# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2290 data_global #============================================================================== _audit_creation_method 'manual editing of form.cif' # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'J.C.S. Dalton Transactions' _journal_year 2000 _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Jagadese J. Vittal' _publ_contact_author_address ; Department of Chemistry National University of Singapore Kent Ridge Singapore 119 260 ; _publ_contact_author_email chmjjv@nus.edu.sg _publ_contact_author_fax '(65) 874 2975 _publ_contact_author_phone '(65) 779 1691 _publ_contact_letter ; Please consider this CIF submission for publication in Inorganic Chemistry. ; _publ_requested_journal 'J.C.S. Dalton Transactions' _publ_requested_category full paper # TITLE AND AUTHOR LIST _publ_section_title ; Chemistry of Thiocarboxylates: Synthesis and structures of neutral silver(I) thiocarboxylates with triphenylphosphine complexes. ; _publ_section_title_footnote ; Contribution No. ... ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Theivanayagam C Deivaraj' ; Department of Chemistry National University of Singapore 3 Science Drive 3 Singapore 117 543 ; 'Jagadese J. Vittal' ; Department of Chemistry National University of Singapore 3 Science Drive 3 Singapore 117 543 ; ############################################################# # Compound 2 data_tcd18 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H35 Ag O P2 S' _chemical_formula_weight 769.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 10.2945(3) _cell_length_b 13.3036(4) _cell_length_c 14.3270(3) _cell_angle_alpha 89.246(1) _cell_angle_beta 76.311(1) _cell_angle_gamma 77.161(1) _cell_volume 1857.13(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4349 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 29.26 _exptl_crystal_description 'plates, cut' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6774 _exptl_absorpt_correction_T_max 0.8622 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11846 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 29.26 _reflns_number_total 8442 _reflns_number_gt 5931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+3.6052P] 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 SHELXL _refine_ls_extinction_coef 0.0015(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8442 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.42744(4) 0.15919(3) 0.27085(3) 0.04535(14) Uani 1 1 d . . . S1 S 0.65343(14) 0.19852(13) 0.19011(12) 0.0648(4) Uani 1 1 d . . . O1 O 0.4509(4) 0.2917(5) 0.1206(4) 0.1031(18) Uani 1 1 d . . . C1 C 0.5752(5) 0.2767(5) 0.1143(4) 0.0556(14) Uani 1 1 d . . . C2 C 0.6610(6) 0.3266(4) 0.0346(4) 0.0551(14) Uani 1 1 d . . . C3 C 0.7986(6) 0.3204(5) 0.0253(4) 0.0679(17) Uani 1 1 d . . . H3 H 0.8411 0.2864 0.0710 0.082 Uiso 1 1 calc R . . C4 C 0.8747(8) 0.3631(7) -0.0496(6) 0.095(2) Uani 1 1 d . . . H4 H 0.9680 0.3571 -0.0553 0.114 Uiso 1 1 calc R . . C5 C 0.8117(9) 0.4150(6) -0.1161(6) 0.100(3) Uani 1 1 d . . . H5 H 0.8627 0.4448 -0.1668 0.120 Uiso 1 1 calc R . . C6 C 0.6758(9) 0.4233(7) -0.1088(5) 0.110(3) Uani 1 1 d . . . H6 H 0.6338 0.4586 -0.1542 0.132 Uiso 1 1 calc R . . C7 C 0.6006(7) 0.3789(6) -0.0333(5) 0.087(2) Uani 1 1 d . . . H7 H 0.5076 0.3844 -0.0283 0.104 Uiso 1 1 calc R . . P1 P 0.26239(13) 0.30332(10) 0.37195(10) 0.0426(3) Uani 1 1 d . . . P2 P 0.38426(13) -0.01165(10) 0.25181(10) 0.0436(3) Uani 1 1 d . . . C1A C 0.1028(5) 0.3357(4) 0.3324(4) 0.0429(11) Uani 1 1 d . . . C2A C -0.0263(5) 0.3436(4) 0.3927(4) 0.0524(13) Uani 1 1 d . . . H2A H -0.0350 0.3331 0.4580 0.063 Uiso 1 1 calc R . . C3A C -0.1423(6) 0.3671(5) 0.3565(5) 0.0608(15) Uani 1 1 d . . . H3A H -0.2283 0.3729 0.3980 0.073 Uiso 1 1 calc R . . C4A C -0.1325(6) 0.3817(5) 0.2615(5) 0.0630(16) Uani 1 1 d . . . H4A H -0.2111 0.3958 0.2379 0.076 Uiso 1 1 calc R . . C5A C -0.0050(6) 0.3757(5) 0.1997(4) 0.0671(16) Uani 1 1 d . . . H5A H 0.0017 0.3877 0.1348 0.080 Uiso 1 1 calc R . . C6A C 0.1123(6) 0.3519(5) 0.2340(4) 0.0580(14) Uani 1 1 d . . . H6A H 0.1978 0.3466 0.1920 0.070 Uiso 1 1 calc R . . C1B C 0.3121(5) 0.4266(4) 0.3713(3) 0.0443(12) Uani 1 1 d . . . C2B C 0.2201(6) 0.5205(4) 0.3722(4) 0.0530(13) Uani 1 1 d . . . H2B H 0.1297 0.5217 0.3714 0.064 Uiso 1 1 calc R . . C3B C 0.2619(7) 0.6129(4) 0.3743(4) 0.0646(16) Uani 1 1 d . . . H3B H 0.2002 0.6754 0.3733 0.077 Uiso 1 1 calc R . . C4B C 0.3947(7) 0.6116(5) 0.3780(5) 0.0694(18) Uani 1 1 d . . . H4B H 0.4224 0.6733 0.3807 0.083 Uiso 1 1 calc R . . C5B C 0.4858(7) 0.5194(5) 0.3778(6) 0.082(2) Uani 1 1 d . . . H5B H 0.5753 0.5185 0.3809 0.099 Uiso 1 1 calc R . . C6B C 0.4457(6) 0.4275(4) 0.3729(5) 0.0690(18) Uani 1 1 d . . . H6B H 0.5094 0.3653 0.3707 0.083 Uiso 1 1 calc R . . C1C C 0.2080(5) 0.2782(4) 0.4995(4) 0.0460(12) Uani 1 1 d . . . C2C C 0.1888(6) 0.1810(4) 0.5240(4) 0.0566(14) Uani 1 1 d . . . H2C H 0.2030 0.1309 0.4758 0.068 Uiso 1 1 calc R . . C3C C 0.1485(7) 0.1566(5) 0.6197(5) 0.0716(18) Uani 1 1 d . . . H3C H 0.1353 0.0909 0.6350 0.086 Uiso 1 1 calc R . . C4C C 0.1287(7) 0.2289(6) 0.6907(5) 0.080(2) Uani 1 1 d . . . H4C H 0.1017 0.2129 0.7547 0.096 Uiso 1 1 calc R . . C5C C 0.1486(7) 0.3261(5) 0.6676(5) 0.0772(19) Uani 1 1 d . . . H5C H 0.1361 0.3753 0.7164 0.093 Uiso 1 1 calc R . . C6C C 0.1870(6) 0.3513(5) 0.5729(4) 0.0622(15) Uani 1 1 d . . . H6C H 0.1989 0.4174 0.5583 0.075 Uiso 1 1 calc R . . C1D C 0.3453(5) -0.0717(4) 0.3671(4) 0.0438(11) Uani 1 1 d . . . C2D C 0.2169(6) -0.0891(4) 0.4103(4) 0.0534(13) Uani 1 1 d . . . H2D H 0.1480 -0.0768 0.3769 0.064 Uiso 1 1 calc R . . C3D C 0.1904(7) -0.1250(5) 0.5035(5) 0.0694(17) Uani 1 1 d . . . H3D H 0.1039 -0.1363 0.5315 0.083 Uiso 1 1 calc R . . C4D C 0.2896(7) -0.1437(5) 0.5538(4) 0.0678(17) Uani 1 1 d . . . H4D H 0.2708 -0.1667 0.6160 0.081 Uiso 1 1 calc R . . C5D C 0.4179(7) -0.1281(5) 0.5116(5) 0.0688(17) Uani 1 1 d . . . H5D H 0.4864 -0.1418 0.5453 0.083 Uiso 1 1 calc R . . C6D C 0.4459(6) -0.0923(4) 0.4195(4) 0.0601(15) Uani 1 1 d . . . H6D H 0.5330 -0.0818 0.3921 0.072 Uiso 1 1 calc R . . C1E C 0.2345(5) -0.0093(4) 0.2042(4) 0.0451(12) Uani 1 1 d . . . C2E C 0.1236(6) 0.0736(4) 0.2303(4) 0.0557(14) Uani 1 1 d . . . H2E H 0.1288 0.1262 0.2703 0.067 Uiso 1 1 calc R . . C3E C 0.0058(6) 0.0806(5) 0.1988(5) 0.0668(16) Uani 1 1 d . . . H3E H -0.0683 0.1363 0.2190 0.080 Uiso 1 1 calc R . . C4E C -0.0018(7) 0.0058(5) 0.1380(5) 0.0726(18) Uani 1 1 d . . . H4E H -0.0803 0.0110 0.1151 0.087 Uiso 1 1 calc R . . C5E C 0.1058(8) -0.0768(6) 0.1107(6) 0.098(3) Uani 1 1 d . . . H5E H 0.0992 -0.1286 0.0703 0.117 Uiso 1 1 calc R . . C6E C 0.2245(7) -0.0851(5) 0.1420(5) 0.078(2) Uani 1 1 d . . . H6E H 0.2977 -0.1414 0.1216 0.094 Uiso 1 1 calc R . . C1F C 0.5231(5) -0.1055(4) 0.1756(4) 0.0506(13) Uani 1 1 d . . . C2F C 0.5452(7) -0.2105(5) 0.1895(5) 0.083(2) Uani 1 1 d . . . H2F H 0.4895 -0.2355 0.2412 0.099 Uiso 1 1 calc R . . C3F C 0.6496(9) -0.2786(6) 0.1267(6) 0.102(3) Uani 1 1 d . . . H3F H 0.6650 -0.3490 0.1369 0.123 Uiso 1 1 calc R . . C4F C 0.7297(9) -0.2428(8) 0.0502(6) 0.108(3) Uani 1 1 d . . . H4F H 0.7976 -0.2888 0.0069 0.130 Uiso 1 1 calc R . . C5F C 0.7107(8) -0.1393(9) 0.0367(6) 0.111(3) Uani 1 1 d . . . H5F H 0.7671 -0.1153 -0.0153 0.133 Uiso 1 1 calc R . . C6F C 0.6086(7) -0.0697(6) 0.0994(5) 0.083(2) Uani 1 1 d . . . H6F H 0.5976 0.0008 0.0905 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0433(2) 0.0425(2) 0.0490(2) 0.00431(16) -0.00497(17) -0.01384(16) S1 0.0425(7) 0.0758(10) 0.0754(10) 0.0256(8) -0.0093(7) -0.0186(7) O1 0.045(2) 0.177(5) 0.086(3) 0.052(3) -0.014(2) -0.026(3) C1 0.043(3) 0.074(4) 0.047(3) -0.003(3) -0.005(2) -0.015(3) C2 0.056(3) 0.058(3) 0.047(3) -0.005(3) -0.002(3) -0.015(3) C3 0.065(4) 0.088(5) 0.060(4) 0.016(3) -0.010(3) -0.040(3) C4 0.086(5) 0.123(7) 0.083(5) 0.021(5) -0.004(4) -0.058(5) C5 0.104(6) 0.099(6) 0.081(5) 0.026(5) 0.013(5) -0.030(5) C6 0.103(6) 0.129(7) 0.070(5) 0.047(5) 0.004(5) 0.002(5) C7 0.067(4) 0.114(6) 0.064(4) 0.021(4) -0.003(3) -0.003(4) P1 0.0402(7) 0.0382(7) 0.0476(8) -0.0003(6) -0.0047(6) -0.0115(5) P2 0.0426(7) 0.0380(7) 0.0470(8) 0.0020(6) -0.0030(6) -0.0105(5) C1A 0.044(3) 0.035(3) 0.048(3) -0.001(2) -0.005(2) -0.012(2) C2A 0.050(3) 0.053(3) 0.050(3) 0.006(3) -0.001(3) -0.015(2) C3A 0.045(3) 0.066(4) 0.069(4) -0.002(3) -0.006(3) -0.015(3) C4A 0.048(3) 0.064(4) 0.081(5) -0.007(3) -0.024(3) -0.014(3) C5A 0.059(4) 0.088(5) 0.055(4) -0.001(3) -0.016(3) -0.017(3) C6A 0.048(3) 0.075(4) 0.050(3) -0.005(3) -0.004(3) -0.020(3) C1B 0.048(3) 0.044(3) 0.042(3) 0.001(2) -0.007(2) -0.015(2) C2B 0.050(3) 0.049(3) 0.060(3) 0.005(3) -0.009(3) -0.015(3) C3B 0.078(4) 0.043(3) 0.070(4) 0.006(3) -0.010(3) -0.016(3) C4B 0.088(5) 0.050(4) 0.074(4) 0.000(3) -0.006(4) -0.039(3) C5B 0.069(4) 0.070(5) 0.118(6) 0.001(4) -0.021(4) -0.040(4) C6B 0.053(3) 0.047(3) 0.110(5) 0.003(3) -0.021(3) -0.016(3) C1C 0.041(3) 0.043(3) 0.051(3) 0.001(2) -0.004(2) -0.010(2) C2C 0.067(4) 0.051(3) 0.050(3) -0.001(3) -0.003(3) -0.021(3) C3C 0.087(5) 0.056(4) 0.067(4) 0.012(3) -0.002(4) -0.024(3) C4C 0.098(5) 0.083(5) 0.051(4) 0.010(4) -0.002(4) -0.022(4) C5C 0.103(5) 0.074(5) 0.051(4) -0.007(3) -0.006(4) -0.025(4) C6C 0.078(4) 0.053(3) 0.052(3) -0.005(3) -0.002(3) -0.021(3) C1D 0.051(3) 0.034(3) 0.046(3) -0.001(2) -0.006(2) -0.013(2) C2D 0.052(3) 0.053(3) 0.055(3) 0.009(3) -0.007(3) -0.018(3) C3D 0.067(4) 0.066(4) 0.071(4) 0.017(3) 0.003(3) -0.027(3) C4D 0.090(5) 0.059(4) 0.052(4) 0.008(3) -0.010(3) -0.019(3) C5D 0.076(4) 0.071(4) 0.061(4) 0.005(3) -0.024(3) -0.012(3) C6D 0.057(3) 0.066(4) 0.060(4) 0.004(3) -0.012(3) -0.023(3) C1E 0.049(3) 0.041(3) 0.044(3) -0.001(2) -0.007(2) -0.011(2) C2E 0.061(3) 0.048(3) 