data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Yao, Jiyong' _publ_contact_author_name 'Yao, Jiyong' _publ_contact_author_email jyao@mail.ipc.ac.cn _publ_section_title ; Ba2AgInS4 and Ba4MGa5Se12 (M = Ag, Li): syntheses, structures, and optical properties ; # Attachment '- BaAgInS paper cifs.cif' data_Ba2AgInS4 _database_code_depnum_ccdc_archive 'CCDC 847971' #TrackingRef '- BaAgInS paper cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag Ba2 In S4' _chemical_formula_weight 625.61 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3434(17) _cell_length_b 7.2579(15) _cell_length_c 14.544(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.80(3) _cell_angle_gamma 90.00 _cell_volume 843.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3051 _cell_measurement_theta_min 2.8065 _cell_measurement_theta_max 29.0856 _exptl_crystal_description Chip _exptl_crystal_colour Red _exptl_crystal_size_max 0.1490 _exptl_crystal_size_mid 0.0890 _exptl_crystal_size_min 0.0530 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 15.095 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.137 _exptl_absorpt_correction_T_max 0.294 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku AFC10 diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7051 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 29.09 _reflns_number_total 2192 _reflns_number_gt 1825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2192 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _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 Ba1 Ba 0.05506(5) 0.34369(5) 0.35764(3) 0.00666(11) Uani 1 1 d . . . Ba2 Ba 0.55529(5) 0.34201(5) 0.36414(3) 0.00619(11) Uani 1 1 d . . . In In 0.18682(6) 0.31889(7) 0.12252(3) 0.00588(12) Uani 1 1 d . . . Ag Ag 0.67786(8) 0.36708(12) 0.10066(5) 0.0395(2) Uani 1 1 d . . . S1 S 0.10119(19) 0.7434(2) 0.46962(11) 0.0082(3) Uani 1 1 d . . . S2 S 0.2447(2) 0.5756(2) 0.23330(11) 0.0069(3) Uani 1 1 d . . . S3 S 0.2560(2) 0.0771(2) 0.25310(10) 0.0064(3) Uani 1 1 d . . . S4 S 0.38154(19) 0.2495(2) 0.02863(11) 0.0083(3) 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 Ba1 0.0059(2) 0.0067(2) 0.00726(18) -0.00002(14) 0.00182(14) 0.00023(15) Ba2 0.0050(2) 0.0067(2) 0.00665(18) -0.00035(13) 0.00144(14) -0.00041(14) In 0.0056(2) 0.0059(2) 0.0059(2) -0.00107(16) 0.00123(16) -0.00048(18) Ag 0.0124(3) 0.0688(6) 0.0385(4) -0.0442(4) 0.0093(3) -0.0102(3) S1 0.0045(7) 0.0110(8) 0.0086(7) 0.0016(6) 0.0012(6) 0.0002(6) S2 0.0083(8) 0.0042(8) 0.0078(7) 0.0000(5) 0.0018(6) 0.0005(6) S3 0.0085(8) 0.0043(8) 0.0058(6) -0.0002(6) 0.0009(6) 0.0001(6) S4 0.0067(7) 0.0112(8) 0.0071(7) -0.0007(6) 0.0022(6) 0.0006(7) _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 Ba1 S3 3.1280(18) 2 ? Ba1 S2 3.1425(18) 2_545 ? Ba1 S4 3.185(2) 4_566 ? Ba1 S2 3.2031(18) . ? Ba1 S1 3.2100(19) 3_566 ? Ba1 S3 3.2157(17) . ? Ba1 S1 3.2947(19) . ? Ba1 In 3.8722(15) 4_566 ? Ba1 In 3.8869(14) . ? Ba1 In 4.0483(9) 2 ? Ba1 Ag 4.0642(11) 2_645 ? Ba1 Ba2 4.1473(10) . ? Ba2 S3 3.1383(17) 2_655 ? Ba2 S2 3.1464(17) 2_645 ? Ba2 S3 3.1951(18) . ? Ba2 S4 3.2048(19) 4_566 ? Ba2 S2 3.2191(19) . ? Ba2 S1 3.231(2) 3_666 ? Ba2 S4 3.3140(19) 2_655 ? Ba2 Ag 3.6261(13) 4_566 ? Ba2 In 3.9476(17) . ? Ba2 In 4.0504(9) 2_655 ? Ba2 Ag 4.0625(11) 2_645 ? In S2 2.4191(17) . ? In S1 2.4513(18) 2_545 ? In S4 2.4576(18) . ? In S3 2.5270(17) . ? In Ba1 3.8722(14) 