#------------------------------------------------------------------------------ #$Date: 2020-02-14 02:18:21 +0200 (Fri, 14 Feb 2020) $ #$Revision: 248139 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557314.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_1557314 loop_ _publ_author_name 'Ye, Yan-Song' 'Li, Wen-Yan' 'Du, Shu-Zong' 'Yang, Jian' 'Nian, Yin' 'Xu, Gang' _publ_section_title ; Congenetic hybrids derived from dearomatized isoprenylated acylphloroglucinol with opposite effects on Cav3.1 low voltage-gated Ca2+ channel. ; _journal_name_full 'Journal of medicinal chemistry' _journal_paper_doi 10.1021/acs.jmedchem.9b02056 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C33 H40 O4' _chemical_formula_sum 'C33 H40 O4' _chemical_formula_weight 500.65 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.4737(2) _cell_length_b 15.6173(3) _cell_length_c 18.4421(4) _cell_measurement_reflns_used 9975 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 70.23 _cell_measurement_theta_min 3.71 _cell_volume 2728.58(10) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_unetI/netI 0.0241 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16977 _diffrn_reflns_point_group_measured_fraction_full 0.964 _diffrn_reflns_point_group_measured_fraction_max 0.941 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 70.223 _diffrn_reflns_theta_min 3.709 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.219 _exptl_crystal_description prism _exptl_crystal_F_000 1080 _exptl_crystal_size_max 0.660 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.180 _exptl_transmission_factor_max 0.5220 _exptl_transmission_factor_min 0.3938 _refine_diff_density_max 0.194 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.045 _refine_ls_abs_structure_details ; Flack x determined using 2005 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 341 _refine_ls_number_reflns 4893 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.070 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0291 _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^)+(0.0413P)^2^+0.5568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.0754 _reflns_Friedel_coverage 0.705 _reflns_Friedel_fraction_full 0.932 _reflns_Friedel_fraction_max 0.898 _reflns_number_gt 4887 _reflns_number_total 4893 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jm9b02056_si_003.cif _cod_data_source_block cu_rxn56_0m _cod_database_code 1557314 _shelx_shelxl_version_number 2014/7 _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 0.686 _shelx_estimated_absorpt_t_max 0.897 _shelx_res_file ; cu_rxn56_0m.res created by SHELXL-2014/7 TITL cu_rxn56_0m in P2(1)2(1)2(1) CELL 1.54178 9.4737 15.6173 18.4421 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0003 0.0004 0.000 0.000 0.000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H O UNIT 132 160 16 L.S. 10 ACTA BOND $H FMAP 2 PLAN -5 CONF HTAB SIZE 0.180 0.220 0.660 TEMP -173.000 WGHT 0.041300 0.556800 FVAR 0.25764 O1 3 0.504798 -0.073372 0.056144 11.00000 0.02258 0.02186 = 0.02815 -0.00519 -0.00992 0.00254 O2 3 0.777251 0.053461 0.030579 11.00000 0.02953 0.02137 = 0.01607 -0.00140 0.00303 -0.00199 O3 3 0.866736 0.179040 0.258632 11.00000 0.01937 0.02078 = 0.02245 -0.00513 -0.00140 -0.00453 O4 3 0.575004 -0.049862 0.243523 11.00000 0.02184 0.01494 = 0.01530 -0.00062 0.00028 -0.00437 C1 1 0.882441 -0.294153 0.088876 11.00000 0.02095 0.01407 = 0.05938 0.00389 0.01387 0.00259 AFIX 43 H1 2 0.940327 -0.343824 0.088980 11.00000 -1.20000 AFIX 0 C2 1 0.790256 -0.279697 0.031675 11.00000 0.02978 0.01421 = 0.04199 -0.00765 0.01529 -0.00353 AFIX 43 H38 2 0.787991 -0.318124 -0.008240 11.00000 -1.20000 AFIX 0 C3 1 0.701517 -0.209160 0.032836 11.00000 0.02285 0.01735 = 0.02453 -0.00363 0.00648 -0.00494 AFIX 43 H37 2 0.634695 -0.201008 -0.004947 11.00000 -1.20000 AFIX 0 C4 1 0.710211 -0.150057 0.089477 11.00000 0.01587 0.01344 = 0.02010 0.00092 0.00326 -0.00105 C5 1 0.614248 -0.074379 0.090114 11.00000 0.01838 0.01388 = 0.01381 -0.00019 0.00036 -0.00230 C6 1 0.659772 0.003194 0.133112 11.00000 0.01360 0.01259 = 0.01842 -0.00160 -0.00223 0.00241 C7 1 0.750098 0.063385 0.094873 11.00000 0.01671 0.01346 = 0.01722 -0.00047 -0.00157 0.00377 C8 1 0.819358 0.137853 0.136363 11.00000 0.01603 0.01345 = 0.01878 0.00032 0.00006 -0.00102 C9 1 0.981684 0.132683 0.125011 11.00000 0.01587 0.01824 = 0.02295 0.00023 0.00310 -0.00145 AFIX 23 H9 2 1.001072 0.127159 0.072469 11.00000 -1.20000 H10 2 1.024594 0.187031 0.141674 11.00000 -1.20000 AFIX 0 C10 1 1.052129 0.059474 0.164112 11.00000 0.01391 0.02227 = 0.01787 -0.00018 0.00051 -0.00295 AFIX 43 H8 2 1.056346 0.063858 0.215445 11.00000 -1.20000 AFIX 0 C11 1 1.109164 -0.010632 0.135231 11.00000 0.01764 0.02248 = 0.02158 0.00014 -0.00067 0.00076 C12 1 1.185212 -0.075327 0.181426 11.00000 0.02144 0.02373 = 0.02989 0.00200 -0.00248 0.00234 AFIX 137 H4 2 1.178638 -0.058476 0.232502 11.00000 -1.50000 H3 2 1.284670 -0.077857 0.166974 11.00000 -1.50000 H2 2 1.141842 -0.131769 0.174878 11.00000 -1.50000 AFIX 0 C13 1 0.890425 -0.236640 0.145677 11.00000 0.02209 0.02518 = 0.04455 0.01026 -0.00167 0.00501 AFIX 43 H40 2 0.952662 -0.247013 0.185101 11.00000 -1.20000 AFIX 0 C14 1 0.807064 -0.163747 0.144752 11.00000 0.02127 0.01914 = 0.02693 -0.00090 -0.00246 0.00185 AFIX 43 H39 2 0.816311 -0.122629 0.182416 11.00000 -1.20000 AFIX 0 C15 1 1.107557 -0.032251 0.056137 11.00000 0.04440 0.03720 = 0.02387 -0.00482 -0.00208 0.01909 AFIX 137 H5 2 1.056066 0.012182 0.029522 11.00000 -1.50000 H7 2 1.060862 -0.087617 0.049057 11.00000 -1.50000 H6 2 1.204690 -0.035466 0.038064 11.00000 -1.50000 AFIX 0 C16 1 0.790162 0.138942 0.218394 11.00000 0.01456 0.01127 = 0.01892 -0.00145 -0.00071 0.00117 C17 1 0.665626 0.089317 0.249944 11.00000 0.01396 0.01385 = 0.01670 -0.00276 0.00036 -0.00056 C18 1 0.632872 0.012972 0.204005 11.00000 0.01157 0.01215 = 0.01986 0.00053 -0.00219 0.00113 C19 1 0.612120 -0.038363 0.321589 11.00000 0.02885 0.01746 = 0.01389 -0.00131 -0.00087 -0.00596 C20 1 0.695617 0.047243 0.324859 11.00000 0.02080 0.01591 = 0.01656 -0.00110 -0.00092 -0.00262 AFIX 13 H11 2 0.798758 0.037861 0.333219 11.00000 -1.20000 AFIX 0 C21 1 0.631282 0.108095 0.380652 11.00000 0.02844 0.01919 = 0.01628 -0.00417 0.00097 -0.00397 AFIX 23 H24 2 0.688323 0.160796 0.386251 11.00000 -1.20000 H23 2 0.619842 0.080162 0.428481 11.00000 -1.20000 AFIX 0 C22 1 0.488298 0.126655 0.344879 11.00000 0.02305 0.02041 = 0.02006 -0.00554 0.00539 -0.00172 AFIX 13 H18 2 0.443497 0.177307 0.368767 11.00000 -1.20000 AFIX 0 C23 1 0.530425 0.150281 0.265388 11.00000 0.01476 0.01620 = 0.02113 -0.00376 0.00249 0.00097 C24 1 0.412713 0.138317 0.209930 11.00000 0.01637 0.02102 = 0.02608 -0.00342 -0.00127 0.00254 AFIX 137 H13 2 0.327796 0.168387 0.226436 11.00000 -1.50000 H14 2 0.391953 0.077164 0.204614 11.00000 -1.50000 H12 2 0.442729 0.161708 0.163094 11.00000 -1.50000 AFIX 0 C25 1 0.570769 0.245680 0.266574 11.00000 0.02305 0.01466 = 0.02609 -0.00417 0.00273 0.00221 AFIX 137 H17 2 0.602449 0.263185 0.218208 11.00000 -1.50000 H15 2 0.647107 0.254790 0.301595 11.00000 -1.50000 H16 2 0.488453 0.279842 0.280673 11.00000 -1.50000 AFIX 0 C26 1 0.391725 0.047598 0.353636 11.00000 0.02470 0.02897 = 0.02522 -0.00337 0.00852 -0.00644 AFIX 23 H19 2 0.329760 0.056207 0.396243 11.00000 -1.20000 H20 2 0.330671 0.042519 0.310282 11.00000 -1.20000 AFIX 0 C27 1 0.474203 -0.035685 0.363377 11.00000 0.03466 0.02250 = 0.02127 -0.00346 0.00701 -0.01019 AFIX 23 H22 2 0.494626 -0.043715 0.415582 11.00000 -1.20000 H21 2 0.414285 -0.084104 0.347467 11.00000 -1.20000 AFIX 0 C28 1 0.699543 -0.115548 0.343341 11.00000 0.03917 0.01657 = 0.02210 0.00192 -0.00449 -0.00286 AFIX 137 H25 2 0.643912 -0.167802 0.336340 11.00000 -1.50000 H26 2 0.726489 -0.110539 0.394471 11.00000 -1.50000 H27 2 0.784720 -0.118180 0.313271 11.00000 -1.50000 AFIX 0 C29 1 0.761783 0.220664 0.098778 11.00000 0.02013 0.01491 = 0.01929 0.00172 0.00035 -0.00028 AFIX 23 H35 2 0.769795 0.213039 0.045646 11.00000 -1.20000 H36 2 0.660114 0.225934 0.110359 11.00000 -1.20000 AFIX 0 C30 1 0.832900 0.303258 0.118783 11.00000 0.02147 0.01651 = 0.02191 -0.00163 0.00235 0.00158 AFIX 43 H34 2 0.842763 0.315822 0.168929 11.00000 -1.20000 AFIX 0 C31 1 0.883166 0.360206 0.071810 11.00000 0.01690 0.01657 = 0.02858 -0.00025 0.00364 0.00254 C32 1 0.882341 0.348883 -0.009416 11.00000 0.04948 0.02871 = 0.02688 0.00345 0.00578 -0.00982 AFIX 137 H29 2 0.870212 0.288124 -0.021146 11.00000 -1.50000 H28 2 0.971962 0.369319 -0.029536 11.00000 -1.50000 H30 2 0.804313 0.381850 -0.030339 11.00000 -1.50000 AFIX 0 C33 1 0.945785 0.443966 0.096043 11.00000 0.02524 0.01764 = 0.03464 -0.00081 0.00590 -0.00250 AFIX 137 H31 2 0.947221 0.446202 0.149144 11.00000 -1.50000 H33 2 0.888567 0.491325 0.077296 11.00000 -1.50000 H32 2 1.042363 0.448941 0.077478 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM cu_rxn56_0m in P2(1)2(1)2(1) REM R1 = 0.0291 for 4887 Fo > 4sig(Fo) and 0.0291 for all 4893 data REM 341 parameters refined using 0 restraints END WGHT 0.0417 0.5531 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.194, deepest hole -0.217, 1-sigma level 0.045 Q1 1 0.8866 0.4000 -0.0389 11.00000 0.05 0.19 Q2 1 0.7836 0.3140 -0.0356 11.00000 0.05 0.18 Q3 1 0.7945 0.1386 0.1750 11.00000 0.05 0.14 Q4 1 1.3026 -0.1070 0.0933 11.00000 0.05 0.14 Q5 1 0.7924 0.1794 0.1212 11.00000 0.05 0.13 ; _shelx_res_checksum 13280 _shelx_hkl_file ; -1 0 0 -0.11 0.01 -1 0 0 -0.11 0.01 -2 0 0 97.12 3.48 -2 0 0 108.48 3.99 -3 0 0 0.09 0.03 -5 0 0 -0.11 0.02 -6 0 0 6.96 0.28 -7 0 0 0.34 0.06 -8 0 0 18.00 0.69 -8 0 0 18.06 0.67 -9 0 0 0.00 0.04 -9 0 0 -0.04 0.05 -10 0 0 76.41 2.61 -11 0 0 0.01 0.03 -11 0 0 0.02 0.03 0 -1 0 -0.39 0.03 -1 -1 0 854.35 30.73 -1 1 0 805.52 30.23 -1 1 0 880.73 31.34 -2 1 0 360.95 14.54 -2 1 0 374.05 12.46 -2 -1 0 365.93 12.40 -3 -1 0 692.11 22.80 -3 1 0 668.83 25.64 -3 1 0 670.97 25.65 -5 -1 0 24.80 0.88 -5 1 0 25.80 0.88 -6 -1 0 2.62 0.14 -6 1 0 2.77 0.14 -7 1 0 4.33 0.21 -7 -1 0 4.72 0.22 -8 -1 0 8.97 0.38 -8 -1 0 9.89 0.40 -8 1 0 9.06 0.38 -8 1 0 9.22 0.39 -9 -1 0 1.94 0.14 -9 1 0 1.82 0.13 -9 1 0 1.73 0.14 -9 -1 0 1.77 0.15 -10 1 0 4.50 0.22 -10 -1 0 4.45 0.22 -11 -1 0 0.06 0.04 -11 1 0 0.08 0.03 -11 1 0 0.06 0.04 0 2 0 588.27 21.69 0 -2 0 601.02 22.24 -1 2 0 34.40 1.20 -1 2 0 35.40 1.23 -2 2 0 220.69 7.37 -2 -2 0 211.22 7.38 -2 2 0 212.86 7.47 -3 -2 0 58.77 2.02 -3 2 0 59.70 2.02 -3 2 0 59.15 2.05 -4 2 0 7.80 0.32 -5 2 0 143.93 4.82 -5 -2 0 144.37 4.83 -6 -2 0 1.46 0.10 -6 2 0 1.14 0.08 -7 -2 0 32.95 1.15 -7 2 0 31.50 1.14 -8 -2 0 3.85 0.21 -8 2 0 3.27 0.18 -8 -2 0 3.47 0.19 -8 2 0 3.76 0.20 -9 2 0 32.63 1.19 -9 2 0 33.93 1.21 -9 -2 0 34.46 1.20 -9 -2 0 33.32 1.21 -10 2 0 1.30 0.09 -10 2 0 1.30 0.11 -10 -2 0 1.29 0.11 -11 2 0 7.47 0.29 -11 2 0 8.24 0.31 -11 -2 0 7.54 0.30 -1 3 0 82.98 2.86 1 -3 0 75.05 2.73 -1 3 0 84.91 2.75 -2 3 0 891.20 34.93 2 -3 0 886.10 31.03 -2 3 0 991.61 31.29 -3 3 0 51.21 1.78 -3 3 0 52.05 1.81 -4 3 0 85.55 2.92 -5 -3 0 27.44 0.95 -5 3 0 26.96 0.94 -6 3 0 0.43 0.05 -6 -3 0 0.20 0.05 -7 -3 0 46.84 1.59 -7 3 0 44.14 1.58 -8 -3 0 117.22 4.11 -8 3 0 123.43 4.12 -8 -3 0 127.57 4.13 -8 3 0 118.06 4.11 -9 -3 0 0.61 0.10 -9 -3 0 0.67 0.09 -9 3 0 0.66 0.08 -9 3 0 0.59 0.09 10 -3 0 4.04 0.27 -10 -3 0 4.96 0.22 -10 3 0 4.99 0.21 -10 3 0 4.62 0.22 -11 3 0 29.61 1.02 -11 3 0 29.37 1.01 -11 -3 0 29.57 1.02 0 4 0 60.20 2.10 0 -4 0 62.90 2.10 0 -4 0 61.13 2.08 -1 4 0 64.81 2.12 1 -4 0 55.82 2.08 -1 4 0 63.20 2.11 -2 4 0 0.16 0.05 -2 4 0 0.28 