#------------------------------------------------------------------------------ #$Date: 2023-04-20 14:53:48 +0300 (Thu, 20 Apr 2023) $ #$Revision: 282777 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/78/1547870.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_1547870 loop_ _publ_author_name 'Yang, Liu-Pan' 'Jia, Fei' 'Pan, Fangfang' 'Pan, Zhi-Sheng' 'Rissanen, Kari' 'Jiang, Wei' _publ_section_title ; Effects of side chains of oxatub[4]arene on its conformational interconversion, molecular recognition and macroscopic self-assembly ; _journal_issue 93 _journal_name_full 'Chemical Communications' _journal_page_first 12572 _journal_page_last 12575 _journal_paper_doi 10.1039/C7CC07630D _journal_volume 53 _journal_year 2017 _chemical_formula_moiety 'C80 H104 O12' _chemical_formula_sum 'C80 H104 O12' _chemical_formula_weight 1257.63 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2017-09-28 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _audit_update_record ; 2017-09-29 deposited with the CCDC. 2017-11-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.169(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 18.8502(5) _cell_length_b 9.25277(17) _cell_length_c 20.4322(5) _cell_measurement_reflns_used 5902 _cell_measurement_temperature 120.01(10) _cell_measurement_theta_max 28.1890 _cell_measurement_theta_min 3.2330 _cell_volume 3422.75(15) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 120.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0107 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.872 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -19.00 24.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - -16.7586 -99.0000 0.0000 43 #__ type_ start__ end____ width___ exp.time_ 2 omega -51.00 39.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 17.8523 -57.0000 -30.0000 90 #__ type_ start__ end____ width___ exp.time_ 3 omega -4.00 87.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 17.8523 57.0000 -120.0000 91 #__ type_ start__ end____ width___ exp.time_ 4 omega -51.00 39.00 1.0000 50.0000 omega____ theta____ kappa____ phi______ frames - 17.8523 -57.0000 90.0000 90 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0144575000 _diffrn_orient_matrix_UB_12 -0.0390886000 _diffrn_orient_matrix_UB_13 -0.0307004000 _diffrn_orient_matrix_UB_21 -0.0046197000 _diffrn_orient_matrix_UB_22 0.0655205000 _diffrn_orient_matrix_UB_23 -0.0187438000 _diffrn_orient_matrix_UB_31 0.0361227000 _diffrn_orient_matrix_UB_32 -0.0073110000 _diffrn_orient_matrix_UB_33 -0.0037132000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_unetI/netI 0.0469 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.872 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 20660 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.872 _diffrn_reflns_theta_full 25.250 _diffrn_reflns_theta_max 28.393 _diffrn_reflns_theta_min 3.026 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_correction_T_min 0.987 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.220 _exptl_crystal_description plate _exptl_crystal_F_000 1360 _exptl_crystal_size_max 0.3063 _exptl_crystal_size_mid 0.1467 _exptl_crystal_size_min 0.0903 _refine_diff_density_max 0.248 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 419 _refine_ls_number_reflns 7487 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0470 _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^)+(0.0374P)^2^+1.6568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.1123 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5352 _reflns_number_total 7487 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cc07630d2.cif _cod_data_source_block 1a _cod_database_code 1547870 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C50 H50 O4 