#------------------------------------------------------------------------------ #$Date: 2021-11-03 23:16:36 +0200 (Wed, 03 Nov 2021) $ #$Revision: 270252 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/91/4519112.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_4519112 loop_ _publ_author_name 'Yamazaki, Shoko' 'Katayama, Kohtaro' 'Wang, Zhichao' 'Mikata, Yuji' 'Morimoto, Tsumoru' 'Ogawa, Akiya' _publ_section_title ; Sequential Knoevenagel Condensation/Cyclization for the Synthesis of Indene and Benzofulvene Derivatives. ; _journal_issue 42 _journal_name_full 'ACS omega' _journal_page_first 28441 _journal_page_last 28454 _journal_paper_doi 10.1021/acsomega.1c05283 _journal_volume 6 _journal_year 2021 _chemical_formula_moiety 'C20 H15 Cl O4' _chemical_formula_sum 'C20 H15 Cl O4' _chemical_formula_weight 354.79 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 94.097(3) _cell_angle_gamma 90.0000 _cell_formula_units_Z 4 _cell_length_a 10.601(3) _cell_length_b 7.695(2) _cell_length_c 20.430(6) _cell_measurement_reflns_used 5199 _cell_measurement_temperature 153 _cell_measurement_theta_max 27.52 _cell_measurement_theta_min 3.00 _cell_volume 1662.3(8) _computing_cell_refinement CrystalClear _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction CrystalClear _computing_molecular_graphics 'CrystalStructure 4.2.5' _computing_publication_material 'CrystalStructure 4.2.5 (Rigaku, 2017)' _computing_structure_refinement 'SHELXL Version 2016/6 (Sheldrick, 2008)' _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _diffrn_ambient_temperature 153 _diffrn_detector_area_resol_mean 7.314 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 12333 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_min 3.274 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_description unknown _exptl_crystal_F_000 736.00 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _refine_diff_density_max 0.30 _refine_diff_density_min -0.26 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment refxyz _refine_ls_number_parameters 286 _refine_ls_number_reflns 3782 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0356 _refine_ls_shift/su_max 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.4760P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0928 _refine_ls_wR_factor_ref 0.0958 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3519 _reflns_number_total 3782 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ao1c05283_si_002.cif _cod_data_source_block 1126X-1-201130 _cod_database_code 4519112 _shelx_res_file ; TITL 1126X-1-201130 shelxl.res created by SHELXL-2016/6 at 10:53:54 on 30-Nov-2020 CELL 0.71075 10.60110 7.69510 20.43000 90.00000 94.09700 90.00000 ZERR 4 0.00310 0.00220 0.00600 0.00000 0.00260 0.00000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC C H CL O UNIT 80 60 4 16 L.S. 5 FMAP 2 PLAN 15 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -119.8 ACTA SIZE 0.400 0.400 0.600 WGHT 0.051900 0.476000 FVAR 0.83758 CL1 3 0.277565 0.103010 1.148128 11.00000 0.03682 0.04425 = 0.02438 0.00419 0.00943 -0.00126 O1 4 0.822234 0.495889 1.016008 11.00000 0.03625 0.03045 = 0.03621 -0.01106 -0.00465 -0.00028 O2 4 0.870489 0.223439 0.989015 11.00000 0.02723 0.02491 = 0.02665 -0.00023 -0.00693 -0.00125 O3 4 0.702401 0.390972 0.805581 11.00000 0.02937 0.06330 = 0.02169 0.00484 -0.00054 -0.00861 O4 4 0.875044 0.471871 0.867629 11.00000 0.02677 0.04026 = 0.02375 -0.00046 0.00404 -0.00889 C1 1 0.591479 0.304853 0.930100 11.00000 0.02342 0.02066 = 0.02113 0.00126 0.00008 0.00132 C2 1 0.495766 0.264552 0.877119 11.00000 0.02348 0.02585 = 0.02139 0.00114 0.00005 0.00008 C3 1 0.390821 0.199380 0.901974 11.00000 0.02338 0.02086 = 0.01992 0.00036 0.00014 0.00133 C4 1 0.331708 0.144443 1.021705 11.00000 0.02396 0.02225 = 0.02441 0.00047 0.00186 0.00054 C5 1 0.374738 0.166098 1.087159 11.00000 0.02976 0.02403 = 0.02178 0.00251 0.00582 0.00374 C6 1 0.491307 0.237790 1.105640 11.00000 