# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 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 ; BaGa2MQ6 (M = Si, Ge; Q = S, Se): A New Series of Promising IR Nonlinear Optical Materials ; # Attachment '- BaGa2MQS6 cif.cif' data_BaGa2GeS6 _database_code_depnum_ccdc_archive 'CCDC 861300' #TrackingRef '- BaGa2MQS6 cif.cif' _audit_update_record ; 2011-11-05 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ba Ga2 Ge S6' _chemical_formula_weight 541.73 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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 trigonal _symmetry_space_group_name_H-M R3 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' _cell_length_a 9.60200(10) _cell_length_b 9.60200(10) _cell_length_c 8.6889(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 693.775(19) _cell_formula_units_Z 3 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 1701 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 28.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.242 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.154 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 14.452 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.120 _exptl_absorpt_correction_T_max 0.230 _exptl_absorpt_process_details 'face indexed' _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 1955 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 28.24 _reflns_number_total 721 _reflns_number_gt 716 _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 0.0108(3) _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 0.027(15) _refine_ls_number_reflns 721 _refine_ls_number_parameters 32 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0177 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0387 _refine_ls_wR_factor_gt 0.0386 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _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_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 1.0000 1.0000 0.94546(3) 0.02815(14) Uani 1 3 d S . . Ga Ga 0.56493(5) 0.71158(5) 0.19048(3) 0.01160(11) Uani 0.67 1 d P . . Ge Ge 0.56493(5) 0.71158(5) 0.19048(3) 0.01160(11) Uani 0.33 1 d P . . S1 S 0.58810(14) 0.72725(13) 0.93168(8) 0.01458(19) Uani 1 1 d . . . S2 S 0.85816(10) 0.57086(11) 0.95774(12) 0.01423(18) 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 0.02894(19) 0.02894(19) 0.0266(2) 0.000 0.000 0.01447(9) Ga 0.0106(2) 0.0124(2) 0.01254(17) -0.00033(16) 0.00087(14) 0.00628(19) Ge 0.0106(2) 0.0124(2) 0.01254(17) -0.00033(16) 0.00087(14) 0.00628(19) S1 0.0201(4) 0.0141(4) 0.0131(4) 0.0009(3) 0.0011(3) 0.0112(4) S2 0.0121(4) 0.0137(4) 0.0171(4) -0.0038(3) -0.0017(3) 0.0066(4) _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 S1 3.4868(11) . ? Ba S1 3.4868(11) 3_675 ? Ba S1 3.4868(11) 2_765 ? Ba S2 3.4886(10) 8_654 ? Ba S2 3.4887(10) 7_554 ? Ba S2 3.4887(10) 9_664 ? Ba S1 3.5509(9) 4 ? Ba S1 3.5509(9) 6_565 ? Ba S1 3.5509(9) 5_665 ? Ba S2 3.6378(9) 2_765 ? Ba S2 3.6378(9) . ? Ba S2 3.6378(9) 3_675 ? Ga S2 2.2462(11) 4_454 ? Ga S2 2.2465(8) 6_564 ? Ga S1 2.2573(7) 1_554 ? Ga S1 2.2641(12) 6_564 ? S1 Ge 2.2573(7) 1_556 ? S1 Ga 2.2573(7) 1_556 ? S1 Ge 2.2642(12) 8_655 ? S1 Ga 2.2642(12) 8_655 ? S1 Ba 3.5509(9) 7_444 ? S2 Ge 2.2462(11) 7_545 ? S2 Ga 2.2462(11) 7_545 ? S2 Ge 2.2465(8) 8_655 ? S2 Ga 2.2465(8) 8_655 ? S2 Ba 3.4887(10) 4_445 ? 