#------------------------------------------------------------------------------ #$Date: 2016-01-09 04:26:59 +0200 (Sat, 09 Jan 2016) $ #$Revision: 173694 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/19/1541918.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_1541918 loop_ _publ_author_name 'Chang, Meng-Yang' 'Cheng, Yu-Chieh' _publ_section_title ; Synthesis of Substituted Tetralins and Benzosuberans via BF3·OEt2-Mediated Formal (4 + 2) and (5 + 2) Stereocontrolled Cycloaddition of 4-Alkenols with Veratrol ; _journal_name_full 'Organic Letters' _journal_paper_doi 10.1021/acs.orglett.5b03696 _journal_year 2016 _chemical_formula_sum 'C25 H26 O2' _chemical_formula_weight 358.46 _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 110.299(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.2155(13) _cell_length_b 18.822(2) _cell_length_c 10.6623(15) _cell_measurement_reflns_used 3006 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.1707 _cell_measurement_theta_min 2.3062 _cell_volume 1922.8(4) _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0455 _diffrn_reflns_laue_measured_fraction_full 0.999 _diffrn_reflns_laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 15767 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.390 _diffrn_reflns_theta_min 2.126 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.8585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Lump _exptl_crystal_F_000 768 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.269 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 247 _refine_ls_number_reflns 3930 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0583 _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^)+(0.0445P)^2^+0.4572P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.1024 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3070 _reflns_number_total 3930 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol5b03696_si_003.cif _cod_data_source_block mo_150631LT_0m _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas ; _cod_database_code 1541918 _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. ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL mo_150631LT_0m in P2(1)/c CELL 0.71073 10.2155 18.8224 10.6623 90.000 110.299 90.000 ZERR 4.00 0.0013 0.0024 0.0015 0.000 0.003 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H O UNIT 100 104 8 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 TEMP -173.000 WGHT 0.044500 0.457200 FVAR 0.65729 O1 3 0.244946 0.205997 0.547165 11.00000 0.02546 0.01241 = 0.01862 0.00062 0.00559 -0.00017 O2 3 0.078097 0.258638 0.326042 11.00000 0.02792 0.01740 = 0.01651 -0.00221 0.00119 -0.00474 C1 1 0.335810 0.175494 0.669314 11.00000 0.02606 0.01738 = 0.02004 0.00352 0.00703 0.00120 AFIX 137 H26 2 0.431285 0.192419 0.687091 11.00000 -1.50000 H1 2 0.333507 0.123597 0.661463 11.00000 -1.50000 H3 2 0.304853 0.189582 0.743022 11.00000 -1.50000 AFIX 0 C2 1 0.235061 0.278750 0.542955 11.00000 0.01698 0.01479 = 0.01928 0.00077 0.01022 -0.00076 C3 1 0.144552 0.307927 0.421630 11.00000 0.01623 0.01788 = 0.01618 -0.00330 0.00685 -0.00456 C4 1 0.132425 0.380826 0.407772 11.00000 0.01406 0.01851 = 0.01536 0.00102 0.00558 -0.00017 AFIX 43 H7 2 0.071252 0.400290 0.326314 11.00000 -1.20000 AFIX 0 C5 1 0.208587 0.427165 0.511531 11.00000 0.01281 0.01612 = 0.01633 -0.00097 0.00725 -0.00173 C6 1 0.196899 0.507804 0.488867 11.00000 0.01251 0.01477 = 0.01730 -0.00141 0.00595 0.00010 AFIX 13 H17 2 0.117764 0.524936 0.515714 11.00000 -1.20000 AFIX 0 C7 1 0.331795 0.544438 0.581938 11.00000 0.01447 0.01606 = 0.01736 -0.00099 0.00601 -0.00098 AFIX 13 H18 2 0.411672 0.525835 0.557834 11.00000 -1.20000 AFIX 0 C8 1 0.330757 0.624597 0.568192 11.00000 0.01718 0.01579 = 0.01299 -0.00198 0.00247 -0.00197 C9 1 0.417885 0.658803 0.512043 11.00000 0.02328 0.02044 = 0.02017 -0.00075 0.01056 -0.00056 AFIX 43 H20 2 0.474804 0.631380 0.476383 11.00000 -1.20000 AFIX 0 C10 1 0.422892 0.732508 0.507344 11.00000 0.02919 0.02074 = 0.02678 0.00293 0.01469 -0.00354 AFIX 43 H21 2 0.482941 0.754892 0.468435 11.00000 -1.20000 AFIX 0 C11 1 0.341083 0.773582 0.558903 11.00000 0.02280 0.01520 = 0.02445 0.00063 0.00379 -0.00146 AFIX 43 H2 2 0.345836 0.823953 0.556833 11.00000 -1.20000 AFIX 0 C12 1 -0.005795 0.283565 0.196759 11.00000 0.02227 0.02485 = 0.01638 -0.00300 0.00258 -0.00078 AFIX 137 H5 2 -0.083144 