#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:43:34 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252628 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240608.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_7240608 loop_ _publ_author_name 'Prohens, Rafel' 'Barbas, Rafael' 'Bofill, Lidia' 'de Sande, Dafne' 'Font-Bardia, Merce' _publ_section_title ; Crystal Engineering of Nutraceutical Phytosterols: New Cocrystal Solid-Solutions ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00704H _journal_year 2020 _chemical_absolute_configuration rm _chemical_formula_moiety '2(C29 H50 O), C6 H7 O5, H2 O' _chemical_formula_sum 'C64 H109 O8' _chemical_formula_weight 1006.51 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2020-05-29 deposited with the CCDC. 2020-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.948(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 77.42(2) _cell_length_b 7.6086(18) _cell_length_c 9.924(3) _cell_measurement_reflns_used 2187 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 18.85 _cell_measurement_theta_min 2.57 _cell_volume 5845(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.3422 _diffrn_reflns_av_unetI/netI 0.2313 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 82 _diffrn_reflns_limit_h_min -82 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 38307 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 22.238 _diffrn_reflns_theta_max 22.238 _diffrn_reflns_theta_min 2.127 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_T_max 0.7447 _exptl_absorpt_correction_T_min 0.4684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.144 _exptl_crystal_description prism _exptl_crystal_F_000 2228 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.268 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.054 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack -0.13(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 638 _refine_ls_number_reflns 7367 _refine_ls_number_restraints 41 _refine_ls_restrained_S_all 0.904 _refine_ls_R_factor_all 0.1580 _refine_ls_R_factor_gt 0.0602 _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^)+(0.0139P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.1154 _reflns_Friedel_coverage 0.832 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 3517 _reflns_number_total 7367 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00704h2.cif _cod_data_source_block mo_023TB174_0ma_a1a _cod_original_sg_symbol_H-M 'C 2' _cod_database_code 7240608 _shelx_shelxl_version_number 2018/1 _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 mo_023TB174_0ma_a.res in P1 New: C2 mo_023TB174_0ma_a1a.res created by SHELXL-2018/1 at 20:18:42 on 27-Apr-2020 CELL 0.71073 77.4200 7.6086 9.9240 90.000 90.948 90.000 ZERR 4 0.0200 0.0018 0.0030 0.000 0.007 0.000 LATT -7 SYMM - X , Y , - Z SFAC C H O UNIT 256 436 32 MERG 0 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 10 FMAP 2 PLAN 20 ACTA BOND $H CONF OMIT 2 0 1 TWIN DFIX 1.5 0.01 c22a c23a c22a c24a DFIX 1.5 0.01 c19a c20a DFIX 1.5 0.01 c20a c21a DFIX 1.5 0.01 c21a c22a DFIX 1.5 0.01 c21a c25a DFIX 1.5 0.01 c25a c26a DFIX 2.4 0.01 c23a c21a DFIX 2.5 0.01 c24a c21a DFIX 2.4 0.01 c23a c24a DFIX 2.5 0.01 c19a c21a DFIX 2.5 0.01 c20a c22a DFIX 2.4 0.01 c21a c26a DFIX 2.5 0.01 c22a c25a DFIX 2.5 0.01 c25a c22a WGHT 0.013900 BASF -0.12522 FVAR 3.18198 O1A 3 0.782275 0.545284 0.320218 11.00000 0.03655 0.03144 = 0.03116 -0.00448 0.00097 0.00632 AFIX 83 H1OA 2 0.774847 0.554154 0.377769 11.00000 -1.20000 AFIX 0 C1A 1 0.799158 0.535249 0.384982 11.00000 0.03199 0.02301 = 0.01789 -0.00656 -0.00330 -0.01721 AFIX 13 H1A 2 0.797821 0.565068 0.480309 11.00000 -1.20000 AFIX 0 C2A 1 0.805536 0.347858 0.377283 11.00000 0.05165 0.01719 = 0.02015 0.00150 0.00379 0.00109 AFIX 23 H2AA 2 0.797577 0.271061 0.423509 11.00000 -1.20000 H2AB 2 0.805924 0.311363 0.283729 11.00000 -1.20000 AFIX 0 C3A 1 0.822963 0.331620 0.439632 11.00000 0.02472 0.04042 = 0.03508 0.00454 -0.00393 0.00584 AFIX 23 H3AA 2 0.827195 0.213828 0.422623 11.00000 -1.20000 H3AB 2 0.821881 0.344195 0.536392 11.00000 -1.20000 AFIX 0 C4A 1 0.836687 0.464013 0.391529 11.00000 0.02698 0.01000 = 0.01216 0.00018 0.00183 -0.00230 C5A 1 0.829799 0.643938 0.389959 11.00000 0.04663 0.02324 = 0.01367 -0.00300 0.01173 0.00124 C6A 1 0.811607 0.663292 0.325790 11.00000 0.02913 0.02996 = 0.03300 -0.00525 -0.00007 0.00355 AFIX 23 H6AA 2 0.807450 0.781997 0.340076 11.00000 -1.20000 H6AB 2 0.812246 0.643833 0.229403 11.00000 -1.20000 AFIX 0 C7A 1 0.838429 0.783675 0.426472 11.00000 0.03715 0.02225 = 0.02929 0.00038 -0.00225 -0.00025 AFIX 43 H7A 2 0.833203 0.892912 0.415503 11.00000 -1.20000 AFIX 0 C8A 1 0.856273 0.776647 0.484959 11.00000 0.04993 0.04139 = 0.02884 -0.00032 0.00505 0.00550 AFIX 23 H8AA 2 0.855770 0.797424 0.581251 11.00000 -1.20000 H8AB 2 0.863100 0.869992 0.445886 11.00000 -1.20000 AFIX 0 EADP c9a c10a C9A 1 0.865233 0.600623 0.460347 11.00000 0.03554 0.01651 = 0.01188 -0.00033 0.00340 -0.00226 AFIX 13 H9A 2 0.868787 0.596664 0.366074 11.00000 -1.20000 AFIX 0 C10A 1 0.853273 0.449169 0.484804 11.00000 0.03554 0.01651 = 0.01188 -0.00033 0.00340 -0.00226 AFIX 13 H10A 2 0.849225 0.463878 0.577165 11.00000 -1.20000 AFIX 0 C14A 1 0.881459 0.580043 0.550874 11.00000 0.04833 0.07383 = 0.01847 -0.00665 -0.00103 -0.00585 AFIX 13 H14A 2 0.877289 0.581834 0.643565 11.00000 -1.20000 AFIX 0 C13A 1 0.891052 0.407828 0.536881 11.00000 0.03647 0.03898 = 0.02516 0.00208 -0.00076 0.00234 C12A 1 0.878998 0.264210 0.568520 11.00000 0.04536 0.10332 = 0.03945 0.00075 -0.00478 -0.00427 AFIX 23 H12A 2 0.876062 0.271564 0.662995 11.00000 -1.20000 H12B 2 0.884784 0.152745 0.554657 11.00000 -1.20000 AFIX 0 C11A 1 0.861779 0.267333 0.480821 11.00000 0.03813 0.03551 = 0.03693 -0.00792 -0.00664 0.00049 AFIX 23 H11A 2 0.864356 0.237206 0.388330 11.00000 -1.20000 H11B 2 0.853822 0.180118 0.514860 11.00000 -1.20000 AFIX 0 C15A 1 0.895368 0.723095 0.545076 11.00000 0.04545 0.06715 = 0.03845 -0.00722 -0.00803 -0.00435 AFIX 23 H15A 2 0.897876 0.754519 0.452716 11.00000 -1.20000 H15B 2 0.891883 0.827623 0.593539 11.00000 -1.20000 AFIX 0 C16A 1 0.910724 0.635694 0.613128 11.00000 0.04114 0.05235 = 0.03955 -0.00810 -0.00577 0.00493 AFIX 23 H16A 2 0.920802 0.647992 0.557118 11.00000 -1.20000 H16B 2 0.913175 0.692697 0.698757 11.00000 -1.20000 AFIX 0 C17A 1 0.907145 0.448350 0.635541 11.00000 0.05118 0.06183 = 0.01706 -0.01305 -0.00152 -0.00118 AFIX 13 H17A 2 0.902865 0.438408 0.727611 11.00000 -1.20000 AFIX 0 C18A 1 0.922583 0.327003 0.627190 11.00000 0.03115 0.11132 = 0.03696 0.00258 -0.00064 0.00247 AFIX 13 H18A 2 0.927526 0.339968 0.537460 11.00000 -1.20000 AFIX 0 C19A 1 0.936595 0.390736 0.734977 11.00000 0.04717 0.11360 = 0.03793 0.00474 -0.00518 -0.01546 AFIX 23 H19A 2 0.937940 0.517160 0.728174 11.00000 -1.20000 H19B 2 