#------------------------------------------------------------------------------ #$Date: 2020-11-25 07:11:19 +0200 (Wed, 25 Nov 2020) $ #$Revision: 259242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022281.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022281 loop_ _publ_author_name 'Rutherford, Ryan Noboru' 'Ura, Shinji' 'Chan, Tak-Hang' 'Fukumoto, Kozo' 'Nishioka, Takanori' 'Renzetti, Andrea' _publ_section_title ; Dibenzoate esters of cis-tetralin-2,3-diol as analogs of (--)-epigallocatechin gallate: synthesis and crystal structure of anticancer drug candidates ; _journal_coeditor_code OP3007 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229620014916 _journal_volume 76 _journal_year 2020 _chemical_formula_iupac 'C26 H24 O6' _chemical_formula_moiety 'C26 H24 O6' _chemical_formula_sum 'C26 H24 O6' _chemical_formula_weight 432.45 _chemical_name_systematic ; (2R,3S)-1,2,3,4-Tetrahydronaphthalene-2,3-diyl bis(4-methoxybenzoate) ; _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 _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3 (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032) ; _cell_angle_alpha 90 _cell_angle_beta 91.948(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.033(3) _cell_length_b 6.427(2) _cell_length_c 37.080(14) _cell_measurement_reflns_used 4943 _cell_measurement_temperature 193.4 _cell_measurement_theta_max 27.4816 _cell_measurement_theta_min 3.1699 _cell_volume 2151.4(13) _computing_cell_refinement ; CrystalClear (Rigaku, 2008) ; _computing_data_collection ; CrystalClear (Rigaku, 2008) ; _computing_data_reduction ; CrystalClear (Rigaku, 2008) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 193.4 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0702 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_number 20997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.541 _diffrn_reflns_theta_min 3.355 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2008)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.335 _exptl_crystal_description prism _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.237 _exptl_crystal_size_mid 0.144 _exptl_crystal_size_min 0.103 _refine_diff_density_max 0.197 _refine_diff_density_min -0.197 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 291 _refine_ls_number_reflns 4916 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0425 _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^)+(0.0577P)^2^+0.2076P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1099 _refine_ls_wR_factor_ref 0.1159 _reflns_number_gt 4213 _reflns_number_total 4916 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file op3007sup1.cif _cod_data_source_block 8 _cod_original_cell_volume 2151.4(14) _cod_database_code 2022281 _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 0.978 _shelx_estimated_absorpt_t_max 0.990 _shelx_hkl_file ; 1 0 -4 0.50 0.73 -1 0 4 -0.10 0.45 -1 0 4 0.08 0.19 1 0 -4 0.09 0.26 -1 0 4 0.48 0.66 1 0 -4 0.30 0.42 0 1 0 2.00 0.68 0 -1 0 1.90 1.55 0 1 0 1.79 1.41 1 0 4 0.35 0.59 -1 0 -4 0.52 0.49 -1 0 -4 0.47 0.51 -1 0 -4 0.54 0.50 1 0 4 0.51 0.47 -1 0 -4 0.55 0.50 0 -1 -2 122.15 27.02 0 1 2 123.09 27.22 0 1 -2 104.69 7.63 0 -1 2 111.37 8.12 0 1 2 108.27 7.97 0 1 -2 119.76 26.51 0 -1 2 116.49 25.80 0 1 2 124.28 2.52 0 -1 -2 132.37 2.71 0 1 -2 112.47 8.13 0 -1 2 111.12 8.05 1 0 -5 3716.21 821.21 1 0 -5 3262.26 720.89 -1 0 5 3360.50 742.61 0 1 -3 1727.57 25.12 0 1 -3 1867.18 27.14 0 1 3 1763.77 25.31 0 -1 3 1635.69 23.85 0 1 3 1854.78 27.10 0 -1 -3 1832.41 26.84 1 0 5 318.21 5.46 -1 0 -5 282.89 4.73 0 0 7 -0.21 0.45 0 0 -7 0.02 0.27 0 0 7 -0.60 3.78 0 0 -7 0.28 0.37 0 1 -4 2328.67 514.61 0 1 -4 1815.10 26.38 0 -1 4 1931.47 28.07 0 1 4 2296.21 507.45 0 -1 4 2297.54 507.71 0 1 -4 1850.88 26.60 0 -1 -4 2445.26 540.39 -1 1 0 7508.73 1659.25 -1 1 0 6979.29 1542.61 1 -1 -1 958.98 14.93 -1 1 1 956.62 14.59 1 1 -1 961.31 14.00 -1 -1 1 981.80 14.29 1 -1 -1 943.01 14.34 1 1 -1 1052.74 15.52 -1 -1 1 986.59 14.51 -1 1 1 981.10 14.71 