#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:02:46 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247583 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125663.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_7125663 loop_ _publ_author_name 'Yi, Xiangyan' 'Feng, Jiajun' 'Huang, Fei' 'Baell, Jonathan Bayldon' _publ_section_title ; Metal-free C-C, C-O, C-S and C-N bond formation enabled by SBA-15 supported TFMSA. ; _journal_issue 8 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1243 _journal_page_last 1246 _journal_paper_doi 10.1039/c9cc08389h _journal_volume 56 _journal_year 2020 _chemical_formula_sum 'C25 H22 O4' _chemical_formula_weight 386.42 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2019-05-22 deposited with the CCDC. 2019-12-17 downloaded from the CCDC. ; _cell_angle_alpha 78.2880(10) _cell_angle_beta 83.3010(10) _cell_angle_gamma 70.1950(10) _cell_formula_units_Z 4 _cell_length_a 10.7065(5) _cell_length_b 12.0739(5) _cell_length_c 17.4608(8) _cell_measurement_reflns_used 9937 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 54.824 _cell_measurement_theta_min 4.592 _cell_volume 2076.61(16) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_unetI/netI 0.0285 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 39159 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.499 _diffrn_reflns_theta_min 2.332 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.236 _exptl_crystal_description prismatic _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.530 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.033 _refine_ls_extinction_coef 0.027(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 526 _refine_ls_number_reflns 7692 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.023 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0485 _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^)+(0.0481P)^2^+0.8031P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1130 _refine_ls_wR_factor_ref 0.1239 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6141 _reflns_number_total 7692 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc08389h2.cif _cod_data_source_block mo_dd19032_0m _cod_depositor_comments 'Adding full bibliography for 7125662--7125663.cif.' _cod_database_code 7125663 _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_estimated_absorpt_t_min 0.984 _shelx_estimated_absorpt_t_max 0.989 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_dd19032_0m_a.res in P-1 CELL 0.71073 10.7065 12.0739 17.4608 78.288 83.301 70.195 ZERR 4 0.0005 0.0005 0.0008 0.001 0.001 0.001 LATT 1 SFAC C H O UNIT 100 88 16 OMIT 1 0 1 OMIT 2 0 3 OMIT 0 1 0 OMIT 1 0 0 OMIT -1 0 1 OMIT -3.00 51.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 HTAB C50 O2_$3 HTAB C27 O7_$2 HTAB C2 O3_$1 size 0.20 0.17 0.13 wpdb -1 mpla c36 > c41 mpla c29 > c34 mpla c42 > c47 mpla c11 > c16 mpla c17 > c22 mpla c4 > c9 htab conf EQIV $1 -x+2, -y+1, -z+1 HTAB C2 O3_$1 EQIV $2 -x+1, -y, -z+2 HTAB C27 O7_$2 EQIV $3 x, y-1, z HTAB C50 O2_$3 DELU 0.003 C49 C50 TEMP -80.17 WGHT 0.048100 0.803100 EXTI 0.027239 FVAR 1.02635 O1 3 1.026808 0.780539 0.570526 11.00000 0.07144 0.06901 = 0.06626 0.00857 -0.02444 -0.04081 O2 3 0.720414 0.840688 0.635228 11.00000 0.06294 0.05840 = 0.08376 -0.03971 -0.01291 0.00380 O3 3 1.112418 0.513294 0.555776 11.00000 0.03814 0.07126 = 0.03761 -0.01270 0.00143 -0.00316 O4 3 1.138956 0.486184 0.683552 11.00000 0.03730 0.08555 = 0.03908 -0.01567 -0.00578 0.00755 C1 1 0.927600 0.603128 0.641316 11.00000 0.03409 0.03705 = 0.03521 -0.00794 0.00042 -0.00754 AFIX 13 H1 2 0.930143 0.651908 0.680694 11.00000 -1.20000 AFIX 0 C2 1 0.862156 0.689147 0.568324 11.00000 0.03573 0.03296 = 0.03783 -0.00681 -0.00162 -0.00713 AFIX 13 H2 2 0.853321 0.642971 0.528913 11.00000 -1.20000 AFIX 0 C3 1 0.944788 0.770379 0.532560 11.00000 0.04308 0.03771 = 0.04759 -0.00537 -0.00511 -0.01209 C4 1 0.920493 0.838393 0.451185 11.00000 0.03968 0.03287 = 0.04445 -0.00648 0.00363 -0.00669 C5 1 0.831810 0.826355 0.403878 11.00000 0.05787 0.04517 = 0.04442 -0.00353 -0.00386 -0.01716 AFIX 43 H5 2 0.783242 0.772668 0.423085 11.00000 -1.20000 AFIX 0 C6 1 0.813863 0.892299 0.328798 11.00000 0.07603 0.06045 = 0.04381 -0.00608 -0.00682 -0.01911 AFIX 43 H6 2 0.753727 0.883388 0.296411 11.00000 -1.20000 AFIX 0 C7 1 0.883942 0.971212 0.301197 11.00000 0.08372 0.05386 = 0.04179 0.00033 0.00895 -0.01417 AFIX 43 H7 2 0.871036 1.017060 0.249937 11.00000 -1.20000 AFIX 0 C8 1 0.971904 0.983625 0.347395 11.00000 0.06670 0.05020 = 0.05446 -0.00273 0.01371 -0.01944 AFIX 43 H8 2 1.019801 1.037819 0.328041 11.00000 -1.20000 AFIX 0 C9 1 0.990807 0.917602 0.421776 11.00000 0.04687 0.04169 = 0.05388 -0.00727 0.00646 -0.01198 AFIX 43 H9 2 1.052350 0.926096 0.453367 11.00000 -1.20000 AFIX 0 C10 1 0.724561 0.769663 0.593610 11.00000 0.04681 0.03550 = 0.04236 -0.00820 -0.00297 -0.00288 C11 1 0.600470 0.761236 0.569423 11.00000 0.03694 0.04331 = 0.03860 -0.00609 0.00154 -0.00156 C12 1 0.596541 0.666439 0.537401 11.00000 0.03615 0.04647 = 0.07170 -0.01100 -0.00103 -0.00642 AFIX 43 H12 2 0.676533 0.604554 0.527943 11.00000 -1.20000 AFIX 0 C13 1 0.476073 0.661905 0.519192 11.00000 0.04627 0.06778 = 0.10430 -0.01640 -0.00802 -0.01923 AFIX 43 H13 2 0.473758 0.597290 0.496740 11.00000 -1.20000 AFIX 0 C14 1 0.359631 0.750704 0.533509 11.00000 0.03607 0.09926 = 0.08258 -0.00398 -0.00492 -0.01456 AFIX 43 H14 2 0.276853 0.746011 0.522623 11.00000 -1.20000 AFIX 0 C15 1 0.363539 0.845916 0.563527 11.00000 0.04062 0.10009 = 0.07154 -0.02541 -0.00456 0.01394 AFIX 43 H15 2 0.283452 0.908383 0.571865 11.00000 -1.20000 AFIX 0 C16 1 0.482145 0.851599 0.581582 11.00000 0.04787 0.06974 = 0.05794 -0.02395 -0.00721 0.01158 AFIX 43 H16 2 0.483573 0.917817 0.602583 11.00000 -1.20000 AFIX 0 C17 1 0.849793 0.519122 0.678582 11.00000 0.03007 0.03898 = 0.03647 -0.00249 -0.00055 -0.00444 C18 1 0.858779 0.420863 0.646196 11.00000 0.04200 0.04342 = 0.04455 -0.00713 0.00449 -0.01104 AFIX 43 H18 2 0.913834 0.405579 0.600201 11.00000 -1.20000 AFIX 0 C19 1 0.787919 0.344621 0.680478 11.00000 0.05027 0.04648 = 0.06347 -0.00606 0.00140 -0.01850 AFIX 43 H19 2 0.795503 0.276844 0.658301 11.00000 -1.20000 AFIX 0 C20 1 0.706434 0.367060 0.746741 11.00000 0.04234 0.05495 = 0.05825 0.00601 -0.00003 -0.01764 AFIX 43 H20 2 0.658426 0.314511 0.770407 11.00000 -1.20000 AFIX 0 C21 1 0.694954 0.465381 0.778319 11.00000 0.03716 0.06768 = 0.04434 0.00083 0.00765 -0.01081 AFIX 43 H21 2 0.637455 0.481721 0.823297 11.00000 -1.20000 AFIX 0 C22 1 0.766816 0.541130 0.744967 11.00000 0.03852 0.05167 = 0.03943 -0.00827 0.00321 -0.00710 AFIX 43 H22 2 0.759230 0.608435 0.767662 11.00000 -1.20000 AFIX 0 C23 1 1.069039 0.531208 0.620286 11.00000 0.03392 0.03783 = 0.03441 -0.00471 -0.00153 -0.01083 C24 1 1.277803 0.415247 0.674262 11.00000 0.03670 0.08520 = 0.05364 -0.01825 -0.01000 0.00886 AFIX 23 H24A 2 1.302048 0.409213 0.618428 11.00000 -1.20000 H24B 2 1.293519 0.333514 0.704704 11.00000 -1.20000 AFIX 0 C25 1 1.359403 0.474128 0.702724 11.00000 0.05362 0.08512 = 0.12160 -0.00256 -0.00897 -0.02022 AFIX 137 H25A 2 1.344486 0.554358 0.671638 11.00000 -1.50000 H25B 2 1.453579 0.426844 0.697537 11.00000 -1.50000 H25C 2 1.334290 0.480252 0.757884 11.00000 -1.50000 AFIX 0 O5 3 0.542420 0.302919 0.910052 11.00000 0.07816 0.09566 = 0.06134 0.00353 0.01819 -0.04765 O6 3 0.226142 0.426219 0.962056 11.00000 0.06924 0.03507 = 0.06107 0.00613 0.01210 -0.00765 O7 3 0.554563 0.045411 0.897162 11.00000 0.05834 0.04932 = 0.04857 0.00603 0.00673 0.00727 O8 3 0.481717 0.147415 0.779917 11.00000 0.07258 0.05541 = 0.03719 -0.00198 0.00951 0.00626 C26 1 0.350744 0.212684 0.889663 11.00000 0.05030 0.03492 = 0.03542 0.00247 0.00216 -0.00281 AFIX 13 H26 2 0.334638 0.292113 0.854501 11.00000 -1.20000 AFIX 