#------------------------------------------------------------------------------ #$Date: 2015-06-04 13:59:15 +0300 (Thu, 04 Jun 2015) $ #$Revision: 137924 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/34/31/4343169.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4343169 loop_ _publ_author_name 'Yamamoto, Ayako' 'Hashizume, Daisuke' 'Bahramy, Mohammad Saeed' 'Tokura, Yoshinori' _publ_section_title ; Coexistence of Monochalocogen and Dichalocogen Ions in BiSe2 and BiS2 Crystals Prepared at High Pressure. ; _journal_issue 8 _journal_name_full 'Inorganic chemistry' _journal_page_first 4114 _journal_page_last 4119 _journal_paper_doi 10.1021/acs.inorgchem.5b00349 _journal_volume 54 _journal_year 2015 _chemical_formula_moiety 'Bi S0.91 Se1.09' _chemical_formula_sum 'Bi S0.91 Se1.09' _chemical_formula_weight 324.10 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_Hall '-C 2y' _space_group_name_H-M_alt 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 127.401(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 16.3670(12) _cell_length_b 4.1040(4) _cell_length_c 11.6772(13) _cell_measurement_reflns_used 5918 _cell_measurement_temperature 300 _cell_measurement_theta_max 31.028 _cell_measurement_theta_min 2.195 _cell_volume 623.10(11) _computing_cell_refinement HKL2000 _computing_data_collection CrystalClear _computing_data_reduction HKL2000 _computing_molecular_graphics 'ORTEP-3 for Windows' _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution SIR2004 _diffrn_ambient_temperature 300 _diffrn_detector_area_resol_mean 7.31 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Rigaku AFC-8 with Saturn70 CCD' _diffrn_measurement_method \w-scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_unetI/netI 0.0406 _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5918 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.028 _diffrn_reflns_theta_min 2.195 _exptl_absorpt_coefficient_mu 69.578 _exptl_absorpt_correction_T_max 0.02832 _exptl_absorpt_correction_T_min 0.00686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; MULABS ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 6.910 _exptl_crystal_description needle _exptl_crystal_F_000 1077 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.012 _exptl_crystal_size_min 0.009 _refine_diff_density_max 2.641 _refine_diff_density_min -1.293 _refine_diff_density_rms 0.365 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 41 _refine_ls_number_reflns 1081 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0417 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+3.9359P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1040 _refine_ls_wR_factor_ref 0.1130 _reflns_Friedel_coverage 0.000 _reflns_number_gt 813 _reflns_number_total 1081 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ic5b00349_si_002.cif _cod_data_source_block BiSeS _cod_database_code 4343169 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.028 _shelx_estimated_absorpt_t_max 0.573 _shelxl_version_number 2013-3 _shelx_res_file ; TITL 130617_yamamoto_BiSe CELL 0.71073 16.3670 4.1040 11.6772 90 127.4012 90 ZERR 8 0.0012 0.0004 0.0013 0 0.0041 0 LATT 7 SYMM -x, y, -z SFAC Bi Se S UNIT 8 8.7 7.3 L.S. 10 FMAP 2 PLAN 10 TEMP 27 SIZE 0.180 0.012 0.009 REM needle, black EADP Se1 S1 EADP Se2 S2 EADP Se3 S3 EADP Se4 S4 EXYZ Se1 S1 EXYZ Se2 S2 EXYZ Se3 S3 EXYZ Se4 S4 BOND CONF ACTA WGHT 0.056200 3.935900 FVAR 0.45403 0.82415 0.47889 0.32791 0.54517 MOLE 1 BI1 1 0.701414 0.000000 0.098501 10.50000 0.05394 0.04831 = 0.05611 0.00000 0.03896 0.00000 SE1 2 0.534984 0.500000 -0.061483 20.50000 0.04341 0.05349 = 0.05342 0.00000 0.03079 0.00000 SE2 2 0.653806 0.000000 -0.164935 30.50000 0.04393 0.04155 = 0.04869 0.00000 0.03050 0.00000 S1 3 0.534984 0.500000 -0.061483 -20.50000 0.04341 0.05349 = 0.05342 0.00000 0.03079 0.00000 S2 3 0.653806 0.000000 -0.164935 -30.50000 0.04393 0.04155 = 0.04869 0.00000 0.03050 0.00000 MOLE 2 BI2 1 0.389511 0.000000 -0.391054 10.50000 0.04595 0.05280 = 0.05669 0.00000 0.03220 0.00000 SE3 2 0.212199 0.000000 -0.654804 40.50000 0.04213 0.04541 = 0.04731 0.00000 0.02860 0.00000 SE4 2 0.417441 -0.500000 -0.541563 50.50000 0.04350 0.04841 = 0.04926 0.00000 0.03164 0.00000 S3 3 0.212199 0.000000 -0.654804 -40.50000 0.04213 0.04541 = 0.04731 0.00000 0.02860 0.00000 S4 3 0.417441 -0.500000 -0.541563 -50.50000 0.04350 0.04841 = 0.04926 0.00000 0.03164 0.00000 HKLF 4 REM 130617_yamamoto_BiSe REM R1 = 0.0417 for 813 Fo > 4sig(Fo) and 0.0570 for all 1081 data REM 41 parameters refined using 0 restraints END WGHT 0.0562 3.9203 REM Highest difference peak 2.641, deepest hole -1.293, 1-sigma level 0.365 Q1 1 0.4372 0.0000 -0.2779 10.50000 0.05 2.64 Q2 1 0.6528 0.0000 0.0054 10.50000 0.05 2.64 Q3 1 0.7459 0.0000 0.2027 10.50000 0.05 2.41 Q4 1 0.3360 0.0000 -0.4859 10.50000 0.05 2.16 Q5 1 0.2524 0.0000 -0.5627 10.50000 0.05 1.70 Q6 1 0.3768 -0.5000 -0.6353 10.50000 0.05 1.69 Q7 1 0.6994 0.0000 -0.0617 10.50000 0.05 1.59 Q8 1 0.4875 0.5000 -0.1661 10.50000 0.05 1.51 Q9 1 0.5518 0.5000 -0.2225 10.50000 0.05 1.29 Q10 1 0.1738 0.0000 -0.7542 10.50000 0.05 1.26 ; _shelx_res_checksum 20266 _shelx_hkl_file ; 23 -1 -8 -18.66 30.64 -23 1 9 120.45 63.45 23 -1 -10 6.69 47.89 23 -1 -11 279.93 81.23 -23 1 11 246.99 39.72 -23 -1 11 240.82 52.59 23 1 -12 52.26 40.16 -23 1 12 9.31 27.64 22 0 -6 94.21 33.27 -22 0 7 4.36 24.23 22 0 -7 -0.79 31.48 -22 0 8 193.31 72.91 -22 0 8 164.02 36.99 22 0 -8 161.29 48.68 -22 0 9 62.03 54.35 22 0 -10 1432.03 140.58 -22 0 10 1014.44 90.68 22 0 -11 58.72 49.79 22 0 -12 258.23 72.91 -22 0 12 204.72 47.37 -22 0 13 35.92 34.51 -22 0 14 408.60 73.62 -22 -2 8 92.83 36.09 22 2 -8 162.24 51.22 -22 2 8 74.51 33.47 22 -2 -9 -28.88 45.51 22 2 -9 43.13 39.75 -22 2 9 26.11 49.48 -22 2 9 13.70 28.02 -22 -2 9 31.06 32.03 22 -2 -10 761.29 128.03 22 2 -10 503.21 75.26 22 2 -10 472.81 74.47 -22 -2 10 544.00 83.97 -22 2 10 496.11 83.04 22 2 -11 99.55 41.36 -22 2 11 102.49 52.30 21 1 -4 30.32 52.84 21 -1 -4 8.44 29.42 -21 1 4 4.34 40.80 -21 -1 4 8.79 48.12 -21 1 4 -25.30 34.01 21 -1 -4 6.88 45.51 -21 1 5 219.42 67.64 -21 -1 5 194.48 58.05 -21 -1 5 135.29 39.49 21 -1 -5 183.39 39.62 21 1 -5 221.30 69.02 -21 1 6 58.62 50.11 21 -1 -6 102.09 49.63 -21 -1 7 1781.68 141.92 -21 -1 7 1705.17 147.04 21 -1 -7 1905.67 138.52 21 1 -7 1923.41 136.25 -21 1 7 1978.95 178.96 -21 1 8 168.70 83.70 21 -1 -8 129.05 53.40 -21 1 8 113.47 34.46 21 1 -8 228.57 81.97 21 1 -8 99.08 45.18 -21 -1 8 110.40 49.57 21 -1 -9 76.04 46.59 21 1 -9 40.08 32.42 21 1 -9 40.88 56.58 -21 1 9 -7.16 49.81 -21 -1 9 34.29 39.05 -21 1 10 44.86 60.23 21 1 -10 49.63 46.79 -21 -1 10 18.30 39.25 -21 1 10 93.29 32.27 21 1 -10 74.75 44.23 21 -1 -10 36.14 50.75 -21 -1 11 1583.89 131.00 21 -1 -11 1916.24 193.46 -21 1 11 1059.68 98.85 21 1 -11 1423.81 146.58 -21 1 11 1293.47 100.71 21 1 -11 1328.02 105.47 21 1 -12 132.18 58.53 -21 1 12 154.04 46.63 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2 2713.02 136.32 9 -1 2 2643.09 213.25 9 -1 2 3039.99 283.52 9 1 3 1534.12 188.97 -9 1 -3 1545.51 176.52 -9 -1 -3 1743.80 228.44 -9 -1 -3 1688.18 177.17 9 -1 3 1821.80 225.24 9 1 4 977.73 119.09 9 1 4 1534.67 176.77 9 1 4 1381.69 145.37 -9 1 -4 1341.29 172.85 -9 1 -4 976.48 165.21 -9 -1 -4 1314.83 196.36 -9 -1 -4 859.75 127.81 9 -1 4 1234.38 187.74 9 -1 4 1018.44 142.37 9 1 5 137.05 50.77 9 1 5 73.77 82.45 9 1 5 48.19 80.02 -9 1 -5 57.27 77.87 -9 1 -5 137.97 73.12 -9 -1 -5 81.34 73.02 9 -1 5 123.91 59.87 9 1 6 1410.10 144.13 9 1 6 2007.91 186.40 -9 1 -6 2170.27 211.09 -9 -1 -6 2025.54 251.89 9 -1 6 1891.20 240.59 9 1 7 81.44 57.89 -9 1 -7 49.24 61.11 -9 -1 -7 96.78 61.25 9 -1 7 74.74 59.45 9 3 0 1176.08 131.82 -9 3 0 1295.60 145.04 -9 3 0 1161.93 127.14 -9 -3 0 1247.30 151.20 -9 -3 0 1089.31 143.13 -9 -3 0 1273.36 159.43 9 -3 0 1074.22 189.50 9 -3 0 1301.55 162.22 9 3 1 -14.79 60.27 -9 3 -1 56.35 64.17 -9 -3 -1 21.91 59.03 -9 -3 -1 23.17 66.56 -9 -3 -1 28.21 53.51 9 -3 1 21.03 56.54 9 -3 1 36.36 60.21 9 -3 1 71.00 51.43 9 3 2 1070.88 119.56 -9 3 -2 928.16 130.87 -9 -3 -2 984.50 160.70 -9 -3 -2 895.34 162.13 -9 -3 -2 973.43 112.26 9 -3 2 862.31 118.86 9 -3 2 875.28 140.15 9 3 3 388.72 88.87 9 3 3 418.85 81.19 -9 3 -3 544.32 90.68 -9 3 -3 493.80 94.88 -9 -3 -3 585.98 126.57 9 3 4 