#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:45:56 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225903 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515778.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_4515778 loop_ _publ_author_name 'Lad, Bapurao Sudam' 'Katukojvala, Sreenivas' _publ_section_title ; Piano-Stool Rhodium Enalcarbenoids: Application to Catalyst-Controlled Metal-Templated Annulations of Diazoenals and 1,3-Dicarbonyls ; _journal_issue 12 _journal_name_full 'ACS Catalysis' _journal_page_first 11807 _journal_paper_doi 10.1021/acscatal.8b03865 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C26 H18 O3' _chemical_formula_sum 'C26 H18 O3' _chemical_formula_weight 378.40 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 100.161(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.897(3) _cell_length_b 5.8589(6) _cell_length_c 26.361(3) _cell_measurement_reflns_used 6876 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.00 _cell_measurement_theta_min 2.48 _cell_volume 3784.9(7) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.969 _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 0.0895 _diffrn_reflns_av_unetI/netI 0.0708 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 18674 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.145 _diffrn_reflns_theta_min 2.480 _exptl_absorpt_correction_type none _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.328 _exptl_crystal_description needle _exptl_crystal_F_000 1584 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.254 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 4081 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0532 _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^)+(0.0346P)^2^+4.4542P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0994 _refine_ls_wR_factor_ref 0.1152 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2760 _reflns_number_total 4081 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b03865_si_002.cif _cod_data_source_block BL_04-404 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 4515778 _shelx_shelxl_version_number 2016/6 _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_res_file ; TITL m1_a.res in C2/c shelx.res created by SHELXL-2016/6 at 15:14:30 on 22-Apr-2017 CELL 0.71073 24.8971 5.8589 26.3611 90.000 100.161 90.000 ZERR 8.00 0.0030 0.0006 0.0031 0.000 0.004 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O UNIT 208 144 24 MERG 2 MORE -1 FMAP 2 PLAN 5 ACTA BOND $H CONF LIST 6 L.S. 11 TEMP -153.14 WGHT 0.034600 4.454200 EXTI 0.002231 FVAR 0.26991 O1 3 0.576749 0.603358 0.299889 11.00000 0.01701 0.02017 = 0.01984 -0.00137 0.00384 -0.00336 O2 3 0.651905 1.255011 0.364815 11.00000 0.02670 0.01783 = 0.03717 -0.00014 0.00106 0.00211 O3 3 0.570089 1.267668 0.521368 11.00000 0.04837 0.06882 = 0.04658 -0.03563 0.01906 -0.01453 C1 1 0.617102 0.767020 0.304097 11.00000 0.01472 0.01503 = 0.02267 0.00114 -0.00004 0.00002 C2 1 0.621311 0.874219 0.350338 11.00000 0.01269 0.01650 = 0.02209 0.00072 0.00132 0.00161 C12 1 0.714297 0.976756 0.403603 11.00000 0.01700 0.02064 = 0.01672 0.00089 0.00577 -0.00375 C4 1 0.556100 0.604997 0.344712 11.00000 0.01751 0.02113 = 0.01768 0.00164 0.00278 0.00279 C10 1 0.646790 0.782766 0.261140 11.00000 0.01377 0.02057 = 0.02051 0.00021 0.00126 0.00239 C3 1 0.581867 0.770076 0.377109 11.00000 0.01475 0.01924 = 0.01890 0.00047 0.00032 0.00167 C18 1 0.512909 0.440813 0.347694 11.00000 0.01582 0.02193 = 0.01790 0.00483 -0.00209 -0.00003 C11 1 0.661917 1.052792 0.372155 11.00000 0.02062 0.01952 = 0.01611 -0.00184 0.00745 -0.00136 C5 1 0.644513 0.606213 0.225051 11.00000 0.01906 0.02129 = 0.02702 -0.00138 0.00357 -0.00086 AFIX 43 H5 2 0.622060 0.476890 0.227383 11.00000 -1.20000 AFIX 0 C24 1 0.570983 0.831345 0.427874 11.00000 0.01671 0.02686 = 0.01894 0.00261 0.00164 0.00047 AFIX 43 H24 2 0.557559 0.714587 0.447307 11.00000 -1.20000 AFIX 0 C9 1 0.679006 0.973771 0.255932 11.00000 0.02207 0.02168 = 0.02218 -0.00241 