# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H100 Ag12 Br2 O20 P10 S20' _chemical_formula_weight 3306.36 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' Br Br -0.2901 2.4595 '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 12.685(3) _cell_length_b 13.348(3) _cell_length_c 16.747(5) _cell_angle_alpha 100.130(4) _cell_angle_beta 103.059(5) _cell_angle_gamma 110.356(3) _cell_volume 2487.1(10) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9355 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.91 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1604 _exptl_absorpt_coefficient_mu 3.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3807 _exptl_absorpt_correction_T_max 0.4548 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20056 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.11 _reflns_number_total 9594 _reflns_number_gt 6715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints on bond lengths and atomic displacement paremeters were applied by using DFIX and DELU command in SHELX program. Those restraints are: DFIX 1.43 0.01 O9 C17 O10 C19 DELU C7 C8 DELU C17 C18 DELU C19 C20 DELU O9 C17 ; _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^)+(0.0475P)^2^+21.3857P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9594 _refine_ls_number_parameters 466 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0859 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.48964(6) 0.79654(6) 0.15564(5) 0.0549(2) Uani 1 1 d . . . Ag2 Ag 0.71133(9) 0.77847(8) 0.28390(7) 0.0786(3) Uani 1 1 d . . . Ag3 Ag 0.54759(7) 0.56748(7) 0.32603(5) 0.0596(2) Uani 1 1 d . . . Ag4 Ag 0.66781(7) 0.46361(7) 0.20747(5) 0.0575(2) Uani 1 1 d . . . Ag5 Ag 0.36036(7) 0.54609(6) 0.15401(5) 0.0544(2) Uani 1 1 d . . . Ag6 Ag 0.55744(8) 0.68312(9) -0.00915(6) 0.0751(3) Uani 1 1 d . . . Br1 Br 0.58178(8) 0.60203(7) 0.12724(6) 0.0443(2) Uani 1 1 d . . . C1 C 0.9127(14) 1.0332(12) 0.0840(10) 0.099(5) Uani 1 1 d . . . H1A H 0.8474 0.9773 0.0364 0.119 Uiso 1 1 calc R . . H1B H 0.9651 0.9996 0.1065 0.119 Uiso 1 1 calc R . . C2 C 0.9768(15) 1.1270(12) 0.0552(11) 0.115(6) Uani 1 1 d . . . H2A H 0.9235 1.1576 0.0304 0.172 Uiso 1 1 calc R . . H2B H 1.0094 1.1017 0.0133 0.172 Uiso 1 1 calc R . . H2C H 1.0396 1.1831 0.1030 0.172 Uiso 1 1 calc R . . C3 C 0.7042(11) 1.1356(10) 0.2420(7) 0.067(3) Uani 1 1 d . . . H3A H 0.6226 1.0977 0.2399 0.081 Uiso 1 1 calc R . . H3B H 0.7047 1.1517 0.1878 0.081 Uiso 1 1 calc R . . C4 C 0.7623(16) 1.2385(13) 0.3112(8) 0.109(6) Uani 1 1 d . . . H4A H 0.7496 1.2233 0.3630 0.163 Uiso 1 1 calc R . . H4B H 0.7299 1.2908 0.2974 0.163 Uiso 1 1 calc R . . H4C H 0.8456 1.2692 0.3187 0.163 Uiso 1 1 calc R . . C5 C 0.2055(14) 0.7693(16) 0.3068(11) 0.109(4) Uani 1 1 d . . . H5A H 0.2061 0.7499 0.3601 0.131 Uiso 1 1 calc R . . H5B H 0.1551 0.7030 0.2601 0.131 Uiso 1 1 calc R . . C6 C 0.1604(12) 0.8556(12) 0.3029(10) 0.093(4) Uani 1 1 d . . . H6A H 0.2083 0.9195 0.3510 0.140 Uiso 1 1 calc R . . H6B H 0.0802 0.8279 0.3040 0.140 Uiso 1 1 calc R . . H6C H 0.1630 0.8764 0.2511 0.140 Uiso 1 1 calc R . . C7 C 0.5238(15) 0.8195(16) 0.5060(10) 0.109(4) Uani 1 1 d U . . H7A H 0.5995 0.8639 0.5008 0.131 Uiso 1 1 calc R . . H7B H 0.5200 0.7450 0.5031 0.131 Uiso 1 1 calc R . . C8 C 0.5152(17) 0.8689(13) 0.5903(9) 0.119(6) Uani 1 1 d U . . H8A H 0.5159 0.9415 0.5926 0.178 Uiso 1 1 calc R . . H8B H 0.5813 0.8748 0.6352 0.178 Uiso 1 1 calc R . . H8C H 0.4430 0.8220 0.5974 0.178 Uiso 1 1 calc R . . C9 C 0.2588(12) 0.2801(13) 0.3295(8) 0.091(4) Uani 1 1 d . . . H9A H 0.3221 0.2565 0.3486 0.109 Uiso 1 1 calc R . . H9B H 0.2733 0.3473 0.3716 0.109 Uiso 1 1 calc R . . C10 C 0.1541(17) 0.199(2) 0.3231(12) 0.187(13) Uani 1 1 d . . . H10A H 0.0922 0.2248 0.3083 0.281 Uiso 1 1 calc R . . H10B H 0.1580 0.1824 0.3768 0.281 Uiso 1 1 calc R . . H10C H 0.1380 0.1338 0.2797 0.281 Uiso 1 1 calc R . . C11 C 0.3814(13) 0.1126(10) 0.1426(9) 0.081(4) Uani 1 1 d . . . H11A H 0.4645 0.1503 0.1758 0.097 Uiso 1 1 calc R . . H11B H 0.3737 0.1197 0.0852 0.097 Uiso 1 1 calc R . . C12 C 0.3389(14) -0.0069(11) 0.1400(11) 0.107(5) Uani 1 1 d . . . H12A H 0.3518 -0.0138 0.1971 0.161 Uiso 1 1 calc R . . H12B H 0.3814 -0.0406 0.1120 0.161 Uiso 1 1 calc R . . H12C H 0.2559 -0.0437 0.1091 0.161 Uiso 1 1 calc R . . C13 C 0.9248(9) 0.3663(11) 0.1589(6) 0.065(3) Uani 1 1 d . . . H13A H 0.9056 0.2942 0.1701 0.078 Uiso 1 1 calc R . . H13B H 0.8899 0.4067 0.1907 0.078 Uiso 1 1 calc R . . C14 C 1.0529(10) 0.4278(11) 0.1870(7) 0.079(4) Uani 1 1 d . . . H14A H 1.0874 0.3866 0.1567 0.119 Uiso 1 1 calc R . . H14B H 1.0838 0.4382 0.2471 0.119 Uiso 1 1 calc R . . H14C H 1.0717 0.4989 0.1757 0.119 Uiso 1 1 calc R . . C15 C 0.9030(9) 0.5831(9) 0.0471(7) 0.063(3) Uani 1 1 d . . . H15A H 0.9719 0.5658 0.0619 0.075 Uiso 1 1 calc R . . H15B H 0.8816 0.5784 -0.0133 0.075 Uiso 1 1 calc R . . C16 C 0.9287(12) 0.6952(9) 0.0981(7) 0.078(4) Uani 1 1 d . . . H16A H 0.8598 0.7112 0.0830 0.117 Uiso 1 1 calc R . . H16B H 0.9931 0.7488 0.0870 0.117 Uiso 1 1 calc R . . H16C H 0.9500 0.6988 0.1576 0.117 Uiso 1 1 calc R . . C17 C 1.0316(15) 0.8564(11) 0.5181(11) 0.124(4) Uani 1 1 d DU . . H17A H 0.9760 0.8904 0.5045 0.148 Uiso 1 1 calc R . . H17B H 1.0307 0.8403 0.5722 0.148 Uiso 1 1 calc R . . C18 C 1.1440(13) 0.9331(13) 0.5279(9) 0.110(5) Uani 1 1 d U . . H18A H 1.1913 0.8945 0.5133 0.164 Uiso 1 1 calc R . . H18B H 1.1802 0.9779 0.5862 0.164 Uiso 1 1 calc R . . H18C H 1.1383 0.9799 0.4911 0.164 Uiso 1 1 calc R . . C19 C 0.7922(14) 0.4916(12) 0.4773(13) 0.124(4) Uani 1 1 d DU . . H19A H 0.7660 0.4422 0.4202 0.148 Uiso 1 1 calc R . . H19B H 0.7241 0.5022 0.4877 0.148 Uiso 1 1 calc R . . C20 C 0.8336(16) 0.4385(15) 0.5375(10) 0.111(5) Uani 1 1 d U . . H20A H 0.8992 0.4249 0.5265 0.167 Uiso 1 1 calc R . . H20B H 0.7709 0.3691 0.5318 0.167 Uiso 1 1 calc R . . H20C H 0.8584 0.4859 0.5944 0.167 Uiso 1 1 calc R . . O1 O 0.8683(6) 1.0732(6) 0.1495(5) 0.0621(18) Uani 1 1 d . . . O2 O 0.7680(5) 1.0655(5) 0.2576(4) 0.0489(15) Uani 1 1 d . . . O3 O 0.3194(7) 0.8094(8) 0.3013(7) 0.092(3) Uani 1 1 d . . . O4 O 0.4353(9) 0.8148(9) 0.4402(6) 0.106(3) Uani 1 1 d . . . O5 O 0.2593(6) 0.3041(6) 0.2473(5) 0.0629(19) Uani 1 1 d . . . O6 O 0.3167(6) 0.1629(5) 0.1790(5) 0.0619(18) Uani 1 1 d . . . O7 O 0.8765(5) 0.3514(6) 0.0686(4) 0.0503(15) Uani 1 1 d . . . O8 O 0.8036(5) 0.5044(5) 0.0664(4) 0.0506(15) Uani 1 1 d . . . O9 O 0.9919(7) 0.7556(8) 0.4552(7) 0.117(4) Uani 1 1 d DU . . O10 O 0.8764(11) 0.5949(9) 0.4801(7) 0.124(4) Uani 1 1 d D . . P1 P 0.7819(2) 0.98569(19) 0.18368(16) 0.0464(5) Uani 1 1 d . . . P2 P 0.4232(2) 0.7728(2) 0.34632(18) 0.0585(7) Uani 1 1 d . . . P3 P 0.3507(2) 0.29190(19) 0.20107(15) 0.0438(5) Uani 1 1 d . . . P4 P 0.76396(18) 0.37566(19) 0.03265(14) 0.0401(5) Uani 1 1 d . . . P5 P 0.8671(2) 0.6575(2) 0.41264(17) 0.0547(6) Uani 1 1 d . . . S1 S 0.8644(2) 0.9011(2) 0.2353(2) 0.0659(7) Uani 1 1 d . . . S2 S 0.6277(2) 0.9055(2) 0.08876(16) 0.0538(6) Uani 1 1 d . . . S3 