N4' _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. ; _reflns_odcompleteness_completeness 98.49 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C12(H12A,H12B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A, H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C7(H7), C8(H8), C15(H15), C16(H16), C19(H19), C20(H20) 2.c Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C40(H40A,H40B, H40C) ; _shelx_res_file ; 1a.res created by SHELXL-2014/7 TITL TA4-TCNQ_150504 in P21/n #14 REM reset to P21/n #14 CELL 0.71073 18.850154 9.252775 20.432247 90 106.169 90 ZERR 2 0.000472 0.000173 0.000532 0 0.0029 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 160 208 24 L.S. 4 PLAN 2 TEMP -153.14(10) BOND MORE -1 BOND $H CONF fmap 2 acta 50.5 OMIT 2 1 1 OMIT 3 6 6 OMIT 2 0 2 OMIT -1 0 3 OMIT 4 8 8 OMIT 1 1 2 REM REM REM WGHT 0.037400 1.656800 FVAR 2.45213 C1 1 0.487373 0.621861 0.913927 11.00000 0.01718 0.01944 = 0.02623 0.00202 0.00817 -0.00121 C2 1 0.534280 0.674379 0.975575 11.00000 0.02309 0.02221 = 0.02012 -0.00030 0.01035 0.00150 AFIX 43 H2 2 0.514728 0.695896 1.012584 11.00000 -1.20000 AFIX 0 C3 1 0.607836 0.694510 0.982361 11.00000 0.02114 0.01929 = 0.01775 0.00032 0.00516 -0.00098 AFIX 43 H3 2 0.638977 0.727619 1.024649 11.00000 -1.20000 AFIX 0 C4 1 0.638653 0.667155 0.927831 11.00000 0.01981 0.01594 = 0.01907 0.00293 0.00613 0.00123 C5 1 0.590691 0.614583 0.865353 11.00000 0.01906 0.01567 = 0.02139 0.00120 0.00657 0.00052 C6 1 0.514511 0.589453 0.859332 11.00000 0.02004 0.01581 = 0.02071 0.00241 0.00604 0.00065 C7 1 0.621321 0.591549 0.810215 11.00000 0.02263 0.02299 = 0.01775 -0.00144 0.00571 -0.00143 AFIX 43 H7 2 0.590993 0.553647 0.768586 11.00000 -1.20000 AFIX 0 C8 1 0.693476 0.622745 0.815775 11.00000 0.02411 0.02932 = 0.01999 -0.00270 0.01098 -0.00167 AFIX 43 H8 2 0.712296 0.608970 0.777659 11.00000 -1.20000 AFIX 0 C9 1 0.740557 0.675366 0.877665 11.00000 0.01760 0.02373 = 0.02335 0.00204 0.00761 -0.00075 C10 1 0.714817 0.695303 0.933763 11.00000 0.01850 0.01663 = 0.02062 0.00137 0.00613 0.00069 C11 1 0.462980 0.529928 0.794880 11.00000 0.02105 0.01895 = 0.02301 -0.00076 0.00582 0.00125 AFIX 23 H11A 2 0.412689 0.520471 0.800495 11.00000 -1.20000 H11B 2 0.460557 0.597278 0.756670 11.00000 -1.20000 AFIX 0 C12 1 0.429701 0.296722 0.745687 11.00000 0.01614 0.02187 = 0.01893 -0.00386 0.00437 -0.00143 AFIX 23 H12A 2 0.447949 0.228658 0.716667 11.00000 -1.20000 H12B 2 0.389347 0.354412 0.715657 11.00000 -1.20000 AFIX 0 C13 1 0.399525 0.211649 0.795285 11.00000 0.01802 0.01726 = 0.01589 -0.00358 0.00451 -0.00163 C14 1 0.446672 0.110698 0.835287 11.00000 0.01576 0.02003 = 0.01970 -0.00337 0.00373 -0.00037 C15 1 0.424432 0.025927 0.883330 11.00000 0.02002 0.02002 = 0.02037 0.00088 0.00272 0.00273 AFIX 43 H15 2 0.457476 -0.042559 0.910330 11.00000 -1.20000 AFIX 0 C16 1 0.355052 0.042593 0.890964 11.00000 0.02362 0.01756 = 0.01863 0.00133 0.00670 -0.00096 AFIX 43 H16 2 0.340682 -0.014808 0.923659 11.00000 -1.20000 AFIX 0 C17 1 0.304071 0.142978 0.851509 11.00000 0.01907 0.01536 = 0.01552 -0.00299 0.00387 -0.00131 C18 1 0.327119 0.229209 0.802852 11.00000 0.01824 0.01760 = 0.01360 -0.00301 0.00337 -0.00176 C19 1 0.275135 0.330380 0.764816 11.00000 0.02138 0.02069 = 0.01450 0.00182 0.00557 -0.00133 AFIX 43 H19 2 0.288682 0.388966 0.732050 11.00000 -1.20000 AFIX 0 C20 1 0.206317 0.346519 0.773639 11.00000 0.01740 0.02249 = 0.01934 0.00264 0.00367 0.00231 AFIX 43 H20 2 0.172912 0.414968 0.747034 11.00000 -1.20000 AFIX 0 C21 1 0.184755 0.261239 0.822439 11.00000 0.01636 0.02043 = 0.01646 -0.00325 0.00516 -0.00196 C22 1 0.232171 0.160629 0.860957 11.00000 0.01907 0.01645 = 0.01624 -0.00169 0.00496 -0.00286 C23 1 0.378877 0.653216 0.953413 11.00000 0.02032 0.02292 = 0.02611 -0.00070 0.01178 0.00000 AFIX 23 H23A 2 0.390634 0.756691 0.963019 11.00000 -1.20000 H23B 2 0.396127 