#------------------------------------------------------------------------------ #$Date: 2020-04-23 23:29:44 +0300 (Thu, 23 Apr 2020) $ #$Revision: 251110 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557895.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_1557895 loop_ _publ_author_name 'Su, Li-Hua' 'Geng, Chang-An' 'Li, Tian-Ze' 'Huang, Xiao-Yan' 'Ma, Yun-Bao' 'Zhang, Xue-Mei' 'Wu, Gang' 'Yang, Zhu-Liang' 'Chen, Ji-Jun' _publ_section_title ; Spiroseoflosterol, a Rearranged Ergostane-Steroid from the Fruiting Bodies of Butyriboletus roseoflavus ; _journal_name_full 'Journal of Natural Products' _journal_paper_doi 10.1021/acs.jnatprod.9b01282 _journal_year 2020 _chemical_absolute_configuration unk _chemical_formula_sum 'C28 H48 O4' _chemical_formula_weight 448.66 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 95.407(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 45.216(2) _cell_length_b 6.5755(3) _cell_length_c 9.0610(4) _cell_measurement_reflns_used 4369 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 70.0137 _cell_measurement_theta_min 3.9281 _cell_volume 2682.0(2) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.1856 _diffrn_reflns_av_unetI/netI 0.1002 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 33984 _diffrn_reflns_theta_full 72.50 _diffrn_reflns_theta_max 72.50 _diffrn_reflns_theta_min 3.93 _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'translucent light colourless' _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 992 _exptl_crystal_size_max 1.000 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.202 _refine_diff_density_min -0.221 _refine_ls_abs_structure_details ; Flack x determined using 823 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.9(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 297 _refine_ls_number_reflns 5115 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0680 _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^)+(0.0613P)^2^+1.3804P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1451 _refine_ls_wR_factor_ref 0.1767 _reflns_number_gt 3048 _reflns_number_total 5115 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np9b01282_si_002.cif _cod_data_source_block jbc54 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 1557895 _shelx_res_file ; TITL jbc54_0m_a.res in C2 jbc54_0m.res created by SHELXL-2017/1 at 17:01:01 on 12-Aug-2019 CELL 1.54178 45.2156 6.5755 9.0610 90.000 95.407 90.000 ZERR 4.00 0.0021 0.0003 0.0004 0.000 0.003 0.000 LATT -7 SYMM -x, y, -z SFAC C H O UNIT 112 192 16 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.130 SIZE 0.010 0.050 1.000 ACTA EQIV $1 x, y+1, z-1 HTAB O4 O3_$1 EQIV $2 -x+3/2, y+1/2, -z HTAB O4 O1_$2 HTAB O1 O4 EQIV $3 x, y, z+1 HTAB O3 O1_$3 HTAB C7 O3 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.061300 1.380400 FVAR 0.33493 O4 3 0.725144 1.133566 -0.067710 11.00000 0.05707 0.04609 = 0.06579 0.01424 -0.00079 -0.00080 AFIX 3 H47 2 0.718701 1.221291 -0.144954 11.00000 -1.50000 H48 2 0.746357 1.170440 -0.053674 11.00000 -1.50000 AFIX 0 O1 3 0.714796 0.751217 0.022901 11.00000 0.05498 0.03848 = 0.03354 -0.00136 0.00468 0.00054 AFIX 147 H45 2 0.716513 0.874501 0.000966 11.00000 -1.50000 AFIX 0 O2 3 0.662247 0.132930 0.543154 11.00000 0.07424 0.03375 = 0.06577 -0.01644 0.02348 -0.01021 O3 3 0.706654 0.496180 0.775073 11.00000 0.05702 0.03670 = 0.03569 0.00128 -0.00600 0.00127 AFIX 147 H46 2 0.709895 0.555777 0.856999 11.00000 -1.50000 AFIX 0 C1 1 0.696608 0.732969 0.145290 11.00000 0.04833 0.04669 = 0.02653 -0.00099 0.00302 0.00148 AFIX 13 H1 2 0.680394 0.836638 0.132036 11.00000 -1.20000 AFIX 0 C2 1 0.682563 0.523305 0.136600 11.00000 0.06131 0.05950 = 0.03395 -0.00782 0.00173 -0.01229 AFIX 23 H44 2 0.698417 0.419831 0.134306 11.00000 -1.20000 H43 2 0.669504 0.512073 0.042926 11.00000 -1.20000 AFIX 0 C3 1 0.664302 0.477713 0.267069 11.00000 0.05876 0.05620 = 0.03503 -0.00770 0.00355 -0.00482 AFIX 23 H42 2 0.646980 0.570284 0.263376 11.00000 -1.20000 H3 2 0.656815 0.336257 0.259468 11.00000 -1.20000 AFIX 0 C4 1 0.683311 0.505640 0.413401 11.00000 0.04765 0.03089 = 0.03487 -0.00706 0.00369 -0.00102 C5 1 0.667530 0.498471 0.560139 11.00000 0.04480 0.02914 = 0.03415 -0.00481 0.00277 0.00427 C6 1 0.660829 0.284623 0.615754 11.00000 0.04143 0.03197 = 0.04697 -0.00151 0.00766 -0.00310 C7 1 0.647472 0.285989 0.762196 11.00000 0.04483 0.03153 = 0.03763 -0.00071 0.00472 0.00172 AFIX 13 H10 2 0.659283 0.382658 0.829524 11.00000 -1.20000 AFIX 0 C8 1 0.615271 0.369419 0.736789 11.00000 0.04014 0.03922 = 0.03601 -0.00153 -0.00188 -0.00370 C9 1 0.605606 0.336668 0.894872 11.00000 0.04773 0.03059 = 0.03572 -0.00436 0.00274 -0.00102 AFIX 13 H14 2 0.616365 0.440482 0.960322 11.00000 -1.20000 AFIX 0 C10 1 0.572673 0.351482 0.921355 11.00000 0.04885 0.03748 = 0.03706 0.00073 0.00472 0.00104 AFIX 13 H15 2 0.561533 0.250943 0.854522 11.00000 -1.20000 AFIX 0 C11 1 0.568616 0.292394 1.079242 11.00000 0.04779 0.04435 = 