355.34 61.68 9 3 4 486.83 87.18 9 3 4 316.74 81.36 -9 3 -4 515.85 108.73 -9 -3 -4 272.42 108.42 9 3 5 40.84 45.90 9 3 5 54.39 60.45 9 3 5 -9.98 44.91 -9 3 -5 -12.41 59.81 -9 -3 -5 -50.33 61.21 9 -3 5 81.44 63.33 9 3 6 227.50 57.83 9 3 6 524.80 89.44 -9 3 -6 511.67 98.47 -9 -3 -6 421.96 105.05 9 -3 6 365.15 86.35 -9 5 0 23.15 66.63 -9 -5 0 24.32 46.62 -9 5 -1 29.05 54.89 10 0 0 7125.27 364.31 10 0 0 8036.33 571.72 -10 0 0 7337.68 352.59 -10 0 0 7927.91 544.05 -10 0 0 7033.42 465.86 10 0 1 2531.86 208.39 10 0 1 2556.88 262.56 -10 0 -1 2416.66 138.47 -10 0 -1 2524.50 246.92 -10 0 -1 2256.52 259.41 10 0 2 3140.15 231.54 10 0 2 3900.79 364.61 -10 0 -2 3291.09 251.28 -10 0 -2 3794.76 337.20 -10 0 -2 3808.79 289.97 10 0 3 35.99 40.60 10 0 3 33.99 85.12 -10 0 -3 63.67 90.75 -10 0 -3 9.00 52.07 -10 0 -3 84.40 68.82 10 0 4 186.27 53.27 10 0 4 235.70 91.33 10 0 4 410.48 96.40 -10 0 -4 496.79 122.86 -10 0 -4 206.83 70.54 10 0 5 26.49 65.70 10 0 5 9.87 62.92 -10 0 -5 18.09 68.29 10 0 6 269.93 88.86 -10 0 -6 394.77 110.25 10 0 7 -30.73 34.67 -10 0 -7 4.81 34.63 10 2 0 3281.74 155.93 10 2 0 3891.65 285.70 -10 2 0 4091.00 317.25 -10 2 0 4148.01 276.68 -10 -2 0 4008.38 276.56 -10 -2 0 3645.80 315.90 -10 -2 0 3898.03 302.10 10 -2 0 3926.03 329.91 10 -2 0 3163.67 290.95 10 2 1 1443.14 148.46 -10 2 -1 1262.24 176.05 -10 2 -1 1393.05 140.16 -10 -2 -1 1196.77 164.98 -10 -2 -1 1235.91 166.68 -10 -2 -1 1395.20 166.51 10 -2 1 1450.98 183.10 10 -2 1 1241.72 182.72 10 2 2 1748.90 193.08 -10 2 -2 2098.67 227.99 -10 2 -2 1751.60 177.81 -10 -2 -2 1892.68 205.25 -10 -2 -2 1911.87 227.44 -10 -2 -2 2062.08 213.21 10 -2 2 1659.00 177.82 10 -2 2 1668.68 203.31 10 2 3 -0.88 57.51 -10 2 -3 80.89 58.47 -10 -2 -3 44.50 60.32 -10 -2 -3 22.39 57.14 10 -2 3 -95.80 63.14 10 -2 3 -44.03 58.14 10 2 4 63.77 54.11 10 2 4 243.45 80.97 10 2 4 163.50 61.12 -10 2 -4 140.34 79.82 -10 -2 -4 155.97 92.95 10 -2 4 168.61 75.40 10 -2 4 96.43 72.46 10 2 5 -1.61 42.10 10 2 5 40.34 51.13 10 2 5 95.70 63.50 -10 2 -5 15.39 56.07 10 -2 5 89.68 56.33 10 2 6 101.32 45.93 -10 2 -6 202.31 74.69 10 -2 6 169.73 67.83 10 4 0 683.23 83.29 -10 4 0 696.46 108.59 -10 -4 0 779.17 125.57 10 -4 0 754.36 142.17 10 -4 0 584.89 84.06 10 4 1 172.46 54.55 -10 4 -1 161.62 66.52 -10 -4 -1 141.66 68.07 -10 4 -2 275.41 67.79 -10 4 -2 286.00 88.33 10 -4 2 288.57 70.54 10 4 3 -6.54 37.93 -10 4 -3 33.31 55.46 10 -4 3 14.18 27.40 11 1 0 384.59 49.98 11 1 0 253.78 85.10 -11 1 0 286.56 41.60 -11 1 0 587.94 115.85 -11 1 0 445.59 83.50 -11 -1 0 290.29 62.40 -11 -1 0 534.02 112.34 -11 -1 0 234.58 58.63 -11 -1 0 342.05 91.38 11 -1 0 137.58 50.30 11 -1 0 375.25 84.30 11 -1 0 452.37 111.37 11 1 1 897.00 75.25 11 1 1 962.49 147.14 -11 1 -1 1110.26 150.41 -11 1 -1 909.51 132.24 -11 -1 -1 