0.932573 0.364110 0.824752 11.00000 -1.20000 AFIX 0 C20A 1 0.953856 0.303873 0.714808 11.00000 0.05889 0.18284 = 0.08423 -0.02656 -0.00015 0.02419 AFIX 23 H20A 2 0.957041 0.316776 0.621206 11.00000 -1.20000 H20B 2 0.952753 0.179207 0.733218 11.00000 -1.20000 AFIX 0 DELU 0.001 c21a c25a DELU 0.001 c22a c21a DELU 0.001 c22a c24a DELU 0.001 c22a c23a C21A 1 0.968502 0.380076 0.805384 11.00000 0.07334 0.21950 = 0.06159 -0.01018 -0.01839 -0.00250 AFIX 13 H21A 2 0.964151 0.406341 0.895344 11.00000 -1.20000 AFIX 0 DELU 0.001 c22b c23b DELU 0.001 c22b c24b DELU 0.001 c22b c21b EADP c23a c24a C22A 1 0.974519 0.548614 0.736948 11.00000 0.12292 0.27302 = 0.27474 0.07641 -0.03051 -0.04716 AFIX 13 H22A 2 0.964817 0.605725 0.689783 11.00000 -1.20000 AFIX 0 C23A 1 0.981870 0.665988 0.839255 11.00000 0.27462 0.66857 = 0.37641 -0.18689 0.07541 -0.15751 AFIX 33 H23A 2 0.973099 0.697777 0.902014 11.00000 -1.50000 H23B 2 0.991146 0.607321 0.886272 11.00000 -1.50000 H23C 2 0.986198 0.770016 0.796723 11.00000 -1.50000 AFIX 0 C24A 1 0.988485 0.498337 0.637384 11.00000 0.27462 0.66857 = 0.37641 -0.18689 0.07541 -0.15751 AFIX 33 H24A 2 0.983676 0.421175 0.570049 11.00000 -1.50000 H24B 2 0.992810 0.602446 0.594949 11.00000 -1.50000 H24C 2 0.997758 0.439750 0.684498 11.00000 -1.50000 AFIX 0 C25A 1 0.984031 0.254269 0.815766 11.00000 0.15722 0.13006 = 0.64778 0.04974 -0.20334 -0.00430 AFIX 23 H25A 2 0.985824 0.193606 0.731174 11.00000 -1.20000 H25B 2 0.994505 0.316856 0.841119 11.00000 -1.20000 AFIX 0 C26A 1 0.978776 0.127321 0.925108 11.00000 0.31176 0.19410 = 0.68568 0.11156 -0.13317 -0.10127 AFIX 137 H26A 2 0.986752 0.136018 0.999912 11.00000 -1.50000 H26B 2 0.978883 0.009614 0.890295 11.00000 -1.50000 H26C 2 0.967360 0.155808 0.954474 11.00000 -1.50000 AFIX 0 C27A 1 0.918548 0.144080 0.646807 11.00000 0.05722 0.08501 = 0.08580 0.01718 -0.00250 -0.00817 AFIX 33 H27A 2 0.928902 0.075418 0.640173 11.00000 -1.20000 H27B 2 0.913692 0.128158 0.734351 11.00000 -1.20000 H27C 2 0.910360 0.106746 0.578973 11.00000 -1.20000 AFIX 0 C28A 1 0.898134 0.388236 0.388170 11.00000 0.05012 0.06733 = 0.01813 -0.00428 0.00048 -0.00958 AFIX 137 H28A 2 0.904157 0.278532 0.380212 11.00000 -1.50000 H28B 2 0.905892 0.483334 0.369669 11.00000 -1.50000 H28C 2 0.888631 0.391011 0.324833 11.00000 -1.50000 AFIX 0 C29A 1 0.841234 0.408046 0.245342 11.00000 0.03737 0.06701 = 0.02310 -0.00648 0.00546 -0.00072 AFIX 137 H29A 2 0.844405 0.286077 0.244580 11.00000 -1.50000 H29B 2 0.850721 0.477610 0.214369 11.00000 -1.50000 H29C 2 0.831377 0.425962 0.186992 11.00000 -1.50000 AFIX 0 DFIX 1.5 0.01 c22b c23b c22b c24b DFIX 1.5 0.01 c19b c20b DFIX 1.5 0.01 c20b c21b DFIX 1.5 0.01 c21b c22b DFIX 1.5 0.01 c21b c25b DFIX 1.5 0.01 c25b c26b DFIX 2.4 0.01 c23b c21b DFIX 2.5 0.01 c24b c21b DFIX 2.4 0.01 c23b c24b DFIX 2.5 0.01 c19b c21b DFIX 2.5 0.01 c20b c22b DFIX 2.4 0.01 c21b c26b DFIX 2.5 0.01 c22b c25b DFIX 2.5 0.01 c25b c22b O1B 3 0.777817 1.023101 -0.261843 11.00000 0.02563 0.02593 = 0.00995 -0.00093 -0.00190 0.00171 AFIX 83 H1OB 2 0.774875 1.066652 -0.190209 11.00000 -1.20000 AFIX 0 C1B 1 0.796217 0.999642 -0.260723 11.00000 0.03465 0.03520 = 0.01603 -0.00513 0.00769 0.00751 AFIX 13 H1B 2 0.799663 0.973549 -0.353172 11.00000 -1.20000 AFIX 0 C2B 1 0.805649 1.158959 -0.216493 11.00000 0.03018 0.01477 = 0.02142 0.00246 0.00264 -0.00605 AFIX 23 H2BA 2 0.801331 1.197078 -0.130072 11.00000 -1.20000 H2BB 2 0.803596 1.252679 -0.281057 11.00000 -1.20000 AFIX 0 C3B 1 0.824903 1.124298 -0.203952 11.00000 0.02475 0.02848 = 0.03122 0.00158 0.00393 0.00401 AFIX 23 H3BA 2 0.829209 1.091110 -0.291589 11.00000 -1.20000 H3BB 2 0.830679 1.232119 -0.176930 11.00000 -1.20000 AFIX 0 C4B 1 0.829457 0.982132 -0.103980 11.00000 0.02051 0.01908 = 0.01619 -0.00077 0.00622 -0.00048 C5B 1 0.820384 0.816937 -0.149416 11.00000 0.03736 0.01258 = 0.03954 -0.00606 0.00246 -0.00375 C6B 1 0.800969 0.841171 -0.173665 11.00000 0.02800 0.02638 = 0.03420 -0.01387 -0.00015 -0.00373 AFIX 23 H6BA 2 0.796397 0.736082 -0.216561 11.00000 -1.20000 H6BB 2 0.795426 0.853224 -0.087211 11.00000 -1.20000 AFIX 0 C7B 1 0.826800 0.658770 -0.137433 11.00000 0.03627 0.03291 = 0.01584 -0.00069 0.00568 -0.00677 AFIX 43 H7B 2 0.819270 0.563963 -0.145343 11.00000 -1.20000 AFIX 0 C8B 1 0.845426 0.621193 -0.111898 11.00000 0.02439 0.03459 = 0.02075 0.00248 -0.00058 -0.00757 AFIX 23 H8BA 2 0.850963 0.594679 -0.196480 11.00000 -1.20000 H8BB 2 0.846568 0.519120 -0.053871 11.00000 -1.20000 AFIX 0 EADP c9b c10b C9B 1 0.854473 0.779879 -0.044609 11.00000 0.03054 0.00582 = 0.01888 -0.00169 0.00206 0.00349 AFIX 13 H9B 2 0.850908 0.783293 0.049651 11.00000 -1.20000 AFIX 0 C10B 1 0.849566 0.952732 -0.107653 11.00000 0.03054 0.00582 = 0.01888 -0.00169 0.00206 0.00349 AFIX 13 H10B 2 0.852693 0.945923 -0.202797 11.00000 -1.20000 AFIX 0 C11B 1 0.860009 1.102966 -0.045769 11.00000 0.02586 0.02796 = 0.03218 0.00171 -0.00945 -0.00475 AFIX 23 H11C 2 0.856437 1.120350 0.046505 11.00000 -1.20000 H11D 2 0.857482 1.210106 -0.095268 11.00000 -1.20000 AFIX 0 C12B 1 0.879740 1.069563 -0.046795 11.00000 0.02453 0.04918 = 0.02668 -0.00287 0.00994 0.00085 AFIX 23 H12C 2 0.883574 1.065273 -0.139297 11.00000 -1.20000 H12D 2 0.885637 1.166508 -0.002288 11.00000 -1.20000 AFIX 0 C13B 1 0.884360 0.907778 0.019966 11.00000 0.01793 0.01066 = 0.02901 -0.00583 0.00018 -0.00407 C14B 1 0.873926 0.755827 -0.045030 11.00000 0.02720 0.05503 = 0.01829 -0.00566 0.00371 0.00566 AFIX 13 H14B 2 0.876817 0.762542 -0.140659 11.00000 -1.20000 AFIX 0 C15B 1 0.882408 0.583183 0.002653 11.00000 0.05773 0.07197 = 0.03342 0.00819 -0.00266 0.00552 AFIX 23 H15C 2 0.881216 0.491397 -0.064694 11.00000 -1.20000 H15D 2 0.877599 0.542768 0.086804 11.00000 -1.20000 AFIX 0 C16B 1 0.901817 0.642473 0.021482 11.00000 0.03327 0.09669 = 0.02952 0.00100 -0.00367 -0.01925 AFIX 23 H16C 2 0.905970 0.610043 0.110820 11.00000 -1.20000 H16D 2 0.908912 0.583096 -0.044073 11.00000 -1.20000 AFIX 0 C17B 1 0.903249 0.833809 0.003799 11.00000 0.03383 0.03636 = 0.01658 -0.00112 -0.00322 -0.00761 AFIX 13 H17B 2 0.906108 0.851877 -0.091028 11.00000 -1.20000 AFIX 0 C18B 1 0.918179 0.913585 0.085302 11.00000 0.04294 0.04248 = 0.03653 -0.00580 -0.00379 0.00337 AFIX 13 H18B 2 0.916682 0.880694 0.179869 11.00000 -1.20000 AFIX 0 C19B 1 0.935388 0.830481 0.037152 11.00000 0.03140 0.14084 = 0.04266 -0.01065 -0.00725 0.00020 AFIX 23 H19C 2 0.933483 0.706127 0.021316 11.00000 -1.20000 H19D 2 0.938373 0.883376 -0.048293 11.00000 -1.20000 AFIX 0 C20B 1 0.950448 0.850710 0.132898 11.00000 0.05274 0.10177 = 0.09113 0.01525 -0.00393 -0.00522 AFIX 23 H20C 2 0.951151 0.972555 0.161220 11.00000 -1.20000 H20D 2 0.960969 0.823250 0.085506 11.00000 -1.20000 AFIX 0 C21B 1 0.949516 0.734526 0.258000 11.00000 0.10578 0.15776 = 0.06478 -0.02761 0.01510 0.05170 AFIX 13 H21B 2 0.937407 0.718940 0.282649 11.00000 -1.20000 