#------------------------------------------------------------------------------ #$Date: 2020-02-14 02:18:06 +0200 (Fri, 14 Feb 2020) $ #$Revision: 248138 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557313.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_1557313 loop_ _publ_author_name 'Ye, Yan-Song' 'Li, Wen-Yan' 'Du, Shu-Zong' 'Yang, Jian' 'Nian, Yin' 'Xu, Gang' _publ_section_title ; Congenetic hybrids derived from dearomatized isoprenylated acylphloroglucinol with opposite effects on Cav3.1 low voltage-gated Ca2+ channel. ; _journal_name_full 'Journal of medicinal chemistry' _journal_paper_doi 10.1021/acs.jmedchem.9b02056 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C30 H44 O5' _chemical_formula_sum 'C30 H44 O5' _chemical_formula_weight 484.65 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.5518(3) _cell_length_b 16.1297(5) _cell_length_c 17.0893(5) _cell_measurement_reflns_used 9809 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 72.3458 _cell_measurement_theta_min 2.7395 _cell_volume 2908.55(15) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.0216 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 30655 _diffrn_reflns_theta_full 72.34 _diffrn_reflns_theta_max 72.34 _diffrn_reflns_theta_min 3.77 _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'translucent light colourless' _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.190 _refine_diff_density_max 0.212 _refine_diff_density_min -0.193 _refine_ls_abs_structure_details ; Flack x determined using 2440 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 5730 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0302 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.4156P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.0787 _reflns_number_gt 5665 _reflns_number_total 5730 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jm9b02056_si_004.cif _cod_data_source_block rxn52 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 1557313 _shelx_res_file ; TITL rxn52_0m_a.res in P2(1)2(1)2(1) rxn52_0m.res created by SHELXL-2017/1 at 15:24:55 on 22-Aug-2019 CELL 1.54178 10.5518 16.1297 17.0893 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0005 0.0005 0.000 0.000 0.000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H O UNIT 120 176 20 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 SIZE 0.190 0.200 0.400 ACTA EQIV $1 -x+3/2, -y+1, z-1/2 HTAB O1 O4_$1 HTAB O5 O3 HTAB O6 O1 HTAB C8 O5 EQIV $2 x+1/2, -y+1/2, -z+1 HTAB C22 O3_$2 HTAB C26 O4 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.043000 0.415600 FVAR 0.79665 O1 3 0.661562 0.456675 0.309996 11.00000 0.03131 0.02552 = 0.02022 0.00049 0.00930 -0.00173 AFIX 148 H1A 2 0.716726 0.451819 0.275438 11.00000 -1.50000 AFIX 0 O3 3 0.471199 0.294524 0.681631 11.00000 0.05165 0.04051 = 0.02113 0.00891 -0.00431 -0.02231 O4 3 0.659603 0.521613 0.703198 11.00000 0.03063 0.02644 = 0.01872 -0.00498 -0.00630 0.00188 O5 3 0.467967 0.319609 0.543721 11.00000 0.04105 0.03021 = 0.01751 0.00333 -0.00237 -0.01818 AFIX 147 H44 2 0.458430 0.296575 0.587410 11.00000 -1.50000 AFIX 0 O6 3 0.686235 0.543105 0.430107 11.00000 0.04086 0.02245 = 0.01821 0.00432 0.00002 -0.00928 AFIX 148 H6A 2 0.675708 0.513439 0.383113 11.00000 -1.50000 AFIX 0 C1 1 0.252527 0.640075 0.504718 11.00000 0.04030 0.05167 = 0.08399 0.00998 -0.01917 0.01138 AFIX 137 H7 2 0.228253 0.605377 0.549343 11.00000 -1.50000 H6 2 0.224487 0.613680 0.456055 11.00000 -1.50000 H1 2 0.212512 0.694654 0.509661 11.00000 -1.50000 AFIX 0 C2 1 0.394623 0.650103 0.503326 11.00000 0.03996 0.02338 = 0.03887 -0.00197 -0.01196 0.00810 C3 1 0.465589 0.618749 0.560353 11.00000 0.03448 0.02172 = 0.02643 -0.00080 -0.00191 0.00617 AFIX 43 H8 2 0.421921 0.589356 0.600274 11.00000 -1.20000 AFIX 0 C4 1 0.606596 0.624491 0.568830 11.00000 0.03446 0.01640 = 0.02523 -0.00067 -0.00706 0.00234 AFIX 23 H9 2 0.626587 0.652057 0.619096 11.00000 -1.20000 H39 2 0.640513 0.659639 0.526205 11.00000 -1.20000 AFIX 0 C5 1 0.674708 0.538364 0.566460 11.00000 0.02478 0.01554 = 0.02040 -0.00070 -0.00348 -0.00097 C6 1 0.642946 0.498229 0.489356 11.00000 0.02310 0.01748 = 0.01749 0.00247 0.00023 0.00105 C7 1 0.575564 0.426940 0.481392 11.00000 0.01922 0.01913 = 0.01499 -0.00068 -0.00048 0.00194 C8 1 0.528555 0.389632 0.404392 11.00000 0.02155 0.01894 = 0.01473 -0.00127 0.00154 -0.00060 AFIX 13 H31 2 0.495991 0.333266 0.418157 