#------------------------------------------------------------------------------ #$Date: 2019-12-13 10:49:55 +0200 (Fri, 13 Dec 2019) $ #$Revision: 245051 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556552.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_1556552 loop_ _publ_author_name 'Nguyen, H.N.' 'Tashima, N.' 'Ikariya, T.' 'Kuwata, S.' _publ_section_title ; Ruthenium-Catalyzed Dimerization of 1,1-Diphenylpropargyl Alcohol to a Hydroxybenzocyclobutene and Related Reactions ; _journal_name_full Inorganics _journal_page_first 80 _journal_paper_doi 10.3390/inorganics5040080 _journal_volume 5 _journal_year 2017 _chemical_formula_moiety 'C30 H24 O2, 0.5(C3 H6 O)' _chemical_formula_sum 'C31.5 H27 O2.5' _chemical_formula_weight 445.56 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 72.216(16) _cell_angle_beta 84.13(2) _cell_angle_gamma 69.554(17) _cell_formula_units_Z 2 _cell_length_a 10.337(6) _cell_length_b 10.816(6) _cell_length_c 12.119(7) _cell_measurement_reflns_used 4435 _cell_measurement_temperature 93 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 3.11 _cell_volume 1208.9(12) _computing_cell_refinement CrystalClear _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction CrystalClear _computing_molecular_graphics 'CrystalStructure 4.2.5' _computing_publication_material 'CrystalStructure 4.2.5 (Rigaku, 2017)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _diffrn_ambient_temperature 93 _diffrn_detector_area_resol_mean 7.314 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.953 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_Laue_measured_fraction_full 0.975 _diffrn_reflns_Laue_measured_fraction_max 0.953 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 9706 _diffrn_reflns_point_group_measured_fraction_full 0.975 _diffrn_reflns_point_group_measured_fraction_max 0.953 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.531 _diffrn_reflns_theta_min 3.110 _diffrn_standards_interval_count . _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 472.00 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.37 _refine_diff_density_min -0.31 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_hydrogen_treatment mixed _refine_ls_number_parameters 329 _refine_ls_number_reflns 5322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0510 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0861P)^2^+0.5301P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1383 _refine_ls_wR_factor_ref 0.1477 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4401 _reflns_number_total 5322 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file Inorganics-2017-5-80.cif _cod_data_source_block compound_2 _cod_original_cell_volume 1209.0(12) _cod_database_code 1556552 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL methylenebenzocyclobutane2 CELL 0.71075 10.33720 10.81600 12.11920 72.21580 84.13040 69.55400 ZERR 2 0.00610 0.00570 0.00740 0.01620 0.01990 0.01650 LATT 1 SFAC C H O UNIT 63 54 5 L.S. 5 FMAP 2 PLAN 25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -179.8 ACTA SIZE 0.200 0.200 0.200 WGHT 0.086100 0.530100 FVAR 2.59470 O1 3 1.066972 0.438198 0.413213 11.00000 0.02384 0.01364 = 0.02045 -0.00553 0.00016 -0.00273 AFIX 147 H1 2 1.040462 0.459022 0.475059 10.50000 -1.50000 AFIX 147 H31 2 1.094442 0.476747 0.348590 10.50000 -1.50000 AFIX 0 O2 3 0.844862 0.403342 0.789051 11.00000 0.02019 0.02108 = 0.02721 -0.00873 -0.00067 -0.00852 AFIX 147 H2 2 0.831448 0.432003 0.847734 10.50000 -1.50000 AFIX 147 H32 2 0.847390 0.463343 0.726365 10.50000 -1.50000 AFIX 0 C1 1 1.130792 0.292654 0.438671 11.00000 0.01576 0.01335 = 0.01607 -0.00646 0.00205 -0.00255 C2 1 1.025240 0.214348 0.454447 11.00000 0.01641 0.01550 = 0.01638 -0.00606 -0.00052 -0.00194 C3 1 1.078369 0.175578 