# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Vivian Yam' 'Eddie Chung-Chin Cheng' 'Nianyong Zhu' _publ_contact_author_name 'Prof Vivian Yam' _publ_contact_author_address ; ? ; _publ_contact_author_email 'wwyan@hku.hk' _publ_section_title ; Synthesis, photophysics, and electrochemistry of hexanuclear siliver(I) chalcogenolate complexes. X-ray crystal structures of [Ag6(m-dppm) 4(m3-SC6HMe-p)4](PF6)2 and [Ag6(m-dppm)4(m3-SeC6H4Cl-p)4](PF6)2 ; data_mar57 _database_code_CSD 171524 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C140 H100 Ag6 P6 S4' _chemical_formula_sum 'C128 H116 Ag6 F12 P10 S4' _chemical_formula_weight 2967.37 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4' 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' _cell_length_a 16.140(2) _cell_length_b 16.140(2) _cell_length_c 27.624(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7195.5(16) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5778 _exptl_absorpt_correction_T_max 0.8209 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29063 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.58 _reflns_number_total 6660 _reflns_number_gt 6118 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0810P)^2^+0.0421P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 6660 _refine_ls_number_parameters 366 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.515 _refine_ls_shift/su_mean 0.043 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 0.02393(2) 0.62848(2) 0.217666(13) 0.06414(13) Uani 1 1 d . . . P1 P 0.00613(9) 0.74253(7) 0.16204(5) 0.0593(3) Uani 1 1 d . . . S1 S -0.00687(7) 0.61709(8) 0.30576(4) 0.0590(3) Uani 1 1 d . . . C19 C -0.1230(5) 0.8205(4) 0.1115(3) 0.0873(17) Uani 1 1 d . . . H19 H -0.0832 0.8455 0.0921 0.105 Uiso 1 1 calc R . . C14 C -0.1000(4) 0.7685(3) 0.1483(2) 0.0715(13) Uani 1 1 d . . . C15 C -0.1615(5) 0.7273(5) 0.1735(4) 0.106(2) Uani 1 1 d . . . H15 H -0.1469 0.6874 0.1963 0.127 Uiso 1 1 calc R . . C8 C 0.0542(4) 0.8388(3) 0.1831(2) 0.0737(14) Uani 1 1 d . . . C6 C -0.0088(5) 0.7697(4) 0.3488(3) 0.0880(17) Uani 1 1 d . . . H6 H 0.0464 0.7600 0.3566 0.106 Uiso 1 1 calc R . . C13 C 0.0818(6) 0.9010(4) 0.1537(3) 0.105(2) Uani 1 1 d . . . H13 H 0.0780 0.8952 0.1202 0.126 Uiso 1 1 calc R . . C4 C -0.1284(8) 0.8611(6) 0.3497(3) 0.121(3) Uani 1 1 d . . . C5 C -0.0461(8) 0.8430(5) 0.3621(3) 0.119(3) Uani 1 1 d . . . H5 H -0.0158 0.8815 0.3798 0.143 Uiso 1 1 calc R . . C1 C -0.0540(4) 0.7102(3) 0.32376(19) 0.0685(13) Uani 1 1 d . . . C18 C -0.2091(8) 0.8357(8) 0.1035(4) 0.148(5) Uani 1 1 d . . . H18 H -0.2271 0.8705 0.0788 0.177 Uiso 1 1 calc R . . C11 C 0.1191(9) 0.9814(6) 0.2221(5) 0.152(5) Uani 1 1 d . . . H11 H 0.1405 1.0293 0.2360 0.182 Uiso 1 1 calc R . . C12 C 0.1153(7) 0.9721(5) 0.1730(4) 0.120(3) Uani 1 1 d . . . H12 H 0.1353 1.0136 0.1527 0.144 Uiso 1 1 calc R . . C10 C 0.0921(13) 0.9217(7) 0.2483(5) 0.211(9) Uani 1 1 d . . . H10 H 0.0933 0.9288 0.2817 0.254 Uiso 1 1 calc R . . C9 C 0.0623(10) 0.8495(6) 0.2312(3) 0.150(5) Uani 1 1 d . . . H9 H 0.0473 0.8074 0.2525 0.180 Uiso 1 1 calc R . . C2 C -0.1376(5) 0.7290(4) 0.3124(3) 0.0856(17) Uani 1 1 d . . . H2 H -0.1697 0.6907 0.2957 0.103 Uiso 1 1 calc R . . C3 C -0.1715(7) 0.8030(6) 0.3261(3) 0.115(3) Uani 1 1 d . . . H3 H -0.2267 0.8134 0.3186 0.138 Uiso 1 1 calc R . . C16 C -0.2458(6) 0.7448(9) 0.1654(6) 0.147(4) Uani 1 1 d . . . H16 H -0.2855 0.7171 0.1836 0.177 Uiso 1 1 calc R . . C7 C -0.1702(11) 0.9444(7) 0.3616(6) 0.189(7) Uani 1 1 d . . . H7A H -0.1311 0.9801 0.3774 0.284 Uiso 1 1 calc R . . H7B H -0.2166 0.9349 0.3827 0.284 Uiso 1 1 calc R . . H7C H -0.1891 0.9700 0.3323 0.284 Uiso 1 1 calc R . . C17 C -0.2680(7) 0.7940(9) 0.1358(6) 0.149(4) Uani 1 1 d . . . H17 H -0.3241 0.8063 0.1333 0.179 Uiso 1 1 calc R . . Ag2 Ag 0.0000 0.5000 0.124439(17) 0.05977(14) Uani 1 2 d S . . P2 P 0.01874(8) 0.62723(7) 0.07425(4) 0.0544(2) Uani 1 1 d . . . C31 C 0.0833(5) 0.5836(4) -0.0166(2) 0.0799(15) Uani 1 1 d . . . H31 H 0.0292 0.5845 -0.0282 0.096 Uiso 1 1 calc R . . C32 C 0.0566(3) 0.7229(3) 0.1042(2) 0.0625(11) Uani 1 1 d . . . H32A H 0.1159 0.7182 0.1094 0.075 Uiso 1 1 calc R . . H32B H 0.0471 0.7697 0.0829 0.075 Uiso 1 1 calc R . . C20 C -0.0672(4) 0.6616(3) 0.0371(2) 0.0664(12) Uani 1 1 d . . . C27 C 0.1840(4) 0.6014(4) 0.0476(2) 0.0748(13) Uani 1 1 d . . . H27 H 0.1964 0.6132 0.0797 0.090 Uiso 1 1 calc R . . C25 C -0.1422(4) 0.6242(4) 0.0417(3) 0.0854(16) Uani 1 1 d . . . H25 H -0.1484 0.5806 0.0634 0.103 Uiso 1 1 calc R . . C26 C 0.1012(3) 0.6054(3) 0.03114(18) 0.0627(11) Uani 1 1 d . . . C24 C -0.2087(5) 0.6498(6) 0.0148(5) 0.125(3) Uani 1 1 d . . . H24 H -0.2603 0.6250 0.0187 0.150 Uiso 1 1 calc R . . C21 C -0.0590(5) 0.7267(4) 0.0049(3) 0.0883(18) Uani 1 1 d . . . H21 H -0.0080 0.7532 0.0024 0.106 Uiso 1 1 calc R . . C22 C -0.1233(7) 0.7537(6) -0.0235(4) 0.117(3) Uani 1 1 d . . . H22 H -0.1160 0.7974 -0.0450 0.141 Uiso 1 1 calc R . . C23 C -0.1974(8) 0.7154(7) -0.0195(5) 0.138(4) Uani 1 1 d . . . H23 H -0.2413 0.7318 -0.0392 0.165 Uiso 1 1 calc R . . C30 C 0.1510(7) 0.5599(6) -0.0472(3) 0.111(3) Uani 1 1 d . . . H30 H 0.1408 0.5449 -0.0792 0.134 Uiso 1 1 calc R . . C28 C 0.2461(5) 0.5800(5) 0.0160(3) 0.093(2) Uani 1 1 d . . . H28 H 0.3008 0.5799 0.0266 0.112 Uiso 1 1 calc R . . C29 C 0.2290(6) 0.5591(5) -0.0302(3) 0.101(2) Uani 1 1 d . . . H29 H 0.2720 0.5438 -0.0507 0.122 Uiso 1 1 calc R . . P4 P 0.0000 1.0000 0.0000 0.0836(8) Uani 1 4 d S . . P3 P 0.5000 0.5000 0.0000 0.0863(9) Uani 1 4 d SD . . F1 F 0.5442(4) 0.4170(4) 0.0027(6) 0.240(6) Uani 1 1 d D . . F2 F 0.5000 0.5000 0.0529(5) 0.322(12) Uani 1 2 d SD . . F3 F -0.0325(7) 1.0823(6) 0.0193(7) 0.192(6) Uani 0.75 1 d P . . F4 F 0.0592(13) 1.0240(10) 0.0397(7) 0.287(12) Uani 0.75 1 d P . . 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 0.0739(2) 0.0576(2) 0.0609(2) 0.00590(16) 0.00553(17) -0.00218(17) P1 0.0763(8) 0.0456(5) 0.0559(6) 0.0021(5) 0.0031(5) 0.0021(5) S1 0.0617(6) 0.0579(6) 0.0576(6) 0.0042(5) 0.0061(5) 0.0026(5) C19 0.105(5) 0.074(3) 0.083(4) 0.003(3) -0.004(3) 0.024(3) C14 0.079(3) 0.062(3) 0.074(3) -0.008(2) -0.001(3) 0.014(2) C15 0.092(5) 0.102(5) 0.125(7) 0.019(5) 0.024(5) 0.007(4) C8 0.104(4) 0.050(3) 0.066(3) -0.001(2) -0.006(3) -0.002(3) C6 0.109(5) 0.074(4) 0.081(4) -0.015(3) 0.006(3) -0.004(3) C13 0.150(7) 0.066(4) 0.098(5) -0.001(3) 0.014(5) -0.027(4) C4 0.171(9) 0.086(5) 0.105(6) -0.018(4) 0.040(6) 0.032(5) C5 0.184(10) 0.081(4) 0.093(5) -0.021(4) 0.028(6) -0.006(5) C1 0.085(3) 0.063(3) 0.058(3) -0.002(2) 0.010(2) 0.005(2) C18 0.171(10) 0.136(8) 0.135(8) -0.037(7) -0.067(8) 0.091(8) C11 0.213(13) 0.086(5) 0.157(10) -0.021(6) -0.043(9) -0.044(7) C12 