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 Ba S1 119.883(2) . 3_675 ? S1 Ba S1 119.883(2) . 2_765 ? S1 Ba S1 119.883(2) 3_675 2_765 ? S1 Ba S2 56.852(19) . 8_654 ? S1 Ba S2 88.381(19) 3_675 8_654 ? S1 Ba S2 119.52(2) 2_765 8_654 ? S1 Ba S2 119.52(2) . 7_554 ? S1 Ba S2 56.852(19) 3_675 7_554 ? S1 Ba S2 88.380(19) 2_765 7_554 ? S2 Ba S2 62.67(2) 8_654 7_554 ? S1 Ba S2 88.381(19) . 9_664 ? S1 Ba S2 119.52(2) 3_675 9_664 ? S1 Ba S2 56.851(19) 2_765 9_664 ? S2 Ba S2 62.67(2) 8_654 9_664 ? S2 Ba S2 62.67(2) 7_554 9_664 ? S1 Ba S1 125.43(3) . 4 ? S1 Ba S1 89.95(3) 3_675 4 ? S1 Ba S1 60.11(2) 2_765 4 ? S2 Ba S1 177.69(2) 8_654 4 ? S2 Ba S1 115.05(2) 7_554 4 ? S2 Ba S1 116.94(2) 9_664 4 ? S1 Ba S1 60.11(2) . 6_565 ? S1 Ba S1 125.43(3) 3_675 6_565 ? S1 Ba S1 89.95(3) 2_765 6_565 ? S2 Ba S1 116.94(2) 8_654 6_565 ? S2 Ba S1 177.69(2) 7_554 6_565 ? S2 Ba S1 115.05(2) 9_664 6_565 ? S1 Ba S1 65.35(3) 4 6_565 ? S1 Ba S1 89.95(3) . 5_665 ? S1 Ba S1 60.11(2) 3_675 5_665 ? S1 Ba S1 125.43(3) 2_765 5_665 ? S2 Ba S1 115.05(2) 8_654 5_665 ? S2 Ba S1 116.95(2) 7_554 5_665 ? S2 Ba S1 177.69(2) 9_664 5_665 ? S1 Ba S1 65.35(3) 4 5_665 ? S1 Ba S1 65.35(3) 6_565 5_665 ? S1 Ba S2 179.45(2) . 2_765 ? S1 Ba S2 59.64(2) 3_675 2_765 ? S1 Ba S2 60.56(2) 2_765 2_765 ? S2 Ba S2 122.71(3) 8_654 2_765 ? S2 Ba S2 60.053(19) 7_554 2_765 ? S2 Ba S2 91.67(2) 9_664 2_765 ? S1 Ba S2 55.00(3) 4 2_765 ? S1 Ba S2 120.33(2) 6_565 2_765 ? S1 Ba S2 89.98(2) 5_665 2_765 ? S1 Ba S2 60.56(2) . . ? S1 Ba S2 179.45(2) 3_675 . ? S1 Ba S2 59.64(2) 2_765 . ? S2 Ba S2 91.67(2) 8_654 . ? S2 Ba S2 122.71(3) 7_554 . ? S2 Ba S2 60.053(19) 9_664 . ? S1 Ba S2 89.98(2) 4 . ? S1 Ba S2 55.00(3) 6_565 . ? S1 Ba S2 120.33(2) 5_665 . ? S2 Ba S2 119.915(2) 2_765 . ? S1 Ba S2 59.64(2) . 3_675 ? S1 Ba S2 60.56(2) 3_675 3_675 ? S1 Ba S2 179.45(2) 2_765 3_675 ? S2 Ba S2 60.054(19) 8_654 3_675 ? S2 Ba S2 91.67(2) 7_554 3_675 ? S2 Ba S2 122.71(3) 9_664 3_675 ? S1 Ba S2 120.33(2) 4 3_675 ? S1 Ba S2 89.98(2) 6_565 3_675 ? S1 Ba S2 55.00(3) 5_665 3_675 ? S2 Ba S2 119.915(2) 2_765 3_675 ? S2 Ba S2 119.915(2) . 3_675 ? S2 Ga S2 107.74(5) 4_454 6_564 ? S2 Ga S1 112.61(4) 4_454 1_554 ? S2 Ga S1 117.19(4) 6_564 1_554 ? S2 Ga S1 110.77(4) 4_454 6_564 ? S2 Ga S1 105.69(4) 6_564 6_564 ? S1 Ga S1 102.47(3) 1_554 6_564 ? Ge S1 Ga 0.00(2) 1_556 1_556 ? Ge S1 Ge 106.20(3) 1_556 8_655 ? Ga S1 Ge 106.20(3) 1_556 8_655 ? Ge S1 Ga 106.20(3) 1_556 8_655 ? Ga S1 Ga 106.20(3) 1_556 8_655 ? Ge S1 Ga 0.000(7) 8_655 8_655 ? Ge S1 Ba 93.03(3) 1_556 . ? Ga S1 Ba 93.03(3) 1_556 . ? Ge S1 Ba 93.62(4) 8_655 . ? Ga S1 Ba 93.62(4) 8_655 . ? Ge S1 Ba 136.99(4) 1_556 7_444 ? Ga S1 Ba 136.99(4) 1_556 7_444 ? Ge S1 Ba 91.25(3) 8_655 7_444 ? Ga S1 Ba 91.25(3) 8_655 7_444 ? Ba S1 Ba 125.43(3) . 7_444 ? Ge S2 Ga 0.000(10) 7_545 7_545 ? Ge S2 Ge 103.90(4) 7_545 8_655 ? Ga S2 Ge 103.90(4) 7_545 8_655 ? Ge S2 Ga 103.90(4) 7_545 8_655 ? Ga S2 Ga 103.90(4) 7_545 8_655 ? Ge S2 Ga 0.000(10) 8_655 8_655 ? Ge S2 Ba 91.38(3) 7_545 4_445 ? Ga S2 Ba 91.38(3) 7_545 4_445 ? Ge S2 Ba 91.38(3) 8_655 4_445 ? Ga S2 Ba 91.38(3) 8_655 4_445 ? Ge S2 Ba 143.13(4) 7_545 . ? Ga S2 Ba 143.13(4) 7_545 . ? Ge S2 Ba 90.01(2) 8_655 . ? Ga S2 Ba 90.01(2) 8_655 . ? Ba S2 Ba 122.71(3) 4_445 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.584 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.106 ################################### data_BaGa2GeSe6 _database_code_depnum_ccdc_archive 'CCDC 861301' #TrackingRef '- BaGa2MQS6 cif.cif' _cell_special_details ? #Added by publCIF _audit_update_record ; 2011-11-05 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ba Ga2 Ge Se6' _chemical_formula_weight 823.