0.312026 0.204102 11.00000 -1.50000 H6 2 -0.043110 0.242918 0.137720 11.00000 -1.50000 H4 2 0.051239 0.312874 0.159642 11.00000 -1.50000 AFIX 0 C13 1 0.295557 0.398055 0.632342 11.00000 0.01386 0.01671 = 0.01537 -0.00093 0.00716 -0.00156 C14 1 0.385270 0.442754 0.749772 11.00000 0.01771 0.01859 = 0.01547 -0.00059 0.00487 -0.00200 AFIX 13 H8 2 0.484956 0.434937 0.758785 11.00000 -1.20000 AFIX 0 C15 1 0.369387 0.420282 0.882280 11.00000 0.02864 0.02007 = 0.01616 -0.00131 0.00628 -0.00440 AFIX 137 H9 2 0.431954 0.448848 0.955459 11.00000 -1.50000 H11 2 0.393411 0.369912 0.898940 11.00000 -1.50000 H10 2 0.272665 0.427751 0.876965 11.00000 -1.50000 AFIX 0 C16 1 0.355316 0.521703 0.726434 11.00000 0.02251 0.01699 = 0.01674 -0.00321 0.00551 -0.00447 AFIX 23 H23 2 0.434712 0.548930 0.787764 11.00000 -1.20000 H24 2 0.271289 0.533669 0.748242 11.00000 -1.20000 AFIX 0 C17 1 0.165719 0.529249 0.343949 11.00000 0.01562 0.01253 = 0.01745 -0.00191 0.00399 -0.00367 C18 1 0.250148 0.505782 0.273566 11.00000 0.01575 0.01638 = 0.01878 0.00022 0.00435 0.00033 AFIX 43 H16 2 0.326981 0.475413 0.316358 11.00000 -1.20000 AFIX 0 C19 1 0.223252 0.526255 0.141931 11.00000 0.02406 0.01957 = 0.01950 -0.00258 0.00885 -0.00366 AFIX 43 H15 2 0.281663 0.509852 0.095428 11.00000 -1.20000 AFIX 0 C20 1 0.111407 0.570586 0.077926 11.00000 0.02872 0.01928 = 0.01705 0.00327 0.00367 -0.00425 AFIX 43 H14 2 0.092558 0.584220 -0.012437 11.00000 -1.20000 AFIX 0 C21 1 0.027531 0.594785 0.146731 11.00000 0.02267 0.01569 = 0.02579 0.00387 0.00147 0.00065 AFIX 43 H13 2 -0.048368 0.625685 0.103854 11.00000 -1.20000 AFIX 0 C22 1 0.054054 0.573971 0.278683 11.00000 0.01727 0.01565 = 0.02434 -0.00037 0.00616 0.00007 AFIX 43 H12 2 -0.004704 0.590469 0.324747 11.00000 -1.20000 AFIX 0 C23 1 0.246757 0.666844 0.617316 11.00000 0.02026 0.02080 = 0.02677 0.00182 0.01191 0.00044 AFIX 43 H19 2 0.184630 0.644694 0.654052 11.00000 -1.20000 AFIX 0 C24 1 0.252226 0.740449 0.613540 11.00000 0.02363 0.01936 = 0.02637 -0.00271 0.00909 0.00260 AFIX 43 H22 2 0.195009 0.768131 0.648440 11.00000 -1.20000 AFIX 0 C25 1 0.307191 0.323769 0.645242 11.00000 0.01573 0.01894 = 0.01401 0.00183 0.00514 -0.00036 AFIX 43 H25 2 0.366741 0.304037 0.727179 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_150631LT_0m in P2(1)/c REM R1 = 0.0417 for 3070 Fo > 4sig(Fo) and 0.0583 for all 3930 data REM 247 parameters refined using 0 restraints END WGHT 0.0445 0.4572 REM Highest difference peak 0.269, deepest hole -0.255, 1-sigma level 0.043 Q1 1 0.3369 0.4217 0.6930 11.00000 0.05 0.27 Q2 1 0.2688 0.5259 0.5328 11.00000 0.05 0.25 Q3 1 0.2374 0.2929 0.4777 11.00000 0.05 0.22 Q4 1 0.1419 0.2895 0.4871 11.00000 0.05 0.22 Q5 1 0.1099 0.5421 0.3137 11.00000 0.05 0.22 ; _shelx_res_checksum 8019 _shelx_hkl_file ; 1 0 0 107.136 5.02945 1 -1 0 0 128.290 5.17106 1 2 0 0 8329.41 257.718 1 -2 0 0 8131.12 257.439 1 3 0 0 2666.42 86.4600 1 -3 0 0 2681.28 86.0045 1 -4 0 0 -0.0046 1.63412 1 4 0 0 -0.9872 1.63625 1 5 0 0 106.157 7.88499 1 -5 0 0 88.8674 6.54872 1 6 0 0 51.7656 5.26885 2 -6 0 0 51.1279 5.91345 1 6 0 0 36.1242 5.66649 1 -7 0 0 144.223 9.54657 1 7 0 0 141.822 11.3922 1 7 0 0 169.326 9.28763 2 8 0 0 58.3472 8.88205 1 8 0 0 73.4909 7.24420 2 9 0 0 254.454 17.6024 1 9 0 0 253.159 13.4226 2 10 0 0 147.061 15.8698 1 11 0 0 159.321 17.7979 1 0 1 0 -0.3381 0.23638 3 0 1 0 0.25234 0.23587 1 1 -1 0 740.531 25.0064 1 -1 1 0 851.679 25.1760 1 1 1 0 754.422 24.1782 1 1 1 0 722.718 23.9371 2 1 1 0 722.677 24.1561 1 2 -1 0 843.026 29.4482 1 2 1 0 841.132 28.5899 1 -2 1 0 918.082 29.4656 1 2 1 0 847.995 27.8695 2 3 -1 0 246.119 11.2275 1 3 1 0 238.874 9.42529 2 -3 1 0 245.886 10.9674 1 3 1 0 250.731 10.5635 1 4 -1 0 166.319 9.64960 1 -4 1 0 164.038 9.13600 1 4 1 0 187.120 9.43631 1 4 1 0 179.972 7.86654 2 5 -1 0 52.8079 6.37670 1 -5 1 0 83.1911 6.38491 1 5 1 0 54.6893 6.18833 1 5 1 0 64.3396 4.64174 2 6 -1 0 38.5591 6.21731 1 6 1 0 48.1242 4.87520 2 6 1 0 40.5984 5.85473 1 -6 1 0 55.9232 6.42485 1 7 -1 0 39.3704 6.93696 1 7 -1 0 49.9510 6.11570 2 -7 1 0 50.2025 6.61985 1 7 1 0 61.2126 7.89345 1 7 1 0 53.3996 5.45260 2 8 -1 0 18.9210 4.44360 2 8 -1 0 11.9047 5.31753 1 8 1 0 17.3763 3.80355 2 8 1 0 11.8709 4.91347 1 9 -1 0 12.0638 5.71884 1 9 -1 0 1.67221 2.93020 2 9 1 0 0.79989 4.15186 1 9 1 0 4.83073 2.94718 2 10 -1 0 41.0559 9.33388 1 10 1 0 48.1531 9.38035 1 11 -1 0 54.9980 11.2310 