H22A H -0.0262 0.7269 -0.1114 0.061 Uiso 1 calc R . . C23 C 0.1023(6) 0.7261(6) -0.0598(3) 0.0509(15) Uani 1 d . . . H23A H 0.1204 0.6767 -0.0888 0.061 Uiso 1 calc R . . C24 C 0.1634(5) 0.7664(5) -0.0046(2) 0.0412(13) Uani 1 d . . . H24A H 0.2216 0.7432 0.0042 0.049 Uiso 1 calc R . . C25 C 0.1349(5) 0.9424(5) 0.1564(2) 0.0364(12) Uani 1 d . . . C26 C 0.1368(5) 1.0505(5) 0.1593(3) 0.0445(14) Uani 1 d . . . H26A H 0.1856 1.0988 0.1374 0.053 Uiso 1 calc R . . C27 C 0.0678(6) 1.0873(7) 0.1940(3) 0.0610(19) Uani 1 d . . . H27A H 0.0689 1.1600 0.1954 0.073 Uiso 1 calc R . . C28 C -0.0015(7) 1.0190(8) 0.2261(4) 0.077(2) Uani 1 d . . . H28A H -0.0488 1.0443 0.2495 0.093 Uiso 1 calc R . . C29 C -0.0036(7) 0.9132(8) 0.2248(4) 0.076(2) Uani 1 d . . . H29A H -0.0508 0.8675 0.2480 0.091 Uiso 1 calc R . . C30 C 0.0634(5) 0.8732(6) 0.1897(3) 0.0513(15) Uani 1 d . . . H30A H 0.0605 0.7997 0.1883 0.062 Uiso 1 calc R . . C31 C 0.3639(4) 1.0175(4) 0.1157(2) 0.0326(11) Uani 1 d . . . C32 C 0.4415(5) 1.0745(5) 0.1687(3) 0.0431(13) Uani 1 d . . . H32A H 0.4143 1.0474 0.2007 0.052 Uiso 1 calc R . . C33 C 0.5573(6) 1.1699(6) 0.1752(3) 0.0578(17) Uani 1 d . . . H33A H 0.6079 1.2091 0.2115 0.069 Uiso 1 calc R . . C34 C 0.5988(6) 1.2074(6) 0.1288(4) 0.0583(18) Uani 1 d . . . H34A H 0.6788 1.2712 0.1329 0.070 Uiso 1 calc R . . C35 C 0.5241(6) 1.1524(6) 0.0764(3) 0.0558(17) Uani 1 d . . . H35A H 0.5531 1.1790 0.0446 0.067 Uiso 1 calc R . . C36 C 0.4059(5) 1.0578(5) 0.0693(3) 0.0413(13) Uani 1 d . . . H36A H 0.3548 1.0214 0.0331 0.050 Uiso 1 calc R . . Ag2 Ag 0.66651(4) 1.09403(4) 0.368668(18) 0.03664(10) Uani 1 d . . . Se2 Se 0.41015(6) 0.82432(5) 0.27488(2) 0.04668(16) Uani 1 d . . . P3 P 0.80145(12) 1.03626(13) 0.40888(7) 0.0376(3) Uani 1 d . . . P4 P 0.63961(12) 1.26792(11) 0.40202(6) 0.0311(3) Uani 1 d . . . O5 O 0.4684(3) 0.9220(4) 0.33660(16) 0.0500(11) Uani 1 d . . . O6 O 0.2871(4) 0.8167(4) 0.2470(2) 0.0644(13) Uani 1 d . . . O7 O 0.3696(5) 0.6923(4) 0.28684(19) 0.0575(12) Uani 1 d . . . H7B H 0.294(7) 0.642(7) 0.270(3) 0.069 Uiso 1 d . . . O8 O 0.5043(5) 0.8426(4) 0.2296(2) 0.0764(16) Uani 1 d . . . O9 O 0.6908(7) 1.0760(5) 0.2691(2) 0.103(2) Uani 1 d D . . H9B H 0.727(7) 1.061(7) 0.237(3) 0.124 Uiso 1 d D . . H9C H 0.615(4) 1.006(5) 0.259(4) 0.124 Uiso 1 d D . . C37 C 0.9614(5) 1.1367(5) 0.4090(2) 0.0380(12) Uani 1 d . . . C38 C 0.9924(5) 1.2451(5) 0.4001(3) 0.0466(14) Uani 1 d . . . H38A H 0.9303 1.2639 0.3920 0.056 Uiso 1 calc R . . C39 C 1.1143(6) 1.3272(5) 0.4030(3) 0.0546(17) Uani 1 d . . . H39A H 1.1351 1.4016 0.3969 0.066 Uiso 1 calc R . . C40 C 1.2043(6) 1.2999(6) 0.4147(3) 0.0581(18) Uani 1 d . . . H40A H 1.2873 1.3559 0.4170 0.070 Uiso 1 calc R . . C41 C 1.1750(5) 1.1921(6) 0.4232(3) 0.0570(17) Uani 1 d . . . H41A H 1.2374 1.1736 0.4314 0.068 Uiso 1 calc R . . C42 C 1.0543(5) 1.1109(6) 0.4198(3) 0.0509(15) Uani 1 d . . . H42A H 1.0341 1.0359 0.4250 0.061 Uiso 1 calc R . . C43 C 0.7895(5) 1.0464(5) 0.4838(2) 0.0359(12) Uani 1 d . . . C44 C 0.6717(5) 0.9914(5) 0.4973(3) 0.0465(14) Uani 1 d . . . H44A H 0.6028 0.9464 0.4678 0.056 Uiso 1 calc R . . C45 C 0.6561(6) 1.0029(6) 0.5539(3) 0.0520(16) Uani 1 d . . . H45A H 0.5765 0.9654 0.5629 0.062 Uiso 1 calc R . . C46 C 0.7548(6) 1.0680(5) 0.5968(3) 0.0489(15) Uani 1 d . . . H46A H 0.7433 1.0755 0.6354 0.059 Uiso 1 calc R . . C47 C 0.8711(6) 1.1229(6) 0.5843(3) 0.0470(14) Uani 1 d . . . H47A H 0.9393 1.1679 0.6143 0.056 Uiso 1 calc R . . C48 C 0.8880(5) 1.1121(5) 0.5280(3) 0.0425(13) Uani 1 d . . . H48A H 0.9681 1.1502 0.5196 0.051 Uiso 1 calc R . . C49 C 0.7809(5) 0.8874(5) 0.3772(3) 0.0406(13) Uani 1 d . . . C50 C 0.8023(5) 0.8219(5) 0.4084(3) 0.0485(15) Uani 1 d . . . H50A H 0.8242 0.8527 0.4487 0.058 Uiso 1 calc R . . C51 C 0.7918(6) 0.7119(6) 0.3808(4) 0.0581(18) Uani 1 d . . . H51A H 0.8079 0.6686 0.4023 0.070 Uiso 1 calc R . . C52 C 0.7584(6) 0.6656(6) 0.3229(4) 0.065(2) Uani 1 d . . . H52A H 0.7520 0.5906 