0.03216 0.02916 = 0.01910 -0.00004 -0.00021 0.00209 C7 1 0.571637 0.287105 1.057526 11.00000 0.02639 0.02655 = 0.02201 -0.00086 -0.00180 -0.00032 C8 1 0.531480 0.265264 0.992094 11.00000 0.02233 0.01916 = 0.02091 0.00118 0.00046 0.00166 C9 1 0.409938 0.198824 0.974497 11.00000 0.02372 0.01846 = 0.01969 0.00039 -0.00022 0.00246 C10 1 0.711291 0.358053 0.923172 11.00000 0.02352 0.02202 = 0.02160 -0.00048 0.00061 0.00119 C11 1 0.806090 0.371689 0.981186 11.00000 0.02148 0.02463 = 0.02050 0.00006 0.00227 -0.00315 C12 1 0.963932 0.220526 1.044330 11.00000 0.03274 0.03549 = 0.03222 0.00550 -0.01332 -0.00399 C13 1 0.757980 0.405733 0.858572 11.00000 0.02294 0.02721 = 0.02480 0.00026 0.00224 -0.00016 C14 1 0.930698 0.528595 0.808540 11.00000 0.03693 0.04612 = 0.02816 0.00029 0.01082 -0.01104 C15 1 0.277679 0.138023 0.862648 11.00000 0.02555 0.02121 = 0.01941 0.00133 -0.00104 -0.00125 C16 1 0.291348 0.049490 0.803904 11.00000 0.02966 0.03381 = 0.02545 -0.00486 0.00160 0.00071 C17 1 0.186257 -0.002659 0.764492 11.00000 0.04137 0.03921 = 0.02665 -0.01094 -0.00362 -0.00158 C18 1 0.065884 0.031234 0.783453 11.00000 0.03273 0.03462 = 0.03208 -0.00360 -0.00942 -0.00539 C19 1 0.051137 0.118365 0.841867 11.00000 0.02343 0.03177 = 0.03305 0.00072 -0.00222 -0.00094 C20 1 0.155965 0.172322 0.881167 11.00000 0.02656 0.02466 = 0.02386 -0.00285 0.00097 -0.00114 H1 2 0.507141 0.278437 0.829510 11.00000 0.02760 H2 2 0.252282 0.094140 1.010498 11.00000 0.03002 H3 2 0.516604 0.254253 1.150416 11.00000 0.03311 H4 2 0.654357 0.338909 1.071115 11.00000 0.03763 H5 2 1.025438 0.311005 1.039297 11.00000 0.04699 H6 2 1.005549 0.106077 1.041546 11.00000 0.04575 H7 2 0.918458 0.230357 1.083912 11.00000 0.04328 H8 2 1.014904 0.563693 0.822859 11.00000 0.05729 H9 2 0.932159 0.434650 0.778389 11.00000 0.04339 H10 2 0.885399 0.626243 0.789828 11.00000 0.06028 H11 2 0.375843 0.022400 0.791171 11.00000 0.03059 H12 2 0.197653 -0.063295 0.724369 11.00000 0.05473 H13 2 -0.005733 -0.003974 0.755316 11.00000 0.04374 H14 2 -0.031956 0.140769 0.854623 11.00000 0.03397 H15 2 0.142154 0.235865 0.921096 11.00000 0.02610 HKLF 4 REM 1126X-1-201130 REM R1 = 0.0356 for 3519 Fo > 4sig(Fo) and 0.0384 for all 3782 data REM 286 parameters refined using 0 restraints END WGHT 0.0519 0.4760 REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+1, -z+2 HTAB C12 O1_$1 REM Highest difference peak 0.299, deepest hole -0.264, 1-sigma level 0.043 Q1 1 0.3865 0.2010 0.9352 11.00000 0.05 0.30 Q2 1 0.3522 0.1715 1.0557 11.00000 0.05 0.25 Q3 1 0.5456 0.2890 0.9007 11.00000 0.05 0.24 Q4 1 0.5263 0.2734 1.0833 11.00000 0.05 0.23 Q5 1 0.5668 0.2864 0.9666 11.00000 0.05 0.23 Q6 1 0.3402 0.1618 0.8840 11.00000 0.05 0.23 Q7 1 0.7326 0.3761 0.8932 11.00000 0.05 0.22 Q8 1 0.7624 0.3643 0.9490 11.00000 0.05 0.22 Q9 1 0.5433 0.3071 1.0218 11.00000 0.05 0.22 Q10 1 0.4457 0.2247 0.8859 11.00000 0.05 0.21 Q11 1 0.4647 0.2358 0.9857 11.00000 0.05 0.21 Q12 1 0.2740 0.1024 0.8313 11.00000 0.05 0.21 Q13 1 0.6500 0.3479 0.9284 11.00000 0.05 0.20 Q14 1 0.2319 0.0132 0.7861 11.00000 0.05 0.20 Q15 1 0.4209 0.2143 1.0947 11.00000 0.05 0.20 ; _shelx_res_checksum 99668 _shelx_hkl_file ; 0 0 4 1046.95 10.02 0 0 -4 1065.73 10.28 0 0 4 1035.45 9.11 0 0 -4 1041.37 9.28 0 0 5 1.43 1.00 0 0 -5 3.98 1.88 0 0 5 0.68 0.42 0 0 -5 2.25 0.86 0 0 6 5416.47 46.38 0 0 -6 5593.23 48.01 0 0 7 0.76 0.58 0 0 -7 -0.49 1.83 0 0 -7 -0.24 0.63 0 0 -8 3097.67 28.57 0 0 8 3046.13 26.12 0 0 -8 3086.37 26.50 0 0 -9 0.71 1.37 0 0 -9 0.62 0.23 0 0 -10 122.43 3.52 0 0 10 118.76 5.25 0 0 -10 123.12 3.24 0 0 -11 -0.40 1.25 0 0 11 0.38 0.30 0 0 -11 0.78 0.37 0 0 -12 52.05 6.79 0 0 12 44.76 2.09 0 0 -12 47.43 1.96 0 0 -13 -0.61 1.75 0 0 13 1.28 0.32 0 0 -13 0.33 0.78 0 0 -14 1849.81 26.29 0 0 14 1754.80 20.36 0 0 -14 1864.08 21.21 0 0 -16 0.03 1.64 0 0 -16 0.49 0.38 0 0 -17 0.40 0.51 0 0 -17 0.97 0.73 0 0 -18 1018.50 15.07 0 0 -18 1024.20 11.68 0 0 -20 118.13 16.26 0 0 -21 0.98 1.21 0 0 -22 39.41 7.07 0 