0.04047 -0.00624 0.00325 0.00543 AFIX 43 H16 2 0.576591 0.382845 1.154506 11.00000 -1.20000 AFIX 0 C12 1 0.555243 0.129376 1.123435 11.00000 0.04696 0.04740 = 0.03622 0.00041 0.00141 -0.00310 AFIX 43 H27 2 0.546428 0.040439 1.049227 11.00000 -1.20000 AFIX 0 C13 1 0.552790 0.072292 1.283131 11.00000 0.06401 0.03874 = 0.03853 0.00314 0.00240 -0.00247 AFIX 13 H20 2 0.564221 0.177220 1.344693 11.00000 -1.20000 AFIX 0 C14 1 0.520794 0.079545 1.327437 11.00000 0.05424 0.05051 = 0.04067 0.00714 0.00191 0.00086 AFIX 13 H24 2 0.521718 0.047878 1.435718 11.00000 -1.20000 AFIX 0 C15 1 0.507559 0.291075 1.305883 11.00000 0.05635 0.07278 = 0.06859 0.01561 0.01388 0.01037 AFIX 137 H26 2 0.488543 0.296814 1.349434 11.00000 -1.50000 H25 2 0.504357 0.321551 1.199709 11.00000 -1.50000 H2 2 0.521243 0.391286 1.354604 11.00000 -1.50000 AFIX 0 C16 1 0.709533 0.352203 0.427410 11.00000 0.05644 0.03654 = 0.05830 0.00247 0.01242 0.00071 AFIX 137 H5 2 0.724780 0.396394 0.364353 11.00000 -1.50000 H4 2 0.702284 0.217103 0.395916 11.00000 -1.50000 H6 2 0.718083 0.346282 0.530804 11.00000 -1.50000 AFIX 0 C17 1 0.636403 0.604745 0.547301 11.00000 0.04705 0.03405 = 0.04120 0.00503 0.00476 0.00425 AFIX 23 H8 2 0.639253 0.750695 0.525856 11.00000 -1.20000 H7 2 0.624183 0.545686 0.461460 11.00000 -1.20000 AFIX 0 C18 1 0.618869 0.587910 0.684566 11.00000 0.04976 0.03750 = 0.03954 -0.00084 0.00132 0.00456 AFIX 23 H9 2 0.629216 0.667837 0.766445 11.00000 -1.20000 H35 2 0.598937 0.648455 0.660976 11.00000 -1.20000 AFIX 0 C19 1 0.645007 0.087676 0.844986 11.00000 0.05634 0.03740 = 0.06402 0.00789 0.01363 0.00167 AFIX 23 H31 2 0.663661 0.057110 0.907212 11.00000 -1.20000 H11 2 0.640401 -0.026514 0.775389 11.00000 -1.20000 AFIX 0 C20 1 0.619175 0.125510 0.941731 11.00000 0.05010 0.03825 = 0.04585 0.00648 0.00808 -0.00178 AFIX 23 H12 2 0.626593 0.126358 1.048075 11.00000 -1.20000 H13 2 0.603992 0.017383 0.925064 11.00000 -1.20000 AFIX 0 C21 1 0.568429 -0.130863 1.318053 11.00000 0.08983 0.06738 = 0.05615 0.01919 0.00602 0.02077 AFIX 137 H18 2 0.589453 -0.118811 1.301252 11.00000 -1.50000 H17 2 0.559112 -0.236921 1.253409 11.00000 -1.50000 H19 2 0.566736 -0.166938 1.421858 11.00000 -1.50000 AFIX 0 C22 1 0.499983 -0.075716 1.246972 11.00000 0.06605 0.08462 = 0.05116 -0.00356 0.00089 -0.02192 AFIX 137 H23 2 0.496703 -0.039759 1.141741 11.00000 -1.50000 H22 2 0.480945 -0.075753 1.290482 11.00000 -1.50000 H21 2 0.508940 -0.211316 1.257032 11.00000 -1.50000 AFIX 0 C23 1 0.559577 0.559420 0.885935 11.00000 0.05693 0.05118 = 0.05544 0.00489 0.00800 0.00926 AFIX 137 H29 2 0.571670 0.663201 0.940776 11.00000 -1.50000 H30 2 0.539239 0.564603 0.914774 11.00000 -1.50000 H28 2 0.559335 0.585195 0.779302 11.00000 -1.50000 AFIX 0 C24 1 0.595814 0.243988 0.624511 11.00000 0.05595 0.05194 = 0.03742 -0.00896 0.00126 -0.01321 AFIX 137 H34 2 0.604661 0.242180 0.529858 11.00000 -1.50000 H32 2 0.575945 0.304523 0.610138 11.00000 -1.50000 H33 2 0.594317 0.104570 0.661304 11.00000 -1.50000 AFIX 0 C25 1 0.689203 0.625458 0.672791 11.00000 0.04746 0.03234 = 0.03544 0.00955 -0.00343 0.00737 AFIX 13 H41 2 0.677277 0.720948 0.729376 11.00000 -1.20000 AFIX 0 C26 1 0.709214 0.749310 0.576741 11.00000 0.05960 0.02776 = 0.03206 0.00015 -0.00487 -0.00703 AFIX 23 H36 2 0.709732 0.894142 0.606723 11.00000 -1.20000 H40 2 0.729745 0.695339 0.586906 11.00000 -1.20000 AFIX 0 C27 1 0.695392 0.726326 0.418971 11.00000 0.04518 0.03426 = 0.03026 -0.00104 0.00277 0.00133 AFIX 13 H39 2 0.677831 0.819322 0.406915 11.00000 -1.20000 AFIX 0 C28 1 0.714231 0.770742 0.292062 11.00000 0.04964 0.03698 = 0.03137 -0.00070 0.00003 0.00103 AFIX 23 H38 2 0.720920 0.914135 0.297514 11.00000 -1.20000 H37 2 0.732061 0.682598 0.301019 11.00000 -1.20000 REM ##### REM ##### AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM jbc54_0m_a.res in C2 REM R1 = 0.0680 for 3048 Fo > 4sig(Fo) and 0.1239 for all 5115 data REM 297 parameters refined using 1 restraints END WGHT 0.0613 1.3803 REM Instructions for potential hydrogen bonds HTAB O4 O3_$1 HTAB O4 O1_$2 HTAB O1 O4 HTAB O3 O1_$3 HTAB C7 O3 REM Highest difference peak 0.202, deepest hole -0.221, 1-sigma level 0.050 Q1 1 0.7111 1.3211 -0.0820 11.00000 0.05 0.20 Q2 1 0.0000 0.2073 0.0000 10.50000 0.05 0.20 Q3 1 0.0211 0.5818 0.8983 11.00000 0.05 0.20 Q4 1 0.2399 0.5582 0.5162 11.00000 0.05 0.19 Q5 1 0.1653 0.6377 0.2631 11.00000 0.05 0.19 ; _shelx_res_checksum 74560 _shelx_hkl_file ; -4 0 0 316.87 16.90 -4 0 0 265.57 17.00 -4 0 0 348.67 17.80 4 0 0 332.27 17.90 -4 0 0 303.67 17.30 -4 0 0 340.97 18.40 4 0 0 305.57 17.50 4 0 0 301.77 17.00 4 0 0 328.57 18.10 -4 0 0 328.67 17.80 4 0 0 318.67 17.00 6 0 0 914.51 40.30 -6 0 0 712.73 47.80 -6 0 0 854.01 42.00 -6 0 0 807.42 39.30 6 0 0 880.71 41.80 6 0 0 875.91 40.60 -8 0 0 1591.14 74.99 -8 0 0 1776.72 82.69 -8 0 0 1807.12 75.19 -8 0 0 1812.82 77.59 8 0 0 1777.82 76.19 8 0 0 1699.43 76.09 -8 0 0 1658.53 79.19 8 0 0 1724.53 78.69 10 0 0 848.42 44.70 -10 0 0 881.11 43.70 