#------------------------------------------------------------------------------ #$Date: 2024-11-07 03:49:43 +0200 (Thu, 07 Nov 2024) $ #$Revision: 295814 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/02/7160206.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_7160206 loop_ _publ_author_name 'Sun, Honghao' 'Ding, Siyuan' 'Wang, Bo' 'Huang, Jiaxing' 'Guo, Hongchao' _publ_section_title ; Palladium-Catalyzed [3+2] Cycloaddition of 4-Vinyl-4-Butyro-lactones with Sulfamate-Derived Cyclic Imines: Construction of Sulfamate-Fused Pyrrolidines ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D4OB01611D _journal_year 2024 _chemical_formula_moiety 'C31 H26 O6' _chemical_formula_sum 'C31 H26 O6' _chemical_formula_weight 494.52 _chemical_name_systematic 1 _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 geom _audit_block_doi 10.5517/ccdc.csd.cc2k1px7 _audit_creation_date 2024-05-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-05-11 deposited with the CCDC. 2024-11-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.201(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.62090(10) _cell_length_b 14.4274(2) _cell_length_c 20.7278(3) _cell_measurement_reflns_used 14294 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 67.9590 _cell_measurement_theta_min 2.1750 _cell_volume 2577.50(6) _computing_cell_refinement 'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293 _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.954 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -35.00 -9.00 0.50 0.50 -- 42.30 -82.00 0.00 52 2 \w -41.00 13.00 0.50 0.50 -- 42.30 -77.00 90.00 108 3 \w 27.00 70.00 0.50 0.50 -- 42.30 -82.00 90.00 86 4 \w 25.00 70.00 0.50 0.50 -- 42.30 -82.00 0.00 90 5 \w 21.00 47.00 0.50 0.50 -- 42.30 -65.00 30.00 52 6 \w -46.00 72.00 0.50 0.50 -- 42.30 -54.00-180.00 236 7 \w 41.00 66.00 0.50 0.50 -- 42.30 -82.00-150.00 50 8 \w 36.00 68.00 0.50 0.50 -- 42.30 -82.00 150.00 64 9 \w 33.00 59.00 0.50 0.50 -- 42.30 -77.00 90.00 52 10 \w -46.00 23.00 0.50 0.50 -- 42.30 -77.00 -90.00 138 11 \w 21.00 132.00 0.50 0.50 -- 42.30 82.00 90.00 222 12 \w 28.00 53.00 0.50 0.50 -- 42.30 -82.00 60.00 50 13 \w -26.00 0.00 0.50 0.50 -- 42.30 -65.00 30.00 52 14 \w -37.00 16.00 0.50 0.50 -- 42.30 -82.00 60.00 106 15 \w 34.00 66.00 0.50 0.50 -- 42.30 -77.00 -90.00 64 16 \w 43.00 68.00 0.50 0.50 -- 42.30 -82.00 -90.00 50 17 \w 21.00 53.00 0.50 0.50 -- 42.30 65.00 30.00 64 18 \w -44.00 7.00 0.50 0.50 -- 42.30 -82.00-150.00 102 19 \w -47.00 8.00 0.50 0.50 -- 42.30 -82.00 150.00 110 20 \w 40.00 80.00 0.50 0.50 -- 42.30 82.00 -30.00 80 21 \w 59.00 113.00 0.50 0.50 -- 93.40 -82.00 30.00 108 22 \w 5.00 110.00 0.50 0.50 -- 93.40 -59.00-180.00 210 23 \w 4.00 182.00 0.50 0.50 -- 93.40 0.00 -90.00 356 24 \w 64.00 90.00 0.50 0.50 -- 93.40 -82.00-120.00 52 25 \w 40.00 128.00 0.50 0.50 -- 93.40 -33.00 0.00 176 26 \w 18.00 121.00 0.50 0.50 -- 93.40 -82.00-180.00 206 27 \w 16.00 127.00 0.50 0.50 -- 93.40 -33.00-150.00 222 28 \w 65.00 91.00 0.50 0.50 -- 93.40 -82.00 90.00 52 29 \w 88.00 113.00 0.50 0.50 -- 93.40 -59.00 0.00 50 30 \w 18.00 98.00 0.50 0.50 -- 93.40 -82.00 150.00 160 31 \w 5.00 56.00 0.50 0.50 -- 93.40 -59.00 0.00 102 32 \w 5.00 31.00 0.50 0.50 -- 93.40 -33.00 0.00 52 33 \w 28.00 121.00 0.50 0.50 -- 93.40 -82.00 -30.00 186 34 \w 67.00 106.00 0.50 0.50 -- 93.40 -82.00-150.00 78 35 \w 69.00 94.00 0.50 0.50 -- 93.40 -82.00 -90.00 50 