4_565 ? In Ba1 4.0483(9) 2_545 ? In Ba2 4.0504(9) 2_645 ? Ag S1 2.5176(18) 2_645 ? Ag S4 2.5378(19) . ? Ag S3 2.5443(17) 2_655 ? Ag Ba2 3.6261(13) 4_565 ? Ag Ba2 4.0625(11) 2_655 ? Ag Ba1 4.0642(11) 2_655 ? S1 In 2.4513(18) 2 ? S1 Ag 2.5176(18) 2_655 ? S1 Ba1 3.2100(19) 3_566 ? S1 Ba2 3.231(2) 3_666 ? S2 Ba1 3.1425(18) 2 ? S2 Ba2 3.1464(17) 2_655 ? S3 Ag 2.5443(17) 2_645 ? S3 Ba1 3.1280(18) 2_545 ? S3 Ba2 3.1383(17) 2_645 ? S4 Ba1 3.185(2) 4_565 ? S4 Ba2 3.2048(19) 4_565 ? S4 Ba2 3.3140(19) 2_645 ? 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 S3 Ba1 S2 71.19(4) 2 2_545 ? S3 Ba1 S4 155.80(4) 2 4_566 ? S2 Ba1 S4 126.44(5) 2_545 4_566 ? S3 Ba1 S2 84.05(4) 2 . ? S2 Ba1 S2 123.40(3) 2_545 . ? S4 Ba1 S2 95.85(5) 4_566 . ? S3 Ba1 S1 92.60(5) 2 3_566 ? S2 Ba1 S1 75.74(5) 2_545 3_566 ? S4 Ba1 S1 78.24(5) 4_566 3_566 ? S2 Ba1 S1 157.50(4) . 3_566 ? S3 Ba1 S3 123.43(3) 2 . ? S2 Ba1 S3 83.61(4) 2_545 . ? S4 Ba1 S3 78.24(5) 4_566 . ? S2 Ba1 S3 68.85(4) . . ? S1 Ba1 S3 129.55(5) 3_566 . ? S3 Ba1 S1 74.85(5) 2 . ? S2 Ba1 S1 135.91(4) 2_545 . ? S4 Ba1 S1 81.36(5) 4_566 . ? S2 Ba1 S1 79.05(4) . . ? S1 Ba1 S1 78.60(5) 3_566 . ? S3 Ba1 S1 139.57(4) . . ? S3 Ba1 In 129.20(4) 2 4_566 ? S2 Ba1 In 101.11(4) 2_545 4_566 ? S4 Ba1 In 39.26(3) 4_566 4_566 ? S2 Ba1 In 132.63(4) . 4_566 ? S1 Ba1 In 39.11(3) 3_566 4_566 ? S3 Ba1 In 104.49(4) . 4_566 ? S1 Ba1 In 79.49(3) . 4_566 ? S3 Ba1 In 88.61(4) 2 . ? S2 Ba1 In 89.66(4) 2_545 . ? S4 Ba1 In 106.35(4) 4_566 . ? S2 Ba1 In 38.39(3) . . ? S1 Ba1 In 164.06(3) 3_566 . ? S3 Ba1 In 40.31(3) . . ? S1 Ba1 In 116.96(3) . . ? In Ba1 In 142.19(2) 4_566 . ? S3 Ba1 In 38.62(3) 2 2 ? S2 Ba1 In 101.83(4) 2_545 2 ? S4 Ba1 In 117.18(3) 4_566 2 ? S2 Ba1 In 86.00(3) . 2 ? S1 Ba1 In 77.78(4) 3_566 2 ? S3 Ba1 In 152.27(3) . 2 ? S1 Ba1 In 37.25(3) . 2 ? In Ba1 In 101.11(2) 4_566 2 ? In Ba1 In 112.071(18) . 2 ? S3 Ba1 Ag 151.09(3) 2 2_645 ? S2 Ba1 Ag 82.60(4) 2_545 2_645 ? S4 Ba1 Ag 52.73(4) 4_566 2_645 ? S2 Ba1 Ag 101.11(3) . 2_645 ? S1 Ba1 Ag 92.57(4) 3_566 2_645 ? S3 Ba1 Ag 38.75(3) . 2_645 ? S1 Ba1 Ag 134.03(4) . 2_645 ? In Ba1 Ag 66.82(2) 4_566 2_645 ? In Ba1 Ag 79.02(2) . 2_645 ? In Ba1 Ag 167.856(18) 2 2_645 ? S3 Ba1 Ba2 133.88(3) 2 . ? S2 Ba1 Ba2 132.92(3) 2_545 . ? S4 Ba1 Ba2 49.74(4) 4_566 . ? S2 Ba1 Ba2 49.95(3) . . ? S1 Ba1 Ba2 127.97(4) 3_566 . ? S3 Ba1 Ba2 49.47(3) . . ? S1 Ba1 Ba2 91.05(3) . . ? In Ba1 Ba2 88.97(3) 4_566 . ? In Ba1 Ba2 58.75(3) . . ? In Ba1 Ba2 121.333(14) 2 . ? Ag Ba1 Ba2 59.294(15) 2_645 . ? S3 Ba2 S2 71.01(4) 2_655 2_645 ? S3 Ba2 S3 119.60(3) 2_655 . ? S2 Ba2 S3 80.87(4) 2_645 . ? S3 Ba2 S4 157.59(4) 2_655 4_566 ? S2 Ba2 S4 128.48(5) 2_645 4_566 ? S3 Ba2 S4 78.26(5) . 4_566 ? S3 Ba2 S2 80.62(4) 2_655 . ? S2 Ba2 S2 119.91(3) 2_645 . ? S3 Ba2 S2 68.91(4) . . ? S4 Ba2 S2 95.15(5) 4_566 . ? S3 Ba2 S1 92.01(4) 2_655 3_666 ? S2 Ba2 S1 75.39(5) 2_645 3_666 ? S3 Ba2 S1 131.10(5) . 3_666 ? S4 Ba2 S1 84.06(5) 4_566 3_666 ? S2 Ba2 S1 158.74(5) . 3_666 ? S3 Ba2 S4 74.57(4) 2_655 2_655 ? S2 Ba2 S4 136.67(4) 2_645 2_655 ? S3 Ba2 S4 140.33(4) . 2_655 ? S4 Ba2 S4 83.02(5) 4_566 2_655 ? S2 Ba2 S4 78.43(5) . 2_655 ? S1 Ba2 S4 80.39(5) 3_666 2_655 ? S3 Ba2 Ag 134.01(4) 2_655 4_566 ? S2 Ba2 Ag 97.43(4) 2_645 4_566 ? S3 Ba2 Ag 101.10(4) . 4_566 ? S4 Ba2 Ag 43.07(3) 4_566 4_566 ? S2 Ba2 Ag 137.68(4) . 