0.149(8) 0.068(4) 0.144(9) 0.012(4) 0.004(6) -0.032(4) C10 0.41(3) 0.114(7) 0.110(7) 0.001(7) -0.069(13) -0.117(12) C9 0.277(15) 0.098(6) 0.076(4) -0.015(4) -0.011(6) -0.061(8) C2 0.094(4) 0.087(4) 0.077(4) -0.018(3) 0.002(3) 0.021(3) C3 0.143(7) 0.104(6) 0.099(6) -0.014(4) 0.013(5) 0.054(5) C16 0.087(6) 0.162(10) 0.193(12) 0.037(9) 0.004(7) 0.022(6) C7 0.29(2) 0.097(7) 0.177(12) -0.038(8) 0.018(12) 0.068(10) C17 0.091(6) 0.157(10) 0.200(13) 0.004(10) -0.006(7) 0.021(6) Ag2 0.0729(3) 0.0532(3) 0.0532(2) 0.000 0.000 -0.0064(2) P2 0.0660(7) 0.0465(6) 0.0507(5) 0.0040(4) 0.0024(5) 0.0011(5) C31 0.098(4) 0.083(4) 0.059(3) -0.005(3) 0.002(3) 0.004(3) C32 0.072(3) 0.050(2) 0.066(3) 0.006(2) 0.012(2) -0.0031(19) C20 0.077(3) 0.053(3) 0.069(3) 0.000(2) 0.000(2) 0.005(2) C27 0.070(3) 0.075(3) 0.080(3) 0.003(3) 0.009(3) 0.002(3) C25 0.083(4) 0.071(3) 0.102(4) -0.006(3) -0.009(3) 0.010(3) C26 0.083(3) 0.048(2) 0.058(2) 0.0046(19) 0.006(2) 0.003(2) C24 0.075(4) 0.123(7) 0.178(10) -0.023(7) -0.033(5) 0.014(4) C21 0.102(4) 0.081(4) 0.082(4) 0.018(3) -0.008(3) 0.012(3) C22 0.131(7) 0.113(6) 0.108(6) 0.021(5) -0.032(5) 0.037(5) C23 0.139(9) 0.126(7) 0.149(9) 0.000(7) -0.063(7) 0.038(7) C30 0.159(9) 0.112(6) 0.063(4) -0.002(4) 0.029(4) 0.023(5) C28 0.082(4) 0.090(4) 0.108(5) -0.013(4) 0.029(4) 0.002(3) C29 0.103(5) 0.102(5) 0.099(5) 0.000(4) 0.039(5) 0.020(4) P4 0.0887(13) 0.0887(13) 0.0735(18) 0.000 0.000 0.000 P3 0.0687(10) 0.0687(10) 0.121(3) 0.000 0.000 0.000 F1 0.091(3) 0.093(3) 0.54(2) 0.003(7) 0.029(7) 0.016(3) F2 0.41(3) 0.44(4) 0.115(9) 0.000 0.000 0.02(3) F3 0.150(7) 0.114(6) 0.313(17) -0.077(8) 0.036(10) -0.001(5) F4 0.33(2) 0.192(13) 0.34(2) -0.097(15) -0.21(2) 0.009(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4151(13) . ? Ag1 S1 2.4906(13) . ? Ag1 S1 2.5557(13) 7_455 ? Ag1 Ag2 3.3288(6) . ? P1 C14 1.803(6) . ? P1 C32 1.820(5) . ? P1 C8 1.831(6) . ? S1 C1 1.757(5) . ? S1 Ag1 2.5557(13) 8 ? S1 Ag2 2.7021(13) 7_455 ? C19 C14 1.369(9) . ? C19 C18 1.429(14) . ? C14 C15 1.383(10) . ? C15 C16 1.408(13) . ? C8 C9 1.348(10) . ? C8 C13 1.366(9) . ? C6 C5 1.377(11) . ? C6 C1 1.390(9) . ? C13 C12 1.377(11) . ? C4 C3 1.337(15) . ? C4 C5 1.403(16) . ? C4 C7 1.539(12) . ? C1 C2 1.418(10) . ? C18 C17 1.47(2) . ? C11 C10 1.283(17) . ? C11 C12 1.366(16) . ? C10 C9 1.346(12) . ? C2 C3 1.366(10) . ? C16 C17 1.194(17) . ? Ag2 P2 2.4959(11) 2_565 ? Ag2 P2 2.4959(11) . ? Ag2 S1 2.7021(13) 7_455 ? Ag2 S1 2.7021(13) 8 ? Ag2 Ag1 3.3288(6) 2_565 ? P2 C20 1.812(6) . ? P2 C26 1.820(5) . ? P2 C32 1.855(5) . ? C31 C26 1.395(8) . ? C31 C30 1.433(11) . ? C20 C25 1.358(9) . ? C20 C21 1.384(9) . ? C27 C28 1.373(9) . ? C27 C26 1.413(8) . ? C25 C24 1.370(12) . ? C24 C23 1.433(17) . ? C21 C22 1.371(11) . ? C22 C23 1.351(16) . ? C30 C29 1.344(13) . ? C28 C29 1.349(12) . ? P4 F4 1.506(11) 4_665 ? P4 F4 1.506(11) . ? P4 F4 1.506(11) 3_465 ? P4 F4 1.506(11) 2_575 ? P4 F3 1.524(9) 4_665 ? P4 F3 1.524(9) 3_465 ? P4 F3 1.524(9) . ? P4 F3 1.524(9) 2_575 ? P3 F2 1.460(13) . ? P3 F2 1.460(13) 3_565 ? P3 F1 1.519(6) 2_665 ? P3 F1 1.519(6) 3_565 ? P3 F1 1.519(6) 4_655 ? P3 F1 1.519(6) . ? F3 F4 1.68(2) 4_665 ? F4 F3 1.68(2) 3_465 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 S1 130.86(5) . . ? P1 Ag1 S1 119.62(4) . 7_455 ? S1 Ag1 S1 107.95(4) . 