#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202360.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202360 loop_ _publ_author_name 'Wu, Yuandong' 'N\"ather, Christian' 'Bensch, Wolfgang' _publ_section_title ; Cs~4~Ge~2~S~8~ ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i137 _journal_page_last i138 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'Cs4 Ge2 S8' _chemical_formula_moiety 'Cs4 Ge2 S8' _chemical_formula_sum 'Cs4 Ge2 S8' _chemical_formula_weight 933.42 _chemical_name_systematic ; Tetracaesium digermanium octasulfide ; _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 122.430(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.721(2) _cell_length_b 7.3640(10) _cell_length_c 9.8200(10) _cell_measurement_reflns_used 108 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 19 _cell_measurement_theta_min 14 _cell_volume 898.5(2) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1990)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1990)' _computing_molecular_graphics 'XP in SHELXTL (Bruker, 1998)' _computing_publication_material 'CIFTAB in SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Phillips PW1100 four-circle' _diffrn_measurement_method \w/\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 0.025 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4059 _diffrn_reflns_theta_full 30.03 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_min 2.46 _diffrn_standards_decay_% none _diffrn_standards_interval_time 120 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 12.228 _exptl_absorpt_correction_T_max 0.480 _exptl_absorpt_correction_T_min 0.322 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE; Stoe & Cie, 1998)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 3.450 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description polyhedron _exptl_crystal_F_000 824 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.92 _refine_diff_density_min -0.87 _refine_ls_extinction_coef 0.00151(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 41 _refine_ls_number_reflns 1417 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.028 _refine_ls_R_factor_gt 0.021 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0206P)^2^+2.6105P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.050 _refine_ls_wR_factor_ref 0.051 _reflns_number_gt 1244 _reflns_number_total 1417 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6330.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/m' _cod_database_code 2202360 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cs1 0.16369(2) 0.0000 0.28823(4) 0.03154(9) Uani d S 1 . . Cs Cs2 0.41590(2) 0.0000 0.15007(3) 0.03007(9) Uani d S 1 . . Cs Ge1 0.15583(4) 0.0000 0.70131(5) 0.02168(10) Uani d S 1 . . Ge S1 0.31312(10) 0.0000 0.73583(14) 0.0323(2) Uani d S 1 . . S S2 0.12490(9) 0.0000 0.89111(13) 0.0283(2) Uani d S 1 . . S S3 0.07944(6) 0.24278(10) 0.53104(9) 0.02617(15) Uani d . 