0 -23 2.74 0.95 0 0 -24 621.39 13.69 0 0 -26 2.15 1.87 0 1 -2 2309.32 19.83 0 1 2 2222.50 19.14 0 1 2 2230.74 19.50 0 -1 2 2275.56 19.53 0 -1 -2 2268.57 19.56 0 -1 -2 2299.77 19.97 0 -1 2 2311.90 19.58 0 1 -3 2031.66 18.31 0 1 3 2011.58 17.78 0 1 3 1976.59 17.48 0 -1 3 1977.52 17.41 0 -1 -3 1990.90 17.61 0 -1 -3 1995.73 17.71 0 -1 3 2003.54 17.01 0 1 -4 259.49 5.32 0 1 4 256.43 5.30 0 1 4 254.72 5.21 0 -1 4 255.24 5.15 0 -1 -4 255.44 5.23 0 -1 -4 269.18 5.56 0 -1 4 259.00 4.74 0 1 -5 73.98 1.58 0 1 -5 72.54 3.38 0 1 5 73.22 2.23 0 1 5 67.68 1.92 0 -1 -5 73.18 2.21 0 -1 -5 71.87 2.12 0 -1 5 71.96 2.13 0 -1 5 72.67 1.59 0 1 -6 71.59 5.13 0 1 6 61.19 2.93 0 1 6 70.92 3.26 0 -1 6 65.46 2.11 0 -1 -6 66.13 2.82 0 -1 -6 70.67 4.34 0 1 -7 97.48 2.95 0 1 7 93.55 2.79 0 1 -7 93.76 2.05 0 1 7 91.88 2.45 0 1 -7 94.17 1.99 0 -1 7 89.72 2.99 0 -1 -7 88.90 4.00 0 -1 -7 91.22 2.49 0 1 -8 35.93 2.17 0 1 -8 35.52 1.10 0 1 8 32.67 4.96 0 1 -8 36.42 1.14 0 -1 -8 42.20 5.25 0 -1 -8 34.03 1.95 0 1 -9 1.06 0.69 0 1 -9 1.31 0.26 0 1 -9 1.34 0.26 0 1 9 1.64 0.51 0 -1 -9 1.74 0.64 0 1 -10 760.64 9.03 0 1 -10 763.27 6.30 0 1 -10 770.41 6.80 0 -1 -10 785.34 8.04 0 -1 -10 766.56 9.19 0 1 -11 739.37 9.32 0 1 -11 713.92 7.57 0 1 11 719.36 7.50 0 1 -11 746.85 6.46 0 -1 -11 707.95 8.95 0 1 -12 797.20 6.54 0 1 -12 780.98 6.43 0 -1 -12 779.35 9.47 0 1 -13 672.11 9.38 0 1 -13 669.66 5.90 0 1 -13 677.50 6.07 0 -1 -13 697.91 8.73 0 -1 -13 672.43 9.10 0 1 -14 0.65 0.62 0 1 -14 0.28 0.42 0 1 -14 1.90 1.13 0 -1 -14 6.65 2.28 0 1 -15 650.88 14.13 0 1 -15 657.49 11.27 0 1 -15 661.92 10.91 0 -1 -15 664.46 12.11 0 -1 -15 649.80 13.82 0 1 -16 577.03 11.70 0 1 -16 591.95 7.24 0 1 -16 592.09 7.68 0 -1 -16 600.92 8.85 0 -1 -16 583.31 13.38 0 1 -17 248.06 3.10 0 -1 -17 262.99 4.46 0 1 -18 1195.23 18.47 0 -1 -18 1262.12 15.51 0 -1 -19 322.96 6.25 0 -1 -20 83.07 6.40 0 1 -21 56.28 8.95 0 -1 -21 57.13 8.10 0 1 -22 63.32 8.31 0 -1 -22 64.43 10.70 0 1 -23 41.61 8.20 0 -1 -23 39.67 8.26 0 1 -24 1.94 0.95 0 -1 -24 0.62 0.89 0 1 -25 1.89 1.05 0 -1 -25 0.94 0.83 0 1 -26 55.49 10.05 0 -1 -26 63.39 9.39 0 2 0 1295.27 12.23 0 2 0 1300.88 12.50 0 -2 0 1291.40 11.92 0 -2 0 1314.02 12.89 0 2 1 1098.73 10.47 0 2 -1 1088.01 10.67 0 2 -1 1100.00 10.50 0 2 1 1072.75 10.79 0 -2 1 1075.33 10.30 0 -2 -1 1102.60 11.64 0 -2 1 1093.04 10.82 0 2 -3 1264.55 12.08 0 2 3 1275.36 12.21 0 2 3 1236.93 12.32 0 -2 3 1244.25 11.84 0 -2 -3 1268.55 12.45 0 -2 -3 1279.63 12.84 0 -2 3 1279.17 12.06 0 2 -4 351.24 6.86 0 2 4 361.32 7.05 0 2 4 345.89 6.95 0 -2 4 349.52 6.79 0 -2 -4 356.24 6.99 0 -2 -4 359.64 7.66 0 -2 4 352.67 6.62 0 2 -5 10.11 1.54 0 2 5 11.04 1.76 0 2 5 7.44 1.00 0 -2 5 8.79 1.62 0 -2 -5 8.48 2.07 0 -2 -5 9.62 2.00 0 -2 5 10.71 1.92 0 2 -6 1126.46 9.59 0 2 -6 1161.47 10.96 0 2 6 1128.14 12.10 0 2 6 1105.30 10.58 0 -2 -6 1146.58 10.96 0 -2 -6 1145.20 10.99 0 -2 6 1117.04 10.51 0 -2 6 1156.87 9.70 0 2 -7 235.32 4.06 0 2 -7 232.65 2.91 0 2 7 226.04 3.89 0 -2 -7 231.66 5.02 0 -2 -7 236.98 4.23 0 -2 7 235.82 2.93 0 2 -8 10.64 2.23 0 2 -8 9.79 1.44 0 -2 -8 10.25 1.85 0 -2 -8 9.23 3.25 0 -2 8 10.64 1.45 0 2 -9 152.48 3.63 0 2 -9 154.77 2.22 0 -2 -9 151.74 4.00 0 -2 -9 146.98 6.25 0 -2 9 150.68 2.39 0 2 -10 221.28 4.62 0 2 -10 220.09 3.01 0 2 -10 229.05 3.15 0 -2 -10 212.55 4.29 0 -2 -10 222.35 4.66 0 2 -11 292.59 5.33 0 2 -11 303.12 3.24 0 2 -11 312.11 3.28 0 -2 -11 308.98 5.33 0 -2 -11 305.59 6.22 0 2 -12 240.38 5.45 0 2 -12 242.26 2.60 0 2 -12 243.15 2.46 0 -2 -12 237.89 4.88 0 2 -13 14.86 2.30 0 2 -13 5.88 1.00 0 2 -13 12.60 1.75 0 -2 -13 10.92 3.22 0 -2 -13 9.05 3.45 0 2 -14 225.49 5.35 0 2 -14 212.77 6.23 0 2 -14 220.42 2.16 0 -2 -14 228.51 7.05 0 -2 -14 204.89 4.93 0 2 -15 1014.44 19.76 0 2 -15 1043.60 16.11 0 2 -15 1077.57 16.53 0 2 -16 9.29 2.04 0 2 -16 3.26 0.64 0 2 -17 279.53 6.81 0 -2 -17 271.97 6.82 0 -2 -17 268.80 5.94 0 2 -18 419.17 14.20 0 -2 -18 403.62 10.57 0 -2 -18 440.93 8.42 0 2 -19 263.83 18.00 0 -2 -19 234.02 6.91 0 -2 -19 255.24 8.11 