#------------------------------------------------------------------------------ #$Date: 2020-10-06 15:03:48 +0300 (Tue, 06 Oct 2020) $ #$Revision: 258170 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557220.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_1557220 loop_ _publ_author_name 'MIKURIYA, Masahiro' 'TANIGUCHI, Kazuki' 'KOYAMA, Yoshiki' 'WATANABE, Hiroaki' 'YOSHIOKA, Daisuke' 'MITSUHASHI, Ryoji' 'ASATO, Eiji' _publ_section_title ; Crystal Structure of S<sub>8</sub> Molecule from Thiourea ; _journal_issue 0 _journal_name_full 'X-ray Structure Analysis Online' _journal_page_first 1 _journal_page_last 2 _journal_paper_doi 10.2116/xraystruct.36.1 _journal_volume 36 _journal_year 2020 _chemical_formula_moiety S8 _chemical_formula_sum S8 _chemical_formula_weight 256.48 _space_group_crystal_system orthorhombic _space_group_IT_number 70 _space_group_name_Hall '-F 2uv 2vw' _space_group_name_H-M_alt 'F d d d :2' _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 10.3310(8) _cell_length_b 12.6786(10) _cell_length_c 24.3519(19) _cell_measurement_reflns_used 1864 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 28.483 _cell_measurement_theta_min 2.677 _cell_volume 3189.7(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'shelXle ' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 90(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0209 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1864 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.483 _diffrn_reflns_theta_min 2.677 _exptl_absorpt_coefficient_mu 2.135 _exptl_absorpt_correction_T_max 0.675 _exptl_absorpt_correction_T_min 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour pale-yellow _exptl_crystal_density_diffrn 2.136 _exptl_crystal_description polyhedron _exptl_crystal_F_000 2048 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.327 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.075 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 38 _refine_ls_number_reflns 1864 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0220 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+1.1306P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.0570 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1639 _reflns_number_total 1864 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 36_1_1.txt _cod_data_source_block twin4 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/current/J-STAGE/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 1557220.cif. ; _cod_original_sg_symbol_H-M 