10 0 0 897.31 48.80 -10 0 0 785.32 43.70 -10 0 0 880.21 46.50 -10 0 0 778.02 56.89 10 0 0 884.41 45.10 -10 0 0 875.11 51.59 -12 0 0 332.47 28.80 -12 0 0 325.47 30.20 -12 0 0 318.27 26.00 -12 0 0 313.37 23.30 12 0 0 309.37 27.10 12 0 0 327.87 24.80 -12 0 0 310.17 24.00 12 0 0 344.87 25.30 -14 0 0 1962.10 101.39 14 0 0 2014.30 91.79 -14 0 0 1933.71 94.49 14 0 0 1964.50 97.99 14 0 0 1997.70 92.49 -14 0 0 1977.20 89.59 -14 0 0 1836.32 92.09 -14 0 0 1841.02 98.89 -16 0 0 38.50 14.90 16 0 0 27.70 8.70 16 0 0 28.70 7.00 -16 0 0 26.40 14.50 -16 0 0 28.90 9.20 16 0 0 27.00 9.20 16 0 0 46.30 15.10 -16 0 0 25.40 10.20 -16 0 0 25.20 11.60 16 0 0 21.20 9.20 -16 0 0 47.10 11.30 18 0 0 1542.25 83.79 -18 0 0 1376.26 88.59 -18 0 0 1516.05 71.69 -18 0 0 1482.35 84.79 18 0 0 1664.63 83.99 18 0 0 1568.24 89.29 18 0 0 1507.45 68.69 18 0 0 1594.84 80.59 -18 0 0 1539.25 78.59 -18 0 0 1533.75 81.59 -20 0 0 7.30 9.70 -20 0 0 18.30 8.70 -20 0 0 19.90 10.30 20 0 0 18.50 13.40 20 0 0 15.50 9.40 20 0 0 13.70 7.20 -20 0 0 0.90 8.20 20 0 0 18.80 6.70 -20 0 0 -4.30 11.00 20 0 0 13.40 8.70 -22 0 0 411.36 45.50 22 0 0 517.45 50.09 22 0 0 550.54 44.10 -22 0 0 484.05 39.50 22 0 0 492.35 30.20 -22 0 0 473.05 32.90 22 0 0 503.05 40.80 -22 0 0 480.95 42.70 -22 0 0 468.65 45.30 22 0 0 411.56 26.30 22 0 0 536.25 44.00 -24 0 0 5.20 15.60 24 0 0 0.50 5.50 24 0 0 17.10 15.80 -24 0 0 -8.20 9.70 24 0 0 4.10 5.10 -24 0 0 -10.90 7.30 24 0 0 6.70 10.10 24 0 0 -7.00 7.10 24 0 0 2.10 17.20 -24 0 0 8.90 9.90 -24 0 0 21.80 12.80 26 0 0 17.00 8.00 -26 0 0 23.60 11.70 -26 0 0 18.10 14.10 -26 0 0 45.60 12.70 26 0 0 50.89 21.30 -26 0 0 34.30 17.40 26 0 0 -1.00 19.00 26 0 0 10.40 9.10 26 0 0 26.50 6.90 -26 0 0 29.90 16.20 -26 0 0 21.20 6.70 28 0 0 8.80 9.00 -28 0 0 21.20 13.10 28 0 0 26.80 16.80 28 0 0 10.00 24.70 28 0 0 -2.30 13.20 -28 0 0 -11.70 15.10 -28 0 0 20.80 12.10 28 0 0 28.10 9.50 -28 0 0 50.59 23.10 28 0 0 -42.20 37.10 28 0 0 22.20 6.30 -28 0 0 9.60 13.40 -30 0 0 -21.50 16.10 30 0 0 -12.90 31.30 -30 0 0 10.90 7.40 30 0 0 5.40 15.70 -30 0 0 2.70 6.20 30 0 0 24.50 12.40 -30 0 0 -12.90 16.20 -30 0 0 30.30 24.80 30 0 0 -8.60 13.80 30 0 0 -1.90 26.40 -30 0 0 -6.00 15.30 -30 0 0 13.00 14.30 30 0 0 -4.10 5.20 30 0 0 0.80 8.50 -32 0 0 17.20 8.70 -32 0 0 23.60 9.20 -32 0 0 67.69 21.70 32 0 0 29.90 9.60 32 0 0 40.30 8.60 -32 0 0 10.40 28.90 -32 0 0 21.70 6.70 32 0 0 36.60 21.90 -32 0 0 30.40 22.90 32 0 0 63.79 15.20 32 0 0 32.00 7.90 32 0 0 116.99 49.10 -32 0 0 55.09 20.70 32 0 0 28.40 8.50 -32 0 0 29.00 13.10 32 0 0 49.50 21.40 -34 0 0 5.70 6.20 34 0 0 6.00 6.20 -34 0 0 -33.30 32.60 34 0 0 7.30 6.80 34 0 0 1.70 6.80 34 0 0 15.10 19.50 -34 0 0 3.00 5.50 -34 0 0 -19.80 25.00 34 0 0 15.00 8.60 34 0 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156.68 17.30 17 -3 0 213.08 26.50 -17 -3 0 143.49 40.50 17 -3 0 154.68 37.60 -17 3 0 161.18 18.40 17 3 0 212.08 27.60 -17 3 0 171.28 18.60 -17 3 0 153.68 24.10 17 3 0 152.68 38.50 17 3 0 157.58 29.20 17 3 0 156.38 36.70 -17 3 0 112.39 25.40 -19 -3 0 83.59 14.00 -19 -3 0 58.99 29.20 19 -3 0 19.80 26.30 19 -3 0 76.79 24.20 19 3 0 88.39 33.20 -19 3 0 66.39 11.60 -19 3 0 35.90 24.70 19 3 0 73.79 26.50 -19 3 0 67.39 20.00 -19 3 0 90.79 14.50 -19 3 0 70.99 19.10 19 3 0 79.29 14.90 19 3 0 80.19 12.10 19 3 0 54.19 17.20 19 3 0 66.99 26.40 21 -3 0 160.88 17.40 21 -3 0 144.89 33.80 -21 -3 0 245.38 24.30 21 -3 0 195.18 17.30 -21 -3 0 167.68 29.80 -21 -3 0 214.88 26.60 21 -3 0 211.28 52.59 -21 -3 0 134.79 45.40 21 3 0 172.68 34.30 -21 3 0 211.88 17.90 21 3 0 185.68 33.10 -21 3 0 219.78 29.80 21 3 0 203.08 18.60 21 3 0 111.59 41.70 21 3 0 202.08 17.00 -21 3 0 221.98 23.20 21 3 0 130.09 37.90 -21 3 0 136.39 38.00 23 -3 0 102.99 14.10 -23 -3 0 109.59 43.50 -23 -3 0 87.59 21.90 -23 -3 0 82.69 19.30 23 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145.49 32.70 -6 -4 0 130.59 40.40 6 -4 0 121.69 41.20 -6 -4 0 133.29 23.10 -6 -4 0 131.69 21.90 6 -4 0 204.48 40.30 -6 -4 0 123.89 33.60 -6 4 0 132.09 26.00 6 4 0 153.28 35.20 -6 4 0 169.38 41.90 6 4 0 189.28 32.20 -6 4 0 131.09 21.80 6 4 0 125.19 34.50 6 4 0 142.49 29.80 -8 -4 0 221.78 24.10 8 -4 0 255.27 37.90 8 -4 0 242.78 47.70 8 -4 0 249.78 22.90 8 -4 0 226.68 50.09 -8 -4 0 138.99 46.00 8 -4 0 266.87 48.00 -8 -4 0 198.28 27.00 -8 -4 0 196.08 42.90 -8 -4 0 152.48 24.00 -8 4 0 211.88 44.40 8 4 0 186.18 32.60 -8 4 0 237.38 30.80 -8 4 0 208.28 28.20 8 4 0 189.48 36.20 8 4 0 155.68 40.20 8 4 0 211.88 39.80 8 4 0 201.48 35.20 -10 -4 0 181.08 26.70 10 -4 0 207.08 39.90 10 -4 0 233.58 22.10 -10 -4 0 239.38 25.40 10 -4 0 266.57 63.59 -10 -4 0 209.78 25.10 -10 -4 0 127.69 40.20 10 -4 0 238.38 45.70 10 -4 0 240.58 23.40 10 -4 0 173.68 28.80 -10 4 0 235.38 30.00 10 4 0 219.58 46.10 10 4 0 184.88 35.60 10 4 0 220.68 42.80 -10 4 0 241.78 32.50 10 4 0 191.48 32.70 -12 -4 0 15.90 10.10 12 -4 0 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-2.00 2.90 16 -4 -9 3.30 6.00 16 4 -9 6.30 4.70 16 4 -9 3.00 3.20 -16 4 9 3.60 5.70 16 4 -9 -0.90 