#------------------------------------------------------------------------------ #$Date: 2021-05-06 03:55:18 +0300 (Thu, 06 May 2021) $ #$Revision: 264977 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/23/1562371.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_1562371 loop_ _publ_author_name 'Hu, Yajing' 'Yao, Yang-Rong' 'Liu, Xuechen' 'Yu, Ao' 'Xie, Xiao-Ming' 'Abella, Laura' 'Rodriguez-Fortea, Antonio' 'Poblet, Josep M.' 'Akasaka, Takeshi' 'Peng, Ping' 'Zhang, Qianyan' 'Xie, Su-Yuan' 'Li, Fang-Fang' 'Lu, Xing' _publ_section_title ; Unexpected Formation of 1,2- and 1,4-Bismethoxyl Sc3N@Ih-C80 Derivatives via Regioselective Anion Addition: Unambiguous Structural Identification and Mechanism Study ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC01178B _journal_year 2021 _chemical_formula_moiety 'C14 H8 O2' _chemical_formula_sum 'C14 H8 O2' _chemical_formula_weight 208.20 _chemical_name_common Anthraquinone _chemical_name_systematic 9,10-Anthracenedione _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2021-03-31 _audit_creation_method ; Olex2 1.3-alpha (compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938) ; _audit_update_record ; 2021-04-06 deposited with the CCDC. 2021-05-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.624(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.8876(7) _cell_length_b 3.9434(4) _cell_length_c 15.7578(19) _cell_measurement_reflns_used 435 _cell_measurement_temperature 223 _cell_measurement_theta_max 29.2346 _cell_measurement_theta_min 3.3041 _cell_volume 478.28(9) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXS n/a (Sheldrick, 2008)' _diffrn_ambient_temperature 223.00(2) _diffrn_detector_area_resol_mean 15.9821 _diffrn_measured_fraction_theta_full 0.960 _diffrn_measured_fraction_theta_max 0.800 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -2.00 83.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 19.6835 57.0000 60.0000 85 #__ type_ start__ end____ width___ exp.time_ 2 omega 35.00 96.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 19.6835 178.0000 -60.0000 61 #__ type_ start__ end____ width___ exp.time_ 3 omega -8.00 79.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 19.6835 19.0000 0.0000 87 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_unetI/netI 0.0541 _diffrn_reflns_Laue_measured_fraction_full 0.960 _diffrn_reflns_Laue_measured_fraction_max 0.800 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 2167 _diffrn_reflns_point_group_measured_fraction_full 0.960 _diffrn_reflns_point_group_measured_fraction_max 0.800 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.299 _diffrn_reflns_theta_min 3.311 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.446 _exptl_crystal_description block _exptl_crystal_F_000 216 _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.157 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 73 _refine_ls_number_reflns 1049 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.010 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0533 _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^)+(0.0583P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1138 _refine_ls_wR_factor_ref 0.1367 _reflns_Friedel_coverage 0.000 _reflns_number_gt 675 _reflns_number_total 1049 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc01178b2.cif _cod_data_source_block anthraquinone-223k _cod_database_code 1562371 _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_max 0.985 _shelx_estimated_absorpt_t_min 