4_566 ? S1 Ba2 Ag 42.59(3) 3_666 4_566 ? S4 Ba2 Ag 87.95(4) 2_655 4_566 ? S3 Ba2 In 85.60(4) 2_655 . ? S2 Ba2 In 87.19(4) 2_645 . ? S3 Ba2 In 39.71(3) . . ? S4 Ba2 In 104.58(4) 4_566 . ? S2 Ba2 In 37.76(3) . . ? S1 Ba2 In 162.20(3) 3_666 . ? S4 Ba2 In 115.71(3) 2_655 . ? Ag Ba2 In 139.49(2) 4_566 . ? S3 Ba2 In 38.60(3) 2_655 2_655 ? S2 Ba2 In 101.71(4) 2_645 2_655 ? S3 Ba2 In 149.90(3) . 2_655 ? S4 Ba2 In 119.34(3) 4_566 2_655 ? S2 Ba2 In 84.49(4) . 2_655 ? S1 Ba2 In 77.53(4) 3_666 2_655 ? S4 Ba2 In 37.33(3) 2_655 2_655 ? Ag Ba2 In 108.18(3) 4_566 2_655 ? In Ba2 In 110.195(18) . 2_655 ? S3 Ba2 Ag 149.71(3) 2_655 2_645 ? S2 Ba2 Ag 82.59(4) 2_645 2_645 ? S3 Ba2 Ag 38.77(3) . 2_645 ? S4 Ba2 Ag 52.67(4) 4_566 2_645 ? S2 Ba2 Ag 100.86(4) . 2_645 ? S1 Ba2 Ag 95.53(4) 3_666 2_645 ? S4 Ba2 Ag 135.62(3) 2_655 2_645 ? Ag Ba2 Ag 62.57(3) 4_566 2_645 ? In Ba2 Ag 78.348(18) . 2_645 ? In Ba2 Ag 170.443(18) 2_655 2_645 ? S3 Ba2 Ba1 130.21(3) 2_655 . ? S2 Ba2 Ba1 130.76(3) 2_645 . ? S3 Ba2 Ba1 49.91(3) . . ? S4 Ba2 Ba1 49.33(4) 4_566 . ? S2 Ba2 Ba1 49.61(3) . . ? S1 Ba2 Ba1 133.38(3) 3_666 . ? S4 Ba2 Ba1 91.73(3) 2_655 . ? Ag Ba2 Ba1 91.65(3) 4_566 . ? In Ba2 Ba1 57.33(3) . . ? In Ba2 Ba1 121.048(14) 2_655 . ? Ag Ba2 Ba1 59.335(14) 2_645 . ? S2 In S1 120.77(6) . 2_545 ? S2 In S4 119.42(6) . . ? S1 In S4 110.58(6) 2_545 . ? S2 In S3 94.37(6) . . ? S1 In S3 103.33(6) 2_545 . ? S4 In S3 103.37(6) . . ? S2 In Ba1 147.35(4) . 4_565 ? S1 In Ba1 55.70(4) 2_545 4_565 ? S4 In Ba1 55.11(4) . 4_565 ? S3 In Ba1 118.27(4) . 4_565 ? S2 In Ba1 55.32(4) . . ? S1 In Ba1 90.54(5) 2_545 . ? S4 In Ba1 154.00(4) . . ? S3 In Ba1 55.41(4) . . ? Ba1 In Ba1 144.91(2) 4_565 . ? S2 In Ba2 54.57(4) . . ? S1 In Ba2 152.17(4) 2_545 . ? S4 In Ba2 91.92(5) . . ? S3 In Ba2 53.88(4) . . ? Ba1 In Ba2 145.36(2) 4_565 . ? Ba1 In Ba2 63.92(2) . . ? S2 In Ba1 128.05(4) . 2_545 ? S1 In Ba1 54.44(4) 2_545 2_545 ? S4 In Ba1 106.76(5) . 2_545 ? S3 In Ba1 50.59(4) . 2_545 ? Ba1 In Ba1 78.89(2) 4_565 2_545 ? Ba1 In Ba1 72.731(16) . 2_545 ? Ba2 In Ba1 104.405(18) . 2_545 ? S2 In Ba2 128.71(5) . 2_645 ? S1 In Ba2 104.98(5) 2_545 2_645 ? S4 In Ba2 54.85(4) . 2_645 ? S3 In Ba2 50.78(4) . 2_645 ? Ba1 In Ba2 77.37(2) 4_565 2_645 ? Ba1 In Ba2 106.190(19) . 2_645 ? Ba2 In Ba2 74.183(16) . 2_645 ? Ba1 In Ba2 62.447(18) 2_545 2_645 ? S1 Ag S4 116.92(6) 2_645 . ? S1 Ag S3 123.08(6) 2_645 2_655 ? S4 Ag S3 119.77(6) . 2_655 ? S1 Ag Ba2 60.29(4) 2_645 4_565 ? S4 Ag Ba2 59.58(4) . 4_565 ? S3 Ag Ba2 167.78(5) 2_655 4_565 ? S1 Ag Ba2 141.92(5) 2_645 2_655 ? S4 Ag Ba2 83.83(5) . 2_655 ? S3 Ag Ba2 51.85(4) 2_655 2_655 ? Ba2 Ag Ba2 117.43(3) 4_565 2_655 ? S1 Ag Ba1 85.97(5) 2_645 2_655 ? S4 Ag Ba1 140.75(5) . 2_655 ? S3 Ag Ba1 52.29(4) 2_655 2_655 ? Ba2 Ag Ba1 119.33(3) 4_565 2_655 ? Ba2 Ag Ba1 61.37(2) 2_655 2_655 ? In S1 Ag 114.55(7) 2 2_655 ? In S1 Ba1 85.19(5) 2 3_566 ? Ag S1 Ba1 153.99(7) 2_655 3_566 ? In S1 Ba2 165.79(7) 2 3_666 ? Ag S1 Ba2 77.11(5) 2_655 3_666 ? Ba1 S1 Ba2 81.35(4) 3_566 3_666 ? In S1 Ba1 88.31(5) 2 . ? Ag S1 Ba1 96.19(6) 2_655 . ? Ba1 S1 Ba1 101.40(5) 3_566 . ? Ba2 S1 Ba1 98.77(5) 3_666 . ? In S2 Ba1 102.43(6) . 2 ? In S2 Ba2 101.71(5) . 2_655 ? Ba1 S2 Ba2 83.76(4) 2 2_655 ? In S2 Ba1 86.28(5) . . ? Ba1 S2 Ba1 95.75(5) 2 . ? Ba2 S2 Ba1 171.92(6) 2_655 . ? In S2 Ba2 87.68(5) . . ? Ba1 S2 Ba2 169.01(6) 2 . ? Ba2 S2 Ba2 98.55(5) 2_655 . ? Ba1 S2 Ba2 80.45(4) . . ? In S3 Ag 172.54(7) . 2_645 ? In S3 Ba1 90.79(5) . 