data_jr1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'As9 S14 Sb' _chemical_formula_weight 1244.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'As' 'As' 0.0499 2.0058 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 25.297(4) _cell_length_b 14.542(3) _cell_length_c 6.4930(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2388.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 14.745 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 26005 _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 30.10 _reflns_number_total 3698 _reflns_number_gt 3152 _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 ? _computing_publication_material ? _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^)+(0.1451P)^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 -0.02(2) _refine_ls_number_reflns 3698 _refine_ls_number_parameters 219 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1958 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2014 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.008 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 As1 As -0.46945(5) -0.27957(8) -0.2507(3) 0.0399(3) Uani 1 1 d . . . As2 As -0.43981(5) -0.22033(9) -0.7436(3) 0.0435(3) Uani 1 1 d . . . As3 As -0.37515(5) -0.43591(8) -0.7518(3) 0.0419(4) Uani 0.853(16) 1 d P . . Sb3 Sb -0.37515(5) -0.43591(8) -0.7518(3) 0.0419(4) Uani 0.147(16) 1 d P . . As4 As -0.33100(5) -0.45027(9) -0.2469(3) 0.0432(3) Uani 1 1 d . . . As5 As -0.09489(5) -0.15589(8) -0.7517(2) 0.0386(3) Uani 1 1 d . . . As6 As -0.11002(5) -0.22985(9) -0.2462(3) 0.0448(3) Uani 1 1 d . . . As7 As -0.32942(9) -0.01362(16) -0.7595(6) 0.0762(6) Uani 1 1 d . . . As8 As -0.29523(11) -0.1155(2) -0.4102(5) 0.0845(7) Uani 1 1 d . . . As9 As -0.21254(6) -0.36238(10) -0.8371(3) 0.0442(3) Uani 1 1 d . . . As10 As -0.07632(7) -0.49819(11) -0.8418(3) 0.0509(3) Uani 1 1 d . . . S1 S -0.49376(12) -0.1742(2) -0.0002(5) 0.0351(6) Uani 1 1 d . . . S2 S -0.00345(12) -0.3233(2) -0.4997(5) 0.0368(6) Uani 1 1 d . . . S3 S -0.45899(11) -0.37483(19) -0.7335(6) 0.0376(5) Uani 1 1 d . . . S4 S -0.34048(14) -0.3325(2) 0.0026(6) 0.0391(6) Uani 1 1 d . . . S5 S -0.33533(12) -0.3467(2) -0.4994(6) 0.0350(6) Uani 1 1 d . . . S6 S -0.41680(10) -0.49758(18) -0.2479(5) 0.0347(5) Uani 1 1 d . . . S7 S -0.16253(11) -0.1569(2) 0.0015(5) 0.0312(5) Uani 1 1 d . . . S8 S -0.15936(13) -0.1701(2) -0.4976(6) 0.0386(6) Uani 1 1 d . . . S9 S -0.04251(10) -0.12255(19) -0.2349(5) 0.0347(5) Uani 1 1 d . . . S10 S -0.25314(13) 0.0005(2) -0.2593(7) 0.0456(6) Uani 1 1 d . . . S11 S -0.20730(15) -0.3798(3) -0.1821(7) 0.0508(8) Uani 1 1 d . . . S12 S -0.12592(11) -0.3776(2) -0.7270(6) 0.0384(6) Uani 1 1 d . . . S13 S -0.08905(18) -0.4987(3) -0.1849(7) 0.0563(9) Uani 1 1 d . . . S14 S -0.37297(12) -0.1210(2) -0.2397(7) 0.0439(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0371(5) 0.0408(6) 0.0418(6) -0.0010(7) 0.0006(6) 0.0006(4) As2 0.0432(6) 0.0436(6) 0.0439(7) 0.0014(7) 0.0000(7) 0.0002(5) As3 0.0411(6) 0.0419(6) 0.0428(6) 0.0004(6) 0.0002(7) -0.0005(4) Sb3 0.0411(6) 0.0419(6) 0.0428(6) 0.0004(6) 0.0002(7) -0.0005(4) As4 0.0433(6) 0.0424(6) 0.0439(7) -0.0014(7) 0.0000(7) -0.0004(4) As5 0.0385(5) 0.0378(5) 0.0396(6) -0.0016(6) -0.0007(6) -0.0003(4) As6 0.0416(6) 0.0458(6) 0.0469(7) 0.0007(7) 0.0007(7) -0.0005(5) As7 0.0750(12) 0.0759(12) 0.0778(14) 0.0014(14) 0.0013(13) 0.0011(9) As8 0.0842(16) 0.0841(15) 0.0853(18) 0.0018(14) 0.0006(13) -0.0003(12) As9 0.0437(6) 0.0435(6) 0.0455(7) 0.0003(6) -0.0002(6) -0.0002(5) As10 0.0508(7) 0.0512(7) 0.0508(7) -0.0003(8) 0.0002(6) 0.0003(7) S1 0.0352(13) 0.0335(14) 