1 1 -1 1042.92 15.70 1 0 -6 1.88 1.77 -1 0 6 1.04 1.06 1 0 -6 0.13 0.49 -1 0 6 0.39 0.46 -1 0 6 0.25 0.29 1 0 -6 0.37 0.70 -1 -1 -1 497.71 8.04 -1 1 -1 471.17 7.87 1 1 1 470.99 7.04 -1 -1 -1 482.80 7.19 1 1 1 433.03 6.72 -1 1 -1 444.72 7.34 1 -1 1 471.21 8.01 -1 1 -1 458.07 7.24 1 -1 1 465.31 7.49 1 1 1 465.37 7.53 1 1 -2 10.20 0.99 -1 1 2 11.06 1.39 -1 -1 2 10.42 1.00 1 1 -2 9.97 0.93 1 -1 -2 9.72 1.39 1 1 -2 11.20 1.01 1 -1 -2 10.27 1.30 1 -1 -2 10.87 1.36 -1 1 2 10.32 1.05 -1 1 2 10.17 1.09 1 1 -2 11.74 1.14 -1 -1 2 9.87 0.97 -1 0 -6 0.16 0.59 1 0 6 0.35 0.49 1 0 6 0.12 0.32 1 0 6 1.56 1.62 1 0 6 0.28 0.35 -1 0 -6 0.20 0.28 1 1 2 3452.81 763.02 -1 -1 -2 2636.61 582.67 -1 -1 -2 3200.73 707.30 1 -1 2 3284.95 725.94 -1 1 -2 3593.17 794.07 -1 1 -2 3492.52 773.48 1 1 2 3049.04 673.78 -1 1 -2 3395.74 750.42 1 -1 2 2407.06 531.96 0 -1 5 4246.99 938.50 0 1 -5 4308.79 952.27 0 1 5 3910.33 864.12 -1 -1 -3 520.31 7.60 1 1 3 495.22 7.74 -1 1 -3 499.83 8.44 1 -1 3 546.86 8.30 -1 1 -3 541.08 8.24 1 -1 3 495.91 8.28 1 1 3 520.93 7.63 -1 0 7 124.55 2.96 1 0 -7 121.67 26.96 -1 0 7 130.82 2.68 -1 0 7 118.20 26.18 1 0 -7 132.81 2.58 0 0 -8 846.95 12.82 0 0 8 766.07 11.45 0 0 8 800.47 12.27 -1 -1 -4 2019.90 29.44 -1 1 -4 1879.50 27.78 -1 -1 -4 2031.58 29.86 -1 1 -4 2040.77 29.38 1 1 4 1968.15 28.73 1 -1 4 1840.34 27.20 -1 -1 -4 1928.71 27.56 1 1 4 2037.03 29.10 -2 0 0 9.99 1.44 2 0 0 11.99 2.20 2 0 0 8.83 1.04 -1 0 -7 3908.16 863.89 2 0 -1 0.79 0.96 -2 0 1 0.51 0.45 -2 0 1 0.68 0.90 2 0 -1 0.59 0.65 2 0 1 0.63 0.78 -2 0 -1 0.68 0.61 2 0 1 0.47 1.02 2 0 -2 3167.37 699.96 -2 0 2 2585.63 571.42 2 0 -2 3407.38 752.98 -2 0 2 2334.74 515.95 -2 0 -2 415.29 7.27 -2 0 -2 413.33 6.77 -1 -1 5 31.26 2.69 -1 1 5 31.09 2.61 1 -1 -5 39.64 3.90 -1 -1 5 29.80 2.37 -1 -1 5 33.43 2.49 1 1 -5 32.29 2.58 1 1 -5 32.38 2.39 -1 1 5 34.41 2.80 1 -1 -5 34.99 2.78 2 0 -3 0.64 0.76 2 0 -3 0.24 0.42 -2 0 3 0.53 0.64 -2 0 3 0.89 1.30 -1 -1 -5 5169.05 1142.27 -2 0 -3 0.99 1.23 -2 0 -3 0.71 0.65 2 0 3 5.53 2.31 -2 0 -3 0.36 0.86 2 0 3 0.95 1.15 -1 0 8 -0.36 0.71 1 0 -8 -0.11 0.58 1 0 -8 0.39 0.55 0 0 9 -0.24 10.41 0 0 9 0.33 0.37 0 0 9 -0.03 0.74 0 0 -9 0.39 0.64 2 0 -4 606.08 9.85 -2 0 4 582.92 9.01 -2 0 4 656.51 10.52 2 0 -4 612.82 9.79 1 0 8 -0.98 2.38 1 0 8 -0.29 0.77 -1 0 -8 -0.01 0.48 1 0 8 0.21 0.53 -1 0 -8 0.84 0.80 2 0 4 8205.63 1813.25 -2 0 -4 6483.33 1432.69 2 0 4 5072.93 1121.03 -1 -1 -6 3084.68 681.64 -1 1 -6 2617.58 578.42 1 1 6 2653.49 586.46 1 -1 6 3523.61 778.70 -1 -1 -6 3122.11 689.97 -2 0 5 0.36 0.73 2 0 -5 0.83 1.14 2 0 -5 0.28 0.36 -2 0 5 0.17 0.30 2 0 5 3.64 1.78 2 0 5 1.72 2.35 1 1 -7 221.92 4.04 1 1 -7 208.78 3.49 -1 -1 7 227.65 3.84 -1 -1 7 195.36 3.69 1 -1 -7 215.43 4.14 1 -1 -7 235.11 5.84 -1 1 7 222.29 4.52 0 1 -8 1617.19 23.18 0 -1 -8 1623.79 85.04 0 1 -8 1749.83 25.93 0 0 10 2486.54 549.49 0 0 10 2274.42 502.65 0 0 10 2970.26 656.43 0 0 -10 3726.06 823.40 -2 0 6 71.84 5.31 -2 0 6 64.35 4.79 2 0 -6 76.87 5.83 -2 0 6 75.18 5.69 -2 -1 0 374.45 5.90 -2 -1 0 381.03 6.26 2 -1 0 391.68 6.65 2 1 0 352.00 6.43 2 -1 0 376.74 6.83 -2 1 0 346.11 6.85 2 1 0 351.14 5.86 -1 -1 -7 1398.68 20.21 1 -1 7 1358.29 20.71 -1 -1 -7 1379.91 21.23 1 1 7 1358.26 23.04 1 -1 7 1314.39 18.95 -1 1 -7 1477.64 21.23 -2 -1 1 245.66 3.89 -2 -1 1 249.18 4.55 2 1 -1 256.90 5.67 2 -1 -1 249.66 4.66 2 -1 -1 273.52 5.39 -2 1 1 266.31 5.77 2 1 -1 268.49 4.26 2 1 1 136.34 2.80 -2 1 -1 142.44 3.45 2 -1 1 127.24 3.32 -2 -1 -1 141.50 2.79 2 1 1 144.88 3.53 2 -1 1 142.94 3.19 -2 -1 -1 122.07 27.12 2 1 1 147.30 2.76 -2 -1 2 702.75 10.27 -2 1 2 751.27 12.20 -2 -1 2 686.87 11.00 2 1 -2 711.62 11.56 -2 -1 -2 498.61 7.85 2 1 2 460.71 7.30 -2 1 -2 494.85 8.71 -2 -1 -2 465.70 7.35 2 -1 2 476.41 8.29 2 1 2 524.60 8.32 -2 1 3 339.22 6.32 -2 -1 3 346.87 6.00 2 1 -3 332.08 4.92 2 -1 -3 335.33 6.40 2 1 -3 344.03 6.41 2 -1 3 106.73 7.99 2 1 3 99.48 7.32 2 -1 3 109.12 8.03 -2 -1 -3 92.69 6.82 -2 1 -3 96.05 7.28 -2 -1 -3 94.77 7.07 2 1 3 93.32 6.85 -2 1 -3 102.07 7.50 2 1 3 97.82 7.38 1 1 -8 1379.78 