7_455 ? P1 Ag1 Ag2 88.21(3) . . ? S1 Ag1 Ag2 133.38(3) . . ? S1 Ag1 Ag2 52.70(3) 7_455 . ? C14 P1 C32 106.3(3) . . ? C14 P1 C8 105.8(3) . . ? C32 P1 C8 103.7(3) . . ? C14 P1 Ag1 115.1(2) . . ? C32 P1 Ag1 111.83(17) . . ? C8 P1 Ag1 113.22(19) . . ? C1 S1 Ag1 107.45(18) . . ? C1 S1 Ag1 104.0(2) . 8 ? Ag1 S1 Ag1 87.09(4) . 8 ? C1 S1 Ag2 114.48(18) . 7_455 ? Ag1 S1 Ag2 137.78(5) . 7_455 ? Ag1 S1 Ag2 78.51(3) 8 7_455 ? C14 C19 C18 119.0(9) . . ? C19 C14 C15 118.3(7) . . ? C19 C14 P1 123.8(5) . . ? C15 C14 P1 117.7(5) . . ? C14 C15 C16 121.1(9) . . ? C9 C8 C13 117.4(6) . . ? C9 C8 P1 117.6(6) . . ? C13 C8 P1 125.0(5) . . ? C5 C6 C1 119.8(8) . . ? C8 C13 C12 120.7(8) . . ? C3 C4 C5 117.7(8) . . ? C3 C4 C7 119.3(12) . . ? C5 C4 C7 123.0(11) . . ? C6 C5 C4 121.9(9) . . ? C6 C1 C2 117.5(6) . . ? C6 C1 S1 120.3(5) . . ? C2 C1 S1 122.2(5) . . ? C19 C18 C17 117.2(10) . . ? C10 C11 C12 117.7(8) . . ? C11 C12 C13 119.6(8) . . ? C11 C10 C9 125.0(12) . . ? C10 C9 C8 119.5(9) . . ? C3 C2 C1 120.4(7) . . ? C4 C3 C2 122.7(9) . . ? C17 C16 C15 122.3(13) . . ? C16 C17 C18 121.7(11) . . ? P2 Ag2 P2 112.52(5) 2_565 . ? P2 Ag2 S1 120.99(4) 2_565 7_455 ? P2 Ag2 S1 106.13(4) . 7_455 ? P2 Ag2 S1 106.13(4) 2_565 8 ? P2 Ag2 S1 120.99(4) . 8 ? S1 Ag2 S1 88.95(6) 7_455 8 ? P2 Ag2 Ag1 162.98(3) 2_565 . ? P2 Ag2 Ag1 84.44(3) . . ? S1 Ag2 Ag1 48.79(3) 7_455 . ? S1 Ag2 Ag1 63.56(3) 8 . ? P2 Ag2 Ag1 84.44(3) 2_565 2_565 ? P2 Ag2 Ag1 162.98(3) . 2_565 ? S1 Ag2 Ag1 63.56(3) 7_455 2_565 ? S1 Ag2 Ag1 48.79(3) 8 2_565 ? Ag1 Ag2 Ag1 78.637(19) . 2_565 ? C20 P2 C26 104.3(3) . . ? C20 P2 C32 104.5(2) . . ? C26 P2 C32 102.3(2) . . ? C20 P2 Ag2 118.26(18) . . ? C26 P2 Ag2 107.04(15) . . ? C32 P2 Ag2 118.44(17) . . ? C26 C31 C30 117.9(7) . . ? P1 C32 P2 112.9(3) . . ? C25 C20 C21 118.9(6) . . ? C25 C20 P2 119.5(5) . . ? C21 C20 P2 121.5(5) . . ? C28 C27 C26 119.9(7) . . ? C20 C25 C24 120.9(8) . . ? C31 C26 C27 119.1(5) . . ? C31 C26 P2 121.1(5) . . ? C27 C26 P2 119.4(4) . . ? C25 C24 C23 118.8(9) . . ? C22 C21 C20 122.4(8) . . ? C23 C22 C21 118.7(9) . . ? C22 C23 C24 120.2(8) . . ? C29 C30 C31 120.6(7) . . ? C29 C28 C27 121.0(8) . . ? C30 C29 C28 121.4(7) . . ? F4 P4 F4 122.1(12) 4_665 . ? F4 P4 F4 86(2) 4_665 3_465 ? F4 P4 F4 122.1(12) . 3_465 ? F4 P4 F4 122.1(12) 4_665 2_575 ? F4 P4 F4 86(2) . 2_575 ? F4 P4 F4 122.1(12) 3_465 2_575 ? F4 P4 F3 74.9(9) 4_665 4_665 ? F4 P4 F3 153.6(15) . 4_665 ? F4 P4 F3 75.6(9) 3_465 4_665 ? F4 P4 F3 67.3(9) 2_575 4_665 ? F4 P4 F3 75.6(9) 4_665 3_465 ? F4 P4 F3 67.3(9) . 3_465 ? F4 P4 F3 74.9(9) 3_465 3_465 ? F4 P4 F3 153.6(15) 2_575 3_465 ? F3 P4 F3 139.1(15) 4_665 3_465 ? F4 P4 F3 67.3(9) 4_665 . ? F4 P4 F3 74.9(9) . . ? F4 P4 F3 153.6(15) 3_465 . ? F4 P4 F3 75.6(9) 2_575 . ? F3 P4 F3 97.0(5) 4_665 . ? F3 P4 F3 97.0(5) 3_465 . ? F4 P4 F3 153.6(15) 4_665 2_575 ? F4 P4 F3 75.6(9) . 2_575 ? F4 P4 F3 67.3(9) 3_465 2_575 ? F4 P4 F3 74.9(9) 2_575 2_575 ? F3 P4 F3 97.0(5) 4_665 2_575 ? F3 P4 F3 97.0(5) 3_465 2_575 ? F3 P4 F3 139.1(15) . 2_575 ? F2 P3 F2 180.0 . 3_565 ? F2 P3 F1 87.2(6) . 2_665 ? F2 P3 F1 92.8(6) 3_565 2_665 ? F2 P3 F1 92.8(6) . 3_565 ? F2 P3 F1 87.2(6) 3_565 3_565 ? F1 P3 F1 90.13(6) 2_665 3_565 ? F2 P3 F1 92.8(6) . 4_655 ? F2 P3 F1 87.2(6) 3_565 4_655 ? F1 P3 F1 90.13(6) 2_665 4_655 ? F1 P3 F1 174.5(13) 3_565 4_655 ? F2 P3 F1 87.2(6) . . ? F2 P3 F1 92.8(6) 3_565 . ? F1 P3 F1 174.5(13) 2_665 . ? F1 P3 F1 90.13(6) 3_565 . ? F1 P3 F1 90.13(6) 4_655 . ? P4 F3 F4 55.9(6) . 