0.3044 0.078 Uiso 1 calc R . . C53 C 0.7335(7) 0.7277(6) 0.2908(3) 0.0631(19) Uani 1 d . . . H53A H 0.7094 0.6950 0.2506 0.076 Uiso 1 calc R . . C54 C 0.7445(6) 0.8377(6) 0.3181(3) 0.0526(15) Uani 1 d . . . H54A H 0.7271 0.8801 0.2964 0.063 Uiso 1 calc R . . C55 C 0.5277(5) 1.2778(5) 0.3580(2) 0.0327(11) Uani 1 d . . . C56 C 0.5410(6) 1.3860(5) 0.3537(2) 0.0413(13) Uani 1 d . . . H56A H 0.6122 1.4581 0.3732 0.050 Uiso 1 calc R . . C57 C 0.4512(6) 1.3888(6) 0.3213(3) 0.0521(16) Uani 1 d . . . H57A H 0.4608 1.4627 0.3186 0.063 Uiso 1 calc R . . C58 C 0.3479(6) 1.2850(6) 0.2929(2) 0.0534(16) Uani 1 d . . . H58A H 0.2864 1.2875 0.2706 0.064 Uiso 1 calc R . . C59 C 0.3329(6) 1.1775(6) 0.2966(2) 0.0486(15) Uani 1 d . . . H59A H 0.2611 1.1060 0.2770 0.058 Uiso 1 calc R . . C60 C 0.4224(5) 1.1734(5) 0.3290(2) 0.0398(12) Uani 1 d . . . H60A H 0.4120 1.0991 0.3313 0.048 Uiso 1 calc R . . C61 C 0.6054(4) 1.2983(4) 0.4742(2) 0.0323(11) Uani 1 d . . . C62 C 0.6533(5) 1.2668(5) 0.5147(2) 0.0404(12) Uani 1 d . . . H62A H 0.7057 1.2339 0.5048 0.048 Uiso 1 calc R . . C63 C 0.6258(6) 1.2827(5) 0.5693(2) 0.0468(14) Uani 1 d . . . H63A H 0.6588 1.2601 0.5965 0.056 Uiso 1 calc R . . C64 C 0.5508(6) 1.3310(5) 0.5842(3) 0.0484(15) Uani 1 d . . . H64A H 0.5326 1.3426 0.6218 0.058 Uiso 1 calc R . . C65 C 0.5016(6) 1.3629(6) 0.5446(3) 0.0506(15) Uani 1 d . . . H65A H 0.4495 1.3960 0.5550 0.061 Uiso 1 calc R . . C66 C 0.5284(5) 1.3465(5) 0.4894(2) 0.0404(13) Uani 1 d . . . H66A H 0.4943 1.3682 0.4622 0.048 Uiso 1 calc R . . C67 C 0.7842(5) 1.3970(5) 0.4030(2) 0.0346(11) Uani 1 d . . . C68 C 0.8270(6) 1.4004(6) 0.3515(3) 0.0532(16) Uani 1 d . . . H68A H 0.7778 1.3409 0.3172 0.064 Uiso 1 calc R . . C69 C 0.9411(7) 1.4899(6) 0.3499(3) 0.0630(19) Uani 1 d . . . H69A H 0.9696 1.4920 0.3146 0.076 Uiso 1 calc R . . C70 C 1.0129(6) 1.5756(6) 0.3993(3) 0.0573(18) Uani 1 d . . . H70A H 1.0919 1.6359 0.3983 0.069 Uiso 1 calc R . . C71 C 0.9707(6) 1.5741(6) 0.4496(3) 0.0536(16) Uani 1 d . . . H71A H 1.0204 1.6346 0.4835 0.064 Uiso 1 calc R . . C72 C 0.8558(5) 1.4854(5) 0.4524(2) 0.0427(13) Uani 1 d . . . H72A H 0.8272 1.4857 0.4878 0.051 Uiso 1 calc R . . O10 O 0.8702(9) 1.2132(8) 0.2207(4) 0.146(3) Uiso 1 d D . . H10B H 0.932(8) 1.257(9) 0.253(3) 0.175 Uiso 1 d D . . H10C H 0.860(11) 1.274(7) 0.213(5) 0.175 Uiso 1 d 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 0.0371(2) 0.0344(2) 0.0335(2) 0.01545(16) 0.01218(16) 0.01901(17) Se1 0.0516(4) 0.0503(4) 0.0394(3) 0.0214(3) 0.0013(3) -0.0019(3) P1 0.0318(7) 0.0270(6) 0.0371(7) 0.0129(5) 0.0105(5) 0.0146(5) P2 0.0283(6) 0.0322(7) 0.0340(7) 0.0142(5) 0.0089(5) 0.0149(5) O1 0.058(3) 0.073(3) 0.040(2) 0.027(2) 0.003(2) -0.015(2) O2 0.063(3) 0.073(4) 0.070(3) 0.037(3) 0.008(3) -0.018(3) O3 0.080(4) 0.064(4) 0.125(5) 0.029(4) -0.038(4) 0.012(3) O4 0.080(4) 0.073(4) 0.072(4) 0.024(3) 0.033(3) 0.016(3) C1 0.034(3) 0.025(2) 0.043(3) 0.016(2) 0.010(2) 0.014(2) C2 0.034(3) 0.043(3) 0.050(3) 0.018(3) 0.010(3) 0.012(3) C3 0.040(3) 0.045(3) 0.052(4) 0.017(3) -0.003(3) 0.007(3) C4 0.053(4) 0.043(3) 0.040(3) 0.009(3) -0.003(3) 0.018(3) C5 0.052(3) 0.044(3) 0.041(3) 0.017(3) 0.013(3) 0.027(3) C6 0.035(3) 0.034(3) 0.043(3) 0.016(2) 0.012(2) 0.017(2) C7 0.030(3) 0.030(3) 0.032(3) 0.011(2) 0.007(2) 0.012(2) C8 0.039(3) 0.035(3) 0.059(4) 0.016(3) 0.011(3) 0.019(3) C9 0.032(3) 0.054(4) 0.081(5) 0.019(3) 0.010(3) 0.024(3) C10 0.034(3) 0.051(4) 0.064(4) 0.023(3) 0.011(3) 0.011(3) C11 0.051(4) 0.039(3) 0.101(6) 0.030(4) 0.022(4) 0.020(3) C12 0.041(3) 0.035(3) 0.078(5) 0.027(3) 0.021(3) 0.020(3) C13 0.033(3) 0.033(3) 0.039(3) 0.017(2) 0.015(2) 0.017(2) C14 0.040(3) 0.034(3) 0.050(3) 0.016(3) 0.008(3) 0.019(2) C15 0.042(3) 0.030(3) 0.067(4) 0.019(3) 0.012(3) 0.016(3) C16 0.051(4) 0.049(4) 0.066(4) 0.038(3) 0.018(3) 0.026(3) C17 0.073(5) 0.056(4) 0.047(4) 0.028(3) 0.012(3) 0.030(4) C18 0.071(4) 0.040(3) 0.039(3) 0.014(3) 0.011(3) 0.025(3) C19 0.031(3) 0.033(3) 