0.347893 11.00000 0.01551 0.01562 = 0.01662 -0.00621 0.00045 -0.00021 C4 1 1.066365 0.104229 0.273791 11.00000 0.02133 0.02137 = 0.02325 -0.01127 0.00149 -0.00582 AFIX 43 H3 2 1.002691 0.055709 0.287153 11.00000 -1.20000 AFIX 0 C5 1 1.154484 0.108779 0.178191 11.00000 0.02513 0.02528 = 0.02147 -0.01463 0.00188 -0.00289 AFIX 43 H4 2 1.150212 0.062460 0.124211 11.00000 -1.20000 AFIX 0 C6 1 1.248433 0.179293 0.159761 11.00000 0.01920 0.02360 = 0.01894 -0.00880 0.00497 -0.00053 AFIX 43 H5 2 1.305918 0.179535 0.093371 11.00000 -1.20000 AFIX 0 C7 1 1.261268 0.249602 0.235182 11.00000 0.01638 0.01733 = 0.02042 -0.00603 0.00274 -0.00179 AFIX 43 H6 2 1.325798 0.297026 0.222989 11.00000 -1.20000 AFIX 0 C8 1 1.172930 0.244948 0.328944 11.00000 0.01572 0.01426 = 0.01621 -0.00592 -0.00085 0.00005 C9 1 1.242886 0.235932 0.530683 11.00000 0.01504 0.01887 = 0.01553 -0.00516 0.00293 -0.00586 C10 1 1.269707 0.319296 0.586259 11.00000 0.02357 0.01997 = 0.03086 -0.00794 -0.00486 -0.00632 AFIX 43 H7 2 1.213083 0.413347 0.570769 11.00000 -1.20000 AFIX 0 C11 1 1.379241 0.265950 0.664715 11.00000 0.02964 0.03089 = 0.03097 -0.00876 -0.00717 -0.01279 AFIX 43 H8 2 1.396778 0.323688 0.702449 11.00000 -1.20000 AFIX 0 C12 1 1.462489 0.128898 0.687692 11.00000 0.01776 0.03364 = 0.02167 -0.00280 -0.00320 -0.00854 AFIX 43 H9 2 1.538774 0.093234 0.739277 11.00000 -1.20000 AFIX 0 C13 1 1.433853 0.044148 0.635009 11.00000 0.01962 0.02384 = 0.02031 -0.00432 0.00063 -0.00087 AFIX 43 H10 2 1.489036 -0.050481 0.652216 11.00000 -1.20000 AFIX 0 C14 1 1.324991 0.097121 0.557357 11.00000 0.02142 0.02023 = 0.02097 -0.00854 0.00025 -0.00248 AFIX 43 H11 2 1.305939 0.038261 0.521789 11.00000 -1.20000 AFIX 0 C15 1 0.923546 0.201556 0.529913 11.00000 0.01624 0.01668 = 0.01883 -0.00753 0.00030 -0.00440 AFIX 43 H12 2 0.869387 0.149812 0.521500 11.00000 -1.20000 AFIX 0 C16 1 0.892779 0.264024 0.624506 11.00000 0.01649 0.01542 = 0.01859 -0.00649 0.00076 -0.00365 AFIX 43 H13 2 0.958185 0.299134 0.641827 11.00000 -1.20000 AFIX 0 C17 1 0.778242 0.275069 0.688515 11.00000 0.01748 0.01724 = 0.01735 -0.00785 0.00015 -0.00503 AFIX 43 H14 2 0.715993 0.234526 0.674244 11.00000 -1.20000 AFIX 0 C18 1 0.740575 0.347657 0.782244 11.00000 0.01351 0.01808 = 0.01821 -0.00770 0.00167 -0.00484 C19 1 0.601921 0.466399 0.755051 11.00000 0.01651 0.01759 = 0.01910 -0.00757 0.00130 -0.00327 C20 1 0.553576 0.531196 0.642581 11.00000 0.03319 0.03029 = 0.01941 -0.01122 0.00049 0.00252 AFIX 43 H15 2 0.602583 0.497081 0.581388 11.00000 -1.20000 AFIX 0 C21 1 0.433764 0.645982 0.618024 11.00000 0.04486 0.03933 = 0.02173 -0.00887 -0.00807 0.01269 AFIX 43 H16 2 0.402022 0.689863 0.540251 11.00000 -1.20000 AFIX 0 C22 1 0.360620 0.696552 0.706235 11.00000 0.02719 0.02871 = 0.03008 -0.00980 -0.00251 0.00740 AFIX 43 H17 2 0.277893 0.773718 0.689441 11.00000 -1.20000 AFIX 0 C23 1 0.408766 0.634040 0.818744 11.00000 0.02544 0.02772 = 0.02443 -0.01118 0.00595 0.00037 AFIX 43 H18 2 0.359717 0.668709 0.879664 11.00000 -1.20000 AFIX 0 C24 1 0.528960 0.520432 0.842790 11.00000 0.02305 0.02734 = 0.01967 -0.00912 0.00097 0.00027 AFIX 43 H19 2 0.562135 0.478735 0.920303 11.00000 -1.20000 AFIX 0 C25 1 0.737097 0.238198 0.897021 11.00000 0.01662 0.01706 = 0.01628 -0.00933 0.00339 -0.00412 C26 1 0.623584 0.192736 0.926684 11.00000 0.01606 0.02440 = 0.02011 -0.01059 0.00068 -0.00546 AFIX 43 H20 2 0.544397 0.234888 0.877788 11.00000 -1.20000 AFIX 0 C27 1 0.625358 0.087127 1.026382 11.00000 0.01919 0.02662 = 0.02481 -0.01085 0.00628 -0.01132 AFIX 43 H21 2 0.547272 0.057724 1.045525 11.00000 -1.20000 AFIX 0 C28 1 0.740469 0.023593 1.098862 11.00000 0.02398 0.01969 = 0.02033 -0.00587 0.00475 -0.00520 AFIX 43 H22 2 0.742104 -0.049656 1.166913 11.00000 -1.20000 AFIX 0 C29 1 0.852511 0.068857 1.070189 11.00000 