0 C27 1 0.370853 0.227574 0.971981 11.00000 0.04285 0.03401 = 0.03637 0.00295 0.00414 -0.00848 AFIX 13 H27 2 0.383379 0.150363 1.009258 11.00000 -1.20000 AFIX 0 C28 1 0.489731 0.270414 0.971882 11.00000 0.04741 0.04252 = 0.05420 0.00213 0.00772 -0.01329 C29 1 0.535170 0.274906 1.048129 11.00000 0.04202 0.03721 = 0.06436 -0.00129 -0.00435 -0.00963 C30 1 0.492809 0.220334 1.119139 11.00000 0.04979 0.04718 = 0.05554 -0.01145 -0.00057 -0.01516 AFIX 43 H30 2 0.430997 0.179132 1.120161 11.00000 -1.20000 AFIX 0 C31 1 0.539518 0.225116 1.188729 11.00000 0.07089 0.05631 = 0.06419 -0.01455 -0.00995 -0.01652 AFIX 43 H31 2 0.510365 0.186631 1.237035 11.00000 -1.20000 AFIX 0 C32 1 0.627464 0.285122 1.187960 11.00000 0.09668 0.06023 = 0.09567 -0.00601 -0.04025 -0.02723 AFIX 43 H32 2 0.660480 0.287358 1.235622 11.00000 -1.20000 AFIX 0 C33 1 0.667834 0.341862 1.118613 11.00000 0.09661 0.07693 = 0.12402 0.01130 -0.04722 -0.05005 AFIX 43 H33 2 0.727314 0.385131 1.118385 11.00000 -1.20000 AFIX 0 C34 1 0.623097 0.336892 1.049084 11.00000 0.07029 0.06601 = 0.09436 0.01885 -0.02162 -0.03524 AFIX 43 H34 2 0.652581 0.376220 1.001220 11.00000 -1.20000 AFIX 0 C35 1 0.247939 0.325115 0.998438 11.00000 0.04639 0.03482 = 0.04075 -0.00187 0.00008 -0.01102 C36 1 0.159731 0.297843 1.066783 11.00000 0.03683 0.03594 = 0.03490 -0.00425 -0.00314 -0.00822 C37 1 0.069156 0.393187 1.097592 11.00000 0.04873 0.03702 = 0.04102 -0.00692 -0.00444 -0.00625 AFIX 43 H37 2 0.063678 0.472781 1.074117 11.00000 -1.20000 AFIX 0 C38 1 -0.012868 0.372988 1.162060 11.00000 0.05028 0.05103 = 0.04477 -0.01420 0.00420 -0.00376 AFIX 43 H38 2 -0.073784 0.438633 1.183223 11.00000 -1.20000 AFIX 0 C39 1 -0.006803 0.258492 1.195715 11.00000 0.04521 0.06233 = 0.04312 -0.00770 0.00736 -0.01303 AFIX 43 H39 2 -0.062397 0.244894 1.240680 11.00000 -1.20000 AFIX 0 C40 1 0.080017 0.162859 1.164353 11.00000 0.05101 0.04545 = 0.05192 -0.00103 0.00884 -0.01483 AFIX 43 H40 2 0.082201 0.083738 1.186903 11.00000 -1.20000 AFIX 0 C41 1 0.163667 0.181943 1.100298 11.00000 0.04540 0.03789 = 0.04880 -0.00614 0.00735 -0.00853 AFIX 43 H41 2 0.223860 0.115967 1.079135 11.00000 -1.20000 AFIX 0 C42 1 0.231081 0.172849 0.888723 11.00000 0.05502 0.04309 = 0.03326 -0.00655 -0.00118 -0.00445 C43 1 0.112041 0.255002 0.861612 11.00000 0.06272 0.05877 = 0.05593 -0.00756 -0.01574 -0.00393 AFIX 43 H43 2 0.107150 0.335343 0.840826 11.00000 -1.20000 AFIX 0 C44 1 0.000981 0.220844 0.864639 11.00000 0.06474 0.09672 = 0.08329 -0.02356 -0.02494 -0.00799 AFIX 43 H44 2 -0.080201 0.278028 0.846373 11.00000 -1.20000 AFIX 0 C45 1 0.006492 0.105387 0.893693 11.00000 0.07425 0.10861 = 0.08354 -0.03738 -0.00794 -0.03615 AFIX 43 H45 2 -0.070770 0.082723 0.895853 11.00000 -1.20000 AFIX 0 C46 1 0.123628 0.022250 0.919730 11.00000 0.08844 0.07015 = 0.07239 -0.02293 0.00514 -0.03465 AFIX 43 H46 2 0.127907 -0.058322 0.939060 11.00000 -1.20000 AFIX 0 C47 1 0.235525 0.055760 0.917834 11.00000 0.06322 0.04859 = 0.05463 -0.00926 0.00191 -0.01169 AFIX 43 H47 2 0.316109 -0.001850 0.936616 11.00000 -1.20000 AFIX 0 C48 1 0.474487 0.125580 0.858257 11.00000 0.05727 0.04079 = 0.04028 0.00160 0.00717 -0.00719 C49 1 0.597504 0.069628 0.741587 11.00000 0.09170 0.05882 = 0.05241 -0.01089 0.01662 0.01118 AFIX 23 H49A 2 0.680172 0.065750 0.763767 11.00000 -1.20000 H49B 2 0.592324 -0.012298 0.749677 11.00000 -1.20000 AFIX 0 C50 1 0.597483 0.120000 0.658145 11.00000 0.09718 0.06858 = 0.06300 -0.01840 0.02332 -0.02926 AFIX 137 H50A 2 0.675478 0.070856 0.630983 11.00000 -1.50000 H50B 2 0.600480 0.201715 0.650941 11.00000 -1.50000 H50C 2 0.516477 0.121229 0.636519 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_dd19032_0m_a.res in P-1 REM R1 = 0.0485 for 6141 Fo > 4sig(Fo) and 0.0630 for all 7692 data REM 526 parameters refined using 1 restraints END WGHT 0.0480 0.7986 REM Instructions for potential hydrogen bonds HTAB C2 O3_$1 HTAB C27 