36 \w 39.00 94.00 0.50 0.50 -- 93.40 -82.00 -60.00 110 37 \w 12.00 92.00 0.50 0.50 -- 93.40 -82.00 60.00 160 38 \w 84.00 125.00 0.50 0.50 -- 93.40 59.00 60.00 82 39 \w 133.00 158.00 0.50 0.50 -- 93.40 59.00 60.00 50 40 \w 143.00 168.00 0.50 0.50 -- 93.40 50.00 -60.00 50 41 \w 101.00 127.00 0.50 0.50 -- 93.40 50.00 -60.00 52 42 \w 11.00 90.00 0.50 0.50 -- 93.40 -82.00 120.00 158 43 \w 8.00 70.00 0.50 0.50 -- 93.40 -33.00-180.00 124 44 \w 86.00 112.00 0.50 0.50 -- 93.40 -82.00 0.00 52 45 \w 18.00 63.00 0.50 0.50 -- 93.40 -82.00 0.00 90 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Pro II AFC12 (RINC): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0664718000 _diffrn_orient_matrix_UB_12 -0.0824778000 _diffrn_orient_matrix_UB_13 0.0376841000 _diffrn_orient_matrix_UB_21 -0.0718237000 _diffrn_orient_matrix_UB_22 0.0676733000 _diffrn_orient_matrix_UB_23 0.0484652000 _diffrn_orient_matrix_UB_31 -0.1496503000 _diffrn_orient_matrix_UB_32 0.0041704000 _diffrn_orient_matrix_UB_33 -0.0418864000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_Laue_measured_fraction_full 0.978 _diffrn_reflns_Laue_measured_fraction_max 0.954 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 25388 _diffrn_reflns_point_group_measured_fraction_full 0.978 _diffrn_reflns_point_group_measured_fraction_max 0.954 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 69.146 _diffrn_reflns_theta_min 3.733 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.65421 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.274 _exptl_crystal_description block _exptl_crystal_F_000 1040 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.220 _refine_diff_density_min -0.154 _refine_diff_density_rms 0.031 _refine_ls_extinction_coef 0.0038(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 4596 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0375 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.3654P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.1095 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4058 _reflns_number_total 4596 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01611d2.cif _cod_data_source_block 1_auto _cod_database_code 7160206 _shelx_shelxl_version_number 2018/3 _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_max 0.965 _shelx_estimated_absorpt_t_min 0.958 _diffrn_oxdiff_digest_frames ; 01fa35ad3f076ad3b14c7ef03003436d14000307995 ; _diffrn_oxdiff_digest_hkl ; 0161d1e73bc882892ed61843a24e4330ad03b0 ; _reflns_odcompleteness_completeness 97.53 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C19(H19) 2.b Secondary CH2 refined with riding coordinates: C27(H27A,H27B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25) 2.d X=CH2 refined with riding coordinates: C9(H9A,H9B) 2.e Idealised Me refined as rotating group: C29(H29A,H29B,H29C), C31(H31A,H31B,H31C) ; _shelx_res_file ; TITL 1_auto_a.res in P2(1)/n 1_auto.res created by SHELXL-2018/3 at 21:58:08 on 07-May-2024 REM Old TITL 1_auto in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.171, Rweak 0.058, Alpha 0.023, Orientation as input REM Formula found by SHELXT: C30 C9 CELL 1.54184 8.6209 14.4274 20.7278 90 91.201 90 ZERR 4 0.0001 0.0002 0.0003 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 124 104 24 L.S. 40 PLAN 1 SIZE 0.06 0.05 0.06 TEMP 19.85 MORE -1 BOND $H CONF fmap 2 acta REM REM REM WGHT 0.059300 0.365400 EXTI 0.003804 FVAR 0.65825 O1 3 0.844977 