#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:43:34 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252628 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240606.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_7240606 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), C3 H6 O2, H2 O' _chemical_formula_sum 'C61 H108 O5' _chemical_formula_weight 921.47 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 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 95.216(6) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.439(2) _cell_length_b 7.5391(16) _cell_length_c 39.635(8) _cell_measurement_reflns_used 1723 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.63 _cell_measurement_theta_min 2.27 _cell_volume 2808.8(10) _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 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'D8 Venture' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.4570 _diffrn_reflns_av_unetI/netI 0.5301 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_number 53621 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.656 _diffrn_reflns_theta_min 2.064 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.090 _exptl_crystal_description prism _exptl_crystal_F_000 1028 _exptl_crystal_size_max 0.353 _exptl_crystal_size_mid 0.071 _exptl_crystal_size_min 0.032 _refine_diff_density_max 0.339 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack -1(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.743 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 599 _refine_ls_number_reflns 12975 _refine_ls_number_restraints 9 _refine_ls_restrained_S_all 0.744 _refine_ls_R_factor_all 0.3086 _refine_ls_R_factor_gt 0.0446 _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^)+(0.0101P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.0920 _reflns_Friedel_coverage 0.858 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.993 _reflns_number_gt 3544 _reflns_number_total 12975 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00704h2.cif _cod_data_source_block 023TB101_0ma_aa _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7240606 _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_023TB101_0ma_a.res in P1 New: P21 mo_023tb101_0ma_aa.res created by SHELXL-2018/1 at 18:07:11 on 21-Apr-2020 CELL 0.71073 9.4390 7.5391 39.6350 90.000 95.216 90.000 ZERR 2 0.0020 0.0016 0.0080 0.000 0.006 0.000 LATT -1 SYMM - X , 0.50000 + Y , - Z SFAC C H O UNIT 122 216 10 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! MERG 0 L.S. 10 FMAP 2 PLAN -20 ACTA BOND $H CONF TWIN DELU 0.001 c22 c23 DELU 0.001 c22 c24 DELU 0.001 c26 c25 DELU 0.001 c3 c7 DELU 0.001 c25a c26a EADP c11a c11 WGHT 0.010100 BASF -1.03871 FVAR 9.85097 O1 3 -0.207063 0.328603 0.063910 11.00000 0.03501 0.08828 = 0.01315 -0.00145 0.00175 0.02010 AFIX 83 H1O 2 -0.147784 0.300322 0.051000 11.00000 -1.50000 AFIX 0 C1 1 -0.146861 0.308897 0.098445 11.00000 0.02088 0.07579 = 0.01265 -0.00606 0.00220 0.01199 AFIX 13 H1 2 -0.048219 0.268645 0.098247 11.00000 -1.20000 AFIX 0 C2 1 -0.226481 0.175272 0.116791 11.00000 0.04989 0.02971 = 0.02338 -0.00566 0.00230 0.00289 AFIX 23 H2A 2 -0.216937 0.060322 0.106240 11.00000 -1.20000 H2B 2 -0.326620 0.206342 0.114566 11.00000 -1.20000 AFIX 0 C3 1 -0.175622 0.160936 0.154290 11.00000 0.03100 0.03219 = 0.02007 -0.00705 -0.00042 0.01772 C4 1 -0.163041 0.333255 0.173475 11.00000 0.01441 0.02522 = 0.01500 0.00343 0.00582 -0.00634 C5 1 -0.084545 0.467988 0.152791 11.00000 0.02358 0.04663 = 0.01645 0.00476 -0.00196 -0.01972 AFIX 23 H5A 2 -0.085889 0.582536 0.163901 11.00000 -1.20000 H5B 2 0.014062 0.431578 0.152905 11.00000 -1.20000 AFIX 0 C6 1 -0.146622 0.489267 0.116098 11.00000 0.03910 0.04238 = 0.02369 0.00892 -0.00270 -0.02280 AFIX 23 H6A 2 -0.089963 0.573011 0.104493 11.00000 -1.20000 H6B 2 -0.242970 0.534712 0.115460 11.00000 -1.20000 AFIX 0 C7 1 -0.152883 0.005330 0.168095 11.00000 0.02314 0.02827 = 0.02219 -0.00692 0.00184 0.00058 AFIX 43 H7 2 -0.170255 -0.093964 0.154419 11.00000 -1.20000 AFIX 0 C8 1 -0.100500 -0.024457 0.204609 11.00000 0.02952 0.02698 = 0.02083 -0.00023 -0.00217 -0.00057 AFIX 23 H8A 2 0.000046 -0.053234 0.206184 11.00000 -1.20000 H8B 2 -0.150502 -0.124628 0.213287 11.00000 -1.20000 AFIX 0 C9 1 -0.123014 0.138210 0.226274 11.00000 0.01711 0.02550 = 0.01643 -0.00437 -0.00440 -0.00328 AFIX 13 H9 2 -0.224436 0.147272 0.229538 11.00000 -1.20000 AFIX 0 C10 1 -0.078063 0.306432 0.208286 11.00000 0.01374 0.01408 = 0.01615 0.00357 0.00140 0.00140 AFIX 13 H10 2 0.021070 0.287825 0.203644 11.00000 -1.20000 AFIX 0 C11 1 -0.038865 0.124167 0.261091 11.00000 0.00799 0.01382 = 0.02189 -0.00033 0.00334 0.00394 AFIX 13 H11 2 0.061585 0.118381 0.256738 11.00000 -1.20000 AFIX 0 C12 1 -0.051473 0.280465 0.284877 11.00000 0.01872 0.02012 = 0.01070 0.00747 0.00138 -0.00073 C13 1 0.004206 0.441072 0.266735 11.00000 0.03162 0.02466 = 0.01564 -0.00430 0.00051 -0.00495 AFIX 23 H13A 2 0.104399 0.424369 0.263982 11.00000 -1.20000 H13B 2 -0.005151 0.546195 0.280468 11.00000 -1.20000 AFIX 0 C14 1 -0.077743 0.468716 0.231722 11.00000 0.03442 0.01148 = 0.02158 0.00774 -0.00439 -0.00438 AFIX 23 H14A 2 -0.175383 0.499665 0.234906 11.00000 -1.20000 H14B 2 -0.036003 0.568141 0.220656 11.00000 -1.20000 AFIX 0 C15 1 -0.065948 -0.039114 0.282572 11.00000 0.04471 0.02419 = 0.03105 0.00679 -0.01583 -0.00555 AFIX 23 H15A 2 -0.020383 -0.143744 0.274281 11.00000 -1.20000 H15B 2 -0.166959 -0.061716 0.282949 11.00000 -1.20000 AFIX 0 C16 1 0.003772 0.016925 0.318577 11.00000 0.03774 0.02642 = 0.02542 0.00537 -0.00088 -0.00540 AFIX 23 H16A 2 -0.062478 -0.001798 0.335566 11.00000 -1.20000 H16B 2 0.088627 -0.052810 0.324658 11.00000 -1.20000 AFIX 0 C17 1 0.042088 0.216171 0.316439 11.00000 0.01731 0.01586 = 0.01692 -0.00077 0.00129 0.00124 AFIX 13 H17 2 0.141435 0.223573 0.311225 11.00000 -1.20000 AFIX 0 C18 1 0.031854 0.307940 0.350829 11.00000 0.02021 0.01505 = 0.02528 -0.00185 0.00788 -0.00121 AFIX 13 H18 2 -0.065105 0.292336 0.357319 11.00000 -1.20000 AFIX 0 C19 1 0.134607 0.219006 0.377646 11.00000 0.02025 0.03155 = 0.01642 0.00591 -0.00083 -0.00306 AFIX 23 H19A 2 0.230670 0.234759 0.371304 11.00000 -1.20000 H19B 2 0.114975 0.092697 