O7_$2 HTAB C50 O2_$3 REM Highest difference peak 0.530, deepest hole -0.229, 1-sigma level 0.033 Q1 1 0.6744 0.0911 0.7069 11.00000 0.05 0.53 Q2 1 0.7332 0.3125 1.0768 11.00000 0.05 0.22 Q3 1 1.3555 0.5117 0.6382 11.00000 0.05 0.21 Q4 1 0.5349 0.0377 0.7234 11.00000 0.05 0.21 Q5 1 1.3041 0.4690 0.6336 11.00000 0.05 0.18 Q6 1 1.2849 0.3639 0.6341 11.00000 0.05 0.17 Q7 1 0.6729 0.3152 0.9988 11.00000 0.05 0.17 Q8 1 1.1524 0.5444 0.6611 11.00000 0.05 0.17 Q9 1 0.3694 0.8058 0.4834 11.00000 0.05 0.17 Q10 1 0.9442 0.8252 0.5835 11.00000 0.05 0.17 Q11 1 0.6836 0.2803 1.1456 11.00000 0.05 0.16 Q12 1 0.6599 0.3616 1.1314 11.00000 0.05 0.16 Q13 1 0.4256 0.1036 0.7756 11.00000 0.05 0.16 Q14 1 0.7913 0.7182 0.5751 11.00000 0.05 0.15 Q15 1 0.8954 0.6440 0.6072 11.00000 0.05 0.15 Q16 1 0.4848 0.7210 0.4720 11.00000 0.05 0.15 Q17 1 0.8787 0.5597 0.6541 11.00000 0.05 0.14 Q18 1 0.6085 0.7373 0.5293 11.00000 0.05 0.14 Q19 1 0.2118 0.3059 1.0431 11.00000 0.05 0.14 Q20 1 -0.0057 0.2151 1.1592 11.00000 0.05 0.14 ; _shelx_res_checksum 48320 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 O1 O 1.02681(15) 0.78054(13) 0.57053(9) 0.0655(4) Uani 1 1 d . . O2 O 0.72041(15) 0.84069(13) 0.63523(9) 0.0696(4) Uani 1 1 d . . O3 O 1.11242(12) 0.51329(12) 0.55578(7) 0.0526(3) Uani 1 1 d . . O4 O 1.13896(12) 0.48618(13) 0.68355(7) 0.0601(4) Uani 1 1 d . . C1 C 0.92760(15) 0.60313(14) 0.64132(9) 0.0364(4) Uani 1 1 d . . H1 H 0.9301 0.6519 0.6807 0.044 Uiso 1 1 calc R U C2 C 0.86216(16) 0.68915(14) 0.56832(9) 0.0365(4) Uani 1 1 d . . H2 H 0.8533 0.6430 0.5289 0.044 Uiso 1 1 calc R U C3 C 0.94479(17) 0.77038(15) 0.53256(11) 0.0431(4) Uani 1 1 d . . C4 C 0.92049(17) 0.83839(14) 0.45118(10) 0.0408(4) Uani 1 1 d . . C5 C 0.8318(2) 0.82635(16) 0.40388(11) 0.0496(4) Uani 1 1 d . . H5 H 0.7832 0.7727 0.4231 0.059 Uiso 1 1 calc R U C6 C 0.8139(2) 0.89230(19) 0.32880(12) 0.0610(5) Uani 1 1 d . . H6 H 0.7537 0.8834 0.2964 0.073 Uiso 1 1 calc R U C7 C 0.8839(2) 0.97121(19) 0.30120(12) 0.0642(6) Uani 1 1 d . . H7 H 0.8710 1.0171 0.2499 0.077 Uiso 1 1 calc R U C8 C 0.9719(2) 0.98363(18) 0.34740(12) 0.0594(5) Uani 1 1 d . . H8 H 1.0198 1.0378 0.3280 0.071 Uiso 1 1 calc R U C9 C 0.99081(19) 0.91760(16) 0.42178(11) 0.0490(4) Uani 1 1 d . . H9 H 1.0524 0.9261 0.4534 0.059 Uiso 1 1 calc R U C10 C 0.72456(18) 0.76966(15) 0.59361(10) 0.0440(4) Uani 1 1 d . . C11 C 0.60047(17) 0.76124(15) 0.56942(10) 0.0430(4) Uani 1 1 d . . C12 C 0.59654(18) 0.66644(17) 0.53740(12) 0.0533(5) Uani 1 1 d . . H12 H 0.6765 0.6046 0.5279 0.064 Uiso 1 1 calc R U C13 C 0.4761(2) 0.6619(2) 0.51919(16) 0.0720(6) Uani 1 1 d . . H13 H 0.4738 0.5973 0.4967 0.086 Uiso 1 1 calc R U C14 C 0.3596(2) 0.7507(2) 0.53351(15) 0.0762(7) Uani 1 1 d . . H14 H 0.2769 0.7460 0.5226 0.091 Uiso 1 1 calc R U C15 C 0.3635(2) 0.8459(3) 0.56353(14) 0.0786(7) Uani 1 1 d . . H15 H 0.2835 0.9084 0.5719 0.094 Uiso 1 1 calc R U C16 C 0.4821(2) 0.8516(2) 0.58158(12) 0.0642(6) Uani 1 1 d . . H16 H 0.4836 0.9178 0.6026 0.077 Uiso 1 1 calc R U C17 C 0.84979(15) 0.51912(14) 0.67858(9) 0.0376(4) Uani 1 1 d . . C18 C 0.85878(17) 0.42086(15) 0.64620(11) 0.0447(4) Uani 1 1 d . . H18 H 0.9138 0.4056 0.6002 0.054 Uiso 1 1 calc R U C19 C 0.78792(19) 0.34462(17) 0.68048(12) 0.0536(5) Uani 1 1 d . . H19 H 0.7955 0.2768 0.6583 0.064 Uiso 1 1 calc R U C20 C 0.70643(18) 0.36706(18) 0.74674(12) 0.0540(5) Uani 1 1 d . . H20 H 0.6584 0.3145 0.7704 0.065 Uiso 1 1 calc R U C21 C 0.69495(18) 0.46538(19) 0.77832(11) 0.0537(5) Uani 1 1 d . . H21 H 0.6375 0.4817 0.8233 0.064 Uiso 1 1 calc R U C22 C 0.76682(17) 0.54113(17) 0.74497(10) 0.0456(4) Uani 1 1 d . . H22 H 0.7592 0.6084 0.7677 0.055 Uiso 1 1 calc R U C23 C 1.06904(15) 0.53121(14) 0.62029(9) 0.0359(4) Uani 1 1 d . . C24 C 1.27780(19) 0.4152(2) 0.67426(13) 0.0644(6) Uani 1 1 d . . H24A H 1.3020 0.4092 0.6184 0.077 Uiso 1 1 calc R U H24B H 1.2935 0.3335 0.7047 0.077 Uiso 1 1 calc