1 . . 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cs1 0.03182(15) 0.03397(15) 0.03260(15) 0.000 0.01977(13) 0.000 Cs2 0.02964(15) 0.03338(14) 0.02519(14) 0.000 0.01336(11) 0.000 Ge1 0.0223(2) 0.02382(19) 0.0194(2) 0.000 0.01150(17) 0.000 S1 0.0250(5) 0.0424(6) 0.0321(6) 0.000 0.0170(5) 0.000 S2 0.0293(5) 0.0352(5) 0.0237(5) 0.000 0.0165(4) 0.000 S3 0.0263(4) 0.0251(3) 0.0265(3) -0.0016(3) 0.0138(3) 0.0019(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cs1 S2 5_556 3.6229(13) y Cs1 S2 1_554 3.6256(12) y Cs1 S3 . 3.6866(8) y Cs1 S3 6 3.6866(8) y Cs1 S1 . 3.7132(13) y Cs1 S1 7_556 3.7170(5) y Cs1 S1 7_546 3.7170(5) y Cs1 S3 7_556 3.7200(9) y Cs1 S3 4_546 3.7200(9) y Cs1 Ge1 . 4.1196(6) n Cs1 Cs2 . 4.5857(7) n Cs1 Cs2 3_445 4.8369(6) n Cs2 S1 1_554 3.4979(13) y Cs2 S1 5_656 3.5177(13) y Cs2 S2 1_554 3.6241(14) y Cs2 S3 7_556 3.6289(8) y Cs2 S3 4_546 3.6289(8) y Cs2 S3 8 3.7040(9) y Cs2 S3 3_545 3.7040(9) y Cs2 S2 7_546 3.7176(5) y Cs2 S2 7_556 3.7176(5) y Cs2 Ge1 1_554 3.9977(9) n Cs2 Ge1 7_556 4.2959(5) n Cs2 Ge1 7_546 4.2959(5) n Ge1 S2 . 2.1428(11) y Ge1 S1 . 2.1528(12) y Ge1 S3 6 2.2891(8) y Ge1 S3 . 2.2891(8) y Ge1 Cs2 1_556 3.9977(9) n Ge1 Cs2 7_556 4.2959(5) n Ge1 Cs2 7_546 4.2959(5) n S1 Cs2 1_556 3.4979(13) n S1 Cs2 5_656 3.5177(13) n S1 Cs1 7_556 3.7170(5) n S1 Cs1 7_546 3.7170(5) n S2 Cs1 5_556 3.6229(13) n S2 Cs2 1_556 3.6241(14) n S2 Cs1 1_556 3.6256(12) n S2 Cs2 7_546 3.7176(5) n S2 Cs2 7_556 3.7176(5) n S3 S3 2_556 2.0767(15) y S3 Cs2 7_556 3.6289(8) n S3 Cs2 3_455 3.7040(9) n S3 Cs1 7_556 3.7200(9) n 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S2 Cs1 S2 5_556 1_554 90.56(3) n S2 Cs1 S3 5_556 . 66.48(2) n S2 Cs1 S3 1_554 . 141.450(18) n S2 Cs1 S3 5_556 6 66.48(2) n S2 Cs1 S3 1_554 6 141.450(18) n S3 Cs1 S3 . 6 58.02(2) n S2 Cs1 S1 5_556 . 111.80(3) n S2 Cs1 S1 1_554 . 157.64(3) n S3 Cs1 S1 . . 54.95(2) n S3 Cs1 S1 6 . 54.95(2) n S2 Cs1 S1 5_556 7_556 95.326(18) n S2 Cs1 S1 1_554 7_556 84.174(18) n S3 Cs1 S1 . 7_556 68.59(2) n S3 Cs1 S1 6 7_556 126.56(2) n S1 Cs1 S1 . 7_556 93.379(19) n S2 Cs1 S1 5_556 7_546 95.326(18) n S2 Cs1 S1 1_554 7_546 84.174(18) n S3 Cs1 S1 . 7_546 126.56(2) n S3 Cs1 S1 6 7_546 68.59(2) n S1 Cs1 S1 . 7_546 93.379(19) n S1 Cs1 S1 7_556 7_546 164.27(4) n S2 Cs1 S3 5_556 7_556 149.192(13) n S2 Cs1 S3 1_554 7_556 92.67(2) n S3 Cs1 S3 . 7_556 93.036(19) n S3 Cs1 S3 6 7_556 123.149(15) n S1 Cs1 S3 . 7_556 68.28(2) n S1 Cs1 S3 7_556 7_556 54.65(2) n S1 Cs1 S3 7_546 7_556 115.48(2) n S2 Cs1 S3 5_556 4_546 149.192(13) n S2 Cs1 S3 1_554 4_546 92.67(2) n S3 Cs1 S3 . 4_546 123.149(15) n S3 Cs1 S3 6 4_546 93.036(19) n S1 Cs1 S3 . 4_546 68.28(2) n S1 Cs1 S3 7_556 4_546 115.48(2) n S1 Cs1 S3 7_546 4_546 54.65(2) n S3 Cs1 S3 7_556 4_546 61.22(3) n S2 Cs1 Ge1 5_556 . 