#------------------------------------------------------------------------------ #$Date: 2024-11-22 01:06:07 +0200 (Fri, 22 Nov 2024) $ #$Revision: 296050 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573252.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_1573252 loop_ _publ_author_name 'Navaneetha, N.' 'Maurya, Sundaram' 'Behera, Prativa' 'Jadhav, Sandip B.' 'Magham, Lakshmi Revati' 'Nanubolu, Jagadeesh Babu' 'Roy, Lisa' 'Chegondi, Rambabu' _publ_section_title ; BINAP-CuH-catalysed enantioselective allylation using alkoxyallenes to access 1,2-syn-tert,sec-diols ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC07002J _journal_year 2024 _chemical_formula_moiety 'C26 H34 O3' _chemical_formula_sum 'C26 H34 O3' _chemical_formula_weight 394.53 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2024-04-21 deposited with the CCDC. 2024-11-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.231(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.9997(8) _cell_length_b 10.7801(6) _cell_length_c 16.7201(11) _cell_measurement_reflns_used 9992 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 28.466 _cell_measurement_theta_min 2.839 _cell_volume 2324.5(2) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON III C7 HPAD' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 27035 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.499 _diffrn_reflns_theta_min 2.839 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_density_diffrn 1.127 _exptl_crystal_description block _exptl_crystal_F_000 856 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM/hexane (1:9)' _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.210 _refine_diff_density_max 0.214 _refine_diff_density_min -0.142 _refine_diff_density_rms 0.031 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 330 _refine_ls_number_reflns 5306 _refine_ls_number_restraints 414 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0506 _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^)+(0.0618P)^2^+0.5674P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1249 _refine_ls_wR_factor_ref 0.1436 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3734 _reflns_number_total 5306 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07002j2.cif _cod_data_source_block KB1077_0m _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1573252 _shelx_shelxl_version_number 2019/3 _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 0.982 _shelx_estimated_absorpt_t_max 0.985 _shelx_res_file ; TITL KB1077_0m_a.res in P2(1)/n KB1077_0m.res created by SHELXL-2019/3 at 12:11:13 on 20-Apr-2024 CELL 0.71073 12.9997 10.7801 16.7201 90.0000 97.2307 90.0000 ZERR 4.00 0.0008 0.0006 0.0011 0.0000 0.0021 0.0000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H O UNIT 104 136 12 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 21 ACTA L.S. 10 FMAP 2 PLAN 5 SIZE 0.26 0.23 0.21 OMIT -3 55 OMIT 2 0 2 OMIT -3 1 1 OMIT -1 0 1 OMIT 1 0 1 OMIT 0 1 1 DELU 0.01 0.01 C2 C2D C3 C3D C4 C4D C5 C5D C6 C6D C7 C7D SIMU 0.01 0.01 C2 C2D C3 C3D C4 C4D C5 C5D C6 C6D C7 C7D DELU 0.01 0.01 C8 C8D C9 C9D C10 C10D C11 C11D C12 C12D C13 C13D SIMU 0.01 0.01 C8 C8D C9 C9D C10 C10D C11 C11D C12 C12D C13 C13D BOND $H CONF WGHT 0.061800 0.567400 FVAR 1.19185 0.64954 C1 1 0.447045 0.441920 0.706088 11.00000 0.03601 0.04465 = 0.04529 -0.00348 0.00396 -0.00488 AFIX 13 H1 2 0.417286 0.411935 0.753523 11.00000 -1.20000 AFIX 66 PART 1 C2 1 0.437791 0.338735 0.642990 21.00000 0.04142 0.03827 = 0.04775 -0.00186 0.00080 -0.00707 C3 1 0.509683 0.242732 0.652296 21.00000 0.05376 0.04556 = 0.05412 -0.00071 -0.00023 0.00263 AFIX 43 H3 2 0.566464 0.247594 0.691998 21.00000 -1.20000 AFIX 65 C4 1 0.496709 0.139463 0.602263 21.00000 0.06802 0.05106 = 0.06905 -0.00764 -0.00257 0.00722 AFIX 43 H4 2 0.544810 0.075231 0.608489 21.00000 -1.20000 AFIX 65 C5 1 0.411843 0.132196 0.542924 21.00000 0.07602 0.06220 = 0.09612 -0.03489 -0.00795 0.00353 AFIX 43 H5 2 0.403163 0.063102 0.509448 21.00000 -1.20000 AFIX 65 C6 1 0.339951 0.228197 0.533617 