'F d d d' _cod_database_code 1557220 _shelx_shelxl_version_number 2018/3 _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 0.567 _shelx_estimated_absorpt_t_max 0.675 _shelx_res_file ; TITL twin4_a.res in Fddd twin4.res created by SHELXL-2018/3 at 00:39:20 on 25-Sep-2019 REM Yadorkari-X generated CELL 0.71073 10.3310 12.6786 24.3519 90.0000 90.0000 90.0000 ZERR 16.0 0.0008 0.0010 0.0019 0.0000 0.0000 0.0000 LATT 4 SYMM 1/4-X, 1/4-Y, +Z SYMM +X, 1/4-Y, 1/4-Z SYMM 1/4-X, +Y, 1/4-Z REM SPGR Fddd orthorhombic SFAC S UNIT 128 SIZE 0.20 0.24 0.30 TEMP -183.0 L.S. 10 FMAP 2 PLAN -20 ACTA CONF LIST 4 BOND $H MERG 2 WGHT 0.033700 1.130600 BASF 0.33534 FVAR 0.16551 S1 1 0.715106 0.659064 0.379781 11.00000 0.01159 0.01859 = 0.01209 0.00135 -0.00165 -0.00018 S2 1 0.715607 0.783414 0.325816 11.00000 0.01955 0.01197 = 0.01355 -0.00236 -0.00036 -0.00067 S3 1 0.794683 0.731991 0.253273 11.00000 0.01485 0.01581 = 0.01320 -0.00011 0.00149 -0.00289 S4 1 0.644124 0.704270 0.200068 11.00000 0.01978 0.01257 = 0.01172 0.00187 -0.00180 -0.00158 HKLF 5 REM twin4_a.res in Fddd REM wR2 = 0.0570, GooF = S = 1.057, Restrained GooF = 1.057 for all data REM R1 = 0.0220 for 1639 Fo > 4sig(Fo) and 0.0261 for all 1864 data REM 38 parameters refined using 0 restraints END WGHT 0.0337 1.1305 REM Highest difference peak 0.327, deepest hole -0.286, 1-sigma level 0.075 Q1 1 0.6250 0.6250 0.1997 10.50000 0.05 0.33 Q2 1 0.7539 0.7435 0.2825 11.00000 0.05 0.31 Q3 1 0.7520 0.7007 0.2146 11.00000 0.05 0.26 Q4 1 0.5809 0.5938 0.4042 11.00000 0.05 0.25 Q5 1 0.5021 0.5850 0.4068 11.00000 0.05 0.24 Q6 1 0.7132 0.7464 0.2369 11.00000 0.05 0.24 Q7 1 0.7701 0.8318 0.3310 11.00000 0.05 0.24 Q8 1 0.7962 0.6708 0.2565 11.00000 0.05 0.24 Q9 1 0.7940 0.8026 0.3407 11.00000 0.05 0.24 Q10 1 0.8738 0.7548 0.2458 11.00000 0.05 0.23 Q11 1 0.6307 0.7670 0.3218 11.00000 0.05 0.23 Q12 1 0.5859 0.7344 0.2154 11.00000 0.05 0.23 Q13 1 0.7457 0.6741 0.2493 11.00000 0.05 0.22 Q14 1 0.6045 0.6564 0.3776 11.00000 0.05 0.22 Q15 1 0.5032 0.6209 0.3425 11.00000 0.05 0.22 Q16 1 0.6919 0.8432 0.3241 11.00000 0.05 0.22 Q17 1 0.6031 0.7545 0.2029 11.00000 0.05 0.21 Q18 1 0.6930 0.6845 0.1715 11.00000 0.05 0.21 Q19 1 0.8666 0.7024 0.2508 11.00000 0.05 0.20 Q20 1 0.5874 0.5464 0.1627 11.00000 0.05 0.20 ; _shelx_res_checksum 17116 _shelx_hkl_file ; 2 0 0 2.91569 0.29558 1 4 0 0 1652.67 16.4625 1 6 0 0 11.2765 2.46768 1 8 0 0 138.113 7.36125 1 10 0 0 1.76716 4.12267 1 12 0 0 2875.42 51.4678 1 2 2 0 1367.87 8.56252 1 4 2 0 0.74724 