80.44(2) n S2 Cs1 Ge1 1_554 . 171.00(2) n S3 Cs1 Ge1 . . 33.523(13) n S3 Cs1 Ge1 6 . 33.523(13) n S1 Cs1 Ge1 . . 31.359(19) n S1 Cs1 Ge1 7_556 . 96.582(18) n S1 Cs1 Ge1 7_546 . 96.582(18) n S3 Cs1 Ge1 7_556 . 95.069(17) n S3 Cs1 Ge1 4_546 . 95.069(17) n S2 Cs1 Cs2 5_556 . 141.31(2) n S2 Cs1 Cs2 1_554 . 50.75(2) n S3 Cs1 Cs2 . . 142.933(13) n S3 Cs1 Cs2 6 . 142.933(13) n S1 Cs1 Cs2 . . 106.89(2) n S1 Cs1 Cs2 7_556 . 82.222(18) n S1 Cs1 Cs2 7_546 . 82.222(18) n S3 Cs1 Cs2 7_556 . 50.508(14) n S3 Cs1 Cs2 4_546 . 50.508(14) n Ge1 Cs1 Cs2 . . 138.250(13) n S2 Cs1 Cs2 5_556 3_445 49.631(7) n S2 Cs1 Cs2 1_554 3_445 92.188(15) n S3 Cs1 Cs2 . 3_445 94.928(16) n S3 Cs1 Cs2 6 3_445 49.277(14) n S1 Cs1 Cs2 . 3_445 102.179(15) n S1 Cs1 Cs2 7_556 3_445 144.82(2) n S1 Cs1 Cs2 7_546 3_445 46.311(19) n S3 Cs1 Cs2 7_556 3_445 160.418(13) n S3 Cs1 Cs2 4_546 3_445 99.610(16) n Ge1 Cs1 Cs2 . 3_445 82.011(10) n Cs2 Cs1 Cs2 . 3_445 121.699(8) n S1 Cs2 S1 1_554 5_656 94.58(3) n S1 Cs2 S2 1_554 1_554 64.70(3) n S1 Cs2 S2 5_656 1_554 159.28(3) n S1 Cs2 S3 1_554 7_556 143.108(16) n S1 Cs2 S3 5_656 7_556 103.40(2) n S2 Cs2 S3 1_554 7_556 94.23(2) n S1 Cs2 S3 1_554 4_546 143.108(16) n S1 Cs2 S3 5_656 4_546 103.40(2) n S2 Cs2 S3 1_554 4_546 94.23(2) n S3 Cs2 S3 7_556 4_546 62.93(2) n S1 Cs2 S3 1_554 8 144.695(16) n S1 Cs2 S3 5_656 8 70.52(2) n S2 Cs2 S3 1_554 8 126.31(2) n S3 Cs2 S3 7_556 8 32.88(2) n S3 Cs2 S3 4_546 8 72.19(2) n S1 Cs2 S3 1_554 3_545 144.695(16) n S1 Cs2 S3 5_656 3_545 70.52(2) n S2 Cs2 S3 1_554 3_545 126.31(2) n S3 Cs2 S3 7_556 3_545 72.19(2) n S3 Cs2 S3 4_546 3_545 32.88(2) n S3 Cs2 S3 8 3_545 61.51(3) n S1 Cs2 S2 1_554 7_546 85.963(18) n S1 Cs2 S2 5_656 7_546 97.128(18) n S2 Cs2 S2 1_554 7_546 82.095(18) n S3 Cs2 S2 7_556 7_546 122.55(2) n S3 Cs2 S2 4_546 7_546 60.27(2) n S3 Cs2 S2 8 7_546 126.58(2) n S3 Cs2 S2 3_545 7_546 65.35(2) n S1 Cs2 S2 1_554 7_556 85.963(18) n S1 Cs2 S2 5_656 7_556 97.128(18) n S2 Cs2 S2 1_554 7_556 82.095(18) n S3 Cs2 S2 7_556 7_556 60.27(2) n S3 Cs2 S2 4_546 7_556 122.55(2) n S3 Cs2 S2 8 7_556 65.35(2) n S3 Cs2 S2 3_545 7_556 126.58(2) n S2 Cs2 S2 7_546 7_556 164.12(4) n S1 Cs2 Ge1 1_554 1_554 32.52(2) n S1 Cs2 Ge1 5_656 1_554 127.10(2) n S2 Cs2 Ge1 1_554 1_554 32.183(19) n S3 Cs2 Ge1 7_556 1_554 120.997(16) n S3 Cs2 Ge1 4_546 1_554 120.997(16) n S3 Cs2 Ge1 8 1_554 146.395(13) n S3 Cs2 Ge1 3_545 1_554 146.395(13) n S2 Cs2 Ge1 7_546 1_554 82.920(18) n S2 Cs2 Ge1 7_556 1_554 82.920(18) n S1 Cs2 Ge1 1_554 7_556 111.300(11) n S1 Cs2 Ge1 5_656 7_556 109.581(12) n S2 Cs2 Ge1 1_554 7_556 79.919(12) n S3 Cs2 Ge1 7_556 7_556 32.198(13) n S3 Cs2 Ge1 4_546 7_556 92.783(16) n S3 Cs2 Ge1 8 7_556 50.477(14) n S3 Cs2 Ge1 3_545 7_556 103.899(16) n S2 Cs2 Ge1 7_546 7_556 146.205(19) n S2 Cs2 Ge1 7_556 7_556 29.921(17) n Ge1 Cs2 