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ba Ba -0.3244 2.2819 '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' Ge Ge 0.1547 1.8001 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R3 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' _cell_length_a 10.0075(14) _cell_length_b 10.0075(14) _cell_length_c 9.0903(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 788.4(2) _cell_formula_units_Z 3 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 1185 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 30.9 _exptl_crystal_description Block _exptl_crystal_colour orange _exptl_crystal_size_max 0.1540 _exptl_crystal_size_mid 0.1340 _exptl_crystal_size_min 0.0880 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1062 _exptl_absorpt_coefficient_mu 32.301 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.041 _exptl_absorpt_correction_T_max 0.126 _exptl_absorpt_process_details 'face indexed' _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 2532 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 30.87 _reflns_number_total 1117 _reflns_number_gt 1019 _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^)+(0.0100P)^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 0.00282(6) _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 0.00(3) _refine_ls_number_reflns 1117 _refine_ls_number_parameters 33 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0509 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _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 1.0000 1.0000 0.99987(11) 0.01975(19) Uani 1 3 d S . . Ga Ga 0.95593(8) 0.76799(8) 0.58714(8) 0.00571(15) Uani 0.67 1 d P . . Ge Ge 0.95593(8) 0.76799(8) 0.58714(8) 0.00571(15) Uani 0.33 1 d P . . Se1 Se 0.75942(8) 0.80535(8) 0.69207(6) 0.00671(15) Uani 1 1 d . . . Se2 Se 0.58915(8) 0.85665(7) 0.99271(6) 0.00729(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 0.0211(3) 0.0211(3) 0.0170(4) 0.000 0.000 0.01056(14) Ga 0.0070(4) 0.0061(3) 0.0045(3) -0.0006(3) 0.0003(3) 0.0036(3) Ge 0.0070(4) 0.0061(3) 0.0045(3) -0.0006(3) 0.0003(3) 0.0036(3) Se1 0.0077(3) 0.0055(3) 0.0067(3) 0.0012(3) 0.0026(3) 0.0032(3) Se2 0.0113(3) 0.0062(3) 0.0054(3) 0.0002(2) 0.0015(2) 0.0051(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 3.5679(12) . ? Ba Se1 3.5679(12) 3_675 ? Ba Se1 3.5679(12) 2_765 ? Ba Se2 3.6151(9) 3_675 ? Ba Se2 3.6151(9) . ? Ba Se2 3.6151(9) 2_765 ? Ba Se2 3.7540(12) 6_565 ? Ba Se2 3.7540(12) 4 ? Ba Se2 3.7540(12) 5_665 ? Ba Se1 3.7741(9) 4 ? Ba Se1 3.7742(9) 6_565 ? Ba Se1 3.7742(9) 5_665 ? Ga Se1 2.3741(9) 2_765 ? Ga Se1 2.3774(11) . ? Ga Se2 2.3844(11) 6_564 ? Ga Se2 2.3915(10) 7_544 ? Se1 Ge 2.3741(9) 3_675 ? Se1 Ga 2.3741(9) 3_675 ? Se1 Ba 3.7741(9) 7_444 ? Se2 Ge 2.3844(10) 8_655 ? Se2 Ga 2.3844(10) 8_655 ? Se2 Ge 2.3915(10) 4_455 ? Se2 Ga 2.3915(10) 4_455 ? Se2 Ba 3.7540(12) 7_444 ? 