0.01931 0.02231 = 0.02192 -0.00707 -0.00186 -0.00339 AFIX 43 H23 2 0.931519 0.026519 1.119291 11.00000 -1.20000 AFIX 0 C30 1 0.851021 0.175295 0.970642 11.00000 0.01591 0.02079 = 0.02268 -0.00799 0.00118 -0.00580 AFIX 43 H24 2 0.928682 0.205482 0.952624 11.00000 -1.20000 AFIX 0 PART -1 O3 3 0.826528 0.474945 0.981191 10.50000 0.04005 0.03212 = 0.02451 -0.01144 -0.00003 -0.01836 C31 1 0.907334 0.509078 1.021466 10.50000 0.03270 0.02339 = 0.02271 -0.00531 -0.00634 -0.00869 C32 1 0.876566 0.545948 1.132375 10.50000 0.04862 0.06047 = 0.02845 -0.02031 -0.00241 -0.02534 AFIX 137 H25 2 0.782558 0.548582 1.156928 10.50000 -1.50000 H26 2 0.884452 0.636690 1.121128 10.50000 -1.50000 H27 2 0.942444 0.476832 1.192048 10.50000 -1.50000 AFIX 0 C33 1 1.040156 0.516167 0.961572 10.50000 0.03208 0.03237 = 0.04032 -0.00838 -0.00329 -0.00815 AFIX 137 H28 2 1.071008 0.449840 0.916401 10.50000 -1.50000 H29 2 1.110625 0.493901 1.019508 10.50000 -1.50000 H30 2 1.025542 0.609388 0.909707 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 REM methylenebenzocyclobutane2 REM R1 = 0.0510 for 4401 Fo > 4sig(Fo) and 0.0620 for all 5322 data REM 329 parameters refined using 0 restraints END WGHT 0.0754 0.3823 REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+1, -z+1 HTAB O1 O1_$1 HTAB O1 O2_$1 HTAB O2 O3 HTAB O2 O1_$1 REM Highest difference peak 0.366, deepest hole -0.315, 1-sigma level 0.056 Q1 1 0.7396 0.2865 0.8411 11.00000 0.05 0.37 Q2 1 1.1755 0.2567 0.4926 11.00000 0.05 0.32 Q3 1 1.0784 0.2439 0.4718 11.00000 0.05 0.28 Q4 1 0.5444 0.4766 0.7043 11.00000 0.05 0.28 Q5 1 0.8043 0.1849 0.9135 11.00000 0.05 0.26 Q6 1 0.6974 0.0400 1.0399 11.00000 0.05 0.24 Q7 1 0.3532 0.6417 0.7612 11.00000 0.05 0.23 Q8 1 0.9191 0.3817 0.8455 11.00000 0.05 0.22 Q9 1 1.0567 0.1599 0.4118 11.00000 0.05 0.21 Q10 1 1.1105 0.2352 0.3106 11.00000 0.05 0.21 Q11 1 0.6348 0.1177 0.9678 11.00000 0.05 0.21 Q12 1 0.6911 0.1978 0.9056 11.00000 0.05 0.21 Q13 1 1.2991 0.3040 0.5242 11.00000 0.05 0.20 Q14 1 0.8447 0.1243 1.0166 11.00000 0.05 0.20 Q15 1 0.4327 0.6877 0.7610 11.00000 0.05 0.20 Q16 1 1.3361 0.2929 0.6066 11.00000 0.05 0.20 Q17 1 1.3630 0.0663 0.6117 11.00000 0.05 0.19 Q18 1 1.1583 0.5019 0.3991 11.00000 0.05 0.19 Q19 1 1.2373 0.2219 0.2984 11.00000 0.05 0.19 Q20 1 1.2292 0.1065 0.2095 11.00000 0.05 0.19 Q21 1 1.0103 0.1663 0.5174 11.00000 0.05 0.18 Q22 1 1.1427 0.0800 0.2383 11.00000 0.05 0.18 Q23 1 1.3864 0.0793 0.5896 11.00000 0.05 0.18 Q24 1 0.3870 0.6004 0.6601 11.00000 0.05 0.18 Q25 1 0.6754 0.3992 0.7688 11.00000 0.05 0.17 ; _shelx_res_checksum 76436 _shelx_hkl_file ; 0 0 2 87.54 10.41 0 0 2 86.99 6.92 0 0 -2 86.42 10.81 0 0 -2 100.83 8.72 0 0 3 3374.52 167.82 0 0 3 3062.94 151.80 0 0 -3 2996.12 148.53 0 0 -3 3576.20 177.49 0 0 4 2024.36 104.28 0 0 -4 2193.87 112.13 0 0 -4 1823.69 92.72 0 0 -4 1728.12 88.13 0 0 5 1100.96 67.00 0 0 -5 1061.51 62.51 0 0 -5 1023.80 60.65 0 0 6 299.03 23.40 0 0 -6 334.01 18.38 0 0 -6 339.37 20.48 0 0 7 192.68 22.51 0 0 -7 232.11 23.67 0 0 -7 218.28 25.50 0 0 8 1279.80 65.15 0 0 -8 1303.12 63.23 0 0 9 987.31 130.04 0 0 -9 1005.95 130.89 0 0 10 368.46 35.55 0 0 -10 332.34 25.03 0 0 11 258.58 34.03 0 0 -11 228.76 27.69 0 0 -12 7.02 13.53 0 0 13 359.24 42.05 0 0 14 188.07 31.87 0 0 15 543.51 44.74 0 -1 14 21.34 17.00 0 1 -13 22.69 18.40 0 -1 13 14.34 15.26 0 1 -12 290.61 27.28 0 -1 12 368.31 42.20 0 1 -11 36.47 12.99 0 -1 11 33.70 23.33 0 1 -10 340.64 35.23 0 -1 10 426.14 31.40 0 1 -9 27.33 16.98 0 -1 9 23.17 17.50 0 1 -8 375.86 29.28 0 -1 8 331.95 28.14 0 1 -7 134.00 27.78 0 -1 7 103.68 19.47 0 1 -6 95.94 15.90 0 -1 6 26.30 17.29 0 1 -517880.16 1051.26 0 1 -518847.55 1107.80 0 -1 519231.45 1131.37 0 1 -4 1562.95 89.66 0 1 -4 1559.79 91.25 0 1 -4 1523.58 87.85 0 -1 4 1657.96 51.96 0 1 -3 377.32 26.18 0 1 -3 396.44 