0.037(3) 0.016(2) 0.008(2) 0.012(2) C20 0.035(3) 0.041(3) 0.050(3) 0.011(3) 0.001(2) 0.018(3) C21 0.047(3) 0.053(4) 0.059(4) 0.022(3) -0.003(3) 0.023(3) C22 0.047(3) 0.056(4) 0.041(3) 0.017(3) -0.001(3) 0.016(3) C23 0.050(4) 0.056(4) 0.039(3) 0.012(3) 0.011(3) 0.020(3) C24 0.043(3) 0.044(3) 0.037(3) 0.010(2) 0.007(2) 0.023(3) C25 0.029(3) 0.041(3) 0.038(3) 0.008(2) 0.007(2) 0.017(2) C26 0.036(3) 0.048(3) 0.049(3) 0.007(3) 0.001(3) 0.023(3) C27 0.054(4) 0.066(4) 0.066(4) -0.002(4) 0.003(3) 0.042(4) C28 0.059(5) 0.095(6) 0.081(6) 0.008(5) 0.028(4) 0.048(5) C29 0.054(4) 0.099(7) 0.074(5) 0.031(5) 0.035(4) 0.032(4) C30 0.039(3) 0.058(4) 0.058(4) 0.025(3) 0.021(3) 0.020(3) C31 0.029(2) 0.031(3) 0.045(3) 0.014(2) 0.009(2) 0.019(2) C32 0.038(3) 0.043(3) 0.048(3) 0.016(3) 0.004(3) 0.018(3) C33 0.038(3) 0.047(4) 0.077(5) 0.011(3) -0.003(3) 0.016(3) C34 0.034(3) 0.039(3) 0.098(6) 0.024(4) 0.014(3) 0.012(3) C35 0.051(4) 0.049(4) 0.079(5) 0.035(4) 0.030(4) 0.024(3) C36 0.043(3) 0.035(3) 0.050(3) 0.021(3) 0.016(3) 0.018(3) Ag2 0.0344(2) 0.0317(2) 0.0402(2) 0.00748(17) 0.00158(17) 0.01485(17) Se2 0.0552(4) 0.0350(3) 0.0313(3) 0.0042(2) -0.0040(3) 0.0103(3) P3 0.0290(7) 0.0330(7) 0.0507(9) 0.0148(6) 0.0066(6) 0.0138(6) P4 0.0325(7) 0.0278(6) 0.0296(6) 0.0092(5) 0.0041(5) 0.0117(5) O5 0.035(2) 0.048(2) 0.036(2) -0.0038(18) 0.0045(17) 0.0024(18) O6 0.057(3) 0.047(3) 0.070(3) 0.022(2) -0.011(2) 0.009(2) O7 0.068(3) 0.043(3) 0.048(3) 0.016(2) -0.007(2) 0.017(2) O8 0.111(4) 0.055(3) 0.043(3) 0.012(2) 0.032(3) 0.024(3) O9 0.125(5) 0.077(4) 0.051(3) 0.017(3) 0.034(3) 0.002(4) C37 0.030(3) 0.036(3) 0.043(3) 0.012(2) 0.010(2) 0.011(2) C38 0.043(3) 0.043(3) 0.057(4) 0.020(3) 0.013(3) 0.020(3) C39 0.048(4) 0.036(3) 0.073(5) 0.025(3) 0.022(3) 0.009(3) C40 0.036(3) 0.053(4) 0.074(5) 0.022(3) 0.022(3) 0.010(3) C41 0.033(3) 0.055(4) 0.082(5) 0.021(4) 0.013(3) 0.020(3) C42 0.037(3) 0.045(3) 0.076(5) 0.025(3) 0.017(3) 0.020(3) C43 0.030(3) 0.032(3) 0.051(3) 0.017(2) 0.012(2) 0.016(2) C44 0.027(3) 0.036(3) 0.070(4) 0.017(3) 0.009(3) 0.009(2) C45 0.041(3) 0.048(4) 0.072(4) 0.030(3) 0.028(3) 0.019(3) C46 0.052(4) 0.047(3) 0.057(4) 0.025(3) 0.020(3) 0.026(3) C47 0.044(3) 0.053(4) 0.050(4) 0.020(3) 0.012(3) 0.026(3) C48 0.030(3) 0.041(3) 0.058(4) 0.021(3) 0.009(3) 0.016(2) C49 0.026(3) 0.031(3) 0.059(4) 0.012(3) 0.008(2) 0.010(2) C50 0.032(3) 0.036(3) 0.071(4) 0.016(3) 0.000(3) 0.011(2) C51 0.044(4) 0.036(3) 0.095(6) 0.022(4) 0.006(4) 0.019(3) C52 0.056(4) 0.037(3) 0.096(6) 0.014(4) 0.020(4) 0.020(3) C53 0.065(4) 0.044(4) 0.068(5) 0.008(3) 0.015(4) 0.019(3) C54 0.050(4) 0.045(4) 0.062(4) 0.020(3) 0.014(3) 0.020(3) C55 0.037(3) 0.037(3) 0.026(2) 0.011(2) 0.004(2) 0.019(2) C56 0.053(3) 0.036(3) 0.035(3) 0.012(2) 0.003(3) 0.022(3) C57 0.080(5) 0.056(4) 0.039(3) 0.019(3) 0.008(3) 0.045(4) C58 0.070(4) 0.073(5) 0.030(3) 0.010(3) 0.001(3) 0.047(4) C59 0.048(3) 0.055(4) 0.037(3) 0.004(3) -0.003(3) 0.025(3) C60 0.039(3) 0.041(3) 0.035(3) 0.010(2) 0.004(2) 0.017(3) C61 0.031(3) 0.029(3) 0.030(3) 0.011(2) 0.002(2) 0.009(2) C62 0.039(3) 0.047(3) 0.038(3) 0.017(3) 0.008(2) 0.021(3) C63 0.057(4) 0.052(4) 0.035(3) 0.021(3) 0.009(3) 0.025(3) C64 0.062(4) 0.045(3) 0.034(3) 0.013(3) 0.014(3) 0.021(3) C65 0.058(4) 0.056(4) 0.051(4) 0.022(3) 0.021(3) 0.035(3) C66 0.048(3) 0.046(3) 0.039(3) 0.017(3) 0.013(3) 0.030(3) C67 0.035(3) 0.032(3) 0.038(3) 0.013(2) 0.009(2) 0.015(2) C68 0.060(4) 0.042(3) 0.041(3) 0.010(3) 0.019(3) 0.012(3) C69 0.069(5) 0.057(4) 0.057(4) 0.027(3) 0.033(4) 0.019(4) C70 0.043(3) 0.048(4) 0.084(5) 0.037(4) 0.022(3) 0.016(3) C71 0.042(3) 0.040(3) 0.058(4) 0.014(3) 0.002(3) 0.004(3) C72 0.042(3) 0.038(3) 0.038(3) 0.010(2) 0.004(2) 0.012(3) _geom_special_details ; ; 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 O1 2.421(4) . y Ag1 P2 2.4349(13) . y Ag1 P1 2.4405(13) . y Se1 O1 1.589(4) . y Se1 O2 1.596(4) . y Se1 O3 1.626(6) . y Se1 O4 1.687(6) . y P1 C1 1.821(6) . y P1 C7 1.829(5) . y