data_2223a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3.2CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H60 Ag Au4 Cl8 F6 P4 Sb' _chemical_formula_weight 2536.23 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 '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 Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 17.952(3) _cell_length_b 17.952(3) _cell_length_c 25.388 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8182.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4269 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 24.05 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4768 _exptl_absorpt_coefficient_mu 8.100 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.2272 _exptl_absorpt_correction_T_max 0.4432 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23539 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 24.95 _reflns_number_total 3693 _reflns_number_gt 2757 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+17.2551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3693 _refine_ls_number_parameters 246 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.562269(18) 0.904116(19) 0.847625(13) 0.03805(17) Uani 1 1 d . . . Ag1 Ag 0.5000 1.0000 0.7500 0.0779(6) Uani 1 4 d S . . Cl1 Cl 0.44082(12) 0.90602(13) 0.81719(9) 0.0477(6) Uani 1 1 d . . . P1 P 0.68117(12) 0.89281(12) 0.87325(8) 0.0354(5) Uani 1 1 d . . . C1 C 0.5765(5) 1.0660(5) 0.9730(4) 0.047(2) Uani 1 1 d . . . H1A H 0.5496 1.1028 0.9548 0.056 Uiso 1 1 calc R . . C2 C 0.6148(5) 1.0134(5) 0.9450(4) 0.043(2) Uani 1 1 d . . . H2A H 0.6140 1.0143 0.9080 0.051 Uiso 1 1 calc R . . C3 C 0.6558(4) 0.9575(4) 0.9717(3) 0.0304(17) Uani 1 1 d . . . C4 C 0.6985(4) 0.9046(4) 0.9444(3) 0.0317(18) Uani 1 1 d . . . C5 C 0.7515(4) 0.8619(5) 0.9719(3) 0.0341(18) Uani 1 1 d . . . C6 C 0.8102(5) 0.8213(5) 0.9464(3) 0.046(2) Uani 1 1 d . . . H6A H 0.8116 0.8210 0.9094 0.055 Uiso 1 1 calc R . . C7 C 0.8636(5) 0.7833(5) 0.9727(4) 0.052(2) Uani 1 1 d . . . H7A H 0.9004 0.7571 0.9541 0.062 Uiso 1 1 calc R . . C1A C 0.7441(4) 0.9558(4) 0.8402(3) 0.0343(19) Uani 1 1 d . . . C2A C 0.8081(5) 0.9825(5) 0.8658(4) 0.044(2) Uani 1 1 d . . . H2AA H 0.8179 0.9697 0.9011 0.053 Uiso 1 1 calc R . . C3A C 0.8571(6) 1.0287(6) 0.8377(5) 0.059(3) Uani 1 1 d . . . H3AA H 0.9003 1.0470 0.8541 0.070 Uiso 1 1 calc R . . C4A C 0.8419(6) 1.0476(5) 0.7855(4) 0.056(3) Uani 1 1 d . . . H4AA H 0.8751 1.0782 0.7667 0.068 Uiso 1 1 calc R . . C5A C 0.7784(6) 1.0214(6) 0.7616(4) 0.059(3) Uani 1 1 d . . . H5AA H 0.7680 1.0348 0.7266 