26.03 0 -1 3 328.99 22.51 0 1 -2 5008.09 273.44 0 1 -2 5227.96 216.60 0 -1 2 5076.07 276.93 0 -1 2 5270.54 218.64 0 1 -1 2247.00 111.44 0 -1 1 2005.71 100.04 0 -1 -2 3431.05 168.74 0 1 3 7585.75 312.36 0 -1 -3 7557.03 310.90 0 -1 -3 6263.79 256.28 0 1 4 1744.81 89.89 0 -1 -4 1925.20 98.56 0 -1 -4 1562.19 78.51 0 -1 -4 1501.37 75.25 0 1 5 9265.72 473.19 0 -1 -5 9063.05 462.98 0 -1 -5 8498.11 431.92 0 -1 -5 8345.38 423.96 0 1 6 182.35 16.09 0 -1 -6 218.25 13.73 0 -1 -6 220.39 19.82 0 1 7 332.91 35.48 0 -1 -7 293.07 26.66 0 -1 -7 279.51 27.66 0 -1 -8 4077.57 166.80 0 1 9 100.83 20.12 0 -1 -9 84.56 13.92 0 1 11 6016.59 423.04 0 -1 -11 5905.33 408.80 0 1 12 762.53 48.92 0 -1 -12 794.99 33.06 0 1 13 21.50 19.24 0 1 14 173.44 32.58 0 1 15 32.95 25.08 0 -2 14 91.29 32.57 0 2 -13 402.83 37.98 0 -2 13 372.97 39.94 0 2 -12 119.10 24.60 0 -2 12 111.66 29.77 0 2 -11 26.42 23.32 0 -2 11 20.64 20.66 0 2 -10 127.72 21.01 0 -2 10 135.78 21.56 0 2 -9 586.95 35.62 0 -2 9 558.20 35.55 0 2 -8 515.05 45.15 0 -2 8 484.84 40.56 0 2 -7 23.29 13.63 0 -2 7 17.73 13.27 0 2 -6 176.78 29.26 0 -2 6 98.37 18.76 0 2 -5 4120.92 248.45 0 2 -4 7.78 9.95 0 2 -4 5.14 10.86 0 -2 4 10.82 12.02 0 2 -3 7582.91 388.65 0 2 -3 7212.52 369.18 0 2 -3 7180.40 368.29 0 -2 3 7514.92 385.32 0 2 -211513.02 474.47 0 2 -212754.55 524.33 0 2 -211392.32 469.67 0 -2 212132.35 499.23 0 2 -141939.20 1711.62 0 2 -145755.48 1866.11 0 2 -141100.68 1677.32 0 -2 145168.94 1842.59 0 2 0 7946.86 327.19 0 2 0 8471.45 348.14 0 2 0 7392.37 304.53 0 -2 0 8441.30 347.01 0 2 111595.64 474.46 0 2 111390.61 466.61 0 2 110906.87 446.48 0 -2 -111088.73 454.36 0 2 2 7715.94 317.18 0 2 2 7859.51 321.31 0 2 2 9176.63 374.94 0 -2 -2 8224.88 337.93 0 2 3 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33.56 -12 -2 3 57.01 19.94 -12 -2 3 68.97 24.52 -12 -2 2 213.10 36.42 -12 -2 2 178.10 31.84 -12 -2 1 12.53 13.36 -12 -2 1 26.92 15.21 -12 -2 0 7.98 11.78 -12 -2 0 18.54 18.10 -12 -2 -1 4.76 10.08 -12 -2 -1 26.57 19.78 -12 -2 -2 335.85 34.80 -12 -2 -3 114.56 32.78 -12 -2 -4 357.50 50.93 -12 -2 -5 21.94 10.65 -12 -2 -6 146.57 35.08 -12 -3 5 44.08 15.96 -12 -3 5 26.66 21.44 -12 -3 4 63.49 22.29 -12 -3 4 73.89 35.36 -12 -3 3 18.82 20.50 -12 -3 3 23.89 20.94 -12 -3 2 99.91 20.50 -12 -3 2 142.65 27.38 -12 -3 1 10.51 11.18 -12 -3 1 3.67 9.22 -12 -3 0 7.08 9.48 -12 -3 0 21.01 21.11 -12 -3 -1 121.13 33.73 -12 -3 -2 777.47 49.62 -12 -3 -3 32.76 27.57 -12 -3 -4 478.34 44.64 -12 -3 -5 158.83 50.38 -12 -3 -6 23.33 19.50 -12 -3 -7 113.17 29.49 -12 -4 5 184.60 29.77 -12 -4 5 128.63 39.51 -12 -4 4 541.95 41.39 -12 -4 4 451.42 49.41 -12 -4 3 9.23 18.14 -12 -4 3 7.92 5.17 -12 -4 2 20.47 17.08 -12 -4 2 20.75 14.04 -12 -4 1 40.01 26.36 -12 -4 0 80.67 28.58 -12 -4 -1 9.86 19.95 -12 -4 -2 125.69 29.43 -12 -4 -3 64.19 32.40 -12 -4 -4 1249.28 73.85 -12 -4 -5 199.04 36.75 -12 -4 -6 11.18 16.81 -12 -4 -7 8.97 13.25 -12 -4 -8 859.33 58.22 -12 -5 5 17.00 19.26 -12 -5 4 201.38 26.50 -12 -5 4 215.39 33.55 -12 -5 3 647.92 47.13 -12 -5 2 143.08 37.16 -12 -5 1 17.47 18.86 -12 -5 0 482.52 40.78 -12 -5 -1 118.68 31.70 -12 -5 -2 868.52 58.09 -12 -5 -3 240.91 42.06 -12 -5 -4 134.27 54.08 -12 -5 -5 8.77 10.10 -12 -5 -6 1150.09 62.29 -12 -5 -7 702.28 49.88 -12 -5 -8 60.24 25.70 -12 -6 4 59.75 22.33 -12 -6 3 14.71 11.67 -12 -6 2 23.98 24.70 -12 -6 1 14.72 13.95 -12 -6 0 505.86 50.59 -12 -6 -1 774.48 52.40 -12 -6 -2 364.78 45.20 -12 -6 -3 982.56 61.21 -12 -6 -4 62.43 27.50 -12 -6 -5 21.08 14.93 -12 -6 -6 41.27 28.20 -12 -6 -7 14.12 21.55 -12 -6 -8 34.67 29.72 -12 -7 3 31.27 28.05 -12 -7 2 31.88 29.67 -12 -7 1 25.77 17.63 -12 -7 0 969.13 64.40 -12 -7 -1 1942.82 97.65 -12 -7 -2 522.34 58.60 -12 -7 -3 171.87 39.12 -12 -7 -4 44.64 54.43 -12 -7 -5 361.35 41.26 -12 -7 -6 61.85 31.14 -12 -7 -7 38.50 21.87 -12 -7 -8 24.09 20.72 -12 -8 2 16.99 19.40 -12 -8 1 614.16 57.72 -12 -8 0 5.97 19.15 -12 -8 -1 585.59 50.00 -12 -8 -2 1599.62 101.72 -12 -8 -3 972.65 66.67 -12 -8 -4 13.45 12.14 -12 -8 -5 145.01 34.25 -12 -8 -6 489.39 45.14 -12 -8 -7 184.83 32.44 -12 -9 1 50.41 42.24 -12 -9 0 356.46 41.35 -12 -9 -1 183.72 52.23 -12 -9 -2 1042.80 61.94 -12 -9 -3 54.04 27.38 -12 -9 -4 18.56 16.20 -12 -9 -5 215.50 34.63 -12 -9 -6 23.54 36.09 -12 -9 -7 1285.42 67.34 -12 -10 -2 9.00 9.34 -12 -10 -3 94.35 34.75 -12 -10 -4 20.60 19.77 -12 -10 -5 298.52 39.95 -13 -2 1 15.81 20.45 -13 -2 0 265.88 32.95 -13 -2 -1 26.80 18.25 -13 -2 -2 939.92 58.93 -13 -3 2 808.51 54.79 -13 -3 1 11.31 12.75 -13 -3 0 271.17 37.85 -13 -3 -1 84.72 27.56 -13 -3 -2 10.25 20.54 -13 -3 -3 78.50 36.90 -13 -3 -4 7.82 17.61 -13 -4 2 48.13 21.26 -13 -4 1 48.55 20.99 -13 -4 0 116.09 38.51 -13 -4 -1 968.08 62.04 -13 -4 -2 21.71 27.87 -13 -4 -3 244.12 48.30 -13 -4 -4 15.39 20.70 -13 -5 2 21.93 17.54 -13 -5 1 102.27 30.51 -13 -5 0 29.81 17.22 -13 -5 -1 49.24 30.86 -13 -5 -2 553.39 55.93 -13 -5 -3 206.05 38.51 -13 -5 -4 113.00 29.39 -13 -5 -5 569.01 48.82 -13 -6 1 107.66 29.17 -13 -6 0 473.55 49.86 -13 -6 -1 122.22 40.08 -13 -6 -2 70.36 32.16 -13 -6 -3 721.09 57.72 -13 -6 -4 225.20 40.09 -13 -6 -5 24.27 20.94 -13 -7 0 153.09 49.74 -13 -7 -1 343.32 58.89 -13 -7 -2 11.67 11.32 -13 -7 -3 716.86 55.45 -13 -7 -4 186.78 35.72 ; _shelx_hkl_checksum 43641 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.06697(11) 0.43820(11) 0.41321(9) 0.0202(2) Uani 1 1 d . . . . . H1 H 1.0405 0.4590 0.4751 0.030 Uiso 0.5 1 calc R U P . . H31 H 1.0944 0.4767 0.3486 0.030 Uiso 0.5 1 calc R U P . . O2 O 0.84486(11) 0.40334(11) 0.78905(10) 0.0219(3) Uani 1 1 d . . . . . H2 H 0.8314 0.4320 0.8477 0.033 Uiso 0.5 1 calc R U P . . H32 H 0.8474 0.4633 0.7264 0.033 Uiso 0.5 1 calc R U P . . C1 C 1.13079(14) 0.29265(14) 0.43867(12) 0.0153(3) Uani 1 1 d . . . . . C2 C 1.02524(15) 0.21435(15) 0.45445(12) 0.0167(3) Uani 1 1 d . . . . . C3 C 1.07837(15) 0.17558(15) 0.34789(13) 0.0170(3) Uani 1 1 d . . . . . C4 C 1.06637(16) 0.10423(16) 0.27379(14) 0.0213(3) Uani 1 1 d . . . . . H3 H 1.0027 0.0557 0.2872 0.026 Uiso 1 1 calc R U . . . C5 C 1.15448(17) 0.10878(17) 0.17819(14) 0.0238(3) Uani 1 1 d . . . . . H4 H 1.1502 0.0625 0.1242 0.029 Uiso 1 1 calc R U . . . C6 C 1.24843(16) 0.17929(16) 0.15976(14) 0.0222(3) Uani 1 1 d . . . . . H5 H 1.3059 0.1795 0.0934 0.027 Uiso 1 1 calc R U . . . C7 C 1.26127(15) 0.24960(15) 0.23518(13) 0.0192(3) Uani 1 1 d . . . . . H6 H 1.3258 0.2970 0.2230 0.023 Uiso 1 1 calc R U . . . C8 C 1.17293(15) 0.24495(14) 0.32894(12) 0.0164(3) Uani 1 1 d . . . . . C9 C 1.24289(14) 0.23593(15) 0.53068(12) 0.0166(3) Uani 1 1 d . . . . . C10 C 1.26971(17) 0.31930(17) 0.58626(15) 0.0246(3) Uani 1 1 d . . . . . H7 H 1.2131 0.4133 0.5708 0.029 Uiso 1 1 calc R U . . . C11 C 1.37924(18) 0.26595(19) 0.66471(16) 0.0293(4) Uani 1 1 d . . . . . H8 H 1.3968 0.3237 0.7024 0.035 Uiso 1 1 calc R U . . . C12 C 1.46249(16) 0.12890(18) 0.68769(14) 0.0254(4) Uani 1 1 d . . . . . H9 H 1.5388 0.0932 0.7393 0.030 Uiso 1 1 calc R U . . . C13 C 1.43385(16) 0.04415(17) 0.63501(14) 0.0236(3) Uani 1 1 d . . . . . H10 H 1.4890 -0.0505 0.6522 0.028 Uiso 1 1 calc R U . . . C14 C 1.32499(16) 0.09712(16) 0.55736(13) 0.0215(3) Uani 1 1 d . . . . . H11 H 1.3059 0.0383 0.5218 0.026 Uiso 1 1 calc R U . . . C15 C 0.92355(15) 0.20156(15) 0.52991(13) 0.0170(3) Uani 1 1 d . . . . . H12 H 0.8694 0.1498 0.5215 0.020 Uiso 1 1 calc R U . . . C16 C 0.89278(15) 0.26402(15) 0.62451(13) 0.0170(3) Uani 1 1 d . . . . . H13 H 0.9582 0.2991 0.6418 0.020 Uiso 1 1 calc R U . . . C17 C 0.77824(15) 0.27507(15) 0.68852(13) 0.0169(3) Uani 1 1 d . . . . . H14 H 0.7160 0.2345 0.6742 0.020 Uiso 1 1 calc R U . . . C18 C 0.74058(14) 0.34766(15) 0.78224(13) 