0.598255 0.996504 11.00000 -1.20000 AFIX 0 C24 1 0.296751 0.632709 0.922583 11.00000 0.01991 0.02719 = 0.02570 0.00224 0.00787 -0.00052 AFIX 23 H24A 2 0.286822 0.530568 0.908596 11.00000 -1.20000 H24B 2 0.280046 0.693600 0.881301 11.00000 -1.20000 AFIX 0 C25 1 0.253078 0.672371 0.972348 11.00000 0.02089 0.02723 = 0.02850 0.00539 0.00932 0.00150 AFIX 23 H25A 2 0.263539 0.774135 0.986784 11.00000 -1.20000 H25B 2 0.269389 0.610644 1.013381 11.00000 -1.20000 AFIX 0 C26 1 0.170345 0.653658 0.941232 11.00000 0.02213 0.04182 = 0.03839 0.00491 0.01080 -0.00064 AFIX 137 H26A 2 0.144327 0.680350 0.974833 11.00000 -1.50000 H26B 2 0.159621 0.552587 0.927738 11.00000 -1.50000 H26C 2 0.153787 0.715979 0.901080 11.00000 -1.50000 AFIX 0 C27 1 0.766241 0.742362 1.000720 11.00000 0.01852 0.02123 = 0.01961 0.00103 0.00648 0.00148 AFIX 23 H27A 2 0.762076 0.675061 1.037136 11.00000 -1.20000 H27B 2 0.817838 0.739634 0.997979 11.00000 -1.20000 AFIX 0 C28 1 0.210330 0.074443 0.915168 11.00000 0.01774 0.02017 = 0.01825 0.00029 0.00490 -0.00414 AFIX 23 H28A 2 0.157107 0.089592 0.910248 11.00000 -1.20000 H28B 2 0.217868 -0.029628 0.908051 11.00000 -1.20000 AFIX 0 C29 1 0.837135 0.731847 0.825374 11.00000 0.02666 0.04035 = 0.02534 -0.00298 0.01387 -0.00579 AFIX 23 H29A 2 0.804758 0.804805 0.796247 11.00000 -1.20000 H29B 2 0.834660 0.641637 0.798777 11.00000 -1.20000 AFIX 0 C30 1 0.915797 0.786572 0.848602 11.00000 0.02299 0.03947 = 0.03016 0.00017 0.01304 -0.00250 AFIX 23 H30A 2 0.946549 0.713246 0.878921 11.00000 -1.20000 H30B 2 0.934708 0.796604 0.808224 11.00000 -1.20000 AFIX 0 C31 1 0.925134 0.929425 0.885813 11.00000 0.02526 0.03430 = 0.03768 -0.00025 0.01269 -0.00178 AFIX 23 H31A 2 0.906901 0.920286 0.926620 11.00000 -1.20000 H31B 2 0.894983 1.003847 0.855749 11.00000 -1.20000 AFIX 0 C32 1 1.005755 0.977775 0.907619 11.00000 0.02648 0.03661 = 0.04742 -0.00112 0.01028 -0.00613 AFIX 137 H32A 2 1.035866 0.903669 0.936859 11.00000 -1.50000 H32B 2 1.009936 1.068914 0.932846 11.00000 -1.50000 H32C 2 1.023213 0.991776 0.867148 11.00000 -1.50000 AFIX 0 C33 1 0.570712 0.019325 0.873996 11.00000 0.02023 0.02940 = 0.03125 0.00824 0.00356 0.00621 AFIX 23 H33A 2 0.558974 -0.085149 0.872040 11.00000 -1.20000 H33B 2 0.573267 0.055078 0.920264 11.00000 -1.20000 AFIX 0 C34 1 0.643628 0.043552 0.858725 11.00000 0.01942 0.03079 = 0.03097 0.00225 0.00515 0.00713 AFIX 23 H34A 2 0.641648 -0.001405 0.814283 11.00000 -1.20000 H34B 2 0.683050 -0.005537 0.894020 11.00000 -1.20000 AFIX 0 C35 1 0.663594 0.201860 0.856404 11.00000 0.02071 0.03859 = 0.02876 -0.00005 0.00684 0.00109 AFIX 23 H35A 2 0.651983 0.253367 0.894625 11.00000 -1.20000 H35B 2 0.633215 0.244879 0.813335 11.00000 -1.20000 AFIX 0 C36 1 0.745254 0.222750 0.861172 11.00000 0.02374 0.05517 = 0.03997 0.00055 0.01230 -0.00138 AFIX 137 H36A 2 0.775515 0.183189 0.904450 11.00000 -1.50000 H36B 2 0.755727 0.326076 0.858866 11.00000 -1.50000 H36C 2 0.756916 0.172390 0.823258 11.00000 -1.50000 AFIX 0 C37 1 0.065188 0.378063 0.796151 11.00000 0.01827 0.02290 = 0.02440 0.00394 0.00575 0.00303 AFIX 23 H37A 2 0.053595 0.356111 0.746877 11.00000 -1.20000 H37B 2 0.085854 0.476974 0.803916 11.00000 -1.20000 AFIX 0 C38 1 -0.003847 0.366790 0.820012 11.00000 0.01774 0.02829 = 0.02945 0.00186 0.00602 0.00253 AFIX 23 H38A 2 -0.023722 0.267439 0.811259 11.00000 -1.20000 H38B 2 -0.041557 0.433767 0.792682 11.00000 -1.20000 AFIX 0 C39 1 0.008492 0.401362 0.895095 11.00000 0.02302 0.03121 = 0.03574 -0.00423 0.01406 -0.00396 AFIX 23 H39A 2 0.025876 0.502402 0.903658 11.00000 -1.20000 H39B 2 0.047668 0.337401 0.922588 11.00000 -1.20000 AFIX 0 C40 1 -0.061296 0.382171 0.918019 11.00000 0.03198 0.04251 = 0.05038 -0.00683 0.02346 -0.00517 AFIX 137 H40A 2 -0.050370 0.403813 0.966768 11.00000 -1.50000 H40B 2 -0.078714 0.282238 0.909759 11.00000 -1.50000 H40C 2 -0.099662 0.448125 0.892263 11.00000 -1.50000 AFIX 0 O1 3 0.488505 0.391368 0.779642 11.00000 0.01609 0.02020 = 0.02860 -0.00442 0.00756 -0.00143 O2 3 0.748271 0.886391 1.017056 11.00000 0.02084 0.01853 = 0.01744 0.00094 0.00450 -0.00044 O3 3 0.413276 0.600320 0.904041 11.00000 0.01778 0.03678 = 0.02800 -0.00687 0.01080 -0.00350 O4 3 0.813914 0.705401 0.885356 11.00000 0.01842 0.04472 = 0.02300 -0.00154 0.00995 -0.00566 O5 3 0.514590 0.096294 0.824033 11.00000 0.01564 0.02507 = 0.02377 0.00274 0.00498 0.00401 O6 3 0.117243 0.275085 0.834836 11.00000 0.01626 0.02555 = 0.02339 0.00498 0.00810 0.00348 HKLF 4 REM TA4-TCNQ_150504 in P21/n #14 REM R1 = 0.0470 for 5352 Fo > 4sig(Fo) and 0.0756 for all 7487 data REM 419 parameters refined using 0 restraints END WGHT 0.0374 1.6566 REM Highest difference peak 0.248, deepest hole -0.224, 1-sigma level 0.045 Q1 1 0.5998 0.6270 0.8330 11.00000 0.05 0.25 Q2 1 0.5425 0.6238 0.8568 11.00000 0.05 0.24 ; _shelx_res_checksum 82768 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 C1 C 0.48737(9) 0.62186(18) 0.91393(9) 0.0205(4) Uani 1 1 d . C2 C 0.53428(9) 0.67438(18) 0.97558(8) 0.0209(4) Uani 1 1 d . H2 H 0.5147 0.6959 1.0126 0.025 Uiso 1 1 calc R C3 C 0.60784(9) 0.69451(18) 0.98236(8) 0.0194(4) Uani 1 1 d . H3 H 0.6390 0.7276 1.0246 0.023 Uiso 1 1 calc R C4 C 0.63865(9) 0.66715(17) 0.92783(8) 0.0181(3) Uani 1 1 d . C5 C 0.59069(9) 0.61458(17) 0.86535(8) 0.0185(3) Uani 1 1 d . C6 C 0.51451(9) 0.58945(17) 0.85933(8) 0.0188(3) Uani 1 1 d . C7 C 0.62132(9) 0.59155(18) 0.81022(8) 0.0211(4) Uani 1 1 d . H7 H 0.5910 0.5536 0.7686 0.025 Uiso 1 1 calc R C8 C 0.69348(9) 0.62274(19) 0.81577(8) 0.0235(4) Uani 1 1 d . H8 H 0.7123 0.6090 0.7777 0.028 Uiso 1 1 calc R C9 C 0.74056(9) 0.67537(19) 0.87767(8) 0.0212(4) Uani 1 1 d . C10 C 0.71482(9) 0.69530(17) 0.93376(8) 0.0184(3) Uani 1 1 d . C11 C 0.46298(9) 0.52993(18) 0.79488(8) 0.0211(4) Uani 1 1 d . H11A H 0.4127 0.5205 0.8005 0.025 Uiso 1 1 calc R H11B H 0.4606 0.5973 0.7567 0.025 Uiso 1 1 calc R C12 C 0.42970(9) 0.29672(18) 0.74569(8) 0.0191(3) Uani 1 1 d . H12A H 0.4479 0.2287 0.7167 0.023 Uiso 1 1 calc R H12B H 0.3893 0.3544 0.7157 0.023 Uiso 1 1 calc R C13 C 0.39952(9) 0.21165(17) 0.79528(8) 0.0171(3) Uani 1 1 d . C14 C 0.44667(9) 0.11070(18) 0.83529(8) 0.0187(3) Uani 1 1 d . C15 C 0.42443(9) 0.02593(18) 0.88333(8) 0.0207(4) Uani 1 1 d . H15 H 0.4575 -0.0426 0.9103 0.025 Uiso 1 1 calc R C16 C 0.35505(9) 0.04259(18) 0.89096(8) 0.0198(4) Uani 1 1 d . H16 H 0.3407 -0.0148 0.9237 0.024 Uiso 1 1 calc R C17 C 0.30407(9) 0.14298(17) 0.85151(8) 0.0168(3) Uani 1 1 d . C18 C 0.32712(9) 0.22921(17) 0.80285(8) 0.0167(3) Uani 1 1 d . C19 C 0.27513(9) 0.33038(18) 0.76482(8) 0.0187(3) Uani 1 1 d . H19 H 0.2887 0.3890 0.7320 0.022 Uiso 1 1 calc R C20 C 0.20632(9) 0.34652(18) 0.77364(8) 0.0200(4) Uani 1 1 d . H20 H 0.1729 0.4150 0.7470 0.024 Uiso 1 1 calc R C21 C 0.18476(9) 0.26124(18) 0.82244(8) 0.0176(3) Uani 1 1 d . C22 C 0.23217(9) 0.16063(17) 0.86096(8) 0.0172(3) Uani 1 1 d . C23 C 0.37888(9) 0.65322(19) 0.95341(9) 0.0220(4) Uani 1 1 d . H23A H 0.3906 0.7567 0.9630 0.026 Uiso 1 1 calc R H23B H 0.3961 0.5983 0.9965 0.026 Uiso 1 1 calc R C24 C 0.29675(9) 0.6327(2) 0.92258(9) 0.0240(4) Uani 1 1 d . H24A H 0.2868 0.5306 0.9086 0.029 Uiso 1 1 calc R H24B H 0.2800 0.6936 0.8813 0.029 Uiso 1 1 calc R C25 C 0.25308(9) 0.6724(2) 0.97235(9) 0.0250(4) Uani 1 1 d . H25A H 0.2635 0.7741 0.9868 0.030 Uiso 1 1 calc R H25B H 0.2694 0.6106 1.0134 0.030 Uiso 1 1 calc R C26 C 0.17034(10) 0.6537(2) 0.94123(10) 0.0336(5) Uani 1 1 d . H26A H 0.1443 0.6804 0.9748 0.050 Uiso 1 1 calc GR H26B H 0.1596 0.5526 0.9277 0.050 Uiso 1 1 calc GR H26C H 0.1538 0.7160 0.9011 0.050 Uiso 1 1 calc GR C27 C 0.76624(9) 0.74236(18) 1.00072(8) 0.0196(4) Uani 1 1 d . H27A H 0.7621 0.6751 