S 0.5593(2) 0.8677(2) 0.31706(16) 0.0528(6) Uani 1 1 d . . . S4 S 0.3658(2) 0.6062(2) 0.31081(16) 0.0516(6) Uani 1 1 d . . . S5 S 0.5167(2) 0.3687(2) 0.28175(16) 0.0489(5) Uani 1 1 d . . . S6 S 0.30759(18) 0.33790(18) 0.09588(14) 0.0435(5) Uani 1 1 d . . . S7 S 0.63690(18) 0.30444(19) 0.08156(14) 0.0442(5) Uani 1 1 d . . . S8 S 0.26988(18) 0.67336(19) 0.09317(14) 0.0427(5) Uani 1 1 d . . . S9 S 0.7408(2) 0.7153(2) 0.41820(16) 0.0567(6) Uani 1 1 d . . . S10 S 0.8714(2) 0.5881(3) 0.3016(2) 0.0769(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0498(4) 0.0491(4) 0.0598(5) 0.0150(3) 0.0188(3) 0.0121(3) Ag2 0.0757(6) 0.0722(6) 0.0871(7) 0.0401(5) 0.0167(5) 0.0256(5) Ag3 0.0512(4) 0.0542(5) 0.0663(5) 0.0126(4) 0.0134(4) 0.0179(3) Ag4 0.0548(4) 0.0604(5) 0.0575(5) 0.0137(4) 0.0208(3) 0.0230(4) Ag5 0.0606(4) 0.0477(4) 0.0578(4) 0.0175(3) 0.0175(3) 0.0243(3) Ag6 0.0761(6) 0.1177(8) 0.0727(6) 0.0538(6) 0.0424(5) 0.0616(6) Br1 0.0461(5) 0.0396(5) 0.0517(5) 0.0179(4) 0.0193(4) 0.0175(4) C1 0.113(11) 0.094(10) 0.103(11) 0.018(8) 0.072(9) 0.038(9) C2 0.131(13) 0.084(10) 0.146(14) 0.031(9) 0.110(12) 0.021(9) C3 0.083(8) 0.073(8) 0.074(7) 0.029(6) 0.036(6) 0.054(7) C4 0.191(17) 0.102(11) 0.069(8) 0.022(8) 0.039(10) 0.102(12) C5 0.100(8) 0.149(11) 0.102(7) 0.042(7) 0.034(7) 0.071(8) C6 0.085(9) 0.094(10) 0.115(11) 0.030(9) 0.041(8) 0.047(8) C7 0.100(8) 0.149(11) 0.102(7) 0.042(7) 0.034(7) 0.071(8) C8 0.191(18) 0.094(11) 0.066(8) 0.012(8) 0.035(10) 0.060(12) C9 0.083(9) 0.124(12) 0.075(8) 0.027(8) 0.048(7) 0.038(8) C10 0.132(16) 0.25(3) 0.099(13) 0.083(16) 0.043(12) -0.036(17) C11 0.106(10) 0.066(8) 0.095(9) 0.028(7) 0.054(8) 0.046(7) C12 0.120(12) 0.051(8) 0.146(14) 0.022(8) 0.032(10) 0.037(8) C13 0.057(6) 0.098(9) 0.052(6) 0.025(6) 0.016(5) 0.044(6) C14 0.059(7) 0.096(9) 0.057(7) 0.010(6) -0.001(5) 0.019(6) C15 0.058(6) 0.061(6) 0.058(6) 0.012(5) 0.030(5) 0.006(5) C16 0.096(9) 0.049(6) 0.063(7) 0.007(5) 0.027(6) 0.001(6) C17 0.107(8) 0.077(7) 0.150(11) 0.020(6) 0.012(8) 0.017(6) C18 0.105(10) 0.091(11) 0.074(9) -0.005(8) 0.009(8) -0.003(8) C19 0.107(8) 0.077(7) 0.150(11) 0.020(6) 0.012(8) 0.017(6) C20 0.141(14) 0.125(14) 0.111(12) 0.064(10) 0.065(11) 0.073(11) O1 0.059(4) 0.052(4) 0.074(5) 0.021(3) 0.035(4) 0.012(3) O2 0.054(4) 0.045(4) 0.051(4) 0.013(3) 0.016(3) 0.025(3) O3 0.065(5) 0.081(6) 0.133(8) 0.025(6) 0.036(5) 0.032(5) O4 0.095(7) 0.116(8) 0.062(5) -0.019(5) 0.033(5) 0.007(6) O5 0.048(4) 0.080(5) 0.075(5) 0.036(4) 0.034(3) 0.026(4) O6 0.065(4) 0.041(4) 0.084(5) 0.030(4) 0.031(4) 0.017(3) O7 0.043(3) 0.068(4) 0.047(3) 0.016(3) 0.017(3) 0.030(3) O8 0.048(3) 0.036(3) 0.064(4) 0.010(3) 0.026(3) 0.010(3) O9 0.059(5) 0.092(7) 0.142(9) -0.036(6) -0.028(5) 0.035(5) O10 0.175(11) 0.112(9) 0.115(8) 0.061(7) 0.036(8) 0.085(9) P1 0.0430(12) 0.0366(12) 0.0602(14) 0.0134(10) 0.0216(11) 0.0132(10) P2 0.0481(14) 0.0561(16) 0.0586(15) -0.0039(12) 0.0213(12) 0.0130(12) P3 0.0413(12) 0.0391(12) 0.0548(13) 0.0200(10) 0.0216(10) 0.0130(9) P4 0.0335(10) 0.0436(12) 0.0430(12) 0.0109(10) 0.0141(9) 0.0147(9) P5 0.0543(14) 0.0497(15) 0.0538(15) 0.0116(12) 0.0048(11) 0.0227(12) S1 0.0527(14) 0.0531(15) 0.100(2) 0.0258(15) 0.0246(14) 0.0281(12) S2 0.0546(14) 0.0476(13) 0.0517(13) 0.0134(11) 0.0186(11) 0.0109(11) S3 0.0570(14) 0.0426(13) 0.0548(14) 0.0056(10) 0.0203(11) 0.0174(11) S4 0.0456(12) 0.0552(14) 0.0531(13) 0.0150(11) 0.0208(10) 0.0159(10) S5 0.0428(12) 0.0520(13) 0.0565(13) 0.0274(11) 0.0167(10) 0.0178(10) S6 0.0394(11) 0.0413(12) 0.0516(12) 0.0156(10) 0.0180(9) 0.0148(9) S7 0.0367(11) 0.0479(13) 0.0477(12) 0.0172(10) 0.0165(9) 0.0127(9) S8 0.0403(11) 0.0449(12) 0.0440(12) 0.0110(9) 0.0158(9) 0.0173(9) S9 0.0518(13) 0.0544(15) 0.0537(14) 0.0033(11) 0.0055(11) 0.0223(11) S10 0.0458(14) 0.089(2) 0.0745(19) -0.0037(16) 0.0165(13) 0.0166(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S2 2.475(3) . ? Ag1 S3 2.535(3) . ? Ag1 S8 2.541(2) . ? Ag1 Ag5 3.1622(12) . ? Ag1 Ag2 3.2409(13) . ? Ag1 Ag6 3.3402(14) . ? Ag2 S1 2.467(3) . ? Ag2 S9 2.533(3) . ? Ag2 S3 2.701(3) . ? Ag2 Br1 2.8836(15) . ? Ag2 Ag3 3.1678(13) . ? Ag3 S9 2.477(3) . ? Ag3 S5 2.489(3) . ? Ag3 S4 2.503(3) . ? Ag3 Ag4 3.1718(12) . ? Ag3 Ag5 3.1888(13) . ? Ag4 S10 2.484(3) . ? Ag4 S7 2.566(2) . ? Ag4 S5 2.602(2) . ? Ag4 Br1 2.8324(13) . ? Ag5 S6 2.565(2) . ? Ag5 S8 2.584(2) . ? Ag5 S4 2.585(3) . ? Ag5 Br1 2.8063(13) . ? Ag6 S6 2.536(2) 2_665 ? Ag6 S7 2.565(2) 2_665 ? Ag6 Br1 2.6959(14) . ? Ag6 S2 2.842(3) . ? C1 O1 1.445(14) . ? C1 C2 1.463(19) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O2 1.454(11) . ? C3 C4 1.457(17) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O3 1.386(17) . ? C5 C6 1.46(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 O4 1.358(17) . ? C7 C8 1.49(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.35(2) . ? C9 O5 1.467(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O6 1.402(13) . ? C11 C12 1.484(17) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O7 1.448(11) . ? C13 C14 1.458(15) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.470(15) . ? C15 O8 1.476(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.39(2) . ? C17 O9 1.401(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O10 1.405(9) . ? C19 C20 1.44(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O1 P1 1.587(7) . ? O2 P1 1.569(6) . ? O3 P2 1.634(9) . ? O4 P2 1.527(8) . ? O5 P3 1.570(7) . ? O6 P3 1.573(7) . ? O7 P4 1.583(6) . ? O8 P4 1.567(6) . ? O9 P5 1.565(9) . ? O10 P5 1.527(10) . ? P1 S1 1.968(4) . ? P1 S2 2.010(4) . ? P2 S3 1.976(4) . ? P2 S4 2.010(4) . ? P3 S6 1.989(3) . ? P3 S5 2.009(3) . ? P4 S8 1.991(3) 2_665 ? P4 S7 1.994(3) . ? P5 S10 1.948(4) . ? P5 S9 2.018(4) . ? S6 Ag6 2.536(2) 2_665 ? S7 Ag6 2.565(2) 2_665 ? S8 P4 1.991(3) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ag1 S3 113.25(8) . . ? S2 Ag1 S8 129.94(8) . . ? S3 Ag1 S8 113.40(8) . . ? S2 Ag1 Ag5 138.84(7) . . ? S3 Ag1 Ag5 93.78(6) . . ? S8 Ag1 Ag5 52.52(5) . . ? S2 Ag1 Ag2 88.87(7) . . ? S3 Ag1 Ag2 54.11(6) . . ? S8 Ag1 Ag2 134.00(6) . . ? Ag5 Ag1 Ag2 82.47(3) . . ? S2 Ag1 Ag6 56.17(6) . . ? S3 Ag1 Ag6 142.89(7) . . ? S8 Ag1 Ag6 94.11(6) . . ? Ag5 Ag1 Ag6 83.39(3) . . ? Ag2 Ag1 Ag6 88.94(4) . . ? S1 Ag2 S9 127.64(10) . . ? S1 Ag2 S3 112.42(9) . . ? S9 Ag2 S3 95.46(9) . . ? S1 Ag2 Br1 99.04(9) . . ? S9 Ag2 Br1 115.17(7) . . ? S3 Ag2 Br1 106.02(6) . . ? S1 Ag2 Ag3 161.99(8) . . ? S9 Ag2 Ag3 50.01(6) . . ? S3 Ag2 Ag3 85.24(6) . . ? Br1 Ag2 Ag3 71.45(4) . . ? S1 Ag2 Ag1 95.74(7) . . ? S9 Ag2 Ag1 134.41(7) . . ? S3 Ag2 Ag1 49.48(6) . . ? Br1 Ag2 Ag1 62.75(3) . . ? Ag3 Ag2 Ag1 93.28(3) . . ? S9 Ag3 S5 122.19(9) . . ? S9 Ag3 S4 118.82(9) . . ? S5 Ag3 S4 116.69(8) . . ? S9 Ag3 Ag2 51.56(7) . . ? S5 Ag3 Ag2 130.66(7) . . ? S4 Ag3 Ag2 99.63(7) . . ? S9 Ag3 Ag4 92.15(7) . . ? S5 Ag3 Ag4 53.07(6) . . ? S4 Ag3 Ag4 138.48(7) . . ? Ag2 Ag3 Ag4 77.60(3) . . ? S9 Ag3 Ag5 133.68(7) . . ? S5 Ag3 Ag5 93.19(6) . . ? S4 Ag3 Ag5 52.36(6) . . ? Ag2 Ag3 Ag5 83.21(3) . . ? Ag4 Ag3 Ag5 