0.00454 -0.00056 AFIX 43 H9 2 0.680028 1.097230 0.279445 11.00000 -1.20000 AFIX 0 C25 1 0.578302 1.038124 0.449409 11.00000 0.02170 0.03034 = 0.02307 -0.00284 0.00407 -0.00029 AFIX 43 H25 2 0.591758 1.158533 0.431010 11.00000 -1.20000 AFIX 0 C23 1 0.509364 0.241670 0.317902 11.00000 0.01967 0.02459 = 0.02289 0.00327 -0.00059 0.00210 AFIX 43 H23 2 0.534634 0.216486 0.295363 11.00000 -1.20000 AFIX 0 C8 1 0.709470 0.984748 0.216791 11.00000 0.02215 0.02397 = 0.02658 0.00296 0.00521 -0.00150 AFIX 43 H8 2 0.731526 1.114706 0.213829 11.00000 -1.20000 AFIX 0 C17 1 0.745299 1.135797 0.435565 11.00000 0.02661 0.02278 = 0.02392 -0.00364 0.00513 -0.00110 AFIX 43 H17 2 0.731478 1.285602 0.438273 11.00000 -1.20000 AFIX 0 C13 1 0.734943 0.757384 0.400196 11.00000 0.02375 0.02189 = 0.02933 -0.00089 -0.00011 -0.00225 AFIX 43 H13 2 0.714031 0.645803 0.379226 11.00000 -1.20000 AFIX 0 C19 1 0.474950 0.475252 0.380442 11.00000 0.01968 0.02803 = 0.02165 0.00273 0.00122 0.00080 AFIX 43 H19 2 0.476202 0.610907 0.400357 11.00000 -1.20000 AFIX 0 C7 1 0.707856 0.807142 0.182049 11.00000 0.02166 0.03141 = 0.02058 0.00282 0.00693 0.00448 AFIX 43 H7 2 0.729251 0.813638 0.155597 11.00000 -1.20000 AFIX 0 C6 1 0.674955 0.619755 0.185928 11.00000 0.02685 0.02701 = 0.02230 -0.00533 0.00379 0.00531 AFIX 43 H6 2 0.673232 0.499373 0.161551 11.00000 -1.20000 AFIX 0 C22 1 0.469239 0.081202 0.321097 11.00000 0.02398 0.02402 = 0.03187 0.00310 -0.00617 -0.00471 AFIX 43 H22 2 0.466745 -0.052171 0.300318 11.00000 -1.20000 AFIX 0 C20 1 0.435637 0.311270 0.383716 11.00000 0.01988 0.03951 = 0.02747 0.01004 0.00476 -0.00309 AFIX 43 H20 2 0.410376 0.334522 0.406350 11.00000 -1.20000 AFIX 0 C16 1 0.795800 1.078380 0.463314 11.00000 0.02333 0.03561 = 0.02430 -0.00469 -0.00119 -0.00744 AFIX 43 H16 2 0.816400 1.187753 0.485215 11.00000 -1.20000 AFIX 0 C15 1 0.816275 0.861839 0.459163 11.00000 0.02194 0.03681 = 0.02615 0.00619 -0.00119 -0.00094 AFIX 43 H15 2 0.851131 0.822489 0.478094 11.00000 -1.20000 AFIX 0 C21 1 0.432652 0.114387 0.354526 11.00000 0.02205 0.03202 = 0.03816 0.01185 -0.00242 -0.01063 AFIX 43 H21 2 0.405732 0.002392 0.357309 11.00000 -1.20000 AFIX 0 C26 1 0.566098 1.082313 0.500342 11.00000 0.02034 0.05332 = 0.02541 -0.00962 0.00230 -0.00498 AFIX 43 H26 2 0.554151 0.957593 0.518526 11.00000 -1.20000 AFIX 0 C14 1 0.786385 0.702216 0.427663 11.00000 0.02516 0.02542 = 0.04256 0.00241 -0.00029 0.00398 AFIX 43 H14 2 0.800923 0.553896 0.424663 11.00000 -1.20000 AFIX 0 HKLF 4 REM m1_a.res in C2/c REM R1 = 0.0532 for 2760 Fo > 4sig(Fo) and 0.0983 for all 4081 data REM 263 parameters refined using 0 restraints END WGHT 0.0346 4.4546 REM Highest difference peak 0.254, deepest hole -0.227, 1-sigma level 0.052 Q1 1 0.6067 0.8835 0.3212 11.00000 0.05 0.25 Q2 1 0.6313 0.7543 0.2322 11.00000 0.05 0.24 Q3 1 0.6497 1.1666 0.3915 11.00000 0.05 0.23 Q4 1 0.7904 0.7628 0.4641 11.00000 0.05 0.22 Q5 1 0.5917 0.8751 0.3629 11.00000 0.05 0.22 ; _shelx_res_checksum 63125 _shelx_hkl_file ; 4 0 0 12.00 2.10 -4 0 0 9.30 1.80 -4 0 0 12.10 1.80 4 0 0 12.40 1.90 6 0 0 442.26 16.20 -6 0 0 409.36 16.00 6 0 0 442.46 16.10 -6 0 0 392.06 15.80 8 0 0 3321.37 102.59 -8 0 0 3287.77 102.69 -8 0 0 3208.68 102.29 8 0 0 3182.68 102.29 10 0 0 117.59 8.40 10 0 0 99.39 8.00 -10 0 0 113.49 8.20 -10 0 0 104.39 7.80 12 0 0 355.16 17.20 12 0 0 363.96 17.10 -12 0 0 345.27 16.90 -12 0 0 342.67 17.30 -14 0 0 2435.96 76.29 14 0 0 2059.79 74.39 -14 0 0 1941.01 73.89 14 0 0 2412.76 75.89 -16 0 0 79.59 10.40 16 0 0 68.59 9.00 -16 0 0 86.99 10.60 16 0 0 86.59 9.90 -18 0 0 28.90 7.80 18 0 0 25.40 7.80 18 0 0 26.60 7.40 -18 0 0 37.60 8.90 -20 0 0 335.67 21.70 -20 0 0 342.67 22.20 20 0 0 346.87 20.70 20 0 0 347.37 21.10 -22 0 0 784.32 37.60 -22 0 0 730.23 35.70 22 0 0 755.32 35.50 22 0 0 754.62 36.50 -24 0 0 31.20 11.30 24 0 0 8.00 9.10 24 0 0 6.20 11.10 -24 0 0 -1.30 11.00 26 0 0 4.70 9.70 -26 0 0 8.50 12.20 26 0 0 8.70 13.10 -28 0 0 193.08 28.50 28 0 0 233.48 43.90 28 0 0 217.38 24.80 -30 0 0 101.99 23.00 