1 11 1 0 42.1262 9.33792 1 0 -2 0 16.3243 1.73479 1 0 2 0 17.2246 1.61030 1 0 2 0 20.0795 1.81390 3 1 -2 0 6.68611 1.66593 1 1 2 0 6.59127 1.09030 2 -1 2 0 4.36363 1.47651 1 1 2 0 6.60501 0.80580 1 1 2 0 5.95755 0.80691 1 -2 2 0 306.516 11.8597 1 2 2 0 273.594 10.1458 1 2 2 0 271.956 10.1021 1 2 2 0 267.094 9.53351 2 3 -2 0 232.566 11.0885 1 -3 2 0 215.564 10.6941 1 3 2 0 229.431 8.55748 2 3 2 0 232.453 9.74032 1 4 -2 0 461.847 19.4513 1 -4 2 0 450.423 18.9027 1 4 2 0 473.626 18.2716 1 4 2 0 461.556 16.4548 2 5 -2 0 230.677 12.8360 1 -5 2 0 225.984 12.0531 1 5 2 0 205.784 9.37346 2 5 2 0 238.224 11.7728 1 6 -2 0 378.719 19.3640 1 6 2 0 378.688 15.3251 2 -6 2 0 397.028 18.2830 1 6 2 0 409.821 18.4252 1 7 -2 0 171.271 12.8660 1 -7 2 0 167.445 11.4213 1 7 2 0 179.283 9.17853 2 7 2 0 192.822 12.4562 1 8 -2 0 20.3770 4.57712 2 8 -2 0 13.2583 5.35437 1 8 2 0 21.5822 3.97791 2 8 2 0 25.3414 6.39125 1 9 -2 0 75.1155 8.47218 2 9 -2 0 49.7858 9.23221 1 9 2 0 66.0479 9.61333 1 10 -2 0 46.5472 7.00781 2 10 -2 0 39.5527 9.12334 1 10 2 0 26.0617 7.34255 1 11 -2 0 25.5708 8.48387 1 11 2 0 23.4615 7.75023 1 0 -3 0 -0.5458 0.81863 1 0 3 0 -2.2029 0.87493 3 0 3 0 -1.0290 0.84976 1 1 -3 0 132.600 6.75780 1 1 3 0 131.987 5.27908 1 -1 3 0 137.739 6.80954 1 1 3 0 157.465 5.42900 1 2 -3 0 3461.57 109.567 1 2 3 0 3424.18 107.100 1 2 3 0 3300.05 106.849 2 -2 3 0 3694.88 109.659 1 2 3 0 3187.35 106.942 1 3 -3 0 81.1151 6.29696 1 3 3 0 77.0682 3.74972 2 3 3 0 86.2514 4.77187 1 -3 3 0 84.9474 6.28905 1 3 3 0 75.1386 4.52651 1 4 -3 0 704.607 27.9179 1 -4 3 0 735.393 27.8155 1 4 3 0 692.882 23.9903 2 4 3 0 746.492 25.9842 1 5 -3 0 224.593 12.8727 1 -5 3 0 209.004 11.9078 1 5 3 0 201.222 8.77048 2 5 3 0 227.595 11.2105 1 6 -3 0 9.78479 4.40056 1 6 3 0 11.0233 2.29589 2 6 3 0 13.5322 3.84249 1 -6 3 0 10.2622 3.80506 1 7 -3 0 54.3853 8.29815 1 -7 3 0 61.3476 8.04010 1 7 3 0 55.3782 4.54846 2 7 3 0 51.8208 7.32825 1 8 -3 0 64.8296 9.54568 1 8 3 0 86.8926 10.0964 1 8 3 0 75.2110 5.65800 2 9 -3 0 4.19718 3.54717 2 9 -3 0 14.5080 6.05543 1 9 3 0 8.24337 4.89319 1 10 -3 0 35.6108 6.61294 2 10 -3 0 24.8228 8.02184 1 10 3 0 16.6168 6.38404 1 11 -3 0 162.645 18.5458 1 11 3 0 119.077 14.7933 1 0 -4 0 3797.48 117.726 1 0 4 0 3770.45 118.219 3 0 4 0 3626.01 117.777 1 1 -4 0 24.5646 3.14207 1 -1 4 0 27.9137 2.93560 3 1 4 0 25.9571 2.20405 1 -1 4 0 20.7249 3.07981 1 1 4 0 20.9532 2.03247 1 2 -4 0 1249.70 43.8170 1 2 4 0 1261.55 41.1842 1 2 4 0 1226.60 41.3507 2 2 4 0 1238.23 41.1121 1 -2 4 0 1470.39 44.4150 1 3 -4 0 302.689 14.0358 1 3 4 0 314.445 11.5973 1 -3 4 0 300.756 13.8993 1 3 4 0 293.677 10.7201 2 3 4 0 295.381 11.4322 1 4 -4 0 457.376 19.8842 1 4 4 0 435.559 17.0910 1 -4 4 0 436.921 19.4487 1 4 4 0 440.977 15.5031 2 4 4 0 478.889 17.4725 1 5 -4 0 416.136 20.1280 1 5 4 0 426.724 17.6936 1 5 4 0 419.478 15.1013 2 -5 4 0 440.309 19.7040 1 6 -4 0 293.719 17.0698 1 -6 4 0 316.529 16.5717 1 6 4 0 300.347 11.7680 2 6 4 0 310.053 15.0675 1 7 -4 0 308.612 18.6893 1 7 4 0 308.539 12.3522 2 -7 4 0 336.167 17.8249 1 7 4 0 295.692 16.0972 1 8 -4 0 37.7568 8.17211 1 8 4 0 40.7097 6.82041 1 -8 4 0 72.1989 14.5898 1 9 -4 0 13.1735 5.88353 1 9 4 0 4.18720 4.10591 1 10 -4 0 65.7061 9.33088 2 10 -4 0 65.0129 11.5117 1 10 4 0 59.2932 9.62345 1 11 -4 0 103.901 15.4278 1 11 4 0 103.724 13.4243 1 0 -5 0 -0.5890 1.25976 1 0 5 0 0.92467 1.61984 3 0 5 0 -0.8373 1.36959 1 1 -5 0 1024.25 34.4638 1 1 5 0 988.875 32.8167 1 -1 5 0 1005.10 34.5523 1 -1 5 0 1046.47 33.8806 3 1 5 0 938.961 32.7654 1 2 -5 0 30.9484 3.99835 1 2 5 0 35.3332 2.62854 1 2 5 0 33.3132 2.68412 1 -2 5 0 43.7023 4.87467 1 3 -5 0 -0.1527 2.07205 1 3 5 0 -1.3288 1.05781 1 3 5 0 -0.5193 1.09257 2 -3 5 0 0.53018 2.02150 1 3 5 0 -1.3092 0.95246 1 4 -5 0 203.330 12.0486 1 4 5 0 210.964 9.47292 1 4 5 0 209.680 9.49766 1 -4 5 0 212.795 12.1649 1 4 5 0 208.344 8.13467 2 5 -5 0 365.728 18.1852 1 5 5 0 317.272 14.9198 1 5 5 0 352.949 15.0512 1 5 5 0 348.367 12.4749 2 -5 5 0 355.126 17.5819 1 6 -5 0 196.539 13.5299 1 6 5 0 178.853 7.64392 2 6 5 0 209.880 11.2108 1 -6 5 0 170.874 12.1900 1 7 -5 0 319.324 19.2610 1 7 5 0 322.984 16.4036 1 7 5 0 312.851 11.9353 2 -7 5 0 320.644 18.2014 1 8 -5 0 0.24042 4.14352 1 -8 5 0 13.2345 4.78275 1 8 5 0 3.24373 3.67505 1 9 -5 0 30.7077 8.74729 1 9 5 0 42.9246 7.78970 1 10 -5 0 92.7576 11.2327 2 10 -5 0 77.6722 12.5286 1 10 5 0 82.3061 11.0163 1 11 -5 