0.42035 1 6 2 0 10.3373 0.80828 1 8 2 0 1.44990 2.11537 1 10 2 0 191.927 5.49558 1 12 2 0 0.55492 4.23047 1 0 4 0 4951.11 65.2140 1 2 4 0 0.15850 0.47605 1 4 4 0 4.12629 0.62463 1 6 4 0 0.54758 0.76888 1 8 4 0 58.8090 2.91386 1 10 4 0 0.24647 3.02892 1 12 4 0 219.101 9.52873 1 0 6 0 0.01857 1.25440 1 2 6 0 21.9074 1.33958 1 4 6 0 1.03324 0.73920 1 6 6 0 5883.83 36.0603 1 8 6 0 -1.1584 2.33869 1 10 6 0 293.540 9.06513 1 12 6 0 0.81493 4.56963 1 2 8 0 1.58995 1.29646 1 4 8 0 471.059 4.96638 1 6 8 0 0.19052 1.30394 1 8 8 0 218.737 7.21055 1 10 8 0 -0.5747 3.67992 1 12 8 0 22.2762 5.63396 1 0 10 0 2.27753 2.53318 1 2 10 0 483.701 8.84817 1 4 10 0 2.47622 1.62687 1 6 10 0 3392.18 26.0281 1 8 10 0 1.56482 3.06761 1 10 10 0 508.825 12.6374 1 0 12 0 436.799 12.9745 1 2 12 0 0.04613 2.35673 1 4 12 0 449.754 7.75577 1 6 12 0 1.36383 2.32352 1 8 12 0 114.740 6.52727 1 0 14 0 -0.6980 3.89717 1 2 14 0 402.608 9.98093 1 4 14 0 0.42364 2.74425 1 6 14 0 20.2577 3.55302 1 0 16 0 1457.62 33.2753 1 2 16 0 2.01489 5.96307 1 4 16 0 341.218 15.3568 1 -13 1 1 223.490 10.2688 1 -11 1 1 49.3171 4.91591 1 -9 1 1 136.428 5.77484 1 -7 1 1 99.8378 4.20827 1 -5 1 1 501.819 4.51578 1 -3 1 1 2240.67 15.3827 1 -1 1 1 95.2761 1.19912 1 -1 1 1 133.147 2.42015 -2 1 1 1 133.147 2.42015 1 3 1 1 2237.23 15.1821 1 5 1 1 501.848 4.23281 1 7 1 1 103.637 4.31651 1 9 1 1 132.201 5.69345 1 11 1 1 41.9421 4.75747 1 13 1 1 227.323 10.7363 1 -13 3 1 275.770 11.1432 1 -11 3 1 29.4538 4.37570 1 -9 3 1 18.8602 2.30032 1 -7 3 1 30.4932 1.71695 1 -5 3 1 13.6577 0.80859 1 -3 3 1 251.204 2.43584 1 -1 3 1 779.754 6.96359 1 1 3 1 771.080 5.87947 1 -3 3 1 361.580 6.95073 -2 3 3 1 361.580 6.95073 1 5 3 1 16.6770 0.85531 1 7 3 1 25.9891 1.95770 1 9 3 1 20.5032 2.35874 1 11 3 1 18.1905 4.13273 1 13 3 1 315.793 11.5996 1 -13 5 1 18.8801 5.82845 1 -11 5 1 10.4411 4.26487 1 -9 5 1 8.61917 2.95872 1 -7 5 1 194.001 3.49405 1 -5 5 1 1075.86 8.05682 1 -3 5 1 2.65856 0.59776 1 -1 5 1 769.752 9.27716 1 1 5 1 794.732 9.48863 1 3 5 1 2.89872 0.61725 1 5 5 1 1076.83 8.07156 1 7 5 1 200.709 4.40580 1 9 5 1 10.4083 3.04433 1 11 5 1 8.62481 4.09674 1 13 5 1 14.5954 5.89289 1 -11 7 1 16.8462 4.61966 1 -9 7 1 764.307 13.7884 1 -7 7 1 556.502 6.91739 1 -5 7 1 2.54170 0.96703 1 -3 7 1 3448.37 24.7452 1 -1 7 1 128.014 3.56480 1 1 7 1 128.870 3.63463 1 3 7 1 3460.14 21.9905 1 5 7 1 2.62538 0.97482 1 7 7 1 575.786 8.07514 1 9 7 1 772.036 13.8289 1 11 7 1 12.6169 4.40701 1 -11 9 1 1.86522 4.64248 1 -9 9 1 95.4290 5.82123 1 -7 9 1 382.695 6.31153 1 -5 9 1 16.1862 1.70947 1 -3 9 1 72.5279 2.94487 1 -1 9 1 189.866 5.10249 1 1 9 1 188.063 5.01664 1 3 9 1 71.3355 3.58864 1 5 9 1 18.4520 1.57594 1 7 9 1 388.610 9.06815 1 9 9 1 106.125 6.03711 1 11 9 1 2.97797 4.53286 1 -9 11 1 2.35432 4.02445 1 -7 11 1 0.32508 2.46729 1 -5 11 1 1.22063 1.98745 1 -3 11 1 172.915 4.64257 1 -1 11 1 449.863 8.91930 1 1 11 1 442.474 8.72303 1 3 11 1 182.449 5.81617 1 5 11 1 2.41134 1.99094 1 7 11 1 0.14179 3.05039 1 9 11 1 4.80006 4.19029 1 -7 13 1 -0.1057 5.21267 1 -5 13 1 10.6643 2.81133 1 -3 13 1 896.263 11.8739 1 -1 13 1 7.47703 2.80549 1 1 13 1 4.98657 2.86597 1 3 13 1 901.160 14.6686 1 5 13 1 6.58658 2.70199 1 7 13 1 4.01566 5.58723 1 -5 15 1 110.961 5.51425 1 -3 15 1 2.05640 3.01497 1 -1 15 1 -1.6514 3.40185 1 1 15 1 -1.9736 3.33974 1 3 15 1 -0.3043 2.96142 1 5 15 1 119.549 5.69904 1 -12 0 2 -2.2472 5.78699 1 -10 0 2 879.068 21.3371 1 -8 0 2 -0.9413 2.93669 1 -6 0 2 5940.58 56.5693 1 -4 0 2 4.22021 0.60523 1 -2 0 2 116.108 1.92390 1 0 0 2 0.00619 0.18176 1 2 0 2 121.648 3.07303 1 4 0 2 -0.2962 1.22588 1 6 0 2 5900.16 82.7982 1 8 0 2 -0.0569 2.80387 1 10 0 2 896.534 21.3845 1 12 0 2 3.75905 6.17905 1 -12 2 2 108.511 7.03963 1 -10 2 2 180.843 6.99194 1 -8 2 2 56.1194 3.67613 1 -6 2 2 198.248 2.76480 1 -4 2 2 878.858 7.08909 1 -2 2 2 6905.98 45.2076 1 0 2 2 298.564 3.01279 1 -2 2 2 9999.99 128.535 -2 2 2 2 9999.99 128.535 1 -4 2 2 1301.64 18.1742 -2 4 2 2 1301.64 18.1742 1 6 2 2 188.334 2.10916 1 8 2 2 63.4051 3.00562 1 10 2 2 177.762 5.37199 1 12 2 2 120.737 7.25068 1 -12 4 2 97.2158 6.87366 1 -10 4 2 20.3958 3.76418 1 -8 4 2 1373.01 18.6260 1 -6 4 2 3.04325 0.80229 1 -4 4 2 271.555 2.84687 1 -2 4 2 204.768 2.19214 1 0 4 2 1.80766 0.67519 1 -2 4 2 291.812 6.47784 -2 2 4 2 291.812 6.47784 1 4 4 2 273.072 2.90083 1 6 4 2 4.64329 0.78936 1 8 4 2 1395.74 14.5716 1 10 4 2 24.5103 2.90797 1 12 4 2 95.1826 6.69282 1 -12 6 2 245.066 10.3282 1 -10 6 2 412.348 10.5723 1 -8 6 2 24.0140 3.20946 1 -6 6 2 5.24246 1.03148 1 -4 6 2 30.5676 1.28431 1 -2 6 2 1094.34 10.4966 1 0 6 2 4655.06 44.6222 1 2 6 2 1101.66 8.97881 1 4 6 2 29.3312 1.27991 1 6 6 2 7.39541 1.09689 1 8 6 2 18.7001 2.35369 1 10 6 2 417.255 10.4682 1 12 6 2 214.175 9.70220 1 -12 8 2 52.4294 6.40066 1 -10 8 2 1.07164 3.74478 1 -8 8 2 1260.74 18.3586 1 -6 8 2 188.988 3.87259 1 -4 8 2 608.494 6.68315 1 -2 8 2 77.6117 3.31852 1 0 8 2 0.06257 1.25877 1 2 8 2 74.1507 3.24454 1 4 8 2 613.200 5.90108 1 6 8 2 201.753 3.46698 1 8 8 2 1278.81 18.4880 1 10 8 2 0.16366 3.70351 1 12 8 2 45.8531 