21.00000 0.06006 0.07406 = 0.08054 -0.03077 -0.01875 0.00119 AFIX 43 H6 2 0.283170 0.223334 0.493915 21.00000 -1.20000 AFIX 65 C7 1 0.352923 0.331467 0.583650 21.00000 0.04965 0.05526 = 0.06008 -0.01076 -0.00676 0.00779 AFIX 43 H7 2 0.304822 0.395699 0.577423 21.00000 -1.20000 AFIX 66 PART 2 C2D 1 0.433556 0.338761 0.645153 -21.00000 0.04156 0.04465 = 0.04806 -0.00215 0.00862 0.00116 C3D 1 0.513307 0.258578 0.631631 -21.00000 0.04460 0.05206 = 0.05316 -0.00871 -0.00191 -0.00044 AFIX 43 H3D 2 0.579481 0.270086 0.658930 -21.00000 -1.20000 AFIX 65 C4D 1 0.494153 0.161197 0.577308 -21.00000 0.06850 0.05526 = 0.08384 -0.02658 -0.00143 0.01201 AFIX 43 H4D 2 0.547512 0.107550 0.568262 -21.00000 -1.20000 AFIX 65 C5D 1 0.395248 0.143997 0.536507 -21.00000 0.07512 0.06589 = 0.09479 -0.04055 -0.00552 -0.00367 AFIX 43 H5D 2 0.382434 0.078842 0.500162 -21.00000 -1.20000 AFIX 65 C6D 1 0.315497 0.224178 0.550028 -21.00000 0.06032 0.07756 = 0.08888 -0.03084 -0.00249 -0.00307 AFIX 43 H6D 2 0.249323 0.212670 0.522729 -21.00000 -1.20000 AFIX 65 C7D 1 0.334649 0.321560 0.604351 -21.00000 0.04802 0.06377 = 0.06170 -0.01585 0.00348 -0.00576 AFIX 43 H7D 2 0.281290 0.375207 0.613398 -21.00000 -1.20000 AFIX 66 PART 0 PART 1 C8 1 0.390794 0.564567 0.677098 21.00000 0.04097 0.04445 = 0.05941 -0.01296 -0.00477 0.00302 C9 1 0.429782 0.632755 0.617085 21.00000 0.05829 0.05673 = 0.05902 0.00548 -0.00817 0.00532 AFIX 43 H9 2 0.485539 0.602507 0.593148 21.00000 -1.20000 AFIX 65 C10 1 0.385435 0.746151 0.592849 21.00000 0.07221 0.06327 = 0.07072 0.00959 -0.00896 0.00399 AFIX 43 H10 2 0.411521 0.791773 0.552696 21.00000 -1.20000 AFIX 65 C11 1 0.302100 0.791361 0.628625 21.00000 0.08377 0.05740 = 0.08543 -0.00134 -0.00905 0.02011 AFIX 43 H11 2 0.272430 0.867231 0.612409 21.00000 -1.20000 AFIX 65 C12 1 0.263111 0.723175 0.688638 21.00000 0.07616 0.05921 = 0.08800 0.00375 0.00870 0.02862 AFIX 43 H12 2 0.207355 0.753424 0.712574 21.00000 -1.20000 AFIX 65 C13 1 0.307457 0.609778 0.712875 21.00000 0.05331 0.05316 = 0.08005 -0.00227 0.00562 0.01430 AFIX 43 H13 2 0.281371 0.564157 0.753028 21.00000 -1.20000 AFIX 66 PART 2 C9D 1 0.390043 0.554757 0.685057 -21.00000 0.04405 0.04797 = 0.05710 -0.01144 -0.01204 -0.00139 C8D 1 0.409330 0.633190 0.622659 -21.00000 0.05619 0.05456 = 0.06070 -0.00695 -0.00863 0.01009 AFIX 43 H8D 2 0.461279 0.613842 0.591237 -21.00000 -1.20000 AFIX 65 C10D 1 0.350972 0.740542 0.607224 -21.00000 0.07090 0.06136 = 0.07233 -0.00057 -0.00903 0.01812 AFIX 43 H10D 2 0.363876 0.793018 0.565475 -21.00000 -1.20000 AFIX 65 C11D 1 0.273328 0.769460 0.654188 -21.00000 0.07793 0.05679 = 0.07847 0.00148 -0.00442 0.02446 AFIX 43 H11D 2 0.234283 0.841286 0.643860 -21.00000 -1.20000 AFIX 65 C12D 1 0.254040 0.691029 0.716586 -21.00000 0.07816 0.06398 = 0.09070 -0.00465 0.00166 0.01972 AFIX 43 H12D 2 0.202091 0.710378 0.748007 -21.00000 -1.20000 AFIX 65 C13D 1 0.312397 0.583677 0.732022 -21.00000 0.05790 0.05878 = 0.08283 -0.01151 -0.00666 0.02039 AFIX 43 H13D 2 0.299493 0.531201 0.773770 -21.00000 -1.20000 AFIX 0 PART 0 C14 1 0.575685 0.516565 0.810005 11.00000 0.04463 0.03823 = 0.03733 -0.00297 0.00403 -0.00317 AFIX 13 H14 2 0.518163 0.570666 0.820195 11.00000 -1.20000 AFIX 0 C15 1 0.582496 0.410489 0.868288 11.00000 0.08302 0.05033 = 0.04791 0.00469 -0.00160 -0.01482 AFIX 43 H15 2 0.637250 0.355053 0.867932 11.00000 -1.20000 AFIX 0 C16 1 0.516516 0.391088 0.919414 11.00000 0.14835 0.08792 = 0.05670 0.00903 0.02253 -0.04470 AFIX 93 H16A 2 0.460936 0.444893 0.921227 11.00000 -1.20000 H16B 2 0.524962 0.323423 0.954124 11.00000 -1.20000 AFIX 0 C17 1 0.675286 0.593991 0.814590 11.00000 0.03645 0.04075 = 0.04136 -0.00341 0.00161 0.00125 C18 1 0.664466 0.699395 0.753194 11.00000 0.04132 0.04311 = 0.03794 -0.00367 0.00743 -0.00830 AFIX 23 H18A 2 0.732073 0.736465 0.751137 11.00000 -1.20000 H18B 2 0.641132 0.665366 0.700310 11.00000 -1.20000 AFIX 0 C19 1 0.588898 0.800346 0.772147 11.00000 0.04364 0.03781 = 0.04092 0.00114 0.00317 -0.00669 AFIX 23 H19A 2 0.519465 0.765903 0.767463 11.00000 -1.20000 