7.90 -16 4 9 1.00 4.00 -16 4 9 4.80 4.40 14 -4 -9 -3.10 6.60 14 4 -9 0.20 3.40 14 4 -9 -0.70 3.40 -14 4 9 -2.40 3.80 14 4 -9 2.60 7.10 -14 4 9 -1.00 5.10 -14 4 9 1.00 3.60 12 -4 -9 6.90 6.10 -12 4 9 9.60 5.70 12 4 -9 11.00 4.70 -12 4 9 13.10 4.90 12 4 -9 16.20 7.70 -12 4 9 15.40 5.60 12 4 -9 9.70 6.10 10 -4 -9 -4.20 4.40 -10 4 9 1.70 4.00 10 4 -9 -2.10 2.70 -10 4 9 2.70 5.20 -10 4 9 15.20 8.50 10 4 -9 12.70 7.40 10 4 -9 4.70 4.00 8 -4 -9 6.80 7.60 8 4 -9 -6.40 3.70 -8 4 9 -1.50 5.20 -8 4 9 -3.50 6.10 8 4 -9 5.50 6.80 -8 4 9 5.50 4.20 8 4 -9 -0.90 3.70 -6 -4 9 1.20 2.00 6 -4 -9 -3.10 5.10 -6 4 9 5.50 4.40 6 4 -9 -2.30 3.50 -6 4 9 1.30 5.20 -6 4 9 0.20 6.40 6 4 -9 2.90 6.60 6 4 -9 -6.00 3.40 -4 -4 9 0.70 2.00 4 -4 -9 -0.10 7.10 4 4 -9 5.40 4.30 -4 4 9 2.30 5.60 4 4 -9 9.00 6.90 -4 4 9 -0.10 5.30 -4 4 9 12.40 5.00 4 4 -9 -3.50 3.50 -2 -4 9 0.50 1.90 2 -4 -9 3.90 4.60 2 4 -9 -0.10 4.00 -2 4 9 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14.70 9.10 0 0 10 4.50 3.10 0 0 -10 4.60 5.40 0 0 -10 4.40 5.70 2 0 10 1.80 5.50 -2 0 -10 -2.30 5.20 4 0 10 5.00 4.80 -4 0 -10 -1.70 5.70 -4 0 -10 0.80 6.00 4 0 10 -0.60 2.60 -6 0 -10 39.90 9.80 -6 0 -10 32.90 7.50 6 0 10 43.50 8.40 -8 0 -10 4.80 7.80 8 0 10 3.40 3.30 8 0 10 -2.20 4.10 -8 0 -10 8.30 6.00 -8 0 -10 5.30 6.60 10 0 10 2.10 4.40 -10 0 -10 2.70 5.40 10 0 10 4.20 2.80 -10 0 -10 1.80 7.00 -12 0 -10 14.50 7.80 -12 0 -10 13.00 5.90 14 0 10 -1.20 5.00 -14 0 -10 7.40 5.00 14 0 10 -1.40 2.10 -16 0 -10 5.40 4.30 16 0 10 -1.70 3.10 16 0 10 0.00 4.40 -18 0 -10 3.00 3.10 18 0 10 -1.80 1.70 -20 0 -10 3.60 3.80 20 0 10 2.80 2.20 -27 -1 10 1.20 1.80 27 1 -10 -3.10 7.00 -27 1 10 1.10 4.20 27 1 -10 -2.80 2.70 -27 1 10 0.40 3.50 25 -1 -10 0.50 3.00 -25 -1 10 1.00 2.50 25 1 -10 3.40 4.10 -25 1 10 4.50 4.10 -25 1 10 -0.60 3.80 25 1 -10 10.10 6.10 23 -1 -10 -6.40 7.70 -23 -1 10 1.60 2.40 23 -1 -10 1.40 3.30 -23 1 10 7.20 4.90 -23 1 10 1.40 3.80 23 1 -10 -5.10 4.50 23 1 -10 1.60 3.60 21 -1 -10 2.30 6.30 21 -1 -10 8.60 4.90 -21 -1 10 6.00 4.50 21 1 -10 10.80 4.40 -21 1 10 7.80 3.60 21 1 -10 12.30 9.90 -21 1 10 16.40 5.60 19 -1 -10 1.80 3.70 19 -1 -10 0.90 6.30 -19 -1 10 4.50 4.00 19 1 -10 -2.50 5.20 19 1 -10 2.70 4.00 -19 1 10 6.30 4.30 -19 1 10 6.90 4.40 -17 -1 10 1.90 2.70 17 -1 -10 13.00 9.00 17 -1 -10 9.10 6.40 17 1 -10 6.90 5.60 -17 1 10 3.50 3.00 -17 1 10 5.30 4.80 17 1 -10 8.50 4.80 -15 -1 10 0.30 2.20 15 -1 -10 2.70 7.50 15 -1 -10 -2.10 3.90 15 1 -10 -0.60 6.70 -15 1 10 -2.20 4.10 -15 1 10 2.90 5.90 15 1 -10 -0.10 3.90 -13 -1 10 0.10 2.00 13 -1 -10 1.30 5.60 13 1 -10 7.80 6.40 -13 1 10 3.80 4.90 13 1 -10 8.80 5.20 -13 1 10 -0.80 5.30 -11 -1 10 7.50 4.30 11 -1 -10 25.10 8.10 -11 1 10 11.00 6.40 11 1 -10 15.90 8.00 11 1 -10 18.90 8.70 -11 1 10 16.30 7.20 9 -1 -10 -6.50 4.90 -9 -1 10 2.60 3.30 9 1 -10 1.90 6.10 9 1 -10 4.40 7.60 -9 1 10 -6.50 3.50 -9 1 10 -2.30 4.40 -7 -1 10 -1.00 1.90 -7 -1 10 0.80 8.20 7 -1 -10 -4.70 4.70 -7 1 10 -1.90 5.70 -7 1 10 -3.90 3.70 7 1 -10 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10 0.90 4.10 -9 -1 -10 9.10 5.50 -9 1 -10 13.30 5.50 9 1 10 -0.20 4.30 9 1 10 9.30 5.00 -9 1 -10 11.60 6.60 11 -1 10 2.30 3.20 -11 -1 -10 3.30 7.60 -11 -1 -10 6.10 4.20 -11 1 -10 -7.00 9.50 -11 1 -10 -3.70 3.60 11 1 10 -8.90 5.00 11 1 10 4.50 3.70 -11 1 -10 -5.70 5.30 13 -1 10 -3.00 2.50 -13 -1 -10 10.20 8.30 -13 -1 -10 -3.90 3.20 -13 1 -10 -0.20 3.50 -13 1 -10 -12.20 9.70 -13 1 -10 -7.60 4.10 13 1 10 -4.10 3.00 13 1 10 -1.30 5.10 15 -1 10 2.30 3.10 -15 -1 -10 6.60 5.20 -15 -1 -10 -1.90 9.30 -15 1 -10 -4.10 5.10 15 1 10 1.30 3.60 -15 1 -10 10.80 4.50 15 1 10 1.30 5.30 17 -1 10 1.80 2.60 -17 -1 -10 3.60 3.50 -17 1 -10 -0.30 5.10 17 1 10 2.30 5.60 -17 1 -10 8.90 4.10 19 -1 10 0.10 1.80 -19 -1 -10 2.90 3.40 19 1 10 2.40 3.60 -19 1 -10 17.70 6.70 24 -2 -10 7.70 4.00 -24 -2 10 5.50 2.70 24 2 -10 6.40 3.50 -24 2 10 12.10 6.20 22 -2 -10 -1.10 2.70 -22 -2 10 -1.00 1.70 22 2 -10 -0.10 2.60 -22 2 10 -0.90 3.80 20 -2 -10 -3.30 6.50 -20 -2 10 4.90 3.40 20 -2 -10 9.10 5.00 20 2 -10 6.30 4.80 -20 2 10 14.70 5.80 18 -2 -10 7.20 4.10 -18 -2 10 -0.20 2.70 18 -2 -10 -5.70 6.50 18 2 -10 0.80 2.80 -18 2 10 2.00 4.10 -16 -2 10 1.70 3.30 16 -2 -10 6.10 4.10 16 -2 -10 -1.70 5.70 -16 2 10 10.10 5.00 16 2 -10 -2.10 2.60 -14 -2 10 1.50 2.40 14 -2 -10 4.50 4.50 14 -2 -10 -1.00 6.00 14 2 -10 -1.80 2.80 -14 2 10 3.70 4.90 -12 -2 10 2.80 2.40 12 -2 -10 4.30 6.10 12 -2 -10 5.60 4.40 12 2 -10 1.90 13.70 -12 2 10 6.90 6.20 -12 2 10 8.40 5.50 12 2 -10 0.90 2.80 10 -2 -10 3.80 4.20 10 -2 -10 5.50 6.90 -10 -2 10 -1.90 2.10 10 2 -10 -7.90 12.80 -10 2 10 5.00 5.30 -10 2 10 0.80 5.70 10 2 -10 1.30 3.10 8 -2 -10 0.40 3.90 8 -2 -10 1.10 7.00 -8 -2 10 3.30 3.40 8 2 -10 -1.00 2.70 -8 2 10 6.40 5.20 -8 2 10 14.50 6.00 6 -2 -10 4.90 4.60 -6 -2 10 3.00 1.90 6 -2 -10 3.60 6.70 6 2 -10 1.00 3.10 -6 2 10 12.70 5.80 6 2 -10 -4.10 10.50 -6 2 10 14.40 4.80 -4 -2 10 2.90 2.80 4 -2 -10 2.50 6.10 4 -2 -10 4.60 4.40 4 2 -10 0.20 3.30 -4 2 10 4.50 5.30 -4 2 