0.198945 0.466828 11.00000 0.04158 0.05535 = 0.08326 0.01944 0.00577 0.01373 O2 3 0.460142 0.425423 0.423397 11.00000 0.04559 0.04242 = 0.08597 0.01427 0.00628 0.01067 O3 3 0.655864 0.004027 0.392987 11.00000 0.08750 0.05967 = 0.06646 0.00837 0.01775 0.03414 O4 3 0.487540 0.040020 0.313202 11.00000 0.08821 0.05660 = 0.04890 -0.01101 0.01127 0.00434 O5 3 0.217374 0.170287 0.362884 11.00000 0.05255 0.06142 = 0.06471 0.01301 -0.01169 -0.00178 O6 3 0.249617 0.040581 0.420935 11.00000 0.05018 0.04338 = 0.06619 0.00393 0.00474 -0.00577 C1 1 0.594808 0.253660 0.564768 11.00000 0.03303 0.04240 = 0.04245 0.00205 0.00281 0.00246 C2 1 0.607827 0.344860 0.585825 11.00000 0.04720 0.04405 = 0.04778 0.00216 0.00436 0.00013 AFIX 43 H2 2 0.571828 0.392576 0.559321 11.00000 -1.20000 AFIX 0 C3 1 0.673398 0.365849 0.645514 11.00000 0.05332 0.05481 = 0.05356 -0.00753 0.00381 -0.00682 AFIX 43 H3 2 0.680750 0.427307 0.658762 11.00000 -1.20000 AFIX 0 C4 1 0.727695 0.296522 0.685323 11.00000 0.05859 0.07489 = 0.05207 -0.00696 -0.01104 -0.00306 AFIX 43 H4 2 0.771670 0.310434 0.725518 11.00000 -1.20000 AFIX 0 C5 1 0.715927 0.206131 0.664731 11.00000 0.07646 0.06415 = 0.05999 0.00755 -0.02189 0.00888 AFIX 43 H5 2 0.753324 0.158756 0.691209 11.00000 -1.20000 AFIX 0 C6 1 0.649476 0.184477 0.605359 11.00000 0.05951 0.04582 = 0.05448 0.00283 -0.01190 0.00523 AFIX 43 H6 2 0.641490 0.122823 0.592622 11.00000 -1.20000 AFIX 0 C7 1 0.513376 0.232784 0.500074 11.00000 0.03505 0.03552 = 0.04006 0.00382 0.00201 0.00408 C8 1 0.345629 0.265438 0.506040 11.00000 0.03701 0.04338 = 0.04528 0.00301 0.00205 0.00637 AFIX 43 H8 2 0.320895 0.323858 0.489891 11.00000 -1.20000 AFIX 0 C9 1 0.234415 0.217857 0.531987 11.00000 0.04265 0.05809 = 0.05451 0.00470 0.00886 0.00429 AFIX 93 H9A 2 0.254514 0.159140 0.548682 11.00000 -1.20000 H9B 2 0.135021 0.242649 0.533793 11.00000 -1.20000 AFIX 0 C10 1 0.598211 0.278962 0.442176 11.00000 0.03561 0.03644 = 0.04299 0.00465 0.00359 0.00502 C11 1 0.581213 0.384094 0.430428 11.00000 0.04174 0.03778 = 0.04573 0.00475 0.00508 0.00491 C12 1 0.737395 0.424711 0.424305 11.00000 0.04545 0.04341 = 0.04485 0.00223 0.00694 -0.00192 C13 1 0.779532 0.515481 0.409319 11.00000 0.06254 0.04337 = 0.06496 0.00312 0.01277 -0.00415 AFIX 43 H13 2 0.705087 0.561303 0.402539 11.00000 -1.20000 AFIX 0 C14 1 0.935035 0.534613 0.404959 11.00000 0.07034 0.05711 = 0.07728 0.00414 0.01388 -0.02165 AFIX 43 H14 2 0.966291 0.594841 0.395914 11.00000 -1.20000 AFIX 0 C15 1 1.046649 0.466137 0.413738 11.00000 0.05089 0.08047 = 0.07386 0.01175 0.00541 -0.01936 AFIX 43 H15 2 1.151002 0.481369 0.410429 11.00000 -1.20000 AFIX 0 C16 1 1.005741 0.376344 0.427216 11.00000 0.04052 0.07283 = 0.06359 0.01283 0.00163 -0.00389 AFIX 43 H16 2 1.080395 0.330189 0.432032 11.00000 -1.20000 AFIX 0 C17 1 0.848951 0.356820 0.433410 11.00000 0.03981 0.05182 = 0.04444 0.00565 0.00203 -0.00073 C18 1 0.775933 0.267660 0.449371 11.00000 0.03638 0.04683 = 0.04680 0.00569 0.00513 0.00640 C19 1 0.526770 0.228367 0.381900 11.00000 0.03940 0.03783 = 0.04216 0.00535 0.00265 0.00496 AFIX 13 H19 2 0.430530 0.261775 0.371408 11.00000 -1.20000 AFIX 0 C20 1 0.621985 0.232942 0.321324 11.00000 0.04996 0.04550 = 0.04211 0.00423 0.00456 -0.00496 C21 1 0.763881 0.188295 0.314749 11.00000 0.06169 0.07011 = 0.05650 0.01011 0.01930 0.01024 AFIX 43 H21 2 0.805475 0.154734 0.349291 11.00000 -1.20000 AFIX 0 C22 1 0.843817 