30 0 0 73.19 20.10 1 -1 0 57.09 2.70 -1 1 0 49.10 2.60 -1 1 0 57.69 2.60 -3 -1 0 650.13 20.50 -5 -1 0 14.20 1.60 -7 -1 0 1026.90 33.40 7 -1 0 984.10 34.20 -7 -1 0 985.50 33.50 7 -1 0 895.71 33.90 7 1 0 923.11 32.90 7 1 0 1005.40 33.40 -7 1 0 987.40 34.40 -7 1 0 1074.09 34.50 9 -1 0 53.19 6.20 -9 -1 0 61.19 5.60 -9 -1 0 54.79 5.60 9 -1 0 63.59 6.20 -9 1 0 49.90 5.70 9 1 0 48.60 5.10 -9 1 0 45.50 6.00 9 1 0 43.00 5.20 11 -1 0 96.79 8.30 -11 -1 0 98.29 8.20 -11 -1 0 106.59 8.20 11 -1 0 108.59 9.00 -11 1 0 111.29 9.10 11 1 0 110.39 8.20 -11 1 0 122.19 8.80 11 1 0 111.79 8.00 -13 -1 0 16.50 5.00 -13 -1 0 18.60 5.10 13 -1 0 11.30 4.60 13 -1 0 16.30 5.10 -13 1 0 14.40 5.40 13 1 0 20.80 4.90 13 1 0 8.30 4.30 -13 1 0 15.70 4.80 15 -1 0 3.90 5.10 15 -1 0 12.00 5.50 -15 -1 0 6.90 4.60 -15 -1 0 4.30 4.70 -15 1 0 14.50 5.40 15 1 0 2.90 4.10 15 1 0 7.70 4.20 -15 1 0 3.80 5.10 17 -1 0 2.80 6.10 17 -1 0 -3.00 5.50 -17 -1 0 7.00 5.70 -17 -1 0 1.20 5.50 -17 1 0 2.00 6.20 -17 1 0 -1.70 6.30 17 1 0 0.70 5.50 17 1 0 3.90 4.60 19 -1 0 26.10 7.50 -19 -1 0 17.50 7.60 19 -1 0 20.10 7.50 -19 -1 0 26.30 8.80 19 1 0 24.30 7.30 -19 1 0 19.30 8.70 19 1 0 22.00 7.50 -19 1 0 21.80 8.00 21 -1 0 147.19 15.00 -21 -1 0 184.98 17.40 -21 -1 0 157.68 16.00 21 -1 0 155.48 16.00 21 1 0 176.98 16.90 21 1 0 157.88 14.80 -21 1 0 144.89 16.90 -21 1 0 166.78 17.60 23 -1 0 9.60 9.60 23 -1 0 17.60 11.20 -23 -1 0 13.60 9.70 -23 -1 0 9.90 9.10 -23 1 0 15.40 10.90 23 1 0 3.50 9.70 23 1 0 28.00 9.50 -23 1 0 17.50 10.10 25 -1 0 12.40 12.40 -25 -1 0 53.09 14.80 25 -1 0 33.50 12.30 25 1 0 34.60 11.60 25 1 0 20.50 12.30 -25 1 0 58.09 15.40 27 -1 0 10.40 13.30 -27 -1 0 17.90 14.20 27 1 0 4.50 10.70 27 1 0 6.00 14.70 -27 1 0 1.90 15.30 29 -1 0 25.70 16.80 -29 1 0 39.80 17.60 29 1 0 19.20 17.80 29 1 0 5.50 13.00 -31 -1 0 1.80 18.00 -31 1 0 5.10 19.40 0 -2 0 286.27 9.20 0 -2 0 270.17 9.20 0 2 0 283.47 8.60 0 2 0 229.58 8.80 -2 -2 0 11.90 1.00 2 -2 0 7.30 1.80 -2 2 0 13.10 2.30 -2 2 0 14.30 1.90 4 -2 0 340.87 13.60 -4 -2 0 346.97 12.00 -4 -2 0 337.47 11.80 4 -2 0 327.77 13.50 4 2 0 341.87 11.40 -4 2 0 341.77 13.20 4 2 0 368.06 11.20 -4 2 0 346.07 13.80 -6 -2 0 431.36 15.50 6 -2 0 440.16 17.30 6 -2 0 406.56 17.00 -6 2 0 435.16 16.90 6 2 0 427.16 15.20 6 2 0 417.16 14.80 -6 2 0 436.96 17.40 -8 -2 0 280.37 10.60 -10 -2 0 250.27 9.90 -12 -2 0 90.19 5.20 -14 -2 0 249.78 10.50 -16 -2 0 54.29 4.90 18 -2 0 8.10 7.10 18 -2 0 14.90 6.70 -18 -2 0 1.30 5.90 -18 -2 0 2.10 5.90 -18 2 0 21.30 7.90 -18 2 0 12.80 8.20 18 2 0 3.90 5.60 18 2 0 7.20 5.60 -20 -2 0 63.49 11.00 -20 -2 0 56.69 11.20 20 -2 0 66.39 12.10 20 -2 0 44.60 11.70 20 2 0 49.30 9.20 -20 2 0 73.39 12.70 -20 2 0 45.90 10.20 20 2 0 37.80 9.00 -22 -2 0 16.00 9.60 22 -2 0 20.20 9.80 -22 -2 0 8.70 9.10 -22 2 0 11.10 10.20 22 2 0 -0.40 7.70 -24 -2 0 12.50 9.80 24 -2 0 22.50 11.40 -24 2 0 31.70 12.00 24 2 0 18.10 10.30 24 2 0 3.90 10.10 -24 2 0 -4.20 12.60 26 -2 0 118.39 21.70 -26 -2 0 116.89 21.40 -26 2 0 142.49 23.00 26 2 0 138.99 19.10 26 2 0 134.09 21.60 -28 -2 0 -4.70 13.90 28 -2 0 -13.60 13.40 28 2 0 -3.20 12.20 28 2 0 -28.10 17.50 -28 2 0 -16.00 14.10 -30 -2 0 23.60 5.20 1 -3 0 6.10 1.90 -1 -3 0 5.10 1.00 1 -3 0 4.90 1.50 -1 -3 0 6.50 1.30 -1 3 0 3.40 1.00 -1 3 0 4.70 1.50 3 -3 0 252.67 10.90 -3 3 0 255.37 10.70 -3 3 0 254.37 10.00 -5 -3 0 52.99 3.70 -5 -3 0 59.09 3.20 5 -3 0 59.79 5.80 -5 3 0 61.99 6.00 -5 3 0 53.49 5.00 -7 -3 0 133.79 7.00 -7 -3 0 129.49 6.50 7 -3 0 125.89 9.10 -7 3 0 136.59 9.30 7 3 0 133.29 5.40 -7 3 0 135.39 8.80 -9 -3 0 450.05 17.60 9 -3 0 474.05 20.50 -9 3 0 435.46 20.10 9 3 0 433.66 16.60 9 3 0 460.45 16.20 -9 3 0 462.85 19.60 -11 -3 0 77.59 7.70 11 -3 0 75.59 9.20 11 -3 0 89.79 9.60 -11 -3 0 78.39 7.20 11 3 0 84.09 6.70 -11 3 0 78.99 8.60 11 3 0 80.19 6.00 -11 3 0 95.29 9.80 -13 -3 0 -1.60 2.60 -15 -3 0 -1.80 2.50 -17 -3 0 11.60 3.50 -19 -3 0 4.80 3.20 -21 -3 0 6.50 3.30 -23 -3 0 38.50 6.00 -25 -3 0 40.60 6.70 -27 -3 0 3.50 4.80 0 -4 0 86.49 4.80 0 -4 0 96.39 4.40 2 -4 0 27.40 4.10 2 -4 0 29.40 3.80 -2 4 0 26.40 2.80 4 -4 0 15.30 3.80 -4 4 0 16.30 3.40 -4 4 0 15.70 2.90 6 -4 0 89.99 7.90 6 -4 0 86.19 7.90 -6 4 0 95.49 6.80 -6 4 0 86.39 7.60 8 -4 0 90.69 9.30 -8 -4 0 112.19 6.60 8 -4 0 94.99 9.00 -8 -4 0 93.19 5.10 -8 4 0 101.49 8.30 -8 4 0 100.09 9.40 -10 -4 0 88.69 6.20 10 -4 0 79.29 9.60 10 -4 0 54.59 9.80 -10 -4 0 76.79 7.50 -10 4 0 67.59 9.90 -10 4 0 61.19 8.40 12 -4 0 -3.00 6.30 -12 -4 0 8.20 4.70 12 -4 0 4.30 6.10 -12 4 0 3.40 5.10 12 4 0 2.60 2.80 -12 4 0 0.90 5.80 12 4 0 1.80 2.40 14 -4 0 68.09 11.90 -14 -4 0 68.49 8.00 14 -4 0 54.19 10.10 -14 -4 0 72.49 10.20 14 4 0 55.09 6.60 -14 4 0 55.59 9.80 -14 4 0 69.69 12.10 14 4 0 67.49 6.40 -16 -4 0 258.07 15.40 16 -4 0 247.58 19.80 16 -4 0 233.28 19.10 -16 -4 0 247.88 16.90 -16 4 0 268.97 19.30 -16 4 0 267.67 19.00 16 4 0 273.67 13.40 16 4 0 257.27 14.00 18 -4 0 14.40 8.70 -18 -4 0 -5.70 6.00 18 -4 0 -6.20 16.10 -18 4 0 1.40 9.20 18 4 0 -1.80 5.70 -18 4 0 13.60 9.90 18 4 0 -4.70 4.70 -20 -4 0 14.40 9.70 -20 -4 0 0.90 8.10 20 -4 0 7.50 11.50 20 4 0 7.30 7.20 20 4 0 10.10 7.10 -20 4 0 24.60 12.10 -20 4 0 7.60 9.80 -22 -4 0 -2.50 9.40 22 -4 0 31.70 14.30 -22 4 0 -22.70 12.10 22 4 0 2.70 7.60 -22 4 0 34.10 14.80 -24 -4 0 4.90 5.60 -26 -4 0 -8.40 5.20 1 -5 0 86.29 4.70 1 -5 0 75.29 5.00 3 -5 0 324.37 12.80 3 -5 0 296.07 13.40 5 -5 0 73.79 7.70 -5 5 0 73.39 5.60 -5 5 0 81.99 6.90 7 -5 0 98.89 10.60 7 -5 0 105.09 9.90 -7 5 0 109.49 9.20 -7 5 0 108.79 8.00 9 -5 0 16.40 6.80 9 -5 0 26.30 7.00 -9 5 0 24.20 5.40 -9 5 0 37.50 7.00 -11 -5 0 4.30 2.70 11 -5 0 14.60 7.70 11 -5 0 7.70 7.30 -11 -5 0 9.50 3.80 -11 5 0 10.60 5.30 -11 5 0 12.10 6.30 13 -5 0 56.89 10.40 -13 -5 0 36.80 5.90 13 -5 0 41.50 10.50 -13 5 0 55.19 9.20 -13 5 0 37.20 8.90 15 -5 0 44.40 11.20 -15 -5 0 54.99 7.80 -15 -5 0 45.60 8.00 -15 5 0 40.40 9.60 -15 5 0 43.40 9.70 -17 -5 0 77.59 13.50 17 -5 0 81.89 14.80 -17 5 0 72.59 13.00 17 5 0 71.49 6.20 17 5 0 66.49 6.40 -17 5 0 69.29 13.20 19 -5 0 17.90 13.10 -19 -5 0 47.30 11.10 19 5 0 17.40 5.00 -19 5 0 37.20 11.70 -19 5 0 17.30 17.20 21 -5 0 -9.10 14.60 -21 5 0 16.70 14.00 21 5 0 -6.60 5.90 23 -5 0 64.89 18.90 23 5 0 78.49 12.80 4 -6 0 28.40 4.70 6 -6 0 2.50 4.90 6 -6 0 4.60 5.40 8 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12.30 -3 1 -29 10.40 13.70 -5 -1 -29 -11.20 13.70 5 -1 29 -13.80 14.10 5 1 29 8.50 14.10 -5 1 -29 45.70 16.80 5 1 29 2.70 14.00 -7 -1 -29 -8.30 16.60 7 -1 29 9.90 17.00 7 1 29 25.20 15.30 -7 1 -29 -16.30 14.90 7 1 29 13.20 14.70 -9 -1 -29 12.10 5.50 18 -2 -29 40.50 14.10 -18 -2 29 49.30 16.80 16 -2 -29 20.30 12.80 -16 -2 29 30.50 15.80 16 2 -29 14.00 11.50 -16 2 29 18.00 13.80 14 -2 -29 -7.00 10.50 -14 -2 29 -10.30 12.80 -14 2 29 -32.30 17.50 -14 2 29 18.30 12.00 14 2 -29 -0.70 9.60 12 -2 -29 5.70 9.10 -12 -2 29 6.00 13.30 12 2 -29 2.50 10.60 -12 2 29 -26.10 15.20 -12 2 29 27.20 11.30 10 -2 -29 -16.30 9.60 -10 2 29 -13.10 10.10 10 2 -29 15.60 10.00 -10 2 29 22.60 14.80 -8 -2 29 13.20 12.10 8 -2 -29 5.80 9.60 -8 2 29 10.60 11.20 -8 2 29 39.60 13.80 8 2 -29 -5.50 10.40 6 -2 -29 -8.10 10.30 -6 -2 29 25.10 13.70 -6 2 29 10.30 13.40 -6 2 29 -13.70 10.70 6 2 -29 4.00 10.90 4 -2 -29 -5.70 10.60 -4 -2 29 -5.90 12.70 4 2 -29 12.90 12.00 -4 2 29 2.50 11.10 2 -2 -29 -15.00 11.00 -2 -2 29 3.40 13.10 -2 2 29 9.30 11.50 2 2 -29 -9.60 11.00 -2 2 29 9.10 12.40 0 -2 -29 47.40 14.00 0 -2 29 49.80 15.70 0 2 29 47.60 13.70 0 2 29 12.50 13.30 0 2 -29 25.70 14.70 -2 -2 -29 -8.20 13.10 2 2 29 0.20 12.50 -2 2 -29 6.80 13.70 2 2 29 -15.30 12.50 4 -2 29 30.00 16.50 -4 -2 -29 -10.90 13.60 -4 2 -29 24.00 15.40 4 2 29 -2.70 14.10 6 -2 29 28.70 19.50 -6 -2 -29 62.49 17.70 6 2 29 52.89 16.90 -6 2 -29 68.99 18.30 -8 -2 -29 12.20 17.50 8 -2 29 -18.00 17.90 -8 2 -29 -18.90 15.90 -13 -3 29 28.40 16.30 13 -3 -29 36.50 12.70 -13 3 29 44.00 20.30 -11 -3 29 -5.60 13.90 11 -3 -29 -1.90 11.40 11 3 -29 -3.60 12.50 -11 3 29 5.90 11.80 9 -3 -29 -12.10 10.60 -9 -3 29 16.70 14.50 9 3 -29 2.50 11.60 -9 3 29 1.90 11.40 -7 -3 29 30.10 14.40 7 -3 -29 22.40 12.70 -7 3 29 17.20 