0.056(3) -0.007(3) -0.012(3) -0.010(3) C3E 0.054(4) 0.073(4) 0.070(4) 0.002(3) -0.016(3) -0.008(3) C4E 0.064(4) 0.081(5) 0.084(5) 0.001(4) -0.037(4) -0.019(4) C5E 0.098(6) 0.085(5) 0.121(7) -0.042(5) -0.050(5) -0.016(4) C6E 0.075(4) 0.057(4) 0.102(5) -0.025(4) -0.033(4) 0.001(3) C1F 0.045(3) 0.054(3) 0.049(3) -0.006(3) -0.006(2) -0.008(2) C2F 0.090(5) 0.056(4) 0.078(5) -0.004(3) 0.011(4) 0.004(3) C3F 0.113(6) 0.073(5) 0.091(6) -0.028(5) -0.005(5) 0.023(5) C4F 0.087(6) 0.130(8) 0.078(6) -0.041(6) -0.006(5) 0.025(6) C5F 0.082(6) 0.146(8) 0.074(5) -0.019(6) 0.031(4) -0.014(6) C6F 0.071(4) 0.087(5) 0.073(5) 0.001(4) 0.015(4) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P2 2.4413(13) . ? Ag1 P1 2.4743(13) . ? Ag1 S1 2.5052(14) . ? S1 C1 1.710(6) . ? O1 C1 1.232(6) . ? C1 C2 1.512(8) . ? C2 C3 1.375(8) . ? C2 C7 1.376(9) . ? C3 C4 1.367(8) . ? C4 C5 1.372(11) . ? C5 C6 1.357(11) . ? C6 C7 1.382(10) . ? P1 C1B 1.823(5) . ? P1 C1A 1.824(5) . ? P1 C1C 1.830(5) . ? P2 C1F 1.816(5) . ? P2 C1E 1.822(5) . ? P2 C1D 1.823(5) . ? C1A C2A 1.386(7) . ? C1A C6A 1.407(7) . ? C2A C3A 1.385(8) . ? C3A C4A 1.356(8) . ? C4A C5A 1.385(8) . ? C5A C6A 1.380(8) . ? C1B C6B 1.383(7) . ? C1B C2B 1.387(7) . ? C2B C3B 1.393(7) . ? C3B C4B 1.377(9) . ? C4B C5B 1.369(9) . ? C5B C6B 1.383(8) . ? C1C C2C 1.380(7) . ? C1C C6C 1.387(7) . ? C2C C3C 1.391(8) . ? C3C C4C 1.357(9) . ? C4C C5C 1.378(9) . ? C5C C6C 1.378(8) . ? C1D C2D 1.388(7) . ? C1D C6D 1.395(7) . ? C2D C3D 1.398(8) . ? C3D C4D 1.362(9) . ? C4D C5D 1.375(9) . ? C5D C6D 1.385(8) . ? C1E C2E 1.381(7) . ? C1E C6E 1.391(8) . ? C2E C3E 1.375(8) . ? C3E C4E 1.358(8) . ? C4E C5E 1.361(9) . ? C5E C6E 1.380(9) . ? C1F C6F 1.383(8) . ? C1F C2F 1.384(8) . ? C2F C3F 1.385(9) . ? C3F C4F 1.356(12) . ? C4F C5F 1.365(12) . ? C5F C6F 1.383(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Ag1 P1 124.51(4) . . ? P2 Ag1 S1 120.78(5) . . ? P1 Ag1 S1 114.68(5) . . ? C1 S1 Ag1 89.61(19) . . ? O1 C1 C2 118.5(5) . . ? O1 C1 S1 122.0(5) . . ? C2 C1 S1 119.4(4) . . ? C3 C2 C7 117.9(6) . . ? C3 C2 C1 123.0(5) . . ? C7 C2 C1 119.1(5) . . ? C4 C3 C2 121.6(7) . . ? C3 C4 C5 119.2(7) . . ? C6 C5 C4 120.8(7) . . ? C5 C6 C7 119.3(8) . . ? C2 C7 C6 121.2(7) . . ? C1B P1 C1A 103.2(2) . . ? C1B P1 C1C 104.5(2) . . ? C1A P1 C1C 104.1(2) . . ? C1B P1 Ag1 117.33(17) . . ? C1A P1 Ag1 110.66(16) . . ? C1C P1 Ag1 115.62(16) . . ? C1F P2 C1E 105.5(2) . . ? C1F P2 C1D 105.3(2) . . ? C1E P2 C1D 103.8(2) . . ? C1F P2 Ag1 116.27(18) . . ? C1E P2 Ag1 113.41(16) . . ? C1D P2 Ag1 111.50(16) . . ? C2A C1A C6A 118.3(5) . . ? C2A C1A P1 124.1(4) . . ? C6A C1A P1 117.6(4) . . ? C3A C2A C1A 120.4(5) . . ? C4A C3A C2A 121.0(5) . . ? C3A C4A C5A 119.8(6) . . ? C6A C5A C4A 120.3(6) . . ? C5A C6A C1A 120.2(5) . . ? C6B C1B C2B 118.3(5) . . ? C6B C1B P1 119.0(4) . . ? C2B C1B P1 122.6(4) . . ? C1B C2B C3B 120.6(5) . . ? C4B C3B C2B 119.9(6) . . ? C5B C4B C3B 119.8(5) . . ? C4B C5B C6B 120.4(6) . . ? C5B C6B C1B 121.0(6) . . ? C2C C1C C6C 118.2(5) . . ? C2C C1C P1 118.3(4) . . ? C6C C1C P1 123.5(4) . . ? C1C C2C C3C 121.2(5) . . ? C4C C3C C2C 119.8(6) . . ? C3C C4C C5C 119.8(6) . . ? C4C C5C C6C 120.7(6) . . ? C5C C6C C1C 120.2(6) . . ? C2D C1D C6D 117.8(5) . . ? C2D C1D P2 123.7(4) . . ? C6D C1D P2 118.2(4) . . ? C1D C2D C3D 120.5(5) . . ? C4D C3D C2D 120.8(6) . . ? C3D C4D C5D 119.4(6) . . ? C4D C5D C6D 120.6(6) . . ? C5D C6D C1D 120.9(5) . . ? C2E C1E C6E 117.4(5) . . ? C2E C1E P2 118.3(4) . . ? C6E C1E P2 124.3(4) . . ? C3E C2E C1E 122.0(5) . . ? C4E C3E C2E 119.7(6) . . ? C3E C4E C5E 119.8(6) . . ? C4E C5E C6E 121.2(6) . . ? C5E C6E C1E 119.9(6) . . ? C6F C1F C2F 119.0(6) . . ? C6F C1F P2 117.9(5) . . ? C2F C1F P2 123.1(4) . . ? C1F C2F C3F 120.4(7) . . ? C4F C3F C2F 120.0(8) . . ? C3F C4F C5F 120.2(7) . . ? C4F C5F C6F 120.7(8) . . ? C5F C6F C1F 119.6(7) . . ? _diffrn_measured_fraction_theta_max 0.833 _diffrn_reflns_theta_full 29.26 _diffrn_measured_fraction_theta_full 0.833 _refine_diff_density_max 0.526 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.093 #=====END ################################################### #Compound 3 data_tcd4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H73 Ag4 Cl2 O4 P4 S4' _chemical_formula_weight 1864.89 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5692(2) _cell_length_b 16.8766(2) _cell_length_c 17.7730(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.656(1) _cell_angle_gamma 90.00 _cell_volume 4209.54(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'multifaced blocks' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1874 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type 'Sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7047 _exptl_absorpt_correction_T_max 0.8312 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20327 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7320 _reflns_number_gt 5677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+6.9792P] 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 SHELXL _refine_ls_extinction_coef 0.00002(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7320 _refine_ls_number_parameters 465 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1650 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.08325(4) 0.59988(3) 0.05775(4) 0.0621(2) Uani 1 1 d . . . Ag2 Ag 0.14448(4) 0.52310(3) -0.09577(3) 0.0620(2) Uani 1 1 d . . . S1 S 0.02731(13) 0.47999(11) 0.10877(10) 0.0635(5) Uani 1 1 d . . . S2 S 0.23997(10) 0.57408(10) 0.05191(9) 0.0500(4) Uani 1 1 d . . . O1 O 0.1544(4) 0.5264(4) 0.2539(4) 0.0970(19) Uani 1 1 d . . . O2 O 0.2507(10) 0.6831(9) -0.0504(8) 0.102(4) Uani 0.70 1 d P . . O2A O 0.312(2) 0.664(2) -0.022(2) 0.111(11) Uani 0.30 1 d P . . C1 C 0.1026(4) 0.4729(4) 0.2161(4) 0.0588(16) Uani 1 1 d . . . C2 C 0.0996(7) 0.3959(6) 0.2570(6) 0.099(3) Uani 1 1 d . . . H2A H 0.0544 0.3611 0.2165 0.149 Uiso 1 1 calc R . . H2B H 0.0809 0.4055 0.3011 0.149 Uiso 1 1 calc R . . H2C H 0.1616 0.3718 0.2797 0.149 Uiso 1 1 calc R . . C3 C 0.2693(5) 0.6669(5) 0.0232(5) 0.0673(18) Uani 1 1 d . . . C4 C 0.2949(6) 0.7340(5) 0.0854(5) 0.082(2) Uani 1 1 d . . . H4A H 0.2973 0.7147 0.1371 0.122 Uiso 1 1 calc R . . H4B H 0.2478 0.7750 0.0638 0.122 Uiso 1 1 calc R . . H4C H 0.3561 0.7550 0.0949 0.122 Uiso 1 1 calc R . . P1 P -0.00397(11) 0.72345(9) 0.03654(10) 0.0514(4) Uani 1 1 d . . . P2 P 0.18134(11) 0.50713(11) -0.21461(10) 0.0534(4) Uani 1 1 d . . . C1A C -0.0357(5) 0.7765(4) -0.0617(4) 0.0567(15) Uani 1 1 d . . . C2A C 0.0310(7) 0.7803(6) -0.0933(5) 0.088(2) Uani 1 1 d . . . H2A1 H 0.0887 0.7539 -0.0658 0.105 Uiso 1 1 calc R . . C3A C 0.0135(9) 0.8237(7) -0.1669(6) 0.110(3) Uani 1 1 d . . . H3A H 0.0611 0.8294 -0.1848 0.131 Uiso 1 1 calc R . . C4A C -0.0733(9) 0.8566(6) -0.2107(6) 0.098(3) Uani 1 1 d . . . H4A1 H -0.0860 0.8834 -0.2601 0.118 Uiso 1 1 calc R . . C5A C -0.1415(7) 0.8509(5) -0.1835(6) 0.098(3) Uani 1 1 d . . . H5A H -0.2011 0.8732 -0.2149 0.118 Uiso 1 1 calc R . . C6A C -0.1237(5) 0.8112(4) -0.1069(5) 0.076(2) Uani 1 1 d . . . H6A H -0.1706 0.8088 -0.0878 0.091 Uiso 1 1 calc R . . C1B C -0.1177(4) 0.7119(4) 0.0422(4) 0.0539(15) Uani 1 1 d . . . C2B C -0.1476(5) 0.7608(5) 0.0897(5) 0.081(2) Uani 1 1 d . . . H2B1 H -0.1073 0.8002 0.1229 0.098 Uiso 1 1 calc R . . C3B C -0.2366(6) 0.7510(5) 0.0875(7) 0.099(3) Uani 1 1 d . . . H3B H -0.2561 0.7843 0.1188 0.119 Uiso 1 1 calc R . . C4B C -0.2964(6) 0.6929(5) 0.0398(6) 0.085(2) Uani 1 1 d . . . H4B1 H -0.3567 0.6873 0.0381 0.102 Uiso 1 1 calc R . . C5B C -0.2669(5) 0.6416(5) -0.0065(5) 0.0716(19) Uani 1 1 d . . . H5B H -0.3073 0.6017 -0.0386 0.086 Uiso 1 1 calc R . . C6B C -0.1781(5) 0.6507(4) -0.0042(4) 0.0587(16) Uani 1 1 d . . . H6B H -0.1579 0.6157 -0.0337 0.070 Uiso 1 1 calc R . . C1C C 0.0604(4) 0.7965(4) 0.1167(4) 0.0577(16) Uani 1 1 d . . . C2C C 0.0548(6) 0.8780(5) 0.0995(6) 0.086(2) Uani 1 1 d . . . H2C1 H 0.0177 0.8980 0.0465 0.103 Uiso 1 1 calc R . . C3C C 0.1105(8) 0.9289(6) 0.1695(8) 0.112(4) Uani 1 1 d . . . H3C H 0.1097 0.9833 0.1608 0.135 Uiso 1 1 calc R . . C4C C 0.1647(7) 0.8994(8) 0.2486(7) 0.103(4) Uani 1 1 d . . . H4C1 H 0.1994 0.9333 0.2926 0.124 Uiso 1 1 calc R . . C5C C 0.1662(7) 0.8219(8) 0.2604(6) 0.112(4) Uani 1 1 d . . . H5C H 0.2025 0.8022 0.3137 0.134 Uiso 1 1 calc R . . C6C C 0.1160(6) 0.7686(6) 0.1966(5) 0.083(2) Uani 1 1 d . . . H6C H 0.1197 0.7145 0.2075 0.100 Uiso 1 1 calc R . . C1D C 0.1205(4) 0.5825(4) -0.2938(4) 0.0572(16) Uani 1 1 d . . . C2D C 0.1307(6) 0.6607(5) -0.2696(5) 0.0719(19) Uani 1 1 d . . . H2D H 0.1688 0.6737 -0.2141 0.086 Uiso 1 1 calc R . . C3D C 0.0846(6) 0.7211(5) -0.3271(5) 0.080(2) Uani 1 1 d . . . H3D H 0.0939 0.7739 -0.3105 0.096 Uiso 1 1 calc R . . C4D C 0.0260(6) 0.7017(6) -0.4079(5) 0.082(2) Uani 1 1 d . . . H4D H -0.0072 0.7414 -0.4456 0.099 Uiso 1 1 calc R . . C5D C 0.0155(7) 0.6246(6) -0.4340(5) 0.093(3) Uani 1 1 d . . . H5D H -0.0220 0.6124 -0.4897 0.112 Uiso 1 1 calc R . . C6D C 0.0611(6) 0.5642(5) -0.3770(5) 0.077(2) Uani 1 1 d . . . H6D H 0.0518 0.5117 -0.3945 0.093 Uiso 1 1 calc R . . C1E C 0.3057(5) 0.5159(4) -0.1963(4) 0.0608(17) Uani 1 1 d . . . C2E C 0.3342(6) 0.5484(6) -0.2530(5) 0.093(3) Uani 1 1 d . . . H2E H 0.2885 0.5707 -0.3018 0.112 Uiso 1 1 calc R . . C3E C 0.4294(6) 0.5490(6) -0.2395(6) 0.100(3) Uani 1 1 d . . . H3E H 0.4465 0.5713 -0.2789 0.120 Uiso 1 1 calc R . . C4E C 0.4967(6) 0.5170(6) -0.1689(6) 0.092(3) Uani 1 1 d . . . H4E H 0.5603 0.5175 -0.1596 0.110 Uiso 1 1 calc R . . C5E C 0.4712(6) 0.4834(7) -0.1100(6) 0.113(4) Uani 1 1 d . . . H5E H 0.5171 0.4603 -0.0619 0.135 Uiso 1 1 calc R . . C6E C 0.3755(6) 0.4848(6) -0.1239(5) 0.098(3) Uani 1 1 d . . . H6E H 0.3587 0.4643 -0.0836 0.117 Uiso 1 1 calc R . . C1F C 0.1436(5) 0.4120(4) -0.2687(4) 0.0602(16) Uani 1 1 d . . . C2F C 0.1917(6) 0.3752(5) -0.3092(5) 0.084(2) Uani 1 1 d . . . H2F H 0.2457 0.3992 -0.3088 0.101 Uiso 1 1 calc R . . C3F C 0.1608(8) 0.3032(6) -0.3502(6) 0.103(3) Uani 1 1 d . . . H3F H 0.1926 0.2797 -0.3782 0.123 Uiso 1 1 calc R . . C4F C 0.0828(11) 0.2677(6) -0.3486(6) 0.120(4) Uani 1 1 d . . . H4F H 0.0627 0.2187 -0.3741 0.144 Uiso 1 1 calc R . . C5F C 0.0334(10) 0.3038(7) -0.3096(7) 0.128(4) Uani 1 1 d . . . H5F H -0.0210 0.2802 -0.3106 0.154 Uiso 1 1 calc R . . C6F C 0.0651(7) 0.3742(6) -0.2697(6) 0.094(3) Uani 1 1 d . . . H6F H 0.0325 0.3973 -0.2422 0.113 Uiso 1 1 calc R . . C1S C -0.2443(9) 0.9761(9) -0.0387(12) 0.1020(18) Uiso 0.50 1 d PD . . Cl1 Cl -0.1743(10) 1.0430(8) 0.0296(8) 0.1020(18) Uiso 0.20 1 d PD . . Cl2 Cl -0.3206(9) 0.9231(8) -0.0214(9) 0.1020(18) Uiso 0.20 1 d PD . . Cl3 Cl -0.1435(8) 1.0067(9) 0.0330(8) 0.1020(18) Uiso 0.20 1 d PD . . Cl4 Cl -0.3341(8) 0.9576(9) -0.0125(9) 0.1020(18) Uiso 0.20 1 d PD . . Cl5 Cl -0.3388(16) 0.9221(14) -0.0602(18) 0.1020(18) Uiso 0.10 1 d PD . . Cl6 Cl -0.2197(19) 1.0571(12) 0.0171(16) 0.1020(18) Uiso 0.10 1 d PD . . 