AFIX 0 C22B 1 0.959519 0.798558 0.376608 11.00000 0.18107 0.27415 = 0.07844 -0.04307 -0.00779 0.00990 AFIX 13 H22B 2 0.961382 0.701092 0.439750 11.00000 -1.20000 AFIX 0 C23B 1 0.976284 0.878588 0.344876 11.00000 0.12832 0.37557 = 0.10639 -0.02797 -0.02525 0.03457 AFIX 33 H23D 2 0.981923 0.916460 0.426719 11.00000 -1.20000 H23E 2 0.983390 0.793636 0.300594 11.00000 -1.20000 H23F 2 0.974468 0.977847 0.286625 11.00000 -1.20000 AFIX 0 C24B 1 0.949573 0.944267 0.446675 11.00000 0.33324 0.21016 = 0.15955 -0.07162 0.04907 -0.02069 AFIX 33 H24D 2 0.938369 0.901650 0.470766 11.00000 -1.20000 H24E 2 0.955790 0.980172 0.526521 11.00000 -1.20000 H24F 2 0.948295 1.042749 0.386866 11.00000 -1.20000 AFIX 0 C25B 1 0.956349 0.563965 0.200658 11.00000 0.14831 0.27554 = 0.10467 0.03675 -0.00134 -0.04266 AFIX 23 H25C 2 0.950495 0.540791 0.115326 11.00000 -1.20000 H25D 2 0.968557 0.577785 0.182910 11.00000 -1.20000 AFIX 0 C26B 1 0.954140 0.417403 0.286408 11.00000 0.16246 0.20268 = 0.06585 -0.02228 -0.00638 -0.02128 AFIX 33 H26D 2 0.958719 0.314232 0.244273 11.00000 -1.20000 H26E 2 0.960140 0.437778 0.370389 11.00000 -1.20000 H26F 2 0.942063 0.400752 0.302746 11.00000 -1.20000 AFIX 0 C27B 1 0.918807 1.102432 0.078335 11.00000 0.03649 0.07251 = 0.02727 -0.00093 -0.00744 -0.00331 AFIX 33 H27F 2 0.928428 1.144540 0.131379 11.00000 -1.20000 H27D 2 0.920121 1.138258 -0.013680 11.00000 -1.20000 H27E 2 0.908290 1.150450 0.112661 11.00000 -1.20000 AFIX 0 C28B 1 0.880626 0.909742 0.175229 11.00000 0.03521 0.08624 = 0.00536 -0.00340 0.00551 -0.00897 AFIX 137 H28D 2 0.886163 1.009768 0.216084 11.00000 -1.50000 H28E 2 0.885045 0.804043 0.215833 11.00000 -1.50000 H28F 2 0.868392 0.916614 0.188559 11.00000 -1.50000 AFIX 0 C29B 1 0.823688 1.033108 0.037949 11.00000 0.03558 0.07829 = 0.02308 0.00203 -0.00004 0.00193 AFIX 137 H29D 2 0.828476 0.951751 0.102380 11.00000 -1.50000 H29E 2 0.811308 1.029827 0.041527 11.00000 -1.50000 H29F 2 0.827670 1.149639 0.058733 11.00000 -1.50000 AFIX 0 O1 3 0.774878 0.862541 0.443110 11.00000 0.03718 0.03604 = 0.01156 -0.00142 -0.00048 0.00639 O2 3 0.759424 1.081348 0.526419 11.00000 0.03597 0.04371 = 0.01339 -0.00158 -0.00673 0.00705 AFIX 83 H2 2 0.764307 1.054872 0.597510 11.00000 -1.20000 AFIX 0 O3 3 0.755140 0.845949 0.219721 11.00000 0.03343 0.04989 = 0.01918 -0.00440 -0.00170 0.00523 O4 3 0.772422 1.161268 0.005176 11.00000 0.04818 0.07420 = 0.01351 0.00742 0.00726 0.00496 AFIX 83 H4 2 0.774810 1.263120 0.025044 11.00000 -1.20000 AFIX 0 O5 3 0.765938 0.793854 0.011004 11.00000 0.05025 0.06272 = 0.03363 -0.02322 0.00066 -0.00031 EADP c1 c2 C1 1 0.763565 0.965690 0.431465 11.00000 0.02070 0.01860 = 0.00741 -0.00007 -0.00366 0.00050 C2 1 0.752309 0.997892 0.303885 11.00000 0.02070 0.01860 = 0.00741 -0.00007 -0.00366 0.00050 C3 1 0.759502 1.164565 0.228982 11.00000 0.01827 0.06965 = 0.02357 0.01097 -0.00923 0.00706 AFIX 23 H3C 2 0.750533 1.250626 0.210347 11.00000 -1.20000 H3D 2 0.768944 1.219482 0.278747 11.00000 -1.20000 AFIX 0 C4 1 0.765136 1.081654 0.111126 11.00000 0.03861 0.03394 = 0.01258 0.01041 -0.00282 0.00423 C5 1 0.762949 0.903433 0.099853 11.00000 0.01863 0.06170 = 0.04288 0.00582 -0.00680 -0.00945 C6 1 0.733372 1.006430 0.334519 11.00000 0.03394 0.03355 = 0.02635 0.00015 -0.00930 0.00640 AFIX 137 H6A 2 0.730685 1.119804 0.371092 11.00000 -1.50000 H6B 2 0.730599 0.916979 0.398866 11.00000 -1.50000 H6C 2 0.726740 0.987958 0.253157 11.00000 -1.50000 AFIX 0 DFIX 0.8 0.01 o1w h1wa DFIX 0.8 0.01 o1w h1wb DFIX 1.3 0.01 h1wa h1wb O1W 3 0.779656 0.476727 0.056060 11.00000 0.05397 0.05465 = 0.03911 -0.00783 0.00331 0.00516 H1WA 2 0.789598 0.499143 0.068277 11.00000 -1.20000 H1WB 2 0.774229 0.566248 0.053108 11.00000 -1.20000 HKLF 4 REM mo_023TB174_0ma_a.res in P1 New: C2 REM R1 = 0.0602 for 3517 Fo > 4sig(Fo) and 0.1580 for all 7367 data REM 638 parameters refined using 41 restraints END WGHT 0.0139 0.0000 REM Highest difference peak 0.268, deepest hole -0.228, 1-sigma level 0.054 Q1 1 0.8502 0.8296 -0.1046 11.00000 0.05 0.24 Q2 1 0.7613 0.9931 -0.0154 11.00000 0.05 0.23 Q3 1 0.8393 0.9502 -0.1135 11.00000 0.05 0.22 Q4 1 0.7974 0.9958 0.3785 11.00000 0.05 0.21 Q5 1 0.8834 0.3708 0.0188 11.00000 0.05 0.21 Q6 1 0.8810 0.8877 0.5160 11.00000 0.05 0.21 Q7 1 0.8003 0.8322 0.3434 11.00000 0.05 0.21 Q8 1 0.8929 0.5359 0.5467 11.00000 0.05 0.21 Q9 1 0.8385 0.7829 -0.0621 11.00000 0.05 0.21 Q10 1 0.7665 0.5023 0.0535 11.00000 0.05 0.20 Q11 1 0.8305 0.9772 0.4162 11.00000 0.05 0.20 Q12 1 0.8147 0.5018 -0.1780 11.00000 0.05 0.20 Q13 1 0.7881 1.0079 -0.2403 11.00000 0.05 0.20 Q14 1 0.8537 0.3385 0.4758 11.00000 0.05 0.20 Q15 1 0.7259 1.2213 0.2937 11.00000 0.05 0.20 Q16 1 0.8704 1.0637 -0.0518 11.00000 0.05 0.20 Q17 1 0.9780 0.3907 0.7935 11.00000 0.05 0.19 Q18 1 0.8770 0.1023 0.5717 11.00000 0.05 0.19 Q19 1 0.8960 0.6070 -0.0059 11.00000 0.05 0.19 Q20 1 0.7732 0.7258 0.4386 11.00000 0.05 0.19 ; _shelx_res_checksum 31410 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1A O 0.78228(6) 0.5453(7) 0.3202(5) 0.0330(17) Uani 1 1 d . . . . . H1OA H 0.774847 0.554154 0.377769 0.040 Uiso 1 1 calc R U . . . C1A C 0.79916(10) 0.5352(11) 0.3850(8) 0.024(2) Uani 1 1 d . . . . . H1A H 0.797821 0.565068 0.480309 0.029 Uiso 1 1 calc R U . . . C2A C 0.80554(10) 0.3479(11) 0.3773(8) 0.030(2) Uani 1 1 d . . . . . H2AA H 0.797577 0.271061 0.423509 0.036 Uiso 1 1 calc R U . . . H2AB H 0.805924 0.311363 0.283729 0.036 Uiso 1 1 calc R U . . . C3A C 0.82296(9) 0.3316(12) 0.4396(8) 0.033(3) Uani 1 1 d . . . . . H3AA H 0.827195 0.213828 0.422623 0.040 Uiso 1 1 calc R U . . . H3AB H 0.821881 0.344195 0.536392 0.040 Uiso 1 1 calc R U . . . C4A C 0.83669(10) 0.4640(11) 0.3915(8) 0.016(2) Uani 1 1 d . . . . . C5A C 0.82980(12) 0.6439(12) 0.3900(8) 0.028(3) Uani 1 1 d . . . . . C6A C 0.81161(10) 0.6633(11) 0.3258(8) 0.031(3) Uani 1 1 d . . . . . H6AA H 0.807450 0.781997 0.340076 0.037 Uiso 1 1 calc R U . . . H6AB H 0.812246 0.643833 0.229403 0.037 Uiso 1 1 calc R U . . . C7A C 0.83843(11) 0.7837(13) 0.4265(8) 0.030(3) Uani 1 1 d . . . . . H7A H 0.833203 0.892912 0.415503 0.036 Uiso 1 1 calc R U . . . C8A C 0.85627(11) 0.7766(11) 0.4850(9) 0.040(3) Uani 1 1 d . . . . . H8AA H 0.855770 0.797424 0.581251 0.048 Uiso 1 1 calc R U . . . H8AB H 0.863100 0.869992 0.445886 0.048 Uiso 1 1 calc R U . . . C9A C 0.86523(10) 0.6006(10) 0.4603(8) 0.0213(16) Uani 1 1 d . . . . . H9A H 0.868787 0.596664 0.366074 0.026 Uiso 1 1 calc R U . . . C10A C 0.85327(10) 0.4492(10) 0.4848(8) 0.0213(16) Uani 1 1 d . . . . . H10A H 0.849225 0.463878 0.577165 0.026 Uiso 1 1 calc R U . . . C14A C 0.88146(12) 0.5800(14) 0.5509(9) 0.047(3) Uani 1 1 d . . . . . H14A H 0.877289 0.581834 0.643565 0.056 Uiso 1 1 calc R U . . . C13A C 0.89105(12) 0.4078(13) 0.5369(9) 0.034(3) Uani 1 1 d . . . . . C12A C 0.87900(11) 0.2642(14) 0.5685(10) 0.063(4) Uani 1 1 d . . . . . H12A H 0.876062 0.271564 0.662995 0.075 Uiso 1 1 calc R U . . . H12B H 0.884784 0.152745 0.554657 0.075 Uiso 1 1 calc R U . . . C11A C 0.86178(10) 0.2673(11) 0.4808(9) 0.037(3) Uani 1 1 d . . . . . H11A H 0.864356 0.237206 0.388330 0.044 Uiso 1 1 calc R U . . . H11B H 0.853822 0.180118 0.514860 0.044 Uiso 1 1 calc R U . . . C15A C 0.89537(12) 0.7231(13) 0.5451(10) 0.050(3) Uani 1 1 d . . . . . H15A H 0.897876 0.754519 0.452716 0.061 Uiso 1 1 calc R U . . . H15B H 0.891883 0.827623 0.593539 0.061 Uiso 1 1 calc R U . . . C16A C 0.91072(12) 0.6357(13) 0.6131(10) 0.044(3) Uani 1 1 d . . . . . H16A H 0.920802 0.647992 0.557118 0.053 Uiso 1 1 calc R U . . . H16B H 0.913175 0.692697 0.698757 0.053 Uiso 1 1 calc R U . . . C17A C 0.90715(12) 0.4483(15) 0.6355(9) 0.043(3) Uani 1 1 d . . . . . H17A H 0.902865 0.438408 0.727611 0.052 Uiso 1 1 calc R U . . . C18A C 0.92258(12) 0.3270(17) 0.6272(10) 0.060(4) Uani 1 1 d . . . . . H18A H 0.927526 0.339968 0.537460 0.072 Uiso 1 1 calc R U . . . C19A C 0.93659(11) 0.3907(14) 0.7350(9) 0.066(4) Uani 1 1 d D . . . . H19A H 0.937940 0.517160 0.728174 0.080 Uiso 1 1 calc R U . . . H19B H 0.932573 0.364110 0.824752 0.080 Uiso 1 1 calc R U . . . C20A C 0.95386(13) 0.3039(16) 0.7148(11) 0.109(5) Uani 1 1 d D . . . . H20A H 0.957041 0.316776 0.621206 0.130 Uiso 1 1 calc R U . . . H20B H 0.952753 0.179207 0.733218 0.130 Uiso 1 1 calc R U . . . C21A C 0.96850(12) 0.3801(17) 0.8054(11) 0.118(6) Uani 1 1 d D U . . . H21A H 0.964151 0.406341 0.895344 0.142 Uiso 1 1 calc R U . . . C22A C 0.97452(17) 0.5486(17) 0.7369(17) 0.224(9) Uani 1 1 d D U . . . H22A H 0.964817 0.605725 0.689783 0.269 Uiso 1 1 calc R U . . . C23A C 0.9819(3) 0.666(3) 0.839(2) 0.439(16) Uani 1 1 d D U . . . H23A H 0.973099 0.697777 0.902014 0.659 Uiso 1 1 calc R U . . . H23B H 0.991146 0.607321 0.886272 0.659 Uiso 1 1 calc R U . . . H23C H 0.986198 0.770016 0.796723 0.659 Uiso 1 1 calc R U . . . C24A C 0.9885(3) 0.498(3) 0.6374(18) 0.439(16) Uani 1 1 d D U . . . H24A H 0.983676 0.421175 0.570049 0.659 Uiso 1 1 calc R U . . . H24B H 0.992810 0.602446 0.594949 0.659 Uiso 1 1 calc R U . . . H24C H 0.997758 0.439750 0.684498 0.659 Uiso 1 1 calc R U . . . C25A C 0.98403(19) 0.254(2) 0.816(2) 0.314(19) Uani 1 1 d D U . . . H25A H 0.985824 0.193606 0.731174 0.377 Uiso 1 1 calc R U . . . H25B H 0.994505 0.316856 0.841119 0.377 Uiso 1 1 calc R U . . . C26A C 0.9788(3) 0.127(3) 0.925(3) 0.40(2) Uani 1 1 d D . . . . H26A H 0.986752 0.136018 0.999912 0.598 Uiso 1 1 calc R U . . . H26B H 0.978883 0.009614 0.890295 0.598 Uiso 1 1 calc R U . . . H26C H 0.967360 0.155808 0.954474 0.598 Uiso 1 1 calc R U . . . C27A C 0.91855(13) 0.1441(15) 0.6468(11) 0.076(4) Uani 1 1 d . . . . . H27A H 0.928902 0.075418 0.640173 0.091 Uiso 1 1 calc R U . . . H27B H 0.913692 0.128158 0.734351 0.091 Uiso 1 1 calc R U . . . H27C H 0.910360 0.106746 0.578973 0.091 Uiso 1 1 calc R U . . . C28A C 0.89813(10) 0.3882(12) 0.3882(8) 0.045(3) Uani 1 1 d . . . . . H28A H 0.904157 0.278532 0.380212 0.068 Uiso 1 1 calc R U . . . H28B H 0.905892 0.483334 0.369669 0.068 Uiso 1 1 calc R U . . . H28C H 0.888631 0.391011 0.324833 0.068 Uiso 1 1 calc R U . . . C29A C 0.84123(9) 0.4080(12) 0.2453(7) 0.042(3) Uani 1 1 d . . . . . H29A H 0.844405 0.286077 0.244580 0.064 Uiso 1 1 calc R U . . . H29B H 0.850721 0.477610 0.214369 0.064 Uiso 1 1 calc R U . . . H29C H 0.831377 0.425962 0.186992 0.064 Uiso 1 1 calc R U . . . O1B O 0.77782(6) 1.0231(7) -0.2618(4) 0.0205(14) Uani 1 1 d . . . . . H1OB H 0.774875 1.066652 -0.190209 0.025 Uiso 1 1 calc R U . . . C1B C 0.79622(10) 0.9996(12) -0.2607(8) 0.029(2) Uani 1 1 d . . . . . H1B H 0.799663 0.973549 -0.353172 0.034 Uiso 1 1 calc R U . . . C2B C 0.80565(10) 1.1590(10) -0.2165(8) 0.022(2) Uani 1 1 d . . . . . H2BA H 0.801331 1.197078 -0.130072 0.027 Uiso 1 1 calc R U . . . H2BB H 0.803596 1.252679 -0.281057 0.027 Uiso 1 1 calc R U . . . C3B C 0.82490(9) 1.1243(11) -0.2040(8) 0.028(2) Uani 1 1 d . . . . . H3BA H 0.829209 1.091110 -0.291589 0.034 Uiso 1 1 calc R U . . . H3BB H 0.830679 1.232119 -0.176930 0.034 Uiso 1 1 calc R U . . . C4B C 0.82946(10) 0.9821(11) -0.1040(8) 0.019(2) Uani 1 1 d . . . . . C5B C 0.82038(11) 0.8169(13) -0.1494(9) 0.030(3) Uani 1 1 d . . . . . C6B C 0.80097(10) 0.8412(12) -0.1737(8) 0.030(2) Uani 1 1 d . . . . . H6BA H 0.796397 0.736082 -0.216561 0.035 Uiso 1 1 calc R U . . . H6BB H 0.795426 0.853224 -0.087211 0.035 Uiso 1 1 calc R U . . . C7B C 0.82680(11) 0.6588(13) -0.1374(8) 0.028(3) Uani 1 1 d . . . . . H7B H 0.819270 0.563963 -0.145343 0.034 Uiso 1 1 calc R U . . . C8B C 0.84543(10) 0.6212(11) -0.1119(8) 0.027(2) Uani 1 1 d . . . . . H8BA H 0.850963 0.594679 -0.196480 0.032 Uiso 1 1 calc R U . . . H8BB H 0.846568 0.519120 -0.053871 0.032 Uiso 1 1 calc R U . . . C9B C 0.85447(10) 0.7799(10) -0.0446(8) 0.0184(16) Uani 1 1 d . . . . . H9B H 0.850908 0.783293 0.049651 0.022 Uiso 1 1 calc R U . . . C10B C 0.84957(9) 0.9527(10) -0.1077(8) 0.0184(16) Uani 1 1 d . . . . . H10B H 0.852693 0.945923 -0.202797 0.022 Uiso 1 1 calc R U . . . C11B C 0.86001(9) 1.1030(11) -0.0458(8) 0.029(3) Uani 1 1 d . . . . . H11C H 0.856437 1.120350 0.046505 0.035 Uiso 1 1 calc R U . . . H11D H 0.857482 1.210106 -0.095268 0.035 Uiso 1 1 calc R U . . . C12B C 0.87974(10) 1.0696(12) -0.0468(8) 0.033(3) Uani 1 1 d . . . . . H12C H 0.883574 1.065273 -0.139297 0.040 Uiso 1 1 calc R U . . . H12D H 0.885637 1.166508 -0.002288 0.040 Uiso 1 1 calc R U . . . C13B C 0.88436(10) 0.9078(11) 0.0200(8) 0.019(2) Uani 1 1 d . . . . . C14B C 0.87393(10) 0.7558(12) -0.0450(8) 0.033(3) Uani 1 1 d . . . . . H14B H 0.876817 0.762542 -0.140659 0.040 Uiso 1 1 calc R U . . . C15B C 0.88241(11) 0.5832(13) 0.0027(9) 0.054(3) Uani 1 1 d . . . . . H15C H 0.881216 0.491397 -0.064694 0.065 Uiso 1 1 calc R U . . . H15D H 0.877599 0.542768 0.086804 0.065 Uiso 1 1 calc R U . . . C16B C 0.90182(11) 0.6425(14) 0.0215(9) 0.053(3) Uani 1 1 d . . . . . H16C H 0.905970 0.610043 0.110820 0.064 Uiso 1 1 calc R U . . . H16D H 0.908912 0.583096 -0.044073 0.064 Uiso 1 1 calc R U . . . C17B C 0.90325(10) 0.8338(13) 0.0038(8) 0.029(2) Uani 1 1 d . . . . . H17B H 0.906108 0.851877 -0.091028 0.035 Uiso 1 1 calc R U . . . C18B C 0.91818(11) 0.9136(13) 0.0853(10) 0.041(3) Uani 1 1 d . . . . . H18B H 0.916682 0.880694 0.179869 0.049 Uiso 1 1 calc R U . . . C19B C 0.93539(11) 0.8305(15) 0.0372(8) 0.072(4) Uani 1 1 d D . . . . H19C H 0.933483 0.706127 0.021316 0.086 Uiso 1 1 calc R U . . . H19D H 0.938373 0.883376 -0.048293 0.086 Uiso 1 1 calc R U . . . C20B C 0.95045(12) 0.8507(15) 0.1329(10) 0.082(4) Uani 1 1 d D . . . . H20C H 0.951151 0.972555 0.161220 0.098 Uiso 1 1 calc R U . . . H20D H 0.960969 0.823250 0.085506 0.098 Uiso 1 1 calc R U . . . C21B C 0.94952(14) 0.7345(14) 0.2580(10) 0.109(6) Uani 1 1 d D U . . . H21B H 0.937407 0.718940 