0 2 -20 1.94 1.57 0 -2 -20 3.72 2.03 0 -2 -20 5.52 1.85 0 2 -21 10.06 1.84 0 -2 -21 13.36 3.01 0 -2 -21 10.01 2.04 0 2 -22 40.50 7.26 0 -2 -22 35.38 6.95 0 2 -23 33.77 6.87 0 -2 -23 29.37 5.55 0 2 -24 30.82 5.86 0 -2 -24 27.79 4.63 0 2 -25 129.78 12.38 0 -2 -25 121.67 10.82 0 3 0 -1.16 0.72 0 3 0 1.49 0.62 0 -3 0 0.10 0.32 0 -3 0 1.70 0.68 0 3 1 3621.15 27.86 0 3 1 3662.85 28.11 0 3 -1 3702.57 28.11 0 3 -1 3670.91 28.66 0 -3 1 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8 6 -3 88.53 15.25 8 -6 -3 100.73 13.12 -8 -6 3 94.60 11.12 8 6 -2 96.00 8.36 8 -6 -2 94.68 11.85 -8 -6 2 85.53 16.18 8 6 -1 50.98 6.00 8 -6 -1 43.83 9.35 -8 -6 1 43.57 8.41 8 6 0 119.38 16.43 8 -6 0 126.40 5.95 -8 -6 0 116.25 16.79 8 6 1 38.53 4.20 8 -6 1 32.32 7.77 -8 -6 -1 37.70 7.13 8 6 2 16.16 3.53 8 -6 2 13.20 2.73 -8 -6 -2 14.05 2.38 8 6 3 112.75 10.40 8 -6 3 93.09 16.35 -8 -6 -3 113.62 9.75 8 6 4 83.47 11.91 8 -6 4 88.07 8.47 -8 -6 -4 89.24 16.42 8 6 5 31.89 5.87 8 -6 5 24.39 5.99 -8 -6 -5 34.81 10.27 8 6 6 165.72 14.45 8 -6 6 158.55 7.83 -8 -6 -6 174.77 14.02 8 6 7 38.70 7.53 -8 -6 -7 37.08 6.39 8 6 8 11.93 2.43 -8 -6 -8 4.92 1.01 8 6 9 8.35 1.74 -8 -6 -9 10.34 1.79 8 6 10 49.81 6.39 -8 -6 -10 50.47 10.14 8 6 11 196.58 16.37 -8 -6 -11 209.88 13.20 8 6 12 3.18 2.26 -8 -6 -12 5.42 1.78 8 6 13 177.44 14.38 -8 -6 -13 188.97 14.60 8 7 -12 17.11 3.09 8 -7 -12 13.09 2.67 -8 -7 12 10.12 2.53 8 7 -11 20.27 4.08 8 -7 -11 24.87 4.33 -8 -7 11 16.37 3.90 8 7 -10 123.41 21.46 8 -7 -10 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221.29 6.94 11 -1 -10 233.55 7.08 11 1 -9 92.42 10.53 11 1 -9 98.45 13.59 11 -1 -9 82.79 13.71 11 1 -8 25.61 5.05 11 1 -8 21.31 4.25 11 -1 -8 24.45 4.50 11 1 -7 24.65 5.28 11 1 -7 24.21 6.16 11 -1 -7 26.65 5.03 11 1 -6 46.39 8.30 11 1 -6 46.45 10.50 11 -1 -6 52.30 9.67 11 1 -5 32.35 6.13 11 1 -5 27.09 5.33 11 -1 -5 37.22 6.31 11 1 -4 545.26 13.34 11 1 -4 497.92 14.94 11 -1 -4 510.07 16.47 11 1 -3 240.88 7.64 11 1 -3 219.56 12.77 11 -1 -3 235.49 7.99 11 1 -2 166.30 6.10 11 1 -2 158.10 6.22 11 -1 -2 160.37 6.29 11 1 -1 203.01 8.41 11 1 -1 192.74 6.85 11 -1 -1 192.24 6.83 11 1 0 60.36 9.50 11 1 0 55.53 10.27 11 -1 0 55.12 11.73 11 1 1 26.13 5.09 11 1 1 24.22 4.81 11 -1 1 24.93 4.42 11 1 2 152.24 6.10 11 1 2 128.01 5.04 11 -1 2 139.43 10.89 11 1 3 9.05 2.38 11 1 3 10.09 1.64 11 -1 3 7.53 1.90 11 1 4 103.34 12.47 11 1 4 97.15 4.22 11 -1 4 94.00 8.25 11 1 5 460.19 12.74 11 1 5 402.27 10.48 11 -1 5 426.63 11.20 11 1 6 14.60 3.44 11 1 6 14.13 2.68 11 -1 6 14.44 2.37 11 1 7 19.14 4.52 11 1 7 16.17 3.31 11 -1 7 19.44 4.34 11 1 8 13.24 2.63 11 1 8 8.92 1.89 11 -1 8 7.27 2.02 11 1 9 1.82 0.91 11 1 9 1.44 0.53 11 1 10 123.79 4.81 11 1 10 100.63 4.09 11 1 11 43.55 9.50 11 1 12 12.59 3.26 11 1 13 0.07 0.72 11 1 14 26.13 6.05 11 2 -16 26.17 6.58 11 2 -16 24.66 6.20 11 -2 -16 26.35 6.54 11 2 -15 0.20 1.34 11 2 -15 2.10 1.33 11 -2 -15 2.26 1.70 11 2 -14 93.65 11.48 11 2 -14 98.05 18.07 11 -2 -14 92.59 11.66 11 2 -13 9.99 2.28 11 2 -13 13.54 2.74 11 -2 -13 12.88 2.56 11 2 -12 85.21 11.39 11 2 -12 97.10 7.38 11 -2 -12 91.38 9.05 11 2 -11 7.38 1.75 11 2 -11 8.60 1.80 11 -2 -11 3.92 1.49 11 2 -10 61.24 13.25 11 2 -10 64.97 13.14 11 -2 -10 69.38 14.28 11 2 -9 58.93 10.83 11 2 -9 63.93 13.34 11 -2 -9 63.36 11.26 11 2 -8 224.82 7.12 11 2 -8 205.72 11.73 11 -2 -8 221.24 22.09 11 2 -7 3.49 2.46 11 2 -7 1.75 1.05 11 -2 -7 3.87 1.07 11 2 -6 4.64 1.30 11 2 -6 6.18 1.22 11 -2 -6 7.49 1.14 11 2 -5 1.09 0.98 11 2 -5 0.67 0.81 11 -2 -5 2.97 2.19 11 2 -4 0.82 1.13 11 2 -4 1.01 0.78 11 -2 -4 0.79 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78.52 10.76 11 4 -2 5.48 1.69 11 -4 -2 4.77 1.72 -11 -4 2 7.85 1.76 11 4 -1 295.41 7.62 11 -4 -1 300.37 7.79 -11 -4 1 303.52 27.84 11 4 0 27.18 5.66 11 -4 0 28.45 4.08 -11 -4 0 27.01 5.13 11 4 1 51.24 9.51 11 -4 1 46.63 10.19 -11 -4 -1 50.70 9.39 11 4 2 2.85 1.60 11 -4 2 1.85 1.19 -11 -4 -2 2.27 0.88 11 4 3 44.16 7.60 11 -4 3 43.69 8.91 -11 -4 -3 52.93 7.32 11 4 4 