P1 C13 1.831(5) . y P2 C25 1.810(5) . y P2 C31 1.816(5) . y P2 C19 1.825(5) . y C1 C6 1.392(7) . ? C1 C2 1.403(7) . ? C2 C3 1.376(8) . ? C3 C4 1.390(9) . ? C4 C5 1.377(8) . ? C5 C6 1.383(8) . ? C7 C12 1.384(7) . ? C7 C8 1.388(7) . ? C8 C9 1.392(8) . ? C9 C10 1.363(9) . ? C10 C11 1.384(9) . ? C11 C12 1.395(8) . ? C13 C14 1.387(7) . ? C13 C18 1.396(8) . ? C14 C15 1.393(8) . ? C15 C16 1.373(9) . ? C16 C17 1.382(9) . ? C17 C18 1.380(8) . ? C19 C20 1.394(7) . ? C19 C24 1.409(8) . ? C20 C21 1.381(8) . ? C21 C22 1.392(9) . ? C22 C23 1.371(9) . ? C23 C24 1.383(8) . ? C25 C30 1.403(8) . ? C25 C26 1.406(8) . ? C26 C27 1.393(8) . ? C27 C28 1.365(11) . ? C28 C29 1.383(12) . ? C29 C30 1.400(10) . ? C31 C36 1.393(7) . ? C31 C32 1.404(8) . ? C32 C33 1.389(8) . ? C33 C34 1.375(10) . ? C34 C35 1.378(10) . ? C35 C36 1.402(8) . ? Ag2 O5 2.402(4) . y Ag2 P4 2.4275(14) . y Ag2 P3 2.4278(15) . y Ag2 O9 2.439(5) . y Se2 O5 1.611(4) . y Se2 O6 1.618(5) . y Se2 O8 1.624(5) . y Se2 O7 1.689(4) . y P3 C49 1.823(6) . y P3 C37 1.825(5) . y P3 C43 1.827(6) . y P4 C55 1.817(5) . y P4 C61 1.826(5) . y P4 C67 1.826(5) . y C37 C38 1.382(8) . ? C37 C42 1.392(8) . ? C38 C39 1.396(8) . ? C39 C40 1.377(9) . ? C40 C41 1.375(9) . ? C41 C42 1.380(8) . ? C43 C48 1.387(8) . ? C43 C44 1.408(7) . ? C44 C45 1.389(9) . ? C45 C46 1.369(9) . ? C46 C47 1.382(8) . ? C47 C48 1.388(8) . ? C49 C50 1.395(8) . ? C49 C54 1.399(9) . ? C50 C51 1.389(9) . ? C51 C52 1.367(11) . ? C52 C53 1.393(11) . ? C53 C54 1.386(9) . ? C55 C60 1.392(7) . ? C55 C56 1.399(7) . ? C56 C57 1.379(8) . ? C57 C58 1.373(9) . ? C58 C59 1.377(9) . ? C59 C60 1.385(8) . ? C61 C62 1.389(7) . ? C61 C66 1.397(7) . ? C62 C63 1.384(8) . ? C63 C64 1.374(9) . ? C64 C65 1.384(9) . ? C65 C66 1.395(8) . ? C67 C72 1.384(8) . ? C67 C68 1.392(8) . ? C68 C69 1.385(9) . ? C69 C70 1.371(10) . ? C70 C71 1.360(9) . ? C71 C72 1.397(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 P2 113.66(15) . . y O1 Ag1 P1 100.99(15) . . y P2 Ag1 P1 131.13(5) . . y O1 Se1 O2 114.5(2) . . ? O1 Se1 O3 112.4(3) . . ? O2 Se1 O3 111.0(3) . . ? O1 Se1 O4 106.5(3) . . ? O2 Se1 O4 107.1(3) . . ? O3 Se1 O4 104.6(3) . . ? C1 P1 C7 104.8(2) . . ? C1 P1 C13 103.5(2) . . ? C7 P1 C13 104.9(2) . . ? C1 P1 Ag1 107.16(17) . . ? C7 P1 Ag1 113.23(17) . . ? C13 P1 Ag1 121.70(17) . . ? C25 P2 C31 104.9(2) . . ? C25 P2 C19 105.0(2) . . ? C31 P2 C19 105.4(2) . . ? C25 P2 Ag1 118.39(19) . . ? C31 P2 Ag1 107.38(16) . . ? C19 P2 Ag1 114.66(18) . . ? Se1 O1 Ag1 129.0(2) . . ? C6 C1 C2 118.3(5) . . ? C6 C1 P1 123.9(4) . . ? C2 C1 P1 117.9(4) . . ? C3 C2 C1 121.0(6) . . ? C2 C3 C4 119.8(6) . . ? C5 C4 C3 119.9(6) . . ? C4 C5 C6 120.4(5) . . ? C5 C6 C1 120.6(5) . . ? C12 C7 C8 118.7(5) . . ? C12 C7 P1 118.9(4) . . ? C8 C7 P1 122.4(4) . . ? C7 C8 C9 120.4(5) . . ? C10 C9 C8 120.8(6) . . ? C9 C10 C11 119.6(6) . . ? C10 C11 C12 120.0(6) . . ? C7 C12 C11 120.5(5) . . ? C14 C13 C18 118.8(5) . . ? C14 C13 P1 123.1(4) . . ? C18 C13 P1 118.2(4) . . ? C13 C14 C15 120.4(6) . . ? C16 C15 C14 120.3(6) . . ? C15 C16 C17 119.6(6) . . ? C18 C17 C16 120.6(6) . . ? C17 C18 C13 120.2(6) . . ? C20 C19 C24 118.5(5) . . ? C20 C19 P2 123.8(4) . . ? C24 C19 P2 117.6(4) . . ? C21 C20 C19 120.4(6) . . ? C20 C21 C22 120.8(6) . . ? C23 C22 C21 119.1(6) . . ? C22 C23 C24 121.2(6) . . ? C23 C24 C19 120.1(6) . . ? C30 C25 C26 118.8(5) . . ? C30 C25 P2 118.2(4) . . ? C26 C25 P2 123.0(4) . . ? C27 C26 C25 120.5(6) . . ? C28 C27 C26 120.1(7) . . ? C27 C28 C29 120.7(7) . . ? C28 C29 C30 120.4(7) . . ? C29 C30 C25 119.5(7) . . ? C36 C31 C32 118.6(5) . . ? C36 C31 P2 124.0(4) . . ? C32 C31 P2 117.2(4) . . ? C33 C32 C31 121.0(6) . . ? C34 C33 C32 119.9(6) . . ? C33 C34 C35 120.0(6) . . ? C34 C35 C36 121.0(6) . . ? C31 C36 C35 119.6(6) . . ? O5 Ag2 P4 108.19(11) . . y O5 Ag2 P3 108.07(12) . . y P4 Ag2 P3 131.20(5) . . y O5 Ag2 O9 88.45(18) . . y P4 Ag2 O9 105.66(19) . . y P3 Ag2 O9 106.9(2) . . y O5 Se2 O6 112.6(2) . . ? O5 