11.80 7 3 -29 31.30 13.30 5 -3 -29 40.10 13.10 -5 -3 29 40.30 15.40 -5 3 29 34.30 13.00 5 3 -29 51.49 15.40 -3 -3 29 10.30 14.70 -3 3 29 17.30 12.90 3 3 -29 -5.50 13.60 -1 -3 29 9.60 14.90 1 -3 -29 12.40 12.30 1 3 -29 21.00 13.90 -1 3 29 5.00 12.50 -1 -3 -29 -2.40 13.70 1 -3 29 2.00 15.60 1 3 29 2.80 13.30 -1 3 -29 0.60 16.10 3 -3 29 68.79 19.30 3 3 29 26.00 14.50 5 -3 29 26.90 19.30 5 3 29 31.70 17.00 -18 0 30 18.80 15.40 18 0 -30 -3.10 12.20 -16 0 30 8.30 13.90 16 0 -30 18.60 11.30 14 0 -30 -10.50 9.70 12 0 -30 25.00 10.80 -12 0 30 14.20 12.10 -10 0 30 39.70 12.80 10 0 -30 40.50 11.70 -8 0 30 34.50 13.10 8 0 -30 14.50 10.60 -6 0 30 2.00 12.00 6 0 -30 14.30 10.70 4 0 -30 8.90 10.20 -4 0 30 -4.10 12.60 2 0 -30 90.79 16.50 -2 0 30 78.09 16.40 0 0 30 -1.90 12.60 0 0 -30 4.30 13.10 2 0 30 142.39 23.00 -2 0 -30 155.38 25.20 -4 0 -30 39.80 16.40 4 0 30 12.70 16.00 6 0 30 100.89 19.30 -8 0 -30 119.69 22.40 -17 -1 30 18.00 14.60 17 -1 -30 -0.90 13.20 -17 1 30 -5.20 15.80 17 1 -30 25.70 12.30 -15 -1 30 17.80 13.40 15 -1 -30 -3.10 11.30 -15 1 30 -17.20 12.40 15 1 -30 -8.70 11.40 13 -1 -30 -4.50 10.20 -13 -1 30 -9.20 12.00 13 1 -30 7.00 10.90 -13 1 30 -1.10 12.60 -11 -1 30 17.80 12.90 -11 1 30 -9.50 10.90 11 1 -30 -16.70 9.90 9 -1 -30 20.60 10.70 -9 -1 30 -7.10 10.70 -9 1 30 50.69 16.20 9 1 -30 12.10 11.00 7 -1 -30 -13.00 10.30 -7 -1 30 21.80 13.30 7 1 -30 6.40 9.40 -7 1 30 5.80 11.20 -7 1 30 23.00 14.20 -5 -1 30 8.80 12.50 5 -1 -30 -5.20 10.10 5 1 -30 14.30 11.60 -5 1 30 12.60 13.70 -5 1 30 -5.00 11.40 -3 -1 30 33.10 13.40 3 -1 -30 17.10 12.20 -3 1 30 11.10 12.60 -3 1 30 5.80 12.80 3 1 -30 28.10 12.30 1 -1 -30 26.70 11.90 -1 -1 30 11.70 13.30 -1 1 30 11.70 12.90 -1 1 30 8.30 13.20 1 1 -30 0.10 13.00 1 -1 30 -5.10 13.80 -1 -1 -30 14.30 13.50 1 1 30 -8.60 13.90 1 1 30 12.60 12.50 -1 1 -30 9.80 13.20 -3 -1 -30 34.30 15.90 3 -1 30 -0.40 15.50 -3 1 -30 39.30 16.80 3 1 30 29.50 14.40 -5 -1 -30 -2.50 16.80 5 -1 30 -2.70 14.40 5 1 30 1.50 14.10 -5 1 -30 57.29 17.30 5 1 30 16.30 15.20 7 -1 30 79.49 21.40 -7 -1 -30 48.80 19.00 -7 1 -30 39.20 17.50 16 -2 -30 35.90 13.80 -16 -2 30 30.00 15.60 14 -2 -30 25.60 12.80 -14 -2 30 27.10 16.30 14 2 -30 20.90 12.50 -14 2 30 25.00 15.60 12 -2 -30 33.10 13.30 -12 -2 30 30.80 15.40 -12 2 30 20.10 18.10 -12 2 30 13.30 12.50 12 2 -30 13.00 12.50 10 -2 -30 0.90 11.00 -10 -2 30 -7.60 12.60 10 2 -30 8.10 12.00 -10 2 30 7.80 12.00 -10 2 30 30.60 16.40 8 -2 -30 8.40 10.90 -8 -2 30 3.50 12.60 8 2 -30 -14.50 11.40 -8 2 30 4.00 10.60 -8 2 30 -4.90 15.30 6 -2 -30 6.00 10.90 6 2 -30 -13.40 11.80 -6 2 30 -16.50 14.10 -6 2 30 3.30 12.00 -4 -2 30 5.90 14.00 4 -2 -30 -11.60 11.30 -4 2 30 -3.60 13.90 -4 2 30 -2.10 11.80 4 2 -30 -11.00 11.60 2 -2 -30 2.00 12.80 -2 -2 30 -12.50 14.40 2 2 -30 13.90 12.10 -2 2 30 19.10 14.00 -2 2 30 -5.90 12.30 0 -2 30 43.00 16.50 0 -2 -30 7.30 13.50 0 2 30 25.70 13.80 0 2 30 13.10 15.10 0 2 -30 25.60 12.80 -2 -2 -30 9.60 15.00 2 -2 30 0.50 15.00 2 2 30 23.90 15.90 4 -2 30 -8.50 16.70 -4 -2 -30 33.50 17.20 -4 2 -30 24.20 16.40 -6 -2 -30 24.20 18.40 6 -2 30 2.60 18.20 -6 2 -30 12.40 25.40 -11 -3 30 15.50 14.50 -9 -3 30 18.00 15.80 9 -3 -30 7.90 13.60 -9 3 30 32.90 14.90 7 -3 -30 44.70 14.20 -7 -3 30 3.60 15.30 -7 3 30 38.40 13.90 -5 -3 30 16.20 15.40 5 -3 -30 9.00 13.80 -5 3 30 12.70 13.20 3 -3 -30 20.00 13.00 -3 -3 30 21.30 16.70 -3 3 30 8.10 13.40 -1 -3 30 -23.80 15.60 -1 3 30 7.80 14.90 1 -3 30 2.20 16.70 1 3 30 -26.10 14.40 16 0 -31 -7.50 12.10 -16 0 31 9.10 12.90 -14 0 31 14.30 14.20 14 0 -31 -12.70 11.40 12 0 -31 6.90 10.20 -12 0 31 -12.70 13.50 10 0 -31 3.80 12.40 -8 0 31 -6.30 11.40 8 0 -31 -6.50 12.40 6 0 -31 -3.50 11.60 4 0 -31 -5.20 11.10 -4 0 31 -2.00 12.60 -2 0 31 11.90 15.20 2 0 -31 33.40 13.10 0 0 -31 4.40 14.40 0 0 31 21.70 14.20 -2 0 -31 10.40 15.10 2 0 31 -13.20 14.20 4 0 31 15.70 17.80 -4 0 -31 4.70 18.20 -6 0 -31 -9.90 16.10 -17 -1 31 -17.90 15.90 15 -1 -31 6.20 12.20 -15 -1 31 8.50 15.10 15 1 -31 1.10 12.40 -13 -1 31 4.80 13.80 13 -1 -31 5.80 12.40 -13 1 31 4.90 