0.192930 0.257989 11.00000 0.07193 0.08953 = 0.06919 0.00038 0.02962 -0.00140 AFIX 43 H22 2 0.938698 0.162786 0.254783 11.00000 -1.20000 AFIX 0 C23 1 0.785417 0.241130 0.206593 11.00000 0.08549 0.10307 = 0.05380 0.00116 0.02496 -0.02024 AFIX 43 H23 2 0.838768 0.242973 0.168080 11.00000 -1.20000 AFIX 0 C24 1 0.647914 0.286688 0.212135 11.00000 0.09524 0.10870 = 0.04516 0.02249 0.00084 -0.01479 AFIX 43 H24 2 0.608177 0.320531 0.177362 11.00000 -1.20000 AFIX 0 C25 1 0.566254 0.283086 0.269351 11.00000 0.06102 0.07241 = 0.04725 0.01248 -0.00428 -0.00735 AFIX 43 H25 2 0.472939 0.314956 0.272464 11.00000 -1.20000 AFIX 0 C26 1 0.474160 0.130713 0.406956 11.00000 0.04339 0.03554 = 0.04034 0.00269 0.00494 0.00392 C27 1 0.517295 0.130314 0.479265 11.00000 0.04162 0.03547 = 0.04153 0.00499 0.00293 0.00386 AFIX 23 H27A 2 0.619951 0.104302 0.486487 11.00000 -1.20000 H27B 2 0.443120 0.094202 0.503253 11.00000 -1.20000 AFIX 0 C28 1 0.551948 0.050494 0.371866 11.00000 0.06260 0.04060 = 0.04776 0.00412 0.01433 0.00610 C29 1 0.558865 -0.027228 0.271416 11.00000 0.14844 0.08044 = 0.07117 -0.02718 0.03519 0.01030 AFIX 137 H29A 2 0.494492 -0.036127 0.233569 11.00000 -1.50000 H29B 2 0.570472 -0.085054 0.293916 11.00000 -1.50000 H29C 2 0.658972 -0.005137 0.259027 11.00000 -1.50000 AFIX 0 C30 1 0.299066 0.118916 0.393777 11.00000 0.04952 0.04096 = 0.04192 -0.00177 0.00230 -0.00034 C31 1 0.086197 0.019770 0.412018 11.00000 0.05431 0.06673 = 0.10228 0.00160 0.00666 -0.01540 AFIX 137 H31A 2 0.061573 0.015257 0.366745 11.00000 -1.50000 H31B 2 0.025605 0.068279 0.430731 11.00000 -1.50000 H31C 2 0.063108 -0.038020 0.432671 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1_auto_a.res in P2(1)/n REM wR2 = 0.1095, GooF = S = 1.059, Restrained GooF = 1.059 for all data REM R1 = 0.0375 for 4058 Fo > 4sig(Fo) and 0.0415 for all 4596 data REM 337 parameters refined using 0 restraints END WGHT 0.0593 0.3654 REM Highest difference peak 0.220, deepest hole -0.154, 1-sigma level 0.031 Q1 1 0.5613 0.2640 0.4720 11.00000 0.05 0.22 ; _shelx_res_checksum 2799 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.735 _oxdiff_exptl_absorpt_empirical_full_min 0.628 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 O1 O 0.84498(11) 0.19895(7) 0.46683(6) 0.0600(3) Uani 1 1 d . . . . . O2 O 0.46014(11) 0.42542(7) 0.42340(5) 0.0579(3) Uani 1 1 d . . . . . O3 O 0.65586(14) 0.00403(8) 0.39299(5) 0.0710(3) Uani 1 1 d . . . . . O4 O 0.48754(14) 0.04002(7) 0.31320(5) 0.0644(3) Uani 1 1 d . . . . . O5 O 0.21737(11) 0.17029(7) 0.36288(5) 0.0597(3) Uani 1 1 d . . . . . O6 O 0.24962(11) 0.04058(6) 0.42094(5) 0.0532(3) Uani 1 1 d . . . . . C1 C 0.59481(13) 0.25366(8) 0.56477(6) 0.0393(3) Uani 1 1 d . . . . . C2 C 0.60783(15) 0.34486(9) 0.58583(6) 0.0463(3) Uani 1 1 d . . . . . H2 H 0.571828 0.392576 0.559321 0.056 Uiso 1 1 calc R . . . . C3 C 0.67340(16) 0.36585(10) 0.64551(7) 0.0539(4) Uani 1 1 d . . . . . H3 H 0.680750 0.427307 0.658762 0.065 Uiso 1 1 calc R . . . . C4 C 0.72769(18) 0.29652(12) 0.68532(8) 0.0620(4) Uani 1 1 d . . . . . H4 H 0.771670 0.310434 0.725518 0.074 Uiso 1 1 calc R . . . . C5 C 0.7159(2) 0.20613(12) 0.66473(8) 0.0672(4) Uani 1 1 d . . . . . H5 H 0.753324 0.158756 0.691209 0.081 Uiso 1 1 calc R . . . . C6 C 0.64948(17) 0.18448(10) 0.60536(7) 0.0535(3) Uani 1 1 d . . . . . H6 H 0.641490 0.122823 0.592622 0.064 Uiso 1 1 calc R . . . . C7 C 0.51338(13) 0.23278(8) 