11.00000 -1.20000 AFIX 0 C9 1 0.413593 0.437120 0.371836 11.00000 0.02211 0.02837 = 0.01669 -0.00331 0.00047 0.00277 AFIX 23 H19 2 0.440959 0.492652 0.353854 11.00000 -1.20000 H20 2 0.350158 0.444790 0.413901 11.00000 -1.20000 AFIX 0 C10 1 0.352509 0.389835 0.303045 11.00000 0.02718 0.03428 = 0.01946 -0.00546 -0.00320 0.00253 AFIX 13 H30 2 0.322113 0.335413 0.323863 11.00000 -1.20000 AFIX 0 C30 1 0.123830 0.401636 0.275298 11.00000 0.03105 0.08001 = 0.03203 -0.02209 -0.00671 0.01334 AFIX 93 H30A 2 0.052759 0.429988 0.254120 11.00000 -1.20000 H30B 2 0.112819 0.349378 0.300021 11.00000 -1.20000 AFIX 0 C11 1 0.238128 0.434926 0.270361 11.00000 0.03479 0.05441 = 0.02246 -0.01154 -0.00922 0.01317 C12 1 0.260114 0.517266 0.231873 11.00000 0.05723 0.06148 = 0.05840 0.00812 -0.02095 0.02194 AFIX 137 H28 2 0.179236 0.539514 0.213064 11.00000 -1.50000 H29 2 0.318177 0.510278 0.187603 11.00000 -1.50000 H2 2 0.297293 0.555797 0.269807 11.00000 -1.50000 AFIX 0 C13 1 0.444586 0.697097 0.433812 11.00000 0.06104 0.04050 = 0.04259 0.01374 -0.01800 0.00816 AFIX 137 H3 2 0.416061 0.754844 0.436563 11.00000 -1.50000 H4 2 0.412817 0.671652 0.385573 11.00000 -1.50000 H5 2 0.537425 0.695403 0.434021 11.00000 -1.50000 AFIX 0 C14 1 0.820182 0.553932 0.572597 11.00000 0.02637 0.02029 = 0.02436 -0.00092 -0.00244 -0.00435 AFIX 23 H18 2 0.848769 0.582207 0.524304 11.00000 -1.20000 H10 2 0.836068 0.591992 0.616975 11.00000 -1.20000 AFIX 0 C15 1 0.898484 0.477674 0.583862 11.00000 0.02692 0.02433 = 0.02793 0.00107 -0.00086 -0.00150 AFIX 43 H17 2 0.888131 0.449901 0.632465 11.00000 -1.20000 AFIX 0 C16 1 0.980986 0.443743 0.534307 11.00000 0.02773 0.02783 = 0.04104 -0.00859 0.00194 -0.00496 C17 1 1.007501 0.475734 0.453539 11.00000 0.04344 0.06960 = 0.04171 -0.01054 0.01549 -0.00764 AFIX 137 H12 2 0.956070 0.525263 0.443806 11.00000 -1.50000 H11 2 0.986238 0.432942 0.415005 11.00000 -1.50000 H13 2 1.097521 0.489901 0.449032 11.00000 -1.50000 AFIX 0 C18 1 1.055651 0.368063 0.556450 11.00000 0.04205 0.03308 = 0.08375 -0.00960 0.01056 0.00635 AFIX 137 H15 2 1.036264 0.352768 0.610642 11.00000 -1.50000 H14 2 1.146411 0.379873 0.551570 11.00000 -1.50000 H16 2 1.033015 0.322149 0.521590 11.00000 -1.50000 AFIX 0 C19 1 0.451054 0.371117 0.239305 11.00000 0.03365 0.03215 = 0.01565 -0.00453 -0.00161 0.00302 AFIX 23 H26 2 0.411849 0.336069 0.198369 11.00000 -1.20000 H27 2 0.478212 0.423694 0.214562 11.00000 -1.20000 AFIX 0 C20 1 0.566815 0.326660 0.272749 11.00000 0.03236 0.02658 = 0.01676 -0.00365 0.00272 0.00444 AFIX 23 H24 2 0.629927 0.318425 0.230594 11.00000 -1.20000 H25 2 0.541038 0.271328 0.292122 11.00000 -1.20000 AFIX 0 C21 1 0.628043 0.375346 0.339671 11.00000 0.02441 0.02183 = 0.01743 -0.00065 0.00329 0.00142 C22 1 0.745161 0.331372 0.370205 11.00000 0.02645 0.03314 = 0.02888 -0.00410 0.00091 0.00856 AFIX 137 H21 2 0.806729 0.325077 0.327683 11.00000 -1.50000 H23 2 0.721453 0.276550 0.390127 11.00000 -1.50000 H22 2 0.782939 0.364089 0.412524 11.00000 -1.50000 AFIX 0 C23 1 0.537347 0.385367 0.551931 11.00000 0.02116 0.02011 = 0.01744 0.00043 -0.00066 -0.00097 C24 1 0.571612 0.411596 0.629661 11.00000 0.02251 0.02330 = 0.01541 -0.00008 -0.00086 -0.00073 C25 1 0.538392 0.357807 0.693959 11.00000 0.03041 0.02785 = 0.01918 0.00251 0.00032 -0.00265 C26 1 0.587268 0.368759 0.776811 11.00000 0.05156 0.02615 = 0.01599 0.00107 -0.00261 -0.00095 AFIX 13 H32 2 0.583206 0.428792 0.791205 11.00000 -1.20000 AFIX 0 C27 1 0.725707 0.340312 0.778018 11.00000 0.05540 0.02977 = 0.03148 -0.00440 -0.02112 0.00367 AFIX 137 H33 2 0.730589 0.282118 0.761813 11.00000 -1.50000 H35 2 0.759717 0.346084 0.831102 11.00000 -1.50000 H34 2 0.775414 0.374527 0.741912 11.00000 -1.50000 AFIX 0 C28 1 0.507838 0.318901 0.834624 11.00000 0.08455 0.04728 = 0.01889 0.00696 0.00530 -0.00683 AFIX 137 H36 2 0.512228 0.259923 0.821116 11.00000 -1.50000 H37 2 0.419542 0.337570 0.832221 11.00000 -1.50000 H38 2 0.540698 0.327168 0.887690 11.00000 -1.50000 AFIX 0 C29 1 0.635214 0.489412 0.638953 11.00000 0.02092 0.02079 = 0.01701 -0.00103 -0.00312 0.00346 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM rxn52_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0302 for 5665 Fo > 4sig(Fo) and 0.0305 for all 5730 data REM 329 parameters refined using 0 restraints END WGHT 0.0430 0.4123 REM Instructions for potential hydrogen bonds HTAB O1 O4_$1 HTAB O5 O3 HTAB O6 O1 HTAB C8 O5 HTAB