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 0.0604(3) 0.0532(3) 0.0815(4) -0.0001(2) 0.0389(3) 0.0046(2) Ag2 0.0748(4) 0.0690(4) 0.0488(3) -0.0057(2) 0.0329(3) -0.0084(3) S1 0.0648(10) 0.0830(12) 0.0490(9) -0.0083(8) 0.0306(8) -0.0246(9) S2 0.0460(8) 0.0587(9) 0.0463(8) 0.0024(7) 0.0210(6) 0.0024(7) O1 0.082(4) 0.111(5) 0.067(3) -0.004(3) 0.003(3) -0.025(3) O2 0.153(12) 0.094(8) 0.070(7) 0.012(5) 0.059(8) -0.027(8) O2A 0.17(3) 0.10(2) 0.11(3) -0.019(18) 0.11(3) -0.04(2) C1 0.042(3) 0.074(5) 0.061(4) 0.004(3) 0.023(3) 0.005(3) C2 0.088(6) 0.110(7) 0.110(7) 0.052(6) 0.053(5) 0.014(5) C3 0.067(4) 0.076(5) 0.064(4) -0.004(4) 0.033(4) -0.020(4) C4 0.084(5) 0.070(5) 0.084(5) -0.011(4) 0.030(4) -0.023(4) P1 0.0523(9) 0.0463(9) 0.0577(9) -0.0057(7) 0.0259(8) 0.0015(7) P2 0.0505(9) 0.0708(11) 0.0422(8) -0.0031(7) 0.0232(7) -0.0005(8) C1A 0.067(4) 0.047(3) 0.056(4) -0.007(3) 0.026(3) -0.006(3) C2A 0.095(6) 0.110(7) 0.069(5) 0.008(5) 0.045(5) 0.017(5) C3A 0.155(10) 0.120(8) 0.087(7) -0.004(6) 0.084(7) -0.009(7) C4A 0.134(9) 0.078(6) 0.072(6) 0.003(5) 0.034(6) -0.011(6) C5A 0.094(6) 0.073(6) 0.091(6) 0.019(5) 0.006(5) 0.002(5) C6A 0.069(5) 0.056(4) 0.089(5) 0.013(4) 0.021(4) 0.005(3) C1B 0.054(3) 0.044(3) 0.066(4) -0.002(3) 0.028(3) 0.008(3) C2B 0.070(5) 0.083(6) 0.100(6) -0.035(4) 0.046(4) -0.008(4) C3B 0.087(6) 0.094(6) 0.145(8) -0.043(6) 0.076(6) -0.012(5) C4B 0.066(5) 0.085(6) 0.119(7) -0.004(5) 0.055(5) 0.002(4) C5B 0.059(4) 0.067(5) 0.087(5) -0.003(4) 0.031(4) -0.006(3) C6B 0.060(4) 0.058(4) 0.062(4) -0.004(3) 0.030(3) 0.002(3) C1C 0.050(3) 0.062(4) 0.066(4) -0.011(3) 0.029(3) -0.005(3) C2C 0.098(6) 0.064(5) 0.106(6) -0.028(4) 0.054(5) -0.025(4) C3C 0.135(9) 0.089(7) 0.153(11) -0.048(7) 0.100(9) -0.044(6) C4C 0.075(6) 0.152(11) 0.094(7) -0.067(7) 0.047(5) -0.037(6) C5C 0.086(6) 0.150(10) 0.080(6) -0.040(7) 0.018(5) 0.003(7) C6C 0.084(5) 0.093(6) 0.063(5) -0.013(4) 0.022(4) 0.005(5) C1D 0.050(3) 0.079(5) 0.048(3) 0.001(3) 0.027(3) 0.004(3) C2D 0.081(5) 0.078(5) 0.058(4) -0.007(4) 0.031(4) -0.008(4) C3D 0.096(6) 0.075(5) 0.084(6) 0.002(4) 0.052(5) 0.009(4) C4D 0.069(5) 0.096(6) 0.084(6) 0.030(5) 0.035(4) 0.026(4) C5D 0.092(6) 0.102(7) 0.062(5) 0.009(5) 0.011(4) 0.018(5) C6D 0.079(5) 0.081(5) 0.059(4) -0.006(4) 0.017(4) 0.008(4) C1E 0.050(3) 0.084(5) 0.050(4) 0.001(3) 0.023(3) 0.005(3) C2E 0.065(5) 0.144(8) 0.083(6) 0.044(6) 0.043(4) 0.028(5) C3E 0.070(5) 0.145(9) 0.105(7) 0.044(6) 0.057(5) 0.024(5) C4E 0.060(5) 0.123(8) 0.096(6) -0.014(6) 0.037(5) 0.003(5) C5E 0.057(5) 0.188(11) 0.077(6) 0.022(6) 0.014(4) 0.008(6) C6E 0.063(5) 0.166(10) 0.056(4) 0.023(5) 0.018(4) -0.004(5) C1F 0.064(4) 0.065(4) 0.047(3) -0.002(3) 0.021(3) 0.007(3) C2F 0.072(5) 0.096(6) 0.077(5) -0.017(4) 0.027(4) 0.014(4) C3F 0.120(8) 0.092(7) 0.087(6) -0.018(5) 0.035(6) 0.036(6) C4F 0.204(13) 0.067(6) 0.060(5) -0.007(4) 0.030(7) -0.011(7) C5F 0.182(12) 0.109(8) 0.116(8) -0.038(7) 0.086(9) -0.068(8) C6F 0.115(7) 0.091(6) 0.099(6) -0.026(5) 0.068(6) -0.026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4273(17) . ? Ag1 S1 2.5217(18) . ? Ag1 S2 2.5245(15) . ? Ag2 P2 2.4317(16) . ? Ag2 S2 2.5417(16) . ? Ag2 S1 2.5834(18) 3_565 ? S1 C1 1.759(7) . ? S1 Ag2 2.5834(18) 3_565 ? S2 C3 1.768(7) . ? O1 C1 1.203(8) . ? O2 O2A 0.92(3) . ? O2 C3 1.241(14) . ? O2A C3 1.25(3) . ? C1 C2 1.500(10) . ? C3 C4 1.511(10) . ? P1 C1C 1.821(7) . ? P1 C1B 1.827(6) . ? P1 C1A 1.830(7) . ? P2 C1E 1.825(7) . ? P2 C1D 1.828(7) . ? P2 C1F 1.832(7) . ? C1A C2A 1.379(10) . ? C1A C6A 1.382(10) . ? C2A C3A 1.417(13) . ? C3A C4A 1.353(14) . ? C4A C5A 1.347(14) . ? C5A C6A 1.433(12) . ? C1B C2B 1.395(9) . ? C1B C6B 1.401(9) . ? C2B C3B 1.380(11) . ? C3B C4B 1.364(11) . ? C4B C5B 1.402(11) . ? C5B C6B 1.374(10) . ? C1C C6C 1.386(10) . ? C1C C2C 1.403(11) . ? C2C C3C 1.451(13) . ? C3C C4C 1.382(15) . ? C4C C5C 1.323(15) . ? C5C C6C 1.394(13) . ? C1D C2D 1.376(10) . ? C1D C6D 1.399(9) . ? C2D C3D 1.402(11) . ? C3D C4D 1.367(11) . ? C4D C5D 1.366(12) . ? C5D C6D 1.395(11) . ? C1E C2E 1.378(10) . ? C1E C6E 1.379(10) . ? C2E C3E 1.395(11) . ? C3E C4E 1.351(12) . ? C4E C5E 1.391(13) . ? C5E C6E 1.401(12) . ? C1F C6F 1.373(11) . ? C1F C2F 1.389(10) . ? C2F C3F 1.392(13) . ? C3F C4F 1.365(16) . ? C4F C5F 1.379(16) . ? C5F C6F 1.362(13) . ? C1S Cl2 1.618(15) . ? C1S Cl3 1.620(14) . ? C1S Cl5 1.629(15) . ? C1S Cl6 1.633(16) . ? C1S Cl1 1.670(15) . ? C1S Cl4 1.683(16) . ? Cl1 Cl6 0.69(3) . ? Cl1 Cl3 0.763(16) . ? Cl2 Cl5 0.62(3) . ? Cl2 Cl4 0.661(18) . ? Cl3 Cl6 1.39(3) . ? Cl4 Cl5 1.02(3) . ? Cl4 Cl6 2.34(2) . ? 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 P1 Ag1 S1 119.21(6) . . ? P1 Ag1 S2 128.87(6) . . ? S1 Ag1 S2 111.52(6) . . ? P2 Ag2 S2 133.00(6) . . ? P2 Ag2 S1 123.00(6) . 3_565 ? S2 Ag2 S1 102.66(5) . 3_565 ? C1 S1 Ag1 105.8(2) . . ? C1 S1 Ag2 105.9(2) . 3_565 ? Ag1 S1 Ag2 119.30(8) . 3_565 ? C3 S2 Ag1 103.5(3) . . ? C3 S2 Ag2 96.3(2) . . ? Ag1 S2 Ag2 87.55(5) . . ? O2A O2 C3 69(2) . . ? O2 O2A C3 68(2) . . ? O1 C1 C2 122.3(7) . . ? O1 C1 S1 121.7(6) . . ? C2 C1 S1 116.0(6) . . ? O2 C3 O2A 43.4(15) . . ? O2 C3 C4 118.2(9) . . ? O2A C3 C4 117.3(17) . . ? O2 C3 S2 121.9(8) . . ? O2A C3 S2 115.3(17) . . ? C4 C3 S2 118.2(5) . . ? C1C P1 C1B 104.3(3) . . ? C1C P1 C1A 104.2(3) . . ? C1B P1 C1A 103.7(3) . . ? C1C P1 Ag1 112.2(2) . . ? C1B P1 Ag1 113.0(2) . . ? C1A P1 Ag1 118.1(2) . . ? C1E P2 C1D 103.7(3) . . ? C1E P2 C1F 103.8(3) . . ? C1D P2 C1F 105.3(3) . . ? C1E P2 Ag2 117.9(2) . . ? C1D P2 Ag2 110.7(2) . . ? C1F P2 Ag2 114.2(2) . . ? C2A C1A C6A 118.4(7) . . ? C2A C1A P1 118.1(6) . . ? C6A C1A P1 123.5(6) . . ? C1A C2A C3A 121.4(9) . . ? C4A C3A C2A 119.2(10) . . ? C5A C4A C3A 120.6(9) . . ? C4A C5A C6A 121.1(9) . . ? C1A C6A C5A 119.0(8) . . ? C2B C1B C6B 118.5(6) . . ? C2B C1B P1 123.7(5) . . ? C6B C1B P1 117.8(5) . . ? C3B C2B C1B 120.4(7) . . ? C4B C3B C2B 120.7(8) . . ? C3B C4B C5B 119.9(7) . . ? C6B C5B C4B 119.7(7) . . ? C5B C6B C1B 120.7(6) . . ? C6C C1C C2C 120.6(7) . . ? C6C C1C P1 117.3(6) . . ? C2C C1C P1 122.1(6) . . ? C1C C2C C3C 115.9(9) . . ? C4C C3C C2C 122.2(10) . . ? C5C C4C C3C 118.7(9) . . ? C4C C5C C6C 123.0(11) . . ? C1C C6C C5C 119.7(9) . . ? C2D C1D C6D 118.5(7) . . ? C2D C1D P2 118.4(5) . . ? C6D C1D P2 123.1(6) . . ? C1D C2D C3D 121.0(7) . . ? C4D C3D C2D 119.4(8) . . ? C5D C4D C3D 120.7(8) . . ? C4D C5D C6D 120.1(8) . . ? C5D C6D C1D 120.1(8) . . ? C2E C1E C6E 117.4(7) . . ? C2E C1E P2 123.7(5) . . ? C6E C1E P2 118.8(6) . . ? C1E C2E C3E 122.1(8) . . ? C4E C3E C2E 119.7(8) . . ? C3E C4E C5E 120.2(8) . . ? C4E C5E C6E 119.3(8) . . ? C1E C6E C5E 121.3(8) . . ? C6F C1F C2F 117.5(7) . . ? C6F C1F P2 119.7(6) . . ? C2F C1F P2 122.8(6) . . ? C1F C2F C3F 121.3(9) . . ? C4F C3F C2F 118.8(9) . . ? C3F C4F C5F 120.7(9) . . ? C6F C5F C4F 119.5(11) . . ? C5F C6F C1F 122.1(9) . . ? Cl2 C1S Cl3 124.6(15) . . ? Cl2 C1S Cl5 22.1(10) . . ? Cl3 C1S Cl5 146.4(18) . . ? Cl2 C1S Cl6 110.3(16) . . ? Cl3 C1S Cl6 50.4(11) . . ? Cl5 C1S Cl6 124.2(17) . . ? Cl2 C1S Cl1 122.5(14) . . ? Cl3 C1S Cl1 26.8(6) . . ? Cl5 C1S Cl1 142.0(17) . . ? Cl6 C1S Cl1 23.9(9) . . ? Cl2 C1S Cl4 23.0(6) . . ? Cl3 C1S Cl4 118.7(14) . . ? Cl5 C1S Cl4 35.7(10) . . ? Cl6 C1S Cl4 89.6(14) . . ? Cl1 C1S Cl4 106.5(13) . . ? Cl6 Cl1 Cl3 146(2) . . ? Cl6 Cl1 C1S 75.0(14) . . ? Cl3 Cl1 C1S 73.0(11) . . ? Cl5 Cl2 Cl4 105(4) . . ? Cl5 Cl2 C1S 80.0(17) . . ? Cl4 Cl2 C1S 84.0(13) . . ? Cl1 Cl3 Cl6 16.1(11) . . ? Cl1 Cl3 C1S 80.3(11) . . ? Cl6 Cl3 C1S 65.3(8) . . ? Cl2 Cl4 Cl5 36(2) . . ? Cl2 Cl4 C1S 73.0(13) . . ? Cl5 Cl4 C1S 69.3(10) . . ? Cl2 Cl4 Cl6 113.3(15) . . ? Cl5 Cl4 Cl6 112.6(13) . . ? C1S Cl4 Cl6 44.3(8) . . ? Cl2 Cl5 Cl4 39(2) . . ? Cl2 Cl5 C1S 78.0(16) . . ? Cl4 Cl5 C1S 75.0(10) . . ? Cl1 Cl6 Cl3 17.9(12) . . ? Cl1 Cl6 C1S 81.1(16) . . ? Cl3 Cl6 C1S 64.3(9) . . ? Cl1 Cl6 Cl4 114(2) . . ? Cl3 Cl6 Cl4 96.2(10) . . ? C1S Cl6 Cl4 46.1(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Ag1 S1 C1 -100.9(2) . . . . ? S2 Ag1 S1 C1 72.5(2) . . . . ? P1 Ag1 S1 Ag2 18.12(10) . . . 3_565 ? S2 Ag1 S1 Ag2 -168.48(6) . . . 3_565 ? P1 Ag1 S2 C3 -2.9(3) . . . . ? S1 Ag1 S2 C3 -175.5(2) . . . . ? P1 Ag1 S2 Ag2 -98.84(7) . . . . ? S1 Ag1 S2 Ag2 88.57(6) . . . . ? P2 Ag2 S2 C3 55.1(3) . . . . ? S1 Ag2 S2 C3 -111.5(3) 3_565 . . . ? P2 Ag2 S2 Ag1 158.49(7) . . . . ? S1 Ag2 S2 Ag1 -8.10(6) 3_565 . . . ? Ag1 S1 C1 O1 13.1(7) . . . . ? Ag2 S1 C1 O1 -114.5(6) 3_565 . . . ? Ag1 S1 C1 C2 -165.8(5) . . . . ? Ag2 S1 C1 C2 66.6(6) 3_565 . . . ? O2A O2 C3 C4 101(3) . . . . ? O2A O2 C3 S2 -94(3) . . . . ? O2 O2A C3 C4 -103(3) . . . . ? O2 O2A C3 S2 110(2) . . . . ? Ag1 S2 C3 O2 -96.5(10) . . . . ? Ag2 S2 C3 O2 -7.5(10) . . . . ? Ag1 S2 C3 O2A -145.7(19) . . . . ? Ag2 S2 C3 O2A -57(2) . . . . ? Ag1 S2 C3 C4 68.3(6) . . . . ? Ag2 S2 C3 C4 157.3(6) . . . . ? S1 Ag1 P1 C1C 107.0(2) . . . . ? S2 Ag1 P1 C1C -65.1(2) . . . . ? S1 Ag1 P1 C1B -10.6(2) . . . . ? S2 Ag1 P1 C1B 177.2(2) . . . . ? S1 Ag1 P1 C1A -131.8(2) . . . . ? S2 Ag1 P1 C1A 56.1(3) . . . . ? S2 Ag2 P2 C1E 12.5(3) . . . . ? S1 Ag2 P2 C1E 176.8(3) 3_565 . . . ? S2 Ag2 P2 C1D -106.6(2) . . . . ? S1 Ag2 P2 C1D 57.8(3) 3_565 . . . ? S2 Ag2 P2 C1F 134.8(2) . . . . ? S1 Ag2 P2 C1F -60.9(3) 3_565 . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.309 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.127 #=====END ################################################### #Compound 4 data_tcd17 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H88 Ag4 O4 P4 S4' _chemical_formula_weight 1965.24 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 monoclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9826(2) _cell_length_b 12.7489(1) _cell_length_c 14.9433(2) _cell_angle_alpha 99.585(1) _cell_angle_beta 91.867(1) _cell_angle_gamma 95.328(1) _cell_volume 2238.53(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7657 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 23.220 _exptl_crystal_description 'rectangular shape, cut' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.8010 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9843 _diffrn_reflns_av_R_equivalents 0.0127 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 23.22 _reflns_number_total 6199 _reflns_number_gt 5570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+1.9703P] 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 SHELXL _refine_ls_extinction_coef 0.0047(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6199 _refine_ls_number_parameters 460 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.33413(2) 0.32346(2) 0.56391(2) 0.05506(12) Uani 1 1 d . . . Ag2 Ag 0.47188(2) 0.35398(2) 0.392812(19) 0.05791(12) Uani 1 1 d . . . S1 S 0.36369(7) 0.51443(7) 0.53655(7) 0.0549(2) Uani 1 1 d . . . S2 S 0.46379(7) 0.19772(7) 0.47658(6) 0.0513(2) Uani 1 1 d . . . O1 O 0.2611(2) 0.6513(2) 0.6464(2) 0.0840(9) Uani 1 1 d . . . O2 O 0.2535(3) 0.1252(3) 0.4273(2) 0.0846(9) Uani 1 1 d . . . P1 P 0.38015(8) 0.37879(7) 0.25180(6) 0.0492(2) Uani 1 1 d . . . P2 P 0.19571(8) 0.25469(7) 0.66413(6) 0.0500(2) Uani 1 1 d . . . C1 C 0.2488(3) 0.5735(3) 0.5876(3) 0.0540(9) Uani 1 1 d . . . C2 C 0.1339(3) 0.5228(4) 0.5514(4) 0.0823(13) Uani 1 1 d . . . H2A H 0.0776 0.5619 0.5822 0.123 Uiso 1 1 calc R . . H2B H 0.1247 0.4501 0.5615 0.123 Uiso 1 1 calc R . . H2C H 0.1263 0.5240 0.4874 0.123 Uiso 1 1 calc R . . C3 C 0.3502(3) 0.1043(3) 0.4286(3) 0.0592(9) Uani 1 1 d . . . C4 C 0.3785(5) -0.0054(4) 0.3926(5) 0.118(2) Uani 1 1 d . . . H4A H 0.4582 -0.0079 0.3992 0.178 Uiso 1 1 calc R . . H4B H 0.3548 -0.0239 0.3295 0.178 Uiso 1 1 calc R . . H4C H 0.3410 -0.0553 0.4259 0.178 Uiso 1 1 calc R . . C1A C 0.4179(3) 0.5107(3) 0.2221(2) 0.0479(8) Uani 1 1 d . . . C2A C 0.4389(3) 0.5294(3) 0.1352(3) 0.0637(10) Uani 1 1 d . . . H2A H 0.4365 0.4718 0.0877 0.076 Uiso 1 1 calc R . . C3A C 0.4632(4) 0.6322(3) 0.1178(3) 0.0770(12) Uani 1 1 d . . . H3A H 0.4780 0.6433 0.0592 0.092 Uiso 1 1 calc R . . C4A C 0.4655(4) 0.7178(3) 0.1875(3) 0.0757(12) Uani 1 1 d . . . H4A H 0.4813 0.7869 0.1759 0.091 Uiso 1 1 calc R . . C5A C 0.4442(3) 0.7013(3) 0.2749(3) 0.0649(10) Uani 1 1 d . . . H5A H 0.4449 0.7594 0.3218 0.078 Uiso 1 1 calc R . . C6A C 0.4219(3) 0.5987(3) 0.2925(2) 0.0537(9) Uani 1 1 d . . . H6A H 0.4095 0.5879 0.3515 0.064 Uiso 1 1 calc R . . C1B C 0.4163(3) 0.2845(3) 0.1536(3) 0.0592(10) Uani 1 1 d . . . C2B C 0.3489(4) 0.2528(4) 0.0756(3) 0.0793(12) Uani 1 1 d . . . H2B H 0.2800 0.2801 0.0712 0.095 Uiso 1 1 calc R . . C3B C 0.3819(6) 0.1809(4) 0.0033(4) 0.0987(17) Uani 1 1 d . . . H3B H 0.3354 0.1600 -0.0489 0.118 Uiso 1 1 calc R . . C4B C 0.4821(8) 0.1416(4) 0.0096(5) 0.115(2) Uani 1 1 d . . . H4B H 0.5044 0.0935 -0.0388 0.138 Uiso 1 1 calc R . . C5B C 0.5510(6) 0.1712(5) 0.0852(5) 0.121(2) Uani 1 1 d . . . H5B H 0.6198 0.1434 0.0884 0.145 Uiso 1 1 calc R . . C6B C 0.5185(5) 0.2428(4) 0.1579(4) 0.0905(15) Uani 1 1 d . . . H6B H 0.5658 0.2629 0.2098 0.109 Uiso 1 1 calc R . . C1C C 0.2268(3) 0.3700(3) 0.2475(2) 0.0519(8) Uani 1 1 d . . . C2C C 0.1695(4) 0.3075(3) 0.3030(3) 0.0692(11) Uani 1 1 d . . . H2C H 0.2092 0.2716 0.3408 0.083 Uiso 1 1 calc R . . C3C C 0.0530(4) 0.2993(4) 0.3015(4) 0.0883(15) Uani 1 1 d . . . H3C H 0.0148 0.2575 0.3383 0.106 Uiso 1 1 calc R . . C4C C -0.0062(4) 0.3525(4) 0.2461(4) 0.0872(15) Uani 1 1 d . . . H4C H -0.0841 0.3461 0.2453 0.105 Uiso 1 1 calc R . . C5C C 0.0488(4) 0.4141(4) 0.1927(3) 0.0785(12) Uani 1 1 d . . . H5C H 0.0082 0.4495 0.1551 0.094 Uiso 1 1 calc R . . C6C C 0.1647(3) 0.4248(3) 0.1938(3) 0.0638(10) Uani 1 1 d . . . H6C H 0.2015 0.4691 0.1582 0.077 Uiso 1 1 calc R . . C1D C 0.0497(3) 0.2471(3) 0.6231(2) 0.0535(9) Uani 1 1 d . . . C2D C 0.0135(4) 0.1716(4) 0.5468(3) 0.0818(13) Uani 1 1 d . . . H2D H 0.0631 0.1261 0.5189 0.098 Uiso 1 1 calc R . . C3D C -0.0974(4) 0.1642(5) 0.5123(4) 0.0982(16) Uani 1 1 d . . . H3D H -0.1215 0.1124 0.4622 0.118 Uiso 1 1 calc R . . C4D C -0.1708(4) 0.2323(5) 0.5513(4) 0.0900(15) Uani 1 1 d . . . H4D H -0.2442 0.2273 0.5275 0.108 Uiso 1 1 calc R . . C5D C -0.1357(4) 0.3072(5) 0.6251(4) 0.0915(15) Uani 1 1 d . . . H5D H -0.1853 0.3537 0.6517 0.110 Uiso 1 1 calc R . . C6D C -0.0261(3) 0.3148(4) 0.6610(3) 0.0700(11) Uani 1 1 d . . . H6D H -0.0034 0.3665 0.7115 0.084 Uiso 1 1 calc R . . C1E C 0.2069(3) 0.1196(3) 0.6891(3) 0.0560(9) Uani 1 1 d . . . C2E C 0.3055(4) 0.0728(3) 0.6730(3) 0.0704(11) Uani 1 1 d . . . H2E H 0.3651 0.1096 0.6494 0.085 Uiso 1 1 calc R . . C3E C 0.3161(4) -0.0298(4) 0.6920(4) 0.0916(15) Uani 1 1 d . . . H3E H 0.3826 -0.0608 0.6806 0.110 Uiso 1 1 calc R . . C4E C 0.2303(5) -0.0841(4) 0.7267(4) 0.0952(16) Uani 1 1 d . . . H4E H 0.2380 -0.1519 0.7399 0.114 Uiso 1 1 calc R . . C5E C 0.1321(5) -0.0390(4) 0.7425(4) 0.0984(17) Uani 1 1 d . . . H5E H 0.0735 -0.0762 0.7669 0.118 Uiso 1 1 calc R . . C6E C 0.1189(4) 0.0613(3) 0.7225(4) 0.0815(13) Uani 1 1 d . . . H6E H 0.0507 0.0899 0.7315 0.098 Uiso 1 1 calc R . . C1F C 0.2009(3) 0.3398(3) 0.7763(2) 0.0542(9) Uani 1 1 d . . . C2F C 0.2608(3) 0.4389(3) 0.7881(3) 0.0666(10) Uani 1 1 d . . . H2F H 0.2995 0.4601 0.7401 0.080 Uiso 1 1 calc R . . C3F C 0.2641(4) 0.5075(4) 0.8709(4) 0.0872(14) Uani 1 1 d . . . H3F H 0.3042 0.5746 0.8777 0.105 Uiso 1 1 calc R . . C4F C 0.2089(5) 0.4772(5) 0.9424(3) 0.0879(14) Uani 1 1 d . . . H4F H 0.2124 0.5230 0.9980 0.105 Uiso 1 1 calc R . . C5F C 0.1488(5) 0.3799(5) 0.9318(3) 0.0977(16) Uani 1 1 d . . . H5F H 0.1104 0.3598 0.9803 0.117 Uiso 1 1 calc R . . C6F C 0.1438(4) 0.3102(4) 0.8498(3) 0.0825(13) Uani 1 1 d . . . H6F H 0.1025 0.2437 0.8436 0.099 Uiso 1 1 calc R . . C1S C -0.1909(15) -0.0335(12) 0.8187(10) 0.185(3) Uiso 0.60 1 d PGD A 1 H1SA H -0.2128 -0.0251 0.7581 0.222 Uiso 0.60 1 calc PR A 1 H1SB H -0.2480 -0.0786 0.8414 0.222 Uiso 0.60 1 calc PR A 1 H2SC H -0.1215 -0.0656 0.8179 0.222 Uiso 0.60 1 calc PR A 1 C2S C -0.1784(11) 0.0565(7) 0.8692(7) 0.185(3) Uiso 0.60 1 d PGD A 1 C3S C -0.1587(10) 0.0611(8) 0.9621(7) 0.185(3) Uiso 0.60 1 d PGD A 1 H3S H -0.1574 -0.0016 0.9859 0.222 Uiso 0.60 1 calc PR A 1 C4S C -0.1408(10) 0.1596(10) 1.0192(6) 0.185(3) Uiso 0.60 1 d PG A 1 H4S H -0.1276 0.1627 1.0813 0.222 Uiso 0.60 1 calc PR A 1 C5S C -0.1427(10) 0.2534(8) 0.9835(8) 0.185(3) Uiso 0.60 1 d PG A 1 H5S H -0.1308 0.3193 1.0218 0.222 Uiso 0.60 1 calc PR A 1 C6S C -0.1625(10) 0.2488(8) 0.8907(8) 0.185(3) Uiso 0.60 1 d PG A 1 H6S H -0.1637 0.3115 0.8668 0.222 Uiso 0.60 1 calc PR A 1 C7S C -0.1803(12) 0.1503(9) 0.8336(6) 0.185(3) Uiso 0.60 1 d PGD A 1 H7S H -0.1935 0.1472 0.7714 0.222 Uiso 0.60 1 calc PR A 1 C1SA C -0.0666(19) 0.1726(16) 1.0372(14) 0.185(4) Uiso 0.40 1 d PGD B 2 H1SD H -0.0718 0.2478 1.0405 0.222 Uiso 0.40 1 calc PR B 2 H1SE H 0.0075 0.1564 1.0210 0.222 Uiso 0.40 1 calc PR B 2 H1SF H -0.0815 0.1528 1.0953 0.222 Uiso 0.40 1 calc PR B 2 C2SA C -0.1390(16) 0.1198(12) 0.9767(9) 0.185(4) Uiso 0.40 1 d PGD B 2 C3SA C -0.1258(15) 0.0112(12) 0.9586(11) 0.185(4) Uiso 0.40 1 d PGD B 2 H3SA H -0.1082 -0.0245 1.0058 0.222 Uiso 0.40 1 calc PR B 2 C4SA C -0.1389(14) -0.0439(10) 0.8699(12) 0.185(4) Uiso 0.40 1 d PG B 2 H4SA H -0.1301 -0.1166 0.8577 0.222 Uiso 0.40 1 calc PR B 2 C5SA C -0.1651(16) 0.0095(14) 0.7993(9) 0.185(4) Uiso 0.40 1 d PG B 2 H5SA H -0.1739 -0.0274 0.7399 0.222 Uiso 0.40 1 calc PR B 2 C6SA C -0.1783(17) 0.1180(15) 0.8174(10) 0.185(4) Uiso 0.40 1 d PG B 2 H6SA H -0.1959 0.1538 0.7702 0.222 Uiso 0.40 1 calc PR B 2 C7SA C -0.1653(16) 0.1732(11) 0.9062(12) 0.185(4) Uiso 0.40 1 d PGD B 2 H7SA H -0.1741 0.2458 0.9183 0.222 Uiso 0.40 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04980(18) 0.04982(18) 0.0652(2) 0.00726(13) 0.01099(13) 0.00460(12) Ag2 0.05605(19) 0.0580(2) 0.0621(2) 0.02134(14) -0.00113(13) -0.00031(13) S1 0.0465(5) 0.0437(5) 0.0732(6) 0.0061(4) 0.0161(4) 0.0000(4) S2 0.0516(5) 0.0442(5) 0.0612(5) 0.0147(4) 0.0066(4) 0.0087(4) O1 0.0679(18) 0.0639(19) 0.113(2) -0.0125(18) 0.0178(17) 0.0120(14) O2 0.0617(19) 0.078(2) 0.110(3) 0.0072(17) 0.0009(17) 0.0005(15) P1 0.0490(5) 0.0473(5) 0.0522(5) 0.0133(4) 0.0021(4) 0.0010(4) P2 0.0467(5) 0.0444(5) 0.0595(6) 0.0101(4) 0.0077(4) 0.0033(4) C1 0.046(2) 0.045(2) 0.073(2) 0.0142(19) 0.0098(17) 0.0057(15) C2 0.046(2) 0.077(3) 0.124(4) 0.021(3) -0.004(2) 0.002(2) C3 0.062(2) 0.047(2) 0.071(2) 0.0146(18) 0.0047(19) 0.0052(18) C4 0.109(4) 0.053(3) 0.182(6) -0.010(3) -0.027(4) 0.010(3) C1A 0.0444(18) 0.0470(19) 0.053(2) 0.0123(16) 0.0017(15) 0.0006(15) C2A 0.079(3) 0.054(2) 0.056(2) 0.0075(18) 0.0115(19) -0.0013(19) C3A 