86.46(4) . . ? S10 Ag4 S7 119.67(9) . . ? S10 Ag4 S5 116.70(10) . . ? S7 Ag4 S5 103.66(8) . . ? S10 Ag4 Br1 105.19(10) . . ? S7 Ag4 Br1 103.32(6) . . ? S5 Ag4 Br1 106.95(6) . . ? S10 Ag4 Ag3 93.27(8) . . ? S7 Ag4 Ag3 146.24(6) . . ? S5 Ag4 Ag3 49.90(6) . . ? Br1 Ag4 Ag3 72.02(3) . . ? S6 Ag5 S8 130.32(8) . . ? S6 Ag5 S4 114.48(8) . . ? S8 Ag5 S4 99.08(8) . . ? S6 Ag5 Br1 91.36(6) . . ? S8 Ag5 Br1 106.52(6) . . ? S4 Ag5 Br1 115.54(6) . . ? S6 Ag5 Ag1 151.10(6) . . ? S8 Ag5 Ag1 51.29(5) . . ? S4 Ag5 Ag1 91.34(6) . . ? Br1 Ag5 Ag1 64.60(3) . . ? S6 Ag5 Ag3 92.88(6) . . ? S8 Ag5 Ag3 136.54(6) . . ? S4 Ag5 Ag3 50.04(6) . . ? Br1 Ag5 Ag3 72.08(3) . . ? Ag1 Ag5 Ag3 94.40(3) . . ? S6 Ag6 S7 119.49(8) 2_665 2_665 ? S6 Ag6 Br1 113.78(6) 2_665 . ? S7 Ag6 Br1 121.34(6) 2_665 . ? S6 Ag6 S2 113.47(8) 2_665 . ? S7 Ag6 S2 85.73(8) 2_665 . ? Br1 Ag6 S2 94.71(6) . . ? S6 Ag6 Ag1 155.64(7) 2_665 . ? S7 Ag6 Ag1 77.07(6) 2_665 . ? Br1 Ag6 Ag1 63.04(3) . . ? S2 Ag6 Ag1 46.33(5) . . ? Ag6 Br1 Ag5 103.70(4) . . ? Ag6 Br1 Ag4 146.34(4) . . ? Ag5 Br1 Ag4 101.17(4) . . ? Ag6 Br1 Ag2 111.42(5) . . ? Ag5 Br1 Ag2 95.77(4) . . ? Ag4 Br1 Ag2 88.04(4) . . ? O1 C1 C2 108.9(12) . . ? O1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? O1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 C4 108.2(10) . . ? O2 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O2 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 108.5(14) . . ? O3 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? O3 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C8 111.6(13) . . ? O4 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? O4 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 O5 111.3(13) . . ? C10 C9 H9A 109.4 . . ? O5 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? O5 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 110.9(11) . . ? O6 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? O6 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 C14 110.2(9) . . ? O7 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? O7 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 O8 107.1(8) . . ? C16 C15 H15A 110.3 . . ? O8 C15 H15A 110.3 . . ? C16 C15 H15B 110.3 . . ? O8 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 O9 115.5(15) . . ? C18 C17 H17A 108.4 . . ? O9 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? O9 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O10 C19 C20 114.7(14) . . ? O10 C19 H19A 108.6 . . ? C20 C19 H19A 108.6 . . ? O10 C19 H19B 108.6 . . ? C20 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1 O1 P1 119.0(8) . . ? C3 O2 P1 122.8(6) . . ? C5 O3 P2 124.2(10) . . ? C7 O4 P2 123.9(10) . . ? C9 O5 P3 123.1(7) . . ? C11 O6 P3 123.0(7) . . ? C13 O7 P4 121.1(6) . . ? C15 O8 P4 120.9(6) . . ? C17 O9 P5 132.1(10) . . ? C19 O10 P5 126.0(12) . . ? O2 P1 O1 100.8(4) . . ? O2 P1 S1 107.9(3) . . ? O1 P1 S1 109.3(3) . . ? O2 P1 S2 110.2(3) . . ? O1 P1 S2 106.8(3) . . ? S1 P1 S2 120.12(16) . . ? O4 P2 O3 100.4(6) . . ? O4 P2 S3 111.3(4) . . ? O3 P2 S3 101.4(4) . . ? O4 P2 S4 110.6(5) . . ? O3 P2 S4 109.9(4) . . ? S3 P2 S4 120.81(16) . . ? O5 P3 O6 102.0(4) . . ? O5 P3 S6 103.9(3) . . ? O6 P3 S6 110.9(3) . . ? O5 P3 S5 111.0(3) . . ? O6 P3 S5 108.0(3) . . ? S6 P3 S5 119.69(14) . . ? O8 P4 O7 106.3(4) . . ? O8 P4 S8 111.9(3) . 2_665 ? O7 P4 S8 102.9(3) . 2_665 ? O8 P4 S7 106.6(3) . . ? O7 P4 S7 110.5(3) . . ? S8 P4 S7 118.05(14) 2_665 . ? O10 P5 O9 96.6(7) . . ? O10 P5 S10 116.3(5) . . ? O9 P5 S10 104.5(5) . . ? O10 P5 S9 108.2(5) . . ? O9 P5 S9 109.4(4) . . ? S10 P5 S9 119.15(17) . . ? P1 S1 Ag2 101.30(13) . . ? P1 S2 Ag1 104.33(12) . . ? P1 S2 Ag6 121.61(14) . . ? Ag1 S2 Ag6 77.50(7) . . ? P2 S3 Ag1 101.90(12) . . ? P2 S3 Ag2 116.84(14) . . ? Ag1 S3 Ag2 76.41(7) . . ? P2 S4 Ag3 105.80(12) . . ? P2 S4 Ag5 107.79(13) . . ? Ag3 S4 Ag5 77.60(7) . . ? P3 S5 Ag3 104.20(12) . . ? P3 S5 Ag4 112.18(12) . . ? Ag3 S5 Ag4 77.04(7) . . ? P3 S6 Ag6 108.53(12) . 2_665 ? P3 S6 Ag5 103.06(12) . . ? Ag6 S6 Ag5 108.24(8) 2_665 . ? P4 S7 Ag6 111.66(12) . 2_665 ? P4 S7 Ag4 102.85(11) . . ? Ag6 S7 Ag4 87.37(8) 2_665 . ? P4 S8 Ag1 106.52(11) 2_665 . ? P4 S8 Ag5 105.65(11) 2_665 . ? Ag1 S8 Ag5 76.18(7) . . ? P5 S9 Ag3 108.09(13) . . ? P5 S9 Ag2 102.37(14) . . ? Ag3 S9 Ag2 78.43(8) . . ? P5 S10 Ag4 110.09(15) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.818 _refine_diff_density_min -1.427 _refine_diff_density_rms 0.165 _database_code_depnum_ccdc_archive 'CCDC 931314' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H100 Ag12 I2 O20 P10 S20' _chemical_formula_weight 3400.34 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' I I -0.4742 1.8119 '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 12.767(2) _cell_length_b 13.476(2) _cell_length_c 16.931(3) _cell_angle_alpha 100.256(3) _cell_angle_beta 102.841(3) _cell_angle_gamma 110.851(3) _cell_volume 2546.3(8) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5610 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.71 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 3.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5289 _exptl_absorpt_correction_T_max 0.7450 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24365 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.76 _reflns_number_total 10620 _reflns_number_gt 5634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints on bond lengths and atomic displacement paremeters were applied by using DFIX and DELU command in SHELX program. Those restraints are: DFIX 1.43 0.01 O4 C7 O10 C19 DELU O4 C7 DELU C7 C8 DELU C17 C18 DELU C19 C20 EADP C18 C20 EADP C17 C19 EADP C5 C7 ; _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^)+(0.0874P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10620 _refine_ls_number_parameters 451 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.014 _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 0.50747(7) 0.70650(7) 0.34441(5) 0.0668(2) Uani 1 1 d . . . Ag2 Ag 0.28430(9) 0.71535(8) 0.21429(7) 0.0891(3) Uani 1 1 d . . . Ag3 Ag 0.45006(8) 0.93230(8) 0.17929(6) 0.0755(3) Uani 1 1 d . . . Ag4 Ag 0.32896(7) 1.04506(7) 0.29069(5) 0.0667(2) Uani 1 1 d . . . Ag5 Ag 0.63701(7) 0.95621(7) 0.34766(5) 0.0644(2) Uani 1 1 d . . . Ag6 Ag 0.44326(9) 0.80938(11) 0.51244(6) 0.0928(4) Uani 1 1 d . . . I1 I 0.40929(5) 0.89784(5) 0.37479(4) 0.05105(18) Uani 1 1 d . . . S1 S 0.1339(3) 0.5920(2) 0.2637(2) 0.0788(9) Uani 1 1 d . . . S2 S 0.3718(2) 0.5897(2) 0.40881(17) 0.0646(7) Uani 1 1 d . . . S3 S 0.4414(3) 0.6337(2) 0.18376(17) 0.0655(7) Uani 1 1 d . . . S4 S 0.6323(2) 0.8959(2) 0.19136(16) 0.0624(7) Uani 1 1 d . . . S5 S 0.4819(2) 1.1316(2) 0.21679(17) 0.0597(7) Uani 1 1 d . . . S6 S 0.6919(2) 1.1681(2) 0.40201(16) 0.0526(6) Uani 1 1 d . . . S7 S 0.36020(19) 1.1991(2) 0.41931(15) 0.0495(6) Uani 1 1 d . . . S8 S 0.7290(2) 0.8293(2) 0.40701(14) 0.0512(6) Uani 1 1 d . . . S9 S 0.2574(2) 0.7851(2) 0.08511(17) 0.0676(7) Uani 1 1 d . . . S10 S 0.1268(3) 0.9154(3) 0.1969(2) 