C22 O3_$2 HTAB C26 O4 REM Highest difference peak 0.212, deepest hole -0.193, 1-sigma level 0.037 Q1 1 0.6387 0.5805 0.5679 11.00000 0.05 0.21 Q2 1 0.7464 0.5457 0.5696 11.00000 0.05 0.19 Q3 1 0.5682 0.4757 0.4864 11.00000 0.05 0.17 Q4 1 0.6486 0.4480 0.4829 11.00000 0.05 0.15 Q5 1 0.9055 0.4431 0.5465 11.00000 0.05 0.14 ; _shelx_res_checksum 56821 _shelx_hkl_file ; -1 0 0 0.80 0.20 -3 0 0 0.10 0.30 -4 0 0 202.58 8.40 -5 0 0 3.80 1.10 -5 0 0 1.60 1.80 -6 0 0 22.80 3.10 -6 0 0 21.60 6.00 -7 0 0 -0.50 3.30 -7 0 0 -1.00 1.60 -8 0 0 10.90 1.30 -8 0 0 6.60 3.00 -9 0 0 1.60 0.70 9 0 0 -0.70 1.80 -9 0 0 1.50 4.20 10 0 0 904.71 45.40 -10 0 0 720.93 26.50 -11 0 0 -0.50 0.60 12 0 0 25.20 1.70 -12 0 0 25.20 2.00 -13 0 0 1.40 0.70 13 0 0 0.10 0.40 13 0 0 0.40 0.40 0 1 0 0.90 0.40 -2 -1 0 3725.93 116.19 2 -1 0 3545.65 112.49 -2 -1 0 3602.84 113.09 -3 1 0 1807.62 59.69 3 -1 0 1742.93 55.29 -3 -1 0 1671.43 56.19 -3 -1 0 1813.42 60.59 -4 -1 0 1736.63 61.39 -4 -1 0 1638.44 57.49 -4 1 0 1650.53 54.79 -4 1 0 1869.31 64.49 4 -1 0 1651.73 54.19 -5 -1 0 4023.40 135.79 -5 -1 0 4042.70 127.79 -5 1 0 3973.30 126.79 -5 1 0 4022.20 134.39 -6 1 0 120.39 6.80 -6 -1 0 119.59 7.50 -6 1 0 118.69 11.50 -6 -1 0 112.59 11.50 -7 -1 0 957.40 34.70 -7 -1 0 869.51 44.30 -7 1 0 911.81 34.50 -7 1 0 883.91 43.70 -8 -1 0 88.49 13.60 -8 1 0 72.09 3.60 -8 -1 0 64.09 7.10 -8 -1 0 71.89 3.80 -8 1 0 68.49 6.80 -8 1 0 64.39 12.70 9 -1 0 37.40 5.70 -9 1 0 22.30 5.30 -9 1 0 33.40 2.40 -9 -1 0 38.20 6.30 9 1 0 21.90 4.60 -9 -1 0 33.80 2.50 10 1 0 9.70 4.80 -11 -1 0 13.70 1.80 -11 1 0 12.40 1.60 12 -1 0 56.29 2.90 -12 -1 0 53.99 3.00 12 1 0 54.89 2.70 -12 1 0 56.59 3.00 -13 1 0 30.10 1.80 13 -1 0 27.80 1.50 13 -1 0 28.20 1.60 13 1 0 26.10 1.40 1 -2 0 8352.16 257.97 -2 -2 0 5220.18 164.18 2 -2 0 5235.18 163.18 -2 -2 0 5336.87 167.88 -3 2 0 1499.85 50.89 3 -2 0 1437.76 46.60 -3 -2 0 1443.66 52.49 -3 -2 0 1512.25 48.10 4 -2 0 4864.51 152.38 -4 -2 0 4944.31 154.38 -4 -2 0 4869.21 160.88 5 -2 0 94.09 4.70 -5 2 0 102.19 8.80 -5 -2 0 101.39 9.90 -5 2 0 95.49 5.20 -5 -2 0 99.89 6.30 -6 2 0 1245.08 42.60 -6 -2 0 1265.37 54.09 -6 2 0 1247.28 51.19 -6 -2 0 1274.57 44.60 -7 2 0 79.79 3.70 -7 -2 0 76.09 12.20 -7 -2 0 85.69 4.10 -7 2 0 77.39 6.10 -7 -2 0 94.49 7.50 -7 2 0 86.89 11.70 8 2 0 0.80 1.40 -8 2 0 -1.40 2.00 -8 -2 0 0.70 0.60 -8 -2 0 0.60 2.90 -8 -2 0 2.00 7.50 -8 2 0 2.00 0.70 -9 -2 0 364.56 13.40 9 -2 0 380.36 18.50 -9 -2 0 336.37 19.40 -9 2 0 348.87 18.60 -9 2 0 366.46 13.00 9 -2 0 356.46 12.50 9 2 0 359.06 18.80 -10 2 0 1.90 0.80 -10 -2 0 3.80 1.10 -11 2 0 79.49 4.00 11 2 0 79.29 3.80 -11 -2 0 78.79 4.20 -12 -2 0 176.38 7.00 -12 2 0 186.08 7.10 12 2 0 182.28 7.70 12 -2 0 189.58 7.00 0 3 0 0.30 0.20 0 3 0 1.10 0.90 -1 -3 0 2869.71 85.99 -1 3 0 2576.64 87.89 1 -3 0 2700.53 84.49 1 -3 0 2805.82 85.59 -1 -3 0 2647.34 89.09 -2 -3 0 1404.46 44.70 2 -3 0 1384.16 43.60 -2 -3 0 1297.47 48.40 -2 3 0 1372.76 46.80 3 -3 0 3427.06 107.69 -3 3 0 3400.96 112.19 -3 -3 0 3508.05 109.49 4 -3 0 1595.64 51.69 -4 3 0 1634.74 57.59 -4 -3 0 1577.74 60.49 -4 -3 0 1672.93 54.19 -5 -3 0 2192.48 70.79 -5 -3 0 2023.60 78.69 -5 3 0 2163.28 68.39 -5 3 0 2122.89 75.59 5 -3 0 2097.59 67.49 -6 -3 0 387.46 17.40 -6 3 0 374.76 15.00 -6 -3 0 368.06 24.20 -6 3 0 382.86 21.90 6 -3 0 379.66 14.20 -7 3 0 1535.55 62.99 -7 -3 0 1567.74 54.29 -7 -3 0 1423.46 65.89 -7 3 0 1444.76 47.30 -7 -3 0 1478.55 48.10 -7 3 0 1521.75 51.09 -8 -3 0 125.19 10.30 8 3 0 129.89 9.60 -8 3 0 121.79 8.80 -8 3 0 126.79 5.30 -8 -3 0 129.99 6.00 -8 -3 0 124.79 18.00 -9 3 0 48.10 2.90 9 -3 0 53.79 6.80 9 3 0 55.49 6.60 -9 3 0 35.80 6.50 -9 -3 0 35.30 6.90 -9 -3 0 54.49 3.50 -10 3 0 88.69 4.70 10 -3 0 87.69 3.90 -10 -3 0 86.49 5.30 -11 -3 0 5.70 1.20 11 3 0 3.80 0.80 -11 3 0 4.60 1.00 12 3 0 10.10 1.30 12 -3 0 10.10 1.20 -12 3 0 11.30 1.30 -12 -3 0 8.60 1.20 12 3 0 10.00 1.30 0 4 0 8210.88 254.07 -1 -4 0 1739.73 63.69 -1 -4 0 1968.10 59.99 1 4 0 1987.10 58.79 1 -4 0 1790.92 57.89 -1 4 0 1792.12 62.69 -2 -4 0 4459.75 142.19 -2 4 0 4485.85 145.19 2 -4 0 4582.54 141.09 -3 4 0 1433.46 49.80 -3 -4 0 1348.47 52.49 3 -4 0 1373.26 44.90 -3 -4 0 1416.96 46.90 -4 4 0 245.48 13.80 -4 -4 0 248.38 11.60 -4 -4 0 232.28 16.00 4 -4 0 241.48 9.30 -5 -4 0 2672.73 87.39 -5 4 0 2663.83 92.19 -5 -4 0 2599.34 96.89 5 -4 0 2620.34 83.59 -6 4 0 2427.76 78.59 -6 -4 0 2417.46 82.99 6 -4 0 2456.05 77.69 -6 -4 0 2425.66 79.59 -6 4 0 2425.36 88.69 -7 -4 0 102.29 5.00 7 4 0 104.59 8.10 -7 4 0 94.39 12.40 -7 -4 0 106.89 8.90 -7 -4 0 106.49 14.10 -7 4 0 98.89 4.30 -7 4 0 104.29 6.70 8 -4 0 6.50 2.60 -8 4 0 2.40 2.60 -8 4 0 5.90 1.60 8 4 0 5.70 2.80 -8 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510.35 30.30 -5 7 0 173.48 6.60 5 7 0 200.68 10.60 -5 -7 0 206.28 12.20 -5 -7 0 171.38 7.50 -5 7 0 187.68 14.90 5 -7 0 192.28 8.70 -5 -7 0 165.68 17.20 -6 -7 0 355.16 13.60 -6 7 0 350.86 12.40 6 -7 0 390.16 15.00 -6 7 0 369.86 23.90 -6 -7 0 344.77 28.00 -6 -7 0 368.46 19.30 6 7 0 387.76 17.70 7 7 0 137.89 9.80 -7 7 0 132.49 5.40 -7 -7 0 138.89 11.60 -7 -7 0 113.29 20.40 -7 -7 0 130.69 6.40 -8 7 0 260.57 9.20 8 7 0 231.38 9.40 -8 -7 0 264.17 10.40 -8 7 0 242.38 13.40 8 7 0 246.88 15.00 -8 -7 0 258.77 17.30 9 7 0 210.98 8.60 -9 -7 0 236.88 9.60 -9 7 0 239.28 8.60 10 -7 0 20.20 1.60 -10 -7 0 19.80 2.00 -10 7 0 18.10 1.70 11 -7 0 51.89 2.50 -11 7 0 48.70 3.60 -11 -7 0 52.69 2.90 11 -7 0 56.09 3.30 12 -7 0 241.18 8.70 -12 7 0 220.88 7.90 0 -8 0 27.00 3.20 0 8 0 20.30 1.90 0 8 0 17.50 4.50 -1 8 0 1079.59 45.10 -1 -8 0 1139.69 39.00 1 8 0 1130.49 36.20 1 -8 0 1077.29 38.60 1 8 0 1013.80 45.40 2 -8 0 5.70 1.50 2 8 0 8.70 1.70 -2 8 0 6.50 2.80 -2 -8 0 6.20 1.90 2 8 0 9.70 4.10 3 -8 0 27.20 3.20 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422.26 24.80 -6 -12 0 503.05 17.40 -7 -12 0 107.09 5.20 -7 12 0 101.39 4.40 7 12 0 102.09 4.80 8 12 0 80.19 3.80 -8 12 0 81.29 3.60 -8 -12 0 78.59 4.00 -9 12 0 11.90 1.30 -9 -12 0 12.00 1.30 9 12 0 12.30 1.10 10 -12 0 7.10 0.80 -10 12 0 6.10 0.70 10 12 0 4.60 0.60 0 13 0 0.20 0.50 0 -13 0 -0.10 2.00 1 13 0 91.29 4.30 -1 13 0 89.79 4.20 1 -13 0 79.99 8.20 -1 -13 0 85.89 9.00 -1 -13 0 86.99 5.10 2 -13 0 28.90 2.00 2 -13 0 29.20 5.30 2 13 0 32.80 2.40 -2 -13 0 29.40 2.40 -2 13 0 33.70 2.20 -3 13 0 39.50 2.30 3 -13 0 40.70 5.80 3 13 0 36.80 2.60 3 -13 0 30.60 2.00 -3 -13 0 37.80 2.70 -3 -13 0 39.00 7.10 4 13 0 117.79 5.30 -4 -13 0 111.89 10.90 -4 -13 0 110.79 5.40 -4 -13 0 93.99 10.70 -4 13 0 114.89 4.70 4 -13 0 95.79 8.60 -5 -13 0 192.48 15.20 5 13 0 197.38 7.80 -5 -13 0 165.88 14.20 -5 -13 0 189.28 8.00 -5 13 0 189.78 7.10 6 13 0 15.30 1.70 -6 13 0 14.80 1.40 -6 -13 0 11.90 1.70 -7 -13 0 0.80 0.70 -7 13 0 -0.20 0.40 7 13 0 0.40 0.60 -8 13 0 27.60 1.70 8 13 0 26.60 1.90 -8 -13 0 28.40 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8 5 -4 55.09 6.80 -8 5 -4 53.59 2.90 -8 -5 4 53.39 3.70 8 -5 -4 54.99 3.10 -8 5 -4 48.50 11.00 8 -5 -4 42.90 6.90 9 5 -4 188.98 7.70 9 5 -4 193.68 8.20 9 5 -4 183.38 13.60 -9 -5 -4 166.28 22.40 -9 5 4 202.48 7.70 -9 5 4 194.18 13.00 -9 -5 -4 213.48 8.20 9 -5 -4 205.18 7.80 -9 5 -4 229.78 22.40 -9 5 -4 202.88 7.70 -9 -5 4 159.38 15.20 -9 -5 4 204.78 8.70 10 5 -4 73.79 3.60 -10 5 4 69.89 3.60 10 5 -4 74.49 3.90 -10 -5 -4 70.59 3.60 -10 -5 4 71.79 4.20 10 -5 -4 70.39 3.50 -10 5 -4 69.69 3.50 10 -5 -4 71.59 3.90 -11 -5 -4 10.30 2.10 -11 5 4 14.60 1.50 11 5 -4 14.70 1.50 11 -5 -4 12.10 1.30 -11 -5 4 14.10 1.60 -11 5 -4 12.80 1.30 11 -5 -4 11.60 1.40 -12 5 4 32.90 2.20 12 5 -4 32.70 1.70 12 -5 -4 35.20 2.10 -12 -5 4 31.40 2.10 12 -5 -4 34.00 1.90 0 6 -4 466.65 22.80 0 -6 4 506.65 18.70 0 -6 -4 507.95 18.90 0 6 -4 518.85 18.80 1 6 -4 181.68 8.60 -1 -6 -4 174.78 8.60 -1 -6 -4 174.38 8.60 1 6 -4 162.88 11.60 1 -6 4 172.58 7.60 1 -6 -4 179.98 8.40 -1 -6 4 170.58 8.70 -1 6 -4 171.68 11.50 -1 6 -4 180.78 8.20 -2 -6 -4 162.18 12.20 2 6 -4 189.18 9.10 -2 -6 -4 193.28 9.20 2 6 -4 167.68 12.40 -2 -6 -4 197.98 9.50 -2 6 -4 190.88 8.70 2 -6 -4 181.48 8.70 -2 -6 4 185.48 9.70 -2 6 -4 178.18 16.60 3 6 -4 111.49 6.90 -3 -6 -4 111.39 6.70 -3 -6 -4 108.89 7.10 -3 -6 -4 106.59 10.30 3 -6 4 109.49 5.60 -3 -6 4 101.79 11.60 3 -6 -4 107.09 6.20 3 -6 -4 97.99 10.60 -3 6 -4 115.29 9.20 -3 -6 4 111.89 7.60 4 -6 4 1893.01 62.29 -4 -6 -4 2006.50 65.29 4 6 -4 2013.80 66.09 -4 -6 -4 2010.10 66.69 -4 -6 -4 1891.81 75.19 4 -6 -4 1997.90 64.69 -4 -6 4 1724.23 81.09 -4 -6 4 2009.00 67.69 -4 6 -4 2100.49 71.89 -5 -6 -4 142.09 9.30 -5 -6 -4 139.99 14.40 -5 -6 -4 135.79 8.00 5 6 -4 135.59 8.80 -5 6 -4 126.39 5.00 -5 -6 4 134.29 9.80 5 -6 -4 142.99 8.90 -5 -6 4 121.09 5.90 -5 6 -4 146.79 12.00 -6 -6 -4 48.30 3.00 6 6 -4 49.20 3.00 -6 -6 -4 45.20 6.20 6 6 -4 47.60 5.60 -6 6 4 46.90 2.50 -6 -6 4 49.80 6.60 -6 6 -4 56.89 8.40 -6 -6 4 50.99 3.40 -6 6 -4 54.79 2.60 6 -6 -4 49.00 4.60 -7 -6 -4 306.57 17.20 -7 -6 