Se2 O8 113.8(2) . . ? O6 Se2 O8 109.3(3) . . ? O5 Se2 O7 105.3(2) . . ? O6 Se2 O7 106.9(2) . . ? O8 Se2 O7 108.5(3) . . ? C49 P3 C37 105.0(2) . . ? C49 P3 C43 104.6(3) . . ? C37 P3 C43 105.0(3) . . ? C49 P3 Ag2 118.84(19) . . ? C37 P3 Ag2 111.99(19) . . ? C43 P3 Ag2 110.25(17) . . ? C55 P4 C61 105.1(2) . . ? C55 P4 C67 104.5(2) . . ? C61 P4 C67 105.5(2) . . ? C55 P4 Ag2 117.16(17) . . ? C61 P4 Ag2 116.44(17) . . ? C67 P4 Ag2 106.94(17) . . ? Se2 O5 Ag2 129.8(2) . . ? C38 C37 C42 118.4(5) . . ? C38 C37 P3 118.7(4) . . ? C42 C37 P3 122.8(4) . . ? C37 C38 C39 120.6(6) . . ? C40 C39 C38 119.7(6) . . ? C41 C40 C39 120.5(6) . . ? C40 C41 C42 119.5(6) . . ? C41 C42 C37 121.4(6) . . ? C48 C43 C44 118.5(5) . . ? C48 C43 P3 124.0(4) . . ? C44 C43 P3 117.3(4) . . ? C45 C44 C43 120.0(6) . . ? C46 C45 C44 120.4(6) . . ? C45 C46 C47 120.4(6) . . ? C46 C47 C48 119.8(6) . . ? C43 C48 C47 120.8(5) . . ? C50 C49 C54 118.4(6) . . ? C50 C49 P3 123.7(5) . . ? C54 C49 P3 117.9(5) . . ? C51 C50 C49 120.3(7) . . ? C52 C51 C50 120.5(7) . . ? C51 C52 C53 120.4(7) . . ? C54 C53 C52 119.3(7) . . ? C53 C54 C49 121.0(7) . . ? C60 C55 C56 118.7(5) . . ? C60 C55 P4 118.5(4) . . ? C56 C55 P4 122.8(4) . . ? C57 C56 C55 120.4(6) . . ? C58 C57 C56 120.2(6) . . ? C57 C58 C59 120.4(6) . . ? C58 C59 C60 120.0(6) . . ? C59 C60 C55 120.4(6) . . ? C62 C61 C66 118.8(5) . . ? C62 C61 P4 118.5(4) . . ? C66 C61 P4 122.6(4) . . ? C63 C62 C61 121.0(5) . . ? C64 C63 C62 120.0(6) . . ? C63 C64 C65 120.2(6) . . ? C64 C65 C66 120.1(6) . . ? C65 C66 C61 119.9(5) . . ? C72 C67 C68 119.3(5) . . ? C72 C67 P4 123.3(4) . . ? C68 C67 P4 117.2(4) . . ? C69 C68 C67 120.3(6) . . ? C70 C69 C68 120.2(6) . . ? C71 C70 C69 119.8(6) . . ? C70 C71 C72 121.3(6) . . ? C67 C72 C71 119.1(6) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.196 _refine_diff_density_min -1.853 _refine_diff_density_rms 0.097 #===END data_gab9959 #Compound 5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Phosphatobis(triphenylphosphine)silver(I). 2Ethanol solvate ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H44 Ag O6 P3' _chemical_formula_weight 821.53 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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.10970(10) _cell_length_b 13.11210(10) _cell_length_c 16.00730(10) _cell_angle_alpha 73.10 _cell_angle_beta 77.5550(10) _cell_angle_gamma 78.8890(10) _cell_volume 1963.23(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8126 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.8018 _exptl_absorpt_correction_T_max 0.8874 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8235 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.04 _reflns_number_total 8235 _reflns_number_gt 7452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.6388P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8235 _refine_ls_number_parameters 465 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.096 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.608555(12) 0.760772(9) 0.710923(8) 0.02848(5) Uani 1 d . . . P1 P 0.65847(4) 0.92357(3) 0.73420(3) 0.02625(9) Uani 1 d . . . P2 P 0.74831(4) 0.65209(3) 0.61306(3) 0.02518(9) Uani 1 d . . . P3 P 0.40441(4) 0.62579(4) 0.84669(3) 0.02832(9) Uani 1 d . . . O1 O 0.39535(12) 0.70151(10) 0.75655(8) 0.0348(3) Uani 1 d . . . O2 O 0.54268(13) 0.60802(10) 0.87507(9) 0.0369(3) Uani 1 d . . . O3 O 0.36878(18) 0.51395(12) 0.84620(9) 0.0480(4) Uani 1 d . . . H3 H 0.365(3) 0.475(2) 0.8894(18) 0.058 Uiso 1 d . . . O4 O 0.29005(16) 0.67076(13) 0.91594(9) 0.0507(4) Uani 1 d . . . H4 H 0.296(3) 0.643(2) 0.9636(18) 0.061 Uiso 1 d . . . C11 C 0.52863(18) 0.98892(14) 0.80814(11) 0.0303(3) Uani 1 d . . . C12 C 0.5121(2) 1.09938(15) 0.80090(13) 0.0420(4) Uani 1 d . . . H12A H 0.5680 1.1442 0.7550 0.050 Uiso 1 calc R . . C13 C 0.4137(3) 1.14360(18) 0.86094(16) 0.0562(6) Uani 1 d . . . H13A H 0.4022 1.2187 0.8559 0.067 Uiso 1 calc R . . C14 C 0.3325(3) 1.0780(2) 