0.0868(10) Uani 1 1 d . . . P1 P 0.2162(2) 0.5097(2) 0.31596(18) 0.0564(7) Uani 1 1 d . . . P2 P 0.5746(3) 0.7307(3) 0.15407(19) 0.0713(8) Uani 1 1 d . . . P3 P 0.6461(2) 1.2123(2) 0.29831(17) 0.0568(6) Uani 1 1 d . . . P4 P 0.23510(19) 1.1239(2) 0.46775(14) 0.0447(5) Uani 1 1 d . . . P5 P 0.1328(2) 0.8437(2) 0.08827(17) 0.0630(7) Uani 1 1 d . . . O1 O 0.1305(7) 0.4243(6) 0.3512(5) 0.081(2) Uani 1 1 d . . . O2 O 0.2274(6) 0.4284(6) 0.2415(4) 0.0676(19) Uani 1 1 d . . . O3 O 0.6815(8) 0.6981(9) 0.1966(8) 0.131(4) Uani 1 1 d . . . O4 O 0.5650(10) 0.6917(10) 0.0632(6) 0.136(4) Uani 1 1 d DU . . O5 O 0.7381(7) 1.2034(7) 0.2527(5) 0.085(2) Uani 1 1 d . . . O6 O 0.6793(8) 1.3392(6) 0.3200(5) 0.088(2) Uani 1 1 d . . . O7 O 0.1225(6) 1.1467(6) 0.4340(4) 0.0580(17) Uani 1 1 d . . . O8 O 0.1966(5) 0.9972(5) 0.4330(4) 0.0578(17) Uani 1 1 d . . . O9 O 0.0084(8) 0.7458(8) 0.0453(7) 0.128(4) Uani 1 1 d . . . O10 O 0.1280(12) 0.9052(10) 0.0216(7) 0.139(4) Uani 1 1 d D . . C1 C 0.0896(16) 0.4593(14) 0.4158(11) 0.134(7) Uani 1 1 d . . . H1A H 0.0353 0.4904 0.3941 0.161 Uiso 1 1 calc R . . H1B H 0.1560 0.5181 0.4604 0.161 Uiso 1 1 calc R . . C2 C 0.0329(19) 0.3775(14) 0.4509(13) 0.161(9) Uani 1 1 d . . . H2A H 0.0069 0.4089 0.4940 0.242 Uiso 1 1 calc R . . H2B H 0.0868 0.3482 0.4751 0.242 Uiso 1 1 calc R . . H2C H -0.0338 0.3191 0.4077 0.242 Uiso 1 1 calc R . . C3 C 0.2894(12) 0.3599(10) 0.2557(9) 0.090(4) Uani 1 1 d . . . H3A H 0.3711 0.3986 0.2589 0.108 Uiso 1 1 calc R . . H3B H 0.2876 0.3425 0.3087 0.108 Uiso 1 1 calc R . . C4 C 0.2348(19) 0.2606(13) 0.1882(10) 0.154(9) Uani 1 1 d . . . H4A H 0.2758 0.2142 0.1974 0.231 Uiso 1 1 calc R . . H4B H 0.2378 0.2782 0.1360 0.231 Uiso 1 1 calc R . . H4C H 0.1542 0.2225 0.1855 0.231 Uiso 1 1 calc R . . C5 C 0.7904(15) 0.7319(18) 0.1926(12) 0.143(5) Uani 1 1 d . . . H5A H 0.8410 0.7979 0.2389 0.171 Uiso 1 1 calc R . . H5B H 0.7917 0.7514 0.1402 0.171 Uiso 1 1 calc R . . C6 C 0.8354(15) 0.6495(16) 0.1966(13) 0.146(7) Uani 1 1 d . . . H6A H 0.9147 0.6777 0.1942 0.219 Uiso 1 1 calc R . . H6B H 0.7870 0.5848 0.1498 0.219 Uiso 1 1 calc R . . H6C H 0.8348 0.6303 0.2485 0.219 Uiso 1 1 calc R . . C7 C 0.4708(14) 0.6798(18) -0.0044(10) 0.143(5) Uani 1 1 d DU . . H7A H 0.4692 0.7514 -0.0036 0.171 Uiso 1 1 calc R . . H7B H 0.3969 0.6317 0.0007 0.171 Uiso 1 1 calc R . . C8 C 0.485(2) 0.6317(15) -0.0851(9) 0.162(9) Uani 1 1 d U . . H8A H 0.4213 0.6239 -0.1315 0.243 Uiso 1 1 calc R . . H8B H 0.4857 0.5604 -0.0859 0.243 Uiso 1 1 calc R . . H8C H 0.5585 0.6798 -0.0899 0.243 Uiso 1 1 calc R . . C9 C 0.7405(16) 1.2211(17) 0.1718(11) 0.133(6) Uani 1 1 d . . . H9A H 0.7202 1.1507 0.1320 0.160 Uiso 1 1 calc R . . H9B H 0.6805 1.2471 0.1522 0.160 Uiso 1 1 calc R . . C10 C 0.8450(18) 1.294(2) 0.1715(12) 0.233(16) Uani 1 1 d . . . H10A H 0.8396 1.3006 0.1153 0.350 Uiso 1 1 calc R . . H10B H 0.9051 1.2686 0.1898 0.350 Uiso 1 1 calc R . . H10C H 0.8648 1.3650 0.2090 0.350 Uiso 1 1 calc R . . C11 C 0.6135(15) 1.3864(13) 0.3539(10) 0.110(5) Uani 1 1 d . . . H11A H 0.6200 1.3783 0.4104 0.132 Uiso 1 1 calc R . . H11B H 0.5313 1.3460 0.3201 0.132 Uiso 1 1 calc R . . C12 C 0.6498(17) 1.5066(12) 0.3585(14) 0.151(8) Uani 1 1 d . . . H12A H 0.6005 1.5337 0.3827 0.227 Uiso 1 1 calc R . . H12B H 0.6415 1.5153 0.3027 0.227 Uiso 1 1 calc R . . H12C H 0.7305 1.5477 0.3931 0.227 Uiso 1 1 calc R . . C13 C 0.0702(10) 1.1283(12) 0.3435(7) 0.084(4) Uani 1 1 d . . . H13A H 0.0956 1.1985 0.3303 0.101 Uiso 1 1 calc R . . H13B H 0.0980 1.0812 0.3117 0.101 Uiso 1 1 calc R . . C14 C -0.0567(10) 1.0771(14) 0.3185(8) 0.108(5) Uani 1 1 d . . . H14A H -0.0882 1.0660 0.2590 0.162 Uiso 1 1 calc R . . H14B H -0.0845 1.1243 0.3490 0.162 Uiso 1 1 calc R . . H14C H -0.0821 1.0071 0.3307 0.162 Uiso 1 1 calc R . . C15 C 0.0994(9) 0.9170(8) 0.4523(7) 0.068(3) Uani 1 1 d . . . H15A H 0.1222 0.9220 0.5120 0.082 Uiso 1 1 calc R . . H15B H 0.0305 0.9334 0.4390 0.082 Uiso 1 1 calc R . . C16 C 0.0717(13) 0.8072(10) 0.4031(8) 0.099(4) Uani 1 1 d . . . H16A H 0.0082 0.7546 0.4154 0.149 Uiso 1 1 calc R . . H16B H 0.1399 0.7910 0.4170 0.149 Uiso 1 1 calc R . . H16C H 0.0488 0.8025 0.3441 0.149 Uiso 1 1 calc R . . C17 C -0.0311(18) 0.6478(16) -0.0121(14) 0.159(5) Uani 1 1 d U . . H17A H 0.0264 0.6172 0.0027 0.190 Uiso 1 1 calc R . . H17B H -0.0287 0.6630 -0.0658 0.190 Uiso 1 1 calc R . . C18 C -0.1420(16) 0.5633(15) -0.0269(12) 0.144(4) Uani 1 1 d U . . H18A H -0.1528 0.4995 -0.0690 0.216 Uiso 1 1 calc R . . H18B H -0.2021 0.5883 -0.0464 0.216 Uiso 1 1 calc R . . H18C H -0.1473 0.5443 0.0245 0.216 Uiso 1 1 calc R . . C19 C 0.2064(16) 1.0059(14) 0.0190(14) 0.159(5) Uani 1 1 d DU . . H19A H 0.2731 0.9958 0.0065 0.190 Uiso 1 1 calc R . . H19B H 0.2357 1.0575 0.0748 0.190 Uiso 1 1 calc R . . C20 C 0.1619(17) 1.0550(16) -0.0399(12) 0.144(4) Uani 1 1 d U . . H20A H 0.2233 1.1240 -0.0363 0.216 Uiso 1 1 calc R . . H20B H 0.0975 1.0681 -0.0273 0.216 Uiso 1 1 calc R . . H20C H 0.1349 1.0062 -0.0959 0.216 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 0.0593(5) 0.0600(5) 0.0694(5) 0.0144(4) 0.0174(4) 0.0148(4) Ag2 0.0904(7) 0.0781(7) 0.0904(7) 0.0345(6) 0.0127(6) 0.0294(6) Ag3 0.0594(5) 0.0680(6) 0.0827(6) 0.0099(5) 0.0085(4) 0.0213(4) Ag4 0.0633(5) 0.0705(6) 0.0627(5) 0.0129(4) 0.0190(4) 0.0266(4) Ag5 0.0653(5) 0.0625(5) 0.0676(5) 0.0200(4) 0.0171(4) 0.0303(4) Ag6 0.0946(7) 0.1519(10) 0.0856(7) 0.0667(7) 0.0499(6) 0.0819(7) I1 0.0540(4) 0.0459(4) 0.0548(4) 0.0150(3) 0.0163(3) 0.0224(3) S1 0.0596(16) 0.0595(18) 0.117(2) 0.0249(17) 0.0237(17) 0.0261(15) S2 0.0614(15) 0.0561(16) 0.0629(16) 0.0142(13) 0.0144(13) 0.0134(13) S3 0.0705(17) 0.0548(16) 0.0636(16) 0.0034(13) 0.0197(14) 0.0242(14) S4 0.0536(14) 0.0718(18) 0.0564(14) 0.0141(13) 0.0215(12) 0.0191(14) S5 0.0559(14) 0.0654(17) 0.0633(15) 0.0299(13) 0.0174(12) 0.0261(13) S6 0.0445(12) 0.0488(14) 0.0615(14) 0.0129(11) 0.0155(11) 0.0177(11) S7 0.0426(12) 0.0492(14) 0.0538(13) 0.0153(11) 0.0122(10) 0.0168(11) S8 0.0478(13) 0.0555(14) 0.0479(12) 0.0089(11) 0.0119(11) 0.0233(12) S9 0.0635(16) 0.0686(18) 0.0557(15) 0.0038(13) 0.0014(13) 0.0273(15) S10 0.0532(16) 0.104(3) 0.079(2) -0.0042(18) 0.0134(15) 0.0248(17) P1 0.0529(14) 0.0422(14) 0.0720(17) 0.0126(13) 0.0248(13) 0.0157(12) P2 0.0591(16) 0.076(2) 0.0631(17) -0.0066(15) 0.0217(14) 0.0205(16) P3 0.0550(15) 0.0503(15) 0.0654(16) 0.0216(13) 0.0259(13) 0.0152(13) P4 0.0375(11) 0.0478(14) 0.0481(12) 0.0111(11) 0.0105(10) 0.0196(11) P5 0.0611(16) 0.0577(17) 0.0571(15) 0.0091(13) -0.0001(13) 0.0243(14) O1 0.072(5) 0.065(5) 0.101(6) 0.022(4) 0.044(5) 0.012(4) O2 0.075(5) 0.057(4) 0.068(4) 0.008(4) 0.015(4) 0.033(4) O3 0.072(6) 0.122(9) 0.211(12) 0.031(8) 0.061(7) 0.053(6) O4 0.137(9) 0.150(10) 0.067(6) -0.006(6) 0.028(5) 0.019(8) O5 0.067(5) 0.118(7) 0.094(6) 0.052(5) 0.051(5) 0.039(5) O6 0.112(7) 0.057(5) 0.097(6) 0.032(4) 0.028(5) 0.036(5) O7 0.058(4) 0.080(5) 0.051(4) 0.021(3) 0.018(3) 0.043(4) O8 0.048(4) 0.049(4) 0.074(4) 0.009(3) 0.022(3) 0.018(3) O9 