4_665 ? P4 F4 F3 56.9(6) . 3_465 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.58 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.103 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.318 data_mar61 _database_code_CSD 171525 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H80 Ag6 Cl4 F12 P10 Se4' _chemical_formula_sum 'C124 H104 Ag6 Cl4 F12 P10 Se4' _chemical_formula_weight 3236.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ag' 'Ag' -0.8971 1.1015 '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' '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' '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4' 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' _cell_length_a 16.021(2) _cell_length_b 16.021(2) _cell_length_c 27.512(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7061.6(16) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 2.094 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8251 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.57 _reflns_number_total 5010 _reflns_number_gt 4059 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(14) _refine_ls_number_reflns 5010 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1112 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Ag1 Ag 0.5000 0.5000 0.87092(3) 0.0617(2) Uani 1 2 d S . . Ag2 Ag 0.62888(4) 0.52535(4) 0.96589(2) 0.07211(19) Uani 1 1 d . . . Se1 Se 0.50442(5) 0.62546(5) 0.94152(3) 0.0693(2) Uani 1 1 d . . . P1 P 0.62855(11) 0.51746(12) 0.82140(6) 0.0570(4) Uani 1 1 d . . . P2 P 0.74424(11) 0.50487(14) 0.90970(7) 0.0634(5) Uani 1 1 d . . . P3 P 0.5000 1.0000 0.7500 0.105(2) Uani 1 4 d S . . P4 P 1.0000 0.5000 0.7500 0.0835(13) Uani 1 4 d S . . Cl1 Cl 0.6968(6) 0.9669(3) 0.8950(2) 0.299(5) Uani 1 1 d . . . C1 C 0.5662(8) 0.7250(5) 0.9261(3) 0.087(3) Uani 1 1 d . . . C2 C 0.6476(8) 0.7350(6) 0.9407(4) 0.100(3) Uani 1 1 d . . . H2 H 0.6747 0.6927 0.9576 0.120 Uiso 1 1 calc R . . C3 C 0.6899(12) 0.8101(10) 0.9296(7) 0.158(7) Uani 1 1 d . . . H3 H 0.7457 0.8190 0.9373 0.190 Uiso 1 1 calc R . . C4 C 0.637(2) 0.8744(10) 0.9045(7) 0.185(12) Uani 1 1 d . . . C5 C 0.5597(16) 0.8610(10) 0.8897(7) 0.164(8) Uani 1 1 d . . . H5 H 0.5307 0.9010 0.8720 0.197 Uiso 1 1 calc R . . C6 C 0.5252(11) 0.7886(8) 0.9011(5) 0.130(5) Uani 1 1 d . . . H6 H 0.4701 0.7796 0.8918 0.156 Uiso 1 1 calc R . . C7 C 0.7253(4) 0.5547(5) 0.8506(3) 0.067(2) Uani 1 1 d . . . H7A H 0.7722 0.5434 0.8292 0.081 Uiso 1 1 calc R . . H7B H 0.7218 0.6146 0.8550 0.081 Uiso 1 1 calc R . . C8 C 0.6048(4) 0.6020(5) 0.7787(3) 0.0633(18) Uani 1 1 d . . . C9 C 0.6006(5) 0.6832(5) 0.7961(4) 0.077(2) Uani 1 1 d . . . H9 H 0.6149 0.6942 0.8282 0.092 Uiso 1 1 calc R . . C10 C 0.5756(6) 0.7476(6) 0.7665(5) 0.093(3) Uani 1 1 d . . . H10 H 0.5738 0.8020 0.7783 0.111 Uiso 1 1 calc R . . C11 C 0.5534(7) 0.7311(8) 0.7193(5) 0.105(3) Uani 1 1 d . . . H11 H 0.5375 0.7746 0.6990 0.126 Uiso 1 1 calc R . . C12 C 0.5545(7) 0.6518(8) 0.7021(4) 0.100(3) Uani 1 1 d . . . H12 H 0.5378 0.6410 0.6704 0.120 Uiso 1 1 calc R . . C13 C 0.5806(6) 0.5858(6) 0.7321(3) 0.080(2) Uani 1 1 d . . . H13 H 0.5814 0.5314 0.7202 0.096 Uiso 1 1 calc R . . C14 C 0.6625(5) 0.4314(5) 0.7832(3) 0.069(2) Uani 1 1 d . . . C15 C 