0.377400 11.00000 -1.20000 AFIX 0 C20 1 0.128925 0.287367 0.414073 11.00000 0.02857 0.04869 = 0.01816 0.00373 0.00152 0.00605 AFIX 23 H20A 2 0.186763 0.393661 0.416740 11.00000 -1.20000 H20B 2 0.031629 0.321456 0.416911 11.00000 -1.20000 AFIX 0 C21 1 0.177062 0.162559 0.441740 11.00000 0.05692 0.07088 = 0.01394 0.00174 0.00283 0.01515 AFIX 13 H21 2 0.110966 0.062497 0.438470 11.00000 -1.20000 AFIX 0 C22 1 0.158179 0.227183 0.477582 11.00000 0.10309 0.06468 = 0.02207 0.00200 0.00298 0.04699 AFIX 13 H22 2 0.184568 0.131729 0.493726 11.00000 -1.20000 AFIX 0 EADP c23 c24 c26 C23 1 0.002318 0.283885 0.481205 11.00000 0.09598 0.08774 = 0.04998 0.00517 0.01365 0.02950 AFIX 137 H23A 2 -0.017940 0.391903 0.468875 11.00000 -1.20000 H23B 2 -0.010400 0.302472 0.504701 11.00000 -1.20000 H23C 2 -0.061166 0.192373 0.472283 11.00000 -1.20000 AFIX 0 C24 1 0.244791 0.386167 0.486975 11.00000 0.09598 0.08774 = 0.04998 0.00517 0.01365 0.02950 AFIX 137 H24A 2 0.342848 0.362006 0.484125 11.00000 -1.20000 H24B 2 0.235199 0.416048 0.510201 11.00000 -1.20000 H24C 2 0.212534 0.483622 0.472693 11.00000 -1.20000 AFIX 0 C25 1 0.319633 0.081783 0.438257 11.00000 0.04820 0.10415 = 0.02799 -0.00044 -0.00273 0.02296 AFIX 23 H25A 2 0.317836 0.031165 0.415722 11.00000 -1.20000 H25B 2 0.389177 0.176832 0.439547 11.00000 -1.20000 AFIX 0 C26 1 0.372036 -0.058133 0.463051 11.00000 0.09598 0.08774 = 0.04998 0.00517 0.01365 0.02950 AFIX 137 H26A 2 0.305857 -0.155099 0.461986 11.00000 -1.20000 H26B 2 0.380648 -0.009198 0.485506 11.00000 -1.20000 H26C 2 0.463254 -0.099953 0.457585 11.00000 -1.20000 AFIX 0 C27 1 -0.313782 0.404322 0.177524 11.00000 0.01982 0.04330 = 0.01331 0.00299 0.00028 -0.00774 AFIX 137 H27A 2 -0.370589 0.396273 0.156224 11.00000 -1.50000 H27B 2 -0.307883 0.525939 0.184692 11.00000 -1.50000 H27C 2 -0.356700 0.334988 0.194177 11.00000 -1.50000 AFIX 0 C28 1 -0.204213 0.311348 0.293378 11.00000 0.02206 0.05145 = 0.01767 -0.00465 0.00220 0.00027 AFIX 137 H28A 2 -0.265439 0.322734 0.272787 11.00000 -1.50000 H28B 2 -0.208442 0.418023 0.306474 11.00000 -1.50000 H28C 2 -0.234726 0.212689 0.306212 11.00000 -1.50000 AFIX 0 C29 1 0.062051 0.504441 0.349134 11.00000 0.03750 0.03343 = 0.01413 -0.01256 -0.00283 0.00331 AFIX 137 H29A 2 0.154042 0.522480 0.341180 11.00000 -1.50000 H29B 2 0.060476 0.555445 0.371290 11.00000 -1.50000 H29C 2 -0.009183 0.560221 0.333856 11.00000 -1.50000 AFIX 0 O1A 3 0.151104 0.973259 0.026867 11.00000 0.02460 0.02626 = 0.01380 -0.00153 0.00285 -0.00400 AFIX 148 H1AA 2 0.226254 0.954464 0.019754 11.00000 -1.50000 AFIX 0 C1A 1 0.164722 0.952911 0.063721 11.00000 0.02636 0.02590 = 0.00620 0.00032 0.00352 0.00678 AFIX 13 H1A 2 0.074638 0.987420 0.072346 11.00000 -1.20000 AFIX 0 C2A 1 0.280156 1.069580 0.079544 11.00000 0.03189 0.01273 = 0.01463 -0.00038 -0.00727 0.00116 AFIX 23 H2AA 2 0.258081 1.192262 0.073872 11.00000 -1.20000 H2AB 2 0.369128 1.039904 0.070433 11.00000 -1.20000 AFIX 0 C3A 1 0.297275 1.048672 0.117937 11.00000 0.03542 0.02002 = 0.00792 -0.00082 0.00121 -0.00157 C4A 1 0.318316 0.861355 0.130560 11.00000 0.01715 0.01413 = 0.02102 -0.00213 0.00224 -0.00200 C5A 1 0.202808 0.741299 0.111864 11.00000 0.04324 0.01805 = 0.01601 -0.00745 -0.00211 -0.00786 AFIX 23 H5AA 2 0.222493 0.618766 0.118114 11.00000 -1.20000 H5AB 2 0.110930 0.771934 0.119372 11.00000 -1.20000 AFIX 0 C6A 1 0.194752 0.757947 0.072808 11.00000 0.02644 0.02339 = 0.01096 -0.00412 -0.00519 -0.00976 AFIX 23 H6AA 2 0.283960 0.720949 0.064649 11.00000 -1.20000 H6AB 2 0.119359 0.683128 0.062418 11.00000 -1.20000 AFIX 0 C7A 1 0.305369 1.188066 0.137798 11.00000 0.02398 0.02387 = 0.01577 0.00580 -0.00076 -0.00249 AFIX 43 H7A 2 0.300777 1.299242 0.127591 11.00000 -1.20000 AFIX 0 C8A 1 0.321427 1.181401 0.175621 11.00000 0.02169 0.00967 = 0.02227 -0.00456 0.00403 -0.00475 AFIX 23 H8AA 2 0.230045 1.205040 0.184085 11.00000 -1.20000 H8AB 2 0.386972 1.273500 0.184140 11.00000 -1.20000 AFIX 0 C9A 1 0.376502 1.001511 0.188945 11.00000 0.00899 0.01472 = 0.00941 0.00079 -0.00096 0.00504 AFIX 13 H9A 2 0.477963 0.992996 0.185690 11.00000 -1.20000 AFIX 0 C10A 1 0.298285 0.852914 0.169134 11.00000 0.01637 0.00744 = 0.01227 -0.00083 -0.00217 -0.00347 AFIX 13 H10A 2 0.196797 0.873332 0.171055 11.00000 -1.20000 AFIX 0 C11A 1 0.358822 0.982844 0.226661 11.00000 0.00799 0.01382 = 0.02189 -0.00033 0.00334 0.00394 AFIX 13 H11A 2 0.256086 0.985096 0.228622 11.00000 -1.20000 AFIX 0 C12A 1 0.411723 0.807374 0.242188 11.00000 0.01420 0.02097 = 0.00961 -0.00096 -0.00062 -0.01406 C13A 1 0.322509 0.661158 0.223866 11.00000 0.02210 0.01405 = 0.01622 0.00301 -0.00706 -0.00106 AFIX 23 H13C 2 0.223989 0.674285 0.228572 11.00000 -1.20000 H13D 2 0.355661 0.546420 0.232382 11.00000 -1.20000 AFIX 0 C14A 1 0.332180 0.668557 0.185099 11.00000 0.02084 0.02990 = 0.00782 -0.00240 -0.00329 -0.00321 AFIX 23 H14C 2 0.427458 0.634317 0.180384 11.00000 -1.20000 H14D 2 0.266548 0.582383 0.174298 11.00000 -1.20000 AFIX 0 C15A 1 0.422643 1.127306 0.250786 11.00000 0.01451 0.01978 = 0.01864 -0.00027 0.00189 -0.00441 AFIX 23 H15C 2 0.361786 1.231145 0.250183 11.00000 -1.20000 H15D 2 0.516327 1.162183 0.244986 11.00000 -1.20000 AFIX 0 C16A 1 0.431242 1.036061 0.286374 11.00000 0.02264 0.01686 = 0.01734 -0.00802 -0.00013 -0.00522 AFIX 23 H16C 2 0.526715 1.045746 0.297544 11.00000 -1.20000 H16D 2 0.365566 1.091882 0.300559 11.00000 -1.20000 AFIX 0 C17A 1 0.391451 0.840506 0.280249 11.00000 0.00331 0.01957 = 0.01849 0.00143 -0.00143 -0.00285 AFIX 13 H17A 2 0.288963 0.832131 0.282274 11.00000 -1.20000 AFIX 0 C18A 1 0.463485 0.719834 0.308093 11.00000 0.01898 0.00812 = 0.01127 -0.00503 -0.00248 0.00419 AFIX 13 H18A 2 0.566412 0.738515 0.308630 11.00000 -1.20000 AFIX 0 C19A 1 0.417192 0.775522 0.342782 11.00000 0.02160 0.02767 = 0.01333 0.00285 0.00110 -0.00277 AFIX 23 H19C 2 0.449649 0.896005 0.347290 11.00000 -1.20000 H19D 2 0.314043 0.777414 0.341156 11.00000 -1.20000 AFIX 0 C20A 1 0.468816 0.662081 0.372978 11.00000 0.01563 0.02836 = 0.01990 -0.00770 -0.00346 0.00212 AFIX 23 H20C 2 0.431096 0.543240 0.369346 11.00000 -1.20000 H20D 2 0.429866 0.709568 0.392919 11.00000 -1.20000 AFIX 0 C21A 1 0.630644 0.649482 0.380168 11.00000 0.02268 0.02759 = 0.01991 -0.00086 0.00013 -0.01421 AFIX 13 H21A 2 0.669830 0.624662 0.358595 11.00000 -1.20000 AFIX 0 C22A 1 0.681031 0.497433 0.405302 11.00000 0.03419 0.02645 = 0.03149 -0.00004 -0.00019 0.00324 AFIX 13 H22A 2 0.785066 0.502960 0.408772 11.00000 -1.20000 AFIX 0 C23A 1 0.622899 0.520823 0.440386 11.00000 0.06325 0.05690 = 0.02422 0.01652 0.00008 0.02344 AFIX 137 H23D 2 0.520797 0.521828 0.437658 11.00000 -1.50000 H23E 2 0.656819 0.630803 0.450302 11.00000 -1.50000 H23F 2 0.655092 0.424319 0.454918 11.00000 -1.50000 AFIX 0 C24A 1 0.640470 0.311900 0.390438 11.00000 0.03886 0.04000 = 0.03940 -0.00210 0.00115 -0.00106 AFIX 137 H24D 2 0.669907 0.302987 0.367945 11.00000 -1.50000 H24E 2 0.539301 0.296201 0.389680 11.00000 -1.50000 H24F 2 0.687117 0.221761 0.404498 11.00000 -1.50000 AFIX 0 C25A 1 0.687408 0.833024 0.392481 11.00000 0.04302 0.03324 = 0.05487 -0.01070 -0.01863 -0.00943 AFIX 23 H25C 2 0.667053 0.918013 0.374312 11.00000 -1.20000 H25D 2 0.635648 0.870213 0.411316 11.00000 -1.20000 AFIX 0 C26A 1 0.845947 0.839720 0.403652 11.00000 0.03600 0.07355 = 0.06326 -0.01087 -0.00023 -0.01004 AFIX 137 H26D 2 0.898556 0.799298 0.385508 11.00000 -1.50000 H26E 2 0.866309 0.764650 0.423052 11.00000 -1.50000 H26F 2 0.872953 0.959436 0.409442 11.00000 -1.50000 AFIX 0 C27A 1 0.466941 0.791977 0.123443 11.00000 0.02913 0.03457 = 0.01376 -0.00403 -0.00249 0.00908 AFIX 137 H27D 2 0.472149 0.666693 0.127706 11.00000 -1.50000 H27E 2 0.538620 0.851649 0.137988 11.00000 -1.50000 H27F 2 0.482284 0.814535 0.100216 11.00000 -1.50000 AFIX 0 C28A 1 0.571611 0.778324 0.238905 11.00000 0.01765 0.01702 = 0.01719 0.00656 0.00638 0.00785 AFIX 137 H28D 2 0.589010 0.781418 0.215422 11.00000 -1.50000 H28E 2 0.599931 0.665122 0.248345 11.00000 -1.50000 H28F 2 0.625423 0.870346 0.250905 11.00000 -1.50000 AFIX 0 C29A 1 0.434431 0.519590 0.301454 11.00000 0.02917 0.02312 = 0.01822 -0.00545 0.00191 -0.00176 AFIX 137 H29D 2 0.333714 0.498514 0.299445 11.00000 -1.50000 H29E 2 0.478663 0.451395 0.319971 11.00000 -1.50000 H29F 2 0.472951 0.485044 0.280839 11.00000 -1.50000 AFIX 0 O1W 3 0.585310 0.395176 -0.007196 11.00000 0.02214 0.07214 = 0.01960 0.00347 0.00430 -0.00307 O2W 3 0.523696 0.397498 0.045670 11.00000 0.02428 0.06917 = 0.02154 0.00103 0.00036 -0.01204 AFIX 83 H20 2 0.609478 0.384002 0.050274 11.00000 -1.20000 AFIX 0 C1W 1 0.495143 0.404529 0.012217 11.00000 0.03944 0.03085 = 0.01739 -0.00201 -0.00433 -0.00236 C2W 1 0.339055 0.427496 0.002306 11.00000 0.02214 0.05045 = 0.03523 0.01089 0.00690 -0.00422 AFIX 23 H2WA 2 0.313901 0.550740 0.005475 11.00000 -1.20000 H2WB 2 0.286283 0.356501 0.017287 11.00000 -1.20000 AFIX 0 C3W 1 0.294657 0.375420 -0.033705 11.00000 0.03465 0.06350 = 0.02912 0.00537 -0.01044 0.00862 AFIX 137 H3WA 2 0.194898 0.398208 -0.038716 11.00000 -1.50000 H3WB 2 0.313002 0.251418 -0.036683 11.00000 -1.50000 H3WC 2 0.347706 0.443367 -0.048722 11.00000 -1.50000 AFIX 0 EQIV $1 -x,-0.5+y,-z DFIX 0.83 0.01 o3w h3we DFIX 0.83 0.01 o3w h3wd DFIX 1.9 0.01 h3we o1a_$1 O3W 3 0.005009 0.297705 0.024739 11.00000 0.03489 0.04800 = 0.02514 0.00598 0.00339 0.01783 H3WD 2 0.038080 0.201658 0.019458 11.00000 -1.20000 H3WE 2 -0.034389 0.342241 0.006799 11.00000 -1.20000 HKLF 4 1 REM mo_023TB101_0ma_a.res in P1 New: P21 REM R1 = 0.0446 for 3544 Fo > 4sig(Fo) and 0.3086 for all 12975 data REM 599 parameters refined using 9 restraints END WGHT 0.0101 0.0000 REM Highest difference peak 0.339, deepest hole -0.328, 1-sigma level 0.051 Q1 1 0.2793 0.3518 0.4879 11.00000 0.05 0.32 Q2 1 0.4129 0.9467 0.2850 11.00000 0.05 0.22 Q3 1 0.1493 0.3013 0.3801 11.00000 0.05 0.21 Q4 1 -0.0408 0.3489 0.0261 11.00000 0.05 0.20 Q5 1 0.0886 0.2892 0.3493 11.00000 0.05 0.20 Q6 1 0.2767 0.2797 -0.0294 11.00000 0.05 0.20 Q7 1 0.4113 0.7822 0.2964 11.00000 0.05 0.20 Q8 1 0.3480 0.8624 0.0526 11.00000 0.05 0.20 Q9 1 0.4104 1.0442 0.2366 11.00000 0.05 0.20 Q10 1 0.3262 0.7828 0.1800 11.00000 0.05 0.19 Q11 1 0.3240 0.9484 0.1816 11.00000 0.05 0.19 Q12 1 0.2812 1.1448 0.0843 11.00000 0.05 0.19 Q13 1 -0.0841 0.1599 0.1447 11.00000 0.05 0.18 Q14 1 -0.1096 0.4097 -0.0233 11.00000 0.05 0.18 Q15 1 0.3406 0.0701 0.4458 11.00000 0.05 0.18 Q16 1 0.0270 0.1477 0.2507 11.00000 0.05 0.18 Q17 1 0.4617 0.0319 0.4657 11.00000 0.05 0.18 Q18 1 0.4317 1.0195 0.1824 11.00000 0.05 0.18 Q19 1 0.2189 -0.0273 0.4452 11.00000 0.05 0.18 Q20 1 -0.2001 0.2810 0.1637 11.00000 0.05 0.18 ; _shelx_res_checksum 1517 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 O1 O -0.2071(4) 0.3286(6) 0.06391(8) 0.0455(14) Uani 1 1 d . . . . . H1O H -0.147784 0.300322 0.051000 0.068 Uiso 1 1 calc R U . . . C1 C -0.1469(7) 0.3089(10) 0.09845(13) 0.036(2) Uani 1 1 d . . . . . H1 H -0.048219 0.268645 0.098247 0.044 Uiso 1 1 calc R U . . . C2 C -0.2265(7) 0.1753(8) 0.11679(13) 0.034(2) Uani 1 1 d . . . . . H2A H -0.216937 0.060322 0.106240 0.041 Uiso 1 1 calc R U . . . H2B H -0.326620 0.206342 0.114566 0.041 Uiso 1 1 calc R U . . . C3 C -0.1756(7) 0.1609(8) 0.15429(14) 0.0279(19) Uani 1 1 d . U . . . C4 C -0.1630(6) 0.3333(8) 0.17348(13) 0.0179(16) Uani 1 1 d . . . . . C5 C -0.0845(6) 0.4680(8) 0.15279(12) 0.0291(18) Uani 1 1 d . . . . . H5A H -0.085889 0.582536 0.163901 0.035 Uiso 1 1 calc R U . . . H5B H 0.014062 0.431578 0.152905 0.035 Uiso 1 1 calc R U . . . C6 C -0.1466(6) 0.4893(8) 0.11610(13) 0.0354(19) Uani 1 1 d . . . . . H6A H -0.089963 0.573011 0.104493 0.042 Uiso 1 1 calc R U . . . H6B H -0.242970 0.534712 0.115460 0.042 Uiso 1 1 calc R U . . . C7 C -0.1529(6) 0.0053(8) 0.16809(13) 0.0245(17) Uani 1 1 d . U . . . H7 H -0.170255 -0.093964 0.154419 0.029 Uiso 1 1 calc R U . . . C8 C -0.1005(6) -0.0245(7) 0.20461(12) 0.0260(17) Uani 1 1 d . . . . . H8A H 0.000046 -0.053234 0.206184 0.031 Uiso 1 1 calc R U . . . H8B H -0.150502 -0.124628 0.213287 0.031 Uiso 1 1 calc R U . . . C9 C -0.1230(6) 0.1382(8) 0.22627(13) 0.0200(16) Uani 1 1 d . . . . . H9 H -0.224436 0.147272 0.229538 0.024 Uiso 1 1 calc R U . . . C10 C -0.0781(6) 0.3064(7) 0.20829(12) 0.0147(15) Uani 1 1 d . . . . . H10 H 0.021070 0.287825 0.203644 0.018 Uiso 1 1 calc R U . . . C11 C -0.0389(6) 0.1242(7) 0.26109(13) 0.0144(11) Uani 1 1 d . . . . . H11 H 0.061585 0.118381 0.256738 0.017 Uiso 1 1 