0.06 2 -4 0 0.17 0.05 -3 4 0 557.79 20.30 -3 4 0 570.92 19.08 3 -4 0 543.36 18.99 -4 4 0 125.40 4.26 -5 -4 0 2.32 0.13 -5 4 0 2.60 0.17 -5 4 0 2.45 0.12 -6 -4 0 115.23 3.86 -6 4 0 113.45 3.85 -7 -4 0 0.80 0.10 -7 4 0 0.93 0.09 -8 4 0 2.50 0.15 -8 -4 0 2.14 0.15 -8 -4 0 2.44 0.16 -8 4 0 2.05 0.15 -9 4 0 0.10 0.06 -9 -4 0 0.07 0.05 9 -4 0 0.30 0.09 -9 4 0 0.22 0.05 -9 -4 0 0.26 0.07 -10 4 0 15.98 0.62 -10 -4 0 16.98 0.62 -10 4 0 17.60 0.61 -11 4 0 2.74 0.13 -11 -4 0 2.62 0.13 -11 4 0 2.53 0.12 -1 5 0 29.93 1.07 1 -5 0 27.45 1.02 -1 5 0 28.86 1.02 -2 5 0 99.51 3.46 2 -5 0 99.09 3.42 -2 5 0 102.94 4.11 3 -5 0 0.94 0.11 -3 5 0 0.62 0.08 -4 5 0 23.10 0.88 -5 5 0 0.81 0.10 -5 5 0 0.81 0.08 -5 -5 0 0.91 0.08 -6 -5 0 0.78 0.08 -6 5 0 0.72 0.06 -7 -5 0 0.36 0.08 -8 -5 0 5.01 0.25 8 -5 0 5.32 0.28 -8 -5 0 4.91 0.26 -9 -5 0 0.14 0.06 -9 -5 0 0.10 0.05 9 -5 0 0.12 0.09 -9 5 0 0.07 0.04 9 5 0 0.12 0.08 -9 5 0 0.14 0.05 -10 5 0 0.52 0.07 -10 5 0 0.65 0.07 -10 -5 0 0.67 0.08 -11 5 0 4.78 0.19 -11 5 0 4.63 0.21 0 -6 0 2.87 0.14 -1 6 0 251.93 8.41 1 -6 0 246.33 8.60 -2 6 0 9.33 0.39 -2 6 0 9.43 0.45 2 -6 0 9.67 0.41 -3 6 0 50.65 1.96 3 -6 0 55.98 1.92 -3 6 0 56.17 1.91 -4 6 0 106.36 3.66 -5 6 0 26.55 0.96 -6 6 0 32.24 1.12 -7 6 0 0.81 0.09 -7 -6 0 1.16 0.12 -8 6 0 2.04 0.13 -8 -6 0 2.12 0.14 -8 -6 0 1.85 0.16 8 -6 0 2.06 0.19 -9 -6 0 24.10 0.90 9 -6 0 25.59 0.97 -9 6 0 25.38 0.90 -9 6 0 24.92 0.89 -10 -6 0 1.28 0.10 -10 6 0 1.26 0.09 -10 6 0 1.54 0.09 0 -7 0 -0.17 0.02 1 -7 0 3.49 0.19 -1 7 0 3.47 0.24 2 -7 0 492.71 16.54 -2 7 0 467.99 16.63 -3 7 0 22.07 0.82 -3 7 0 19.27 0.87 3 -7 0 21.00 0.82 -4 7 0 23.53 0.87 -4 7 0 22.68 0.92 4 -7 0 24.06 0.94 -5 7 0 15.26 0.60 -6 7 0 111.26 3.76 7 -7 0 230.51 7.53 -7 -7 0 211.17 7.47 -7 7 0 226.90 7.47 8 -7 0 22.66 0.87 -8 7 0 22.05 0.80 -8 7 0 22.70 0.79 -8 -7 0 20.54 0.80 -9 -7 0 1.63 0.12 -9 7 0 1.62 0.10 -9 7 0 1.48 0.11 -10 7 0 0.60 0.06 -10 7 0 0.51 0.05 0 8 0 85.70 3.10 0 -8 0 89.75 3.02 -1 -8 0 28.37 1.08 -1 8 0 29.67 1.17 1 -8 0 31.11 1.07 1 -8 0 28.72 1.09 -2 -8 0 9.45 0.41 2 -8 0 9.00 0.42 -2 8 0 9.43 0.49 2 -8 0 9.21 0.42 3 -8 0 2.00 0.17 -3 8 0 1.73 0.20 -4 8 0 14.51 0.57 4 -8 0 13.63 0.62 -4 8 0 13.43 0.64 -5 8 0 3.30 0.20 -6 8 0 5.07 0.24 7 -8 0 0.52 0.11 -7 8 0 0.32 0.06 -7 8 0 0.33 0.06 -8 8 0 3.87 0.19 -8 8 0 3.70 0.18 -9 8 0 32.78 1.15 -9 8 0 34.67 1.18 -10 8 0 6.44 0.25 0 -9 0 0.09 0.06 0 9 0 0.09 0.07 1 -9 0 3.08 0.21 -1 9 0 3.19 0.27 1 -9 0 3.32 0.18 -1 -9 0 3.19 0.21 2 -9 0 23.06 0.94 -2 9 0 25.13 1.06 -2 -9 0 24.26 0.93 2 -9 0 24.40 0.93 -3 -9 0 22.60 0.89 3 -9 0 23.58 0.93 -4 9 0 0.38 0.09 -4 -9 0 0.62 0.11 4 -9 0 0.48 0.11 -5 -9 0 6.14 0.34 5 -9 0 6.19 0.38 -5 9 0 6.07 0.31 -6 9 0 2.14 0.14 -6 9 0 2.06 0.15 -6 -9 0 2.24 0.20 -7 9 0 11.21 0.44 -8 9 0 32.50 1.14 -9 9 0 4.73 0.21 -10 9 0 1.11 0.07 0 -10 0 469.03 15.72 1 -10 0 54.76 1.94 -1 -10 0 52.33 1.92 -2 -10 0 57.55 2.03 2 -10 0 56.19 2.00 2 -10 0 56.36 2.04 -3 -10 0 17.54 0.71 3 -10 0 15.90 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-7 17 0.08 0.03 -5 -7 -17 0.12 0.03 6 -7 17 0.12 0.03 -6 -7 -17 0.22 0.03 0 8 -17 5.78 0.29 0 8 17 6.33 0.28 1 8 -17 18.17 0.76 -1 8 17 21.04 0.72 1 8 17 19.23 0.73 -1 8 -17 19.95 0.73 -2 8 17 4.66 0.19 2 8 -17 3.80 0.25 -2 -8 -17 4.22 0.18 2 8 17 4.61 0.22 -3 -8 -17 11.63 0.42 3 8 17 11.58 0.50 4 -8 17 6.61 0.26 -4 -8 -17 7.12 0.26 5 -8 17 0.86 0.06 -5 -8 -17 0.88 0.06 0 9 -17 3.97 0.22 0 9 17 3.99 0.20 -1 9 17 4.49 0.20 1 9 17 4.00 0.21 -2 -9 -17 10.91 0.39 2 9 17 10.51 0.43 -3 -9 -17 5.88 0.23 3 9 17 5.72 0.26 -4 -9 -17 6.13 0.23 4 -9 17 5.85 0.23 -5 -9 -17 1.56 0.07 0 10 17 7.26 0.30 -1 10 17 4.86 0.21 1 10 17 4.83 0.23 -2 -10 -17 3.89 0.16 2 10 17 4.05 0.20 -3 -10 -17 6.82 0.25 3 10 17 6.57 0.28 -4 -10 -17 1.56 0.08 0 11 17 9.15 0.36 -1 11 17 7.19 0.28 1 11 17 7.32 0.30 -2 -11 -17 3.93 0.16 2 11 17 4.20 0.19 -3 -11 -17 0.39 0.04 3 11 17 0.42 0.07 0 12 17 17.99 0.63 1 12 17 0.28 0.05 0 0 -18 50.62 1.85 0 0 18 54.13 2.39 0 0 18 52.99 1.80 0 0 18 53.23 1.87 1 0 18 95.31 3.22 1 0 -18 91.68 3.20 1 0 18 89.63 3.27 -1 0 -18 92.50 3.25 1 0 -18 93.67 3.27 -1 0 18 97.17 3.27 -1 0 18 100.64 3.73 -1 0 18 100.75 3.23 1 0 18 94.92 3.93 2 0 -18 17.70 0.64 2 0 18 16.20 0.61 -2 0 18 17.47 0.61 -2 0 -18 15.77 0.62 -2 0 18 16.00 0.63 2 0 -18 16.05 0.67 2 0 18 15.90 0.65 3 0 -18 0.30 0.08 -3 0 -18 0.30 0.05 3 0 -18 0.26 0.08 -3 0 18 0.28 0.04 -3 0 -18 0.31 0.06 3 0 18 0.39 0.06 4 0 -18 11.43 0.50 -4 0 -18 11.97 0.43 4 0 18 11.59 0.45 -5 0 -18 0.68 0.06 5 0 18 0.65 0.08 -6 0 -18 0.05 0.02 6 0 18 0.04 0.03 6 0 18 0.08 0.04 0 1 -18 11.49 0.50 0 1 18 11.76 0.52 0 1 18 13.08 0.46 0 1 18 11.94 0.89 0 -1 18 12.19 0.87 0 -1 18 12.19 0.51 1 1 -18 24.66 0.98 -1 1 18 26.01 0.98 1 -1 18 25.75 1.49 1 1 -18 25.97 0.93 -1 1 18 26.54 0.94 1 -1 18 23.98 0.96 -1 1 18 26.46 1.35 1 -1 18 27.06 0.92 -1 -1 18 28.01 0.93 1 1 18 26.72 0.93 1 1 18 25.31 1.51 -1 1 -18 25.29 0.96 1 1 18 25.12 0.98 -1 -1 18 26.37 0.96 -1 -1 18 26.73 1.32 -2 1 18 12.01 0.50 2 -1 18 13.04 0.47 2 1 -18 12.57 0.50 -2 1 18 12.66 0.47 2 1 -18 11.56 0.52 2 -1 18 11.18 0.49 2 1 18 11.32 0.51 2 1 18 12.53 0.48 -2 -1 18 12.51 0.45 -2 -1 18 11.97 0.48 -2 1 -18 11.49 0.48 2 -1 -18 12.01 0.47 -3 1 18 0.35 0.05 3 -1 18 0.33 0.06 3 1 -18 0.23 0.07 3 1 -18 0.27 0.09 -3 -1 -18 0.35 0.05 -3 1 -18 0.34 0.05 -3 1 -18 0.33 0.06 -3 -1 18 0.50 0.05 3 -1 -18 0.24 0.07 3 1 18 0.34 0.06 -4 -1 -18 3.35 0.15 -4 1 18 3.24 0.13 4 -1 18 3.40 0.17 4 1 -18 3.09 0.21 4 -1 -18 3.23 0.20 4 1 18 3.35 0.17 -4 1 -18 3.29 0.15 5 -1 18 2.06 0.12 -5 -1 -18 1.90 0.10 5 -1 18 1.93 0.12 5 1 18 2.06 0.13 -5 1 -18 1.88 0.10 6 -1 18 5.05 0.21 6 -1 18 5.18 0.21 -6 -1 -18 4.78 0.19 6 1 18 5.11 0.22 -6 1 -18 4.73 0.19 6 1 18 5.43 0.21 0 2 18 4.14 0.52 0 2 -18 3.96 0.23 0 -2 18 4.34 0.20 0 2 18 4.08 0.20 0 2 18 4.14 0.25 0 -2 18 4.08 0.48 0 -2 18 4.11 0.22 1 2 -18 3.04 0.18 1 -2 18 2.84 0.18 -1 2 18 2.90 0.39 1 -2 18 2.90 0.15 1 2 -18 2.76 0.20 -1 2 18 2.79 0.19 1 2 18 3.01 0.50 1 2 18 3.06 0.21 1 2 18 3.09 0.17 -1 2 -18 2.87 0.18 -1 -2 18 2.93 0.18 -1 -2 18 3.05 0.15 2 2 -18 0.95 0.13 2 -2 18 0.97 0.09 -2 2 18 0.90 0.16 2 2 -18 1.04 0.12 -2 2 18 1.02 0.10 -2 2 -18 0.91 0.10 2 2 18 1.17 0.10 2 2 18 0.97 0.15 -2 -2 18 1.01 0.10 -2 -2 18 1.28 0.08 3 -2 18 7.15 0.29 3 2 -18 6.57 0.34 -3 -2 -18 7.30 0.28 3 2 -18 7.01 0.36 3 -2 18 7.60 0.32 -3 2 18 6.71 0.28 -3 2 -18 7.20 0.28 -3 2 -18 6.83 0.30 -3 -2 18 7.05 0.26 3 -2 -18 7.07 0.30 3 2 18 7.55 0.31 -4 -2 -18 2.15 0.11 4 -2 18 2.24 0.12 4 -2 18 2.11 0.13 -4 2 18 1.99 0.10 4 2 -18 2.04 0.17 4 -2 -18 2.05 0.15 -4 2 -18 1.97 0.11 4 2 18 2.02 0.13 5 -2 18 6.45 0.26 -5 -2 -18 6.04 0.24 5 -2 18 6.22 0.25 5 2 18 6.17 0.27 -5 2 -18 6.02 0.24 -6 -2 -18 14.30 0.52 6 -2 18 15.48 0.53 6 -2 18 15.69 0.54 6 2 18 14.68 0.54 -6 2 -18 14.38 0.52 0 3 -18 10.87 0.44 0 3 -18 11.77 0.50 0 3 18 11.79 0.46 0 3 18 12.33 1.07 0 3 18 11.97 0.52 0 -3 18 11.50 0.47 0 -3 18 12.18 0.45 -1 3 18 3.74 0.23 1 -3 18 3.90 0.19 1 3 -18 4.16 0.24 1 -3 18 3.75 0.20 1 3 -18 4.08 0.22 -1 3 18 4.04 0.18 -1 -3 18 4.07 0.21 -1 3 -18 4.05 0.22 1 3 18 3.73 0.24 1 3 18 4.01 0.20 -1 -3 18 4.10 0.18 -2 3 18 8.41 0.36 2 3 -18 8.10 0.39 2 3 -18 8.30 0.40 2 -3 18 8.67 0.33 -2 3 -18 8.44 0.37 2 3 18 8.93 0.36 -2 -3 18 9.16 0.33 3 -3 18 0.16 0.04 -3 3 18 0.23 0.05 3 3 -18 0.20 0.07 -3 -3 -18 0.12 0.03 3 3 18 0.13 0.05 -3 3 -18 0.10 0.04 4 -3 18 5.90 0.24 4 -3 18 5.58 0.23 -4 3 18 5.41 0.22 -4 -3 -18 5.60 0.22 4 3 -18 5.20 0.29 -4 3 -18 5.57 0.22 4 -3 -18 5.04 0.26 4 3 18 5.73 0.25 5 -3 18 5.34 0.22 -5 -3 -18 5.24 0.21 5 -3 18 5.55 0.23 -5 3 -18 5.38 0.21 5 3 18 5.51 0.24 6 -3 18 2.62 0.12 6 -3 18 2.65 0.12 -6 -3 -18 2.60 0.11 -6 3 -18 2.49 0.11 6 3 18 2.56 0.13 0 4 18 12.89 0.60 