0 26.8678 8.57897 1 11 -5 0 22.5042 6.74939 2 11 5 0 33.4565 8.36343 1 0 -6 0 806.938 27.1222 1 0 6 0 744.070 27.4780 1 0 6 0 808.810 28.1035 3 1 -6 0 1157.13 40.3017 1 -1 6 0 1181.55 40.6848 1 1 6 0 1192.63 39.2981 1 -1 6 0 1235.42 40.0210 3 1 6 0 1133.67 38.8597 1 2 -6 0 2413.79 80.5634 1 2 6 0 2425.10 77.6018 1 -2 6 0 2452.28 80.9075 1 2 6 0 2436.54 77.6483 1 -2 6 0 2453.16 79.1758 3 3 -6 0 295.099 14.1074 1 -3 6 0 267.424 13.9819 1 3 6 0 292.601 11.0728 1 3 6 0 258.084 10.6762 1 4 -6 0 5.58765 3.28412 1 4 6 0 12.4094 2.35371 1 4 6 0 12.8587 2.47705 1 4 6 0 10.7434 1.90155 2 -4 6 0 6.53853 3.01003 1 5 -6 0 30.7161 5.84856 1 5 6 0 25.9584 3.78949 1 5 6 0 23.0972 3.84174 1 -5 6 0 27.1309 5.42287 1 5 6 0 25.5011 2.56545 2 6 -6 0 160.564 12.3850 1 6 6 0 130.813 9.11376 1 6 6 0 151.581 6.12925 2 -6 6 0 122.110 10.7286 1 7 -6 0 75.9353 10.3730 1 -7 6 0 81.6710 10.2123 1 7 6 0 62.3554 7.53628 1 8 -6 0 6.42605 5.09977 1 -8 6 0 10.6619 4.95351 1 8 6 0 11.3402 4.25589 1 9 -6 0 6.54996 5.57661 1 9 6 0 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16.9901 2 1 0 -12 69.5958 12.7855 1 1 0 -12 57.3905 10.5359 3 -1 0 12 57.0461 12.2590 2 0 0 12 74.5386 14.0351 2 0 0 -12 53.2783 11.7574 1 1 0 12 86.0907 15.0057 2 -1 0 -12 119.774 17.6815 1 -9 -1 12 6.85169 5.83647 2 9 -1 -12 3.49404 5.53591 1 -9 1 12 0.21226 5.37738 2 9 1 -12 -1.1426 4.71597 1 8 -1 -12 8.46801 6.42093 1 -8 -1 12 3.54556 5.36731 2 8 1 -12 2.43999 5.06778 1 -8 1 12 -2.4187 4.88395 2 8 1 -12 8.35627 5.52801 1 -7 -1 12 48.5304 9.86240 2 7 -1 -12 65.4489 11.9948 1 7 -1 -12 51.9223 10.7315 1 7 1 -12 39.9311 9.13063 1 -7 1 12 65.7798 12.0696 2 6 -1 -12 204.843 20.3836 1 -6 -1 12 156.115 17.2671 2 -6 1 12 181.712 19.0903 2 6 1 -12 190.061 19.0195 1 6 1 -12 167.651 14.1669 3 5 -1 -12 123.141 16.0642 1 -5 -1 12 76.5177 12.9986 2 5 1 -12 67.0850 11.3227 1 5 1 -12 98.3721 12.3203 3 -5 1 12 73.3575 12.5951 2 4 -1 -12 39.6010 8.23743 3 -4 -1 12 24.7081 9.30215 2 4 -1 -12 26.5239 8.53318 1 -4 1 12 43.2045 10.9033 2 4 1 -12 44.3393 8.98189 3 4 1 -12 38.0595 9.72122 1 -3 -1 12 10.0995 7.82492 2 3 -1 -12 2.83275 5.00425 3 3 -1 -12 0.99753 4.75107 1 -3 1 12 7.21755 6.90410 2 3 1 -12 4.53000 5.09138 3 3 1 -12 7.22894 6.27835 1 -2 -1 12 22.8537 9.13473 2 2 -1 -12 21.9153 6.95398 3 2 -1 -12 6.00675 6.40301 1 2 1 -12 8.13287 6.85490 1 -2 1 12 29.5826 9.42079 2 2 1 -12 12.7178 6.27479 3 -1 -1 12 10.0942 7.73552 2 1 -1 -12 10.2674 7.26522 1 -1 1 12 4.14794 6.57746 2 1 1 -12 6.73519 6.37644 1 1 1 -12 10.8789 5.92982 3 0 -1 12 22.4516 9.13727 2 0 -1 -12 21.5287 9.11872 1 0 1 12 22.5344 8.96868 2 0 1 -12 12.7084 7.23502 1 -1 -1 -12 -0.5541 6.03620 1 1 -1 12 11.5863 7.50279 2 1 1 12 5.36206 6.88131 2 -1 1 -12 -2.0287 5.87715 1 -9 -2 12 12.3686 6.88326 2 9 -2 -12 25.8388 8.81935 1 9 2 -12 8.82540 5.99120 1 -9 2 12 25.1063 8.28516 2 8 -2 -12 72.3716 12.3880 1 -8 -2 12 94.5089 13.2401 2 8 2 -12 91.8725 13.1793 1 8 2 -12 91.6379 13.2257 1 -8 2 12 78.9985 12.7229 2 7 -2 -12 12.1312 6.78659 1 7 -2 -12 -1.3298 4.85047 1 -7 -2 12 -5.7234 4.94092 2 7 2 -12 -4.8556 4.14380 1 -7 2 12 -2.9782 4.66699 2 -6 -2 12 4.03360 5.46181 2 6 -2 -12 -2.6719 4.81274 1 6 -2 -12 2.49540 5.36269 1 6 2 -12 0.37784 4.88703 1 -6 2 12 0.86992 5.83754 2 6 2 -12 3.00713 4.59433 3 -5 -2 12 71.2201 12.5665 2 5 -2 -12 53.8580 10.8292 1 -5 2 12 69.7152 13.1397 2 5 2 -12 77.4629 11.4969 3 5 2 -12 75.4988 12.0132 1 4 -2 -12 212.038 18.6753 1 -4 -2 12 181.488 19.2873 2 4 -2 -12 207.198 15.5881 3 -4 2 12 243.563 22.8650 2 4 2 -12 224.196 16.9999 3 4 2 -12 216.510 18.6856 1 -3 -2 12 5.62811 5.62126 2 3 -2 -12 17.1797 6.42478 3 3 -2 -12 28.5532 8.91562 1 3 2 -12 17.1591 6.26095 3 -3 2 12 20.7246 8.83461 2 3 2 -12 0.72337 5.68704 1 -2 -2 12 36.4249 9.44519 2 2 -2 -12 49.5417 10.7801 1 2 -2 -12 48.5486 9.30055 3 -2 2 12 53.0591 11.7676 2 2 2 -12 50.5997 9.81384 3 2 2 -12 39.6959 10.0789 1 -1 -2 12 -1.1039 4.88827 2 1 -2 -12 -5.0426 3.91793 1 1 2 -12 -7.0491 3.51927 3 -1 2 12 5.14040 6.56572 2 1 2 -12 -3.0617 4.88306 1 0 -2 12 50.3664 11.6661 2 0 -2 -12 60.1613 12.3440 1 0 2 12 26.1938 8.86102 2 0 2 -12 55.4508 11.6575 1 1 -2 12 3.82175 6.61779 2 -1 -2 -12 -8.4536 5.25317 1 -1 2 -12 6.99459 7.08208 1 1 2 12 3.79251 7.56686 2 8 -3 -12 9.16287 6.28743 1 -8 -3 12 9.56419 6.18958 2 8 3 -12 10.5715 5.98228 1 -8 3 12 19.7638 7.82599 2 7 -3 -12 0.70712 5.89047 1 -7 -3 12 -9.3088 3.56368 2 -7 3 12 -0.2584 