20.14 -1 -1 8 1444.32 21.12 1 -1 -8 1488.98 27.28 1 1 -8 1477.13 21.80 -1 -1 8 1500.13 22.22 2 0 -7 1.04 1.09 -2 0 7 0.32 0.54 -2 0 7 -0.13 0.73 1 0 -10 -1.30 1.92 -1 0 10 -1.17 2.21 -1 0 10 -0.81 1.68 0 -1 -9 448.51 9.91 0 1 -9 457.68 6.75 0 -1 9 428.48 7.19 0 -1 9 394.47 9.87 0 1 9 462.28 7.29 0 -1 -9 461.31 7.44 2 -1 -4 1828.55 27.28 2 1 -4 1851.69 27.65 1 1 8 7678.85 1696.91 -2 1 -4 105.39 7.93 -2 -1 -4 107.96 7.91 2 1 4 97.35 7.23 2 -1 4 96.93 7.36 2 1 4 103.61 7.79 2 1 4 108.73 7.95 -2 1 -4 105.92 7.77 2 -1 4 102.52 7.54 1 0 10 0.26 0.33 1 0 10 -0.37 2.81 1 0 10 -0.45 0.89 -1 0 -10 0.40 0.41 2 0 7 0.44 0.72 2 0 7 1.30 2.38 0 0 -11 0.43 0.69 0 0 11 0.69 0.69 0 0 11 1.25 1.41 0 0 11 0.34 0.91 -2 -1 5 8.51 1.13 2 -1 -5 6.95 0.97 2 1 -5 8.30 1.05 2 -1 -5 8.48 1.78 -2 1 5 7.18 1.16 -2 0 8 259.09 4.83 -2 0 8 248.17 5.13 2 -1 5 312.27 5.35 -2 1 -5 273.40 6.07 2 1 5 314.60 5.24 -2 -1 -5 301.56 5.09 2 1 5 291.89 5.33 -2 1 -5 267.82 4.83 -1 -1 9 8849.65 1955.66 0 2 0 114.25 25.31 0 -2 0 108.99 8.25 0 2 0 107.46 7.88 0 -2 0 109.96 8.18 0 -1 -10 164.07 3.08 0 1 10 161.75 3.16 0 -1 10 178.63 12.76 0 -1 10 193.06 4.06 0 1 -10 181.46 2.88 0 -1 -10 165.89 98.02 2 1 -6 38.88 3.27 -2 1 6 32.69 2.76 -2 -1 6 33.70 2.75 2 -1 -6 34.76 3.48 2 -1 -6 37.98 3.19 1 -1 9 9999.00 2209.67 0 -2 -1 53.22 4.12 0 -2 1 55.80 4.27 0 -2 1 52.22 4.04 0 2 1 49.05 3.86 0 -2 1 53.45 4.08 0 2 1 50.75 3.84 0 2 -1 50.68 3.83 0 2 1 51.56 3.87 0 2 2 66.40 4.92 0 2 2 74.97 5.71 0 2 2 64.71 4.85 0 -2 -2 67.42 5.14 0 -2 2 70.52 5.39 2 -1 6 1525.69 22.50 -2 1 -6 1520.23 22.39 -2 1 -6 1493.61 23.04 2 -1 6 1624.03 24.70 -2 -1 -6 1605.50 23.57 2 1 6 1533.98 24.00 2 1 6 1511.34 22.22 -1 0 -11 127.04 2.73 1 0 11 123.87 2.59 1 0 11 125.12 3.11 1 0 11 145.60 3.68 0 2 3 717.43 11.83 0 -2 3 732.93 11.67 0 2 3 698.57 10.62 0 -2 3 676.57 10.92 0 2 3 665.64 10.17 -2 0 9 0.41 0.78 -2 0 9 0.23 0.64 2 0 -9 0.77 0.73 2 0 -9 0.13 0.33 0 0 -12 1.30 1.09 0 0 12 0.63 0.72 0 0 12 0.77 0.77 0 0 12 1.17 1.02 -2 1 7 5000.58 1105.07 2 -1 -7 5942.64 1315.09 -2 -1 7 5594.16 1236.22 -2 1 7 5091.60 1125.18 2 1 -7 6035.78 1333.81 -1 1 10 2313.07 511.20 -1 -1 10 2700.80 597.07 1 1 -10 2478.90 547.81 1 1 -10 2036.41 29.75 1 -1 -10 2604.17 576.15 -1 -1 10 2248.20 496.84 -1 -1 10 2468.98 545.63 0 -2 4 3944.17 871.59 0 2 -4 3477.00 768.43 0 2 4 3170.40 700.65 0 -2 4 4020.12 888.41 0 2 4 3218.41 711.21 0 -2 -4 3199.94 707.12 1 2 0 31.28 2.70 1 -2 0 26.97 2.36 1 -2 0 30.75 2.57 -1 -2 0 34.50 2.89 1 2 0 33.09 2.62 -1 -2 0 35.44 2.81 -1 2 0 30.15 2.53 -1 2 1 122.76 27.24 1 2 -1 105.68 7.72 -1 -2 1 108.52 7.94 1 2 -1 103.14 7.64 1 2 -1 100.10 7.35 1 -2 -1 117.59 26.10 -1 -2 1 112.63 8.77 1 2 1 3.27 0.80 -1 2 -1 3.05 0.64 1 2 1 2.91 0.60 -1 -2 -1 3.23 1.32 1 -2 1 3.17 1.46 1 -2 1 4.52 1.39 -1 -2 -1 4.04 0.95 -3 0 0 2.03 1.24 3 0 0 1.05 0.92 3 0 -1 296.31 5.35 3 0 -1 348.42 6.68 -1 -1 -10 4711.92 1041.46 1 1 10 5787.10 1278.81 1 -1 10 4736.20 1046.71 1 1 10 5091.64 1125.31 1 -1 10 4892.22 1081.19 1 2 -2 522.22 8.69 1 2 -2 549.29 8.74 -1 2 2 569.14 9.51 -1 -2 2 572.90 9.75 1 -2 -2 559.88 9.31 1 2 -2 554.98 8.97 -1 -2 2 569.28 9.14 2 0 9 1.44 3.06 -2 0 -9 0.48 1.72 2 0 9 1.52 1.77 -3 0 -1 5052.49 1116.54 2 -1 7 243.17 4.38 2 1 7 232.03 4.21 -2 1 -7 232.49 5.02 -2 -1 -7 243.29 4.42 2 1 7 248.77 4.93 2 1 7 243.10 5.01 -2 1 -7 252.20 4.50 3 0 -2 0.05 0.70 3 0 -2 0.88 1.27 0 -1 11 5685.28 1256.36 0 -1 -11 5781.89 1278.24 0 1 11 5298.51 1170.89 0 -1 -11 4419.37 977.13 0 -1 11 5708.29 1263.47 -1 -2 -2 2339.88 517.07 1 -2 2 2310.26 510.61 1 2 2 2165.52 31.84 1 2 2 2328.52 514.56 -1 2 -2 2184.76 32.65 -3 0 -2 1.56 1.96 3 0 2 1.42 1.29 3 0 2 2.68 1.46 1 0 -12 -0.50 0.98 -1 0 12 -0.01 1.00 -1 0 12 -0.37 1.70 0 2 5 1002.10 15.72 0 2 -5 995.09 15.33 0 -2 5 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33 40.91 11.33 -4 3 -41 7.46 4.12 4 -3 41 6.07 3.85 4 3 41 4.12 3.17 -5 0 44 2.49 2.05 5 3 39 29.53 7.72 5 -3 39 28.97 5.40 5 3 39 31.83 5.84 -5 3 -39 27.55 11.39 0 -4 42 10.43 7.58 0 4 42 9.59 5.90 5 7 15 53.76 9.20 -5 7 -15 44.03 7.96 5 -7 15 43.49 9.19 6 7 7 113.90 17.63 6 -7 7 90.96 15.13 -6 7 -7 108.38 17.65 0 8 13 4.57 2.76 0 -8 -13 -0.61 1.73 -8 6 6 1.85 1.19 -8 6 6 1.34 1.86 8 6 -6 1.68 1.29 -3 8 -4 11.78 11.57 3 8 4 10.95 10.67 5 4 36 3.46 2.44 5 4 36 6.52 3.86 -5 4 -36 6.98 4.41 5 -4 36 7.48 4.26 4 2 43 9.15 5.37 4 -2 43 6.95 8.85 -4 2 -43 6.95 7.61 -9 5 -9 14.64 12.47 9 5 9 19.61 8.17 9 -5 9 15.80 13.23 -7 1 -37 2.48 2.34 7 1 37 2.46 2.95 -6 0 42 56.11 9.36 -8 6 -4 1.53 1.77 8 6 4 1.96 2.12 8 -6 4 2.47 2.10 9 3 24 6.12 3.59 -9 3 -24 8.39 4.65 9 -3 24 8.68 4.88 9 3 24 5.78 3.18 -3 8 5 2.75 2.17 3 8 -5 0.66 1.47 11 -2 -13 58.33 10.22 11 2 -13 60.75 9.99 -11 -2 13 51.37 8.44 -11 2 13 58.14 11.20 -2 8 -10 28.74 5.28 -2 -8 -10 26.33 12.37 -1 -4 42 0.67 1.40 -1 4 42 0.65 1.85 6 7 -9 4.57 3.88 -6 7 9 9.78 6.17 2 0 47 0.12 0.81 2 0 47 0.04 1.45 11 -2 10 2.50 1.61 -11 2 -10 14.53 6.36 11 -2 10 1.47 1.25 11 2 10 2.26 2.28 1 5 38 1.13 1.43 1 -5 38 0.00 1.51 -2 -4 -41 0.67 0.85 2 -4 41 0.82 1.44 2 4 41 0.61 1.87 2 -4 41 1.11 1.25 10 4 8 4.65 2.94 10 -4 8 5.49 3.51 0 0 48 8.36 4.28 0 0 48 8.97 4.97 0 7 26 3.47 4.31 0 7 -26 2.77 2.51 9 4 19 1.18 2.82 9 -4 19 1.83 1.67 -9 4 -19 1.91 1.68 3 0 46 2.14 1.94 -3 0 -46 2.33 2.35 -2 -6 -32 67.72 11.26 2 6 32 71.50 11.44 -2 6 -32 71.13 13.50 2 -6 32 67.70 10.97 -6 1 -40 5.78 4.95 6 -1 40 4.73 3.34 6 1 40 6.38 5.89 8 -2 32 2.15 1.37 8 2 32 0.37 2.01 -8 2 -32 1.89 2.41 8 2 32 2.76 1.70 -1 0 48 0.66 1.33 -1 0 48 1.18 1.11 3 8 5 11.30 7.98 -3 8 -5 10.39 9.50 3 5 36 4.82 3.15 -3 5 -36 2.23 2.83 -3 -5 -36 2.93 1.91 3 -5 36 1.84 1.75 -7 6 -16 1.04 2.19 7 -6 16 1.13 1.33 7 6 16 0.88 1.79 -11 0 -15 3.49 3.55 11 0 15 7.38 3.83 11 0 15 4.88 2.93 8 0 34 0.65 1.93 -11 1 -14 42.08 7.63 11 -1 14 40.75 6.86 -11 -1 -14 37.19 6.95 11 1 14 41.94 7.06 -10 1 -23 14.92 7.44 10 -1 23 19.48 7.92 10 1 23 19.80 7.83 8 6 5 1.54 1.85 8 -6 5 1.33 1.42 -8 6 -5 1.10 1.29 -9 1 -29 5.30 5.62 9 1 29 4.76 3.10 9 -1 29 4.97 3.55 1 6 33 7.68 7.39 -1 6 -33 12.55 5.49 -8 5 -19 0.59 2.12 8 -5 19 0.75 1.27 8 5 19 1.55 1.95 -7 4 -30 3.66 2.83 7 4 30 2.40 2.04 7 -4 30 4.45 3.80 7 4 30 4.12 2.50 -3 4 -40 22.31 9.11 3 -4 40 24.41 9.71 -3 -4 -40 23.62 9.23 3 4 40 24.57 10.34 -10 2 -21 7.90 5.06 10 2 21 4.29 3.04 10 -2 21 5.58 3.79 10 2 21 3.32 3.58 10 3 17 1.52 1.73 10 -3 17 2.74 2.77 -10 3 -17 2.21 1.68 7 2 36 0.13 1.42 7 -2 36 -0.04 1.91 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT2018 (Sheldrick, 2015a)' ; _shelx_hkl_checksum 18073 _shelx_res_file ; TITL shelx_trans_a.res in P2(1)/n shelx_trans.res created by SHELXL-2018/3 at 15:31:38 on 20-Oct-2020 REM Old TITL USJ-2A REM SHELXT solution in P2(1)/n: R1 0.147, Rweak 0.320, Alpha 0.019 REM 0.872 for 406 systematic absences, Orientation as input REM Formula found by SHELXT: C26 O6 CELL 0.71075 9.033 6.4267 37.0804 90 91.948 90 ZERR 4 0.0034 0.0023 0.0138 0 0.007 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 104 96 24 L.S. 30 PLAN 5 SIZE 0.103 0.144 0.237 TEMP -79.75 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.057700 0.207600 FVAR 0.79773 O4 3 -0.351543 -0.427173 -0.584113 11.00000 0.03256 0.03312 = 0.03501 -0.00357 0.00882 -0.00415 O1 3 -0.433590 -0.418522 -0.656571 11.00000 0.02849 0.03923 = 0.03878 -0.00877 -0.00005 -0.00103 O6 3 -0.874346 -0.254090 -0.479626 11.00000 0.03699 0.03917 = 0.04355 -0.00273 0.01364 -0.00228 O2 3 -0.376389 -0.714937 -0.685056 11.00000 0.03496 0.04280 = 0.05313 -0.01130 -0.00121 0.00654 O3 3 -1.061723 -0.577491 -0.725741 11.00000 0.03131 0.06880 = 0.04677 -0.01125 -0.00219 0.00197 O5 3 -0.464713 -0.739397 -0.585740 11.00000 0.04661 0.03602 = 0.07221 -0.01520 0.02299 -0.00964 C23 1 -0.768387 -0.314632 -0.502619 11.00000 0.02783 0.03502 = 0.02865 0.00311 0.00242 0.00097 C21 1 -0.552059 -0.267555 -0.537432 11.00000 0.02676 0.03476 = 0.03260 -0.00083 0.00078 -0.00674 AFIX 43 H21 2 -0.473892 -0.181427 -0.545233 11.00000 -1.20000 AFIX 0 C4 1 -0.021740 -0.248332 -0.608696 11.00000 0.03035 0.03126 = 0.02371 -0.00261 0.00553 0.00157 C20 1 -0.563633 -0.470167 -0.550019 11.00000 0.02702 0.03165 = 0.02871 0.00145 -0.00043 -0.00056 C22 1 -0.652957 -0.188907 -0.513625 11.00000 0.03137 0.03198 = 0.03336 -0.00294 0.00067 -0.00475 AFIX 43 H22 2 -0.643396 -0.050410 -0.504898 11.00000 -1.20000 AFIX 0 C11 1 -0.466081 -0.585834 -0.677326 11.00000 0.03501 0.03272 = 0.02857 0.00011 0.00322 -0.00162 C5 1 -0.100242 -0.108863 -0.630824 11.00000 0.03014 0.03048 = 0.02639 -0.00198 0.00384 0.00148 C17 1 -0.719364 -0.422174 -0.681366 11.00000 0.03546 0.03495 = 0.03215 -0.00361 0.00554 -0.00207 AFIX 43 H17 2 -0.684389 -0.309222 -0.666912 11.00000 -1.20000 AFIX 0 C1 1 -0.280127 -0.386950 -0.645510 11.00000 0.02587 0.03502 = 0.03274 -0.00285 0.00147 -0.00132 AFIX 13 H1 2 -0.214919 -0.442561 -0.664524 11.00000 -1.20000 AFIX 0 C2 1 -0.245249 -0.497869 -0.610143 11.00000 0.03124 0.02939 = 0.03470 -0.00068 0.00711 -0.00003 AFIX 13 H2 2 -0.255637 -0.651483 -0.613700 11.00000 -1.20000 AFIX 0 C25 1 -0.680814 -0.593694 -0.539092 11.00000 0.03460 0.02741 = 0.03841 0.00186 0.00244 -0.00201 AFIX 43 H25 2 -0.690507 -0.732139 -0.547836 11.00000 -1.20000 AFIX 0 C7 1 0.125043 -0.205378 -0.598941 11.00000 0.03184 0.04023 = 0.03001 -0.00101 0.00114 0.00245 AFIX 43 H7 2 0.179121 -0.300670 -0.583993 11.00000 -1.20000 AFIX 0 C12 1 -0.623238 -0.583776 -0.689717 11.00000 0.03117 0.03467 = 0.02657 -0.00133 0.00400 -0.00193 C24 1 -0.782837 -0.516379 -0.515670 11.00000 0.03198 0.03043 = 0.04054 0.00674 0.00689 -0.00546 AFIX 43 H24 2 -0.862836 -0.601075 -0.508487 11.00000 -1.20000 AFIX 0 C16 1 -0.864505 -0.425245 -0.693921 11.00000 0.03428 0.04106 = 0.03652 -0.00281 0.00692 0.00433 AFIX 43 H16 2 -0.929370 -0.315037 -0.687967 11.00000 -1.20000 AFIX 0 C19 1 -0.457828 -0.562138 -0.575050 11.00000 0.02969 0.03268 = 0.03547 -0.00039 0.00091 -0.00322 C3 1 -0.089535 -0.448377 -0.595777 11.00000 0.03165 0.03580 = 0.03980 0.00805 0.00048 0.00200 AFIX 23 H3A 2 -0.091137 -0.443758 -0.569106 11.00000 -1.20000 H3B 2 -0.023784 -0.564625 -0.602348 11.00000 -1.20000 AFIX 0 C10 1 -0.029733 0.068999 -0.642882 11.00000 0.04015 0.03346 = 0.03450 0.00322 0.00341 -0.00045 AFIX 43 H10 2 -0.082449 0.163325 -0.658299 11.00000 -1.20000 AFIX 0 C6 1 -0.258248 -0.154331 -0.642217 11.00000 0.03148 0.03243 = 0.03484 0.00314 -0.00061 0.00190 AFIX 23 H6A 2 -0.282076 -0.086860 -0.665704 11.00000 -1.20000 H6B 2 -0.325647 -0.097433 -0.624166 11.00000 -1.20000 AFIX 0 C15 1 -0.916185 -0.588368 -0.715184 11.00000 0.03034 0.05049 = 0.02847 0.00030 0.00275 -0.00204 C8 1 0.193857 -0.026333 -0.610607 11.00000 0.03070 0.04812 = 0.04020 -0.00375 0.00240 -0.00687 AFIX 43 H8 2 0.293782 0.001968 -0.603418 11.00000 -1.20000 AFIX 0 C13 1 -0.676093 -0.745696 -0.711227 11.00000 0.03691 0.03909 = 0.03587 -0.00741 0.00162 0.00218 AFIX 43 H13 2 -0.611327 -0.855941 -0.717221 11.00000 -1.20000 AFIX 0 C9 1 0.116156 0.110740 -0.632763 11.00000 0.04251 0.03893 = 0.04279 0.00267 0.00615 -0.01085 AFIX 43 H9 2 0.162704 0.233501 -0.641052 11.00000 -1.20000 AFIX 0 C14 1 -0.821771 -0.749425 -0.724127 11.00000 0.03799 0.04719 = 0.03457 -0.01128 -0.00052 -0.00305 AFIX 43 H14 2 -0.856705 -0.860928 -0.738927 11.00000 -1.20000 AFIX 0 C26 1 -0.859864 -0.056981 -0.462366 11.00000 0.04781 0.04437 = 0.04795 -0.01014 0.01257 0.00132 AFIX 137 H26A 2 -0.941190 -0.037839 -0.445851 11.00000 -1.50000 H26B 2 -0.863363 0.053378 -0.480614 11.00000 -1.50000 H26C 2 -0.765068 -0.050762 -0.448749 11.00000 -1.50000 AFIX 0 C18 1 -1.121696 -0.743241 -0.747154 11.00000 0.03774 0.08931 = 0.06083 -0.02745 -0.00807 -0.00220 AFIX 137 H18A 2 -1.104362 -0.875685 -0.734611 11.00000 -1.50000 H18B 2 -1.073554 -0.746097 -0.770438 11.00000 -1.50000 H18C 2 -1.228428 -0.721964 -0.751144 11.00000 -1.50000 AFIX 0 HKLF 4 REM shelx_trans_a.res in P2(1)/n REM wR2 = 0.1159, GooF = S = 1.044, Restrained GooF = 1.044 for all data REM R1 = 0.0425 for 4213 Fo > 4sig(Fo) and 0.0487 for all 4916 data REM 291 parameters refined using 0 restraints END WGHT 0.0576 0.2084 REM Highest difference peak 0.197, deepest hole -0.197, 1-sigma