6.14291 1 -10 10 2 242.741 9.86268 1 -8 10 2 6.92103 3.43294 1 -6 10 2 105.157 3.64641 1 -4 10 2 283.970 5.53169 1 -2 10 2 14.4511 2.25678 1 0 10 2 1538.28 18.9740 1 2 10 2 17.6235 2.38680 1 4 10 2 279.018 5.50647 1 6 10 2 104.847 3.57017 1 8 10 2 1.98451 3.21989 1 10 10 2 239.595 9.72565 1 -8 12 2 236.331 8.59168 1 -6 12 2 38.5831 3.33653 1 -4 12 2 854.617 11.2193 1 -2 12 2 207.302 6.71013 1 0 12 2 -0.9751 2.15343 1 2 12 2 200.794 6.48656 1 4 12 2 830.927 11.0480 1 6 12 2 35.0525 3.22941 1 8 12 2 251.720 9.14194 1 -6 14 2 22.0339 3.53878 1 -4 14 2 -0.9917 2.72662 1 -2 14 2 176.832 7.42333 1 0 14 2 668.232 12.7858 1 2 14 2 180.151 7.37092 1 4 14 2 1.84560 2.68104 1 6 14 2 21.3381 3.60157 1 -4 16 2 326.377 14.7208 1 0 16 2 -0.5740 4.51153 1 2 16 2 108.382 15.6427 1 4 16 2 294.974 14.7427 1 -13 1 3 3.95503 5.08131 1 -11 1 3 129.705 6.97466 1 -9 1 3 706.980 12.6076 1 -7 1 3 671.821 6.29493 1 -5 1 3 32.5969 1.20284 1 -3 1 3 2501.10 17.2440 1 -1 1 3 362.336 3.47402 1 1 1 3 356.061 3.90504 1 -3 1 3 3733.34 49.9820 -2 3 1 3 3733.34 49.9820 1 5 1 3 32.5641 2.10053 1 7 1 3 676.372 10.5854 1 9 1 3 688.780 12.1439 1 11 1 3 143.646 7.33285 1 13 1 3 1.39248 5.00213 1 -13 3 3 13.7152 5.50827 1 -11 3 3 406.704 10.9811 1 -9 3 3 569.719 11.2215 1 -7 3 3 882.225 7.01342 1 -5 3 3 151.333 2.11919 1 -3 3 3 726.717 5.27943 1 -1 3 3 615.835 5.02959 1 -1 3 3 945.549 14.1782 -2 1 3 3 945.549 14.1782 1 -3 3 3 1069.33 15.7585 -2 3 3 3 1069.33 15.7585 1 5 3 3 151.824 2.02866 1 7 3 3 893.479 10.1298 1 9 3 3 592.750 8.65776 1 11 3 3 450.766 8.63511 1 13 3 3 17.1196 5.58526 1 -13 5 3 2.10697 5.57778 1 -11 5 3 31.8045 4.74699 1 -9 5 3 -0.7813 2.66497 1 -7 5 3 27.8259 1.65680 1 -5 5 3 413.593 4.08468 1 -3 5 3 450.536 4.02164 1 -1 5 3 12.5862 1.22687 1 1 5 3 14.8994 1.07897 1 3 5 3 458.147 4.14106 1 5 5 3 420.976 4.16541 1 7 5 3 24.7034 2.08960 1 9 5 3 0.97060 2.12683 1 11 5 3 28.9748 4.68894 1 13 5 3 0.99164 5.41095 1 -11 7 3 6.00167 4.45559 1 -9 7 3 499.515 10.9509 1 -7 7 3 58.0722 2.45732 1 -5 7 3 134.520 3.00152 1 -3 7 3 1265.24 10.6968 1 -1 7 3 289.386 5.49767 1 1 7 3 286.025 5.45032 1 3 7 3 1256.55 10.3763 1 5 7 3 131.954 2.59995 1 7 7 3 67.9077 3.19435 1 9 7 3 513.066 11.1173 1 11 7 3 10.0864 4.35847 1 -11 9 3 100.957 7.21554 1 -9 9 3 342.957 9.73031 1 -7 9 3 159.470 4.06877 1 -5 9 3 1251.33 11.5649 1 -3 9 3 1886.46 17.7334 1 -1 9 3 230.065 5.60266 1 1 9 3 219.562 5.48026 1 3 9 3 1902.46 21.7053 1 5 9 3 1298.60 10.4477 1 7 9 3 168.739 6.16926 1 9 9 3 341.556 9.68702 1 11 9 3 97.8000 6.89624 1 -9 11 