0 4 18 13.63 0.51 0 4 -18 13.20 0.54 0 4 -18 13.17 0.51 0 -4 18 13.29 0.49 0 -4 18 12.58 0.52 1 -4 18 9.36 0.38 1 4 -18 9.96 0.42 1 4 -18 9.93 0.44 -1 4 18 9.71 0.38 -1 -4 18 9.69 0.37 1 4 18 9.97 0.40 -1 4 -18 9.99 0.42 2 4 -18 20.07 0.78 2 4 -18 19.04 0.76 -2 4 18 18.84 0.72 -2 4 -18 19.73 0.73 2 4 18 20.10 0.73 -3 4 18 3.42 0.17 3 4 -18 3.32 0.22 -3 -4 -18 3.51 0.15 3 -4 18 3.56 0.17 3 4 18 3.35 0.18 4 -4 18 3.62 0.16 -4 -4 -18 3.70 0.16 4 -4 18 3.49 0.16 -4 4 -18 3.47 0.16 4 4 18 3.86 0.19 5 -4 18 2.27 0.12 5 -4 18 2.41 0.12 -5 -4 -18 2.42 0.11 5 4 18 2.48 0.14 -5 4 -18 2.46 0.11 -6 -4 -18 2.92 0.12 6 -4 18 2.79 0.12 6 -4 18 2.62 0.11 -6 4 -18 2.60 0.11 6 4 18 2.54 0.13 0 5 -18 17.73 0.66 0 5 -18 17.10 0.68 0 5 18 17.47 0.65 1 5 -18 9.56 0.41 -1 5 18 9.66 0.37 1 5 -18 9.38 0.42 -1 5 -18 9.26 0.40 1 5 18 9.68 0.39 2 5 -18 3.25 0.21 -2 -5 -18 3.68 0.17 2 5 18 3.51 0.19 -3 5 18 0.99 0.09 -3 -5 -18 0.99 0.07 3 5 -18 0.92 0.12 3 5 18 0.93 0.09 4 -5 18 5.95 0.25 -4 -5 -18 6.64 0.25 4 5 18 6.61 0.28 -4 5 -18 6.47 0.25 -5 -5 -18 4.35 0.17 5 -5 18 4.36 0.18 -5 5 -18 4.37 0.17 5 5 18 4.21 0.20 -6 -5 -18 13.07 0.45 6 -5 18 12.88 0.45 -6 5 -18 12.36 0.45 0 6 -18 5.29 0.24 0 6 18 5.05 0.24 1 6 -18 3.98 0.23 -1 6 18 4.30 0.19 1 6 18 4.11 0.21 2 6 -18 2.75 0.19 -2 -6 -18 2.85 0.13 2 6 18 3.02 0.17 -3 -6 -18 7.95 0.30 3 6 18 8.00 0.34 -4 -6 -18 8.67 0.31 4 -6 18 7.72 0.31 4 6 18 8.67 0.34 -4 6 -18 7.96 0.31 -5 -6 -18 7.26 0.27 5 -6 18 7.46 0.27 -5 6 -18 7.47 0.27 5 6 18 7.06 0.29 0 7 18 2.12 0.13 0 7 -18 1.99 0.14 -1 7 18 11.90 0.42 1 7 -18 10.49 0.46 1 7 18 11.01 0.44 -2 -7 -18 6.83 0.26 2 7 18 6.84 0.30 -3 -7 -18 3.20 0.14 3 7 18 3.33 0.17 -4 -7 -18 8.50 0.30 4 -7 18 7.85 0.30 4 7 18 7.85 0.32 -5 -7 -18 16.21 0.57 5 -7 18 16.81 0.57 0 8 18 1.99 0.13 -1 8 18 21.73 0.76 1 8 18 21.10 0.78 -2 -8 -18 4.05 0.17 2 8 18 3.90 0.20 -3 -8 -18 5.49 0.21 3 8 18 5.50 0.24 -4 -8 -18 0.56 0.04 4 8 18 0.55 0.07 0 9 18 6.40 0.27 -1 9 18 19.87 0.71 1 9 18 20.82 0.74 -2 -9 -18 2.33 0.11 2 9 18 2.55 0.14 -3 -9 -18 0.17 0.03 3 9 18 0.16 0.05 -4 -9 -18 11.19 0.39 0 10 18 0.31 0.05 -1 10 18 16.08 0.57 1 10 18 16.35 0.59 -2 -10 -18 1.59 0.08 2 10 18 1.68 0.10 3 10 18 5.41 0.25 0 11 18 3.00 0.13 1 11 18 2.97 0.14 0 0 -19 0.01 0.05 -1 0 19 2.92 0.15 1 0 19 3.19 0.15 2 0 19 0.41 0.06 -2 0 19 0.34 0.05 3 0 19 0.19 0.05 -3 0 19 0.17 0.03 3 0 -19 0.17 0.05 -3 0 -19 0.17 0.05 4 0 19 7.29 0.30 -4 0 -19 7.35 0.28 -5 0 -19 1.01 0.06 5 0 19 0.98 0.07 5 0 19 1.05 0.08 6 0 19 0.27 0.04 6 0 19 0.27 0.04 -6 0 -19 0.23 0.03 0 -1 19 26.25 0.92 0 1 -19 26.00 0.97 -1 1 19 17.16 0.64 -1 -1 19 17.40 0.64 1 1 19 18.32 0.64 -2 1 19 6.53 0.28 2 -1 19 7.09 0.28 2 1 -19 6.59 0.29 2 1 19 7.15 0.29 -2 -1 19 7.12 0.27 3 1 -19 2.85 0.17 3 -1 19 3.15 0.15 -3 -1 -19 2.72 0.13 -3 1 19 2.92 0.13 3 1 19 2.98 0.15 -3 -1 19 2.81 0.12 4 -1 19 1.63 0.10 -4 -1 -19 1.56 0.08 4 -1 19 1.35 0.09 -4 1 -19 1.54 0.08 4 1 19 1.48 0.10 5 -1 19 3.56 0.16 5 -1 19 3.38 0.15 -5 -1 -19 3.26 0.14 5 1 19 3.40 0.16 -5 1 -19 3.48 0.14 5 1 19 3.66 0.16 6 -1 19 9.09 0.32 -6 -1 -19 8.22 0.31 6 -1 19 9.37 0.33 6 1 19 9.18 0.33 6 1 19 9.04 0.33 -6 1 -19 8.22 0.31 0 2 -19 3.66 0.28 0 -2 19 4.77 0.21 0 2 19 4.86 0.20 -1 2 19 12.41 0.48 1 2 19 13.33 0.48 -1 -2 19 12.20 0.46 -2 2 19 1.41 0.10 2 -2 19 1.73 0.09 2 2 -19 1.52 0.12 2 2 19 1.51 0.11 -2 -2 19 1.49 0.09 -3 -2 -19 0.13 0.03 3 -2 19 0.11 0.04 -3 2 19 0.13 0.03 3 2 -19 0.16 0.06 3 2 19 0.10 0.04 4 -2 19 3.83 0.17 -4 -2 -19 4.00 0.16 4 -2 19 4.10 0.18 4 2 19 3.98 0.19 -4 2 -19 3.99 0.16 5 -2 19 13.35 0.50 -5 -2 -19 13.90 0.50 5 -2 19 14.27 0.51 5 2 19 14.83 0.52 -5 2 -19 14.14 0.50 6 -2 19 2.34 0.12 -6 -2 -19 2.36 0.10 6 2 19 2.44 0.13 6 2 19 2.54 0.11 -6 2 -19 2.11 0.11 0 3 19 6.94 0.27 0 -3 19 6.42 0.27 1 -3 19 0.52 0.07 1 3 -19 0.41 0.06 1 3 19 0.45 0.07 -1 -3 19 0.47 0.06 -2 3 19 2.13 0.13 