3.79 0.80 11 -4 4 1.50 0.97 -11 -4 -4 1.31 0.80 11 4 5 65.53 14.73 11 -4 5 72.12 11.42 -11 -4 -5 68.15 9.60 11 4 6 9.75 2.05 -11 -4 -6 3.61 1.23 11 4 7 14.68 3.29 -11 -4 -7 16.39 3.05 11 4 8 2.09 1.24 -11 -4 -8 1.24 0.67 11 4 9 65.03 10.31 -11 -4 -9 53.85 12.17 11 4 10 24.63 4.34 -11 -4 -10 22.76 6.48 11 5 -10 7.65 1.89 11 -5 -10 13.21 3.11 -11 -5 10 7.97 2.51 11 5 -9 54.98 8.03 11 -5 -9 48.64 10.02 -11 -5 9 50.45 10.16 11 5 -8 175.73 21.43 11 -5 -8 182.26 21.05 -11 -5 8 175.75 11.67 11 5 -7 4.99 1.55 11 -5 -7 8.66 2.17 -11 -5 7 5.21 1.62 11 5 -6 56.51 11.20 11 -5 -6 51.51 13.21 -11 -5 6 55.66 12.54 11 5 -5 0.38 0.88 11 -5 -5 1.34 1.19 -11 -5 5 1.12 0.84 11 5 -4 5.75 1.64 11 -5 -4 6.81 3.03 -11 -5 4 5.40 1.53 11 5 -3 1.09 1.02 11 -5 -3 -1.20 1.90 -11 -5 3 -0.71 1.56 11 5 -2 57.36 9.04 11 -5 -2 62.70 13.61 -11 -5 2 65.88 12.81 11 5 -1 1.81 1.14 11 -5 -1 2.48 1.08 -11 -5 1 1.15 1.01 11 5 0 60.98 13.46 11 -5 0 60.86 13.52 -11 -5 0 63.24 8.36 -11 -5 -1 19.78 5.11 11 5 2 2.92 1.48 11 -5 2 2.15 1.48 -11 -5 -2 2.42 0.96 11 5 3 -0.16 1.79 11 -5 3 0.18 0.74 -11 -5 -3 -0.36 1.54 11 5 4 6.03 1.81 11 -5 4 5.36 1.91 -11 -5 -4 5.10 1.44 11 5 5 17.65 2.79 -11 -5 -5 14.80 2.75 11 5 6 268.49 7.94 -11 -5 -6 266.09 21.31 11 5 7 3.51 0.89 -11 -5 -7 3.66 2.08 11 6 -2 18.88 5.05 11 -6 -2 16.86 4.10 -11 -6 2 17.44 3.48 11 6 -1 8.61 1.94 -11 -6 1 7.11 2.96 12 0 -14 5.69 2.25 12 0 -13 1.41 1.04 12 0 -12 142.23 11.98 12 0 -11 -0.55 1.03 12 0 -10 7.58 2.12 12 0 -9 -0.43 1.57 12 0 -8 45.93 8.01 12 0 -7 1.35 1.21 12 0 -6 319.40 8.11 12 0 -5 -1.08 1.69 12 0 -4 1.06 1.07 12 0 -3 -0.17 1.58 12 0 -2 120.91 12.75 12 0 -1 1.11 0.54 12 0 0 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1 0 8.99 1.34 12 -1 0 6.84 2.18 12 1 1 148.44 5.06 12 1 1 136.28 10.12 12 -1 1 155.82 5.91 12 1 2 33.44 7.38 12 1 2 32.71 6.45 12 -1 2 31.71 7.75 12 1 3 8.14 1.41 12 1 3 10.64 2.41 12 -1 3 10.40 2.59 12 1 4 3.33 0.73 12 1 4 5.84 1.09 12 -1 4 4.02 1.92 12 1 5 35.48 6.09 12 1 5 34.49 6.11 12 -1 5 36.91 7.03 12 1 6 202.37 5.66 12 1 6 186.11 7.97 12 -1 6 184.95 8.55 12 1 7 44.85 10.50 12 1 7 45.93 9.08 12 -1 7 40.92 7.83 12 1 8 1.36 1.07 12 1 8 0.76 1.02 12 2 -13 38.84 7.84 12 2 -13 51.31 6.55 12 -2 -13 51.30 8.27 12 2 -12 6.54 1.46 12 2 -12 5.99 2.47 12 -2 -12 5.57 2.13 12 2 -11 42.70 8.17 12 2 -11 48.82 7.39 12 -2 -11 47.73 8.59 12 2 -10 7.54 1.99 12 2 -10 5.17 1.51 12 -2 -10 4.59 1.79 12 2 -9 59.44 14.84 12 2 -9 69.55 11.15 12 -2 -9 71.01 11.68 12 2 -8 6.01 1.47 12 2 -8 9.33 1.40 12 -2 -8 3.87 0.87 12 2 -7 75.09 16.94 12 2 -7 81.74 12.39 12 -2 -7 80.52 14.53 12 2 -6 17.92 3.57 12 2 -6 14.28 3.04 12 -2 -6 17.26 4.06 12 2 -5 5.01 1.04 12 2 -5 7.48 1.27 12 -2 -5 7.65 1.73 12 2 -4 211.59 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6.13 12 -3 -7 33.77 6.74 12 3 -6 34.89 5.64 12 3 -6 38.28 7.27 12 -3 -6 34.02 7.63 12 3 -5 69.75 14.49 12 -3 -5 74.44 17.32 12 3 -4 163.16 6.18 12 -3 -4 151.30 11.31 -12 -3 4 162.71 13.83 12 3 -3 112.26 20.35 12 -3 -3 137.00 5.72 -12 -3 3 139.41 13.26 12 3 -2 30.11 7.15 12 -3 -2 36.82 8.83 -12 -3 2 39.10 9.03 12 3 -1 6.34 1.68 12 -3 -1 6.02 1.48 -12 -3 1 8.21 1.38 12 3 0 51.42 9.77 12 -3 0 47.43 9.52 -12 -3 0 47.16 10.95 12 3 1 10.65 2.05 12 -3 1 11.27 2.93 -12 -3 -1 10.09 2.45 12 3 2 2.61 1.23 12 -3 2 1.12 0.75 -12 -3 -2 2.07 1.20 12 3 3 6.86 2.08 12 -3 3 9.45 2.35 -12 -3 -3 9.78 1.73 12 3 4 202.20 7.96 12 -3 4 205.62 9.42 -12 -3 -4 202.69 17.08 12 3 5 95.97 13.42 12 -3 5 101.94 4.56 -12 -3 -5 110.09 8.70 12 3 6 28.25 4.80 -12 -3 -6 28.67 4.62 12 3 7 14.73 2.79 -12 -3 -7 17.75 3.43 12 3 8 1.81 1.08 -12 -3 -8 1.46 1.58 12 4 -9 12.19 1.78 12 4 -9 11.09 3.19 12 -4 -9 4.27 1.31 12 4 -8 136.34 20.23 12 -4 -8 155.81 15.95 -12 -4 8 128.05 18.27 12 4 -7 5.39 1.93 12 -4 -7 1.27 1.54 -12 -4 7 2.01 1.34 12 4 -6 26.76 3.32 12 -4 -6 29.35 5.62 -12 -4 6 24.21 5.75 12 4 -5 56.41 9.68 12 -4 -5 60.55 12.61 -12 -4 5 55.25 9.23 12 4 -4 66.01 9.02 12 -4 -4 71.16 15.28 -12 -4 4 72.43 13.11 12 4 -3 2.34 1.14 12 -4 -3 