1.0371 0.023 Uiso 1 1 calc R H27B H 0.8178 0.7396 0.9980 0.023 Uiso 1 1 calc R C28 C 0.21033(9) 0.07444(18) 0.91517(8) 0.0187(4) Uani 1 1 d . H28A H 0.1571 0.0896 0.9102 0.022 Uiso 1 1 calc R H28B H 0.2179 -0.0296 0.9081 0.022 Uiso 1 1 calc R C29 C 0.83714(10) 0.7318(2) 0.82537(9) 0.0294(4) Uani 1 1 d . H29A H 0.8048 0.8048 0.7962 0.035 Uiso 1 1 calc R H29B H 0.8347 0.6416 0.7988 0.035 Uiso 1 1 calc R C30 C 0.91580(10) 0.7866(2) 0.84860(10) 0.0297(4) Uani 1 1 d . H30A H 0.9465 0.7132 0.8789 0.036 Uiso 1 1 calc R H30B H 0.9347 0.7966 0.8082 0.036 Uiso 1 1 calc R C31 C 0.92513(10) 0.9294(2) 0.88581(10) 0.0316(4) Uani 1 1 d . H31A H 0.9069 0.9203 0.9266 0.038 Uiso 1 1 calc R H31B H 0.8950 1.0038 0.8557 0.038 Uiso 1 1 calc R C32 C 1.00576(10) 0.9778(2) 0.90762(11) 0.0368(5) Uani 1 1 d . H32A H 1.0359 0.9037 0.9369 0.055 Uiso 1 1 calc GR H32B H 1.0099 1.0689 0.9328 0.055 Uiso 1 1 calc GR H32C H 1.0232 0.9918 0.8671 0.055 Uiso 1 1 calc GR C33 C 0.57071(9) 0.0193(2) 0.87400(9) 0.0277(4) Uani 1 1 d . H33A H 0.5590 -0.0851 0.8720 0.033 Uiso 1 1 calc R H33B H 0.5733 0.0551 0.9203 0.033 Uiso 1 1 calc R C34 C 0.64363(9) 0.0436(2) 0.85873(10) 0.0274(4) Uani 1 1 d . H34A H 0.6416 -0.0014 0.8143 0.033 Uiso 1 1 calc R H34B H 0.6831 -0.0055 0.8940 0.033 Uiso 1 1 calc R C35 C 0.66359(9) 0.2019(2) 0.85640(10) 0.0294(4) Uani 1 1 d . H35A H 0.6520 0.2534 0.8946 0.035 Uiso 1 1 calc R H35B H 0.6332 0.2449 0.8133 0.035 Uiso 1 1 calc R C36 C 0.74525(10) 0.2228(3) 0.86117(11) 0.0389(5) Uani 1 1 d . H36A H 0.7755 0.1832 0.9045 0.058 Uiso 1 1 calc GR H36B H 0.7557 0.3261 0.8589 0.058 Uiso 1 1 calc GR H36C H 0.7569 0.1724 0.8233 0.058 Uiso 1 1 calc GR C37 C 0.06519(9) 0.37806(19) 0.79615(9) 0.0219(4) Uani 1 1 d . H37A H 0.0536 0.3561 0.7469 0.026 Uiso 1 1 calc R H37B H 0.0859 0.4770 0.8039 0.026 Uiso 1 1 calc R C38 C -0.00385(9) 0.3668(2) 0.82001(9) 0.0253(4) Uani 1 1 d . H38A H -0.0237 0.2674 0.8113 0.030 Uiso 1 1 calc R H38B H -0.0416 0.4338 0.7927 0.030 Uiso 1 1 calc R C39 C 0.00849(10) 0.4014(2) 0.89509(9) 0.0288(4) Uani 1 1 d . H39A H 0.0259 0.5024 0.9037 0.035 Uiso 1 1 calc R H39B H 0.0477 0.3374 0.9226 0.035 Uiso 1 1 calc R C40 C -0.06130(11) 0.3822(2) 0.91802(11) 0.0392(5) Uani 1 1 d . H40A H -0.0504 0.4038 0.9668 0.059 Uiso 1 1 calc GR H40B H -0.0787 0.2822 0.9098 0.059 Uiso 1 1 calc GR H40C H -0.0997 0.4481 0.8923 0.059 Uiso 1 1 calc GR O1 O 0.48851(6) 0.39137(12) 0.77964(6) 0.0214(3) Uani 1 1 d . O2 O 0.74827(6) 0.88639(12) 1.01706(5) 0.0191(3) Uani 1 1 d . O3 O 0.41328(6) 0.60032(14) 0.90404(6) 0.0266(3) Uani 1 1 d . O4 O 0.81391(6) 0.70540(15) 0.88536(6) 0.0279(3) Uani 1 1 d . O5 O 0.51459(6) 0.09629(13) 0.82403(6) 0.0216(3) Uani 1 1 d . O6 O 0.11724(6) 0.27509(13) 0.83484(6) 0.0212(3) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0172(8) 0.0194(9) 0.0262(9) 0.0020(7) 0.0082(7) -0.0012(7) C2 0.0231(9) 0.0222(9) 0.0201(8) -0.0003(7) 0.0103(7) 0.0015(7) C3 0.0211(9) 0.0193(8) 0.0177(8) 0.0003(7) 0.0052(7) -0.0010(7) C4 0.0198(8) 0.0159(8) 0.0191(8) 0.0029(7) 0.0061(7) 0.0012(7) C5 0.0191(8) 0.0157(8) 0.0214(8) 0.0012(7) 0.0066(7) 0.0005(7) C6 0.0200(8) 0.0158(8) 0.0207(8) 0.0024(7) 0.0060(7) 0.0006(7) C7 0.0226(9) 0.0230(9) 0.0178(8) -0.0014(7) 0.0057(7) -0.0014(7) C8 0.0241(9) 0.0293(10) 0.0200(8) -0.0027(8) 0.0110(7) -0.0017(8) C9 0.0176(8) 0.0237(9) 0.0233(9) 0.0020(7) 0.0076(7) -0.0008(7) C10 0.0185(8) 0.0166(8) 0.0206(8) 0.0014(7) 0.0061(7) 0.0007(7) C11 0.0211(9) 0.0189(9) 0.0230(9) -0.0008(7) 0.0058(7) 0.0012(7) C12 0.0161(8) 0.0219(9) 0.0189(8) -0.0039(7) 0.0044(7) -0.0014(7) C13 0.0180(8) 0.0173(8) 0.0159(8) -0.0036(7) 0.0045(7) -0.0016(7) C14 0.0158(8) 0.0200(9) 0.0197(8) -0.0034(7) 0.0037(7) -0.0004(7) C15 0.0200(8) 0.0200(9) 0.0204(8) 0.0009(7) 0.0027(7) 0.0027(7) C16 0.0236(9) 0.0176(8) 0.0186(8) 0.0013(7) 0.0067(7) -0.0010(7) C17 