0.943 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C5(H5), C3(H3), C6(H6), C4(H4) ; _shelx_res_file ; TITL BKS-SS-DI-ANTH-223K-ss in P21/c #14 anthraquinone-223k.res created by SHELXL-2018/3 at 17:36:27 on 31-Mar-2021 REM reset to P21/c #14 CELL 0.71073 7.887631 3.943396 15.757786 90 102.6236 90 ZERR 2 0.000696 0.000446 0.0019 0 0.0107 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 28 16 4 L.S. 4 PLAN 5 SIZE 0.62 0.26 0.16 TEMP -50.15(2) CONF BOND $H HTAB MORE -1 fmap 2 acta 50 REM REM REM WGHT 0.058300 FVAR 13.26666 C2 1 0.435785 0.653463 0.415104 11.00000 0.03443 0.03251 = 0.03259 -0.00409 0.00550 -0.00371 C7 1 0.326169 0.639498 0.474037 11.00000 0.03142 0.03062 = 0.03736 -0.00425 0.00702 -0.00237 C1 1 0.614872 0.513081 0.438478 11.00000 0.03338 0.04299 = 0.03687 -0.00393 0.01160 -0.00375 C5 1 0.100105 0.914606 0.368555 11.00000 0.03603 0.04207 = 0.05332 -0.00243 -0.00098 0.00342 AFIX 43 H5 2 -0.013066 1.003271 0.352945 11.00000 -1.20000 AFIX 0 O1 3 0.710865 0.523314 0.386848 11.00000 0.04658 0.09219 = 0.04696 0.01106 0.02398 0.01110 C3 1 0.375200 0.798712 0.333340 11.00000 0.04617 0.04513 = 0.03593 -0.00075 0.00983 -0.00208 AFIX 43 H3 2 0.448283 0.809124 0.293613 11.00000 -1.20000 AFIX 0 C6 1 0.158059 0.771682 0.449582 11.00000 0.03307 0.04452 = 0.04703 -0.00288 0.00914 0.00040 AFIX 43 H6 2 0.083800 0.763036 0.488767 11.00000 -1.20000 AFIX 0 C4 1 0.207624 0.927996 0.310272 11.00000 0.05282 0.04416 = 0.03808 0.00228 -0.00122 0.00248 AFIX 43 H4 2 0.167433 1.024577 0.254994 11.00000 -1.20000 AFIX 0 HKLF 4 REM BKS-SS-DI-ANTH-223K-ss in P21/c #14 REM wR2 = 0.1367, GooF = S = 1.010, Restrained GooF = 1.010 for all data REM R1 = 0.0533 for 675 Fo > 4sig(Fo) and 0.0904 for all 1049 data REM 73 parameters refined using 0 restraints END WGHT 0.0583 0.0000 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.157, deepest hole -0.188, 1-sigma level 0.043 Q1 1 0.1846 1.1571 0.2205 11.00000 0.05 0.16 Q2 1 0.0389 1.3975 0.3765 11.00000 0.05 0.15 Q3 1 0.4959 0.8365 0.2790 11.00000 0.05 0.15 Q4 1 0.6941 0.6426 0.3168 11.00000 0.05 0.14 Q5 1 0.2774 1.2550 0.3631 11.00000 0.05 0.13 ; _shelx_res_checksum 65195 _shelx_hkl_file ; 0 0 -3-75.2374 147.056 1 0 0 3-37.0121 123.506 1 0 0 -4 199655. 3543.10 1 0 0 4 198459. 3484.20 1 0 0 5-186.432 187.767 1 0 0 -5-107.445 272.359 1 0 0 -6-72.8582 208.338 1 0 0 6 439.253 167.128 1 0 0 -7 192.249 234.915 1 0 0 -8 15713.3 1169.71 1 0 0 -9 197.383 292.110 1 0 0 -10 275.033 370.805 1 0 0 -11-440.458 399.237 1 0 0 -12 2249.90 716.087 1 0 0 -13-69.9160 422.897 1 0 0 -14 5828.55 971.146 1 0 0 -15 85.1812 413.631 1 0 0 -16 2438.75 822.456 1 0 0 -17 444.016 499.855 1 0 0 -18-593.257 701.589 1 0 0 -19-666.920 639.297 1 0 1 0 367.680 148.581 2 0 1 1 160523. 2876.42 2 0 1 -1 164895. 2886.46 1 0 -1 -1 158137. 2913.00 2 0 -1 -2 571174. 8200.41 2 0 1 2 579964. 8132.40 2 0 1 -2 572350. 8141.30 1 0 -1 2 579721. 8120.86 1 0 -1 3 181477. 3358.60 1 0 1 3 186716. 3481.78 2 0 1 -3 175252. 3427.92 1 0 -1 -3 183369. 3443.07 2 0 -1 4 26934.5 1110.13 1 0 -1 -4 24240.8 1124.38 2 0 1 -4 25229.6 1176.78 1 0 1 4 25915.4 1150.36 2 0 1 -5 143029. 3395.78 1 0 -1 -5 147417. 3275.14 2 0 1 5 147131. 