H19B 2 0.588949 0.866401 0.732759 11.00000 -1.20000 AFIX 0 C20 1 0.616310 0.854504 0.856644 11.00000 0.04239 0.03999 = 0.04525 -0.00606 0.00657 -0.00871 C21 1 0.627677 0.749023 0.918272 11.00000 0.05101 0.04856 = 0.03745 -0.00658 0.00617 -0.01107 AFIX 23 H21A 2 0.651466 0.783049 0.971075 11.00000 -1.20000 H21B 2 0.560221 0.711757 0.920687 11.00000 -1.20000 AFIX 0 C22 1 0.702937 0.648930 0.898645 11.00000 0.04802 0.04792 = 0.04084 -0.00052 -0.00318 -0.00562 AFIX 23 H22A 2 0.703803 0.583024 0.938221 11.00000 -1.20000 H22B 2 0.772151 0.683911 0.902767 11.00000 -1.20000 AFIX 0 C23 1 0.768537 0.967138 0.922776 11.00000 0.07371 0.07908 = 0.06234 -0.01120 -0.00505 -0.03305 AFIX 137 H23A 2 0.837320 0.990546 0.913562 11.00000 -1.50000 H23B 2 0.772421 0.908664 0.966356 11.00000 -1.50000 H23C 2 0.731209 1.039406 0.936345 11.00000 -1.50000 AFIX 0 C24 1 0.538117 0.953127 0.878214 11.00000 0.05999 0.05282 = 0.06546 -0.01506 0.01184 -0.00061 AFIX 13 H24 2 0.564544 0.984999 0.931767 11.00000 -1.20000 AFIX 0 C25 1 0.429935 0.903157 0.883748 11.00000 0.05683 0.08073 = 0.09683 -0.00746 0.02102 0.01021 AFIX 137 H25A 2 0.401755 0.869158 0.832580 11.00000 -1.50000 H25B 2 0.386220 0.969251 0.898012 11.00000 -1.50000 H25C 2 0.433488 0.839494 0.924150 11.00000 -1.50000 AFIX 0 C26 1 0.530908 1.063450 0.820710 11.00000 0.10559 0.04691 = 0.14639 0.00947 0.03979 0.01829 AFIX 137 H26A 2 0.496576 1.038445 0.769024 11.00000 -1.50000 H26B 2 0.599402 1.092486 0.814957 11.00000 -1.50000 H26C 2 0.492209 1.128879 0.841944 11.00000 -1.50000 AFIX 0 O1 3 0.554766 0.466789 0.729386 11.00000 0.03710 0.04531 = 0.03932 -0.00576 0.00157 -0.00337 O2 3 0.759963 0.514682 0.802379 11.00000 0.04365 0.06130 = 0.06037 -0.00897 -0.00083 0.01248 H2O 2 0.751667 0.489178 0.751184 11.00000 0.09349 O3 3 0.716481 0.912335 0.852162 11.00000 0.04955 0.05034 = 0.04941 -0.00584 0.00393 -0.01780 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KB1077_0m_a.res in P2(1)/n REM wR2 = 0.1436, GooF = S = 1.031, Restrained GooF = 1.032 for all data REM R1 = 0.0506 for 3734 Fo > 4sig(Fo) and 0.0771 for all 5306 data REM 330 parameters refined using 414 restraints END WGHT 0.0618 0.5674 REM Highest difference peak 0.214, deepest hole -0.142, 1-sigma level 0.031 Q1 1 0.7357 0.9629 0.9734 11.00000 0.05 0.21 Q2 1 0.6243 0.5597 0.8099 11.00000 0.05 0.21 Q3 1 0.5968 0.8235 0.8178 11.00000 0.05 0.17 Q4 1 0.6822 0.6168 0.8538 11.00000 0.05 0.17 Q5 1 0.6658 0.6463 0.7884 11.00000 0.05 0.16 ; _shelx_res_checksum 47401 _shelx_hkl_file ; 1 0 0 0.03 0.24 1 0 0 0.17 0.47 -1 0 0 0.20 0.22 -1 0 0 0.61 0.50 -2 0 0 2081.38 71.82 3 0 0 -1.42 1.99 3 0 0 2.45 1.56 -3 0 0 -0.69 1.38 -3 0 0 0.65 2.97 4 0 0 1055.62 38.06 4 0 0 1046.70 39.07 -4 0 0 1107.56 38.16 -4 0 0 1032.96 40.63 4 0 0 1173.53 38.52 5 0 0 -1.14 2.16 -5 0 0 2.12 3.39 -5 0 0 3.05 1.86 5 0 0 1.80 1.87 5 0 0 0.81 1.93 6 0 0 4106.96 138.09 6 0 0 3958.53 138.81 7 0 0 6.07 3.02 7 0 0 2.47 2.49 7 0 0 2.60 2.48 -7 0 0 6.14 2.60 -8 0 0 379.25 16.87 8 0 0 404.49 17.68 8 0 0 416.99 17.68 8 0 0 422.11 18.05 9 0 0 1.24 3.09 9 0 0 0.64 2.88 9 0 0 3.37 3.74 -9 0 0 4.89 3.17 10 0 0 12.35 4.21 10 0 0 11.05 4.38 10 0 0 15.53 4.91 -10 0 0 14.78 4.20 11 0 0 -1.68 4.07 11 0 0 -1.43 3.75 11 0 0 0.41 3.98 -11 0 0 0.40 3.65 12 0 0 72.07 7.77 -12 0 0 82.52 8.10 13 0 0 -0.77 3.99 -13 0 0 -3.46 3.91 14 0 0 4.88 5.02 -14 0 0 0.05 4.70 -15 0 0 -5.83 4.80 15 0 0 6.24 5.60 -16 0 0 43.73 8.84 -17 0 0 0.29 6.26 -18 0 0 34.42 8.88 0 -1 0 0.57 0.44 0 -1 0 1.27 0.39 0 -1 0 0.01 0.31 0 1 0 -0.07 0.42 3 -1 0 1565.53 55.98 -3 -1 0 1571.80 55.91 -3 1 0 1575.10 57.10 3 1 0 1636.21 54.44 3 1 0 1578.97 54.28 -4 -1 0 2000.96 71.62 4 -1 0 2039.19 71.08 4 1 0 2017.40 69.65 -4 1 0 1937.78 72.57 4 1 0 2066.41 69.29 4 1 0 2039.26 69.41 -5 -1 0 109.35 5.90 5 -1 0 104.52 5.76 5 -1 0 99.07 7.05 5 1 0 97.72 5.80 5 1 0 102.31 5.99 -5 1 0 92.79 8.04 5 1 0 104.21 5.06 5 1 0 107.13 5.58 -5 1 0 99.39 5.47 6 -1 0 357.60 15.31 -6 -1 0 367.47 14.98 6 -1 0 368.29 15.50 6 -1 0 388.47 16.78 -6 1 0 401.14 15.28 6 1 0 369.41 15.41 6 1 0 