# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpd1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(diphenyltellane)silver trifluoromethylsulfonate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H30 Ag F3 O3 S Te3' _chemical_formula_weight 1102.34 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' F F 0.0171 0.0103 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.225(2) _cell_length_b 16.727(3) _cell_length_c 21.626(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3698.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6877 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 2.971 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5880 _exptl_absorpt_correction_T_max 0.7555 _exptl_absorpt_process_details 'SADABS in SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius Kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29635 _diffrn_reflns_av_R_equivalents 0.1333 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7266 _reflns_number_gt 6877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker, 2008)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Branderburg, 2006)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0550P)^2^+7.3972P] 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 SHELXL _refine_ls_extinction_coef 0.0070(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 7266 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.44854(5) 0.00002(3) 0.57641(2) 0.02345(14) Uani 1 1 d . . . Te1 Te 0.23503(4) 0.04932(3) 0.50972(2) 0.02135(13) Uani 1 1 d . . . Te2 Te 0.45486(5) -0.14207(3) 0.63875(2) 0.02439(13) Uani 1 1 d . . . Te3 Te 0.60946(4) 0.12104(3) 0.61565(2) 0.02397(13) Uani 1 1 d . . . S1 S 0.59660(19) -0.03433(11) 0.43688(8) 0.0276(4) Uani 1 1 d . . . F1 F 0.4332(7) -0.1317(6) 0.3829(3) 0.097(3) Uani 1 1 d . . . F2 F 0.5677(8) -0.0741(5) 0.3220(2) 0.075(2) Uani 1 1 d . . . F3 F 0.6326(8) -0.1693(3) 0.3786(3) 0.0658(18) Uani 1 1 d . . . O1 O 0.5800(6) -0.0795(4) 0.4932(2) 0.0394(14) Uani 1 1 d . . . O2 O 0.5041(8) 0.0274(5) 0.4279(3) 0.064(2) Uani 1 1 d . . . O3 O 0.7291(6) -0.0131(3) 0.4223(3) 0.0405(14) Uani 1 1 d . . . C1 C 0.5571(11) -0.1071(7) 0.3778(4) 0.050(2) Uani 1 1 d . . . C111 C 0.1314(7) -0.0610(4) 0.5042(3) 0.0225(14) Uani 1 1 d . . . C112 C -0.0029(7) -0.0621(4) 0.4964(3) 0.0247(14) Uani 1 1 d . . . H11 H -0.0498 -0.0132 0.4929 0.030 Uiso 1 1 calc R . . C113 C -0.0684(7) -0.1333(4) 0.4939(3) 0.0273(15) Uani 1 1 d . . . H113 H -0.1607 -0.1337 0.4890 0.033 Uiso 1 1 calc R . . C114 C -0.0007(9) -0.2054(5) 0.4984(3) 0.0346(18) Uani 1 1 d . . . H114 H -0.0469 -0.2547 0.4975 0.042 Uiso 1 1 calc R . . C115 C 0.1332(8) -0.2047(5) 0.5041(4) 0.0359(18) Uani 1 1 d . . . H115 H 0.1799 -0.2538 0.5060 0.043 Uiso 1 1 calc R . . C116 C 0.2012(7) -0.1322(4) 0.5071(4) 0.0303(16) Uani 1 1 d . . . H116 H 0.2937 -0.1317 0.5111 0.036 Uiso 1 1 calc R . . C121 C 0.1383(7) 0.0956(4) 0.5901(3) 0.0251(15) Uani 1 1 d . . . C122 C 0.0774(9) 0.0468(5) 0.6315(4) 0.0387(19) Uani 1 1 d . . . H122 H 0.0717 -0.0091 0.6243 0.046 Uiso 1 1 calc R . . C123 C 0.0245(11) 0.0799(6) 0.6839(4) 0.053(3) Uani 1 1 d . . . H123 H -0.0189 0.0463 0.7127 0.063 Uiso 1 1 calc R . . C124 C 0.0330(10) 0.1607(5) 0.6956(4) 0.042(2) Uani 1 1 d . . . H124 H -0.0010 0.1824 0.7328 0.050 Uiso 1 1 calc R . . C125 C 0.0916(8) 0.2096(5) 0.6523(4) 0.0370(18) Uani 1 1 d . . . H125 H 0.0957 0.2656 0.6590 0.044 Uiso 1 1 calc R . . C126 C 0.1448(7) 0.1770(5) 0.5988(4) 0.0280(15) Uani 1 1 d . . . H126 H 0.1849 0.2104 0.5687 0.034 Uiso 1 1 calc R . . C211 C 0.6442(7) -0.1332(4) 0.6787(3) 0.0281(15) Uani 1 1 d . . . C212 C 0.7493(8) -0.1514(6) 0.6414(4) 0.0397(19) Uani 1 1 d . . . H212 H 0.7351 -0.1672 0.5998 0.048 Uiso 1 1 calc R . . C213 C 0.8773(8) -0.1467(7) 0.6648(4) 0.045(2) Uani 1 1 d . . . H213 H 0.9497 -0.1593 0.6390 0.055 Uiso 1 1 calc R . . C214 C 0.8971(8) -0.1239(5) 0.7247(4) 0.0395(19) Uani 1 1 d . . . H214 H 0.9836 -0.1210 0.7406 0.047 Uiso 1 1 calc R . . C215 C 0.7933(9) -0.1051(5) 0.7622(4) 0.0388(19) Uani 1 1 d . . . H215 H 0.8087 -0.0887 0.8036 0.047 Uiso 1 1 calc R . . C216 C 0.6621(8) -0.1099(5) 0.7395(4) 0.0325(17) Uani 1 1 d . . . H216 H 0.5898 -0.0975 0.7653 0.039 Uiso 1 1 calc R . . C221 C 0.3421(6) -0.1272(4) 0.7200(3) 0.0213(13) Uani 1 1 d . . . C222 C 0.3165(9) -0.0543(5) 0.7463(4) 0.042(2) Uani 1 1 d . . . H222 H 0.3495 -0.0070 0.7276 0.051 Uiso 1 1 calc R . . C223 C 0.2431(9) -0.0490(6) 0.7997(5) 0.049(2) Uani 1 1 d . . . H223 H 0.2254 0.0019 0.8174 0.058 Uiso 1 1 calc R . . C224 C 0.1953(7) -0.1173(6) 0.8276(4) 0.0369(18) Uani 1 1 d . . . H224 H 0.1450 -0.1137 0.8645 0.044 Uiso 1 1 calc R . . C225 C 0.2211(8) -0.1905(5) 0.8016(4) 0.0356(18) Uani 1 1 d . . . H225 H 0.1882 -0.2375 0.8208 0.043 Uiso 1 1 calc R . . C46 C 0.2934(7) -0.1969(4) 0.7488(4) 0.0281(16) Uani 1 1 d . . . H226 H 0.3107 -0.2480 0.7315 0.034 Uiso 1 1 calc R . . C311 C 0.5326(7) 0.1265(4) 0.7068(3) 0.0255(14) Uani 1 1 d . . . C312 C 0.6082(8) 0.0960(4) 0.7552(4) 0.0304(16) Uani 1 1 d . . . H312 H 0.6922 0.0743 0.7469 0.036 Uiso 1 1 calc R . . C313 C 0.5609(9) 0.0974(5) 0.8151(3) 0.0347(18) Uani 1 1 d . . . H313 H 0.6116 0.0754 0.8477 0.042 Uiso 1 1 calc R . . C314 C 0.4413(10) 0.1304(5) 0.8273(4) 0.0378(19) Uani 1 1 d . . . H314 H 0.4112 0.1336 0.8688 0.045 Uiso 1 1 calc R . . C315 C 0.3634(8) 0.1594(4) 0.7795(4) 0.0322(17) Uani 1 1 d . . . H315 H 0.2794 0.1808 0.7883 0.039 Uiso 1 1 calc R . . C316 C 0.4088(7) 0.1570(4) 0.7188(3) 0.0266(15) Uani 1 1 d . . . H316 H 0.3556 0.1760 0.6859 0.032 Uiso 1 1 calc R . . C321 C 0.5045(7) 0.2182(4) 0.5761(3) 0.0242(14) Uani 1 1 d . . . C322 C 0.4775(7) 0.2869(4) 0.6100(4) 0.0293(16) Uani 1 1 d . . . H322 H 0.5075 0.2915 0.6514 0.035 Uiso 1 1 calc R . . C323 C 0.4067(8) 0.3489(4) 0.5835(4) 0.0307(16) Uani 1 1 d . . . H323 H 0.3884 0.3960 0.6065 0.037 Uiso 1 1 calc R . . C324 C 0.3622(7) 0.3414(5) 0.5220(4) 0.0290(16) Uani 1 1 d . . . H324 H 0.3123 0.3832 0.5039 0.035 Uiso 1 1 calc R . . C325 C 0.3908(8) 0.2735(4) 0.4880(3) 0.0285(15) Uani 1 1 d . . . H325 H 0.3614 0.2691 0.4465 0.034 Uiso 1 1 calc R . . C326 C 0.4629(7) 0.2113(4) 0.5147(3) 0.0256(14) Uani 1 1 d . . . H326 H 0.4835 0.1649 0.4913 0.031 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 0.0255(3) 0.0233(3) 0.0215(2) 0.00070(19) -0.0013(2) -0.0003(2) Te1 0.0230(2) 0.0214(2) 0.0196(2) 0.00027(16) -0.00005(17) 0.00025(17) Te2 0.0318(2) 0.0212(2) 0.0201(2) 0.00006(16) 0.00037(19) 0.00057(18) Te3 0.0215(2) 0.0231(2) 0.0272(2) 0.00044(17) -0.00255(18) 0.00027(18) S1 0.0296(9) 0.0306(9) 0.0226(8) -0.0009(7) 0.0033(7) 0.0098(8) F1 0.066(4) 0.157(8) 0.069(5) -0.001(5) -0.014(4) -0.062(5) F2 0.103(5) 0.102(5) 0.020(3) 0.004(3) -0.009(3) -0.018(5) F3 0.111(5) 0.035(3) 0.052(4) -0.018(3) 0.021(4) -0.015(3) O1 0.049(3) 0.049(3) 0.020(3) -0.001(2) 0.010(2) 0.012(3) O2 0.070(5) 0.066(5) 0.056(4) 0.022(3) 0.023(4) 0.050(4) O3 0.037(3) 0.031(3) 0.054(4) -0.003(3) 0.000(3) -0.008(3) C1 0.055(5) 0.064(6) 0.031(4) -0.002(4) -0.003(4) -0.023(5) C111 0.027(3) 0.021(3) 0.020(3) 0.005(3) 0.002(3) -0.001(3) C112 0.025(3) 0.023(3) 0.025(4) -0.001(3) -0.001(3) 0.004(3) C113 0.025(3) 0.032(4) 0.025(3) -0.005(3) -0.003(3) -0.001(3) C114 0.050(5) 0.032(4) 0.022(4) -0.007(3) -0.008(3) -0.009(3) C115 0.037(4) 0.031(4) 0.040(5) -0.006(3) -0.009(4) 0.013(3) C116 0.029(4) 0.027(4) 0.035(4) -0.008(3) -0.012(3) 0.005(3) C121 0.029(4) 0.018(3) 0.028(4) 0.001(3) -0.002(3) 0.001(3) C122 0.060(5) 0.025(4) 0.031(4) 0.003(3) 0.014(4) -0.001(4) C123 0.077(7) 0.042(5) 0.039(5) 0.004(4) 0.025(5) 0.005(5) C124 0.060(6) 0.040(5) 0.025(4) -0.004(3) 0.011(4) 0.009(4) C125 0.036(4) 0.035(4) 0.041(5) -0.010(3) -0.005(4) 0.002(4) C126 0.025(3) 0.024(4) 0.035(4) -0.004(3) -0.001(3) -0.001(3) C211 0.035(4) 0.024(4) 0.025(4) 0.001(3) 0.003(3) 0.001(3) C212 0.035(4) 0.055(5) 0.029(4) -0.006(4) 0.004(4) 0.007(4) C213 0.027(4) 0.068(6) 0.042(5) 0.006(4) -0.002(4) -0.001(4) C214 0.035(4) 0.034(4) 0.050(5) 0.005(4) -0.011(4) -0.005(4) C215 0.049(5) 0.033(4) 0.035(4) -0.001(3) -0.021(4) 0.002(4) C216 0.038(4) 0.030(4) 0.030(4) 0.004(3) 0.001(3) 0.008(3) C221 0.022(3) 0.024(3) 0.018(3) 0.003(3) 0.001(3) -0.007(3) C222 0.055(5) 0.024(4) 0.048(5) -0.007(4) 0.017(4) -0.013(4) C223 0.044(5) 0.049(5) 0.054(5) -0.027(4) 0.026(4) -0.016(4) C224 0.025(4) 0.058(5) 0.028(4) -0.005(4) -0.004(3) 0.000(4) C225 0.028(4) 0.046(5) 0.033(4) 0.018(4) 0.000(3) 0.006(3) C46 0.028(3) 0.023(3) 0.034(4) 0.002(3) -0.007(3) 0.005(3) C311 0.033(4) 0.022(3) 0.022(3) 0.004(3) -0.008(3) -0.001(3) C312 0.030(4) 0.025(4) 0.036(4) 0.004(3) -0.007(3) -0.004(3) C313 0.047(5) 0.036(4) 0.021(4) 0.008(3) -0.016(4) -0.006(4) C314 0.061(5) 0.031(4) 0.022(4) -0.005(3) -0.006(4) -0.009(4) C315 0.046(5) 0.023(4) 0.028(4) 0.003(3) 0.009(3) -0.003(3) C316 0.029(4) 0.027(4) 0.024(4) 0.003(3) -0.005(3) 0.004(3) C321 0.019(3) 0.025(3) 0.029(4) 0.001(3) -0.002(3) -0.006(3) C322 0.036(4) 0.024(4) 0.028(4) 0.004(3) -0.008(3) -0.006(3) C323 0.037(4) 0.024(4) 0.031(4) 0.004(3) -0.002(3) -0.001(3) C324 0.022(3) 0.032(4) 0.033(4) 0.011(3) -0.008(3) -0.005(3) C325 0.033(4) 0.033(4) 0.020(3) 0.005(3) -0.001(3) -0.002(3) C326 0.026(3) 0.031(4) 0.020(3) 0.002(3) 0.001(3) -0.002(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 Te2 2.7333(8) . ? Ag1 Te1 2.7433(8) . ? Ag1 Te3 2.7432(8) . ? Te1 C111 2.132(7) . ? Te1 C121 2.143(7) . ? Te2 C221 2.117(7) . ? Te2 C211 2.125(8) . ? Te3 C311 2.124(7) . ? Te3 C321 2.127(7) . ? S1 O2 1.414(7) . ? S1 O3 1.435(6) . ? S1 O1 1.444(6) . ? S1 C1 1.811(10) . ? F1 C1 1.337(12) . ? F2 C1 1.331(11) . ? F3 C1 1.295(13) . ? C111 C116 1.390(10) . ? C111 C112 1.384(10) . ? C112 C113 1.368(10) . ? C112 H11 0.9500 . ? C113 C114 1.394(11) . ? C113 H113 0.9500 . ? C114 C115 1.375(12) . ? C114 H114 0.9500 . ? C115 C116 1.399(11) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.363(11) . ? C121 C126 1.377(10) . ? C122 C123 1.370(12) . ? C122 H122 0.9500 . ? C123 C124 1.378(13) . ? C123 H123 0.9500 . ? C124 C125 1.381(13) . ? C124 H124 0.9500 . ? C125 C126 1.389(11) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C211 C212 1.377(11) . ? C211 C216 1.384(11) . ? C212 C213 1.405(12) . ? C212 H212 0.9500 . ? C213 C214 1.366(13) . ? C213 H213 0.9500 . ? C214 C215 1.372(13) . ? C214 H214 0.9500 . ? C215 C216 1.430(12) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.371(11) . ? C221 C46 1.411(10) . ? C222 C223 1.381(12) . ? C222 H222 0.9500 . ? C223 C224 1.382(13) . ? C223 H223 0.9500 . ? C224 C225 1.371(13) . ? C224 H224 0.9500 . ? C225 C46 1.365(12) . ? C225 H225 0.9500 . ? C46 H226 0.9500 . ? C311 C316 1.389(10) . ? C311 C312 1.396(10) . ? C312 C313 1.383(11) . ? C312 H312 0.9500 . ? C313 C314 1.368(13) . ? C313 H313 0.9500 . ? C314 C315 1.392(12) . ? C314 H314 0.9500 . ? C315 C316 1.394(11) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? C321 C322 1.391(11) . ? C321 C326 1.400(10) . ? C322 C323 1.389(11) . ? C322 H322 0.9500 . ? C323 C324 1.410(11) . ? C323 H323 0.9500 . ? C324 C325 1.386(11) . ? C324 H324 0.9500 . ? C325 C326 1.399(10) . ? C325 H325 0.9500 . ? C326 H326 0.9500 . ? 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 Te2 Ag1 Te1 122.65(2) . . ? Te2 Ag1 Te3 118.35(2) . . ? Te1 Ag1 Te3 114.72(2) . . ? C111 Te1 C121 97.4(3) . . ? C111 Te1 Ag1 99.48(18) . . ? C121 Te1 Ag1 92.84(19) . . ? C221 Te2 C211 98.7(3) . . ? C221 Te2 Ag1 107.15(19) . . ? C211 Te2 Ag1 99.3(2) . . ? C311 Te3 C321 98.8(3) . . ? C311 Te3 Ag1 95.6(2) . . ? C321 Te3 Ag1 97.86(19) . . ? O2 S1 O3 114.9(5) . . ? O2 S1 O1 114.8(4) . . ? O3 S1 O1 115.2(4) . . ? O2 S1 C1 104.2(5) . . ? O3 S1 C1 102.8(4) . . ? O1 S1 C1 102.6(4) . . ? F3 C1 F1 108.5(9) . . ? F3 C1 F2 107.3(9) . . ? F1 C1 F2 106.2(9) . . ? F3 C1 S1 113.4(7) . . ? F1 C1 S1 111.1(8) . . ? F2 C1 S1 110.0(7) . . ? C116 C111 C112 120.3(7) . . ? C116 C111 Te1 119.0(5) . . ? C112 C111 Te1 120.7(5) . . ? C113 C112 C111 120.1(7) . . ? C113 C112 H11 120.0 . . ? C111 C112 H11 120.0 . . ? C112 C113 C114 120.6(7) . . ? C112 C113 H113 119.7 . . ? C114 C113 H113 119.7 . . ? C115 C114 C113 119.5(8) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C114 C115 C116 120.4(8) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C111 C116 C115 119.1(7) . . ? C111 C116 H116 120.5 . . ? C115 C116 H116 120.5 . . ? C122 C121 C126 121.6(7) . . ? C122 C121 Te1 121.9(6) . . ? C126 C121 Te1 116.5(5) . . ? C121 C122 C123 118.8(8) . . ? C121 C122 H122 120.6 . . ? C123 C122 H122 120.6 . . ? C122 C123 C124 121.5(9) . . ? C122 C123 H123 119.2 . . ? C124 C123 H123 119.2 . . ? C125 C124 C123 118.9(8) . . ? C125 C124 H124 120.5 . . ? C123 C124 H124 120.5 . . ? C124 C125 C126 120.2(8) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C121 C126 C125 118.9(8) . . ? C121 C126 H126 120.6 . . ? C125 C126 H126 120.6 . . ? C212 C211 C216 121.0(8) . . ? C212 C211 Te2 117.3(6) . . ? C216 C211 Te2 121.8(6) . . ? C211 C212 C213 120.3(8) . . ? C211 C212 H212 119.8 . . ? C213 C212 H212 119.8 . . ? C212 C213 C214 119.6(8) . . ? C212 C213 H213 120.2 . . ? C214 C213 H213 120.2 . . ? C215 C214 C213 120.7(8) . . ? C215 C214 H214 119.7 . . ? C213 C214 H214 119.7 . . ? C214 C215 C216 120.7(8) . . ? C214 C215 H215 119.7 . . ? C216 C215 H215 119.7 . . ? C211 C216 C215 117.8(8) . . ? C211 C216 H216 121.1 . . ? C215 C216 H216 121.1 . . ? C222 C221 C46 119.0(7) . . ? C222 C221 Te2 123.5(5) . . ? C46 C221 Te2 117.5(5) . . ? C221 C222 C223 120.5(8) . . ? C221 C222 H222 119.8 . . ? C223 C222 H222 119.8 . . ? C222 C223 C224 120.3(8) . . ? C222 C223 H223 119.9 . . ? C224 C223 H223 119.9 . . ? C225 C224 C223 119.4(8) . . ? C225 C224 H224 120.3 . . ? C223 C224 H224 120.3 . . ? C46 C225 C224 121.1(8) . . ? C46 C225 H225 119.4 . . ? C224 C225 H225 119.4 . . ? C225 C46 C221 119.7(7) . . ? C225 C46 H226 120.2 . . ? C221 C46 H226 120.2 . . ? C316 C311 C312 120.0(7) . . ? C316 C311 Te3 121.7(5) . . ? C312 C311 Te3 118.3(6) . . ? C313 C312 C311 120.1(8) . . ? C313 C312 H312 119.9 . . ? C311 C312 H312 119.9 . . ? C314 C313 C312 120.0(7) . . ? C314 C313 H313 120.0 . . ? C312 C313 H313 120.0 . . ? C313 C314 C315 120.6(7) . . ? C313 C314 H314 119.7 . . ? C315 C314 H314 119.7 . . ? C316 C315 C314 120.0(8) . . ? C316 C315 H315 120.0 . . ? C314 C315 H315 120.0 . . ? C311 C316 C315 119.3(7) . . ? C311 C316 H316 120.4 . . ? C315 C316 H316 120.4 . . ? C322 C321 C326 120.6(7) . . ? C322 C321 Te3 121.3(5) . . ? C326 C321 Te3 118.1(5) . . ? C323 C322 C321 120.2(7) . . ? C323 C322 H322 119.9 . . ? C321 C322 H322 119.9 . . ? C322 C323 C324 119.4(7) . . ? C322 C323 H323 120.3 . . ? C324 C323 H323 120.3 . . ? C325 C324 C323 120.4(7) . . ? C325 C324 H324 119.8 . . ? C323 C324 H324 119.8 . . ? C324 C325 C326 120.1(7) . . ? C324 C325 H325 119.9 . . ? C326 C325 H325 119.9 . . ? C321 C326 C325 119.3(7) . . ? C321 C326 H326 120.3 . . ? C325 C326 H326 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Te2 Ag1 Te1 C111 -14.95(19) . . . . ? Te3 Ag1 Te1 C111 -171.28(19) . . . . ? Te2 Ag1 Te1 C121 83.05(19) . . . . ? Te3 Ag1 Te1 C121 -73.28(19) . . . . ? Te1 Ag1 Te2 C221 -76.26(19) . . . . ? Te3 Ag1 Te2 C221 79.26(19) . . . . ? Te1 Ag1 Te2 C211 -178.4(2) . . . . ? Te3 Ag1 Te2 C211 -22.9(2) . . . . ? Te2 Ag1 Te3 C311 -58.50(19) . . . . ? Te1 Ag1 Te3 C311 98.92(19) . . . . ? Te2 Ag1 Te3 C321 -158.2(2) . . . . ? Te1 Ag1 Te3 C321 -0.8(2) . . . . ? O2 S1 C1 F3 -179.9(7) . . . . ? O3 S1 C1 F3 59.9(7) . . . . ? O1 S1 C1 F3 -60.0(7) . . . . ? O2 S1 C1 F1 -57.4(9) . . . . ? O3 S1 C1 F1 -177.6(8) . . . . ? O1 S1 C1 F1 62.6(9) . . . . ? O2 S1 C1 F2 59.9(9) . . . . ? O3 S1 C1 F2 -60.3(9) . . . . ? O1 S1 C1 F2 179.8(8) . . . . ? C121 Te1 C111 C116 -121.0(6) . . . . ? Ag1 Te1 C111 C116 -26.9(6) . . . . ? C121 Te1 C111 C112 60.4(6) . . . . ? Ag1 Te1 C111 C112 154.5(6) . . . . ? C116 C111 C112 C113 2.4(11) . . . . ? Te1 C111 C112 C113 -179.0(5) . . . . ? C111 C112 C113 C114 -0.6(11) . . . . ? C112 C113 C114 C115 -1.5(12) . . . . ? C113 C114 C115 C116 1.8(13) . . . . ? C112 C111 C116 C115 -2.0(11) . . . . ? Te1 C111 C116 C115 179.4(6) . . . . ? C114 C115 C116 C111 0.0(12) . . . . ? C111 Te1 C121 C122 22.8(7) . . . . ? Ag1 Te1 C121 C122 -77.2(7) . . . . ? C111 Te1 C121 C126 -159.4(6) . . . . ? Ag1 Te1 C121 C126 100.6(6) . . . . ? C126 C121 C122 C123 -1.7(13) . . . . ? Te1 C121 C122 C123 176.0(8) . . . . ? C121 C122 C123 C124 -0.7(16) . . . . ? C122 C123 C124 C125 2.6(17) . . . . ? C123 C124 C125 C126 -2.0(14) . . . . ? C122 C121 C126 C125 2.2(12) . . . . ? Te1 C121 C126 C125 -175.6(6) . . . . ? C124 C125 C126 C121 -0.3(12) . . . . ? C221 Te2 C211 C212 170.9(6) . . . . ? Ag1 Te2 C211 C212 -80.0(6) . . . . ? C221 Te2 C211 C216 -9.4(7) . . . . ? Ag1 Te2 C211 C216 99.7(6) . . . . ? C216 C211 C212 C213 0.1(13) . . . . ? Te2 C211 C212 C213 179.9(7) . . . . ? C211 C212 C213 C214 0.0(15) . . . . ? C212 C213 C214 C215 -0.4(15) . . . . ? C213 C214 C215 C216 0.8(14) . . . . ? C212 C211 C216 C215 0.2(12) . . . . ? Te2 C211 C216 C215 -179.5(6) . . . . ? C214 C215 C216 C211 -0.7(13) . . . . ? C211 Te2 C221 C222 80.3(7) . . . . ? Ag1 Te2 C221 C222 -22.3(7) . . . . ? C211 Te2 C221 C46 -98.6(6) . . . . ? Ag1 Te2 C221 C46 158.8(5) . . . . ? C46 C221 C222 C223 -0.6(13) . . . . ? Te2 C221 C222 C223 -179.4(7) . . . . ? C221 C222 C223 C224 0.4(15) . . . . ? C222 C223 C224 C225 -0.2(14) . . . . ? C223 C224 C225 C46 0.1(12) . . . . ? C224 C225 C46 C221 -0.3(12) . . . . ? C222 C221 C46 C225 0.5(11) . . . . ? Te2 C221 C46 C225 179.4(6) . . . . ? C321 Te3 C311 C316 27.4(6) . . . . ? Ag1 Te3 C311 C316 -71.4(6) . . . . ? C321 Te3 C311 C312 -154.7(6) . . . . ? Ag1 Te3 C311 C312 106.4(5) . . . . ? C316 C311 C312 C313 -1.2(11) . . . . ? Te3 C311 C312 C313 -179.1(6) . . . . ? C311 C312 C313 C314 -1.6(12) . . . . ? C312 C313 C314 C315 3.1(12) . . . . ? C313 C314 C315 C316 -1.9(12) . . . . ? C312 C311 C316 C315 2.4(11) . . . . ? Te3 C311 C316 C315 -179.8(5) . . . . ? C314 C315 C316 C311 -0.9(11) . . . . ? C311 Te3 C321 C322 36.6(6) . . . . ? Ag1 Te3 C321 C322 133.5(6) . . . . ? C311 Te3 C321 C326 -143.5(6) . . . . ? Ag1 Te3 C321 C326 -46.5(6) . . . . ? C326 C321 C322 C323 1.2(11) . . . . ? Te3 C321 C322 C323 -178.8(6) . . . . ? C321 C322 C323 C324 0.2(11) . . . . ? C322 C323 C324 C325 -1.2(11) . . . . ? C323 C324 C325 C326 0.7(11) . . . . ? C322 C321 C326 C325 -1.7(11) . . . . ? Te3 C321 C326 C325 178.4(5) . . . . ? C324 C325 C326 C321 0.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.043 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.264 _database_code_depnum_ccdc_archive 'CCDC 949145' ####################################################################### # # 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_cmpd2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(diphenyltellane)copper trifluoromethylsulfonate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H30 Cu F3 O3 S Te3' _chemical_formula_weight 1058.01 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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.768(2) _cell_length_b 16.439(3) _cell_length_c 20.769(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3676.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6879 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 26.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 3.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5175 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details 'SADABS in SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32374 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7222 _reflns_number_gt 6879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker, 2008)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Branderburg, 2006)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0352P)^2^+3.1116P] 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 SHELXL _refine_ls_extinction_coef 0.00322(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(18) _refine_ls_number_reflns 7222 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.45573(5) -0.00478(3) 0.56818(3) 0.01999(13) Uani 1 1 d . . . Te1 Te 0.26065(3) 0.041142(19) 0.509250(14) 0.02000(9) Uani 1 1 d . . . Te2 Te 0.46365(3) -0.134608(18) 0.635916(14) 0.02003(9) Uani 1 1 d . . . Te3 Te 0.59827(3) 0.110644(18) 0.605603(15) 0.01952(9) Uani 1 1 d . . . S1 S 0.60813(12) -0.02877(8) 0.43538(6) 0.0247(3) Uani 1 1 d . . . F1 F 0.4595(4) -0.1244(4) 0.3716(2) 0.0879(18) Uani 1 1 d . . . F2 F 0.6092(4) -0.0766(3) 0.31509(16) 0.0497(10) Uani 1 1 d . . . F3 F 0.6436(5) -0.1707(2) 0.38287(19) 0.0654(13) Uani 1 1 d . . . O1 O 0.5652(4) -0.0702(2) 0.49324(17) 0.0317(9) Uani 1 1 d . . . O2 O 0.5327(5) 0.0391(3) 0.4161(2) 0.0587(14) Uani 1 1 d . . . O3 O 0.7388(4) -0.0163(3) 0.4326(2) 0.0437(10) Uani 1 1 d . . . C1 C 0.5786(6) -0.1042(4) 0.3733(3) 0.0381(14) Uani 1 1 d . . . C111 C 0.1525(4) -0.0668(3) 0.5064(2) 0.0203(10) Uani 1 1 d . . . C112 C 0.0246(5) -0.0629(3) 0.5058(3) 0.0286(11) Uani 1 1 d . . . H11 H -0.0163 -0.0117 0.5074 0.034 Uiso 1 1 calc R . . C113 C -0.0439(5) -0.1339(4) 0.5026(3) 0.0335(12) Uani 1 1 d . . . H113 H -0.1321 -0.1315 0.5018 0.040 Uiso 1 1 calc R . . C114 C 0.0156(6) -0.2088(3) 0.5007(3) 0.0373(14) Uani 1 1 d . . . H114 H -0.0317 -0.2576 0.5010 0.045 Uiso 1 1 calc R . . C115 C 0.1430(6) -0.2122(4) 0.4983(3) 0.0396(14) Uani 1 1 d . . . H115 H 0.1834 -0.2633 0.4941 0.048 Uiso 1 1 calc R . . C116 C 0.2133(5) -0.1415(3) 0.5019(3) 0.0309(12) Uani 1 1 d . . . H116 H 0.3015 -0.1439 0.5013 0.037 Uiso 1 1 calc R . . C121 C 0.1735(4) 0.0942(3) 0.5906(2) 0.0204(10) Uani 1 1 d . . . C122 C 0.1435(5) 0.0486(4) 0.6443(3) 0.0312(12) Uani 1 1 d . . . H122 H 0.1577 -0.0084 0.6446 0.037 Uiso 1 1 calc R . . C123 C 0.0925(6) 0.0866(4) 0.6981(3) 0.0383(13) Uani 1 1 d . . . H123 H 0.0698 0.0552 0.7347 0.046 Uiso 1 1 calc R . . C124 C 0.0751(5) 0.1689(4) 0.6984(3) 0.0376(14) Uani 1 1 d . . . H124 H 0.0416 0.1946 0.7355 0.045 Uiso 1 1 calc R . . C125 C 0.1058(5) 0.2153(3) 0.6450(3) 0.0306(12) Uani 1 1 d . . . H125 H 0.0926 0.2724 0.6456 0.037 Uiso 1 1 calc R . . C126 C 0.1558(5) 0.1787(3) 0.5906(3) 0.0255(11) Uani 1 1 d . . . H126 H 0.1776 0.2104 0.5540 0.031 Uiso 1 1 calc R . . C211 C 0.6368(5) -0.1178(3) 0.6829(2) 0.0221(10) Uani 1 1 d . . . C212 C 0.7402(5) -0.1045(4) 0.6445(3) 0.0433(15) Uani 1 1 d . . . H212 H 0.7318 -0.1027 0.5990 0.052 Uiso 1 1 calc R . . C213 C 0.8555(6) -0.0941(6) 0.6726(4) 0.058(2) Uani 1 1 d . . . H213 H 0.9262 -0.0850 0.6462 0.070 Uiso 1 1 calc R . . C214 C 0.8687(6) -0.0968(4) 0.7391(3) 0.0411(15) Uani 1 1 d . . . H214 H 0.9483 -0.0906 0.7583 0.049 Uiso 1 1 calc R . . C215 C 0.7648(6) -0.1085(3) 0.7771(3) 0.0338(12) Uani 1 1 d . . . H215 H 0.7728 -0.1087 0.8226 0.041 Uiso 1 1 calc R . . C216 C 0.6487(5) -0.1199(3) 0.7492(2) 0.0263(11) Uani 1 1 d . . . H216 H 0.5779 -0.1291 0.7756 0.032 Uiso 1 1 calc R . . C221 C 0.3493(4) -0.1303(3) 0.7184(2) 0.0206(10) Uani 1 1 d . . . C222 C 0.3295(5) -0.0598(3) 0.7540(3) 0.0292(12) Uani 1 1 d . . . H222 H 0.3691 -0.0105 0.7419 0.035 Uiso 1 1 calc R . . C223 C 0.2521(6) -0.0617(3) 0.8070(3) 0.0304(12) Uani 1 1 d . . . H223 H 0.2395 -0.0135 0.8314 0.036 Uiso 1 1 calc R . . C224 C 0.1929(5) -0.1325(4) 0.8251(2) 0.0294(12) Uani 1 1 d . . . H224 H 0.1398 -0.1330 0.8616 0.035 Uiso 1 1 calc R . . C225 C 0.2112(5) -0.2030(3) 0.7897(3) 0.0301(12) Uani 