3149.00 1 0 1 6 45977.4 1696.37 1 0 -1 -6 47344.9 1803.60 2 0 1 -7 21908.6 1366.76 1 0 -1 -7 22357.7 1343.37 2 0 -1 -8 16719.7 1277.47 2 0 1 -8 16256.9 1245.43 1 0 -1 -9 6783.99 868.455 2 0 1 -9 7274.60 879.656 1 0 1 -10 2203.53 602.327 1 0 -1 -10 1888.77 545.809 2 0 1 -11 163.483 362.043 1 0 -1 -11-203.940 536.628 2 0 1 -12 2498.75 733.919 1 0 -1 -12 2380.69 731.719 2 0 1 -13 479.897 515.882 1 0 -1 -13-359.243 525.063 2 0 -1 -14 1644.38 724.232 2 0 1 -14 631.801 499.496 1 0 1 -15 1073.47 771.253 1 0 -1 -15 2591.49 891.260 2 0 1 -16 782.494 663.509 1 0 -1 -16-904.893 779.783 2 0 -1 -17 484.786 731.774 2 0 1 -17-25.3327 551.775 1 0 1 -18 272.292 608.654 1 0 -1 -18-684.080 742.970 2 0 -1 -19 319.659 689.146 2 0 1 -19-96.2425 543.436 1 0 -1 -20-234.929 740.144 2 0 2 1 14674.1 562.143 3 0 2 -1 17545.0 989.053 1 0 -2 -2 3495.38 490.928 2 0 2 -2 4259.43 517.506 1 0 2 2 3608.37 304.421 3 0 -2 -3 31828.7 1500.94 2 0 2 -3 32665.5 1446.08 1 0 -2 4 24106.9 759.072 3 0 -2 -4 25806.3 1383.79 2 0 2 -5 63417.5 2367.13 1 0 -2 -5 62818.2 2299.08 2 0 2 -6 8719.77 917.284 1 0 -2 -6 8504.27 839.264 2 0 2 -7 5831.52 802.353 1 0 -2 -7 4778.72 706.331 2 0 2 -8 6872.31 1000.70 1 0 -2 -8 6232.13 834.004 2 0 2 -9-431.360 359.787 1 0 -2 -9 179.781 302.861 2 0 2 -10 4408.07 853.560 1 0 -2 -10 4252.02 765.337 2 0 2 -11 1118.95 462.712 1 0 -2 -11-15.5142 474.044 2 0 -2 -12 3612.95 739.363 2 0 2 -12 4935.39 1010.58 1 0 -2 -13 6160.37 1060.50 2 0 2 -13 4922.94 980.939 1 0 2 -14 856.893 608.448 1 0 -2 -14-378.236 617.007 2 0 2 -15 7553.62 1397.26 1 0 -2 -15 9765.04 1446.36 2 0 -2 -16 12523.6 1661.79 2 0 2 -16 8083.56 1427.09 1 0 2 -17 82.5087 688.601 1 0 -2 -17-319.756 666.811 2 0 -2 -18 773.111 723.509 2 0 -2 -19-310.257 598.237 2 0 3 0 1.41441 128.949 1 0 3 1 245.622 192.547 1 0 3 1 127.794 38.0428 3 0 3 -2 10336.4 987.962 1 0 3 2 7261.48 460.386 3 0 3 3 5802.85 469.102 3 0 3 -3 7404.23 851.418 1 0 3 -4 554.588 302.349 1 0 -3 -4 765.129 293.487 2 0 3 4 768.387 186.109 3 0 3 -5 558.041 363.570 1 0 -3 -5 574.592 302.904 2 0 3 5 986.848 236.610 3 0 -3 -6 2064.72 502.678 2 0 3 6 1469.73 308.923 3 0 3 -6 1949.82 559.976 1 0 3 -7 525.998 296.186 1 0 -3 -7 356.143 326.521 2 0 -3 -8 1923.84 534.555 2 0 3 -8 1828.63 562.215 1 0 3 -9 3372.46 763.888 1 0 -3 -9 3037.71 662.018 2 0 -3 -10 1206.25 500.512 2 0 3 -10 975.458 469.690 1 0 -3 -11 2209.96 601.824 2 0 3 -11 2630.34 836.316 1 0 3 -12 2265.05 828.128 1 0 -3 -12 1959.52 609.136 2 0 -3 -13-387.813 406.657 2 0 3 -13-251.522 437.291 1 0 3 -14-129.896 505.295 1 0 -3 -14 521.623 442.334 2 0 -3 -15-761.279 571.078 2 0 3 -15-259.115 677.328 1 0 -3 -16 3241.67 897.608 2 0 4 0 170.190 192.537 1 0 4 1 633.356 317.820 1 0 4 -1 455.404 262.291 1 0 4 -2-100.845 182.538 1 0 4 -3-269.670 296.869 1 0 4 -4 98.9084 218.840 1 0 4 -5 56.1942 324.033 1 0 4 -6 308.663 342.526 1 0 4 -7 714.847 510.767 1 0 -4 -7 746.437 406.152 2 0 -4 -8 1311.71 495.584 2 0 4 -8 3515.52 868.870 1 0 4 -9-39.2515 379.380 1 0 -4 -9-38.7079 222.094 2 0 4 -10 2594.47 931.574 1 0 -4 -10 1760.78 576.561 2 0 -4 -11 2248.73 600.554 2 0 4 -11 1902.45 798.761 1 0 4 -12-203.324 552.867 1 0 -4 -12 148.595 280.833 2 1 0 -16 1468.18 682.612 1 1 0 -15 442.918 552.640 1 1 0 -14 3054.15 805.951 1 1 0 -13-595.942 501.380 1 1 0 -12 39382.4 2330.19 1 1 0 -11-214.480 436.084 1 1 0 -10 636.859 347.442 1 1 0 -9-20.7093 356.135 1 1 0 -8 18490.8 1264.41 1 1 0 -7-182.988 264.929 1 1 0 -6 87532.8 2491.00 1 -1 0 6 86956.6 2368.13 1 1 0 -5 181.224 205.887 1 -1 0 5 232.851 217.349 1 1 0 -4 79956.8 2091.32 1 -1 0 4 86505.6 2053.60 1 -1 0 3-51.0247 145.988 1 -1 0 3-21.7919 60.6308 3 1 0 -2 260662. 3855.51 3 -1 0 -2 11405.5 502.418 1 1 0 2 11512.8 505.071 1 -1 0 -3 273.149 190.497 1 1 0 3 108.084 119.398 1 -1 0 -4 30047.4 1139.42 1 1 0 4 31689.1 1082.23 1 1 0 5-27.8184 103.089 1 -1 0 -5-96.6006 184.484 1 -1 0 -6 304547. 