0.0191(8) 0.0154(8) 0.0155(8) -0.0030(6) 0.0039(6) -0.0013(6) C18 0.0182(8) 0.0176(8) 0.0136(7) -0.0030(6) 0.0034(6) -0.0018(6) C19 0.0214(8) 0.0207(9) 0.0145(8) 0.0018(7) 0.0056(7) -0.0013(7) C20 0.0174(8) 0.0225(9) 0.0193(8) 0.0026(7) 0.0037(7) 0.0023(7) C21 0.0164(8) 0.0204(9) 0.0165(8) -0.0033(7) 0.0052(7) -0.0020(7) C22 0.0191(8) 0.0164(8) 0.0162(8) -0.0017(7) 0.0050(7) -0.0029(7) C23 0.0203(9) 0.0229(9) 0.0261(9) -0.0007(7) 0.0118(7) 0.0000(7) C24 0.0199(9) 0.0272(10) 0.0257(9) 0.0022(8) 0.0079(7) -0.0005(7) C25 0.0209(9) 0.0272(10) 0.0285(9) 0.0054(8) 0.0093(8) 0.0015(7) C26 0.0221(9) 0.0418(12) 0.0384(11) 0.0049(9) 0.0108(8) -0.0006(9) C27 0.0185(8) 0.0212(9) 0.0196(8) 0.0010(7) 0.0065(7) 0.0015(7) C28 0.0177(8) 0.0202(9) 0.0183(8) 0.0003(7) 0.0049(7) -0.0041(7) C29 0.0267(10) 0.0404(11) 0.0253(9) -0.0030(9) 0.0139(8) -0.0058(8) C30 0.0230(9) 0.0395(11) 0.0302(10) 0.0002(9) 0.0130(8) -0.0025(8) C31 0.0253(10) 0.0343(11) 0.0377(11) -0.0002(9) 0.0127(8) -0.0018(8) C32 0.0265(10) 0.0366(12) 0.0474(12) -0.0011(10) 0.0103(9) -0.0061(9) C33 0.0202(9) 0.0294(10) 0.0312(10) 0.0082(8) 0.0036(8) 0.0062(8) C34 0.0194(9) 0.0308(10) 0.0310(10) 0.0023(8) 0.0051(8) 0.0071(8) C35 0.0207(9) 0.0386(11) 0.0288(10) 0.0000(9) 0.0068(8) 0.0011(8) C36 0.0237(10) 0.0552(14) 0.0400(12) 0.0006(11) 0.0123(9) -0.0014(9) C37 0.0183(8) 0.0229(9) 0.0244(9) 0.0039(7) 0.0057(7) 0.0030(7) C38 0.0177(8) 0.0283(10) 0.0294(9) 0.0019(8) 0.0060(7) 0.0025(7) C39 0.0230(9) 0.0312(10) 0.0357(10) -0.0042(9) 0.0141(8) -0.0040(8) C40 0.0320(11) 0.0425(13) 0.0504(13) -0.0068(11) 0.0235(10) -0.0052(9) O1 0.0161(6) 0.0202(6) 0.0286(6) -0.0044(5) 0.0076(5) -0.0014(5) O2 0.0208(6) 0.0185(6) 0.0174(6) 0.0009(5) 0.0045(5) -0.0004(5) O3 0.0178(6) 0.0368(7) 0.0280(6) -0.0069(6) 0.0108(5) -0.0035(5) O4 0.0184(6) 0.0447(8) 0.0230(6) -0.0015(6) 0.0100(5) -0.0057(6) O5 0.0156(6) 0.0251(6) 0.0238(6) 0.0027(5) 0.0050(5) 0.0040(5) O6 0.0163(6) 0.0255(7) 0.0234(6) 0.0050(5) 0.0081(5) 0.0035(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 3 13 3 0.0590 3.0000 13.0000 3.0000 -0.6436 0.7817 0.0022 8 -12 -8 0.0697 8.0000 -12.0000 -8.0000 0.5990 -0.6733 0.4064 -16 -10 3 0.0846 -16.0000 -10.0000 3.0000 0.5301 -0.6375 -0.5160 -25 5 11 0.1328 -25.0000 5.0000 11.0000 -0.1717 0.2369 -0.9805 26 -1 -11 0.1443 26.0000 -1.0000 -11.0000 0.0009 0.0205 0.9873 12 -2 20 0.0426 12.0000 -2.0000 20.0000 -0.7093 -0.5614 0.3738 -10 2 -22 0.0394 -10.0000 2.0000 -22.0000 0.7418 0.5896 -0.2942 -10 -1 29 0.0975 -10.0000 -1.0000 29.0000 -0.7066 -0.5629 -0.4616 4 8 -23 0.0932 4.0000 8.0000 -23.0000 0.3356 0.9368 0.1714 -6 -7 -21 0.0576 -6.0000 -7.0000 -21.0000 1.0051 -0.0373 -0.0876 -15 -6 -15 0.0667 -15.0000 -6.0000 -15.0000 0.9119 -0.0427 -0.4423 4 -7 -24 0.0903 4.0000 -7.0000 -24.0000 0.9526 -0.0273 0.2848 7 2 24 0.0482 7.0000 2.0000 24.0000 -0.9162 -0.3511 0.1491 15 1 18 0.0557 15.0000 1.0000 18.0000 -0.8086 -0.3412 0.4677 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 C6 C1 C2 120.99(15) . O3 C1 C2 122.87(14) . O3 C1 C6 116.14(15) . C1 C2 H2 119.9 . C3 C2 C1 120.26(15) . C3 C2 H2 119.9 . C2 C3 H3 119.2 . C2 C3 C4 121.52(15) . C4 C3 H3 119.2 . C3 C4 C5 117.90(14) . C3 C4 C10 121.53(15) . C5 C4 C10 120.54(14) . C6 C5 C4 120.28(14) . C7 C5 C4 117.70(14) . C7 C5 C6 122.01(15) . C1 C6 C5 119.00(15) . C1 C6 C11 119.41(14) . C5 C6 C11 121.59(14) . C5 C7 H7 119.4 . C8 C7 C5 121.29(15) . C8 C7 H7 119.4 . C7 C8 H8 119.7 . C7 C8 C9 120.69(15) . C9 C8 H8 119.7 . C10 C9 C8 120.81(15) . C10 C9 O4 117.01(15) . O4 C9 C8 122.16(14) . C4 C10 C27 120.47(14) . C9 C10 C4 118.91(15) . C9 C10 C27 120.60(14) . C6 C11 H11A 109.6 . C6 C11 H11B 109.6 . H11A C11 H11B 108.2 . O1 C11 C6 110.07(13) . O1 C11 H11A 109.6 . O1 C11 H11B 109.6 . H12A C12 H12B 107.9 . C13 C12 H12A 109.2 . C13 C12 H12B 109.2 . O1 C12 H12A 109.2 . O1 C12 