3 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10 22 201.784 15.8150 1 -9 1 23 28.1087 4.65745 1 -7 1 23 3.03026 3.17927 1 -5 1 23 10.4013 2.86860 1 -3 1 23 0.81813 2.19843 1 -1 1 23 8.30316 1.90533 1 1 1 23 11.7182 1.66815 1 3 1 23 -0.5531 1.51228 1 5 1 23 13.7785 3.21220 1 7 1 23 0.32487 3.47555 1 9 1 23 31.3203 5.20960 1 -9 3 23 166.759 8.43742 1 -7 3 23 405.793 10.1807 1 -5 3 23 208.279 7.14278 1 -3 3 23 121.428 5.42540 1 -1 3 23 661.174 9.25765 1 1 3 23 664.503 9.14594 1 -3 3 23 208.853 11.1712 -2 3 3 23 208.853 11.1712 1 5 3 23 204.238 7.44506 1 7 3 23 451.646 11.0913 1 9 3 23 153.778 8.01350 1 -7 5 23 1.30934 2.89024 1 -5 5 23 187.274 7.29409 1 -3 5 23 357.900 8.82506 1 -1 5 23 20.9693 3.02719 1 1 5 23 22.8578 2.56963 1 -3 5 23 571.047 15.4357 -2 3 5 23 571.047 15.4357 1 -5 5 23 297.604 13.9794 -2 5 5 23 297.604 13.9794 1 7 5 23 -0.3268 3.82347 1 -7 7 23 438.239 9.17052 1 -5 7 23 175.384 7.48064 1 -3 7 23 140.027 6.61597 1 -1 7 23 0.79202 2.64628 1 1 7 23 -1.1643 2.26897 1 -3 7 23 197.266 11.3340 -2 3 7 23 197.266 11.3340 1 5 7 23 202.042 12.6973 1 7 7 23 461.176 11.7471 1 -5 9 23 21.2541 6.10312 1 -3 9 23 2.83078 2.73815 1 -1 9 23 43.6643 4.55909 1 1 9 23 39.8354 4.33731 1 -3 9 23 5.36097 9.10709 -2 3 9 23 5.36097 9.10709 1 -5 9 23 22.2005 8.51558 -2 5 9 23 22.2005 8.51558 1 1 11 23 6.02026 3.93986 1 -3 11 23 -3.2389 13.4077 -2 3 11 23 -3.2389 13.4077 1 -8 0 24 80.1337 7.98808 1 -6 0 24 -0.1546 4.45973 1 -4 0 24 375.611 12.6472 1 -2 0 24 3.19865 3.41030 1 0 0 24 3485.65 36.8295 1 2 0 24 0.28899 2.22384 1 4 0 24 362.922 12.4389 1 6 0 24 0.09948 4.53917 1 8 0 24 77.7797 8.68200 1 -8 2 24 7.34547 3.98907 1 -6 2 24 17.1809 3.56836 1 -4 2 24 669.398 12.2951 1 -2 2 24 39.1422 3.54554 1 0 2 24 0.08571 1.86606 1 2 2 24 45.3894 2.57314 1 4 2 24 730.694 12.7726 1 6 2 24 21.7531 3.98460 1 8 2 24 14.2239 4.48359 1 -8 4 24 28.9288 5.03471 1 -6 4 24 253.910 8.61874 1 -4 4 24 1.20882 2.86067 1 -2 4 24 523.025 10.6713 1 0 4 24 277.173 6.19725 1 2 4 24 535.694 8.48715 1 -4 4 24 0.72804 9.88914 -2 4 4 24 0.72804 9.88914 1 6 4 24 251.667 8.90569 1 8 4 24 35.4967 5.31335 1 -8 6 24 386.791 18.6326 1 -6 6 24 597.939 12.9199 1 -4 6 24 345.069 9.32726 1 -2 6 24 22.1566 3.42718 1 0 6 24 -0.0746 2.24266 1 2 6 24 25.8354 3.65474 1 4 6 24 313.401 13.9040 1 6 6 24 678.578 13.7286 1 8 6 24 431.085 12.5451 1 -4 8 24 39.1713 4.83562 1 -2 8 24 37.5098 4.30458 1 0 8 24 25.8839 3.86034 1 -2 8 24 75.8661 11.4289 -2 2 8 24 75.8661 11.4289 1 4 8 24 54.4782 8.10332 1 6 8 24 69.0352 8.91400 