0.071 Uiso 1 1 calc R . . C6A C 0.7303(5) 0.9763(5) 0.7883(3) 0.046(2) Uani 1 1 d . . . H6AA H 0.6873 0.9587 0.7713 0.055 Uiso 1 1 calc R . . C1B C 0.7046(5) 0.7985(5) 0.8542(3) 0.040(2) Uani 1 1 d . . . C2B C 0.7630(5) 0.7806(6) 0.8215(4) 0.052(2) Uani 1 1 d . . . H2BA H 0.7932 0.8188 0.8079 0.062 Uiso 1 1 calc R . . C3B C 0.7782(7) 0.7082(6) 0.8082(4) 0.064(3) Uani 1 1 d . . . H3BA H 0.8184 0.6977 0.7858 0.077 Uiso 1 1 calc R . . C4B C 0.7358(8) 0.6514(7) 0.8271(6) 0.089(4) Uani 1 1 d . . . H4BA H 0.7463 0.6017 0.8181 0.107 Uiso 1 1 calc R . . C5B C 0.6772(8) 0.6689(6) 0.8597(6) 0.086(4) Uani 1 1 d . . . H5BA H 0.6471 0.6303 0.8728 0.103 Uiso 1 1 calc R . . C6B C 0.6611(6) 0.7411(6) 0.8739(5) 0.066(3) Uani 1 1 d . . . H6BA H 0.6211 0.7514 0.8966 0.079 Uiso 1 1 calc R . . Sb1 Sb 0.5000 0.5000 0.86215(13) 0.0562(7) Uani 0.50 4 d SPD . . F1 F 0.5014(8) 0.5954(10) 0.8566(10) 0.145(8) Uani 0.50 1 d PDU . . F2 F 0.5000 0.5000 0.7957(10) 0.31(3) Uani 0.50 4 d SPDU . . F3 F 0.5000 0.5000 0.9282(10) 0.22(2) Uani 0.50 4 d SPDU . . Sb2 Sb 0.0000 0.0000 0.0000 0.0465(4) Uani 1 8 d S . . F4 F 0.1002(5) 0.0150(6) 0.0000 0.115(4) Uani 1 2 d S . . F5 F 0.0000 0.0000 0.0719(6) 0.174(9) Uani 1 4 d S . . Cl2B Cl 0.7612(8) 0.4577(7) 1.0000 0.277(7) Uani 1 2 d SD . . Cl2A Cl 0.7161(10) 0.5961(17) 1.0000 0.443(15) Uani 1 2 d SD . . C100 C 0.739(2) 0.5274(12) 0.9500(16) 0.134(13) Uiso 0.50 1 d PD . . H10A H 0.7814 0.5414 0.9281 0.161 Uiso 0.50 1 calc PR . . H10B H 0.6960 0.5136 0.9280 0.161 Uiso 0.50 1 calc PR . . 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 Au1 0.0384(2) 0.0492(3) 0.0265(2) -0.00583(14) -0.00115(14) 0.00133(15) Ag1 0.0909(8) 0.0909(8) 0.0519(11) 0.000 0.000 0.000 Cl1 0.0376(11) 0.0633(14) 0.0422(13) -0.0143(11) -0.0031(10) 0.0016(10) P1 0.0410(12) 0.0437(12) 0.0214(11) -0.0049(9) 0.0000(9) 0.0026(10) C1 0.057(6) 0.047(5) 0.037(5) 0.001(4) -0.008(4) 0.010(4) C2 0.043(5) 0.050(5) 0.035(5) -0.013(4) -0.008(4) 0.000(4) C3 0.030(4) 0.035(4) 0.027(4) 0.000(3) -0.002(3) -0.004(3) C4 0.038(4) 0.036(4) 0.021(4) -0.001(3) 0.004(3) -0.003(3) C5 0.039(4) 0.044(5) 0.020(4) 0.002(4) -0.001(3) -0.002(4) C6 0.047(5) 0.063(6) 0.026(5) -0.012(4) 0.000(4) 0.017(5) C7 0.049(5) 0.054(6) 0.053(6) -0.010(4) 0.003(4) 0.017(5) C1A 0.039(5) 0.034(4) 0.029(5) -0.007(3) 0.005(4) 0.004(4) C2A 0.051(6) 0.040(5) 0.040(5) 0.003(4) -0.004(4) 0.000(4) C3A 0.049(6) 0.058(6) 0.069(8) 0.001(5) 0.004(5) -0.008(5) C4A 0.070(7) 0.040(5) 0.060(7) 0.011(5) 0.021(6) -0.004(5) C5A 0.074(7) 0.067(7) 0.037(6) 0.013(5) -0.001(5) -0.013(6) C6A 