H12B 109.2 . O1 C12 C13 112.23(13) . C14 C13 C12 116.48(14) . C14 C13 C18 119.24(14) . C18 C13 C12 124.28(14) . C13 C14 C15 121.28(15) . O5 C14 C13 116.24(14) . O5 C14 C15 122.46(14) . C14 C15 H15 120.1 . C16 C15 C14 119.75(15) . C16 C15 H15 120.1 . C15 C16 H16 119.1 . C15 C16 C17 121.86(15) . C17 C16 H16 119.1 . C16 C17 C18 118.12(14) . C16 C17 C22 121.09(14) . C22 C17 C18 120.77(14) . C13 C18 C17 119.75(14) . C19 C18 C13 123.48(14) . C19 C18 C17 116.77(14) . C18 C19 H19 118.8 . C20 C19 C18 122.38(15) . C20 C19 H19 118.8 . C19 C20 H20 120.0 . C19 C20 C21 120.05(15) . C21 C20 H20 120.0 . C22 C21 C20 120.75(15) . O6 C21 C20 122.74(14) . O6 C21 C22 116.49(14) . C17 C22 C28 120.01(14) . C21 C22 C17 119.28(14) . C21 C22 C28 120.65(14) . H23A C23 H23B 108.7 . C24 C23 H23A 110.5 . C24 C23 H23B 110.5 . O3 C23 H23A 110.5 . O3 C23 H23B 110.5 . O3 C23 C24 106.03(13) . C23 C24 H24A 109.2 . C23 C24 H24B 109.2 . C23 C24 C25 111.92(14) . H24A C24 H24B 107.9 . C25 C24 H24A 109.2 . C25 C24 H24B 109.2 . C24 C25 H25A 109.2 . C24 C25 H25B 109.2 . C24 C25 C26 112.08(15) . H25A C25 H25B 107.9 . C26 C25 H25A 109.2 . C26 C25 H25B 109.2 . C25 C26 H26A 109.5 . C25 C26 H26B 109.5 . C25 C26 H26C 109.5 . H26A C26 H26B 109.5 . H26A C26 H26C 109.5 . H26B C26 H26C 109.5 . C10 C27 H27A 109.6 . C10 C27 H27B 109.6 . H27A C27 H27B 108.1 . O2 C27 C10 110.23(13) . O2 C27 H27A 109.6 . O2 C27 H27B 109.6 . C22 C28 H28A 109.0 . C22 C28 H28B 109.0 . H28A C28 H28B 107.8 . O2 C28 C22 112.84(13) 3_667 O2 C28 H28A 109.0 3_667 O2 C28 H28B 109.0 3_667 H29A C29 H29B 108.5 . C30 C29 H29A 110.3 . C30 C29 H29B 110.3 . O4 C29 H29A 110.3 . O4 C29 H29B 110.3 . O4 C29 C30 107.16(14) . C29 C30 H30A 108.6 . C29 C30 H30B 108.6 . H30A C30 H30B 107.6 . C31 C30 C29 114.67(15) . C31 C30 H30A 108.6 . C31 C30 H30B 108.6 . C30 C31 H31A 109.3 . C30 C31 H31B 109.3 . C30 C31 C32 111.73(16) . H31A C31 H31B 107.9 . C32 C31 H31A 109.3 . C32 C31 H31B 109.3 . C31 C32 H32A 109.5 . C31 C32 H32B 109.5 . C31 C32 H32C 109.5 . H32A C32 H32B 109.5 . H32A C32 H32C 109.5 . H32B C32 H32C 109.5 . H33A C33 H33B 108.4 . C34 C33 H33A 110.1 . C34 C33 H33B 110.1 . O5 C33 H33A 110.1 . O5 C33 H33B 110.1 . O5 C33 C34 108.19(14) . C33 C34 H34A 108.9 . C33 C34 H34B 108.9 . C33 C34 C35 113.48(15) . H34A C34 H34B 107.7 . C35 C34 H34A 108.9 . C35 C34 H34B 108.9 . C34 C35 H35A 109.2 . C34 C35 H35B 109.2 . C34 C35 C36 112.01(16) . H35A C35 H35B 107.9 . C36 C35 H35A 109.2 . C36 C35 H35B 109.2 . C35 C36 H36A 109.5 . C35 C36 H36B 109.5 . C35 C36 H36C 109.5 . H36A C36 H36B 109.5 . H36A C36 H36C 109.5 . H36B C36 H36C 109.5 . H37A C37 H37B 108.6 . C38 C37 H37A 110.3 . C38 C37 H37B 110.3 . O6 C37 H37A 110.3 . O6 C37 H37B 110.3 . O6 C37 C38 107.07(13) . C37 C38 H38A 108.8 . C37 C38 H38B 108.8 . C37 C38 C39 113.98(14) . H38A C38 H38B 107.7 . C39 C38 H38A 108.8 . C39 C38 H38B 108.8 . C38 C39 H39A 109.1 . C38 C39 H39B 109.1 . C38 C39 C40 112.51(15) . H39A C39 H39B 107.8 . C40 C39 H39A 109.1 . C40 C39 H39B 109.1 . C39 C40 H40A 109.5 . C39 C40 H40B 109.5 . C39 C40 H40C 109.5 . H40A C40 H40B 109.5 . H40A C40 H40C 109.5 . H40B C40 H40C 109.5 . C12 O1 C11 113.01(12) . C28 O2 C27 111.01(12) 3_667 C1 O3 C23 119.40(13) . C9 O4 C29 118.27(13) . C14 O5 C33 117.82(13) . C21 O6 C37 119.16(12) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C2 1.409(2) . C1 C6 1.383(2) . C1 O3 1.3690(19) . C2 H2 0.9500 . C2 C3 1.367(2) . C3 H3 0.9500 . C3 C4 1.415(2) . C4 C5 1.429(2) . C4 C10 1.431(2) . C5 C6 1.426(2) . C5 C7 1.418(2) . C6 C11 1.506(2) . C7 H7 0.9500 . C7 C8 1.364(2) . C8 H8 0.9500 . C8 C9 1.414(2) . C9 C10 1.376(2) . C9 O4 1.3759(19) . C10 C27 1.504(2) . C11 H11A 0.9900 . C11 H11B 0.9900 . C11 O1 1.4337(19) . C12 H12A 0.9900 . C12 H12B 0.9900 . C12 C13 1.514(2) . C12 O1 1.4313(19) . C13 C14 1.388(2) . C13 C18 1.425(2) . C14 C15 1.408(2) . C14 O5 