2 3 -19 2.20 0.15 2 3 19 2.07 0.13 -3 -3 -19 9.62 0.35 3 3 19 9.37 0.38 -4 -3 -19 6.81 0.25 4 -3 19 6.23 0.25 4 -3 19 6.29 0.25 4 3 19 6.89 0.28 -4 3 -19 6.54 0.25 -5 -3 -19 3.07 0.13 5 -3 19 3.13 0.13 5 -3 19 3.08 0.14 -5 3 -19 3.14 0.13 5 3 19 3.20 0.15 0 4 19 0.16 0.05 1 4 -19 5.18 0.24 1 4 19 5.53 0.24 2 4 -19 12.05 0.48 2 4 19 11.72 0.46 -3 -4 -19 1.39 0.08 3 4 19 1.35 0.10 4 -4 19 6.20 0.24 -4 -4 -19 6.63 0.24 4 4 19 6.58 0.27 -4 4 -19 5.90 0.24 5 -4 19 2.50 0.11 -5 -4 -19 2.39 0.11 -5 4 -19 2.36 0.11 5 4 19 2.58 0.13 0 5 19 0.04 0.04 1 5 -19 4.23 0.21 1 5 19 4.42 0.20 2 5 19 0.88 0.09 -3 -5 -19 19.25 0.67 3 5 19 19.10 0.70 -4 -5 -19 0.60 0.05 4 -5 19 0.61 0.07 -4 5 -19 0.54 0.05 4 5 19 0.66 0.07 -5 -5 -19 14.43 0.51 5 -5 19 15.23 0.52 5 5 19 15.03 0.53 -5 5 -19 14.16 0.51 0 6 19 11.56 0.44 1 6 19 0.39 0.06 2 6 19 16.08 0.60 -3 -6 -19 3.90 0.16 3 6 19 4.09 0.19 -4 -6 -19 0.67 0.05 4 6 19 0.62 0.07 0 7 19 0.15 0.04 1 7 19 4.10 0.19 2 7 19 3.63 0.18 -3 -7 -19 6.92 0.26 3 7 19 7.27 0.29 -4 -7 -19 2.06 0.09 4 7 19 2.08 0.11 0 8 19 13.17 0.48 1 8 19 1.02 0.08 2 8 19 3.38 0.16 -3 -8 -19 2.38 0.10 3 8 19 2.55 0.13 0 9 19 2.24 0.11 1 9 19 1.57 0.10 2 9 19 3.17 0.15 1 10 19 1.24 0.08 2 0 20 4.92 0.20 3 0 20 0.18 0.04 4 0 20 0.33 0.05 -4 0 -20 0.31 0.03 4 0 20 0.31 0.04 -5 0 -20 4.14 0.17 5 0 20 4.38 0.17 5 0 20 4.35 0.18 1 1 20 0.61 0.07 2 1 20 40.08 1.37 3 -1 20 0.90 0.07 3 1 20 0.90 0.08 4 -1 20 7.79 0.29 -4 -1 -20 7.51 0.29 4 -1 20 8.00 0.29 4 1 20 8.42 0.30 -4 1 -20 7.47 0.29 4 1 20 8.10 0.30 5 -1 20 0.78 0.08 -5 -1 -20 0.60 0.06 5 1 20 0.68 0.06 5 1 20 0.78 0.06 1 2 20 3.38 0.15 2 2 20 11.40 0.43 3 2 20 9.93 0.38 -4 -2 -20 2.52 0.11 -4 2 -20 2.26 0.10 4 2 20 2.69 0.13 5 2 20 10.70 0.39 1 3 20 11.60 0.43 2 3 20 3.02 0.15 3 3 20 12.82 0.47 -4 -3 -20 9.80 0.37 4 3 20 10.92 0.39 1 4 20 4.40 0.19 2 4 20 5.58 0.23 3 4 20 2.45 0.13 -4 -4 -20 3.74 0.15 4 4 20 4.37 0.18 0 5 20 3.39 0.15 1 5 20 1.27 0.09 2 5 20 2.77 0.14 3 5 20 2.37 0.12 4 5 20 4.26 0.18 0 6 20 4.83 0.19 1 6 20 1.91 0.11 2 6 20 6.75 0.27 3 6 20 10.29 0.38 1 7 20 5.87 0.23 2 7 20 1.60 0.09 3 7 20 0.79 0.07 1 8 20 4.63 0.18 2 8 20 9.54 0.36 3 1 21 2.43 0.11 2 2 21 10.34 0.38 3 2 21 0.37 0.05 2 3 21 1.39 0.08 3 3 21 7.67 0.28 2 4 21 5.15 0.20 3 4 21 2.06 0.10 2 5 21 16.50 0.57 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 46951 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.50480(14) -0.07337(8) 0.05614(7) 0.0242(3) Uani 1 1 d . . . . . O2 O 0.77725(13) 0.05346(8) 0.03058(6) 0.0223(3) Uani 1 1 d . . . . . O3 O 0.86674(13) 0.17904(8) 0.25863(6) 0.0209(3) Uani 1 1 d . . . . . O4 O 0.57500(12) -0.04986(7) 0.24352(6) 0.0174(2) Uani 1 1 d . . . . . C1 C 0.8824(2) -0.29415(11) 0.08888(13) 0.0315(5) Uani 1 1 d . . . . . H1 H 0.9403 -0.3438 0.0890 0.038 Uiso 1 1 calc R U . . . C2 C 0.7903(2) -0.27970(11) 0.03168(12) 0.0287(4) Uani 1 1 d . . . . . H38 H 0.7880 -0.3181 -0.0082 0.034 Uiso 1 1 calc R U . . . C3 C 0.70152(19) -0.20916(11) 0.03284(10) 0.0216(4) Uani 1 1 d . . . . . H37 H 0.6347 -0.2010 -0.0049 0.026 Uiso 1 1 calc R U . . . C4 C 0.71021(17) -0.15006(10) 0.08948(9) 0.0165(3) Uani 1 1 d . . . . . C5 C 0.61425(17) -0.07438(10) 0.09011(8) 0.0154(3) Uani 1 1 d . . . . . C6 C 0.65977(17) 0.00319(10) 0.13311(9) 0.0149(3) Uani 1 1 d . . . . . C7 C 0.75010(17) 0.06339(10) 0.09487(9) 0.0158(3) Uani 1 1 d . . . . . C8 C 0.81936(17) 0.13785(10) 0.13636(9) 0.0161(3) Uani 1 1 d . . . . . C9 C 0.98168(17) 0.13268(11) 0.12501(9) 0.0190(3) Uani 1 1 d . . . . . H9 H 1.0011 0.1272 0.0725 0.023 Uiso 1 1 calc R U . . . H10 H 1.0246 0.1870 0.1417 0.023 Uiso 1 1 calc R U . . . C10 C 1.05213(17) 0.05947(11) 0.16411(9) 0.0180(3) Uani 1 1 d . . . . . H8 H 1.0563 0.0639 0.2154 0.022 Uiso 1 1 calc R U . . . C11 C 1.10916(18) -0.01063(11) 0.13523(9) 0.0206(4) Uani 1 1 d . . . . . C12 C 1.1852(2) -0.07533(12) 