5521.74 1 1 0 6 302791. 5277.16 1 -1 0 -7-98.3183 273.925 1 -1 0 -8 190062. 4464.99 1 -1 0 -9 10.5970 309.903 1 -1 0 -10 10813.3 1079.30 1 -1 0 -11 728.788 452.722 1 -1 0 -12 7191.76 1041.37 1 -1 0 -13-305.403 412.693 1 -1 0 -14 1370.00 632.679 1 -1 0 -15 960.317 536.533 1 -1 0 -16 7739.88 1261.11 1 -1 0 -17 661.097 582.449 1 -1 0 -18 331.539 515.637 1 -1 0 -19-1076.36 794.666 1 1 -1 -20 456.447 699.677 2 1 1 -19 1840.16 709.773 1 1 -1 -19 5901.93 1276.87 2 1 -1 -18 238.735 682.079 2 1 1 -18 1080.06 711.131 1 1 1 -17 268.429 593.675 1 1 -1 -17-1563.85 790.379 2 1 -1 -16 759.419 751.844 2 1 1 -16 1634.98 731.122 1 1 -1 -15 37449.3 2496.25 2 1 1 -15 33900.4 2621.30 1 1 -1 -14 30394.3 2123.49 2 1 1 -14 27374.8 2217.83 1 1 -1 -13 1936.38 652.432 2 1 1 -13 2824.09 767.320 1 1 1 -12 2862.25 804.863 1 1 -1 -12 2070.26 630.954 2 1 -1 -11 5500.48 886.910 2 1 1 -11 4728.91 791.859 1 1 1 -10 453.380 408.204 1 1 -1 -10 687.523 424.309 2 1 -1 -9 4377.50 655.079 2 1 1 -9 3389.43 647.747 1 1 1 -8 6418.85 793.922 1 1 -1 -8 7755.21 768.122 2 1 -1 -7 2282.75 400.439 2 1 1 -7 1670.95 414.869 1 1 1 -6 15543.1 1033.22 1 1 -1 -6 16014.2 900.606 2 1 -1 -5-27.6796 143.654 2 1 1 -5-95.4181 172.835 1 -1 -1 5 159.595 143.829 1 1 1 -4 4930.29 505.124 1 1 -1 -4 5117.85 436.483 2 -1 -1 4 5801.46 482.670 1 -1 1 4 5336.49 505.163 2 1 -1 -3 74334.2 1715.99 2 1 1 -3 73059.2 1842.27 1 -1 1 3 72144.1 1717.33 2 -1 1 3 73829.4 1778.88 3 -1 -1 3 73143.7 1446.75 3 -1 -1 3 73930.9 1740.23 1 1 1 -2 846.556 276.331 2 1 -1 -2 502.466 137.315 2 -1 1 2 376.745 110.941 3 -1 -1 2 382.042 87.2628 3 -1 1 2 253.675 111.356 2 -1 -1 2 217.768 93.5404 1 1 1 -2 956.844 218.471 1 -1 1 1 920.225 152.389 3 1 1 -1 1228.55 218.018 2 -1 -1 1 678.511 167.353 2 -1 -1 1 942.997 117.537 3 1 1 -1 1127.60 154.622 1 1 -1 -1 1044.49 164.239 3 1 1 -1 892.771 102.663 3 -1 -1 1 1005.13 155.545 1 -1 1 1 1048.96 215.833 2 -1 1 0 425623. 5878.36 3 1 1 0 409497. 5762.54 3 1 1 0 422250. 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-11 932.915 637.064 2 -6 1 -11 810.032 399.498 1 -6 -1 -12 530.491 768.347 2 -6 1 -12-675.858 408.541 1 -6 1 -13 1415.50 766.357 1 -6 1 -14 890.252 429.025 1 -6 -2 16-43.4165 292.373 3 -6 2 16 432.276 220.909 3 -6 -2 15 533.973 278.802 3 -6 2 15 538.635 373.605 3 -6 -2 14 633.739 258.598 3 -6 2 14 644.898 366.954 3 -6 -2 13-137.984 174.482 3 -6 2 13 99.4080 220.558 3 -6 -2 12 637.008 257.215 3 -6 2 12 681.758 349.652 3 -6 -2 11 11.2949 127.222 3 -6 2 11-608.135 320.335 3 -6 -2 10 167.306 199.572 3 -6 2 10-317.933 290.385 3 -6 -2 9 22686.7 1617.26 3 -6 2 9 21427.8 1748.89 3 -6 -2 8 9524.42 1020.66 3 -6 2 8 9419.76 1141.21 3 -6 -2 7 7133.40 850.713 3 -6 2 7 7598.88 1003.09 3 -6 -2 6 1682.05 421.795 3 -6 2 6 1814.50 472.364 3 -6 -2 5 3503.66 608.405 3 -6 2 5 4106.27 727.178 3 -6 -2 4 82.1205 109.467 3 -6 2 4 529.790 353.174 3 -6 2 3 22.4703 217.260 3 -6 -2 3 31.3742 159.283 2 -6 -2 3 154.445 125.888 3 -6 2 2 4020.42 714.981 3 -6 -2 2 3172.66 616.968 2 -6 2 1 790.090 314.094 3 -6 -2 1 902.095 411.074 2 -6 2 0 3586.26 683.777 3 -6 -2 0 3841.03 681.157 2 -6 -2 -1 1164.42 383.327 2 -6 2 -1 1652.57 487.211 3 -6 2 -2 2105.05 561.246 1 -6 -2 -2 1420.81 418.975 2 -6 -2 -3 900.927 399.256 2 -6 2 -3 684.083 338.966 1 -6 2 -4 156.649 231.541 1 -6 -2 -4 392.677 411.259 2 -6 2 -5-51.2932 242.382 1 -6 -2 -5-463.268 496.482 2 -6 2 -6-488.310 414.417 1 -6 -2 -6 212.109 420.139 2 -6 2 -7-410.266 375.614 1 -6 -2 -7-317.840 539.585 2 -6 2 -8 84.8517 