0.110(4) 0.060(3) 0.064(3) 0.022(2) 0.017(2) -0.001(2) C4A 0.101(3) 0.049(2) 0.079(3) 0.021(2) 0.007(2) -0.005(2) C5A 0.075(3) 0.048(2) 0.069(3) 0.0051(19) -0.001(2) 0.0058(19) C6A 0.056(2) 0.056(2) 0.050(2) 0.0135(17) 0.0024(16) 0.0044(17) C1B 0.070(2) 0.043(2) 0.067(2) 0.0140(17) 0.017(2) 0.0040(18) C2B 0.090(3) 0.069(3) 0.072(3) -0.004(2) 0.010(2) 0.000(2) C3B 0.144(5) 0.070(3) 0.077(3) 0.001(3) 0.018(3) 0.000(3) C4B 0.202(8) 0.054(3) 0.099(4) 0.020(3) 0.068(5) 0.030(4) C5B 0.147(6) 0.102(5) 0.126(5) 0.021(4) 0.048(5) 0.065(4) C6B 0.101(4) 0.078(3) 0.099(4) 0.017(3) 0.021(3) 0.035(3) C1C 0.053(2) 0.048(2) 0.051(2) 0.0047(16) 0.0039(16) -0.0033(16) C2C 0.067(3) 0.065(3) 0.075(3) 0.016(2) 0.010(2) -0.007(2) C3C 0.072(3) 0.085(3) 0.103(4) 0.013(3) 0.029(3) -0.021(3) C4C 0.053(3) 0.100(4) 0.099(4) -0.007(3) 0.009(3) -0.004(2) C5C 0.060(3) 0.095(3) 0.078(3) 0.006(3) -0.007(2) 0.014(2) C6C 0.054(2) 0.076(3) 0.060(2) 0.014(2) 0.0001(18) 0.0023(19) C1D 0.048(2) 0.053(2) 0.060(2) 0.0139(17) 0.0057(16) 0.0005(16) C2D 0.066(3) 0.092(3) 0.081(3) -0.005(3) 0.000(2) 0.005(2) C3D 0.078(3) 0.118(4) 0.088(4) 0.003(3) -0.019(3) -0.011(3) C4D 0.055(3) 0.115(4) 0.104(4) 0.042(3) -0.013(3) -0.003(3) C5D 0.060(3) 0.109(4) 0.112(4) 0.028(3) 0.006(3) 0.024(3) C6D 0.060(2) 0.072(3) 0.079(3) 0.010(2) 0.006(2) 0.014(2) C1E 0.057(2) 0.046(2) 0.066(2) 0.0133(17) 0.0096(18) 0.0025(17) C2E 0.061(2) 0.061(2) 0.094(3) 0.023(2) 0.008(2) 0.009(2) C3E 0.085(3) 0.075(3) 0.123(4) 0.033(3) 0.008(3) 0.027(3) C4E 0.121(4) 0.057(3) 0.115(4) 0.033(3) 0.012(3) 0.015(3) C5E 0.111(4) 0.058(3) 0.132(5) 0.035(3) 0.031(3) -0.006(3) C6E 0.078(3) 0.057(3) 0.114(4) 0.027(2) 0.028(3) 0.004(2) C1F 0.050(2) 0.057(2) 0.057(2) 0.0124(17) 0.0001(16) 0.0107(17) C2F 0.066(2) 0.062(3) 0.067(3) 0.002(2) 0.007(2) -0.001(2) C3F 0.091(3) 0.076(3) 0.085(3) -0.004(3) -0.003(3) -0.005(3) C4F 0.099(4) 0.099(4) 0.060(3) -0.004(3) -0.012(3) 0.017(3) C5F 0.121(4) 0.118(5) 0.055(3) 0.020(3) 0.009(3) 0.008(4) C6F 0.101(4) 0.083(3) 0.062(3) 0.019(2) 0.009(2) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P2 2.4680(9) . ? Ag1 S1 2.5300(9) . ? Ag1 S2 2.5661(9) . ? Ag1 Ag2 3.1464(4) . ? Ag2 P1 2.4257(9) . ? Ag2 S2 2.5194(9) . ? Ag2 S1 2.5440(9) 2_666 ? S1 C1 1.765(4) . ? S1 Ag2 2.5440(9) 2_666 ? S2 C3 1.770(4) . ? O1 C1 1.205(5) . ? O2 C3 1.213(5) . ? P1 C1B 1.826(4) . ? P1 C1C 1.829(4) . ? P1 C1A 1.830(3) . ? P2 C1D 1.824(4) . ? P2 C1F 1.834(4) . ? P2 C1E 1.837(4) . ? C1 C2 1.508(5) . ? C3 C4 1.487(6) . ? C1A C2A 1.386(5) . ? C1A C6A 1.400(5) . ? C2A C3A 1.386(5) . ? C3A C4A 1.375(6) . ? C4A C5A 1.385(6) . ? C5A C6A 1.381(5) . ? C1B C2B 1.376(6) . ? C1B C6B 1.384(6) . ? C2B C3B 1.389(7) . ? C3B C4B 1.350(9) . ? C4B C5B 1.356(10) . ? C5B C6B 1.389(8) . ? C1C C6C 1.390(5) . ? C1C C2C 1.395(5) . ? C2C C3C 1.389(6) . ? C3C C4C 1.372(7) . ? C4C C5C 1.354(7) . ? C5C C6C 1.383(6) . ? C1D C6D 1.381(5) . ? C1D C2D 1.391(6) . ? C2D C3D 1.399(7) . ? C3D C4D 1.369(8) . ? C4D C5D 1.360(8) . ? C5D C6D 1.391(6) . ? C1E C2E 1.382(5) . ? C1E C6E 1.389(6) . ? C2E C3E 1.400(6) . ? C3E C4E 1.352(7) . ? C4E C5E 1.367(7) . ? C5E C6E 1.382(6) . ? C1F C2F 1.375(5) . ? C1F C6F 1.399(6) . ? C2F C3F 1.388(6) . ? C3F C4F 1.366(7) . ? C4F C5F 1.358(7) . ? C5F C6F 1.385(7) . ? C1S C2S 1.258(15) . ? C2S C3S 1.3900 . ? C2S C7S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C6S C7S 1.3900 . ? C1SA C2SA 1.289(17) . ? C2SA C3SA 1.3900 . ? C2SA C7SA 1.3900 . ? C3SA C4SA 1.3900 . ? C4SA C5SA 1.3900 . ? C5SA C6SA 1.3900 . ? C6SA C7SA 1.3900 . ? 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 P2 Ag1 S1 125.62(3) . . ? P2 Ag1 S2 120.18(3) . . ? S1 Ag1 S2 114.21(3) . . ? P2 Ag1 Ag2 162.41(3) . . ? S1 Ag1 Ag2 65.46(2) . . ? S2 Ag1 Ag2 51.11(2) . . ? P1 Ag2 S2 131.99(3) . . ? P1 Ag2 S1 119.51(3) . 2_666 ? S2 Ag2 S1 107.33(3) . 2_666 ? P1 Ag2 Ag1 121.44(2) . . ? S2 Ag2 Ag1 52.45(2) . . ? S1 Ag2 Ag1 101.76(2) 2_666 . ? C1 S1 Ag1 103.43(12) . . ? C1 S1 Ag2 101.76(13) . 2_666 ? Ag1 S1 Ag2 123.48(4) . 2_666 ? C3 S2 Ag2 108.40(13) . . ? C3 S2 Ag1 92.86(13) . . ? Ag2 S2 Ag1 76.44(3) . . ? C1B P1 C1C 105.52(17) . . ? C1B P1 C1A 104.58(16) . . ? C1C P1 C1A 102.35(16) . . ? C1B P1 Ag2 113.05(13) . . ? C1C P1 Ag2 116.75(12) . . ? C1A P1 Ag2 113.30(11) . . ? C1D P2 C1F 104.35(17) . . ? C1D P2 C1E 102.44(17) . . ? C1F P2 C1E 104.35(17) . . ? C1D P2 Ag1 114.94(12) . . ? C1F P2 Ag1 111.91(12) . . ? C1E P2 Ag1 117.41(12) . . ? O1 C1 C2 121.8(4) . . ? O1 C1 S1 122.1(3) . . ? C2 C1 S1 116.0(3) . . ? O2 C3 C4 120.4(4) . . ? O2 C3 S2 123.3(3) . . ? C4 C3 S2 116.2(3) . . ? C2A C1A C6A 118.3(3) . . ? C2A C1A P1 124.7(3) . . ? C6A C1A P1 117.0(3) . . ? C1A C2A C3A 121.2(4) . . ? C4A C3A C2A 119.7(4) . . ? C3A C4A C5A 120.2(4) . . ? C6A C5A C4A 120.0(4) . . ? C5A C6A C1A 120.5(3) . . ? C2B C1B C6B 118.0(4) . . ? C2B C1B P1 124.4(3) . . ? C6B C1B P1 117.6(4) . . ? C1B C2B C3B 121.3(5) . . ? C4B C3B C2B 119.4(6) . . ? C3B C4B C5B 121.1(5) . . ? C4B C5B C6B 119.9(6) . . ? C1B C6B C5B 120.3(6) . . ? C6C C1C C2C 118.4(4) . . ? C6C C1C P1 123.2(3) . . ? C2C C1C P1 118.3(3) . . ? C3C C2C C1C 119.8(4) . . ? C4C C3C C2C 120.5(4) . . ? C5C C4C C3C 120.1(4) . . ? C4C C5C C6C 120.5(5) . . ? C5C C6C C1C 120.6(4) . . ? C6D C1D C2D 117.9(4) . . ? C6D C1D P2 123.8(3) . . ? C2D C1D P2 118.2(3) . . ? C1D C2D C3D 120.1(5) . . ? C4D C3D C2D 120.7(5) . . ? C5D C4D C3D 119.5(5) . . ? C4D C5D C6D 120.5(5) . . ? C1D C6D C5D 121.2(4) . . ? C2E C1E C6E 118.2(4) . . ? C2E C1E P2 119.5(3) . . ? C6E C1E P2 122.4(3) . . ? C1E C2E C3E 120.4(4) . . ? C4E C3E C2E 120.4(5) . . ? C3E C4E C5E 119.8(5) . . ? C4E C5E C6E 120.8(5) . . ? C5E C6E C1E 120.3(5) . . ? C2F C1F C6F 118.3(4) . . ? C2F C1F P2 118.6(3) . . ? C6F C1F P2 123.1(3) . . ? C1F C2F C3F 120.7(4) . . ? C4F C3F C2F 120.5(5) . . ? C5F C4F C3F 119.6(5) . . ? C4F C5F C6F 120.9(5) . . ? C5F C6F C1F 120.0(5) . . ? C1S C2S C3S 118.7(8) . . ? C1S C2S C7S 121.2(8) . . ? C3S C2S C7S 120.0 . . ? C4S C3S C2S 120.0 . . ? C3S C4S C5S 120.0 . . ? C4S C5S C6S 120.0 . . ? C7S C6S C5S 120.0 . . ? C6S C7S C2S 120.0 . . ? C1SA C2SA C3SA 112.9(9) . . ? C1SA C2SA C7SA 114.7(9) . . ? C3SA C2SA C7SA 120.0 . . ? C4SA C3SA C2SA 120.0 . . ? C3SA C4SA C5SA 120.0 . . ? C4SA C5SA C6SA 120.0 . . ? C5SA C6SA C7SA 120.0 . . ? C6SA C7SA C2SA 120.0 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 23.22 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.592 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.067 #=====END ################################################### #compound 5 data_tcd6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H84 Ag4 Cl4 O4 P4 S4' _chemical_formula_weight 2199.09 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0019(4) _cell_length_b 13.1172(4) _cell_length_c 14.8424(4) _cell_angle_alpha 104.381(1) _cell_angle_beta 100.511(1) _cell_angle_gamma 100.170(1) _cell_volume 2344.52(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 29.26 _exptl_crystal_description 'multifaceted blocks' _exptl_crystal_colour 'creamy ' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.60886 _exptl_absorpt_correction_T_max 0.77872 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14856 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 29.26 _reflns_number_total 10574 _reflns_number_gt 9060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+2.8745P] 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 SHELXL _refine_ls_extinction_coef 0.0016(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10574 _refine_ls_number_parameters 561 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.14667(2) 0.54397(2) 0.947112(18) 0.04875(8) Uani 1 1 d . . . Ag2 Ag -0.13858(2) 0.31752(2) 0.796566(19) 0.05160(9) Uani 1 1 d . . . S1 S 0.21628(7) 0.53307(7) 1.11226(6) 0.04572(18) Uani 1 1 d . . . S2 S 0.05901(7) 0.35403(7) 0.83849(6) 0.04963(19) Uani 1 1 d . . . O1 O 0.0385(2) 0.3778(2) 1.05858(19) 0.0590(6) Uani 1 1 d . . . O2 O 0.0160(2) 0.3195(3) 0.6521(2) 0.0780(9) Uani 1 1 d . . . C1 C 0.1249(2) 0.4183(3) 1.1167(2) 0.0422(7) Uani 1 1 d . . . C2 C 0.0868(3) 0.3444(3) 0.7247(2) 0.0502(8) Uani 1 1 d . . . C11 C 0.1592(3) 0.3681(3) 1.1944(2) 0.0435(7) Uani 1 1 d . . . C12 C 0.1045(3) 0.2630(3) 1.1859(3) 0.0560(8) Uani 1 1 d . . . H12 H 0.0478 0.2262 1.1331 0.067 Uiso 1 1 calc R . . C13 C 0.1341(4) 0.2138(4) 1.2554(3) 0.0711(11) Uani 1 1 d . . . H13 H 0.0977 0.1437 1.2491 0.085 Uiso 1 1 calc R . . C14 C 0.2177(4) 0.2685(4) 1.3344(3) 0.0768(13) Uani 1 1 d . . . H14 H 0.2376 0.2350 1.3811 0.092 Uiso 1 1 calc R . . C15 C 0.2710(4) 0.3710(4) 1.3440(3) 0.0754(12) Uani 1 1 d . . . H15 H 0.3268 0.4075 1.3975 0.090 Uiso 1 1 calc R . . C16 C 0.2427(3) 0.4219(3) 1.2743(3) 0.0581(9) Uani 1 1 d . . . H16 H 0.2797 0.4920 1.2813 0.070 Uiso 1 1 calc R . . C21 C 0.2028(3) 0.3685(3) 0.7201(2) 0.0489(8) Uani 1 1 d . . . C22 C 0.2254(4) 0.3829(3) 0.6355(3) 0.0653(10) Uani 1 1 d . . . H22 H 0.1696 0.3796 0.5850 0.078 Uiso 1 1 calc R . . C23 C 0.3300(4) 0.4021(4) 0.6259(4) 0.0792(13) Uani 1 1 d . . . H23 H 0.3442 0.4122 0.5692 0.095 Uiso 1 1 calc R . . C24 C 0.4136(4) 0.4066(4) 0.7000(4) 0.0752(12) Uani 1 1 d . . . H24 H 0.4840 0.4187 0.6930 0.090 Uiso 1 1 calc R . . C25 C 0.3922(4) 0.3931(4) 0.7838(3) 0.0718(11) Uani 1 1 d . . . H25 H 0.4484 0.3966 0.8341 0.086 Uiso 1 1 calc R . . C26 C 0.2877(3) 0.3743(3) 0.7940(3) 0.0604(9) Uani 1 1 d . . . H26 H 0.2741 0.3654 0.8513 0.072 Uiso 1 1 calc R . . P1 P 0.22924(6) 0.69134(6) 0.89210(6) 0.03907(17) Uani 1 1 d . . . P2 P -0.27149(7) 0.17813(7) 0.66915(6) 0.04350(18) Uani 1 1 d . . . C1A C 0.1611(3) 0.7034(3) 0.7774(2) 0.0434(7) Uani 1 1 d . . . C2A C 0.0858(3) 0.6135(3) 0.7149(2) 0.0545(8) Uani 1 1 d . . . H2A H 0.0696 0.5508 0.7332 0.065 Uiso 1 1 calc R . . C3A C 0.0345(4) 