1030.31 102.27 -11 -1 -1 1105.22 166.46 -11 -1 -1 1068.32 117.91 11 -1 1 1081.43 114.40 11 -1 1 968.89 178.31 11 1 2 140.35 84.31 -11 1 -2 116.56 75.05 -11 1 -2 99.13 90.23 -11 -1 -2 133.49 52.01 -11 -1 -2 143.00 104.30 -11 -1 -2 58.52 50.56 -11 -1 -2 149.02 79.82 11 -1 2 160.40 48.45 11 -1 2 215.61 91.80 11 1 3 738.07 85.76 11 1 3 1068.61 146.76 -11 1 -3 960.42 142.86 -11 1 -3 577.43 124.50 -11 1 -3 934.57 127.42 -11 -1 -3 626.66 165.21 -11 -1 -3 947.60 126.88 11 -1 3 982.52 169.55 11 1 4 156.28 42.03 11 1 4 89.40 73.88 11 1 4 193.01 74.62 -11 1 -4 187.20 78.82 -11 1 -4 53.57 65.49 -11 -1 -4 159.37 92.54 11 -1 4 116.46 71.74 11 -1 4 145.91 63.35 11 1 5 28.77 32.20 11 1 5 -21.89 31.12 11 1 5 -15.17 32.82 -11 1 -5 -36.29 30.81 -11 -1 -5 -61.20 31.41 11 -1 5 4.78 32.94 11 1 6 137.46 63.99 -11 1 -6 125.10 65.90 -11 -1 -6 135.77 77.37 11 -1 6 121.81 64.50 11 -1 6 116.79 67.10 11 3 0 223.58 61.61 -11 3 0 96.62 70.80 -11 -3 0 123.14 67.33 -11 -3 0 185.87 69.63 -11 -3 0 211.31 70.05 11 -3 0 114.17 70.68 11 3 1 326.64 79.81 -11 3 -1 292.31 79.99 -11 -3 -1 231.98 92.05 -11 -3 -1 211.83 100.16 -11 -3 -1 357.46 82.10 11 -3 1 395.09 97.10 11 3 2 27.45 47.74 -11 3 -2 6.08 57.67 -11 -3 -2 9.42 54.82 -11 -3 -2 79.58 86.11 -11 -3 -2 64.31 65.05 11 -3 2 43.92 53.13 11 3 3 257.23 68.42 11 3 3 270.87 73.91 11 3 3 176.87 62.81 -11 3 -3 179.93 71.29 -11 3 -3 99.83 67.76 11 -3 3 178.22 72.70 11 3 4 35.76 30.58 11 3 4 44.67 47.41 11 3 4 18.48 46.52 11 3 5 -6.11 35.02 11 3 5 4.81 34.52 -11 3 -5 -1.41 34.23 -12 0 0 2764.22 165.35 -12 0 0 2886.02 232.10 12 0 1 2300.93 134.45 12 0 1 2715.27 281.88 -12 0 -1 2499.44 226.51 -12 0 -1 2608.33 267.15 -12 0 -1 2939.16 218.43 12 0 2 6.77 37.36 12 0 2 -13.12 37.16 12 0 2 -86.36 35.97 -12 0 -2 -72.38 36.07 -12 0 -2 -61.59 37.88 12 0 3 1972.32 208.93 -12 0 -3 1645.35 195.32 -12 0 -3 1332.04 124.12 -12 0 -3 1608.62 193.89 12 0 4 1190.73 167.19 12 0 4 1012.30 117.94 -12 0 -4 1389.08 150.16 -12 0 -4 476.24 94.46 12 0 5 89.63 60.71 12 0 5 127.05 64.36 -12 0 -5 136.21 75.84 12 2 0 1505.29 155.53 -12 2 0 1624.55 181.70 -12 2 0 1427.62 170.02 -12 -2 0 1742.63 161.54 -12 -2 0 1429.34 192.15 -12 -2 0 1624.85 154.71 12 -2 0 1751.56 193.18 12 -2 0 1322.75 166.09 -12 2 -1 1691.29 200.28 -12 2 -1 1632.12 173.78 -12 -2 -1 1234.72 179.32 -12 -2 -1 1343.51 202.81 -12 -2 -1 1130.67 152.09 12 -2 1 1413.76 162.09 12 2 2 -18.63 60.10 -12 2 -2 -19.16 60.37 -12 2 -2 3.35 60.57 -12 -2 -2 29.87 61.64 -12 -2 -2 -153.90 64.26 -12 -2 -2 29.64 59.64 12 -2 2 60.76 66.85 12 2 3 620.11 99.80 -12 2 -3 845.16 120.62 -12 2 -3 889.71 130.17 -12 -2 -3 1087.39 158.18 12 -2 3 1085.94 144.40 12 -2 3 719.90 114.49 12 2 4 420.96 94.86 12 2 4 530.38 99.00 12 2 4 560.41 91.04 -12 2 -4 765.84 102.79 -12 -2 -4 469.92 113.25 