0.282649 0.131 Uiso 1 1 calc R U . . . C22B C 0.95952(18) 0.7986(19) 0.3766(11) 0.178(8) Uani 1 1 d D U . . . H22B H 0.961382 0.701092 0.439750 0.214 Uiso 1 1 calc R U . . . C23B C 0.97628(14) 0.879(2) 0.3449(14) 0.204(10) Uani 1 1 d D U . . . H23D H 0.981923 0.916460 0.426719 0.244 Uiso 1 1 calc R U . . . H23E H 0.983390 0.793636 0.300594 0.244 Uiso 1 1 calc R U . . . H23F H 0.974468 0.977847 0.286625 0.244 Uiso 1 1 calc R U . . . C24B C 0.94957(18) 0.944(2) 0.4467(15) 0.234(10) Uani 1 1 d D U . . . H24D H 0.938369 0.901650 0.470766 0.281 Uiso 1 1 calc R U . . . H24E H 0.955790 0.980172 0.526521 0.281 Uiso 1 1 calc R U . . . H24F H 0.948295 1.042749 0.386866 0.281 Uiso 1 1 calc R U . . . C25B C 0.9563(2) 0.5640(19) 0.2007(13) 0.176(9) Uani 1 1 d D . . . . H25C H 0.950495 0.540791 0.115326 0.211 Uiso 1 1 calc R U . . . H25D H 0.968557 0.577785 0.182910 0.211 Uiso 1 1 calc R U . . . C26B C 0.95414(18) 0.4174(17) 0.2864(13) 0.144(7) Uani 1 1 d D . . . . H26D H 0.958719 0.314232 0.244273 0.173 Uiso 1 1 calc R U . . . H26E H 0.960140 0.437778 0.370389 0.173 Uiso 1 1 calc R U . . . H26F H 0.942063 0.400752 0.302746 0.173 Uiso 1 1 calc R U . . . C27B C 0.91881(11) 1.1024(13) 0.0783(9) 0.046(3) Uani 1 1 d . . . . . H27F H 0.928428 1.144540 0.131379 0.055 Uiso 1 1 calc R U . . . H27D H 0.920121 1.138258 -0.013680 0.055 Uiso 1 1 calc R U . . . H27E H 0.908290 1.150450 0.112661 0.055 Uiso 1 1 calc R U . . . C28B C 0.88063(9) 0.9097(12) 0.1752(7) 0.042(3) Uani 1 1 d . . . . . H28D H 0.886163 1.009768 0.216084 0.063 Uiso 1 1 calc R U . . . H28E H 0.885045 0.804043 0.215833 0.063 Uiso 1 1 calc R U . . . H28F H 0.868392 0.916614 0.188559 0.063 Uiso 1 1 calc R U . . . C29B C 0.82369(9) 1.0331(13) 0.0379(8) 0.046(3) Uani 1 1 d . . . . . H29D H 0.828476 0.951751 0.102380 0.068 Uiso 1 1 calc R U . . . H29E H 0.811308 1.029827 0.041527 0.068 Uiso 1 1 calc R U . . . H29F H 0.827670 1.149639 0.058733 0.068 Uiso 1 1 calc R U . . . O1 O 0.77488(7) 0.8625(7) 0.4431(5) 0.0283(16) Uani 1 1 d . . . . . O2 O 0.75942(6) 1.0813(7) 0.5264(5) 0.0311(16) Uani 1 1 d . . . . . H2 H 0.764307 1.054872 0.597510 0.037 Uiso 1 1 calc R U . . . O3 O 0.75514(6) 0.8459(8) 0.2197(6) 0.0342(17) Uani 1 1 d . . . . . O4 O 0.77242(7) 1.1613(8) 0.0052(5) 0.045(2) Uani 1 1 d . . . . . H4 H 0.774810 1.263120 0.025044 0.054 Uiso 1 1 calc R U . . . O5 O 0.76594(8) 0.7939(9) 0.0110(6) 0.049(2) Uani 1 1 d . . . . . C1 C 0.76357(10) 0.9657(12) 0.4315(8) 0.0156(15) Uani 1 1 d . . . . . C2 C 0.75231(10) 0.9979(11) 0.3039(7) 0.0156(15) Uani 1 1 d . . . . . C3 C 0.75950(10) 1.1646(12) 0.2290(9) 0.037(3) Uani 1 1 d . . . . . H3C H 0.750533 1.250626 0.210347 0.045 Uiso 1 1 calc R U . . . H3D H 0.768944 1.219482 0.278747 0.045 Uiso 1 1 calc R U . . . C4 C 0.76514(11) 1.0817(14) 0.1111(9) 0.028(2) Uani 1 1 d . . . . . C5 C 0.76295(11) 0.9034(16) 0.0999(11) 0.041(3) Uani 1 1 d . . . . . C6 C 0.73337(9) 1.0064(11) 0.3345(7) 0.031(2) Uani 1 1 d . . . . . H6A H 0.730685 1.119804 0.371092 0.047 Uiso 1 1 calc R U . . . H6B H 0.730599 0.916979 0.398866 0.047 Uiso 1 1 calc R U . . . H6C H 0.726740 0.987958 0.253157 0.047 Uiso 1 1 calc R U . . . O1W O 0.77966(8) 0.4767(8) 0.0561(7) 0.0492(19) Uani 1 1 d D . . . . H1WA H 0.7896(3) 0.499(9) 0.068(9) 0.059 Uiso 1 1 d D U . . . H1WB H 0.7742(8) 0.566(6) 0.053(10) 0.059 Uiso 1 1 d D 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 O1A 0.037(4) 0.031(5) 0.031(4) -0.004(3) 0.001(3) 0.006(3) C1A 0.032(6) 0.023(6) 0.018(5) -0.007(5) -0.003(4) -0.017(5) C2A 0.052(7) 0.017(6) 0.020(6) 0.001(5) 0.004(5) 0.001(5) C3A 0.025(6) 0.040(7) 0.035(6) 0.005(5) -0.004(5) 0.006(5) C4A 0.027(6) 0.010(6) 0.012(5) 0.000(4) 0.002(4) -0.002(5) C5A 0.047(7) 0.023(7) 0.014(6) -0.003(5) 0.012(5) 0.001(6) C6A 0.029(6) 0.030(7) 0.033(7) -0.005(5) 0.000(5) 0.004(5) C7A 0.037(6) 0.022(7) 0.029(6) 0.000(5) -0.002(5) 0.000(5) C8A 0.050(7) 0.041(8) 0.029(7) 0.000(6) 0.005(5) 0.006(6) C9A 0.036(5) 0.017(5) 0.012(4) 0.000(3) 0.003(3) -0.002(3) C10A 0.036(5) 0.017(5) 0.012(4) 0.000(3) 0.003(3) -0.002(3) C14A 0.048(7) 0.074(9) 0.018(6) -0.007(6) -0.001(5) -0.006(7) C13A 0.036(7) 0.039(8) 0.025(6) 0.002(6) -0.001(5) 0.002(6) C12A 0.045(7) 0.103(11) 0.039(8) 0.001(7) -0.005(6) -0.004(7) C11A 0.038(6) 0.036(7) 0.037(7) -0.008(5) -0.007(5) 0.000(5) C15A 0.045(7) 0.067(9) 0.038(7) -0.007(6) -0.008(6) -0.004(7) C16A 0.041(7) 0.052(9) 0.040(7) -0.008(6) -0.006(5) 0.005(6) C17A 0.051(7) 0.062(9) 0.017(6) -0.013(6) -0.002(5) -0.001(7) C18A 0.031(7) 0.111(11) 0.037(7) 0.003(8) -0.001(6) 0.002(8) C19A 0.047(7) 0.114(12) 0.038(7) 0.005(7) -0.005(6) -0.015(8) C20A 0.059(9) 0.183(16) 0.084(11) -0.027(11) 0.000(8) 0.024(10) C21A 0.073(10) 0.220(17) 0.062(10) -0.010(11) -0.018(8) -0.003(10) C22A 0.123(16) 0.27(2) 0.27(3) 0.076(16) -0.031(11) -0.047(16) C23A 0.27(2) 0.67(5) 0.38(3) -0.19(3) 0.075(15) -0.16(2) C24A 0.27(2) 0.67(5) 0.38(3) -0.19(3) 0.075(15) -0.16(2) C25A 0.157(19) 0.13(2) 0.65(6) 0.05(3) -0.20(3) -0.004(13) C26A 0.31(3) 0.19(3) 0.69(7) 0.11(3) -0.13(3) -0.10(3) C27A 0.057(9) 0.085(11) 0.086(10) 0.017(9) -0.003(7) -0.008(8) C28A 0.050(6) 0.067(8) 0.018(6) -0.004(6) 0.000(5) -0.010(6) C29A 0.037(6) 0.067(8) 0.023(6) -0.006(6) 0.005(5) -0.001(5) O1B 0.026(4) 0.026(4) 0.010(3) -0.001(3) -0.002(3) 0.002(3) C1B 0.035(6) 0.035(7) 0.016(5) -0.005(5) 0.008(4) 0.008(6) C2B 0.030(6) 0.015(6) 0.021(6) 0.002(5) 0.003(4) -0.006(5) C3B 0.025(6) 0.028(6) 0.031(6) 0.002(5) 0.004(5) 0.004(5) C4B 0.021(5) 0.019(6) 0.016(5) -0.001(5) 0.006(4) 0.000(5) C5B 0.037(7) 0.013(7) 0.040(7) -0.006(5) 0.002(5) -0.004(6) C6B 0.028(6) 0.026(7) 0.034(6) -0.014(5) 0.000(5) -0.004(5) C7B 0.036(7) 0.033(7) 0.016(6) -0.001(5) 0.006(5) -0.007(6) C8B 0.024(6) 0.035(7) 0.021(6) 0.002(5) -0.001(4) -0.008(5) C9B 0.031(4) 0.006(4) 0.019(4) -0.002(3) 0.002(3) 0.003(3) C10B 0.031(4) 0.006(4) 0.019(4) -0.002(3) 0.002(3) 0.003(3) C11B 0.026(6) 0.028(6) 0.032(6) 0.002(5) -0.009(5) -0.005(5) C12B 0.025(6) 0.049(8) 0.027(6) -0.003(6) 0.010(5) 0.001(5) C13B 0.018(5) 0.011(6) 0.029(6) -0.006(5) 0.000(5) -0.004(5) C14B 0.027(6) 0.055(8) 0.018(6) -0.006(6) 0.004(5) 0.006(6) C15B 0.058(8) 0.072(10) 0.033(7) 0.008(6) -0.003(6) 0.006(7) C16B 0.033(7) 0.097(11) 0.030(7) 0.001(7) -0.004(5) -0.019(7) C17B 0.034(6) 0.036(7) 0.017(6) -0.001(5) -0.003(5) -0.008(6) C18B 0.043(7) 0.042(8) 0.037(7) -0.006(6) -0.004(6) 0.003(6) C19B 0.031(7) 0.141(12) 0.043(8) -0.011(8) -0.007(6) 0.000(8) C20B 0.053(8) 0.102(11) 0.091(11) 0.015(9) -0.004(8) -0.005(8) C21B 0.106(12) 0.158(16) 0.065(10) -0.028(11) 0.015(8) 0.052(11) C22B 0.181(17) 0.27(3) 0.078(13) -0.043(13) -0.008(11) 0.010(15) C23B 0.128(13) 0.38(3) 0.106(14) -0.028(17) -0.025(11) 0.035(15) C24B 0.33(3) 0.21(2) 0.160(19) -0.072(16) 0.049(16) -0.021(17) C25B 0.148(16) 0.28(3) 0.105(15) 0.037(18) -0.001(12) -0.043(18) C26B 0.162(15) 0.20(2) 0.066(12) -0.022(12) -0.006(11) -0.021(14) C27B 