13.60 13 1 -31 9.50 10.50 11 -1 -31 26.00 12.20 -11 -1 31 5.60 14.70 11 1 -31 36.00 13.40 -11 1 31 11.10 13.40 9 -1 -31 -4.50 11.40 -9 -1 31 29.70 14.30 9 1 -31 -7.60 10.30 -9 1 31 -12.30 11.20 7 -1 -31 -6.40 11.30 -7 -1 31 -9.70 12.80 7 1 -31 -14.90 10.90 -7 1 31 -2.00 11.60 -5 -1 31 13.40 13.90 5 -1 -31 3.30 12.00 5 1 -31 7.90 12.30 -5 1 31 10.30 13.00 -5 1 31 8.10 16.10 -3 -1 31 22.90 13.70 3 -1 -31 32.90 13.70 3 1 -31 38.10 14.50 -3 1 31 19.20 15.60 -3 1 31 29.40 13.30 -1 -1 31 -2.70 12.80 1 -1 -31 -3.30 12.90 -1 1 31 -18.30 12.60 1 1 -31 -2.90 13.50 1 -1 31 1.50 15.10 -1 -1 -31 -6.00 14.40 -1 1 -31 29.60 16.80 1 1 31 15.50 14.90 1 1 31 8.30 17.20 -3 -1 -31 65.29 18.80 -3 1 -31 67.29 18.10 3 1 31 54.09 17.60 5 -1 31 19.50 18.20 -5 -1 -31 22.60 17.10 -5 1 -31 30.50 19.40 14 -2 -31 2.60 12.80 -14 -2 31 14.60 15.70 12 -2 -31 15.20 13.80 -10 -2 31 28.40 15.90 10 -2 -31 15.10 12.90 10 2 -31 22.80 12.40 -10 2 31 47.00 29.20 8 -2 -31 20.10 13.60 -8 -2 31 48.20 17.20 -8 2 31 71.49 21.80 8 2 -31 23.80 13.60 -8 2 31 32.40 14.80 6 -2 -31 6.80 12.50 6 2 -31 -9.00 12.50 -6 2 31 0.60 13.60 -6 2 31 15.60 23.40 4 -2 -31 46.60 14.50 -4 -2 31 60.29 17.80 -4 2 31 40.40 14.80 4 2 -31 17.70 14.10 2 -2 -31 17.00 14.10 -2 -2 31 10.20 15.50 2 2 -31 13.60 15.20 -2 2 31 -0.70 13.80 0 -2 31 11.30 16.80 0 -2 -31 -15.60 12.40 0 2 31 15.60 14.90 0 2 -31 35.90 15.70 -2 -2 -31 -0.10 16.40 2 -2 31 8.40 18.10 -2 2 -31 -1.30 16.80 4 -2 31 -28.60 18.50 -4 -2 -31 5.00 17.40 -14 0 32 -16.30 16.90 12 0 -32 20.70 12.30 -12 0 32 21.00 14.90 10 0 -32 -5.70 12.60 8 0 -32 27.90 13.20 -8 0 32 17.20 14.30 -6 0 32 -4.90 14.20 6 0 -32 -1.50 12.30 -4 0 32 9.20 14.80 -2 0 32 25.10 15.30 2 0 -32 30.20 15.90 0 0 -32 145.79 27.60 0 0 32 156.08 25.70 2 0 32 -16.90 19.90 -2 0 -32 9.90 18.00 -4 0 -32 160.48 25.00 13 -1 -32 11.60 14.40 -13 -1 32 42.60 16.20 13 1 -32 15.80 11.60 11 -1 -32 11.80 11.60 11 1 -32 -10.10 12.20 -11 1 32 -8.10 16.30 -9 -1 32 10.00 13.90 9 1 -32 11.20 12.70 -9 1 32 8.00 12.30 7 -1 -32 36.50 13.80 -7 -1 32 42.40 16.70 7 1 -32 36.00 15.30 -7 1 32 56.49 16.30 5 -1 -32 0.60 12.90 5 1 -32 0.40 12.90 -5 1 32 0.60 14.30 3 -1 -32 -7.40 13.10 -3 -1 32 5.90 14.10 3 1 -32 -4.30 14.10 -3 1 32 -1.40 14.70 -1 -1 32 24.50 15.50 1 -1 -32 -4.50 15.10 1 1 -32 15.80 16.20 -1 1 32 -8.90 15.70 1 -1 32 -1.60 15.10 -1 -1 -32 -12.50 15.40 -1 1 -32 24.60 15.50 -3 -1 -32 78.79 20.70 3 -1 32 68.99 32.70 -3 1 -32 33.00 17.60 10 -2 -32 4.30 14.10 -10 -2 32 45.60 17.20 -8 -2 32 28.70 16.70 8 -2 -32 6.00 14.10 -6 -2 32 -0.10 15.60 6 -2 -32 20.30 14.30 4 -2 -32 -10.00 14.00 -4 -2 32 20.00 17.10 4 2 -32 -16.20 17.90 -2 -2 32 12.20 16.60 2 -2 -32 0.70 15.50 0 -2 32 59.39 17.80 0 -2 -32 63.89 18.30 12 0 -33 -17.50 13.30 10 0 -33 -18.30 12.70 8 0 -33 -6.50 11.50 -8 0 33 -5.10 16.30 -6 0 33 24.60 16.60 6 0 -33 -2.80 14.40 4 0 -33 -0.50 15.30 -4 0 33 27.50 18.50 2 0 -33 7.30 16.60 0 0 -33 16.10 17.30 -9 -1 33 3.20 15.20 9 -1 -33 -2.40 13.40 9 1 -33 10.80 14.90 7 -1 -33 25.40 15.00 -7 -1 33 11.70 14.90 7 1 -33 11.90 14.00 -5 -1 33 30.30 18.70 5 -1 -33 26.90 17.00 5 1 -33 25.30 16.80 -3 -1 33 32.00 17.70 3 1 -33 20.90 16.60 -1 -1 33 2.90 22.70 1 1 -33 -25.10 14.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 21972 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 0.57675(5) 0.6034(2) 0.29989(5) 0.0189(3) Uani 1 1 d . . O2 O 0.65191(6) 1.2550(2) 0.36481(5) 0.0278(4) Uani 1 1 d . . O3 O 0.57009(7) 1.2677(3) 0.52137(6) 0.0533(5) Uani 1 1 d . . C1 C 0.61710(7) 0.7670(3) 0.30410(7) 0.0179(4) Uani 1 1 d . . C2 C 0.62131(7) 0.8742(3) 0.35034(7) 0.0173(4) Uani 1 1 d . . C12 C 0.71430(8) 0.9768(3) 0.40360(7) 0.0178(4) Uani 1 1 d . . C4 C 0.55610(8) 0.6050(3) 0.34471(7) 0.0188(4) Uani 1 1 d . . C10 C 0.64679(7) 0.7828(3) 0.26114(7) 0.0185(4) Uani 1 1 d . . C3 C 0.58187(7) 0.7701(3) 0.37711(7) 0.0180(4) Uani 1 1 d . . C18 C 0.51291(8) 0.4408(3) 0.34769(7) 0.0192(4) Uani 1 1 d . . C11 C 0.66192(8) 1.0528(3) 0.37216(7) 0.0182(4) Uani 1 1 d . . C5 C 0.64451(8) 0.6062(3) 0.22505(7) 