5.35020 2 7 3 -12 7.97269 5.38113 1 6 -3 -12 152.923 17.9134 1 -6 -3 12 207.850 19.6033 2 6 -3 -12 183.570 19.2558 1 -6 3 12 168.119 18.2996 2 6 3 -12 232.004 17.5988 1 6 3 -12 176.752 17.1801 3 5 -3 -12 52.4942 10.8177 1 5 -3 -12 47.7138 10.2489 1 -5 -3 12 54.8322 10.7669 2 5 3 -12 57.6592 11.2089 1 -5 3 12 57.8421 11.7122 2 5 3 -12 68.3586 10.9566 3 -4 -3 12 277.025 21.4405 2 4 -3 -12 279.684 21.4447 1 -4 3 12 279.908 22.0571 2 4 3 -12 269.655 19.3411 3 4 3 -12 304.170 21.8459 1 3 -3 -12 6.93089 5.47051 3 3 -3 -12 5.01204 6.06384 1 -3 -3 12 1.91412 5.87165 2 3 3 -12 10.7027 5.25368 3 3 3 -12 3.52782 6.04413 1 -3 3 12 0.24777 6.31654 2 2 -3 -12 15.7314 7.30751 1 -2 -3 12 23.6811 9.09355 2 2 -3 -12 7.73503 5.49903 3 2 3 -12 12.5939 6.92861 1 2 3 -12 10.0312 5.98684 3 -2 3 12 19.3787 8.36215 2 1 -3 -12 9.05840 6.01022 1 -1 -3 12 5.69666 6.82572 2 1 3 -12 5.51747 5.83314 1 1 3 -12 15.4940 6.72774 3 -1 3 12 6.12703 6.55720 2 0 -3 12 13.2179 7.65653 2 0 -3 -12 26.6656 8.44967 1 0 3 -12 12.9892 6.93513 3 0 3 12 10.5892 7.55745 2 0 3 -12 12.7199 7.19559 1 -8 -4 12 14.1690 6.44053 2 8 -4 -12 1.28168 5.83966 1 -8 4 12 -2.2099 5.61414 2 8 4 -12 2.69540 5.02049 1 -7 -4 12 -2.6261 4.52757 2 7 -4 -12 1.10982 4.83467 1 7 4 -12 0.32903 3.94988 1 -7 4 12 -0.7470 5.63635 2 6 -4 -12 50.2836 10.8954 1 -6 -4 12 88.5898 13.4236 2 6 -4 -12 80.8664 13.5669 1 6 4 -12 77.2032 12.0877 1 -6 4 12 67.6090 12.5790 2 6 4 -12 92.9279 12.8605 3 5 -4 -12 6.04007 6.50792 1 -5 -4 12 -1.3727 4.68554 2 5 -4 -12 -4.2541 4.80552 1 -5 4 12 5.68090 6.85670 2 5 4 -12 1.92559 4.65719 3 5 4 -12 3.95265 5.66777 1 4 -4 -12 12.0777 6.82848 1 -4 -4 12 0.73428 5.76853 2 4 -4 -12 4.81245 5.63920 1 4 4 -12 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-12 20.8989 7.64329 1 -5 5 12 17.4179 8.59620 2 5 5 -12 22.0761 7.72403 1 5 5 -12 23.9349 7.33640 3 -4 -5 12 5.20792 6.11754 2 4 -5 -12 0.55640 5.56722 1 4 -5 -12 -3.6289 4.74770 1 -4 5 12 8.22323 6.97644 2 4 5 -12 1.92002 4.19438 3 4 5 -12 -0.5356 4.52052 1 3 -5 -12 4.03336 5.55158 1 -3 -5 12 6.83372 6.85947 2 3 -5 -12 2.48775 4.93940 1 3 5 -12 9.77143 6.23974 3 3 5 -12 0.52973 5.17453 1 -3 5 12 2.33881 6.16679 2 -2 -5 12 3.92768 6.68962 2 2 -5 -12 2.95439 5.92619 1 2 5 -12 3.66072 5.29909 3 2 5 -12 5.95712 6.36730 1 -2 5 12 1.73924 5.58090 2 -1 -5 12 2.05222 5.87231 2 1 -5 -12 6.35405 6.79588 1 1 5 -12 3.62863 5.46898 3 -1 5 12 11.1005 7.43944 2 1 5 -12 19.0383 7.71858 1 0 -5 -12 8.84489 7.11709 1 0 -5 12 12.3803 7.32291 2 0 5 -12 18.8411 8.12942 3 0 5 -12 20.2302 8.45749 1 0 5 12 8.60325 7.70591 2 -8 -6 12 9.20536 9.10381 2 8 -6 -12 10.8061 7.22942 1 -8 6 12 5.75907 6.50941 2 8 6 -12 7.34168 5.85723 1 -7 -6 12 15.4843 7.09251 2 7 -6 -12 9.33044 6.95100 1 -7 6 12 9.44208 7.09862 2 7 6 -12 8.68809 5.67356 1 6 -6 -12 15.2892 7.73459 1 -6 -6 12 14.6675 6.98944 2 6 6 -12 18.3629 6.96613 1 -6 6 12 10.9762 7.50363 2 6 6 -12 19.5723 7.14713 3 -5 -6 12 9.84952 6.86043 2 5 -6 -12 6.53407 6.21031 1 -5 6 12 16.5036 7.61086 2 5 6 -12 7.31074 5.96235 3 5 6 -12 2.13255 5.19689 1 4 -6 -12 10.5077 6.27596 1 4 -6 -12 5.68900 6.55393 1 -4 -6 12 3.48603 5.78574 2 -4 6 12 2.78845 6.07995 2 4 6 -12 6.64316 5.33551 3 4 6 -12 -0.3748 5.03605 1 -3 -6 12 83.5385 13.9632 2 3 -6 -12 96.5267 14.8065 1 3 -6 -12 76.6236 13.9585 1 3 6 -12 72.3958 12.3678 1 -3 6 12 85.6994 14.5634 2 3 6 -12 85.9622 13.0994 3 2 -6 -12 12.8816 7.12964 1 -2 -6 12 15.2832 7.59700 2 2 -6 -12 9.56854 7.40711 1 2 6 -12 8.89937 5.67449 3 -2 6 12 2.05564 6.61889 2 2 6 -12 10.6492 6.44393 1 1 -6 -12 5.99963 6.40853 1 -1 -6 12 23.7515 8.77396 2 1 6 -12 4.53349 6.25411 3 -1 6 12 5.52274 6.05509 2 1 6 -12 8.20662 6.58822 1 0 -6 -12 8.05661 6.67512 1 0 -6 12 20.9089 9.34954 2 0 6 12 20.6197 9.29812 2 0 6 -12 2.58468 6.35539 1 0 6 -12 8.56428 7.02805 3 0 6 12 10.5618 11.5104 1 -7 -7 12 15.5493 6.96880 2 7 -7 -12 5.98101 6.67564 1 7 7 -12 8.80374 6.04756 1 -7 7 12 13.4131 7.81293 2 6 -7 -12 29.2328 9.08393 1 -6 -7 12 35.8739 9.39541 2 6 7 -12 37.2159 9.12356 3 6 7 -12 34.0948 8.46709 1 -6 7 12 38.0559 10.5455 2 -5 -7 12 3.85364 6.33989 2 5 -7 -12 -3.3315 5.14614 1 5 7 -12 3.40505 4.84309 1 -5 7 12 4.51022 6.19672 2 5 7 -12 1.05625 4.71853 3 -4 -7 12 4.61599 6.10959 2 4 -7 -12 16.4606 8.06661 1 4 7 -12 6.52535 5.78044 1 4 7 -12 7.05124 5.82204 3 -4 7 12 8.53902 7.79250 2 3 -7 -12 8.54928 6.60461 1 3 -7 -12 3.03365 6.42096 1 -3 -7 12 -0.1868 