level 0.046 Q1 1 -0.0632 -0.3231 -0.5987 11.00000 0.05 0.20 Q2 1 -0.1682 -0.1406 -0.6417 11.00000 0.05 0.20 Q3 1 -0.9685 -0.5970 -0.7188 11.00000 0.05 0.18 Q4 1 0.0449 -0.2118 -0.5994 11.00000 0.05 0.17 Q5 1 -0.6923 -0.2610 -0.4986 11.00000 0.05 0.17 ; _shelx_res_checksum 24541 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O4 -0.35154(8) -0.42717(12) -0.58411(2) 0.0334(2) Uani d 1 . . O O1 -0.43359(9) -0.41852(13) -0.65657(2) 0.0355(2) Uani d 1 . . O O6 -0.87435(10) -0.25409(13) -0.47963(2) 0.0396(2) Uani d 1 . . O O2 -0.37639(10) -0.71494(14) -0.68506(3) 0.0437(2) Uani d 1 . . O O3 -1.06172(10) -0.57749(17) -0.72574(3) 0.0490(3) Uani d 1 . . O O5 -0.46471(11) -0.73940(14) -0.58574(3) 0.0511(3) Uani d 1 . . C C23 -0.76839(12) -0.31463(18) -0.50262(3) 0.0305(2) Uani d 1 . . C C21 -0.55206(12) -0.26755(18) -0.53743(3) 0.0314(2) Uani d 1 . . H H21 -0.473892 -0.181427 -0.545233 0.038 Uiso calc 1 . . C C4 -0.02174(12) -0.24833(17) -0.60870(3) 0.0283(2) Uani d 1 . . C C20 -0.56363(11) -0.47017(18) -0.55002(3) 0.0292(2) Uani d 1 . . C C22 -0.65296(12) -0.18891(19) -0.51362(3) 0.0322(3) Uani d 1 . . H H22 -0.643396 -0.050410 -0.504898 0.039 Uiso calc 1 . . C C11 -0.46608(13) -0.58583(18) -0.67733(3) 0.0320(3) Uani d 1 . . C C5 -0.10024(12) -0.10886(17) -0.63082(3) 0.0289(2) Uani d 1 . . C C17 -0.71936(13) -0.42217(19) -0.68137(3) 0.0341(3) Uani d 1 . . H H17 -0.684389 -0.309222 -0.666912 0.041 Uiso calc 1 . . C C1 -0.28013(12) -0.38695(18) -0.64551(3) 0.0312(2) Uani d 1 . . H H1 -0.214919 -0.442561 -0.664524 0.037 Uiso calc 1 . . C C2 -0.24525(12) -0.49787(18) -0.61014(3) 0.0316(2) Uani d 1 . . H H2 -0.255637 -0.651483 -0.613700 0.038 Uiso calc 1 . . C C25 -0.68081(13) -0.59369(18) -0.53909(3) 0.0334(3) Uani d 1 . . H H25 -0.690507 -0.732139 -0.547836 0.040 Uiso calc 1 . . C C7 0.12504(13) -0.20538(19) -0.59894(3) 0.0340(3) Uani d 1 . . H H7 0.179121 -0.300670 -0.583993 0.041 Uiso calc 1 . . C C12 -0.62324(12) -0.58378(18) -0.68972(3) 0.0307(2) Uani d 1 . . C C24 -0.78284(13) -0.51638(18) -0.51567(3) 0.0342(3) Uani d 1 . . H H24 -0.862836 -0.601075 -0.508487 0.041 Uiso calc 1 . . C C16 -0.86451(13) -0.4252(2) -0.69392(3) 0.0372(3) Uani d 1 . . H H16 -0.929370 -0.315037 -0.687967 0.045 Uiso calc 1 . . C C19 -0.45783(12) -0.56214(18) -0.57505(3) 0.0326(3) Uani d 1 . . C C3 -0.08953(13) -0.44838(19) -0.59578(3) 0.0358(3) Uani d 1 . . H H3A -0.091137 -0.443758 -0.569106 0.043 Uiso calc 1 . . H H3B -0.023784 -0.564625 -0.602348 0.043 Uiso calc 1 . . C C10 -0.02973(14) 0.06900(19) -0.64288(3) 0.0360(3) Uani d 1 . . H H10 -0.082449 0.163325 -0.658299 0.043 Uiso calc 1 . . C C6 -0.25825(13) -0.15433(18) -0.64222(3) 0.0330(3) Uani d 1 . . H H6A -0.282076 -0.086860 -0.665704 0.040 Uiso calc 1 . . H H6B -0.325647 -0.097433 -0.624166 0.040 Uiso calc 1 . . C C15 -0.91618(13) -0.5884(2) -0.71518(3) 0.0364(3) Uani d 1 . . C C8 0.19386(13) -0.0263(2) -0.61061(3) 0.0396(3) Uani d 1 . . H H8 0.293782 0.001968 -0.603418 0.048 Uiso calc 1 . . C C13 -0.67609(14) -0.7457(2) -0.71123(3) 0.0373(3) Uani d 1 . . H H13 -0.611327 -0.855941 -0.717221 0.045 Uiso calc 1 . . C C9 0.11616(14) 0.1107(2) -0.63276(4) 0.0413(3) Uani d 1 . . H H9 0.162704 0.233501 -0.641052 0.050 Uiso calc 1 . . C C14 -0.82177(14) -0.7494(2) -0.72413(3) 0.0400(3) Uani d 1 . . H H14 -0.856705 -0.860928 -0.738927 0.048 Uiso calc 1 . . C C26 -0.85986(16) -0.0570(2) -0.46237(4) 0.0465(3) Uani d 1 . . H H26A -0.941190 -0.037839 -0.445851 0.070 Uiso calc 1 . . H H26B -0.863363 0.053378 -0.480614 0.070 Uiso calc 1 . . H H26C -0.765068 -0.050762 -0.448749 0.070 Uiso calc 1 . . C C18 -1.12170(16) -0.7432(3) -0.74715(5) 0.0628(5) Uani d 1 . . H H18A -1.104362 -0.875685 -0.734611 0.094 Uiso calc 1 . . H H18B -1.073554 -0.746097 -0.770438 0.094 Uiso calc 1 . . H H18C -1.228428 -0.721964 -0.751144 0.094 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O4 0.0326(4) 0.0331(4) 0.0350(4) -0.0042(3) 0.0088(3) -0.0036(3) O1 0.0285(4) 0.0392(5) 0.0388(4) -0.0010(3) -0.0001(3) -0.0088(4) O6 