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 Se1 65.01(2) . 3_675 ? Se1 Ba Se1 65.01(2) . 2_765 ? Se1 Ba Se1 65.01(2) 3_675 2_765 ? Se1 Ba Se2 121.38(3) . 3_675 ? Se1 Ba Se2 56.366(18) 3_675 3_675 ? Se1 Ba Se2 89.477(19) 2_765 3_675 ? Se1 Ba Se2 56.366(17) . . ? Se1 Ba Se2 89.477(19) 3_675 . ? Se1 Ba Se2 121.38(3) 2_765 . ? Se2 Ba Se2 119.968(1) 3_675 . ? Se1 Ba Se2 89.477(19) . 2_765 ? Se1 Ba Se2 121.38(3) 3_675 2_765 ? Se1 Ba Se2 56.366(17) 2_765 2_765 ? Se2 Ba Se2 119.968(1) 3_675 2_765 ? Se2 Ba Se2 119.968(1) . 2_765 ? Se1 Ba Se2 113.993(18) . 6_565 ? Se1 Ba Se2 177.483(15) 3_675 6_565 ? Se1 Ba Se2 116.905(17) 2_765 6_565 ? Se2 Ba Se2 124.58(3) 3_675 6_565 ? Se2 Ba Se2 88.09(2) . 6_565 ? Se2 Ba Se2 60.565(17) 2_765 6_565 ? Se1 Ba Se2 177.484(15) . 4 ? Se1 Ba Se2 116.904(17) 3_675 4 ? Se1 Ba Se2 113.994(18) 2_765 4 ? Se2 Ba Se2 60.564(17) 3_675 4 ? Se2 Ba Se2 124.58(3) . 4 ? Se2 Ba Se2 88.09(2) 2_765 4 ? Se2 Ba Se2 64.17(3) 6_565 4 ? Se1 Ba Se2 116.904(17) . 5_665 ? Se1 Ba Se2 113.993(18) 3_675 5_665 ? Se1 Ba Se2 177.484(15) 2_765 5_665 ? Se2 Ba Se2 88.09(2) 3_675 5_665 ? Se2 Ba Se2 60.564(17) . 5_665 ? Se2 Ba Se2 124.58(3) 2_765 5_665 ? Se2 Ba Se2 64.17(3) 6_565 5_665 ? Se2 Ba Se2 64.17(3) 4 5_665 ? Se1 Ba Se1 125.37(3) . 4 ? Se1 Ba Se1 93.41(2) 3_675 4 ? Se1 Ba Se1 60.421(16) 2_765 4 ? Se2 Ba Se1 61.634(14) 3_675 4 ? Se2 Ba Se1 177.09(3) . 4 ? Se2 Ba Se1 58.649(14) 2_765 4 ? Se2 Ba Se1 89.02(2) 6_565 4 ? Se2 Ba Se1 53.573(16) 4 4 ? Se2 Ba Se1 117.72(3) 5_665 4 ? Se1 Ba Se1 60.420(16) . 6_565 ? Se1 Ba Se1 125.37(3) 3_675 6_565 ? Se1 Ba Se1 93.41(2) 2_765 6_565 ? Se2 Ba Se1 177.09(3) 3_675 6_565 ? Se2 Ba Se1 58.648(14) . 6_565 ? Se2 Ba Se1 61.635(14) 2_765 6_565 ? Se2 Ba Se1 53.573(16) 6_565 6_565 ? Se2 Ba Se1 117.72(3) 4 6_565 ? Se2 Ba Se1 89.02(2) 5_665 6_565 ? Se1 Ba Se1 119.626(4) 4 6_565 ? Se1 Ba Se1 93.41(2) . 5_665 ? Se1 Ba Se1 60.421(16) 3_675 5_665 ? Se1 Ba Se1 125.37(3) 2_765 5_665 ? Se2 Ba Se1 58.648(14) 3_675 5_665 ? Se2 Ba Se1 61.634(14) . 5_665 ? Se2 Ba Se1 177.09(3) 2_765 5_665 ? Se2 Ba Se1 117.72(3) 6_565 5_665 ? Se2 Ba Se1 89.02(2) 4 5_665 ? Se2 Ba Se1 53.572(16) 5_665 5_665 ? Se1 Ba Se1 119.625(4) 4 5_665 ? Se1 Ba Se1 119.624(4) 6_565 5_665 ? Se1 Ga Se1 107.61(4) 2_765 . ? Se1 Ga Se2 118.95(4) 2_765 6_564 ? Se1 Ga Se2 111.94(4) . 6_564 ? Se1 Ga Se2 105.28(3) 2_765 7_544 ? Se1 Ga Se2 110.34(4) . 7_544 ? Se2 Ga Se2 102.24(3) 6_564 7_544 ? Ge Se1 Ga 0.00(5) 3_675 3_675 ? Ge Se1 Ga 102.25(4) 3_675 . ? Ga Se1 Ga 102.25(4) 3_675 . ? Ge Se1 Ba 90.92(3) 3_675 . ? Ga Se1 Ba 90.92(3) 3_675 . ? Ga Se1 Ba 90.86(3) . . ? Ge Se1 Ba 89.24(2) 3_675 7_444 ? Ga Se1 Ba 89.24(2) 3_675 7_444 ? Ga Se1 Ba 142.07(3) . 7_444 ? Ba Se1 Ba 125.37(3) . 7_444 ? Ge Se2 Ga 0.00(7) 8_655 8_655 ? Ge Se2 Ge 104.14(3) 8_655 4_455 ? Ga Se2 Ge 104.14(3) 8_655 4_455 ? Ge Se2 Ga 104.14(3) 8_655 4_455 ? Ga Se2 Ga 104.14(3) 8_655 4_455 ? Ge Se2 Ga 0.00(4) 4_455 4_455 ? Ge Se2 Ba 94.27(3) 8_655 . ? Ga Se2 Ba 94.27(3) 8_655 . ? Ge Se2 Ba 92.84(3) 4_455 . ? Ga Se2 Ba 92.84(3) 4_455 . ? Ge Se2 Ba 137.90(3) 8_655 7_444 ? Ga Se2 Ba 137.90(3) 8_655 7_444 ? Ge Se2 Ba 90.72(3) 4_455 7_444 ? Ga Se2 Ba 90.72(3) 4_455 7_444 ? Ba Se2 Ba 124.58(3) . 