275.171 1 -6 -2 -8-403.126 436.928 2 -6 2 -9 2967.66 774.249 1 -6 -2 -9 3471.59 934.580 2 -6 2 -10 4799.19 1028.89 1 -6 -2 -10 4953.93 1121.83 2 -6 2 -11 6560.98 1123.14 1 -6 3 14-155.476 243.350 3 -6 3 13 974.008 404.070 3 -6 3 12 278.671 309.552 3 -6 3 11 200.354 158.834 3 -6 3 10 1008.97 440.770 3 -6 3 9 116.235 222.015 3 -6 3 8-205.588 307.385 3 -6 3 7-132.048 199.779 3 -6 3 6-160.376 208.902 3 -6 3 5-128.817 190.935 3 -6 3 4 70.5533 135.060 3 -6 3 3 1649.00 558.656 3 -6 3 2 4584.85 850.312 3 -6 3 1 873.865 270.905 3 -6 -3 1 2274.72 573.872 2 -6 -3 0 139.762 257.717 2 -6 3 0-24.7171 137.011 3 -6 3 -1 412.662 308.631 1 -6 -3 -1 473.678 299.289 2 -6 3 -2 1619.98 549.368 1 -6 -3 -2 823.539 340.155 2 -6 3 -3 205.894 236.692 1 -6 -3 -3-463.479 488.392 2 -6 -3 -4 2942.89 705.387 2 -6 3 -4 3002.51 751.868 1 -6 3 -5 7255.23 1231.29 1 -6 -3 -5 5011.47 990.007 2 -6 3 -6 375.638 370.050 1 -6 -3 -6 205.007 326.878 2 -6 3 -7 3202.86 799.879 1 -6 -3 -7 1712.83 634.435 2 -6 -4 -1-393.635 473.257 2 -7 0 17-187.518 309.325 3 -7 0 16 1304.32 541.189 3 -7 0 15 15.8253 152.248 3 -7 0 14 692.509 367.740 3 -7 0 13-127.254 286.066 3 -7 0 12 635.831 291.741 3 -7 0 11 35.9010 135.368 3 -7 0 10 3369.37 687.125 3 -7 0 9-135.800 254.334 3 -7 0 8 1369.12 473.745 3 -7 0 7-8.30055 144.349 3 -7 0 6 113030. 4126.93 3 -7 0 5 67.3731 191.509 3 -7 0 4 60525.9 1621.92 2 -7 0 4 54295.8 2812.20 3 -7 0 3 33.1761 173.732 3 -7 0 3 45.1024 180.864 2 -7 0 2 5013.77 546.501 2 -7 0 2 5656.07 903.023 3 -7 0 1 73.2141 207.286 3 -7 0 1-166.435 331.962 2 -7 0 0 1621.45 508.777 2 -7 0 0 2355.11 604.643 3 -7 0 -1 29.6841 371.885 2 -7 0 -2 5252.33 871.714 2 -7 0 -2 6511.68 821.126 1 -7 0 -3-113.709 256.348 1 -7 0 -4 6613.86 878.154 1 -7 0 -5 225.347 267.398 1 -7 0 -6 367.976 307.890 1 -7 0 -7-202.660 289.025 1 -7 0 -8 503.259 321.872 1 -7 0 -9-104.141 330.085 1 -7 -1 17-197.448 252.178 3 -7 -1 16 383.441 173.612 3 -7 1 16 198.481 408.121 3 -7 -1 15 322.763 147.351 3 -7 1 15 758.561 376.973 3 -7 -1 14 572.067 283.343 3 -7 1 14 117.070 278.491 3 -7 -1 13 730.234 395.470 3 -7 1 13 650.890 313.301 3 -7 -1 12 2488.92 604.717 3 -7 1 12 1963.62 591.098 3 -7 -1 11 4768.75 811.059 3 -7 1 11 5158.71 914.548 3 -7 -1 10 67.8209 208.808 3 -7 1 10 19.1199 152.698 3 -7 -1 9 1520.31 435.382 3 -7 1 9 1135.28 410.983 3 -7 1 8 5334.69 877.188 3 -7 -1 8 5969.46 897.057 3 -7 -1 7 458.775 281.511 3 -7 1 7 401.294 204.493 3 -7 -1 6 343.603 201.967 3 -7 1 6 257.812 268.655 3 -7 -1 5 8822.76 1072.48 3 -7 1 5 9730.48 1196.32 3 -7 -1 4 35197.7 1585.42 2 -7 -1 4 36482.6 2219.32 3 -7 1 4 33439.2 2223.02 3 -7 -1 3 35353.9 1637.16 2 -7 -1 3 40277.0 2370.13 3 -7 1 3 33944.2 2240.27 3 -7 -1 2 11297.6 960.782 2 -7 -1 2 10501.9 1173.64 3 -7 1 2 12577.0 1370.98 3 -7 1 1 642.304 347.126 3 -7 -1 1 162.557 198.823 2 -7 -1 1 257.689 256.000 3 -7 -1 0 1739.98 440.957 2 -7 1 0 1129.84 412.774 3 -7 -1 -1 8594.40 996.031 2 -7 -1 -1 9351.00 814.400 1 -7 1 -1 10767.8 1342.53 3 -7 1 -2 2338.33 569.332 1 -7 -1 -2 2466.66 663.670 2 -7 -1 -3-209.488 394.387 2 -7 1 -3 132.984 235.734 1 -7 -1 -4 1677.30 615.424 2 -7 1 -4 1606.36 473.111 1 -7 -1 -5-29.7866 446.994 2 -7 1 -5-214.251 192.372 1 -7 -1 -6 1320.65 624.371 2 -7 1 -6 1213.33 444.834 1 -7 -1 -7 1494.72 632.483 2 -7 1 -7 516.764 305.270 1 -7 -1 -8 1901.67 961.280 2 -7 1 -8 402.513 382.129 1 -7 -1 -9 4575.60 1098.21 2 -7 1 -9 2900.64 824.059 1 -7 1 -10 326.059 370.641 1 -7 -1 -10-180.767 693.653 2 -7 1 -11 1442.11 596.932 1 -7 1 -12 15.1644 437.719 1 -7 -2 15 