0.6163(4) 0.6254(3) 0.0718(12) Uani 1 1 d . . . H3A H -0.0153 0.5553 0.5840 0.086 Uiso 1 1 calc R . . C4A C 0.0566(4) 0.7081(4) 0.5976(3) 0.0754(13) Uani 1 1 d . . . H4A H 0.0223 0.7093 0.5373 0.090 Uiso 1 1 calc R . . C5A C 0.1297(4) 0.7985(4) 0.6589(3) 0.0726(12) Uani 1 1 d . . . H5A H 0.1449 0.8609 0.6400 0.087 Uiso 1 1 calc R . . C6A C 0.1807(3) 0.7968(3) 0.7490(3) 0.0585(9) Uani 1 1 d . . . H6A H 0.2286 0.8589 0.7908 0.070 Uiso 1 1 calc R . . C1B C 0.3659(3) 0.6819(3) 0.8815(2) 0.0430(7) Uani 1 1 d . . . C2B C 0.4106(3) 0.7030(3) 0.8082(3) 0.0526(8) Uani 1 1 d . . . H2B H 0.3697 0.7215 0.7591 0.063 Uiso 1 1 calc R . . C3B C 0.5160(3) 0.6966(3) 0.8077(3) 0.0650(10) Uani 1 1 d . . . H3B H 0.5450 0.7101 0.7578 0.078 Uiso 1 1 calc R . . C4B C 0.5778(3) 0.6705(4) 0.8803(3) 0.0731(12) Uani 1 1 d . . . H4B H 0.6489 0.6680 0.8805 0.088 Uiso 1 1 calc R . . C5B C 0.5334(3) 0.6481(4) 0.9529(3) 0.0763(13) Uani 1 1 d . . . H5B H 0.5746 0.6295 1.0017 0.092 Uiso 1 1 calc R . . C6B C 0.4280(3) 0.6531(4) 0.9536(3) 0.0628(10) Uani 1 1 d . . . H6B H 0.3987 0.6371 1.0025 0.075 Uiso 1 1 calc R . . C1C C 0.2533(2) 0.8253(3) 0.9767(2) 0.0421(7) Uani 1 1 d . . . C2C C 0.1862(3) 0.8417(3) 1.0391(2) 0.0527(8) Uani 1 1 d . . . H2C H 0.1291 0.7859 1.0355 0.063 Uiso 1 1 calc R . . C3C C 0.2043(4) 0.9416(4) 1.1068(3) 0.0654(10) Uani 1 1 d . . . H3C H 0.1598 0.9520 1.1491 0.079 Uiso 1 1 calc R . . C4C C 0.2878(4) 1.0251(3) 1.1116(3) 0.0711(12) Uani 1 1 d . . . H4C H 0.2993 1.0918 1.1568 0.085 Uiso 1 1 calc R . . C5C C 0.3537(3) 1.0099(3) 1.0501(3) 0.0691(11) Uani 1 1 d . . . H5C H 0.4097 1.0666 1.0532 0.083 Uiso 1 1 calc R . . C6C C 0.3378(3) 0.9109(3) 0.9834(3) 0.0567(9) Uani 1 1 d . . . H6C H 0.3839 0.9010 0.9425 0.068 Uiso 1 1 calc R . . C1D C -0.2226(3) 0.0708(3) 0.5972(2) 0.0466(7) Uani 1 1 d . . . C2D C -0.1253(3) 0.0515(3) 0.6360(3) 0.0565(9) Uani 1 1 d . . . H2D H -0.0862 0.0928 0.6970 0.068 Uiso 1 1 calc R . . C3D C -0.0862(4) -0.0301(4) 0.5830(4) 0.0718(12) Uani 1 1 d . . . H3D H -0.0207 -0.0428 0.6089 0.086 Uiso 1 1 calc R . . C4D C -0.1435(4) -0.0918(4) 0.4931(4) 0.0782(13) Uani 1 1 d . . . H4D H -0.1171 -0.1465 0.4586 0.094 Uiso 1 1 calc R . . C5D C -0.2399(4) -0.0729(3) 0.4539(3) 0.0754(12) Uani 1 1 d . . . H5D H -0.2786 -0.1146 0.3928 0.090 Uiso 1 1 calc R . . C6D C -0.2792(4) 0.0082(3) 0.5054(3) 0.0644(10) Uani 1 1 d . . . H6D H -0.3443 0.0210 0.4784 0.077 Uiso 1 1 calc R . . C1E C -0.3313(3) 0.2409(3) 0.5818(2) 0.0467(7) Uani 1 1 d . . . C2E C -0.4404(3) 0.2351(3) 0.5553(3) 0.0573(9) Uani 1 1 d . . . H2E H -0.4881 0.1953 0.5805 0.069 Uiso 1 1 calc R . . C3E C -0.4789(4) 0.2885(4) 0.4913(3) 0.0689(11) Uani 1 1 d . . . H3E H -0.5524 0.2837 0.4733 0.083 Uiso 1 1 calc R . . C4E C -0.4086(4) 0.3488(4) 0.4541(3) 0.0705(12) Uani 1 1 d . . . H4E H -0.4345 0.3855 0.4120 0.085 Uiso 1 1 calc R . . C5E C -0.3006(4) 0.3542(4) 0.4795(3) 0.0751(12) Uani 1 1 d . . . H5E H -0.2533 0.3932 0.4535 0.090 Uiso 1 1 calc R . . C6E C -0.2618(3) 0.3017(3) 0.5437(3) 0.0654(10) Uani 1 1 d . . . H6E H -0.1882 0.3073 0.5617 0.078 Uiso 1 1 calc R . . C1F C -0.3867(3) 0.1108(3) 0.7041(2) 0.0462(7) Uani 1 1 d . . . C2F C -0.4249(3) 0.1736(3) 0.7736(3) 0.0624(10) Uani 1 1 d . . . H2F H -0.3910 0.2464 0.8014 0.075 Uiso 1 1 calc R . . C3F C -0.5139(4) 0.1288(4) 0.8024(3) 0.0776(13) Uani 1 1 d . . . H3F H -0.5402 0.1718 0.8485 0.093 Uiso 1 1 calc R . . C4F C -0.5630(4) 0.0207(4) 0.7628(3) 0.0734(12) Uani 1 1 d . . . H4F H -0.6225 -0.0092 0.7822 0.088 Uiso 1 1 calc R . . C5F C -0.5247(4) -0.0428(3) 0.6949(3) 0.0688(11) Uani 1 1 d . . . H5F H -0.5579 -0.1160 0.6686 0.083 Uiso 1 1 calc R . . C6F C -0.4363(3) 0.0018(3) 0.6654(3) 0.0574(9) Uani 1 1 d . . . H6F H -0.4103 -0.0417 0.6194 0.069 Uiso 1 1 calc R . . C1S C 0.1633(7) 0.1416(7) 0.9120(6) 0.100(3) Uani 0.70 1 d PD A 1 H1SA H 0.2298 0.1533 0.9593 0.120 Uiso 0.70 1 calc PR A 1 H1SB H 0.1373 0.2075 0.9231 0.120 Uiso 0.70 1 calc PR A 1 Cl1 Cl 0.1833(3) 0.1003(2) 0.7908(3) 0.1342(10) Uani 0.70 1 d PD A 1 Cl2 Cl 0.0665(3) 0.0323(3) 0.9166(3) 0.1488(14) Uani 0.70 1 d PD A 1 C2S C 0.2049(18) 0.187(2) 0.9681(18) 0.159(3) Uiso 0.30 1 d PD B 2 H2SA H 0.1988 0.2613 0.9756 0.191 Uiso 0.30 1 calc PR B 2 H2SB H 0.2523 0.1822 1.0246 0.191 Uiso 0.30 1 calc PR B 2 Cl1A Cl 0.2420(8) 0.1300(8) 0.8609(7) 0.159(3) Uiso 0.30 1 d PD B 2 Cl2A Cl 0.0718(10) 0.0893(9) 0.9344(9) 0.159(3) Uiso 0.30 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.05010(15) 0.04778(14) 0.04901(15) 0.01930(11) 0.01194(11) 0.00536(11) Ag2 0.05011(15) 0.04605(14) 0.05015(15) 0.01015(11) 0.00723(11) -0.00017(11) S1 0.0465(4) 0.0469(4) 0.0417(4) 0.0135(3) 0.0102(3) 0.0048(3) S2 0.0480(4) 0.0481(4) 0.0447(4) 0.0067(3) 0.0085(3) 0.0028(4) O1 0.0453(13) 0.0655(16) 0.0608(15) 0.0258(13) -0.0003(11) 0.0022(12) O2 0.0681(18) 0.103(2) 0.0484(15) 0.0199(15) -0.0017(13) 0.0016(17) C1 0.0404(16) 0.0450(16) 0.0429(16) 0.0128(13) 0.0135(13) 0.0104(13) C2 0.057(2) 0.0428(17) 0.0460(18) 0.0097(14) 0.0080(15) 0.0079(15) C11 0.0432(16) 0.0516(18) 0.0417(16) 0.0157(14) 0.0170(13) 0.0159(14) C12 0.061(2) 0.052(2) 0.057(2) 0.0174(16) 0.0163(17) 0.0107(17) C13 0.088(3) 0.059(2) 0.080(3) 0.036(2) 0.030(3) 0.020(2) C14 0.088(3) 0.092(3) 0.071(3) 0.051(3) 0.023(2) 0.030(3) C15 0.077(3) 0.097(3) 0.056(2) 0.038(2) 0.006(2) 0.017(3) C16 0.062(2) 0.063(2) 0.0478(19) 0.0201(17) 0.0094(16) 0.0093(18) C21 0.062(2) 0.0385(16) 0.0460(18) 0.0096(14) 0.0144(15) 0.0129(15) C22 0.082(3) 0.062(2) 0.050(2) 0.0147(18) 0.019(2) 0.011(2) C23 0.100(4) 0.074(3) 0.069(3) 0.019(2) 0.044(3) 0.012(3) C24 0.075(3) 0.065(3) 0.092(3) 0.016(2) 0.048(3) 0.015(2) C25 0.062(2) 0.082(3) 0.079(3) 0.027(2) 0.021(2) 0.026(2) C26 0.060(2) 0.071(2) 0.059(2) 0.0255(19) 0.0209(18) 0.0214(19) P1 0.0379(4) 0.0411(4) 0.0379(4) 0.0142(3) 0.0076(3) 0.0060(3) P2 0.0409(4) 0.0401(4) 0.0431(4) 0.0073(3) 0.0058(3) 0.0042(3) C1A 0.0411(16) 0.0492(17) 0.0413(16) 0.0154(13) 0.0081(13) 0.0128(13) C2A 0.058(2) 0.052(2) 0.0463(18) 0.0076(15) 0.0038(16) 0.0147(16) C3A 0.071(3) 0.082(3) 0.048(2) 0.001(2) -0.0042(19) 0.022(2) C4A 0.072(3) 0.115(4) 0.047(2) 0.030(2) 0.008(2) 0.041(3) C5A 0.072(3) 0.091(3) 0.069(3) 0.046(2) 0.013(2) 0.028(2) C6A 0.056(2) 0.062(2) 0.061(2) 0.0317(18) 0.0079(17) 0.0081(17) C1B 0.0435(16) 0.0416(16) 0.0422(16) 0.0101(13) 0.0097(13) 0.0089(13) C2B 0.0496(19) 0.063(2) 0.0477(18) 0.0174(16) 0.0146(15) 0.0137(16) C3B 0.059(2) 0.075(3) 0.061(2) 0.012(2) 0.0263(19) 0.012(2) C4B 0.048(2) 0.089(3) 0.077(3) 0.006(2) 0.019(2) 0.023(2) C5B 0.054(2) 0.113(4) 0.066(3) 0.028(3) 0.008(2) 0.032(2) C6B 0.052(2) 0.090(3) 0.056(2) 0.030(2) 0.0147(17) 0.026(2) C1C 0.0401(15) 0.0438(16) 0.0395(15) 0.0106(13) 0.0042(12) 0.0101(13) C2C 0.0528(19) 0.057(2) 0.0476(18) 0.0150(16) 0.0129(15) 0.0116(16) C3C 0.075(3) 0.072(3) 0.051(2) 0.0090(18) 0.0170(19) 0.029(2) C4C 0.071(3) 0.057(2) 0.065(3) -0.0037(19) -0.006(2) 0.017(2) C5C 0.052(2) 0.050(2) 0.087(3) 0.004(2) 0.003(2) 0.0022(17) C6C 0.0452(18) 0.051(2) 0.064(2) 0.0062(17) 0.0114(16) 0.0022(15) C1D 0.0485(18) 0.0412(16) 0.0478(18) 0.0109(14) 0.0116(14) 0.0077(14) C2D 0.056(2) 0.054(2) 0.063(2) 0.0197(17) 0.0152(17) 0.0138(17) C3D 0.068(3) 0.063(2) 0.097(3) 0.029(2) 0.031(2) 0.030(2) C4D 0.098(4) 0.053(2) 0.093(3) 0.015(2) 0.051(3) 0.024(2) C5D 0.098(4) 0.057(2) 0.059(2) -0.0032(19) 0.023(2) 0.011(2) C6D 0.067(2) 0.063(2) 0.054(2) 0.0065(18) 0.0074(18) 0.0127(19) C1E 0.0505(18) 0.0424(16) 0.0426(17) 0.0063(13) 0.0088(14) 0.0097(14) C2E 0.052(2) 0.061(2) 0.058(2) 0.0180(18) 0.0107(16) 0.0118(17) C3E 0.066(2) 0.080(3) 0.062(2) 0.018(2) 0.006(2) 0.030(2) C4E 0.099(3) 0.065(3) 0.055(2) 0.0221(19) 0.015(2) 0.034(2) C5E 0.084(3) 0.077(3) 0.076(3) 0.039(2) 0.025(2) 0.019(2) C6E 0.056(2) 0.074(3) 0.072(3) 0.032(2) 0.0175(19) 0.0135(19) C1F 0.0437(17) 0.0428(16) 0.0453(17) 0.0118(14) 0.0030(13) 0.0019(13) C2F 0.061(2) 0.052(2) 0.065(2) 0.0064(18) 0.0214(19) -0.0009(17) C3F 0.071(3) 0.080(3) 0.079(3) 0.014(2) 0.035(2) 0.004(2) C4F 0.061(2) 0.082(3) 0.074(3) 0.030(2) 0.020(2) -0.007(2) C5F 0.067(3) 0.056(2) 0.069(3) 0.019(2) 0.007(2) -0.0121(19) C6F 0.061(2) 0.0458(19) 0.056(2) 0.0099(16) 0.0086(17) -0.0005(16) C1S 0.090(6) 0.075(5) 0.130(7) 0.040(5) 0.004(5) 0.018(4) Cl1 0.169(3) 0.1048(18) 0.170(3) 0.0519(18) 0.101(2) 0.0547(18) Cl2 0.1049(19) 0.163(3) 0.192(4) 0.095(3) 0.037(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4345(8) . ? Ag1 S1 2.5017(8) . ? Ag1 S2 2.5372(9) . ? Ag2 P2 2.4249(8) . ? Ag2 S2 2.4598(9) . ? Ag2 S1 2.5640(9) 2_567 ? S1 C1 1.769(3) . ? S1 Ag2 2.5640(9) 2_567 ? S2 C2 1.769(4) . ? O1 C1 1.223(4) . ? O2 C2 1.214(4) . ? C1 C11 1.503(4) . ? C2 C21 1.503(5) . ? C11 C16 1.388(5) . ? C11 C12 1.398(5) . ? C12 C13 1.379(5) . ? C13 C14 1.384(7) . ? C14 C15 1.360(7) . ? C15 C16 1.393(5) . ? C21 C26 1.383(5) . ? C21 C22 1.389(5) . ? C22 C23 1.378(6) . ? C23 C24 1.380(7) . ? C24 C25 1.369(6) . ? C25 C26 1.381(6) . ? P1 C1C 1.824(3) . ? P1 C1A 1.828(3) . ? P1 C1B 1.835(3) . ? P2 C1F 1.827(3) . ? P2 C1D 1.828(3) . ? P2 C1E 1.831(3) . ? C1A C2A 1.388(5) . ? C1A C6A 1.390(5) . ? C2A C3A 1.385(5) . ? C3A C4A 1.368(7) . ? C4A C5A 1.374(7) . ? C5A C6A 1.388(5) . ? C1B C2B 1.385(5) . ? C1B C6B 1.390(5) . ? C2B C3B 1.389(5) . ? C3B C4B 1.374(6) . ? C4B C5B 1.381(6) . ? C5B C6B 1.385(5) . ? C1C C2C 1.388(5) . ? C1C C6C 1.395(5) . ? C2C C3C 1.390(5) . ? C3C C4C 1.377(6) . ? C4C C5C 1.365(6) . ? C5C C6C 1.379(5) . ? C1D C2D 1.384(5) . ? C1D C6D 1.392(5) . ? C2D C3D 1.393(5) . ? C3D C4D 1.371(7) . ? C4D C5D 1.373(7) . ? C5D C6D 1.381(6) . ? C1E C2E 1.384(5) . ? C1E C6E 1.388(5) . ? C2E C3E 1.387(6) . ? C3E C4E 1.382(6) . ? C4E C5E 1.371(7) . ? C5E C6E 1.381(6) . ? C1F C2F 1.378(5) . ? C1F C6F 1.386(5) . ? C2F C3F 1.391(6) . ? C3F C4F 1.375(6) . ? C4F C5F 1.367(6) . ? C5F C6F 1.389(6) . ? C1S Cl2 1.757(8) . ? C1S Cl1 1.826(9) . ? C2S Cl1A 1.772(16) . ? C2S Cl2A 1.864(16) . ? 