7_444 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.87 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.848 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.266 ################################# data_BaGa2SiS6 _database_code_depnum_ccdc_archive 'CCDC 861302' #TrackingRef '- BaGa2MQS6 cif.cif' _audit_update_record ; 2011-11-05 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ba Ga2 S6 Si' _chemical_formula_weight 497.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 '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' Ga Ga 0.2307 1.6083 '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 trigonal _symmetry_space_group_name_H-M R3 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' _cell_length_a 9.5544(2) _cell_length_b 9.5544(2) _cell_length_c 8.6498(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 683.82(4) _cell_formula_units_Z 3 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.221 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.145 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 11.561 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.102 _exptl_absorpt_correction_T_max 0.205 _exptl_absorpt_process_details 'face indexed' _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 1875 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.33 _reflns_number_total 666 _reflns_number_gt 664 _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^)+(0.0100P)^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 0.00483(16) _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 0.048(18) _refine_ls_number_reflns 666 _refine_ls_number_parameters 32 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0144 _refine_ls_R_factor_gt 0.0144 _refine_ls_wR_factor_ref 0.0313 _refine_ls_wR_factor_gt 0.0313 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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_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 1.0000 1.0000 0.540056(1) 0.02948(13) Uani 1 3 d S . . Ga Ga 0.04444(6) 0.81373(6) 0.96271(5) 0.01302(11) Uani 0.67 1 d P . . Si Si 0.04444(6) 0.81373(6) 0.96271(5) 0.01302(11) Uani 0.33 1 d P . . S1 S 0.86364(11) 0.58816(12) 0.55307(9) 0.01939(18) Uani 1 1 d . . . S2 S 0.80899(10) 0.76403(9) 0.86552(12) 0.01832(17) 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 0.03095(17) 0.03095(17) 0.02655(17) 0.000 0.000 0.01547(9) Ga 0.0140(3) 0.0126(3) 0.01293(18) 0.00106(17) 0.00053(18) 0.0070(2) Si 0.0140(3) 0.0126(3) 0.01293(18) 0.00106(17) 0.00053(18) 0.0070(2) S1 0.0169(4) 0.0256(4) 0.0171(4) -0.0019(3) 0.0001(3) 0.0117(4) S2 0.0146(4) 0.0180(4) 0.0198(4) -0.0030(3) -0.0015(3) 0.0062(4) _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 S1 3.4737(10) 2_765 ? Ba S1 3.4737(10) . ? Ba S1 3.4737(10) 3_675 ? Ba S2 3.4963(10) 2_765 ? Ba S2 3.4963(10) 3_675 ? Ba S2 3.4963(10) . ? Ba S1 3.5446(9) 8_654 ? Ba S1 3.5446(9) 7_554 ? Ba S1 3.5447(9) 9_664 ? Ba S2 3.6320(8) 7_554 ? Ba S2 3.6321(8) 8_654 ? Ba S2 3.6321(8) 9_664 ? Ga S2 2.2121(11) 2_665 ? Ga S2 2.2191(8) 1_455 ? Ga S1 2.2322(10) 9_565 ? Ga S1 2.2387(12) 5 ? S1 Si 2.2322(10) 5_664 ? S1 Ga 2.2322(10) 5_664 ? S1 Si 2.2388(12) 9_554 ? S1 Ga 2.2388(12) 9_554 ? S1 Ba 3.5446(9) 4_445 ? S2 Si 2.2121(11) 3_565 ? S2 Ga 2.2121(11) 3_565 ? S2 Si 2.2191(8) 1_655 ? S2 Ga 2.2191(8) 1_655 ? S2 Ba 3.6320(8) 4_445 ? 