12 -2 4 625.72 104.90 12 2 5 47.61 52.84 12 4 0 214.94 64.05 -12 4 0 308.80 76.15 -12 -4 0 386.04 80.50 12 -4 0 292.09 89.51 12 4 1 254.00 62.95 -12 -4 -1 196.75 69.82 12 -4 1 63.69 34.05 13 1 0 1231.55 114.75 13 1 0 1671.98 187.96 -13 1 0 1643.67 170.64 -13 1 0 1678.14 193.53 -13 -1 0 1610.77 131.28 -13 -1 0 1342.62 179.44 -13 -1 0 1587.15 159.99 13 -1 0 1452.74 138.97 13 -1 0 1466.48 183.60 13 1 1 223.96 44.45 13 1 1 340.56 102.31 -13 1 -1 452.59 107.79 -13 1 -1 553.95 106.66 -13 -1 -1 399.02 86.24 -13 -1 -1 423.11 110.89 -13 -1 -1 397.78 77.68 13 -1 1 488.31 69.20 13 -1 1 366.94 86.11 -13 1 -2 76.41 73.45 -13 1 -2 178.31 75.39 -13 -1 -2 83.41 50.32 -13 -1 -2 129.25 91.68 -13 -1 -2 144.04 79.92 13 -1 2 155.47 56.71 13 -1 2 97.65 81.10 13 1 3 73.60 49.31 -13 1 -3 38.69 71.36 -13 1 -3 67.89 60.35 -13 -1 -3 9.00 72.87 -13 -1 -3 52.12 67.32 13 -1 3 46.08 58.15 13 1 4 253.85 90.39 13 1 4 165.51 67.52 13 -1 4 229.12 80.97 13 1 5 -43.57 39.22 -13 1 -5 -9.96 39.16 13 3 0 492.99 75.21 -13 3 0 320.75 73.79 -13 3 0 335.69 80.17 -13 -3 0 463.12 97.30 -13 -3 0 345.95 105.67 -13 -3 0 407.93 91.74 13 -3 0 522.89 89.36 -13 3 -1 96.22 58.94 -13 -3 -1 99.04 41.77 -13 -3 -1 76.57 84.06 13 -3 1 60.86 53.81 13 3 2 61.41 49.43 -13 3 -2 68.78 46.61 -13 3 -2 110.36 66.17 13 3 3 2.68 41.97 13 3 3 49.60 55.53 13 3 3 -5.61 45.56 14 0 0 110.84 49.76 14 0 0 152.00 76.02 -14 0 0 117.69 43.20 -14 0 0 122.81 86.06 -14 0 0 90.46 75.51 14 0 1 974.81 92.82 14 0 1 1277.18 185.05 -14 0 -1 1471.27 173.85 -14 0 -1 1155.09 136.85 14 0 2 -54.26 68.20 -14 0 -2 56.39 68.73 -14 0 -2 -15.14 72.68 14 0 3 103.16 70.76 -14 0 -3 102.17 65.31 -14 0 -3 100.85 74.57 14 0 4 78.88 60.44 -14 0 -4 38.34 64.84 14 2 0 91.77 54.27 -14 2 0 22.20 69.45 -14 2 0 155.65 64.78 -14 -2 0 124.31 44.57 -14 -2 0 167.68 102.56 -14 -2 0 56.22 66.46 14 -2 0 69.54 45.67 14 -2 0 5.78 81.43 14 2 1 590.02 91.41 -14 2 -1 607.84 102.87 -14 2 -1 439.50 89.73 -14 -2 -1 623.91 103.74 -14 -2 -1 567.36 151.79 -14 -2 -1 712.35 99.92 14 -2 1 698.07 99.23 14 -2 1 740.35 131.25 14 2 2 -39.43 55.27 -14 2 -2 -13.82 55.28 -14 -2 -2 3.17 58.42 -14 -2 -2 45.98 55.20 14 -2 2 -43.56 60.03 -14 2 -3 44.18 51.80 -14 2 -3 94.43 47.65 -14 -2 -3 15.62 60.83 14 -2 3 11.47 50.32 15 1 0 141.27 75.87 -15 1 0 16.58 70.03 -15 1 0 18.04 63.65 -15 -1 0 62.80 44.04 -15 -1 0 89.92 81.05 -15 -1 0 -44.79 61.27 15 -1 0 55.33 46.07 15 -1 0 97.42 80.85 -15 1 -1 1758.10 190.15 -15 1 -1 1775.20 175.64 -15 -1 -1 1425.17 93.22 -15 -1 -1 1880.91 208.13 -15 -1 -1 1780.82 190.78 15 -1 1 1427.42 143.91 15 -1 1 1934.11 203.49 15 1 2 42.98 39.81 -15 1 -2 -12.42 54.82 -15 1 -2 -0.44 53.31 -15 -1 -2 27.17 62.51 -15 -1 -2 6.29 49.98 15 1 3 23.83 50.57 15 -1 3 6.73 42.87 15 -1 3 3.19 42.54 15 3 0 4.45 42.52 -15 -3 