0.92806(18) 0.0665(7) Uani 1 d . . . H14A H 0.2654 1.1083 0.9690 0.080 Uiso 1 calc R . . C15 C 0.3486(3) 0.9686(2) 0.93574(17) 0.0665(7) Uani 1 d . . . H15A H 0.2930 0.9239 0.9820 0.080 Uiso 1 calc R . . C16 C 0.4463(2) 0.92381(17) 0.87567(14) 0.0461(5) Uani 1 d . . . H16A H 0.4567 0.8488 0.8807 0.055 Uiso 1 calc R . . C21 C 0.82017(17) 0.91208(13) 0.77308(11) 0.0283(3) Uani 1 d . . . C22 C 0.8379(2) 0.97367(15) 0.82693(12) 0.0366(4) Uani 1 d . . . H22A H 0.7646 1.0246 0.8444 0.044 Uiso 1 calc R . . C23 C 0.9630(2) 0.96057(17) 0.85503(14) 0.0451(5) Uani 1 d . . . H23A H 0.9745 1.0027 0.8916 0.054 Uiso 1 calc R . . C24 C 1.0710(2) 0.88628(16) 0.82983(14) 0.0434(4) Uani 1 d . . . H24A H 1.1558 0.8775 0.8493 0.052 Uiso 1 calc R . . C25 C 1.0545(2) 0.82499(15) 0.77620(13) 0.0404(4) Uani 1 d . . . H25A H 1.1284 0.7746 0.7585 0.048 Uiso 1 calc R . . C26 C 0.93001(19) 0.83733(14) 0.74839(12) 0.0342(4) Uani 1 d . . . H26A H 0.9191 0.7946 0.7122 0.041 Uiso 1 calc R . . C31 C 0.67683(17) 1.02344(12) 0.62613(11) 0.0272(3) Uani 1 d . . . C32 C 0.80232(18) 1.05484(14) 0.58048(12) 0.0323(4) Uani 1 d . . . H32A H 0.8805 1.0324 0.6087 0.039 Uiso 1 calc R . . C33 C 0.8140(2) 1.11964(15) 0.49277(13) 0.0402(4) Uani 1 d . . . H33A H 0.9001 1.1403 0.4619 0.048 Uiso 1 calc R . . C34 C 0.7000(2) 1.15354(15) 0.45114(12) 0.0404(4) Uani 1 d . . . H34A H 0.7079 1.1969 0.3918 0.048 Uiso 1 calc R . . C35 C 0.5743(2) 1.12355(15) 0.49697(13) 0.0409(4) Uani 1 d . . . H35A H 0.4959 1.1476 0.4690 0.049 Uiso 1 calc R . . C36 C 0.56204(19) 1.05862(15) 0.58352(12) 0.0359(4) Uani 1 d . . . H36A H 0.4757 1.0380 0.6139 0.043 Uiso 1 calc R . . C41 C 0.91601(17) 0.61066(13) 0.64684(11) 0.0270(3) Uani 1 d . . . C42 C 0.9196(2) 0.56463(16) 0.73726(12) 0.0405(4) Uani 1 d . . . H42A H 0.8371 0.5530 0.7781 0.049 Uiso 1 calc R . . C43 C 1.0453(3) 0.53602(18) 0.76687(14) 0.0507(5) Uani 1 d . . . H43A H 1.0478 0.5043 0.8281 0.061 Uiso 1 calc R . . C44 C 1.1660(2) 0.55322(17) 0.70832(15) 0.0465(5) Uani 1 d . . . H44A H 1.2508 0.5341 0.7293 0.056 Uiso 1 calc R . . C45 C 1.1629(2) 0.59843(15) 0.61899(14) 0.0394(4) Uani 1 d . . . H45A H 1.2458 0.6099 0.5786 0.047 Uiso 1 calc R . . C46 C 1.03850(17) 0.62724(14) 0.58804(11) 0.0311(3) Uani 1 d . . . H46A H 1.0371 0.6583 0.5267 0.037 Uiso 1 calc R . . C51 C 0.69379(17) 0.52541(13) 0.61690(11) 0.0281(3) Uani 1 d . . . C52 C 0.7850(2) 0.43016(14) 0.61871(12) 0.0358(4) Uani 1 d . . . H52A H 0.8789 0.4291 0.6195 0.043 Uiso 1 calc R . . C53 C 0.7375(2) 0.33667(15) 0.61933(13) 0.0431(5) Uani 1 d . . . H53A H 0.7992 0.2718 0.6213 0.052 Uiso 1 calc R . . C54 C 0.6014(2) 0.33806(16) 0.61710(13) 0.0453(5) Uani 1 d . . . H54A H 0.5703 0.2749 0.6154 0.054 Uiso 1 calc R . . C55 C 0.5104(2) 0.43145(17) 0.61732(16) 0.0510(5) Uani 1 d . . . H55A H 0.4165 0.4319 0.6166 0.061 Uiso 1 calc R . . C56 C 0.5554(2) 0.52498(15) 0.61860(14) 0.0413(4) Uani 1 d . . . H56A H 0.4920 0.5883 0.6206 0.050 Uiso 1 calc R . . C61 C 0.78551(16) 0.71999(13) 0.49472(11) 0.0264(3) Uani 1 d . . . C62 C 0.8002(2) 0.66699(15) 0.42838(12) 0.0353(4) Uani 1 d . . . H62A H 0.7914 0.5927 0.4441 0.042 Uiso 1 calc R . . C63 C 0.8276(2) 0.72240(18) 0.33938(13) 0.0477(5) Uani 1 d . . . H63A H 0.8362 0.6859 0.2948 0.057 Uiso 1 calc R . . C64 C 0.8424(2) 0.83062(18) 0.31547(13) 0.0482(5) Uani 1 d . . . H64A H 0.8608 0.8681 0.2547 0.058 Uiso 1 calc R . . C65 C 0.8301(2) 0.88402(15) 0.38069(14) 0.0441(5) Uani 1 d . . . H65A H 0.8420 0.9578 0.3644 0.053 Uiso 1 calc R . . C66 C 0.80048(19) 0.82975(14) 0.46969(12) 0.0349(4) Uani 1 d . . . H66A H 0.7903 0.8671 0.5139 0.042 Uiso 1 calc R . . O5 O 0.64715(17) 0.64037(12) 1.00408(9) 0.0452(3) Uani 1 d . . . H5 H 0.606(3) 0.634(2) 0.9684(17) 0.054 Uiso 1 d . . . C1 C 0.7752(4) 0.6643(4) 0.95781(19) 0.132(2) Uani 1 d U . . H1A H 0.7629 0.7386 0.9194 0.158 Uiso 1 calc R . . H1B H 0.8088 0.6158 0.9183 0.158 Uiso 1 calc R . . C2 C 0.8787(3) 0.6572(3) 1.0061(2) 0.0822(9) Uani 