1 0 10 24 -2.1276 3.61093 1 -2 10 24 162.994 14.7545 -2 2 10 24 162.994 14.7545 1 -4 10 24 452.549 16.6256 -2 4 10 24 452.549 16.6256 1 -7 1 25 93.5732 5.93999 1 -5 1 25 414.534 9.93488 1 -3 1 25 49.7137 4.14093 1 -1 1 25 0.91038 2.30190 1 1 1 25 0.36490 1.89987 1 3 1 25 68.1050 3.04790 1 5 1 25 419.406 10.1339 1 7 1 25 111.917 6.70444 1 -7 3 25 182.961 7.88407 1 -5 3 25 34.3947 4.17488 1 -3 3 25 4.84971 2.72555 1 -1 3 25 36.5791 3.01197 1 1 3 25 35.7360 2.94571 1 3 3 25 11.3293 2.06591 1 5 3 25 47.0432 4.72752 1 7 3 25 192.355 8.65998 1 -7 5 25 278.938 9.47468 1 -5 5 25 64.7881 5.29517 1 -3 5 25 1.79984 2.99353 1 -1 5 25 145.283 6.26017 1 1 5 25 149.738 5.21659 1 -3 5 25 2.45748 8.78088 -2 3 5 25 2.45748 8.78088 1 -5 5 25 109.214 13.6101 -2 5 5 25 109.214 13.6101 1 7 5 25 314.902 10.4453 1 -5 7 25 -0.8406 3.88416 1 -3 7 25 488.411 11.2750 1 -1 7 25 39.6500 4.36756 1 1 7 25 40.5385 3.56865 1 3 7 25 479.813 11.1250 1 5 7 25 -0.9150 5.91020 1 -1 9 25 117.318 6.68626 1 1 9 25 106.259 6.25882 1 -3 9 25 121.498 12.6781 -2 3 9 25 121.498 12.6781 1 5 9 25 -0.4852 6.95475 1 -6 0 26 187.280 11.4166 1 -4 0 26 3.48841 4.39256 1 -2 0 26 500.825 15.0495 1 2 0 26 502.853 10.1090 1 4 0 26 2.22163 4.57631 1 6 0 26 223.868 12.4457 1 8 0 26 -1.0474 6.41545 1 -6 2 26 25.2459 4.32906 1 -4 2 26 408.223 9.91198 1 -2 2 26 597.075 11.6078 1 0 2 26 54.2665 3.45024 1 2 2 26 640.788 9.44585 1 4 2 26 429.218 10.1373 1 6 2 26 33.5387 4.76691 1 8 2 26 58.7559 6.15744 1 -6 4 26 142.148 7.32026 1 -4 4 26 796.221 14.3607 1 -2 4 26 304.182 8.59972 1 0 4 26 1.06063 2.33156 1 2 4 26 337.374 7.17607 1 4 4 26 869.189 21.9665 1 6 4 26 159.889 7.98883 1 -4 6 26 294.451 9.40095 1 -2 6 26 777.818 14.2474 1 0 6 26 187.714 6.08067 1 2 6 26 808.402 11.6259 1 4 6 26 308.555 14.7009 1 6 6 26 2.88043 6.61638 1 -2 8 26 61.0776 5.37776 1 0 8 26 4.16371 3.55035 1 2 8 26 72.7220 4.65481 1 4 8 26 235.733 14.7347 1 -5 1 27 2.15722 3.55932 1 -3 1 27 350.636 9.38720 1 -1 1 27 214.049 7.30909 1 1 1 27 222.283 5.91634 1 3 1 27 364.685 6.32449 1 5 1 27 3.70162 3.65295 1 7 1 27 1.25492 4.30605 1 -5 3 27 101.819 6.19539 1 -3 3 27 121.298 6.44640 1 -1 3 27 458.428 10.2877 1 1 3 27 494.546 8.60550 1 3 3 27 136.288 5.15910 1 5 3 27 136.675 7.12436 1 7 3 27 5.86544 4.67771 1 -5 5 27 25.3665 5.53860 1 -3 5 27 77.1994 5.53062 1 -1 5 27 134.431 6.72374 1 1 5 27 134.274 5.43770 1 3 5 27 78.6370 4.35307 1 5 5 27 30.1564 7.42138 1 -1 7 27 207.162 8.03663 1 1 7 27 188.467 6.59838 1 3 7 27 215.499 8.76226 1 5 7 27 5.45816 7.27948 1 -4 0 28 