109.345 161.061 3 -7 -2 14 852.617 335.062 3 -7 2 14 1375.30 539.300 3 -7 -2 13-33.1144 322.577 3 -7 2 13 609.584 384.074 3 -7 -2 12 1285.10 466.697 3 -7 2 12 726.717 329.228 3 -7 -2 11 67.1806 199.911 3 -7 2 11 3.61960 195.308 3 -7 -2 10 8696.63 1102.69 3 -7 2 10 9425.20 1253.12 3 -7 -2 9 2280.34 559.357 3 -7 2 9 1350.17 449.936 3 -7 -2 8 7826.74 1000.38 3 -7 2 8 6617.35 1040.21 3 -7 -2 7 191.301 138.968 3 -7 2 7 228.671 217.688 3 -7 -2 6-136.304 221.189 3 -7 2 6 189.919 249.798 3 -7 -2 5 1475.80 422.708 3 -7 2 5 1442.99 497.984 3 -7 2 4 1004.24 485.070 3 -7 -2 4 882.477 357.571 3 -7 2 3 1690.83 522.981 3 -7 -2 3 1452.26 435.606 2 -7 -2 3 1662.41 464.450 3 -7 2 2 1514.79 532.086 3 -7 -2 2 1475.24 454.363 2 -7 -2 1 19470.5 1559.99 2 -7 2 1 24554.3 1999.13 3 -7 -2 0 829.061 357.302 2 -7 2 0 1052.66 446.602 3 -7 2 -1 246.785 246.641 3 -7 -2 -1 407.138 339.271 2 -7 2 -2 822.928 419.416 1 -7 -2 -2 484.518 326.983 2 -7 2 -3 437.357 297.637 1 -7 -2 -3 524.456 295.573 2 -7 -2 -4 1687.03 617.180 2 -7 2 -4 2577.15 687.931 1 -7 2 -5 506.622 392.317 1 -7 -2 -5 42.8486 326.766 2 -7 2 -6 1777.01 633.894 1 -7 -2 -6 1042.09 459.740 2 -7 2 -7 2964.26 760.547 1 -7 -2 -7 3070.52 770.117 2 -7 2 -8 2012.89 659.185 1 -7 -2 -8 2368.40 866.990 2 -7 2 -9 1075.54 544.239 1 -7 -2 -9 2350.56 830.404 2 -7 3 12 998.606 461.399 3 -7 3 11 682.357 363.876 3 -7 3 10-145.789 291.234 3 -7 3 9 3585.54 786.409 3 -7 3 8 1504.45 537.680 3 -7 3 7 1013.66 363.386 3 -7 3 6 493.635 293.493 3 -7 3 5 162.868 191.264 3 -7 3 4-207.189 312.430 3 -7 3 3-264.736 413.587 3 -7 3 2 87.1841 206.989 3 -7 -3 2-177.024 218.055 2 -7 -3 1-111.177 257.842 2 -7 3 1-758.139 385.075 3 -7 -3 0-76.2765 252.504 2 -7 3 0 220.200 300.934 3 -7 3 -1 1065.69 483.302 1 -7 -3 -1 10.0539 258.160 2 -7 -3 -2 220.994 303.715 2 -7 3 -2 403.865 376.073 1 -7 3 -3-622.276 413.000 1 -7 -3 -3 143.230 297.458 2 -7 3 -4 848.097 490.327 1 -7 -3 -4 1067.67 514.672 2 -7 -3 -5 1422.39 542.152 2 -8 0 15 31.0647 177.212 3 -8 0 14-42.2619 395.204 3 -8 0 13 88.2163 153.545 3 -8 0 12 5916.61 1001.58 3 -8 0 11-206.877 266.771 3 -8 0 10 935.576 420.542 3 -8 0 9-177.071 241.415 3 -8 0 8 3289.57 736.709 3 -8 0 7 45.7743 212.641 3 -8 0 6 1137.61 426.945 3 -8 0 5-64.2820 189.078 3 -8 0 4 1756.73 544.992 3 -8 0 3 136.244 160.234 3 -8 0 2 3626.11 750.927 3 -8 0 1-346.494 318.022 3 -8 0 0 635.184 361.739 2 -8 0 0 1427.48 470.848 3 -8 0 -1 376.597 459.686 2 -8 0 -1 37.0992 146.999 1 -8 0 -2 13428.0 1479.84 2 -8 0 -2 12912.0 1226.93 1 -8 0 -3 182.403 537.567 2 -8 0 -3-71.6400 166.622 1 -8 0 -4 76.0084 198.395 1 -8 0 -4 1203.23 706.125 2 -8 0 -5-194.517 614.863 2 -8 0 -5-484.803 309.544 1 -8 0 -6 1399.86 762.526 2 -8 0 -7 634.008 689.992 2 -8 -1 16 634.226 349.601 3 -8 -1 15 265.399 165.609 3 -8 -1 14-173.822 173.059 3 -8 1 14 142.405 273.375 3 -8 -1 13 438.895 299.319 3 -8 1 13 529.262 363.010 3 -8 -1 12 799.430 290.684 3 -8 1 12 544.359 346.012 3 -8 -1 11 191.017 153.897 3 -8 1 11-104.814 213.920 3 -8 -1 10 3863.32 808.707 3 -8 1 10 3894.58 848.112 3 -8 -1 9 2084.55 566.509 3 -8 1 9 1810.36 554.335 3 -8 -1 8 363.133 284.416 3 -8 1 8 490.439 308.873 3 -8 -1 7 5179.32 917.495 3 -8 1 7 5033.93 920.454 3 -8 -1 6 4309.51 778.508 3 -8 1 6 4006.77 823.826 3 -8 -1 5 5687.42 951.750 3 -8 1 5 6247.13 1037.63 3 -8 -1 4 2680.02 657.727 3 -8 1 4 2682.13 662.214 3 -8 -1 3 4785.64 857.020 3 -8 1 3 3761.29 796.334 3 -8 1 2-123.694 280.345 3 -8 -1 2 420.406 288.333 3 -8 1 1 1601.87 545.325 3 -8 -1 1 1068.01 341.861 2 -8 -1 0 58.9947 298.594 