10 12.90 4.20 4 2 -10 10.40 12.00 -2 -2 10 3.30 3.40 2 -2 -10 2.40 7.20 2 -2 -10 -2.30 3.60 -2 2 10 9.30 5.70 -2 2 10 15.30 5.40 2 2 -10 2.40 3.10 2 2 -10 1.70 11.60 0 -2 -10 10.10 5.20 0 -2 -10 11.90 8.20 0 2 10 20.40 6.40 0 2 10 19.50 6.50 0 2 -10 21.50 12.20 -2 -2 -10 16.50 5.60 2 -2 10 7.70 3.60 -2 -2 -10 8.60 8.30 -2 2 -10 23.50 11.60 2 2 10 11.60 5.40 -2 2 -10 7.40 3.40 2 2 10 13.60 6.50 -4 -2 -10 1.30 3.50 -4 -2 -10 3.30 8.00 4 -2 10 4.50 3.30 4 2 10 16.60 6.40 4 2 10 11.00 4.60 -4 2 -10 -0.20 10.90 -4 2 -10 6.10 2.90 6 -2 10 -1.90 3.30 -6 -2 -10 -3.30 3.10 -6 -2 -10 3.70 6.00 -6 2 -10 -20.80 10.50 -6 2 -10 -1.50 3.20 6 2 10 3.90 4.00 -8 -2 -10 6.20 4.80 -8 -2 -10 -0.70 6.90 8 -2 10 1.20 3.00 -8 2 -10 4.30 3.30 -8 2 -10 7.10 12.10 8 2 10 10.60 5.80 -10 -2 -10 0.20 3.00 10 -2 10 0.40 2.60 -10 -2 -10 8.60 6.50 -10 2 -10 0.60 3.20 10 2 10 1.40 4.80 -12 -2 -10 -7.10 5.20 -12 -2 -10 0.90 3.20 12 -2 10 3.90 2.80 12 2 10 1.80 3.60 -12 2 -10 1.30 2.80 14 -2 10 3.10 2.00 -14 -2 -10 4.40 3.70 -14 -2 -10 -6.60 8.70 14 2 10 12.00 4.20 -14 2 -10 -0.70 2.90 -16 -2 -10 6.90 3.30 16 -2 10 1.60 1.90 16 2 10 3.10 3.10 -16 2 -10 0.50 2.50 -19 -3 10 2.50 2.60 -19 3 10 -1.10 3.60 19 3 -10 0.10 2.20 17 -3 -10 8.60 9.30 -17 3 10 6.90 6.10 15 -3 -10 -3.20 5.10 15 -3 -10 3.50 2.70 -15 -3 10 1.00 1.70 15 3 -10 0.60 2.70 -15 3 10 1.40 3.60 -15 3 10 8.20 4.20 13 -3 -10 -0.40 5.90 -13 -3 10 0.30 2.00 13 -3 -10 -3.20 2.90 -13 3 10 -6.10 4.10 -13 3 10 0.10 3.60 13 3 -10 -0.20 2.90 11 -3 -10 6.60 4.80 11 -3 -10 6.90 6.50 -11 -3 10 4.60 2.80 -11 3 10 4.60 5.50 -11 3 10 14.70 6.30 11 3 -10 5.70 3.80 9 -3 -10 3.40 3.00 -9 -3 10 1.40 2.10 9 -3 -10 -5.30 3.80 -9 3 10 -1.80 4.70 -9 3 10 -1.00 3.50 9 3 -10 -0.50 4.00 9 3 -10 -6.40 5.70 -7 -3 10 0.30 2.50 7 -3 -10 -0.10 6.00 7 -3 -10 -4.10 3.10 -7 3 10 -1.00 6.50 -7 3 10 -4.60 3.40 7 3 -10 -2.60 4.00 5 -3 -10 -1.20 5.40 5 -3 -10 -0.10 3.30 -5 -3 10 -1.50 2.30 -5 3 10 5.70 3.90 -5 3 10 4.00 8.30 5 3 -10 -0.10 3.80 5 3 -10 -3.70 4.30 3 -3 -10 7.00 4.30 3 -3 -10 -6.40 6.20 -3 -3 10 2.00 2.60 3 3 -10 1.20 4.50 3 3 -10 3.00 4.10 -3 3 10 11.90 9.30 -3 3 10 10.90 3.90 -1 -3 10 0.50 2.00 1 -3 -10 1.10 3.20 1 -3 -10 3.30 6.00 -1 3 10 12.10 6.20 -1 3 10 6.10 3.60 1 3 -10 0.60 3.00 -1 -3 -10 11.00 6.80 1 3 10 15.10 5.40 1 3 10 17.20 3.90 -3 -3 -10 -0.20 4.10 -3 -3 -10 2.00 2.80 3 -3 10 1.30 1.90 3 3 10 -4.50 3.70 -3 3 -10 -0.80 2.40 3 3 10 -0.20 3.50 -5 -3 -10 -3.60 4.30 5 -3 10 -1.00 1.70 -5 -3 -10 2.40 2.90 5 3 10 1.20 3.80 -5 3 -10 2.70 2.70 -7 -3 -10 2.00 4.70 7 -3 10 -1.50 1.50 -7 3 -10 2.00 2.70 7 3 10 -1.50 4.20 7 3 10 8.70 3.60 9 -3 10 -0.70 1.10 -9 -3 -10 5.50 4.60 -9 3 -10 -2.20 2.10 9 3 10 -3.60 3.10 -14 0 11 0.00 1.90 14 0 -11 -5.50 3.10 14 0 -11 8.90 5.70 12 0 -11 -5.00 4.50 12 0 -11 2.90 3.40 -12 0 11 1.20 3.60 10 0 -11 -1.90 4.30 -10 0 11 -0.50 2.50 10 0 -11 6.80 5.50 8 0 -11 -3.30 3.70 -8 0 11 0.00 2.70 8 0 -11 -3.90 5.10 6 0 -11 -0.60 5.30 6 0 -11 -5.60 3.40 -6 0 11 -1.90 2.20 -4 0 11 6.20 3.60 4 0 -11 15.00 5.80 4 0 -11 8.80 7.00 2 0 -11 15.60 6.50 -2 0 11 7.50 4.10 2 0 -11 8.20 6.40 0 0 11 2.60 3.00 0 0 -11 4.50 7.50 0 0 -11 15.50 5.30 -2 0 -11 4.20 4.20 -2 0 -11 -3.10 5.10 2 0 11 2.30 2.90 -4 0 -11 7.10 3.50 -4 0 -11 -7.60 4.60 4 0 11 4.00 2.70 -13 1 11 38.00 6.60 11 -1 -11 -1.70 5.20 -11 -1 11 1.90 2.10 11 -1 -11 3.60 4.00 11 1 -11 5.50 6.60 11 1 -11 13.20 7.60 -11 1 11 1.70 3.90 -9 -1 11 0.50 2.00 9 -1 -11 -1.80 4.20 9 -1 -11 1.30 4.10 -9 1 11 -0.90 3.20 9 1 -11 -7.70 6.40 9 1 -11 2.30 5.00 7 -1 -11 7.90 5.90 -7 -1 11 3.80 3.40 -7 1 11 15.60 4.80 7 1 -11 -0.70 7.50 7 1 -11 16.30 6.20 5 -1 -11 10.60 6.20 5 -1 -11 21.40 6.30 5 1 -11 14.40 4.70 -5 1 11 14.00 5.10 5 1 -11 9.40 7.00 3 -1 -11 4.60 6.90 -3 -1 11 -1.80 2.70 -3 1 11 2.70 3.70 3 1 -11 -5.00 7.70 3 1 -11 -8.00 6.70 1 -1 -11 4.40 3.70 1 -1 -11 -0.70 5.50 -1 1 11 -2.00 3.20 1 1 -11 3.80 7.90 1 1 -11 -5.00 5.80 1 -1 11 7.90 2.70 -1 -1 -11 12.10 6.10 -1 -1 -11 14.10 5.10 1 1 11 17.30 4.20 -1 1 -11 14.70 6.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 44563 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' 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_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O4 0.72514(10) 1.1336(8) -0.0677(5) 0.0567(12) Uani d . . . 1 . . H H47 0.718701 1.221291 -0.144954 0.085 Uiso d U . R 1 . . H H48 0.746357 1.17044 -0.053674 0.085 Uiso d U . R 1 . . O O1 0.71480(9) 0.7512(7) 0.0229(4) 0.0423(10) Uani d . . . 1 . . H H45 0.716513 0.874501 0.000966 0.063 Uiso calc U . R 1 . . O O2 0.66225(11) 0.1329(7) 0.5432(5) 0.0568(13) Uani d . . . 1 . . O O3 0.70665(9) 0.4962(7) 0.7751(4) 0.0438(10) Uani d . . . 1 . . H H46 0.709895 0.555777 0.856999 0.066 Uiso calc U . R 1 . . C C1 0.69661(13) 0.7330(11) 0.1453(6) 0.0405(15) Uani d . . . 1 . . H H1 0.680394 0.836638 0.132036 0.049 Uiso calc U . R 1 . . C C2 0.68256(15) 0.5233(11) 0.1366(6) 0.0518(18) Uani d . . . 