407.575 15.3632 1 -2 0 28 -0.2623 4.33757 1 0 0 28 1.08670 3.92569 1 2 0 28 -0.6178 3.95700 1 4 0 28 409.046 14.9707 1 6 0 28 2.82214 6.11664 1 -4 2 28 74.7067 5.75228 1 -2 2 28 327.495 9.32029 1 0 2 28 1.88757 2.99593 1 2 2 28 342.252 7.33998 1 4 2 28 88.9956 5.94141 1 6 2 28 164.051 8.43700 1 -4 4 28 449.233 11.2966 1 -2 4 28 271.216 8.81317 1 0 4 28 690.970 10.7609 1 2 4 28 304.853 7.35108 1 4 4 28 472.900 17.1388 1 6 4 28 -2.9747 4.51103 1 -2 6 28 477.209 11.7293 1 0 6 28 1.66612 3.39676 1 2 6 28 505.745 9.61476 1 4 6 28 51.1920 8.66108 1 2 8 28 13.1165 3.96302 1 -3 1 29 3.48650 3.57729 1 -1 1 29 82.0268 5.40997 1 1 1 29 89.3484 5.39818 1 3 1 29 3.78565 3.42997 1 5 1 29 7.64339 4.41952 1 -3 3 29 45.2876 4.89085 1 -1 3 29 282.944 8.69096 1 1 3 29 305.325 7.44050 1 3 3 29 50.0888 7.49897 1 5 3 29 786.109 22.7205 1 -1 5 29 347.939 9.88158 1 1 5 29 368.363 8.37774 1 3 5 29 192.090 13.6597 1 1 7 29 60.3778 9.09596 1 -2 0 30 12.7483 5.54255 1 0 0 30 1.25753 4.60322 1 2 0 30 9.10868 4.70228 1 4 0 30 6.04388 6.13553 1 -2 2 30 136.412 7.21862 1 0 2 30 246.291 8.72462 1 2 2 30 137.454 5.66976 1 4 2 30 107.098 9.81181 1 0 4 30 -0.6869 3.59757 1 2 4 30 5.76922 3.24206 1 4 4 30 15.3547 7.48563 1 2 6 30 12.5018 5.60643 1 -1 1 31 166.144 8.28184 1 1 1 31 170.425 7.90248 1 1 3 31 16.0415 4.15344 1 3 3 31 27.5012 7.54942 1 1 5 31 28.7760 8.07331 1 2 0 32 5.09323 5.55284 1 2 2 32 6.74056 4.90466 1 0 0 0 0.00 0.00 0 ) _shelx_hkl_checksum 64251 ; _shelx_hkl_checksum 38658 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' 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 S1 S 0.71511(4) 0.65906(4) 0.37978(2) 0.01409(13) Uani 1 1 d S2 S 0.71561(4) 0.78341(3) 0.32582(2) 0.01502(13) Uani 1 1 d S3 S 0.79468(4) 0.73199(4) 0.25327(2) 0.01462(13) Uani 1 1 d S4 S 0.64412(4) 0.70427(4) 0.20007(2) 0.01469(13) 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 S1 0.0116(2) 0.0186(3) 0.0121(2) 0.00135(17) -0.00165(16) -0.00018(16) S2 0.0195(3) 0.0120(2) 0.0135(2) -0.00236(17) -0.00036(17) -0.00067(16) S3 0.0148(2) 0.0158(2) 0.0132(2) -0.00011(17) 0.00149(16) -0.00289(16) S4 0.0198(2) 0.0126(2) 0.0117(2) 0.00187(17) -0.00180(16) -0.00158(16) 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' 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 S1 S1 S2 109.00(3) 2_665 S1 S2 S3 107.94(3) . S2 S3 S4 107.20(3) . S4 S4 S3 108.29(3) 2_665 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 S1 S1 2.0524(9) 2_665 S1 S2 2.0525(7) . S2 S3 2.0526(6) . S3 S4 2.0546(6) . S4 S4 2.0485(9) 2_665