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 Ba S1 119.896(2) 2_765 . ? S1 Ba S1 119.896(2) 2_765 3_675 ? S1 Ba S1 119.896(2) . 3_675 ? S1 Ba S2 57.606(15) 2_765 2_765 ? S1 Ba S2 88.089(18) . 2_765 ? S1 Ba S2 119.39(2) 3_675 2_765 ? S1 Ba S2 88.089(18) 2_765 3_675 ? S1 Ba S2 119.39(2) . 3_675 ? S1 Ba S2 57.606(15) 3_675 3_675 ? S2 Ba S2 61.80(2) 2_765 3_675 ? S1 Ba S2 119.39(2) 2_765 . ? S1 Ba S2 57.606(15) . . ? S1 Ba S2 88.089(18) 3_675 . ? S2 Ba S2 61.80(2) 2_765 . ? S2 Ba S2 61.80(2) 3_675 . ? S1 Ba S1 124.96(2) 2_765 8_654 ? S1 Ba S1 90.54(3) . 8_654 ? S1 Ba S1 59.58(2) 3_675 8_654 ? S2 Ba S1 177.42(2) 2_765 8_654 ? S2 Ba S1 117.18(2) 3_675 8_654 ? S2 Ba S1 115.624(17) . 8_654 ? S1 Ba S1 59.58(2) 2_765 7_554 ? S1 Ba S1 124.96(2) . 7_554 ? S1 Ba S1 90.54(3) 3_675 7_554 ? S2 Ba S1 117.17(2) 2_765 7_554 ? S2 Ba S1 115.624(17) 3_675 7_554 ? S2 Ba S1 177.42(2) . 7_554 ? S1 Ba S1 65.39(2) 8_654 7_554 ? S1 Ba S1 90.54(3) 2_765 9_664 ? S1 Ba S1 59.58(2) . 9_664 ? S1 Ba S1 124.96(2) 3_675 9_664 ? S2 Ba S1 115.623(17) 2_765 9_664 ? S2 Ba S1 177.42(2) 3_675 9_664 ? S2 Ba S1 117.17(2) . 9_664 ? S1 Ba S1 65.39(2) 8_654 9_664 ? S1 Ba S1 65.39(2) 7_554 9_664 ? S1 Ba S2 60.104(18) 2_765 7_554 ? S1 Ba S2 179.22(3) . 7_554 ? S1 Ba S2 60.023(19) 3_675 7_554 ? S2 Ba S2 91.30(2) 2_765 7_554 ? S2 Ba S2 59.856(18) 3_675 7_554 ? S2 Ba S2 121.65(3) . 7_554 ? S1 Ba S2 90.05(2) 8_654 7_554 ? S1 Ba S2 55.78(2) 7_554 7_554 ? S1 Ba S2 121.16(2) 9_664 7_554 ? S1 Ba S2 179.22(3) 2_765 8_654 ? S1 Ba S2 60.022(18) . 8_654 ? S1 Ba S2 60.105(18) 3_675 8_654 ? S2 Ba S2 121.65(3) 2_765 8_654 ? S2 Ba S2 91.30(2) 3_675 8_654 ? S2 Ba S2 59.856(18) . 8_654 ? S1 Ba S2 55.78(2) 8_654 8_654 ? S1 Ba S2 121.16(2) 7_554 8_654 ? S1 Ba S2 90.05(2) 9_664 8_654 ? S2 Ba S2 119.966(1) 7_554 8_654 ? S1 Ba S2 60.023(18) 2_765 9_664 ? S1 Ba S2 60.104(18) . 9_664 ? S1 Ba S2 179.22(3) 3_675 9_664 ? S2 Ba S2 59.856(18) 2_765 9_664 ? S2 Ba S2 121.65(3) 3_675 9_664 ? S2 Ba S2 91.30(2) . 9_664 ? S1 Ba S2 121.16(2) 8_654 9_664 ? S1 Ba S2 90.05(2) 7_554 9_664 ? S1 Ba S2 55.78(2) 9_664 9_664 ? S2 Ba S2 119.965(1) 7_554 9_664 ? S2 Ba S2 119.964(1) 8_654 9_664 ? S2 Ga S2 108.28(5) 2_665 1_455 ? S2 Ga S1 112.74(4) 2_665 9_565 ? S2 Ga S1 116.28(4) 1_455 9_565 ? S2 Ga S1 110.61(5) 2_665 5 ? S2 Ga S1 106.04(4) 1_455 5 ? S1 Ga S1 102.52(3) 9_565 5 ? Si S1 Ga 0.0 5_664 5_664 ? Si S1 Si 107.42(4) 5_664 9_554 ? Ga S1 Si 107.42(4) 5_664 9_554 ? Si S1 Ga 107.42(4) 5_664 9_554 ? Ga S1 Ga 107.42(4) 5_664 9_554 ? Si S1 Ga 0.00(3) 9_554 9_554 ? Si S1 Ba 93.24(3) 5_664 . ? Ga S1 Ba 93.24(3) 5_664 . ? Si S1 Ba 93.86(3) 9_554 . ? Ga S1 Ba 93.86(3) 9_554 . ? Si S1 Ba 136.59(3) 5_664 4_445 ? Ga S1 Ba 136.59(3) 5_664 4_445 ? Si S1 Ba 91.26(3) 9_554 4_445 ? Ga S1 Ba 91.26(3) 9_554 4_445 ? Ba S1 Ba 124.96(2) . 4_445 ? Si S2 Ga 0.00(3) 3_565 3_565 ? Si S2 Si 104.70(4) 3_565 1_655 ? Ga S2 Si 104.70(4) 3_565 1_655 ? Si S2 Ga 104.70(4) 3_565 1_655 ? Ga S2 Ga 104.70(4) 3_565 1_655 ? Si S2 Ga 0.00(3) 1_655 1_655 ? Si S2 Ba 91.30(3) 3_565 . ? Ga S2 Ba 91.30(3) 3_565 . ? Si S2 Ba 91.18(3) 1_655 . ? Ga S2 Ba 91.18(3) 1_655 . ? Si S2 Ba 143.92(4) 3_565 4_445 ? Ga S2 Ba 143.92(4) 3_565 4_445 ? Si S2 Ba 90.03(2) 1_655 4_445 ? Ga S2 Ba 90.03(2) 1_655 4_445 ? Ba S2 Ba 121.65(3) . 