calc R U . . . C12 C -0.0515(6) 0.2805(8) 0.28488(13) 0.0165(16) Uani 1 1 d . . . . . C13 C 0.0042(6) 0.4411(7) 0.26674(12) 0.0241(17) Uani 1 1 d . . . . . H13A H 0.104399 0.424369 0.263982 0.029 Uiso 1 1 calc R U . . . H13B H -0.005151 0.546195 0.280468 0.029 Uiso 1 1 calc R U . . . C14 C -0.0777(6) 0.4687(7) 0.23172(12) 0.0229(17) Uani 1 1 d . . . . . H14A H -0.175383 0.499665 0.234906 0.028 Uiso 1 1 calc R U . . . H14B H -0.036003 0.568141 0.220656 0.028 Uiso 1 1 calc R U . . . C15 C -0.0659(6) -0.0391(7) 0.28257(13) 0.0345(18) Uani 1 1 d . . . . . H15A H -0.020383 -0.143744 0.274281 0.041 Uiso 1 1 calc R U . . . H15B H -0.166959 -0.061716 0.282949 0.041 Uiso 1 1 calc R U . . . C16 C 0.0038(6) 0.0169(7) 0.31858(13) 0.0301(18) Uani 1 1 d . . . . . H16A H -0.062478 -0.001798 0.335566 0.036 Uiso 1 1 calc R U . . . H16B H 0.088627 -0.052810 0.324658 0.036 Uiso 1 1 calc R U . . . C17 C 0.0421(6) 0.2162(7) 0.31644(13) 0.0167(16) Uani 1 1 d . . . . . H17 H 0.141435 0.223573 0.311225 0.020 Uiso 1 1 calc R U . . . C18 C 0.0319(6) 0.3079(7) 0.35083(13) 0.0198(16) Uani 1 1 d . . . . . H18 H -0.065105 0.292336 0.357319 0.024 Uiso 1 1 calc R U . . . C19 C 0.1346(6) 0.2190(7) 0.37765(12) 0.0229(18) Uani 1 1 d . . . . . H19A H 0.230670 0.234759 0.371304 0.027 Uiso 1 1 calc R U . . . H19B H 0.114975 0.092697 0.377400 0.027 Uiso 1 1 calc R U . . . C20 C 0.1289(6) 0.2874(8) 0.41407(13) 0.0318(18) Uani 1 1 d . . . . . H20A H 0.186763 0.393661 0.416740 0.038 Uiso 1 1 calc R U . . . H20B H 0.031629 0.321456 0.416911 0.038 Uiso 1 1 calc R U . . . C21 C 0.1771(8) 0.1626(9) 0.44174(14) 0.047(2) Uani 1 1 d . . . . . H21 H 0.110966 0.062497 0.438470 0.057 Uiso 1 1 calc R U . . . C22 C 0.1582(8) 0.2272(9) 0.47758(16) 0.063(2) Uani 1 1 d . U . . . H22 H 0.184568 0.131729 0.493726 0.076 Uiso 1 1 calc R U . . . C23 C 0.0023(7) 0.2839(9) 0.48121(14) 0.0775(16) Uani 1 1 d . U . . . H23A H -0.017940 0.391903 0.468875 0.093 Uiso 1 1 calc R U . . . H23B H -0.010400 0.302472 0.504701 0.093 Uiso 1 1 calc R U . . . H23C H -0.061166 0.192373 0.472283 0.093 Uiso 1 1 calc R U . . . C24 C 0.2448(7) 0.3862(10) 0.48697(16) 0.0775(16) Uani 1 1 d . U . . . H24A H 0.342848 0.362006 0.484125 0.093 Uiso 1 1 calc R U . . . H24B H 0.235199 0.416048 0.510201 0.093 Uiso 1 1 calc R U . . . H24C H 0.212534 0.483622 0.472693 0.093 Uiso 1 1 calc R U . . . C25 C 0.3196(7) 0.0818(9) 0.43826(14) 0.060(2) Uani 1 1 d . U . . . H25A H 0.317836 0.031165 0.415722 0.073 Uiso 1 1 calc R U . . . H25B H 0.389177 0.176832 0.439547 0.073 Uiso 1 1 calc R U . . . C26 C 0.3720(7) -0.0581(8) 0.46305(14) 0.0775(16) Uani 1 1 d . U . . . H26A H 0.305857 -0.155099 0.461986 0.093 Uiso 1 1 calc R U . . . H26B H 0.380648 -0.009198 0.485506 0.093 Uiso 1 1 calc R U . . . H26C H 0.463254 -0.099953 0.457585 0.093 Uiso 1 1 calc R U . . . C27 C -0.3138(5) 0.4043(7) 0.17752(12) 0.0256(17) Uani 1 1 d . . . . . H27A H -0.370589 0.396273 0.156224 0.038 Uiso 1 1 calc R U . . . H27B H -0.307883 0.525939 0.184692 0.038 Uiso 1 1 calc R U . . . H27C H -0.356700 0.334988 0.194177 0.038 Uiso 1 1 calc R U . . . C28 C -0.2042(5) 0.3113(8) 0.29338(12) 0.0304(18) Uani 1 1 d . . . . . H28A H -0.265439 0.322734 0.272787 0.046 Uiso 1 1 calc R U . . . H28B H -0.208442 0.418023 0.306474 0.046 Uiso 1 1 calc R U . . . H28C H -0.234726 0.212689 0.306212 0.046 Uiso 1 1 calc R U . . . C29 C 0.0621(6) 0.5044(7) 0.34913(12) 0.0287(18) Uani 1 1 d . . . . . H29A H 0.154042 0.522480 0.341180 0.043 Uiso 1 1 calc R U . . . H29B H 0.060476 0.555445 0.371290 0.043 Uiso 1 1 calc R U . . . H29C H -0.009183 0.560221 0.333856 0.043 Uiso 1 1 calc R U . . . O1A O 0.1511(4) 0.9733(6) 0.02687(8) 0.0215(12) Uani 1 1 d . . . . . H1AA H 0.226(5) 0.954(8) 0.0198(5) 0.032 Uiso 1 1 calc R U . . . C1A C 0.1647(6) 0.9529(7) 0.06372(12) 0.0194(16) Uani 1 1 d . . . . . H1A H 0.074638 0.987420 0.072346 0.023 Uiso 1 1 calc R U . . . C2A C 0.2802(6) 1.0696(7) 0.07954(12) 0.0203(18) Uani 1 1 d . . . . . H2AA H 0.258081 1.192262 0.073872 0.024 Uiso 1 1 calc R U . . . H2AB H 0.369128 1.039904 0.070433 0.024 Uiso 1 1 calc R U . . . C3A C 0.2973(7) 1.0487(8) 0.11794(14) 0.0212(17) Uani 1 1 d . . . . . C4A C 0.3183(6) 0.8614(7) 0.13056(14) 0.0174(17) Uani 1 1 d . . . . . C5A C 0.2028(6) 0.7413(7) 0.11186(12) 0.0261(18) Uani 1 1 d . . . . . H5AA H 0.222493 0.618766 0.118114 0.031 Uiso 1 1 calc R U . . . H5AB H 0.110930 0.771934 0.119372 0.031 Uiso 1 1 calc R U . . . C6A C 0.1948(6) 0.7579(7) 0.07281(12) 0.0207(17) Uani 1 1 d . . . . . H6AA H 0.283960 0.720949 0.064649 0.025 Uiso 1 1 calc R U . . . H6AB H 0.119359 0.683128 0.062418 0.025 Uiso 1 1 calc R U . . . C7A C 0.3054(6) 1.1881(8) 0.13780(13) 0.0214(17) Uani 1 1 d . . . . . H7A H 0.300777 1.299242 0.127591 0.026 Uiso 1 1 calc R U . . . C8A C 0.3214(6) 1.1814(6) 0.17562(12) 0.0178(16) Uani 1 1 d . . . . . H8AA H 0.230045 1.205040 0.184085 0.021 Uiso 1 1 calc R U . . . H8AB H 0.386972 1.273500 0.184140 0.021 Uiso 1 1 calc R U . . . C9A C 0.3765(6) 1.0015(7) 0.18895(12) 0.0111(15) Uani 1 1 d . . . . . H9A H 0.477963 0.992996 0.185690 0.013 Uiso 1 1 calc R U . . . C10A C 0.2983(6) 0.8529(7) 0.16913(12) 0.0122(15) Uani 1 1 d . . . . . H10A H 0.196797 0.873332 0.171055 0.015 Uiso 1 1 calc R U . . . C11A C 0.3588(6) 0.9828(7) 0.22666(13) 0.0144(11) Uani 1 1 d . . . . . H11A H 0.256086 0.985096 0.228622 0.017 Uiso 1 1 calc R U . . . C12A C 0.4117(6) 0.8074(8) 0.24219(12) 0.0150(16) Uani 1 1 d . . . . . C13A C 0.3225(6) 0.6612(7) 0.22387(12) 0.0180(16) Uani 1 1 d . . . . . H13C H 0.223989 0.674285 0.228572 0.022 Uiso 1 1 calc R U . . . H13D H 0.355661 0.546420 0.232382 0.022 Uiso 1 1 calc R U . . . C14A C 0.3322(6) 0.6686(7) 0.18510(11) 0.0198(17) Uani 1 1 d . . . . . H14C H 0.427458 0.634317 0.180384 0.024 Uiso 1 1 calc R U . . . H14D H 0.266548 0.582383 0.174298 0.024 Uiso 1 1 calc R U . . . C15A C 0.4226(6) 1.1273(7) 0.25079(12) 0.0176(16) Uani 1 1 d . . . . . H15C H 0.361786 1.231145 0.250183 0.021 Uiso 1 1 calc R U . . . H15D H 0.516327 1.162183 0.244986 0.021 Uiso 1 1 calc R U . . . C16A C 0.4312(6) 1.0361(6) 0.28637(12) 0.0191(17) Uani 1 1 d . . . . . H16C H 0.526715 1.045746 0.297544 0.023 Uiso 1 1 calc R U . . . H16D H 0.365566 1.091882 0.300559 