0 11.87 38.58 -15 -3 0 20.08 43.41 15 -3 0 -2.60 37.37 15 3 1 418.64 70.24 -15 3 -1 315.40 80.68 15 -3 1 358.94 73.39 16 0 0 120.06 40.27 16 0 0 216.24 87.08 -16 0 0 200.71 71.53 -16 0 0 124.65 76.64 16 0 1 -16.07 52.11 -16 0 -1 27.65 56.47 16 0 2 415.03 91.92 -16 0 -2 550.20 108.66 -16 0 -2 597.07 108.24 16 2 0 90.90 59.82 -16 2 0 61.93 57.11 -16 2 0 169.65 53.84 -16 -2 0 28.94 36.45 -16 -2 0 118.45 76.32 -16 -2 0 68.73 58.36 16 -2 0 44.44 49.36 16 -2 0 66.18 71.32 16 2 1 -10.34 59.12 -16 -2 -1 5.50 60.68 -16 -2 -1 -11.34 62.24 -16 -2 -1 -9.72 59.04 16 -2 1 -0.28 60.73 16 -2 1 -17.39 63.72 -17 1 0 36.23 54.52 -17 -1 0 -25.45 68.01 -17 -1 0 19.33 55.18 17 -1 0 11.87 33.58 17 -1 0 63.88 57.49 -17 1 -1 258.19 76.11 -17 1 -1 134.04 71.01 -17 -1 -1 182.92 65.49 -17 -1 -1 235.91 82.38 18 0 0 43.17 46.16 -18 0 0 -0.34 51.63 ; _shelx_hkl_checksum 83017 loop_ _space_group_symop_operation_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_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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Bi1 Bi 0.70141(5) 0.0000 0.09850(7) 0.0492(2) Uani 1 2 d S T P Se1 Se 0.53498(15) 0.5000 -0.0615(2) 0.0492(7) Uani 0.824(14) 2 d S T P Se2 Se 0.65381(18) 0.0000 -0.1649(3) 0.0432(8) Uani 0.479(14) 2 d S T P S1 S 0.53498(15) 0.5000 -0.0615(2) 0.0492(7) Uani 0.176(14) 2 d S T P S2 S 0.65381(18) 0.0000 -0.1649(3) 0.0432(8) Uani 0.521(14) 2 d S T P Bi2 Bi 0.38951(5) 0.0000 -0.39105(8) 0.0511(2) Uani 1 2 d S T P Se3 Se 0.2122(2) 0.0000 -0.6548(3) 0.0440(9) Uani 0.328(14) 2 d S T P Se4 Se 0.41744(18) -0.5000 -0.5416(3) 0.0448(8) Uani 0.545(13) 2 d S T P S3 S 0.2122(2) 0.0000 -0.6548(3) 0.0440(9) Uani 0.672(14) 2 d S T P S4 S 0.41744(18) -0.5000 -0.5416(3) 0.0448(8) Uani 0.455(13) 2 d S T P 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 Bi1 0.0539(4) 0.0483(4) 0.0561(4) 0.000 0.0390(3) 0.000 Se1 0.0434(10) 0.0535(12) 0.0534(12) 0.000 0.0308(9) 0.000 Se2 0.0439(13) 0.0416(14) 0.0487(14) 0.000 0.0305(11) 0.000 S1 0.0434(10) 0.0535(12) 0.0534(12) 0.000 0.0308(9) 0.000 S2 0.0439(13) 0.0416(14) 0.0487(14) 0.000 0.0305(11) 0.000 Bi2 0.0459(4) 0.0528(4) 0.0567(4) 0.000 0.0322(3) 0.000 Se3 0.0421(14) 0.0454(16) 0.0473(16) 0.000 0.0286(13) 0.000 Se4 0.0435(12) 0.0484(14) 0.0493(14) 0.000 0.0316(11) 0.000 S3 0.0421(14) 0.0454(16) 0.0473(16) 0.000 0.0286(13) 0.000 S4 0.0435(12) 0.0484(14) 0.0493(14) 0.000 0.0316(11) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 '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' S S 0.1246 0.1234 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 Se2 Bi1 S2 85.79(6) . 7_655 Se2 Bi1 Se2 85.79(6) . 7_655 S2 Bi1 Se2 0.00(9) 7_655 7_655 Se2 Bi1 S2 85.79(6) . 7_645 S2 Bi1 S2 91.59(7) 7_655 7_645 Se2 Bi1 S2 91.59(7) 7_655 7_645 Se2 Bi1 Se2 85.79(6) . 