0.0370(5) 0.0392(5) 0.0435(5) -0.0023(4) 0.0136(4) -0.0027(4) O2 0.0350(5) 0.0428(5) 0.0531(5) 0.0065(4) -0.0012(4) -0.0113(4) O3 0.0313(5) 0.0688(7) 0.0468(5) 0.0020(4) -0.0022(4) -0.0112(5) O5 0.0466(6) 0.0360(5) 0.0722(7) -0.0096(4) 0.0230(5) -0.0152(5) C23 0.0278(5) 0.0350(6) 0.0286(5) 0.0010(4) 0.0024(4) 0.0031(4) C21 0.0268(5) 0.0348(6) 0.0326(6) -0.0067(4) 0.0008(4) -0.0008(5) C4 0.0304(5) 0.0313(6) 0.0237(5) 0.0016(4) 0.0055(4) -0.0026(4) C20 0.0270(5) 0.0317(6) 0.0287(5) -0.0006(4) -0.0004(4) 0.0015(4) C22 0.0314(6) 0.0320(6) 0.0334(6) -0.0047(5) 0.0007(4) -0.0029(5) C11 0.0350(6) 0.0327(6) 0.0286(5) -0.0016(5) 0.0032(4) 0.0001(4) C5 0.0301(5) 0.0305(6) 0.0264(5) 0.0015(4) 0.0038(4) -0.0020(4) C17 0.0355(6) 0.0349(6) 0.0322(6) -0.0021(5) 0.0055(5) -0.0036(5) C1 0.0259(5) 0.0350(6) 0.0327(6) -0.0013(4) 0.0015(4) -0.0029(5) C2 0.0312(6) 0.0294(6) 0.0347(6) 0.0000(4) 0.0071(4) -0.0007(5) C25 0.0346(6) 0.0274(6) 0.0384(6) -0.0020(4) 0.0024(5) 0.0019(5) C7 0.0318(6) 0.0402(7) 0.0300(6) 0.0024(5) 0.0011(4) -0.0010(5) C12 0.0312(6) 0.0347(6) 0.0266(5) -0.0019(4) 0.0040(4) -0.0013(4) C24 0.0320(6) 0.0304(6) 0.0405(6) -0.0055(5) 0.0069(5) 0.0067(5) C16 0.0343(6) 0.0411(7) 0.0365(6) 0.0043(5) 0.0069(5) -0.0028(5) C19 0.0297(6) 0.0327(6) 0.0355(6) -0.0032(4) 0.0009(4) -0.0004(5) C3 0.0317(6) 0.0358(6) 0.0398(6) 0.0020(5) 0.0005(5) 0.0081(5) C10 0.0402(6) 0.0335(6) 0.0345(6) -0.0004(5) 0.0034(5) 0.0032(5) C6 0.0315(6) 0.0324(6) 0.0348(6) 0.0019(5) -0.0006(4) 0.0031(5) C15 0.0303(6) 0.0505(7) 0.0285(6) -0.0020(5) 0.0028(4) 0.0003(5) C8 0.0307(6) 0.0481(7) 0.0402(6) -0.0069(5) 0.0024(5) -0.0037(6) C13 0.0369(6) 0.0391(7) 0.0359(6) 0.0022(5) 0.0016(5) -0.0074(5) C9 0.0425(7) 0.0389(7) 0.0428(7) -0.0109(5) 0.0062(5) 0.0027(5) C14 0.0380(6) 0.0472(8) 0.0346(6) -0.0031(5) -0.0005(5) -0.0113(5) C26 0.0478(8) 0.0444(8) 0.0479(7) 0.0013(6) 0.0126(6) -0.0101(6) C18 0.0377(7) 0.0893(13) 0.0608(9) -0.0022(8) -0.0081(7) -0.0275(9) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C19 O4 C2 . . 117.16(9) ? C11 O1 C1 . . 117.48(9) ? C23 O6 C26 . . 118.73(10) ? C15 O3 C18 . . 117.86(11) ? O6 C23 C22 . . 124.62(11) ? O6 C23 C24 . . 115.20(10) ? C24 C23 C22 . . 120.17(11) ? C20 C21 H21 . . 119.6 ? C22 C21 H21 . . 119.6 ? C22 C21 C20 . . 120.90(10) ? C5 C4 C3 . . 122.09(10) ? C7 C4 C5 . . 119.18(10) ? C7 C4 C3 . . 118.71(10) ? C21 C20 C25 . . 119.10(10) ? C21 C20 C19 . . 122.97(10) ? C25 C20 C19 . . 117.92(10) ? C23 C22 H22 . . 120.3 ? C21 C22 C23 . . 119.39(11) ? C21 C22 H22 . . 120.3 ? O1 C11 C12 . . 111.01(10) ? O2 C11 O1 . . 123.46(11) ? O2 C11 C12 . . 125.51(11) ? C4 C5 C6 . . 120.00(10) ? C10 C5 C4 . . 119.28(11) ? C10 C5 C6 . . 120.70(10) ? C12 C17 H17 . . 119.8 ? C16 C17 H17 . . 119.8 ? C16 C17 C12 . . 120.47(11) ? O1 C1 H1 . . 109.4 ? O1 C1 C2 . . 110.38(9) ? O1 C1 C6 . . 106.43(9) ? C2 C1 H1 . . 109.4 ? C6 C1 H1 . . 109.4 ? C6 C1 C2 . . 111.85(10) ? O4 C2 C1 . . 107.71(9) ? O4 C2 H2 . . 109.5 ? O4 C2 C3 . . 108.98(10) ? C1 C2 H2 . . 109.5 ? C1 C2 C3 . . 111.54(9) ? C3 C2 H2 . . 109.5 ? C20 C25 H25 . . 119.7 ? C24 C25 C20 . . 120.51(11) ? C24 C25 H25 . . 119.7 ? C4 C7 H7 . . 119.4 ? C8 C7 C4 . . 121.22(11) ? C8 C7 H7 . . 119.4 ? C17 C12 C11 . . 122.44(11) ? C13 C12 C11 . . 118.74(10) ? C13 C12 C17 . . 118.80(11) ? C23 C24 H24 . . 120.0 ? C25 C24 C23 . . 119.91(10) ? C25 C24 H24 . . 120.0 ? C17 C16 H16 . . 119.9 ? C17 C16 C15 . . 120.18(11) ? C15 C16 H16 . . 119.9 ? O4 C19 C20 . . 112.41(10) ? O5 C19 O4 . . 123.77(11) ? O5 C19 C20 . . 123.81(11) ? C4 C3 C2 . . 116.58(10) ? C4 C3 H3A . . 108.1 ? C4 C3 H3B . . 108.1 ? C2 C3 H3A . . 108.1 ? C2 C3 H3B . . 108.1 ? H3A C3 H3B . . 107.3 ? C5 C10 H10 . . 119.5 ? C9 C10 C5 . . 120.98(12) ? C9 C10 H10 . . 119.5 ? C5 C6 C1 . . 109.57(9) ? C5 C6 H6A . . 109.8 ? C5 C6 H6B . . 109.8 ? C1 C6 H6A . . 109.8 ? C1 C6 H6B . . 109.8 ? H6A C6 H6B . . 108.2 ? O3 C15 C16 . . 115.41(11) ? O3 C15 C14 . . 124.39(11) ? C16 C15 C14 . . 120.19(11) ? C7 C8 H8 . . 120.3 ? C9 C8 C7 . . 119.47(12) ? C9 C8 H8 . . 