0.0163(3) Uani 1 1 d . . . . . C19 C 0.60192(15) 0.46640(15) 0.75505(13) 0.0180(3) Uani 1 1 d . . . . . C20 C 0.55358(19) 0.53120(19) 0.64258(15) 0.0303(4) Uani 1 1 d . . . . . H15 H 0.6026 0.4971 0.5814 0.036 Uiso 1 1 calc R U . . . C21 C 0.4338(2) 0.6460(2) 0.61802(16) 0.0421(5) Uani 1 1 d . . . . . H16 H 0.4020 0.6899 0.5403 0.051 Uiso 1 1 calc R U . . . C22 C 0.36062(19) 0.69655(19) 0.70624(16) 0.0328(4) Uani 1 1 d . . . . . H17 H 0.2779 0.7737 0.6894 0.039 Uiso 1 1 calc R U . . . C23 C 0.40877(18) 0.63404(18) 0.81874(15) 0.0280(4) Uani 1 1 d . . . . . H18 H 0.3597 0.6687 0.8797 0.034 Uiso 1 1 calc R U . . . C24 C 0.52896(17) 0.52043(18) 0.84279(14) 0.0253(4) Uani 1 1 d . . . . . H19 H 0.5621 0.4787 0.9203 0.030 Uiso 1 1 calc R U . . . C25 C 0.73710(15) 0.23820(15) 0.89702(12) 0.0163(3) Uani 1 1 d . . . . . C26 C 0.62358(15) 0.19274(16) 0.92668(13) 0.0196(3) Uani 1 1 d . . . . . H20 H 0.5444 0.2349 0.8778 0.024 Uiso 1 1 calc R U . . . C27 C 0.62536(16) 0.08713(17) 1.02638(14) 0.0222(3) Uani 1 1 d . . . . . H21 H 0.5473 0.0577 1.0455 0.027 Uiso 1 1 calc R U . . . C28 C 0.74047(16) 0.02359(16) 1.09886(14) 0.0223(3) Uani 1 1 d . . . . . H22 H 0.7421 -0.0497 1.1669 0.027 Uiso 1 1 calc R U . . . C29 C 0.85251(16) 0.06886(16) 1.07019(14) 0.0219(3) Uani 1 1 d . . . . . H23 H 0.9315 0.0265 1.1193 0.026 Uiso 1 1 calc R U . . . C30 C 0.85102(15) 0.17529(16) 0.97064(13) 0.0196(3) Uani 1 1 d . . . . . H24 H 0.9287 0.2055 0.9526 0.023 Uiso 1 1 calc R U . . . O3 O 0.8265(3) 0.4749(3) 0.9812(2) 0.0297(5) Uani 0.5 1 d . . P A -1 C31 C 0.9073(6) 0.5091(6) 1.0215(5) 0.0263(10) Uani 0.5 1 d . . P A -1 C32 C 0.8766(5) 0.5459(5) 1.1324(3) 0.0419(10) Uani 0.5 1 d . . P A -1 H25 H 0.7826 0.5486 1.1569 0.063 Uiso 0.5 1 calc R U P A -1 H26 H 0.8845 0.6367 1.1211 0.063 Uiso 0.5 1 calc R U P A -1 H27 H 0.9424 0.4768 1.1920 0.063 Uiso 0.5 1 calc R U P A -1 C33 C 1.0402(5) 0.5162(7) 0.9616(7) 0.0359(13) Uani 0.5 1 d . . P A -1 H28 H 1.0710 0.4498 0.9164 0.054 Uiso 0.5 1 calc R U P A -1 H29 H 1.1106 0.4939 1.0195 0.054 Uiso 0.5 1 calc R U P A -1 H30 H 1.0255 0.6094 0.9097 0.054 Uiso 0.5 1 calc R U P A -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0238(6) 0.0136(5) 0.0204(5) -0.0055(4) 0.0002(4) -0.0027(4) O2 0.0202(5) 0.0211(5) 0.0272(6) -0.0087(5) -0.0007(4) -0.0085(4) C1 0.0158(6) 0.0133(6) 0.0161(7) -0.0065(5) 0.0021(5) -0.0026(5) C2 0.0164(7) 0.0155(7) 0.0164(7) -0.0061(5) -0.0005(5) -0.0019(5) C3 0.0155(7) 0.0156(6) 0.0166(7) -0.0062(5) 0.0005(5) -0.0002(5) C4 0.0213(7) 0.0214(7) 0.0232(8) -0.0113(6) 0.0015(6) -0.0058(6) C5 0.0251(8) 0.0253(8) 0.0215(8) -0.0146(6) 0.0019(6) -0.0029(6) C6 0.0192(7) 0.0236(8) 0.0189(7) -0.0088(6) 0.0050(6) -0.0005(6) C7 0.0164(7) 0.0173(7) 0.0204(7) -0.0060(6) 0.0027(6) -0.0018(5) C8 0.0157(7) 0.0143(6) 0.0162(7) -0.0059(5) -0.0008(5) 0.0000(5) C9 0.0150(6) 0.0189(7) 0.0155(7) -0.0052(6) 0.0029(5) -0.0059(6) C10 0.0236(8) 0.0200(7) 0.0309(9) -0.0079(7) -0.0049(6) -0.0063(6) C11 0.0296(9) 0.0309(9) 0.0310(9) -0.0088(7) -0.0072(7) -0.0128(7) C12 0.0178(7) 0.0336(9) 0.0217(8) -0.0028(7) -0.0032(6) -0.0085(7) C13 0.0196(7) 0.0238(8) 0.0203(7) -0.0043(6) 0.0006(6) -0.0009(6) C14 0.0214(7) 0.0202(7) 0.0210(7) -0.0085(6) 0.0002(6) -0.0025(6) C15 0.0162(7) 0.0167(7) 0.0188(7) -0.0075(6) 0.0003(5) -0.0044(5) C16 0.0165(7) 0.0154(7) 0.0186(7) -0.0065(6) 0.0008(5) -0.0037(5) C17 0.0175(7) 0.0172(7) 0.0174(7) -0.0079(6) 0.0001(5) -0.0050(5) C18 0.0135(6) 0.0181(7) 0.0182(7) -0.0077(6) 0.0017(5) -0.0048(5) C19 0.0165(7) 0.0176(7) 0.0191(7) -0.0076(6) 0.0013(5) -0.0033(6) C20 0.0332(9) 0.0303(9) 0.0194(8) -0.0112(7) 0.0005(7) 0.0025(7) C21 0.0449(11) 0.0393(11) 0.0217(9) -0.0089(8) -0.0081(8) 0.0127(9) C22 0.0272(9) 0.0287(9) 0.0301(9) -0.0098(7) -0.0025(7) 0.0074(7) C23 0.0254(8) 0.0277(8) 0.0244(8) -0.0112(7) 