1 . . H H44 0.698417 0.419831 0.134306 0.062 Uiso calc U . R 1 . . H H43 0.669504 0.512073 0.042926 0.062 Uiso calc U . R 1 . . C C3 0.66430(15) 0.4777(12) 0.2671(6) 0.0501(17) Uani d . . . 1 . . H H42 0.64698 0.570284 0.263376 0.06 Uiso calc U . R 1 . . H H3 0.656815 0.336257 0.259468 0.06 Uiso calc U . R 1 . . C C4 0.68331(13) 0.5056(10) 0.4134(6) 0.0378(13) Uani d . . . 1 . . C C5 0.66753(13) 0.4985(9) 0.5601(6) 0.0361(13) Uani d . . . 1 . . C C6 0.66083(12) 0.2846(10) 0.6158(6) 0.0399(14) Uani d . . . 1 . . C C7 0.64747(12) 0.2860(9) 0.7622(6) 0.0379(13) Uani d . . . 1 . . H H10 0.659283 0.382658 0.829524 0.046 Uiso calc U . R 1 . . C C8 0.61527(13) 0.3694(10) 0.7368(6) 0.0388(14) Uani d . . . 1 . . C C9 0.60561(13) 0.3367(9) 0.8949(6) 0.0381(14) Uani d . . . 1 . . H H14 0.616365 0.440482 0.960322 0.046 Uiso calc U . R 1 . . C C10 0.57267(13) 0.3515(10) 0.9214(6) 0.0411(14) Uani d . . . 1 . . H H15 0.561533 0.250943 0.854522 0.049 Uiso calc U . R 1 . . C C11 0.56862(13) 0.2924(11) 1.0792(6) 0.0443(15) Uani d . . . 1 . . H H16 0.576591 0.382845 1.154506 0.053 Uiso calc U . R 1 . . C C12 0.55524(13) 0.1294(11) 1.1234(6) 0.0437(15) Uani d . . . 1 . . H H27 0.546428 0.040439 1.049227 0.052 Uiso calc U . R 1 . . C C13 0.55279(15) 0.0723(10) 1.2831(6) 0.0472(16) Uani d . . . 1 . . H H20 0.564221 0.17722 1.344693 0.057 Uiso calc U . R 1 . . C C14 0.52079(14) 0.0795(11) 1.3274(7) 0.0486(17) Uani d . . . 1 . . H H24 0.521718 0.047878 1.435718 0.058 Uiso calc U . R 1 . . C C15 0.50756(15) 0.2911(13) 1.3059(8) 0.065(2) Uani d . . . 1 . . H H26 0.488543 0.296814 1.349434 0.098 Uiso calc U . R 1 . . H H25 0.504357 0.321551 1.199709 0.098 Uiso calc U . R 1 . . H H2 0.521243 0.391286 1.354604 0.098 Uiso calc U . R 1 . . C C16 0.70953(14) 0.3522(11) 0.4274(7) 0.0500(16) Uani d . . . 1 . . H H5 0.72478 0.396394 0.364353 0.075 Uiso calc U . R 1 . . H H4 0.702284 0.217103 0.395916 0.075 Uiso calc U . R 1 . . H H6 0.718083 0.346282 0.530804 0.075 Uiso calc U . R 1 . . C C17 0.63640(13) 0.6047(10) 0.5473(6) 0.0407(14) Uani d . . . 1 . . H H8 0.639253 0.750695 0.525856 0.049 Uiso calc U . R 1 . . H H7 0.624183 0.545686 0.46146 0.049 Uiso calc U . R 1 . . C C18 0.61887(14) 0.5879(10) 0.6846(6) 0.0424(15) Uani d . . . 1 . . H H9 0.629216 0.667837 0.766445 0.051 Uiso calc U . R 1 . . H H35 0.598937 0.648455 0.660976 0.051 Uiso calc U . R 1 . . C C19 0.64501(15) 0.0877(11) 0.8450(7) 0.0521(17) Uani d . . . 1 . . H H31 0.663661 0.05711 0.907212 0.062 Uiso calc U . R 1 . . H H11 0.640401 -0.026514 0.775389 0.062 Uiso calc U . R 1 . . C C20 0.61918(14) 0.1255(11) 0.9417(6) 0.0445(15) Uani d . . . 1 . . H H12 0.626593 0.126358 1.048075 0.053 Uiso calc U . R 1 . . H H13 0.603992 0.017383 0.925064 0.053 Uiso calc U . R 1 . . C C21 0.56843(19) -0.1309(13) 1.3181(8) 0.071(2) Uani d . . . 1 . . H H18 0.589453 -0.118811 1.301252 0.107 Uiso calc U . R 1 . . H H17 0.559112 -0.236921 1.253409 0.107 Uiso calc U . R 1 . . H H19 0.566736 -0.166938 1.421858 0.107 Uiso calc U . R 1 . . C C22 0.49998(17) -0.0757(14) 1.2470(8) 0.068(2) Uani d . . . 1 . . H H23 0.496703 -0.039759 1.141741 0.101 Uiso calc U . R 1 . . H H22 0.480945 -0.075753 1.290482 0.101 Uiso calc U . R 1 . . H H21 0.50894 -0.211316 1.257032 0.101 Uiso calc U . R 1 . . C C23 0.55958(15) 0.5594(11) 0.8859(7) 0.0543(18) Uani d . . . 1 . . H H29 0.57167 0.663201 0.940776 0.082 Uiso calc U . R 1 . . H H30 0.539239 0.564603 0.914774 0.082 Uiso calc U . R 1 . . H H28 0.559335 0.585195 0.779302 0.082 Uiso calc U . R 1 . . C C24 0.59581(14) 0.2440(12) 0.6245(6) 0.0486(16) Uani d . . . 1 . . H H34 0.604661 0.24218 0.529858 0.073 Uiso calc U . R 1 . . H H32 0.575945 0.304523 0.610138 0.073 Uiso calc U . R 1 . . H H33 0.594317 0.10457 0.661304 0.073 Uiso calc U . R 1 . . C C25 0.68920(13) 0.6255(10) 0.6728(6) 0.0389(14) Uani d . . . 1 . . H H41 0.677277 0.720948 0.729376 0.047 Uiso calc U . R 1 . . C C26 0.70921(13) 0.7493(10) 0.5767(5) 0.0404(14) Uani d . . . 1 . . H H36 0.709732 0.894142 0.606723 0.048 Uiso calc U . R 1 . . H H40 0.729745 0.695339 0.586906 0.048 Uiso calc U . R 1 . . C C27 0.69539(13) 0.7263(9) 0.4190(6) 0.0366(14) Uani d . . . 1 . . H H39 0.677831 0.819322 0.406915 0.044 Uiso calc U . R 1 . . C C28 0.71423(13) 0.7707(11) 0.2921(5) 0.0396(14) Uani d . . . 1 . . H H38 0.72092 0.914135 0.297514 0.047 Uiso calc U . R 1 . . H H37 0.732061 0.682598 0.301019 0.047 Uiso calc U . R 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 0.057(3) 0.046(3) 0.066(3) -0.001(2) -0.001(2) 0.014(2) O1 0.055(2) 0.038(3) 0.034(2) 0.001(2) 0.0047(18) -0.0014(19) O2 0.074(3) 0.034(3) 0.066(3) -0.010(2) 0.023(2) -0.016(2) O3 0.057(3) 0.037(3) 0.036(2) 0.001(2) -0.0060(19) 0.0013(19) C1 0.048(3) 0.047(4) 0.027(3) 0.001(3) 0.003(2) -0.001(3) C2 0.061(4) 0.059(5) 0.034(3) -0.012(4) 0.002(3) -0.008(3) C3 0.059(4) 0.056(5) 0.035(3) -0.005(4) 0.004(3) -0.008(3) C4 0.048(3) 0.031(4) 0.035(3) -0.001(3) 0.004(2) -0.007(3) C5 0.045(3) 0.029(3) 0.034(3) 0.004(3) 0.003(2) -0.005(2) C6 0.041(3) 0.032(4) 0.047(3) -0.003(3) 