5.35957 2 3 7 -12 5.70976 5.26472 3 -3 7 12 1.99309 6.20987 2 3 7 -12 3.18817 4.92988 1 2 -7 -12 60.5588 12.3709 1 -2 -7 12 65.4950 12.5554 2 2 -7 -12 37.1140 10.0795 1 2 7 -12 49.5273 10.2380 3 -2 7 12 60.8554 12.8326 2 2 7 -12 48.0537 10.9769 1 -1 -7 12 7.78821 7.06369 2 1 -7 -12 -1.3843 5.86153 1 1 -7 -12 8.76570 6.89264 1 1 7 -12 -2.5285 5.40528 3 -1 7 12 0.30699 5.62169 2 1 7 -12 -1.0038 5.43413 1 7 -8 -12 93.4763 15.8252 1 -7 -8 12 93.4568 12.9126 2 -7 8 12 91.5812 14.4715 2 7 8 -12 81.7101 11.9202 1 6 -8 -12 97.4910 15.6936 1 -6 -8 12 110.706 14.5232 2 6 8 -12 103.317 13.7003 1 6 8 -12 102.837 14.4403 3 -6 8 12 119.181 16.6397 2 5 -8 -12 37.3552 10.1980 1 -5 -8 12 32.9020 9.58089 2 5 8 -12 28.6595 9.14507 3 -5 8 12 49.6404 11.4176 2 5 8 -12 51.6845 10.4456 1 4 -8 -12 13.8756 7.44153 1 -4 -8 12 8.47918 7.14185 2 4 8 -12 11.5398 6.26178 1 4 8 -12 6.73832 5.89398 3 -4 8 12 0.03414 6.06332 2 -3 -8 12 35.8507 9.93977 2 3 -8 -12 30.0853 9.31532 1 3 8 -12 41.6098 10.0100 3 3 8 -12 17.3365 7.41300 1 -3 8 12 30.6858 10.2850 2 -2 -8 12 1.22413 5.89535 2 2 -8 -12 -3.8745 5.38287 1 2 -8 -12 -1.6946 5.58428 1 -2 8 12 -0.9660 5.90569 2 2 8 -12 -4.3047 4.61162 1 2 8 -12 4.99642 5.72330 3 1 -8 -12 -2.2851 5.29907 1 1 -8 -12 -6.2001 5.05031 1 -1 -8 12 1.45081 6.70877 2 -1 8 12 -1.0583 5.95061 2 1 8 -12 -6.8731 4.63601 1 1 8 -12 -0.5359 5.41191 3 -1 8 12 -3.6495 5.80580 1 6 -9 -12 10.1426 6.92529 1 -6 -9 12 16.9643 7.26260 2 -6 9 12 18.2922 8.58869 2 6 9 -12 9.34895 6.28756 3 6 9 -12 11.8949 6.36970 1 -5 -9 12 59.3877 11.8219 2 5 -9 -12 71.7110 13.6385 1 5 9 -12 45.1777 10.6291 3 5 9 -12 67.7661 11.3016 1 -5 9 12 53.6809 12.5829 2 -4 -9 12 30.4053 8.68659 2 4 -9 -12 44.8355 10.9682 1 4 9 -12 53.9477 11.0215 3 -4 9 12 30.6587 10.2988 2 4 9 -12 46.3153 10.6264 1 3 -9 -12 88.7902 15.0430 1 -3 -9 12 68.0582 13.0093 2 3 9 -12 107.414 15.0063 1 3 9 -12 121.338 16.0832 3 -3 9 12 84.6964 14.7836 2 2 -9 -12 19.7454 9.46241 1 -2 -9 12 9.39809 7.69611 2 2 9 -12 26.1539 9.03385 1 2 9 -12 41.0224 10.0551 3 -2 9 12 23.8487 9.99352 2 -5 -10 12 -2.6268 5.00633 2 -5 10 12 3.26728 7.26657 2 -4 -10 12 10.3194 6.95812 2 4 -10 -12 8.06937 7.93572 1 4 10 -12 7.97385 6.64005 3 -4 10 12 19.1241 9.45295 2 4 10 -12 13.1633 6.77271 1 -3 -10 12 62.9210 12.5170 2 -3 10 12 53.8713 12.3959 2 -6 0 13 3.62981 6.65714 2 6 0 -13 -5.3319 4.94029 1 -5 0 13 -1.3251 5.88227 2 5 0 -13 6.02108 6.27155 1 -4 0 13 4.69518 6.69460 2 4 0 -13 6.06943 6.18712 1 4 0 -13 0.75682 5.01616 3 3 0 -13 3.69712 5.02661 3 3 0 -13 3.53724 5.58592 1 -3 0 13 -1.2706 6.02636 2 2 0 -13 2.79376 6.04265 1 -2 0 13 3.97583 7.09248 2 2 0 -13 -3.6017 4.70769 3 6 -1 -13 320.499 23.8162 1 -6 -1 13 340.588 24.1334 2 6 1 -13 336.246 24.0176 1 -6 1 13 307.262 23.7329 2 -5 -1 13 182.092 20.0437 2 5 -1 -13 137.653 17.4801 1 5 1 -13 174.089 17.2223 3 -5 1 13 138.139 17.7279 2 5 1 -13 175.625 19.5647 1 -4 -1 13 98.6286 15.9405 2 4 -1 -13 105.172 15.5820 1 4 1 -13 89.0014 12.5354 3 4 1 -13 106.342 15.2522 1 -4 1 13 93.3582 15.7283 2 -3 -1 13 16.3316 8.32943 2 3 -1 -13 24.8111 7.37154 3 3 -1 -13 29.2243 9.15806 1 -3 1 13 27.7549 10.4702 2 3 1 -13 35.2486 10.6123 1 3 1 -13 32.1348 8.63144 3 2 -1 -13 61.4936 11.0004 3 -2 -1 13 63.4358 13.4693 2 2 -1 -13 40.0139 10.5091 1 2 1 -13 50.8033 10.2566 3 2 1 -13 54.6425 12.5545 1 -2 1 13 45.9576 11.8978 2 6 -2 -13 3.70686 5.85820 1 6 -2 -13 5.77572 6.26599 1 -6 -2 13 -1.1028 5.37593 2 6 2 -13 -3.7586 4.89352 1 -6 2 13 5.53611 7.36244 2 -5 -2 13 13.1198 7.58932 2 5 -2 -13 24.0499 8.47541 1 5 2 -13 23.1781 7.49416 3 -5 2 13 36.8034 11.4522 2 5 2 -13 31.4009 8.41607 1 -4 -2 13 6.71276 7.42048 2 4 -2 -13 33.1165 9.05106 1 -4 2 13 16.1373 8.27161 2 4 2 -13 13.0845 7.52218 1 4 2 -13 12.9181 6.45265 3 -3 -2 13 6.27616 6.63779 2 3 -2 -13 2.73087 5.29562 3 3 -2 -13 -0.7431 5.43020 1 3 2 -13 12.5946 7.41022 1 3 2 -13 3.41170 5.10164 3 -3 2 13 5.93533 7.58246 2 2 -2 -13 50.1803 9.69927 3 2 -2 -13 26.7643 8.83447 1 -2 -2 13 29.9056 10.1920 2 2 2 -13 32.2157 10.5252 1 2 2 -13 20.8426 8.08201 3 -2 2 13 60.5732 13.5146 2 6 -3 -13 12.3036 7.42701 1 -6 -3 13 13.8876 7.50880 2 6 -3 -13 4.72560 6.22160 1 -6 3 13 4.54793 6.63242 2 6 3 -13 8.53260 6.51834 1 6 3 -13 10.7867 6.14780 3 5 -3 -13 -4.3552 5.02085 1 5 -3 -13 4.29832 6.20672 1 -5 -3 13 7.08126 6.46668 2 5 3 -13 4.54955 5.48783 3 5 3 -13 1.70021 5.76723 1 -5 3 13 0.97861 6.19752 2 -4 -3 13 