2_545 ? Ag S3 Ba1 93.04(6) 2_645 2_545 ? In S3 Ba2 90.62(5) . 2_645 ? Ag S3 Ba2 96.13(6) 2_645 2_645 ? Ba1 S3 Ba2 84.13(4) 2_545 2_645 ? In S3 Ba2 86.41(5) . . ? Ag S3 Ba2 89.37(5) 2_645 . ? Ba1 S3 Ba2 175.64(6) 2_545 . ? Ba2 S3 Ba2 99.23(5) 2_645 . ? In S3 Ba1 84.28(5) . . ? Ag S3 Ba1 88.96(5) 2_645 . ? Ba1 S3 Ba1 95.79(5) 2_545 . ? Ba2 S3 Ba1 174.90(6) 2_645 . ? Ba2 S3 Ba1 80.62(4) . . ? In S4 Ag 115.04(7) . . ? In S4 Ba1 85.63(5) . 4_565 ? Ag S4 Ba1 154.81(7) . 4_565 ? In S4 Ba2 166.29(7) . 4_565 ? Ag S4 Ba2 77.35(5) . 4_565 ? Ba1 S4 Ba2 80.93(4) 4_565 4_565 ? In S4 Ba2 87.83(5) . 2_645 ? Ag S4 Ba2 95.87(6) . 2_645 ? Ba1 S4 Ba2 99.30(5) 4_565 2_645 ? Ba2 S4 Ba2 96.98(5) 4_565 2_645 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 2.328 _refine_diff_density_min -5.882 _refine_diff_density_rms 0.427 #===END data_Ba4AgGa5Se12 _database_code_depnum_ccdc_archive 'CCDC 847972' #TrackingRef '- BaAgInS paper cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ag Ba4 Ga5 Se12' _chemical_formula_weight 1953.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ga Ga 0.2307 1.6083 '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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-421c 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 13.6544(19) _cell_length_b 13.6544(19) _cell_length_c 6.5215(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1215.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5787 _cell_measurement_theta_min 2.1083 _cell_measurement_theta_max 29.1095 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1090 _exptl_crystal_size_mid 0.0730 _exptl_crystal_size_min 0.0670 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 30.542 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.108 _exptl_absorpt_correction_T_max 0.321 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku AFC10 diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10337 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 29.09 _reflns_number_total 1629 _reflns_number_gt 1568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00075(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_number_reflns 1629 _refine_ls_number_parameters 54 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0522 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.000 _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 Ba Ba 0.28823(4) 0.02597(3) 0.45840(8) 0.02210(13) Uani 1 1 d . . . Ag Ag 0.0000 0.5000 0.2912(3) 0.0208(3) Uani 0.50 2 d SP . . Ga1 Ga 0.13795(5) 0.24285(5) 0.05220(12) 0.00621(15) Uani 1 1 d . . . Ga2 Ga 0.0000 0.0000 0.0000 0.0054(3) Uani 1 4 d S . . Se1 Se 0.00343(5) 0.35351(5) 0.03900(11) 0.01820(17) Uani 1 1 d . . . Se2 Se 0.28615(5) 0.30679(5) 0.20766(10) 0.00845(14) Uani 1 1 d . . . Se3 Se 0.08294(5) 0.10353(5) 0.24152(10) 0.00995(15) 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 Ba 0.0399(3) 0.0136(2) 0.0128(2) -0.00255(18) -0.0007(2) -0.0084(2) Ag 0.0125(8) 0.0115(7) 0.0384(10) 0.000 0.000 -0.0019(5) Ga1 0.0078(3) 0.0063(3) 0.0046(3) -0.0003(3) 0.0003(3) 0.0000(3) Ga2 0.0068(4) 0.0068(4) 0.0028(7) 0.000 0.000 0.000 Se1 0.0233(4) 0.0239(4) 0.0073(3) 0.0002(3) 0.0005(4) 0.0175(3) Se2 0.0072(3) 0.0136(3) 0.0046(3) -0.0017(2) 0.0000(2) -0.0008(3) Se3 0.0160(3) 0.0094(3) 0.0045(3) 0.0002(2) -0.0007(3) -0.0061(3) _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 Ba Se2 3.3026(9) 7 ? Ba Se3 3.3135(9) . ? Ba