1 1 d . . . H225 H 0.1706 -0.2519 0.8021 0.036 Uiso 1 1 calc R . . C46 C 0.2896(5) -0.2024(3) 0.7357(2) 0.0227(10) Uani 1 1 d . . . H226 H 0.3019 -0.2506 0.7112 0.027 Uiso 1 1 calc R . . C311 C 0.5320(5) 0.1219(3) 0.7020(2) 0.0210(10) Uani 1 1 d . . . C312 C 0.6059(5) 0.0888(3) 0.7500(2) 0.0236(10) Uani 1 1 d . . . H312 H 0.6836 0.0646 0.7398 0.028 Uiso 1 1 calc R . . C313 C 0.5646(5) 0.0914(3) 0.8133(3) 0.0303(12) Uani 1 1 d . . . H313 H 0.6132 0.0673 0.8464 0.036 Uiso 1 1 calc R . . C314 C 0.4539(6) 0.1285(3) 0.8285(3) 0.0307(12) Uani 1 1 d . . . H314 H 0.4274 0.1312 0.8721 0.037 Uiso 1 1 calc R . . C315 C 0.3807(5) 0.1620(3) 0.7801(3) 0.0279(11) Uani 1 1 d . . . H315 H 0.3048 0.1881 0.7908 0.034 Uiso 1 1 calc R . . C316 C 0.4188(5) 0.1572(3) 0.7159(2) 0.0234(11) Uani 1 1 d . . . H316 H 0.3676 0.1778 0.6824 0.028 Uiso 1 1 calc R . . C321 C 0.5094(4) 0.2152(3) 0.5671(2) 0.0215(10) Uani 1 1 d . . . C322 C 0.5041(5) 0.2880(3) 0.6016(3) 0.0267(11) Uani 1 1 d . . . H322 H 0.5443 0.2926 0.6422 0.032 Uiso 1 1 calc R . . C323 C 0.4399(5) 0.3534(3) 0.5764(3) 0.0295(12) Uani 1 1 d . . . H323 H 0.4360 0.4028 0.5999 0.035 Uiso 1 1 calc R . . C324 C 0.3813(5) 0.3479(3) 0.5174(3) 0.0263(11) Uani 1 1 d . . . H324 H 0.3347 0.3926 0.5014 0.032 Uiso 1 1 calc R . . C325 C 0.3904(5) 0.2770(3) 0.4816(2) 0.0235(10) Uani 1 1 d . . . H325 H 0.3531 0.2740 0.4402 0.028 Uiso 1 1 calc R . . C326 C 0.4544(4) 0.2101(3) 0.5061(2) 0.0230(10) Uani 1 1 d . . . H326 H 0.4605 0.1614 0.4817 0.028 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 Cu1 0.0218(3) 0.0221(3) 0.0161(3) 0.0009(2) -0.0003(2) -0.0002(2) Te1 0.02065(16) 0.02199(16) 0.01735(15) 0.00027(12) -0.00051(12) 0.00030(12) Te2 0.02717(17) 0.01892(16) 0.01399(15) -0.00052(12) 0.00096(13) -0.00099(13) Te3 0.01977(15) 0.02014(16) 0.01865(16) 0.00165(12) -0.00018(12) -0.00021(12) S1 0.0299(6) 0.0246(6) 0.0196(6) 0.0009(5) 0.0066(5) 0.0067(5) F1 0.057(3) 0.157(5) 0.050(2) -0.022(3) 0.010(2) -0.063(3) F2 0.051(2) 0.081(3) 0.0177(16) 0.0049(17) 0.0001(16) -0.003(2) F3 0.131(4) 0.0324(19) 0.032(2) -0.0077(16) 0.023(2) 0.002(2) O1 0.050(2) 0.0305(19) 0.0143(17) 0.0002(14) 0.0090(17) 0.0104(17) O2 0.077(3) 0.055(3) 0.044(3) 0.023(2) 0.029(3) 0.044(3) O3 0.031(2) 0.059(3) 0.040(2) -0.018(2) 0.0057(19) -0.013(2) C1 0.046(3) 0.052(4) 0.016(3) -0.001(3) 0.007(2) -0.011(3) C111 0.027(2) 0.020(2) 0.014(2) -0.0017(18) -0.006(2) -0.0030(19) C112 0.028(3) 0.027(3) 0.030(3) -0.004(2) 0.000(2) 0.002(2) C113 0.029(3) 0.047(3) 0.025(3) -0.008(2) 0.008(2) -0.015(3) C114 0.056(4) 0.031(3) 0.025(3) -0.011(2) 0.006(3) -0.019(3) C115 0.052(3) 0.025(3) 0.041(4) -0.006(3) -0.006(3) 0.007(3) C116 0.031(3) 0.029(3) 0.033(3) -0.010(2) -0.010(2) 0.009(2) C121 0.018(2) 0.026(2) 0.018(2) -0.0012(19) 0.0026(19) 0.0042(19) C122 0.031(3) 0.031(3) 0.031(3) -0.003(2) 0.006(2) 0.004(2) C123 0.039(3) 0.049(3) 0.026(3) 0.002(3) 0.009(3) 0.000(3) C124 0.029(3) 0.048(4) 0.036(3) -0.019(3) 0.000(2) 0.011(3) C125 0.025(3) 0.029(3) 0.038(3) -0.009(2) -0.004(2) 0.005(2) C126 0.023(2) 0.024(2) 0.030(3) -0.004(2) 0.000(2) 0.002(2) C211 0.026(2) 0.020(2) 0.021(2) -0.0029(19) 0.000(2) -0.001(2) C212 0.031(3) 0.070(4) 0.029(3) 0.006(3) 0.003(3) -0.005(3) C213 0.027(3) 0.107(7) 0.041(4) 0.012(4) 0.004(3) -0.012(4) C214 0.028(3) 0.052(4) 0.042(4) 0.003(3) -0.011(3) 0.001(3) C215 0.045(3) 0.032(3) 0.024(3) 0.003(2) -0.012(3) 0.010(3) C216 0.032(3) 0.024(3) 0.024(3) 0.001(2) 0.004(2) 0.004(2) C221 0.021(2) 0.021(2) 0.020(2) 0.005(2) -0.0019(19) 0.0016(19) C222 0.043(3) 0.021(3) 0.023(3) -0.003(2) 0.012(2) -0.004(2) C223 0.041(3) 0.025(3) 0.025(3) -0.003(2) 0.004(3) 0.005(2) C224 0.025(3) 0.043(3) 0.019(2) 0.001(2) 0.004(2) 0.002(2) C225 0.026(3) 0.032(3) 0.032(3) 0.011(2) 0.003(2) -0.008(2) C46 0.028(2) 0.021(2) 0.019(2) 0.000(2) -0.001(2) -0.003(2) C311 0.029(3) 0.020(2) 0.014(2) -0.0006(18) -0.003(2) -0.008(2) C312 0.027(3) 0.021(2) 0.023(2) 0.004(2) -0.011(2) -0.001(2) C313 0.043(3) 0.025(3) 0.023(3) 0.006(2) -0.012(2) -0.010(2) C314 0.048(3) 0.023(3) 0.021(2) -0.005(2) -0.001(2) -0.014(3) C315 0.037(3) 0.022(2) 0.025(3) -0.002(2) 0.003(2) -0.005(2) C316 0.029(3) 0.023(2) 0.019(2) 0.0007(19) -0.004(2) -0.001(2) C321 0.018(2) 0.023(2) 0.024(2) 0.003(2) 0.0036(19) -0.0039(19) C322 0.032(3) 0.025(3) 0.024(3) 0.002(2) -0.001(2) -0.003(2) C323 0.039(3) 0.023(2) 0.026(3) 0.000(2) 0.000(2) -0.005(2) C324 0.029(3) 0.022(2) 0.028(3) 0.010(2) 0.003(2) 0.003(2) C325 0.026(2) 0.027(3) 0.018(2) 0.005(2) -0.001(2) -0.006(2) C326 0.024(2) 0.027(2) 0.018(2) 0.002(2) -0.001(2) -0.003(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 Cu1 O1 2.229(3) . ? Cu1 Te1 2.5457(7) . ? Cu1 Te2 2.5575(7) . ? Cu1 Te3 2.5613(7) . ? Te1 C121 2.120(5) . ? Te1 C111 2.123(5) . ? Te2 C221 2.111(5) . ? Te2 C211 2.123(5) . ? Te3 C321 2.124(5) . ? Te3 C311 2.134(5) . ? S1 O3 1.423(4) . ? S1 O2 1.437(4) . ? S1 O1 1.456(4) . ? S1 C1 1.817(6) . ? F1 C1 1.325(7) . ? F2 C1 1.333(6) . ? F3 C1 1.313(8) . ? C111 C112 1.379(7) . ? C111 C116 1.395(7) . ? C112 C113 1.383(8) . ? C112 H11 0.9500 . ? C113 C114 1.388(8) . ? C113 H113 0.9500 . ? C114 C115 1.374(9) . ? C114 H114 0.9500 . ? C115 C116 1.389(8) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.383(7) . ? C121 C126 1.402(7) . ? C122 C123 1.392(8) . ? C122 H122 0.9500 . ? C123 C124 1.367(9) . ? C123 H123 0.9500 . ? C124 C125 1.384(9) . ? C124 H124 0.9500 . ? C125 C126 1.389(8) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C211 C216 1.383(7) . ? C211 C212 1.387(8) . ? C212 C213 1.383(9) . ? C212 H212 0.9500 . ? C213 C214 1.389(10) . ? C213 H213 0.9500 . ? C214 C215 1.382(9) . ? C214 H214 0.9500 . ? C215 C216 1.391(8) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.390(7) . ? C221 C46 1.397(7) . ? C222 C223 1.381(8) . ? C222 H222 0.9500 . ? C223 C224 1.379(8) . ? C223 H223 0.9500 . ? C224 C225 1.386(8) . ? C224 H224 0.9500 . ? C225 C46 1.403(7) . ? C225 H225 0.9500 . ? C46 H226 0.9500 . ? C311 C316 1.380(7) . ? C311 C312 1.387(7) . ? C312 C313 1.388(8) . ? C312 H312 0.9500 . ? C313 C314 1.376(8) . ? C313 H313 0.9500 . ? C314 C315 1.390(8) . ? C314 H314 0.9500 . ? C315 C316 1.397(7) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? C321 C322 1.396(7) . ? C321 C326 1.400(7) . ? C322 C323 1.381(7) . ? C322 H322 0.9500 . ? C323 C324 1.381(8) . ? C323 H323 0.9500 . ? C324 C325 1.386(7) . ? C324 H324 0.9500 . ? C325 C326 1.394(7) . ? C325 H325 0.9500 . ? C326 H326 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 Te1 104.11(10) . . ? O1 Cu1 Te2 87.94(10) . . ? Te1 Cu1 Te2 122.64(3) . . ? O1 Cu1 Te3 104.60(11) . . ? Te1 Cu1 Te3 114.87(3) . . ? Te2 Cu1 Te3 115.55(3) . . ? C121 Te1 C111 97.08(19) . . ? C121 Te1 Cu1 95.99(13) . . ? C111 Te1 Cu1 102.61(13) . . ? C221 Te2 C211 97.72(19) . . ? C221 Te2 Cu1 113.50(13) . . ? C211 Te2 Cu1 100.00(14) . . ? C321 Te3 C311 97.63(19) . . ? C321 Te3 Cu1 102.45(13) . . ? C311 Te3 Cu1 98.57(12) . . ? O3 S1 O2 115.9(3) . . ? O3 S1 O1 114.4(3) . . ? O2 S1 O1 114.4(2) . . ? O3 S1 C1 104.1(3) . . ? O2 S1 C1 103.5(3) . . ? O1 S1 C1 102.2(2) . . ? S1 O1 Cu1 121.2(2) . . ? F3 C1 F1 108.1(6) . . ? F3 C1 F2 106.8(5) . . ? F1 C1 F2 107.5(5) . . ? F3 C1 S1 111.6(4) . . ? F1 C1 S1 111.0(4) . . ? F2 C1 S1 111.5(4) . . ? C112 C111 C116 120.6(5) . . ? C112 C111 Te1 120.6(4) . . ? C116 C111 Te1 118.7(4) . . ? C111 C112 C113 119.6(5) . . ? C111 C112 H11 120.2 . . ? C113 C112 H11 120.2 . . ? C112 C113 C114 120.3(5) . . ? C112 C113 H113 119.9 . . ? C114 C113 H113 119.9 . . ? C115 C114 C113 119.9(5) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C114 C115 C116 120.5(5) . . ? C114 C115 H115 119.7 . . ? C116 C115 H115 119.7 . . ? C115 C116 C111 119.0(5) . . ? C115 C116 H116 120.5 . . ? C111 C116 H116 120.5 . . ? C122 C121 C126 120.3(5) . . ? C122 C121 Te1 121.6(4) . . ? C126 C121 Te1 117.9(4) . . ? C121 C122 C123 119.8(5) . . ? C121 C122 H122 120.1 . . ? C123 C122 H122 120.1 . . ? C124 C123 C122 120.1(6) . . ? C124 C123 H123 120.0 . . ? C122 C123 H123 120.0 . . ? C123 C124 C125 120.6(5) . . ? C123 C124 H124 119.7 . . ? C125 C124 H124 119.7 . . ? C124 C125 C126 120.4(5) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C126 C121 118.8(5) . . ? C125 C126 H126 120.6 . . ? C121 C126 H126 120.6 . . ? C216 C211 C212 120.2(5) . . ? C216 C211 Te2 122.4(4) . . ? C212 C211 Te2 117.4(4) . . ? C213 C212 C211 119.8(5) . . ? C213 C212 H212 120.1 . . ? C211 C212 H212 120.1 . . ? C212 C213 C214 120.5(6) . . ? C212 C213 H213 119.7 . . ? C214 C213 H213 119.7 . . ? C215 C214 C213 119.3(6) . . ? C215 C214 H214 120.4 . . ? C213 C214 H214 120.4 . . ? C214 C215 C216 120.6(5) . . ? C214 C215 H215 119.7 . . ? C216 C215 H215 119.7 . . ? C211 C216 C215 119.6(5) . . ? C211 C216 H216 120.2 . . ? C215 C216 H216 120.2 . . ? C222 C221 C46 120.0(4) . . ? C222 C221 Te2 123.3(4) . . ? C46 C221 Te2 116.7(3) . . ? C223 C222 C221 119.9(5) . . ? C223 C222 H222 120.1 . . ? C221 C222 H222 120.1 . . ? C224 C223 C222 121.0(5) . . ? C224 C223 H223 119.5 . . ? C222 C223 H223 119.5 . . ? C223 C224 C225 119.7(5) . . ? C223 C224 H224 120.1 . . ? C225 C224 H224 120.1 . . ? C224 C225 C46 120.2(5) . . ? C224 C225 H225 119.9 . . ? C46 C225 H225 119.9 . . ? C221 C46 C225 119.3(5) . . ? C221 C46 H226 120.4 . . ? C225 C46 H226 120.4 . . ? C316 C311 C312 121.4(5) . . ? C316 C311 Te3 121.9(3) . . ? C312 C311 Te3 116.7(4) . . ? C311 C312 C313 119.0(5) . . ? C311 C312 H312 120.5 . . ? C313 C312 H312 120.5 . . ? C314 C313 C312 120.5(5) . . ? C314 C313 H313 119.7 . . ? C312 C313 H313 119.7 . . ? C313 C314 C315 120.0(5) . . ? C313 C314 H314 120.0 . . ? C315 C314 H314 120.0 . . ? C314 C315 C316 120.1(5) . . ? C314 C315 H315 120.0 . . ? C316 C315 H315 120.0 . . ? C311 C316 C315 118.8(5) . . ? C311 C316 H316 120.6 . . ? C315 C316 H316 120.6 . . ? C322 C321 C326 119.9(5) . . ? C322 C321 Te3 121.2(4) . . ? C326 C321 Te3 118.9(4) . . ? C323 C322 C321 119.5(5) . . ? C323 C322 H322 120.3 . . ? C321 C322 H322 120.3 . . ? C322 C323 C324 121.0(5) . . ? C322 C323 H323 119.5 . . ? C324 C323 H323 119.5 . . ? C323 C324 C325 119.9(5) . . ? C323 C324 H324 120.0 . . ? C325 C324 H324 120.0 . . ? C324 C325 C326 120.1(5) . . ? C324 C325 H325 119.9 . . ? C326 C325 H325 119.9 . . ? C325 C326 C321 119.5(5) . . ? C325 C326 H326 120.2 . . ? C321 C326 H326 120.2 . . ? 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 O1 Cu1 Te1 C121 177.35(17) . . . . ? Te2 Cu1 Te1 C121 80.63(14) . . . . ? Te3 Cu1 Te1 C121 -68.88(14) . . . . ? O1 Cu1 Te1 C111 78.70(17) . . . . ? Te2 Cu1 Te1 C111 -18.02(14) . . . . ? Te3 Cu1 Te1 C111 -167.53(14) . . . . ? O1 Cu1 Te2 C221 -171.31(18) . . . . ? Te1 Cu1 Te2 C221 -65.84(15) . . . . ? Te3 Cu1 Te2 C221 83.48(15) . . . . ? O1 Cu1 Te2 C211 85.67(17) . . . . ? Te1 Cu1 Te2 C211 -168.86(14) . . . . ? Te3 Cu1 Te2 C211 -19.55(14) . . . . ? O1 Cu1 Te3 C321 109.21(17) . . . . ? Te1 Cu1 Te3 C321 -4.27(14) . . . . ? Te2 Cu1 Te3 C321 -156.00(14) . . . . ? O1 Cu1 Te3 C311 -150.96(17) . . . . ? Te1 Cu1 Te3 C311 95.56(14) . . . . ? Te2 Cu1 Te3 C311 -56.17(14) . . . . ? O3 S1 O1 Cu1 110.1(3) . . . . ? O2 S1 O1 Cu1 -27.0(4) . . . . ? C1 S1 O1 Cu1 -138.2(3) . . . . ? Te1 Cu1 O1 S1 61.1(3) . . . . ? Te2 Cu1 O1 S1 -175.7(3) . . . . ? Te3 Cu1 O1 S1 -59.8(3) . . . . ? O3 S1 C1 F3 57.1(5) . . . . ? O2 S1 C1 F3 178.6(4) . . . . ? O1 S1 C1 F3 -62.3(5) . . . . ? O3 S1 C1 F1 177.8(5) . . . . ? O2 S1 C1 F1 -60.7(5) . . . . ? O1 S1 C1 F1 58.4(5) . . . . ? O3 S1 C1 F2 -62.4(5) . . . . ? O2 S1 C1 F2 59.1(5) . . . . ? O1 S1 C1 F2 178.3(4) . . . . ? C121 Te1 C111 C112 52.8(4) . . . . ? Cu1 Te1 C111 C112 150.6(4) . . . . ? C121 Te1 C111 C116 -130.4(4) . . . . ? Cu1 Te1 C111 C116 -32.6(4) . . . . ? C116 C111 C112 C113 2.0(8) . . . . ? Te1 C111 C112 C113 178.8(4) . . . . ? C111 C112 C113 C114 0.5(8) . . . . ? C112 C113 C114 C115 -3.6(9) . . . . ? C113 C114 C115 C116 4.1(10) . . . . ? C114 C115 C116 C111 -1.6(9) . . . . ? C112 C111 C116 C115 -1.5(8) . . . . ? Te1 C111 C116 C115 -178.3(4) . . . . ? C111 Te1 C121 C122 42.6(4) . . . . ? Cu1 Te1 C121 C122 -61.0(4) . . . . ? C111 Te1 C121 C126 -142.5(4) . . . . ? Cu1 Te1 C121 C126 113.9(4) . . . . ? C126 C121 C122 C123 1.7(8) . . . . ? Te1 C121 C122 C123 176.5(4) . . . . ? C121 C122 C123 C124 -1.7(9) . . . . ? C122 C123 C124 C125 1.1(10) . . . . ? C123 C124 C125 C126 -0.6(9) . . . . ? C124 C125 C126 C121 0.6(8) . . . . ? C122 C121 C126 C125 -1.1(8) . . . . ? Te1 C121 C126 C125 -176.1(4) . . . . ? C221 Te2 C211 C216 9.5(5) . . . . ? Cu1 Te2 C211 C216 125.1(4) . . . . ? C221 Te2 C211 C212 -170.7(5) . . . . ? Cu1 Te2 C211 C212 -55.0(5) . . . . ? C216 C211 C212 C213 0.5(10) . . . . ? Te2 C211 C212 C213 -179.3(6) . . . . ? C211 C212 C213 C214 0.0(13) . . . . ? C212 C213 C214 C215 -1.3(12) . . . . ? C213 C214 C215 C216 1.9(10) . . . . ? C212 C211 C216 C215 0.1(8) . . . . ? Te2 C211 C216 C215 180.0(4) . . . . ? C214 C215 C216 C211 -1.4(8) . . . . ? C211 Te2 C221 C222 69.3(5) . . . . ? Cu1 Te2 C221 C222 -35.1(5) . . . . ? C211 Te2 C221 C46 -112.3(4) . . . . ? Cu1 Te2 C221 C46 143.2(3) . . . . ? C46 C221 C222 C223 1.0(8) . . . . ? Te2 C221 C222 C223 179.2(4) . . . . ? C221 C222 C223 C224 -0.6(9) . . . . ? C222 C223 C224 C225 0.1(9) . . . . ? C223 C224 C225 C46 -0.1(8) . . . . ? C222 C221 C46 C225 -0.9(7) . . . . ? Te2 C221 C46 C225 -179.3(4) . . . . ? C224 C225 C46 C221 0.4(8) . . . . ? C321 Te3 C311 C316 30.0(4) . . . . ? Cu1 Te3 C311 C316 -73.8(4) . . . . ? C321 Te3 C311 C312 -152.8(4) . . . . ? Cu1 Te3 C311 C312 103.3(4) . . . . ? C316 C311 C312 C313 -0.1(7) . . . . ? Te3 C311 C312 C313 -177.3(4) . . . . ? C311 C312 C313 C314 -2.0(8) . . . . ? C312 C313 C314 C315 1.6(8) . . . . ? C313 C314 C315 C316 0.7(8) . . . . ? C312 C311 C316 C315 2.4(7) . . . . ? Te3 C311 C316 C315 179.5(4) . . . . ? C314 C315 C316 C311 -2.7(7) . . . . ? C311 Te3 C321 C322 41.0(4) . . . . ? Cu1 Te3 C321 C322 141.6(4) . . . . ? C311 Te3 C321 C326 -138.3(4) . . . . ? Cu1 Te3 C321 C326 -37.7(4) . . . . ? C326 C321 C322 C323 2.7(7) . . . . ? Te3 C321 C322 C323 -176.6(4) . . . . ? C321 C322 C323 C324 -0.2(8) . . . . ? C322 C323 C324 C325 -2.5(8) . . . . ? C323 C324 C325 C326 2.7(8) . . . . ? C324 C325 C326 C321 -0.2(7) . . . . ? C322 C321 C326 C325 -2.4(7) . . . . ? Te3 C321 C326 C325 176.8(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.645 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.134 _database_code_depnum_ccdc_archive 'CCDC 949146' ####################################################################### # # 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_cmpd3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tri(diphenylselane)copper trfluoromethylsulfonate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H30 Cu F3 O3 S Se3' _chemical_formula_weight 912.09 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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.785(2) _cell_length_b 16.192(3) _cell_length_c 20.157(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3520.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6506 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 3.834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5144 _exptl_absorpt_correction_T_max 0.9627 _exptl_absorpt_process_details 'SADABS in SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25202 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6885 _reflns_number_gt 6506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker, 2008)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Branderburg, 2006)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0554P)^2^+1.8562P] 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 SHELXL _refine_ls_extinction_coef 0.0036(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(9) _refine_ls_number_reflns 6885 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Cu1 Cu 0.44895(4) -0.00001(3) 0.56971(2) 0.01899(13) Uani 1 1 d . . . Se1 Se 0.25858(4) 0.03534(3) 0.51396(2) 0.01881(12) Uani 1 1 d . . . Se2 Se 0.46721(4) -0.12312(3) 0.63767(2) 0.01879(12) Uani 1 1 d . . . Se3 Se 0.57906(4) 0.11594(3) 0.60093(2) 0.01792(11) Uani 1 1 d . . . S1 S 0.60575(10) -0.02825(7) 0.43436(6) 0.0230(2) Uani 1 1 d . . . F1 F 0.4584(3) -0.1253(3) 0.36751(19) 0.0826(16) Uani 1 1 d . . . F2 F 0.6149(3) -0.0813(2) 0.31244(14) 0.0416(8) Uani 1 1 d . . . F3 F 0.6398(4) -0.1755(2) 0.38488(18) 0.0623(11) Uani 1 1 d . . . O1 O 0.5555(3) -0.0669(2) 0.49394(15) 0.0273(7) Uani 1 1 d . . . O2 O 0.5372(4) 0.0414(3) 0.4112(2) 0.0525(12) Uani 1 1 d . . . O3 O 0.7372(3) -0.0194(3) 0.4345(2) 0.0430(10) Uani 1 1 d . . . C1 C 0.5791(5) -0.1072(4) 0.3719(2) 0.0350(12) Uani 1 1 d . . . C111 C 0.1643(4) -0.0650(3) 0.5083(2) 0.0195(9) Uani 1 1 d . . . C112 C 0.0359(4) -0.0634(3) 0.5098(2) 0.0242(9) Uani 1 1 d . . . H11 H -0.0068 -0.0126 0.5155 0.029 Uiso 1 1 calc R . . C113 C -0.0304(5) -0.1367(3) 0.5027(2) 0.0325(11) Uani 1 1 d . . . H113 H -0.1184 -0.1360 0.5037 0.039 Uiso 1 1 calc R . . C114 C 0.0321(5) -0.2106(3) 0.4942(2) 0.0322(11) Uani 1 1 d . . . H114 H -0.0134 -0.2606 0.4903 0.039 Uiso 1 1 calc R . . C115 C 0.1596(5) -0.2123(3) 0.4914(3) 0.0356(12) Uani 1 1 d . . . H115 H 0.2018 -0.2631 0.4847 0.043 Uiso 1 1 calc R . . C116 C 0.2260(4) -0.1395(3) 0.4984(2) 0.0288(10) Uani 1 1 d . . . H116 H 0.3140 -0.1404 0.4965 0.035 Uiso 1 1 calc R . . C121 C 0.1758(4) 0.0886(3) 0.5875(2) 0.0214(9) Uani 1 1 d . . . C122 C 0.1487(4) 0.0449(3) 0.6448(2) 0.0250(10) Uani 1 1 d . . . H122 H 0.1642 -0.0128 0.6473 0.030 Uiso 1 1 calc R . . C123 C 0.0983(5) 0.0869(3) 0.6986(3) 0.0324(11) Uani 1 1 d . . . H123 H 0.0779 0.0577 0.7380 0.039 Uiso 1 1 calc R . . C124 C 0.0778(4) 0.1715(3) 0.6949(3) 0.0328(12) Uani 1 1 d . . . H124 H 0.0450 0.2001 0.7321 0.039 Uiso 1 1 calc R . . C125 C 0.1048(4) 0.2139(3) 0.6376(3) 0.0304(11) Uani 1 1 d . . . H125 H 0.0901 0.2717 0.6352 0.036 Uiso 1 1 calc R . . C126 C 0.1536(4) 0.1723(3) 0.5830(2) 0.0238(9) Uani 1 1 d . . . H126 H 0.1714 0.2013 0.5431 0.029 Uiso 1 1 calc R . . C211 C 0.6264(4) -0.1098(3) 0.6805(2) 0.0202(9) Uani 1 1 d . . . C212 C 0.7274(4) -0.0938(3) 0.6402(2) 0.0308(11) Uani 1 1 d . . . H212 H 0.7175 -0.0879 0.5936 0.037 Uiso 1 1 calc R . . C213 C 0.8431(5) -0.0864(4) 0.6691(3) 0.0419(14) Uani 1 1 d . . . H213 H 0.9131 -0.0756 0.6419 0.050 Uiso 1 1 calc R . . C214 C 0.8592(5) -0.0945(4) 0.7369(3) 0.0364(12) Uani 1 1 d . . . H214 H 0.9396 -0.0898 0.7558 0.044 Uiso 1 1 calc R . . C215 C 0.7573(4) -0.1096(3) 0.7772(2) 0.0276(10) Uani 1 1 d . . . H215 H 0.7671 -0.1137 0.8239 0.033 Uiso 1 1 calc R . . C216 C 0.6410(4) -0.1186(3) 0.7486(2) 0.0228(9) Uani 1 1 d . . . H216 H 0.5712 -0.1307 0.7757 0.027 Uiso 1 1 calc R . . C221 C 0.3581(4) -0.1255(3) 0.7133(2) 0.0202(8) Uani 1 1 d . . . C222 C 0.3389(4) -0.0573(3) 0.7529(2) 0.0252(10) Uani 1 1 d . . . H222 H 0.3811 -0.0071 0.7436 0.030 Uiso 1 1 calc R . . C223 C 0.2581(5) -0.0619(3) 0.8062(2) 0.0297(10) Uani 1 1 d . . . H223 H 0.2457 -0.0151 0.8338 0.036 Uiso 1 1 calc R . . C224 C 0.1952(4) -0.1351(4) 0.8192(2) 0.0315(11) Uani 1 1 d . . . H224 H 0.1380 -0.1379 0.8549 0.038 Uiso 1 1 calc R . . C225 C 0.2161(4) -0.2033(3) 0.7802(3) 0.0330(11) Uani 1 1 d . . . H225 H 0.1747 -0.2537 0.7900 0.040 Uiso 1 1 calc R . . C46 C 0.2974(4) -0.1995(3) 0.7265(3) 0.0257(10) Uani 1 1 d . . . H226 H 0.3110 -0.2466 0.6994 0.031 Uiso 1 1 calc R . . C311 C 0.5294(4) 0.1258(3) 0.6927(2) 0.0193(8) Uani 1 1 d . . . C312 C 0.6082(4) 0.0918(3) 0.7400(2) 0.0230(9) Uani 1 1 d . . . H312 H 0.6849 0.0677 0.7272 0.028 Uiso 1 1 calc R . . C313 C 0.5730(5) 0.0935(3) 0.8064(2) 0.0276(10) Uani 1 1 d . . . H313 H 0.6255 0.0700 0.8392 0.033 Uiso 1 1 calc R . . C314 C 0.4620(5) 0.1295(3) 0.8250(2) 0.0287(10) Uani 1 1 d . . . H314 H 0.4383 0.1299 0.8704 0.034 Uiso 1 1 calc R . . C315 C 0.3849(4) 0.1648(3) 0.7780(2) 0.0264(10) Uani 1 1 d . . . H315 H 0.3103 0.1913 0.7913 0.032 Uiso 1 1 calc R . . C316 C 0.4167(4) 0.1615(3) 0.7112(2) 0.0218(9) Uani 1 1 d . . . H316 H 0.3624 0.1834 0.6785 0.026 Uiso 1 1 calc R . . C321 C 0.5008(4) 0.2131(3) 0.5641(2) 0.0196(8) Uani 1 1 d . . . C322 C 0.5082(4) 0.2881(3) 0.5973(2) 0.0256(9) Uani 1 1 d . . . H322 H 0.5545 0.2926 0.6372 0.031 Uiso 1 1 calc R . . C323 C 0.4467(5) 0.3569(3) 0.5713(2) 0.0304(11) Uani 1 1 d . . . H323 H 0.4510 0.4086 0.5935 0.036 Uiso 1 1 calc R . . C324 C 0.3790(4) 0.3496(3) 0.5127(2) 0.0270(10) Uani 1 1 d . . . H324 H 0.3329 0.3954 0.4966 0.032 Uiso 1 1 calc R . . C325 C 0.3786(4) 0.2760(3) 0.4779(2) 0.0247(10) Uani 1 1 d . . . H325 H 0.3371 0.2727 0.4364 0.030 Uiso 1 1 calc R . . C326 C 0.4391(4) 0.2064(3) 0.5034(2) 0.0208(9) Uani 1 1 d . . . H326 H 0.4381 0.1556 0.4799 0.025 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 Cu1 0.0193(2) 0.0208(3) 0.0169(2) -0.0007(2) -0.0002(2) 0.0002(2) Se1 0.0183(2) 0.0199(2) 0.0183(2) -0.00067(15) -0.00006(17) 0.00016(16) Se2 0.0223(2) 0.0189(2) 0.0151(2) -0.00073(16) 0.00058(16) -0.00105(16) Se3 0.0176(2) 0.0190(2) 0.0171(2) 0.00013(16) 0.00014(16) -0.00029(16) S1 0.0253(5) 0.0240(5) 0.0195(5) -0.0022(4) 0.0048(4) 0.0047(4) F1 0.058(2) 0.153(5) 0.037(2) -0.030(3) 0.0079(18) -0.064(3) F2 0.0401(17) 0.068(2) 0.0170(14) 0.0013(14) 0.0026(13) -0.0040(15) F3 0.119(3) 0.0303(18) 0.0378(19) -0.0054(15) 0.022(2) 0.007(2) O1 0.0382(18) 0.0272(16) 0.0163(15) -0.0004(13) 0.0095(14) 0.0051(14) O2 0.071(3) 0.046(2) 0.040(2) 0.0167(19) 0.023(2) 0.034(2) O3 0.0256(17) 0.063(3) 0.041(2) -0.0211(19) 0.0061(17) -0.0129(18) C1 0.038(3) 0.053(3) 0.014(2) -0.001(2) 0.004(2) -0.014(3) C111 0.023(2) 0.020(2) 0.0148(19) -0.0003(17) -0.0003(17) -0.0005(17) C112 0.025(2) 0.023(2) 0.025(2) -0.0016(18) 0.0046(19) 0.0014(18) C113 0.033(2) 0.038(3) 0.027(2) -0.009(2) 0.003(2) -0.016(2) C114 0.048(3) 0.024(2) 0.024(2) 0.0002(19) 0.000(2) -0.013(2) C115 0.045(3) 0.024(2) 0.038(3) -0.010(2) -0.011(3) 0.002(2) C116 0.030(2) 0.027(2) 0.029(2) -0.0041(19) -0.010(2) 0.0069(19) C121 0.0132(18) 0.024(2) 0.027(2) -0.0046(18) 0.0006(17) 0.0034(17) C122 0.025(2) 0.026(2) 0.025(2) 0.0015(19) 0.0025(19) 0.0037(18) C123 0.031(3) 0.042(3) 0.024(2) -0.001(2) 0.011(2) 0.003(2) C124 0.020(2) 0.048(3) 0.030(3) -0.012(2) 0.002(2) 0.007(2) C125 0.024(2) 0.028(2) 0.040(3) -0.010(2) -0.002(2) 0.0046(19) C126 0.018(2) 0.027(2) 0.026(2) -0.0042(19) -0.0040(18) -0.0006(17) C211 0.024(2) 0.019(2) 0.018(2) -0.0033(17) 0.0000(17) -0.0001(17) C212 0.028(2) 0.047(3) 0.018(2) -0.004(2) 0.005(2) 0.002(2) C213 0.019(2) 0.067(4) 0.039(3) -0.004(3) 0.004(2) 0.000(2) C214 0.028(2) 0.045(3) 0.036(3) -0.002(2) -0.006(2) 0.001(2) C215 0.030(2) 0.028(2) 0.025(2) 0.0017(19) -0.008(2) 0.006(2) C216 0.028(2) 0.021(2) 0.020(2) 0.0052(18) 0.0019(18) 0.0020(19) C221 0.0194(19) 0.024(2) 0.018(2) 0.0031(18) -0.0044(17) -0.0031(17) C222 0.034(2) 0.020(2) 0.021(2) 0.0005(18) 0.005(2) -0.0033(18) C223 0.040(3) 0.024(2) 0.024(2) -0.0019(19) 0.007(2) 0.005(2) C224 0.020(2) 0.050(3) 0.024(2) 0.011(2) 0.0050(19) 0.006(2) C225 0.024(2) 0.034(3) 0.041(3) 0.007(2) 0.008(2) -0.007(2) C46 0.026(2) 0.020(2) 0.030(2) 0.0019(19) -0.002(2) -0.0039(18) C311 0.026(2) 0.0141(19) 0.0175(19) 0.0012(16) -0.0028(17) -0.0015(18) C312 0.025(2) 0.020(2) 0.024(2) -0.0037(17) -0.0096(18) 0.0001(17) C313 0.033(2) 0.026(2) 0.023(2) 0.0013(19) -0.010(2) -0.005(2) C314 0.039(3) 0.026(2) 0.021(2) -0.0027(18) -0.001(2) -0.005(2) C315 0.032(2) 0.023(2) 0.024(2) -0.0020(18) 0.007(2) -0.0031(19) C316 0.022(2) 0.020(2) 0.023(2) 0.0022(17) -0.0042(19) 0.0012(17) C321 0.0191(19) 0.021(2) 0.018(2) 0.0043(17) 0.0012(17) -0.0028(16) C322 0.031(2) 0.030(2) 0.016(2) 0.0016(18) -0.0001(19) -0.0039(19) C323 0.040(3) 0.021(2) 0.030(3) -0.0027(19) 0.007(2) 0.002(2) C324 0.027(2) 0.027(2) 0.027(2) 0.0115(19) 0.005(2) 0.0018(19) C325 0.022(2) 0.027(2) 0.025(2) 0.0076(19) 0.0021(19) -0.0029(18) C326 0.024(2) 0.019(2) 0.020(2) 0.0021(17) 0.0008(18) -0.0016(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 2.196(3) . ? Cu1 Se1 2.4095(7) . ? Cu1 Se2 2.4266(8) . ? Cu1 Se3 2.4269(7) . ? Se1 C111 1.920(4) . ? Se1 C121 1.934(4) . ? Se2 C221 1.925(4) . ? Se2 C211 1.933(4) . ? Se3 C311 1.932(4) . ? Se3 C321 1.933(4) . ? S1 O3 1.425(4) . ? S1 O2 1.428(4) . ? S1 O1 1.459(3) . ? S1 C1 1.817(5) . ? F1 C1 1.337(6) . ? F2 C1 1.327(6) . ? F3 C1 1.311(7) . ? C111 C112 1.386(6) . ? C111 C116 1.391(6) . ? C112 C113 1.392(7) . ? C112 H11 0.9500 . ? C113 C114 1.383(7) . ? C113 H113 0.9500 . ? C114 C115 1.377(8) . ? C114 H114 0.9500 . ? C115 C116 1.387(7) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.380(6) . ? C121 C122 1.386(7) . ? C122 C123 1.390(7) . ? C122 H122 0.9500 . ? C123 C124 1.389(8) . ? C123 H123 0.9500 . ? C124 C125 1.376(8) . ? C124 H124 0.9500 . ? C125 C126 1.394(7) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C211 C212 1.383(6) . ? C211 C216 1.390(6) . ? C212 C213 1.383(7) . ? C212 H212 0.9500 . ? C213 C214 1.383(8) . ? C213 H213 0.9500 . ? C214 C215 1.388(7) . ? C214 H214 0.9500 . ? C215 C216 1.388(7) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.379(6) . ? C221 C46 1.391(6) . ? C222 C223 1.385(7) . ? C222 H222 0.9500 . ? C223 C224 1.390(7) . ? C223 H223 0.9500 . ? C224 C225 1.374(8) . ? C224 H224 0.9500 . ? C225 C46 1.394(7) . ? C225 H225 0.9500 . ? C46 H226 0.9500 . ? C311 C312 1.392(6) . ? C311 C316 1.396(6) . ? C312 C313 1.393(7) . ? C312 H312 0.9500 . ? C313 C314 1.383(7) . ? C313 H313 0.9500 . ? C314 C315 1.385(7) . ? C314 H314 0.9500 . ? C315 C316 1.390(7) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? C321 C322 1.388(7) . ? C321 C326 1.397(6) . ? C322 C323 1.399(7) . ? C322 H322 0.9500 . ? C323 C324 1.393(7) . ? C323 H323 0.9500 . ? C324 C325 1.382(7) . ? C324 H324 0.9500 . ? C325 C326 1.400(6) . ? C325 H325 0.9500 . ? C326 H326 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 Se1 103.80(9) . . ? O1 Cu1 Se2 86.86(9) . . ? Se1 Cu1 Se2 121.84(3) . . ? O1 Cu1 Se3 105.02(9) . . ? Se1 Cu1 Se3 115.46(3) . . ? Se2 Cu1 Se3 116.24(3) . . ? C111 Se1 C121 100.27(19) . . ? C111 Se1 Cu1 106.12(13) . . ? C121 Se1 Cu1 98.14(13) . . ? C221 Se2 C211 101.06(18) . . ? C221 Se2 Cu1 114.41(13) . . ? C211 Se2 Cu1 103.43(13) . . ? C311 Se3 C321 100.29(18) . . ? C311 Se3 Cu1 98.75(12) . . ? C321 Se3 Cu1 106.13(13) . . ? O3 S1 O2 115.9(3) . . ? O3 S1 O1 114.3(2) . . ? O2 S1 O1 114.6(2) . . ? O3 S1 C1 103.2(2) . . ? O2 S1 C1 104.3(3) . . ? O1 S1 C1 102.1(2) . . ? S1 O1 Cu1 123.75(19) . . ? F3 C1 F2 107.6(4) . . ? F3 C1 F1 108.3(5) . . ? F2 C1 F1 107.0(4) . . ? F3 C1 S1 112.1(4) . . ? F2 C1 S1 110.9(4) . . ? F1 C1 S1 110.7(4) . . ? C112 C111 C116 119.8(4) . . ? C112 C111 Se1 120.8(3) . . ? C116 C111 Se1 119.3(3) . . ? C111 C112 C113 119.7(4) . . ? C111 C112 H11 120.2 . . ? C113 C112 H11 120.2 . . ? C114 C113 C112 120.0(5) . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C115 C114 C113 120.6(5) . . ? C115 C114 H114 119.7 . . ? C113 C114 H114 119.7 . . ? C114 C115 C116 119.6(5) . . ? C114 C115 H115 120.2 . . ? C116 C115 H115 120.2 . . ? C115 C116 C111 120.3(5) . . ? C115 C116 H116 119.8 . . ? C111 C116 H116 119.8 . . ? C126 C121 C122 121.4(4) . . ? C126 C121 Se1 117.8(4) . . ? C122 C121 Se1 120.6(3) . . ? C121 C122 C123 118.9(4) . . ? C121 C122 H122 120.6 . . ? C123 C122 H122 120.6 . . ? C124 C123 C122 120.1(5) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C125 C124 C123 120.3(5) . . ? C125 C124 H124 119.8 . . ? C123 C124 H124 119.8 . . ? C124 C125 C126 120.1(5) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C121 C126 C125 119.2(5) . . ? C121 C126 H126 120.4 . . ? C125 C126 H126 120.4 . . ? C212 C211 C216 120.7(4) . . ? C212 C211 Se2 117.3(3) . . ? C216 C211 Se2 122.0(3) . . ? C213 C212 C211 118.6(5) . . ? C213 C212 H212 120.7 . . ? C211 C212 H212 120.7 . . ? C212 C213 C214 121.5(5) . . ? C212 C213 H213 119.3 . . ? C214 C213 H213 119.3 . . ? C213 C214 C215 119.7(5) . . ? C213 C214 H214 120.2 . . ? C215 C214 H214 120.2 . . ? C214 C215 C216 119.4(4) . . ? C214 C215 H215 120.3 . . ? C216 C215 H215 120.3 . . ? C215 C216 C211 120.1(4) . . ? C215 C216 H216 119.9 . . ? C211 C216 H216 119.9 . . ? C222 C221 C46 120.5(4) . . ? C222 C221 Se2 122.3(3) . . ? C46 C221 Se2 117.2(3) . . ? C221 C222 C223 120.1(4) . . ? C221 C222 H222 120.0 . . ? C223 C222 H222 120.0 . . ? C222 C223 C224 119.9(4) . . ? C222 C223 H223 120.0 . . ? C224 C223 H223 120.0 . . ? C225 C224 C223 119.9(4) . . ? C225 C224 H224 120.1 . . ? C223 C224 H224 120.1 . . ? C224 C225 C46 120.7(5) . . ? C224 C225 H225 119.6 . . ? C46 C225 H225 119.6 . . ? C221 C46 C225 118.9(5) . . ? C221 C46 H226 120.5 . . ? C225 C46 H226 120.5 . . ? C312 C311 C316 120.8(4) . . ? C312 C311 Se3 117.0(3) . . ? C316 C311 Se3 122.1(3) . . ? C311 C312 C313 119.0(4) . . ? C311 C312 H312 120.5 . . ? C313 C312 H312 120.5 . . ? C314 C313 C312 120.3(4) . . ? C314 C313 H313 119.8 . . ? C312 C313 H313 119.8 . . ? C313 C314 C315 120.6(4) . . ? C313 C314 H314 119.7 . . ? C315 C314 H314 119.7 . . ? C314 C315 C316 119.9(4) . . ? C314 C315 H315 120.1 . . ? C316 C315 H315 120.1 . . ? C315 C316 C311 119.3(4) . . ? C315 C316 H316 120.3 . . ? C311 C316 H316 120.3 . . ? C322 C321 C326 121.1(4) . . ? C322 C321 Se3 120.2(3) . . ? C326 C321 Se3 118.8(3) . . ? C321 C322 C323 119.3(4) . . ? C321 C322 H322 120.3 . . ? C323 C322 H322 120.3 . . ? C324 C323 C322 119.8(4) . . ? C324 C323 H323 120.1 . . ? C322 C323 H323 120.1 . . ? C325 C324 C323 120.4(4) . . ? C325 C324 H324 119.8 . . ? C323 C324 H324 119.8 . . ? C324 C325 C326 120.4(4) . . ? C324 C325 H325 119.8 . . ? C326 C325 H325 119.8 . . ? C321 C326 C325 118.8(4) . . ? C321 C326 H326 120.6 . . ? C325 C326 H326 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 Se1 C111 74.60(16) . . . . ? Se2 Cu1 Se1 C111 -20.34(14) . . . . ? Se3 Cu1 Se1 C111 -171.04(13) . . . . ? O1 Cu1 Se1 C121 177.83(16) . . . . ? Se2 Cu1 Se1 C121 82.89(14) . . . . ? Se3 Cu1 Se1 C121 -67.81(14) . . . . ? O1 Cu1 Se2 C221 -166.14(16) . . . . ? Se1 Cu1 Se2 C221 -61.83(14) . . . . ? Se3 Cu1 Se2 C221 88.65(14) . . . . ? O1 Cu1 Se2 C211 84.90(16) . . . . ? Se1 Cu1 Se2 C211 -170.80(13) . . . . ? Se3 Cu1 Se2 C211 -20.31(13) . . . . ? O1 Cu1 Se3 C311 -148.29(16) . . . . ? Se1 Cu1 Se3 C311 98.05(13) . . . . ? Se2 Cu1 Se3 C311 -54.34(13) . . . . ? O1 Cu1 Se3 C321 108.25(16) . . . . ? Se1 Cu1 Se3 C321 -5.40(14) . . . . ? Se2 Cu1 Se3 C321 -157.79(13) . . . . ? O3 S1 O1 Cu1 108.6(3) . . . . ? O2 S1 O1 Cu1 -28.6(4) . . . . ? C1 S1 O1 Cu1 -140.7(3) . . . . ? Se1 Cu1 O1 S1 68.1(2) . . . . ? Se2 Cu1 O1 S1 -169.9(2) . . . . ? Se3 Cu1 O1 S1 -53.5(2) . . . . ? O3 S1 C1 F3 56.5(4) . . . . ? O2 S1 C1 F3 178.0(4) . . . . ? O1 S1 C1 F3 -62.4(4) . . . . ? O3 S1 C1 F2 -63.8(4) . . . . ? O2 S1 C1 F2 57.7(4) . . . . ? O1 S1 C1 F2 177.3(4) . . . . ? O3 S1 C1 F1 177.5(4) . . . . ? O2 S1 C1 F1 -60.9(5) . . . . ? O1 S1 C1 F1 58.6(4) . . . . ? C121 Se1 C111 C112 46.9(4) . . . . ? Cu1 Se1 C111 C112 148.6(4) . . . . ? C121 Se1 C111 C116 -137.2(4) . . . . ? Cu1 Se1 C111 C116 -35.5(4) . . . . ? C116 C111 C112 C113 1.4(7) . . . . ? Se1 C111 C112 C113 177.2(3) . . . . ? C111 C112 C113 C114 -0.1(7) . . . . ? C112 C113 C114 C115 -1.2(8) . . . . ? C113 C114 C115 C116 1.3(8) . . . . ? C114 C115 C116 C111 0.1(8) . . . . ? C112 C111 C116 C115 -1.4(7) . . . . ? Se1 C111 C116 C115 -177.3(4) . . . . ? C111 Se1 C121 C126 -138.6(3) . . . . ? Cu1 Se1 C121 C126 113.3(3) . . . . ? C111 Se1 C121 C122 46.3(4) . . . . ? Cu1 Se1 C121 C122 -61.8(4) . . . . ? C126 C121 C122 C123 -0.2(7) . . . . ? Se1 C121 C122 C123 174.8(4) . . . . ? C121 C122 C123 C124 -1.0(8) . . . . ? C122 C123 C124 C125 1.3(8) . . . . ? C123 C124 C125 C126 -0.4(7) . . . . ? C122 C121 C126 C125 1.1(7) . . . . ? Se1 C121 C126 C125 -174.0(3) . . . . ? C124 C125 C126 C121 -0.8(7) . . . . ? C221 Se2 C211 C212 -171.0(4) . . . . ? Cu1 Se2 C211 C212 -52.3(4) . . . . ? C221 Se2 C211 C216 11.1(4) . . . . ? Cu1 Se2 C211 C216 129.8(4) . . . . ? C216 C211 C212 C213 -0.2(8) . . . . ? Se2 C211 C212 C213 -178.0(4) . . . . ? C211 C212 C213 C214 -0.2(9) . . . . ? C212 C213 C214 C215 -0.6(10) . . . . ? C213 C214 C215 C216 1.7(8) . . . . ? C214 C215 C216 C211 -2.1(7) . . . . ? C212 C211 C216 C215 1.3(7) . . . . ? Se2 C211 C216 C215 179.1(3) . . . . ? C211 Se2 C221 C222 67.5(4) . . . . ? Cu1 Se2 C221 C222 -42.9(4) . . . . ? C211 Se2 C221 C46 -113.0(3) . . . . ? Cu1 Se2 C221 C46 136.6(3) . . . . ? C46 C221 C222 C223 -0.4(7) . . . . ? Se2 C221 C222 C223 179.1(4) . . . . ? C221 C222 C223 C224 -0.8(7) . . . . ? C222 C223 C224 C225 1.9(8) . . . . ? C223 C224 C225 C46 -1.7(8) . . . . ? C222 C221 C46 C225 0.5(7) . . . . ? Se2 C221 C46 C225 -179.0(4) . . . . ? C224 C225 C46 C221 0.6(7) . . . . ? C321 Se3 C311 C312 -151.6(3) . . . . ? Cu1 Se3 C311 C312 100.2(3) . . . . ? C321 Se3 C311 C316 31.7(4) . . . . ? Cu1 Se3 C311 C316 -76.6(3) . . . . ? C316 C311 C312 C313 0.2(6) . . . . ? Se3 C311 C312 C313 -176.6(3) . . . . ? C311 C312 C313 C314 -0.7(7) . . . . ? C312 C313 C314 C315 -0.6(7) . . . . ? C313 C314 C315 C316 2.5(7) . . . . ? C314 C315 C316 C311 -3.0(7) . . . . ? C312 C311 C316 C315 1.7(6) . . . . ? Se3 C311 C316 C315 178.3(3) . . . . ? C311 Se3 C321 C322 44.5(4) . . . . ? Cu1 Se3 C321 C322 146.8(3) . . . . ? C311 Se3 C321 C326 -136.6(3) . . . . ? Cu1 Se3 C321 C326 -34.2(4) . . . . ? C326 C321 C322 C323 3.7(7) . . . . ? Se3 C321 C322 C323 -177.4(3) . . . . ? C321 C322 C323 C324 0.0(7) . . . . ? C322 C323 C324 C325 -4.0(7) . . . . ? C323 C324 C325 C326 4.4(7) . . . . ? C322 C321 C326 C325 -3.3(6) . . . . ? Se3 C321 C326 C325 177.8(3) . . . . ? C324 C325 C326 C321 -0.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.499 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 949147' ####################################################################### # # 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_cmpd4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(dithienyltellane)copper trifluoromethylsulfonate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 Cu F3 O3 S7 Te3' _chemical_formula_weight 1094.15 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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.323(3) _cell_length_b 10.798(2) _cell_length_c 20.054(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.42(3) _cell_angle_gamma 90.00 _cell_volume 3438.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 3.599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.487 _exptl_absorpt_correction_T_max 0.492 _exptl_absorpt_process_details 'XPREP in SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27347 _diffrn_reflns_av_R_equivalents 0.1383 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6722 _reflns_number_gt 5499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker, 2008)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Branderburg, 2006)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0815P)^2^+13.9225P] 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 SHELXL _refine_ls_extinction_coef 0.0031(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6722 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1343 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Cu1 Cu 0.73243(5) 0.13267(7) 0.37022(4) 0.0235(2) Uani 1 1 d . . . Te1 Te 0.57694(3) 0.09377(4) 0.30955(2) 0.02779(17) Uani 1 1 d . C . Te2 Te 0.77907(3) 0.35767(4) 0.36556(2) 0.02945(17) Uani 1 1 d . . . Te3 Te 0.84915(3) -0.02080(4) 0.36219(2) 0.02992(17) Uani 1 1 d . . . S1 S 0.71376(11) -0.02876(15) 0.50284(9) 0.0279(4) Uani 1 1 d . . . S11 S 0.53633(11) 0.38910(16) 0.33983(9) 0.0275(4) Uani 1 1 d . . . S31 S 0.73713(13) 0.60080(18) 0.44902(11) 0.0396(5) Uani 1 1 d . . . S41 S 0.95225(12) 0.24507(19) 0.47243(11) 0.0416(5) Uani 1 1 d . . . S51 S 0.85164(17) 0.1410(5) 0.2204(2) 0.1197(19) Uani 1 1 d . . . S61 S 0.70016(13) -0.1173(2) 0.22791(11) 0.0421(5) Uani 1 1 d . . . O1 O 0.7059(4) 0.0914(5) 0.4695(3) 0.0377(12) Uani 1 1 d . . . O2 O 0.6436(3) -0.0640(6) 0.5299(3) 0.0436(13) Uani 1 1 d . . . O3 O 0.7480(4) -0.1218(5) 0.4664(3) 0.0435(14) Uani 1 1 d . . . F1 F 0.7733(4) 0.0852(6) 0.6185(3) 0.0705(17) Uani 1 1 d . . . F2 F 0.8155(3) -0.1048(6) 0.6152(3) 0.0618(16) Uani 1 1 d . . . F3 F 0.8665(3) 0.0403(6) 0.5623(3) 0.0698(18) Uani 1 1 d . . . C1 C 0.7968(5) 0.0003(9) 0.5796(4) 0.043(2) Uani 1 1 d . . . C11 C 0.5375(4) 0.2373(6) 0.3656(3) 0.0239(13) Uani 1 1 d . . . C12 C 0.5104(4) 0.2249(7) 0.4243(4) 0.0297(15) Uani 1 1 d . . . H12 H 0.5064 0.1479 0.4463 0.036 Uiso 1 1 calc R . . C13 C 0.4887(5) 0.3401(8) 0.4490(4) 0.0379(18) Uani 1 1 d . . . H13 H 0.4693 0.3491 0.4900 0.045 Uiso 1 1 calc R . . C14 C 0.4984(5) 0.4371(8) 0.4078(4) 0.0366(17) Uani 1 1 d . . . H14 H 0.4857 0.5207 0.4161 0.044 Uiso 1 1 calc R . . C21 C 0.5528(4) 0.1940(7) 0.2168(4) 0.0297(15) Uani 1 1 d . . . C23 C 0.4813(5) 0.2911(8) 0.1159(4) 0.0411(19) Uani 1 1 d . . . H23 H 0.4366 0.3181 0.0795 0.049 Uiso 1 1 calc R A 1 C24 C 0.5608(6) 0.3180(8) 0.1176(4) 0.044(2) Uani 1 1 d . C . H24 H 0.5774 0.3648 0.0829 0.052 Uiso 1 1 calc R B 1 C31 C 0.7446(4) 0.4432(7) 0.4479(4) 0.0283(14) Uani 1 1 d . . . C32 C 0.7290(4) 0.3826(6) 0.5111(4) 0.0319(17) Uani 1 1 d . . . H32 H 0.7324 0.2969 0.5221 0.038 Uiso 1 1 calc R . . C33 C 0.7078(6) 0.4823(8) 0.5515(5) 0.045(2) Uani 1 1 d . . . H33 H 0.6916 0.4678 0.5933 0.054 Uiso 1 1 calc R . . C34 C 0.7124(5) 0.5985(7) 0.5265(4) 0.0375(18) Uani 1 1 d . . . H34 H 0.7026 0.6712 0.5502 0.045 Uiso 1 1 calc R . . C41 C 0.9089(5) 0.3476(7) 0.4077(4) 0.0359(17) Uani 1 1 d . . . C42 C 0.9701(5) 0.4166(9) 0.3895(6) 0.056(3) Uani 1 1 d . . . H42 H 0.9592 0.4795 0.3554 0.067 Uiso 1 1 calc R . . C43 C 1.0516(6) 0.3840(11) 0.4268(7) 0.070(3) Uani 1 1 d . . . H43 H 1.1015 0.4219 0.4198 0.084 Uiso 1 1 calc R . . C44 C 1.0519(5) 0.2935(9) 0.4736(6) 0.057(3) Uani 1 1 d . . . H44 H 1.1013 0.2612 0.5032 0.068 Uiso 1 1 calc R . . C51 C 0.9055(4) 0.0737(7) 0.2920(4) 0.0355(17) Uani 1 1 d . . . C52 C 0.9851(6) 0.1081(14) 0.3041(6) 0.079(4) Uani 1 1 d . . . H52A H 1.0261 0.0838 0.3437 0.095 Uiso 1 1 calc R . . C53 C 1.0034(7) 0.1847(13) 0.2523(6) 0.073(3) Uani 1 1 d . . . H53 H 1.0581 0.2161 0.2535 0.088 Uiso 1 1 calc R . . C54 C 0.9380(7) 0.2081(11) 0.2027(7) 0.072(3) Uani 1 1 d . . . H54 H 0.9387 0.2555 0.1629 0.087 Uiso 1 1 calc R . . C61 C 0.7841(4) -0.1547(7) 0.2948(4) 0.0287(15) Uani 1 1 d . . . C62 C 0.7960(5) -0.2784(7) 0.2984(4) 0.0333(16) Uani 1 1 d . . . H62 H 0.8381 -0.3177 0.3324 0.040 Uiso 1 1 calc R . . C63 C 0.7384(6) -0.3439(7) 0.2456(4) 0.0402(19) Uani 1 1 d . . . H63 H 0.7383 -0.4315 0.2410 0.048 Uiso 1 1 calc R . . C64 C 0.6851(5) -0.2694(8) 0.2038(4) 0.0372(17) Uani 1 1 d . . . H64 H 0.6437 -0.2971 0.1652 0.045 Uiso 1 1 calc R . . C22A C 0.4654(4) 0.2170(5) 0.1736(3) 0.047(2) Uani 0.832(10) 1 d P C 1 H22A H 0.4129 0.1903 0.1814 0.056 Uiso 0.832(10) 1 calc PR C 1 S21A S 0.63013(14) 0.2616(2) 0.18683(11) 0.0382(8) Uani 0.832(10) 1 d P C 1 C22B C 0.63013(14) 0.2616(2) 0.18683(11) 0.0382(8) Uani 0.168(10) 1 d P C 2 H22B H 0.6896 0.2662 0.2027 0.046 Uiso 0.168(10) 1 calc PR C 2 S21B S 0.4654(4) 0.2170(5) 0.1736(3) 0.047(2) Uani 0.168(10) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0281(4) 0.0191(4) 0.0235(4) 0.0018(3) 0.0061(3) 0.0041(3) Te1 0.0390(3) 0.0213(3) 0.0226(3) 0.00148(17) 0.00598(19) 0.00050(18) Te2 0.0324(3) 0.0243(3) 0.0314(3) 0.00138(18) 0.0069(2) 0.00170(18) Te3 0.0287(3) 0.0305(3) 0.0284(3) 0.00175(18) 0.00200(19) 0.00568(18) S1 0.0347(9) 0.0233(8) 0.0238(8) -0.0004(6) 0.0026(7) -0.0018(7) S11 0.0334(9) 0.0248(8) 0.0253(9) 0.0037(7) 0.0089(7) 0.0037(7) S31 0.0386(10) 0.0302(10) 0.0492(12) -0.0050(8) 0.0085(9) 0.0012(8) S41 0.0332(9) 0.0414(11) 0.0476(12) 0.0059(9) 0.0042(8) -0.0032(9) S51 0.0399(14) 0.210(5) 0.099(3) 0.111(3) -0.0058(15) -0.021(2) S61 0.0360(10) 0.0403(11) 0.0438(12) -0.0031(9) -0.0032(8) 0.0065(8) O1 0.064(3) 0.022(3) 0.027(3) 0.002(2) 0.011(2) 0.011(2) O2 0.038(3) 0.054(3) 0.040(3) -0.001(3) 0.012(2) -0.013(3) O3 0.073(4) 0.020(3) 0.041(3) 0.001(2) 0.021(3) 0.001(3) F1 0.093(4) 0.080(4) 0.035(3) -0.023(3) 0.006(3) -0.028(3) F2 0.047(3) 0.080(4) 0.052(3) 0.042(3) 0.000(2) -0.002(3) F3 0.042(3) 0.107(5) 0.054(3) 0.023(3) -0.003(2) -0.035(3) C1 0.039(4) 0.055(5) 0.032(4) 0.013(4) 0.005(3) -0.013(4) C11 0.024(3) 0.021(3) 0.024(3) 0.008(3) 0.001(3) 0.003(3) C12 0.033(3) 0.033(4) 0.024(3) 0.006(3) 0.009(3) 0.001(3) C13 0.040(4) 0.047(5) 0.030(4) 0.005(3) 0.014(3) 0.006(4) C14 0.045(4) 0.035(4) 0.030(4) -0.002(3) 0.008(3) 0.010(4) C21 0.033(4) 0.029(4) 0.027(4) -0.001(3) 0.007(3) 0.004(3) C23 0.055(5) 0.037(4) 0.026(4) -0.007(3) -0.003(3) 0.013(4) C24 0.066(6) 0.038(4) 0.029(4) -0.001(3) 0.014(4) -0.008(4) C31 0.027(3) 0.023(3) 0.034(4) 0.001(3) 0.003(3) -0.003(3) C32 0.026(3) 0.016(3) 0.057(5) -0.025(3) 0.016(3) -0.009(3) C33 0.051(5) 0.042(5) 0.046(5) -0.002(4) 0.022(4) -0.007(4) C34 0.036(4) 0.030(4) 0.050(5) -0.007(3) 0.017(4) 0.003(3) C41 0.032(4) 0.026(4) 0.051(5) 0.006(3) 0.012(3) 0.003(3) C42 0.030(4) 0.058(6) 0.082(7) 0.022(5) 0.020(4) 0.002(4) C43 0.033(5) 0.077(7) 0.101(9) 0.039(7) 0.016(5) 0.000(5) C44 0.025(4) 0.053(6) 0.083(7) 0.007(5) -0.005(4) 0.001(4) C51 0.025(3) 0.039(4) 0.041(4) -0.004(3) 0.005(3) 0.005(3) C52 0.038(5) 0.150(12) 0.052(6) 0.016(7) 0.014(5) -0.017(6) C53 0.049(6) 0.109(9) 0.071(7) 0.009(7) 0.035(5) -0.023(6) C54 0.063(6) 0.074(8) 0.090(8) 0.041(7) 0.038(6) 0.012(6) C61 0.024(3) 0.031(4) 0.032(4) 0.000(3) 0.009(3) 0.002(3) C62 0.046(4) 0.026(4) 0.031(4) 0.004(3) 0.015(3) 0.006(3) C63 0.064(5) 0.026(4) 0.038(4) -0.004(3) 0.027(4) -0.002(4) C64 0.035(4) 0.045(4) 0.034(4) -0.007(3) 0.013(3) -0.001(3) C22A 0.074(4) 0.037(3) 0.028(3) -0.003(2) 0.010(3) 0.003(3) S21A 0.0431(13) 0.0466(14) 0.0256(12) 0.0071(9) 0.0091(9) 0.0006(10) C22B 0.0431(13) 0.0466(14) 0.0256(12) 0.0071(9) 0.0091(9) 0.0006(10) S21B 0.074(4) 0.037(3) 0.028(3) -0.003(2) 0.010(3) 0.003(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 Cu1 O1 2.180(5) . ? Cu1 Te2 2.5544(10) . ? Cu1 Te3 2.5582(9) . ? Cu1 Te1 2.5817(12) . ? Te1 C11 2.100(7) . ? Te1 C21 2.109(7) . ? Te2 C31 2.081(7) . ? Te2 C41 2.094(8) . ? Te3 C61 2.092(7) . ? Te3 C51 2.114(8) . ? S1 O2 1.428(5) . ? S1 O3 1.430(6) . ? S1 O1 1.451(5) . ? S1 C1 1.826(8) . ? S11 C14 1.703(8) . ? S11 C11 1.718(6) . ? S31 C34 1.695(9) . ? S31 C31 1.707(7) . ? S41 C44 1.704(9) . ? S41 C41 1.728(8) . ? S51 C51 1.667(8) . ? S51 C54 1.694(10) . ? S61 C64 1.714(8) . ? S61 C61 1.729(7) . ? F1 C1 1.317(11) . ? F2 C1 1.338(10) . ? F3 C1 1.335(9) . ? C11 C12 1.359(10) . ? C12 C13 1.415(11) . ? C12 H12 0.9500 . ? C13 C14 1.366(11) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C21 C22A 1.509(9) . ? C21 S21A 1.685(7) . ? C23 C24 1.323(12) . ? C23 C22A 1.478(10) . ? C23 H23 0.9500 . ? C24 S21A 1.689(9) . ? C24 H24 0.9500 . ? C31 C32 1.498(11) . ? C32 C33 1.436(11) . ? C32 H32 0.9500 . ? C33 C34 1.358(12) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C41 C42 1.364(11) . ? C42 C43 1.411(13) . ? C42 H42 0.9500 . ? C43 C44 1.354(14) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C51 C52 1.318(12) . ? C52 C53 1.413(16) . ? C52 H52A 0.9500 . ? C53 C54 1.304(16) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C61 C62 1.348(10) . ? C62 C63 1.429(12) . ? C62 H62 0.9500 . ? C63 C64 1.331(12) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C22A H22A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 Te2 110.62(14) . . ? O1 Cu1 Te3 103.52(14) . . ? Te2 Cu1 Te3 112.41(4) . . ? O1 Cu1 Te1 90.86(16) . . ? Te2 Cu1 Te1 113.97(3) . . ? Te3 Cu1 Te1 122.01(4) . . ? C11 Te1 C21 94.3(3) . . ? C11 Te1 Cu1 91.00(17) . . ? C21 Te1 Cu1 107.12(19) . . ? C31 Te2 C41 97.9(3) . . ? C31 Te2 Cu1 104.78(19) . . ? C41 Te2 Cu1 102.6(2) . . ? C61 Te3 C51 97.9(3) . . ? C61 Te3 Cu1 102.41(18) . . ? C51 Te3 Cu1 100.1(2) . . ? O2 S1 O3 116.8(4) . . ? O2 S1 O1 114.8(4) . . ? O3 S1 O1 113.3(3) . . ? O2 S1 C1 103.2(3) . . ? O3 S1 C1 104.5(4) . . ? O1 S1 C1 101.8(4) . . ? C14 S11 C11 91.8(4) . . ? C34 S31 C31 91.7(4) . . ? C44 S41 C41 92.1(4) . . ? C51 S51 C54 93.9(5) . . ? C64 S61 C61 91.8(4) . . ? S1 O1 Cu1 126.0(3) . . ? F1 C1 F3 108.1(8) . . ? F1 C1 F2 109.7(7) . . ? F3 C1 F2 108.0(7) . . ? F1 C1 S1 111.0(6) . . ? F3 C1 S1 110.3(6) . . ? F2 C1 S1 109.7(6) . . ? C12 C11 S11 111.8(5) . . ? C12 C11 Te1 126.4(5) . . ? S11 C11 Te1 121.8(4) . . ? C11 C12 C13 112.1(7) . . ? C11 C12 H12 124.0 . . ? C13 C12 H12 124.0 . . ? C14 C13 C12 112.8(7) . . ? C14 C13 H13 123.6 . . ? C12 C13 H13 123.6 . . ? C13 C14 S11 111.5(6) . . ? C13 C14 H14 124.2 . . ? S11 C14 H14 124.2 . . ? C22A C21 S21A 114.3(5) . . ? C22A C21 Te1 123.4(5) . . ? S21A C21 Te1 122.3(4) . . ? C24 C23 C22A 116.6(7) . . ? C24 C23 H23 121.7 . . ? C22A C23 H23 121.7 . . ? C23 C24 S21A 114.1(6) . . ? C23 C24 H24 122.9 . . ? S21A C24 H24 122.9 . . ? C32 C31 S31 113.4(5) . . ? C32 C31 Te2 127.4(5) . . ? S31 C31 Te2 119.1(4) . . ? C33 C32 C31 105.0(6) . . ? C33 C32 H32 127.5 . . ? C31 C32 H32 127.5 . . ? C34 C33 C32 116.3(8) . . ? C34 C33 H33 121.8 . . ? C32 C33 H33 121.8 . . ? C33 C34 S31 113.3(6) . . ? C33 C34 H34 123.3 . . ? S31 C34 H34 123.3 . . ? C42 C41 S41 110.7(6) . . ? C42 C41 Te2 126.8(6) . . ? S41 C41 Te2 122.4(4) . . ? C41 C42 C43 112.4(9) . . ? C41 C42 H42 123.8 . . ? C43 C42 H42 123.8 . . ? C44 C43 C42 113.6(8) . . ? C44 C43 H43 123.2 . . ? C42 C43 H43 123.2 . . ? C43 C44 S41 111.2(7) . . ? C43 C44 H44 124.4 . . ? S41 C44 H44 124.4 . . ? C52 C51 S51 109.6(8) . . ? C52 C51 Te3 125.2(7) . . ? S51 C51 Te3 124.1(4) . . ? C51 C52 C53 113.4(10) . . ? C51 C52 H52A 123.3 . . ? C53 C52 H52A 123.3 . . ? C54 C53 C52 113.5(9) . . ? C54 C53 H53 123.2 . . ? C52 C53 H53 123.2 . . ? C53 C54 S51 109.3(8) . . ? C53 C54 H54 125.3 . . ? S51 C54 H54 125.3 . . ? C62 C61 S61 110.5(6) . . ? C62 C61 Te3 127.3(6) . . ? S61 C61 Te3 122.1(4) . . ? C61 C62 C63 113.0(7) . . ? C61 C62 H62 123.5 . . ? C63 C62 H62 123.5 . . ? C64 C63 C62 112.9(7) . . ? C64 C63 H63 123.6 . . ? C62 C63 H63 123.6 . . ? C63 C64 S61 111.8(6) . . ? C63 C64 H64 124.1 . . ? S61 C64 H64 124.1 . . ? C23 C22A C21 103.0(6) . . ? C23 C22A H22A 128.5 . . ? C21 C22A H22A 128.5 . . ? C24 S21A C21 92.