335.40 14.20 6 1 0 368.04 15.13 6 1 0 359.32 14.95 7 -1 0 470.12 19.47 7 -1 0 454.29 19.27 7 -1 0 489.51 20.49 -7 -1 0 503.83 18.91 7 1 0 471.80 19.08 7 1 0 476.74 19.00 7 1 0 472.14 19.04 -7 1 0 458.00 18.82 7 1 0 429.73 17.90 8 -1 0 143.52 10.13 8 -1 0 158.50 9.46 -8 -1 0 163.28 8.80 8 -1 0 174.30 9.59 8 1 0 162.63 8.93 8 1 0 164.45 9.09 8 1 0 158.46 7.97 -8 1 0 165.96 8.98 8 1 0 163.60 9.28 9 -1 0 1463.38 56.26 9 -1 0 1496.09 55.96 9 -1 0 1561.90 56.11 -9 -1 0 1488.09 54.89 9 1 0 1496.83 55.43 9 1 0 1464.77 55.18 -9 1 0 1631.52 55.35 9 1 0 1570.34 55.16 9 1 0 1508.34 53.80 10 -1 0 64.19 7.36 -10 -1 0 68.57 6.62 10 -1 0 64.71 7.58 10 -1 0 63.34 7.75 10 1 0 68.62 6.85 10 1 0 72.75 7.78 -10 1 0 61.93 6.61 10 1 0 66.05 5.31 10 1 0 62.58 7.05 11 -1 0 36.42 6.61 -11 -1 0 42.56 6.23 11 1 0 35.75 6.61 -11 1 0 37.29 5.93 11 1 0 32.75 6.14 11 1 0 29.28 5.20 12 -1 0 2.89 4.11 12 -1 0 13.87 5.90 -12 -1 0 14.90 5.04 -12 1 0 8.60 4.73 12 1 0 7.62 3.89 13 -1 0 -2.92 5.29 -13 -1 0 9.33 4.74 -13 1 0 2.97 4.41 13 1 0 4.72 4.31 14 -1 0 0.55 5.22 -14 -1 0 1.56 5.05 14 1 0 5.60 5.35 -14 1 0 0.30 4.84 -15 -1 0 40.78 7.44 15 -1 0 29.66 7.20 -15 1 0 32.29 7.51 -16 -1 0 4.80 5.88 -16 1 0 5.35 6.24 -17 -1 0 26.74 7.84 -17 1 0 17.81 7.51 -18 -1 0 -1.61 6.54 -18 1 0 5.22 7.32 0 -2 0 177.05 6.93 0 -2 0 176.60 6.59 0 2 0 157.01 8.11 1 -2 0 932.34 32.71 1 -2 0 923.15 31.67 -1 -2 0 932.99 32.31 1 2 0 879.06 32.57 2 -2 0 1930.56 65.40 -2 2 0 1805.73 66.01 -3 -2 0 1067.44 36.92 3 -2 0 1078.28 39.15 3 -2 0 994.09 37.37 3 2 0 1098.87 36.79 3 2 0 1088.22 36.40 -3 2 0 1049.56 40.37 -3 2 0 1078.99 37.49 3 2 0 1096.21 36.87 -4 2 0 4833.11 167.74 5 -2 0 514.45 18.85 5 -2 0 469.96 20.48 -5 -2 0 483.58 18.48 5 2 0 475.07 18.11 -5 2 0 460.50 18.47 5 2 0 487.67 17.68 5 2 0 466.46 17.72 5 2 0 476.20 16.86 6 -2 0 4246.42 145.10 6 -2 0 4168.65 146.70 6 2 0 4274.18 144.35 7 -2 0 2177.37 77.20 -7 -2 0 2310.87 76.75 7 -2 0 2186.41 78.67 7 -2 0 2121.40 77.26 7 2 0 2192.95 76.52 7 2 0 2212.11 75.91 -7 2 0 2228.42 76.82 7 2 0 2080.83 75.81 8 -2 0 757.46 31.11 8 -2 0 729.63 29.96 -8 -2 0 808.73 29.29 8 -2 0 724.38 29.83 8 2 0 776.56 28.46 8 2 0 751.02 28.57 8 2 0 776.28 26.82 -8 2 0 768.61 29.41 8 2 0 756.23 29.23 -9 -2 0 10.82 3.51 9 -2 0 4.66 3.69 9 -2 0 13.18 4.86 9 -2 0 16.07 4.59 9 2 0 12.79 3.22 9 2 0 10.09 1.66 -9 2 0 13.36 3.98 9 2 0 8.39 3.31 9 2 0 14.25 3.90 10 -2 0 285.33 15.63 -10 -2 0 286.18 13.74 10 -2 0 249.21 14.56 10 -2 0 258.37 16.22 -10 2 0 292.38 14.30 10 2 0 286.47 12.98 10 2 0 281.37 14.71 11 -2 0 339.38 21.25 -11 -2 0 406.63 18.25 11 -2 0 411.36 20.03 11 2 0 406.57 17.09 -11 2 0 399.73 18.59 11 2 0 395.75 19.43 12 -2 0 62.60 8.75 12 -2 0 36.80 7.43 -12 -2 0 59.30 7.62 -12 2 0 54.91 7.36 12 2 0 60.14 6.63 -13 -2 0 22.66 5.68 13 -2 0 27.42 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2 0 23 23.72 13.29 -7 -1 23 10.26 9.91 -6 -1 23 15.08 10.15 -5 -1 23 -3.58 9.56 -5 1 23 26.94 13.70 -4 -1 23 30.24 13.31 -4 1 23 36.80 13.48 -3 -1 23 25.59 12.01 -3 1 23 45.48 14.44 -2 -1 23 34.79 12.28 -2 1 23 29.15 11.90 -1 -1 23 27.63 12.58 -1 1 23 23.40 11.07 0 -1 23 22.22 12.06 0 1 23 28.39 11.70 1 -1 23 3.61 10.18 1 1 23 42.69 13.27 2 1 23 35.90 12.42 -6 -2 23 -2.71 9.60 -5 -2 23 -5.53 8.92 -5 2 23 36.40 14.24 -4 -2 23 54.30 14.27 -4 -2 23 -4.64 9.66 -4 2 23 27.72 13.32 -3 -2 23 27.80 13.05 -3 -2 23 -6.76 9.89 -3 2 23 45.66 13.80 -2 -2 23 -1.66 8.68 -2 -2 23 33.11 8.78 -2 -2 23 19.55 12.74 -2 2 23 25.41 11.77 -1 -2 23 36.06 13.16 -1 2 23 46.56 13.76 0 -2 23 25.28 8.18 0 -2 23 25.80 18.38 0 2 23 53.22 12.92 1 2 23 39.05 12.70 2 2 23 40.00 12.69 -5 -3 23 4.21 11.16 -4 -3 23 48.75 13.81 -4 3 23 62.56 15.12 -3 -3 23 36.77 9.67 -3 -3 23 16.19 10.48 -3 3 23 53.38 14.61 -2 -3 23 49.08 10.69 -2 -3 23 32.97 11.30 -2 3 23 75.12 15.33 -1 -3 23 -1.11 9.46 -1 3 23 20.00 11.22 0 -3 23 -4.70 8.79 0 -3 23 29.32 9.03 -3 -4 23 32.63 13.69 -3 4 23 41.21 13.81 -2 -4 23 -0.12 10.58 -2 4 23 26.51 12.28 -1 -4 23 5.10 9.70 -1 -4 23 23.01 10.18 -1 4 23 63.12 14.28 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6268 