2 -8 1 0 372.166 330.003 3 -8 -1 -1-40.6034 347.677 2 -8 1 -2 766.630 288.564 1 -8 -1 -2 227.925 354.060 2 -8 1 -3 693.339 384.895 1 -8 -1 -3 1039.72 441.348 2 -8 -1 -4 5755.94 1028.02 2 -8 1 -4 4526.51 829.989 1 -8 -1 -5-254.797 705.350 2 -8 1 -5 1169.45 468.903 1 -8 -1 -6 1095.83 749.190 2 -8 1 -6 123.995 412.558 1 -8 -1 -7 420.058 562.542 2 -8 1 -7 1696.26 628.406 1 -8 -1 -8 1228.02 764.454 2 -8 1 -8 2887.65 749.864 1 -8 1 -9 867.937 665.008 1 -8 1 -10 965.270 554.457 1 -8 -2 13 1841.24 495.612 3 -8 -2 12-234.832 386.882 3 -8 2 12 491.435 288.183 3 -8 -2 11 263.338 304.198 3 -8 2 11-103.533 233.599 3 -8 -2 10-220.144 305.142 3 -8 2 10-79.8849 249.887 3 -8 -2 9 467.045 346.734 3 -8 2 9-220.716 367.822 3 -8 -2 8 289.401 225.588 3 -8 2 8 703.016 439.271 3 -8 -2 7 189.931 324.911 3 -8 2 7 153.889 301.856 3 -8 -2 6 1397.86 417.094 3 -8 2 6 1677.47 545.088 3 -8 2 5 384.740 290.111 3 -8 -2 5 314.464 195.999 3 -8 2 4 3525.04 800.046 3 -8 -2 4 4227.20 822.643 3 -8 2 3 11631.4 1478.30 3 -8 -2 2 16505.7 1428.97 2 -8 2 2 20585.3 1955.48 3 -8 -2 1 1850.07 505.523 2 -8 2 1 2389.98 712.099 3 -8 -2 0-6.22370 243.153 2 -8 2 0 633.975 484.047 3 -8 2 -1-48.0046 180.571 1 -8 -2 -1 577.562 341.681 2 -8 2 -2 811.420 500.240 1 -8 -2 -2 1381.25 538.056 2 -8 2 -3-228.218 320.218 1 -8 -2 -3 1217.80 470.636 2 -8 2 -4-849.859 455.816 1 -8 -2 -4 45.7420 383.211 2 -8 2 -5-65.2627 248.982 1 -8 -2 -5 2.84007 379.217 2 -8 -2 -6 3147.62 831.533 2 -8 2 -6 1939.93 581.916 1 -8 -2 -7-710.929 505.368 2 -8 3 9 2926.29 754.189 3 -8 3 8 71.7764 258.085 3 -8 3 7 6185.14 1153.61 3 -8 3 6 1015.25 474.928 3 -8 3 5-101.178 287.290 3 -8 3 4 418.541 241.445 3 -8 3 3 377.348 312.380 3 -8 3 2 1347.13 540.778 3 -8 -3 1 3373.90 728.775 2 -8 3 1 5625.73 1109.65 3 -8 -3 0 5762.50 991.312 2 -8 -3 -1 3153.38 750.590 2 -8 -3 -2 26.0748 315.951 2 -8 -3 -3 874.182 445.301 2 -9 0 12 1147.13 485.986 3 -9 0 11 220.786 273.878 3 -9 0 10 3719.38 840.752 3 -9 0 9-371.444 374.549 3 -9 0 8 1129.30 509.124 3 -9 0 7-160.293 341.836 3 -9 0 6 2936.67 735.664 3 -9 0 5-189.282 283.954 3 -9 0 4 1094.25 491.014 3 -9 0 3 228.310 226.456 3 -9 0 2 129.752 165.395 3 -9 0 1-398.237 430.693 3 -9 0 -5-309.196 774.500 2 -9 0 -6-318.838 713.651 2 -9 0 -7-371.700 1002.10 2 -9 -1 13 1543.02 581.107 3 -9 -1 12 1332.39 590.350 3 -9 -1 11-105.250 324.758 3 -9 -1 10 187.528 270.044 3 -9 1 10 37.6410 188.910 3 -9 -1 9 827.065 482.053 3 -9 1 9-314.064 261.320 3 -9 -1 8 1492.67 393.117 3 -9 1 8 1591.89 539.827 3 -9 -1 7 2241.97 684.132 3 -9 1 7 1999.87 565.354 3 -9 -1 6-12.4000 266.292 3 -9 1 6-115.841 290.674 3 -9 -1 5 6894.52 1139.98 3 -9 1 5 8673.60 1316.00 3 -9 -1 4-101.048 282.072 3 -9 1 4 92.6214 274.984 3 -9 1 3 1865.99 665.909 3 -9 -1 3 1759.90 580.345 3 -9 1 2 270.239 293.924 3 -9 1 1 3175.71 776.424 3 -9 1 -1 52.3477 360.054 1 -9 1 -2 261.036 383.756 1 -9 1 -3 407.903 324.645 1 -9 1 -4-429.921 390.350 1 -9 -1 -4-1107.73 828.490 2 -9 1 -5 256.172 249.351 1 -9 -1 -5 1620.11 474.597 2 -9 -1 -6-224.430 566.489 2 -9 1 -6 868.525 446.782 1 -9 -1 -7-723.994 736.883 2 -9 1 -7-567.181 420.499 1 -9 -2 11 735.653 370.055 3 -9 -2 10 1322.30 562.893 3 -9 -2 9 456.457 316.214 3 -9 -2 8 456.477 299.506 3 -9 -2 7 1853.59 556.168 3 -9 2 7 1963.92 668.948 3 -9 2 6 7230.65 1219.74 3 -9 -2 6 6733.42 1075.00 3 -9 2 5 2255.19 684.635 3 -9 -2 5 1945.43 618.995 3 -9 2 4-109.258 347.519 3 -9 2 3 83.9596 374.357 3 -9 2 2-185.617 230.502 3 -9 2 1 867.946 483.582 3 -9 2 -1 752.228 454.053 1 -9 -2 -3 1576.80 655.556 2 -9 -2 -4-116.740 327.356 2 -9 -2 -5 562.641 459.954 2 -10 -1 7 74.6387 222.706 3 -10 -1 6 3534.70 917.547 3 -10 -1 5 2347.41 672.123 3 -10 -1 4 2826.77 888.168 3 -10 1 0 307.701 233.211 1 -10 1 -1 484.291 219.208 1 -10 1 -2 1364.49 455.902 1 -10 -2 6 551.065 357.237 3 0 0 0 0.00 0.00 0 TITL BKS-SS-DI-ANTH-223K-ss in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 7.887631 3.943396 15.757786 90.0000 102.6236 90.0000 ZERR 2.00 0.000696 0.000446 0.001900 0.0000 0.0107 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H O UNIT 24.00 16.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 60846 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.4358(2) 0.6535(4) 0.41510(12) 0.0335(5) Uani 1 1 d . . . . . C7 C 0.3262(2) 0.6395(4) 0.47404(12) 0.0332(5) Uani 1 1 d . . . . . C1 C 0.6149(2) 0.5131(4) 0.43848(13) 0.0371(5) Uani 1 1 d . . . . . C5 C 0.1001(2) 0.9146(5) 0.36856(15) 0.0455(6) Uani 1 1 d . . . . . H5 H -0.013066 1.003271 0.352945 0.055 Uiso 1 1 calc R U . . . O1 O 0.71086(18) 0.5233(4) 0.38685(10) 0.0598(5) Uani 1 1 d . . . . . C3 C 0.3752(2) 0.7987(5) 0.33334(13) 0.0423(5) Uani 1 1 d . . . . . H3 H 0.448283 0.809124 0.293613 0.051 Uiso 1 1 calc R U . . . C6 C 0.1581(2) 0.7717(5) 0.44958(13) 0.0415(5) Uani 1 1 d . . . . . H6 H 0.083800 0.763036 0.488767 0.050 Uiso 1 1 calc R U . . . C4 C 0.2076(3) 0.9280(5) 0.31027(14) 0.0467(6) Uani 1 1 d . . . . . H4 H 0.167433 1.024577 0.254994 0.056 Uiso 1 1 calc R U . . . 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 C2 0.0344(10) 0.0325(10) 0.0326(11) -0.0041(8) 0.0055(8) -0.0037(8) C7 0.0314(9) 0.0306(10) 0.0374(12) -0.0043(8) 0.0070(8) -0.0024(7) C1 0.0334(10) 0.0430(11) 0.0369(12) -0.0039(8) 0.0116(9) -0.0038(8) C5 0.0360(10) 0.0421(13) 0.0533(15) -0.0024(10) -0.0010(9) 0.0034(9) O1 0.0466(9) 0.0922(12) 0.0470(10) 0.0111(8) 0.0240(8) 0.0111(8) C3 0.0462(12) 0.0451(12) 0.0359(12) -0.0007(9) 0.0098(9) -0.0021(9) C6 0.0331(10) 0.0445(13) 0.0470(13) -0.0029(9) 0.0091(9) 0.0004(8) C4 0.0528(13) 0.0442(12) 0.0381(13) 0.0023(9) -0.0012(10) 0.0025(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 _geom_angle_publ_flag C7 C2 C1 120.77(17) . . ? C3 C2 C7 119.44(17) . . ? C3 C2 C1 119.78(16) . . ? C2 C7 C1 121.23(16) . 3_666 ? C6 C7 C2 119.21(18) . . ? C6 C7 C1 119.56(17) . 3_666 ? C7 C1 C2 118.00(15) 3_666 . ? O1 C1 C2 120.93(18) . . ? O1 C1 C7 121.07(17) . 3_666 ? C6 C5 H5 119.9 . . ? C6 C5 C4 120.27(18) . . ? C4 C5 H5 119.9 . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.44(18) . . ? C4 C3 H3 119.8 . . ? C7 C6 H6 119.7 . . ? C5 C6 C7 120.67(18) . . ? C5 C6 H6 119.7 . . ? C5 C4 C3 120.0(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? 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 C2 C7 1.401(2) . ? C2 C1 1.487(2) . ? C2 C3 1.395(3) . ? C7 C1 1.483(3) 3_666 ? C7 C6 1.398(2) . ? C1 O1 1.227(2) . ? C5 H5 0.9400 . ? C5 C6 1.379(3) . ? C5 C4 1.381(3) . ? C3 H3 0.9400 . ? C3 C4 1.389(3) . ? C6 H6 0.9400 . ? C4 H4 0.9400 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C7 C6 C5 0.0(3) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C7 C2 C1 C7 -0.4(3) . . . 3_666 ? C7 C2 C1 O1 179.61(17) . . . . ? C7 C2 C3 C4 -0.1(3) . . . . ? C1 C2 C7 C1 0.4(3) . . . 3_666 ? C1 C2 C7 C6 -179.50(15) . . . . ? C1 C2 C3 C4 179.38(16) . . . . ? C1 C7 C6 C5 -179.94(17) 3_666 . . . ? C3 C2 C7 C1 179.90(16) . . . 3_666 ? C3 C2 C7 C6 0.0(3) . . . . ? C3 C2 C1 C7 -179.88(16) . . . 3_666 ? C3 C2 C1 O1 0.1(3) . . . . ? C6 C5 C4 C3 -0.3(3) . . . . ? C4 C5 C6 C7 0.2(3) . . . . ?