0.058(6) 0.055(5) 0.024(4) 0.004(4) -0.001(4) -0.008(5) C1B 0.050(5) 0.042(5) 0.029(5) -0.003(4) -0.012(4) 0.004(4) C2B 0.058(6) 0.058(6) 0.039(5) -0.002(5) 0.003(5) 0.010(5) C3B 0.093(8) 0.056(6) 0.044(6) -0.007(5) 0.006(6) 0.020(6) C4B 0.105(11) 0.050(7) 0.113(12) -0.029(8) -0.006(9) 0.004(7) C5B 0.097(10) 0.035(6) 0.126(12) -0.004(7) 0.006(9) -0.006(6) C6B 0.071(7) 0.054(6) 0.072(8) 0.000(6) 0.001(6) -0.007(5) Sb1 0.0474(10) 0.0474(10) 0.074(2) 0.000 0.000 0.000 F1 0.056(9) 0.121(13) 0.26(2) 0.006(13) 0.004(11) 0.011(9) F2 0.31(3) 0.31(3) 0.32(4) 0.000 0.000 0.000 F3 0.22(2) 0.22(2) 0.22(3) 0.000 0.000 0.000 Sb2 0.0548(7) 0.0548(7) 0.0299(9) 0.000 0.000 0.000 F4 0.059(6) 0.097(8) 0.191(14) 0.000 0.000 -0.002(6) F5 0.243(15) 0.243(15) 0.035(10) 0.000 0.000 0.000 Cl2B 0.292(14) 0.179(10) 0.36(2) 0.000 0.000 -0.068(10) Cl2A 0.32(2) 0.69(4) 0.32(2) 0.000 0.000 0.22(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 Au1 P1 2.241(2) . ? Au1 Cl1 2.313(2) . ? Au1 Ag1 3.2180(4) . ? Ag1 Cl1 2.624(2) 2_675 ? Ag1 Cl1 2.624(2) 15_466 ? Ag1 Cl1 2.624(2) . ? Ag1 Cl1 2.624(2) 16_656 ? Ag1 Au1 3.2180(4) 15_466 ? Ag1 Au1 3.2180(4) 16_656 ? Ag1 Au1 3.2180(4) 2_675 ? P1 C1A 1.805(9) . ? P1 C1B 1.810(9) . ? P1 C4 1.844(8) . ? C1 C2 1.366(13) . ? C1 C1 1.37(2) 10_557 ? C2 C3 1.416(11) . ? C3 C4 1.404(10) . ? C3 C3 1.437(15) 10_557 ? C4 C5 1.407(11) . ? C5 C5 1.427(15) 10_557 ? C5 C6 1.437(11) . ? C6 C7 1.352(12) . ? C7 C7 1.384(19) 10_557 ? C1A C6A 1.390(11) . ? C1A C2A 1.405(12) . ? C2A C3A 1.404(13) . ? C3A C4A 1.394(14) . ? C4A C5A 1.375(14) . ? C5A C6A 1.363(12) . ? C1B C2B 1.377(13) . ? C1B C6B 1.385(14) . ? C2B C3B 1.369(13) . ? C3B C4B 1.360(16) . ? C4B C5B 1.376(19) . ? C5B C6B 1.376(15) . ? Sb1 F3 1.68(3) . ? Sb1 F2 1.69(3) . ? Sb1 F1 1.719(18) 2_665 ? Sb1 F1 1.719(18) 3_655 ? Sb1 F1 1.719(19) 4_565 ? Sb1 F1 1.719(18) . ? Sb2 F4 1.819(10) 9 ? Sb2 F4 1.819(10) . ? Sb2 F4 1.819(10) 3 ? Sb2 F4 1.819(10) 11 ? Sb2 F5 1.826(16) 9 ? Sb2 F5 1.826(16) . ? Cl2B C100 1.83(3) 10_557 ? Cl2B C100 1.83(3) . ? Cl2A C100 1.82(3) . ? Cl2A C100 1.82(3) 10_557 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 174.95(8) . . ? P1 Au1 Ag1 127.08(6) . . ? Cl1 Au1 Ag1 53.66(6) . . ? Cl1 Ag1 Cl1 115.00(5) 2_675 15_466 ? Cl1 Ag1 Cl1 98.90(9) 2_675 . ? Cl1 Ag1 Cl1 115.00(5) 15_466 . ? Cl1 Ag1 Cl1 115.00(5) 2_675 16_656 ? Cl1 Ag1 Cl1 98.90(9) 15_466 16_656 ? Cl1 Ag1 Cl1 115.00(5) . 16_656 ? Cl1 Ag1 Au1 160.16(5) 2_675 15_466 ? Cl1 Ag1 Au1 45.25(5) 15_466 15_466 ? Cl1 Ag1 Au1 93.48(5) . 