95.0332 15.2631 2 4 -3 -13 85.5109 14.3071 1 -4 3 13 108.285 17.1477 2 4 3 -13 109.722 14.4444 3 4 3 -13 81.1510 14.3164 1 3 -3 -13 -1.7167 6.37925 1 -3 -3 13 6.46013 6.74788 2 -3 3 13 -4.7416 6.03366 2 3 3 -13 9.88452 5.78760 3 3 3 -13 13.2447 7.80278 1 5 -4 -13 4.75251 6.39066 1 5 -4 -13 5.28368 5.96795 1 -5 -4 13 0.36913 5.86438 2 -5 4 13 1.81297 6.16531 2 5 4 -13 11.6289 6.23243 3 5 4 -13 8.36423 6.55031 1 -4 -4 13 10.7985 7.79341 2 4 -4 -13 10.7238 7.20561 1 4 -4 -13 14.3518 7.39439 1 4 4 -13 21.0068 7.74830 3 -4 4 13 27.7815 9.92740 2 4 4 -13 16.4134 7.84755 1 3 -4 -13 29.9171 9.83852 1 -3 -4 13 18.3145 8.18759 2 -3 4 13 46.5328 11.9647 2 3 4 -13 23.1368 8.67391 1 3 4 -13 12.1187 6.69106 3 -4 -5 13 -0.8099 6.17943 2 -4 5 13 19.6376 8.63658 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.8585 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71072 10.215 18.801 10.652 89.968 110.267 89.993 ) ; _shelx_hkl_checksum 89002 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 O1 O 0.24495(11) 0.20600(5) 0.54717(9) 0.0194(2) Uani 1 1 d . . O2 O 0.07810(11) 0.25864(5) 0.32604(9) 0.0223(3) Uani 1 1 d . . C1 C 0.33581(16) 0.17549(8) 0.66931(14) 0.0214(3) Uani 1 1 d . . H26 H 0.4313 0.1924 0.6871 0.032 Uiso 1 1 calc R U H1 H 0.3335 0.1236 0.6615 0.032 Uiso 1 1 calc R U H3 H 0.3049 0.1896 0.7430 0.032 Uiso 1 1 calc R U C2 C 0.23506(15) 0.27875(7) 0.54295(13) 0.0160(3) Uani 1 1 d . . C3 C 0.14455(14) 0.30793(7) 0.42163(13) 0.0164(3) Uani 1 1 d . . C4 C 0.13243(14) 0.38083(7) 0.40777(13) 0.0159(3) Uani 1 1 d . . H7 H 0.0713 0.4003 0.3263 0.019 Uiso 1 1 calc R U C5 C 0.20859(14) 0.42716(7) 0.51153(13) 0.0145(3) Uani 1 1 d . . C6 C 0.19690(14) 0.50780(7) 0.48887(13) 0.0147(3) Uani 1 1 d . . H17 H 0.1178 0.5249 0.5157 0.018 Uiso 1 1 calc R U C7 C 0.33179(15) 0.54444(7) 0.58194(13) 0.0158(3) Uani 1 1 d . . H18 H 0.4117 0.5258 0.5578 0.019 Uiso 1 1 calc R U C8 C 0.33076(15) 0.62460(7) 0.56819(13) 0.0160(3) Uani 1 1 d . . C9 C 0.41788(16) 0.65880(8) 0.51204(14) 0.0205(3) Uani 1 1 d . . H20 H 0.4748 0.6314 0.4764 0.025 Uiso 1 1 calc R U C10 C 0.42289(17) 0.73251(8) 0.50734(15) 0.0243(4) Uani 1 1 d . . H21 H 0.4829 0.7549 0.4684 0.029 Uiso 1 1 calc R U C11 C 0.34108(16) 0.77358(8) 0.55890(14) 0.0220(3) Uani 1 1 d . . H2 H 0.3458 0.8240 0.5568 0.026 Uiso 1 1 calc R U C12 C -0.00579(16) 0.28356(8) 0.19676(13) 0.0223(3) Uani 1 1 d . . H5 H -0.0831 0.3120 0.2041 0.033 Uiso 1 1 calc R U H6 H -0.0431 0.2429 0.1377 0.033 Uiso 1 1 calc R U H4 H 0.0512 0.3129 0.1596 0.033 Uiso 1 1 calc R U C13 C 0.29556(14) 0.39805(7) 0.63234(13) 0.0148(3) Uani 1 1 d . . C14 C 0.38527(15) 0.44275(8) 0.74977(13) 0.0175(3) Uani 1 1 d . . H8 H 0.4850 0.4349 0.7588 0.021 Uiso 1 1 calc R U C15 C 0.36939(17) 0.42028(8) 0.88228(13) 0.0220(3) Uani 1 1 d . . H9 H 0.4320 0.4488 0.9555 0.033 Uiso 1 1 calc R U H11 H 0.3934 0.3699 0.8989 0.033 Uiso 1 1 calc R U H10 H 0.2727 0.4278 0.8770 0.033 Uiso 1 1 calc R U C16 C 0.35532(16) 0.52170(7) 0.72643(13) 0.0191(3) Uani 1 1 d . . H23 H 0.4347 0.5489 0.7878 0.023 Uiso 1 1 calc R U H24 H 0.2713 0.5337 0.7482 0.023 Uiso 1 1 calc R U C17 C 0.16572(15) 0.52925(7) 0.34395(13) 0.0157(3) Uani 1 1 d . . C18 C 0.25015(15) 0.50578(8) 0.27357(13) 0.0174(3) Uani 1 1 d . . H16 H 0.3270 0.4754 0.3164 0.021 Uiso 1 1 calc R U C19 C 0.22325(16) 0.52626(8) 0.14193(14) 0.0207(3) Uani 1 1 d . . H15 H 0.2817 0.5099 0.0954 0.025 Uiso 1 1 calc R U C20 C 0.11141(16) 0.57059(8) 0.07793(14) 0.0228(3) Uani 1 1 d . . H14 H 0.0926 0.5842 -0.0124 0.027 Uiso 1 1 calc R U C21 C 0.02753(16) 0.59478(8) 0.14673(15) 0.0232(3) Uani 1 1 d . . H13 H -0.0484 0.6257 0.1039 0.028 Uiso 1 1 calc R U C22 C 0.05405(15) 0.57397(7) 0.27868(14) 0.0194(3) Uani 1 1 d . . H12 H -0.0047 0.5905 0.3247 0.023 Uiso 1 1 calc R U C23 C 0.24676(16) 0.66684(8) 0.61732(15) 0.0216(3) Uani 1 1 d . . H19 H 0.1846 0.6447 0.6541 0.026 Uiso 1 1 calc R U C24 C 0.25223(16) 0.74045(8) 0.61354(15) 0.0230(3) Uani 1 1 d . . H22 H 0.1950 0.7681 0.6484 0.028 Uiso 1 1 calc R U C25 C 0.30719(15) 0.32377(7) 0.64524(13) 0.0162(3) Uani 1 1 d . . H25 H 0.3667 0.3040 0.7272 0.019 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 O1 0.0255(6) 0.0124(5) 0.0186(5) 0.0006(4) 0.0056(4) -0.0002(4) O2 0.0279(6) 0.0174(6) 0.0165(5) -0.0022(4) 0.0012(4) -0.0047(4) C1 0.0261(9) 0.0174(8) 0.0200(7) 0.0035(6) 0.0070(6) 0.0012(6) C2 0.0170(8) 0.0148(7) 0.0193(7) 0.0008(5) 