0.0225(5) Uani 1 1 d . . H5 H 0.622060 0.476890 0.227383 0.027 Uiso 1 1 calc R U C24 C 0.57098(8) 0.8313(3) 0.42787(7) 0.0210(4) Uani 1 1 d . . H24 H 0.557559 0.714587 0.447307 0.025 Uiso 1 1 calc R U C9 C 0.67901(8) 0.9738(3) 0.25593(7) 0.0219(4) Uani 1 1 d . . H9 H 0.680028 1.097230 0.279445 0.026 Uiso 1 1 calc R U C25 C 0.57830(8) 1.0381(4) 0.44941(8) 0.0250(5) Uani 1 1 d . . H25 H 0.591758 1.158533 0.431010 0.030 Uiso 1 1 calc R U C23 C 0.50936(8) 0.2417(3) 0.31790(7) 0.0229(5) Uani 1 1 d . . H23 H 0.534634 0.216486 0.295363 0.027 Uiso 1 1 calc R U C8 C 0.70947(8) 0.9847(3) 0.21679(8) 0.0241(5) Uani 1 1 d . . H8 H 0.731526 1.114706 0.213829 0.029 Uiso 1 1 calc R U C17 C 0.74530(8) 1.1358(3) 0.43556(7) 0.0244(5) Uani 1 1 d . . H17 H 0.731478 1.285602 0.438273 0.029 Uiso 1 1 calc R U C13 C 0.73494(8) 0.7574(3) 0.40020(8) 0.0256(5) Uani 1 1 d . . H13 H 0.714031 0.645803 0.379226 0.031 Uiso 1 1 calc R U C19 C 0.47495(8) 0.4753(3) 0.38044(7) 0.0234(5) Uani 1 1 d . . H19 H 0.476202 0.610907 0.400357 0.028 Uiso 1 1 calc R U C7 C 0.70786(8) 0.8071(3) 0.18205(7) 0.0242(5) Uani 1 1 d . . H7 H 0.729251 0.813638 0.155597 0.029 Uiso 1 1 calc R U C6 C 0.67496(8) 0.6198(3) 0.18593(8) 0.0255(5) Uani 1 1 d . . H6 H 0.673232 0.499373 0.161551 0.031 Uiso 1 1 calc R U C22 C 0.46924(8) 0.0812(3) 0.32110(8) 0.0280(5) Uani 1 1 d . . H22 H 0.466745 -0.052171 0.300318 0.034 Uiso 1 1 calc R U C20 C 0.43564(8) 0.3113(4) 0.38372(8) 0.0289(5) Uani 1 1 d . . H20 H 0.410376 0.334522 0.406350 0.035 Uiso 1 1 calc R U C16 C 0.79580(8) 1.0784(4) 0.46331(8) 0.0284(5) Uani 1 1 d . . H16 H 0.816400 1.187753 0.485215 0.034 Uiso 1 1 calc R U C15 C 0.81627(9) 0.8618(4) 0.45916(8) 0.0290(5) Uani 1 1 d . . H15 H 0.851131 0.822489 0.478094 0.035 Uiso 1 1 calc R U C21 C 0.43265(9) 0.1144(4) 0.35453(8) 0.0317(5) Uani 1 1 d . . H21 H 0.405732 0.002392 0.357309 0.038 Uiso 1 1 calc R U C26 C 0.56610(8) 1.0823(4) 0.50034(8) 0.0332(5) Uani 1 1 d . . H26 H 0.554151 0.957593 0.518526 0.040 Uiso 1 1 calc R U C14 C 0.78639(9) 0.7022(4) 0.42766(8) 0.0318(5) Uani 1 1 d . . H14 H 0.800923 0.553896 0.424663 0.038 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 0.0170(7) 0.0202(7) 0.0198(7) -0.0014(5) 0.0038(5) -0.0034(6) O2 0.0267(8) 0.0178(8) 0.0372(9) -0.0001(6) 0.0011(6) 0.0021(6) O3 0.0484(11) 0.0688(13) 0.0466(11) -0.0356(10) 0.0191(9) -0.0145(10) C1 0.0147(10) 0.0150(10) 0.0227(10) 0.0011(8) 0.0000(8) 0.0000(8) C2 0.0127(10) 0.0165(10) 0.0221(10) 0.0007(8) 0.0013(8) 0.0016(8) C12 0.0170(10) 0.0206(10) 0.0167(10) 0.0009(8) 0.0058(8) -0.0037(8) C4 0.0175(10) 0.0211(10) 0.0177(10) 0.0016(8) 0.0028(8) 0.0028(8) C10 0.0138(10) 0.0206(10) 0.0205(10) 0.0002(8) 0.0013(8) 0.0024(8) C3 0.0147(10) 0.0192(10) 0.0189(10) 0.0005(8) 0.0003(8) 0.0017(8) C18 0.0158(10) 0.0219(10) 0.0179(10) 0.0048(8) -0.0021(8) 0.0000(8) C11 0.0206(10) 0.0195(11) 0.0161(10) -0.0018(8) 0.0074(8) -0.0014(8) C5 0.0191(11) 0.0213(11) 0.0270(11) -0.0014(8) 0.0036(9) -0.0009(8) C24 0.0167(10) 0.0269(11) 0.0189(10) 0.0026(8) 0.0016(8) 0.0005(8) C9 0.0221(11) 0.0217(11) 0.0222(11) -0.0024(8) 0.0045(8) -0.0006(9) C25 0.0217(11) 0.0303(12) 0.0231(11) -0.0028(9) 0.0041(9) -0.0003(9) C23 0.0197(11) 0.0246(11) 0.0229(11) 0.0033(9) -0.0006(8) 0.0021(9) C8 0.0222(11) 0.0240(11) 0.0266(11) 0.0030(9) 0.0052(9) -0.0015(9) C17 0.0266(12) 0.0228(11) 0.0239(11) -0.0036(9) 0.0051(9) -0.0011(9) C13 0.0237(11) 0.0219(11) 0.0293(12) -0.0009(9) -0.0001(9) -0.0022(9) C19 0.0197(11) 0.0280(11) 0.0217(11) 0.0027(8) 0.0012(8) 0.0008(9) C7 0.0217(11) 0.0314(12) 0.0206(11) 0.0028(9) 0.0069(8) 0.0045(9) C6 0.0268(12) 0.0270(11) 0.0223(11) -0.0053(9) 0.0038(9) 0.0053(9) C22 0.0240(12) 0.0240(11) 0.0319(12) 0.0031(9) -0.0062(9) -0.0047(9) C20 0.0199(11) 0.0395(13) 0.0275(12) 0.0100(10) 0.0048(9) -0.0031(9) C16 0.0233(12) 0.0356(13) 0.0243(11) -0.0047(9) -0.0012(9) -0.0074(10) C15 0.0219(11) 0.0368(13) 0.0262(11) 0.0062(10) -0.0012(9) -0.0009(10) C21 0.0221(12) 0.0320(13) 0.0382(13) 0.0119(10) -0.0024(10) -0.0106(10) C26 