0.036(7) 0.073(9) 0.027(7) -0.001(7) -0.007(5) -0.003(6) C28B 0.035(6) 0.086(9) 0.005(5) -0.003(5) 0.006(4) -0.009(6) C29B 0.036(6) 0.078(9) 0.023(6) 0.002(6) 0.000(5) 0.002(6) O1 0.037(4) 0.036(4) 0.012(4) -0.001(3) 0.000(3) 0.006(3) O2 0.036(4) 0.044(4) 0.013(3) -0.002(3) -0.007(3) 0.007(3) O3 0.033(4) 0.050(5) 0.019(4) -0.004(4) -0.002(3) 0.005(3) O4 0.048(4) 0.074(6) 0.014(4) 0.007(4) 0.007(3) 0.005(4) O5 0.050(5) 0.063(6) 0.034(5) -0.023(4) 0.001(4) 0.000(4) C1 0.021(4) 0.019(4) 0.007(3) 0.000(3) -0.004(3) 0.000(3) C2 0.021(4) 0.019(4) 0.007(3) 0.000(3) -0.004(3) 0.000(3) C3 0.018(6) 0.070(8) 0.024(6) 0.011(6) -0.009(5) 0.007(5) C4 0.039(6) 0.034(8) 0.013(6) 0.010(6) -0.003(5) 0.004(6) C5 0.019(6) 0.062(11) 0.043(9) 0.006(7) -0.007(6) -0.009(6) C6 0.034(6) 0.034(6) 0.026(6) 0.000(5) -0.009(4) 0.006(5) O1W 0.054(5) 0.055(5) 0.039(4) -0.008(4) 0.003(4) 0.005(4) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A O1A H1OA 109.5 . . ? O1A C1A C6A 111.9(7) . . ? O1A C1A C2A 108.7(6) . . ? C6A C1A C2A 112.4(7) . . ? O1A C1A H1A 107.9 . . ? C6A C1A H1A 107.9 . . ? C2A C1A H1A 107.9 . . ? C3A C2A C1A 110.7(7) . . ? C3A C2A H2AA 109.5 . . ? C1A C2A H2AA 109.5 . . ? C3A C2A H2AB 109.5 . . ? C1A C2A H2AB 109.5 . . ? H2AA C2A H2AB 108.1 . . ? C2A C3A C4A 116.3(7) . . ? C2A C3A H3AA 108.2 . . ? C4A C3A H3AA 108.2 . . ? C2A C3A H3AB 108.2 . . ? C4A C3A H3AB 108.2 . . ? H3AA C3A H3AB 107.4 . . ? C5A C4A C3A 111.1(7) . . ? C5A C4A C29A 109.4(7) . . ? C3A C4A C29A 106.1(7) . . ? C5A C4A C10A 111.4(7) . . ? C3A C4A C10A 109.3(6) . . ? C29A C4A C10A 109.5(6) . . ? C7A C5A C4A 124.9(9) . . ? C7A C5A C6A 119.8(9) . . ? C4A C5A C6A 115.0(8) . . ? C1A C6A C5A 111.4(7) . . ? C1A C6A H6AA 109.3 . . ? C5A C6A H6AA 109.3 . . ? C1A C6A H6AB 109.3 . . ? C5A C6A H6AB 109.3 . . ? H6AA C6A H6AB 108.0 . . ? C5A C7A C8A 123.1(9) . . ? C5A C7A H7A 118.4 . . ? C8A C7A H7A 118.4 . . ? C7A C8A C9A 112.9(7) . . ? C7A C8A H8AA 109.0 . . ? C9A C8A H8AA 109.0 . . ? C7A C8A H8AB 109.0 . . ? C9A C8A H8AB 109.0 . . ? H8AA C8A H8AB 107.8 . . ? C10A C9A C8A 111.3(7) . . ? C10A C9A C14A 109.1(7) . . ? C8A C9A C14A 111.3(7) . . ? C10A C9A H9A 108.3 . . ? C8A C9A H9A 108.3 . . ? C14A C9A H9A 108.3 . . ? C9A C10A C11A 115.0(7) . . ? C9A C10A C4A 110.4(6) . . ? C11A C10A C4A 113.3(7) . . ? C9A C10A H10A 105.7 . . ? C11A C10A H10A 105.7 . . ? C4A C10A H10A 105.7 . . ? C13A C14A C15A 105.4(8) . . ? C13A C14A C9A 115.5(8) . . ? C15A C14A C9A 118.2(8) . . ? C13A C14A H14A 105.5 . . ? C15A C14A H14A 105.5 . . ? C9A C14A H14A 105.5 . . ? C12A C13A C14A 108.0(8) . . ? C12A C13A C28A 110.9(8) . . ? C14A C13A C28A 110.1(8) . . ? C12A C13A C17A 120.1(8) . . ? C14A C13A C17A 98.9(8) . . ? C28A C13A C17A 108.0(7) . . ? C13A C12A C11A 113.8(8) . . ? C13A C12A H12A 108.8 . . ? C11A C12A H12A 108.8 . . ? C13A C12A H12B 108.8 . . ? C11A C12A H12B 108.8 . . ? H12A C12A H12B 107.7 . . ? C10A C11A C12A 111.0(7) . . ? C10A C11A H11A 109.4 . . ? C12A C11A H11A 109.4 . . ? C10A C11A H11B 109.4 . . ? C12A C11A H11B 109.4 . . ? H11A C11A H11B 108.0 . . ? C16A C15A C14A 102.6(8) . . ? C16A C15A H15A 111.2 . . ? C14A C15A H15A 111.2 . . ? C16A C15A H15B 111.2 . . ? C14A C15A H15B 111.2 . . ? H15A C15A H15B 109.2 . . ? C17A C16A C15A 110.2(9) . . ? C17A C16A H16A 109.6 . . ? C15A C16A H16A 109.6 . . ? C17A C16A H16B 109.6 . . ? C15A C16A H16B 109.6 . . ? H16A C16A H16B 108.1 . . ? C16A C17A C18A 115.6(9) . . ? C16A C17A C13A 103.9(9) . . ? C18A C17A C13A 117.1(8) . . ? C16A C17A H17A 106.5 . . ? C18A C17A H17A 106.5 . . ? C13A C17A H17A 106.5 . . ? C27A C18A C17A 114.1(9) . . ? C27A C18A C19A 110.6(9) . . ? C17A C18A C19A 108.0(9) . . ? C27A C18A H18A 108.0 . . ? C17A C18A H18A 108.0 . . ? C19A C18A H18A 108.0 . . ? C20A C19A C18A 112.0(8) . . ? C20A C19A H19A 109.2 . . ? C18A C19A H19A 109.2 . . ? C20A C19A H19B 109.2 . . ? C18A C19A H19B 109.2 . . ? H19A C19A H19B 107.9 . . ? C19A C20A C21A 113.7(8) . . ? C19A C20A H20A 108.8 . . ? C21A C20A H20A 108.8 . . ? C19A C20A H20B 108.8 . . ? C21A C20A H20B 108.8 . . ? H20A C20A H20B 107.7 . . ? C22A C21A C25A 108.0(8) . . ? C22A C21A C20A 106.4(8) . . ? C25A C21A C20A 111.7(12) . . ? C22A C21A H21A 110.2 . . ? C25A C21A H21A 110.2 . . ? C20A C21A H21A 110.2 . . ? C23A C22A C24A 109.4(11) . . ? C23A C22A C21A 108.8(11) . . ? C24A C22A C21A 107.6(10) . . ? C23A C22A H22A 110.3 . . ? C24A C22A H22A 110.3 . . ? C21A C22A H22A 110.3 . . ? C22A C23A H23A 109.5 . . ? C22A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C22A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? C22A C24A H24A 109.5 . . ? C22A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C22A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C26A C25A C21A 103.1(12) . . ? C26A C25A H25A 111.2 . . ? C21A C25A H25A 111.2 . . ? C26A C25A H25B 111.2 . . ? C21A C25A H25B 111.2 . . ? H25A C25A H25B 109.1 . . ? C25A C26A H26A 109.5 . . ? C25A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C25A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C18A C27A H27A 109.5 . . ? C18A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C18A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C13A C28A H28A 109.5 . . ? C13A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C13A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C4A C29A H29A 109.5 . . ? C4A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C4A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C1B O1B H1OB 109.5 . . ? O1B C1B C2B 112.7(7) . . ? O1B C1B C6B 109.4(7) . . ? C2B C1B C6B 111.5(7) . . ? O1B C1B H1B 107.7 . . ? C2B C1B H1B 107.7 . . ? C6B C1B H1B 107.7 . . ? C1B C2B C3B 111.2(7) . . ? C1B C2B H2BA 109.4 . . ? C3B C2B H2BA 109.4 . . ? C1B C2B H2BB 109.4 . . ? C3B C2B H2BB 109.4 . . ? H2BA C2B H2BB 108.0 . . ? C4B C3B C2B 113.5(7) . . ? C4B C3B H3BA 108.9 . . ? C2B C3B H3BA 108.9 . . ? C4B C3B H3BB 108.9 . . ? C2B C3B H3BB 108.9 . . ? H3BA C3B H3BB 107.7 . . ? C5B C4B C3B 107.4(7) . . ? C5B C4B C29B 110.2(7) . . ? C3B C4B C29B 110.8(7) . . ? C5B C4B C10B 109.3(7) . . ? C3B C4B C10B 107.9(6) . . ? C29B C4B C10B 111.1(6) . . ? C7B C5B C4B 124.5(8) . . ? C7B C5B C6B 119.8(8) . . ? C4B C5B C6B 113.5(8) . . ? C1B C6B C5B 114.3(7) . . ? C1B C6B H6BA 108.7 . . ? C5B C6B H6BA 108.7 . . ? C1B C6B H6BB 108.7 . . ? C5B C6B H6BB 108.7 . . ? H6BA C6B H6BB 107.6 . . ? C5B C7B C8B 124.0(8) . . ? C5B C7B H7B 118.0 . . ? C8B C7B H7B 118.0 . . ? C7B C8B C9B 110.8(7) . . ? C7B C8B H8BA 109.5 . . ? C9B C8B H8BA 109.5 . . ? C7B C8B H8BB 109.5 . . ? C9B C8B H8BB 109.5 . . ? H8BA C8B H8BB 108.1 . . ? C10B C9B C14B 110.4(7) . . ? C10B C9B C8B 113.3(6) . . ? C14B C9B C8B 110.4(6) . . ? C10B C9B H9B 107.5 . . ? C14B C9B H9B 107.5 . . ? C8B C9B H9B 107.5 . . ? C9B C10B C11B 111.1(6) . . ? C9B C10B C4B 111.0(7) . . ? C11B C10B C4B 113.7(6) . . ? C9B C10B H10B 106.9 . . ? C11B