R U C25 C 1.3594(2) 0.4741(2) 0.70272(19) 0.0893(8) Uani 1 1 d . . H25A H 1.3445 0.5544 0.6716 0.134 Uiso 1 1 calc R U H25B H 1.4536 0.4268 0.6975 0.134 Uiso 1 1 calc R U H25C H 1.3343 0.4803 0.7579 0.134 Uiso 1 1 calc R U O5 O 0.54242(17) 0.30292(16) 0.91005(9) 0.0778(5) Uani 1 1 d . . O6 O 0.22614(14) 0.42622(11) 0.96206(8) 0.0610(4) Uani 1 1 d . . O7 O 0.55456(14) 0.04541(12) 0.89716(8) 0.0615(4) Uani 1 1 d . . O8 O 0.48172(15) 0.14741(12) 0.77992(7) 0.0640(4) Uani 1 1 d . . C26 C 0.35074(18) 0.21268(15) 0.88966(10) 0.0447(4) Uani 1 1 d . . H26 H 0.3346 0.2921 0.8545 0.054 Uiso 1 1 calc R U C27 C 0.37085(17) 0.22757(14) 0.97198(10) 0.0407(4) Uani 1 1 d . . H27 H 0.3834 0.1504 1.0093 0.049 Uiso 1 1 calc R U C28 C 0.48973(19) 0.27041(16) 0.97188(11) 0.0508(5) Uani 1 1 d . . C29 C 0.53517(18) 0.27491(15) 1.04813(12) 0.0497(5) Uani 1 1 d . . C30 C 0.49281(19) 0.22033(17) 1.11914(11) 0.0508(5) Uani 1 1 d . . H30 H 0.4310 0.1791 1.1202 0.061 Uiso 1 1 calc R U C31 C 0.5395(2) 0.22512(19) 1.18873(14) 0.0637(6) Uani 1 1 d . . H31 H 0.5104 0.1866 1.2370 0.076 Uiso 1 1 calc R U C32 C 0.6275(3) 0.2851(2) 1.18796(17) 0.0819(8) Uani 1 1 d . . H32 H 0.6605 0.2874 1.2356 0.098 Uiso 1 1 calc R U C33 C 0.6678(3) 0.3419(2) 1.11861(19) 0.0943(9) Uani 1 1 d . . H33 H 0.7273 0.3851 1.1184 0.113 Uiso 1 1 calc R U C34 C 0.6231(2) 0.3369(2) 1.04908(16) 0.0769(7) Uani 1 1 d . . H34 H 0.6526 0.3762 1.0012 0.092 Uiso 1 1 calc R U C35 C 0.24794(17) 0.32512(15) 0.99844(10) 0.0421(4) Uani 1 1 d . . C36 C 0.15973(16) 0.29784(14) 1.06678(9) 0.0370(4) Uani 1 1 d . . C37 C 0.06916(18) 0.39319(15) 1.09759(10) 0.0440(4) Uani 1 1 d . . H37 H 0.0637 0.4728 1.0741 0.053 Uiso 1 1 calc R U C38 C -0.01287(19) 0.37299(17) 1.16206(11) 0.0517(5) Uani 1 1 d . . H38 H -0.0738 0.4386 1.1832 0.062 Uiso 1 1 calc R U C39 C -0.00680(19) 0.25849(18) 1.19572(11) 0.0524(5) Uani 1 1 d . . H39 H -0.0624 0.2449 1.2407 0.063 Uiso 1 1 calc R U C40 C 0.08002(19) 0.16286(17) 1.16435(11) 0.0518(5) Uani 1 1 d . . H40 H 0.0822 0.0837 1.1869 0.062 Uiso 1 1 calc R U C41 C 0.16367(18) 0.18194(15) 1.10030(11) 0.0464(4) Uani 1 1 d . . H41 H 0.2239 0.1160 1.0791 0.056 Uiso 1 1 calc R U C42 C 0.23108(19) 0.17285(16) 0.88872(10) 0.0469(4) Uani 1 1 d . . C43 C 0.1120(2) 0.2550(2) 0.86161(12) 0.0625(6) Uani 1 1 d . . H43 H 0.1071 0.3353 0.8408 0.075 Uiso 1 1 calc R U C44 C 0.0010(3) 0.2208(3) 0.86464(16) 0.0833(8) Uani 1 1 d . . H44 H -0.0802 0.2780 0.8464 0.100 Uiso 1 1 calc R U C45 C 0.0065(3) 0.1054(3) 0.89369(16) 0.0837(8) Uani 1 1 d . . H45 H -0.0708 0.0827 0.8959 0.100 Uiso 1 1 calc R U C46 C 0.1236(3) 0.0223(2) 0.91973(14) 0.0739(7) Uani 1 1 d . . H46 H 0.1279 -0.0583 0.9391 0.089 Uiso 1 1 calc R U C47 C 0.2355(2) 0.05576(18) 0.91783(12) 0.0575(5) Uani 1 1 d . . H47 H 0.3161 -0.0018 0.9366 0.069 Uiso 1 1 calc R U C48 C 0.4745(2) 0.12558(16) 0.85826(11) 0.0505(5) Uani 1 1 d . . C49 C 0.5975(3) 0.0696(2) 0.74159(13) 0.0784(8) Uani 1 1 d . U H49A H 0.6802 0.0658 0.7638 0.094 Uiso 1 1 calc R U H49B H 0.5923 -0.0123 0.7497 0.094 Uiso 1 1 calc R U C50 C 0.5975(3) 0.1200(2) 0.65815(14) 0.0769(7) Uani 1 1 d . U H50A H 0.6755 0.0709 0.6310 0.115 Uiso 1 1 calc R U H50B H 0.6005 0.2017 0.6509 0.115 Uiso 1 1 calc R U H50C H 0.5165 0.1212 0.6365 0.115 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0714(10) 0.0690(9) 0.0663(9) 0.0086(7) -0.0244(8) -0.0408(8) O2 0.0629(9) 0.0584(9) 0.0838(11) -0.0397(8) -0.0129(8) 0.0038(7) O3 0.0381(7) 0.0713(9) 0.0376(7) -0.0127(6) 0.0014(5) -0.0032(6) O4 0.0373(7) 0.0855(10) 0.0391(7) -0.0157(7) -0.0058(5) 0.0076(6) C1 0.0341(8) 0.0370(8) 0.0352(9) -0.0079(7) 0.0004(7) -0.0075(7) C2 0.0357(8) 0.0330(8) 0.0378(9) -0.0068(7) -0.0016(7) -0.0071(7) C3 0.0431(10) 0.0377(9) 0.0476(10) -0.0054(7) -0.0051(8) -0.0121(7) C4 0.0397(9) 0.0329(8) 0.0444(10) -0.0065(7) 0.0036(7) -0.0067(7) C5 0.0579(11) 0.0452(10) 0.0444(10) -0.0035(8) -0.0039(9) -0.0172(9) C6 