Ag 3.3370(12) 5_545 ? Ba Ag 3.3398(12) 3_556 ? Ba Se2 3.3408(9) 5_545 ? Ba Se1 3.3679(9) 6 ? Ba Se1 3.3879(11) 3 ? Ba Se1 3.4203(11) 3_556 ? Ba Se3 3.5216(9) 3_556 ? Ba Se1 3.6930(11) 5_545 ? Ag Se1 2.5721(15) 7 ? Ag Se1 2.5721(15) 8_455 ? Ag Se1 2.5899(15) . ? Ag Se1 2.5899(15) 2_565 ? Ag Ag 3.2607(6) 7 ? Ag Ag 3.2608(6) 7_554 ? Ag Ba 3.3371(12) 6_455 ? Ag Ba 3.3370(12) 5 ? Ag Ba 3.3398(12) 3_566 ? Ag Ba 3.3398(12) 4_556 ? Ga1 Se1 2.3799(10) . ? Ga1 Se3 2.3890(10) . ? Ga1 Se2 2.4032(11) 7_554 ? Ga1 Se2 2.4259(10) . ? Ga2 Se3 2.4003(7) . ? Ga2 Se3 2.4003(7) 4 ? Ga2 Se3 2.4003(7) 3 ? Ga2 Se3 2.4003(7) 2 ? Se1 Ag 2.5721(15) 7_554 ? Se1 Ba 3.3679(9) 6_455 ? Se1 Ba 3.3879(11) 4 ? Se1 Ba 3.4203(11) 4_556 ? Se1 Ba 3.6930(11) 5 ? Se2 Ga1 2.4032(11) 7 ? Se2 Ba 3.3026(9) 7_554 ? Se2 Ba 3.3408(9) 5 ? Se3 Ba 3.5216(9) 4_556 ? 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 Se2 Ba Se3 68.25(2) 7 . ? Se2 Ba Ag 131.53(2) 7 5_545 ? Se3 Ba Ag 123.97(4) . 5_545 ? Se2 Ba Ag 100.48(3) 7 3_556 ? Se3 Ba Ag 167.18(2) . 3_556 ? Ag Ba Ag 58.466(15) 5_545 3_556 ? Se2 Ba Se2 137.39(3) 7 5_545 ? Se3 Ba Se2 83.73(2) . 5_545 ? Ag Ba Se2 90.58(2) 5_545 5_545 ? Ag Ba Se2 109.065(18) 3_556 5_545 ? Se2 Ba Se1 87.75(2) 7 6 ? Se3 Ba Se1 125.73(2) . 6 ? Ag Ba Se1 45.44(2) 5_545 6 ? Ag Ba Se1 45.09(2) 3_556 6 ? Se2 Ba Se1 134.80(2) 5_545 6 ? Se2 Ba Se1 131.81(2) 7 3 ? Se3 Ba Se1 81.47(2) . 3 ? Ag Ba Se1 44.97(3) 5_545 3 ? Ag Ba Se1 103.17(4) 3_556 3 ? Se2 Ba Se1 70.335(19) 5_545 3 ? Se1 Ba Se1 80.40(2) 6 3 ? Se2 Ba Se1 73.85(2) 7 3_556 ? Se3 Ba Se1 131.84(2) . 3_556 ? Ag Ba Se1 103.24(4) 5_545 3_556 ? Ag Ba Se1 45.03(3) 3_556 3_556 ? Se2 Ba Se1 106.54(2) 5_545 3_556 ? Se1 Ba Se1 79.93(2) 6 3_556 ? Se1 Ba Se1 146.62(3) 3 3_556 ? Se2 Ba Se3 76.89(2) 7 3_556 ? Se3 Ba Se3 76.49(3) . 3_556 ? Ag Ba Se3 147.86(2) 5_545 3_556 ? Ag Ba Se3 107.67(3) 3_556 3_556 ? Se2 Ba Se3 65.427(19) 5_545 3_556 ? Se1 Ba Se3 145.93(2) 6 3_556 ? Se1 Ba Se3 132.10(2) 3 3_556 ? Se1 Ba Se3 66.71(2) 3_556 3_556 ? Se2 Ba Se1 142.72(2) 7 5_545 ? Se3 Ba Se1 149.03(2) . 5_545 ? Ag Ba Se1 42.86(2) 5_545 5_545 ? Ag Ba Se1 42.53(2) 3_556 5_545 ? Se2 Ba Se1 70.394(17) 5_545 5_545 ? Se1 Ba Se1 68.87(2) 6 5_545 ? Se1 Ba Se1 74.109(19) 3 5_545 ? Se1 Ba Se1 73.743(19) 3_556 5_545 ? Se3 Ba Se1 106.252(19) 3_556 5_545 ? Se1 Ag Se1 102.14(8) 7 8_455 ? Se1 Ag Se1 111.77(3) 7 . ? Se1 Ag Se1 115.28(3) 8_455 . ? Se1 Ag Se1 115.28(3) 7 2_565 ? Se1 Ag Se1 111.77(3) 8_455 2_565 ? Se1 Ag Se1 101.17(8) . 2_565 ? Se1 Ag Ag 51.07(4) 7 7 ? Se1 Ag Ag 51.07(4) 8_455 7 ? Se1 Ag Ag 129.42(4) . 7 ? Se1 Ag Ag 129.42(4) 2_565 7 ? Se1 Ag Ag 128.93(4) 7 7_554 ? Se1 Ag Ag 128.93(4) 8_455 7_554 ? Se1 Ag Ag 50.58(4) . 7_554 ? Se1 Ag Ag 50.58(4) 2_565 7_554 ? Ag Ag Ag 180.000(1) 7 7_554 ? Se1 Ag Ba 168.07(6) 7 6_455 ? Se1 Ag Ba 68.56(2) 8_455 6_455 ? Se1 Ag Ba 67.91(4) . 6_455 ? Se1 Ag Ba 75.92(4) 2_565 6_455 ? Ag Ag Ba 119.19(3) 7 6_455 ? Ag Ag Ba 60.81(3) 7_554 6_455 ? Se1 Ag Ba 68.56(2) 7 5 ? Se1 Ag Ba 168.07(6) 8_455 5 ? Se1 Ag Ba 75.92(4) . 5 ? Se1 Ag Ba 67.91(4) 2_565 5 ? Ag Ag Ba 119.19(3) 7 5 ? Ag Ag Ba 60.81(3) 7_554 5 ? Ba Ag Ba 121.62(6) 6_455 5 ? Se1 Ag Ba 68.03(3) 7 3_566 ? Se1 Ag Ba 76.08(4) 8_455 3_566 ? Se1 Ag Ba 167.76(6) . 3_566 ? Se1 Ag Ba 69.13(2) 2_565 3_566 ? Ag Ag Ba 60.72(3) 7 3_566 ? Ag Ag Ba 119.28(3) 7_554 3_566 ? Ba Ag Ba 114.991(14) 6_455 3_566 ? Ba Ag Ba 93.126(14) 5 3_566 ? Se1 Ag Ba 76.08(4) 7 4_556 ? Se1 Ag Ba 68.03(3) 8_455 4_556 ? Se1 Ag Ba 69.13(2) . 