2.59 1.14 -12 -4 3 0.94 1.09 12 4 -2 112.78 15.50 12 -4 -2 116.70 16.68 -12 -4 2 109.07 15.00 12 4 -1 32.10 6.90 12 -4 -1 31.77 6.29 -12 -4 1 30.12 7.48 12 4 0 58.39 14.32 12 -4 0 59.07 11.16 -12 -4 0 63.35 8.23 12 4 1 22.40 3.65 12 -4 1 22.23 5.58 -12 -4 -1 23.19 5.48 12 4 2 5.52 1.28 12 -4 2 4.28 0.97 -12 -4 -2 3.24 2.12 12 4 3 -0.13 1.61 12 -4 3 0.89 0.63 -12 -4 -3 1.53 1.03 12 4 4 38.79 6.49 -12 -4 -4 39.64 7.13 12 4 5 1.91 1.58 -12 -4 -5 0.80 0.82 13 0 -10 1.91 1.12 13 0 -9 20.02 3.54 13 0 -8 -1.59 1.66 13 0 -7 172.37 18.03 13 0 -6 1.52 1.12 13 0 -5 2.95 1.03 13 0 -4 -0.86 1.38 13 0 -3 25.73 6.77 13 0 -2 1.77 1.03 13 0 -1 191.30 7.83 13 0 0 -1.26 1.41 13 0 1 77.44 15.06 13 0 2 -0.02 1.10 13 0 3 6.74 1.52 13 0 4 0.56 0.60 13 0 5 2.28 1.05 13 0 6 1.21 0.51 13 1 -10 65.70 12.65 13 -1 -10 63.04 11.67 13 1 -9 31.94 5.50 13 -1 -9 28.02 6.10 13 1 -8 4.74 1.99 13 -1 -8 3.85 1.58 13 1 -7 8.52 1.82 13 -1 -7 9.50 2.33 13 1 -6 -0.47 1.56 13 -1 -6 -0.52 1.69 13 1 -5 0.81 1.17 13 -1 -5 1.85 1.17 13 1 -4 1.24 0.71 13 -1 -4 0.85 1.47 13 1 -3 146.11 9.92 13 -1 -3 159.12 6.15 13 1 -2 67.07 13.36 13 -1 -2 74.30 15.77 13 1 -1 47.87 10.22 13 -1 -1 46.87 8.83 13 1 0 14.90 3.73 13 -1 0 15.38 3.31 13 1 1 1.55 1.01 13 -1 1 0.83 1.47 13 1 2 10.57 2.37 13 -1 2 12.18 2.79 13 1 3 23.50 4.46 13 -1 3 24.10 5.37 13 1 4 32.20 7.70 13 -1 4 29.96 6.35 13 1 5 1.27 0.74 13 -1 5 1.53 0.64 13 1 6 127.85 4.79 13 2 -8 37.66 8.92 13 2 -8 50.47 8.53 13 -2 -8 45.47 8.03 13 2 -7 20.11 4.08 13 2 -7 19.46 3.96 13 -2 -7 21.20 4.09 13 2 -6 15.83 4.77 13 2 -6 15.98 3.15 13 -2 -6 14.10 2.94 13 2 -5 10.03 3.29 13 2 -5 12.96 2.49 13 -2 -5 10.27 2.68 13 2 -4 70.78 14.47 13 2 -4 77.60 15.64 13 -2 -4 73.57 16.03 13 2 -3 3.38 1.36 13 2 -3 2.24 1.14 13 -2 -3 2.68 1.66 13 2 -2 169.86 5.77 13 2 -2 148.77 13.39 13 -2 -2 165.42 6.19 13 2 -1 2.39 1.26 13 2 -1 3.83 2.04 13 -2 -1 1.75 1.24 13 2 0 44.92 7.52 13 2 0 46.19 10.99 13 -2 0 45.42 9.17 13 2 1 6.69 1.75 13 2 1 6.62 1.55 13 -2 1 9.41 1.92 13 2 2 6.36 1.36 13 2 2 7.74 2.27 13 -2 2 7.36 1.77 13 2 3 3.90 1.56 13 2 3 5.99 1.36 13 -2 3 6.83 1.51 13 2 4 27.74 7.91 13 -2 4 30.66 8.13 13 2 5 2.62 1.17 13 -2 5 1.48 0.61 13 3 -5 48.89 10.56 13 3 -5 43.62 8.09 13 -3 -5 47.65 9.65 13 3 -4 2.93 1.65 13 3 -4 5.39 2.02 13 -3 -4 4.09 1.93 13 3 -3 27.98 5.40 13 3 -3 22.47 4.82 13 -3 -3 27.95 5.25 13 3 -2 11.08 2.47 13 -3 -2 10.00 3.19 13 3 -1 7.40 2.35 13 -3 -1 5.12 1.62 13 3 0 0.56 0.83 13 -3 0 1.29 0.96 -13 -3 0 2.28 1.02 13 3 1 64.30 13.11 13 -3 1 58.61 13.89 -13 -3 -1 70.10 15.23 ; _shelx_hkl_checksum 10444 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 -1/2+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 _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.27756(3) 0.10301(5) 1.14813(2) 0.03480(11) Uani 1 1 d . . . . . O1 O 0.82223(9) 0.49589(13) 1.01601(5) 0.0347(2) Uani 1 1 d . . . . . O2 O 0.87049(8) 0.22344(11) 0.98901(4) 0.0267(2) Uani 1 1 d . . . . . O3 O 0.70240(9) 0.39097(15) 0.80558(5) 0.0382(3) Uani 1 1 d . . . . . O4 O 0.87504(8) 0.47187(13) 0.86763(4) 0.0302(2) Uani 1 1 d . . . . . C1 C 0.59148(11) 0.30485(15) 0.93010(6) 0.0218(2) Uani 1 1 d . . . . . C2 C 0.49577(11) 0.26455(16) 0.87712(6) 0.0236(2) Uani 1 1 d . . . . . C3 C 0.39082(11) 0.19938(15) 0.90197(6) 0.0215(2) Uani 1 1 d . . . . . C4 C 0.33171(12) 0.14444(16) 1.02171(6) 0.0235(2) Uani 1 1 d . . . . . C5 C 0.37474(12) 0.16610(16) 1.08716(6) 0.0250(3) Uani 1 1 d . . . . . C6 C 0.49131(13) 0.23779(17) 1.10564(6) 0.0269(3) Uani 1 1 d . . . . . C7 C 0.57164(12) 0.28710(17) 1.05753(6) 0.0251(3) Uani 1 1 d . . . . . C8 C 0.53148(11) 0.26526(15) 0.99209(6) 0.0209(2) Uani 1 1 d . . . . . C9 C 0.40994(11) 0.19882(15) 0.97450(6) 0.0207(2) Uani 1 1 d . . . . . C10 C 0.71129(11) 0.35805(16) 0.92317(6) 0.0224(2) Uani 1 1 d . . . . . C11 C 0.80609(11) 0.37169(15) 0.98119(6) 0.0222(2) Uani 1 1 d . . . . . C12 C 0.96393(14) 0.2205(2) 1.04433(7) 0.0342(3) Uani 1 1 d . . . . . C13 C 0.75798(12) 0.40573(16) 0.85857(6) 