0.0760(14) 0.0605(12) 0.0438(11) -0.0061(9) -0.0068(10) -0.0191(11) C7 0.0837(16) 0.0539(12) 0.0418(11) 0.0003(9) 0.0089(11) -0.0142(11) C8 0.0667(13) 0.0502(11) 0.0545(12) -0.0027(9) 0.0137(10) -0.0194(10) C9 0.0469(10) 0.0417(10) 0.0539(11) -0.0073(8) 0.0065(8) -0.0120(8) C10 0.0468(10) 0.0355(9) 0.0424(10) -0.0082(8) -0.0030(8) -0.0029(7) C11 0.0369(9) 0.0433(9) 0.0386(9) -0.0061(7) 0.0015(7) -0.0016(7) C12 0.0362(10) 0.0465(10) 0.0717(13) -0.0110(9) -0.0010(9) -0.0064(8) C13 0.0463(12) 0.0678(14) 0.1043(19) -0.0164(13) -0.0080(12) -0.0192(10) C14 0.0361(11) 0.0993(19) 0.0826(17) -0.0040(14) -0.0049(10) -0.0146(12) C15 0.0406(12) 0.1001(19) 0.0715(15) -0.0254(14) -0.0046(10) 0.0139(12) C16 0.0479(12) 0.0697(14) 0.0579(13) -0.0240(11) -0.0072(9) 0.0116(10) C17 0.0301(8) 0.0390(9) 0.0365(9) -0.0025(7) -0.0005(7) -0.0044(7) C18 0.0420(10) 0.0434(10) 0.0446(10) -0.0071(8) 0.0045(8) -0.0110(8) C19 0.0503(11) 0.0465(10) 0.0635(13) -0.0061(9) 0.0014(9) -0.0185(9) C20 0.0423(10) 0.0549(12) 0.0583(12) 0.0060(9) 0.0000(9) -0.0176(9) C21 0.0372(10) 0.0677(13) 0.0443(11) 0.0008(9) 0.0077(8) -0.0108(9) C22 0.0385(9) 0.0517(10) 0.0394(10) -0.0083(8) 0.0032(7) -0.0071(8) C23 0.0339(8) 0.0378(9) 0.0344(9) -0.0047(7) -0.0015(7) -0.0108(7) C24 0.0367(10) 0.0852(15) 0.0536(12) -0.0183(11) -0.0100(9) 0.0089(10) C25 0.0536(14) 0.0851(18) 0.122(2) -0.0026(16) -0.0090(14) -0.0202(13) O5 0.0782(11) 0.0957(12) 0.0613(10) 0.0035(8) 0.0182(8) -0.0476(9) O6 0.0692(9) 0.0351(7) 0.0611(9) 0.0061(6) 0.0121(7) -0.0076(6) O7 0.0583(8) 0.0493(8) 0.0486(8) 0.0060(6) 0.0067(6) 0.0073(6) O8 0.0726(9) 0.0554(8) 0.0372(7) -0.0020(6) 0.0095(6) 0.0063(7) C26 0.0503(10) 0.0349(9) 0.0354(9) 0.0025(7) 0.0022(7) -0.0028(7) C27 0.0428(9) 0.0340(8) 0.0364(9) 0.0029(7) 0.0041(7) -0.0085(7) C28 0.0474(10) 0.0425(10) 0.0542(12) 0.0021(8) 0.0077(9) -0.0133(8) C29 0.0420(10) 0.0372(9) 0.0644(12) -0.0013(8) -0.0044(9) -0.0096(8) C30 0.0498(11) 0.0472(10) 0.0555(12) -0.0115(9) -0.0006(9) -0.0152(8) C31 0.0709(14) 0.0563(12) 0.0642(14) -0.0146(10) -0.0099(11) -0.0165(11) C32 0.0967(19) 0.0602(14) 0.096(2) -0.0060(13) -0.0402(16) -0.0272(14) C33 0.097(2) 0.0769(17) 0.124(2) 0.0113(17) -0.0472(18) -0.0501(16) C34 0.0703(15) 0.0660(14) 0.0944(18) 0.0188(13) -0.0216(13) -0.0352(12) C35 0.0464(10) 0.0348(9) 0.0407(9) -0.0019(7) 0.0001(7) -0.0110(7) C36 0.0368(9) 0.0359(8) 0.0349(9) -0.0042(7) -0.0031(7) -0.0082(7) C37 0.0487(10) 0.0370(9) 0.0410(10) -0.0069(7) -0.0044(8) -0.0063(7) C38 0.0503(11) 0.0510(11) 0.0448(11) -0.0142(9) 0.0042(8) -0.0038(9) C39 0.0452(10) 0.0623(12) 0.0431(10) -0.0077(9) 0.0074(8) -0.0130(9) C40 0.0510(11) 0.0454(10) 0.0519(11) -0.0010(8) 0.0088(9) -0.0148(8) C41 0.0454(10) 0.0379(9) 0.0488(10) -0.0061(8) 0.0073(8) -0.0085(8) C42 0.0550(11) 0.0431(10) 0.0333(9) -0.0066(7) -0.0012(8) -0.0044(8) C43 0.0627(13) 0.0588(12) 0.0559(13) -0.0076(10) -0.0157(10) -0.0039(10) C44 0.0647(15) 0.097(2) 0.0833(18) -0.0236(15) -0.0249(13) -0.0080(14) C45 0.0743(17) 0.109(2) 0.0835(18) -0.0374(16) -0.0079(14) -0.0361(16) C46 0.0884(18) 0.0701(15) 0.0724(16) -0.0229(12) 0.0051(13) -0.0346(14) C47 0.0632(13) 0.0486(11) 0.0546(12) -0.0093(9) 0.0019(10) -0.0117(10) C48 0.0573(12) 0.0408(10) 0.0403(10) 0.0016(8) 0.0072(8) -0.0072(9) C49 0.0917(18) 0.0588(13) 0.0524(12) -0.0109(10) 0.0166(12) 0.0112(12) C50 0.0972(19) 0.0686(15) 0.0630(13) -0.0184(11) 0.0233(13) -0.0293(13) 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 C23 O4 C24 118.34(14) C23 C1 C17 109.85(13) C23 C1 C2 110.17(13) C17 C1 C2 112.04(13) C23 C1 H1 108.2 C17 C1 H1 108.2 C2 C1 H1 108.2 C3 C2 C10 107.46(13) C3 C2 C1 110.02(13) C10 C2 C1 108.59(13) C3 C2 H2 110.2 C10 C2 H2 110.2 C1 C2 H2 110.2 O1 C3 C4 120.82(16) O1 C3 C2 120.18(16) C4 C3 C2 118.98(15) C5 C4 C9 118.88(17) C5 C4 C3 123.23(16) C9 C4 C3 117.90(16) C6 C5 C4 120.31(18) C6 C5 H5 119.8 C4 C5 H5 119.8 C7 C6 C5 119.7(2) C7 C6 H6 