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 Te1 C11 60.8(2) . . . . ? Te2 Cu1 Te1 C11 -52.32(17) . . . . ? Te3 Cu1 Te1 C11 167.33(17) . . . . ? O1 Cu1 Te1 C21 155.6(2) . . . . ? Te2 Cu1 Te1 C21 42.5(2) . . . . ? Te3 Cu1 Te1 C21 -97.8(2) . . . . ? O1 Cu1 Te2 C31 -15.5(2) . . . . ? Te3 Cu1 Te2 C31 -130.70(19) . . . . ? Te1 Cu1 Te2 C31 85.13(19) . . . . ? O1 Cu1 Te2 C41 86.3(3) . . . . ? Te3 Cu1 Te2 C41 -28.9(2) . . . . ? Te1 Cu1 Te2 C41 -173.1(2) . . . . ? O1 Cu1 Te3 C61 103.4(3) . . . . ? Te2 Cu1 Te3 C61 -137.2(2) . . . . ? Te1 Cu1 Te3 C61 3.7(2) . . . . ? O1 Cu1 Te3 C51 -156.1(3) . . . . ? Te2 Cu1 Te3 C51 -36.7(2) . . . . ? Te1 Cu1 Te3 C51 104.1(2) . . . . ? O2 S1 O1 Cu1 -133.1(4) . . . . ? O3 S1 O1 Cu1 4.6(6) . . . . ? C1 S1 O1 Cu1 116.1(4) . . . . ? Te2 Cu1 O1 S1 -151.4(4) . . . . ? Te3 Cu1 O1 S1 -30.8(4) . . . . ? Te1 Cu1 O1 S1 92.5(4) . . . . ? O2 S1 C1 F1 -57.3(6) . . . . ? O3 S1 C1 F1 -179.9(6) . . . . ? O1 S1 C1 F1 62.0(6) . . . . ? O2 S1 C1 F3 -177.1(7) . . . . ? O3 S1 C1 F3 60.3(7) . . . . ? O1 S1 C1 F3 -57.8(7) . . . . ? O2 S1 C1 F2 64.0(7) . . . . ? O3 S1 C1 F2 -58.5(6) . . . . ? O1 S1 C1 F2 -176.7(6) . . . . ? C14 S11 C11 C12 -0.4(6) . . . . ? C14 S11 C11 Te1 179.4(4) . . . . ? C21 Te1 C11 C12 157.1(6) . . . . ? Cu1 Te1 C11 C12 -95.7(6) . . . . ? C21 Te1 C11 S11 -22.8(4) . . . . ? Cu1 Te1 C11 S11 84.5(4) . . . . ? S11 C11 C12 C13 -0.3(8) . . . . ? Te1 C11 C12 C13 179.9(5) . . . . ? C11 C12 C13 C14 1.1(10) . . . . ? C12 C13 C14 S11 -1.4(9) . . . . ? C11 S11 C14 C13 1.0(6) . . . . ? C11 Te1 C21 C22A -74.6(5) . . . . ? Cu1 Te1 C21 C22A -167.0(5) . . . . ? C11 Te1 C21 S21A 102.3(4) . . . . ? Cu1 Te1 C21 S21A 9.9(5) . . . . ? C22A C23 C24 S21A -0.2(10) . . . . ? C34 S31 C31 C32 -1.2(6) . . . . ? C34 S31 C31 Te2 -178.0(4) . . . . ? C41 Te2 C31 C32 -83.2(6) . . . . ? Cu1 Te2 C31 C32 22.2(6) . . . . ? C41 Te2 C31 S31 93.2(4) . . . . ? Cu1 Te2 C31 S31 -161.5(3) . . . . ? S31 C31 C32 C33 3.0(7) . . . . ? Te2 C31 C32 C33 179.5(5) . . . . ? C31 C32 C33 C34 -4.0(10) . . . . ? C32 C33 C34 S31 3.4(10) . . . . ? C31 S31 C34 C33 -1.2(7) . . . . ? C44 S41 C41 C42 -0.9(8) . . . . ? C44 S41 C41 Te2 178.7(6) . . . . ? C31 Te2 C41 C42 -107.6(9) . . . . ? Cu1 Te2 C41 C42 145.3(8) . . . . ? C31 Te2 C41 S41 72.9(5) . . . . ? Cu1 Te2 C41 S41 -34.3(5) . . . . ? S41 C41 C42 C43 1.3(12) . . . . ? Te2 C41 C42 C43 -178.3(8) . . . . ? C41 C42 C43 C44 -1.2(16) . . . . ? C42 C43 C44 S41 0.6(15) . . . . ? C41 S41 C44 C43 0.2(10) . . . . ? C54 S51 C51 C52 4.0(10) . . . . ? C54 S51 C51 Te3 172.3(6) . . . . ? C61 Te3 C51 C52 -134.2(10) . . . . ? Cu1 Te3 C51 C52 121.6(10) . . . . ? C61 Te3 C51 S51 59.3(6) . . . . ? Cu1 Te3 C51 S51 -44.9(6) . . . . ? S51 C51 C52 C53 -3.4(14) . . . . ? Te3 C51 C52 C53 -171.6(9) . . . . ? C51 C52 C53 C54 0.8(19) . . . . ? C52 C53 C54 S51 2.3(17) . . . . ? C51 S51 C54 C53 -3.6(11) . . . . ? C64 S61 C61 C62 -2.3(6) . . . . ? C64 S61 C61 Te3 -178.5(4) . . . . ? C51 Te3 C61 C62 116.4(7) . . . . ? Cu1 Te3 C61 C62 -141.4(6) . . . . ? C51 Te3 C61 S61 -68.0(4) . . . . ? Cu1 Te3 C61 S61 34.2(4) . . . . ? S61 C61 C62 C63 1.7(8) . . . . ? Te3 C61 C62 C63 177.6(5) . . . . ? C61 C62 C63 C64 0.1(10) . . . . ? C62 C63 C64 S61 -1.8(9) . . . . ? C61 S61 C64 C63 2.4(6) . . . . ? C24 C23 C22A C21 -1.2(9) . . . . ? S21A C21 C22A C23 2.1(7) . . . . ? Te1 C21 C22A C23 179.2(5) . . . . ? C23 C24 S21A C21 1.3(7) . . . . ? C22A C21 S21A C24 -2.1(6) . . . . ? Te1 C21 S21A C24 -179.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.865 _refine_diff_density_min -1.584 _refine_diff_density_rms 0.274 # start Validation Reply Form _vrf_PLAT241_cmpd4 ; PROBLEM: Check High Ueq as Compared to Neighbors for S51 RESPONSE: Due to orientational disorder, the thienyl ring can adopt several different orientations near to each other. ; _vrf_PLAT213_cmpd4 ; PROBLEM: Atom C32 has ADP max/min Ratio ..... 4.2 prola RESPONSE: Due to orientational disorder, the thienyl ring can adopt several different orientations near to each other. ; _vrf_PLAT220_cmpd4 ; PROBLEM: Large Non-Solvent S Ueq(max)/Ueq(min) ... 4.4 Ratio RESPONSE: Due to orientational disorder, the thienyl ring can adopt several different orientations near to each other. ; _vrf_PLAT232_cmpd4 ; PROBLEM: Hirshfeld Test Diff (M-X) Te1 -- Cu1 .. 15.4 su RESPONSE: This is due to the empirical multi-scan absorption correction. ; _vrf_PLAT919_cmpd4 ; PROBLEM: Reflection # Likely Affected by the Beamstop ... 1 RESPONSE: This reflection is indeed behind the beam stop. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 949148' ####################################################################### # # 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_cmpd5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(dithienyltellane)silver trifluoromethylsulfonate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H12 Ag F3 O3 S5 Te2' _chemical_formula_weight 844.64 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' F F 0.0171 0.0103 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.909(2) _cell_length_b 11.569(2) _cell_length_c 12.339(3) _cell_angle_alpha 76.21(3) _cell_angle_beta 70.18(3) _cell_angle_gamma 67.81(3) _cell_volume 1222.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 3.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4088 _exptl_absorpt_correction_T_max 0.7128 _exptl_absorpt_process_details 'XPREP in SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15003 _diffrn_reflns_av_R_equivalents 0.1338 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4669 _reflns_number_gt 4295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker, 2008)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Branderburg, 2006)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0882P)^2^+4.8173P] 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 SHELXL _refine_ls_extinction_coef 0.0229(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4669 _refine_ls_number_parameters 287 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.070 _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 0.58939(5) 0.35404(4) 0.65164(4) 0.0287(2) Uani 1 1 d . . . Te1 Te 0.88764(4) 0.24751(4) 0.64741(3) 0.02386(19) Uani 1 1 d . F . C11 C 0.9123(7) 0.0577(5) 0.6567(5) 0.0208(11) Uani 1 1 d . . . C12 C 0.8178(8) 0.0081(6) 0.6374(6) 0.0307(14) Uani 1 1 d . F . H12 H 0.7240 0.0564 0.6205 0.037 Uiso 1 1 calc R . . C13 C 0.8794(8) -0.1255(7) 0.6462(7) 0.0348(15) Uani 1 1 d . . . H13 H 0.8310 -0.1767 0.6348 0.042 Uiso 1 1 calc R F . C14 C 1.0146(8) -0.1730(6) 0.6727(6) 0.0303(14) Uani 1 1 d . F . H14 H 1.0697 -0.2602 0.6833 0.036 Uiso 1 1 calc R . . S11 S 1.07209(19) -0.05707(16) 0.68421(17) 0.0341(4) Uani 1 1 d . F . C15 C 0.8536(8) 0.2462(7) 0.8244(6) 0.0302(14) Uani 1 1 d . . . C16 C 0.9613(10) 0.1914(8) 0.8853(7) 0.0433(18) Uani 1 1 d . F . H16 H 1.0644 0.1460 0.8518 0.052 Uiso 1 1 calc R . . C17 C 0.9001(12) 0.2108(10) 1.0026(8) 0.054(2) Uani 1 1 d . . . H17 H 0.9589 0.1792 1.0565 0.065 Uiso 1 1 calc R F . C18 C 0.7497(12) 0.2785(9) 1.0328(7) 0.049(2) Uani 1 1 d . F . H18 H 0.6915 0.2996 1.1086 0.059 Uiso 1 1 calc R . . S12 S 0.6809(2) 0.32006(19) 0.91376(16) 0.0369(4) Uani 1 1 d . F . Te2 Te 0.33461(4) 0.40358(4) 0.83349(3) 0.02428(19) Uani 1 1 d . E . C21 C 0.3335(7) 0.2203(6) 0.8945(6) 0.0288(13) Uani 1 1 d . . . C23 C 0.2981(10) 0.0380(8) 1.0200(10) 0.062(3) Uani 1 1 d . . . H23 H 0.2699 -0.0174 1.0874 0.074 Uiso 1 1 calc R A 1 C24 C 0.3595(10) -0.0005(8) 0.9122(10) 0.056(2) Uani 1 1 d . E . H24 H 0.3774 -0.0837 0.9001 0.067 Uiso 1 1 calc R B 1 C25 C 0.1428(7) 0.4655(6) 0.7712(6) 0.0248(12) Uani 1 1 d . . . C27 C -0.0211(10) 0.5316(7) 0.6543(7) 0.0398(17) Uani 1 1 d . . . H27 H -0.0565 0.5544 0.5872 0.048 Uiso 1 1 calc R C 3 C28 C -0.1184(8) 0.5462(7) 0.7622(7) 0.0329(15) Uani 1 1 d . E . H28 H -0.2256 0.5752 0.7769 0.039 Uiso 1 1 calc R D 3 O1 O 0.6520(5) 0.3192(5) 0.3008(4) 0.0331(10) Uani 1 1 d D . . C22A C 0.2766(6) 0.1758(5) 1.0272(6) 0.064(2) Uani 0.704(12) 1 d P E 1 H22A H 0.2399 0.2201 1.0926 0.077 Uiso 0.704(12) 1 calc PR E 1 S21A S 0.4002(3) 0.1077(2) 0.8046(2) 0.0414(9) Uani 0.704(12) 1 d P E 1 C22B C 0.4002(3) 0.1077(2) 0.8046(2) 0.0414(9) Uani 0.296(12) 1 d P E 2 H22B H 0.4443 0.1073 0.7232 0.050 Uiso 0.296(12) 1 calc PR E 2 S21B S 0.2766(6) 0.1758(5) 1.0272(6) 0.064(2) Uani 0.296(12) 1 d P E 2 C26A C 0.1375(6) 0.4804(5) 0.6465(6) 0.0501(18) Uani 0.773(11) 1 d P E 3 H26A H 0.2202 0.4604 0.5791 0.060 Uiso 0.773(11) 1 calc PR E 3 S22A S -0.0315(2) 0.50802(19) 0.86650(17) 0.0291(7) Uani 0.773(11) 1 d P E 3 C26B C -0.0315(2) 0.50802(19) 0.86650(17) 0.0291(7) Uani 0.227(11) 1 d P E 4 H26B H -0.0665 0.5096 0.9481 0.035 Uiso 0.227(11) 1 calc PR E 4 S22B S 0.1375(6) 0.4804(5) 0.6465(6) 0.0501(18) Uani 0.227(11) 1 d P E 4 S1A S 0.5252(5) 0.3185(3) 0.4005(3) 0.0240(7) Uani 0.720(5) 1 d PD F 5 C1A C 0.4642(12) 0.1956(10) 0.3885(11) 0.034(2) Uani 0.720(5) 1 d P F 5 F1A F 0.5720(8) 0.0848(7) 0.3891(7) 0.0533(11) Uani 0.720(5) 1 d P F 5 F2A F 0.3411(9) 0.1871(7) 0.4725(8) 0.0533(11) Uani 0.720(5) 1 d P F 5 F3A F 0.4333(8) 0.2166(7) 0.2846(7) 0.0533(11) Uani 0.720(5) 1 d P F 5 O2A O 0.5686(10) 0.2723(7) 0.5068(7) 0.0490(13) Uani 0.720(5) 1 d PD F 5 O3A O 0.3910(10) 0.4279(7) 0.4035(7) 0.0490(13) Uani 0.720(5) 1 d PD . 5 S1B S 0.5075(14) 0.3466(12) 0.3816(11) 0.0240(7) Uani 0.280(5) 1 d PD F 6 C1B C 0.468(4) 0.197(3) 0.442(3) 0.034(2) Uani 0.280(5) 1 d P F 6 F1B F 0.558(2) 0.1277(17) 0.5116(19) 0.0533(11) Uani 0.280(5) 1 d P F 6 F2B F 0.486(2) 0.136(2) 0.361(2) 0.0533(11) Uani 0.280(5) 1 d P F 6 F3B F 0.332(2) 0.218(2) 0.514(2) 0.0533(11) Uani 0.280(5) 1 d P F 6 O2B O 0.482(3) 0.4081(18) 0.4760(17) 0.0490(13) Uani 0.280(5) 1 d PD F 6 O3B O 0.390(2) 0.4148(18) 0.3275(19) 0.0490(13) Uani 0.280(5) 1 d PD F 6 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 0.0243(3) 0.0222(3) 0.0328(3) -0.0042(2) -0.0052(2) -0.0021(2) Te1 0.0227(3) 0.0194(3) 0.0252(3) -0.00175(17) -0.00235(18) -0.00663(17) C11 0.019(3) 0.019(3) 0.020(3) 0.002(2) -0.004(2) -0.006(2) C12 0.031(3) 0.022(3) 0.042(4) -0.003(3) -0.018(3) -0.005(3) C13 0.031(4) 0.029(4) 0.046(4) -0.008(3) -0.010(3) -0.009(3) C14 0.030(3) 0.022(3) 0.033(3) -0.005(3) -0.004(3) -0.005(3) S11 0.0258(8) 0.0253(8) 0.0495(10) -0.0056(7) -0.0160(8) -0.0011(7) C15 0.033(3) 0.034(3) 0.033(3) -0.009(3) -0.010(3) -0.017(3) C16 0.045(4) 0.053(5) 0.043(4) -0.006(4) -0.016(4) -0.025(4) C17 0.064(6) 0.079(7) 0.042(5) 0.006(4) -0.026(4) -0.048(5) C18 0.082(7) 0.063(5) 0.027(4) 0.001(4) -0.017(4) -0.054(5) S12 0.0410(10) 0.0431(10) 0.0294(9) -0.0102(7) -0.0020(7) -0.0200(8) Te2 0.0200(3) 0.0202(3) 0.0283(3) -0.00529(17) -0.00256(18) -0.00404(17) C21 0.020(3) 0.022(3) 0.037(4) 0.002(3) -0.006(3) -0.004(2) C23 0.041(5) 0.037(4) 0.087(8) 0.026(5) -0.009(5) -0.019(4) C24 0.037(4) 0.032(4) 0.078(7) 0.001(4) 0.000(4) -0.008(3) C25 0.021(3) 0.018(3) 0.030(3) -0.004(2) -0.003(2) -0.002(2) C27 0.062(5) 0.026(3) 0.037(4) 0.000(3) -0.024(4) -0.013(3) C28 0.025(3) 0.031(3) 0.043(4) -0.002(3) -0.016(3) -0.003(3) O1 0.028(2) 0.029(2) 0.036(3) -0.008(2) 0.000(2) -0.009(2) C22A 0.040(3) 0.046(3) 0.082(4) 0.026(3) -0.013(2) -0.011(2) S21A 0.0376(14) 0.0224(12) 0.0549(17) -0.0042(10) -0.0023(11) -0.0095(10) C22B 0.0376(14) 0.0224(12) 0.0549(17) -0.0042(10) -0.0023(11) -0.0095(10) S21B 0.040(3) 0.046(3) 0.082(4) 0.026(3) -0.013(2) -0.011(2) C26A 0.042(3) 0.031(3) 0.071(4) -0.007(2) -0.012(3) -0.008(2) S22A 0.0211(11) 0.0330(12) 0.0253(11) -0.0027(8) -0.0046(8) -0.0024(8) C26B 0.0211(11) 0.0330(12) 0.0253(11) -0.0027(8) -0.0046(8) -0.0024(8) S22B 0.042(3) 0.031(3) 0.071(4) -0.007(2) -0.012(3) -0.008(2) S1A 0.0311(14) 0.015(2) 0.0233(17) -0.0015(13) -0.0059(10) -0.0066(14) C1A 0.032(4) 0.026(4) 0.047(7) -0.007(6) -0.018(5) -0.006(3) F1A 0.043(2) 0.045(2) 0.079(3) -0.0060(19) -0.019(2) -0.0223(18) F2A 0.043(2) 0.045(2) 0.079(3) -0.0060(19) -0.019(2) -0.0223(18) F3A 0.043(2) 0.045(2) 0.079(3) -0.0060(19) -0.019(2) -0.0223(18) O2A 0.063(4) 0.032(3) 0.044(3) 0.000(2) -0.016(3) -0.009(2) O3A 0.063(4) 0.032(3) 0.044(3) 0.000(2) -0.016(3) -0.009(2) S1B 0.0311(14) 0.015(2) 0.0233(17) -0.0015(13) -0.0059(10) -0.0066(14) C1B 0.032(4) 0.026(4) 0.047(7) -0.007(6) -0.018(5) -0.006(3) F1B 0.043(2) 0.045(2) 0.079(3) -0.0060(19) -0.019(2) -0.0223(18) F2B 0.043(2) 0.045(2) 0.079(3) -0.0060(19) -0.019(2) -0.0223(18) F3B 0.043(2) 0.045(2) 0.079(3) -0.0060(19) -0.019(2) -0.0223(18) O2B 0.063(4) 0.032(3) 0.044(3) 0.000(2) -0.016(3) -0.009(2) O3B 0.063(4) 0.032(3) 0.044(3) 0.000(2) -0.016(3) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O2A 2.310(8) . ? Ag1 O3A 2.516(8) 2_666 ? Ag1 O2B 2.574(19) . ? Ag1 Te2 2.7231(13) . ? Ag1 Te1 2.7261(10) . ? Te1 C15 2.091(7) . ? Te1 C11 2.095(6) . ? C11 C12 1.373(9) . ? C11 S11 1.716(6) . ? C12 C13 1.424(10) . ? C12 H12 0.9500 . ? C13 C14 1.363(10) . ? C13 H13 0.9500 . ? C14 S11 1.693(7) . ? C14 H14 0.9500 . ? C15 C16 1.382(10) . ? C15 S12 1.715(7) . ? C16 C17 1.403(13) . ? C16 H16 0.9500 . ? C17 C18 1.362(15) . ? C17 H17 0.9500 . ? C18 S12 1.718(8) . ? C18 H18 0.9500 . ? Te2 C21 2.077(7) . ? Te2 C25 2.101(6) . ? C21 C22A 1.567(9) . ? C21 S21A 1.705(7) . ? C23 C24 1.366(16) . ? C23 C22A 1.547(11) . ? C23 H23 0.9500 . ? C24 S21A 1.648(10) . ? C24 H24 0.9500 . ? C25 C26A 1.524(9) . ? C25 S22A 1.693(7) . ? C27 C28 1.357(11) . ? C27 C26A 1.432(10) . ? C27 H27 0.9500 . ? C28 S22A 1.670(7) . ? C28 H28 0.9500 . ? O1 S1B 1.409(13) . ? O1 S1A 1.430(7) . ? C22A H22A 0.9500 . ? C26A H26A 0.9500 . ? S1A O2A 1.437(8) . ? S1A O3A 1.445(8) . ? S1A C1A 1.793(12) . ? C1A F1A 1.323(13) . ? C1A F2A 1.326(14) . ? C1A F3A 1.363(15) . ? O3A Ag1 2.516(8) 2_666 ? S1B O2B 1.410(16) . ? S1B O3B 1.414(16) . ? S1B C1B 1.85(4) . ? C1B F2B 1.28(4) . ? C1B F3B 1.31(4) . ? C1B F1B 1.34(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2A Ag1 O3A 115.1(3) . 2_666 ? O2A Ag1 O2B 35.4(4) . . ? O3A Ag1 O2B 84.9(5) 2_666 . ? O2A Ag1 Te2 113.9(2) . . ? O3A Ag1 Te2 97.9(2) 2_666 . ? O2B Ag1 Te2 102.9(5) . . ? O2A Ag1 Te1 104.3(2) . . ? O3A Ag1 Te1 92.4(2) 2_666 . ? O2B Ag1 Te1 126.0(5) . . ? Te2 Ag1 Te1 130.73(3) . . ? C15 Te1 C11 96.5(2) . . ? C15 Te1 Ag1 96.06(19) . . ? C11 Te1 Ag1 99.70(16) . . ? C12 C11 S11 112.0(5) . . ? C12 C11 Te1 128.2(5) . . ? S11 C11 Te1 119.7(3) . . ? C11 C12 C13 110.7(6) . . ? C11 C12 H12 124.6 . . ? C13 C12 H12 124.6 . . ? C14 C13 C12 113.6(6) . . ? C14 C13 H13 123.2 . . ? C12 C13 H13 123.2 . . ? C13 C14 S11 111.5(5) . . ? C13 C14 H14 124.3 . . ? S11 C14 H14 124.3 . . ? C14 S11 C11 92.1(3) . . ? C16 C15 S12 110.6(6) . . ? C16 C15 Te1 127.0(6) . . ? S12 C15 Te1 122.4(4) . . ? C15 C16 C17 111.9(8) . . ? C15 C16 H16 124.0 . . ? C17 C16 H16 124.0 . . ? C18 C17 C16 114.7(8) . . ? C18 C17 H17 122.7 . . ? C16 C17 H17 122.7 . . ? C17 C18 S12 109.9(6) . . ? C17 C18 H18 125.0 . . ? S12 C18 H18 125.0 . . ? C15 S12 C18 92.9(4) . . ? C21 Te2 C25 96.9(3) . . ? C21 Te2 Ag1 98.51(19) . . ? C25 Te2 Ag1 109.18(18) . . ? C22A C21 S21A 115.8(5) . . ? C22A C21 Te2 121.8(5) . . ? S21A C21 Te2 122.4(4) . . ? C24 C23 C22A 116.9(7) . . ? C24 C23 H23 121.6 . . ? C22A C23 H23 121.6 . . ? C23 C24 S21A 115.3(7) . . ? C23 C24 H24 122.3 . . ? S21A C24 H24 122.3 . . ? C26A C25 S22A 113.0(4) . . ? C26A C25 Te2 128.2(4) . . ? S22A C25 Te2 118.8(4) . . ? C28 C27 C26A 116.9(6) . . ? C28 C27 H27 121.5 . . ? C26A C27 H27 121.5 . . ? C27 C28 S22A 113.5(6) . . ? C27 C28 H28 123.3 . . ? S22A C28 H28 123.3 . . ? S1B O1 S1A 15.1(5) . . ? C23 C22A C21 99.0(6) . . ? C23 C22A H22A 130.5 . . ? C21 C22A H22A 130.5 . . ? C24 S21A C21 93.0(5) . . ? C27 C26A C25 104.0(5) . . ? C27 C26A H26A 128.0 . . ? C25 C26A H26A 128.0 . . ? C28 S22A C25 92.6(4) . . ? O1 S1A O2A 112.6(5) . . ? O1 S1A O3A 116.1(5) . . ? O2A S1A O3A 116.3(6) . . ? O1 S1A C1A 104.9(5) . . ? O2A S1A C1A 101.6(6) . . ? O3A S1A C1A 102.8(6) . . ? F1A C1A F2A 108.7(9) . . ? F1A C1A F3A 105.2(10) . . ? F2A C1A F3A 108.2(9) . . ? F1A C1A S1A 111.9(7) . . ? F2A C1A S1A 112.4(9) . . ? F3A C1A S1A 110.1(8) . . ? S1A O2A Ag1 137.8(5) . . ? S1A O3A Ag1 120.8(5) . 2_666 ? O1 S1B O2B 118.1(14) . . ? O1 S1B O3B 112.1(13) . . ? O2B S1B O3B 107.8(15) . . ? O1 S1B C1B 107.8(13) . . ? O2B S1B C1B 107.3(16) . . ? O3B S1B C1B 102.5(15) . . ? F2B C1B F3B 112(3) . . ? F2B C1B F1B 111(2) . . ? F3B C1B F1B 103(3) . . ? F2B C1B S1B 111(2) . . ? F3B C1B S1B 110(2) . . ? F1B C1B S1B 110(2) . . ? S1B O2B Ag1 135.5(13) . . ? 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 O2A Ag1 Te1 C15 -149.4(3) . . . . ? O3A Ag1 Te1 C15 93.9(3) 2_666 . . . ? O2B Ag1 Te1 C15 179.3(6) . . . . ? Te2 Ag1 Te1 C15 -8.80(19) . . . . ? O2A Ag1 Te1 C11 -51.8(3) . . . . ? O3A Ag1 Te1 C11 -168.5(3) 2_666 . . . ? O2B Ag1 Te1 C11 -83.1(6) . . . . ? Te2 Ag1 Te1 C11 88.86(17) . . . . ? C15 Te1 C11 C12 113.1(6) . . . . ? Ag1 Te1 C11 C12 15.8(6) . . . . ? C15 Te1 C11 S11 -70.6(4) . . . . ? Ag1 Te1 C11 S11 -167.9(3) . . . . ? S11 C11 C12 C13 0.2(8) . . . . ? Te1 C11 C12 C13 176.7(5) . . . . ? C11 C12 C13 C14 0.7(10) . . . . ? C12 C13 C14 S11 -1.4(9) . . . . ? C13 C14 S11 C11 1.3(6) . . . . ? C12 C11 S11 C14 -0.9(5) . . . . ? Te1 C11 S11 C14 -177.7(4) . . . . ? C11 Te1 C15 C16 72.6(7) . . . . ? Ag1 Te1 C15 C16 173.2(6) . . . . ? C11 Te1 C15 S12 -109.0(4) . . . . ? Ag1 Te1 C15 S12 -8.5(4) . . . . ? S12 C15 C16 C17 0.2(9) . . . . ? Te1 C15 C16 C17 178.7(6) . . . . ? C15 C16 C17 C18 0.0(11) . . . . ? C16 C17 C18 S12 -0.1(10) . . . . ? C16 C15 S12 C18 -0.2(6) . . . . ? Te1 C15 S12 C18 -178.8(4) . . . . ? C17 C18 S12 C15 0.2(7) . . . . ? O2A Ag1 Te2 C21 65.4(3) . . . . ? O3A Ag1 Te2 C21 -172.6(3) 2_666 . . . ? O2B Ag1 Te2 C21 100.9(5) . . . . ? Te1 Ag1 Te2 C21 -72.36(19) . . . . ? O2A Ag1 Te2 C25 -35.0(3) . . . . ? O3A Ag1 Te2 C25 87.1(3) 2_666 . . . ? O2B Ag1 Te2 C25 0.6(5) . . . . ? Te1 Ag1 Te2 C25 -172.74(18) . . . . ? C25 Te2 C21 C22A -103.9(5) . . . . ? Ag1 Te2 C21 C22A 145.5(4) . . . . ? C25 Te2 C21 S21A 78.5(4) . . . . ? Ag1 Te2 C21 S21A -32.1(4) . . . . ? C22A C23 C24 S21A -0.6(12) . . . . ? C21 Te2 C25 C26A -100.4(5) . . . . ? Ag1 Te2 C25 C26A 1.1(5) . . . . ? C21 Te2 C25 S22A 80.7(4) . . . . ? Ag1 Te2 C25 S22A -177.8(3) . . . . ? C26A C27 C28 S22A 3.3(9) . . . . ? C24 C23 C22A C21 2.4(9) . . . . ? S21A C21 C22A C23 -3.4(6) . . . . ? Te2 C21 C22A C23 178.9(5) . . . . ? C23 C24 S21A C21 -1.4(8) . . . . ? C22A C21 S21A C24 3.0(6) . . . . ? Te2 C21 S21A C24 -179.3(5) . . . . ? C28 C27 C26A C25 -3.3(8) . . . . ? S22A C25 C26A C27 1.9(6) . . . . ? Te2 C25 C26A C27 -177.0(5) . . . . ? C27 C28 S22A C25 -1.7(6) . . . . ? C26A C25 S22A C28 -0.3(5) . . . . ? Te2 C25 S22A C28 178.7(4) . . . . ? S1B O1 S1A O2A -147(3) . . . . ? S1B O1 S1A O3A -9(3) . . . . ? S1B O1 S1A C1A 103(3) . . . . ? O1 S1A C1A F1A 60.6(10) . . . . ? O2A S1A C1A F1A -56.8(10) . . . . ? O3A S1A C1A F1A -177.5(9) . . . . ? O1 S1A C1A F2A -176.8(7) . . . . ? O2A S1A C1A F2A 65.8(9) . . . . ? O3A S1A C1A F2A -54.9(9) . . . . ? O1 S1A C1A F3A -56.0(8) . . . . ? O2A S1A C1A F3A -173.5(8) . . . . ? O3A S1A C1A F3A 65.9(9) . . . . ? O1 S1A O2A Ag1 93.9(8) . . . . ? O3A S1A O2A Ag1 -43.6(11) . . . . ? C1A S1A O2A Ag1 -154.4(8) . . . . ? O3A Ag1 O2A S1A -20.3(10) 2_666 . . . ? O2B Ag1 O2A S1A 13.5(11) . . . . ? Te2 Ag1 O2A S1A 91.8(9) . . . . ? Te1 Ag1 O2A S1A -120.0(8) . . . . ? O1 S1A O3A Ag1 -43.9(7) . . . 2_666 ? O2A S1A O3A Ag1 92.1(7) . . . 2_666 ? C1A S1A O3A Ag1 -157.8(6) . . . 2_666 ? S1A O1 S1B O2B 79(3) . . . . ? S1A O1 S1B O3B -155(4) . . . . ? S1A O1 S1B C1B -43(3) . . . . ? O1 S1B C1B F2B -53(2) . . . . ? O2B S1B C1B F2B 179(2) . . . . ? O3B S1B C1B F2B 65(2) . . . . ? O1 S1B C1B F3B -177.1(19) . . . . ? O2B S1B C1B F3B 55(3) . . . . ? O3B S1B C1B F3B -59(3) . . . . ? O1 S1B C1B F1B 70(2) . . . . ? O2B S1B C1B F1B -58(3) . . . . ? O3B S1B C1B F1B -171(2) . . . . ? O1 S1B O2B Ag1 -64(2) . . . . ? O3B S1B O2B Ag1 167.8(18) . . . . ? C1B S1B O2B Ag1 58(2) . . . . ? O2A Ag1 O2B S1B -15.8(15) . . . . ? O3A Ag1 O2B S1B 134(2) 2_666 . . . ? Te2 Ag1 O2B S1B -129(2) . . . . ? Te1 Ag1 O2B S1B 45(2) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.423 _refine_diff_density_min -1.842 _refine_diff_density_rms 0.291 # start Validation Reply Form _vrf_PLAT232_cmpd5 ; PROBLEM: Hirshfeld Test Diff (M-X) Te2 -- Ag1 .. 13.3 su RESPONSE: This is due to the empirical multi-scan absorption correction. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 949149' ####################################################################### # # 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_cmpd1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(diphenylselane)silver trifluoromethylsulfonate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 Ag F3 O3 S Se2' _chemical_formula_weight 723.26 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' F F 0.0171 0.0103 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.087(5) _cell_length_b 10.175(5) _cell_length_c 13.076(5) _cell_angle_alpha 93.697(5) _cell_angle_beta 104.738(5) _cell_angle_gamma 104.824(5) _cell_volume 1242.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4354 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 3.