0.071(6) 0.095(7) 0.140(9) -0.054(6) -0.036(6) 0.028(5) O10 0.209(13) 0.133(10) 0.116(8) 0.063(8) 0.054(9) 0.101(10) C1 0.144(15) 0.110(13) 0.135(14) 0.006(11) 0.088(13) 0.026(12) C2 0.22(2) 0.102(13) 0.163(17) 0.026(12) 0.132(18) 0.036(14) C3 0.109(10) 0.078(9) 0.110(10) 0.029(8) 0.043(9) 0.062(8) C4 0.29(3) 0.114(13) 0.104(12) 0.015(10) 0.048(14) 0.145(17) C5 0.121(9) 0.207(15) 0.147(9) 0.065(10) 0.058(8) 0.101(11) C6 0.108(13) 0.180(19) 0.20(2) 0.068(16) 0.065(13) 0.093(14) C7 0.121(9) 0.207(15) 0.147(9) 0.065(10) 0.058(8) 0.101(11) C8 0.27(3) 0.133(15) 0.065(9) 0.014(10) 0.029(12) 0.079(17) C9 0.129(14) 0.168(18) 0.114(13) 0.050(13) 0.063(12) 0.055(14) C10 0.147(17) 0.33(4) 0.096(13) 0.080(18) 0.040(13) -0.06(2) C11 0.141(14) 0.107(12) 0.111(11) 0.038(9) 0.049(11) 0.074(11) C12 0.172(18) 0.063(10) 0.21(2) 0.037(12) 0.031(16) 0.056(11) C13 0.069(7) 0.126(11) 0.069(7) 0.041(7) 0.020(6) 0.048(8) C14 0.058(7) 0.171(16) 0.073(8) 0.035(9) 0.001(6) 0.035(9) C15 0.062(6) 0.053(6) 0.083(8) 0.017(6) 0.034(6) 0.011(6) C16 0.112(10) 0.061(8) 0.090(9) 0.012(7) 0.040(8) -0.005(8) C17 0.142(11) 0.112(11) 0.180(14) 0.024(10) 0.017(11) 0.033(8) C18 0.152(11) 0.139(11) 0.136(11) 0.044(9) 0.049(10) 0.050(8) C19 0.142(11) 0.112(11) 0.180(14) 0.024(10) 0.017(11) 0.033(8) C20 0.152(11) 0.139(11) 0.136(11) 0.044(9) 0.049(10) 0.050(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 S2 2.485(3) . ? Ag1 S3 2.552(3) . ? Ag1 S8 2.564(3) . ? Ag1 Ag5 3.1613(13) . ? Ag1 Ag2 3.2452(13) . ? Ag1 I1 3.2557(11) . ? Ag1 Ag6 3.3360(14) . ? Ag2 S1 2.468(3) . ? Ag2 S9 2.533(3) . ? Ag2 S3 2.707(3) . ? Ag2 I1 2.9796(13) . ? Ag2 Ag3 3.1854(15) . ? Ag3 S9 2.487(3) . ? Ag3 S5 2.507(3) . ? Ag3 S4 2.517(3) . ? Ag3 Ag5 3.1668(12) . ? Ag3 Ag4 3.1945(13) . ? Ag4 S10 2.493(3) . ? Ag4 S7 2.574(3) . ? Ag4 S5 2.593(3) . ? Ag4 I1 2.9699(11) . ? Ag5 S4 2.607(3) . ? Ag5 S8 2.614(2) . ? Ag5 S6 2.617(3) . ? Ag5 I1 2.8943(12) . ? Ag6 S6 2.548(3) 2_676 ? Ag6 S7 2.571(2) 2_676 ? Ag6 I1 2.8193(11) . ? Ag6 S2 2.862(3) . ? S1 P1 1.970(4) . ? S2 P1 2.016(4) . ? S3 P2 1.971(4) . ? S4 P2 2.006(4) . ? S5 P3 2.010(4) . ? S6 P3 1.985(4) . ? S6 Ag6 2.548(3) 2_676 ? S7 P4 1.994(3) . ? S7 Ag6 2.571(2) 2_676 ? S8 P4 1.998(3) 2_676 ? S9 P5 2.017(4) . ? S10 P5 1.951(4) . ? P1 O2 1.583(7) . ? P1 O1 1.586(8) . ? P2 O4 1.497(10) . ? P2 O3 1.635(10) . ? P3 O6 1.559(8) . ? P3 O5 1.569(8) . ? P4 O8 1.555(7) . ? P4 O7 1.580(6) . ? P4 S8 1.998(3) 2_676 ? P5 O10 1.518(10) . ? P5 O9 1.564(9) . ? O1 C1 1.392(16) . ? O2 C3 1.433(12) . ? O3 C5 1.321(18) . ? O4 C7 1.403(9) . ? O5 C9 1.436(17) . ? O6 C11 1.380(16) . ? O7 C13 1.464(12) . ? O8 C15 1.472(12) . ? O9 C17 1.34(2) . ? O10 C19 1.386(9) . ? C1 C2 1.40(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.421(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.43(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.48(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.35(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.50(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.441(16) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.438(15) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.40(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.42(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ag1 S3 112.76(10) . . ? S2 Ag1 S8 129.41(9) . . ? S3 Ag1 S8 112.58(9) . . ? S2 Ag1 Ag5 141.13(8) . . ? S3 Ag1 Ag5 94.32(7) . . ? S8 Ag1 Ag5 53.10(6) . . ? S2 Ag1 Ag2 89.83(7) . . ? S3 Ag1 Ag2 54.09(7) . . ? S8 Ag1 Ag2 135.72(7) . . ? Ag5 Ag1 Ag2 83.99(3) . . ? S2 Ag1 I1 92.08(7) . . ? S3 Ag1 I1 102.91(7) . . ? S8 Ag1 I1 98.67(6) . . ? Ag5 Ag1 I1 53.60(3) . . ? Ag2 Ag1 I1 54.56(3) . . ? S2 Ag1 Ag6 56.65(7) . . ? S3 Ag1 Ag6 146.15(7) . . ? S8 Ag1 Ag6 94.14(6) . . ? Ag5 Ag1 Ag6 85.22(3) . . ? Ag2 Ag1 Ag6 92.34(4) . . ? I1 Ag1 Ag6 50.63(2) . . ? S1 Ag2 S9 129.23(11) . . ? S1 Ag2 S3 112.92(10) . . ? S9 Ag2 S3 96.75(10) . . ? S1 Ag2 I1 97.44(9) . . ? S9 Ag2 I1 112.82(7) . . ? S3 Ag2 I1 106.64(7) . . ? S1 Ag2 Ag3 160.90(9) . . ? S9 Ag2 Ag3 49.98(7) . . ? S3 Ag2 Ag3 85.10(7) . . ? I1 Ag2 Ag3 70.17(3) . . ? S1 Ag2 Ag1 95.32(8) . . ? S9 Ag2 Ag1 134.31(8) . . ? S3 Ag2 Ag1 49.77(6) . . ? I1 Ag2 Ag1 62.90(3) . . ? Ag3 Ag2 Ag1 91.77(4) . . ? S9 Ag3 S5 121.12(9) . . ? S9 Ag3 S4 118.60(10) . . ? S5 Ag3 S4 116.19(9) . . ? S9 Ag3 Ag5 135.19(8) . . ? S5 Ag3 Ag5 94.90(6) . . ? S4 Ag3 Ag5 53.12(6) . . ? S9 Ag3 Ag2 51.25(7) . . ? S5 Ag3 Ag2 134.51(8) . . ? S4 Ag3 Ag2 99.85(7) . . ? Ag5 Ag3 Ag2 84.89(3) . . ? S9 Ag3 Ag4 92.87(7) . . ? S5 Ag3 Ag4 52.43(7) . . ? S4 Ag3 Ag4 141.38(7) . . ? Ag5 Ag3 Ag4 89.08(3) . . ? Ag2 Ag3 Ag4 82.12(4) . . ? S10 Ag4 S7 120.99(10) . . ? S10 Ag4 S5 116.58(11) . . ? S7 Ag4 S5 107.04(9) . . ? S10 Ag4 I1 102.22(10) . . ? S7 Ag4 I1 101.05(6) . . ? S5 Ag4 I1 106.69(6) . . ? S10 Ag4 Ag3 92.37(8) . . ? S7 Ag4 Ag3 146.62(6) . . ? S5 Ag4 Ag3 50.03(7) . . ? I1 Ag4 Ag3 70.16(3) . . ? S4 Ag5 S8 98.38(9) . . ? S4 Ag5 S6 112.68(9) . . ? S8 Ag5 S6 131.50(8) . . ? S4 Ag5 I1 115.67(6) . . ? S8 Ag5 I1 107.22(6) . . ? S6 Ag5 I1 92.19(6) . . ? S4 Ag5 Ag1 90.97(7) . . ? S8 Ag5 Ag1 51.66(6) . . ? S6 Ag5 Ag1 153.04(7) . . ? I1 Ag5 Ag1 64.87(3) . . ? S4 Ag5 Ag3 50.55(6) . . ? S8 Ag5 Ag3 136.15(6) . . ? S6 Ag5 Ag3 91.90(6) . . ? I1 Ag5 Ag3 71.48(3) . . ? Ag1 Ag5 Ag3 93.71(3) . . ? S6 Ag6 S7 121.56(9) 2_676 2_676 ? S6 Ag6 I1 109.71(6) 2_676 . ? S7 Ag6 I1 122.39(7) 2_676 . ? S6 Ag6 S2 115.21(9) 2_676 . ? S7 Ag6 S2 86.76(8) 2_676 . ? I1 Ag6 S2 94.35(6) . . ? S6 Ag6 Ag1 155.56(7) 2_676 . ? S7 Ag6 Ag1 77.86(6) 2_676 . ? I1 Ag6 Ag1 63.21(3) . . ? S2 Ag6 Ag1 46.50(6) . . ? Ag6 I1 Ag5 100.74(3) . . ? Ag6 I1 Ag4 151.05(4) . . ? Ag5 I1 Ag4 99.08(3) . . ? Ag6 I1 Ag2 109.90(4) . . ? Ag5 I1 Ag2 93.73(3) . . ? Ag4 I1 Ag2 89.56(3) . . ? Ag6 I1 Ag1 66.16(3) . . ? Ag5 I1 Ag1 61.53(3) . . ? Ag4 I1 Ag1 142.66(3) . . ? Ag2 I1 Ag1 62.54(3) . . ? P1 S1 Ag2 102.34(15) . . ? P1 S2 Ag1 104.93(14) . . ? P1 S2 Ag6 122.04(14) . . ? Ag1 S2 Ag6 76.85(8) . . ? P2 S3 Ag1 102.82(14) . . ? P2 S3 Ag2 116.83(16) . . ? Ag1 S3 Ag2 76.13(8) . . ? P2 S4 Ag3 105.51(14) . . ? P2 S4 Ag5 108.75(15) . . ? Ag3 S4 Ag5 76.33(8) . . ? P3 S5 Ag3 104.73(13) . . ? P3 S5 Ag4 111.94(13) . . ? Ag3 S5 Ag4 77.54(8) . . ? P3 S6 Ag6 106.89(13) . 2_676 ? P3 S6 Ag5 104.58(13) . . ? Ag6 S6 Ag5 107.54(9) 2_676 . ? P4 S7 Ag6 112.06(12) . 2_676 ? P4 S7 Ag4 103.04(12) . . ? Ag6 S7 Ag4 87.76(8) 2_676 . ? P4 S8 Ag1 107.00(12) 2_676 . ? P4 S8 Ag5 106.49(12) 2_676 . ? Ag1 S8 Ag5 75.25(7) . . ? P5 S9 Ag3 107.85(14) . . ? P5 S9 Ag2 105.10(15) . . ? Ag3 S9 Ag2 78.77(8) . . ? P5 S10 Ag4 110.42(16) . . ? O2 P1 O1 101.1(4) . . ? O2 P1 S1 106.9(3) . . ? O1 P1 S1 109.1(3) . . ? O2 P1 S2 110.2(3) . . ? O1 P1 S2 106.7(3) . . ? S1 P1 S2 121.01(17) . . ? O4 P2 O3 98.8(7) . . ? O4 P2 S3 112.5(5) . . ? O3 P2 S3 102.4(4) . . ? O4 P2 S4 110.6(5) . . ? O3 P2 S4 108.3(4) . . ? S3 P2 S4 121.24(18) . . ? O6 P3 O5 101.0(5) . . ? O6 P3 S6 110.8(3) . . ? O5 P3 S6 103.5(3) . . ? O6 P3 S5 109.0(4) . . ? O5 P3 S5 110.0(4) . . ? S6 P3 S5 120.58(16) . . ? O8 P4 O7 106.4(4) . . ? O8 P4 S7 107.0(3) . . ? O7 P4 S7 110.1(3) . . ? O8 P4 S8 111.9(3) . 