Ge1 1_554 7_556 96.311(9) n S1 Cs2 Ge1 1_554 7_546 111.300(11) n S1 Cs2 Ge1 5_656 7_546 109.581(12) n S2 Cs2 Ge1 1_554 7_546 79.919(12) n S3 Cs2 Ge1 7_556 7_546 92.783(16) n S3 Cs2 Ge1 4_546 7_546 32.198(13) n S3 Cs2 Ge1 8 7_546 103.899(16) n S3 Cs2 Ge1 3_545 7_546 50.477(14) n S2 Cs2 Ge1 7_546 7_546 29.921(17) n S2 Cs2 Ge1 7_556 7_546 146.205(19) n Ge1 Cs2 Ge1 1_554 7_546 96.311(9) n Ge1 Cs2 Ge1 7_556 7_546 117.983(14) n S2 Ge1 S1 . . 125.13(5) y S2 Ge1 S3 . 6 112.65(3) y S1 Ge1 S3 . 6 100.40(3) y S2 Ge1 S3 . . 112.65(3) y S1 Ge1 S3 . . 100.40(3) y S3 Ge1 S3 6 . 102.71(4) y S2 Ge1 Cs2 . 1_556 64.26(4) n S1 Ge1 Cs2 . 1_556 60.86(3) n S3 Ge1 Cs2 6 1_556 127.60(2) n S3 Ge1 Cs2 . 1_556 127.60(2) n S2 Ge1 Cs1 . . 171.03(4) n S1 Ge1 Cs1 . . 63.85(4) n S3 Ge1 Cs1 6 . 62.80(2) n S3 Ge1 Cs1 . . 62.80(2) n Cs2 Ge1 Cs1 1_556 . 124.710(15) n S2 Ge1 Cs2 . 7_556 59.926(8) n S1 Ge1 Cs2 . 7_556 112.711(15) n S3 Ge1 Cs2 6 7_556 143.47(3) n S3 Ge1 Cs2 . 7_556 57.64(2) n Cs2 Ge1 Cs2 1_556 7_556 83.689(9) n Cs1 Ge1 Cs2 . 7_556 118.446(7) n S2 Ge1 Cs2 . 7_546 59.927(8) n S1 Ge1 Cs2 . 7_546 112.711(15) n S3 Ge1 Cs2 6 7_546 57.64(2) n S3 Ge1 Cs2 . 7_546 143.47(3) n Cs2 Ge1 Cs2 1_556 7_546 83.689(9) n Cs1 Ge1 Cs2 . 7_546 118.446(7) n Cs2 Ge1 Cs2 7_556 7_546 117.983(14) n Ge1 S1 Cs2 . 1_556 86.62(4) n Ge1 S1 Cs2 . 5_656 172.04(5) n Cs2 S1 Cs2 1_556 5_656 85.42(3) n Ge1 S1 Cs1 . . 84.79(4) n Cs2 S1 Cs1 1_556 . 171.41(4) n Cs2 S1 Cs1 5_656 . 103.17(3) n Ge1 S1 Cs1 . 7_556 96.758(18) n Cs2 S1 Cs1 1_556 7_556 94.400(19) n Cs2 S1 Cs1 5_656 7_556 83.865(18) n Cs1 S1 Cs1 . 7_556 86.621(19) n Ge1 S1 Cs1 . 7_546 96.758(18) n Cs2 S1 Cs1 1_556 7_546 94.400(19) n Cs2 S1 Cs1 5_656 7_546 83.865(18) n Cs1 S1 Cs1 . 7_546 86.621(19) n Cs1 S1 Cs1 7_556 7_546 164.27(4) n Ge1 S2 Cs1 . 5_556 108.54(4) n Ge1 S2 Cs2 . 1_556 83.55(4) n Cs1 S2 Cs2 5_556 1_556 167.91(3) n Ge1 S2 Cs1 . 1_556 162.03(5) n Cs1 S2 Cs1 5_556 1_556 89.44(3) n Cs2 S2 Cs1 1_556 1_556 78.47(3) n Ge1 S2 Cs2 . 7_546 90.153(18) n Cs1 S2 Cs2 5_556 7_546 82.427(18) n Cs2 S2 Cs2 1_556 7_546 97.905(18) n Cs1 S2 Cs2 1_556 7_546 92.297(17) n Ge1 S2 Cs2 . 7_556 90.153(18) n Cs1 S2 Cs2 5_556 7_556 82.427(18) n Cs2 S2 Cs2 1_556 7_556 97.905(18) n Cs1 S2 Cs2 1_556 7_556 92.297(17) n Cs2 S2 Cs2 7_546 7_556 164.12(4) n S3 S3 Ge1 2_556 . 104.43(3) n S3 S3 Cs2 2_556 7_556 75.55(4) n Ge1 S3 Cs2 . 7_556 90.16(3) n S3 S3 Cs1 2_556 . 121.78(4) n Ge1 S3 Cs1 . . 83.67(2) n Cs2 S3 Cs1 7_556 . 162.56(2) n S3 S3 Cs2 2_556 3_455 71.57(4) n Ge1 S3 Cs2 . 3_455 159.35(3) n Cs2 S3 Cs2 7_556 3_455 107.81(2) n Cs1 S3 Cs2 . 3_455 81.758(18) n S3 S3 Cs1 2_556 7_556 146.79(2) n Ge1 S3 Cs1 . 7_556 94.23(3) n Cs2 S3 Cs1 7_556 7_556 77.205(18) n Cs1 S3 Cs1 . 7_556 86.964(19) n Cs2 S3 Cs1 3_455 7_556 99.51(2) n _cod_database_fobs_code 2202360 _journal_paper_doi 10.1107/S1600536803018695