4_556 ? Se1 Ag Ba 167.76(6) 2_565 4_556 ? Ag Ag Ba 60.72(3) 7 4_556 ? Ag Ag Ba 119.28(3) 7_554 4_556 ? Ba Ag Ba 93.126(14) 6_455 4_556 ? Ba Ag Ba 114.991(14) 5 4_556 ? Ba Ag Ba 121.45(6) 3_566 4_556 ? Se1 Ga1 Se3 106.36(4) . . ? Se1 Ga1 Se2 108.25(4) . 7_554 ? Se3 Ga1 Se2 116.79(3) . 7_554 ? Se1 Ga1 Se2 115.50(3) . . ? Se3 Ga1 Se2 109.44(4) . . ? Se2 Ga1 Se2 100.84(3) 7_554 . ? Se3 Ga2 Se3 115.503(19) . 4 ? Se3 Ga2 Se3 115.503(19) . 3 ? Se3 Ga2 Se3 97.98(3) 4 3 ? Se3 Ga2 Se3 97.98(3) . 2 ? Se3 Ga2 Se3 115.503(19) 4 2 ? Se3 Ga2 Se3 115.503(19) 3 2 ? Ga1 Se1 Ag 122.04(4) . 7_554 ? Ga1 Se1 Ag 118.77(4) . . ? Ag Se1 Ag 78.35(2) 7_554 . ? Ga1 Se1 Ba 169.54(4) . 6_455 ? Ag Se1 Ba 66.88(2) 7_554 6_455 ? Ag Se1 Ba 66.65(2) . 6_455 ? Ga1 Se1 Ba 87.65(3) . 4 ? Ag Se1 Ba 66.47(4) 7_554 4 ? Ag Se1 Ba 144.00(4) . 4 ? Ba Se1 Ba 91.72(2) 6_455 4 ? Ga1 Se1 Ba 83.71(3) . 4_556 ? Ag Se1 Ba 143.39(4) 7_554 4_556 ? Ag Se1 Ba 65.84(4) . 4_556 ? Ba Se1 Ba 91.15(2) 6_455 4_556 ? Ba Se1 Ba 146.62(3) 4 4_556 ? Ga1 Se1 Ba 79.05(3) . 5 ? Ag Se1 Ba 61.38(2) 7_554 5 ? Ag Se1 Ba 61.22(2) . 5 ? Ba Se1 Ba 111.13(2) 6_455 5 ? Ba Se1 Ba 105.27(2) 4 5 ? Ba Se1 Ba 104.61(2) 4_556 5 ? Ga1 Se2 Ga1 111.49(3) 7 . ? Ga1 Se2 Ba 135.36(3) 7 7_554 ? Ga1 Se2 Ba 107.51(3) . 7_554 ? Ga1 Se2 Ba 88.38(3) 7 5 ? Ga1 Se2 Ba 86.18(3) . 5 ? Ba Se2 Ba 115.37(3) 7_554 5 ? Ga1 Se3 Ga2 106.15(3) . . ? Ga1 Se3 Ba 102.07(3) . . ? Ga2 Se3 Ba 119.41(2) . . ? Ga1 Se3 Ba 81.35(3) . 4_556 ? Ga2 Se3 Ba 125.96(3) . 4_556 ? Ba Se3 Ba 110.42(2) . 4_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.09 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.207 _refine_diff_density_min -1.685 _refine_diff_density_rms 0.222 #===END data_Ba4LiGa5Se12 _database_code_depnum_ccdc_archive 'CCDC 847973' #TrackingRef '- BaAgInS paper cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ba4 Ga5 Li Se12' _chemical_formula_weight 1852.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-421c 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 13.5906(19) _cell_length_b 13.5906(19) _cell_length_c 6.5148(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1203.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 4514 _cell_measurement_theta_min 2.9978 _cell_measurement_theta_max 30.0323 _exptl_crystal_description Chip _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1180 _exptl_crystal_size_mid 0.1030 _exptl_crystal_size_min 0.0900 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 30.071 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.156 _exptl_absorpt_correction_T_max 0.354 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku AFC10 diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10608 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.01 _reflns_number_total 1764 _reflns_number_gt 1701 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _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 0.06(3) _refine_ls_number_reflns 1764 _refine_ls_number_parameters 50 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.000 _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 Ba Ba 0.29970(4) 0.02236(3) 0.45216(8) 0.01302(11) Uani 1 1 d . . . Li Li 0.0000 0.0000 0.5000 0.056(13) Uani 1 4 d S . . Ga1 Ga 0.14161(6) 0.24344(6) 0.05297(14) 0.00443(16) Uani 1 1 d . . . Ga2 