2_676 ? O7 P4 S8 103.2(3) . 2_676 ? S7 P4 S8 117.70(15) . 2_676 ? O10 P5 O9 97.3(7) . . ? O10 P5 S10 116.0(5) . . ? O9 P5 S10 104.9(5) . . ? O10 P5 S9 107.7(5) . . ? O9 P5 S9 108.9(4) . . ? S10 P5 S9 119.45(17) . . ? C1 O1 P1 121.7(9) . . ? C3 O2 P1 122.9(7) . . ? C5 O3 P2 129.6(13) . . ? C7 O4 P2 123.8(12) . . ? C9 O5 P3 126.3(9) . . ? C11 O6 P3 122.5(9) . . ? C13 O7 P4 120.9(6) . . ? C15 O8 P4 121.0(6) . . ? C17 O9 P5 133.5(13) . . ? C19 O10 P5 130.9(14) . . ? O1 C1 C2 115.4(15) . . ? O1 C1 H1A 108.4 . . ? C2 C1 H1A 108.4 . . ? O1 C1 H1B 108.4 . . ? C2 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 O2 109.1(12) . . ? C4 C3 H3A 109.9 . . ? O2 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? O2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 112.2(18) . . ? O3 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? O3 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C8 109.3(14) . . ? O4 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O4 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 O5 114.6(16) . . ? C10 C9 H9A 108.6 . . ? O5 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? O5 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 114.1(15) . . ? O6 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? O6 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 O7 111.5(10) . . ? C14 C13 H13A 109.3 . . ? O7 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? O7 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 O8 109.2(9) . . ? C16 C15 H15A 109.8 . . ? O8 C15 H15A 109.8 . . ? C16 C15 H15B 109.8 . . ? O8 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O9 C17 C18 122(2) . . ? O9 C17 H17A 106.8 . . ? C18 C17 H17A 106.8 . . ? O9 C17 H17B 106.8 . . ? C18 C17 H17B 106.8 . . ? H17A C17 H17B 106.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O10 C19 C20 116.4(16) . . ? O10 C19 H19A 108.2 . . ? C20 C19 H19A 108.2 . . ? O10 C19 H19B 108.2 . . ? C20 C19 H19B 108.2 . . ? H19A C19 H19B 107.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.76 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.269 _refine_diff_density_min -1.598 _refine_diff_density_rms 0.157 _database_code_depnum_ccdc_archive 'CCDC 931315' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H100 Ag12 I2 O20 P10 Se20' _chemical_formula_weight 4338.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 12.927(2) _cell_length_b 13.628(2) _cell_length_c 16.945(2) _cell_angle_alpha 99.812(4) _cell_angle_beta 102.430(4) _cell_angle_gamma 110.352(4) _cell_volume 2633.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2053 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.84 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 9.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2427 _exptl_absorpt_correction_T_max 0.3837 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14634 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.1102 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9092 _reflns_number_gt 5162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints on bond lengths and atomic displacement paremeters were applied by using DFIX and DELU command in SHELX program. Those restraints are: DFIX 1.43 0.01 O3 C5 O9 C17 DFIX 1.54 0.01 C7 C8 DELU C7 C8 DELU C19 C20 EADP C17 C19 EADP C7 C5 EADP O9 O10 EADP O3 O4 ; _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^)+(0.0917P)^2^+4.4638P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9092 _refine_ls_number_parameters 445 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1222 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.000 _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 0.50926(13) 0.20526(12) 0.34307(9) 0.0537(4) Uani 1 1 d . . . Ag2 Ag 0.29444(15) 0.22176(13) 0.21702(11) 0.0691(5) Uani 1 1 d . . . Ag3 Ag 0.44932(13) 0.42934(12) 0.17589(10) 0.0608(4) Uani 1 1 d . . . Ag4 Ag 0.33271(13) 0.54278(12) 0.28596(9) 0.0559(4) Uani 1 1 d . . . Ag5 Ag 0.63525(13) 0.45093(11) 0.34281(9) 0.0514(4) Uani 1 1 d . . . Ag6 Ag 0.44032(16) 0.30404(16) 0.50921(11) 0.0724(5) Uani 1 1 d . . . C1 C 0.094(2) -0.042(2) 0.4165(19) 0.106(10) Uani 1 1 d . . . H1A H 0.0435 -0.0069 0.3968 0.127 Uiso 1 1 calc R . . H1B H 0.1602 0.0123 0.4616 0.127 Uiso 1 1 calc R . . C2 C 0.034(3) -0.129(2) 0.448(2) 0.143(15) Uani 1 1 d . . . H2A H 0.0076 -0.1011 0.4918 0.214 Uiso 1 1 calc R . . H2B H 0.0852 -0.1613 0.4691 0.214 Uiso 1 1 calc R . . H2C H -0.0309 -0.1821 0.4030 0.214 Uiso 1 1 calc R . . C3 C 0.2804(18) -0.1385(16) 0.2546(13) 0.061(5) Uani 1 1 d . . . H3A H 0.2657 -0.1654 0.3023 0.073 Uiso 1 1 calc R . . H3B H 0.3632 -0.0986 0.2678 0.073 Uiso 1 1 calc R . . C4 C 0.239(3) -0.235(2) 0.1777(19) 0.151(16) Uani 1 1 d . . . H4A H 0.2797 -0.2808 0.1891 0.226 Uiso 1 1 calc R . . H4B H 0.2552 -0.2088 0.1306 0.226 Uiso 1 1 calc R . . H4C H 0.1579 -0.2757 0.1652 0.226 Uiso 1 1 calc R . . C5 C 0.8012(14) 0.2345(18) 0.1871(17) 0.089(5) Uani 1 1 d D . . H5A H 0.8472 0.3029 0.2294 0.107 Uiso 1 1 calc R . . H5B H 0.7997 0.2475 0.1324 0.107 Uiso 1 1 calc R . . C6 C 0.857(2) 0.150(2) 0.2000(17) 0.099(9) Uani 1 1 d . . . H6A H 0.9338 0.1774 0.1955 0.149 Uiso 1 1 calc R . . H6B H 0.8110 0.0823 0.1579 0.149 Uiso 1 1 calc R . . H6C H 0.8592 0.1381 0.2546 0.149 Uiso 1 1 calc R . . C7 C 0.491(2) 0.190(2) -0.0021(14) 0.089(5) Uani 1 1 d DU . . H7A H 0.5120 0.2651 -0.0041 0.107 Uiso 1 1 calc R . . H7B H 0.4217 0.1686 0.0152 0.107 Uiso 1 1 calc R . . C8 C 0.463(4) 0.120(2) -0.0907(15) 0.18(2) Uani 1 1 d DU . . H8A H 0.4025 0.1309 -0.1278 0.266 Uiso 1 1 calc R . . H8B H 0.4376 0.0453 -0.0907 0.266 Uiso 1 1 calc R . . H8C H 0.5304 0.1410 -0.1093 0.266 Uiso 1 1 calc R . . C9 C 0.750(2) 0.718(2) 0.1664(15) 0.103(9) Uani 1 1 d . . . H9A H 0.7407 0.6530 0.1269 0.123 Uiso 1 1 calc R . . H9B H 0.6882 0.7399 0.1445 0.123 Uiso 1 1 calc R . . C10 C 0.856(3) 0.801(3) 0.1765(17) 0.169(18) Uani 1 1 d . . . H10A H 0.8596 0.8155 0.1234 0.253 Uiso 1 1 calc R . . H10B H 0.9175 0.7790 0.1976 0.253 Uiso 1 1 calc R . . H10C H 0.8653 0.8655 0.2154 0.253 Uiso 1 1 calc R . . C11 C 0.622(2) 0.8893(17) 0.3525(15) 0.073(7) Uani 1 1 d . . . H11A H 0.6334 0.8847 0.4100 0.088 Uiso 1 1 calc R . . H11B H 0.5401 0.8526 0.3227 0.088 Uiso 1 1 calc R . . C12 C 0.666(2) 1.0063(16) 0.3502(18) 0.096(9) Uani 1 1 d . . . H12A H 0.6250 1.0421 0.3763 0.144 Uiso 1 1 calc R . . H12B H 0.6541 1.0098 0.2930 0.144 Uiso 1 1 calc R . . H12C H 0.7470 1.0416 0.3799 0.144 Uiso 1 1 calc R . . C13 C 0.0806(16) 0.6347(18) 0.3400(11) 0.059(5) Uani 1 1 d . . . H13A H 0.1146 0.5927 0.3106 0.071 Uiso 1 1 calc R . . H13B H 0.1000 0.7037 0.3261 0.071 Uiso 1 1 calc R . . C14 C -0.0511(15) 0.5727(18) 0.3144(12) 0.065(6) Uani 1 1 d . . . H14A H -0.0827 0.5597 0.2551 0.097 Uiso 1 1 calc R . . H14B H -0.0838 0.6152 0.3437 0.097 Uiso 1 1 calc R . . H14C H -0.0693 0.5047 0.3285 0.097 Uiso 1 1 calc R . . C15 C 0.0918(17) 