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 P1 Ag1 S1 121.03(3) . . ? P1 Ag1 S2 123.92(3) . . ? S1 Ag1 S2 108.58(3) . . ? P2 Ag2 S2 131.17(3) . . ? P2 Ag2 S1 113.83(3) . 2_567 ? S2 Ag2 S1 114.37(3) . 2_567 ? C1 S1 Ag1 102.42(11) . . ? C1 S1 Ag2 99.36(10) . 2_567 ? Ag1 S1 Ag2 97.77(3) . 2_567 ? C2 S2 Ag2 100.80(12) . . ? C2 S2 Ag1 108.43(12) . . ? Ag2 S2 Ag1 112.97(4) . . ? O1 C1 C11 120.0(3) . . ? O1 C1 S1 123.0(3) . . ? C11 C1 S1 117.0(2) . . ? O2 C2 C21 120.1(3) . . ? O2 C2 S2 122.2(3) . . ? C21 C2 S2 117.7(3) . . ? C16 C11 C12 118.8(3) . . ? C16 C11 C1 122.6(3) . . ? C12 C11 C1 118.5(3) . . ? C13 C12 C11 120.3(4) . . ? C12 C13 C14 120.1(4) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C16 120.6(4) . . ? C11 C16 C15 120.0(4) . . ? C26 C21 C22 118.3(4) . . ? C26 C21 C2 123.8(3) . . ? C22 C21 C2 117.8(3) . . ? C23 C22 C21 120.5(4) . . ? C22 C23 C24 120.5(4) . . ? C25 C24 C23 119.5(4) . . ? C24 C25 C26 120.3(4) . . ? C25 C26 C21 120.9(4) . . ? C1C P1 C1A 105.25(15) . . ? C1C P1 C1B 101.95(14) . . ? C1A P1 C1B 105.83(15) . . ? C1C P1 Ag1 114.22(11) . . ? C1A P1 Ag1 117.68(11) . . ? C1B P1 Ag1 110.45(11) . . ? C1F P2 C1D 106.36(15) . . ? C1F P2 C1E 104.04(15) . . ? C1D P2 C1E 103.67(15) . . ? C1F P2 Ag2 115.91(11) . . ? C1D P2 Ag2 116.92(11) . . ? C1E P2 Ag2 108.53(11) . . ? C2A C1A C6A 118.2(3) . . ? C2A C1A P1 117.9(3) . . ? C6A C1A P1 123.9(3) . . ? C3A C2A C1A 120.6(4) . . ? C4A C3A C2A 120.5(4) . . ? C3A C4A C5A 119.9(4) . . ? C4A C5A C6A 120.0(4) . . ? C5A C6A C1A 120.7(4) . . ? C2B C1B C6B 118.8(3) . . ? C2B C1B P1 124.6(3) . . ? C6B C1B P1 116.7(3) . . ? C1B C2B C3B 120.4(4) . . ? C4B C3B C2B 120.5(4) . . ? C3B C4B C5B 119.3(4) . . ? C4B C5B C6B 120.6(4) . . ? C5B C6B C1B 120.3(4) . . ? C2C C1C C6C 118.6(3) . . ? C2C C1C P1 118.4(3) . . ? C6C C1C P1 123.0(3) . . ? C1C C2C C3C 120.1(4) . . ? C4C C3C C2C 120.3(4) . . ? C5C C4C C3C 120.1(4) . . ? C4C C5C C6C 120.4(4) . . ? C5C C6C C1C 120.6(4) . . ? C2D C1D C6D 118.9(3) . . ? C2D C1D P2 118.4(3) . . ? C6D C1D P2 122.7(3) . . ? C1D C2D C3D 119.7(4) . . ? C4D C3D C2D 120.6(4) . . ? C3D C4D C5D 120.1(4) . . ? C4D C5D C6D 119.8(4) . . ? C5D C6D C1D 120.8(4) . . ? C2E C1E C6E 118.6(3) . . ? C2E C1E P2 123.8(3) . . ? C6E C1E P2 117.5(3) . . ? C1E C2E C3E 120.3(4) . . ? C4E C3E C2E 120.3(4) . . ? C5E C4E C3E 119.7(4) . . ? C4E C5E C6E 120.2(4) . . ? C5E C6E C1E 120.9(4) . . ? C2F C1F C6F 119.1(3) . . ? C2F C1F P2 116.9(3) . . ? C6F C1F P2 124.0(3) . . ? C1F C2F C3F 120.3(4) . . ? C4F C3F C2F 120.0(4) . . ? C5F C4F C3F 120.3(4) . . ? C4F C5F C6F 120.0(4) . . ? C1F C6F C5F 120.4(4) . . ? Cl2 C1S Cl1 104.0(5) . . ? Cl1A C2S Cl2A 94.5(11) . . ? _diffrn_measured_fraction_theta_max 0.828 _diffrn_reflns_theta_full 29.26 _diffrn_measured_fraction_theta_full 0.828 _refine_diff_density_max 1.043 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.067 #=====END ####################################################################### #Compound 6 data_tcd15 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C107 H88 Ag8 O8 P8 S8' _chemical_formula_weight 2868.97 _chemical_melting_point ? _chemical_compound_source ? 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 12.8097(3) _cell_length_b 14.5568(1) _cell_length_c 16.0524(3) _cell_angle_alpha 63.426(1) _cell_angle_beta 68.868(1) _cell_angle_gamma 64.198(1) _cell_volume 2358.51(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3541 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'small blocks' _exptl_crystal_colour cream _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.020 _exptl_crystal_density_method ? _exptl_crystal_F_000 1418 _exptl_absorpt_coefficient_mu 2.000 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7071 _exptl_absorpt_correction_T_max 0.9280 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker AXS 3-circle CCD system' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11652 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.1094 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7764 _reflns_number_observed 4488 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 162 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0410P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7602 _refine_ls_number_parameters 540 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1381 _refine_ls_R_factor_obs 0.0679 _refine_ls_wR_factor_all 0.1668 _refine_ls_wR_factor_obs 0.1206 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.144 _refine_ls_restrained_S_all 1.175 _refine_ls_restrained_S_obs 1.144 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ag1 Ag 0.53579(5) 0.59125(5) 0.41482(4) 0.0518(2) Uani 1 d . . Ag2 Ag 0.66001(5) 0.44427(5) 0.26272(5) 0.0600(2) Uani 1 d . . S1 S 0.4789(2) 0.5982(2) 0.27249(14) 0.0490(5) Uani 1 d . . S2 S 0.6526(2) 0.3732(2) 0.45316(13) 0.0483(5) Uani 1 d . . P1 P 0.6476(2) 0.7010(2) 0.39815(14) 0.0441(5) Uani 1 d . . P2 P 0.7863(2) 0.3236(2) 0.17655(14) 0.0441(5) Uani 1 d . . O1 O 0.5835(7) 0.7115(5) 0.1122(5) 0.131(3) Uani 1 d . . O2 O 0.7714(5) 0.4153(5) 0.5271(4) 0.069(2) Uani 1 d . . C1 C 0.4975(8) 0.7142(6) 0.1763(6) 0.058(2) Uani 1 d . . C11 C 0.3987(7) 0.8188(6) 0.1742(6) 0.050(2) Uani 1 d . . C12 C 0.2997(7) 0.8295(7) 0.2475(6) 0.060(2) Uani 1 d . . H12 H 0.2913(7) 0.7684(7) 0.3004(6) 0.072 Uiso 1 calc R . C13 C 0.2141(8) 0.9290(9) 0.2430(8) 0.079(3) Uani 1 d . . H13 H 0.1499(8) 0.9349(9) 0.2937(8) 0.094 Uiso 1 calc R . C14 C 0.2221(10) 1.0181(8) 0.1660(10) 0.090(3) Uani 1 d . . H14 H 0.1633(10) 1.0851(8) 0.1633(10) 0.108 Uiso 1 calc R . C15 C 0.3172(10) 1.0099(8) 0.0916(8) 0.084(3) Uani 1 d . . H15 H 0.3221(10) 1.0717(8) 0.0385(8) 0.101 Uiso 1 calc R . C16 C 0.4056(8) 0.9122(8) 0.0938(6) 0.067(2) Uani 1 d . . H16 H 0.4694(8) 0.9079(8) 0.0425(6) 0.081 Uiso 1 calc R . C2 C 0.7768(6) 0.3630(6) 0.4835(5) 0.046(2) Uani 1 d . . C21 C 0.8939(7) 0.2866(6) 0.4523(5) 0.048(2) Uani 1 d . . C22 C 0.9960(7) 0.3116(8) 0.4327(5) 0.069(3) Uani 1 d . . H22 H 0.9899(7) 0.3732(8) 0.4410(5) 0.083 Uiso 1 calc R . C23 C 1.1047(9) 0.2458(13) 0.4016(8) 0.113(5) Uani 1 d . . H23 H 1.1720(9) 0.2640(13) 0.3869(8) 0.135 Uiso 1 calc R . C24 C 1.1147(11) 0.1533(14) 0.3920(9) 0.133(6) Uani 1 d . . H24 H 1.1891(11) 0.1074(14) 0.3730(9) 0.160 Uiso 1 calc R . C25 C 1.0134(12) 0.1278(9) 0.4108(8) 0.113(4) Uani 1 d . . H25 H 1.0199(12) 0.0656(9) 0.4034(8) 0.135 Uiso 1 calc R . C26 C 0.9040(8) 0.1949(8) 0.4403(6) 0.076(3) Uani 1 d . . H26 H 0.8364(8) 0.1784(8) 0.4522(6) 0.092 Uiso 1 calc R . C1A C 0.8075(6) 0.6511(6) 0.3586(5) 0.041(2) Uani 1 d . . C2A C 0.8890(7) 0.6489(7) 0.3970(6) 0.062(2) Uani 1 d . . H2A H 0.8624(7) 0.6734(7) 0.4479(6) 0.074 Uiso 1 calc R . C3A C 1.0099(7) 0.6109(8) 0.3618(7) 0.075(3) Uani 1 d . . H3A H 1.0635(7) 0.6119(8) 0.3878(7) 0.090 Uiso 1 calc R . C4A C 1.0494(8) 0.5723(8) 0.2894(7) 0.084(3) Uani 1 d . . H4A H 1.1304(8) 0.5455(8) 0.2664(7) 0.100 Uiso 1 calc R . C5A C 0.9706(9) 0.5727(8) 0.2496(6) 0.075(3) Uani 1 d . . H5A H 0.9982(9) 0.5479(8) 0.1988(6) 0.090 Uiso 1 calc R . C6A C 0.8505(7) 0.6096(7) 0.2849(5) 0.059(2) Uani 1 d . . H6A H 0.7977(7) 0.6068(7) 0.2593(5) 0.070 Uiso 1 calc R . C1B C 0.6029(7) 0.8391(6) 0.3149(5) 0.045(2) Uani 1 d . . C2B C 0.6806(8) 0.8927(7) 0.2463(6) 0.065(2) Uani 1 d . . H2B H 0.7617(8) 0.8565(7) 0.2411(6) 0.078 Uiso 1 calc R . C3B C 0.6410(10) 0.9977(8) 0.1858(7) 0.082(3) Uani 1 d . . H3B H 0.6953(10) 1.0316(8) 0.1411(7) 0.099 Uiso 1 calc R . C4B C 0.5234(11) 1.0521(8) 0.1910(7) 0.084(3) Uani 1 d . . H4B H 0.4971(11) 1.1229(8) 0.1495(7) 0.100 Uiso 1 calc R . C5B C 0.4426(9) 1.0024(9) 0.2580(7) 0.075(3) Uani 1 d . . H5B H 0.3617(9) 1.0397(9) 0.2620(7) 0.090 Uiso 1 calc R . C6B C 0.4824(8) 0.8972(8) 0.3188(6) 0.062(2) Uani 1 d . . H6B H 0.4274(8) 0.8642(8) 0.3636(6) 0.074 Uiso 1 calc R . C1C C 0.6238(6) 0.7208(6) 0.5097(5) 0.042(2) Uani 1 d . . C2C C 0.6012(6) 0.8211(7) 0.5138(6) 0.051(2) Uani 1 d . . H2C H 0.6019(6) 0.8811(7) 0.4580(6) 0.061 Uiso 1 calc R . C3C C 0.5773(6) 0.8323(7) 0.6014(6) 0.054(2) Uani 1 d . . H3C H 0.5622(6) 0.8995(7) 0.6041(6) 0.065 Uiso 1 calc R . C4C C 0.5763(7) 0.7448(8) 0.6825(6) 0.060(2) Uani 1 d . . H4C H 0.5601(7) 0.7525(8) 0.7408(6) 0.072 Uiso 1 calc R . C5C C 0.5988(7) 0.6454(8) 0.6795(6) 0.064(2) Uani 1 d . . H5C H 0.5977(7) 0.5857(8) 0.7355(6) 0.077 Uiso 1 calc R . C6C C 0.6235(7) 0.6338(7) 0.5916(6) 0.055(2) Uani 1 d . . H6C H 0.6399(7) 0.5660(7) 0.5893(6) 0.066 Uiso 1 calc R . C1D C 0.7259(7) 0.3498(7) 0.0789(5) 0.048(2) Uani 1 d . . C2D C 0.7069(9) 0.4502(8) 0.0104(7) 0.088(3) Uani 1 d . . H2D H 0.7270(9) 0.5018(8) 0.0149(7) 0.106 Uiso 1 calc R . C3D C 0.6582(11) 0.4787(9) -0.0665(8) 0.109(4) Uani 1 d . . H3D H 0.6501(11) 0.5467(9) -0.1140(8) 0.130 Uiso 1 calc R . C4D C 0.6233(10) 0.4062(10) -0.0706(7) 0.097(3) Uani 1 d . . H4D H 0.5873(10) 0.4253(10) -0.1197(7) 0.116 Uiso 1 calc R . C5D C 0.6404(11) 0.3061(10) -0.0039(8) 0.103(4) Uani 1 d . . H5D H 0.6194(11) 0.2556(10) -0.0091(8) 0.123 Uiso 1 calc R . C6D C 0.6892(9) 0.2769(8) 0.0730(7) 0.083(3) Uani 1 d . . H6D H 0.6969(9) 0.2086(8) 0.1202(7) 0.100 Uiso 1 calc R . C1E C 0.8039(6) 0.1825(6) 0.2469(5) 0.043(2) Uani 1 d . . C2E C 0.7299(7) 0.1552(7) 0.3370(5) 0.051(2) Uani 1 d . . H2E H 0.6709(7) 0.2099(7) 0.3590(5) 0.061 Uiso 1 calc R . C3E C 0.7442(8) 0.0486(7) 0.3926(6) 0.064(2) Uani 1 d . . H3E H 0.6952(8) 0.0319(7) 0.4525(6) 0.077 Uiso 1 calc R . C4E C 0.8286(8) -0.0337(7) 0.3623(6) 0.064(2) Uani 1 d . . H4E H 0.8370(8) -0.1057(7) 0.4014(6) 0.076 Uiso 1 calc R . C5E C 0.9010(8) -0.0103(7) 0.2742(7) 0.069(3) Uani 1 d . . H5E H 0.9574(8) -0.0662(7) 0.2525(7) 0.083 Uiso 1 calc R . C6E C 0.8898(7) 0.0967(7) 