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1 -20 74.19 3.50 -2 1 -20 76.79 3.30 -3 -1 -20 47.50 2.40 3 1 -20 41.00 2.00 -3 1 -20 46.10 2.40 -4 -1 -20 9.20 0.90 -4 1 -20 10.10 0.90 4 -1 -20 11.30 0.90 0 2 -20 2.70 0.70 0 2 -20 2.60 0.70 0 2 -20 2.60 0.60 0 -2 -20 3.10 0.80 -1 -2 -20 27.10 1.90 1 2 -20 27.90 1.70 1 2 -20 28.10 1.70 1 2 -20 24.20 2.30 -1 2 -20 29.70 2.10 -1 2 -20 30.70 1.90 2 2 -20 28.30 1.60 -2 -2 -20 28.30 2.00 2 2 -20 26.40 1.50 2 2 -20 25.20 2.00 -2 2 -20 26.80 1.60 -2 2 -20 29.30 1.90 3 2 -20 93.39 3.70 -3 -2 -20 95.79 3.90 -3 2 -20 93.69 3.90 0 3 -20 26.90 1.70 0 -3 -20 25.30 2.80 0 3 -20 31.60 2.30 0 3 -20 28.50 2.00 1 3 -20 91.69 3.70 1 3 -20 89.89 3.80 -1 -3 -20 80.29 5.10 1 3 -20 90.09 3.70 -1 3 -20 101.69 4.50 -1 3 -20 88.39 3.90 2 3 -20 52.79 2.40 2 3 -20 54.79 3.10 2 3 -20 54.09 2.80 -2 -3 -20 49.70 3.40 -2 3 -20 60.29 2.70 -2 3 -20 58.29 3.80 3 3 -20 6.30 0.70 3 3 -20 4.40 0.60 -3 3 -20 6.40 1.00 -3 3 -20 4.20 0.70 0 4 -20 6.90 0.90 0 -4 -20 6.10 1.40 0 4 -20 7.20 0.90 0 4 -20 7.90 0.90 -1 -4 -20 0.10 0.60 1 4 -20 0.60 0.40 1 4 -20 0.30 0.30 1 4 -20 0.70 0.40 -1 4 -20 0.70 0.40 -1 4 -20 -0.10 0.40 2 4 -20 34.80 2.00 -2 -4 -20 29.00 2.50 -2 4 -20 36.70 1.90 -2 4 -20 34.20 1.90 3 4 -20 17.10 1.10 3 4 -20 17.90 1.20 -3 4 -20 17.90 1.20 -3 4 -20 19.10 1.40 0 -5 -20 114.49 6.30 0 5 -20 127.89 5.00 0 5 -20 128.49 4.90 0 5 -20 125.09 4.80 1 5 -20 109.39 4.20 1 5 -20 118.89 4.50 -1 -5 -20 103.49 6.00 1 5 -20 116.99 4.90 1 -5 -20 104.49 4.80 -1 5 -20 116.89 4.40 -1 5 -20 115.29 4.50 1 -5 -20 111.19 6.20 -2 -5 -20 29.80 2.50 2 5 -20 36.60 1.80 2 5 -20 35.10 1.80 0 6 -20 47.80 2.40 0 -6 -20 37.30 3.10 0 6 -20 43.40 2.00 0 -6 -20 42.70 1.90 0 6 -20 44.40 2.10 -1 -6 -20 88.29 5.10 1 6 -20 102.39 3.90 1 6 -20 100.99 3.90 -1 6 -20 99.29 3.80 -1 6 -20 101.19 3.90 1 -6 -20 97.19 3.70 0 0 -21 0.80 0.40 -1 0 -21 11.90 1.00 0 1 -21 232.68 8.10 -1 1 -21 19.60 1.30 0 2 -21 84.69 3.30 0 2 -21 71.09 3.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 3622 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.66156(11) 0.45667(7) 0.31000(6) 0.0257(2) Uani d . . . 1 . . H H1A 0.717(2) 0.45182(19) 0.2754(14) 0.039 Uiso calc U . R 1 . . O O3 0.47120(14) 0.29452(8) 0.68163(7) 0.0378(3) Uani d . . . 1 . . O O4 0.65960(11) 0.52161(7) 0.70320(6) 0.0253(2) Uani d . . . 1 . . O O5 0.46797(12) 0.31961(7) 0.54372(6) 0.0296(3) Uani d . . . 1 . . H H44 0.45843 0.296575 0.58741 0.044 Uiso calc U . R 1 . . O O6 0.68624(12) 0.54311(7) 0.43011(6) 0.0272(2) Uani d . . . 1 . . H H6A 0.676(2) 0.5134(10) 0.3831(13) 0.041 Uiso calc U . R 1 . . C C1 0.2525(2) 0.64008(16) 0.50472(17) 0.0587(6) Uani d . . . 1 . . H H7 0.228253 0.605377 0.549343 0.088 Uiso calc U . R 1 . . H H6 0.224487 0.61368 0.456055 0.088 Uiso calc U . R 1 . . H H1 0.212512 0.694654 0.509661 0.088 Uiso calc U . R 1 . . C C2 0.39462(18) 0.65010(11) 0.50333(11) 0.0341(4) Uani d . . . 1 . . C C3 0.46559(17) 0.61875(10) 0.56035(10) 0.0275(3) Uani d . . . 1 . . H H8 0.421921 0.589356 0.600274 0.033 Uiso calc U . R 1 . . C C4 0.60660(16) 0.62449(9) 0.56883(9) 0.0254(3) Uani d . . . 1 . . H H9 0.626587 0.652057 0.619096 0.03 Uiso calc U . R 1 . . H H39 0.640513 0.659639 0.526205 0.03 Uiso calc U . R 1 . . C C5 0.67471(14) 0.53836(8) 0.56646(9) 0.0202(3) Uani d . . . 1 . . C C6 0.64295(14) 0.49823(9) 0.48936(8) 0.0194(3) Uani d . . . 1 . . C C7 0.57556(14) 0.42694(9) 0.48139(8) 0.0178(3) Uani d . . . 1 . . C C8 0.52856(14) 0.38963(9) 0.40439(8) 0.0184(3) Uani d . . . 1 . . H H31 0.495991 0.333266 0.418157 0.022 Uiso calc U . R 1 . . C C9 0.41359(14) 0.43712(10) 0.37184(8) 0.0224(3) Uani d . . . 1 . . H H19 0.440959 0.492652 0.353854 0.027 Uiso calc U . R 1 . . H H20 0.350158 0.44479 0.413901 0.027 Uiso calc U . R 1 . . C C10 0.35251(16) 0.38984(11) 0.30304(9) 0.0270(3) Uani d . . . 1 . . H H30 0.322113 0.335413 0.323863 0.032 Uiso calc U . R 1 . . C C30 0.12383(19) 0.40164(17) 0.27530(11) 0.0477(5) Uani d . . . 1 . . H H30A 0.052759 0.429988 0.25412 0.057 Uiso calc U . R 1 . . H H30B 0.112819 0.349378 0.300021 0.057 Uiso calc U . R 1 . . C C11 0.23813(18) 0.43493(13) 0.27036(10) 0.0372(4) Uani d . . . 1 . . C C12 0.2601(3) 0.51727(16) 0.23187(15) 0.0590(6) Uani d . . . 1 . . H H28 0.179236 0.539514 0.213064 0.089 Uiso calc U . R 1 . . H H29 0.318177 0.510278 0.187603 0.089 Uiso calc U . R 1 . . H H2 0.297293 0.555797 0.269807 0.089 Uiso calc U . R 1 . . C C13 0.4446(2) 0.69710(13) 0.43381(13) 0.0480(5) Uani d . . . 