120.1 C5 C6 H6 120.1 C8 C7 C6 120.42(19) C8 C7 H7 119.8 C6 C7 H7 119.8 C7 C8 C9 120.04(19) C7 C8 H8 120.0 C9 C8 H8 120.0 C8 C9 C4 120.62(19) C8 C9 H9 119.7 C4 C9 H9 119.7 O2 C10 C11 120.59(16) O2 C10 C2 117.69(16) C11 C10 C2 121.71(14) C12 C11 C16 118.83(18) C12 C11 C10 123.17(15) C16 C11 C10 117.98(17) C13 C12 C11 120.04(18) C13 C12 H12 120.0 C11 C12 H12 120.0 C14 C13 C12 120.3(2) C14 C13 H13 119.9 C12 C13 H13 119.9 C15 C14 C13 119.8(2) C15 C14 H14 120.1 C13 C14 H14 120.1 C16 C15 C14 120.5(2) C16 C15 H15 119.8 C14 C15 H15 119.8 C15 C16 C11 120.6(2) C15 C16 H16 119.7 C11 C16 H16 119.7 C18 C17 C22 118.86(16) C18 C17 C1 120.72(14) C22 C17 C1 120.41(15) C17 C18 C19 120.45(17) C17 C18 H18 119.8 C19 C18 H18 119.8 C20 C19 C18 120.12(18) C20 C19 H19 119.9 C18 C19 H19 119.9 C21 C20 C19 119.83(17) C21 C20 H20 120.1 C19 C20 H20 120.1 C20 C21 C22 120.37(17) C20 C21 H21 119.8 C22 C21 H21 119.8 C21 C22 C17 120.36(18) C21 C22 H22 119.8 C17 C22 H22 119.8 O3 C23 O4 123.76(15) O3 C23 C1 125.43(15) O4 C23 C1 110.76(13) O4 C24 C25 108.31(19) O4 C24 H24A 110.0 C25 C24 H24A 110.0 O4 C24 H24B 110.0 C25 C24 H24B 110.0 H24A C24 H24B 108.4 C24 C25 H25A 109.5 C24 C25 H25B 109.5 H25A C25 H25B 109.5 C24 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C48 O8 C49 116.44(15) C48 C26 C42 110.59(15) C48 C26 C27 110.39(15) C42 C26 C27 111.60(14) C48 C26 H26 108.0 C42 C26 H26 108.0 C27 C26 H26 108.0 C28 C27 C26 111.14(14) C28 C27 C35 106.65(14) C26 C27 C35 108.56(14) C28 C27 H27 110.1 C26 C27 H27 110.1 C35 C27 H27 110.1 O5 C28 C29 121.61(18) O5 C28 C27 119.64(19) C29 C28 C27 118.71(15) C30 C29 C34 118.0(2) C30 C29 C28 122.73(17) C34 C29 C28 119.28(19) C29 C30 C31 120.77(19) C29 C30 H30 119.6 C31 C30 H30 119.6 C32 C31 C30 120.1(2) C32 C31 H31 120.0 C30 C31 H31 120.0 C33 C32 C31 119.9(2) C33 C32 H32 120.0 C31 C32 H32 120.0 C32 C33 C34 120.5(2) C32 C33 H33 119.7 C34 C33 H33 119.7 C33 C34 C29 120.7(2) C33 C34 H34 119.7 C29 C34 H34 119.7 O6 C35 C36 120.93(15) O6 C35 C27 117.49(15) C36 C35 C27 121.57(14) C37 C36 C41 119.13(16) C37 C36 C35 117.92(15) C41 C36 C35 122.95(15) C38 C37 C36 120.37(17) C38 C37 H37 119.8 C36 C37 H37 119.8 C39 C38 C37 120.21(17) C39 C38 H38 119.9 C37 C38 H38 119.9 C38 C39 C40 120.10(17) C38 C39 H39 120.0 C40 C39 H39 120.0 C41 C40 C39 120.18(17) C41 C40 H40 119.9 C39 C40 H40 119.9 C40 C41 C36 119.97(16) C40 C41 H41 120.0 C36 C41 H41 120.0 C43 C42 C47 118.4(2) C43 C42 C26 120.15(17) C47 C42 C26 121.37(17) C44 C43 C42 120.4(2) C44 C43 H43 119.8 C42 C43 H43 119.8 C45 C44 C43 120.6(2) C45 C44 H44 119.7 C43 C44 H44 119.7 C44 C45 C46 120.0(3) C44 C45 H45 120.0 C46 C45 H45 120.0 C45 C46 C47 120.0(2) C45 C46 H46 120.0 C47 C46 H46 120.0 C46 C47 C42 120.6(2) C46 C47 H47 119.7 C42 C47 H47 119.7 O7 C48 O8 123.78(17) O7 C48 C26 125.56(17) O8 C48 C26 110.64(15) C50 C49 O8 107.54(18) C50 C49 H49A 110.2 O8 C49 H49A 110.2 C50 C49 H49B 110.2 O8 C49 H49B 110.2 H49A C49 H49B 108.5 C49 C50 H50A 109.5 C49 C50 H50B 109.5 H50A C50 H50B 109.5 C49 C50 H50C 109.5 H50A C50 H50C 109.5 H50B C50 H50C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C3 1.211(2) O2 C10 1.219(2) O3 C23 1.2000(19) O4 C23 1.323(2) O4 C24 1.452(2) C1 C23 1.513(2) C1 C17 1.525(2) C1 C2 1.540(2) C1 H1 1.0000 C2 C3 1.531(2) C2 C10 1.537(2) C2 H2 1.0000 C3 C4 1.493(2) C4 C5 1.389(3) C4 C9 1.394(2) C5 C6 1.386(3) C5 H5 0.9500 C6 C7 1.384(3) C6 H6 0.9500 C7 C8 1.372(3) C7 H7 0.9500 C8 C9 1.377(3) C8 H8 0.9500 C9 H9 0.9500 C10 C11 1.481(3) C11 C12 1.387(3) C11 C16 1.391(2) C12 C13 1.385(3) C12 H12 0.9500 C13 C14 1.377(3) C13 H13 0.9500 C14 C15 1.371(4) C14 H14 0.9500 C15 C16 1.370(3) C15 H15 0.9500 C16 H16 0.9500 C17 C18 1.385(2) C17 C22 1.389(2) C18 C19 1.387(2) C18 H18 0.9500 C19 C20 1.380(3) C19 H19 0.9500 C20 C21 1.371(3) C20 H20 0.9500 C21 C22 1.387(3) C21 H21 0.9500 C22 H22 0.9500 C24 C25 1.477(3) C24 H24A 0.9900 C24 H24B 0.9900 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 