4_445 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.592 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.090 ############################## data_BaGa2SiSe6 _database_code_depnum_ccdc_archive 'CCDC 861303' #TrackingRef '- BaGa2MQS6 cif.cif' _audit_update_record ; 2011-11-05 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ba Ga2 Se6 Si' _chemical_formula_weight 778.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 '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 trigonal _symmetry_space_group_name_H-M R3 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' _cell_length_a 9.9666(14) _cell_length_b 9.9666(14) _cell_length_c 9.0471(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 778.3(2) _cell_formula_units_Z 3 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 30.95 _exptl_crystal_description Chunk _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2970 _exptl_crystal_size_mid 0.2180 _exptl_crystal_size_min 0.1120 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 29.997 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.050 _exptl_absorpt_correction_T_max 0.150 _exptl_absorpt_process_details 'face indexed' _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 2476 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 30.95 _reflns_number_total 1104 _reflns_number_gt 898 _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 SHELXL _refine_ls_extinction_coef 0.00083(7) _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 0.02(4) _refine_ls_number_reflns 1104 _refine_ls_number_parameters 32 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.835 _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_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 0.6667 0.3333 0.35080(15) 0.0194(3) Uani 1 3 d S . . Ga Ga 0.71042(17) 0.14625(16) 0.76465(16) 0.0062(3) Uani 0.67 1 d P . . Si Si 0.71042(17) 0.14625(16) 0.76465(16) 0.0062(3) Uani 0.33 1 d P . . Se1 Se 0.23917(12) 0.04532(12) 0.32880(9) 0.0094(3) Uani 1 1 d . . . Se2 Se 0.72935(12) 0.14090(11) 0.02328(10) 0.0106(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 Ba 0.0209(4) 0.0209(4) 0.0164(5) 0.000 0.000 0.0104(2) Ga 0.0058(6) 0.0060(7) 0.0069(6) 0.0018(5) 0.0008(5) 0.0031(6) Si 0.0058(6) 0.0060(7) 0.0069(6) 0.0018(5) 0.0008(5) 0.0031(6) Se1 0.0091(5) 0.0125(5) 0.0095(6) 0.0022(4) 0.0025(4) 0.0075(4) Se2 0.0094(5) 0.0069(5) 0.0116(6) 0.0000(4) -0.0015(4) 0.0012(4) _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 3.5697(16) 4 ? Ba Se1 3.5698(16) 6 ? Ba Se1 3.5698(16) 5 ? Ba Se2 3.6110(12) 5_545 ? Ba Se2 3.6110(12) 6_665 ? Ba Se2 3.6110(12) 4_455 ? Ba Se2 3.7479(16) . ? Ba Se2 3.7479(16) 3_665 ? Ba Se2 3.7479(16) 2_655 ? Ba Se1 3.7686(12) 2_655 ? Ba Se1 3.7686(12) . ? Ba Se1 3.7686(12) 3_665 ? Ga Se1 2.3468(19) 4 ? Ga Se1 2.3470(16) 6 ? Ga Se2 2.3502(19) 1_556 ? Ga Se2 2.3720(18) 9_655 ? Se1 Si 2.3468(19) 7_444 ? Se1 Ga 2.3468(19) 7_444 ? Se1 Si 2.3469(16) 8_544 ? Se1 Ga 2.3469(16) 8_544 ? Se1 Ba 3.5697(16) 7_444 ? Se2 Si 2.3502(19) 1_554 ? Se2 Ga 2.3502(19) 1_554 ? Se2 Si 2.3719(18) 5_544 ? Se2 Ga 2.3719(18) 5_544 ? Se2 Ba 3.6110(12) 7_544 ? 