Ga 0.0000 0.0000 0.0000 0.0063(3) Uani 1 4 d S . . Se1 Se 0.01227(5) 0.35951(5) 0.04553(12) 0.00585(14) Uani 1 1 d . . . Se2 Se 0.29188(5) 0.30396(6) 0.20967(12) 0.00608(15) Uani 1 1 d . . . Se3 Se 0.08964(6) 0.10000(5) 0.23915(12) 0.00898(16) 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 Ba 0.0206(2) 0.0084(2) 0.0100(2) -0.00328(18) -0.0033(2) -0.00066(18) Li 0.08(2) 0.08(2) 0.011(19) 0.000 0.000 0.000 Ga1 0.0046(3) 0.0050(3) 0.0036(4) -0.0002(3) 0.0002(3) 0.0001(3) Ga2 0.0054(4) 0.0054(4) 0.0082(8) 0.000 0.000 0.000 Se1 0.0059(3) 0.0057(3) 0.0061(3) -0.0002(3) -0.0004(3) 0.0014(3) Se2 0.0038(3) 0.0107(3) 0.0037(3) -0.0025(3) 0.0001(3) -0.0002(3) Se3 0.0122(4) 0.0062(3) 0.0086(4) 0.0032(3) -0.0035(3) -0.0052(3) _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 Ba Se1 3.3052(10) 6 ? Ba Se2 3.3426(10) 7 ? Ba Se3 3.3450(10) . ? Ba Se1 3.3756(11) 3 ? Ba Se1 3.3806(10) 5_545 ? Ba Se2 3.3867(10) 5_545 ? Ba Se1 3.4047(11) 3_556 ? Ba Se3 3.7050(10) 3_556 ? Ba Ga1 3.8739(10) 5_545 ? Ba Li 4.0963(8) . ? Ba Ba 4.7231(9) 7 ? Ba Ba 4.7231(9) 7_554 ? Li Se3 2.4938(8) 2 ? Li Se3 2.4938(8) 3_556 ? Li Se3 2.4938(8) 4_556 ? Li Se3 2.4938(8) . ? Li Ga2 3.2574(6) . ? Li Ga2 3.2574(6) 1_556 ? Li Ba 4.0962(8) 2 ? Li Ba 4.0963(8) 4_556 ? Li Ba 4.0963(8) 3_556 ? Ga1 Se1 2.3624(11) . ? Ga1 Se3 2.4021(12) . ? Ga1 Se2 2.4040(12) 7_554 ? Ga1 Se2 2.4270(11) . ? Ga1 Ba 3.8739(10) 5 ? Ga2 Se3 2.3997(8) . ? Ga2 Se3 2.3997(8) 4 ? Ga2 Se3 2.3997(8) 3 ? Ga2 Se3 2.3997(8) 2 ? Ga2 Li 3.2574(6) 1_554 ? Se1 Ba 3.3052(10) 6_455 ? Se1 Ba 3.3756(11) 4 ? Se1 Ba 3.3806(10) 5 ? Se1 Ba 3.4047(11) 4_556 ? Se2 Ga1 2.4040(12) 7 ? Se2 Ba 3.3426(10) 7_554 ? Se2 Ba 3.3867(10) 5 ? Se3 Ba 3.7050(10) 4_556 ? 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 Se1 Ba Se2 89.96(2) 6 7 ? Se1 Ba Se3 126.49(2) 6 . ? Se2 Ba Se3 67.06(2) 7 . ? Se1 Ba Se1 82.04(2) 6 3 ? Se2 Ba Se1 133.54(2) 7 3 ? Se3 Ba Se1 81.43(2) . 3 ? Se1 Ba Se1 69.95(2) 6 5_545 ? Se2 Ba Se1 144.17(3) 7 5_545 ? Se3 Ba Se1 148.60(2) . 5_545 ? Se1 Ba Se1 74.394(19) 3 5_545 ? Se1 Ba Se2 138.45(2) 6 5_545 ? Se2 Ba Se2 131.55(3) 7 5_545 ? Se3 Ba Se2 80.43(2) . 5_545 ? Se1 Ba Se2 70.57(2) 3 5_545 ? Se1 Ba Se2 72.871(19) 5_545 5_545 ? Se1 Ba Se1 81.61(2) 6 3_556 ? Se2 Ba Se1 73.89(2) 7 3_556 ? Se3 Ba Se1 130.25(3) . 3_556 ? Se1 Ba Se1 147.83(3) 3 3_556 ? Se1 Ba Se1 74.02(2) 5_545 3_556 ? Se2 Ba Se1 105.42(2) 5_545 3_556 ? Se1 Ba Se3 146.86(3) 6 3_556 ? Se2 Ba Se3 74.28(2) 7 3_556 ? Se3 Ba Se3 74.31(3) . 3_556 ? Se1 Ba Se3 129.83(2) 3 3_556 ? Se1 Ba Se3 106.40(2) 5_545 3_556 ? Se2 Ba Se3 62.60(2) 5_545 3_556 ? Se1 Ba Se3 66.20(2) 3_556 3_556 ? Se1 Ba Ga1 107.18(2) 6 5_545 ? Se2 Ba Ga1 146.12(2) 7 5_545 ? Se3 Ba Ga1 118.74(2) . 5_545 ? Se1 Ba Ga1 78.80(2) 3 5_545 ? Se1 Ba Ga1 37.230(17) 5_545 5_545 ? Se2 Ba Ga1 38.319(18) 5_545 5_545 ? Se1 Ba Ga1 79.86(2) 3_556 5_545 ? Se3 Ba Ga1 75.73(2) 3_556 5_545 ? Se1 Ba Li 154.799(19) 6 . ? Se2 Ba Li 66.343(16) 7 . ? Se3 Ba Li 37.472(15) . . ? Se1 Ba Li 107.591(18) 3 . ? Se1 Ba Li 134.647(17) 5_545 . ? Se2 Ba Li 66.000(15) 5_545 . ? Se1 Ba Li 98.861(18) 3_556 . ? Se3 Ba Li 36.855(13) 3_556 . ? Ga1 Ba Li 97.633(16) 5_545 . ? Se1 Ba Ba 45.618(19) 6 7 ? Se2 Ba Ba 58.864(17) 7 7 ? Se3 Ba Ba 124.165(16) . 7 ? Se1 Ba Ba 127.63(2) 3 7 ? Se1 Ba Ba 86.851(15) 5_545 7 ? Se2 Ba Ba 148.386(17) 5_545 7 ? Se1 Ba Ba 44.407(13) 3_556 7 ? Se3 Ba Ba 102.186(19) 3_556 7 ? Ga1 Ba Ba 113.675(15) 5_545 7 ? Li Ba Ba 119.646(9) . 