0.023 Uiso 1 1 calc R U . . . C17A C 0.3915(6) 0.8405(7) 0.28025(12) 0.0139(16) Uani 1 1 d . . . . . H17A H 0.288963 0.832131 0.282274 0.017 Uiso 1 1 calc R U . . . C18A C 0.4635(6) 0.7198(6) 0.30809(12) 0.0130(16) Uani 1 1 d . . . . . H18A H 0.566412 0.738515 0.308630 0.016 Uiso 1 1 calc R U . . . C19A C 0.4172(6) 0.7755(7) 0.34278(11) 0.0209(16) Uani 1 1 d . . . . . H19C H 0.449649 0.896005 0.347290 0.025 Uiso 1 1 calc R U . . . H19D H 0.314043 0.777414 0.341156 0.025 Uiso 1 1 calc R U . . . C20A C 0.4688(6) 0.6621(7) 0.37298(12) 0.0216(16) Uani 1 1 d . . . . . H20C H 0.431096 0.543240 0.369346 0.026 Uiso 1 1 calc R U . . . H20D H 0.429866 0.709568 0.392919 0.026 Uiso 1 1 calc R U . . . C21A C 0.6306(6) 0.6495(8) 0.38017(14) 0.0235(17) Uani 1 1 d . . . . . H21A H 0.669830 0.624662 0.358595 0.028 Uiso 1 1 calc R U . . . C22A C 0.6810(6) 0.4974(8) 0.40530(14) 0.0309(17) Uani 1 1 d . . . . . H22A H 0.785066 0.502960 0.408772 0.037 Uiso 1 1 calc R U . . . C23A C 0.6229(6) 0.5208(8) 0.44039(13) 0.048(2) Uani 1 1 d . . . . . H23D H 0.520797 0.521828 0.437658 0.073 Uiso 1 1 calc R U . . . H23E H 0.656819 0.630803 0.450302 0.073 Uiso 1 1 calc R U . . . H23F H 0.655092 0.424319 0.454918 0.073 Uiso 1 1 calc R U . . . C24A C 0.6405(6) 0.3119(7) 0.39044(13) 0.0396(19) Uani 1 1 d . . . . . H24D H 0.669907 0.302987 0.367945 0.059 Uiso 1 1 calc R U . . . H24E H 0.539301 0.296201 0.389680 0.059 Uiso 1 1 calc R U . . . H24F H 0.687117 0.221761 0.404498 0.059 Uiso 1 1 calc R U . . . C25A C 0.6874(6) 0.8330(8) 0.39248(15) 0.045(2) Uani 1 1 d . U . . . H25C H 0.667053 0.918013 0.374312 0.054 Uiso 1 1 calc R U . . . H25D H 0.635648 0.870213 0.411316 0.054 Uiso 1 1 calc R U . . . C26A C 0.8459(6) 0.8397(9) 0.40365(14) 0.058(2) Uani 1 1 d . U . . . H26D H 0.898556 0.799298 0.385508 0.087 Uiso 1 1 calc R U . . . H26E H 0.866309 0.764650 0.423052 0.087 Uiso 1 1 calc R U . . . H26F H 0.872953 0.959436 0.409442 0.087 Uiso 1 1 calc R U . . . C27A C 0.4669(5) 0.7920(7) 0.12344(11) 0.0261(17) Uani 1 1 d . . . . . H27D H 0.472149 0.666693 0.127706 0.039 Uiso 1 1 calc R U . . . H27E H 0.538620 0.851649 0.137988 0.039 Uiso 1 1 calc R U . . . H27F H 0.482284 0.814535 0.100216 0.039 Uiso 1 1 calc R U . . . C28A C 0.5716(5) 0.7783(7) 0.23891(11) 0.0170(16) Uani 1 1 d . . . . . H28D H 0.589010 0.781418 0.215422 0.025 Uiso 1 1 calc R U . . . H28E H 0.599931 0.665122 0.248345 0.025 Uiso 1 1 calc R U . . . H28F H 0.625423 0.870346 0.250905 0.025 Uiso 1 1 calc R U . . . C29A C 0.4344(5) 0.5196(7) 0.30145(12) 0.0235(17) Uani 1 1 d . . . . . H29D H 0.333714 0.498514 0.299445 0.035 Uiso 1 1 calc R U . . . H29E H 0.478663 0.451395 0.319971 0.035 Uiso 1 1 calc R U . . . H29F H 0.472951 0.485044 0.280839 0.035 Uiso 1 1 calc R U . . . O1W O 0.5853(4) 0.3952(6) -0.00720(9) 0.0378(14) Uani 1 1 d . . . . . O2W O 0.5237(4) 0.3975(5) 0.04567(9) 0.0384(13) Uani 1 1 d . . . . . H20 H 0.609478 0.384002 0.050274 0.046 Uiso 1 1 calc R U . . . C1W C 0.4951(7) 0.4045(8) 0.01222(15) 0.0297(19) Uani 1 1 d . . . . . C2W C 0.3391(6) 0.4275(9) 0.00231(14) 0.0357(19) Uani 1 1 d . . . . . H2WA H 0.313901 0.550740 0.005475 0.043 Uiso 1 1 calc R U . . . H2WB H 0.286283 0.356501 0.017287 0.043 Uiso 1 1 calc R U . . . C3W C 0.2947(6) 0.3754(8) -0.03371(12) 0.043(2) Uani 1 1 d . . . . . H3WA H 0.194898 0.398208 -0.038716 0.065 Uiso 1 1 calc R U . . . H3WB H 0.313002 0.251418 -0.036683 0.065 Uiso 1 1 calc R U . . . H3WC H 0.347706 0.443367 -0.048722 0.065 Uiso 1 1 calc R U . . . O3W O 0.0050(5) 0.2977(6) 0.02474(10) 0.0360(12) Uani 1 1 d D . . . . H3WD H 0.038(6) 0.202(4) 0.0195(14) 0.043 Uiso 1 1 d D U . . . H3WE H -0.034(5) 0.342(6) 0.0068(8) 0.043 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 O1 0.035(3) 0.088(4) 0.013(2) -0.001(3) 0.002(2) 0.020(3) C1 0.021(5) 0.076(6) 0.013(4) -0.006(4) 0.002(3) 0.012(5) C2 0.050(6) 0.030(4) 0.023(4) -0.006(4) 0.002(4) 0.003(4) C3 0.031(5) 0.032(4) 0.020(4) -0.007(3) 0.000(4) 0.018(4) C4 0.014(4) 0.025(4) 0.015(4) 0.003(4) 0.006(3) -0.006(4) C5 0.024(4) 0.047(5) 0.016(4) 0.005(4) -0.002(3) -0.020(4) C6 0.039(5) 0.042(5) 0.024(4) 0.009(4) -0.003(4) -0.023(4) C7 0.023(4) 0.028(4) 0.022(4) -0.007(3) 0.002(3) 0.001(4) C8 0.030(4) 0.027(5) 0.021(4) 0.000(4) -0.002(3) -0.001(4) C9 0.017(4) 0.026(4) 0.016(4) -0.004(4) -0.004(3) -0.003(4) C10 0.014(4) 0.014(4) 0.016(4) 0.004(3) 0.001(3) 0.001(3) C11 0.008(3) 0.014(3) 0.022(3) 0.000(2) 0.003(2) 0.004(2) C12 0.019(4) 0.020(4) 0.011(4) 0.007(3) 0.001(3) -0.001(4) C13 0.032(4) 0.025(4) 0.016(4) -0.004(3) 0.001(3) -0.005(4) C14 0.034(4) 0.011(4) 0.022(4) 0.008(3) -0.004(3) -0.004(4) C15 0.045(5) 0.024(4) 0.031(4) 0.007(4) -0.016(4) -0.006(4) C16 0.038(5) 0.026(4) 0.025(4) 0.005(4) -0.001(4) -0.005(4) C17 0.017(4) 0.016(4) 0.017(4) -0.001(3) 0.001(3) 0.001(3) C18 0.020(4) 0.015(4) 0.025(4) -0.002(4) 0.008(3) -0.001(4) C19 0.020(4) 0.032(5) 0.016(4) 0.006(3) -0.001(3) -0.003(4) C20 0.029(4) 0.049(5) 0.018(4) 0.004(4) 0.002(3) 0.006(4) C21 0.057(6) 0.071(6) 0.014(4) 0.002(4) 0.003(4) 0.015(5) C22 0.103(5) 0.065(5) 0.022(4) 0.002(4) 0.003(5) 0.047(4) C23 0.096(4) 0.088(4) 0.050(3) 0.005(3) 0.014(3) 0.029(3) C24 0.096(4) 0.088(4) 0.050(3) 0.005(3) 0.014(3) 0.029(3) C25 0.048(6) 0.104(7) 0.028(4) 0.000(4) -0.003(4) 0.023(5) C26 0.096(4) 0.088(4) 0.050(3) 0.005(3) 0.014(3) 0.029(3) C27 0.020(4) 0.043(4) 0.013(3) 0.003(3) 0.000(3) -0.008(4) C28 0.022(4) 0.051(5) 0.018(4) -0.005(4) 0.002(3) 0.000(4) C29 0.037(5) 0.033(5) 0.014(4) -0.013(4) -0.003(3) 0.003(4) O1A 0.025(3) 0.026(3) 0.014(2) -0.002(2) 0.003(2) -0.004(3) C1A 0.026(4) 0.026(4) 0.006(3) 0.000(3) 0.004(3) 0.007(4) C2A 0.032(5) 0.013(4) 0.015(4) 0.000(3) -0.007(3) 0.001(3) C3A 0.035(5) 0.020(4) 0.008(4) -0.001(3) 0.001(3) -0.002(4) C4A 0.017(4) 0.014(4) 0.021(4) -0.002(3) 0.002(3) -0.002(3) C5A 0.043(5) 0.018(4) 0.016(4) -0.007(3) -0.002(3) -0.008(4) C6A 0.026(4) 0.023(4) 0.011(4) -0.004(3) -0.005(3) -0.010(4) C7A 0.024(5) 0.024(4) 0.016(4) 0.006(3) -0.001(3) -0.002(4) C8A 0.022(4) 0.010(4) 0.022(4) -0.005(3) 0.004(3) -0.005(3) C9A 0.009(4) 0.015(4) 0.009(3) 0.001(3) -0.001(3) 0.005(3) C10A 0.016(4) 0.007(4) 0.012(3) -0.001(3) -0.002(3) -0.003(3) C11A 0.008(3) 0.014(3) 0.022(3) 0.000(2) 0.003(2) 