0.0366(15) 0.0017(11) -0.0006(12) 0.0004(10) S2 0.0360(13) 0.0358(14) 0.0385(15) -0.0019(11) 0.0007(13) -0.0003(10) S3 0.0363(11) 0.0345(11) 0.0420(15) 0.0016(14) -0.0019(14) 0.0013(9) S4 0.0382(13) 0.0373(14) 0.0417(15) -0.0020(13) 0.0012(13) -0.0003(11) S5 0.0357(12) 0.0347(14) 0.0347(13) 0.0015(12) -0.0002(12) 0.0001(11) S6 0.0333(10) 0.0357(10) 0.0350(12) 0.0002(16) -0.0002(12) 0.0003(9) S7 0.0304(11) 0.0314(12) 0.0319(12) 0.0009(11) 0.0011(11) 0.0009(10) S8 0.0376(13) 0.0385(14) 0.0397(15) 0.0025(12) 0.0011(13) -0.0009(11) S9 0.0342(11) 0.0364(11) 0.0334(12) 0.0021(13) -0.0004(13) 0.0002(9) S10 0.0420(13) 0.0484(14) 0.0464(15) -0.0006(18) -0.0012(15) -0.0019(12) S11 0.0482(17) 0.0529(19) 0.051(2) 0.0053(16) -0.0016(14) -0.0011(14) S12 0.0374(12) 0.0391(12) 0.0387(15) 0.0005(13) 0.0002(13) -0.0008(10) S13 0.0595(19) 0.0547(18) 0.055(2) 0.0000(17) 0.0007(17) -0.0004(17) S14 0.0414(13) 0.0451(14) 0.0451(16) 0.0036(17) 0.0000(16) -0.0015(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 As1 S1 2.318(4) . ? As1 S9 2.335(3) 4_445 ? As1 S2 2.364(4) 4_445 ? As2 S1 2.256(4) 1_554 ? As2 S3 2.300(3) . ? As2 S2 2.346(4) 4_445 ? As3 S3 2.303(3) . ? As3 S5 2.320(4) . ? As3 S4 2.361(4) 1_554 ? As4 S5 2.228(4) . ? As4 S6 2.277(3) . ? As4 S4 2.370(4) . ? As5 S6 2.321(3) 3_454 ? As5 S8 2.329(4) . ? As5 S7 2.344(3) 1_554 ? As6 S8 2.231(4) . ? As6 S9 2.314(3) . ? As6 S7 2.340(3) . ? As7 S13 2.130(5) 3_454 ? As7 S11 2.214(5) 3_454 ? As7 As8 2.843(5) . ? As8 S10 2.223(5) . ? As8 S14 2.259(4) . ? As9 S10 2.233(4) 3_444 ? As9 S11 2.258(5) 1_554 ? As9 S12 2.316(3) . ? As10 S13 2.251(5) 1_554 ? As10 S12 2.282(3) . ? As10 S14 2.296(4) 3_444 ? S1 As2 2.256(4) 1_556 ? S2 As2 2.346(4) 4_545 ? S2 As1 2.364(4) 4_545 ? S4 Sb3 2.361(4) 1_556 ? S4 As3 2.361(4) 1_556 ? S6 As5 2.321(3) 3_445 ? S7 As5 2.344(3) 1_556 ? S9 As1 2.335(3) 4_545 ? S10 As9 2.233(4) 3_455 ? S11 As7 2.214(5) 3_445 ? S11 As9 2.258(5) 1_556 ? S13 As7 2.130(5) 3_445 ? S13 As10 2.251(5) 1_556 ? S14 As10 2.296(4) 3_455 ? 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 S1 As1 S9 99.33(12) . 4_445 ? S1 As1 S2 88.01(11) . 4_445 ? S9 As1 S2 97.34(12) 4_445 4_445 ? S1 As2 S3 100.59(14) 1_554 . ? S1 As2 S2 90.17(13) 1_554 4_445 ? S3 As2 S2 95.73(13) . 4_445 ? S3 As3 S5 98.50(13) . . ? S3 As3 S4 97.55(13) . 1_554 ? S5 As3 S4 87.70(12) . 1_554 ? S5 As4 S6 98.93(13) . . ? S5 As4 S4 90.54(13) . . ? S6 As4 S4 97.11(12) . . ? S6 As5 S8 99.78(13) 3_454 . ? S6 As5 S7 96.12(11) 3_454 1_554 ? S8 As5 S7 88.43(11) . 1_554 ? S8 As6 S9 99.99(13) . . ? S8 As6 S7 90.50(12) . . ? S9 As6 S7 95.25(12) . . ? S13 As7 S11 105.37(19) 3_454 3_454 ? S13 As7 As8 99.59(18) 3_454 . ? S11 As7 As8 98.60(17) 3_454 . ? S10 As8 S14 103.15(19) . . ? S10 As8 As7 95.85(15) . . ? S14 As8 As7 98.31(15) . . ? S10 As9 S11 98.47(17) 3_444 1_554 ? S10 As9 S12 102.29(13) 3_444 . ? S11 As9 S12 103.89(15) 1_554 . ? S13 As10 S12 104.30(16) 1_554 . ? S13 As10 S14 101.74(18) 1_554 3_444 ? S12 As10 S14 101.31(13) . 3_444 ? As2 S1 As1 99.28(14) 1_556 . ? As2 S2 As1 92.35(13) 4_545 4_545 ? As2 S3 As3 100.43(11) . . ? Sb3 S4 As3 0.00(9) 1_556 1_556 ? Sb3 S4 As4 92.23(13) 1_556 . ? As3 S4 As4 92.23(13) 1_556 . ? As4 S5 As3 99.40(13) . . ? As4 S6 As5 100.27(11) . 3_445 ? As6 S7 As5 93.34(11) . 1_556 ? As6 S8 As5 99.28(14) . . ? As6 S9 As1 99.88(11) . 4_545 ? As8 S10 As9 113.06(19) . 3_455 ? As7 S11 As9 110.4(2) 3_445 1_556 ? As10 S12 As9 119.53(15) . . ? As7 S13 As10 111.3(2) 3_445 1_556 ? As8 S14 As10 108.51(18) . 3_455 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.307 _refine_diff_density_min -4.465 _refine_diff_density_rms 0.454