1.3688(19) . C15 H15 0.9500 . C15 C16 1.368(2) . C16 H16 0.9500 . C16 C17 1.416(2) . C17 C18 1.433(2) . C17 C22 1.431(2) . C18 C19 1.420(2) . C19 H19 0.9500 . C19 C20 1.367(2) . C20 H20 0.9500 . C20 C21 1.417(2) . C21 C22 1.376(2) . C21 O6 1.3710(18) . C22 C28 1.512(2) . C23 H23A 0.9900 . C23 H23B 0.9900 . C23 C24 1.512(2) . C23 O3 1.4290(19) . C24 H24A 0.9900 . C24 H24B 0.9900 . C24 C25 1.521(2) . C25 H25A 0.9900 . C25 H25B 0.9900 . C25 C26 1.521(2) . C26 H26A 0.9800 . C26 H26B 0.9800 . C26 H26C 0.9800 . C27 H27A 0.9900 . C27 H27B 0.9900 . C27 O2 1.4370(19) . C28 H28A 0.9900 . C28 H28B 0.9900 . C28 O2 1.4340(19) 3_667 C29 H29A 0.9900 . C29 H29B 0.9900 . C29 C30 1.513(2) . C29 O4 1.433(2) . C30 H30A 0.9900 . C30 H30B 0.9900 . C30 C31 1.511(3) . C31 H31A 0.9900 . C31 H31B 0.9900 . C31 C32 1.527(3) . C32 H32A 0.9800 . C32 H32B 0.9800 . C32 H32C 0.9800 . C33 H33A 0.9900 . C33 H33B 0.9900 . C33 C34 1.509(2) . C33 O5 1.438(2) . C34 H34A 0.9900 . C34 H34B 0.9900 . C34 C35 1.516(3) . C35 H35A 0.9900 . C35 H35B 0.9900 . C35 C36 1.527(2) . C36 H36A 0.9800 . C36 H36B 0.9800 . C36 H36C 0.9800 . C37 H37A 0.9900 . C37 H37B 0.9900 . C37 C38 1.515(2) . C37 O6 1.4365(19) . C38 H38A 0.9900 . C38 H38B 0.9900 . C38 C39 1.520(2) . C39 H39A 0.9900 . C39 H39B 0.9900 . C39 C40 1.525(2) . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . O2 C28 1.4340(19) 3_667 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_4 C1 C2 C3 C4 1.6(3) . C1 C6 C11 O1 -121.07(16) . C2 C1 C6 C5 -2.1(2) . C2 C1 C6 C11 178.44(15) . C2 C1 O3 C23 10.0(2) . C2 C3 C4 C5 -1.3(2) . C2 C3 C4 C10 176.71(16) . C3 C4 C5 C6 -0.7(2) . C3 C4 C5 C7 178.11(15) . C3 C4 C10 C9 -175.87(16) . C3 C4 C10 C27 5.6(2) . C4 C5 C6 C1 2.4(2) . C4 C5 C6 C11 -178.17(15) . C4 C5 C7 C8 -2.0(2) . C4 C10 C27 O2 -69.53(19) . C5 C4 C10 C9 2.1(2) . C5 C4 C10 C27 -176.43(15) . C5 C6 C11 O1 59.5(2) . C5 C7 C8 C9 1.8(3) . C6 C1 C2 C3 0.1(3) . C6 C1 O3 C23 -169.74(14) . C6 C5 C7 C8 176.78(16) . C6 C11 O1 C12 148.51(13) . C7 C5 C6 C1 -176.39(15) . C7 C5 C6 C11 3.0(2) . C7 C8 C9 C10 0.5(3) . C7 C8 C9 O4 178.80(16) . C8 C9 C10 C4 -2.4(2) . C8 C9 C10 C27 176.13(16) . C8 C9 O4 C29 21.6(2) . C9 C10 C27 O2 111.99(17) . C10 C4 C5 C6 -178.75(15) . C10 C4 C5 C7 0.1(2) . C10 C9 O4 C29 -160.00(16) . C10 C27 O2 C28 171.89(12) 3_667 C12 C13 C14 C15 179.76(15) . C12 C13 C14 O5 -1.8(2) . C12 C13 C18 C17 -179.95(14) . C12 C13 C18 C19 -0.7(2) . C13 C12 O1 C11 -87.33(16) . C13 C14 C15 C16 0.1(2) . C13 C14 O5 C33 165.85(15) . C13 C18 C19 C20 -179.12(16) . C14 C13 C18 C17 0.1(2) . C14 C13 C18 C19 179.39(15) . C14 C15 C16 C17 0.3(2) . C15 C14 O5 C33 -15.8(2) . C15 C16 C17 C18 -0.5(2) . C15 C16 C17 C22 -178.97(15) . C16 C17 C18 C13 0.3(2) . C16 C17 C18 C19 -179.08(14) . C16 C17 C22 C21 178.82(15) . C16 C17 C22 C28 1.8(2) . C17 C18 C19 C20 0.2(2) . C17 C22 C28 O2 66.66(19) 3_667 C18 C13 C14 C15 -0.3(2) . C18 C13 C14 O5 178.13(14) . C18 C17 C22 C21 0.3(2) . C18 C17 C22 C28 -176.69(14) . C18 C19 C20 C21 0.4(2) . C19 C20 C21 C22 -0.6(2) . C19 C20 C21 O6 178.28(15) . C20 C21 C22 C17 0.2(2) . C20 C21 C22 C28 177.27(15) . C20 C21 O6 C37 1.2(2) . C21 C22 C28 O2 -110.35(17) 3_667 C22 C17 C18 C13 178.78(14) . C22 C17 C18 C19 -0.6(2) . C22 C21 O6 C37 -179.84(14) . C23 C24 C25 C26 179.30(16) . C24 C23 O3 C1 171.57(14) . C29 C30 C31 C32 -179.97(16) . C30 C29 O4 C9 170.44(15) . C33 C34 C35 C36 163.76(16) . C34 C33 O5 C14 -168.47(14) . C37 C38 C39 C40 -177.35(16) . C38 C37 O6 C21 178.97(13) . O1 C12 C13 C14 -66.91(19) . O1 C12 C13 C18 113.13(16) . O3 C1 C2 C3 -179.63(16) . O3 C1 C6 C5 177.67(14) . O3 C1 C6 C11 -1.8(2) . O3 C23 C24 C25 174.95(14) . O4 C9 C10 C4 179.21(15) . O4 C9 C10 C27 -2.3(2) . O4 C29 C30 C31 -63.8(2) . O5 C14 C15 C16 -178.22(15) . O5 C33 C34 C35 56.2(2) . O6 C21 C22 C17 -178.72(14) . O6 C21 C22 C28 -1.7(2) . O6 C37 C38 C39 60.95(19) .