0.0060(6) 0.0004(7) C24 0.0231(8) 0.0273(8) 0.0197(8) -0.0091(6) 0.0010(6) 0.0003(7) C25 0.0166(7) 0.0171(7) 0.0163(7) -0.0093(6) 0.0034(5) -0.0041(5) C26 0.0161(7) 0.0244(8) 0.0201(7) -0.0106(6) 0.0007(5) -0.0055(6) C27 0.0192(7) 0.0266(8) 0.0248(8) -0.0109(7) 0.0063(6) -0.0113(6) C28 0.0240(8) 0.0197(7) 0.0203(7) -0.0059(6) 0.0048(6) -0.0052(6) C29 0.0193(7) 0.0223(7) 0.0219(8) -0.0071(6) -0.0019(6) -0.0034(6) C30 0.0159(7) 0.0208(7) 0.0227(8) -0.0080(6) 0.0012(6) -0.0058(6) O3 0.0401(14) 0.0321(13) 0.0245(12) -0.0114(10) 0.0000(10) -0.0184(11) C31 0.033(3) 0.023(2) 0.023(2) -0.0053(18) -0.006(2) -0.009(2) C32 0.049(2) 0.060(3) 0.0284(19) -0.0203(19) -0.0024(17) -0.025(2) C33 0.032(3) 0.032(3) 0.040(3) -0.008(2) -0.003(3) -0.008(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C1 O1 H1 109.5 . . C1 O1 H31 109.5 . . H1 O1 H31 135.5 . . C18 O2 H2 109.5 . . C18 O2 H32 109.5 . . H2 O2 H32 114.2 . . O1 C1 C9 112.07(12) . . O1 C1 C8 112.70(12) . . C9 C1 C8 115.25(12) . . O1 C1 C2 113.37(12) . . C9 C1 C2 116.63(12) . . C8 C1 C2 84.14(11) . . C15 C2 C3 137.20(15) . . C15 C2 C1 133.32(14) . . C3 C2 C1 89.27(11) . . C4 C3 C8 122.18(14) . . C4 C3 C2 144.71(15) . . C8 C3 C2 93.11(12) . . C3 C4 C5 115.37(15) . . C3 C4 H3 122.3 . . C5 C4 H3 122.3 . . C6 C5 C4 121.94(15) . . C6 C5 H4 119.0 . . C4 C5 H4 119.0 . . C5 C6 C7 122.51(14) . . C5 C6 H5 118.7 . . C7 C6 H5 118.7 . . C8 C7 C6 114.93(15) . . C8 C7 H6 122.5 . . C6 C7 H6 122.5 . . C7 C8 C3 123.06(14) . . C7 C8 C1 143.46(15) . . C3 C8 C1 93.48(12) . . C10 C9 C14 118.71(14) . . C10 C9 C1 121.95(14) . . C14 C9 C1 119.30(14) . . C9 C10 C11 120.49(15) . . C9 C10 H7 119.8 . . C11 C10 H7 119.8 . . C12 C11 C10 120.13(16) . . C12 C11 H8 119.9 . . C10 C11 H8 119.9 . . C11 C12 C13 119.65(15) . . C11 C12 H9 120.2 . . C13 C12 H9 120.2 . . C14 C13 C12 120.14(15) . . C14 C13 H10 119.9 . . C12 C13 H10 119.9 . . C13 C14 C9 120.82(15) . . C13 C14 H11 119.6 . . C9 C14 H11 119.6 . . C2 C15 C16 122.42(14) . . C2 C15 H12 118.8 . . C16 C15 H12 118.8 . . C17 C16 C15 124.11(15) . . C17 C16 H13 117.9 . . C15 C16 H13 117.9 . . C16 C17 C18 124.70(14) . . C16 C17 H14 117.7 . . C18 C17 H14 117.7 . . O2 C18 C17 109.20(12) . . O2 C18 C25 108.98(12) . . C17 C18 C25 106.98(13) . . O2 C18 C19 108.43(13) . . C17 C18 C19 111.05(12) . . C25 C18 C19 112.14(12) . . C20 C19 C24 118.29(15) . . C20 C19 C18 121.23(14) . . C24 C19 C18 120.15(14) . . C19 C20 C21 120.68(16) . . C19 C20 H15 119.7 . . C21 C20 H15 119.7 . . C22 C21 C20 120.42(17) . . C22 C21 H16 119.8 . . C20 C21 H16 119.8 . . C23 C22 C21 119.51(16) . . C23 C22 H17 120.2 . . C21 C22 H17 120.2 . . C22 C23 C24 119.92(15) . . C22 C23 H18 120.0 . . C24 C23 H18 120.0 . . C23 C24 C19 121.15(15) . . C23 C24 H19 119.4 . . C19 C24 H19 119.4 . . C30 C25 C26 118.34(14) . . C30 C25 C18 120.41(13) . . C26 C25 C18 121.12(13) . . C27 C26 C25 120.73(14) . . C27 C26 H20 119.6 . . C25 C26 H20 119.6 . . C26 C27 C28 120.56(15) . . C26 C27 H21 119.7 . . C28 C27 H21 119.7 . . C29 C28 C27 118.86(15) . . C29 C28 H22 120.6 . . C27 C28 H22 120.6 . . C28 C29 C30 120.84(15) . . C28 C29 H23 119.6 . . C30 C29 H23 119.6 . . C29 C30 C25 120.66(15) . . C29 C30 H24 119.7 . . C25 C30 H24 119.7 . . O3 C31 C32 120.6(5) . . O3 C31 C33 121.6(4) . . C32 C31 C33 117.8(4) . . C31 C32 H25 109.5 . . C31 C32 H26 109.5 . . H25 C32 H26 109.5 . . C31 C32 H27 109.5 . . H25 C32 H27 109.5 . . H26 C32 H27 109.5 . . C31 C33 H28 109.5 . . C31 C33 H29 109.5 . . H28 C33 H29 109.5 . . C31 C33 H30 109.5 . . H28 C33 H30 109.5 . . H29 C33 H30 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 C1 1.4241(18) . O1 H1 0.8400 . O1 H31 0.8400 . O2 C18 1.4261(19) . O2 H2 0.8400 . O2 H32 0.8400 . C1 C9 1.521(2) . C1 C8 1.539(2) . C1 C2 1.565(2) . C2 C15 1.337(2) . C2 C3 1.473(2) . C3 C4 1.389(2) . C3 