7_645 S2 Bi1 Se2 91.59(7) 7_655 7_645 Se2 Bi1 Se2 91.59(7) 7_655 7_645 S2 Bi1 Se2 0.00(12) 7_645 7_645 Se2 Bi1 Se1 76.29(6) . . S2 Bi1 Se1 88.13(5) 7_655 . Se2 Bi1 Se1 88.13(5) 7_655 . S2 Bi1 Se1 162.06(7) 7_645 . Se2 Bi1 Se1 162.06(7) 7_645 . Se2 Bi1 S1 76.29(6) . 1_545 S2 Bi1 S1 162.06(7) 7_655 1_545 Se2 Bi1 S1 162.06(7) 7_655 1_545 S2 Bi1 S1 88.13(5) 7_645 1_545 Se2 Bi1 S1 88.13(5) 7_645 1_545 Se1 Bi1 S1 86.68(6) . 1_545 Se2 Bi1 Se1 76.29(6) . 1_545 S2 Bi1 Se1 162.06(7) 7_655 1_545 Se2 Bi1 Se1 162.06(7) 7_655 1_545 S2 Bi1 Se1 88.13(5) 7_645 1_545 Se2 Bi1 Se1 88.13(5) 7_645 1_545 Se1 Bi1 Se1 86.68(6) . 1_545 S1 Bi1 Se1 0.00(16) 1_545 1_545 S1 Se1 Se1 0.00(6) 5_665 5_665 S1 Se1 Bi1 102.61(9) 5_665 . Se1 Se1 Bi1 102.61(9) 5_665 . S1 Se1 Bi1 102.61(9) 5_665 1_565 Se1 Se1 Bi1 102.61(9) 5_665 1_565 Bi1 Se1 Bi1 86.68(6) . 1_565 Bi1 Se2 Bi1 94.21(6) . 7_655 Bi1 Se2 Bi1 94.21(6) . 7_645 Bi1 Se2 Bi1 91.59(7) 7_655 7_645 Se3 Bi2 S3 82.42(8) . 7_544 Se3 Bi2 Se3 82.42(8) . 7_544 S3 Bi2 Se3 0.00(10) 7_544 7_544 Se3 Bi2 S3 82.42(8) . 7_554 S3 Bi2 S3 90.48(8) 7_544 7_554 Se3 Bi2 S3 90.48(8) 7_544 7_554 Se3 Bi2 Se3 82.42(8) . 7_554 S3 Bi2 Se3 90.48(8) 7_544 7_554 Se3 Bi2 Se3 90.48(8) 7_544 7_554 S3 Bi2 Se3 0.00(12) 7_554 7_554 Se3 Bi2 Se4 76.21(7) . . S3 Bi2 Se4 86.03(5) 7_544 . Se3 Bi2 Se4 86.03(5) 7_544 . S3 Bi2 Se4 158.62(7) 7_554 . Se3 Bi2 Se4 158.62(7) 7_554 . Se3 Bi2 S4 76.21(7) . 1_565 S3 Bi2 S4 158.62(7) 7_544 1_565 Se3 Bi2 S4 158.62(7) 7_544 1_565 S3 Bi2 S4 86.03(5) 7_554 1_565 Se3 Bi2 S4 86.03(5) 7_554 1_565 Se4 Bi2 S4 89.57(7) . 1_565 Se3 Bi2 Se4 76.21(7) . 1_565 S3 Bi2 Se4 158.62(7) 7_544 1_565 Se3 Bi2 Se4 158.62(7) 7_544 1_565 S3 Bi2 Se4 86.03(5) 7_554 1_565 Se3 Bi2 Se4 86.03(5) 7_554 1_565 Se4 Bi2 Se4 89.57(7) . 1_565 S4 Bi2 Se4 0.00(10) 1_565 1_565 Bi2 Se3 Bi2 97.58(8) . 7_544 Bi2 Se3 Bi2 97.58(8) . 7_554 Bi2 Se3 Bi2 90.48(8) 7_544 7_554 S4 Se4 Se4 0.00(12) 5_644 5_644 S4 Se4 Bi2 109.11(10) 5_644 . Se4 Se4 Bi2 109.11(10) 5_644 . S4 Se4 Bi2 109.11(10) 5_644 1_545 Se4 Se4 Bi2 109.11(10) 5_644 1_545 Bi2 Se4 Bi2 89.57(7) . 1_545 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Bi1 Se2 2.676(3) . Bi1 S2 2.8626(17) 7_655 Bi1 Se2 2.8626(17) 7_655 Bi1 S2 2.8626(17) 7_645 Bi1 Se2 2.8626(17) 7_645 Bi1 Se1 2.9898(15) . Bi1 S1 2.9898(15) 1_545 Bi1 Se1 2.9898(15) 1_545 Se1 S1 2.317(4) 5_665 Se1 Se1 2.317(4) 5_665 Se1 Bi1 2.9898(15) 1_565 Se2 Bi1 2.8626(17) 7_655 Se2 Bi1 2.8626(17) 7_645 Bi2 Se3 2.655(3) . Bi2 S3 2.890(2) 7_544 Bi2 Se3 2.890(2) 7_544 Bi2 S3 2.890(2) 7_554 Bi2 Se3 2.890(2) 7_554 Bi2 Se4 2.9128(17) . Bi2 S4 2.9129(17) 1_565 Bi2 Se4 2.9129(17) 1_565 Se3 Bi2 2.890(2) 7_544 Se3 Bi2 2.890(2) 7_554 Se4 S4 2.249(5) 5_644 Se4 Se4 2.249(5) 5_644 Se4 Bi2 2.9128(17) 1_545