0.50007(6) 0.0369(3) Uani 1 1 d . . . . . C8 C 0.34563(14) 0.26544(9) 0.50604(6) 0.0419(3) Uani 1 1 d . . . . . H8 H 0.320895 0.323858 0.489891 0.050 Uiso 1 1 calc R . . . . C9 C 0.23441(16) 0.21786(10) 0.53199(7) 0.0516(3) Uani 1 1 d . . . . . H9A H 0.254514 0.159140 0.548682 0.062 Uiso 1 1 calc R . . . . H9B H 0.135021 0.242649 0.533793 0.062 Uiso 1 1 calc R . . . . C10 C 0.59821(13) 0.27896(8) 0.44218(6) 0.0383(3) Uani 1 1 d . . . . . C11 C 0.58121(14) 0.38409(8) 0.43043(6) 0.0417(3) Uani 1 1 d . . . . . C12 C 0.73740(15) 0.42471(9) 0.42430(6) 0.0445(3) Uani 1 1 d . . . . . C13 C 0.77953(18) 0.51548(10) 0.40932(8) 0.0568(4) Uani 1 1 d . . . . . H13 H 0.705087 0.561303 0.402539 0.068 Uiso 1 1 calc R . . . . C14 C 0.9350(2) 0.53461(12) 0.40496(9) 0.0681(4) Uani 1 1 d . . . . . H14 H 0.966291 0.594841 0.395914 0.082 Uiso 1 1 calc R . . . . C15 C 1.04665(19) 0.46614(13) 0.41374(9) 0.0684(5) Uani 1 1 d . . . . . H15 H 1.151002 0.481369 0.410429 0.082 Uiso 1 1 calc R . . . . C16 C 1.00574(16) 0.37634(12) 0.42722(8) 0.0590(4) Uani 1 1 d . . . . . H16 H 1.080395 0.330189 0.432032 0.071 Uiso 1 1 calc R . . . . C17 C 0.84895(14) 0.35682(9) 0.43341(6) 0.0453(3) Uani 1 1 d . . . . . C18 C 0.77593(14) 0.26766(9) 0.44937(6) 0.0433(3) Uani 1 1 d . . . . . C19 C 0.52677(14) 0.22837(8) 0.38190(6) 0.0398(3) Uani 1 1 d . . . . . H19 H 0.430530 0.261775 0.371408 0.048 Uiso 1 1 calc R . . . . C20 C 0.62199(16) 0.23294(9) 0.32132(6) 0.0458(3) Uani 1 1 d . . . . . C21 C 0.76388(18) 0.18830(12) 0.31475(8) 0.0625(4) Uani 1 1 d . . . . . H21 H 0.805475 0.154734 0.349291 0.075 Uiso 1 1 calc R . . . . C22 C 0.8438(2) 0.19293(15) 0.25799(9) 0.0765(5) Uani 1 1 d . . . . . H22 H 0.938698 0.162786 0.254783 0.092 Uiso 1 1 calc R . . . . C23 C 0.7854(2) 0.24113(15) 0.20659(9) 0.0805(6) Uani 1 1 d . . . . . H23 H 0.838768 0.242973 0.168080 0.097 Uiso 1 1 calc R . . . . C24 C 0.6479(3) 0.28669(15) 0.21213(8) 0.0830(6) Uani 1 1 d . . . . . H24 H 0.608177 0.320531 0.177362 0.100 Uiso 1 1 calc R . . . . C25 C 0.56625(19) 0.28309(12) 0.26935(7) 0.0603(4) Uani 1 1 d . . . . . H25 H 0.472939 0.314956 0.272464 0.072 Uiso 1 1 calc R . . . . C26 C 0.47416(14) 0.13071(8) 0.40696(6) 0.0397(3) Uani 1 1 d . . . . . C27 C 0.51729(14) 0.13031(8) 0.47926(6) 0.0395(3) Uani 1 1 d . . . . . H27A H 0.619951 0.104302 0.486487 0.047 Uiso 1 1 calc R . . . . H27B H 0.443120 0.094202 0.503253 0.047 Uiso 1 1 calc R . . . . C28 C 0.55195(17) 0.05049(9) 0.37187(7) 0.0501(3) Uani 1 1 d . . . . . C29 C 0.5589(3) -0.02723(15) 0.27142(10) 0.0996(7) Uani 1 1 d . . . . . H29A H 0.494492 -0.036127 0.233569 0.149 Uiso 1 1 calc GR . . . . H29B H 0.570472 -0.085054 0.293916 0.149 Uiso 1 1 calc GR . . . . H29C H 0.658972 -0.005137 0.259027 0.149 Uiso 1 1 calc GR . . . . C30 C 0.29907(15) 0.11892(9) 0.39378(6) 0.0441(3) Uani 1 1 d . . . . . C31 C 0.08620(19) 0.01977(13) 0.41202(10) 0.0744(5) Uani 1 1 d . . . . . H31A H 0.061573 0.015257 0.366745 0.112 Uiso 1 1 calc GR . . . . H31B H 0.025605 0.068279 0.430731 0.112 Uiso 1 1 calc GR . . . . H31C H 0.063108 -0.038020 0.432671 0.112 Uiso 1 1 calc GR . . . . 