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71080 13.006 10.774 16.714 90.037 97.220 89.983 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 14739 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.44705(11) 0.44192(13) 0.70609(9) 0.0421(3) Uani 1 1 d . . . . . H1 H 0.417286 0.411935 0.753523 0.050 Uiso 1 1 calc R U . A 1 C2 C 0.4378(4) 0.3387(4) 0.6430(2) 0.0429(11) Uani 0.650(11) 1 d G U P B 1 C3 C 0.5097(4) 0.2427(5) 0.6523(3) 0.0517(10) Uani 0.650(11) 1 d G U P B 1 H3 H 0.566464 0.247594 0.691998 0.062 Uiso 0.650(11) 1 calc R U P B 1 C4 C 0.4967(4) 0.1395(4) 0.6023(3) 0.0637(10) Uani 0.650(11) 1 d G U P B 1 H4 H 0.544810 0.075231 0.608489 0.076 Uiso 0.650(11) 1 calc R U P B 1 C5 C 0.4118(4) 0.1322(4) 0.5429(2) 0.0797(13) Uani 0.650(11) 1 d G U P B 1 H5 H 0.403163 0.063102 0.509448 0.096 Uiso 0.650(11) 1 calc R U P B 1 C6 C 0.3400(4) 0.2282(5) 0.5336(3) 0.0739(13) Uani 0.650(11) 1 d G U P B 1 H6 H 0.283170 0.223334 0.493915 0.089 Uiso 0.650(11) 1 calc R U P B 1 C7 C 0.3529(4) 0.3315(5) 0.5836(3) 0.0562(11) Uani 0.650(11) 1 d G U P B 1 H7 H 0.304822 0.395699 0.577423 0.067 Uiso 0.650(11) 1 calc R U P B 1 C2D C 0.4336(8) 0.3388(8) 0.6452(4) 0.044(2) Uani 0.350(11) 1 d G U P B 2 C3D C 0.5133(6) 0.2586(10) 0.6316(6) 0.0506(16) Uani 0.350(11) 1 d G U P B 2 H3D H 0.579481 0.270086 0.658930 0.061 Uiso 0.350(11) 1 calc R U P B 2 C4D C 0.4942(7) 0.1612(9) 0.5773(6) 0.0701(19) Uani 0.350(11) 1 d G U P B 2 H4D H 0.547512 0.107550 0.568262 0.084 Uiso 0.350(11) 1 calc R U P B 2 C5D C 0.3952(8) 0.1440(9) 0.5365(5) 0.0800(19) Uani 0.350(11) 1 d G U P B 2 H5D H 0.382434 0.078842 0.500162 0.096 Uiso 0.350(11) 1 calc R U P B 2 C6D C 0.3155(7) 0.2242(11) 0.5500(6) 0.077(2) Uani 0.350(11) 1 d G U P B 2 H6D H 0.249323 0.212670 0.522729 0.092 Uiso 0.350(11) 1 calc R U P B 2 C7D C 0.3346(7) 0.3216(10) 0.6044(6) 0.0581(18) Uani 0.350(11) 1 d G U P B 2 H7D H 0.281290 0.375207 0.613398 0.070 Uiso 0.350(11) 1 calc R U P B 2 C8 C 0.3908(5) 0.5646(5) 0.6771(4) 0.0492(10) Uani 0.650(11) 1 d G U P B 1 C9 C 0.4298(4) 0.6328(6) 0.6171(4) 0.0593(10) Uani 0.650(11) 1 d G U P B 1 H9 H 0.485539 0.602507 0.593148 0.071 Uiso 0.650(11) 1 calc R U P B 1 C10 C 0.3854(4) 0.7462(5) 0.5928(3) 0.0703(11) Uani 0.650(11) 1 d G U P B 1 H10 H 0.411521 0.791773 0.552696 0.084 Uiso 0.650(11) 1 calc R U P B 1 C11 C 0.3021(4) 0.7914(4) 0.6286(3) 0.0772(14) Uani 0.650(11) 1 d G U P B 1 H11 H 0.272430 0.867231 0.612409 0.093 Uiso 0.650(11) 1 calc R U P B 1 C12 C 0.2631(3) 0.7232(4) 0.6886(4) 0.0746(13) Uani 0.650(11) 1 d G U P B 1 H12 H 0.207355 0.753424 0.712574 0.090 Uiso 0.650(11) 1 calc R U P B 1 C13 C 0.3075(4) 0.6098(5) 0.7129(4) 0.0624(10) Uani 0.650(11) 1 d G U P B 1 H13 H 0.281371 0.564157 0.753028 0.075 Uiso 0.650(11) 1 calc R U P B 1 C9D C 0.3900(9) 0.5548(10) 0.6851(8) 0.0513(17) Uani 0.350(11) 1 d G U P B 2 C8D C 0.4093(8) 0.6332(11) 0.6227(7) 0.0585(16) Uani 0.350(11) 1 d G U P B 2 H8D H 0.461279 0.613842 0.591237 0.070 Uiso 0.350(11) 1 calc R U P B 2 C10D C 0.3510(8) 0.7405(9) 0.6072(6) 0.0697(17) Uani 0.350(11) 1 d G U P B 2 H10D H 0.363876 0.793018 0.565475 0.084 Uiso 0.350(11) 1 calc R U P B 2 C11D C 0.2733(7) 0.7695(8) 0.6542(6) 0.072(2) Uani 0.350(11) 1 d G U P B 2 H11D H 0.234283 0.841286 0.643860 0.087 Uiso 0.350(11) 1 calc R U P B 2 C12D C 0.2540(6) 0.6910(9) 0.7166(6) 0.0784(19) Uani 0.350(11) 1 d G U P B 2 H12D H 0.202091 0.710378 0.748007 0.094 Uiso 0.350(11) 1 calc R U P B 2 C13D C 0.3124(9) 0.5837(9) 0.7320(7) 0.0678(17) Uani 0.350(11) 1 d G U P B 2 H13D H 0.299493 0.531201 0.773770 0.081 Uiso 0.350(11) 1 calc R U P B 2 C14 C 0.57569(11) 0.51656(13) 0.81001(8) 0.0402(3) Uani 1 1 d . . . . . H14 H 0.518163 0.570666 0.820195 0.048 Uiso 1 1 calc R U . . . C15 C 0.58250(16) 0.41049(16) 0.86829(10) 0.0613(5) Uani 1 1 d . . . . . H15 H 0.637250 0.355053 0.867932 0.074 Uiso 1 1 calc R U . . . C16 C 0.5165(2) 0.3911(2) 0.91941(12) 0.0968(8) Uani 1 1 d . . . . . H16A H 0.460936 0.444893 0.921227 0.116 Uiso 1 1 calc R U . . . H16B H 0.524962 0.323423 0.954124 0.116 