1 . . H H3 0.416061 0.754844 0.436563 0.072 Uiso calc U . R 1 . . H H4 0.412817 0.671652 0.385573 0.072 Uiso calc U . R 1 . . H H5 0.537425 0.695403 0.434021 0.072 Uiso calc U . R 1 . . C C14 0.82018(15) 0.55393(9) 0.57260(9) 0.0237(3) Uani d . . . 1 . . H H18 0.848769 0.582207 0.524304 0.028 Uiso calc U . R 1 . . H H10 0.836068 0.591992 0.616975 0.028 Uiso calc U . R 1 . . C C15 0.89848(15) 0.47767(10) 0.58386(9) 0.0264(3) Uani d . . . 1 . . H H17 0.888131 0.449901 0.632465 0.032 Uiso calc U . R 1 . . C C16 0.98099(17) 0.44374(10) 0.53431(11) 0.0322(4) Uani d . . . 1 . . C C17 1.0075(2) 0.47573(17) 0.45354(12) 0.0516(5) Uani d . . . 1 . . H H12 0.95607 0.525263 0.443806 0.077 Uiso calc U . R 1 . . H H11 0.986238 0.432942 0.415005 0.077 Uiso calc U . R 1 . . H H13 1.097521 0.489901 0.449032 0.077 Uiso calc U . R 1 . . C C18 1.0557(2) 0.36806(13) 0.55645(17) 0.0530(6) Uani d . . . 1 . . H H15 1.036264 0.352768 0.610642 0.079 Uiso calc U . R 1 . . H H14 1.146411 0.379873 0.55157 0.079 Uiso calc U . R 1 . . H H16 1.033015 0.322149 0.52159 0.079 Uiso calc U . R 1 . . C C19 0.45105(16) 0.37112(10) 0.23931(8) 0.0272(3) Uani d . . . 1 . . H H26 0.411849 0.336069 0.198369 0.033 Uiso calc U . R 1 . . H H27 0.478212 0.423694 0.214562 0.033 Uiso calc U . R 1 . . C C20 0.56681(16) 0.32666(10) 0.27275(9) 0.0252(3) Uani d . . . 1 . . H H24 0.629927 0.318425 0.230594 0.03 Uiso calc U . R 1 . . H H25 0.541038 0.271328 0.292122 0.03 Uiso calc U . R 1 . . C C21 0.62804(15) 0.37535(9) 0.33967(8) 0.0212(3) Uani d . . . 1 . . C C22 0.74516(16) 0.33137(11) 0.37020(10) 0.0295(3) Uani d . . . 1 . . H H21 0.806729 0.325077 0.327683 0.044 Uiso calc U . R 1 . . H H23 0.721453 0.27655 0.390127 0.044 Uiso calc U . R 1 . . H H22 0.782939 0.364089 0.412524 0.044 Uiso calc U . R 1 . . C C23 0.53735(14) 0.38537(9) 0.55193(8) 0.0196(3) Uani d . . . 1 . . C C24 0.57161(14) 0.41160(9) 0.62966(8) 0.0204(3) Uani d . . . 1 . . C C25 0.53839(16) 0.35781(10) 0.69396(9) 0.0258(3) Uani d . . . 1 . . C C26 0.58727(19) 0.36876(11) 0.77681(9) 0.0312(4) Uani d . . . 1 . . H H32 0.583206 0.428792 0.791205 0.037 Uiso calc U . R 1 . . C C27 0.7257(2) 0.34031(12) 0.77802(11) 0.0389(4) Uani d . . . 1 . . H H33 0.730589 0.282118 0.761813 0.058 Uiso calc U . R 1 . . H H35 0.759717 0.346084 0.831102 0.058 Uiso calc U . R 1 . . H H34 0.775414 0.374527 0.741912 0.058 Uiso calc U . R 1 . . C C28 0.5078(3) 0.31890(14) 0.83462(11) 0.0502(6) Uani d . . . 1 . . H H36 0.512228 0.259923 0.821116 0.075 Uiso calc U . R 1 . . H H37 0.419542 0.33757 0.832221 0.075 Uiso calc U . R 1 . . H H38 0.540698 0.327168 0.88769 0.075 Uiso calc U . R 1 . . C C29 0.63521(14) 0.48941(9) 0.63895(8) 0.0196(3) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0313(6) 0.0255(5) 0.0202(5) -0.0017(4) 0.0093(5) 0.0005(4) O3 0.0517(8) 0.0405(7) 0.0211(6) -0.0223(6) -0.0043(5) 0.0089(5) O4 0.0306(6) 0.0264(5) 0.0187(5) 0.0019(4) -0.0063(4) -0.0050(4) O5 0.0411(6) 0.0302(6) 0.0175(5) -0.0182(5) -0.0024(5) 0.0033(4) O6 0.0409(6) 0.0224(5) 0.0182(5) -0.0093(5) 0.0000(4) 0.0043(4) C1 0.0403(12) 0.0517(13) 0.0840(17) 0.0114(10) -0.0192(12) 0.0100(12) C2 0.0400(10) 0.0234(8) 0.0389(9) 0.0081(7) -0.0120(8) -0.0020(7) C3 0.0345(8) 0.0217(7) 0.0264(7) 0.0062(6) -0.0019(7) -0.0008(6) C4 0.0345(8) 0.0164(7) 0.0252(7) 0.0023(6) -0.0071(6) -0.0007(6) C5 0.0248(7) 0.0155(6) 0.0204(7) -0.0010(5) -0.0035(6) -0.0007(5) C6 0.0231(7) 0.0175(6) 0.0175(6) 0.0010(5) 0.0002(5) 0.0025(5) C7 0.0192(7) 0.0191(6) 0.0150(6) 0.0019(5) -0.0005(5) -0.0007(5) C8 0.0215(7) 0.0189(6) 0.0147(6) -0.0006(6) 0.0015(6) -0.0013(5) C9 0.0221(7) 0.0284(8) 0.0167(6) 0.0028(6) 0.0005(6) -0.0033(6) C10 0.0272(8) 0.0343(8) 0.0195(7) 0.0025(7) -0.0032(6) -0.0055(6) C30 0.0311(9) 0.0800(16) 0.0320(9) 0.0133(10) -0.0067(8) -0.0221(10) C11 0.0348(9) 0.0544(11) 0.0225(7) 0.0132(8) -0.0092(7) -0.0115(7) C12 0.0572(14) 0.0615(15) 0.0584(13) 0.0219(12) -0.0209(11) 0.0081(11) C13 0.0610(13) 0.0405(10) 0.0426(10) 0.0082(10) -0.0180(10) 0.0137(9) C14 0.0264(7) 0.0203(7) 0.0244(7) -0.0043(6) -0.0024(6) -0.0009(6) C15 0.0269(8) 0.0243(7) 0.0279(7) -0.0015(6) -0.0009(6) 0.0011(6) C16 0.0277(8) 0.0278(8) 0.0410(9) -0.0050(7) 0.0019(7) -0.0086(7) C17 0.0434(11) 0.0696(14) 0.0417(11) -0.0076(10) 0.0155(9) -0.0105(10) C18 0.0420(11) 0.0331(10) 0.0838(17) 0.0063(8) 0.0106(11) -0.0096(10) C19 0.0336(9) 0.0322(8) 