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 0.0416(5) 0.0554(6) 0.0833(7) 0.0194(5) 0.0058(5) 0.0137(4) O2 0.0456(5) 0.0424(5) 0.0860(7) 0.0143(5) 0.0063(5) 0.0107(4) O3 0.0875(8) 0.0597(6) 0.0665(7) 0.0084(5) 0.0178(6) 0.0341(6) O4 0.0882(8) 0.0566(6) 0.0489(6) -0.0110(4) 0.0113(5) 0.0043(5) O5 0.0526(6) 0.0614(6) 0.0647(6) 0.0130(5) -0.0117(5) -0.0018(5) O6 0.0502(5) 0.0434(5) 0.0662(6) 0.0039(4) 0.0047(5) -0.0058(4) C1 0.0330(6) 0.0424(6) 0.0424(6) 0.0020(5) 0.0028(5) 0.0025(5) C2 0.0472(7) 0.0440(7) 0.0478(7) 0.0022(6) 0.0044(6) 0.0001(5) C3 0.0533(8) 0.0548(8) 0.0536(8) -0.0075(6) 0.0038(6) -0.0068(6) C4 0.0586(9) 0.0749(10) 0.0521(8) -0.0070(7) -0.0110(7) -0.0031(7) C5 0.0765(11) 0.0641(10) 0.0600(9) 0.0075(7) -0.0219(8) 0.0089(8) C6 0.0595(8) 0.0458(7) 0.0545(8) 0.0028(6) -0.0119(7) 0.0052(6) C7 0.0350(6) 0.0355(6) 0.0401(6) 0.0038(5) 0.0020(5) 0.0041(5) C8 0.0370(6) 0.0434(7) 0.0453(7) 0.0030(5) 0.0020(5) 0.0064(5) C9 0.0426(7) 0.0581(8) 0.0545(8) 0.0047(6) 0.0089(6) 0.0043(6) C10 0.0356(6) 0.0364(6) 0.0430(6) 0.0047(5) 0.0036(5) 0.0050(5) C11 0.0417(6) 0.0378(6) 0.0457(7) 0.0047(5) 0.0051(5) 0.0049(5) C12 0.0455(7) 0.0434(7) 0.0448(7) 0.0022(5) 0.0069(6) -0.0019(5) C13 0.0625(9) 0.0434(7) 0.0650(9) 0.0031(6) 0.0128(7) -0.0042(6) C14 0.0703(10) 0.0571(9) 0.0773(11) 0.0041(8) 0.0139(8) -0.0216(8) C15 0.0509(8) 0.0805(12) 0.0739(11) 0.0117(9) 0.0054(8) -0.0194(8) C16 0.0405(7) 0.0728(10) 0.0636(9) 0.0128(7) 0.0016(7) -0.0039(7) C17 0.0398(7) 0.0518(7) 0.0444(7) 0.0056(6) 0.0020(5) -0.0007(5) C18 0.0364(6) 0.0468(7) 0.0468(7) 0.0057(5) 0.0051(5) 0.0064(5) C19 0.0394(6) 0.0378(6) 0.0422(6) 0.0054(5) 0.0027(5) 0.0050(5) C20 0.0500(7) 0.0455(7) 0.0421(7) 0.0042(5) 0.0046(6) -0.0050(6) C21 0.0617(9) 0.0701(10) 0.0565(9) 0.0101(7) 0.0193(7) 0.0102(7) C22 0.0719(11) 0.0895(13) 0.0692(11) 0.0004(9) 0.0296(9) -0.0014(9) C23 0.0855(13) 0.1031(15) 0.0538(10) 0.0012(9) 0.0250(9) -0.0202(11) C24 0.0952(14) 0.1087(16) 0.0452(9) 0.0225(9) 0.0008(9) -0.0148(12) C25 0.0610(9) 0.0724(10) 0.0472(8) 0.0125(7) -0.0043(7) -0.0073(7) C26 0.0434(6) 0.0355(6) 0.0403(6) 0.0027(5) 0.0049(5) 0.0039(5) C27 0.0416(6) 0.0355(6) 0.0415(6) 0.0050(5) 0.0029(5) 0.0039(5) C28 0.0626(8) 0.0406(7) 0.0478(7) 0.0041(6) 0.0143(6) 0.0061(6) C29 0.148(2) 0.0804(13) 0.0712(12) -0.0272(10) 0.0352(13) 0.0103(13) C30 0.0495(7) 0.0410(7) 0.0419(7) -0.0018(5) 0.0023(6) -0.0003(6) C31 0.0543(9) 0.0667(11) 0.1023(14) 0.0016(9) 0.0067(9) -0.0154(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _citation_id _citation_doi _citation_year 1 10.1021/acs.joc.4c01532 2024 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 C28 O4 C29 116.59(15) . . ? C30 O6 C31 116.07(12) . . ? C2 C1 C7 119.60(11) . . ? C6 C1 C2 117.92(12) . . ? C6 C1 C7 122.39(11) . . ? C1 C2 H2 119.4 . . ? C3 C2 C1 121.13(12) . . ? C3 C2 H2 119.4 . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.40(14) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 120.6 . . ? C3 C4 C5 118.84(14) . . ? C5 C4 H4 120.6 . . ? C4 C5 H5 119.4 . . ? C4 C5 C6 121.14(14) . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 120.56(14) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C1 C7 C10 111.99(9) . . ? C1 C7 C27 114.95(9) . . ? C8 C7 C1 106.61(9) . . ? C8 C7 C10 112.86(9) . . ? C8 C7 C27 110.17(10) . . ? C27 C7 C10 100.38(9) . . ? C7 C8 H8 117.4 . . ? C9 C8 C7 125.17(12) . . ? C9 C8 H8 117.4 . . ? C8 C9 H9A 120.0 . . ? C8 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? C11 C10 C7 119.64(10) . . ? C11 C10 C18 102.11(9) . . ? C11 C10 C19 107.37(9) . . ? C18 C10 C7 111.04(9) . . ? C18 C10 C19 113.67(10) . . ? C19 C10 C7 103.37(9) . . ? O2 C11 C10 125.68(11) . . ? O2 C11 C12 125.51(11) . . ? C12 C11 C10 