Uiso 1 1 calc R U . . . C17 C 0.67529(10) 0.59399(13) 0.81459(8) 0.0398(3) Uani 1 1 d . . . . . C18 C 0.66447(11) 0.69939(13) 0.75319(8) 0.0406(3) Uani 1 1 d . . . . . H18A H 0.732073 0.736465 0.751137 0.049 Uiso 1 1 calc R U . . . H18B H 0.641132 0.665366 0.700310 0.049 Uiso 1 1 calc R U . . . C19 C 0.58890(11) 0.80035(13) 0.77215(8) 0.0410(3) Uani 1 1 d . . . . . H19A H 0.519465 0.765903 0.767463 0.049 Uiso 1 1 calc R U . . . H19B H 0.588949 0.866401 0.732759 0.049 Uiso 1 1 calc R U . . . C20 C 0.61631(11) 0.85450(13) 0.85664(9) 0.0425(3) Uani 1 1 d . . . . . C21 C 0.62768(12) 0.74902(14) 0.91827(8) 0.0456(4) Uani 1 1 d . . . . . H21A H 0.651466 0.783049 0.971075 0.055 Uiso 1 1 calc R U . . . H21B H 0.560221 0.711757 0.920687 0.055 Uiso 1 1 calc R U . . . C22 C 0.70294(12) 0.64893(14) 0.89865(9) 0.0463(4) Uani 1 1 d . . . . . H22A H 0.703803 0.583024 0.938221 0.056 Uiso 1 1 calc R U . . . H22B H 0.772151 0.683911 0.902767 0.056 Uiso 1 1 calc R U . . . C23 C 0.76854(16) 0.9671(2) 0.92278(11) 0.0729(6) Uani 1 1 d . . . . . H23A H 0.837320 0.990546 0.913562 0.109 Uiso 1 1 calc R U . . . H23B H 0.772421 0.908664 0.966356 0.109 Uiso 1 1 calc R U . . . H23C H 0.731209 1.039406 0.936345 0.109 Uiso 1 1 calc R U . . . C24 C 0.53812(14) 0.95313(16) 0.87821(11) 0.0591(4) Uani 1 1 d . . . . . H24 H 0.564544 0.984999 0.931767 0.071 Uiso 1 1 calc R U . . . C25 C 0.42994(15) 0.9032(2) 0.88375(14) 0.0772(6) Uani 1 1 d . . . . . H25A H 0.401755 0.869158 0.832580 0.116 Uiso 1 1 calc R U . . . H25B H 0.386220 0.969251 0.898012 0.116 Uiso 1 1 calc R U . . . H25C H 0.433488 0.839494 0.924150 0.116 Uiso 1 1 calc R U . . . C26 C 0.5309(2) 1.06345(19) 0.82071(18) 0.0976(8) Uani 1 1 d . . . . . H26A H 0.496576 1.038445 0.769024 0.146 Uiso 1 1 calc R U . . . H26B H 0.599402 1.092486 0.814957 0.146 Uiso 1 1 calc R U . . . H26C H 0.492209 1.128879 0.841944 0.146 Uiso 1 1 calc R U . . . O1 O 0.55477(7) 0.46679(9) 0.72939(5) 0.0409(3) Uani 1 1 d . . . . . O2 O 0.75996(8) 0.51468(11) 0.80238(8) 0.0557(3) Uani 1 1 d . . . . . H2O H 0.7517(18) 0.489(2) 0.7512(15) 0.093(8) Uiso 1 1 d . . . . . O3 O 0.71648(8) 0.91234(10) 0.85216(6) 0.0500(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0360(7) 0.0447(8) 0.0453(8) -0.0035(6) 0.0040(6) -0.0049(6) C2 0.041(2) 0.0383(19) 0.048(2) -0.0019(18) 0.0008(18) -0.0071(18) C3 0.0538(17) 0.0456(17) 0.054(2) -0.0007(16) -0.0002(15) 0.0026(13) C4 0.0680(18) 0.0511(19) 0.069(2) -0.0076(17) -0.0026(17) 0.0072(15) C5 0.076(2) 0.062(2) 0.096(2) -0.035(2) -0.008(2) 0.0035(19) C6 0.060(2) 0.074(2) 0.081(2) -0.0308(19) -0.0187(19) 0.001(2) C7 0.050(2) 0.0553(17) 0.060(2) -0.0108(17) -0.0068(16) 0.0078(16) C2D 0.042(3) 0.045(4) 0.048(4) -0.002(3) 0.009(3) 0.001(3) C3D 0.045(3) 0.052(3) 0.053(3) -0.009(3) -0.002(2) 0.000(2) C4D 0.068(3) 0.055(3) 0.084(4) -0.027(3) -0.001(3) 0.012(3) C5D 0.075(4) 0.066(3) 0.095(4) -0.041(3) -0.006(3) -0.004(3) C6D 0.060(3) 0.078(3) 0.089(4) -0.031(3) -0.002(3) -0.003(3) C7D 0.048(3) 0.064(3) 0.062(4) -0.016(3) 0.003(3) -0.006(3) C8 0.0410(19) 0.0445(19) 0.059(2) -0.0130(17) -0.0048(17) 0.0030(16) C9 0.058(2) 0.0567(19) 0.0590(19) 0.0055(16) -0.0082(17) 0.0053(17) C10 0.072(3) 0.0633(18) 0.071(2) 0.0096(16) -0.0090(18) 0.004(2) C11 0.084(3) 0.057(2) 0.085(3) -0.0013(18) -0.009(2) 0.020(2) C12 0.076(2) 0.059(3) 0.088(3) 0.004(2) 0.009(2) 0.0286(18) C13 0.0533(17) 0.053(2) 0.080(3) -0.0023(17) 0.0056(18) 0.0143(16) C9D 0.044(3) 0.048(3) 0.057(3) -0.011(3) -0.012(3) -0.001(3) C8D 0.056(3) 0.055(3) 0.061(3) -0.007(3) -0.009(3) 0.010(3) C10D 0.071(4) 0.061(3) 0.072(3) -0.001(3) -0.009(3) 0.018(3) C11D 0.078(4) 0.057(3) 0.078(4) 0.001(3) -0.004(3) 0.024(3) C12D 0.078(3) 0.064(4) 0.091(4) -0.005(3) 0.002(3) 0.020(3) C13D 0.058(3) 0.059(3) 0.083(4) -0.012(3) -0.007(3) 0.020(3) C14 0.0446(8) 0.0382(7) 0.0373(7) -0.0030(6) 0.0040(6) -0.0032(6) C15 0.0830(12) 0.0503(10) 0.0479(9) 0.0047(7) -0.0016(8) -0.0148(9) C16 0.148(2) 0.0879(16) 0.0567(12) 0.0090(11) 0.0225(13) -0.0447(16) C17 0.0365(7) 0.0408(8) 0.0414(7) -0.0034(6) 0.0016(6) 