# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1241 data_agsepm _audit_creation_method SHELXTL _chemical_formula_sum 'C36 H84 Ag7 O12 P6 Se12.50' _chemical_formula_weight 2636.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 22.7866(12) _cell_length_b 22.7866(12) _cell_length_c 12.8738(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5788.9(6) _cell_formula_units_Z 3 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description irregule _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.269 _exptl_crystal_density_method ? _exptl_crystal_F_000 3720 _exptl_absorpt_coefficient_mu 7.800 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4270 _exptl_absorpt_correction_T_max 0.6848 _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 5631 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2228 _reflns_number_gt 1979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+56.3109P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'NOT INCLUDE' _refine_ls_hydrogen_treatment 'NOT INCLUDE' _refine_ls_extinction_method SHELXTL _refine_ls_extinction_coef 0.00038(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2228 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_all 0.0992 _refine_ls_wR_factor_ref 0.0943 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.069 _refine_ls_restrained_S_obs 1.082 _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Se Se 0.3333 0.6667 0.1667 0.0608(9) Uani 0.497(3) d SP . Se1 Se 0.23677(3) 0.77396(3) 0.09266(5) 0.0551(2) Uani 1 d . . Se2 Se 0.41942(3) 0.78943(4) -0.08221(6) 0.0702(3) Uani 1 d . . Ag1 Ag 0.36128(3) 0.79592(3) 0.08831(4) 0.0685(2) Uani 1 d . . Ag2 Ag 0.3333 0.6667 -0.0441(2) 0.0662(7) Uani 0.497(3) d SP . P1 P 0.18299(8) 0.70320(8) -0.03265(13) 0.0504(4) Uani 1 d . . O1 O 0.1068(2) 0.6689(2) 0.0031(4) 0.0639(12) Uani 1 d . . O2 O 0.1836(3) 0.7457(2) -0.1296(4) 0.0686(12) Uani 1 d . . C1 C 0.0501(4) 0.6081(4) -0.0462(7) 0.079(2) Uani 1 d . . C2 C 0.0194(13) 0.6330(13) -0.1282(19) 0.115(7) Uiso 0.50 d P 1 C2' C 0.0390(10) 0.6182(10) -0.1584(15) 0.085(5) Uiso 0.50 d P 2 C3 C -0.0047(5) 0.5791(6) 0.0315(10) 0.123(4) Uani 1 d . . C4 C 0.2417(6) 0.7812(5) -0.2000(7) 0.101(3) Uani 1 d . . C5 C 0.2725(7) 0.8548(5) -0.1843(10) 0.142(5) Uani 1 d . . C6 C 0.1940(12) 0.7745(11) -0.3077(17) 0.108(6) Uiso 0.50 d P 3 C6' C 