108.67(10) . . ? C13 C12 C11 129.32(12) . . ? C17 C12 C11 109.88(11) . . ? C17 C12 C13 120.76(12) . . ? C12 C13 H13 121.2 . . ? C14 C13 C12 117.52(14) . . ? C14 C13 H13 121.2 . . ? C13 C14 H14 119.2 . . ? C13 C14 C15 121.54(15) . . ? C15 C14 H14 119.2 . . ? C14 C15 H15 119.4 . . ? C16 C15 C14 121.19(14) . . ? C16 C15 H15 119.4 . . ? C15 C16 H16 121.2 . . ? C15 C16 C17 117.69(15) . . ? C17 C16 H16 121.2 . . ? C12 C17 C16 121.26(13) . . ? C12 C17 C18 110.49(11) . . ? C16 C17 C18 128.25(12) . . ? O1 C18 C10 126.66(12) . . ? O1 C18 C17 125.02(11) . . ? C17 C18 C10 108.29(10) . . ? C10 C19 H19 105.4 . . ? C10 C19 C26 105.44(9) . . ? C20 C19 C10 115.52(10) . . ? C20 C19 H19 105.4 . . ? C20 C19 C26 118.54(10) . . ? C26 C19 H19 105.4 . . ? C21 C20 C19 123.59(12) . . ? C25 C20 C19 119.02(12) . . ? C25 C20 C21 117.38(13) . . ? C20 C21 H21 119.4 . . ? C22 C21 C20 121.17(16) . . ? C22 C21 H21 119.4 . . ? C21 C22 H22 119.7 . . ? C23 C22 C21 120.68(18) . . ? C23 C22 H22 119.7 . . ? C22 C23 H23 120.4 . . ? C22 C23 C24 119.28(16) . . ? C24 C23 H23 120.4 . . ? C23 C24 H24 119.7 . . ? C23 C24 C25 120.66(17) . . ? C25 C24 H24 119.7 . . ? C20 C25 C24 120.79(16) . . ? C20 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C27 C26 C19 105.07(9) . . ? C27 C26 C30 112.92(10) . . ? C28 C26 C19 112.88(10) . . ? C28 C26 C27 111.19(10) . . ? C28 C26 C30 105.68(10) . . ? C30 C26 C19 109.24(10) . . ? C7 C27 H27A 110.7 . . ? C7 C27 H27B 110.7 . . ? C26 C27 C7 105.26(9) . . ? C26 C27 H27A 110.7 . . ? C26 C27 H27B 110.7 . . ? H27A C27 H27B 108.8 . . ? O3 C28 O4 124.39(13) . . ? O3 C28 C26 125.68(13) . . ? O4 C28 C26 109.92(11) . . ? O4 C29 H29A 109.5 . . ? O4 C29 H29B 109.5 . . ? O4 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O5 C30 O6 123.98(12) . . ? O5 C30 C26 126.16(12) . . ? O6 C30 C26 109.84(10) . . ? O6 C31 H31A 109.5 . . ? O6 C31 H31B 109.5 . . ? O6 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 C18 1.2079(15) . ? O2 C11 1.2082(14) . ? O3 C28 1.1947(17) . ? O4 C28 1.3347(18) . ? O4 C29 1.446(2) . ? O5 C30 1.1985(16) . ? O6 C30 1.3364(16) . ? O6 C31 1.4485(18) . ? C1 C2 1.3901(18) . ? C1 C6 1.3819(18) . ? C1 C7 1.5305(17) . ? C2 H2 0.9300 . ? C2 C3 1.3830(19) . ? C3 H3 0.9300 . ? C3 C4 1.373(2) . ? C4 H4 0.9300 . ? C4 C5 1.375(2) . ? C5 H5 0.9300 . ? C5 C6 1.382(2) . ? C6 H6 0.9300 . ? C7 C8 1.5284(16) . ? C7 C10 1.5671(16) . ? C7 C27 1.5406(16) . ? C8 H8 0.9300 . ? C8 C9 1.3044(19) . ? C9 H9A 0.9300 . ? C9 H9B 0.9300 . ? C10 C11 1.5427(16) . ? C10 C18 1.5449(16) . ? C10 C19 1.5623(17) . ? C11 C12 1.4763(17) . ? C12 C13 1.3958(19) . ? C12 C17 1.3829(18) . ? C13 H13 0.9300 . ? C13 C14 1.374(2) . ? C14 H14 0.9300 . ? C14 C15 1.388(3) . ? C15 H15 0.9300 . ? C15 C16 1.373(2) . ? C16 H16 0.9300 . ? C16 C17 1.3893(18) . ? C17 C18 1.4728(18) . ? C19 H19 0.9800 . ? C19 C20 1.5159(18) . ? C19 C26 1.5717(16) . ? C20 C21 1.392(2) . ? C20 C25 1.3759(19) . ? C21 H21 0.9300 . ? C21 C22 1.378(2) . ? C22 H22 0.9300 . ? C22 C23 1.360(3) . ? C23 H23 0.9300 . ? C23 C24 1.362(3) . ? C24 H24 0.9300 . ? C24 C25 1.393(2) . ? C25 H25 0.9300 . ? C26 C27 1.5367(16) . ? C26 C28 1.5293(18) . ? C26 C30 1.5378(18) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 O2 C11 C12 C13 -0.5(2) . . . . ? O2 C11 C12 C17 -178.05(13) . . . . ? C1 C2 C3 C4 0.2(2) . . . . ? C1 C7 C8 C9 -83.05(16) . . . . ? C1 C7 C10 C11 -75.62(13) . . . . ? C1 C7 C10 C18 42.89(13) . . . . ? C1 C7 C10 C19 