0.0157(7) 0.0030(7) -0.0016(6) -0.0045(6) C20 0.0324(8) 0.0266(7) 0.0168(6) 0.0044(6) 0.0027(6) -0.0037(6) C21 0.0244(7) 0.0218(7) 0.0174(6) 0.0014(6) 0.0033(6) -0.0006(5) C22 0.0264(8) 0.0331(9) 0.0289(8) 0.0086(7) 0.0009(6) -0.0041(7) C23 0.0212(7) 0.0201(7) 0.0174(6) -0.0010(6) -0.0007(6) 0.0004(5) C24 0.0225(7) 0.0233(7) 0.0154(6) -0.0007(6) -0.0009(5) -0.0001(5) C25 0.0304(8) 0.0278(8) 0.0192(7) -0.0026(6) 0.0003(6) 0.0025(6) C26 0.0516(11) 0.0261(8) 0.0160(7) -0.0010(7) -0.0026(7) 0.0011(6) C27 0.0554(12) 0.0298(9) 0.0315(8) 0.0037(8) -0.0211(8) -0.0044(7) C28 0.0846(17) 0.0473(11) 0.0189(8) -0.0068(11) 0.0053(9) 0.0070(8) C29 0.0209(6) 0.0208(7) 0.0170(6) 0.0035(6) -0.0031(5) -0.0010(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C21 O1 H1A . . 109.5 ? C23 O5 H44 . . 109.5 ? C6 O6 H6A . . 109.5 ? C2 C1 H7 . . 109.5 ? C2 C1 H6 . . 109.5 ? H7 C1 H6 . . 109.5 ? C2 C1 H1 . . 109.5 ? H7 C1 H1 . . 109.5 ? H6 C1 H1 . . 109.5 ? C3 C2 C13 . . 124.98(18) ? C3 C2 C1 . . 120.5(2) ? C13 C2 C1 . . 114.51(18) ? C2 C3 C4 . . 127.38(17) ? C2 C3 H8 . . 116.3 ? C4 C3 H8 . . 116.3 ? C3 C4 C5 . . 113.51(13) ? C3 C4 H9 . . 108.9 ? C5 C4 H9 . . 108.9 ? C3 C4 H39 . . 108.9 ? C5 C4 H39 . . 108.9 ? H9 C4 H39 . . 107.7 ? C6 C5 C29 . . 115.27(11) ? C6 C5 C14 . . 110.32(12) ? C29 C5 C14 . . 107.30(12) ? C6 C5 C4 . . 107.58(12) ? C29 C5 C4 . . 108.22(12) ? C14 C5 C4 . . 107.91(12) ? O6 C6 C7 . . 124.46(13) ? O6 C6 C5 . . 110.91(12) ? C7 C6 C5 . . 124.60(12) ? C6 C7 C23 . . 117.24(12) ? C6 C7 C8 . . 126.07(13) ? C23 C7 C8 . . 116.55(12) ? C7 C8 C9 . . 111.77(11) ? C7 C8 C21 . . 117.07(12) ? C9 C8 C21 . . 110.59(11) ? C7 C8 H31 . . 105.5 ? C9 C8 H31 . . 105.5 ? C21 C8 H31 . . 105.5 ? C8 C9 C10 . . 111.03(12) ? C8 C9 H19 . . 109.4 ? C10 C9 H19 . . 109.4 ? C8 C9 H20 . . 109.4 ? C10 C9 H20 . . 109.4 ? H19 C9 H20 . . 108.0 ? C11 C10 C19 . . 111.84(13) ? C11 C10 C9 . . 112.11(13) ? C19 C10 C9 . . 110.78(13) ? C11 C10 H30 . . 107.3 ? C19 C10 H30 . . 107.3 ? C9 C10 H30 . . 107.3 ? C11 C30 H30A . . 120.0 ? C11 C30 H30B . . 120.0 ? H30A C30 H30B . . 120.0 ? C30 C11 C12 . . 121.89(19) ? C30 C11 C10 . . 120.5(2) ? C12 C11 C10 . . 117.60(18) ? C11 C12 H28 . . 109.5 ? C11 C12 H29 . . 109.5 ? H28 C12 H29 . . 109.5 ? C11 C12 H2 . . 109.5 ? H28 C12 H2 . . 109.5 ? H29 C12 H2 . . 109.5 ? C2 C13 H3 . . 109.5 ? C2 C13 H4 . . 109.5 ? H3 C13 H4 . . 109.5 ? C2 C13 H5 . . 109.5 ? H3 C13 H5 . . 109.5 ? H4 C13 H5 . . 109.5 ? C15 C14 C5 . . 114.87(12) ? C15 C14 H18 . . 108.6 ? C5 C14 H18 . . 108.6 ? C15 C14 H10 . . 108.6 ? C5 C14 H10 . . 108.6 ? H18 C14 H10 . . 107.5 ? C16 C15 C14 . . 128.15(16) ? C16 C15 H17 . . 115.9 ? C14 C15 H17 . . 115.9 ? C15 C16 C17 . . 124.44(18) ? C15 C16 C18 . . 121.11(18) ? C17 C16 C18 . . 114.44(18) ? C16 C17 H12 . . 109.5 ? C16 C17 H11 . . 109.5 ? H12 C17 H11 . . 109.5 ? C16 C17 H13 . . 109.5 ? H12 C17 H13 . . 109.5 ? H11 C17 H13 . . 109.5 ? C16 C18 H15 . . 109.5 ? C16 C18 H14 . . 109.5 ? H15 C18 H14 . . 109.5 ? C16 C18 H16 . . 109.5 ? H15 C18 H16 . . 109.5 ? H14 C18 H16 . . 109.5 ? C20 C19 C10 . . 111.61(12) ? C20 C19 H26 . . 109.3 ? C10 C19 H26 . . 109.3 ? C20 C19 H27 . . 109.3 ? C10 C19 H27 . . 109.3 ? H26 C19 H27 . . 108.0 ? C19 C20 C21 . . 112.11(12) ? C19 C20 H24 . . 109.2 ? C21 C20 H24 . . 109.2 ? C19 C20 H25 . . 109.2 ? C21 C20 H25 . . 109.2 ? H24 C20 H25 . . 107.9 ? O1 C21 C22 . . 110.15(13) ? O1 C21 C20 . . 107.81(12) ? C22 C21 C20 . . 111.16(12) ? O1 C21 C8 . . 106.36(11) ? C22 C21 C8 . . 112.18(12) ? C20 C21 C8 . . 108.98(12) ? C21 C22 H21 . . 109.5 ? C21 C22 H23 . . 109.5 ? H21 C22 H23 . . 109.5 ? C21 C22 H22 . . 109.5 ? H21 C22 H22 . . 109.5 ? H23 C22 H22 . . 109.5 ? O5 C23 C7 . . 116.71(12) ? O5 C23 C24 . . 118.81(13) ? C7 C23 C24 . . 124.48(13) ? C29 C24 C23 . . 118.51(13) ? C29 C24 C25 . . 123.80(13) ? C23 C24 C25 . . 117.69(13) ? O3 C25 C24 . . 119.74(14) ? O3 C25 C26 . . 116.20(14) ? C24 C25 C26 . . 123.91(14) ? C25 C26 C28 . . 110.88(16) ? C25 C26 C27 . . 107.58(14) ? C28 C26 C27 . . 110.95(16) ? C25 C26 H32 . . 109.1 ? C28 C26 H32 . . 109.1 ? C27 C26 H32 . . 109.1 ? C26 C27 H33 . . 109.5 ? C26 C27 H35 . . 109.5 ? H33 C27 H35 . . 109.5 ? C26 C27 H34 . . 109.5 ? H33 C27 H34 . . 109.5 ? H35 C27 H34 . . 109.5 ? C26 C28 H36 . . 109.5 ? C26 C28 H37 . . 109.5 ? H36 C28 H37 . . 109.5 ? C26 C28 H38 . . 109.5 ? H36 C28 H38 . . 109.5 ? H37 C28 H38 . . 109.5 ? O4 C29 C24 . . 124.18(14) ? O4 C29 C5 . . 