data_SnSb4S7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'S7 Sb4 Sn' _chemical_formula_weight 836.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 '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 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.331(4) _cell_length_b 3.8646(15) _cell_length_c 13.940(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.281(6) _cell_angle_gamma 90.00 _cell_volume 588.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 546(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 4.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 737 _exptl_absorpt_coefficient_mu 12.446 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 546(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 5081 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.12 _reflns_number_total 1416 _reflns_number_gt 1331 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0506P)^2^+25.1815P] 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 SHELXL _refine_ls_extinction_coef 0.0000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1416 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 2.438 _refine_ls_shift/su_mean 0.031 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 Sb1 Sb 0.66948(9) 0.2500 0.47533(8) 0.0173(4) Uani 0.998(11) 2 d SP . . Sb2 Sb 0.94774(10) 0.2500 0.88644(8) 0.0171(4) Uani 0.976(11) 2 d SP . . Sb3 Sb 0.66084(12) 0.2500 0.05000(10) 0.0315(5) Uani 0.995(11) 2 d SP . . Sn Sn 0.37909(13) 0.2500 0.21412(10) 0.0306(5) Uani 0.992(11) 2 d SP . . Sb4 Sb 0.07683(10) 0.2500 0.62599(8) 0.0220(4) Uani 1.000(11) 2 d S . . S1 S 0.7524(3) 0.2500 0.3251(3) 0.0153(8) Uani 1 2 d S . . S2 S 0.9573(4) 0.2500 0.1838(3) 0.0221(9) Uani 1 2 d S . . S3 S 0.1079(3) 0.2500 0.4583(3) 0.0145(8) Uani 1 2 d S . . S4 S 0.7646(4) 0.2500 0.7418(3) 0.0199(9) Uani 1 2 d S . . S5 S 0.4696(3) 0.2500 0.6040(3) 0.0151(8) Uani 1 2 d S . . S6 S 0.4934(4) 0.2500 0.8896(3) 0.0207(9) Uani 1 2 d S . . S7 S 0.2324(3) 0.2500 0.0371(3) 0.0161(8) Uani 1 2 d S . . 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 Sb1 0.0208(6) 0.0114(5) 0.0195(6) 0.000 0.0049(4) 0.000 Sb2 0.0221(6) 0.0110(6) 0.0204(6) 0.000 0.0095(4) 0.000 Sb3 0.0400(8) 0.0173(7) 0.0368(8) 0.000 0.0096(6) 0.000 Sn 0.0454(8) 0.0212(7) 0.0257(8) 0.000 0.0100(5) 0.000 Sb4 0.0298(7) 0.0190(6) 0.0199(6) 0.000 0.0116(4) 0.000 S1 0.0150(16) 0.0172(18) 0.0140(17) 0.000 0.0045(13) 0.000 S2 0.027(2) 0.020(2) 0.022(2) 0.000 0.0110(15) 0.000 S3 0.0175(17) 0.0136(17) 0.0151(17) 0.000 0.0090(13) 0.000 S4 0.0221(18) 0.0179(19) 0.020(2) 0.000 0.0056(14) 0.000 S5 0.0140(16) 0.0114(17) 0.0209(19) 0.000 0.0064(13) 0.000 S6 0.0219(18) 0.0189(19) 0.021(2) 0.000 0.0060(15) 