0.0102(6) -0.0008(5) C3 0.0162(7) 0.0179(8) 0.0162(7) -0.0033(5) 0.0069(6) -0.0046(6) C4 0.0141(7) 0.0185(8) 0.0154(7) 0.0010(5) 0.0056(6) -0.0002(6) C5 0.0128(7) 0.0161(7) 0.0163(7) -0.0010(5) 0.0073(5) -0.0017(5) C6 0.0125(7) 0.0148(7) 0.0173(7) -0.0014(5) 0.0060(5) 0.0001(5) C7 0.0145(7) 0.0161(7) 0.0174(7) -0.0010(5) 0.0060(5) -0.0010(6) C8 0.0172(7) 0.0158(7) 0.0130(6) -0.0020(5) 0.0025(5) -0.0020(6) C9 0.0233(8) 0.0204(8) 0.0202(7) -0.0007(6) 0.0106(6) -0.0006(6) C10 0.0292(9) 0.0207(8) 0.0268(8) 0.0029(6) 0.0147(7) -0.0035(7) C11 0.0228(8) 0.0152(8) 0.0245(8) 0.0006(6) 0.0038(6) -0.0015(6) C12 0.0223(8) 0.0248(8) 0.0164(7) -0.0030(6) 0.0026(6) -0.0008(6) C13 0.0139(7) 0.0167(7) 0.0154(7) -0.0009(5) 0.0072(5) -0.0016(5) C14 0.0177(8) 0.0186(8) 0.0155(7) -0.0006(5) 0.0049(6) -0.0020(6) C15 0.0286(9) 0.0201(8) 0.0162(7) -0.0013(6) 0.0063(6) -0.0044(6) C16 0.0225(8) 0.0170(8) 0.0167(7) -0.0032(6) 0.0055(6) -0.0045(6) C17 0.0156(7) 0.0125(7) 0.0175(7) -0.0019(5) 0.0040(5) -0.0037(5) C18 0.0157(7) 0.0164(8) 0.0188(7) 0.0002(5) 0.0044(6) 0.0003(6) C19 0.0241(8) 0.0196(8) 0.0195(7) -0.0026(6) 0.0089(6) -0.0037(6) C20 0.0287(9) 0.0193(8) 0.0170(7) 0.0033(6) 0.0037(6) -0.0042(6) C21 0.0227(8) 0.0157(8) 0.0258(8) 0.0039(6) 0.0015(6) 0.0006(6) C22 0.0173(8) 0.0156(8) 0.0243(7) -0.0004(6) 0.0062(6) 0.0001(6) C23 0.0203(8) 0.0208(8) 0.0268(8) 0.0018(6) 0.0119(6) 0.0004(6) C24 0.0236(8) 0.0194(8) 0.0264(8) -0.0027(6) 0.0091(7) 0.0026(6) C25 0.0157(7) 0.0189(8) 0.0140(6) 0.0018(5) 0.0051(5) -0.0004(6) 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 C2 O1 C1 116.55(11) C3 O2 C12 118.18(11) O1 C1 H26 109.5 O1 C1 H1 109.5 H26 C1 H1 109.5 O1 C1 H3 109.5 H26 C1 H3 109.5 H1 C1 H3 109.5 O1 C2 C25 125.13(12) O1 C2 C3 115.76(12) C25 C2 C3 119.10(13) O2 C3 C4 126.14(12) O2 C3 C2 114.53(12) C4 C3 C2 119.31(12) C3 C4 C5 121.70(13) C3 C4 H7 119.2 C5 C4 H7 119.2 C13 C5 C4 118.76(13) C13 C5 C6 121.49(12) C4 C5 C6 119.73(12) C17 C6 C5 113.58(11) C17 C6 C7 111.00(11) C5 C6 C7 109.59(11) C17 C6 H17 107.5 C5 C6 H17 107.5 C7 C6 H17 107.5 C8 C7 C16 111.59(11) C8 C7 C6 113.92(11) C16 C7 C6 108.23(11) C8 C7 H18 107.6 C16 C7 H18 107.6 C6 C7 H18 107.6 C9 C8 C23 117.74(13) C9 C8 C7 121.22(13) C23 C8 C7 120.97(13) C10 C9 C8 120.97(14) C10 C9 H20 119.5 C8 C9 H20 119.5 C11 C10 C9 120.55(14) C11 C10 H21 119.7 C9 C10 H21 119.7 C10 C11 C24 119.30(14) C10 C11 H2 120.3 C24 C11 H2 120.3 O2 C12 H5 109.5 O2 C12 H6 109.5 H5 C12 H6 109.5 O2 C12 H4 109.5 H5 C12 H4 109.5 H6 C12 H4 109.5 C5 C13 C25 119.01(12) C5 C13 C14 123.35(13) C25 C13 C14 117.56(12) C16 C14 C13 112.08(11) C16 C14 C15 109.89(12) C13 C14 C15 112.24(12) C16 C14 H8 107.5 C13 C14 H8 107.5 C15 C14 H8 107.5 C14 C15 H9 109.5 C14 C15 H11 109.5 H9 C15 H11 109.5 C14 C15 H10 109.5 H9 C15 H10 109.5 H11 C15 H10 109.5 C14 C16 C7 112.91(11) C14 C16 H23 109.0 C7 C16 H23 109.0 C14 C16 H24 109.0 C7 C16 H24 109.0 H23 C16 H24 107.8 C22 C17 C18 118.27(13) C22 C17 C6 120.96(13) C18 C17 C6 120.76(12) C19 C18 C17 120.86(14) C19 C18 H16 119.6 C17 C18 H16 119.6 C18 C19 C20 120.30(14) C18 C19 H15 119.8 C20 C19 H15 119.8 C21 C20 C19 119.51(13) C21 C20 H14 120.2 C19 C20 H14 120.2 C20 C21 C22 120.22(14) C20 C21 H13 119.9 C22 C21 H13 119.9 C21 C22 C17 120.84(14) C21 C22 H12 119.6 C17 C22 H12 119.6 C24 C23 C8 121.39(14) C24 C23 H19 119.3 C8 C23 H19 119.3 C11 C24 C23 120.03(14) C11 C24 H22 120.0 C23 C24 H22 120.0 C2 C25 C13 122.08(13) C2 C25 H25 119.0 C13 C25 H25 119.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C2 1.3727(17) O1 C1 1.4313(17) O2 C3 1.3712(16) O2 C12 1.4265(17) C1 H26 0.9800 C1 H1 0.9800 C1 H3 0.9800 C2 C25 1.3758(19) C2 C3 1.4142(19) C3 C4 1.381(2) C4 C5 1.4117(19) C4 H7 0.9500 C5 C13 1.3981(18) C5 C6 1.5351(19) C6 C17 1.5200(18) C6 C7 1.5525(19) C6 H17 1.0000 C7 C8 1.516(2) C7 C16 1.5355(18) C7 H18 1.0000 C8 C9 1.391(2) C8 C23 1.398(2) C9 C10 1.390(2) C9 H20 0.9500 C10 C11 1.385(2) C10 H21 0.9500 C11 C24 1.385(2) C11 H2 0.9500 C12 H5 0.9800 C12 H6 0.9800 C12 H4 0.9800 C13 C25 1.406(2) C13 C14 1.5229(18) C14 C16 1.520(2) C14 C15 1.5364(19) C14 H8 1.0000 C15 H9 0.9800 C15 H11 0.9800 C15 H10 0.9800 C16 H23 0.9900 C16 H24 0.9900 C17 C22 1.394(2) C17 C18 1.397(2) C18 C19 1.3879(19) C18 H16 0.9500 C19 C20 1.388(2) C19 H15 0.9500 C20 C21 1.384(2) C20 H14 0.9500 C21 C22 1.393(2) C21 H13 0.9500 C22 H12 0.9500 C23 C24 1.388(2) C23 H19 0.9500 C24 H22 0.9500 C25 H25 0.9500