O5 C28 1.214(2) O6 C35 1.214(2) O7 C48 1.200(2) O8 C48 1.338(2) O8 C49 1.463(2) C26 C48 1.511(2) C26 C42 1.516(3) C26 C27 1.532(2) C26 H26 1.0000 C27 C28 1.527(3) C27 C35 1.537(2) C27 H27 1.0000 C28 C29 1.487(3) C29 C30 1.384(3) C29 C34 1.390(3) C30 C31 1.386(3) C30 H30 0.9500 C31 C32 1.366(3) C31 H31 0.9500 C32 C33 1.365(4) C32 H32 0.9500 C33 C34 1.375(4) C33 H33 0.9500 C34 H34 0.9500 C35 C36 1.488(2) C36 C37 1.389(2) C36 C41 1.391(2) C37 C38 1.379(3) C37 H37 0.9500 C38 C39 1.371(3) C38 H38 0.9500 C39 C40 1.381(3) C39 H39 0.9500 C40 C41 1.381(2) C40 H40 0.9500 C41 H41 0.9500 C42 C43 1.388(3) C42 C47 1.388(3) C43 C44 1.377(3) C43 H43 0.9500 C44 C45 1.367(4) C44 H44 0.9500 C45 C46 1.372(4) C45 H45 0.9500 C46 C47 1.383(3) C46 H46 0.9500 C47 H47 0.9500 C49 C50 1.460(3) C49 H49A 0.9900 C49 H49B 0.9900 C50 H50A 0.9800 C50 H50B 0.9800 C50 H50C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C50 H50A O2 0.98 2.64 3.268(3) 122.0 1_545 C27 H27 O7 1.00 2.51 3.508(2) 172.7 2_657 C2 H2 O3 1.00 2.53 3.508(2) 164.7 2_766 C2 H2 O3 1.00 2.53 3.508(2) 164.7 2_766 C27 H27 O7 1.00 2.51 3.508(2) 172.7 2_657 C50 H50A O2 0.98 2.64 3.268(3) 122.0 1_545 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 C23 C1 C2 C3 -56.69(17) C17 C1 C2 C3 -179.30(13) C23 C1 C2 C10 -174.04(13) C17 C1 C2 C10 63.35(17) C10 C2 C3 O1 101.26(19) C1 C2 C3 O1 -16.8(2) C10 C2 C3 C4 -77.45(18) C1 C2 C3 C4 164.51(14) O1 C3 C4 C5 177.20(18) C2 C3 C4 C5 -4.1(2) O1 C3 C4 C9 -2.8(3) C2 C3 C4 C9 175.92(15) C9 C4 C5 C6 -0.1(3) C3 C4 C5 C6 179.97(17) C4 C5 C6 C7 -0.5(3) C5 C6 C7 C8 0.6(3) C6 C7 C8 C9 -0.1(3) C7 C8 C9 C4 -0.5(3) C5 C4 C9 C8 0.6(3) C3 C4 C9 C8 -179.45(16) C3 C2 C10 O2 -52.3(2) C1 C2 C10 O2 66.7(2) C3 C2 C10 C11 128.42(17) C1 C2 C10 C11 -112.61(17) O2 C10 C11 C12 -165.25(19) C2 C10 C11 C12 14.0(3) O2 C10 C11 C16 13.0(3) C2 C10 C11 C16 -167.73(17) C16 C11 C12 C13 -1.0(3) C10 C11 C12 C13 177.24(19) C11 C12 C13 C14 -0.7(4) C12 C13 C14 C15 2.1(4) C13 C14 C15 C16 -2.0(4) C14 C15 C16 C11 0.3(4) C12 C11 C16 C15 1.2(3) C10 C11 C16 C15 -177.1(2) C23 C1 C17 C18 -45.2(2) C2 C1 C17 C18 77.59(19) C23 C1 C17 C22 135.89(16) C2 C1 C17 C22 -101.31(18) C22 C17 C18 C19 -1.2(3) C1 C17 C18 C19 179.87(16) C17 C18 C19 C20 0.8(3) C18 C19 C20 C21 0.4(3) C19 C20 C21 C22 -1.3(3) C20 C21 C22 C17 0.9(3) C18 C17 C22 C21 0.4(3) C1 C17 C22 C21 179.29(16) C24 O4 C23 O3 2.8(3) C24 O4 C23 C1 -179.42(17) C17 C1 C23 O3 101.97(19) C2 C1 C23 O3 -21.9(2) C17 C1 C23 O4 -75.78(17) C2 C1 C23 O4 160.33(14) C23 O4 C24 C25 119.6(2) C48 C26 C27 C28 57.87(18) C42 C26 C27 C28 -178.72(14) C48 C26 C27 C35 174.86(14) C42 C26 C27 C35 -61.73(17) C26 C27 C28 O5 9.8(2) C35 C27 C28 O5 -108.4(2) C26 C27 C28 C29 -172.22(15) C35 C27 C28 C29 69.63(19) O5 C28 C29 C30 -168.78(19) C27 C28 C29 C30 13.3(3) O5 C28 C29 C34 11.7(3) C27 C28 C29 C34 -166.26(18) C34 C29 C30 C31 -1.6(3) C28 C29 C30 C31 178.90(18) C29 C30 C31 C32 0.6(3) C30 C31 C32 C33 0.9(4) C31 C32 C33 C34 -1.5(4) C32 C33 C34 C29 0.5(4) C30 C29 C34 C33 1.0(3) C28 C29 C34 C33 -179.5(2) C28 C27 C35 O6 55.0(2) C26 C27 C35 O6 -64.9(2) C28 C27 C35 C36 -124.05(17) C26 C27 C35 C36 116.12(17) O6 C35 C36 C37 -12.9(3) C27 C35 C36 C37 166.04(16) O6 C35 C36 C41 166.56(18) C27 C35 C36 C41 -14.5(3) C41 C36 C37 C38 2.0(3) C35 C36 C37 C38 -178.47(17) C36 C37 C38 C39 -0.8(3) C37 C38 C39 C40 -1.1(3) C38 C39 C40 C41 1.8(3) C39 C40 C41 C36 -0.6(3) C37 C36 C41 C40 -1.3(3) C35 C36 C41 C40 179.20(17) C48 C26 C42 C43 -135.16(18) C27 C26 C42 C43 101.54(19) C48 C26 C42 C47 47.7(2) C27 C26 C42 C47 -75.6(2) C47 C42 C43 C44 0.8(3) C26 C42 C43 C44 -176.38(19) C42 C43 C44 C45 -0.6(4) C43 C44 C45 C46 -0.4(4) C44 C45 C46 C47 1.1(4) C45 C46 C47 C42 -0.9(3) C43 C42 C47 C46 -0.1(3) C26 C42 C47 C46 177.09(18) C49 O8 C48 O7 -2.0(3) C49 O8 C48 C26 179.74(19) C42 C26 C48 O7 -96.5(2) C27 C26 C48 O7 27.5(3) C42 C26 C48 O8 81.66(19) C27 C26 C48 O8 -154.35(16) C48 O8 C49 C50 -170.9(2)