0.4223(15) 0.4526(12) 0.057(5) Uani 1 1 d . . . H15A H 0.1094 0.4286 0.5124 0.068 Uiso 1 1 calc R . . H15B H 0.0216 0.4339 0.4340 0.068 Uiso 1 1 calc R . . C16 C 0.080(2) 0.3125(15) 0.4041(13) 0.077(7) Uani 1 1 d . . . H16A H 0.0177 0.2561 0.4130 0.115 Uiso 1 1 calc R . . H16B H 0.1505 0.3034 0.4232 0.115 Uiso 1 1 calc R . . H16C H 0.0636 0.3087 0.3454 0.115 Uiso 1 1 calc R . . C17 C -0.037(2) 0.1433(17) -0.0212(14) 0.091(5) Uani 1 1 d D . . H17A H -0.0506 0.1627 -0.0738 0.109 Uiso 1 1 calc R . . H17B H 0.0236 0.1166 -0.0184 0.109 Uiso 1 1 calc R . . C18 C -0.137(2) 0.0571(19) -0.0253(15) 0.115(11) Uani 1 1 d . . . H18A H -0.1499 -0.0048 -0.0689 0.173 Uiso 1 1 calc R . . H18B H -0.2017 0.0773 -0.0374 0.173 Uiso 1 1 calc R . . H18C H -0.1286 0.0392 0.0274 0.173 Uiso 1 1 calc R . . C19 C 0.203(2) 0.495(2) 0.0155(16) 0.091(5) Uani 1 1 d U . . H19A H 0.2595 0.4757 -0.0049 0.109 Uiso 1 1 calc R . . H19B H 0.2398 0.5389 0.0731 0.109 Uiso 1 1 calc R . . C20 C 0.160(2) 0.561(2) -0.0378(17) 0.110(10) Uani 1 1 d U . . H20A H 0.2243 0.6246 -0.0352 0.165 Uiso 1 1 calc R . . H20B H 0.1051 0.5811 -0.0168 0.165 Uiso 1 1 calc R . . H20C H 0.1238 0.5173 -0.0949 0.165 Uiso 1 1 calc R . . I1 I 0.41272(10) 0.39897(8) 0.37373(7) 0.0394(3) Uani 1 1 d . . . O1 O 0.1324(10) -0.0786(9) 0.3513(8) 0.048(3) Uani 1 1 d . . . O2 O 0.2258(10) -0.0690(8) 0.2421(7) 0.041(3) Uani 1 1 d . . . O3 O 0.6867(11) 0.1934(11) 0.1932(9) 0.070(3) Uani 1 1 d D . . O4 O 0.5744(12) 0.1864(12) 0.0559(9) 0.070(3) Uani 1 1 d . . . O5 O 0.7475(10) 0.6981(11) 0.2475(8) 0.062(4) Uani 1 1 d . . . O6 O 0.6881(11) 0.8388(9) 0.3118(8) 0.061(4) Uani 1 1 d . . . O7 O 0.1243(10) 0.6521(9) 0.4304(7) 0.045(3) Uani 1 1 d . . . O8 O 0.1924(10) 0.5032(8) 0.4326(7) 0.043(3) Uani 1 1 d . . . O9 O 0.0062(13) 0.2398(12) 0.0440(10) 0.087(3) Uani 1 1 d D . . O10 O 0.1111(14) 0.3994(13) 0.0131(10) 0.087(3) Uani 1 1 d . . . P1 P 0.2151(4) 0.0076(3) 0.3157(3) 0.0414(11) Uani 1 1 d . . . P2 P 0.5836(4) 0.2243(4) 0.1497(3) 0.0457(11) Uani 1 1 d . . . P3 P 0.6533(4) 0.7130(4) 0.2928(3) 0.0454(11) Uani 1 1 d . . . P4 P 0.2311(4) 0.6281(3) 0.4666(3) 0.0335(9) Uani 1 1 d . . . P5 P 0.1250(4) 0.3379(4) 0.0811(3) 0.0471(12) Uani 1 1 d . . . Se1 Se 0.12926(18) 0.09845(16) 0.26298(14) 0.0608(6) Uani 1 1 d . . . Se2 Se 0.37834(16) 0.08578(14) 0.41546(11) 0.0483(5) Uani 1 1 d . . . Se3 Se 0.43655(17) 0.12192(14) 0.17895(12) 0.0489(5) Uani 1 1 d . . . Se4 Se 0.63964(16) 0.40020(15) 0.18372(11) 0.0466(5) Uani 1 1 d . . . Se5 Se 0.48087(16) 0.63229(15) 0.20478(11) 0.0470(5) Uani 1 1 d . . . Se6 Se 0.69930(15) 0.66618(13) 0.40521(11) 0.0411(4) Uani 1 1 d . . . Se7 Se 0.36388(15) 0.70552(14) 0.41254(10) 0.0402(4) Uani 1 1 d . . . Se8 Se 0.73434(15) 0.32212(13) 0.39965(10) 0.0387(4) Uani 1 1 d . . . Se9 Se 0.26017(17) 0.27846(15) 0.07510(11) 0.0514(5) Uani 1 1 d . . . Se10 Se 0.12178(18) 0.41735(18) 0.19909(13) 0.0642(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0442(9) 0.0510(9) 0.0574(9) 0.0140(7) 0.0142(7) 0.0100(7) Ag2 0.0651(11) 0.0641(11) 0.0781(12) 0.0319(9) 0.0144(9) 0.0241(9) Ag3 0.0475(9) 0.0468(9) 0.0754(11) 0.0052(7) 0.0040(8) 0.0175(7) Ag4 0.0516(9) 0.0595(9) 0.0556(9) 0.0127(7) 0.0169(7) 0.0218(8) Ag5 0.0564(10) 0.0481(9) 0.0533(9) 0.0150(7) 0.0132(7) 0.0261(7) Ag6 0.0768(12) 0.1098(14) 0.0690(11) 0.0506(10) 0.0368(9) 0.0606(11) C1 0.057(17) 0.090(19) 0.16(3) 0.007(18) 0.064(17) 0.007(14) C2 0.19(4) 0.08(2) 0.16(3) 0.011(19) 0.15(3) 0.01(2) C3 0.062(14) 0.059(13) 0.081(15) 0.029(11) 0.036(12) 0.032(11) C4 0.23(4) 0.09(2) 0.13(3) 0.02(2) -0.01(3) 0.09(3) C5 0.068(12) 0.124(15) 0.125(14) 0.050(11) 0.062(11) 0.070(12) C6 0.09(2) 0.12(2) 0.13(2) 0.037(18) 0.051(17) 0.072(18) C7 0.068(12) 0.124(15) 0.125(14) 0.050(11) 0.062(11) 0.070(12) C8 0.30(5) 0.08(2) 0.13(2) -0.006(18) -0.02(3) 0.11(3) C9 0.09(2) 0.14(2) 0.075(18) 0.030(17) 0.048(16) 0.020(19) C10 0.10(3) 0.27(5) 0.064(19) 0.03(2) 0.031(18) -0.01(3) C11 0.080(17) 0.074(16) 0.113(19) 0.038(13) 0.059(14) 0.062(14) C12 0.073(17) 0.044(13) 0.18(3) 0.003(14) 0.078(18) 0.023(12) C13 0.038(11) 0.098(16) 0.057(13) 0.028(11) 0.015(9) 0.042(11) C14 0.031(11) 0.101(17) 0.068(14) 0.023(12) 0.018(9) 0.031(11) C15 0.048(12) 0.061(13) 0.055(12) 0.028(10) 0.017(9) 0.007(10) C16 0.098(19) 0.035(12) 0.071(15) 0.012(10) 0.014(13) 0.004(11) C17 0.056(11) 0.107(15) 0.102(14) 0.010(10) 0.017(10) 0.037(11) C18 0.10(2) 0.076(18) 0.076(18) -0.035(14) -0.012(15) -0.021(16) C19 0.056(11) 0.107(15) 0.102(14) 0.010(10) 0.017(10) 0.037(11) C20 0.10(2) 0.17(3) 0.11(2) 0.072(19) 0.058(18) 0.08(2) I1 0.0410(7) 0.0363(6) 0.0451(7) 0.0149(5) 0.0143(5) 0.0175(5) O1 0.037(7) 0.051(7) 0.073(9) 0.017(6) 0.044(6) 0.021(6) O2 0.043(7) 0.031(6) 0.062(8) 0.011(5) 0.021(6) 0.026(6) O3 0.054(6) 0.082(7) 0.073(7) 0.007(5) 0.023(5) 0.029(6) O4 0.054(6) 0.082(7) 0.073(7) 0.007(5) 0.023(5) 0.029(6) O5 0.029(7) 0.088(10) 0.072(9) 0.032(8) 0.028(6) 0.014(7) O6 0.056(9) 0.036(7) 0.086(10) 0.019(7) 0.024(7) 0.011(6) O7 0.045(7) 0.067(8) 0.039(7) 0.023(6) 0.010(5) 0.039(7) O8 0.043(7) 0.024(6) 0.050(7) 0.005(5) 0.014(6) 0.000(5) O9 0.059(7) 0.077(8) 0.112(9) 0.009(6) 0.010(6) 0.028(6) O10 0.059(7) 0.077(8) 0.112(9) 0.009(6) 0.010(6) 0.028(6) P1 0.041(3) 0.027(2) 0.050(3) 0.008(2) 0.015(2) 0.006(2) P2 0.041(3) 0.051(3) 0.046(3) 0.002(2) 0.015(2) 0.024(2) P3 0.049(3) 0.036(3) 0.049(3) 0.017(2) 0.016(2) 0.011(2) P4 0.027(2) 0.037(2) 0.040(2) 0.0124(19) 0.0116(18) 0.0162(19) P5 0.038(3) 0.044(3) 0.051(3) 0.007(2) -0.001(2) 0.018(2) Se1 0.0482(12) 0.0461(12) 0.0919(16) 0.0191(11) 0.0182(11) 0.0244(10) Se2 0.0466(11) 0.0420(10) 0.0455(11) 0.0100(8) 0.0086(8) 0.0088(9) Se3 0.0481(12) 0.0411(11) 0.0525(12) 0.0030(8) 0.0141(9) 0.0168(9) Se4 0.0457(11) 0.0472(11) 0.0481(11) 0.0134(8) 0.0184(9) 0.0172(9) Se5 0.0463(11) 0.0459(11) 0.0519(11) 0.0242(8) 0.0129(9) 0.0177(9) Se6 0.0376(10) 0.0373(10) 0.0461(10) 0.0093(8) 0.0101(8) 0.0146(8) Se7 0.0348(10) 0.0427(10) 0.0429(10) 0.0155(8) 0.0110(8) 0.0139(8) Se8 0.0361(10) 0.0441(10) 0.0401(10) 0.0115(8) 0.0135(7) 0.0196(8) Se9 0.0457(11) 0.0541(12) 0.0450(11) 0.0033(9) 0.0003(8) 0.0216(9) Se10 0.0400(12) 0.0744(15) 0.0663(14) 0.0022(11) 0.0162(10) 0.0167(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 Se2 2.584(2) . ? Ag1 Se3 2.639(2) . ? Ag1 Se8 2.642(2) . ? Ag1 Ag5 3.175(2) . ? Ag1 Ag2 3.220(2) . ? Ag1 Ag6 3.340(2) . ? Ag2 Se1 2.580(3) . ? Ag2 Se9 2.644(2) . ? Ag2 Se3 2.755(2) . ? Ag2 I1 2.953(2) . ? Ag2 Ag3 3.135(2) . ? Ag3 Se9 2.575(2) . ? Ag3 Se5 2.593(2) . ? Ag3 Se4 2.605(2) . ? Ag3 Ag4 3.161(2) . ? Ag3 Ag5 3.188(2) . ? Ag4 Se10 2.588(3) . ? Ag4 Se7 2.658(2) . ? Ag4 Se5 2.670(2) . ? Ag4 I1 2.9771(18) . ? Ag5 Se4 2.684(2) . ? Ag5 Se8 2.694(2) . ? Ag5 Se6 2.699(2) . ? Ag5 I1 2.8999(19) . ? Ag6 Se6 2.638(2) 2_666 ? Ag6 Se7 2.651(2) 2_666 ? Ag6 I1 2.8377(18) . ? Ag6 Se2 2.863(3) . ? C1 O1 1.39(2) . ? C1 C2 1.43(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 O2 1.38(2) . ? C3 C4 1.53(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O3 