0.7257(6) 0.4421(7) 0.7491(4) 0.090(3) Uani 1 1 d . . . H15 H 0.7506 0.4942 0.7458 0.108 Uiso 1 1 calc R . . C16 C 0.7517(9) 0.3774(10) 0.7203(5) 0.127(4) Uani 1 1 d . . . H16 H 0.7937 0.3847 0.6973 0.153 Uiso 1 1 calc R . . C17 C 0.7140(10) 0.3023(10) 0.7265(7) 0.139(5) Uani 1 1 d . . . H17 H 0.7303 0.2580 0.7068 0.167 Uiso 1 1 calc R . . C18 C 0.6521(8) 0.2886(8) 0.7610(7) 0.128(5) Uani 1 1 d . . . H18 H 0.6285 0.2360 0.7650 0.154 Uiso 1 1 calc R . . C19 C 0.6267(6) 0.3547(5) 0.7891(5) 0.090(3) Uani 1 1 d . . . H19 H 0.5850 0.3472 0.8122 0.108 Uiso 1 1 calc R . . C20 C 0.7705(5) 0.3968(5) 0.8961(3) 0.070(2) Uani 1 1 d . . . C21 C 0.7353(7) 0.3372(7) 0.9245(5) 0.107(3) Uani 1 1 d . . . H21 H 0.7003 0.3532 0.9498 0.129 Uiso 1 1 calc R . . C22 C 0.7499(11) 0.2533(9) 0.9167(8) 0.162(7) Uani 1 1 d . . . H22 H 0.7268 0.2134 0.9373 0.195 Uiso 1 1 calc R . . C23 C 0.7989(11) 0.2295(10) 0.8783(8) 0.151(6) Uani 1 1 d . . . H23 H 0.8067 0.1733 0.8712 0.181 Uiso 1 1 calc R . . C24 C 0.8354(8) 0.2887(11) 0.8511(5) 0.120(4) Uani 1 1 d . . . H24 H 0.8726 0.2730 0.8268 0.144 Uiso 1 1 calc R . . C25 C 0.8192(6) 0.3727(7) 0.8584(4) 0.095(3) Uani 1 1 d . . . H25 H 0.8415 0.4124 0.8374 0.114 Uiso 1 1 calc R . . C26 C 0.8415(5) 0.5537(6) 0.9307(3) 0.074(2) Uani 1 1 d . . . C27 C 0.9025(5) 0.5811(7) 0.9005(4) 0.103(3) Uani 1 1 d . . . H27 H 0.8969 0.5768 0.8669 0.123 Uiso 1 1 calc R . . C28 C 0.9735(7) 0.6159(10) 0.9211(7) 0.133(5) Uani 1 1 d . . . H28 H 1.0155 0.6349 0.9006 0.159 Uiso 1 1 calc R . . C29 C 0.9840(8) 0.6231(11) 0.9668(7) 0.147(6) Uani 1 1 d . . . H29 H 1.0334 0.6456 0.9787 0.176 Uiso 1 1 calc R . . C30 C 0.9223(9) 0.5978(15) 0.9990(6) 0.199(10) Uani 1 1 d . . . H30 H 0.9285 0.6048 1.0324 0.239 Uiso 1 1 calc R . . C31 C 0.8500(8) 0.5613(11) 0.9792(4) 0.148(6) Uani 1 1 d . . . H31 H 0.8079 0.5423 0.9997 0.177 Uiso 1 1 calc R . . F1 F 0.5806(5) 0.9553(5) 0.7562(8) 0.242(8) Uani 1 1 d . . . F2 F 0.5000 1.0000 0.7006(14) 0.53(4) Uani 1 2 d S . . F3 F 0.9168(9) 0.5302(10) 0.7705(8) 0.186(6) Uani 0.75 1 d P . . F4 F 1.0278(12) 0.5636(15) 0.7848(10) 0.271(13) Uani 0.75 1 d P . . 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 0.0551(4) 0.0756(5) 0.0545(4) 0.000 0.000 -0.0071(4) Ag2 0.0644(3) 0.0819(4) 0.0700(4) -0.0003(3) 0.0114(3) -0.0051(3) Se1 0.0724(5) 0.0695(5) 0.0661(4) -0.0161(4) 0.0064(4) -0.0019(4) P1 0.0511(10) 0.0672(11) 0.0526(9) 0.0015(8) 0.0027(8) 0.0006(9) P2 0.0484(9) 0.0854(14) 0.0565(11) 0.0022(10) 0.0023(8) -0.0005(9) P3 0.0720(19) 0.0720(19) 0.171(7) 0.000 0.000 0.000 P4 0.0905(19) 0.0905(19) 0.070(3) 0.000 0.000 0.000 Cl1 0.574(14) 0.133(3) 0.191(5) -0.020(3) 0.187(8) -0.161(6) C1 0.133(9) 0.068(5) 0.061(5) -0.011(4) 0.019(5) -0.007(5) C2 0.127(9) 0.092(6) 0.082(6) 0.008(6) 0.013(7) -0.041(6) C3 0.210(16) 0.132(12) 0.131(12) -0.027(10) 0.077(11) -0.087(12) C4 0.38(3) 0.081(9) 0.097(11) -0.007(8) 0.097(17) -0.082(16) C5 0.30(3) 0.079(10) 0.115(13) 0.007(8) 0.029(15) -0.023(12) C6 0.217(14) 0.090(8) 0.083(8) 0.003(6) 0.009(9) 0.027(8) C7 0.052(4) 0.077(5) 0.072(5) 0.005(4) 0.012(4) -0.004(4) C8 0.059(4) 0.072(5) 0.060(5) 0.006(4) 0.007(3) 0.001(3) C9 0.074(5) 0.078(5) 0.078(6) 0.004(5) 0.005(4) 0.006(4) C10 0.096(6) 0.071(6) 0.110(9) 0.025(5) 0.005(6) 0.006(5) C11 0.114(8) 0.109(8) 0.092(8) 0.039(7) 0.009(7) 0.016(6) C12 0.107(7) 0.126(9) 