0.0012(6) C18 0.0413(7) 0.0431(8) 0.0379(7) -0.0037(6) 0.0074(6) -0.0083(6) C19 0.0436(8) 0.0378(7) 0.0409(7) 0.0011(6) 0.0032(6) -0.0067(6) C20 0.0424(8) 0.0400(8) 0.0453(8) -0.0061(6) 0.0066(6) -0.0087(6) C21 0.0510(8) 0.0486(9) 0.0374(7) -0.0066(6) 0.0062(6) -0.0111(7) C22 0.0480(8) 0.0479(8) 0.0408(8) -0.0005(6) -0.0032(6) -0.0056(7) C23 0.0737(12) 0.0791(13) 0.0623(11) -0.0112(10) -0.0051(9) -0.0330(11) C24 0.0600(10) 0.0528(10) 0.0655(11) -0.0151(8) 0.0118(8) -0.0006(8) C25 0.0568(11) 0.0807(14) 0.0968(15) -0.0075(12) 0.0210(10) 0.0102(10) C26 0.1056(18) 0.0469(11) 0.146(2) 0.0095(13) 0.0398(16) 0.0183(12) O1 0.0371(5) 0.0453(6) 0.0393(5) -0.0058(4) 0.0016(4) -0.0034(4) O2 0.0436(6) 0.0613(7) 0.0604(7) -0.0090(6) -0.0008(5) 0.0125(5) O3 0.0496(6) 0.0503(6) 0.0494(6) -0.0058(5) 0.0039(5) -0.0178(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 O1 C1 C9D 111.3(6) . . ? O1 C1 C2D 110.5(4) . . ? C9D C1 C2D 116.4(7) . . ? O1 C1 C2 108.3(2) . . ? O1 C1 C8 109.3(3) . . ? C2 C1 C8 114.2(4) . . ? O1 C1 H1 108.3 . . ? C2 C1 H1 108.3 . . ? C8 C1 H1 108.3 . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 118.1(3) . . ? C7 C2 C1 121.4(3) . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C3D C2D C7D 120.0 . . ? C3D C2D C1 123.0(6) . . ? C7D C2D C1 116.9(6) . . ? C4D C3D C2D 120.0 . . ? C4D C3D H3D 120.0 . . ? C2D C3D H3D 120.0 . . ? C5D C4D C3D 120.0 . . ? C5D C4D H4D 120.0 . . ? C3D C4D H4D 120.0 . . ? C4D C5D C6D 120.0 . . ? C4D C5D H5D 120.0 . . ? C6D C5D H5D 120.0 . . ? C7D C6D C5D 120.0 . . ? C7D C6D H6D 120.0 . . ? C5D C6D H6D 120.0 . . ? C6D C7D C2D 120.0 . . ? C6D C7D H7D 120.0 . . ? C2D C7D H7D 120.0 . . ? C9 C8 C13 120.0 . . ? C9 C8 C1 118.3(3) . . ? C13 C8 C1 121.6(3) . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.0 . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C8D C9D C13D 120.0 . . ? C8D C9D C1 124.0(7) . . ? C13D C9D C1 116.0(7) . . ? C10D C8D C9D 120.0 . . ? C10D C8D H8D 120.0 . . ? C9D C8D H8D 120.0 . . ? C11D C10D C8D 120.0 . . ? C11D C10D H10D 120.0 . . ? C8D C10D H10D 120.0 . . ? C10D C11D C12D 120.0 . . ? C10D C11D H11D 120.0 . . ? C12D C11D H11D 120.0 . . ? C13D C12D C11D 120.0 . . ? C13D C12D H12D 120.0 . . ? C11D C12D H12D 120.0 . . ? C12D C13D C9D 120.0 . . ? C12D C13D H13D 120.0 . . ? C9D C13D H13D 120.0 . . ? O1 C14 C15 108.20(12) . . ? O1 C14 C17 107.89(11) . . ? C15 C14 C17 113.73(12) . . ? O1 C14 H14 109.0 . . ? C15 C14 H14 109.0 . . ? C17 C14 H14 109.0 . . ? C16 C15 C14 124.1(2) . . ? C16 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? C15 C16 H16A 120.0 . . ? C15 C16 H16B 120.0 . . ? H16A C16 H16B 120.0 . . ? O2 C17 C22 105.52(11) . . ? O2 C17 C18 110.91(12) . . ? C22 C17 C18 108.77(12) . . ? O2 C17 C14 109.14(11) . . ? C22 C17 C14 110.90(12) . . ? C18 C17 C14 111.45(11) . . ? C19 C18 C17 113.49(11) . . ? C19 C18 H18A 108.9 . . ? C17 C18 H18A 108.9 . . ? C19 C18 H18B 108.9 . . ? C17 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C18 C19 C20 112.52(12) . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? O3 C20 C19 102.84(11) . . ? O3 C20 C21 110.02(12) . . ? C19 C20 C21 109.29(11) . . ? O3 C20 C24 109.68(12) . . ? C19 C20 C24 113.26(13) . . ? C21 C20 C24 111.41(12) . . ? C22 C21 C20 113.12(12) . . ? C22 C21 H21A 109.0 . . ? C20 C21 H21A 109.0 . . ? C22 C21 H21B 109.0 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C17 113.02(12) . . ? C21 C22 H22A 109.0 . . ? C17 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C17 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? O3 C23 H23A 109.5 . . ? O3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 109.33(17) . . ? C25 C24 C20 114.30(14) . . ? C26 C24 C20 112.31(15) . . ? C25 C24 H24 106.8 . . ? C26 C24 H24 106.8 . . ? C20 C24 H24 106.8 . . ? 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 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C1 O1 C14 112.74(10) . . ? C17 O2 H2O 108.6(15) . . ? C23 O3 C20 118.27(12) . . ? 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 C1 O1 1.4308(16) . ? C1 C9D 1.445(7) . ? C1 C2D 1.504(8) . ? C1 C2 1.527(4) . ? C1 C8 1.558(4) . ? C1 H1 0.9800 . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C2D C3D 1.3900 . ? C2D C7D 1.3900 . ? C3D C4D 1.3900 . ? C3D H3D 0.9300 . ? C4D C5D 1.3900 . ? C4D H4D 0.9300 . ? C5D C6D 1.3900 . ? C5D H5D 0.9300 . ? C6D C7D 1.3900 . ? C6D H6D 0.9300 . ? C7D H7D 0.9300 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C9D C8D 1.3900 . ? C9D C13D 1.3900 . ? C8D C10D 1.3900 . ? C8D H8D 0.9300 . ? C10D C11D 1.3900 . ? C10D H10D 0.9300 . ? C11D C12D 1.3900 . ? C11D H11D 0.9300 . ? C12D C13D 1.3900 . ? C12D H12D 0.9300 . ? C13D H13D 0.9300 . ? C14 O1 1.4445(16) . ? C14 C15 1.498(2) . ? C14 C17 1.5343(19) . ? C14 H14 0.9800 . ? C15 C16 1.302(3) . ? C15 H15 0.9300 . ? C16 H16A 0.9300 . ? C16 H16B 0.9300 . ? C17 O2 1.4286(17) . ? C17 C22 1.5258(19) . ? C17 C18 1.526(2) . ? C18 C19 1.526(2) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.5287(19) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O3 1.4542(17) . ? C20 C21 1.529(2) . ? C20 C24 1.545(2) . ? C21 C22 1.520(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O3 1.4141(19) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.520(3) . ? C24 C26 1.525(3) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? O2 H2O 0.89(3) . ? 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 38.0(3) . . . . ? C8 C1 C2 C3 160.0(3) . . . . ? O1 C1 C2 C7 -150.2(3) . . . . ? C8 C1 C2 C7 -28.1(4) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 172.0(4) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C2 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 -171.7(4) . . . . ? O1 C1 C2D C3D 16.4(7) . . . . ? C9D C1 C2D C3D 144.6(7) . . . . ? O1 C1 C2D C7D -166.9(5) . . . . ? C9D C1 C2D C7D -38.7(8) . . . . ? C7D C2D C3D C4D 0.0 . . . . ? C1 C2D C3D C4D 176.7(7) . . . . ? C2D C3D C4D C5D 0.0 . . . . ? C3D C4D C5D C6D 0.0 . . . . ? C4D C5D C6D C7D 0.0 . . . . ? C5D C6D C7D C2D 0.0 . . . . ? C3D C2D C7D C6D 0.0 . . . . ? C1 C2D C7D C6D -176.9(7) . . . . ? O1 C1 C8 C9 53.7(4) . . . . ? C2 C1 C8 C9 -67.8(4) . . . . ? O1 C1 C8 C13 -122.6(3) . . . . ? C2 C1 C8 C13 115.9(4) . . . . ? C13 C8 C9 C10 0.0 . . . . ? C1 C8 C9 C10 -176.3(6) . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C8 0.0 . . . . ? C9 C8 C13 C12 0.0 . . . . ? C1 C8 C13 C12 176.2(6) . . . . ? O1 C1 C9D C8D 60.9(8) . . . . ? C2D C1 C9D C8D -66.9(9) . . . . ? O1 C1 C9D C13D -118.6(5) . . . . ? C2D C1 C9D C13D 113.6(7) . . . . ? C13D C9D C8D C10D 0.0 . . . . ? C1 C9D C8D C10D -179.5(12) . . . . ? C9D C8D C10D C11D 0.0 . . . . ? C8D C10D C11D C12D 0.0 . . . . ? C10D C11D C12D C13D 0.0 . . . . ? C11D C12D C13D C9D 0.0 . . . . ? C8D C9D C13D C12D 0.0 . . . . ? C1 C9D C13D C12D 179.5(11) . . . . ? O1 C14 C15 C16 -113.67(19) . . . . ? C17 C14 C15 C16 126.47(19) . . . . ? O1 C14 C17 O2 -63.69(14) . . . . ? C15 C14 C17 O2 56.34(16) . . . . ? O1 C14 C17 C22 -179.51(11) . . . . ? C15 C14 C17 C22 -59.48(16) . . . . ? O1 C14 C17 C18 59.15(14) . . . . ? C15 C14 C17 C18 179.18(13) . . . . ? O2 C17 C18 C19 -169.38(11) . . . . ? C22 C17 C18 C19 -53.77(15) . . . . ? C14 C17 C18 C19 68.79(14) . . . . ? C17 C18 C19 C20 55.40(15) . . . . ? C18 C19 C20 O3 64.05(14) . . . . ? C18 C19 C20 C21 -52.81(15) . . . . ? C18 C19 C20 C24 -177.66(12) . . . . ? O3 C20 C21 C22 -58.92(15) . . . . ? C19 C20 C21 C22 53.29(15) . . . . ? C24 C20 C21 C22 179.22(12) . . . . ? C20 C21 C22 C17 -55.68(16) . . . . ? O2 C17 C22 C21 172.70(12) . . . . ? C18 C17 C22 C21 53.65(16) . . . . ? C14 C17 C22 C21 -69.25(16) . . . . ? O3 C20 C24 C25 179.43(15) . . . . ? C19 C20 C24 C25 65.18(19) . . . . ? C21 C20 C24 C25 -58.51(19) . . . . ? O3 C20 C24 C26 54.13(19) . . . . ? C19 C20 C24 C26 -60.12(19) . . . . ? C21 C20 C24 C26 176.19(16) . . . . ? C9D C1 O1 C14 76.9(6) . . . . ? C2D C1 O1 C14 -152.2(4) . . . . ? C2 C1 O1 C14 -153.4(2) . . . . ? C8 C1 O1 C14 81.6(3) . . . . ? C15 C14 O1 C1 82.73(15) . . . . ? C17 C14 O1 C1 -153.82(11) . . . . ? C19 C20 O3 C23 -176.66(14) . . . . ? C21 C20 O3 C23 -60.33(18) . . . . ? C24 C20 O3 C23 62.56(18) . . . . ?