1.423(9) . ? C5 C6 1.58(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 O4 1.31(2) . ? C7 C8 1.525(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.39(4) . ? C9 O5 1.45(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O6 1.48(2) . ? C11 C12 1.51(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O7 1.46(2) . ? C13 C14 1.54(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.52(2) . ? C15 O8 1.53(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.39(3) . ? C17 O9 1.411(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O10 1.41(3) . ? C19 C20 1.53(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O1 P1 1.591(12) . ? O2 P1 1.547(11) . ? O3 P2 1.603(14) . ? O4 P2 1.550(14) . ? O5 P3 1.622(12) . ? O6 P3 1.567(12) . ? O7 P4 1.553(11) . ? O8 P4 1.558(11) . ? O9 P5 1.553(16) . ? O10 P5 1.553(18) . ? P1 Se1 2.114(5) . ? P1 Se2 2.176(5) . ? P2 Se3 2.145(5) . ? P2 Se4 2.178(5) . ? P3 Se6 2.141(5) . ? P3 Se5 2.170(5) . ? P4 Se8 2.152(4) 2_666 ? P4 Se7 2.154(4) . ? P5 Se10 2.121(5) . ? P5 Se9 2.180(5) . ? Se6 Ag6 2.638(2) 2_666 ? Se7 Ag6 2.651(2) 2_666 ? Se8 P4 2.152(4) 2_666 ? 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 Se2 Ag1 Se3 111.25(8) . . ? Se2 Ag1 Se8 128.42(8) . . ? Se3 Ag1 Se8 112.47(8) . . ? Se2 Ag1 Ag5 141.87(7) . . ? Se3 Ag1 Ag5 97.02(7) . . ? Se8 Ag1 Ag5 54.26(5) . . ? Se2 Ag1 Ag2 92.83(7) . . ? Se3 Ag1 Ag2 55.03(6) . . ? Se8 Ag1 Ag2 134.92(7) . . ? Ag5 Ag1 Ag2 82.63(5) . . ? Se2 Ag1 Ag6 56.07(6) . . ? Se3 Ag1 Ag6 144.94(7) . . ? Se8 Ag1 Ag6 97.70(7) . . ? Ag5 Ag1 Ag6 86.07(5) . . ? Ag2 Ag1 Ag6 91.12(6) . . ? Se1 Ag2 Se9 123.18(9) . . ? Se1 Ag2 Se3 112.18(8) . . ? Se9 Ag2 Se3 94.73(8) . . ? Se1 Ag2 I1 98.79(8) . . ? Se9 Ag2 I1 117.06(7) . . ? Se3 Ag2 I1 111.38(7) . . ? Se1 Ag2 Ag3 158.61(8) . . ? Se9 Ag2 Ag3 52.09(6) . . ? Se3 Ag2 Ag3 89.20(7) . . ? I1 Ag2 Ag3 71.43(5) . . ? Se1 Ag2 Ag1 98.83(7) . . ? Se9 Ag2 Ag1 135.33(8) . . ? Se3 Ag2 Ag1 51.70(6) . . ? I1 Ag2 Ag1 64.50(5) . . ? Ag3 Ag2 Ag1 93.98(6) . . ? Se9 Ag3 Se5 121.53(8) . . ? Se9 Ag3 Se4 117.52(8) . . ? Se5 Ag3 Se4 113.01(8) . . ? Se9 Ag3 Ag2 54.08(6) . . ? Se5 Ag3 Ag2 136.69(8) . . ? Se4 Ag3 Ag2 102.49(7) . . ? Se9 Ag3 Ag4 96.42(7) . . ? Se5 Ag3 Ag4 54.22(6) . . ? Se4 Ag3 Ag4 141.68(8) . . ? Ag2 Ag3 Ag4 82.56(6) . . ? Se9 Ag3 Ag5 135.90(8) . . ? Se5 Ag3 Ag5 97.19(6) . . ? Se4 Ag3 Ag5 54.09(5) . . ? Ag2 Ag3 Ag5 83.78(6) . . ? Ag4 Ag3 Ag5 89.53(6) . . ? Se10 Ag4 Se7 117.12(8) . . ? Se10 Ag4 Se5 118.36(8) . . ? Se7 Ag4 Se5 104.79(8) . . ? Se10 Ag4 I1 103.21(8) . . ? Se7 Ag4 I1 102.52(6) . . ? Se5 Ag4 I1 109.58(7) . . ? Se10 Ag4 Ag3 95.90(7) . . ? Se7 Ag4 Ag3 146.82(8) . . ? Se5 Ag4 Ag3 51.98(5) . . ? I1 Ag4 Ag3 70.76(5) . . ? Se4 Ag5 Se8 97.37(7) . . ? Se4 Ag5 Se6 112.31(7) . . ? Se8 Ag5 Se6 128.23(8) . . ? Se4 Ag5 I1 118.40(7) . . ? Se8 Ag5 I1 109.85(6) . . ? Se6 Ag5 I1 92.49(6) . . ? Se4 Ag5 Ag1 94.02(6) . . ? Se8 Ag5 Ag1 52.73(5) . . ? Se6 Ag5 Ag1 152.05(7) . . ? I1 Ag5 Ag1 65.66(5) . . ? Se4 Ag5 Ag3 51.81(6) . . ? Se8 Ag5 Ag3 135.66(7) . . ? Se6 Ag5 Ag3 95.26(6) . . ? I1 Ag5 Ag3 71.33(5) . . ? Ag1 Ag5 Ag3 93.86(5) . . ? Se6 Ag6 Se7 119.77(8) 2_666 2_666 ? Se6 Ag6 I1 107.40(7) 2_666 . ? Se7 Ag6 I1 124.51(8) 2_666 . ? Se6 Ag6 Se2 116.25(9) 2_666 . ? Se7 Ag6 Se2 85.72(7) 2_666 . ? I1 Ag6 Se2 98.89(7) . . ? Se6 Ag6 Ag1 156.04(9) 2_666 . ? Se7 Ag6 Ag1 80.61(6) 2_666 . ? I1 Ag6 Ag1 64.01(5) . . ? Se2 Ag6 Ag1 48.49(5) . . ? O1 C1 C2 111(2) . . ? O1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? O1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 C4 112.3(18) . . ? O2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? O2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 109.6(17) . . ? O3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C8 117(2) . . ? O4 C7 H7A 108.1 . . ? C8 C7 H7A 108.1 . . ? O4 C7 H7B 108.1 . . ? C8 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 O5 109(2) . . ? C10 C9 H9A 110.0 . . ? O5 C9 H9A 110.0 . . ? C10 C9 H9B 110.0 . . ? O5 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 107.0(16) . . ? O6 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? O6 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 C14 107.3(15) . . ? O7 C13 H13A 110.3 . . ? C14 C13 H13A 110.3 . . ? O7 C13 H13B 110.3 . . ? C14 C13 H13B 110.3 . . ? H13A C13 H13B 108.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 O8 103.6(15) . . ? C16 C15 H15A 111.0 . . ? O8 C15 H15A 111.0 . . ? C16 C15 H15B 111.0 . . ? O8 C15 H15B 111.0 . . ? H15A C15 H15B 109.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 O9 120(2) . . ? C18 C17 H17A 107.4 . . ? O9 C17 H17A 107.4 . . ? C18 C17 H17B 107.4 . . ? O9 C17 H17B 107.4 . . ? H17A C17 H17B 106.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O10 C19 C20 111(2) . . ? O10 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? O10 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Ag6 I1 Ag5 101.64(6) . . ? Ag6 I1 Ag2 107.98(6) . . ? Ag5 I1 Ag2 92.33(5) . . ? Ag6 I1 Ag4 152.54(6) . . ? Ag5 I1 Ag4 99.04(5) . . ? Ag2 I1 Ag4 88.93(5) . . ? C1 O1 P1 119.1(13) . . ? C3 O2 P1 122.4(12) . . ? C5 O3 P2 125.8(14) . . ? C7 O4 P2 119.7(13) . . ? C9 O5 P3 123.0(15) . . ? C11 O6 P3 120.5(12) . . ? C13 O7 P4 119.6(9) . . ? C15 O8 P4 121.2(10) . . ? C17 O9 P5 133.8(16) . . ? C19 O10 P5 120.5(15) . . ? O2 P1 O1 100.6(6) . . ? O2 P1 Se1 107.1(5) . . ? O1 P1 Se1 110.3(5) . . ? O2 P1 Se2 110.4(5) . . ? O1 P1 Se2 104.8(5) . . ? Se1 P1 Se2 121.7(2) . . ? O4 P2 O3 100.8(7) . . ? O4 P2 Se3 111.4(6) . . ? O3 P2 Se3 104.2(5) . . ? O4 P2 Se4 108.1(6) . . ? O3 P2 Se4 109.5(5) . . ? Se3 P2 Se4 121.0(2) . . ? O6 P3 O5 101.8(7) . . ? O6 P3 Se6 111.2(6) . . ? O5 P3 Se6 101.9(5) . . ? O6 P3 Se5 108.4(6) . . ? O5 P3 Se5 110.1(5) . . ? Se6 P3 Se5 121.6(2) . . ? O7 P4 O8 105.8(7) . . ? O7 P4 Se8 104.4(4) . 2_666 ? O8 P4 Se8 112.4(5) . 2_666 ? O7 P4 Se7 108.1(5) . . ? O8 P4 Se7 106.9(5) . . ? Se8 P4 Se7 118.5(2) 2_666 . ? O9 P5 O10 98.0(9) . . ? O9 P5 Se10 105.0(7) . . ? O10 P5 Se10 113.5(6) . . ? O9 P5 Se9 108.3(6) . . ? O10 P5 Se9 109.9(6) . . ? Se10 P5 Se9 119.6(2) . . ? P1 Se1 Ag2 98.23(15) . . ? P1 Se2 Ag1 101.34(14) . . ? P1 Se2 Ag6 117.84(14) . . ? Ag1 Se2 Ag6 75.44(7) . . ? P2 Se3 Ag1 98.30(14) . . ? P2 Se3 Ag2 114.16(14) . . ? Ag1 Se3 Ag2 73.27(6) . . ? P2 Se4 Ag3 104.13(14) . . ? P2 Se4 Ag5 104.47(14) . . ? Ag3 Se4 Ag5 74.10(7) . . ? P3 Se5 Ag3 102.54(14) . . ? P3 Se5 Ag4 108.89(14) . . ? Ag3 Se5 Ag4 73.80(7) . . ? P3 Se6 Ag6 105.69(15) . 2_666 ? P3 Se6 Ag5 100.98(14) . . ? Ag6 Se6 Ag5 108.91(8) 2_666 . ? P4 Se7 Ag6 109.33(13) . 2_666 ? P4 Se7 Ag4 101.63(13) . . ? Ag6 Se7 Ag4 89.21(7) 2_666 . ? P4 Se8 Ag1 104.06(13) 2_666 . ? P4 Se8 Ag5 103.79(12) 2_666 . ? Ag1 Se8 Ag5 73.01(6) . . ? P5 Se9 Ag3 106.09(15) . . ? P5 Se9 Ag2 101.73(16) . . ? Ag3 Se9 Ag2 73.83(7) . . ? P5 Se10 Ag4 107.65(16) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.794 _refine_diff_density_min -1.862 _refine_diff_density_rms 0.250 _database_code_depnum_ccdc_archive 'CCDC 931692'