165.14(9) . . . . ? C1 C7 C27 C26 -163.81(9) . . . . ? C2 C1 C6 C5 -0.5(2) . . . . ? C2 C1 C7 C8 -62.24(14) . . . . ? C2 C1 C7 C10 61.65(14) . . . . ? C2 C1 C7 C27 175.37(11) . . . . ? C2 C3 C4 C5 0.1(2) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C4 C5 C6 C1 0.8(3) . . . . ? C6 C1 C2 C3 0.00(19) . . . . ? C6 C1 C7 C8 114.18(13) . . . . ? C6 C1 C7 C10 -121.93(13) . . . . ? C6 C1 C7 C27 -8.21(17) . . . . ? C7 C1 C2 C3 176.58(11) . . . . ? C7 C1 C6 C5 -176.98(14) . . . . ? C7 C10 C11 O2 -55.28(18) . . . . ? C7 C10 C11 C12 128.93(11) . . . . ? C7 C10 C18 O1 41.85(18) . . . . ? C7 C10 C18 C17 -136.16(11) . . . . ? C7 C10 C19 C20 -159.56(10) . . . . ? C7 C10 C19 C26 -26.63(11) . . . . ? C8 C7 C10 C11 44.69(15) . . . . ? C8 C7 C10 C18 163.21(10) . . . . ? C8 C7 C10 C19 -74.54(12) . . . . ? C8 C7 C27 C26 75.74(12) . . . . ? C10 C7 C8 C9 153.59(13) . . . . ? C10 C7 C27 C26 -43.47(11) . . . . ? C10 C11 C12 C13 175.34(14) . . . . ? C10 C11 C12 C17 -2.25(14) . . . . ? C10 C19 C20 C21 68.43(17) . . . . ? C10 C19 C20 C25 -112.09(14) . . . . ? C10 C19 C26 C27 0.06(11) . . . . ? C10 C19 C26 C28 -121.27(11) . . . . ? C10 C19 C26 C30 121.47(10) . . . . ? C11 C10 C18 O1 170.49(14) . . . . ? C11 C10 C18 C17 -7.52(13) . . . . ? C11 C10 C19 C20 73.06(12) . . . . ? C11 C10 C19 C26 -154.01(9) . . . . ? C11 C12 C13 C14 -178.27(14) . . . . ? C11 C12 C17 C16 177.06(13) . . . . ? C11 C12 C17 C18 -2.82(15) . . . . ? C12 C13 C14 C15 1.3(3) . . . . ? C12 C17 C18 O1 -171.29(13) . . . . ? C12 C17 C18 C10 6.76(15) . . . . ? C13 C12 C17 C16 -0.8(2) . . . . ? C13 C12 C17 C18 179.35(13) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C17 -1.6(3) . . . . ? C15 C16 C17 C12 2.0(2) . . . . ? C15 C16 C17 C18 -178.13(14) . . . . ? C16 C17 C18 O1 8.9(2) . . . . ? C16 C17 C18 C10 -173.10(13) . . . . ? C17 C12 C13 C14 -0.9(2) . . . . ? C18 C10 C11 O2 -178.28(13) . . . . ? C18 C10 C11 C12 5.94(13) . . . . ? C18 C10 C19 C20 -39.09(14) . . . . ? C18 C10 C19 C26 93.84(11) . . . . ? C19 C10 C11 O2 61.90(16) . . . . ? C19 C10 C11 C12 -113.88(11) . . . . ? C19 C10 C18 O1 -74.20(17) . . . . ? C19 C10 C18 C17 107.79(12) . . . . ? C19 C20 C21 C22 178.39(15) . . . . ? C19 C20 C25 C24 -178.03(15) . . . . ? C19 C26 C27 C7 27.28(11) . . . . ? C19 C26 C28 O3 103.76(16) . . . . ? C19 C26 C28 O4 -75.65(14) . . . . ? C19 C26 C30 O5 7.97(18) . . . . ? C19 C26 C30 O6 -173.41(10) . . . . ? C20 C19 C26 C27 131.28(11) . . . . ? C20 C19 C26 C28 9.95(15) . . . . ? C20 C19 C26 C30 -107.31(12) . . . . ? C20 C21 C22 C23 -0.3(3) . . . . ? C21 C20 C25 C24 1.5(2) . . . . ? C21 C22 C23 C24 1.4(3) . . . . ? C22 C23 C24 C25 -1.0(3) . . . . ? C23 C24 C25 C20 -0.5(3) . . . . ? C25 C20 C21 C22 -1.1(2) . . . . ? C26 C19 C20 C21 -58.11(18) . . . . ? C26 C19 C20 C25 121.36(14) . . . . ? C27 C7 C8 C9 42.29(17) . . . . ? C27 C7 C10 C11 161.93(10) . . . . ? C27 C7 C10 C18 -79.55(11) . . . . ? C27 C7 C10 C19 42.69(10) . . . . ? C27 C26 C28 O3 -14.04(19) . . . . ? C27 C26 C28 O4 166.55(11) . . . . ? C27 C26 C30 O5 124.49(14) . . . . ? C27 C26 C30 O6 -56.88(13) . . . . ? C28 C26 C27 C7 149.71(10) . . . . ? C28 C26 C30 O5 -113.75(14) . . . . ? C28 C26 C30 O6 64.88(13) . . . . ? C29 O4 C28 O3 -5.4(2) . . . . ? C29 O4 C28 C26 174.01(14) . . . . ? C30 C26 C27 C7 -91.69(12) . . . . ? C30 C26 C28 O3 -136.91(15) . . . . ? C30 C26 C28 O4 43.68(14) . . . . ? C31 O6 C30 O5 -0.8(2) . . . . ? C31 O6 C30 C26 -179.50(12) . . . . ?