0.008(3) -0.002(3) C7 0.045(3) 0.032(4) 0.038(3) 0.002(3) 0.005(2) -0.001(3) C8 0.040(3) 0.039(4) 0.036(3) -0.004(3) -0.002(2) -0.002(3) C9 0.048(3) 0.031(4) 0.036(3) -0.001(3) 0.003(2) -0.004(2) C10 0.049(4) 0.037(4) 0.037(3) 0.001(3) 0.005(3) 0.001(3) C11 0.048(3) 0.044(4) 0.040(3) 0.005(3) 0.003(3) -0.006(3) C12 0.047(3) 0.047(4) 0.036(3) -0.003(3) 0.001(3) 0.000(3) C13 0.064(4) 0.039(4) 0.039(3) -0.002(3) 0.002(3) 0.003(3) C14 0.054(4) 0.051(5) 0.041(3) 0.001(3) 0.002(3) 0.007(3) C15 0.056(4) 0.073(6) 0.069(5) 0.010(4) 0.014(4) 0.016(4) C16 0.056(4) 0.037(4) 0.058(4) 0.001(3) 0.012(3) 0.002(3) C17 0.047(3) 0.034(4) 0.041(3) 0.004(3) 0.005(3) 0.005(3) C18 0.050(4) 0.037(4) 0.040(3) 0.005(3) 0.001(3) -0.001(3) C19 0.056(4) 0.037(4) 0.064(4) 0.002(3) 0.014(3) 0.008(3) C20 0.050(4) 0.038(4) 0.046(3) -0.002(3) 0.008(3) 0.006(3) C21 0.090(6) 0.067(6) 0.056(4) 0.021(5) 0.006(4) 0.019(4) C22 0.066(5) 0.085(7) 0.051(4) -0.022(4) 0.001(4) -0.004(4) C23 0.057(4) 0.051(5) 0.055(4) 0.009(4) 0.008(3) 0.005(3) C24 0.056(4) 0.052(4) 0.037(3) -0.013(3) 0.001(3) -0.009(3) C25 0.047(3) 0.032(3) 0.035(3) 0.007(3) -0.003(2) 0.010(3) C26 0.060(4) 0.028(3) 0.032(3) -0.007(3) -0.005(3) 0.000(3) C27 0.045(3) 0.034(4) 0.030(3) 0.001(3) 0.003(2) -0.001(2) C28 0.050(3) 0.037(4) 0.031(3) 0.001(3) 0.000(2) -0.001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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_ _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 H47 O4 H48 . . 100.1 ? C1 O1 H45 . . 109.5 ? C25 O3 H46 . . 109.5 ? O1 C1 C28 . . 111.8(5) ? O1 C1 C2 . . 107.5(5) ? C28 C1 C2 . . 112.3(5) ? O1 C1 H1 . . 108.3 ? C28 C1 H1 . . 108.3 ? C2 C1 H1 . . 108.3 ? C1 C2 C3 . . 113.0(5) ? C1 C2 H44 . . 109.0 ? C3 C2 H44 . . 109.0 ? C1 C2 H43 . . 109.0 ? C3 C2 H43 . . 109.0 ? H44 C2 H43 . . 107.8 ? C4 C3 C2 . . 110.3(5) ? C4 C3 H42 . . 109.6 ? C2 C3 H42 . . 109.6 ? C4 C3 H3 . . 109.6 ? C2 C3 H3 . . 109.6 ? H42 C3 H3 . . 108.1 ? C3 C4 C27 . . 108.0(5) ? C3 C4 C16 . . 110.9(5) ? C27 C4 C16 . . 110.0(5) ? C3 C4 C5 . . 118.1(5) ? C27 C4 C5 . . 100.8(4) ? C16 C4 C5 . . 108.4(5) ? C6 C5 C17 . . 103.3(5) ? C6 C5 C4 . . 115.2(5) ? C17 C5 C4 . . 113.7(5) ? C6 C5 C25 . . 113.6(5) ? C17 C5 C25 . . 108.0(5) ? C4 C5 C25 . . 103.1(5) ? O2 C6 C7 . . 122.2(6) ? O2 C6 C5 . . 124.0(5) ? C7 C6 C5 . . 113.0(5) ? C6 C7 C19 . . 119.0(5) ? C6 C7 C8 . . 108.6(5) ? C19 C7 C8 . . 105.4(5) ? C6 C7 H10 . . 107.8 ? C19 C7 H10 . . 107.8 ? C8 C7 H10 . . 107.8 ? C24 C8 C18 . . 112.0(5) ? C24 C8 C9 . . 110.3(5) ? C18 C8 C9 . . 117.7(5) ? C24 C8 C7 . . 112.5(5) ? C18 C8 C7 . . 104.6(5) ? C9 C8 C7 . . 99.0(4) ? C10 C9 C8 . . 119.9(5) ? C10 C9 C20 . . 112.1(5) ? C8 C9 C20 . . 103.7(5) ? C10 C9 H14 . . 106.8 ? C8 C9 H14 . . 106.8 ? C20 C9 H14 . . 106.8 ? C11 C10 C23 . . 110.7(5) ? C11 C10 C9 . . 109.8(5) ? C23 C10 C9 . . 113.0(5) ? C11 C10 H15 . . 107.7 ? C23 C10 H15 . . 107.7 ? C9 C10 H15 . . 107.7 ? C12 C11 C10 . . 126.9(6) ? C12 C11 H16 . . 116.6 ? C10 C11 H16 . . 116.6 ? C11 C12 C13 . . 125.0(6) ? C11 C12 H27 . . 117.5 ? C13 C12 H27 . . 117.5 ? C12 C13 C21 . . 109.9(5) ? C12 C13 C14 . . 113.5(5) ? C21 C13 C14 . . 113.6(6) ? C12 C13 H20 . . 106.4 ? C21 C13 H20 . . 106.4 ? C14 C13 H20 . . 106.4 ? C15 C14 C22 . . 109.5(6) ? C15 C14 C13 . . 111.3(6) ? C22 C14 C13 . . 114.0(6) ? C15 C14 H24 . . 107.2 ? C22 C14 H24 . . 107.2 ? C13 C14 H24 . . 107.2 ? C14 C15 H26 . . 109.5 ? C14 C15 H25 . . 109.5 ? H26 C15 H25 . . 109.5 ? C14 C15 H2 . . 109.5 ? H26 C15 H2 . . 109.5 ? H25 C15 H2 . . 109.5 ? C4 C16 H5 . . 109.5 ? C4 C16 H4 . . 109.5 ? H5 C16 H4 . . 109.5 ? C4 C16 H6 . . 109.5 ? H5 C16 H6 . . 109.5 ? H4 C16 H6 . . 109.5 ? C18 C17 C5 . . 115.8(5) ? C18 C17 H8 . . 108.3 ? C5 C17 H8 . . 108.3 ? C18 C17 H7 . . 108.3 ? C5 C17 H7 . . 108.3 ? H8 C17 H7 . . 107.4 ? C8 C18 C17 . . 113.3(5) ? C8 C18 H9 . . 108.9 ? C17 C18 H9 . . 108.9 ? C8 C18 H35 . . 108.9 ? C17 C18 H35 . . 108.9 ? H9 C18 H35 . . 107.7 ? C7 C19 C20 . . 103.7(5) ? C7 C19 H31 . . 111.0 ? C20 C19 H31 . . 111.0 ? C7 C19 H11 . . 111.0 ? C20 C19 H11 . . 111.0 ? H31 C19 H11 . . 109.0 ? C19 C20 C9 . . 106.7(5) ? C19 C20 H12 . . 110.4 ? C9 C20 H12 . . 110.4 ? C19 C20 H13 . . 110.4 ? C9 C20 H13 . . 110.4 ? H12 C20 H13 . . 108.6 ? C13 C21 H18 . . 109.5 ? C13 C21 H17 . . 109.5 ? H18 C21 H17 . . 109.5 ? C13 C21 H19 . . 109.5 ? H18 C21 H19 . . 109.5 ? H17 C21 H19 . . 109.5 ? C14 C22 H23 . . 109.5 ? C14 C22 H22 . . 109.5 ? H23 C22 H22 . . 109.5 ? C14 C22 H21 . . 109.5 ? H23 C22 H21 . . 109.5 ? H22 C22 H21 . . 109.5 ? C10 C23 H29 . . 109.5 ? C10 C23 H30 . . 109.5 ? H29 C23 H30 . . 109.5 ? C10 C23 H28 . . 109.5 ? H29 C23 H28 . . 109.5 ? H30 C23 H28 . . 109.5 ? C8 C24 H34 . . 109.5 ? C8 C24 H32 . . 109.5 ? H34 C24 H32 . . 109.5 ? C8 C24 H33 . . 109.5 ? H34 C24 H33 . . 109.5 ? H32 C24 H33 . . 109.5 ? O3 C25 C26 . . 111.1(5) ? O3 C25 C5 . . 111.9(5) ? C26 C25 C5 . . 105.9(4) ? O3 C25 H41 . . 109.3 ? C26 C25 H41 . . 109.3 ? C5 C25 H41 . . 109.3 ? C27 C26 C25 . . 