7 ? Se1 Ba Ba 46.12(2) 6 7_554 ? Se2 Ba Ba 100.092(19) 7 7_554 ? Se3 Ba Ba 89.390(17) . 7_554 ? Se1 Ba Ba 44.409(13) 3 7_554 ? Se1 Ba Ba 87.204(15) 5_545 7_554 ? Se2 Ba Ba 114.975(19) 5_545 7_554 ? Se1 Ba Ba 127.69(2) 3_556 7_554 ? Se3 Ba Ba 163.696(16) 3_556 7_554 ? Ga1 Ba Ba 112.933(15) 5_545 7_554 ? Li Ba Ba 126.841(8) . 7_554 ? Ba Ba Ba 87.21(2) 7 7_554 ? Se3 Li Se3 117.67(2) 2 3_556 ? Se3 Li Se3 117.67(2) 2 4_556 ? Se3 Li Se3 94.09(4) 3_556 4_556 ? Se3 Li Se3 94.09(4) 2 . ? Se3 Li Se3 117.67(2) 3_556 . ? Se3 Li Se3 117.67(2) 4_556 . ? Se3 Li Ga2 47.044(19) 2 . ? Se3 Li Ga2 132.956(19) 3_556 . ? Se3 Li Ga2 132.956(19) 4_556 . ? Se3 Li Ga2 47.044(19) . . ? Se3 Li Ga2 132.956(19) 2 1_556 ? Se3 Li Ga2 47.044(19) 3_556 1_556 ? Se3 Li Ga2 47.044(19) 4_556 1_556 ? Se3 Li Ga2 132.956(19) . 1_556 ? Ga2 Li Ga2 180.0 . 1_556 ? Se3 Li Ba 54.69(2) 2 2 ? Se3 Li Ba 123.883(19) 3_556 2 ? Se3 Li Ba 63.01(2) 4_556 2 ? Se3 Li Ba 118.32(2) . 2 ? Ga2 Li Ba 85.636(8) . 2 ? Ga2 Li Ba 94.364(8) 1_556 2 ? Se3 Li Ba 123.883(19) 2 4_556 ? Se3 Li Ba 118.32(2) 3_556 4_556 ? Se3 Li Ba 54.69(2) 4_556 4_556 ? Se3 Li Ba 63.01(2) . 4_556 ? Ga2 Li Ba 94.364(8) . 4_556 ? Ga2 Li Ba 85.636(8) 1_556 4_556 ? Ba Li Ba 90.332(1) 2 4_556 ? Se3 Li Ba 118.32(2) 2 . ? Se3 Li Ba 63.01(2) 3_556 . ? Se3 Li Ba 123.883(19) 4_556 . ? Se3 Li Ba 54.69(2) . . ? Ga2 Li Ba 85.636(8) . . ? Ga2 Li Ba 94.364(8) 1_556 . ? Ba Li Ba 171.272(15) 2 . ? Ba Li Ba 90.332(1) 4_556 . ? Se3 Li Ba 63.01(2) 2 3_556 ? Se3 Li Ba 54.69(2) 3_556 3_556 ? Se3 Li Ba 118.32(2) 4_556 3_556 ? Se3 Li Ba 123.883(19) . 3_556 ? Ga2 Li Ba 94.364(8) . 3_556 ? Ga2 Li Ba 85.636(8) 1_556 3_556 ? Ba Li Ba 90.332(1) 2 3_556 ? Ba Li Ba 171.272(15) 4_556 3_556 ? Ba Li Ba 90.332(1) . 3_556 ? Se1 Ga1 Se3 109.48(4) . . ? Se1 Ga1 Se2 110.07(4) . 7_554 ? Se3 Ga1 Se2 113.46(4) . 7_554 ? Se1 Ga1 Se2 114.11(4) . . ? Se3 Ga1 Se2 108.06(4) . . ? Se2 Ga1 Se2 101.54(4) 7_554 . ? Se1 Ga1 Ba 59.97(3) . 5 ? Se3 Ga1 Ba 149.20(4) . 5 ? Se2 Ga1 Ba 97.12(3) 7_554 5 ? Se2 Ga1 Ba 59.91(2) . 5 ? Se3 Ga2 Se3 114.93(2) . 4 ? Se3 Ga2 Se3 114.93(2) . 3 ? Se3 Ga2 Se3 99.03(4) 4 3 ? Se3 Ga2 Se3 99.03(4) . 2 ? Se3 Ga2 Se3 114.93(2) 4 2 ? Se3 Ga2 Se3 114.93(2) 3 2 ? Se3 Ga2 Li 49.52(2) . . ? Se3 Ga2 Li 130.49(2) 4 . ? Se3 Ga2 Li 130.49(2) 3 . ? Se3 Ga2 Li 49.52(2) 2 . ? Se3 Ga2 Li 130.49(2) . 1_554 ? Se3 Ga2 Li 49.51(2) 4 1_554 ? Se3 Ga2 Li 49.51(2) 3 1_554 ? Se3 Ga2 Li 130.48(2) 2 1_554 ? Li Ga2 Li 180.0 . 1_554 ? Ga1 Se1 Ba 167.07(4) . 6_455 ? Ga1 Se1 Ba 87.86(3) . 4 ? Ba Se1 Ba 89.97(2) 6_455 4 ? Ga1 Se1 Ba 82.80(3) . 5 ? Ba Se1 Ba 110.04(2) 6_455 5 ? Ba Se1 Ba 105.51(3) 4 5 ? Ga1 Se1 Ba 85.62(3) . 4_556 ? Ba Se1 Ba 89.47(2) 6_455 4_556 ? Ba Se1 Ba 147.83(3) 4 4_556 ? Ba Se1 Ba 104.86(3) 5 4_556 ? Ga1 Se2 Ga1 109.12(4) 7 . ? Ga1 Se2 Ba 138.37(3) 7 7_554 ? Ga1 Se2 Ba 106.36(3) . 7_554 ? Ga1 Se2 Ba 86.94(3) 7 5 ? Ga1 Se2 Ba 81.77(3) . 5 ? Ba Se2 Ba 119.39(3) 7_554 5 ? Ga2 Se3 Ga1 106.32(4) . . ? Ga2 Se3 Li 83.44(3) . . ? Ga1 Se3 Li 158.43(4) . . ? Ga2 Se3 Ba 121.60(3) . . ? Ga1 Se3 Ba 102.39(3) . . ? Li Se3 Ba 87.84(2) . . ? Ga2 Se3 Ba 123.97(3) . 4_556 ? Ga1 Se3 Ba 78.49(3) . 4_556 ? Li Se3 Ba 80.13(2) . 4_556 ? Ba Se3 Ba 110.89(2) . 4_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.315 _refine_diff_density_min -1.647 _refine_diff_density_rms 0.322 #===END