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5113 _exptl_absorpt_correction_T_max 0.5942 _exptl_absorpt_process_details 'SADABS in SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Nonius kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17446 _diffrn_reflns_av_R_equivalents 0.1304 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4805 _reflns_number_gt 4354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker, 2008)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Branderburg, 2006)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.034(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4805 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.83030(3) 0.39492(3) 0.38082(2) 0.02000(17) Uani 1 1 d . . . Se1 Se 0.87694(4) 0.16881(4) 0.31188(3) 0.01709(17) Uani 1 1 d . . . Se2 Se 0.61594(4) 0.49305(4) 0.31306(3) 0.01932(18) Uani 1 1 d . . . S1 S 0.87680(11) 0.29287(10) 0.62213(8) 0.0173(2) Uani 1 1 d . . . O1 O 0.9601(3) 0.3984(3) 0.5730(3) 0.0230(7) Uani 1 1 d . . . O2 O 0.7616(3) 0.1950(3) 0.5448(3) 0.0296(7) Uani 1 1 d . . . O3 O 0.8472(4) 0.3447(3) 0.7155(3) 0.0297(8) Uani 1 1 d . . . F1 F 1.0363(4) 0.1350(4) 0.5952(3) 0.0524(10) Uani 1 1 d . . . F2 F 1.1201(3) 0.2746(3) 0.7430(3) 0.0470(9) Uani 1 1 d . . . F3 F 0.9425(3) 0.0962(3) 0.7244(2) 0.0298(6) Uani 1 1 d . . . C1 C 1.0012(5) 0.1945(5) 0.6731(4) 0.0248(9) Uani 1 1 d . . . C111 C 0.9200(4) 0.2077(4) 0.1795(4) 0.0197(8) Uani 1 1 d . . . C112 C 0.8868(5) 0.1045(5) 0.0949(4) 0.0229(9) Uani 1 1 d . . . H112 H 0.8402 0.0125 0.1004 0.028 Uiso 1 1 calc R . . C113 C 0.9226(5) 0.1371(5) 0.0017(4) 0.0268(10) Uani 1 1 d . . . H113 H 0.8973 0.0678 -0.0577 0.032 Uiso 1 1 calc R . . C114 C 0.9954(5) 0.2710(5) -0.0042(4) 0.0304(11) Uani 1 1 d . . . H114 H 1.0192 0.2933 -0.0680 0.036 Uiso 1 1 calc R . . C115 C 1.0335(5) 0.3722(5) 0.0826(4) 0.0289(10) Uani 1 1 d . . . H115 H 1.0869 0.4627 0.0794 0.035 Uiso 1 1 calc R . . C116 C 0.9938(5) 0.3417(4) 0.1740(4) 0.0231(9) Uani 1 1 d . . . H116 H 1.0166 0.4117 0.2326 0.028 Uiso 1 1 calc R . . C121 C 0.6826(4) 0.0543(4) 0.2619(3) 0.0172(8) Uani 1 1 d . . . C122 C 0.6391(5) -0.0386(4) 0.3286(4) 0.0218(9) Uani 1 1 d . . . H122 H 0.7063 -0.0483 0.3913 0.026 Uiso 1 1 calc R . . C123 C 0.4972(5) -0.1174(4) 0.3035(4) 0.0214(9) Uani 1 1 d . . . H123 H 0.4669 -0.1803 0.3492 0.026 Uiso 1 1 calc R . . C124 C 0.3999(5) -0.1031(4) 0.2109(4) 0.0234(9) Uani 1 1 d . . . H124 H 0.3028 -0.1559 0.1934 0.028 Uiso 1 1 calc R . . C125 C 0.4453(4) -0.0117(4) 0.1442(4) 0.0210(9) Uani 1 1 d . . . H125 H 0.3789 -0.0040 0.0804 0.025 Uiso 1 1 calc R . . C126 C 0.5855(5) 0.0684(4) 0.1690(3) 0.0206(9) Uani 1 1 d . . . H126 H 0.6151 0.1319 0.1235 0.025 Uiso 1 1 calc R . . C211 C 0.5504(4) 0.4047(4) 0.1667(3) 0.0185(8) Uani 1 1 d . . . C212 C 0.4068(5) 0.3376(4) 0.1184(4) 0.0225(9) Uani 1 1 d . . . H212 H 0.3388 0.3311 0.1578 0.027 Uiso 1 1 calc R . . C213 C 0.3637(5) 0.2801(5) 0.0112(4) 0.0263(10) Uani 1 1 d . . . H213 H 0.2659 0.2333 -0.0219 0.032 Uiso 1 1 calc R . . C214 C 0.4612(5) 0.2904(5) -0.0475(4) 0.0252(10) Uani 1 1 d . . . H214 H 0.4308 0.2516 -0.1206 0.030 Uiso 1 1 calc R . . C215 C 0.6049(5) 0.3582(5) 0.0019(4) 0.0283(10) Uani 1 1 d . . . H215 H 0.6727 0.3649 -0.0378 0.034 Uiso 1 1 calc R . . C216 C 0.6501(5) 0.4164(4) 0.1090(4) 0.0233(9) Uani 1 1 d . . . H216 H 0.7478 0.4634 0.1420 0.028 Uiso 1 1 calc R . . C221 C 0.4692(4) 0.3803(4) 0.3653(3) 0.0189(8) Uani 1 1 d . . . C222 C 0.4686(5) 0.2471(4) 0.3821(4) 0.0206(9) Uani 1 1 d . . . H222 H 0.5425 0.2112 0.3705 0.025 Uiso 1 1 calc R . . C223 C 0.3592(5) 0.1672(4) 0.4158(4) 0.0226(9) Uani 1 1 d . . . H223 H 0.3565 0.0751 0.4260 0.027 Uiso 1 1 calc R . . C224 C 0.2538(4) 0.2209(5) 0.4349(3) 0.0236(9) Uani 1 1 d . . . H224 H 0.1797 0.1661 0.4594 0.028 Uiso 1 1 calc R . . C225 C 0.2555(5) 0.3543(5) 0.4184(3) 0.0230(9) Uani 1 1 d . . . H225 H 0.1826 0.3908 0.4315 0.028 Uiso 1 1 calc R . . C226 C 0.3638(4) 0.4352(4) 0.3828(3) 0.0204(9) Uani 1 1 d . . . H226 H 0.3652 0.5266 0.3707 0.024 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 0.0181(2) 0.0198(2) 0.0210(2) 0.00144(15) 0.00565(15) 0.00367(14) Se1 0.0163(3) 0.0163(2) 0.0179(3) 0.00384(17) 0.00479(17) 0.00302(17) Se2 0.0190(3) 0.0153(2) 0.0237(3) 0.00256(18) 0.00740(18) 0.00376(17) S1 0.0188(5) 0.0138(5) 0.0200(5) 0.0053(4) 0.0073(4) 0.0031(4) O1 0.0254(16) 0.0166(14) 0.0248(16) 0.0102(12) 0.0091(13) -0.0017(12) O2 0.0222(16) 0.0281(16) 0.0287(18) 0.0084(14) 0.0002(13) -0.0041(13) O3 0.046(2) 0.0200(15) 0.0333(19) 0.0091(14) 0.0240(16) 0.0128(14) F1 0.078(3) 0.063(2) 0.056(2) 0.0312(18) 0.049(2) 0.0549(19) F2 0.0217(15) 0.057(2) 0.051(2) 0.0291(16) -0.0048(13) 0.0001(13) F3 0.0405(16) 0.0222(13) 0.0338(16) 0.0165(11) 0.0165(12) 0.0124(11) C1 0.027(2) 0.031(2) 0.025(2) 0.0117(19) 0.0162(19) 0.0135(19) C111 0.018(2) 0.022(2) 0.022(2) 0.0050(17) 0.0073(16) 0.0077(16) C112 0.025(2) 0.025(2) 0.022(2) 0.0032(18) 0.0102(18) 0.0100(17) C113 0.023(2) 0.038(3) 0.025(2) -0.0005(19) 0.0077(18) 0.0182(19) C114 0.024(2) 0.054(3) 0.024(2) 0.017(2) 0.0153(19) 0.019(2) C115 0.020(2) 0.033(2) 0.035(3) 0.013(2) 0.0094(19) 0.0056(19) C116 0.021(2) 0.023(2) 0.025(2) 0.0051(17) 0.0064(17) 0.0057(17) C121 0.017(2) 0.0136(18) 0.022(2) 0.0007(16) 0.0079(16) 0.0042(15) C122 0.026(2) 0.023(2) 0.019(2) 0.0056(17) 0.0068(17) 0.0091(17) C123 0.021(2) 0.020(2) 0.025(2) 0.0082(17) 0.0118(17) 0.0019(16) C124 0.016(2) 0.022(2) 0.032(3) 0.0019(18) 0.0102(18) 0.0032(16) C125 0.019(2) 0.0180(19) 0.024(2) -0.0007(17) 0.0034(17) 0.0051(16) C126 0.024(2) 0.0175(19) 0.021(2) 0.0030(16) 0.0092(17) 0.0041(16) C211 0.024(2) 0.0124(18) 0.022(2) 0.0040(16) 0.0087(17) 0.0079(16) C212 0.021(2) 0.026(2) 0.024(2) 0.0038(18) 0.0077(17) 0.0118(17) C213 0.027(2) 0.025(2) 0.026(2) 0.0073(18) 0.0024(18) 0.0112(18) C214 0.036(3) 0.026(2) 0.018(2) 0.0049(18) 0.0064(19) 0.0157(19) C215 0.036(3) 0.025(2) 0.034(3) 0.014(2) 0.021(2) 0.013(2) C216 0.024(2) 0.0158(19) 0.032(3) 0.0058(17) 0.0114(19) 0.0058(17) C221 0.021(2) 0.021(2) 0.013(2) 0.0015(16) 0.0018(15) 0.0048(16) C222 0.023(2) 0.022(2) 0.020(2) 0.0030(16) 0.0085(16) 0.0104(17) C223 0.022(2) 0.023(2) 0.023(2) 0.0085(17) 0.0071(17) 0.0054(17) C224 0.015(2) 0.038(2) 0.016(2) 0.0088(18) 0.0045(16) 0.0048(18) C225 0.019(2) 0.034(2) 0.018(2) 0.0026(18) 0.0050(17) 0.0120(18) C226 0.022(2) 0.0192(19) 0.020(2) -0.0030(16) 0.0035(16) 0.0081(16) _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 O1 2.484(3) 2_766 ? Ag1 O1 2.515(3) . ? Ag1 Se2 2.5887(11) . ? Ag1 Se1 2.6133(11) . ? Se1 C121 1.926(4) . ? Se1 C111 1.930(5) . ? Se2 C221 1.929(4) . ? Se2 C211 1.933(4) . ? S1 O3 1.428(3) . ? S1 O2 1.430(3) . ? S1 O1 1.474(3) . ? S1 C1 1.824(5) . ? O1 Ag1 2.484(3) 2_766 ? F1 C1 1.321(6) . ? F2 C1 1.336(6) . ? F3 C1 1.336(5) . ? C111 C112 1.385(6) . ? C111 C116 1.393(6) . ? C112 C113 1.393(7) . ? C112 H112 0.9500 . ? C113 C114 1.390(7) . ? C113 H113 0.9500 . ? C114 C115 1.386(8) . ? C114 H114 0.9500 . ? C115 C116 1.382(7) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.391(6) . ? C121 C126 1.394(6) . ? C122 C123 1.393(6) . ? C122 H122 0.9500 . ? C123 C124 1.393(7) . ? C123 H123 0.9500 . ? C124 C125 1.388(6) . ? C124 H124 0.9500 . ? C125 C126 1.382(6) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C211 C216 1.390(6) . ? C211 C212 1.392(6) . ? C212 C213 1.396(7) . ? C212 H212 0.9500 . ? C213 C214 1.381(7) . ? C213 H213 0.9500 . ? C214 C215 1.396(7) . ? C214 H214 0.9500 . ? C215 C216 1.396(7) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C226 1.381(6) . ? C221 C222 1.385(6) . ? C222 C223 1.381(6) . ? C222 H222 0.9500 . ? C223 C224 1.380(6) . ? C223 H223 0.9500 . ? C224 C225 1.385(6) . ? C224 H224 0.9500 . ? C225 C226 1.391(6) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ag1 O1 73.83(11) 2_766 . ? O1 Ag1 Se2 103.43(8) 2_766 . ? O1 Ag1 Se2 125.92(7) . . ? O1 Ag1 Se1 115.28(8) 2_766 . ? O1 Ag1 Se1 95.16(7) . . ? Se2 Ag1 Se1 130.26(2) . . ? C121 Se1 C111 101.73(18) . . ? C121 Se1 Ag1 99.14(12) . . ? C111 Se1 Ag1 103.02(13) . . ? C221 Se2 C211 98.33(17) . . ? C221 Se2 Ag1 103.03(13) . . ? C211 Se2 Ag1 98.83(12) . . ? O3 S1 O2 117.3(2) . . ? O3 S1 O1 114.46(18) . . ? O2 S1 O1 112.5(2) . . ? O3 S1 C1 103.7(2) . . ? O2 S1 C1 103.7(2) . . ? O1 S1 C1 103.0(2) . . ? S1 O1 Ag1 141.77(19) . 2_766 ? S1 O1 Ag1 111.18(16) . . ? Ag1 O1 Ag1 106.17(11) 2_766 . ? F1 C1 F3 107.9(4) . . ? F1 C1 F2 108.9(4) . . ? F3 C1 F2 107.2(4) . . ? F1 C1 S1 111.5(3) . . ? F3 C1 S1 110.3(3) . . ? F2 C1 S1 111.0(3) . . ? C112 C111 C116 120.8(4) . . ? C112 C111 Se1 121.3(3) . . ? C116 C111 Se1 117.7(3) . . ? C111 C112 C113 119.3(4) . . ? C111 C112 H112 120.4 . . ? C113 C112 H112 120.4 . . ? C114 C113 C112 119.9(4) . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C115 C114 C113 120.3(4) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C116 C115 C114 120.1(4) . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C115 C116 C111 119.5(4) . . ? C115 C116 H116 120.2 . . ? C111 C116 H116 120.2 . . ? C122 C121 C126 120.6(4) . . ? C122 C121 Se1 116.0(3) . . ? C126 C121 Se1 123.3(3) . . ? C121 C122 C123 120.0(4) . . ? C121 C122 H122 120.0 . . ? C123 C122 H122 120.0 . . ? C122 C123 C124 119.5(4) . . ? C122 C123 H123 120.3 . . ? C124 C123 H123 120.3 . . ? C125 C124 C123 119.9(4) . . ? C125 C124 H124 120.1 . . ? C123 C124 H124 120.1 . . ? C126 C125 C124 121.2(4) . . ? C126 C125 H125 119.4 . . ? C124 C125 H125 119.4 . . ? C125 C126 C121 118.9(4) . . ? C125 C126 H126 120.5 . . ? C121 C126 H126 120.5 . . ? C216 C211 C212 120.6(4) . . ? C216 C211 Se2 117.9(3) . . ? C212 C211 Se2 121.3(3) . . ? C211 C212 C213 119.3(4) . . ? C211 C212 H212 120.4 . . ? C213 C212 H212 120.4 . . ? C214 C213 C212 121.0(4) . . ? C214 C213 H213 119.5 . . ? C212 C213 H213 119.5 . . ? C213 C214 C215 119.2(4) . . ? C213 C214 H214 120.4 . . ? C215 C214 H214 120.4 . . ? C216 C215 C214 120.7(4) . . ? C216 C215 H215 119.7 . . ? C214 C215 H215 119.7 . . ? C211 C216 C215 119.2(4) . . ? C211 C216 H216 120.4 . . ? C215 C216 H216 120.4 . . ? C226 C221 C222 121.4(4) . . ? C226 C221 Se2 118.0(3) . . ? C222 C221 Se2 120.6(3) . . ? C223 C222 C221 119.2(4) . . ? C223 C222 H222 120.4 . . ? C221 C222 H222 120.4 . . ? C224 C223 C222 120.2(4) . . ? C224 C223 H223 119.9 . . ? C222 C223 H223 119.9 . . ? C223 C224 C225 120.2(4) . . ? C223 C224 H224 119.9 . . ? C225 C224 H224 119.9 . . ? C224 C225 C226 120.2(4) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? C221 C226 C225 118.8(4) . . ? C221 C226 H226 120.6 . . ? C225 C226 H226 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ag1 Se1 C121 -169.13(16) 2_766 . . . ? O1 Ag1 Se1 C121 116.33(15) . . . . ? Se2 Ag1 Se1 C121 -31.70(14) . . . . ? O1 Ag1 Se1 C111 -64.74(15) 2_766 . . . ? O1 Ag1 Se1 C111 -139.28(14) . . . . ? Se2 Ag1 Se1 C111 72.70(13) . . . . ? O1 Ag1 Se2 C221 -143.52(14) 2_766 . . . ? O1 Ag1 Se2 C221 -63.92(15) . . . . ? Se1 Ag1 Se2 C221 75.45(13) . . . . ? O1 Ag1 Se2 C211 115.74(14) 2_766 . . . ? O1 Ag1 Se2 C211 -164.66(14) . . . . ? Se1 Ag1 Se2 C211 -25.30(12) . . . . ? O3 S1 O1 Ag1 43.6(4) . . . 2_766 ? O2 S1 O1 Ag1 -179.2(3) . . . 2_766 ? C1 S1 O1 Ag1 -68.2(3) . . . 2_766 ? O3 S1 O1 Ag1 -123.5(2) . . . . ? O2 S1 O1 Ag1 13.7(3) . . . . ? C1 S1 O1 Ag1 124.70(19) . . . . ? O1 Ag1 O1 S1 171.7(3) 2_766 . . . ? Se2 Ag1 O1 S1 76.63(18) . . . . ? Se1 Ag1 O1 S1 -73.44(17) . . . . ? O1 Ag1 O1 Ag1 0.0 2_766 . . 2_766 ? Se2 Ag1 O1 Ag1 -95.09(11) . . . 2_766 ? Se1 Ag1 O1 Ag1 114.85(10) . . . 2_766 ? O3 S1 C1 F1 177.9(3) . . . . ? O2 S1 C1 F1 54.9(4) . . . . ? O1 S1 C1 F1 -62.5(4) . . . . ? O3 S1 C1 F3 58.1(4) . . . . ? O2 S1 C1 F3 -64.9(4) . . . . ? O1 S1 C1 F3 177.7(3) . . . . ? O3 S1 C1 F2 -60.5(4) . . . . ? O2 S1 C1 F2 176.5(3) . . . . ? O1 S1 C1 F2 59.0(4) . . . . ? C121 Se1 C111 C112 -46.9(4) . . . . ? Ag1 Se1 C111 C112 -149.3(3) . . . . ? C121 Se1 C111 C116 137.1(3) . . . . ? Ag1 Se1 C111 C116 34.7(3) . . . . ? C116 C111 C112 C113 -2.8(6) . . . . ? Se1 C111 C112 C113 -178.7(3) . . . . ? C111 C112 C113 C114 2.3(7) . . . . ? C112 C113 C114 C115 0.4(7) . . . . ? C113 C114 C115 C116 -2.8(7) . . . . ? C114 C115 C116 C111 2.3(7) . . . . ? C112 C111 C116 C115 0.5(7) . . . . ? Se1 C111 C116 C115 176.5(3) . . . . ? C111 Se1 C121 C122 152.9(3) . . . . ? Ag1 Se1 C121 C122 -101.7(3) . . . . ? C111 Se1 C121 C126 -32.0(4) . . . . ? Ag1 Se1 C121 C126 73.4(3) . . . . ? C126 C121 C122 C123 -0.7(6) . . . . ? Se1 C121 C122 C123 174.5(3) . . . . ? C121 C122 C123 C124 0.6(6) . . . . ? C122 C123 C124 C125 0.5(6) . . . . ? C123 C124 C125 C126 -1.4(6) . . . . ? C124 C125 C126 C121 1.2(6) . . . . ? C122 C121 C126 C125 -0.1(6) . . . . ? Se1 C121 C126 C125 -175.0(3) . . . . ? C221 Se2 C211 C216 -155.9(3) . . . . ? Ag1 Se2 C211 C216 -51.2(3) . . . . ? C221 Se2 C211 C212 27.6(4) . . . . ? Ag1 Se2 C211 C212 132.3(3) . . . . ? C216 C211 C212 C213 1.0(6) . . . . ? Se2 C211 C212 C213 177.4(3) . . . . ? C211 C212 C213 C214 -0.8(7) . . . . ? C212 C213 C214 C215 0.6(7) . . . . ? C213 C214 C215 C216 -0.6(7) . . . . ? C212 C211 C216 C215 -1.0(6) . . . . ? Se2 C211 C216 C215 -177.5(3) . . . . ? C214 C215 C216 C211 0.7(6) . . . . ? C211 Se2 C221 C226 -105.0(3) . . . . ? Ag1 Se2 C221 C226 153.9(3) . . . . ? C211 Se2 C221 C222 73.5(4) . . . . ? Ag1 Se2 C221 C222 -27.7(4) . . . . ? C226 C221 C222 C223 0.8(6) . . . . ? Se2 C221 C222 C223 -177.6(3) . . . . ? C221 C222 C223 C224 -1.5(7) . . . . ? C222 C223 C224 C225 1.2(7) . . . . ? C223 C224 C225 C226 -0.1(6) . . . . ? C222 C221 C226 C225 0.3(6) . . . . ? Se2 C221 C226 C225 178.7(3) . . . . ? C224 C225 C226 C221 -0.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.136 _refine_diff_density_min -1.408 _refine_diff_density_rms 0.333 _database_code_depnum_ccdc_archive 'CCDC 949150' ####################################################################### # # 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_cmpd7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis[mu-bis(trimethylsilylmethyl)tellane)- pentasilver pentakis(trifluoromethylsulfonate) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H85 Ag5 F15 O15 S5 Si8 Te4' _chemical_formula_weight 2489.82 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.885(2) _cell_length_b 27.949(6) _cell_length_c 12.674(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.85(3) _cell_angle_gamma 90.00 _cell_volume 4209.3(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12889 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 26.00 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2394 _exptl_absorpt_coefficient_mu 2.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6026 _exptl_absorpt_correction_T_max 0.7658 _exptl_absorpt_process_details 'XPREP in SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26190 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_av_sigmaI/netI 0.1044 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13917 _reflns_number_gt 12889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker, 2008)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Branderburg, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.1605P)^2^+4.8309P] 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 SHELXL _refine_ls_extinction_coef 0.0141(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 13917 _refine_ls_number_parameters 826 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.2015 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Te1 Te 0.94508(8) 0.34419(3) 0.80073(7) 0.0362(2) Uani 1 1 d . . . Te2 Te 0.74984(9) 0.63198(4) 0.79436(7) 0.0415(3) Uani 1 1 d . . . Te3 Te 0.96314(7) 0.38849(3) 1.14232(7) 0.0324(2) Uani 1 1 d . . . Te4 Te 0.82125(7) 0.56180(3) 1.13799(7) 0.0356(2) Uani 1 1 d . . . Ag1 Ag 0.86289(9) 0.42801(4) 0.73892(9) 0.0419(3) Uani 1 1 d . . . Ag2 Ag 0.79784(11) 0.55638(4) 0.67811(9) 0.0455(3) Uani 1 1 d . . . Ag3 Ag 1.02772(9) 0.32065(4) 0.99875(9) 0.0375(3) Uani 1 1 d . . . Ag4 Ag 0.83468(9) 0.63439(4) 1.00150(9) 0.0414(3) Uani 1 1 d . . . Ag5 Ag 0.88927(9) 0.47436(4) 1.07658(9) 0.0395(3) Uani 1 1 d . . . S1 S 0.6768(3) 0.48954(13) 0.8825(3) 0.0369(7) Uani 1 1 d . . . S2 S 1.0071(3) 0.51592(14) 0.8491(3) 0.0415(8) Uani 1 1 d . . . S3 S 0.7824(4) 0.47132(15) 0.4814(3) 0.0442(8) Uani 1 1 d . . . S4 S 0.7427(3) 0.75503(13) 1.0586(3) 0.0394(8) Uani 1 1 d . . . S5 S 1.0576(4) 0.70737(17) 0.9815(4) 0.0586(11) Uani 1 1 d . . . Si11 Si 1.1799(4) 0.36657(19) 0.6594(4) 0.0484(10) Uani 1 1 d . . . Si12 Si 0.7124(4) 0.29838(17) 0.6679(4) 0.0450(9) Uani 1 1 d . . . Si21 Si 0.9109(4) 0.70230(18) 0.6315(4) 0.0492(10) Uani 1 1 d . . . Si22 Si 0.4985(4) 0.6398(2) 0.6548(4) 0.0567(12) Uani 1 1 d . . . Si31 Si 1.2347(3) 0.40300(16) 1.2270(3) 0.0392(8) Uani 1 1 d . . . Si32 Si 0.6927(3) 0.35038(15) 1.1689(3) 0.0377(8) Uani 1 1 d . . . Si41 Si 1.0512(4) 0.57927(18) 1.2995(4) 0.0515(11) Uani 1 1 d . . . Si42 Si 0.5593(3) 0.60356(16) 1.2025(3) 0.0405(9) Uani 1 1 d . . . O11 O 0.7091(8) 0.4829(4) 0.7728(8) 0.040(2) Uani 1 1 d . . . O12 O 0.7300(9) 0.4560(4) 0.9517(9) 0.041(2) Uani 1 1 d . . . O13 O 0.6757(9) 0.5383(4) 0.9170(9) 0.045(2) Uani 1 1 d . . . O21 O 0.9612(9) 0.5068(4) 0.7438(8) 0.040(2) Uani 1 1 d . . . O22 O 1.0137(9) 0.4731(5) 0.9138(9) 0.048(3) Uani 1 1 d . . . O23 O 0.9636(10) 0.5578(5) 0.9007(11) 0.056(3) Uani 1 1 d . . . O31 O 0.8292(10) 0.4367(4) 0.5554(10) 0.050(3) Uani 1 1 d . . . O32 O 0.7854(10) 0.5203(4) 0.5166(9) 0.049(3) Uani 1 1 d . . . O33 O 0.8130(12) 0.4659(5) 0.3721(10) 0.056(3) Uani 1 1 d . . . O41 O 0.8047(9) 0.7797(5) 0.9761(11) 0.059(3) Uani 1 1 d . . . O42 O 0.7675(11) 0.7702(6) 1.1623(11) 0.066(4) Uani 1 1 d . . . O43 O 0.7324(11) 0.7042(4) 1.0462(14) 0.067(4) Uani 1 1 d . . . O51 O 0.9933(11) 0.6734(5) 0.9273(11) 0.059(3) Uani 1 1 d . . . O52 O 1.0212(15) 0.7131(8) 1.0930(13) 0.091(6) Uani 1 1 d . . . O53 O 1.0766(11) 0.7512(5) 0.9350(19) 0.091(6) Uani 1 1 d . . . F11 F 0.4849(9) 0.4819(5) 0.9773(10) 0.067(3) Uani 1 1 d . . . F12 F 0.4713(9) 0.4985(6) 0.8141(11) 0.079(4) Uani 1 1 d . . . F13 F 0.5141(10) 0.4274(5) 0.8642(14) 0.089(5) Uani 1 1 d . . . F21 F 1.2047(8) 0.4985(4) 0.7671(10) 0.062(3) Uani 1 1 d . . . F22 F 1.1591(11) 0.5722(5) 0.7757(15) 0.092(5) Uani 1 1 d . . . F23 F 1.2111(9) 0.5354(6) 0.9156(12) 0.080(4) Uani 1 1 d . . . F31 F 0.6171(10) 0.4109(4) 0.4510(8) 0.059(2) Uani 1 1 d . . . F32 F 0.5758(9) 0.4848(4) 0.4118(8) 0.059(3) Uani 1 1 d . . . F33 F 0.5894(9) 0.4605(4) 0.5775(8) 0.061(3) Uani 1 1 d . . . F41 F 0.5918(10) 0.8225(5) 1.0303(13) 0.078(4) Uani 1 1 d . . . F42 F 0.5288(9) 0.7590(5) 1.1038(11) 0.073(3) Uani 1 1 d . . . F43 F 0.5635(9) 0.7586(5) 0.9375(10) 0.073(3) Uani 1 1 d . . . F51 F 1.2641(12) 0.7072(7) 1.0512(17) 0.117(7) Uani 1 1 d . . . F52 F 1.1936(12) 0.6393(7) 1.0380(15) 0.105(6) Uani 1 1 d . . . F53 F 1.2406(12) 0.6756(7) 0.9013(11) 0.092(5) Uani 1 1 d . . . C1 C 0.5297(12) 0.4731(6) 0.8827(15) 0.047(4) Uani 1 1 d . . . C2 C 1.1550(13) 0.5310(6) 0.8264(15) 0.047(4) Uani 1 1 d . . . C3 C 0.6339(16) 0.4561(6) 0.4812(13) 0.050(4) Uani 1 1 d . . . C4 C 0.5986(13) 0.7744(6) 1.0327(15) 0.048(4) Uani 1 1 d . . . C5 C 1.2005(16) 0.6810(7) 0.9911(18) 0.059(5) Uani 1 1 d . . . C110 C 1.0607(12) 0.3225(7) 0.6810(12) 0.046(3) Uani 1 1 d . . . H11A H 1.0933 0.2911 0.7009 0.055 Uiso 1 1 calc R . . H11B H 1.0186 0.3182 0.6137 0.055 Uiso 1 1 calc R . . C111 C 1.2343(18) 0.3887(8) 0.7899(16) 0.066(5) Uani 1 1 d . . . H11C H 1.2551 0.3614 0.8345 0.098 Uiso 1 1 calc R . . H11D H 1.1756 0.4074 0.8245 0.098 Uiso 1 1 calc R . . H11E H 1.3005 0.4089 0.7790 0.098 Uiso 1 1 calc R . . C112 C 1.1248(17) 0.4167(8) 0.5757(15) 0.061(5) Uani 1 1 d . . . H11F H 1.0570 0.4300 0.6076 0.092 Uiso 1 1 calc R . . H11G H 1.1063 0.4047 0.5049 0.092 Uiso 1 1 calc R . . H11H H 1.1822 0.4417 0.5707 0.092 Uiso 1 1 calc R . . C113 C 1.2906(17) 0.3313(10) 0.590(2) 0.079(7) Uani 1 1 d . . . H11I H 1.3370 0.3141 0.6418 0.119 Uiso 1 1 calc R . . H11J H 1.3381 0.3530 0.5493 0.119 Uiso 1 1 calc R . . H11K H 1.2544 0.3083 0.5417 0.119 Uiso 1 1 calc R . . C120 C 0.8251(14) 0.2893(6) 0.7719(12) 0.044(3) Uani 1 1 d . . . H12A H 0.8670 0.2600 0.7533 0.052 Uiso 1 1 calc R . . H12B H 0.7870 0.2828 0.8394 0.052 Uiso 1 1 calc R . . C121 C 0.6202(15) 0.3494(8) 0.7092(15) 0.058(4) Uani 1 1 d . . . H12C H 0.5482 0.3477 0.6707 0.087 Uiso 1 1 calc R . . H12D H 0.6574 0.3798 0.6932 0.087 Uiso 1 1 calc R . . H12E H 0.6069 0.3474 0.7852 0.087 Uiso 1 1 calc R . . C122 C 0.6333(19) 0.2416(8) 0.6646(19) 0.069(6) Uani 1 1 d . . . H12F H 0.5644 0.2457 0.6220 0.103 Uiso 1 1 calc R . . H12G H 0.6136 0.2324 0.7366 0.103 Uiso 1 1 calc R . . H12H H 0.6799 0.2165 0.6333 0.103 Uiso 1 1 calc R . . C123 C 0.7767(19) 0.3105(8) 0.5367(14) 0.064(5) Uani 1 1 d . . . H12I H 0.8264 0.2839 0.5180 0.096 Uiso 1 1 calc R . . H12J H 0.8202 0.3402 0.5403 0.096 Uiso 1 1 calc R . . H12K H 0.7170 0.3136 0.4829 0.096 Uiso 1 1 calc R . . C210 C 0.7989(14) 0.7020(6) 0.7309(14) 0.047(4) Uani 1 1 d . . . H21A H 0.7311 0.7171 0.6990 0.057 Uiso 1 1 calc R . . H21B H 0.8236 0.7224 0.7907 0.057 Uiso 1 1 calc R . . C211 C 0.8532(19) 0.6933(11) 0.4937(16) 0.078(7) Uani 1 1 d . . . H21C H 0.8323 0.6597 0.4839 0.117 Uiso 1 1 calc R . . H21D H 0.9106 0.7021 0.4425 0.117 Uiso 1 1 calc R . . H21E H 0.7866 0.7135 0.4830 0.117 Uiso 1 1 calc R . . C212 C 0.968(2) 0.7638(11) 0.642(3) 0.105(11) Uani 1 1 d . . . H21F H 0.9121 0.7866 0.6142 0.158 Uiso 1 1 calc R . . H21G H 1.0370 0.7662 0.6014 0.158 Uiso 1 1 calc R . . H21H H 0.9842 0.7712 0.7163 0.158 Uiso 1 1 calc R . . C213 C 1.019(2) 0.6560(12) 0.655(2) 0.094(9) Uani 1 1 d . . . H21I H 1.0433 0.6567 0.7297 0.140 Uiso 1 1 calc R . . H21J H 1.0843 0.6622 0.6107 0.140 Uiso 1 1 calc R . . H21K H 0.9882 0.6244 0.6385 0.140 Uiso 1 1 calc R . . C220 C 0.5702(13) 0.6419(6) 0.7885(12) 0.045(3) Uani 1 1 d . . . H22A H 0.5357 0.6169 0.8332 0.054 Uiso 1 1 calc R . . H22B H 0.5531 0.6732 0.8210 0.054 Uiso 1 1 calc R . . C221 C 0.3452(18) 0.6530(13) 0.672(2) 0.090(8) Uani 1 1 d . . . H22C H 0.3113 0.6616 0.6035 0.135 Uiso 1 1 calc R . . H22D H 0.3367 0.6797 0.7212 0.135 Uiso 1 1 calc R . . H22E H 0.3075 0.6247 0.6999 0.135 Uiso 1 1 calc R . . C222 C 0.544(3) 0.6896(17) 0.570(2) 0.140(19) Uani 1 1 d . . . H22F H 0.6136 0.6806 0.5345 0.210 Uiso 1 1 calc R . . H22G H 0.5585 0.7180 0.6142 0.210 Uiso 1 1 calc R . . H22H H 0.4854 0.6968 0.5180 0.210 Uiso 1 1 calc R . . C223 C 0.523(5) 0.585(2) 0.587(3) 0.21(3) Uani 1 1 d . . . H22I H 0.5396 0.5912 0.5132 0.312 Uiso 1 1 calc R . . H22J H 0.4552 0.5645 0.5911 0.312 Uiso 1 1 calc R . . H22K H 0.5864 0.5679 0.6206 0.312 Uiso 1 1 calc R . . C310 C 1.0820(12) 0.4027(6) 1.2689(13) 0.043(3) Uani 1 1 d . . . H31A H 1.0641 0.4341 1.3004 0.051 Uiso 1 1 calc R . . H31B H 1.0725 0.3781 1.3244 0.051 Uiso 1 1 calc R . . C311 C 1.2462(14) 0.4229(8) 1.0867(15) 0.055(4) Uani 1 1 d . . . H31C H 1.3239 0.4324 1.0728 0.083 Uiso 1 1 calc R . . H31D H 1.1959 0.4502 1.0741 0.083 Uiso 1 1 calc R . . H31E H 1.2247 0.3965 1.0396 0.083 Uiso 1 1 calc R . . C312 C 1.3100(12) 0.4450(7) 1.3182(18) 0.057(5) Uani 1 1 d . . . H31F H 1.3170 0.4304 1.3883 0.086 Uiso 1 1 calc R . . H31G H 1.2674 0.4749 1.3232 0.086 Uiso 1 1 calc R . . H31H H 1.3851 0.4517 1.2910 0.086 Uiso 1 1 calc R . . C313 C 1.2907(15) 0.3412(7) 1.2399(14) 0.051(4) Uani 1 1 d . . . C320 C 0.8347(12) 0.3584(6) 1.2371(11) 0.043(3) Uani 1 1 d . . . H32A H 0.8607 0.3267 1.2628 0.052 Uiso 1 1 calc R . . H32B H 0.8247 0.3791 1.2996 0.052 Uiso 1 1 calc R . . C321 C 0.6092(13) 0.4062(7) 1.1750(15) 0.049(4) Uani 1 1 d . . . H32C H 0.5385 0.4019 1.1353 0.074 Uiso 1 1 calc R . . H32D H 0.6521 0.4325 1.1441 0.074 Uiso 1 1 calc R . . H32E H 0.5928 0.4136 1.2487 0.074 Uiso 1 1 calc R . . C322 C 0.7142(13) 0.3354(6) 1.0281(12) 0.041(3) Uani 1 1 d . . . H32F H 0.7609 0.3066 1.0232 0.062 Uiso 1 1 calc R . . H32G H 0.7520 0.3621 0.9932 0.062 Uiso 1 1 calc R . . H32H H 0.6412 0.3296 0.9936 0.062 Uiso 1 1 calc R . . C323 C 0.6256(17) 0.3020(7) 1.2431(17) 0.060(5) Uani 1 1 d . . . H32I H 0.5941 0.3150 1.3082 0.089 Uiso 1 1 calc R . . H32J H 0.6817 0.2775 1.2608 0.089 Uiso 1 1 calc R . . H32K H 0.5652 0.2878 1.2000 0.089 Uiso 1 1 calc R . . C410 C 0.8920(12) 0.5778(7) 1.2909(12) 0.047(4) Uani 1 1 d . . . H41A H 0.8630 0.6093 1.3137 0.056 Uiso 1 1 calc R . . H41B H 0.8646 0.5536 1.3415 0.056 Uiso 1 1 calc R . . C411 C 1.1123(14) 0.5483(8) 1.1833(17) 0.060(5) Uani 1 1 d . . . H41C H 1.0907 0.5654 1.1186 0.090 Uiso 1 1 calc R . . H41D H 1.0839 0.5154 1.1797 0.090 Uiso 1 1 calc R . . H41E H 1.1946 0.5478 1.1904 0.090 Uiso 1 1 calc R . . C412 C 1.093(2) 0.5481(12) 1.4242(19) 0.086(8) Uani 1 1 d . . . H41F H 1.1734 0.5523 1.4373 0.129 Uiso 1 1 calc R . . H41G H 1.0753 0.5139 1.4178 0.129 Uiso 1 1 calc R . . H41H H 1.0506 0.5617 1.4831 0.129 Uiso 1 1 calc R . . C413 C 1.0963(18) 0.6415(9) 1.308(2) 0.072(6) Uani 1 1 d . . . H41I H 1.0605 0.6568 1.3684 0.108 Uiso 1 1 calc R . . H41J H 1.0744 0.6583 1.2430 0.108 Uiso 1 1 calc R . . H41K H 1.1782 0.6428 1.3172 0.108 Uiso 1 1 calc R . . C420 C 0.6530(14) 0.5506(6) 1.1907(14) 0.049(4) Uani 1 1 d . . . H42A H 0.6162 0.5277 1.1417 0.059 Uiso 1 1 calc R . . H42B H 0.6576 0.5349 1.2607 0.059 Uiso 1 1 calc R . . C421 C 0.6342(15) 0.6512(7) 1.2777(15) 0.055(4) Uani 1 1 d . . . H42C H 0.6503 0.6400 1.3496 0.083 Uiso 1 1 calc R . . H42D H 0.5868 0.6799 1.2803 0.083 Uiso 1 1 calc R . . H42E H 0.7049 0.6589 1.2427 0.083 Uiso 1 1 calc R . . C422 C 0.5155(13) 0.6240(6) 1.0701(13) 0.045(3) Uani 1 1 d . . . H42F H 0.5818 0.6344 1.0311 0.067 Uiso 1 1 calc R . . H42G H 0.4631 0.6509 1.0766 0.067 Uiso 1 1 calc R . . H42H H 0.4783 0.5978 1.0322 0.067 Uiso 1 1 calc R . . C423 C 0.4326(17) 0.5830(10) 1.2739(16) 0.073(7) Uani 1 1 d . . . H42I H 0.3878 0.5620 1.2279 0.109 Uiso 1 1 calc R . . H42J H 0.3874 0.6107 1.2940 0.109 Uiso 1 1 calc R . . H42K H 0.4560 0.5654 1.3374 0.109 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 Te1 0.0418(5) 0.0313(5) 0.0353(4) -0.0009(3) -0.0097(4) 0.0007(4) Te2 0.0586(6) 0.0299(5) 0.0358(4) -0.0005(4) -0.0085(4) 0.0017(4) Te3 0.0319(4) 0.0299(5) 0.0350(4) -0.0011(3) -0.0092(3) 0.0010(3) Te4 0.0365(4) 0.0288(5) 0.0412(5) 0.0001(4) -0.0099(4) 