1 d U . . H2B H 0.9465 0.7036 0.9698 0.123 Uiso 1 calc R . . H2C H 0.9232 0.5826 1.0219 0.123 Uiso 1 calc R . . H2D H 0.8387 0.6805 1.0601 0.123 Uiso 1 calc R . . O6 O 0.70283(15) 0.41748(12) 0.91446(9) 0.0426(3) Uani 1 d . . . H6 H 0.649(3) 0.471(2) 0.9037(16) 0.051 Uiso 1 d . . . C3 C 0.6910(3) 0.34105(18) 0.86894(15) 0.0509(5) Uani 1 d . . . H3B H 0.6660 0.3791 0.8101 0.061 Uiso 1 calc R . . H3C H 0.6187 0.2967 0.9034 0.061 Uiso 1 calc R . . C4 C 0.8265(3) 0.2703(2) 0.8582(2) 0.0699(8) Uani 1 d . . . H4B H 0.8191 0.2159 0.8291 0.105 Uiso 1 calc R . . H4C H 0.8518 0.2347 0.9166 0.105 Uiso 1 calc R . . H4D H 0.8967 0.3144 0.8219 0.105 Uiso 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 0.03004(7) 0.02462(7) 0.03044(7) -0.00951(5) 0.00145(5) -0.00681(5) P1 0.0289(2) 0.02193(19) 0.0272(2) -0.00779(16) 0.00027(16) -0.00529(16) P2 0.0264(2) 0.02271(19) 0.0272(2) -0.00925(16) 0.00076(16) -0.00678(15) P3 0.0274(2) 0.0318(2) 0.0238(2) -0.00064(17) -0.00600(16) -0.00773(17) O1 0.0308(6) 0.0407(7) 0.0273(6) 0.0038(5) -0.0057(5) -0.0103(5) O2 0.0328(6) 0.0403(7) 0.0389(7) -0.0063(6) -0.0135(5) -0.0057(5) O3 0.0714(10) 0.0445(8) 0.0332(7) 0.0057(6) -0.0219(7) -0.0297(7) O4 0.0455(8) 0.0612(10) 0.0285(7) -0.0011(7) -0.0007(6) 0.0101(7) C11 0.0316(8) 0.0300(8) 0.0295(8) -0.0110(7) -0.0008(7) -0.0041(7) C12 0.0485(11) 0.0302(9) 0.0420(10) -0.0111(8) 0.0037(9) -0.0033(8) C13 0.0644(15) 0.0411(11) 0.0612(14) -0.0272(11) 0.0025(11) 0.0035(10) C14 0.0652(16) 0.0695(16) 0.0622(15) -0.0384(13) 0.0199(12) -0.0052(13) C15 0.0695(16) 0.0677(16) 0.0565(14) -0.0275(13) 0.0311(12) -0.0254(13) C16 0.0519(12) 0.0401(10) 0.0440(11) -0.0164(9) 0.0125(9) -0.0157(9) C21 0.0330(8) 0.0228(7) 0.0268(8) -0.0030(6) -0.0024(6) -0.0065(6) C22 0.0412(10) 0.0310(9) 0.0393(10) -0.0113(8) -0.0072(8) -0.0050(7) C23 0.0538(12) 0.0414(10) 0.0466(11) -0.0134(9) -0.0155(9) -0.0113(9) C24 0.0405(10) 0.0423(10) 0.0459(11) -0.0009(9) -0.0158(9) -0.0092(8) C25 0.0359(10) 0.0340(9) 0.0447(11) -0.0046(8) -0.0048(8) -0.0005(8) C26 0.0371(9) 0.0297(8) 0.0350(9) -0.0096(7) -0.0034(7) -0.0035(7) C31 0.0343(8) 0.0212(7) 0.0267(8) -0.0088(6) -0.0028(6) -0.0043(6) C32 0.0336(9) 0.0276(8) 0.0354(9) -0.0064(7) -0.0045(7) -0.0078(7) C33 0.0467(11) 0.0342(9) 0.0354(10) -0.0047(8) 0.0036(8) -0.0144(8) C34 0.0585(12) 0.0304(9) 0.0300(9) -0.0042(7) -0.0074(8) -0.0066(8) C35 0.0483(11) 0.0357(10) 0.0402(10) -0.0087(8) -0.0168(9) -0.0007(8) C36 0.0338(9) 0.0357(9) 0.0388(10) -0.0102(8) -0.0059(7) -0.0055(7) C41 0.0320(8) 0.0237(7) 0.0278(8) -0.0094(6) -0.0044(6) -0.0066(6) C42 0.0507(11) 0.0404(10) 0.0280(9) -0.0065(8) -0.0039(8) -0.0070(9) C43 0.0717(15) 0.0488(12) 0.0330(10) -0.0090(9) -0.0231(10) 0.0014(11) C44 0.0492(12) 0.0446(11) 0.0554(13) -0.0196(10) -0.0267(10) 0.0007(9) C45 0.0332(9) 0.0388(10) 0.0499(11) -0.0128(9) -0.0113(8) -0.0069(8) C46 0.0311(8) 0.0327(9) 0.0305(8) -0.0070(7) -0.0063(7) -0.0073(7) C51 0.0333(8) 0.0249(8) 0.0268(8) -0.0089(6) 0.0009(6) -0.0096(6) C52 0.0398(10) 0.0288(8) 0.0380(9) -0.0126(7) 0.0024(8) -0.0070(7) C53 0.0611(13) 0.0257(9) 0.0409(10) -0.0128(8) 0.0037(9) -0.0097(8) C54 0.0695(14) 0.0321(9) 0.0400(10) -0.0105(8) -0.0031(10) -0.0259(9) C55 0.0477(12) 0.0445(11) 0.0680(14) -0.0129(10) -0.0134(11) -0.0222(10) C56 0.0368(10) 0.0323(9) 0.0574(12) -0.0121(9) -0.0087(9) -0.0096(8) C61 0.0232(7) 0.0261(8) 0.0294(8) -0.0075(6) -0.0029(6) -0.0037(6) C62 0.0439(10) 0.0313(9) 0.0325(9) -0.0102(7) -0.0040(8) -0.0095(7) C63 0.0671(14) 0.0477(11) 0.0314(10) -0.0131(9) -0.0027(9) -0.0172(10) C64 0.0630(13) 0.0468(11) 0.0302(9) -0.0006(8) -0.0028(9) -0.0175(10) C65 0.0530(12) 0.0294(9) 0.0448(11) -0.0022(8) -0.0019(9) -0.0121(8) C66 0.0415(10) 0.0276(8) 0.0361(9) -0.0102(7) -0.0013(8) -0.0087(7) O5 0.0621(9) 0.0435(8) 0.0314(7) -0.0011(6) -0.0138(6) -0.0174(7) C1 0.135(3) 0.251(5) 0.0414(15) -0.025(2) 0.0090(17) -0.150(4) C2 0.0623(17) 0.106(2) 0.0712(19) -0.0112(17) -0.0186(14) -0.0040(16) O6 