0.0203(11) 0.0533(15) 0.0254(12) -0.0096(11) 0.0023(9) -0.0050(11) C14 0.0252(12) 0.0254(12) 0.0426(14) 0.0024(10) -0.0003(10) 0.0040(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 C4 O1 C1 107.75(14) C2 C1 O1 109.47(16) C2 C1 C10 134.19(17) O1 C1 C10 116.28(15) C1 C2 C3 106.98(16) C1 C2 C11 127.41(17) C3 C2 C11 125.42(16) C13 C12 C17 118.97(18) C13 C12 C11 122.58(17) C17 C12 C11 118.35(17) O1 C4 C3 109.66(16) O1 C4 C18 115.82(16) C3 C4 C18 134.51(17) C9 C10 C5 118.69(17) C9 C10 C1 120.30(17) C5 C10 C1 121.00(17) C4 C3 C2 106.12(16) C4 C3 C24 127.10(17) C2 C3 C24 126.77(17) C23 C18 C19 118.84(18) C23 C18 C4 119.64(17) C19 C18 C4 121.52(17) O2 C11 C12 121.00(17) O2 C11 C2 120.85(17) C12 C11 C2 118.15(16) C6 C5 C10 120.11(18) C6 C5 H5 119.9 C10 C5 H5 119.9 C25 C24 C3 125.46(18) C25 C24 H24 117.3 C3 C24 H24 117.3 C8 C9 C10 120.62(18) C8 C9 H9 119.7 C10 C9 H9 119.7 C24 C25 C26 121.3(2) C24 C25 H25 119.3 C26 C25 H25 119.3 C22 C23 C18 120.41(19) C22 C23 H23 119.8 C18 C23 H23 119.8 C7 C8 C9 120.18(19) C7 C8 H8 119.9 C9 C8 H8 119.9 C16 C17 C12 120.85(19) C16 C17 H17 119.6 C12 C17 H17 119.6 C12 C13 C14 119.75(19) C12 C13 H13 120.1 C14 C13 H13 120.1 C20 C19 C18 119.93(19) C20 C19 H19 120.0 C18 C19 H19 120.0 C8 C7 C6 119.78(18) C8 C7 H7 120.1 C6 C7 H7 120.1 C7 C6 C5 120.59(18) C7 C6 H6 119.7 C5 C6 H6 119.7 C23 C22 C21 120.3(2) C23 C22 H22 119.8 C21 C22 H22 119.8 C21 C20 C19 120.9(2) C21 C20 H20 119.5 C19 C20 H20 119.5 C15 C16 C17 119.8(2) C15 C16 H16 120.1 C17 C16 H16 120.1 C14 C15 C16 120.3(2) C14 C15 H15 119.9 C16 C15 H15 119.9 C20 C21 C22 119.58(19) C20 C21 H21 120.2 C22 C21 H21 120.2 O3 C26 C25 124.6(2) O3 C26 H26 117.7 C25 C26 H26 117.7 C15 C14 C13 120.3(2) C15 C14 H14 119.8 C13 C14 H14 119.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C4 1.369(2) O1 C1 1.379(2) O2 C11 1.219(2) O3 C26 1.215(3) C1 C2 1.359(3) C1 C10 1.460(3) C2 C3 1.442(3) C2 C11 1.497(3) C12 C13 1.393(3) C12 C17 1.394(3) C12 C11 1.485(3) C4 C3 1.372(3) C4 C18 1.455(3) C10 C9 1.398(3) C10 C5 1.400(3) C3 C24 1.456(3) C18 C23 1.401(3) C18 C19 1.402(3) C5 C6 1.386(3) C5 H5 0.9500 C24 C25 1.337(3) C24 H24 0.9500 C9 C8 1.386(3) C9 H9 0.9500 C25 C26 1.451(3) C25 H25 0.9500 C23 C22 1.385(3) C23 H23 0.9500 C8 C7 1.382(3) C8 H8 0.9500 C17 C16 1.380(3) C17 H17 0.9500 C13 C14 1.394(3) C13 H13 0.9500 C19 C20 1.385(3) C19 H19 0.9500 C7 C6 1.384(3) C7 H7 0.9500 C6 H6 0.9500 C22 C21 1.388(3) C22 H22 0.9500 C20 C21 1.381(3) C20 H20 0.9500 C16 C15 1.379(3) C16 H16 0.9500 C15 C14 1.378(3) C15 H15 0.9500 C21 H21 0.9500 C26 H26 0.9500 C14 H14 0.9500 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 C4 O1 C1 C2 -1.23(19) C4 O1 C1 C10 176.34(16) O1 C1 C2 C3 0.8(2) C10 C1 C2 C3 -176.1(2) O1 C1 C2 C11 176.05(17) C10 C1 C2 C11 -0.9(3) C1 O1 C4 C3 1.16(19) C1 O1 C4 C18 -179.54(15) C2 C1 C10 C9 -18.1(3) O1 C1 C10 C9 165.07(16) C2 C1 C10 C5 160.6(2) O1 C1 C10 C5 -16.2(3) O1 C4 C3 C2 -0.7(2) C18 C4 C3 C2 -179.8(2) O1 C4 C3 C24 178.26(17) C18 C4 C3 C24 -0.9(3) C1 C2 C3 C4 -0.1(2) C11 C2 C3 C4 -175.45(17) C1 C2 C3 C24 -179.02(18) C11 C2 C3 C24 5.6(3) O1 C4 C18 C23 25.0(2) C3 C4 C18 C23 -155.9(2) O1 C4 C18 C19 -155.97(17) C3 C4 C18 C19 23.1(3) C13 C12 C11 O2 -159.50(18) C17 C12 C11 O2 16.8(3) C13 C12 C11 C2 21.4(3) C17 C12 C11 C2 -162.28(17) C1 C2 C11 O2 91.2(2) C3 C2 C11 O2 -94.4(2) C1 C2 C11 C12 -89.7(2) C3 C2 C11 C12 84.7(2) C9 C10 C5 C6 1.7(3) C1 C10 C5 C6 -177.04(18) C4 C3 C24 C25 -150.8(2) C2 C3 C24 C25 27.9(3) C5 C10 C9 C8 -2.1(3) C1 C10 C9 C8 176.71(18) C3 C24 C25 C26 179.86(18) C19 C18 C23 C22 -0.4(3) C4 C18 C23 C22 178.60(17) C10 C9 C8 C7 0.7(3) C13 C12 C17 C16 0.3(3) C11 C12 C17 C16 -176.12(17) C17 C12 C13 C14 -1.4(3) C11 C12 C13 C14 174.84(18) C23 C18 C19 C20 1.4(3) C4 C18 C19 C20 -177.59(17) C9 C8 C7 C6 1.1(3) C8 C7 C6 C5 -1.4(3) C10 C5 C6 C7 0.0(3) C18 C23 C22 C21 -1.1(3) C18 C19 C20 C21 -0.9(3) C12 C17 C16 C15 0.6(3) C17 C16 C15 C14 -0.4(3) C19 C20 C21 C22 -0.6(3) C23 C22 C21 C20 1.6(3) C24 C25 C26 O3 -177.4(2) C16 C15 C14 C13 -0.8(3) C12 C13 C14 C15 1.7(3)