0.0009(3) Ag1 0.0468(5) 0.0323(6) 0.0464(6) 0.0025(4) -0.0097(5) 0.0006(4) Ag2 0.0611(7) 0.0338(6) 0.0413(6) -0.0030(5) -0.0073(5) 0.0010(5) Ag3 0.0392(5) 0.0323(5) 0.0408(5) -0.0027(4) -0.0096(4) 0.0024(4) Ag4 0.0475(6) 0.0325(6) 0.0439(6) 0.0008(4) -0.0090(5) -0.0012(5) Ag5 0.0411(5) 0.0324(6) 0.0446(6) 0.0009(4) -0.0111(4) 0.0033(4) S1 0.0361(16) 0.0343(18) 0.0398(17) 0.0012(14) -0.0110(14) -0.0024(13) S2 0.0389(16) 0.039(2) 0.0462(19) -0.0037(15) -0.0060(15) -0.0029(15) S3 0.058(2) 0.039(2) 0.0351(17) -0.0041(15) -0.0092(16) -0.0018(16) S4 0.0390(16) 0.0322(18) 0.0467(19) 0.0000(14) -0.0075(15) -0.0026(14) S5 0.052(2) 0.039(2) 0.084(3) -0.008(2) -0.028(2) 0.0009(18) Si11 0.045(2) 0.054(3) 0.045(2) 0.0045(19) -0.0059(19) 0.0011(19) Si12 0.048(2) 0.043(2) 0.043(2) -0.0017(18) -0.0130(18) -0.0048(19) Si21 0.047(2) 0.047(3) 0.053(3) -0.001(2) -0.007(2) -0.0026(19) Si22 0.056(2) 0.073(4) 0.041(2) -0.001(2) -0.005(2) 0.017(2) Si31 0.0312(16) 0.046(2) 0.0406(19) -0.0042(17) -0.0091(15) 0.0009(15) Si32 0.0320(16) 0.039(2) 0.0419(19) 0.0033(16) -0.0112(15) -0.0023(15) Si41 0.044(2) 0.045(3) 0.065(3) -0.009(2) -0.018(2) -0.0007(19) Si42 0.0390(18) 0.040(2) 0.042(2) 0.0004(16) -0.0089(17) 0.0025(16) O11 0.044(5) 0.038(6) 0.039(5) 0.001(4) -0.010(4) -0.006(4) O12 0.045(5) 0.029(5) 0.048(6) 0.009(4) -0.020(5) -0.006(4) O13 0.057(6) 0.035(6) 0.041(5) 0.000(4) -0.013(5) -0.003(5) O21 0.048(5) 0.036(5) 0.036(5) 0.006(4) -0.009(4) 0.000(4) O22 0.045(5) 0.056(7) 0.042(5) 0.006(5) -0.002(5) -0.004(5) O23 0.053(6) 0.048(7) 0.066(8) -0.018(6) -0.017(6) -0.002(5) O31 0.069(7) 0.033(6) 0.048(6) 0.008(5) -0.014(5) 0.002(5) O32 0.063(7) 0.043(6) 0.042(6) -0.008(5) -0.005(5) -0.007(5) O33 0.074(8) 0.044(7) 0.049(6) 0.004(5) 0.000(6) 0.001(6) O41 0.035(5) 0.075(9) 0.065(8) 0.007(7) -0.017(5) -0.019(5) O42 0.056(7) 0.082(10) 0.060(8) 0.003(7) -0.005(6) -0.002(7) O43 0.054(6) 0.022(6) 0.126(13) -0.007(6) 0.018(8) 0.003(5) O51 0.063(7) 0.043(7) 0.071(8) 0.001(6) -0.011(6) -0.012(6) O52 0.084(10) 0.121(16) 0.067(9) 0.000(10) -0.016(8) 0.040(11) O53 0.050(7) 0.038(8) 0.19(2) -0.001(10) 0.001(9) 0.001(6) F11 0.048(5) 0.074(8) 0.080(8) -0.001(6) 0.005(5) -0.007(5) F12 0.039(5) 0.123(12) 0.076(8) -0.009(7) -0.020(5) 0.019(6) F13 0.064(6) 0.068(9) 0.134(12) -0.044(8) 0.005(7) -0.033(6) F21 0.045(5) 0.051(6) 0.089(8) -0.003(5) 0.001(5) 0.005(4) F22 0.065(7) 0.060(8) 0.150(14) 0.042(8) -0.005(8) -0.019(6) F23 0.048(5) 0.100(10) 0.092(9) -0.011(7) -0.028(6) -0.014(6) F31 0.081(7) 0.039(5) 0.055(5) -0.003(4) -0.011(5) -0.010(5) F32 0.065(6) 0.059(7) 0.052(5) 0.008(5) -0.017(5) 0.009(5) F33 0.070(6) 0.069(7) 0.044(5) -0.003(5) 0.006(5) -0.006(5) F41 0.059(6) 0.051(7) 0.123(11) -0.001(7) -0.030(7) 0.015(5) F42 0.048(5) 0.075(8) 0.096(9) 0.018(7) 0.015(6) 0.008(5) F43 0.055(6) 0.089(10) 0.075(8) -0.004(7) -0.027(5) -0.011(6) F51 0.069(8) 0.110(13) 0.169(17) -0.073(12) -0.058(10) 0.022(8) F52 0.078(8) 0.101(12) 0.136(14) 0.054(11) -0.001(9) 0.023(8) F53 0.080(8) 0.131(13) 0.065(8) -0.010(8) 0.015(7) 0.039(9) C1 0.029(6) 0.043(9) 0.070(10) -0.010(8) -0.006(7) -0.008(6) C2 0.047(8) 0.029(8) 0.066(10) 0.007(7) -0.005(8) -0.001(6) C3 0.070(10) 0.038(9) 0.042(8) 0.001(6) -0.019(8) -0.001(7) C4 0.041(7) 0.032(8) 0.072(11) -0.009(7) -0.012(8) 0.000(6) C5 0.062(10) 0.034(9) 0.080(13) -0.007(8) -0.023(10) -0.003(8) C110 0.037(7) 0.064(10) 0.035(7) -0.001(7) -0.014(6) 0.010(7) C111 0.074(11) 0.052(11) 0.070(12) 0.006(9) -0.050(10) -0.014(9) C112 0.062(10) 0.070(13) 0.052(9) 0.014(9) -0.006(8) -0.008(9) C113 0.052(10) 0.089(18) 0.096(17) -0.040(14) 0.009(11) -0.004(10) C120 0.051(8) 0.040(8) 0.040(7) -0.001(6) -0.011(6) 0.006(6) C121 0.054(9) 0.060(12) 0.058(10) -0.003(8) -0.018(8) 0.006(8) C122 0.074(12) 0.047(11) 0.083(14) -0.013(10) -0.040(11) 0.003(9) C123 0.082(12) 0.073(14) 0.036(8) 0.006(8) -0.014(8) -0.020(10) C210 0.050(8) 0.035(8) 0.058(9) 0.011(7) 0.002(8) 0.014(6) C211 0.064(11) 0.12(2) 0.047(10) -0.007(11) 0.006(9) 0.025(12) C212 0.098(17) 0.10(2) 0.12(2) -0.051(18) 0.062(19) -0.046(16) C213 0.066(12) 0.13(2) 0.084(16) 0.003(15) -0.014(12) 0.062(15) C220 0.052(8) 0.041(9) 0.042(7) 0.003(6) -0.001(7) 0.001(7) C221 0.052(11) 0.13(3) 0.083(16) 0.006(16) -0.007(11) 0.002(13) C222 0.093(17) 0.25(5) 0.079(17) 0.11(3) -0.049(15) -0.06(2) C223 0.25(5) 0.23(5) 0.14(3) -0.15(4) -0.16(4) 0.16(4) C310 0.037(6) 0.041(8) 0.049(8) -0.019(7) -0.014(6) 0.004(6) C311 0.040(7) 0.063(11) 0.063(10) 0.000(9) 0.000(7) 0.008(7) C312 0.031(6) 0.050(10) 0.090(14) -0.006(9) -0.007(8) -0.004(7) C313 0.059(9) 0.042(9) 0.052(9) 0.008(7) -0.008(8) 0.005(8) C320 0.043(7) 0.055(10) 0.030(6) 0.008(6) -0.018(6) -0.009(7) C321 0.042(7) 0.050(9) 0.056(9) 0.004(8) 0.000(7) 0.007(7) C322 0.044(7) 0.035(8) 0.044(8) -0.007(6) -0.005(6) 0.006(6) C323 0.060(10) 0.050(10) 0.068(11) 0.011(9) -0.009(9) -0.027(8) C410 0.040(7) 0.063(11) 0.038(7) -0.001(7) 0.000(6) 0.006(7) C411 0.041(8) 0.067(13) 0.072(12) -0.024(10) -0.007(8) 0.009(8) C412 0.068(12) 0.12(2) 0.067(13) -0.009(14) -0.018(11) 0.040(14) C413 0.060(10) 0.069(15) 0.087(15) -0.024(11) -0.006(10) -0.009(10) C420 0.051(8) 0.041(9) 0.056(9) 0.014(7) -0.015(7) 0.001(7) C421 0.052(9) 0.049(10) 0.065(11) -0.008(8) -0.026(8) 0.016(8) C422 0.046(7) 0.038(8) 0.051(8) 0.010(6) -0.019(7) 0.005(6) C423 0.062(10) 0.103(18) 0.053(10) 0.047(11) -0.001(9) 0.020(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 Te1 C120 2.123(17) . ? Te1 C110 2.150(15) . ? Te1 Ag1 2.6520(15) . ? Te1 Ag3 2.7609(15) . ? Te2 C220 2.154(16) . ? Te2 C210 2.197(16) . ? Te2 Ag2 2.6430(15) . ? Te2 Ag4 2.7989(16) . ? Te3 C320 2.130(15) . ? Te3 C310 2.158(14) . ? Te3 Ag5 2.6840(14) . ? Te3 Ag3 2.7452(14) . ? Te4 C420 2.140(17) . ? Te4 C410 2.148(16) . ? Te4 Ag4 2.6726(15) . ? Te4 Ag5 2.6925(15) . ? Ag1 O31 2.366(12) . ? Ag1 O11 2.429(11) . ? Ag1 O21 2.494(11) . ? Ag2 O32 2.285(11) . ? Ag2 O21 2.517(11) . ? Ag3 O41 2.315(11) 2_747 ? Ag3 O53 2.457(16) 2_747 ? Ag4 O43 2.372(12) . ? Ag4 O51 2.383(13) . ? Ag5 O12 2.502(10) . ? Ag5 O22 2.557(11) . ? S1 O12 1.425(10) . ? S1 O13 1.430(12) . ? S1 O11 1.459(11) . ? S1 C1 1.807(14) . ? S2 O23 1.441(13) . ? S2 O22 1.451(13) . ? S2 O21 1.456(11) . ? S2 C2 1.834(16) . ? S3 O32 1.441(13) . ? S3 O33 1.445(13) . ? S3 O31 1.454(12) . ? S3 C3 1.81(2) . ? S4 O42 1.408(15) . ? S4 O43 1.434(12) . ? S4 O41 1.461(13) . ? S4 C4 1.821(16) . ? S5 O53 1.381(18) . ? S5 O51 1.393(14) . ? S5 O52 1.492(18) . ? S5 C5 1.85(2) . ? Si11 C112 1.87(2) . ? Si11 C111 1.872(19) . ? Si11 C113 1.88(2) . ? Si11 C110 1.900(18) . ? Si12 C122 1.84(2) . ? Si12 C123 1.871(19) . ? Si12 C121 1.88(2) . ? Si12 C120 1.883(16) . ? Si21 C210 1.845(17) . ? Si21 C213 1.85(2) . ? Si21 C212 1.85(3) . ? Si21 C211 1.88(2) . ? Si22 C223 1.79(3) . ? Si22 C222 1.84(3) . ? Si22 C221 1.88(2) . ? Si22 C220 1.886(17) . ? Si31 C313 1.858(19) . ? Si31 C312 1.87(2) . ? Si31 C311 1.87(2) . ? Si31 C310 1.900(15) . ? Si32 C323 1.835(18) . ? Si32 C321 1.850(17) . ? Si32 C322 1.855(15) . ? Si32 C320 1.898(14) . ? Si41 C413 1.82(2) . ? Si41 C412 1.86(3) . ? Si41 C411 1.865(19) . ? Si41 C410 1.894(16) . ? Si42 C422 1.840(16) . ? Si42 C421 1.857(19) . ? Si42 C420 1.859(18) . ? Si42 C423 1.86(2) . ? O41 Ag3 2.315(11) 2_757 ? O53 Ag3 2.457(16) 2_757 ? F11 C1 1.34(2) . ? F12 C1 1.31(2) . ? F13 C1 1.31(2) . ? F21 C2 1.32(2) . ? F22 C2 1.32(2) . ? F23 C2 1.31(2) . ? F31 C3 1.33(2) . ? F32 C3 1.37(2) . ? F33 C3 1.34(2) . ? F41 C4 1.35(2) . ? F42 C4 1.31(2) . ? F43 C4 1.35(2) . ? F51 C5 1.29(2) . ? F52 C5 1.31(3) . ? F53 C5 1.25(3) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C113 H11I 0.9800 . ? C113 H11J 0.9800 . ? C113 H11K 0.9800 . ? C120 H12A 0.9900 . ? C120 H12B 0.9900 . ? C121 H12C 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C122 H12F 0.9800 . ? C122 H12G 0.9800 . ? C122 H12H 0.9800 . ? C123 H12I 0.9800 . ? C123 H12J 0.9800 . ? C123 H12K 0.9800 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 H21C 0.9800 . ? C211 H21D 0.9800 . ? C211 H21E 0.9800 . ? C212 H21F 0.9800 . ? C212 H21G 0.9800 . ? C212 H21H 0.9800 . ? C213 H21I 0.9800 . ? C213 H21J 0.9800 . ? C213 H21K 0.9800 . ? C220 H22A 0.9900 . ? C220 H22B 0.9900 . ? C221 H22C 0.9800 . ? C221 H22D 0.9800 . ? C221 H22E 0.9800 . ? C222 H22F 0.9800 . ? C222 H22G 0.9800 . ? C222 H22H 0.9800 . ? C223 H22I 0.9800 . ? C223 H22J 0.9800 . ? C223 H22K 0.9800 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 H31C 0.9800 . ? C311 H31D 0.9800 . ? C311 H31E 0.9800 . ? C312 H31F 0.9800 . ? C312 H31G 0.9800 . ? C312 H31H 0.9800 . ? C320 H32A 0.9900 . ? C320 H32B 0.9900 . ? C321 H32C 0.9800 . ? C321 H32D 0.9800 . ? C321 H32E 0.9800 . ? C322 H32F 0.9800 . ? C322 H32G 0.9800 . ? C322 H32H 0.9800 . ? C323 H32I 0.9800 . ? C323 H32J 0.9800 . ? C323 H32K 0.9800 . ? C410 H41A 0.9900 . ? C410 H41B 0.9900 . ? C411 H41C 0.9800 . ? C411 H41D 0.9800 . ? C411 H41E 0.9800 . ? C412 H41F 0.9800 . ? C412 H41G 0.9800 . ? C412 H41H 0.9800 . ? C413 H41I 0.9800 . ? C413 H41J 0.9800 . ? C413 H41K 0.9800 . ? C420 H42A 0.9900 . ? C420 H42B 0.9900 . ? C421 H42C 0.9800 . ? C421 H42D 0.9800 . ? C421 H42E 0.9800 . ? C422 H42F 0.9800 . ? C422 H42G 0.9800 . ? C422 H42H 0.9800 . ? C423 H42I 0.9800 . ? C423 H42J 0.9800 . ? C423 H42K 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C120 Te1 C110 96.3(7) . . ? C120 Te1 Ag1 110.1(4) . . ? C110 Te1 Ag1 106.1(5) . . ? C120 Te1 Ag3 102.3(4) . . ? C110 Te1 Ag3 110.6(4) . . ? Ag1 Te1 Ag3 127.12(5) . . ? C220 Te2 C210 98.1(6) . . ? C220 Te2 Ag2 107.8(4) . . ? C210 Te2 Ag2 116.5(5) . . ? C220 Te2 Ag4 111.9(4) . . ? C210 Te2 Ag4 103.2(5) . . ? Ag2 Te2 Ag4 117.67(5) . . ? C320 Te3 C310 96.9(6) . . ? C320 Te3 Ag5 107.1(5) . . ? C310 Te3 Ag5 105.9(4) . . ? C320 Te3 Ag3 108.1(5) . . ? C310 Te3 Ag3 115.7(4) . . ? Ag5 Te3 Ag3 120.35(5) . . ? C420 Te4 C410 95.9(6) . . ? C420 Te4 Ag4 112.2(4) . . ? C410 Te4 Ag4 113.6(5) . . ? C420 Te4 Ag5 104.1(5) . . ? C410 Te4 Ag5 109.5(5) . . ? Ag4 Te4 Ag5 118.74(5) . . ? O31 Ag1 O11 89.6(4) . . ? O31 Ag1 O21 90.4(4) . . ? O11 Ag1 O21 78.0(3) . . ? O31 Ag1 Te1 115.9(3) . . ? O11 Ag1 Te1 141.3(2) . . ? O21 Ag1 Te1 127.0(2) . . ? O32 Ag2 O21 95.3(4) . . ? O32 Ag2 Te2 147.2(3) . . ? O21 Ag2 Te2 115.3(3) . . ? O41 Ag3 O53 90.0(5) 2_747 2_747 ? O41 Ag3 Te3 119.9(3) 2_747 . ? O53 Ag3 Te3 99.9(5) 2_747 . ? O41 Ag3 Te1 122.5(3) 2_747 . ? O53 Ag3 Te1 108.9(5) 2_747 . ? Te3 Ag3 Te1 109.80(5) . . ? O43 Ag4 O51 97.4(5) . . ? O43 Ag4 Te4 115.7(4) . . ? O51 Ag4 Te4 131.1(3) . . ? O43 Ag4 Te2 93.7(5) . . ? O51 Ag4 Te2 85.2(3) . . ? Te4 Ag4 Te2 124.38(5) . . ? O12 Ag5 O22 85.8(4) . . ? O12 Ag5 Te3 104.7(2) . . ? O22 Ag5 Te3 92.8(3) . . ? O12 Ag5 Te4 98.1(3) . . ? O22 Ag5 Te4 115.2(3) . . ? Te3 Ag5 Te4 145.09(5) . . ? O12 S1 O13 116.3(7) . . ? O12 S1 O11 112.4(7) . . ? O13 S1 O11 114.6(7) . . ? O12 S1 C1 104.6(8) . . ? O13 S1 C1 103.2(7) . . ? O11 S1 C1 103.7(7) . . ? O23 S2 O22 115.5(8) . . ? O23 S2 O21 115.2(7) . . ? O22 S2 O21 112.9(7) . . ? O23 S2 C2 103.6(8) . . ? O22 S2 C2 103.6(7) . . ? O21 S2 C2 104.1(8) . . ? O32 S3 O33 113.1(7) . . ? O32 S3 O31 115.2(7) . . ? O33 S3 O31 116.7(8) . . ? O32 S3 C3 104.0(8) . . ? O33 S3 C3 103.5(8) . . ? O31 S3 C3 102.0(8) . . ? O42 S4 O43 114.6(10) . . ? O42 S4 O41 115.1(8) . . ? O43 S4 O41 115.6(9) . . ? O42 S4 C4 105.2(9) . . ? O43 S4 C4 101.3(8) . . ? O41 S4 C4 102.4(8) . . ? O53 S5 O51 119.1(11) . . ? O53 S5 O52 111.2(13) . . ? O51 S5 O52 112.1(11) . . ? O53 S5 C5 103.0(9) . . ? O51 S5 C5 104.8(8) . . ? O52 S5 C5 105.0(10) . . ? C112 Si11 C111 111.5(10) . . ? C112 Si11 C113 111.7(12) . . ? C111 Si11 C113 110.7(11) . . ? C112 Si11 C110 108.2(8) . . ? C111 Si11 C110 109.6(9) . . ? C113 Si11 C110 104.8(10) . . ? C122 Si12 C123 110.5(11) . . ? C122 Si12 C121 111.1(10) . . ? C123 Si12 C121 111.0(10) . . ? C122 Si12 C120 104.9(8) . . ? C123 Si12 C120 110.6(9) . . ? C121 Si12 C120 108.6(8) . . ? C210 Si21 C213 113.2(11) . . ? C210 Si21 C212 102.8(9) . . ? C213 Si21 C212 112.7(17) . . ? C210 Si21 C211 112.1(9) . . ? C213 Si21 C211 107.6(12) . . ? C212 Si21 C211 108.5(15) . . ? C223 Si22 C222 109(3) . . ? C223 Si22 C221 113(2) . . ? C222 Si22 C221 102.4(16) . . ? C223 Si22 C220 112.5(12) . . ? C222 Si22 C220 111.4(12) . . ? C221 Si22 C220 108.4(10) . . ? C313 Si31 C312 111.3(9) . . ? C313 Si31 C311 109.2(8) . . ? C312 Si31 C311 111.2(10) . . ? C313 Si31 C310 108.2(8) . . ? C312 Si31 C310 106.3(7) . . ? C311 Si31 C310 110.5(7) . . ? C323 Si32 C321 111.2(9) . . ? C323 Si32 C322 113.2(9) . . ? C321 Si32 C322 108.2(8) . . ? C323 Si32 C320 104.1(8) . . ? C321 Si32 C320 110.9(8) . . ? C322 Si32 C320 109.3(7) . . ? C413 Si41 C412 108.8(13) . . ? C413 Si41 C411 111.8(11) . . ? C412 Si41 C411 110.6(11) . . ? C413 Si41 C410 108.5(9) . . ? C412 Si41 C410 106.8(10) . . ? C411 Si41 C410 110.2(8) . . ? C422 Si42 C421 111.8(9) . . ? C422 Si42 C420 109.6(8) . . ? C421 Si42 C420 109.2(8) . . ? C422 Si42 C423 108.6(8) . . ? C421 Si42 C423 110.9(12) . . ? C420 Si42 C423 106.4(10) . . ? S1 O11 Ag1 117.3(6) . . ? S1 O12 Ag5 125.4(6) . . ? S2 O21 Ag1 110.2(6) . . ? S2 O21 Ag2 118.9(6) . . ? Ag1 O21 Ag2 96.8(4) . . ? S2 O22 Ag5 114.7(7) . . ? S3 O31 Ag1 139.5(7) . . ? S3 O32 Ag2 134.3(7) . . ? S4 O41 Ag3 125.3(7) . 2_757 ? S4 O43 Ag4 142.9(8) . . ? S5 O51 Ag4 123.3(9) . . ? S5 O53 Ag3 117.9(11) . 2_757 ? F13 C1 F12 109.7(16) . . ? F13 C1 F11 106.3(15) . . ? F12 C1 F11 106.2(13) . . ? F13 C1 S1 112.5(11) . . ? F12 C1 S1 111.3(13) . . ? F11 C1 S1 110.5(11) . . ? F23 C2 F22 108.5(16) . . ? F23 C2 F21 109.1(14) . . ? F22 C2 F21 107.6(16) . . ? F23 C2 S2 111.3(13) . . ? F22 C2 S2 108.6(11) . . ? F21 C2 S2 111.6(11) . . ? F31 C3 F33 106.7(15) . . ? F31 C3 F32 107.3(13) . . ? F33 C3 F32 109.3(15) . . ? F31 C3 S3 111.3(13) . . ? F33 C3 S3 111.9(11) . . ? F32 C3 S3 110.2(12) . . ? F42 C4 F43 108.6(14) . . ? F42 C4 F41 107.9(15) . . ? F43 C4 F41 106.9(16) . . ? F42 C4 S4 112.5(13) . . ? F43 C4 S4 110.0(12) . . ? F41 C4 S4 110.9(11) . . ? F53 C5 F51 112.2(19) . . ? F53 C5 F52 109.4(19) . . ? F51 C5 F52 106(2) . . ? F53 C5 S5 110.5(14) . . ? F51 C5 S5 109.9(14) . . ? F52 C5 S5 108.7(14) . . ? Si11 C110 Te1 113.9(9) . . ? Si11 C110 H11A 108.8 . . ? Te1 C110 H11A 108.8 . . ? Si11 C110 H11B 108.8 . . ? Te1 C110 H11B 108.8 . . ? H11A C110 H11B 107.7 . . ? Si11 C111 H11C 109.5 . . ? Si11 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? Si11 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? Si11 C112 H11F 109.5 . . ? Si11 C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? Si11 C112 H11H 109.5 . . ? H11F C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? Si11 C113 H11I 109.5 . . ? Si11 C113 H11J 109.5 . . ? H11I C113 H11J 109.5 . . ? Si11 C113 H11K 109.5 . . ? H11I C113 H11K 109.5 . . ? H11J C113 H11K 109.5 . . ? Si12 C120 Te1 119.5(8) . . ? Si12 C120 H12A 107.4 . . ? Te1 C120 H12A 107.4 . . ? Si12 C120 H12B 107.4 . . ? Te1 C120 H12B 107.4 . . ? H12A C120 H12B 107.0 . . ? Si12 C121 H12C 109.5 . . ? Si12 C121 H12D 109.5 . . ? H12C C121 H12D 109.5 . . ? Si12 C121 H12E 109.5 . . ? H12C C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? Si12 C122 H12F 109.5 . . ? Si12 C122 H12G 109.5 . . ? H12F C122 H12G 109.5 . . ? Si12 C122 H12H 109.5 . . ? H12F C122 H12H 109.5 . . ? H12G C122 H12H 109.5 . . ? Si12 C123 H12I 109.5 . . ? Si12 C123 H12J 109.5 . . ? H12I C123 H12J 109.5 . . ? Si12 C123 H12K 109.5 . . ? H12I C123 H12K 109.5 . . ? H12J C123 H12K 109.5 . . ? Si21 C210 Te2 116.9(8) . . ? Si21 C210 H21A 108.1 . . ? Te2 C210 H21A 108.1 . . ? Si21 C210 H21B 108.1 . . ? Te2 C210 H21B 108.1 . . ? H21A C210 H21B 107.3 . . ? Si21 C211 H21C 109.5 . . ? Si21 C211 H21D 109.5 . . ? H21C C211 H21D 109.5 . . ? Si21 C211 H21E 109.5 . . ? H21C C211 H21E 109.5 . . ? H21D C211 H21E 109.5 . . ? Si21 C212 H21F 109.5 . . ? Si21 C212 H21G 109.5 . . ? H21F C212 H21G 109.5 . . ? Si21 C212 H21H 109.5 . . ? H21F C212 H21H 109.5 . . ? H21G C212 H21H 109.5 . . ? Si21 C213 H21I 109.5 . . ? Si21 C213 H21J 109.5 . . ? H21I C213 H21J 109.5 . . ? Si21 C213 H21K 109.5 . . ? H21I C213 H21K 109.5 . . ? H21J C213 H21K 109.5 . . ? Si22 C220 Te2 117.4(8) . . ? Si22 C220 H22A 107.9 . . ? Te2 C220 H22A 107.9 . . ? Si22 C220 H22B 107.9 . . ? Te2 C220 H22B 107.9 . . ? H22A C220 H22B 107.2 . . ? Si22 C221 H22C 109.5 . . ? Si22 C221 H22D 109.5 . . ? H22C C221 H22D 109.5 . . ? Si22 C221 H22E 109.5 . . ? H22C C221 H22E 109.5 . . ? H22D C221 H22E 109.5 . . ? Si22 C222 H22F 109.5 . . ? Si22 C222 H22G 109.5 . . ? H22F C222 H22G 109.5 . . ? Si22 C222 H22H 109.5 . . ? H22F C222 H22H 109.5 . . ? H22G C222 H22H 109.5 . . ? Si22 C223 H22I 109.5 . . ? Si22 C223 H22J 109.5 . . ? H22I C223 H22J 109.5 . . ? Si22 C223 H22K 109.5 . . ? H22I C223 H22K 109.5 . . ? H22J C223 H22K 109.5 . . ? Si31 C310 Te3 114.2(8) . . ? Si31 C310 H31A 108.7 . . ? Te3 C310 H31A 108.7 . . ? Si31 C310 H31B 108.7 . . ? Te3 C310 H31B 108.7 . . ? H31A C310 H31B 107.6 . . ? Si31 C311 H31C 109.5 . . ? Si31 C311 H31D 109.5 . . ? H31C C311 H31D 109.5 . . ? Si31 C311 H31E 109.5 . . ? H31C C311 H31E 109.5 . . ? H31D C311 H31E 109.5 . . ? Si31 C312 H31F 109.5 . . ? Si31 C312 H31G 109.5 . . ? H31F C312 H31G 109.5 . . ? Si31 C312 H31H 109.5 . . ? H31F C312 H31H 109.5 . . ? H31G C312 H31H 109.5 . . ? Si32 C320 Te3 115.4(7) . . ? Si32 C320 H32A 108.4 . . ? Te3 C320 H32A 108.4 . . ? Si32 C320 H32B 108.4 . . ? Te3 C320 H32B 108.4 . . ? H32A C320 H32B 107.5 . . ? Si32 C321 H32C 109.5 . . ? Si32 C321 H32D 109.5 . . ? H32C C321 H32D 109.5 . . ? Si32 C321 H32E 109.5 . . ? H32C C321 H32E 109.5 . . ? H32D C321 H32E 109.5 . . ? Si32 C322 H32F 109.5 . . ? Si32 C322 H32G 109.5 . . ? H32F C322 H32G 109.5 . . ? Si32 C322 H32H 109.5 . . ? H32F C322 H32H 109.5 . . ? H32G C322 H32H 109.5 . . ? Si32 C323 H32I 109.5 . . ? Si32 C323 H32J 109.5 . . ? H32I C323 H32J 109.5 . . ? Si32 C323 H32K 109.5 . . ? H32I C323 H32K 109.5 . . ? H32J C323 H32K 109.5 . . ? Si41 C410 Te4 115.7(7) . . ? Si41 C410 H41A 108.4 . . ? Te4 C410 H41A 108.4 . . ? Si41 C410 H41B 108.4 . . ? Te4 C410 H41B 108.4 . . ? H41A C410 H41B 107.4 . . ? Si41 C411 H41C 109.5 . . ? Si41 C411 H41D 109.5 . . ? H41C C411 H41D 109.5 . . ? Si41 C411 H41E 109.5 . . ? H41C C411 H41E 109.5 . . ? H41D C411 H41E 109.5 . . ? Si41 C412 H41F 109.5 . . ? Si41 C412 H41G 109.5 . . ? H41F C412 H41G 109.5 . . ? Si41 C412 H41H 109.5 . . ? H41F C412 H41H 109.5 . . ? H41G C412 H41H 109.5 . . ? Si41 C413 H41I 109.5 . . ? Si41 C413 H41J 109.5 . . ? H41I C413 H41J 109.5 . . ? Si41 C413 H41K 109.5 . . ? H41I C413 H41K 109.5 . . ? H41J C413 H41K 109.5 . . ? Si42 C420 Te4 118.2(8) . . ? Si42 C420 H42A 107.8 . . ? Te4 C420 H42A 107.8 . . ? Si42 C420 H42B 107.8 . . ? Te4 C420 H42B 107.8 . . ? H42A C420 H42B 107.1 . . ? Si42 C421 H42C 109.5 . . ? Si42 C421 H42D 109.5 . . ? H42C C421 H42D 109.5 . . ? Si42 C421 H42E 109.5 . . ? H42C C421 H42E 109.5 . . ? H42D C421 H42E 109.5 . . ? Si42 C422 H42F 109.5 . . ? Si42 C422 H42G 109.5 . . ? H42F C422 H42G 109.5 . . ? Si42 C422 H42H 109.5 . . ? H42F C422 H42H 109.5 . . ? H42G C422 H42H 109.5 . . ? Si42 C423 H42I 109.5 . . ? Si42 C423 H42J 109.5 . . ? H42I C423 H42J 109.5 . . ? Si42 C423 H42K 109.5 . . ? H42I C423 H42K 109.5 . . ? H42J C423 H42K 109.5 . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 2.056 _refine_diff_density_min -1.259 _refine_diff_density_rms 0.287 # start Validation Reply Form _vrf_PLAT213_cmpd7 ; PROBLEM: Atom C223 has ADP max/min Ratio ..... 5.9 prola RESPONSE: Me3Si- groups often show orientational variation due to rotational disorder. The elongation of ADP in all three carbo atoms C221 C222 C223 is consistent with this inference. ; _vrf_PLAT029_cmpd7 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.945 RESPONSE: The completeness is sufficient (> 0.9) ; _vrf_PLAT220_cmpd7 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.1 Ratio RESPONSE: This is due to orientational disorder. ; _vrf_PLAT242_cmpd7 ; PROBLEM: Check Low Ueq as Compared to Neighbors for Si22 RESPONSE: This is due to orientational disorder. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 949151' ####################################################################### # # 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_cmpd8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly{[mu-bis(trimethylsilylmethyl)tellane]silver trifluoro- methylsulfonate} ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H132 Ag6 F18 O18 S6 Si12 Te6' _chemical_formula_weight 3353.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 30.819(6) _cell_length_b 16.649(3) _cell_length_c 22.780(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.28(3) _cell_angle_gamma 90.00 _cell_volume 11679(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 15151 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6480 _exptl_absorpt_coefficient_mu 2.