120.3 ? C12 C13 H13 . . 119.5 ? C14 C13 C12 . . 121.09(11) ? C14 C13 H13 . . 119.5 ? C10 C9 H9 . . 120.1 ? C8 C9 C10 . . 119.87(12) ? C8 C9 H9 . . 120.1 ? C15 C14 H14 . . 120.4 ? C13 C14 C15 . . 119.26(11) ? C13 C14 H14 . . 120.4 ? O6 C26 H26A . . 109.5 ? O6 C26 H26B . . 109.5 ? O6 C26 H26C . . 109.5 ? H26A C26 H26B . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? O3 C18 H18A . . 109.5 ? O3 C18 H18B . . 109.5 ? O3 C18 H18C . . 109.5 ? H18A C18 H18B . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O4 C2 . 1.4570(13) ? O4 C19 . 1.3450(14) ? O1 C11 . 1.3488(14) ? O1 C1 . 1.4465(14) ? O6 C23 . 1.3601(14) ? O6 C26 . 1.4233(16) ? O2 C11 . 1.2012(14) ? O3 C15 . 1.3607(15) ? O3 C18 . 1.4246(18) ? O5 C19 . 1.2071(15) ? C23 C22 . 1.3912(16) ? C23 C24 . 1.3885(17) ? C21 H21 . 0.9500 ? C21 C20 . 1.3860(16) ? C21 C22 . 1.3857(16) ? C4 C5 . 1.3928(16) ? C4 C7 . 1.3901(16) ? C4 C3 . 1.5091(17) ? C20 C25 . 1.3943(16) ? C20 C19 . 1.4780(16) ? C22 H22 . 0.9500 ? C11 C12 . 1.4772(16) ? C5 C10 . 1.3898(17) ? C5 C6 . 1.5033(16) ? C17 H17 . 0.9500 ? C17 C12 . 1.3953(17) ? C17 C16 . 1.3764(17) ? C1 H1 . 1.0000 ? C1 C2 . 1.5163(17) ? C1 C6 . 1.5124(17) ? C2 H2 . 1.0000 ? C2 C3 . 1.5207(16) ? C25 H25 . 0.9500 ? C25 C24 . 1.3802(16) ? C7 H7 . 0.9500 ? C7 C8 . 1.3841(18) ? C12 C13 . 1.3860(16) ? C24 H24 . 0.9500 ? C16 H16 . 0.9500 ? C16 C15 . 1.3833(18) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C10 H10 . 0.9500 ? C10 C9 . 1.3841(18) ? C6 H6A . 0.9900 ? C6 H6B . 0.9900 ? C15 C14 . 1.3885(18) ? C8 H8 . 0.9500 ? C8 C9 . 1.3800(19) ? C13 H13 . 0.9500 ? C13 C14 . 1.3850(18) ? C9 H9 . 0.9500 ? C14 H14 . 0.9500 ? C26 H26A . 0.9800 ? C26 H26B . 0.9800 ? C26 H26C . 0.9800 ? C18 H18A . 0.9800 ? C18 H18B . 0.9800 ? C18 H18C . 0.9800 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O4 C2 C3 C4 . . . . -95.62(12) ? O1 C11 C12 C17 . . . . 2.17(15) ? O1 C11 C12 C13 . . . . -179.58(10) ? O1 C1 C2 O4 . . . . -54.30(12) ? O1 C1 C2 C3 . . . . -173.84(9) ? O1 C1 C6 C5 . . . . -179.86(8) ? O6 C23 C22 C21 . . . . -179.50(10) ? O6 C23 C24 C25 . . . . -179.75(10) ? O2 C11 C12 C17 . . . . -176.18(12) ? O2 C11 C12 C13 . . . . 2.08(18) ? O3 C15 C14 C13 . . . . -178.78(11) ? C21 C20 C25 C24 . . . . -0.88(17) ? C21 C20 C19 O4 . . . . -0.39(16) ? C21 C20 C19 O5 . . . . 178.58(12) ? C4 C5 C10 C9 . . . . -1.02(17) ? C4 C5 C6 C1 . . . . -31.79(14) ? C4 C7 C8 C9 . . . . -0.96(18) ? C20 C21 C22 C23 . . . . -0.82(17) ? C20 C25 C24 C23 . . . . -0.49(18) ? C22 C23 C24 C25 . . . . 1.22(17) ? C22 C21 C20 C25 . . . . 1.54(17) ? C22 C21 C20 C19 . . . . -179.20(10) ? C11 O1 C1 C2 . . . . -89.50(12) ? C11 O1 C1 C6 . . . . 148.93(10) ? C11 C12 C13 C14 . . . . -178.80(11) ? C5 C4 C7 C8 . . . . 0.45(17) ? C5 C4 C3 C2 . . . . 3.93(16) ? C5 C10 C9 C8 . . . . 0.51(19) ? C17 C12 C13 C14 . . . . -0.48(18) ? C17 C16 C15 O3 . . . . 179.16(11) ? C17 C16 C15 C14 . . . . -0.31(19) ? C1 O1 C11 O2 . . . . 4.77(16) ? C1 O1 C11 C12 . . . . -173.61(9) ? C1 C2 C3 C4 . . . . 23.17(14) ? C2 O4 C19 O5 . . . . 4.04(17) ? C2 O4 C19 C20 . . . . -176.99(9) ? C2 C1 C6 C5 . . . . 59.51(12) ? C25 C20 C19 O4 . . . . 178.88(10) ? C25 C20 C19 O5 . . . . -2.15(18) ? C7 C4 C5 C10 . . . . 0.54(16) ? C7 C4 C5 C6 . . . . 178.92(10) ? C7 C4 C3 C2 . . . . -174.26(10) ? C7 C8 C9 C10 . . . . 0.48(19) ? C12 C17 C16 C15 . . . . -0.43(18) ? C12 C13 C14 C15 . . . . -0.24(19) ? C24 C23 C22 C21 . . . . -0.57(17) ? C16 C17 C12 C11 . . . . 179.07(10) ? C16 C17 C12 C13 . . . . 0.82(17) ? C16 C15 C14 C13 . . . . 0.64(19) ? C19 O4 C2 C1 . . . . 107.25(11) ? C19 O4 C2 C3 . . . . -131.59(10) ? C19 C20 C25 C24 . . . . 179.82(10) ? C3 C4 C5 C10 . . . . -177.65(10) ? C3 C4 C5 C6 . . . . 0.73(16) ? C3 C4 C7 C8 . . . . 178.69(11) ? C10 C5 C6 C1 . . . . 146.56(11) ? C6 C5 C10 C9 . . . . -179.39(11) ? C6 C1 C2 O4 . . . . 64.00(12) ? C6 C1 C2 C3 . . . . -55.54(13) ? C26 O6 C23 C22 . . . . -6.92(17) ? C26 O6 C23 C24 . . . . 174.11(11) ? C18 O3 C15 C16 . . . . -178.89(13) ? C18 O3 C15 C14 . . . . 0.55(19) ? _cod_database_fobs_code 2022281