0.2177(6) 0.058(2) Uani 1 d . . H6E H 0.9408(7) 0.1119(7) 0.1587(6) 0.069 Uiso 1 calc R . C1F C 0.9382(6) 0.3269(6) 0.1223(5) 0.047(2) Uani 1 d . . C2F C 0.9997(8) 0.3151(7) 0.0339(5) 0.063(2) Uani 1 d . . H2F H 0.9625(8) 0.3080(7) -0.0020(5) 0.075 Uiso 1 calc R . C3F C 1.1144(8) 0.3140(7) 0.0004(6) 0.072(3) Uani 1 d . . H3F H 1.1541(8) 0.3065(7) -0.0587(6) 0.086 Uiso 1 calc R . C4F C 1.1718(8) 0.3236(7) 0.0506(7) 0.071(3) Uani 1 d . . H4F H 1.2502(8) 0.3219(7) 0.0271(7) 0.085 Uiso 1 calc R . C5F C 1.1118(9) 0.3358(8) 0.1371(7) 0.080(3) Uani 1 d . . H5F H 1.1504(9) 0.3425(8) 0.1722(7) 0.096 Uiso 1 calc R . C6F C 0.9949(7) 0.3383(7) 0.1733(6) 0.064(2) Uani 1 d . . H6F H 0.9553(7) 0.3477(7) 0.2317(6) 0.077 Uiso 1 calc R . C1S C 1.0511(18) 0.8073(17) 0.1170(15) 0.093(6) Uiso 0.50 d PD . H1S1 H 0.9935(18) 0.7752(17) 0.1285(15) 0.140 Uiso 0.50 calc PR . H1S2 H 1.0527(18) 0.8088(17) 0.1757(15) 0.140 Uiso 0.50 calc PR . H1S3 H 1.1279(18) 0.7652(17) 0.0915(15) 0.140 Uiso 0.50 calc PR . C2S C 1.0264(13) 0.8934(13) 0.0643(10) 0.138(5) Uiso 1 d D . C3S C 0.9254(12) 0.9453(11) 0.0245(9) 0.120(4) Uiso 1 d D . H3S H 0.8718(12) 0.9096(11) 0.0412(9) 0.144 Uiso 1 calc R . C4S C 1.0916(11) 0.9591(11) 0.0344(9) 0.115(4) Uiso 1 d D . H4S H 1.1578(11) 0.9296(11) 0.0609(9) 0.138 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 Ag1 0.0511(4) 0.0623(5) 0.0525(4) -0.0248(3) -0.0030(3) -0.0287(3) Ag2 0.0533(4) 0.0558(5) 0.0707(5) -0.0378(4) 0.0046(3) -0.0151(4) S1 0.0556(13) 0.0447(12) 0.0441(12) -0.0196(10) -0.0118(10) -0.0086(11) S2 0.0386(11) 0.0627(14) 0.0429(12) -0.0284(11) -0.0023(9) -0.0105(11) P1 0.0449(12) 0.0521(13) 0.0429(12) -0.0210(11) -0.0001(10) -0.0249(11) P2 0.0473(12) 0.0427(12) 0.0397(12) -0.0182(10) -0.0038(10) -0.0124(10) O1 0.103(6) 0.073(5) 0.105(6) -0.021(4) 0.058(5) -0.006(4) O2 0.063(4) 0.081(4) 0.082(4) -0.053(4) -0.008(3) -0.019(3) C1 0.063(6) 0.045(5) 0.059(6) -0.024(5) -0.004(5) -0.013(5) C11 0.053(5) 0.047(5) 0.046(5) -0.016(4) -0.014(4) -0.010(4) C12 0.055(6) 0.050(6) 0.065(6) -0.021(5) -0.013(5) -0.006(5) C13 0.048(6) 0.073(7) 0.103(8) -0.049(7) -0.007(5) 0.001(6) C14 0.070(8) 0.039(6) 0.148(11) -0.031(7) -0.047(8) 0.010(6) C15 0.086(8) 0.051(7) 0.103(9) -0.008(6) -0.036(7) -0.019(6) C16 0.069(6) 0.060(6) 0.063(6) -0.010(5) -0.016(5) -0.021(6) C2 0.046(5) 0.052(5) 0.034(4) -0.017(4) 0.000(4) -0.016(4) C21 0.049(5) 0.050(5) 0.039(5) -0.020(4) -0.010(4) -0.007(4) C22 0.045(5) 0.106(8) 0.052(5) -0.027(5) -0.009(4) -0.023(6) C23 0.032(6) 0.193(15) 0.091(9) -0.064(10) 0.000(6) -0.014(8) C24 0.059(8) 0.184(16) 0.093(9) -0.076(10) -0.023(7) 0.050(10) C25 0.111(10) 0.087(8) 0.109(10) -0.062(8) -0.039(8) 0.036(8) C26 0.075(7) 0.075(7) 0.081(7) -0.048(6) -0.018(5) -0.004(6) C1A 0.040(4) 0.047(5) 0.038(4) -0.020(4) 0.007(4) -0.022(4) C2A 0.050(5) 0.084(7) 0.054(5) -0.034(5) -0.005(4) -0.020(5) C3A 0.038(5) 0.110(8) 0.081(7) -0.048(6) -0.002(5) -0.020(5) C4A 0.051(6) 0.103(8) 0.075(7) -0.034(7) 0.013(5) -0.024(6) C5A 0.079(7) 0.089(8) 0.053(6) -0.039(6) 0.010(5) -0.027(6) C6A 0.062(6) 0.064(6) 0.050(5) -0.030(5) 0.004(4) -0.023(5) C1B 0.049(5) 0.050(5) 0.047(5) -0.023(4) -0.005(4) -0.022(4) C2B 0.058(6) 0.055(6) 0.069(6) -0.018(5) 0.002(5) -0.023(5) C3B 0.099(9) 0.042(6) 0.068(7) 0.000(5) 0.010(6) -0.032(6) C4B 0.113(9) 0.057(7) 0.070(7) -0.022(6) -0.027(7) -0.013(7) C5B 0.071(7) 0.075(8) 0.080(7) -0.042(7) -0.030(6) 0.003(6) C6B 0.057(6) 0.069(7) 0.057(6) -0.019(5) -0.020(5) -0.016(5) C1C 0.045(5) 0.052(5) 0.035(4) -0.014(4) 0.000(4) -0.028(4) C2C 0.050(5) 0.061(6) 0.053(5) -0.023(4) 0.000(4) -0.031(4) C3C 0.048(5) 0.060(6) 0.066(6) -0.037(5) 0.002(4) -0.022(5) C4C 0.066(6) 0.081(7) 0.053(6) -0.037(6) 0.001(4) -0.037(5) C5C 0.086(7) 0.071(7) 0.043(5) -0.017(5) -0.009(5) -0.038(6) C6C 0.063(6) 0.061(6) 0.053(5) -0.030(5) -0.007(4) -0.025(5) C1D 0.051(5) 0.048(5) 0.040(5) -0.018(4) -0.001(4) -0.017(4) C2D 0.142(10) 0.062(7) 0.077(7) 0.005(6) -0.063(7) -0.045(7) C3D 0.179(12) 0.063(7) 0.103(9) 0.017(6) -0.088(9) -0.057(8) C4D 0.139(10) 0.085(8) 0.080(8) -0.002(7) -0.061(7) -0.044(8) C5D 0.156(11) 0.091(9) 0.101(9) -0.022(8) -0.067(8) -0.054(8) C6D 0.125(9) 0.059(6) 0.082(7) -0.009(6) -0.047(7) -0.040(6) C1E 0.041(4) 0.045(5) 0.043(5) -0.021(4) -0.002(4) -0.014(4) C2E 0.056(5) 0.050(5) 0.042(5) -0.016(4) 0.000(4) -0.021(4) C3E 0.071(6) 0.064(7) 0.055(6) -0.014(5) -0.006(5) -0.033(6) C4E 0.080(7) 0.039(5) 0.063(6) -0.009(5) -0.024(5) -0.014(5) C5E 0.065(6) 0.044(6) 0.087(7) -0.029(5) -0.002(5) -0.013(5) C6E 0.052(5) 0.056(6) 0.059(6) -0.026(5) 0.001(4) -0.016(5) C1F 0.044(5) 0.046(5) 0.039(5) -0.016(4) 0.003(4) -0.014(4) C2F 0.066(6) 0.079(7) 0.045(5) -0.034(5) 0.002(5) -0.023(5) C3F 0.055(6) 0.077(7) 0.059(6) -0.026(5) 0.016(5) -0.021(5) C4F 0.047(5) 0.071(7) 0.094(8) -0.036(6) -0.003(5) -0.019(5) C5F 0.079(7) 0.104(8) 0.088(8) -0.049(7) -0.009(6) -0.046(7) C6F 0.059(6) 0.083(7) 0.066(6) -0.039(5) 0.004(5) -0.035(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.452(2) . ? Ag1 S1 2.587(2) . ? Ag1 S2 2.606(2) 2_666 ? Ag1 S2 2.735(2) . ? Ag1 Ag1 3.0315(12) 2_666 ? Ag2 P2 2.388(2) . ? Ag2 S1 2.440(2) . ? Ag2 S2 2.733(2) . ? S1 C1 1.745(8) . ? S2 C2 1.755(8) . ? S2 Ag1 2.606(2) 2_666 ? P1 C1B 1.817(8) . ? P1 C1A 1.818(7) . ? P1 C1C 1.836(7) . ? P2 C1E 1.802(8) . ? P2 C1D 1.811(8) . ? P2 C1F 1.836(7) . ? O1 C1 1.207(9) . ? O2 C2 1.213(8) . ? C1 C11 1.493(11) . ? C11 C12 1.390(10) . ? C11 C16 1.406(11) . ? C12 C13 1.374(11) . ? C13 C14 1.346(13) . ? C14 C15 1.370(13) . ? C15 C16 1.374(12) . ? C2 C21 1.498(10) . ? C21 C26 1.376(11) . ? C21 C22 1.399(10) . ? C22 C23 1.368(13) . ? C23 C24 1.37(2) . ? C24 C25 1.40(2) . ? C25 C26 1.373(13) . ? C1A C2A 1.374(10) . ? C1A C6A 1.396(9) . ? C2A C3A 1.389(10) . ? C3A C4A 1.355(12) . ? C4A C5A 1.373(12) . ? C5A C6A 1.378(11) . ? C1B C2B 1.389(10) . ? C1B C6B 1.394(10) . ? C2B C3B 1.374(12) . ? C3B C4B 1.355(13) . ? C4B C5B 1.380(12) . ? C5B C6B 1.378(12) . ? C1C C6C 1.358(10) . ? C1C C2C 1.387(10) . ? C2C C3C 1.396(10) . ? C3C C4C 1.355(11) . ? C4C C5C 1.367(11) . ? C5C C6C 1.402(10) . ? C1D C2D 1.360(11) . ? C1D C6D 1.383(11) . ? C2D C3D 1.398(12) . ? C3D C4D 1.347(12) . ? C4D C5D 1.347(13) . ? C5D C6D 1.397(12) . ? C1E C6E 1.396(10) . ? C1E C2E 1.405(9) . ? C2E C3E 1.367(11) . ? C3E C4E 1.362(11) . ? C4E C5E 1.370(11) . ? C5E C6E 1.379(11) . ? C1F C6F 1.372(10) . ? C1F C2F 1.399(9) . ? C2F C3F 1.366(11) . ? C3F C4F 1.351(12) . ? C4F C5F 1.371(11) . ? C5F C6F 1.388(11) . ? C1S C2S 1.13(2) . ? C2S C4S 1.356(13) . ? C2S C3S 1.403(14) . ? C3S C4S 1.259(14) 2_775 ? C4S C3S 1.259(14) 2_775 ? 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 P1 Ag1 S1 123.19(7) . . ? P1 Ag1 S2 106.10(6) . 2_666 ? S1 Ag1 S2 109.97(6) . 2_666 ? P1 Ag1 S2 116.96(7) . . ? S1 Ag1 S2 88.91(6) . . ? S2 Ag1 S2 110.88(5) 2_666 . ? P1 Ag1 Ag1 130.34(6) . 2_666 ? S1 Ag1 Ag1 106.05(5) . 2_666 ? S2 Ag1 Ag1 57.44(5) 2_666 2_666 ? S2 Ag1 Ag1 53.44(4) . 2_666 ? P2 Ag2 S1 145.71(7) . . ? P2 Ag2 S2 118.87(7) . . ? S1 Ag2 S2 92.05(6) . . ? C1 S1 Ag2 109.1(3) . . ? C1 S1 Ag1 108.2(3) . . ? Ag2 S1 Ag1 86.97(7) . . ? C2 S2 Ag1 110.6(2) . 2_666 ? C2 S2 Ag2 115.8(2) . . ? Ag1 S2 Ag2 126.45(8) 2_666 . ? C2 S2 Ag1 98.8(3) . . ? Ag1 S2 Ag1 69.12(5) 2_666 . ? Ag2 S2 Ag1 78.54(6) . . ? C1B P1 C1A 104.1(3) . . ? C1B P1 C1C 103.2(3) . . ? C1A P1 C1C 105.5(3) . . ? C1B P1 Ag1 113.5(2) . . ? C1A P1 Ag1 117.0(2) . . ? C1C P1 Ag1 112.3(2) . . ? C1E P2 C1D 104.4(3) . . ? C1E P2 C1F 104.6(3) . . ? C1D P2 C1F 104.9(3) . . ? C1E P2 Ag2 113.6(2) . . ? C1D P2 Ag2 111.3(3) . . ? C1F P2 Ag2 117.0(2) . . ? O1 C1 C11 120.4(8) . . ? O1 C1 S1 122.8(7) . . ? C11 C1 S1 116.8(6) . . ? C12 C11 C16 117.8(8) . . ? C12 C11 C1 123.8(8) . . ? C16 C11 C1 118.4(7) . . ? C13 C12 C11 121.0(9) . . ? C14 C13 C12 120.7(9) . . ? C13 C14 C15 119.7(9) . . ? C14 C15 C16 121.4(10) . . ? C15 C16 C11 119.3(9) . . ? O2 C2 C21 119.7(7) . . ? O2 C2 S2 123.0(6) . . ? C21 C2 S2 117.3(6) . . ? C26 C21 C22 119.4(8) . . ? C26 C21 C2 122.6(8) . . ? C22 C21 C2 118.0(7) . . ? C23 C22 C21 120.2(10) . . ? C22 C23 C24 120.2(11) . . ? C23 C24 C25 120.0(11) . . ? C26 C25 C24 119.7(12) . . ? C25 C26 C21 120.4(10) . . ? C2A C1A C6A 117.7(7) . . ? C2A C1A P1 125.1(6) . . ? C6A C1A P1 117.3(6) . . ? C1A C2A C3A 121.7(8) . . ? C4A C3A C2A 119.5(8) . . ? C3A C4A C5A 120.4(8) . . ? C4A C5A C6A 120.2(8) . . ? C5A C6A C1A 120.5(8) . . ? C2B C1B C6B 116.5(8) . . ? C2B C1B P1 124.7(6) . . ? C6B C1B P1 118.8(6) . . ? C3B C2B C1B 121.9(9) . . ? C4B C3B C2B 120.4(9) . . ? C3B C4B C5B 119.9(10) . . ? C6B C5B C4B 119.6(9) . . ? C5B C6B C1B 121.7(8) . . ? C6C C1C C2C 119.2(7) . . ? C6C C1C P1 117.9(6) . . ? C2C C1C P1 122.8(6) . . ? C1C C2C C3C 120.2(8) . . ? C4C C3C C2C 119.8(8) . . ? C3C C4C C5C 120.7(8) . . ? C4C C5C C6C 119.6(8) . . ? C1C C6C C5C 120.5(8) . . ? C2D C1D C6D 117.3(8) . . ? C2D C1D P2 118.3(6) . . ? C6D C1D P2 124.1(7) . . ? C1D C2D C3D 122.4(9) . . ? C4D C3D C2D 119.0(9) . . ? C5D C4D C3D 120.1(10) . . ? C4D C5D C6D 121.2(10) . . ? C1D C6D C5D 119.8(9) . . ? C6E C1E C2E 117.0(7) . . ? C6E C1E P2 123.5(6) . . ? C2E C1E P2 119.5(6) . . ? C3E C2E C1E 120.4(8) . . ? C4E C3E C2E 121.5(8) . . ? C3E C4E C5E 119.9(8) . . ? C4E C5E C6E 119.6(8) . . ? C5E C6E C1E 121.7(7) . . ? C6F C1F C2F 118.7(7) . . ? C6F C1F P2 117.5(6) . . ? C2F C1F P2 123.7(6) . . ? C3F C2F C1F 120.0(8) . . ? C4F C3F C2F 121.8(8) . . ? C3F C4F C5F 118.5(8) . . ? C4F C5F C6F 121.6(8) . . ? C1F C6F C5F 119.4(8) . . ? C1S C2S C4S 122.9(20) . . ? C1S C2S C3S 124.9(20) . . ? C4S C2S C3S 112.2(14) . . ? C4S C3S C2S 118.9(13) 2_775 . ? C3S C4S C2S 128.8(14) 2_775 . ? _refine_diff_density_max 0.614 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.104 #=====END ###################################################