105.5(5) ? C27 C26 H36 . . 110.6 ? C25 C26 H36 . . 110.6 ? C27 C26 H40 . . 110.6 ? C25 C26 H40 . . 110.6 ? H36 C26 H40 . . 108.8 ? C26 C27 C28 . . 118.9(5) ? C26 C27 C4 . . 103.7(5) ? C28 C27 C4 . . 112.1(5) ? C26 C27 H39 . . 107.2 ? C28 C27 H39 . . 107.2 ? C4 C27 H39 . . 107.2 ? C1 C28 C27 . . 110.4(5) ? C1 C28 H38 . . 109.6 ? C27 C28 H38 . . 109.6 ? C1 C28 H37 . . 109.6 ? C27 C28 H37 . . 109.6 ? H38 C28 H37 . . 108.1 ? 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 H47 . 0.9322 ? O4 H48 . 0.9859 ? O1 C1 . 1.447(6) ? O1 H45 . 0.84 ? O2 C6 . 1.200(7) ? O3 C25 . 1.437(6) ? O3 H46 . 0.84 ? C1 C28 . 1.505(7) ? C1 C2 . 1.517(9) ? C1 H1 . 1.0 ? C2 C3 . 1.534(8) ? C2 H44 . 0.99 ? C2 H43 . 0.99 ? C3 C4 . 1.522(8) ? C3 H42 . 0.99 ? C3 H3 . 0.99 ? C4 C27 . 1.550(8) ? C4 C16 . 1.553(9) ? C4 C5 . 1.568(8) ? C5 C6 . 1.534(9) ? C5 C17 . 1.566(8) ? C5 C25 . 1.585(8) ? C6 C7 . 1.509(8) ? C7 C19 . 1.514(9) ? C7 C8 . 1.553(8) ? C7 H10 . 1.0 ? C8 C24 . 1.523(8) ? C8 C18 . 1.526(9) ? C8 C9 . 1.551(8) ? C9 C10 . 1.534(8) ? C9 C20 . 1.561(9) ? C9 H14 . 1.0 ? C10 C11 . 1.510(8) ? C10 C23 . 1.512(9) ? C10 H15 . 1.0 ? C11 C12 . 1.312(9) ? C11 H16 . 0.95 ? C12 C13 . 1.509(8) ? C12 H27 . 0.95 ? C13 C21 . 1.531(10) ? C13 C14 . 1.538(9) ? C13 H20 . 1.0 ? C14 C15 . 1.519(11) ? C14 C22 . 1.526(10) ? C14 H24 . 1.0 ? C15 H26 . 0.98 ? C15 H25 . 0.98 ? C15 H2 . 0.98 ? C16 H5 . 0.98 ? C16 H4 . 0.98 ? C16 H6 . 0.98 ? C17 C18 . 1.541(8) ? C17 H8 . 0.99 ? C17 H7 . 0.99 ? C18 H9 . 0.99 ? C18 H35 . 0.99 ? C19 C20 . 1.545(8) ? C19 H31 . 0.99 ? C19 H11 . 0.99 ? C20 H12 . 0.99 ? C20 H13 . 0.99 ? C21 H18 . 0.98 ? C21 H17 . 0.98 ? C21 H19 . 0.98 ? C22 H23 . 0.98 ? C22 H22 . 0.98 ? C22 H21 . 0.98 ? C23 H29 . 0.98 ? C23 H30 . 0.98 ? C23 H28 . 0.98 ? C24 H34 . 0.98 ? C24 H32 . 0.98 ? C24 H33 . 0.98 ? C25 C26 . 1.545(8) ? C25 H41 . 1.0 ? C26 C27 . 1.513(7) ? C26 H36 . 0.99 ? C26 H40 . 0.99 ? C27 C28 . 1.522(7) ? C27 H39 . 1.0 ? C28 H38 . 0.99 ? C28 H37 . 0.99 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O4 H47 O3 1_564 0.93 2.00 2.862(6) 152.2 ? O4 H48 O1 4_655 0.99 1.83 2.816(6) 177.0 ? O1 H45 O4 . 0.84 1.87 2.699(7) 170.4 ? O3 H46 O1 1_556 0.84 1.97 2.799(6) 167.0 ? C7 H10 O3 . 1.00 2.36 3.004(7) 121.0 ? 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 O1 C1 C2 C3 . . . . 175.9(5) ? C28 C1 C2 C3 . . . . 52.5(7) ? C1 C2 C3 C4 . . . . -55.4(8) ? C2 C3 C4 C27 . . . . 57.5(7) ? C2 C3 C4 C16 . . . . -63.1(7) ? C2 C3 C4 C5 . . . . 170.9(6) ? C3 C4 C5 C6 . . . . 80.1(7) ? C27 C4 C5 C6 . . . . -162.6(5) ? C16 C4 C5 C6 . . . . -47.1(7) ? C3 C4 C5 C17 . . . . -38.8(8) ? C27 C4 C5 C17 . . . . 78.5(6) ? C16 C4 C5 C17 . . . . -166.0(5) ? C3 C4 C5 C25 . . . . -155.5(6) ? C27 C4 C5 C25 . . . . -38.2(5) ? C16 C4 C5 C25 . . . . 77.3(6) ? C17 C5 C6 O2 . . . . 111.5(6) ? C4 C5 C6 O2 . . . . -13.0(8) ? C25 C5 C6 O2 . . . . -131.7(6) ? C17 C5 C6 C7 . . . . -59.2(6) ? C4 C5 C6 C7 . . . . 176.3(5) ? C25 C5 C6 C7 . . . . 57.6(6) ? O2 C6 C7 C19 . . . . 20.5(9) ? C5 C6 C7 C19 . . . . -168.6(5) ? O2 C6 C7 C8 . . . . -100.1(7) ? C5 C6 C7 C8 . . . . 70.8(6) ? C6 C7 C8 C24 . . . . 58.4(7) ? C19 C7 C8 C24 . . . . -70.2(6) ? C6 C7 C8 C18 . . . . -63.4(6) ? C19 C7 C8 C18 . . . . 168.0(5) ? C6 C7 C8 C9 . . . . 174.8(5) ? C19 C7 C8 C9 . . . . 46.2(6) ? C24 C8 C9 C10 . . . . -48.3(8) ? C18 C8 C9 C10 . . . . 81.8(7) ? C7 C8 C9 C10 . . . . -166.3(5) ? C24 C8 C9 C20 . . . . 77.7(6) ? C18 C8 C9 C20 . . . . -152.2(5) ? C7 C8 C9 C20 . . . . -40.4(5) ? C8 C9 C10 C11 . . . . 174.1(5) ? C20 C9 C10 C11 . . . . 52.2(7) ? C8 C9 C10 C23 . . . . -61.8(7) ? C20 C9 C10 C23 . . . . 176.3(5) ? C23 C10 C11 C12 . . . . 123.1(7) ? C9 C10 C11 C12 . . . . -111.4(7) ? C10 C11 C12 C13 . . . . 177.4(6) ? C11 C12 C13 C21 . . . . -118.2(8) ? C11 C12 C13 C14 . . . . 113.3(7) ? C12 C13 C14 C15 . . . . -59.6(8) ? C21 C13 C14 C15 . . . . 173.8(6) ? C12 C13 C14 C22 . . . . 64.8(8) ? C21 C13 C14 C22 . . . . -61.7(8) ? C6 C5 C17 C18 . . . . 50.0(6) ? C4 C5 C17 C18 . . . . 175.5(5) ? C25 C5 C17 C18 . . . . -70.7(7) ? C24 C8 C18 C17 . . . . -66.5(7) ? C9 C8 C18 C17 . . . . 164.2(5) ? C7 C8 C18 C17 . . . . 55.6(6) ? C5 C17 C18 C8 . . . . -53.3(7) ? C6 C7 C19 C20 . . . . -155.2(5) ? C8 C7 C19 C20 . . . . -33.1(6) ? C7 C19 C20 C9 . . . . 6.6(7) ? C10 C9 C20 C19 . . . . 152.6(5) ? C8 C9 C20 C19 . . . . 21.9(6) ? C6 C5 C25 O3 . . . . 21.7(7) ? C17 C5 C25 O3 . . . . 135.7(5) ? C4 C5 C25 O3 . . . . -103.7(5) ? C6 C5 C25 C26 . . . . 142.9(5) ? C17 C5 C25 C26 . . . . -103.1(5) ? C4 C5 C25 C26 . . . . 17.5(6) ? O3 C25 C26 C27 . . . . 132.4(5) ? C5 C25 C26 C27 . . . . 10.8(6) ? C25 C26 C27 C28 . . . . -160.7(5) ? C25 C26 C27 C4 . . . . -35.5(6) ? C3 C4 C27 C26 . . . . 170.5(5) ? C16 C4 C27 C26 . . . . -68.3(6) ? C5 C4 C27 C26 . . . . 46.0(5) ? C3 C4 C27 C28 . . . . -60.0(6) ? C16 C4 C27 C28 . . . . 61.2(6) ? C5 C4 C27 C28 . . . . 175.6(5) ? O1 C1 C28 C27 . . . . -173.4(5) ? C2 C1 C28 C27 . . . . -52.4(7) ? C26 C27 C28 C1 . . . . 178.4(6) ? C4 C27 C28 C1 . . . . 57.3(7) ?