0.004(2) C12A 0.014(4) 0.021(4) 0.010(4) -0.001(3) -0.001(3) -0.014(4) C13A 0.022(4) 0.014(4) 0.016(4) 0.003(3) -0.007(3) -0.001(3) C14A 0.021(4) 0.030(4) 0.008(4) -0.002(3) -0.003(3) -0.003(4) C15A 0.015(4) 0.020(4) 0.019(4) 0.000(3) 0.002(3) -0.004(3) C16A 0.023(4) 0.017(4) 0.017(4) -0.008(3) 0.000(3) -0.005(3) C17A 0.003(4) 0.020(4) 0.018(4) 0.001(3) -0.001(3) -0.003(3) C18A 0.019(4) 0.008(4) 0.011(4) -0.005(3) -0.002(3) 0.004(3) C19A 0.022(4) 0.028(4) 0.013(3) 0.003(3) 0.001(3) -0.003(4) C20A 0.016(4) 0.028(4) 0.020(4) -0.008(4) -0.003(3) 0.002(4) C21A 0.023(5) 0.028(4) 0.020(4) -0.001(4) 0.000(3) -0.014(4) C22A 0.034(5) 0.026(4) 0.031(4) 0.000(4) 0.000(3) 0.003(4) C23A 0.063(6) 0.057(5) 0.024(4) 0.017(4) 0.000(4) 0.023(5) C24A 0.039(5) 0.040(5) 0.039(4) -0.002(4) 0.001(4) -0.001(4) C25A 0.043(4) 0.033(5) 0.055(5) -0.011(4) -0.019(4) -0.009(4) C26A 0.036(4) 0.074(6) 0.063(5) -0.011(5) 0.000(4) -0.010(5) C27A 0.029(4) 0.035(4) 0.014(3) -0.004(3) -0.002(3) 0.009(4) C28A 0.018(4) 0.017(4) 0.017(3) 0.007(3) 0.006(3) 0.008(4) C29A 0.029(4) 0.023(4) 0.018(4) -0.005(3) 0.002(3) -0.002(4) O1W 0.022(3) 0.072(4) 0.020(3) 0.003(3) 0.004(2) -0.003(3) O2W 0.024(3) 0.069(4) 0.022(3) 0.001(2) 0.000(2) -0.012(3) C1W 0.039(6) 0.031(4) 0.017(4) -0.002(4) -0.004(4) -0.002(4) C2W 0.022(5) 0.050(5) 0.035(4) 0.011(4) 0.007(4) -0.004(4) C3W 0.035(5) 0.064(5) 0.029(4) 0.005(4) -0.010(4) 0.009(4) O3W 0.035(3) 0.048(4) 0.025(3) 0.006(3) 0.003(2) 0.018(3) 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 C1 O1 H1O 109.5 . . ? O1 C1 C2 111.2(5) . . ? O1 C1 C6 109.1(5) . . ? C2 C1 C6 111.0(5) . . ? O1 C1 H1 108.5 . . ? C2 C1 H1 108.5 . . ? C6 C1 H1 108.5 . . ? C1 C2 C3 113.4(5) . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C7 C3 C4 124.2(6) . . ? C7 C3 C2 119.9(6) . . ? C4 C3 C2 115.8(5) . . ? C3 C4 C5 108.7(5) . . ? C3 C4 C27 108.7(5) . . ? C5 C4 C27 108.7(5) . . ? C3 C4 C10 110.4(5) . . ? C5 C4 C10 109.1(5) . . ? C27 C4 C10 111.2(4) . . ? C6 C5 C4 114.6(5) . . ? C6 C5 H5A 108.6 . . ? C4 C5 H5A 108.6 . . ? C6 C5 H5B 108.6 . . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C5 C6 C1 109.1(5) . . ? C5 C6 H6A 109.9 . . ? C1 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? C1 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C3 C7 C8 124.4(6) . . ? C3 C7 H7 117.8 . . ? C8 C7 H7 117.8 . . ? C7 C8 C9 111.8(5) . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C11 111.4(5) . . ? C8 C9 C10 110.2(4) . . ? C11 C9 C10 109.5(5) . . ? C8 C9 H9 108.6 . . ? C11 C9 H9 108.6 . . ? C10 C9 H9 108.6 . . ? C9 C10 C14 111.3(4) . . ? C9 C10 C4 112.4(5) . . ? C14 C10 C4 114.1(5) . . ? C9 C10 H10 106.1 . . ? C14 C10 H10 106.1 . . ? C4 C10 H10 106.1 . . ? C12 C11 C15 104.6(4) . . ? C12 C11 C9 116.2(5) . . ? C15 C11 C9 117.2(5) . . ? C12 C11 H11 106.0 . . ? C15 C11 H11 106.0 . . ? C9 C11 H11 106.0 . . ? C11 C12 C13 105.8(4) . . ? C11 C12 C28 112.5(5) . . ? C13 C12 C28 110.8(5) . . ? C11 C12 C17 100.8(4) . . ? C13 C12 C17 115.8(5) . . ? C28 C12 C17 110.6(4) . . ? C12 C13 C14 111.4(5) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C10 C14 C13 114.2(5) . . ? C10 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? C10 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C11 C15 C16 102.2(4) . . ? C11 C15 H15A 111.3 . . ? C16 C15 H15A 111.3 . . ? C11 C15 H15B 111.3 . . ? C16 C15 H15B 111.3 . . ? H15A C15 H15B 109.2 . . ? C17 C16 C15 106.9(5) . . ? C17 C16 H16A 110.3 . . ? C15 C16 H16A 110.3 . . ? C17 C16 H16B 110.3 . . ? C15 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C18 C17 C12 120.0(5) . . ? C18 C17 C16 110.7(4) . . ? C12 C17 C16 103.3(5) . . ? C18 C17 H17 107.4 . . ? C12 C17 H17 107.4 . . ? C16 C17 H17 107.4 . . ? C29 C18 C19 110.5(5) . . ? C29 C18 C17 112.0(4) . . ? C19 C18 C17 109.4(4) . . ? C29 C18 H18 108.3 . . ? C19 C18 H18 108.3 . . ? C17 C18 H18 108.3 . . ? C18 C19 C20 115.6(5) . . ? C18 C19 H19A 108.4 . . ? C20 C19 H19A 108.4 . . ? C18 C19 H19B 108.4 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? C21 C20 C19 116.5(5) . . ? C21 C20 H20A 108.2 . . ? C19 C20 H20A 108.2 . . ? C21 C20 H20B 108.2 . . ? C19 C20 H20B 108.2 . . ? H20A C20 H20B 107.3 . . ? C20 C21 C25 114.1(5) . . ? C20 C21 C22 115.5(6) . . ? C25 C21 C22 113.4(6) . . ? C20 C21 H21 104.0 . . ? C25 C21 H21 104.0 . . ? C22 C21 H21 104.0 . . ? C24 C22 C21 112.6(7) . . ? C24 C22 C23 105.1(6) . . ? C21 C22 C23 111.5(6) . . ? C24 C22 H22 109.2 . . ? C21 C22 H22 109.2 . . ? C23 C22 H22 109.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C21 118.3(6) . . ? C26 C25 H25A 107.7 . . ? C21 C25 H25A 107.7 . . ? C26 C25 H25B 107.7 . . ? C21 C25 H25B 107.7 . . ? H25A C25 H25B 107.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C4 C27 H27A 109.5 . . ? C4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C12 C28 H28A 109.5 . . ? C12 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C12 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C18 C29 H29A 109.5 . . ? C18 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C18 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C1A O1A H1AA 109.5 . . ? O1A C1A C2A 110.6(4) . . ? O1A C1A C6A 109.4(4) . . ? C2A C1A C6A 110.7(5) . . ? O1A C1A H1A 108.7 . . ? C2A C1A H1A 108.7 . . ? C6A C1A H1A 108.7 . . ? C1A C2A C3A 111.4(5) . . ? C1A C2A H2AA 109.3 . . ? C3A C2A H2AA 109.3 . . ? C1A C2A H2AB 109.3 . . ? C3A C2A H2AB 109.3 . . ? H2AA C2A H2AB 108.0 . . ? C7A C3A C4A 123.6(5) . . ? C7A C3A C2A 120.8(5) . . ? C4A C3A C2A 115.3(5) . . ? C3A C4A C27A 110.5(5) . . ? C3A C4A C5A 108.8(5) . . ? C27A C4A C5A 109.0(5) . . ? C3A C4A C10A 109.9(5) . . ? C27A C4A C10A 111.0(5) . . ? C5A C4A C10A 107.6(4) . . ? C6A C5A C4A 113.5(4) . . ? C6A C5A H5AA 108.9 . . ? C4A C5A H5AA 108.9 . . ? C6A C5A H5AB 108.9 . . ? C4A C5A H5AB 108.9 . . ? H5AA C5A H5AB 107.7 . . ? C1A C6A C5A 107.7(4) . . ? C1A C6A H6AA 110.2 . . ? C5A C6A H6AA 110.2 . . ? C1A C6A H6AB 110.2 . . ? C5A C6A H6AB 110.2 . . ? H6AA C6A H6AB 108.5 . . ? C3A C7A C8A 124.8(5) . . ? C3A C7A H7A 117.6 . . ? C8A C7A H7A 117.6 . . ? C7A C8A C9A 112.1(4) . . ? C7A C8A H8AA 109.2 . . ? C9A C8A H8AA 109.2 . . ? C7A C8A H8AB 109.2 . . ? C9A C8A H8AB 109.2 . . ? H8AA C8A H8AB 107.9 . . ? C10A C9A C11A 110.3(4) . . ? C10A