0.0250(3) Uani 1 1 d . . . . . C14 C 0.93070(15) 0.5286(2) 0.80854(7) 0.0367(3) Uani 1 1 d . . . . . C15 C 0.27768(11) 0.13802(15) 0.86265(6) 0.0222(2) Uani 1 1 d . . . . . C16 C 0.29135(13) 0.04949(18) 0.80390(6) 0.0297(3) Uani 1 1 d . . . . . C17 C 0.18626(14) -0.0027(2) 0.76449(7) 0.0360(3) Uani 1 1 d . . . . . C18 C 0.06588(13) 0.03123(19) 0.78345(7) 0.0337(3) Uani 1 1 d . . . . . C19 C 0.05114(12) 0.11836(18) 0.84187(7) 0.0296(3) Uani 1 1 d . . . . . C20 C 0.15597(12) 0.17232(16) 0.88117(6) 0.0251(3) Uani 1 1 d . . . . . H1 H 0.5071(14) 0.2784(19) 0.8295(7) 0.028(4) Uiso 1 1 d . . . . . H2 H 0.2523(15) 0.094(2) 1.0105(8) 0.030(4) Uiso 1 1 d . . . . . H3 H 0.5166(15) 0.254(2) 1.1504(8) 0.033(4) Uiso 1 1 d . . . . . H4 H 0.6544(16) 0.339(2) 1.0711(8) 0.038(4) Uiso 1 1 d . . . . . H5 H 1.0254(17) 0.311(3) 1.0393(9) 0.047(5) Uiso 1 1 d . . . . . H6 H 1.0055(17) 0.106(3) 1.0415(9) 0.046(5) Uiso 1 1 d . . . . . H7 H 0.9185(17) 0.230(2) 1.0839(9) 0.043(5) Uiso 1 1 d . . . . . H8 H 1.015(2) 0.564(3) 0.8229(10) 0.057(6) Uiso 1 1 d . . . . . H9 H 0.9322(16) 0.435(2) 0.7784(9) 0.043(5) Uiso 1 1 d . . . . . H10 H 0.885(2) 0.626(3) 0.7898(10) 0.060(6) Uiso 1 1 d . . . . . H11 H 0.3758(15) 0.022(2) 0.7912(8) 0.031(4) Uiso 1 1 d . . . . . H12 H 0.1977(18) -0.063(3) 0.7244(10) 0.055(5) Uiso 1 1 d . . . . . H13 H -0.0057(17) -0.004(2) 0.7553(9) 0.044(5) Uiso 1 1 d . . . . . H14 H -0.0320(16) 0.141(2) 0.8546(8) 0.034(4) Uiso 1 1 d . . . . . H15 H 0.1422(14) 0.236(2) 0.9211(8) 0.026(4) Uiso 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 Cl1 0.0368(2) 0.0443(2) 0.02438(18) 0.00419(13) 0.00943(13) -0.00126(14) O1 0.0363(5) 0.0305(5) 0.0362(5) -0.0111(4) -0.0047(4) -0.0003(4) O2 0.0272(4) 0.0249(4) 0.0267(5) -0.0002(3) -0.0069(3) -0.0013(3) O3 0.0294(5) 0.0633(7) 0.0217(5) 0.0048(4) -0.0005(4) -0.0086(5) O4 0.0268(4) 0.0403(5) 0.0237(4) -0.0005(4) 0.0040(3) -0.0089(4) C1 0.0234(6) 0.0207(5) 0.0211(6) 0.0013(4) 0.0001(4) 0.0013(4) C2 0.0235(6) 0.0258(6) 0.0214(6) 0.0011(4) 0.0000(4) 0.0001(5) C3 0.0234(5) 0.0209(5) 0.0199(5) 0.0004(4) 0.0001(4) 0.0013(4) C4 0.0240(6) 0.0222(6) 0.0244(6) 0.0005(5) 0.0019(5) 0.0005(5) C5 0.0298(6) 0.0240(6) 0.0218(6) 0.0025(5) 0.0058(5) 0.0037(5) C6 0.0322(6) 0.0292(6) 0.0191(6) 0.0000(5) -0.0002(5) 0.0021(5) C7 0.0264(6) 0.0265(6) 0.0220(6) -0.0009(5) -0.0018(5) -0.0003(5) C8 0.0223(5) 0.0192(5) 0.0209(6) 0.0012(4) 0.0005(4) 0.0017(4) C9 0.0237(6) 0.0185(5) 0.0197(5) 0.0004(4) -0.0002(4) 0.0025(4) C10 0.0235(6) 0.0220(5) 0.0216(6) -0.0005(4) 0.0006(4) 0.0012(4) C11 0.0215(5) 0.0246(6) 0.0205(6) 0.0001(4) 0.0023(4) -0.0031(4) C12 0.0327(7) 0.0355(8) 0.0322(7) 0.0055(6) -0.0133(6) -0.0040(6) C13 0.0229(6) 0.0272(6) 0.0248(6) 0.0003(5) 0.0022(5) -0.0002(5) C14 0.0369(8) 0.0461(9) 0.0282(7) 0.0003(6) 0.0108(6) -0.0110(7) C15 0.0256(6) 0.0212(5) 0.0194(6) 0.0013(4) -0.0010(4) -0.0013(4) C16 0.0297(7) 0.0338(7) 0.0254(6) -0.0049(5) 0.0016(5) 0.0007(5) C17 0.0414(8) 0.0392(8) 0.0267(7) -0.0109(6) -0.0036(6) -0.0016(6) C18 0.0327(7) 0.0346(7) 0.0321(7) -0.0036(6) -0.0094(5) -0.0054(6) C19 0.0234(6) 0.0318(7) 0.0330(7) 0.0007(5) -0.0022(5) -0.0009(5) C20 0.0266(6) 0.0247(6) 0.0239(6) -0.0029(5) 0.0010(5) -0.0011(5) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (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 C11 O2 C12 115.00(10) . . ? C13 O4 C14 115.29(10) . . ? C10 C1 C2 126.44(11) . . ? C10 C1 C8 127.80(11) . . ? C2 C1 C8 105.67(10) . . ? C3 C2 C1 110.28(11) . . ? C3 C2 H1 124.6(9) . . ? C1 C2 H1 125.1(9) . . ? C2 C3 C15 125.03(11) . . ? C2 C3 C9 108.62(10) . . ? C15 C3 C9 126.35(10) . . ? C9 C4 C5 117.57(11) . . ? C9 C4 H2 121.8(10) . . ? C5 C4 H2 120.6(10) . . ? C6 C5 C4 122.41(11) . . ? C6 C5 Cl1 118.64(10) . . ? C4 C5 Cl1 118.94(10) . . ? C5 C6 C7 119.62(12) . . ? C5 C6 H3 120.4(10) . . ? C7 C6 H3 120.0(10) . . ? C8 C7 C6 119.04(12) . . ? C8 C7 H4 121.8(10) . . ? C6 C7 H4 119.1(10) . . ? C7 C8 C9 120.21(11) . . ? C7 C8 C1 132.55(11) . . ? C9 C8 C1 