0.066(6) 0.016(6) -0.003(5) 0.017(6) C13 0.088(6) 0.084(5) 0.067(5) -0.001(4) 0.006(5) 0.014(5) C14 0.063(4) 0.074(5) 0.069(5) 0.000(4) 0.001(4) 0.017(4) C15 0.082(6) 0.103(7) 0.086(7) -0.007(5) 0.016(5) 0.018(5) C16 0.131(10) 0.131(11) 0.119(11) -0.016(8) 0.037(8) 0.042(9) C17 0.138(12) 0.117(11) 0.162(14) -0.054(10) 0.000(10) 0.041(9) C18 0.099(8) 0.089(8) 0.196(17) -0.033(8) -0.004(9) 0.016(6) C19 0.076(5) 0.071(5) 0.122(9) -0.020(6) -0.011(5) 0.014(4) C20 0.066(4) 0.082(5) 0.062(5) 0.006(4) -0.005(4) 0.010(4) C21 0.118(8) 0.085(7) 0.118(10) 0.021(6) 0.015(7) 0.019(6) C22 0.178(14) 0.096(9) 0.21(2) 0.032(10) 0.060(14) 0.016(9) C23 0.170(14) 0.109(10) 0.174(18) -0.014(10) 0.004(13) 0.037(10) C24 0.102(8) 0.153(12) 0.107(9) -0.027(9) -0.007(7) 0.050(8) C25 0.086(6) 0.117(8) 0.082(7) -0.003(6) -0.006(5) 0.031(6) C26 0.054(4) 0.105(6) 0.062(5) 0.005(4) -0.005(4) -0.009(4) C27 0.066(5) 0.154(10) 0.088(7) -0.001(7) 0.006(5) -0.032(6) C28 0.065(6) 0.201(15) 0.132(13) -0.010(10) 0.012(7) -0.037(7) C29 0.088(8) 0.205(15) 0.146(15) -0.011(13) -0.029(9) -0.050(9) C30 0.108(9) 0.38(3) 0.107(10) -0.038(16) -0.023(9) -0.093(14) C31 0.095(8) 0.273(18) 0.075(7) -0.009(9) -0.010(6) -0.071(10) F1 0.089(5) 0.093(5) 0.54(3) -0.005(9) -0.011(8) 0.005(4) F2 0.76(10) 0.63(9) 0.21(4) 0.000 0.000 -0.25(8) F3 0.134(9) 0.175(12) 0.248(18) -0.049(12) 0.073(11) -0.007(8) F4 0.213(16) 0.26(2) 0.34(3) -0.18(2) -0.087(19) 0.006(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4852(18) 2_665 ? Ag1 P1 2.4852(18) . ? Ag1 Se1 2.7960(10) . ? Ag1 Se1 2.7960(10) 2_665 ? Ag1 Ag2 3.3548(10) . ? Ag1 Ag2 3.3548(10) 2_665 ? Ag2 P2 2.432(2) . ? Ag2 Se1 2.5921(11) 3_567 ? Ag2 Se1 2.6453(11) . ? Se1 C1 1.925(10) . ? Se1 Ag2 2.5921(11) 4_657 ? P1 C14 1.817(8) . ? P1 C8 1.832(8) . ? P1 C7 1.844(8) . ? P2 C20 1.820(8) . ? P2 C26 1.837(8) . ? P2 C7 1.838(9) . ? P3 F2 1.36(4) 7_466 ? P3 F2 1.36(4) . ? P3 F1 1.487(8) 7_466 ? P3 F1 1.487(8) . ? P3 F1 1.487(8) 2_675 ? P3 F1 1.487(8) 8_656 ? P4 F4 1.467(13) 7_566 ? P4 F4 1.467(13) . ? P4 F4 1.467(13) 2_765 ? P4 F4 1.467(13) 8_646 ? P4 F3 1.526(11) 8_646 ? P4 F3 1.526(11) 2_765 ? P4 F3 1.526(11) . ? P4 F3 1.526(11) 7_566 ? Cl1 C4 1.785(16) . ? C1 C2 1.375(16) . ? C1 C6 1.393(16) . ? C2 C3 1.414(16) . ? C3 C4 1.50(3) . ? C4 C5 1.32(3) . ? C5 C6 1.32(2) . ? C8 C13 1.366(13) . ? C8 C9 1.388(12) . ? C9 C10 1.375(13) . ? C10 C11 1.370(17) . ? C11 C12 1.356(16) . ? C12 C13 1.404(13) . ? C14 C19 1.365(12) . ? C14 C15 1.391(13) . ? C15 C16 1.370(16) . ? C16 C17 1.36(2) . ? C17 C18 1.39(2) . ? C18 C19 1.371(17) . ? C20 C25 1.355(13) . ? C20 C21 1.357(14) . ? C21 C22 1.381(17) . ? C22 C23 1.37(2) . ? C23 C24 1.34(2) . ? C24 C25 1.385(18) . ? C26 C31 1.346(16) . ? C26 C27 1.357(13) . ? C27 C28 1.388(16) . ? C28 C29 1.27(2) . ? C29 C30 1.39(2) . ? C30 C31 1.408(16) . ? F3 F4 1.55(3) 8_646 ? F4 F3 1.55(3) 7_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 P1 113.51(9) 2_665 . ? P1 Ag1 Se1 118.86(5) 2_665 . ? P1 Ag1 Se1 106.20(5) . . ? P1 Ag1 Se1 106.20(5) 2_665 2_665 ? P1 Ag1 Se1 118.86(5) . 2_665 ? Se1 Ag1 Se1 92.00(4) . 2_665 ? P1 Ag1 Ag2 161.92(5) 2_665 . ? P1 Ag1 Ag2 84.45(4) . . ? Se1 Ag1 Ag2 49.94(2) . . ? Se1 Ag1 Ag2 64.00(3) 2_665 . ? P1 Ag1 Ag2 84.45(4) 2_665 2_665 ? P1 Ag1 Ag2 161.92(5) . 2_665 ? Se1 Ag1 Ag2 64.00(3) . 