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6081 _exptl_absorpt_correction_T_max 0.7697 _exptl_absorpt_process_details 'XPREP in SHELXTL (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 Nonius kappaccd' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20411 _diffrn_reflns_av_R_equivalents 0.1220 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20411 _reflns_number_gt 15151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker, 2008)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Branderburg, 2006)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. Some parts of the structure are disordered. In order to achive convergence in the least-squares refinement, some bond lengths and angles had to be restrained (23 restraints). These restraints do not involve silver or tellurium atoms. ; _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^)+(0.0696P)^2^+171.4277P] 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 SHELXL _refine_ls_extinction_coef 0.00064(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 20411 _refine_ls_number_parameters 1073 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.1956 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 C1 C 0.4814(4) -0.1781(8) 0.8932(6) 0.050(3) Uani 1 1 d . . . C2 C 0.7433(4) 0.0775(8) 0.9370(6) 0.049(3) Uani 1 1 d . . . C3 C 0.6883(5) -0.0089(8) 0.6056(6) 0.056(4) Uani 1 1 d . . . C4 C 0.7670(4) 0.5886(9) 0.9421(6) 0.052(3) Uani 1 1 d . . . C5 C 0.7938(5) 0.5210(9) 0.6102(6) 0.053(3) Uani 1 1 d . . . C110 C 0.6824(4) -0.1753(7) 0.9211(5) 0.035(3) Uani 1 1 d . . . H11A H 0.7004 -0.2241 0.9265 0.042 Uiso 1 1 calc R . . H11B H 0.7011 -0.1288 0.9321 0.042 Uiso 1 1 calc R . . C111 C 0.6022(5) -0.2682(9) 0.9605(7) 0.057(4) Uani 1 1 d . . . H11C H 0.6200 -0.3170 0.9591 0.085 Uiso 1 1 calc . . . H11D H 0.5862 -0.2612 0.9229 0.085 Uiso 1 1 calc . . . H11E H 0.5817 -0.2730 0.9921 0.085 Uiso 1 1 calc . . . C112 C 0.6069(5) -0.0837(9) 0.9701(6) 0.056(4) Uani 1 1 d . . . H11F H 0.5943 -0.0769 0.9302 0.084 Uiso 1 1 calc . . . H11G H 0.6266 -0.0389 0.9795 0.084 Uiso 1 1 calc . . . H11H H 0.5836 -0.0847 0.9982 0.084 Uiso 1 1 calc . . . C113 C 0.6668(6) -0.1889(13) 1.0476(6) 0.078(5) Uani 1 1 d . . . H11I H 0.6456 -0.1949 1.0782 0.117 Uiso 1 1 calc . . . H11J H 0.6842 -0.1404 1.0552 0.117 Uiso 1 1 calc . . . H11K H 0.6860 -0.2359 1.0479 0.117 Uiso 1 1 calc . . . C120 C 0.6516(4) -0.2891(7) 0.8137(5) 0.039(3) Uani 1 1 d . . . H12A H 0.6741 -0.3220 0.8345 0.047 Uiso 1 1 calc R . . H12B H 0.6233 -0.3024 0.8302 0.047 Uiso 1 1 calc R . . C121 C 0.6420(5) -0.4275(9) 0.7279(7) 0.060(4) Uani 1 1 d . . . H12C H 0.6371 -0.4423 0.6865 0.090 Uiso 1 1 calc . . . H12D H 0.6169 -0.4435 0.7501 0.090 Uiso 1 1 calc . . . H12E H 0.6680 -0.4550 0.7438 0.090 Uiso 1 1 calc . . . C122 C 0.7022(4) -0.2910(9) 0.7036(6) 0.048(3) Uani 1 1 d . . . H12F H 0.7050 -0.3184 0.6659 0.072 Uiso 1 1 calc . . . H12G H 0.7258 -0.3081 0.7310 0.072 Uiso 1 1 calc . . . H12H H 0.7039 -0.2328 0.6977 0.072 Uiso 1 1 calc . . . C123 C 0.6041(5) -0.2618(10) 0.6971(6) 0.059(4) Uani 1 1 d . . . H12I H 0.6121 -0.2052 0.6923 0.089 Uiso 1 1 calc . . . H12J H 0.5785 -0.2654 0.7211 0.089 Uiso 1 1 calc . . . H12K H 0.5976 -0.2857 0.6585 0.089 Uiso 1 1 calc . . . C210 C 0.8550(5) -0.1240(9) 0.7102(6) 0.052(3) Uani 1 1 d . . . H21A H 0.8443 -0.0680 0.7103 0.063 Uiso 1 1 calc R . . H21B H 0.8868 -0.1222 0.7187 0.063 Uiso 1 1 calc R . . C211 C 0.8739(4) -0.2636(9) 0.6284(6) 0.052(3) Uani 1 1 d . . . H21C H 0.8603 -0.3031 0.6537 0.078 Uiso 1 1 calc . . . H21D H 0.9044 -0.2565 0.6411 0.078 Uiso 1 1 calc . . . H21E H 0.8721 -0.2826 0.5876 0.078 Uiso 1 1 calc . . . C212 C 0.7869(5) -0.1825(13) 0.6186(7) 0.081(6) Uani 1 1 d . . . H21F H 0.7825 -0.2138 0.5824 0.121 Uiso 1 1 calc . . . H21G H 0.7724 -0.1304 0.6139 0.121 Uiso 1 1 calc . . . H21H H 0.7747 -0.2116 0.6514 0.121 Uiso 1 1 calc . . . C213 C 0.8669(6) -0.0886(9) 0.5846(7) 0.069(5) Uani 1 1 d . . . H21I H 0.8594 -0.1022 0.5436 0.103 Uiso 1 1 calc . . . H21J H 0.8986 -0.0861 0.5903 0.103 Uiso 1 1 calc . . . H21K H 0.8543 -0.0364 0.5940 0.103 Uiso 1 1 calc . . . C220 C 0.8607(5) -0.1206(10) 0.8472(6) 0.060(4) Uani 1 1 d . . . H22A H 0.8918 -0.1209 0.8377 0.072 Uiso 1 1 calc R . . H22B H 0.8507 -0.0641 0.8448 0.072 Uiso 1 1 calc R . . C221 C 0.7990(5) -0.1563(9) 0.9478(7) 0.056(4) Uani 1 1 d . . . H22C H 0.7978 -0.1635 0.9904 0.084 Uiso 1 1 calc . . . H22D H 0.7836 -0.2004 0.9276 0.084 Uiso 1 1 calc . . . H22E H 0.7853 -0.1051 0.9365 0.084 Uiso 1 1 calc . . . C222 C 0.8801(5) -0.2585(13) 0.9346(8) 0.085(6) Uani 1 1 d . . . H22F H 0.8826 -0.2728 0.9764 0.128 Uiso 1 1 calc . . . H22G H 0.9090 -0.2594 0.9180 0.128 Uiso 1 1 calc . . . H22H H 0.8612 -0.2972 0.9138 0.128 Uiso 1 1 calc . . . C223 C 0.8899(6) -0.0828(14) 0.9709(7) 0.099(8) Uani 1 1 d . . . H22I H 0.8786 -0.0284 0.9644 0.148 Uiso 1 1 calc . . . H22J H 0.9201 -0.0853 0.9589 0.148 Uiso 1 1 calc . . . H22K H 0.8887 -0.0965 1.0126 0.148 Uiso 1 1 calc . . . C310 C 0.9838(6) 0.5840(14) 0.7945(8) 0.094(7) Uani 1 1 d . . . H31A H 1.0037 0.5386 0.7875 0.112 Uiso 1 1 calc R . . H31B H 0.9929 0.6295 0.7699 0.112 Uiso 1 1 calc R . . C311 C 0.9506(5) 0.5643(10) 0.9194(7) 0.061(4) Uani 1 1 d . . . H31C H 0.9571 0.5067 0.9219 0.092 Uiso 1 1 calc . . . H31D H 0.9212 0.5720 0.9023 0.092 Uiso 1 1 calc . . . H31E H 0.9525 0.5878 0.9589 0.092 Uiso 1 1 calc . . . C312 C 0.9832(17) 0.7224(15) 0.872(2) 0.33(4) Uani 1 1 d . . . H31F H 0.9698 0.7392 0.9086 0.495 Uiso 1 1 calc . . . H31G H 0.9644 0.7379 0.8384 0.495 Uiso 1 1 calc . . . H31H H 1.0115 0.7485 0.8696 0.495 Uiso 1 1 calc . . . C313 C 1.0440(8) 0.580(3) 0.8957(11) 0.24(3) Uani 1 1 d . . . H31I H 1.0649 0.5975 0.8670 0.367 Uiso 1 1 calc . . . H31J H 1.0443 0.5214 0.8985 0.367 Uiso 1 1 calc . . . H31K H 1.0520 0.6033 0.9342 0.367 Uiso 1 1 calc . . . C320 C 0.9325(5) 0.5519(11) 0.6744(7) 0.072(5) Uani 1 1 d . A . H32A H 0.9044 0.5488 0.6520 0.086 Uiso 1 1 calc R . . H32B H 0.9453 0.6050 0.6660 0.086 Uiso 1 1 calc R . . C410 C 0.8168(10) 0.280(2) 0.9002(10) 0.20(2) Uani 1 1 d . . . H41A H 0.7855 0.2755 0.9078 0.237 Uiso 1 1 calc R . . H41B H 0.8270 0.2253 0.8917 0.237 Uiso 1 1 calc R . . C411 C 0.8745(6) 0.4033(11) 0.9615(8) 0.077(5) Uani 1 1 d . . . H41C H 0.9002 0.3931 0.9387 0.115 Uiso 1 1 calc . . . H41D H 0.8836 0.4226 1.0007 0.115 Uiso 1 1 calc . . . H41E H 0.8563 0.4440 0.9416 0.115 Uiso 1 1 calc . . . C412 C 0.8761(9) 0.2269(16) 0.992(3) 0.27(3) Uani 1 1 d . . . H41F H 0.8585 0.1869 1.0120 0.404 Uiso 1 1 calc . . . H41G H 0.8990 0.2466 1.0197 0.404 Uiso 1 1 calc . . . H41H H 0.8894 0.2021 0.9583 0.404 Uiso 1 1 calc . . . C413 C 0.7972(11) 0.321(2) 1.0184(13) 0.21(2) Uani 1 1 d . . . H41I H 0.7787 0.3656 1.0045 0.310 Uiso 1 1 calc . . . H41J H 0.8087 0.3325 1.0582 0.310 Uiso 1 1 calc . . . H41K H 0.7799 0.2715 1.0188 0.310 Uiso 1 1 calc . . . C420 C 0.8113(5) 0.2482(12) 0.7612(10) 0.090(7) Uani 1 1 d . . . H42A H 0.7858 0.2183 0.7749 0.109 Uiso 1 1 calc R . . H42B H 0.8017 0.2738 0.7237 0.109 Uiso 1 1 calc R . . C421 C 0.8688(10) 0.1106(16) 0.8044(16) 0.176(16) Uani 1 1 d . . . H42C H 0.8988 0.1255 0.8153 0.264 Uiso 1 1 calc . . . H42D H 0.8676 0.0539 0.7930 0.264 Uiso 1 1 calc . . . H42E H 0.8505 0.1194 0.8380 0.264 Uiso 1 1 calc . . . C422 C 0.8192(9) 0.1022(11) 0.6901(11) 0.123(10) Uani 1 1 d . . . H42F H 0.8068 0.0583 0.7127 0.184 Uiso 1 1 calc . . . H42G H 0.8395 0.0802 0.6623 0.184 Uiso 1 1 calc . . . H42H H 0.7958 0.1309 0.6685 0.184 Uiso 1 1 calc . . . C423 C 0.9005(10) 0.222(3) 0.7166(15) 0.21(2) Uani 1 1 d . . . H42I H 0.8933 0.2623 0.6865 0.317 Uiso 1 1 calc . . . H42J H 0.9192 0.1807 0.7002 0.317 Uiso 1 1 calc . . . H42K H 0.9157 0.2477 0.7502 0.317 Uiso 1 1 calc . . . C510 C 0.6392(4) 0.3534(8) 0.6943(5) 0.043(3) Uani 1 1 d . . . H51A H 0.6110 0.3250 0.6916 0.052 Uiso 1 1 calc R . . H51B H 0.6330 0.4118 0.6939 0.052 Uiso 1 1 calc R . . C511 C 0.7269(4) 0.3009(8) 0.6451(6) 0.048(3) Uani 1 1 d . . . H51C H 0.7278 0.2524 0.6696 0.072 Uiso 1 1 calc . . . H51D H 0.7414 0.3451 0.6665 0.072 Uiso 1 1 calc . . . H51E H 0.7418 0.2905 0.6087 0.072 Uiso 1 1 calc . . . C512 C 0.6646(6) 0.4197(11) 0.5816(8) 0.080(5) Uani 1 1 d . . . H51F H 0.6841 0.4156 0.5488 0.120 Uiso 1 1 calc . . . H51G H 0.6724 0.4669 0.6054 0.120 Uiso 1 1 calc . . . H51H H 0.6346 0.4249 0.5664 0.120 Uiso 1 1 calc . . . C513 C 0.6437(5) 0.2412(10) 0.5919(8) 0.069(5) Uani 1 1 d . . . H51I H 0.6460 0.1948 0.6184 0.103 Uiso 1 1 calc . . . H51J H 0.6581 0.2289 0.5555 0.103 Uiso 1 1 calc . . . H51K H 0.6130 0.2532 0.5830 0.103 Uiso 1 1 calc . . . C520 C 0.6192(4) 0.3580(8) 0.8330(5) 0.044(3) Uani 1 1 d . . . H52A H 0.6009 0.3978 0.8113 0.052 Uiso 1 1 calc R . . H52B H 0.6010 0.3100 0.8394 0.052 Uiso 1 1 calc R . . C521 C 0.5906(4) 0.3833(8) 0.9576(6) 0.046(3) Uani 1 1 d . . . H52C H 0.5626 0.3968 0.9380 0.069 Uiso 1 1 calc . . . H52D H 0.5951 0.4169 0.9926 0.069 Uiso 1 1 calc . . . H52E H 0.5907 0.3266 0.9690 0.069 Uiso 1 1 calc . . . C522 C 0.6412(5) 0.5123(9) 0.8987(6) 0.059(4) Uani 1 1 d . . . H52F H 0.6134 0.5359 0.8850 0.089 Uiso 1 1 calc . . . H52G H 0.6633 0.5237 0.8701 0.089 Uiso 1 1 calc . . . H52H H 0.6501 0.5356 0.9368 0.089 Uiso 1 1 calc . . . C523 C 0.6867(4) 0.3549(9) 0.9340(6) 0.052(3) Uani 1 1 d . . . H52I H 0.6927 0.3709 0.9749 0.078 Uiso 1 1 calc . . . H52J H 0.7104 0.3728 0.9098 0.078 Uiso 1 1 calc . . . H52K H 0.6841 0.2962 0.9317 0.078 Uiso 1 1 calc . . . C610 C 0.5387(4) 0.1476(8) 0.8129(5) 0.041(3) Uani 1 1 d . . . H61A H 0.5422 0.2045 0.8014 0.049 Uiso 1 1 calc R . . H61B H 0.5103 0.1291 0.7961 0.049 Uiso 1 1 calc R . . C611 C 0.5936(5) 0.1466(9) 0.9274(6) 0.057(4) Uani 1 1 d . . . H61C H 0.5929 0.1449 0.9703 0.086 Uiso 1 1 calc . . . H61D H 0.6074 0.1966 0.9153 0.086 Uiso 1 1 calc . . . H61E H 0.6101 0.1007 0.9134 0.086 Uiso 1 1 calc . . . C612 C 0.5056(5) 0.2309(9) 0.9186(7) 0.059(4) Uani 1 1 d . . . H61F H 0.4754 0.2256 0.9039 0.088 Uiso 1 1 calc . . . H61G H 0.5182 0.2798 0.9026 0.088 Uiso 1 1 calc . . . H61H H 0.5064 0.2340 0.9616 0.088 Uiso 1 1 calc . . . C613 C 0.5100(5) 0.0490(9) 0.9166(7) 0.062(4) Uani 1 1 d . . . H61I H 0.4797 0.0499 0.9019 0.093 Uiso 1 1 calc . . . H61J H 0.5110 0.0442 0.9595 0.093 Uiso 1 1 calc . . . H61K H 0.5249 0.0029 0.8997 0.093 Uiso 1 1 calc . . . C620 C 0.5659(4) 0.0952(8) 0.6855(5) 0.042(3) Uani 1 1 d . . . H62A H 0.5555 0.1512 0.6813 0.050 Uiso 1 1 calc R . . H62B H 0.5909 0.0891 0.6599 0.050 Uiso 1 1 calc R . . C621 C 0.5039(5) 0.0643(10) 0.5815(7) 0.067(4) Uani 1 1 d . . . H62C H 0.4821 0.0279 0.5638 0.100 Uiso 1 1 calc . . . H62D H 0.5291 0.0666 0.5568 0.100 Uiso 1 1 calc . . . H62E H 0.4914 0.1182 0.5849 0.100 Uiso 1 1 calc . . . C622 C 0.5425(6) -0.0784(10) 0.6520(10) 0.084(6) Uani 1 1 d . . . H62F H 0.5606 -0.0904 0.6873 0.126 Uiso 1 1 calc . . . H62G H 0.5600 -0.0837 0.6172 0.126 Uiso 1 1 calc . . . H62H H 0.5181 -0.1162 0.6491 0.126 Uiso 1 1 calc . . . C623 C 0.4742(5) 0.0288(9) 0.7044(7) 0.061(4) Uani 1 1 d . . . H62I H 0.4822 0.0039 0.7423 0.092 Uiso 1 1 calc . . . H62J H 0.4499 -0.0009 0.6856 0.092 Uiso 1 1 calc . . . H62K H 0.4654 0.0846 0.7108 0.092 Uiso 1 1 calc . . . O11 O 0.5322(3) -0.2534(6) 0.8244(4) 0.053(2) Uani 1 1 d . . . O12 O 0.4628(3) -0.2054(6) 0.7847(4) 0.059(3) Uani 1 1 d . . . O13 O 0.5195(3) -0.1100(6) 0.8098(4) 0.050(2) Uani 1 1 d . . . O21 O 0.7626(3) -0.0045(5) 0.8464(4) 0.044(2) Uani 1 1 d . . . O22 O 0.7316(4) 0.1289(6) 0.8318(4) 0.064(3) Uani 1 1 d . A . O23 O 0.6858(3) 0.0201(6) 0.8625(5) 0.058(3) Uani 1 1 d . . . O31 O 0.6950(3) 0.0881(6) 0.6938(4) 0.056(2) Uani 1 1 d . A . O32 O 0.7316(3) -0.0409(5) 0.7025(4) 0.048(2) Uani 1 1 d . . . O33 O 0.6528(3) -0.0334(6) 0.7049(4) 0.055(2) Uani 1 1 d . . . O41 O 0.7632(3) 0.6836(5) 0.8531(4) 0.053(2) Uani 1 1 d . . . O42 O 0.8148(3) 0.5718(6) 0.8506(4) 0.050(2) Uani 1 1 d . . . O43 O 0.7375(3) 0.5475(6) 0.8388(4) 0.057(3) Uani 1 1 d . A . O51 O 0.8315(3) 0.4694(6) 0.7057(4) 0.053(2) Uani 1 1 d . . . O52 O 0.7531(3) 0.4923(5) 0.7050(4) 0.044(2) Uani 1 1 d . A . O53 O 0.8031(3) 0.6053(5) 0.7042(4) 0.048(2) Uani 1 1 d . . . F11 F 0.5131(3) -0.1564(5) 0.9320(4) 0.063(2) Uani 1 1 d . . . F12 F 0.4503(3) -0.1239(5) 0.8961(4) 0.062(2) Uani 1 1 d . . . F13 F 0.4653(3) -0.2480(5) 0.9127(4) 0.069(2) Uani 1 1 d . . . F21 F 0.7365(3) 0.0162(4) 0.9713(3) 0.0544(19) Uani 1 1 d . . . F22 F 0.7852(3) 0.0979(6) 0.9439(4) 0.070(2) Uani 1 1 d . . . F23 F 0.7204(3) 0.1393(5) 0.9545(4) 0.072(3) Uani 1 1 d . . . F31 F 0.7230(3) 0.0211(6) 0.5812(4) 0.081(3) Uani 1 1 d . . . F32 F 0.6534(3) 0.0285(6) 0.5828(4) 0.078(3) Uani 1 1 d . . . F33 F 0.6854(3) -0.0864(6) 0.5909(4) 0.074(3) Uani 1 1 d . . . F41 F 0.7704(4) 0.5147(7) 0.9579(5) 0.101(4) Uani 1 1 d . . . F42 F 0.7298(3) 0.6165(6) 0.9585(4) 0.071(2) Uani 1 1 d . . . F43 F 0.7977(3) 0.6307(8) 0.9694(4) 0.091(3) Uani 1 1 d . . . F51 F 0.8301(3) 0.5482(7) 0.5895(4) 0.078(3) Uani 1 1 d . . . F52 F 0.7615(3) 0.5660(6) 0.5892(3) 0.065(2) Uani 1 1 d . . . F53 F 0.7861(3) 0.4480(5) 0.5889(4) 0.067(2) Uani 1 1 d . . . Si11 Si 0.63784(11) -0.1804(2) 0.97466(15) 0.0421(8) Uani 1 1 d . . . Si12 Si 0.64989(10) -0.3164(2) 0.73396(15) 0.0376(7) Uani 1 1 d . . . Si21 Si 0.84510(11) -0.1666(2) 0.63348(15) 0.0436(8) Uani 1 1 d . . . Si22 Si 0.85646(11) -0.1556(3) 0.92663(16) 0.0477(9) Uani 1 1 d . . . Si31 Si 0.99026(13) 0.6139(3) 0.8727(2) 0.0660(13) Uani 1 1 d . . . Si32 Si 0.96883(16) 0.4738(3) 0.6447(2) 0.0689(12) Uani 1 1 d D . . Si41 Si 0.84276(13) 0.3080(3) 0.96841(17) 0.0534(10) Uani 1 1 d . . . Si42 Si 0.84875(16) 0.1737(3) 0.7417(2) 0.0634(12) Uani 1 1 d . . . Si51 Si 0.66983(11) 0.3284(2) 0.62751(14) 0.0373(7) Uani 1 1 d . . . Si52 Si 0.63483(10) 0.4017(2) 0.90650(14) 0.0364(7) Uani 1 1 d . . . Si61 Si 0.53717(12) 0.1424(2) 0.89542(15) 0.0414(8) Uani 1 1 d . . . Si62 Si 0.52121(12) 0.0267(2) 0.65651(18) 0.0493(9) Uani 1 1 d . . . S1 S 0.50128(10) -0.1883(2) 0.81981(15) 0.0438(7) Uani 1 1 d . . . S2 S 0.72968(10) 0.05290(19) 0.86093(14) 0.0419(7) Uani 1 1 d . . . S3 S 0.69208(11) 0.0020(2) 0.68540(13) 0.0431(7) Uani 1 1 d . . . S4 S 0.77146(10) 0.5992(2) 0.86229(13) 0.0398(7) Uani 1 1 d . . . S5 S 0.79578(9) 0.52104(19) 0.68988(13) 0.0374(7) Uani 1 1 d . . . Ag1 Ag 0.59234(3) -0.07987(5) 0.80784(4) 0.0382(2) Uani 1 1 d . . . Ag2 Ag 0.74376(3) -0.12704(6) 0.78523(4) 0.0393(2) Uani 1 1 d . . . Ag3 Ag 0.85506(3) 0.65899(6) 0.77845(4) 0.0443(3) Uani 1 1 d . . . Ag4 Ag 0.90190(3) 0.40052(6) 0.80654(5) 0.0463(3) Uani 1 1 d . . . Ag5 Ag 0.74211(3) 0.42055(6) 0.79454(5) 0.0461(3) Uani 1 1 d . . . Ag6 Ag 0.66485(3) 0.16150(5) 0.77506(4) 0.0420(2) Uani 1 1 d . . . Te1 Te 0.66532(2) -0.16490(4) 0.82929(3) 0.03138(19) Uani 1 1 d . . . Te2 Te 0.82552(2) -0.18794(5) 0.78038(3) 0.0379(2) Uani 1 1 d . . . Te3 Te 0.91929(2) 0.54897(6) 0.76565(4) 0.0490(3) Uani 1 1 d . A . Te4 Te 0.82021(3) 0.34412(5) 0.82131(3) 0.0389(2) Uani 1 1 d . A . Te5 Te 0.67126(2) 0.32357(4) 0.77786(3) 0.03157(19) Uani 1 1 d . A . Te6 Te 0.58885(2) 0.07870(5) 0.77420(3) 0.0364(2) Uani 1 1 d . A . C6A C 1.0012(8) 0.2945(14) 0.9209(5) 0.092(7) Uani 0.627(6) 1 d PD A 1 F61A F 0.9809(7) 0.3496(14) 0.9533(10) 0.109(4) Uani 0.627(6) 1 d PD A 1 F62A F 0.9886(6) 0.2212(14) 0.9384(9) 0.109(4) Uani 0.627(6) 1 d PD A 1 F63A F 1.0434(7) 0.2970(15) 0.9381(13) 0.109(4) Uani 0.627(6) 1 d PD A 1 S6A S 0.9951(2) 0.3074(4) 0.8422(4) 0.0698(19) Uani 0.627(6) 1 d PD A 1 O61A O 0.9482(3) 0.3024(14) 0.8354(11) 0.101(4) Uani 0.627(6) 1 d PD A 1 O62A O 1.0127(6) 0.3864(8) 0.8343(11) 0.101(4) Uani 0.627(6) 1 d PD A 1 O63A O 1.0191(7) 0.2437(12) 0.8155(12) 0.101(4) Uani 0.627(6) 1 d PD A 1 C6B C 1.0058(9) 0.2864(19) 0.9307(9) 0.092(7) Uani 0.373(6) 1 d PD A 2 F61B F 0.9798(11) 0.315(2) 0.9720(18) 0.109(4) Uani 0.373(6) 1 d PD A 2 F62B F 1.0171(10) 0.2117(18) 0.9482(15) 0.109(4) Uani 0.373(6) 1 d PD A 2 F63B F 1.0425(11) 0.330(2) 0.929(2) 0.109(4) Uani 0.373(6) 1 d PD A 2 S6B S 0.9768(4) 0.2739(7) 0.8606(6) 0.0698(19) Uani 0.373(6) 1 d PD A 2 O61B O 0.9356(6) 0.238(2) 0.8749(17) 0.101(4) Uani 0.373(6) 1 d PD A 2 O62B O 0.9722(11) 0.3565(12) 0.8416(18) 0.101(4) Uani 0.373(6) 1 d PD A 2 O63B O 1.0050(11) 0.224(2) 0.8265(19) 0.101(4) Uani 0.373(6) 1 d PD A 2 C31A C 0.9811(13) 0.504(2) 0.5688(8) 0.120(7) Uani 0.616(18) 1 d PD B 3 H1AA H 0.9557 0.4938 0.5425 0.180 Uiso 0.62 1 calc P B 3 H1BA H 1.0059 0.4728 0.5556 0.180 Uiso 0.62 1 calc P B 3 H1CA H 0.9883 0.5614 0.5681 0.180 Uiso 0.62 1 calc P B 3 C32A C 0.9312(9) 0.3866(14) 0.6449(19) 0.120(7) Uani 0.616(18) 1 d PD B 3 H2AA H 0.9045 0.3999 0.6221 0.180 Uiso 0.62 1 calc P B 3 H2BA H 0.9241 0.3739 0.6854 0.180 Uiso 0.62 1 calc P B 3 H2CA H 0.9452 0.3401 0.6272 0.180 Uiso 0.62 1 calc P B 3 C33A C 1.0165(9) 0.460(2) 0.6962(14) 0.120(7) Uani 0.616(18) 1 d PD B 3 H3AA H 1.0127 0.4106 0.7190 0.180 Uiso 0.62 1 calc P B 3 H3BA H 1.0190 0.5059 0.7228 0.180 Uiso 0.62 1 calc P B 3 H3CA H 1.0429 0.4555 0.6738 0.180 Uiso 0.62 1 calc P B 3 C31B C 0.9517(19) 0.425(4) 0.5739(18) 0.120(7) Uani 0.384(18) 1 d PD B 4 H1AB H 0.9200 0.4211 0.5712 0.180 Uiso 0.38 1 calc P B 4 H1BB H 0.9646 0.3716 0.5720 0.180 Uiso 0.38 1 calc P B 4 H1CB H 0.9617 0.4579 0.5412 0.180 Uiso 0.38 1 calc P B 4 C32B C 1.0183(11) 0.534(3) 0.632(3) 0.120(7) Uani 0.384(18) 1 d PD B 4 H2AB H 1.0150 0.5615 0.5936 0.180 Uiso 0.38 1 calc P B 4 H2BB H 1.0437 0.4987 0.6315 0.180 Uiso 0.38 1 calc P B 4 H2CB H 1.0224 0.5742 0.6629 0.180 Uiso 0.38 1 calc P B 4 C33B C 0.994(2) 0.389(3) 0.687(2) 0.120(7) Uani 0.384(18) 1 d PD B 4 H3AB H 0.9740 0.3434 0.6867 0.180 Uiso 0.38 1 calc P B 4 H3BB H 0.9998 0.4063 0.7281 0.180 Uiso 0.38 1 calc P B 4 H3CB H 1.0212 0.3736 0.6698 0.180 Uiso 0.38 1 calc P B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.045(7) 0.044(8) 0.061(9) 0.003(7) 0.007(7) -0.005(6) C2 0.049(8) 0.046(8) 0.052(8) 0.004(7) 0.003(6) 0.004(6) C3 0.090(11) 0.040(8) 0.037(7) 0.000(6) -0.007(8) 0.019(8) C4 0.049(8) 0.069(10) 0.037(7) 0.008(7) 0.003(6) -0.008(7) C5 0.055(8) 0.064(10) 0.039(7) 0.000(7) 0.001(6) 0.003(7) C110 0.032(6) 0.045(7) 0.028(6) -0.005(5) 0.003(5) 0.003(5) C111 0.054(8) 0.053(9) 0.065(10) 0.009(7) 0.015(7) 0.003(7) C112 0.055(8) 0.056(9) 0.057(9) -0.018(7) 0.007(7) 0.017(7) C113 0.087(12) 0.115(15) 0.031(8) 0.012(9) -0.001(8) 0.005(11) C120 0.049(7) 0.036(7) 0.033(6) -0.003(5) 0.003(5) 0.003(6) C121 0.074(10) 0.050(8) 0.057(9) -0.015(7) 0.007(8) 0.003(7) C122 0.041(7) 0.064(9) 0.039(7) -0.002(6) 0.005(5) -0.007(6) C123 0.050(8) 0.080(11) 0.048(8) -0.014(8) -0.008(6) 0.010(8) C210 0.060(9) 0.048(8) 0.050(8) -0.004(7) 0.013(7) -0.009(7) C211 0.055(8) 0.057(9) 0.045(8) 0.009(7) 0.021(6) -0.003(7) C212 0.048(9) 0.134(17) 0.061(10) 0.005(11) 0.013(8) 0.029(10) C213 0.111(13) 0.053(9) 0.044(8) 0.005(7) 0.024(8) 0.021(9) C220 0.055(8) 0.076(11) 0.048(8) -0.018(8) 0.006(7) -0.011(8) C221 0.055(8) 0.050(8) 0.064(10) -0.013(7) 0.005(7) -0.003(7) C222 0.047(9) 0.118(16) 0.088(13) -0.011(11) -0.025(9) 0.026(10) C223 0.103(14) 0.16(2) 0.033(8) -0.014(10) 0.004(8) -0.092(14) C310 0.061(11) 0.133(19) 0.086(14) 0.034(13) -0.015(9) -0.017(11) C311 0.058(9) 0.062(10) 0.064(10) -0.018(8) -0.001(7) -0.008(7) C312 0.50(7) 0.066(15) 0.45(7) -0.12(3) 0.42(6) -0.12(3) C313 0.060(14) 0.59(8) 0.081(18) 0.06(3) 0.003(12) 0.04(3) C320 0.038(7) 0.107(14) 0.072(11) 0.040(10) 0.020(7) 0.020(8) C410 0.23(3) 0.28(4) 0.078(15) 0.10(2) -0.066(18) -0.20(3) C411 0.085(12) 0.071(11) 0.074(12) -0.011(9) 0.002(9) -0.030(9) C412 0.10(2) 0.077(17) 0.62(9) 0.07(3) -0.14(3) -0.009(15) C413 0.23(3) 0.25(4) 0.15(2) -0.09(2) 0.16(3) -0.17(3) C420 0.050(9) 0.085(13) 0.135(18) -0.046(12) -0.017(10) 0.014(9) C421 0.17(3) 0.100(19) 0.25(4) -0.03(2) -0.13(3) 0.062(18) C422 0.17(2) 0.052(11) 0.14(2) -0.048(12) -0.063(17) 0.038(13) C423 0.14(2) 0.32(5) 0.19(3) -0.13(3) 0.12(2) -0.10(3) C510 0.062(8) 0.042(7) 0.026(6) -0.012(5) 0.000(5) 0.008(6) C511 0.050(8) 0.046(8) 0.048(8) -0.007(6) 0.001(6) -0.002(6) C512 0.077(11) 0.088(13) 0.077(12) 0.039(10) 0.028(9) 0.017(10) C513 0.071(10) 0.059(10) 0.076(11) -0.035(9) -0.004(8) 0.002(8) C520 0.045(7) 0.045(7) 0.041(7) -0.013(6) 0.004(6) -0.006(6) C521 0.045(7) 0.050(8) 0.045(7) -0.001(6) 0.022(6) -0.002(6) C522 0.078(10) 0.048(8) 0.054(9) -0.018(7) 0.020(8) -0.024(7) C523 0.053(8) 0.073(10) 0.031(7) 0.001(7) 0.001(6) 0.007(7) C610 0.043(7) 0.043(7) 0.037(7) 0.003(6) 0.003(5) 0.006(6) C611 0.066(9) 0.060(9) 0.045(8) -0.004(7) -0.006(7) 0.017(7) C612 0.066(9) 0.041(8) 0.068(10) -0.005(7) -0.010(8) 0.011(7) C613 0.081(11) 0.045(8) 0.064(10) 0.012(7) 0.036(8) 0.001(7) C620 0.042(7) 0.044(7) 0.039(7) 0.002(6) 0.006(5) -0.004(6) C621 0.074(10) 0.072(11) 0.053(9) 0.006(8) -0.028(8) -0.010(8) C622 0.067(11) 0.052(10) 0.131(17) -0.011(10) -0.023(11) 0.013(8) C623 0.048(8) 0.051(9) 0.084(11) 0.007(8) -0.004(7) -0.022(7) O11 0.051(5) 0.052(6) 0.058(6) -0.003(5) 0.008(4) 0.008(4) O12 0.043(5) 0.073(7) 0.061(6) -0.014(5) -0.002(4) -0.010(5) O13 0.044(5) 0.053(6) 0.054(6) 0.005(5) 0.002(4) -0.011(4) O21 0.045(5) 0.050(5) 0.038(5) -0.011(4) -0.004(4) 0.010(4) O22 0.093(8) 0.044(6) 0.052(6) 0.018(5) -0.011(5) 0.000(5) O23 0.039(5) 0.055(6) 0.078(7) -0.014(5) -0.013(5) -0.001(4) O31 0.084(7) 0.047(5) 0.038(5) -0.001(4) 0.016(5) 0.003(5) O32 0.061(6) 0.051(5) 0.034(5) 0.011(4) 0.004(4) 0.008(4) O33 0.059(6) 0.059(6) 0.048(5) 0.005(5) 0.013(5) 0.010(5) O41 0.071(6) 0.035(5) 0.053(6) 0.008(4) 0.014(5) 0.001(4) O42 0.036(5) 0.063(6) 0.052(6) -0.001(5) 0.006(4) 0.001(4) O43 0.047(5) 0.057(6) 0.068(6) -0.024(5) 0.008(5) -0.016(5) O51 0.049(5) 0.066(6) 0.045(5) 0.014(5) 0.005(4) 0.007(5) O52 0.043(5) 0.052(5) 0.038(5) -0.003(4) 0.005(4) -0.008(4) O53 0.051(5) 0.049(5) 0.044(5) -0.001(4) -0.009(4) -0.008(4) F11 0.064(5) 0.064(5) 0.060(5) 0.000(4) -0.008(4) -0.005(4) F12 0.053(5) 0.063(5) 0.069(5) -0.014(4) 0.015(4) 0.004(4) F13 0.072(6) 0.058(5) 0.079(6) 0.000(5) 0.024(5) -0.018(4) F21 0.079(5) 0.044(4) 0.041(4) 0.003(4) 0.011(4) 0.005(4) F22 0.076(6) 0.082(6) 0.051(5) -0.015(4) -0.014(4) -0.029(5) F23 0.116(8) 0.051(5) 0.051(5) -0.013(4) 0.016(5) 0.015(5) F31 0.103(7) 0.102(8) 0.041(5) 0.011(5) 0.032(5) 0.004(6) F32 0.114(8) 0.077(6) 0.042(5) 0.002(4) -0.008(5) 0.033(6) F33 0.101(7) 0.073(6) 0.047(5) -0.018(4) -0.013(5) 0.025(5) F41 0.125(9) 0.092(8) 0.089(7) 0.058(6) 0.050(7) 0.032(7) F42 0.061(5) 0.093(7) 0.059(5) -0.020(5) 0.025(4) -0.003(5) F43 0.062(6) 0.173(11) 0.037(5) -0.009(6) -0.009(4) -0.015(6) F51 0.056(5) 0.126(8) 0.052(5) 0.018(5) 0.014(4) -0.026(5) F52 0.065(5) 0.087(6) 0.043(4) 0.013(4) -0.005(4) -0.001(5) F53 0.099(7) 0.058(5) 0.046(5) -0.014(4) 0.011(4) -0.006(5) Si11 0.0444(19) 0.051(2) 0.0314(18) -0.0015(16) 0.0022(14) 0.0022(16) Si12 0.0336(16) 0.0423(19) 0.0367(18) -0.0057(15) -0.0009(14) 0.0049(14) Si21 0.0421(19) 0.057(2) 0.0321(18) 0.0019(16) 0.0077(14) 0.0060(16) Si22 0.0365(18) 0.070(3) 0.0370(19) -0.0119(18) 0.0018(15) -0.0067(17) Si31 0.046(2) 0.061(3) 0.092(3) -0.037(3) 0.018(2) -0.017(2) Si32 0.069(3) 0.061(3) 0.076(3) 0.006(2) -0.003(2) 0.002(2) Si41 0.058(2) 0.059(2) 0.043(2) 0.0070(19) -0.0078(17) -0.0082(19) Si42 0.077(3) 0.055(3) 0.059(3) -0.011(2) 0.023(2) -0.016(2) Si51 0.0420(18) 0.0407(19) 0.0298(17) -0.0047(14) 0.0069(14) -0.0003(15) Si52 0.0324(16) 0.0439(19) 0.0331(17) -0.0055(15) 0.0046(13) 0.0008(14) Si61 0.049(2) 0.0377(19) 0.0372(19) 0.0011(15) 0.0045(15) 0.0028(16) Si62 0.049(2) 0.043(2) 0.055(2) 0.0026(18) -0.0082(17) -0.0044(17) S1 0.0353(16) 0.0438(18) 0.0526(19) -0.0065(15) 0.0050(14) -0.0061(13) S2 0.0495(18) 0.0370(16) 0.0385(17) -0.0017(14) -0.0079(14) 0.0030(14) S3 0.060(2) 0.0421(17) 0.0279(15) -0.0005(13) 0.0079(14) 0.0085(15) S4 0.0383(16) 0.0479(18) 0.0334(16) -0.0011(14) 0.0053(12) -0.0085(14) S5 0.0326(15) 0.0465(17) 0.0334(15) 0.0031(13) 0.0034(12) -0.0029(13) Ag1 0.0354(5) 0.0357(5) 0.0436(5) 0.0029(4) 0.0020(4) 0.0012(4) Ag2 0.0364(5) 0.0427(5) 0.0392(5) 0.0011(4) 0.0054(4) 0.0011(4) Ag3 0.0399(5) 0.0483(6) 0.0447(6) 0.0026(4) 0.0018(4) -0.0070(4) Ag4 0.0372(5) 0.0499(6) 0.0522(6) 0.0092(5) 0.0058(4) 0.0071(4) Ag5 0.0422(5) 0.0420(6) 0.0550(6) 0.0007(5) 0.0137(4) -0.0083(4) Ag6 0.0492(6) 0.0313(5) 0.0454(6) -0.0006(4) 0.0003(4) -0.0018(4) Te1 0.0319(4) 0.0301(4) 0.0323(4) 0.0009(3) 0.0038(3) 0.0002(3) Te2 0.0334(4) 0.0501(5) 0.0304(4) -0.0025(4) 0.0030(3) -0.0004(3) Te3 0.0255(4) 0.0676(6) 0.0538(5) 0.0214(5) -0.0014(4) -0.0055(4) Te4 0.0445(5) 0.0371(4) 0.0352(4) 0.0025(3) 0.0014(3) -0.0047(3) Te5 0.0352(4) 0.0292(4) 0.0306(4) -0.0021(3) 0.0049(3) -0.0026(3) Te6 0.0372(4) 0.0333(4) 0.0387(4) 0.0034(3) 0.0021(3) 0.0004(3) C6A 0.047(11) 0.097(16) 0.13(2) -0.053(15) -0.008(12) 0.009(11) F61A 0.062(4) 0.150(12) 0.115(9) -0.027(8) 0.005(5) 0.011(7) F62A 0.062(4) 0.150(12) 0.115(9) -0.027(8) 0.005(5) 0.011(7) F63A 0.062(4) 0.150(12) 0.115(9) -0.027(8) 0.005(5) 0.011(7) S6A 0.048(4) 0.046(4) 0.114(6) 0.011(3) -0.026(4) 0.010(3) O61A 0.068(7) 0.093(9) 0.139(10) 0.009(7) -0.027(7) 0.022(6) O62A 0.068(7) 0.093(9) 0.139(10) 0.009(7) -0.027(7) 0.022(6) O63A 0.068(7) 0.093(9) 0.139(10) 0.009(7) -0.027(7) 0.022(6) C6B 0.047(11) 0.097(16) 0.13(2) -0.053(15) -0.008(12) 0.009(11) F61B 0.062(4) 0.150(12) 0.115(9) -0.027(8) 0.005(5) 0.011(7) F62B 0.062(4) 0.150(12) 0.115(9) -0.027(8) 0.005(5) 0.011(7) F63B 0.062(4) 0.150(12) 0.115(9) -0.027(8) 0.005(5) 0.011(7) S6B 0.048(4) 0.046(4) 0.114(6) 0.011(3) -0.026(4) 0.010(3) O61B 0.068(7) 0.093(9) 0.139(10) 0.009(7) -0.027(7) 0.022(6) O62B 0.068(7) 0.093(9) 0.139(10) 0.009(7) -0.027(7) 0.022(6) O63B 0.068(7) 0.093(9) 0.139(10) 0.009(7) -0.027(7) 0.022(6) C31A 0.115(15) 0.105(15) 0.139(17) -0.037(13) 0.003(12) 0.046(12) C32A 0.115(15) 0.105(15) 0.139(17) -0.037(13) 0.003(12) 0.046(12) C33A 0.115(15) 0.105(15) 0.139(17) -0.037(13) 0.003(12) 0.046(12) C31B 0.115(15) 0.105(15) 0.139(17) -0.037(13) 0.003(12) 0.046(12) C32B 0.115(15) 0.105(15) 0.139(17) -0.037(13) 0.003(12) 0.046(12) C33B 0.115(15) 0.105(15) 0.139(17) -0.037(13) 0.003(12) 0.046(12) _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 C1 F12 1.323(15) . ? C1 F11 1.340(16) . ? C1 F13 1.348(15) . ? C1 S1 1.811(15) . ? C2 F21 1.308(15) . ? C2 F23 1.319(15) . ? C2 F22 1.338(15) . ? C2 S2 1.813(14) . ? C3 F31 1.321(18) . ? C3 F32 1.332(16) . ? C3 F33 1.335(16) . ? C3 S3 1.827(14) . ? C4 F41 1.285(17) . ? C4 F42 1.306(16) . ? C4 F43 1.314(16) . ? C4 S4 1.837(14) . ? C5 F51 1.314(16) . ? C5 F52 1.319(16) . ? C5 F53 1.326(17) . ? C5 S5 1.814(14) . ? C110 Si11 1.876(11) . ? C110 Te1 2.143(11) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 Si11 1.848(15) . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C112 Si11 1.871(14) . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C113 Si11 1.861(15) . ? C113 H11I 0.9800 . ? C113 H11J 0.9800 . ? C113 H11K 0.9800 . ? C120 Si12 1.870(12) . ? C120 Te1 2.138(12) . ? C120 H12A 0.9900 . ? C120 H12B 0.9900 . ? C121 Si12 1.870(15) . ? C121 H12C 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C122 Si12 1.830(13) . ? C122 H12F 0.9800 . ? C122 H12G 0.9800 . ? C122 H12H 0.9800 . ? C123 Si12 1.852(15) . ? C123 H12I 0.9800 . ? C123 H12J 0.9800 . ? C123 H12K 0.9800 . ? C210 Si21 1.900(14) . ? C210 Te2 2.153(13) . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 Si21 1.847(15) . ? C211 H21C 0.9800 . ? C211 H21D 0.9800 . ? C211 H21E 0.9800 . ? C212 Si21 1.831(17) . ? C212 H21F 0.9800 . ? C212 H21G 0.9800 . ? C212 H21H 0.9800 . ? C213 Si21 1.855(16) . ? C213 H21I 0.9800 . ? C213 H21J 0.9800 . ? C213 H21K 0.9800 . ? C220 Si22 1.911(15) . ? C220 Te2 2.149(14) . ? C220 H22A 0.9900 . ? C220 H22B 0.9900 . ? C221 Si22 1.854(15) . ? C221 H22C 0.9800 . ? C221 H22D 0.9800 . ? C221 H22E 0.9800 . ? C222 Si22 1.87(2) . ? C222 H22F 0.9800 . ? C222 H22G 0.9800 . ? C222 H22H 0.9800 . ? C223 Si22 1.862(16) . ? C223 H22I 0.9800 . ? C223 H22J 0.9800 . ? C223 H22K 0.9800 . ? C310 Si31 1.85(2) . ? C310 Te3 2.148(17) . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 Si31 1.847(17) . ? C311 H31C 0.9800 . ? C311 H31D 0.9800 . ? C311 H31E 0.9800 . ? C312 Si31 1.82(3) . ? C312 H31F 0.9800 . ? C312 H31G 0.9800 . ? C312 H31H 0.9800 . ? C313 Si31 1.81(3) . ? C313 H31I 0.9800 . ? C313 H31J 0.9800 . ? C313 H31K 0.9800 . ? C320 Si32 1.860(17) . ? C320 Te3 2.134(15) . ? C320 H32A 0.9900 . ? C320 H32B 0.9900 . ? C410 Si41 1.78(2) . ? C410 Te4 2.093(18) . ? C410 H41A 0.9900 . ? C410 H41B 0.9900 . ? C411 Si41 1.874(17) . ? C411 H41C 0.9800 . ? C411 H41D 0.9800 . ? C411 H41E 0.9800 . ? C412 Si41 1.77(3) . ? C412 H41F 0.9800 . ? C412 H41G 0.9800 . ? C412 H41H 0.9800 . ? C413 Si41 1.86(2) . ? C413 H41I 0.9800 . ? C413 H41J 0.9800 . ? C413 H41K 0.9800 . ? C420 Si42 1.763(16) . ? C420 Te4 2.115(17) . ? C420 H42A 0.9900 . ? C420 H42B 0.9900 . ? C421 Si42 1.86(3) . ? C421 H42C 0.9800 . ? C421 H42D 0.9800 . ? C421 H42E 0.9800 . ? C422 Si42 1.88(2) . ? C422 H42F 0.9800 . ? C422 H42G 0.9800 . ? C422 H42H 0.9800 . ? C423 Si42 1.89(3) . ? C423 H42I 0.9800 . ? C423 H42J 0.9800 . ? C423 H42K 0.9800 . ? C510 Si51 1.869(12) . ? C510 Te5 2.167(12) . ? C510 H51A 0.9900 . ? C510 H51B 0.9900 . ? C511 Si51 1.847(14) . ? C511 H51C 0.9800 . ? C511 H51D 0.9800 . ? C511 H51E 0.9800 . ? C512 Si51 1.847(16) . ? C512 H51F 0.9800 . ? C512 H51G 0.9800 . ? C512 H51H 0.9800 . ? C513 Si51 1.834(15) . ? C513 H51I 0.9800 . ? C513 H51J 0.9800 . ? C513 H51K 0.9800 . ? C520 Si52 1.870(12) . ? C520 Te5 2.154(12) . ? C520 H52A 0.9900 . ? C520 H52B 0.9900 . ? C521 Si52 1.852(12) . ? C521 H52C 0.9800 . ? C521 H52D 0.9800 . ? C521 H52E 0.9800 . ? C522 Si52 1.862(15) . ? C522 H52F 0.9800 . ? C522 H52G 0.9800 . ? C522 H52H 0.9800 . ? C523 Si52 1.864(14) . ? C523 H52I 0.9800 . ? C523 H52J 0.9800 . ? C523 H52K 0.9800 . ? C610 Si61 1.884(12) . ? C610 Te6 2.144(12) . ? C610 H61A 0.9900 . ? C610 H61B 0.9900 . ? C611 Si61 1.860(15) . ? C611 H61C 0.9800 . ? C611 H61D 0.9800 . ? C611 H61E 0.9800 . ? C612 Si61 1.855(14) . ? C612 H61F 0.9800 . ? C612 H61G 0.9800 . ? C612 H61H 0.9800 . ? C613 Si61 1.839(14) . ? C613 H61I 0.9800 . ? C613 H61J 0.9800 . ? C613 H61K 0.9800 . ? C620 Si62 1.887(12) . ? C620 Te6 2.132(12) . ? C620 H62A 0.9900 . ? C620 H62B 0.9900 . ? C621 Si62 1.877(15) . ? C621 H62C 0.9800 . ? C621 H62D 0.9800 . ? C621 H62E 0.9800 . ? C622 Si62 1.874(17) . ? C622 H62F 0.9800 . ? C622 H62G 0.9800 . ? C622 H62H 0.9800 . ? C623 Si62 1.850(16) . ? C623 H62I 0.9800 . ? C623 H62J 0.9800 . ? C623 H62K 0.9800 . ? O11 S1 1.444(9) . ? O12 S1 1.434(9) . ? O13 S1 1.441(9) . ? O13 Ag1 2.302(8) . ? O21 S2 1.443(9) . ? O21 Ag2 2.526(8) . ? O22 S2 1.432(10) . ? O22 Ag6 2.445(10) . ? O23 S2 1.460(9) . ? O31 S3 1.448(10) . ? O31 Ag6 2.433(9) . ? O32 S3 1.452(9) . ? O32 Ag2 2.387(8) . ? O33 S3 1.433(10) . ? O41 S4 1.443(9) . ? O42 S4 1.446(9) . ? O42 Ag3 2.551(9) . ? O43 S4 1.440(9) . ? O43 Ag5 2.348(9) . ? O51 S5 1.431(9) . ? O52 S5 1.453(9) . ? O52 Ag5 2.400(8) . ? O53 S5 1.455(9) . ? O53 Ag3 2.451(8) . ? Si32 C31A 1.855(10) . ? Si32 C33A 1.857(10) . ? Si32 C32A 1.858(10) . ? Si32 C32B 1.861(10) . ? Si32 C31B 1.862(10) . ? Si32 C33B 1.862(10) . ? Ag1 Te1 2.6858(12) . ? Ag1 Te6 2.7498(13) . ? Ag2 Te2 2.7224(12) . ? Ag2 Te1 2.7283(13) . ? Ag3 Te2 2.7072(14) 1_565 ? Ag3 Te3 2.7212(14) . ? Ag4 O61A 2.249(19) . ? Ag4 O62B 2.39(3) . ? Ag4 Te3 2.7025(14) . ? Ag4 Te4 2.7205(13) . ? Ag5 Te5 2.7300(13) . ? Ag5 Te4 2.7691(14) . ? Ag6 Te5 2.7061(13) . ? Ag6 Te6 2.7172(13) . ? Te2 Ag3 2.7072(14) 1_545 ? C6A F63A 1.342(10) . ? C6A F62A 1.345(10) . ? C6A F61A 1.348(10) . ? C6A S6A 1.809(10) . ? S6A O62A 1.436(10) . ? S6A O63A 1.441(10) . ? S6A O61A 1.453(9) . ? C6B F62B 1.347(10) . ? C6B F63B 1.348(10) . ? C6B F61B 1.349(10) . ? C6B S6B 1.811(10) . ? S6B O62B 1.447(10) . ? S6B O63B 1.449(10) . ? S6B O61B 1.450(10) . ? C31A H1AA 0.9800 . ? C31A H1BA 0.9800 . ? C31A H1CA 0.9800 . ? C32A H2AA 0.9800 . ? C32A H2BA 0.9800 . ? C32A H2CA 0.9800 . ? C33A H3AA 0.9800 . ? C33A H3BA 0.9800 . ? C33A H3CA 0.9800 . ? C31B H1AB 0.9800 . ? C31B H1BB 0.9800 . ? C31B H1CB 0.9800 . ? C32B H2AB 0.9800 . ? C32B H2BB 0.9800 . ? C32B H2CB 0.9800 . ? C33B H3AB 0.9800 . ? C33B H3BB 0.9800 . ? C33B H3CB 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F12 C1 F11 107.1(11) . . ? F12 C1 F13 107.1(11) . . ? F11 C1 F13 106.5(12) . . ? F12 C1 S1 112.5(10) . . ? F11 C1 S1 111.7(9) . . ? F13 C1 S1 111.6(10) . . ? F21 C2 F23 109.0(11) . . ? F21 C2 F22 107.7(11) . . ? F23 C2 F22 107.0(12) . . ? F21 C2 S2 111.1(10) . . ? F23 C2 S2 111.0(9) . . ? F22 C2 S2 110.9(9) . . ? F31 C3 F32 108.3(12) . . ? F31 C3 F33 107.9(12) . . ? F32 C3 F33 108.1(12) . . ? F31 C3 S3 111.1(11) . . ? F32 C3 S3 111.0(10) . . ? F33 C3 S3 110.2(9) . . ? F41 C4 F42 108.9(12) . . ? F41 C4 F43 109.1(13) . . ? F42 C4 F43 107.5(12) . . ? F41 C4 S4 111.1(11) . . ? F42 C4 S4 110.5(10) . . ? F43 C4 S4 109.7(9) . . ? F51 C5 F52 108.4(12) . . ? F51 C5 F53 109.1(12) . . ? F52 C5 F53 105.6(11) . . ? F51 C5 S5 111.3(10) . . ? F52 C5 S5 110.9(10) . . ? F53 C5 S5 111.4(10) . . ? Si11 C110 Te1 118.7(6) . . ? Si11 C110 H11A 107.6 . . ? Te1 C110 H11A 107.6 . . ? Si11 C110 H11B 107.6 . . ? Te1 C110 H11B 107.6 . . ? H11A C110 H11B 107.1 . . ? Si11 C111 H11C 109.5 . . ? Si11 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? Si11 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? Si11 C112 H11F 109.5 . . ? Si11 C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? Si11 C112 H11H 109.5 . . ? H11F C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? Si11 C113 H11I 109.5 . . ? Si11 C113 H11J 109.5 . . ? H11I C113 H11J 109.5 . . ? Si11 C113 H11K 109.5 . . ? H11I C113 H11K 109.5 . . ? H11J C113 H11K 109.5 . . ? Si12 C120 Te1 113.2(6) . . ? Si12 C120 H12A 108.9 . . ? Te1 C120 H12A 108.9 . . ? Si12 C120 H12B 108.9 . . ? Te1 C120 H12B 108.9 . . ? H12A C120 H12B 107.7 . . ? Si12 C121 H12C 109.5 . . ? Si12 C121 H12D 109.5 . . ? H12C C121 H12D 109.5 . . ? Si12 C121 H12E 109.5 . . ? H12C C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? Si12 C122 H12F 109.5 . . ? Si12 C122 H12G 109.5 . . ? H12F C122 H12G 109.5 . . ? Si12 C122 H12H 109.5 . . ? H12F C122 H12H 109.5 . . ? H12G C122 H12H 109.5 . . ? Si12 C123 H12I 109.5 . . ? Si12 C123 H12J 109.5 . . ? H12I C123 H12J 109.5 . . ? Si12 C123 H12K 109.5 . . ? H12I C123 H12K 109.5 . . ? H12J C123 H12K 109.5 . . ? Si21 C210 Te2 116.2(7) . . ? Si21 C210 H21A 108.2 . . ? Te2 C210 H21A 108.2 . . ? Si21 C210 H21B 108.2 . . ? Te2 C210 H21B 108.2 . . ? H21A C210 H21B 107.4 . . ? Si21 C211 H21C 109.5 . . ? Si21 C211 H21D 109.5 . . ? H21C C211 H21D 109.5 . . ? Si21 C211 H21E 109.5 . . ? H21C C211 H21E 109.5 . . ? H21D C211 H21E 109.5 . . ? Si21 C212 H21F 109.5 . . ? Si21 C212 H21G 109.5 . . ? H21F C212 H21G 109.5 . . ? Si21 C212 H21H 109.5 . . ? H21F C212 H21H 109.5 . . ? H21G C212 H21H 109.5 . . ? Si21 C213 H21I 109.5 . . ? Si21 C213 H21J 109.5 . . ? H21I C213 H21J 109.5 . . ? Si21 C213 H21K 109.5 . . ? H21I C213 H21K 109.5 . . ? H21J C213 H21K 109.5 . . ? Si22 C220 Te2 117.3(8) . . ? Si22 C220 H22A 108.0 . . ? Te2 C220 H22A 108.0 . . ? Si22 C220 H22B 108.0 . . ? Te2 C220 H22B 108.0 . . ? H22A C220 H22B 107.2 . . ? Si22 C221 H22C 109.5 . . ? Si22 C221 H22D 109.5 . . ? H22C C221 H22D 109.5 . . ? Si22 C221 H22E 109.5 . . ? H22C C221 H22E 109.5 . . ? H22D C221 H22E 109.5 . . ? Si22 C222 H22F 109.5 . . ? Si22 C222 H22G 109.5 . . ? H22F C222 H22G 109.5 . . ? Si22 C222 H22H 109.5 . . ? H22F C222 H22H 109.5 . . ? H22G C222 H22H 109.5 . . ? Si22 C223 H22I 109.5 . . ? Si22 C223 H22J 109.5 . . ? H22I C223 H22J 109.5 . . ? Si22 C223 H22K 109.5 . . ? H22I C223 H22K 109.5 . . ? H22J C223 H22K 109.5 . . ? Si31 C310 Te3 115.5(10) . . ? Si31 C310 H31A 108.4 . . ? Te3 C310 H31A 108.4 . . ? Si31 C310 H31B 108.4 . . ? Te3 C310 H31B 108.4 . . ? H31A C310 H31B 107.5 . . ? Si31 C311 H31C 109.5 . . ? Si31 C311 H31D 109.5 . . ? H31C C311 H31D 109.5 . . ? Si31 C311 H31E 109.5 . . ? H31C C311 H31E 109.5 . . ? H31D C311 H31E 109.5 . . ? Si31 C312 H31F 109.5 . . ? Si31 C312 H31G 109.5 . . ? H31F C312 H31G 109.5 . . ? Si31 C312 H31H 109.5 . . ? H31F C312 H31H 109.5 . . ? H31G C312 H31H 109.5 . . ? Si31 C313 H31I 109.5 . . ? Si31 C313 H31J 109.5 . . ? H31I C313 H31J 109.5 . . ? Si31 C313 H31K 109.5 . . ? H31I C313 H31K 109.5 . . ? H31J C313 H31K 109.5 . . ? Si32 C320 Te3 118.7(8) . . ? Si32 C320 H32A 107.6 . . ? Te3 C320 H32A 107.6 . . ? Si32 C320 H32B 107.6 . . ? Te3 C320 H32B 107.6 . . ? H32A C320 H32B 107.1 . . ? Si41 C410 Te4 125.6(12) . . ? Si41 C410 H41A 105.9 . . ? Te4 C410 H41A 105.9 . . ? Si41 C410 H41B 105.9 . . ? Te4 C410 H41B 105.9 . . ? H41A C410 H41B 106.3 . . ? Si41 C411 H41C 109.5 . . ? Si41 C411 H41D 109.5 . . ? H41C C411 H41D 109.5 . . ? Si41 C411 H41E 109.5 . . ? H41C C411 H41E 109.5 . . ? H41D C411 H41E 109.5 . . ? Si41 C412 H41F 109.5 . . ? Si41 C412 H41G 109.5 . . ? H41F C412 H41G 109.5 . . ? Si41 C412 H41H 109.5 . . ? H41F C412 H41H 109.5 . . ? H41G C412 H41H 109.5 . . ? Si41 C413 H41I 109.5 . . ? Si41 C413 H41J 109.5 . . ? H41I C413 H41J 109.5 . . ? Si41 C413 H41K 109.5 . . ? H41I C413 H41K 109.5 . . ? H41J C413 H41K 109.5 . . ? Si42 C420 Te4 128.7(9) . . ? Si42 C420 H42A 105.1 . . ? Te4 C420 H42A 105.1 . . ? Si42 C420 H42B 105.1 . . ? Te4 C420 H42B 105.1 . . ? H42A C420 H42B 105.9 . . ? Si42 C421 H42C 109.5 . . ? Si42 C421 H42D 109.5 . . ? H42C C421 H42D 109.5 . . ? Si42 C421 H42E 109.5 . . ? H42C C421 H42E 109.5 . . ? H42D C421 H42E 109.5 . . ? Si42 C422 H42F 109.5 . . ? Si42 C422 H42G 109.5 . . ? H42F C422 H42G 109.5 . . ? Si42 C422 H42H 109.5 . . ? H42F C422 H42H 109.5 . . ? H42G C422 H42H 109.5 . . ? Si42 C423 H42I 109.5 . . ? Si42 C423 H42J 109.5 . . ? H42I C423 H42J 109.5 . . ? Si42 C423 H42K 109.5 . . ? H42I C423 H42K 109.5 . . ? H42J C423 H42K 109.5 . . ? Si51 C510 Te5 115.9(6) . . ? Si51 C510 H51A 108.3 . . ? Te5 C510 H51A 108.3 . . ? Si51 C510 H51B 108.3 . . ? Te5 C510 H51B 108.3 . . ? H51A C510 H51B 107.4 . . ? Si51 C511 H51C 109.5 . . ? Si51 C511 H51D 109.5 . . ? H51C C511 H51D 109.5 . . ? Si51 C511 H51E 109.5 . . ? H51C C511 H51E 109.5 . . ? H51D C511 H51E 109.5 . . ? Si51 C512 H51F 109.5 . . ? Si51 C512 H51G 109.5 . . ? H51F C512 H51G 109.5 . . ? Si51 C512 H51H 109.5 . . ? H51F C512 H51H 109.5 . . ? H51G C512 H51H 109.5 . . ? Si51 C513 H51I 109.5 . . ? Si51 C513 H51J 109.5 . . ? H51I C513 H51J 109.5 . . ? Si51 C513 H51K 109.5 . . ? H51I C513 H51K 109.5 . . ? H51J C513 H51K 109.5 . . ? Si52 C520 Te5 117.0(6) . . ? Si52 C520 H52A 108.0 . . ? Te5 C520 H52A 108.0 . . ? Si52 C520 H52B 108.0 . . ? Te5 C520 H52B 108.0 . . ? H52A C520 H52B 107.3 . . ? Si52 C521 H52C 109.5 . . ? Si52 C521 H52D 109.5 . . ? H52C C521 H52D 109.5 . . ? Si52 C521 H52E 109.5 . . ? H52C C521 H52E 109.5 . . ? H52D C521 H52E 109.5 . . ? Si52 C522 H52F 109.5 . . ? Si52 C522 H52G 109.5 . . ? H52F C522 H52G 109.5 . . ? Si52 C522 H52H 109.5 . . ? H52F C522 H52H 109.5 . . ? H52G C522 H52H 109.5 . . ? Si52 C523 H52I 109.5 . . ? Si52 C523 H52J 109.5 . . ? H52I C523 H52J 109.5 . . ? Si52 C523 H52K 109.5 . . ? H52I C523 H52K 109.5 . . ? H52J C523 H52K 109.5 . . ? Si61 C610 Te6 115.6(6) . . ? Si61 C610 H61A 108.4 . . ? Te6 C610 H61A 108.4 . . ? Si61 C610 H61B 108.4 . . ? Te6 C610 H61B 108.4 . . ? H61A C610 H61B 107.4 . . ? Si61 C611 H61C 109.5 . . ? Si61 C611 H61D 109.5 . . ? H61C C611 H61D 109.5 . . ? Si61 C611 H61E 109.5 . . ? H61C C611 H61E 109.5 . . ? H61D C611 H61E 109.5 . . ? Si61 C612 H61F 109.5 . . ? Si61 C612 H61G 109.5 . . ? H61F C612 H61G 109.5 . . ? Si61 C612 H61H 109.5 . . ? H61F C612 H61H 109.5 . . ? H61G C612 H61H 109.5 . . ? Si61 C613 H61I 109.5 . . ? Si61 C613 H61J 109.5 . . ? H61I C613 H61J 109.5 . . ? Si61 C613 H61K 109.5 . . ? H61I C613 H61K 109.5 . . ? H61J C613 H61K 109.5 . . ? Si62 C620 Te6 117.7(6) . . ? Si62 C620 H62A 107.9 . . ? Te6 C620 H62A 107.9 . . ? Si62 C620 H62B 107.9 . . ? Te6 C620 H62B 107.9 . . ? H62A C620 H62B 107.2 . . ? Si62 C621 H62C 109.5 . . ? Si62 C621 H62D 109.5 . . ? H62C C621 H62D 109.5 . . ? Si62 C621 H62E 109.5 . . ? H62C C621 H62E 109.5 . . ? H62D C621 H62E 109.5 . . ? Si62 C622 H62F 109.5 . . ? Si62 C622 H62G 109.5 . . ? H62F C622 H62G 109.5 . . ? Si62 C622 H62H 109.5 . . ? H62F C622 H62H 109.5 . . ? H62G C622 H62H 109.5 . . ? Si62 C623 H62I 109.5 . . ? Si62 C623 H62J 109.5 . . ? H62I C623 H62J 109.5 . . ? Si62 C623 H62K 109.5 . . ? H62I C623 H62K 109.5 . . ? H62J C623 H62K 109.5 . . ? S1 O13 Ag1 126.0(6) . . ? S2 O21 Ag2 120.9(5) . . ? S2 O22 Ag6 113.1(6) . . ? S3 O31 Ag6 125.1(5) . . ? S3 O32 Ag2 127.7(5) . . ? S4 O42 Ag3 114.6(5) . . ? S4 O43 Ag5 129.9(6) . . ? S5 O52 Ag5 121.7(5) . . ? S5 O53 Ag3 126.7(5) . . ? C111 Si11 C113 110.8(8) . . ? C111 Si11 C112 111.9(7) . . ? C113 Si11 C112 109.9(8) . . ? C111 Si11 C110 111.6(6) . . ? C113 Si11 C110 104.3(7) . . ? C112 Si11 C110 108.0(6) . . ? C122 Si12 C123 112.4(7) . . ? C122 Si12 C121 108.3(7) . . ? C123 Si12 C121 111.0(7) . . ? C122 Si12 C120 108.6(6) . . ? C123 Si12 C120 108.2(6) . . ? C121 Si12 C120 108.1(6) . . ? C212 Si21 C211 109.3(8) . . ? C212 Si21 C213 111.4(9) . . ? C211 Si21 C213 112.8(6) . . ? C212 Si21 C210 110.2(7) . . ? C211 Si21 C210 108.9(7) . . ? C213 Si21 C210 104.0(7) . . ? C221 Si22 C223 112.2(8) . . ? C221 Si22 C222 110.0(8) . . ? C223 Si22 C222 109.8(10) . . ? C221 Si22 C220 110.5(7) . . ? C223 Si22 C220 104.9(7) . . ? C222 Si22 C220 109.3(8) . . ? C313 Si31 C312 115(3) . . ? C313 Si31 C311 108.3(13) . . ? C312 Si31 C311 111.4(10) . . ? C313 Si31 C310 105.0(13) . . ? C312 Si31 C310 104.7(18) . . ? C311 Si31 C310 112.6(8) . . ? C31A Si32 C33A 115.9(19) . . ? C31A Si32 C32A 111.4(19) . . ? C33A Si32 C32A 112.2(19) . . ? C31A Si32 C320 107.4(11) . . ? C33A Si32 C320 109.3(12) . . ? C32A Si32 C320 99.2(12) . . ? C31A Si32 C32B 60(2) . . ? C33A Si32 C32B 62(2) . . ? C32A Si32 C32B 159.7(19) . . ? C320 Si32 C32B 101.0(17) . . ? C31A Si32 C31B 51(3) . . ? C33A Si32 C31B 133(2) . . ? C32A Si32 C31B 61(3) . . ? C320 Si32 C31B 117.7(18) . . ? C32B Si32 C31B 108(3) . . ? C31A Si32 C33B 127(2) . . ? C33A Si32 C33B 43(2) . . ? C32A Si32 C33B 70(2) . . ? C320 Si32 C33B 125.6(19) . . ? C32B Si32 C33B 100(3) . . ? C31B Si32 C33B 103(3) . . ? C412 Si41 C410 108(2) . . ? C412 Si41 C413 110(2) . . ? C410 Si41 C413 103.9(16) . . ? C412 Si41 C411 111.9(11) . . ? C410 Si41 C411 111.4(9) . . ? C413 Si41 C411 111.3(11) . . ? C420 Si42 C421 113.8(13) . . ? C420 Si42 C422 107.2(9) . . ? C421 Si42 C422 105.1(11) . . ? C420 Si42 C423 110.2(15) . . ? C421 Si42 C423 102.3(19) . . ? C422 Si42 C423 118.3(13) . . ? C513 Si51 C512 112.0(9) . . ? C513 Si51 C511 107.3(7) . . ? C512 Si51 C511 112.8(7) . . ? C513 Si51 C510 108.0(7) . . ? C512 Si51 C510 104.0(7) . . ? C511 Si51 C510 112.7(6) . . ? C521 Si52 C522 107.8(6) . . ? C521 Si52 C523 111.3(6) . . ? C522 Si52 C523 110.8(7) . . ? C521 Si52 C520 109.2(6) . . ? C522 Si52 C520 108.8(7) . . ? C523 Si52 C520 109.0(6) . . ? C613 Si61 C612 110.4(7) . . ? C613 Si61 C611 110.9(8) . . ? C612 Si61 C611 110.6(7) . . ? C613 Si61 C610 109.3(7) . . ? C612 Si61 C610 106.4(6) . . ? C611 Si61 C610 109.2(6) . . ? C623 Si62 C622 109.6(8) . . ? C623 Si62 C621 109.2(8) . . ? C622 Si62 C621 110.5(9) . . ? C623 Si62 C620 111.1(6) . . ? C622 Si62 C620 109.3(7) . . ? C621 Si62 C620 107.1(6) . . ? O12 S1 O13 114.3(6) . . ? O12 S1 O11 114.8(6) . . ? O13 S1 O11 115.4(6) . . ? O12 S1 C1 103.4(6) . . ? O13 S1 C1 102.1(6) . . ? O11 S1 C1 104.5(6) . . ? O22 S2 O21 116.0(6) . . ? O22 S2 O23 113.4(6) . . ? O21 S2 O23 114.8(6) . . ? O22 S2 C2 103.4(6) . . ? O21 S2 C2 103.3(6) . . ? O23 S2 C2 103.9(6) . . ? O33 S3 O31 114.5(6) . . ? O33 S3 O32 115.1(6) . . ? O31 S3 O32 113.9(6) . . ? O33 S3 C3 104.3(7) . . ? O31 S3 C3 103.4(6) . . ? O32 S3 C3 103.7(6) . . ? O43 S4 O41 114.0(6) . . ? O43 S4 O42 114.0(6) . . ? O41 S4 O42 116.0(6) . . ? O43 S4 C4 103.2(6) . . ? O41 S4 C4 102.5(6) . . ? O42 S4 C4 104.9(6) . . ? O51 S5 O52 115.9(6) . . ? O51 S5 O53 114.3(6) . . ? O52 S5 O53 113.5(5) . . ? O51 S5 C5 104.3(6) . . ? O52 S5 C5 103.9(6) . . ? O53 S5 C5 102.9(6) . . ? O13 Ag1 Te1 133.7(2) . . ? O13 Ag1 Te6 100.8(2) . . ? Te1 Ag1 Te6 125.44(4) . . ? O32 Ag2 O21 88.7(3) . . ? O32 Ag2 Te2 108.0(2) . . ? O21 Ag2 Te2 97.48(19) . . ? O32 Ag2 Te1 108.4(2) . . ? O21 Ag2 Te1 99.9(2) . . ? Te2 Ag2 Te1 139.83(4) . . ? O53 Ag3 O42 85.2(3) . . ? O53 Ag3 Te2 98.3(2) . 1_565 ? O42 Ag3 Te2 110.6(2) . 1_565 ? O53 Ag3 Te3 97.9(2) . . ? O42 Ag3 Te3 93.5(2) . . ? Te2 Ag3 Te3 151.88(5) 1_565 . ? O61A Ag4 O62B 29.0(6) . . ? O61A Ag4 Te3 129.3(5) . . ? O62B Ag4 Te3 101.9(5) . . ? O61A Ag4 Te4 107.0(5) . . ? O62B Ag4 Te4 133.1(6) . . ? Te3 Ag4 Te4 123.75(4) . . ? O43 Ag5 O52 86.0(3) . . ? O43 Ag5 Te5 122.0(2) . . ? O52 Ag5 Te5 108.4(2) . . ? O43 Ag5 Te4 112.7(2) . . ? O52 Ag5 Te4 105.3(2) . . ? Te5 Ag5 Te4 116.25(4) . . ? O31 Ag6 O22 87.3(4) . . ? O31 Ag6 Te5 119.3(2) . . ? O22 Ag6 Te5 98.6(2) . . ? O31 Ag6 Te6 95.4(2) . . ? O22 Ag6 Te6 126.7(2) . . ? Te5 Ag6 Te6 124.62(4) . . ? C120 Te1 C110 97.1(5) . . ? C120 Te1 Ag1 108.7(3) . . ? C110 Te1 Ag1 113.0(3) . . ? C120 Te1 Ag2 109.5(3) . . ? C110 Te1 Ag2 101.0(3) . . ? Ag1 Te1 Ag2 124.00(4) . . ? C220 Te2 C210 93.0(6) . . ? C220 Te2 Ag3 110.0(5) . 1_545 ? C210 Te2 Ag3 107.5(4) . 1_545 ? C220 Te2 Ag2 102.6(4) . . ? C210 Te2 Ag2 105.4(4) . . ? Ag3 Te2 Ag2 131.57(4) 1_545 . ? C320 Te3 C310 94.7(7) . . ? C320 Te3 Ag4 113.9(5) . . ? C310 Te3 Ag4 109.7(6) . . ? C320 Te3 Ag3 104.9(4) . . ? C310 Te3 Ag3 116.9(7) . . ? Ag4 Te3 Ag3 115.06(4) . . ? C410 Te4 C420 99.4(12) . . ? C410 Te4 Ag4 111.1(7) . . ? C420 Te4 Ag4 106.1(5) . . ? C410 Te4 Ag5 110.4(11) . . ? C420 Te4 Ag5 96.6(4) . . ? Ag4 Te4 Ag5 127.93(4) . . ? C520 Te5 C510 97.3(5) . . ? C520 Te5 Ag6 102.9(4) . . ? C510 Te5 Ag6 100.2(3) . . ? C520 Te5 Ag5 111.8(3) . . ? C510 Te5 Ag5 108.7(4) . . ? Ag6 Te5 Ag5 130.56(4) . . ? C620 Te6 C610 95.9(5) . . ? C620 Te6 Ag6 101.3(3) . . ? C610 Te6 Ag6 111.2(4) . . ? C620 Te6 Ag1 113.3(3) . . ? C610 Te6 Ag1 114.8(3) . . ? Ag6 Te6 Ag1 117.45(4) . . ? F63A C6A F62A 103.3(18) . . ? F63A C6A F61A 106.6(19) . . ? F62A C6A F61A 108.1(19) . . ? F63A C6A S6A 110.2(19) . . ? F62A C6A S6A 112.4(15) . . ? F61A C6A S6A 115.5(16) . . ? O62A S6A O63A 114.7(15) . . ? O62A S6A O61A 114.8(12) . . ? O63A S6A O61A 115.9(14) . . ? O62A S6A C6A 102.1(13) . . ? O63A S6A C6A 107.3(14) . . ? O61A S6A C6A 99.4(13) . . ? S6A O61A Ag4 127.4(13) . . ? F62B C6B F63B 108(2) . . ? F62B C6B F61B 106(2) . . ? F63B C6B F61B 111(2) . . ? F62B C6B S6B 106(2) . . ? F63B C6B S6B 115(3) . . ? F61B C6B S6B 112(3) . . ? O62B S6B O63B 116(3) . . ? O62B S6B O61B 113(2) . . ? O63B S6B O61B 116(2) . . ? O62B S6B C6B 101(2) . . ? O63B S6B C6B 105(2) . . ? O61B S6B C6B 105(2) . . ? S6B O62B Ag4 117.8(19) . . ? Si32 C31A H1AA 109.5 . . ? Si32 C31A H1BA 109.5 . . ? H1AA C31A H1BA 109.5 . . ? Si32 C31A H1CA 109.5 . . ? H1AA C31A H1CA 109.5 . . ? H1BA C31A H1CA 109.5 . . ? Si32 C32A H2AA 109.5 . . ? Si32 C32A H2BA 109.5 . . ? H2AA C32A H2BA 109.5 . . ? Si32 C32A H2CA 109.5 . . ? H2AA C32A H2CA 109.5 . . ? H2BA C32A H2CA 109.5 . . ? Si32 C33A H3AA 109.5 . . ? Si32 C33A H3BA 109.5 . . ? H3AA C33A H3BA 109.5 . . ? Si32 C33A H3CA 109.5 . . ? H3AA C33A H3CA 109.5 . . ? H3BA C33A H3CA 109.5 . . ? Si32 C31B H1AB 109.5 . . ? Si32 C31B H1BB 109.5 . . ? H1AB C31B H1BB 109.5 . . ? Si32 C31B H1CB 109.5 . . ? H1AB C31B H1CB 109.5 . . ? H1BB C31B H1CB 109.5 . . ? Si32 C32B H2AB 109.5 . . ? Si32 C32B H2BB 109.5 . . ? H2AB C32B H2BB 109.5 . . ? Si32 C32B H2CB 109.5 . . ? H2AB C32B H2CB 109.5 . . ? H2BB C32B H2CB 109.5 . . ? Si32 C33B H3AB 109.5 . . ? Si32 C33B H3BB 109.5 . . ? H3AB C33B H3BB 109.5 . . ? Si32 C33B H3CB 109.5 . . ? H3AB C33B H3CB 109.5 . . ? H3BB C33B H3CB 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.372 _refine_diff_density_min -1.934 _refine_diff_density_rms 0.219 # start Validation Reply Form _vrf_PLAT213_cmpd8 ; PROBLEM: Atom C312 has ADP max/min Ratio ..... 5.3 prola RESPONSE: Me3Si- groups often show orientational variation due to rotational disorder resulting in the elongation of thermal ellipsoids. ; _vrf_PLAT222_cmpd8 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 10.0 Ratio RESPONSE: This is due to orientational disorder. ; _vrf_PLAT241_cmpd8 ; PROBLEM: Check High Ueq as Compared to Neighbors for C410 RESPONSE: This is due to orientational disorder. ; _vrf_PLAT411_cmpd8 ; PROBLEM: Short Inter H...H Contact H3BA .. H31A .. 1.66 Ang. RESPONSE: This is due to orientational disorder. ; _vrf_PLAT220_cmpd8 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 9.4 Ratio RESPONSE: This is due to orientational disorder. ; _vrf_PLAT232_cmpd8 ; PROBLEM: Hirshfeld Test Diff (M-X) Te4 -- Ag5 .. 10.1 su RESPONSE: This is due to the empirical multi-scan absorption correction. ; _vrf_PLAT242_cmpd8 ; PROBLEM: Check Low Ueq as Compared to Neighbors for Te4 RESPONSE: This is due to orientational disorder of one of the organic substituents. ; _vrf_PLAT413_cmpd8 ; PROBLEM: Short Inter XH3 .. XHn H2BA .. H42I .. 2.09 Ang. RESPONSE: This is due to disorder. ; # end Validation Reply Form #=============================================================================# # END of CIF # #=============================================================================# _database_code_depnum_ccdc_archive 'CCDC 949152'