107.20(10) . . ? C4 C9 C8 121.04(11) . . ? C4 C9 C3 130.80(11) . . ? C8 C9 C3 108.15(10) . . ? C1 C10 C13 122.83(11) . . ? C1 C10 C11 121.29(11) . . ? C13 C10 C11 115.88(10) . . ? O1 C11 O2 124.19(11) . . ? O1 C11 C10 125.75(11) . . ? O2 C11 C10 110.06(10) . . ? O2 C12 H5 109.6(11) . . ? O2 C12 H6 104.6(11) . . ? H5 C12 H6 109.2(15) . . ? O2 C12 H7 107.2(10) . . ? H5 C12 H7 114.3(16) . . ? H6 C12 H7 111.5(15) . . ? O3 C13 O4 123.35(11) . . ? O3 C13 C10 127.13(12) . . ? O4 C13 C10 109.52(10) . . ? O4 C14 H8 104.9(12) . . ? O4 C14 H9 109.7(11) . . ? H8 C14 H9 110.7(16) . . ? O4 C14 H10 110.3(13) . . ? H8 C14 H10 109.3(17) . . ? H9 C14 H10 111.7(17) . . ? C20 C15 C16 118.68(11) . . ? C20 C15 C3 121.61(11) . . ? C16 C15 C3 119.65(11) . . ? C17 C16 C15 120.79(13) . . ? C17 C16 H11 120.0(9) . . ? C15 C16 H11 119.2(9) . . ? C18 C17 C16 120.09(13) . . ? C18 C17 H12 120.4(12) . . ? C16 C17 H12 119.5(12) . . ? C17 C18 C19 119.63(12) . . ? C17 C18 H13 119.0(11) . . ? C19 C18 H13 121.3(11) . . ? C20 C19 C18 120.51(13) . . ? C20 C19 H14 120.4(10) . . ? C18 C19 H14 119.1(10) . . ? C19 C20 C15 120.29(12) . . ? C19 C20 H15 118.3(9) . . ? C15 C20 H15 121.4(9) . . ? 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 Cl1 C5 1.7412(13) . ? O1 C11 1.1964(15) . ? O2 C11 1.3332(15) . ? O2 C12 1.4488(15) . ? O3 C13 1.2004(16) . ? O4 C13 1.3418(16) . ? O4 C14 1.4483(16) . ? C1 C10 1.3515(17) . ? C1 C2 1.4630(16) . ? C1 C8 1.4888(16) . ? C2 C3 1.3520(17) . ? C2 H1 0.994(15) . ? C3 C15 1.4729(16) . ? C3 C9 1.4810(16) . ? C4 C9 1.3811(17) . ? C4 C5 1.3917(18) . ? C4 H2 0.940(16) . ? C5 C6 1.3811(19) . ? C6 C7 1.3982(18) . ? C6 H3 0.943(16) . ? C7 C8 1.3839(17) . ? C7 H4 0.985(17) . ? C8 C9 1.4088(16) . ? C10 C13 1.4882(17) . ? C10 C11 1.5018(16) . ? C12 H5 0.96(2) . ? C12 H6 0.988(19) . ? C12 H7 0.974(19) . ? C14 H8 0.96(2) . ? C14 H9 0.951(19) . ? C14 H10 0.96(2) . ? C15 C20 1.3955(17) . ? C15 C16 1.3965(18) . ? C16 C17 1.3865(19) . ? C16 H11 0.973(16) . ? C17 C18 1.385(2) . ? C17 H12 0.96(2) . ? C18 C19 1.387(2) . ? C18 H13 0.958(18) . ? C19 C20 1.3873(18) . ? C19 H14 0.952(17) . ? C20 H15 0.971(16) . ? 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 C10 C1 C2 C3 174.07(12) . . . . ? C8 C1 C2 C3 -2.78(14) . . . . ? C1 C2 C3 C15 -177.36(11) . . . . ? C1 C2 C3 C9 2.05(14) . . . . ? C9 C4 C5 C6 -0.45(18) . . . . ? C9 C4 C5 Cl1 178.77(9) . . . . ? C4 C5 C6 C7 -1.68(19) . . . . ? Cl1 C5 C6 C7 179.10(10) . . . . ? C5 C6 C7 C8 0.98(19) . . . . ? C6 C7 C8 C9 1.77(18) . . . . ? C6 C7 C8 C1 179.29(12) . . . . ? C10 C1 C8 C7 7.9(2) . . . . ? C2 C1 C8 C7 -175.35(13) . . . . ? C10 C1 C8 C9 -174.40(12) . . . . ? C2 C1 C8 C9 2.40(13) . . . . ? C5 C4 C9 C8 3.26(17) . . . . ? C5 C4 C9 C3 -177.77(12) . . . . ? C7 C8 C9 C4 -3.99(18) . . . . ? C1 C8 C9 C4 177.93(10) . . . . ? C7 C8 C9 C3 176.83(11) . . . . ? C1 C8 C9 C3 -1.25(13) . . . . ? C2 C3 C9 C4 -179.54(12) . . . . ? C15 C3 C9 C4 -0.1(2) . . . . ? C2 C3 C9 C8 -0.47(13) . . . . ? C15 C3 C9 C8 178.93(11) . . . . ? C2 C1 C10 C13 8.3(2) . . . . ? C8 C1 C10 C13 -175.54(11) . . . . ? C2 C1 C10 C11 -171.44(11) . . . . ? C8 C1 C10 C11 4.72(19) . . . . ? C12 O2 C11 O1 0.43(18) . . . . ? C12 O2 C11 C10 -179.19(10) . . . . ? C1 C10 C11 O1 -87.67(17) . . . . ? C13 C10 C11 O1 92.58(15) . . . . ? C1 C10 C11 O2 91.94(14) . . . . ? C13 C10 C11 O2 -87.81(13) . . . . ? C14 O4 C13 O3 1.11(19) . . . . ? C14 O4 C13 C10 -178.31(12) . . . . ? C1 C10 C13 O3 -6.4(2) . . . . ? C11 C10 C13 O3 173.38(13) . . . . ? C1 C10 C13 O4 173.03(11) . . . . ? C11 C10 C13 O4 -7.22(15) . . . . ? C2 C3 C15 C20 -139.77(13) . . . . ? C9 C3 C15 C20 40.92(18) . . . . ? C2 C3 C15 C16 37.52(18) . . . . ? C9 C3 C15 C16 -141.78(13) . . . . ? C20 C15 C16 C17 0.3(2) . . . . ? C3 C15 C16 C17 -177.04(13) . . . . ? C15 C16 C17 C18 -0.7(2) . . . . ? C16 C17 C18 C19 0.3(2) . . . . ? C17 C18 C19 C20 0.3(2) . . . . ? C18 C19 C20 C15 -0.6(2) . . . . ? C16 C15 C20 C19 0.30(19) . . . . ? C3 C15 C20 C19 177.62(12) . . . . ?