C9A C8A 110.0(4) . . ? C11A C9A C8A 110.9(4) . . ? C10A C9A H9A 108.6 . . ? C11A C9A H9A 108.6 . . ? C8A C9A H9A 108.6 . . ? C9A C10A C14A 112.2(4) . . ? C9A C10A C4A 112.3(4) . . ? C14A C10A C4A 113.5(4) . . ? C9A C10A H10A 106.0 . . ? C14A C10A H10A 106.0 . . ? C4A C10A H10A 106.0 . . ? C12A C11A C9A 114.5(4) . . ? C12A C11A C15A 105.6(4) . . ? C9A C11A C15A 118.2(5) . . ? C12A C11A H11A 105.9 . . ? C9A C11A H11A 105.9 . . ? C15A C11A H11A 105.9 . . ? C11A C12A C13A 106.7(4) . . ? C11A C12A C28A 112.1(4) . . ? C13A C12A C28A 111.0(5) . . ? C11A C12A C17A 100.8(5) . . ? C13A C12A C17A 117.7(4) . . ? C28A C12A C17A 108.2(4) . . ? C12A C13A C14A 111.4(4) . . ? C12A C13A H13C 109.3 . . ? C14A C13A H13C 109.3 . . ? C12A C13A H13D 109.3 . . ? C14A C13A H13D 109.3 . . ? H13C C13A H13D 108.0 . . ? C10A C14A C13A 114.2(4) . . ? C10A C14A H14C 108.7 . . ? C13A C14A H14C 108.7 . . ? C10A C14A H14D 108.7 . . ? C13A C14A H14D 108.7 . . ? H14C C14A H14D 107.6 . . ? C11A C15A C16A 103.6(4) . . ? C11A C15A H15C 111.0 . . ? C16A C15A H15C 111.0 . . ? C11A C15A H15D 111.0 . . ? C16A C15A H15D 111.0 . . ? H15C C15A H15D 109.0 . . ? C17A C16A C15A 106.7(4) . . ? C17A C16A H16C 110.4 . . ? C15A C16A H16C 110.4 . . ? C17A C16A H16D 110.4 . . ? C15A C16A H16D 110.4 . . ? H16C C16A H16D 108.6 . . ? C16A C17A C18A 111.6(4) . . ? C16A C17A C12A 104.9(5) . . ? C18A C17A C12A 120.9(5) . . ? C16A C17A H17A 106.1 . . ? C18A C17A H17A 106.1 . . ? C12A C17A H17A 106.1 . . ? C19A C18A C17A 109.7(4) . . ? C19A C18A C29A 110.9(4) . . ? C17A C18A C29A 113.2(4) . . ? C19A C18A H18A 107.6 . . ? C17A C18A H18A 107.6 . . ? C29A C18A H18A 107.6 . . ? C20A C19A C18A 117.1(4) . . ? C20A C19A H19C 108.0 . . ? C18A C19A H19C 108.0 . . ? C20A C19A H19D 108.0 . . ? C18A C19A H19D 108.0 . . ? H19C C19A H19D 107.3 . . ? C19A C20A C21A 115.2(5) . . ? C19A C20A H20C 108.5 . . ? C21A C20A H20C 108.5 . . ? C19A C20A H20D 108.5 . . ? C21A C20A H20D 108.5 . . ? H20C C20A H20D 107.5 . . ? C20A C21A C25A 108.3(5) . . ? C20A C21A C22A 113.9(5) . . ? C25A C21A C22A 112.2(5) . . ? C20A C21A H21A 107.4 . . ? C25A C21A H21A 107.4 . . ? C22A C21A H21A 107.4 . . ? C23A C22A C24A 110.3(5) . . ? C23A C22A C21A 112.1(5) . . ? C24A C22A C21A 111.6(5) . . ? C23A C22A H22A 107.5 . . ? C24A C22A H22A 107.5 . . ? C21A C22A H22A 107.5 . . ? C22A C23A H23D 109.5 . . ? C22A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C22A C24A H24D 109.5 . . ? C22A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C22A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C26A C25A C21A 115.1(5) . . ? C26A C25A H25C 108.5 . . ? C21A C25A H25C 108.5 . . ? C26A C25A H25D 108.5 . . ? C21A C25A H25D 108.5 . . ? H25C C25A H25D 107.5 . . ? C25A C26A H26D 109.5 . . ? C25A C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C25A C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? C4A C27A H27D 109.5 . . ? C4A C27A H27E 109.5 . . ? H27D C27A H27E 109.5 . . ? C4A C27A H27F 109.5 . . ? H27D C27A H27F 109.5 . . ? H27E C27A H27F 109.5 . . ? C12A C28A H28D 109.5 . . ? C12A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C12A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C18A C29A H29D 109.5 . . ? C18A C29A H29E 109.5 . . ? H29D C29A H29E 109.5 . . ? C18A C29A H29F 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C1W O2W H20 109.5 . . ? O1W C1W O2W 123.1(6) . . ? O1W C1W C2W 125.2(6) . . ? O2W C1W C2W 111.8(5) . . ? C1W C2W C3W 113.6(5) . . ? C1W C2W H2WA 108.8 . . ? C3W C2W H2WA 108.8 . . ? C1W C2W H2WB 108.8 . . ? C3W C2W H2WB 108.8 . . ? H2WA C2W H2WB 107.7 . . ? C2W C3W H3WA 109.5 . . ? C2W C3W H3WB 109.5 . . ? H3WA C3W H3WB 109.5 . . ? C2W C3W H3WC 109.5 . . ? H3WA C3W H3WC 109.5 . . ? H3WB C3W H3WC 109.5 . . ? H3WD O3W H3WE 107(5) . . ? 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 O1 C1 1.441(6) . ? O1 H1O 0.8200 . ? C1 C2 1.486(7) . ? C1 C6 1.529(7) . ? C1 H1 0.9800 . ? C2 C3 1.524(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C7 1.304(7) . ? C3 C4 1.505(7) . ? C4 C5 1.537(6) . ? C4 C27 1.542(6) . ? C4 C10 1.545(6) . ? C5 C6 1.526(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.503(6) . ? C7 H7 0.9300 . ? C8 C9 1.523(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.532(6) . ? C9 C10 1.534(6) . ? C9 H9 0.9800 . ? C10 C14 1.536(6) . ? C10 H10 0.9800 . ? C11 C12 1.520(7) . ? C11 C15 1.531(6) . ? C11 H11 0.9800 . ? C12 C13 1.526(7) . ? C12 C28 1.528(7) . ? C12 C17 1.542(7) . ? C13 C14 1.540(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.574(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.549(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.539(6) . ? C17 H17 0.9800 . ? C18 C29 1.511(6) . ? C18 C19 1.527(6) . ? C18 H18 0.9800 . ? C19 C20 1.539(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.484(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C25 1.495(7) . ? C21 C22 1.528(7) . ? C21 H21 0.9800 . ? C22 C24 1.479(8) . ? C22 C23 1.551(8) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.495(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O1A C1A 1.463(5) . ? O1A H1AA 0.80(5) . ? C1A C2A 1.493(7) . ? C1A C6A 1.534(7) . ? C1A H1A 0.9800 . ? C2A C3A 1.524(6) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C7A 1.311(7) . ? C3A C4A 1.505(7) . ? C4A C27A 1.547(7) . ? C4A C5A 1.552(7) . ? C4A C10A 1.559(6) . ? C5A C6A 1.548(6) . ? C5A H5AA 0.9700 . ? C5A H5AB 0.9700 . ? C6A H6AA 0.9700 . ? C6A H6AB 0.9700 . ? C7A C8A 1.494(6) . ? C7A H7A 0.9300 . ? C8A C9A 1.529(6) . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C9A C10A 1.520(6) . ? C9A C11A 1.526(6) . ? C9A H9A 0.9800 . ? C10A C14A 1.548(6) . ? C10A H10A 0.9800 . ? C11A C12A 1.524(7) . ? C11A C15A 1.536(6) . ? C11A H11A 0.9800 . ? C12A C13A 1.530(7) . ? C12A C28A 1.542(6) . ? C12A C17A 1.558(6) . ? C13A C14A 1.549(6) . ? C13A H13C 0.9700 . ? C13A H13D 0.9700 . ? C14A H14C 0.9700 . ? C14A H14D 0.9700 . ? C15A C16A 1.565(6) . ? C15A H15C 0.9700 . ? C15A H15D 0.9700 . ? C16A C17A 1.535(6) . ? C16A H16C 0.9700 . ? C16A H16D 0.9700 . ? C17A C18A 1.540(6) . ? C17A H17A 0.9800 . ? C18A C19A 1.538(6) . ? C18A C29A 1.553(6) . ? C18A H18A 0.9800 . ? C19A C20A 1.515(6) . ? C19A H19C 0.9700 . ? C19A H19D 0.9700 . ? C20A C21A 1.531(7) . ? C20A H20C 0.9700 . ? C20A H20D 0.9700 . ? C21A C25A 1.547(7) . ? C21A C22A 1.564(7) . ? C21A H21A 0.9800 . ? C22A C23A 1.551(6) . ? C22A C24A 1.552(7) . ? C22A H22A 0.9800 . ? C23A H23D 0.9600 . ? C23A H23E 0.9600 . ? C23A H23F 0.9600 . ? C24A H24D 0.9600 . ? C24A H24E 0.9600 . ? C24A H24F 0.9600 . ? C25A C26A 1.522(7) . ? C25A H25C 0.9700 . ? C25A H25D 0.9700 . ? C26A H26D 0.9600 . ? C26A H26E 0.9600 . ? C26A H26F 0.9600 . ? C27A H27D 0.9600 . ? C27A H27E 0.9600 . ? C27A H27F 0.9600 . ? C28A H28D 0.9600 . ? C28A H28E 0.9600 . ? C28A H28F 0.9600 . ? C29A H29D 0.9600 . ? C29A H29E 0.9600 . ? C29A H29F 0.9600 . ? O1W C1W 1.200(6) . ? O2W C1W 1.330(6) . ? O2W H20 0.8200 . ? C1W C2W 1.500(7) . ? C2W C3W 1.503(6) . ? C2W H2WA 0.9700 . ? C2W H2WB 0.9700 . ? C3W H3WA 0.9600 . ? C3W H3WB 0.9600 . ? C3W H3WC 0.9600 . ? O3W H3WD 0.823(14) . ? O3W H3WE 0.842(11) . ? 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 O1 C1 C2 C3 -174.9(5) . . . . ? C6 C1 C2 C3 -53.2(7) . . . . ? C1 C2 C3 C7 -133.3(6) . . . . ? C1 C2 C3 C4 50.0(8) . . . . ? C7 C3 C4 C5 136.6(6) . . . . ? C2 C3 C4 C5 -46.9(7) . . . . ? C7 C3 C4 C27 -105.3(7) . . . . ? C2 C3 C4 C27 71.2(6) . . . . ? C7 C3 C4 C10 17.0(9) . . . . ? C2 C3 C4 C10 -166.5(5) . . . . ? C3 C4 C5 C6 52.0(7) . . . . ? C27 C4 C5 C6 -66.2(6) . . . . ? C10 C4 C5 C6 172.5(5) . . . . ? C4 C5 C6 C1 -57.6(7) . . . . ? O1 C1 C6 C5 179.3(4) . . . . ? C2 C1 C6 C5 56.5(7) . . . . ? C4 C3 C7 C8 -4.7(10) . . . . ? C2 C3 C7 C8 179.0(5) . . . . ? C3 C7 C8 C9 18.9(8) . . . . ? C7 C8 C9 C11 -166.4(5) . . . . ? C7 C8 C9 C10 -44.7(6) . . . . ? C8 C9 C10 C14 -171.3(5) . . . . ? C11 C9 C10 C14 -48.4(6) . . . . ? C8 C9 C10 C4 59.4(6) . . . . ? C11 C9 C10 C4 -177.8(5) . . . . ? C3 C4 C10 C9 -43.9(6) . . . . ? C5 C4 C10 C9 -163.3(5) . . . . ? C27 C4 C10 C9 76.9(6) . . . . ? C3 C4 C10 C14 -171.8(5) . . . . ? C5 C4 C10 C14 68.8(6) . . . . ? C27 C4 C10 C14 -51.0(6) . . . . ? C8 C9 C11 C12 179.2(5) . . . . ? C10 C9 C11 C12 57.1(6) . . . . ? C8 C9 C11 C15 -56.1(6) . . . . ? C10 C9 C11 C15 -178.2(5) . . . . ? C15 C11 C12 C13 168.8(5) . . . . ? C9 C11 C12 C13 -60.3(6) . . . . ? C15 C11 C12 C28 -70.0(6) . . . . ? C9 C11 C12 C28 60.9(6) . . . . ? C15 C11 C12 C17 47.8(5) . . . . ? C9 C11 C12 C17 178.7(5) . . . . ? C11 C12 C13 C14 56.6(6) . . . . ? C28 C12 C13 C14 -65.7(6) . . . . ? C17 C12 C13 C14 167.4(5) . . . . ? C9 C10 C14 C13 50.4(6) . . . . ? C4 C10 C14 C13 178.8(5) . . . . ? C12 C13 C14 C10 -55.6(6) . . . . ? C12 C11 C15 C16 -35.1(6) . . . . ? C9 C11 C15 C16 -165.4(5) . . . . ? C11 C15 C16 C17 9.3(6) . . . . ? C11 C12 C17 C18 -164.1(5) . . . . ? C13 C12 C17 C18 82.3(6) . . . . ? C28 C12 C17 C18 -44.8(7) . . . . ? C11 C12 C17 C16 -40.3(5) . . . . ? C13 C12 C17 C16 -154.0(5) . . . . ? C28 C12 C17 C16 78.9(6) . . . . ? C15 C16 C17 C18 148.8(5) . . . . ? C15 C16 C17 C12 19.2(6) . . . . ? C12 C17 C18 C29 -57.3(7) . . . . ? C16 C17 C18 C29 -177.4(5) . . . . ? C12 C17 C18 C19 179.9(5) . . . . ? C16 C17 C18 C19 59.8(6) . . . . ? C29 C18 C19 C20 60.5(6) . . . . ? C17 C18 C19 C20 -175.7(4) . . . . ? C18 C19 C20 C21 155.1(5) . . . . ? C19 C20 C21 C25 51.1(8) . . . . ? C19 C20 C21 C22 -174.8(6) . . . . ? C20 C21 C22 C24 -63.8(9) . . . . ? C25 C21 C22 C24 70.6(8) . . . . ? C20 C21 C22 C23 54.0(9) . . . . ? C25 C21 C22 C23 -171.6(6) . . . . ? C20 C21 C25 C26 -174.5(6) . . . . ? C22 C21 C25 C26 50.4(9) . . . . ? O1A C1A C2A C3A -179.3(4) . . . . ? C6A C1A C2A C3A -57.8(6) . . . . ? C1A C2A C3A C7A -132.3(6) . . . . ? C1A C2A C3A C4A 53.5(7) . . . . ? C7A C3A C4A C27A -103.5(7) . . . . ? C2A C3A C4A C27A 70.6(6) . . . . ? C7A C3A C4A C5A 136.9(6) . . . . ? C2A C3A C4A C5A -49.1(7) . . . . ? C7A C3A C4A C10A 19.3(8) . . . . ? C2A C3A C4A C10A -166.6(5) . . . . ? C3A C4A C5A C6A 52.4(6) . . . . ? C27A C4A C5A C6A -68.2(6) . . . . ? C10A C4A C5A C6A 171.4(5) . . . . ? O1A C1A C6A C5A -177.9(4) . . . . ? C2A C1A C6A C5A 59.9(6) . . . . ? C4A C5A C6A C1A -58.2(6) . . . . ? C4A C3A C7A C8A -6.6(10) . . . . ? C2A C3A C7A C8A 179.7(5) . . . . ? C3A C7A C8A C9A 19.1(9) . . . . ? C7A C8A C9A C10A -44.4(6) . . . . ? C7A C8A C9A C11A -166.6(5) . . . . ? C11A C9A C10A C14A -48.3(6) . . . . ? C8A C9A C10A C14A -170.9(4) . . . . ? C11A C9A C10A C4A -177.6(5) . . . . ? C8A C9A C10A C4A 59.8(6) . . . . ? C3A C4A C10A C9A -45.9(6) . . . . ? C27A C4A C10A C9A 76.7(6) . . . . ? C5A C4A C10A C9A -164.2(4) . . . . ? C3A C4A C10A C14A -174.5(5) . . . . ? C27A C4A C10A C14A -51.9(6) . . . . ? C5A C4A C10A C14A 67.2(6) . . . . ? C10A C9A C11A C12A 58.3(6) . . . . ? C8A C9A C11A C12A -179.7(5) . . . . ? C10A C9A C11A C15A -176.3(5) . . . . ? C8A C9A C11A C15A -54.3(6) . . . . ? C9A C11A C12A C13A -61.7(6) . . . . ? C15A C11A C12A C13A 166.5(4) . . . . ? C9A C11A C12A C28A 60.1(6) . . . . ? C15A C11A C12A C28A -71.8(5) . . . . ? C9A C11A C12A C17A 174.9(4) . . . . ? C15A C11A C12A C17A 43.1(5) . . . . ? C11A C12A C13A C14A 56.6(6) . . . . ? C28A C12A C13A C14A -65.8(6) . . . . ? C17A C12A C13A C14A 168.9(5) . . . . ? C9A C10A C14A C13A 47.5(7) . . . . ? C4A C10A C14A C13A 176.2(5) . . . . ? C12A C13A C14A C10A -52.4(6) . . . . ? C12A C11A C15A C16A -31.7(5) . . . . ? C9A C11A C15A C16A -161.3(4) . . . . ? C11A C15A C16A C17A 7.3(6) . . . . ? C15A C16A C17A C18A 151.6(4) . . . . ? C15A C16A C17A C12A 18.9(6) . . . . ? C11A C12A C17A C16A -37.7(5) . . . . ? C13A C12A C17A C16A -153.2(5) . . . . ? C28A C12A C17A C16A 80.1(6) . . . . ? C11A C12A C17A C18A -164.8(5) . . . . ? C13A C12A C17A C18A 79.7(7) . . . . ? C28A C12A C17A C18A -47.0(7) . . . . ? C16A C17A C18A C19A 59.7(6) . . . . ? C12A C17A C18A C19A -176.3(5) . . . . ? C16A C17A C18A C29A -175.9(5) . . . . ? C12A C17A C18A C29A -51.9(7) . . . . ? C17A C18A C19A C20A 175.4(5) . . . . ? C29A C18A C19A C20A 49.7(7) . . . . ? C18A C19A C20A C21A 59.9(7) . . . . ? C19A C20A C21A C25A 68.7(6) . . . . ? C19A C20A C21A C22A -165.7(5) . . . . ? C20A C21A C22A C23A -60.3(6) . . . . ? C25A C21A C22A C23A 63.2(7) . . . . ? C20A C21A C22A C24A 64.1(6) . . . . ? C25A C21A C22A C24A -172.4(5) . . . . ? C20A C21A C25A C26A 175.0(5) . . . . ? C22A C21A C25A C26A 48.5(7) . . . . ? O1W C1W C2W C3W 20.3(10) . . . . ? O2W C1W C2W C3W -160.4(5) . . . . ?