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 Se1 64.29(3) 4 6 ? Se1 Ba Se1 64.28(3) 4 5 ? Se1 Ba Se1 64.28(3) 6 5 ? Se1 Ba Se2 89.32(3) 4 5_545 ? Se1 Ba Se2 57.09(3) 6 5_545 ? Se1 Ba Se2 121.38(4) 5 5_545 ? Se1 Ba Se2 57.09(3) 4 6_665 ? Se1 Ba Se2 121.38(4) 6 6_665 ? Se1 Ba Se2 89.32(3) 5 6_665 ? Se2 Ba Se2 119.980(1) 5_545 6_665 ? Se1 Ba Se2 121.38(4) 4 4_455 ? Se1 Ba Se2 89.32(3) 6 4_455 ? Se1 Ba Se2 57.09(3) 5 4_455 ? Se2 Ba Se2 119.979(1) 5_545 4_455 ? Se2 Ba Se2 119.978(1) 6_665 4_455 ? Se1 Ba Se2 114.64(2) 4 . ? Se1 Ba Se2 117.07(2) 6 . ? Se1 Ba Se2 177.93(2) 5 . ? Se2 Ba Se2 59.99(2) 5_545 . ? Se2 Ba Se2 88.63(3) 6_665 . ? Se2 Ba Se2 123.96(4) 4_455 . ? Se1 Ba Se2 177.94(2) 4 3_665 ? Se1 Ba Se2 114.64(2) 6 3_665 ? Se1 Ba Se2 117.07(2) 5 3_665 ? Se2 Ba Se2 88.63(3) 5_545 3_665 ? Se2 Ba Se2 123.96(4) 6_665 3_665 ? Se2 Ba Se2 59.99(2) 4_455 3_665 ? Se2 Ba Se2 64.05(3) . 3_665 ? Se1 Ba Se2 117.07(2) 4 2_655 ? Se1 Ba Se2 177.93(2) 6 2_655 ? Se1 Ba Se2 114.64(2) 5 2_655 ? Se2 Ba Se2 123.96(4) 5_545 2_655 ? Se2 Ba Se2 59.99(2) 6_665 2_655 ? Se2 Ba Se2 88.63(3) 4_455 2_655 ? Se2 Ba Se2 64.05(3) . 2_655 ? Se2 Ba Se2 64.05(3) 3_665 2_655 ? Se1 Ba Se1 60.32(2) 4 2_655 ? Se1 Ba Se1 93.04(3) 6 2_655 ? Se1 Ba Se1 124.55(4) 5 2_655 ? Se2 Ba Se1 61.12(2) 5_545 2_655 ? Se2 Ba Se1 59.08(2) 6_665 2_655 ? Se2 Ba Se1 177.58(4) 4_455 2_655 ? Se2 Ba Se1 54.33(2) . 2_655 ? Se2 Ba Se1 118.37(4) 3_665 2_655 ? Se2 Ba Se1 89.01(3) 2_655 2_655 ? Se1 Ba Se1 124.55(4) 4 . ? Se1 Ba Se1 60.31(2) 6 . ? Se1 Ba Se1 93.04(3) 5 . ? Se2 Ba Se1 59.08(2) 5_545 . ? Se2 Ba Se1 177.58(4) 6_665 . ? Se2 Ba Se1 61.12(2) 4_455 . ? Se2 Ba Se1 89.01(3) . . ? Se2 Ba Se1 54.33(2) 3_665 . ? Se2 Ba Se1 118.37(4) 2_655 . ? Se1 Ba Se1 119.724(5) 2_655 . ? Se1 Ba Se1 93.04(3) 4 3_665 ? Se1 Ba Se1 124.55(4) 6 3_665 ? Se1 Ba Se1 60.31(2) 5 3_665 ? Se2 Ba Se1 177.58(4) 5_545 3_665 ? Se2 Ba Se1 61.12(2) 6_665 3_665 ? Se2 Ba Se1 59.08(2) 4_455 3_665 ? Se2 Ba Se1 118.37(4) . 3_665 ? Se2 Ba Se1 89.01(3) 3_665 3_665 ? Se2 Ba Se1 54.33(2) 2_655 3_665 ? Se1 Ba Se1 119.724(5) 2_655 3_665 ? Se1 Ba Se1 119.724(5) . 3_665 ? Se1 Ga Se1 108.05(8) 4 6 ? Se1 Ga Se2 112.30(6) 4 1_556 ? Se1 Ga Se2 118.16(7) 6 1_556 ? Se1 Ga Se2 109.93(8) 4 9_655 ? Se1 Ga Se2 105.44(7) 6 9_655 ? Se2 Ga Se2 102.43(6) 1_556 9_655 ? Si Se1 Ga 0.00(12) 7_444 7_444 ? Si Se1 Si 102.72(8) 7_444 8_544 ? Ga Se1 Si 102.72(8) 7_444 8_544 ? Si Se1 Ga 102.72(8) 7_444 8_544 ? Ga Se1 Ga 102.72(8) 7_444 8_544 ? Si Se1 Ga 0.00(9) 8_544 8_544 ? Si Se1 Ba 90.85(5) 7_444 7_444 ? Ga Se1 Ba 90.85(5) 7_444 7_444 ? Si Se1 Ba 90.85(5) 8_544 7_444 ? Ga Se1 Ba 90.85(5) 8_544 7_444 ? Si Se1 Ba 142.67(6) 7_444 . ? Ga Se1 Ba 142.67(6) 7_444 . ? Si Se1 Ba 89.44(4) 8_544 . ? Ga Se1 Ba 89.44(4) 8_544 . ? Ba Se1 Ba 124.55(4) 7_444 . ? Si Se2 Ga 0.00(14) 1_554 1_554 ? Si Se2 Si 105.52(5) 1_554 5_544 ? Ga Se2 Si 105.52(5) 1_554 5_544 ? Si Se2 Ga 105.52(5) 1_554 5_544 ? Ga Se2 Ga 105.52(5) 1_554 5_544 ? Si Se2 Ga 0.00(14) 5_544 5_544 ? Si Se2 Ba 94.49(5) 1_554 7_544 ? Ga Se2 Ba 94.49(5) 1_554 7_544 ? Si Se2 Ba 92.92(5) 5_544 7_544 ? Ga Se2 Ba 92.92(5) 5_544 7_544 ? Si Se2 Ba 137.71(5) 1_554 . ? Ga Se2 Ba 137.71(5) 1_554 . ? Si Se2 Ba 90.71(5) 5_544 . ? Ga Se2 Ba 90.71(5) 5_544 . ? Ba Se2 Ba 123.96(4) 7_544 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.95 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.570 _refine_diff_density_min -2.785 _refine_diff_density_rms 0.411