C8 1.390(2) . C4 C5 1.398(2) . C4 H3 0.9500 . C5 C6 1.394(2) . C5 H4 0.9500 . C6 C7 1.397(2) . C6 H5 0.9500 . C7 C8 1.383(2) . C7 H6 0.9500 . C9 C10 1.388(2) . C9 C14 1.396(2) . C10 C11 1.396(2) . C10 H7 0.9500 . C11 C12 1.386(3) . C11 H8 0.9500 . C12 C13 1.386(3) . C12 H9 0.9500 . C13 C14 1.385(2) . C13 H10 0.9500 . C14 H11 0.9500 . C15 C16 1.456(2) . C15 H12 0.9500 . C16 C17 1.337(2) . C16 H13 0.9500 . C17 C18 1.516(2) . C17 H14 0.9500 . C18 C25 1.533(2) . C18 C19 1.538(2) . C19 C20 1.382(2) . C19 C24 1.396(2) . C20 C21 1.393(2) . C20 H15 0.9500 . C21 C22 1.384(3) . C21 H16 0.9500 . C22 C23 1.380(3) . C22 H17 0.9500 . C23 C24 1.388(2) . C23 H18 0.9500 . C24 H19 0.9500 . C25 C30 1.389(2) . C25 C26 1.399(2) . C26 C27 1.383(2) . C26 H20 0.9500 . C27 C28 1.390(2) . C27 H21 0.9500 . C28 C29 1.383(2) . C28 H22 0.9500 . C29 C30 1.387(2) . C29 H23 0.9500 . C30 H24 0.9500 . O3 C31 1.217(6) . C31 C32 1.489(7) . C31 C33 1.501(6) . C32 H25 0.9800 . C32 H26 0.9800 . C32 H27 0.9800 . C33 H28 0.9800 . C33 H29 0.9800 . C33 H30 0.9800 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O1 . . 2_766 2.821(2) 0.840 2.013 161.2 no O1 H31 O2 . . 2_766 2.8009(19) 0.8400(11) 1.9726(14) 168.55(10) no O2 H2 O3 . . . 2.639(3) 0.840 1.806 171.7 no O2 H32 O1 . . 2_766 2.8009(19) 0.8400(11) 2.0077(14) 157.14(8) no 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 O1 C1 C2 C15 -62.4(2) . . . . C9 C1 C2 C15 70.1(2) . . . . C8 C1 C2 C15 -174.59(17) . . . . O1 C1 C2 C3 112.85(12) . . . . C9 C1 C2 C3 -114.74(13) . . . . C8 C1 C2 C3 0.62(10) . . . . C15 C2 C3 C4 -6.0(4) . . . . C1 C2 C3 C4 179.1(2) . . . . C15 C2 C3 C8 174.19(18) . . . . C1 C2 C3 C8 -0.68(11) . . . . C8 C3 C4 C5 -0.9(2) . . . . C2 C3 C4 C5 179.36(19) . . . . C3 C4 C5 C6 0.5(2) . . . . C4 C5 C6 C7 0.2(2) . . . . C5 C6 C7 C8 -0.5(2) . . . . C6 C7 C8 C3 0.2(2) . . . . C6 C7 C8 C1 179.69(17) . . . . C4 C3 C8 C7 0.5(2) . . . . C2 C3 C8 C7 -179.60(14) . . . . C4 C3 C8 C1 -179.17(14) . . . . C2 C3 C8 C1 0.70(11) . . . . O1 C1 C8 C7 66.8(2) . . . . C9 C1 C8 C7 -63.5(3) . . . . C2 C1 C8 C7 179.8(2) . . . . O1 C1 C8 C3 -113.57(13) . . . . C9 C1 C8 C3 116.07(14) . . . . C2 C1 C8 C3 -0.66(11) . . . . O1 C1 C9 C10 3.91(19) . . . . C8 C1 C9 C10 134.58(15) . . . . C2 C1 C9 C10 -129.10(15) . . . . O1 C1 C9 C14 -173.65(12) . . . . C8 C1 C9 C14 -42.99(19) . . . . C2 C1 C9 C14 53.33(18) . . . . C14 C9 C10 C11 1.8(2) . . . . C1 C9 C10 C11 -175.74(15) . . . . C9 C10 C11 C12 0.1(3) . . . . C10 C11 C12 C13 -1.9(3) . . . . C11 C12 C13 C14 1.8(2) . . . . C12 C13 C14 C9 0.2(2) . . . . C10 C9 C14 C13 -2.0(2) . . . . C1 C9 C14 C13 175.67(14) . . . . C3 C2 C15 C16 -174.89(15) . . . . C1 C2 C15 C16 -1.9(2) . . . . C2 C15 C16 C17 167.44(15) . . . . C15 C16 C17 C18 -176.00(13) . . . . C16 C17 C18 O2 1.0(2) . . . . C16 C17 C18 C25 -116.78(16) . . . . C16 C17 C18 C19 120.55(16) . . . . O2 C18 C19 C20 94.83(18) . . . . C17 C18 C19 C20 -25.2(2) . . . . C25 C18 C19 C20 -144.78(16) . . . . O2 C18 C19 C24 -78.51(18) . . . . C17 C18 C19 C24 161.51(15) . . . . C25 C18 C19 C24 41.9(2) . . . . C24 C19 C20 C21 -1.1(3) . . . . C18 C19 C20 C21 -174.57(18) . . . . C19 C20 C21 C22 -0.4(3) . . . . C20 C21 C22 C23 1.3(4) . . . . C21 C22 C23 C24 -0.7(3) . . . . C22 C23 C24 C19 -0.9(3) . . . . C20 C19 C24 C23 1.7(3) . . . . C18 C19 C24 C23 175.27(16) . . . . O2 C18 C25 C30 -21.21(18) . . . . C17 C18 C25 C30 96.75(16) . . . . C19 C18 C25 C30 -141.27(14) . . . . O2 C18 C25 C26 163.03(13) . . . . C17 C18 C25 C26 -79.01(16) . . . . C19 C18 C25 C26 42.97(19) . . . . C30 C25 C26 C27 -0.5(2) . . . . C18 C25 C26 C27 175.37(13) . . . . C25 C26 C27 C28 -0.3(2) . . . . C26 C27 C28 C29 0.7(2) . . . . C27 C28 C29 C30 -0.3(2) . . . . C28 C29 C30 C25 -0.5(2) . . . . C26 C25 C30 C29 0.8(2) . . . . C18 C25 C30 C29 -175.03(14) . . . .