15_466 ? Cl1 Ag1 Au1 72.70(5) 16_656 15_466 ? Cl1 Ag1 Au1 93.48(5) 2_675 16_656 ? Cl1 Ag1 Au1 72.70(5) 15_466 16_656 ? Cl1 Ag1 Au1 160.16(5) . 16_656 ? Cl1 Ag1 Au1 45.25(5) 16_656 16_656 ? Au1 Ag1 Au1 79.256(15) 15_466 16_656 ? Cl1 Ag1 Au1 45.25(5) 2_675 2_675 ? Cl1 Ag1 Au1 93.48(5) 15_466 2_675 ? Cl1 Ag1 Au1 72.70(5) . 2_675 ? Cl1 Ag1 Au1 160.16(5) 16_656 2_675 ? Au1 Ag1 Au1 126.385(9) 15_466 2_675 ? Au1 Ag1 Au1 126.385(9) 16_656 2_675 ? Cl1 Ag1 Au1 72.70(5) 2_675 . ? Cl1 Ag1 Au1 160.16(5) 15_466 . ? Cl1 Ag1 Au1 45.25(5) . . ? Cl1 Ag1 Au1 93.48(5) 16_656 . ? Au1 Ag1 Au1 126.385(9) 15_466 . ? Au1 Ag1 Au1 126.385(9) 16_656 . ? Au1 Ag1 Au1 79.256(15) 2_675 . ? Au1 Cl1 Ag1 81.08(7) . . ? C1A P1 C1B 108.5(4) . . ? C1A P1 C4 106.1(4) . . ? C1B P1 C4 109.2(4) . . ? C1A P1 Au1 113.8(3) . . ? C1B P1 Au1 103.2(3) . . ? C4 P1 Au1 115.8(3) . . ? C2 C1 C1 121.2(6) . 10_557 ? C1 C2 C3 120.2(8) . . ? C4 C3 C2 121.8(7) . . ? C4 C3 C3 119.6(4) . 10_557 ? C2 C3 C3 118.5(5) . 10_557 ? C3 C4 C5 119.4(7) . . ? C3 C4 P1 118.0(6) . . ? C5 C4 P1 122.5(6) . . ? C4 C5 C5 119.8(4) . 10_557 ? C4 C5 C6 123.3(7) . . ? C5 C5 C6 116.8(5) 10_557 . ? C7 C6 C5 123.6(8) . . ? C6 C7 C7 119.6(5) . 10_557 ? C6A C1A C2A 119.7(8) . . ? C6A C1A P1 119.7(7) . . ? C2A C1A P1 120.6(7) . . ? C3A C2A C1A 118.5(9) . . ? C4A C3A C2A 120.3(10) . . ? C5A C4A C3A 119.8(9) . . ? C6A C5A C4A 120.6(9) . . ? C5A C6A C1A 121.0(9) . . ? C2B C1B C6B 118.2(9) . . ? C2B C1B P1 123.8(7) . . ? C6B C1B P1 117.9(8) . . ? C3B C2B C1B 121.4(10) . . ? C4B C3B C2B 121.0(11) . . ? C3B C4B C5B 117.9(11) . . ? C6B C5B C4B 122.2(12) . . ? C5B C6B C1B 119.2(11) . . ? F3 Sb1 F2 180.000(13) . . ? F3 Sb1 F1 94.7(8) . 2_665 ? F2 Sb1 F1 85.3(8) . 2_665 ? F3 Sb1 F1 94.7(8) . 3_655 ? F2 Sb1 F1 85.3(8) . 3_655 ? F1 Sb1 F1 89.62(14) 2_665 3_655 ? F3 Sb1 F1 94.7(8) . 4_565 ? F2 Sb1 F1 85.3(8) . 4_565 ? F1 Sb1 F1 89.62(14) 2_665 4_565 ? F1 Sb1 F1 170.6(17) 3_655 4_565 ? F3 Sb1 F1 94.7(8) . . ? F2 Sb1 F1 85.3(8) . . ? F1 Sb1 F1 170.6(17) 2_665 . ? F1 Sb1 F1 89.62(14) 3_655 . ? F1 Sb1 F1 89.62(14) 4_565 . ? F4 Sb2 F4 180.0(7) 9 . ? F4 Sb2 F4 90.0 9 3 ? F4 Sb2 F4 90.0 . 3 ? F4 Sb2 F4 90.0 9 11 ? F4 Sb2 F4 90.0 . 11 ? F4 Sb2 F4 180.0 3 11 ? F4 Sb2 F5 90.0 9 9 ? F4 Sb2 F5 90.0 . 9 ? F4 Sb2 F5 90.0 3 9 ? F4 Sb2 F5 90.0 11 9 ? F4 Sb2 F5 90.0 9 . ? F4 Sb2 F5 90.0 . . ? F4 Sb2 F5 90.0 3 . ? F4 Sb2 F5 90.0 11 . ? F5 Sb2 F5 180.0 9 . ? C100 Cl2B C100 88(2) 10_557 . ? C100 Cl2A C100 89(2) . 10_557 ? Cl2A C100 Cl2B 92(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.505 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.222