C10B H10B 106.9 . . ? C4B C10B H10B 106.9 . . ? C10B C11B C12B 113.0(7) . . ? C10B C11B H11C 109.0 . . ? C12B C11B H11C 109.0 . . ? C10B C11B H11D 109.0 . . ? C12B C11B H11D 109.0 . . ? H11C C11B H11D 107.8 . . ? C13B C12B C11B 112.0(7) . . ? C13B C12B H12C 109.2 . . ? C11B C12B H12C 109.2 . . ? C13B C12B H12D 109.2 . . ? C11B C12B H12D 109.2 . . ? H12C C12B H12D 107.9 . . ? C12B C13B C14B 108.9(7) . . ? C12B C13B C28B 113.2(7) . . ? C14B C13B C28B 108.2(7) . . ? C12B C13B C17B 118.8(7) . . ? C14B C13B C17B 99.8(7) . . ? C28B C13B C17B 106.8(6) . . ? C9B C14B C15B 121.4(7) . . ? C9B C14B C13B 114.9(7) . . ? C15B C14B C13B 107.0(7) . . ? C9B C14B H14B 103.8 . . ? C15B C14B H14B 103.8 . . ? C13B C14B H14B 103.8 . . ? C14B C15B C16B 101.1(8) . . ? C14B C15B H15C 111.5 . . ? C16B C15B H15C 111.5 . . ? C14B C15B H15D 111.5 . . ? C16B C15B H15D 111.5 . . ? H15C C15B H15D 109.4 . . ? C17B C16B C15B 110.0(8) . . ? C17B C16B H16C 109.7 . . ? C15B C16B H16C 109.7 . . ? C17B C16B H16D 109.7 . . ? C15B C16B H16D 109.7 . . ? H16C C16B H16D 108.2 . . ? C16B C17B C18B 112.9(8) . . ? C16B C17B C13B 105.6(7) . . ? C18B C17B C13B 120.0(7) . . ? C16B C17B H17B 105.8 . . ? C18B C17B H17B 105.8 . . ? C13B C17B H17B 105.8 . . ? C27B C18B C17B 113.4(9) . . ? C27B C18B C19B 111.2(9) . . ? C17B C18B C19B 108.7(7) . . ? C27B C18B H18B 107.8 . . ? C17B C18B H18B 107.8 . . ? C19B C18B H18B 107.8 . . ? C20B C19B C18B 115.1(8) . . ? C20B C19B H19C 108.5 . . ? C18B C19B H19C 108.5 . . ? C20B C19B H19D 108.5 . . ? C18B C19B H19D 108.5 . . ? H19C C19B H19D 107.5 . . ? C19B C20B C21B 114.1(8) . . ? C19B C20B H20C 108.7 . . ? C21B C20B H20C 108.7 . . ? C19B C20B H20D 108.7 . . ? C21B C20B H20D 108.7 . . ? H20C C20B H20D 107.6 . . ? C22B C21B C25B 113.5(8) . . ? C22B C21B C20B 115.1(9) . . ? C25B C21B C20B 99.7(10) . . ? C22B C21B H21B 109.3 . . ? C25B C21B H21B 109.3 . . ? C20B C21B H21B 109.3 . . ? C23B C22B C21B 114.7(9) . . ? C23B C22B C24B 104.5(10) . . ? C21B C22B C24B 109.9(10) . . ? C23B C22B H22B 109.2 . . ? C21B C22B H22B 109.2 . . ? C24B C22B H22B 109.2 . . ? C22B C23B H23D 109.5 . . ? C22B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C22B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C22B C24B H24D 109.5 . . ? C22B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C22B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C26B C25B C21B 113.7(10) . . ? C26B C25B H25C 108.8 . . ? C21B C25B H25C 108.8 . . ? C26B C25B H25D 108.8 . . ? C21B C25B H25D 108.8 . . ? H25C C25B H25D 107.7 . . ? C25B C26B H26D 109.5 . . ? C25B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C25B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C18B C27B H27F 109.5 . . ? C18B C27B H27D 109.5 . . ? H27F C27B H27D 109.5 . . ? C18B C27B H27E 109.5 . . ? H27F C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C13B C28B H28D 109.5 . . ? C13B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C13B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C4B C29B H29D 109.5 . . ? C4B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C4B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C1 O2 H2 109.5 . . ? C5 O3 C2 108.1(7) . . ? C4 O4 H4 109.5 . . ? O1 C1 O2 123.8(7) . . ? O1 C1 C2 126.4(8) . . ? O2 C1 C2 109.6(7) . . ? O3 C2 C6 108.0(6) . . ? O3 C2 C1 104.9(6) . . ? C6 C2 C1 112.3(6) . . ? O3 C2 C3 108.2(6) . . ? C6 C2 C3 114.4(7) . . ? C1 C2 C3 108.4(6) . . ? C4 C3 C2 98.5(8) . . ? C4 C3 H3C 112.1 . . ? C2 C3 H3C 112.1 . . ? C4 C3 H3D 112.1 . . ? C2 C3 H3D 112.1 . . ? H3C C3 H3D 109.7 . . ? O4 C4 C5 115.7(10) . . ? O4 C4 C3 126.0(9) . . ? C5 C4 C3 118.2(10) . . ? O5 C5 C4 134.4(11) . . ? O5 C5 O3 118.6(10) . . ? C4 C5 O3 107.0(10) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? H1WA O1W H1WB 109(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1A C1A 1.449(8) . ? O1A H1OA 0.8200 . ? C1A C6A 1.497(10) . ? C1A C2A 1.511(10) . ? C1A H1A 0.9800 . ? C2A C3A 1.480(9) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C4A 1.545(10) . ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C4A C5A 1.469(11) . ? C4A C29A 1.558(10) . ? C4A C10A 1.575(9) . ? C5A C7A 1.304(11) . ? C5A C6A 1.543(11) . ? C6A H6AA 0.9700 . ? C6A H6AB 0.9700 . ? C7A C8A 1.491(10) . ? C7A H7A 0.9300 . ? C8A C9A 1.530(10) . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C9A C10A 1.501(10) . ? C9A C14A 1.540(10) . ? C9A H9A 0.9800 . ? C10A C11A 1.533(10) . ? C10A H10A 0.9800 . ? C14A C13A 1.514(11) . ? C14A C15A 1.533(11) . ? C14A H14A 0.9800 . ? C13A C12A 1.474(12) . ? C13A C28A 1.590(10) . ? C13A C17A 1.602(11) . ? C12A C11A 1.580(10) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C15A C16A 1.512(11) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C16A C17A 1.470(11) . ? C16A H16A 0.9700 . ? C16A H16B 0.9700 . ? C17A C18A 1.514(12) . ? C17A H17A 0.9800 . ? C18A C27A 1.440(13) . ? C18A C19A 1.587(11) . ? C18A H18A 0.9800 . ? C19A C20A 1.507(9) . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C20A C21A 1.548(10) . ? C20A H20A 0.9700 . ? C20A H20B 0.9700 . ? C21A C22A 1.527(10) . ? C21A C25A 1.539(11) . ? C21A H21A 0.9800 . ? C22A C23A 1.461(12) . ? C22A C24A 1.525(12) . ? C22A H22A 0.9800 . ? C23A H23A 0.9600 . ? C23A H23B 0.9600 . ? C23A H23C 0.9600 . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C25A C26A 1.513(13) . ? C25A H25A 0.9700 . ? C25A H25B 0.9700 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? O1B C1B 1.436(8) . ? O1B H1OB 0.8200 . ? C1B C2B 1.478(10) . ? C1B C6B 1.525(10) . ? C1B H1B 0.9800 . ? C2B C3B 1.517(9) . ? C2B H2BA 0.9700 . ? C2B H2BB 0.9700 . ? C3B C4B 1.506(10) . ? C3B H3BA 0.9700 . ? C3B H3BB 0.9700 . ? C4B C5B 1.505(11) . ? C4B C29B 1.534(10) . ? C4B C10B 1.574(9) . ? C5B C7B 1.307(10) . ? C5B C6B 1.529(10) . ? C6B H6BA 0.9700 . ? C6B H6BB 0.9700 . ? C7B C8B 1.488(10) . ? C7B H7B 0.9300 . ? C8B C9B 1.542(10) . ? C8B H8BA 0.9700 . ? C8B H8BB 0.9700 . ? C9B C10B 1.503(10) . ? C9B C14B 1.517(10) . ? C9B H9B 0.9800 . ? C10B C11B 1.523(9) . ? C10B H10B 0.9800 . ? C11B C12B 1.549(9) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B C13B 1.440(10) . ? C12B H12C 0.9700 . ? C12B H12D 0.9700 . ? C13B C14B 1.545(10) . ? C13B C28B 1.572(10) . ? C13B C17B 1.578(10) . ? C14B C15B 1.540(11) . ? C14B H14B 0.9800 . ? C15B C16B 1.577(10) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16B C17B 1.471(11) . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? C17B C18B 1.526(11) . ? C17B H17B 0.9800 . ? C18B C27B 1.439(10) . ? C18B C19B 1.557(11) . ? C18B H18B 0.9800 . ? C19B C20B 1.500(9) . ? C19B H19C 0.9700 . ? C19B H19D 0.9700 . ? C20B C21B 1.527(10) . ? C20B H20C 0.9700 . ? C20B H20D 0.9700 . ? C21B C22B 1.481(10) . ? C21B C25B 1.516(11) . ? C21B H21B 0.9800 . ? C22B C23B 1.472(11) . ? C22B C24B 1.524(11) . ? C22B H22B 0.9800 . ? C23B H23D 0.9600 . ? C23B H23E 0.9600 . ? C23B H23F 0.9600 . ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 0.9600 . ? C25B C26B 1.415(11) . ? C25B H25C 0.9700 . ? C25B H25D 0.9700 . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B H27F 0.9600 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? O1 C1 1.180(8) . ? O2 C1 1.332(8) . ? O2 H2 0.8200 . ? O3 C5 1.413(10) . ? O3 C2 1.445(9) . ? O4 C4 1.345(9) . ? O4 H4 0.8200 . ? O5 C5 1.238(11) . ? C1 C2 1.545(9) . ? C2 C6 1.504(9) . ? C2 C3 1.576(11) . ? C3 C4 1.405(11) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 C5 1.371(12) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? O1W H1WA 0.796(14) . ? O1W H1WB 0.801(14) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A C1A C2A C3A 178.7(6) . . . . ? C6A C1A C2A C3A 54.3(9) . . . . ? C1A C2A C3A C4A -50.9(10) . . . . ? C2A C3A C4A C5A 47.1(10) . . . . ? C2A C3A C4A C29A -71.7(9) . . . . ? C2A C3A C4A C10A 170.4(7) . . . . ? C3A C4A C5A C7A 140.7(9) . . . . ? C29A C4A C5A C7A -102.6(10) . . . . ? C10A C4A C5A C7A 18.6(12) . . . . ? C3A C4A C5A C6A -45.8(9) . . . . ? C29A C4A C5A C6A 70.9(9) . . . . ? C10A C4A C5A C6A -167.9(6) . . . . ? O1A C1A C6A C5A -176.7(6) . . . . ? C2A C1A C6A C5A -54.1(9) . . . . ? C7A C5A C6A C1A -134.9(8) . . . . ? C4A C5A C6A C1A 51.2(9) . . . . ? C4A C5A C7A C8A -4.7(14) . . . . ? C6A C5A C7A C8A -177.9(7) . . . . ? C5A C7A C8A C9A 16.7(12) . . . . ? C7A C8A C9A C10A -43.6(9) . . . . ? C7A C8A C9A C14A -165.6(7) . . . . ? C8A C9A C10A C11A -172.3(7) . . . . ? C14A C9A C10A C11A -49.0(9) . . . . ? C8A C9A C10A C4A 57.9(9) . . . . ? C14A C9A C10A C4A -178.8(7) . . . . ? C5A C4A C10A C9A -44.7(9) . . . . ? C3A C4A C10A C9A -167.8(7) . . . . ? C29A C4A C10A C9A 76.5(8) . . . . ? C5A C4A C10A C11A -175.4(7) . . . . ? C3A C4A C10A C11A 61.5(9) . . . . ? C29A C4A C10A C11A -54.2(9) . . . . ? C10A C9A C14A C13A 55.3(9) . . . . ? C8A C9A C14A C13A 178.5(8) . . . . ? C10A C9A C14A C15A -178.6(8) . . . . ? C8A C9A C14A C15A -55.4(10) . . . . ? C15A C14A C13A C12A 168.9(8) . . . . ? C9A C14A C13A C12A -58.6(10) . . . . ? C15A C14A C13A C28A -69.8(9) . . . . ? C9A C14A C13A C28A 62.6(10) . . . . ? C15A C14A C13A C17A 43.2(8) . . . . ? C9A C14A C13A C17A 175.6(8) . . . . ? C14A C13A C12A C11A 55.1(10) . . . . ? C28A C13A C12A C11A -65.6(10) . . . . ? C17A C13A C12A C11A 167.3(8) . . . . ? C9A C10A C11A C12A 47.8(9) . . . . ? C4A C10A C11A C12A 176.2(7) . . . . ? C13A C12A C11A C10A -51.3(10) . . . . ? C13A C14A C15A C16A -33.9(9) . . . . ? C9A C14A C15A C16A -164.8(8) . . . . ? C14A C15A C16A C17A 9.1(10) . . . . ? C15A C16A C17A C18A 147.1(8) . . . . ? C15A C16A C17A C13A 17.3(11) . . . . ? C12A C13A C17A C16A -153.6(9) . . . . ? C14A C13A C17A C16A -36.7(9) . . . . ? C28A C13A C17A C16A 78.0(9) . . . . ? C12A C13A C17A C18A 77.6(12) . . . . ? C14A C13A C17A C18A -165.5(8) . . . . ? C28A C13A C17A C18A -50.9(12) . . . . ? C16A C17A C18A C27A -178.7(9) . . . . ? C13A C17A C18A C27A -55.7(12) . . . . ? C16A C17A C18A C19A 57.9(11) . . . . ? C13A C17A C18A C19A -179.0(8) . . . . ? C27A C18A C19A C20A 66.8(12) . . . . ? C17A C18A C19A C20A -167.7(9) . . . . ? C18A C19A C20A C21A 172.3(9) . . . . ? C19A C20A C21A C22A -80.5(12) . . . . ? C19A C20A C21A C25A 161.9(11) . . . . ? C25A C21A C22A C23A -86.1(16) . . . . ? C20A C21A C22A C23A 153.8(14) . . . . ? C25A C21A C22A C24A 32.2(17) . . . . ? C20A C21A C22A C24A -87.8(13) . . . . ? C22A C21A C25A C26A 160.3(17) . . . . ? C20A C21A C25A C26A -83(2) . . . . ? O1B C1B C2B C3B 174.7(6) . . . . ? C6B C1B C2B C3B 51.1(9) . . . . ? C1B C2B C3B C4B -59.9(9) . . . . ? C2B C3B C4B C5B 58.9(9) . . . . ? C2B C3B C4B C29B -61.4(9) . . . . ? C2B C3B C4B C10B 176.7(6) . . . . ? C3B C4B C5B C7B 144.1(9) . . . . ? C29B C4B C5B C7B -95.2(10) . . . . ? C10B C4B C5B C7B 27.2(11) . . . . ? C3B C4B C5B C6B -52.8(9) . . . . ? C29B C4B C5B C6B 67.9(9) . . . . ? C10B C4B C5B C6B -169.7(7) . . . . ? O1B C1B C6B C5B -172.4(6) . . . . ? C2B C1B C6B C5B -47.0(10) . . . . ? C7B C5B C6B C1B -147.0(8) . . . . ? C4B C5B C6B C1B 49.0(10) . . . . ? C4B C5B C7B C8B -17.0(14) . . . . ? C6B C5B C7B C8B -179.1(7) . . . . ? C5B C7B C8B C9B 23.6(12) . . . . ? C7B C8B C9B C10B -44.1(9) . . . . ? C7B C8B C9B C14B -168.4(7) . . . . ? C14B C9B C10B C11B -50.7(9) . . . . ? C8B C9B C10B C11B -175.0(7) . . . . ? C14B C9B C10B C4B -178.3(6) . . . . ? C8B C9B C10B C4B 57.4(8) . . . . ? C5B C4B C10B C9B -46.1(9) . . . . ? C3B C4B C10B C9B -162.6(7) . . . . ? C29B C4B C10B C9B 75.7(9) . . . . ? C5B C4B C10B C11B -172.2(7) . . . . ? C3B C4B C10B C11B 71.2(8) . . . . ? C29B C4B C10B C11B -50.4(9) . . . . ? C9B C10B C11B C12B 52.4(9) . . . . ? C4B C10B C11B C12B 178.5(7) . . . . ? C10B C11B C12B C13B -56.1(9) . . . . ? C11B C12B C13B C14B 54.9(9) . . . . ? C11B C12B C13B C28B -65.5(9) . . . . ? C11B C12B C13B C17B 168.0(7) . . . . ? C10B C9B C14B C15B -174.8(7) . . . . ? C8B C9B C14B C15B -48.8(10) . . . . ? C10B C9B C14B C13B 53.9(9) . . . . ? C8B C9B C14B C13B 179.9(7) . . . . ? C12B C13B C14B C9B -56.3(9) . . . . ? C28B C13B C14B C9B 67.2(9) . . . . ? C17B C13B C14B C9B 178.6(7) . . . . ? C12B C13B C14B C15B 165.8(7) . . . . ? C28B C13B C14B C15B -70.7(8) . . . . ? C17B C13B C14B C15B 40.7(8) . . . . ? C9B C14B C15B C16B -164.8(7) . . . . ? C13B C14B C15B C16B -30.3(8) . . . . ? C14B C15B C16B C17B 7.1(10) . . . . ? C15B C16B C17B C18B 150.8(7) . . . . ? C15B C16B C17B C13B 17.9(10) . . . . ? C12B C13B C17B C16B -153.1(8) . . . . ? C14B C13B C17B C16B -35.1(9) . . . . ? C28B C13B C17B C16B 77.4(8) . . . . ? C12B C13B C17B C18B 78.1(11) . . . . ? C14B C13B C17B C18B -163.9(8) . . . . ? C28B C13B C17B C18B -51.4(11) . . . . ? C16B C17B C18B C27B -174.8(8) . . . . ? C13B C17B C18B C27B -49.4(12) . . . . ? C16B C17B C18B C19B 61.0(11) . . . . ? C13B C17B C18B C19B -173.5(8) . . . . ? C27B C18B C19B C20B 72.7(11) . . . . ? C17B C18B C19B C20B -161.8(9) . . . . ? C18B C19B C20B C21B 73.1(13) . . . . ? C19B C20B C21B C22B -156.0(9) . . . . ? C19B C20B C21B C25B 82.2(11) . . . . ? C25B C21B C22B C23B 75.6(15) . . . . ? C20B C21B C22B C23B -38.4(15) . . . . ? C25B C21B C22B C24B -167.0(12) . . . . ? C20B C21B C22B C24B 78.9(14) . . . . ? C22B C21B C25B C26B 68.1(17) . . . . ? C20B C21B C25B C26B -168.9(13) . . . . ? C5 O3 C2 C6 123.1(7) . . . . ? C5 O3 C2 C1 -116.9(7) . . . . ? C5 O3 C2 C3 -1.4(8) . . . . ? O1 C1 C2 O3 15.9(11) . . . . ? O2 C1 C2 O3 -168.3(6) . . . . ? O1 C1 C2 C6 133.0(9) . . . . ? O2 C1 C2 C6 -51.2(9) . . . . ? O1 C1 C2 C3 -99.5(10) . . . . ? O2 C1 C2 C3 76.2(8) . . . . ? O3 C2 C3 C4 1.0(8) . . . . ? C6 C2 C3 C4 -119.5(7) . . . . ? C1 C2 C3 C4 114.3(7) . . . . ? C2 C3 C4 O4 179(100) . . . . ? C2 C3 C4 C5 -0.3(10) . . . . ? O4 C4 C5 O5 -1.4(17) . . . . ? C3 C4 C5 O5 177.7(10) . . . . ? O4 C4 C5 O3 -179.8(6) . . . . ? C3 C4 C5 O3 -0.6(12) . . . . ? C2 O3 C5 O5 -177.4(8) . . . . ? C2 O3 C5 C4 1.2(9) . . . . ?