0.000 S7 0.0152(16) 0.0151(18) 0.0182(18) 0.000 0.0049(13) 0.000 _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 Sb1 S1 2.511(4) . ? Sb1 S5 2.554(2) 3_656 ? Sb1 S5 2.554(2) 3_666 ? Sb2 S4 2.483(4) . ? Sb2 S2 2.531(3) 3_766 ? Sb2 S2 2.531(3) 3_756 ? Sb3 S6 2.522(4) 1_554 ? Sb3 S7 2.729(3) 3_665 ? Sb3 S7 2.729(3) 3_655 ? Sb3 S6 2.877(3) 3_656 ? Sb3 S6 2.877(3) 3_666 ? Sn S7 2.586(4) . ? Sn S4 2.700(3) 3_656 ? Sn S4 2.700(3) 3_666 ? Sb4 S3 2.453(4) . ? Sb4 S1 2.692(3) 3_666 ? Sb4 S1 2.692(3) 3_656 ? Sb4 S3 2.864(3) 3_556 ? Sb4 S3 2.864(3) 3_566 ? S1 Sb4 2.692(3) 3_666 ? S1 Sb4 2.692(3) 3_656 ? S2 Sb2 2.531(3) 3_766 ? S2 Sb2 2.531(3) 3_756 ? S3 Sb4 2.864(3) 3_556 ? S3 Sb4 2.864(3) 3_566 ? S4 Sn 2.700(3) 3_656 ? S4 Sn 2.700(3) 3_666 ? S5 Sb1 2.554(2) 3_656 ? S5 Sb1 2.554(2) 3_666 ? S6 Sb3 2.522(4) 1_556 ? S6 Sb3 2.877(3) 3_656 ? S6 Sb3 2.877(3) 3_666 ? S7 Sb3 2.729(3) 3_665 ? S7 Sb3 2.729(3) 3_655 ? 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 Sb1 S5 87.87(10) . 3_656 ? S1 Sb1 S5 87.87(10) . 3_666 ? S5 Sb1 S5 98.35(13) 3_656 3_666 ? S4 Sb2 S2 92.01(12) . 3_766 ? S4 Sb2 S2 92.01(12) . 3_756 ? S2 Sb2 S2 99.54(15) 3_766 3_756 ? S6 Sb3 S7 85.62(11) 1_554 3_665 ? S6 Sb3 S7 85.62(11) 1_554 3_655 ? S7 Sb3 S7 90.15(12) 3_665 3_655 ? S6 Sb3 S6 83.47(12) 1_554 3_656 ? S7 Sb3 S6 168.77(12) 3_665 3_656 ? S7 Sb3 S6 91.70(9) 3_655 3_656 ? S6 Sb3 S6 83.47(12) 1_554 3_666 ? S7 Sb3 S6 91.70(9) 3_665 3_666 ? S7 Sb3 S6 168.77(12) 3_655 3_666 ? S6 Sb3 S6 84.40(12) 3_656 3_666 ? S7 Sn S4 86.71(11) . 3_656 ? S7 Sn S4 86.71(11) . 3_666 ? S4 Sn S4 91.39(13) 3_656 3_666 ? S3 Sb4 S1 88.12(10) . 3_666 ? S3 Sb4 S1 88.12(10) . 3_656 ? S1 Sb4 S1 91.73(12) 3_666 3_656 ? S3 Sb4 S3 83.23(10) . 3_556 ? S1 Sb4 S3 170.81(11) 3_666 3_556 ? S1 Sb4 S3 91.07(8) 3_656 3_556 ? S3 Sb4 S3 83.23(10) . 3_566 ? S1 Sb4 S3 91.07(8) 3_666 3_566 ? S1 Sb4 S3 170.81(11) 3_656 3_566 ? S3 Sb4 S3 84.86(11) 3_556 3_566 ? Sb1 S1 Sb4 100.99(10) . 3_666 ? Sb1 S1 Sb4 100.99(10) . 3_656 ? Sb4 S1 Sb4 91.73(12) 3_666 3_656 ? Sb2 S2 Sb2 99.54(15) 3_766 3_756 ? Sb4 S3 Sb4 96.77(10) . 3_556 ? Sb4 S3 Sb4 96.77(10) . 3_566 ? Sb4 S3 Sb4 84.86(11) 3_556 3_566 ? Sb2 S4 Sn 103.89(12) . 3_656 ? Sb2 S4 Sn 103.89(12) . 3_666 ? Sn S4 Sn 91.39(13) 3_656 3_666 ? Sb1 S5 Sb1 98.35(13) 3_656 3_666 ? Sb3 S6 Sb3 96.53(12) 1_556 3_656 ? Sb3 S6 Sb3 96.53(12) 1_556 3_666 ? Sb3 S6 Sb3 84.40(12) 3_656 3_666 ? Sn S7 Sb3 100.11(11) . 3_665 ? Sn S7 Sb3 100.11(11) . 3_655 ? Sb3 S7 Sb3 90.15(12) 3_665 3_655 ? _diffrn_measured_fraction_theta_max 0.860 _diffrn_reflns_theta_full 28.12 _diffrn_measured_fraction_theta_full 0.860 _refine_diff_density_max 3.391 _refine_diff_density_min -2.225 _refine_diff_density_rms 0.372