116.39(13) ? C24 C29 C5 . . 119.41(12) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C21 . 1.4502(18) ? O1 H1A . 0.83(3) ? O3 C25 . 1.261(2) ? O4 C29 . 1.2415(18) ? O5 C23 . 1.2964(18) ? O5 H44 . 0.84 ? O6 C6 . 1.3258(17) ? O6 H6A . 0.94(2) ? C1 C2 . 1.508(3) ? C1 H7 . 0.98 ? C1 H6 . 0.98 ? C1 H1 . 0.98 ? C2 C3 . 1.329(2) ? C2 C13 . 1.505(3) ? C3 C4 . 1.498(2) ? C3 H8 . 0.95 ? C4 C5 . 1.565(2) ? C4 H9 . 0.99 ? C4 H39 . 0.99 ? C5 C6 . 1.5059(19) ? C5 C29 . 1.527(2) ? C5 C14 . 1.559(2) ? C6 C7 . 1.359(2) ? C7 C23 . 1.4371(19) ? C7 C8 . 1.5296(18) ? C8 C9 . 1.539(2) ? C8 C21 . 1.542(2) ? C8 H31 . 1.0 ? C9 C10 . 1.542(2) ? C9 H19 . 0.99 ? C9 H20 . 0.99 ? C10 C11 . 1.516(2) ? C10 C19 . 1.536(2) ? C10 H30 . 1.0 ? C30 C11 . 1.323(3) ? C30 H30A . 0.95 ? C30 H30B . 0.95 ? C11 C12 . 1.500(3) ? C12 H28 . 0.98 ? C12 H29 . 0.98 ? C12 H2 . 0.98 ? C13 H3 . 0.98 ? C13 H4 . 0.98 ? C13 H5 . 0.98 ? C14 C15 . 1.494(2) ? C14 H18 . 0.99 ? C14 H10 . 0.99 ? C15 C16 . 1.332(2) ? C15 H17 . 0.95 ? C16 C17 . 1.500(3) ? C16 C18 . 1.501(3) ? C17 H12 . 0.98 ? C17 H11 . 0.98 ? C17 H13 . 0.98 ? C18 H15 . 0.98 ? C18 H14 . 0.98 ? C18 H16 . 0.98 ? C19 C20 . 1.527(2) ? C19 H26 . 0.99 ? C19 H27 . 0.99 ? C20 C21 . 1.530(2) ? C20 H24 . 0.99 ? C20 H25 . 0.99 ? C21 C22 . 1.517(2) ? C22 H21 . 0.98 ? C22 H23 . 0.98 ? C22 H22 . 0.98 ? C23 C24 . 1.4402(19) ? C24 C29 . 1.432(2) ? C24 C25 . 1.443(2) ? C25 C26 . 1.517(2) ? C26 C28 . 1.525(3) ? C26 C27 . 1.531(3) ? C26 H32 . 1.0 ? C27 H33 . 0.98 ? C27 H35 . 0.98 ? C27 H34 . 0.98 ? C28 H36 . 0.98 ? C28 H37 . 0.98 ? C28 H38 . 0.98 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1A O4 4_664 0.83 1.85 2.6485(15) 161.1 ? O5 H44 O3 . 0.84 1.62 2.3915(14) 152.2 ? O6 H6A O1 . 0.94 1.56 2.4949(16) 174.4 ? C8 H31 O5 . 1.00 2.18 2.7118(17) 111.7 ? C22 H21 O3 2_556 0.98 2.60 3.255(2) 124.4 ? C26 H32 O4 . 1.00 2.27 2.871(2) 117.4 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C13 C2 C3 C4 . . . . 1.3(3) ? C1 C2 C3 C4 . . . . -178.67(19) ? C2 C3 C4 C5 . . . . -117.42(18) ? C3 C4 C5 C6 . . . . 58.80(17) ? C3 C4 C5 C29 . . . . -66.35(16) ? C3 C4 C5 C14 . . . . 177.83(14) ? C29 C5 C6 O6 . . . . -176.92(13) ? C14 C5 C6 O6 . . . . -55.22(16) ? C4 C5 C6 O6 . . . . 62.26(16) ? C29 C5 C6 C7 . . . . 5.0(2) ? C14 C5 C6 C7 . . . . 126.68(15) ? C4 C5 C6 C7 . . . . -115.84(15) ? O6 C6 C7 C23 . . . . 179.16(14) ? C5 C6 C7 C23 . . . . -3.0(2) ? O6 C6 C7 C8 . . . . -5.3(2) ? C5 C6 C7 C8 . . . . 172.55(13) ? C6 C7 C8 C9 . . . . -75.27(18) ? C23 C7 C8 C9 . . . . 100.30(15) ? C6 C7 C8 C21 . . . . 53.7(2) ? C23 C7 C8 C21 . . . . -130.70(14) ? C7 C8 C9 C10 . . . . -169.61(12) ? C21 C8 C9 C10 . . . . 58.06(16) ? C8 C9 C10 C11 . . . . 179.45(14) ? C8 C9 C10 C19 . . . . -54.84(17) ? C19 C10 C11 C30 . . . . 119.50(18) ? C9 C10 C11 C30 . . . . -115.37(18) ? C19 C10 C11 C12 . . . . -59.8(2) ? C9 C10 C11 C12 . . . . 65.3(2) ? C6 C5 C14 C15 . . . . -71.91(16) ? C29 C5 C14 C15 . . . . 54.39(17) ? C4 C5 C14 C15 . . . . 170.81(12) ? C5 C14 C15 C16 . . . . 112.65(19) ? C14 C15 C16 C17 . . . . -2.5(3) ? C14 C15 C16 C18 . . . . 177.75(17) ? C11 C10 C19 C20 . . . . 179.28(14) ? C9 C10 C19 C20 . . . . 53.43(18) ? C10 C19 C20 C21 . . . . -55.84(18) ? C19 C20 C21 O1 . . . . -57.38(16) ? C19 C20 C21 C22 . . . . -178.19(13) ? C19 C20 C21 C8 . . . . 57.67(16) ? C7 C8 C21 O1 . . . . -72.12(15) ? C9 C8 C21 O1 . . . . 57.43(15) ? C7 C8 C21 C22 . . . . 48.36(17) ? C9 C8 C21 C22 . . . . 177.92(13) ? C7 C8 C21 C20 . . . . 171.90(12) ? C9 C8 C21 C20 . . . . -58.54(15) ? C6 C7 C23 O5 . . . . 176.79(14) ? C8 C7 C23 O5 . . . . 0.8(2) ? C6 C7 C23 C24 . . . . -3.6(2) ? C8 C7 C23 C24 . . . . -179.62(13) ? O5 C23 C24 C29 . . . . -172.66(14) ? C7 C23 C24 C29 . . . . 7.8(2) ? O5 C23 C24 C25 . . . . 6.7(2) ? C7 C23 C24 C25 . . . . -172.81(14) ? C29 C24 C25 O3 . . . . 172.79(15) ? C23 C24 C25 O3 . . . . -6.6(2) ? C29 C24 C25 C26 . . . . -11.8(3) ? C23 C24 C25 C26 . . . . 168.87(15) ? O3 C25 C26 C28 . . . . -20.5(2) ? C24 C25 C26 C28 . . . . 163.89(17) ? O3 C25 C26 C27 . . . . 100.98(18) ? C24 C25 C26 C27 . . . . -74.6(2) ? C23 C24 C29 O4 . . . . 173.59(14) ? C25 C24 C29 O4 . . . . -5.8(2) ? C23 C24 C29 C5 . . . . -5.2(2) ? C25 C24 C29 C5 . . . . 175.43(14) ? C6 C5 C29 O4 . . . . -179.48(13) ? C14 C5 C29 O4 . . . . 57.21(17) ? C4 C5 C29 O4 . . . . -59.00(17) ? C6 C5 C29 C24 . . . . -0.6(2) ? C14 C5 C29 C24 . . . . -123.91(14) ? C4 C5 C29 C24 . . . . 119.88(14) ?