0.2297(13) 0.7554(13) -0.3029(19) 0.121(7) Uiso 0.50 d P 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 Se 0.0598(12) 0.0598(12) 0.063(2) 0.000 0.000 0.0299(6) Se1 0.0534(4) 0.0539(4) 0.0598(4) -0.0070(3) -0.0051(3) 0.0282(3) Se2 0.0512(4) 0.0959(6) 0.0559(4) 0.0066(3) -0.0023(3) 0.0310(4) Ag1 0.0597(3) 0.0717(4) 0.0734(4) 0.0078(3) 0.0034(2) 0.0324(3) Ag2 0.0628(8) 0.0628(8) 0.0730(13) 0.000 0.000 0.0314(4) P1 0.0501(8) 0.0469(8) 0.0561(9) -0.0012(7) -0.0068(7) 0.0256(7) O1 0.050(2) 0.054(2) 0.083(3) -0.007(2) -0.001(2) 0.022(2) O2 0.078(3) 0.064(3) 0.062(3) 0.006(2) -0.010(2) 0.034(2) C1 0.053(4) 0.056(4) 0.107(6) -0.010(4) -0.012(4) 0.012(3) C3 0.067(5) 0.113(8) 0.143(10) -0.011(7) 0.015(6) 0.011(5) C4 0.125(8) 0.090(6) 0.081(6) 0.017(5) 0.031(5) 0.048(6) C5 0.156(11) 0.068(6) 0.145(11) 0.006(6) 0.030(9) 0.013(6) 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 Se Ag2 2.714(2) 13_565 ? Se Ag2 2.714(2) . ? Se Ag1 2.8675(6) . ? Se Ag1 2.8676(6) 15 ? Se Ag1 2.8675(6) 2_665 ? Se Ag1 2.8675(6) 14_455 ? Se Ag1 2.8674(6) 13_565 ? Se Ag1 2.8675(6) 3_565 ? Se1 P1 2.174(2) . ? Se1 Ag1 2.6236(8) . ? Se1 Ag1 2.6330(9) 15 ? Se2 P1 2.153(2) 3_565 ? Se2 Ag2 2.5349(9) . ? Se2 Ag1 2.6062(9) . ? Ag1 Se1 2.6330(9) 14_455 ? Ag1 Ag2 3.1800(12) . ? Ag1 Ag1 3.3578(8) 14_455 ? Ag1 Ag1 3.3579(8) 15 ? Ag2 Se2 2.5350(9) 2_665 ? Ag2 Se2 2.5350(9) 3_565 ? Ag2 Ag1 3.1800(12) 2_665 ? Ag2 Ag1 3.1800(12) 3_565 ? P1 O1 1.575(5) . ? P1 O2 1.576(5) . ? P1 Se2 2.153(2) 2_665 ? O1 C1 1.484(8) . ? O2 C4 1.468(10) . ? C1 C3 1.474(13) . ? C1 C2' 1.50(2) . ? C1 C2 1.52(3) . ? C4 C6' 1.42(3) . ? C4 C5 1.471(14) . ? C4 C6 1.72(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag2 Se Ag2 180.0 13_565 . ? Ag2 Se Ag1 110.595(12) 13_565 . ? Ag2 Se Ag1 69.403(12) . . ? Ag2 Se Ag1 69.401(12) 13_565 15 ? Ag2 Se Ag1 110.597(12) . 15 ? Ag1 Se Ag1 71.677(12) . 15 ? Ag2 Se Ag1 110.596(12) 13_565 2_665 ? Ag2 Se Ag1 69.403(12) . 2_665 ? Ag1 Se Ag1 108.323(12) . 2_665 ? Ag1 Se Ag1 71.678(12) 15 2_665 ? Ag2 Se Ag1 69.403(12) 13_565 14_455 ? Ag2 Se Ag1 110.598(12) . 14_455 ? Ag1 Se Ag1 71.676(12) . 14_455 ? Ag1 Se Ag1 108.320(12) 15 14_455 ? Ag1 Se Ag1 180.0 2_665 14_455 ? Ag2 Se Ag1 69.404(12) 13_565 13_565 ? Ag2 Se Ag1 110.598(12) . 13_565 ? Ag1 Se Ag1 180.0 . 