2_665 ? Se1 Ag1 Ag2 49.94(2) 2_665 2_665 ? Ag2 Ag1 Ag2 77.70(3) . 2_665 ? P2 Ag2 Se1 128.02(6) . 3_567 ? P2 Ag2 Se1 119.58(6) . . ? Se1 Ag2 Se1 110.16(3) 3_567 . ? P2 Ag2 Ag1 87.50(5) . . ? Se1 Ag2 Ag1 136.89(3) 3_567 . ? Se1 Ag2 Ag1 53.99(2) . . ? C1 Se1 Ag2 107.1(3) . 4_657 ? C1 Se1 Ag2 99.9(4) . . ? Ag2 Se1 Ag2 84.40(3) 4_657 . ? C1 Se1 Ag1 117.1(3) . . ? Ag2 Se1 Ag1 133.89(4) 4_657 . ? Ag2 Se1 Ag1 76.07(3) . . ? C14 P1 C8 104.6(4) . . ? C14 P1 C7 104.2(4) . . ? C8 P1 C7 102.4(4) . . ? C14 P1 Ag1 118.7(3) . . ? C8 P1 Ag1 105.2(2) . . ? C7 P1 Ag1 119.6(3) . . ? C20 P2 C26 105.9(4) . . ? C20 P2 C7 105.6(4) . . ? C26 P2 C7 103.5(4) . . ? C20 P2 Ag2 115.8(3) . . ? C26 P2 Ag2 112.8(3) . . ? C7 P2 Ag2 112.3(2) . . ? F2 P3 F2 180.00(3) 7_466 . ? F2 P3 F1 96.6(8) 7_466 7_466 ? F2 P3 F1 83.4(8) . 7_466 ? F2 P3 F1 83.4(8) 7_466 . ? F2 P3 F1 96.6(8) . . ? F1 P3 F1 90.8(2) 7_466 . ? F2 P3 F1 83.4(8) 7_466 2_675 ? F2 P3 F1 96.6(8) . 2_675 ? F1 P3 F1 90.8(2) 7_466 2_675 ? F1 P3 F1 166.8(17) . 2_675 ? F2 P3 F1 96.6(8) 7_466 8_656 ? F2 P3 F1 83.4(8) . 8_656 ? F1 P3 F1 166.8(17) 7_466 8_656 ? F1 P3 F1 90.8(2) . 8_656 ? F1 P3 F1 90.8(2) 2_675 8_656 ? F4 P4 F4 115.1(15) 7_566 . ? F4 P4 F4 115.1(15) 7_566 2_765 ? F4 P4 F4 99(3) . 2_765 ? F4 P4 F4 99(3) 7_566 8_646 ? F4 P4 F4 115.1(15) . 8_646 ? F4 P4 F4 115.1(15) 2_765 8_646 ? F4 P4 F3 73.4(10) 7_566 8_646 ? F4 P4 F3 161(2) . 8_646 ? F4 P4 F3 62.5(11) 2_765 8_646 ? F4 P4 F3 78.7(10) 8_646 8_646 ? F4 P4 F3 62.5(11) 7_566 2_765 ? F4 P4 F3 73.4(10) . 2_765 ? F4 P4 F3 78.7(10) 2_765 2_765 ? F4 P4 F3 161(2) 8_646 2_765 ? F3 P4 F3 97.8(6) 8_646 2_765 ? F4 P4 F3 161(2) 7_566 . ? F4 P4 F3 78.7(10) . . ? F4 P4 F3 73.4(10) 2_765 . ? F4 P4 F3 62.5(11) 8_646 . ? F3 P4 F3 97.8(6) 8_646 . ? F3 P4 F3 136.6(19) 2_765 . ? F4 P4 F3 78.7(10) 7_566 7_566 ? F4 P4 F3 62.5(11) . 7_566 ? F4 P4 F3 161(2) 2_765 7_566 ? F4 P4 F3 73.4(10) 8_646 7_566 ? F3 P4 F3 136.6(19) 8_646 7_566 ? F3 P4 F3 97.8(6) 2_765 7_566 ? F3 P4 F3 97.8(6) . 7_566 ? C2 C1 C6 120.4(11) . . ? C2 C1 Se1 121.3(8) . . ? C6 C1 Se1 118.2(10) . . ? C1 C2 C3 119.4(14) . . ? C2 C3 C4 114.3(16) . . ? C5 C4 C3 124.1(15) . . ? C5 C4 Cl1 126(2) . . ? C3 C4 Cl1 109(2) . . ? C4 C5 C6 118(2) . . ? C5 C6 C1 124.1(18) . . ? P2 C7 P1 112.6(4) . . ? C13 C8 C9 119.2(8) . . ? C13 C8 P1 121.4(6) . . ? C9 C8 P1 118.9(6) . . ? C10 C9 C8 121.0(10) . . ? C11 C10 C9 119.4(10) . . ? C12 C11 C10 120.6(10) . . ? C11 C12 C13 120.3(11) . . ? C8 C13 C12 119.5(9) . . ? C19 C14 C15 119.8(9) . . ? C19 C14 P1 119.3(7) . . ? C15 C14 P1 120.9(7) . . ? C16 C15 C14 121.2(11) . . ? C17 C16 C15 117.5(12) . . ? C16 C17 C18 122.9(12) . . ? C19 C18 C17 118.3(12) . . ? C14 C19 C18 120.3(12) . . ? C25 C20 C21 118.6(9) . . ? C25 C20 P2 124.2(8) . . ? C21 C20 P2 117.1(7) . . ? C20 C21 C22 121.8(12) . . ? C23 C22 C21 119.2(14) . . ? C24 C23 C22 118.9(14) . . ? C23 C24 C25 121.6(13) . . ? C20 C25 C24 119.7(12) . . ? C31 C26 C27 120.4(9) . . ? C31 C26 P2 115.8(7) . . ? C27 C26 P2 123.8(7) . . ? C26 C27 C28 118.0(11) . . ? C29 C28 C27 123.2(13) . . ? C28 C29 C30 120.7(12) . . ? C29 C30 C31 117.4(14) . . ? C26 C31 C30 120.3(12) . . ? P4 F3 F4 56.9(8) . 8_646 ? P4 F4 F3 60.6(8) . 7_566 ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.57 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.343 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.329