0.0497(8) 0.0403(7) 0.0317(7) -0.0086(6) -0.0057(6) 0.0057(6) C3 0.0638(14) 0.0450(11) 0.0408(11) -0.0130(9) -0.0029(10) -0.0037(10) C4 0.0759(18) 0.0438(13) 0.0788(18) -0.0224(12) 0.0091(14) 0.0034(12) _geom_special_details ; ? ; 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 O1 2.3281(12) . ? Ag P1 2.4309(4) . ? Ag P2 2.4595(4) . ? Ag O2 2.8388(13) . ? P1 C11 1.8289(17) . ? P1 C21 1.8360(18) . ? P1 C31 1.8384(17) . ? P2 C41 1.8251(17) . ? P2 C51 1.8291(16) . ? P2 C61 1.8340(17) . ? P3 O1 1.5050(12) . ? P3 O2 1.5169(13) . ? P3 O4 1.5743(15) . ? P3 O3 1.5786(15) . ? C11 C16 1.393(3) . ? C11 C12 1.399(2) . ? C12 C13 1.393(3) . ? C13 C14 1.387(4) . ? C14 C15 1.384(4) . ? C15 C16 1.393(3) . ? C21 C22 1.398(2) . ? C21 C26 1.402(2) . ? C22 C23 1.396(3) . ? C23 C24 1.390(3) . ? C24 C25 1.387(3) . ? C25 C26 1.389(3) . ? C31 C32 1.393(2) . ? C31 C36 1.406(2) . ? C32 C33 1.407(3) . ? C33 C34 1.389(3) . ? C34 C35 1.390(3) . ? C35 C36 1.393(3) . ? C41 C46 1.396(2) . ? C41 C42 1.403(2) . ? C42 C43 1.397(3) . ? C43 C44 1.381(3) . ? C44 C45 1.384(3) . ? C45 C46 1.395(2) . ? C51 C56 1.394(3) . ? C51 C52 1.399(2) . ? C52 C53 1.397(3) . ? C53 C54 1.380(3) . ? C54 C55 1.383(3) . ? C55 C56 1.395(3) . ? C61 C62 1.398(2) . ? C61 C66 1.406(2) . ? C62 C63 1.393(3) . ? C63 C64 1.387(3) . ? C64 C65 1.390(3) . ? C65 C66 1.391(3) . ? O5 C1 1.390(3) . ? C1 C2 1.403(4) . ? O6 C3 1.434(3) . ? C3 C4 1.506(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 O1 Ag P1 123.96(3) . . ? O1 Ag P2 107.28(3) . . ? P1 Ag P2 127.671(15) . . ? O1 Ag O2 58.04(4) . . ? P1 Ag O2 110.84(3) . . ? P2 Ag O2 104.23(3) . . ? C11 P1 C21 105.30(8) . . ? C11 P1 C31 105.76(8) . . ? C21 P1 C31 104.32(8) . . ? C11 P1 Ag 116.76(6) . . ? C21 P1 Ag 116.07(5) . . ? C31 P1 Ag 107.49(5) . . ? C41 P2 C51 103.81(8) . . ? C41 P2 C61 104.32(7) . . ? C51 P2 C61 104.80(7) . . ? C41 P2 Ag 107.16(5) . . ? C51 P2 Ag 118.22(5) . . ? C61 P2 Ag 116.96(5) . . ? O1 P3 O2 114.81(7) . . ? O1 P3 O4 107.93(8) . . ? O2 P3 O4 109.97(8) . . ? O1 P3 O3 107.88(8) . . ? O2 P3 O3 108.89(8) . . ? O4 P3 O3 107.06(9) . . ? P3 O1 Ag 103.77(6) . . ? P3 O2 Ag 83.29(5) . . ? C16 C11 C12 119.59(17) . . ? C16 C11 P1 117.50(14) . . ? C12 C11 P1 122.88(14) . . ? C13 C12 C11 119.98(19) . . ? C14 C13 C12 120.0(2) . . ? C15 C14 C13 120.3(2) . . ? C14 C15 C16 120.1(2) . . ? C15 C16 C11 120.1(2) . . ? C22 C21 C26 118.69(16) . . ? C22 C21 P1 122.88(13) . . ? C26 C21 P1 118.43(13) . . ? C23 C22 C21 120.21(17) . . ? C24 C23 C22 120.37(18) . . ? C25 C24 C23 119.88(18) . . ? C24 C25 C26 119.98(18) . . ? C25 C26 C21 120.86(17) . . ? C32 C31 C36 118.91(16) . . ? C32 C31 P1 122.78(13) . . ? C36 C31 P1 117.81(13) . . ? C31 C32 C33 120.38(17) . . ? C34 C33 C32 120.23(18) . . ? C33 C34 C35 119.49(17) . . ? C34 C35 C36 120.67(18) . . ? C35 C36 C31 120.31(17) . . ? C46 C41 C42 119.20(16) . . ? C46 C41 P2 123.26(13) . . ? C42 C41 P2 117.47(14) . . ? C43 C42 C41 119.58(19) . . ? C44 C43 C42 120.85(18) . . ? C43 C44 C45 119.75(19) . . ? C44 C45 C46 120.30(19) . . ? C45 C46 C41 120.32(16) . . ? C56 C51 C52 119.45(16) . . ? C56 C51 P2 117.95(13) . . ? C52 C51 P2 122.59(13) . . ? C53 C52 C51 119.82(18) . . ? C54 C53 C52 120.37(18) . . ? C53 C54 C55 119.97(17) . . ? C54 C55 C56 120.4(2) . . ? C51 C56 C55 119.87(18) . . ? C62 C61 C66 118.64(16) . . ? C62 C61 P2 122.70(13) . . ? C66 C61 P2 118.66(12) . . ? C63 C62 C61 120.47(17) . . ? C64 C63 C62 120.38(18) . . ? C63 C64 C65 119.82(18) . . ? C64 C65 C66 120.16(18) . . ? C65 C66 C61 120.51(16) . . ? O5 C1 C2 118.6(3) . . ? O6 C3 C4 108.5(2) . . ? 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 O3 H3 O5 0.73(3) 1.92(3) 2.6463(19) 173(3) 2_667 O4 H4 O6 0.75(3) 1.88(3) 2.634(2) 174(3) 2_667 O5 H5 O2 0.81(3) 1.88(3) 2.6800(19) 169(3) . O6 H6 O2 0.80(3) 1.89(3) 2.6880(19) 172(3) . _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.661 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.048 #===END