13_565 ? Ag1 Se Ag1 108.321(12) 15 13_565 ? Ag1 Se Ag1 71.677(12) 2_665 13_565 ? Ag1 Se Ag1 108.324(12) 14_455 13_565 ? Ag2 Se Ag1 110.599(12) 13_565 3_565 ? Ag2 Se Ag1 69.403(12) . 3_565 ? Ag1 Se Ag1 108.323(12) . 3_565 ? Ag1 Se Ag1 180.0 15 3_565 ? Ag1 Se Ag1 108.323(12) 2_665 3_565 ? Ag1 Se Ag1 71.679(12) 14_455 3_565 ? Ag1 Se Ag1 71.679(12) 13_565 3_565 ? P1 Se1 Ag1 106.28(5) . . ? P1 Se1 Ag1 103.24(5) . 15 ? Ag1 Se1 Ag1 79.40(3) . 15 ? P1 Se2 Ag2 112.88(6) 3_565 . ? P1 Se2 Ag1 103.43(5) 3_565 . ? Ag2 Se2 Ag1 76.41(4) . . ? Se2 Ag1 Se1 122.62(3) . . ? Se2 Ag1 Se1 117.37(3) . 14_455 ? Se1 Ag1 Se1 115.80(2) . 14_455 ? Se2 Ag1 Se 95.52(3) . . ? Se1 Ag1 Se 97.64(2) . . ? Se1 Ag1 Se 97.43(2) 14_455 . ? Se2 Ag1 Ag2 50.79(3) . . ? Se1 Ag1 Ag2 97.94(2) . . ? Se1 Ag1 Ag2 138.79(3) 14_455 . ? Se Ag1 Ag2 53.02(3) . . ? Se2 Ag1 Ag1 94.48(2) . 14_455 ? Se1 Ag1 Ag1 137.01(3) . 14_455 ? Se1 Ag1 Ag1 50.17(2) 14_455 14_455 ? Se Ag1 Ag1 54.162(6) . 14_455 ? Ag2 Ag1 Ag1 89.13(2) . 14_455 ? Se2 Ag1 Ag1 139.74(3) . 15 ? Se1 Ag1 Ag1 50.42(2) . 15 ? Se1 Ag1 Ag1 94.55(3) 14_455 15 ? Se Ag1 Ag1 54.163(6) . 15 ? Ag2 Ag1 Ag1 89.13(2) . 15 ? Ag1 Ag1 Ag1 87.62(2) 14_455 15 ? Se2 Ag2 Se2 116.36(3) 2_665 . ? Se2 Ag2 Se2 116.36(3) 2_665 3_565 ? Se2 Ag2 Se2 116.36(3) . 3_565 ? Se2 Ag2 Se 101.15(5) 2_665 . ? Se2 Ag2 Se 101.15(5) . . ? Se2 Ag2 Se 101.15(5) 3_565 . ? Se2 Ag2 Ag1 94.93(3) 2_665 . ? Se2 Ag2 Ag1 52.81(2) . . ? Se2 Ag2 Ag1 146.05(5) 3_565 . ? Se Ag2 Ag1 57.57(3) . . ? Se2 Ag2 Ag1 52.81(2) 2_665 2_665 ? Se2 Ag2 Ag1 146.05(5) . 2_665 ? Se2 Ag2 Ag1 94.93(3) 3_565 2_665 ? Se Ag2 Ag1 57.57(3) . 2_665 ? Ag1 Ag2 Ag1 93.94(4) . 2_665 ? Se2 Ag2 Ag1 146.05(5) 2_665 3_565 ? Se2 Ag2 Ag1 94.93(3) . 3_565 ? Se2 Ag2 Ag1 52.81(2) 3_565 3_565 ? Se Ag2 Ag1 57.57(3) . 3_565 ? Ag1 Ag2 Ag1 93.94(4) . 3_565 ? Ag1 Ag2 Ag1 93.94(4) 2_665 3_565 ? O1 P1 O2 101.8(3) . . ? O1 P1 Se2 112.2(2) . 2_665 ? O2 P1 Se2 109.0(2) . 2_665 ? O1 P1 Se1 102.9(2) . . ? O2 P1 Se1 107.7(2) . . ? Se2 P1 Se1 121.33(7) 2_665 . ? C1 O1 P1 124.6(4) . . ? C4 O2 P1 123.8(5) . . ? C3 C1 O1 106.0(7) . . ? C3 C1 C2' 123.5(10) . . ? O1 C1 C2' 113.7(9) . . ? C3 C1 C2 101.2(12) . . ? O1 C1 C2 107.2(11) . . ? C6' C4 O2 114.4(13) . . ? C6' C4 C5 118.9(13) . . ? O2 C4 C5 109.2(8) . . ? O2 C4 C6 95.3(10) . . ? C5 C4 C6 97.6(11) . . ? _refine_diff_density_max 0.838 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.098