0.18143(10) 0.0250(4) Uani 1 1 d . . . . . H4 H 1.1786 -0.0585 0.2325 0.038 Uiso 1 1 calc R U . . . H3 H 1.2847 -0.0779 0.1670 0.038 Uiso 1 1 calc R U . . . H2 H 1.1418 -0.1318 0.1749 0.038 Uiso 1 1 calc R U . . . C13 C 0.8904(2) -0.23664(12) 0.14568(12) 0.0306(4) Uani 1 1 d . . . . . H40 H 0.9527 -0.2470 0.1851 0.037 Uiso 1 1 calc R U . . . C14 C 0.80706(19) -0.16375(11) 0.14475(10) 0.0224(4) Uani 1 1 d . . . . . H39 H 0.8163 -0.1226 0.1824 0.027 Uiso 1 1 calc R U . . . C15 C 1.1076(3) -0.03225(14) 0.05614(11) 0.0352(5) Uani 1 1 d . . . . . H5 H 1.0561 0.0122 0.0295 0.053 Uiso 1 1 calc R U . . . H7 H 1.0609 -0.0876 0.0491 0.053 Uiso 1 1 calc R U . . . H6 H 1.2047 -0.0355 0.0381 0.053 Uiso 1 1 calc R U . . . C16 C 0.79016(17) 0.13894(10) 0.21839(9) 0.0149(3) Uani 1 1 d . . . . . C17 C 0.66563(17) 0.08932(10) 0.24994(9) 0.0148(3) Uani 1 1 d . . . . . C18 C 0.63287(16) 0.01297(10) 0.20401(9) 0.0145(3) Uani 1 1 d . . . . . C19 C 0.61212(19) -0.03836(11) 0.32159(9) 0.0201(4) Uani 1 1 d . . . . . C20 C 0.69562(18) 0.04724(10) 0.32486(9) 0.0178(3) Uani 1 1 d . . . . . H11 H 0.7988 0.0379 0.3332 0.021 Uiso 1 1 calc R U . . . C21 C 0.63128(19) 0.10809(11) 0.38065(9) 0.0213(4) Uani 1 1 d . . . . . H24 H 0.6883 0.1608 0.3863 0.026 Uiso 1 1 calc R U . . . H23 H 0.6198 0.0802 0.4285 0.026 Uiso 1 1 calc R U . . . C22 C 0.48830(19) 0.12666(11) 0.34488(9) 0.0212(4) Uani 1 1 d . . . . . H18 H 0.4435 0.1773 0.3688 0.025 Uiso 1 1 calc R U . . . C23 C 0.53043(17) 0.15028(11) 0.26539(9) 0.0174(3) Uani 1 1 d . . . . . C24 C 0.41271(18) 0.13832(11) 0.20993(10) 0.0212(4) Uani 1 1 d . . . . . H13 H 0.3278 0.1684 0.2264 0.032 Uiso 1 1 calc R U . . . H14 H 0.3920 0.0772 0.2046 0.032 Uiso 1 1 calc R U . . . H12 H 0.4427 0.1617 0.1631 0.032 Uiso 1 1 calc R U . . . C25 C 0.57077(19) 0.24568(11) 0.26657(10) 0.0213(4) Uani 1 1 d . . . . . H17 H 0.6024 0.2632 0.2182 0.032 Uiso 1 1 calc R U . . . H15 H 0.6471 0.2548 0.3016 0.032 Uiso 1 1 calc R U . . . H16 H 0.4885 0.2798 0.2807 0.032 Uiso 1 1 calc R U . . . C26 C 0.3917(2) 0.04760(12) 0.35364(10) 0.0263(4) Uani 1 1 d . . . . . H19 H 0.3298 0.0562 0.3962 0.032 Uiso 1 1 calc R U . . . H20 H 0.3307 0.0425 0.3103 0.032 Uiso 1 1 calc R U . . . C27 C 0.4742(2) -0.03569(12) 0.36338(10) 0.0261(4) Uani 1 1 d . . . . . H22 H 0.4946 -0.0437 0.4156 0.031 Uiso 1 1 calc R U . . . H21 H 0.4143 -0.0841 0.3475 0.031 Uiso 1 1 calc R U . . . C28 C 0.6995(2) -0.11555(11) 0.34334(10) 0.0259(4) Uani 1 1 d . . . . . H25 H 0.6439 -0.1678 0.3363 0.039 Uiso 1 1 calc R U . . . H26 H 0.7265 -0.1105 0.3945 0.039 Uiso 1 1 calc R U . . . H27 H 0.7847 -0.1182 0.3133 0.039 Uiso 1 1 calc R U . . . C29 C 0.76178(18) 0.22066(10) 0.09878(9) 0.0181(3) Uani 1 1 d . . . . . H35 H 0.7698 0.2130 0.0456 0.022 Uiso 1 1 calc R U . . . H36 H 0.6601 0.2259 0.1104 0.022 Uiso 1 1 calc R U . . . C30 C 0.83290(18) 0.30326(11) 0.11878(10) 0.0200(4) Uani 1 1 d . . . . . H34 H 0.8428 0.3158 0.1689 0.024 Uiso 1 1 calc R U . . . C31 C 0.88317(18) 0.36021(11) 0.07181(10) 0.0207(3) Uani 1 1 d . . . . . C32 C 0.8823(3) 0.34888(14) -0.00942(11) 0.0350(5) Uani 1 1 d . . . . . H29 H 0.8702 0.2881 -0.0211 0.053 Uiso 1 1 calc R U . . . H28 H 0.9720 0.3693 -0.0295 0.053 Uiso 1 1 calc R U . . . H30 H 0.8043 0.3819 -0.0303 0.053 Uiso 1 1 calc R U . . . C33 C 0.9458(2) 0.44397(11) 0.09604(11) 0.0258(4) Uani 1 1 d . . . . . H31 H 0.9472 0.4462 0.1491 0.039 Uiso 1 1 calc R U . . . H33 H 0.8886 0.4913 0.0773 0.039 Uiso 1 1 calc R U . . . H32 H 1.0424 0.4489 0.0775 0.039 Uiso 1 1 calc R U . . . 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 0.0226(6) 0.0219(6) 0.0282(7) -0.0052(5) -0.0099(5) 0.0025(5) O2 0.0295(7) 0.0214(6) 0.0161(6) -0.0014(5) 0.0030(5) -0.0020(5) O3 0.0194(6) 0.0208(6) 0.0224(6) -0.0051(5) -0.0014(5) -0.0045(5) O4 0.0218(6) 0.0149(5) 0.0153(6) -0.0006(4) 0.0003(5) -0.0044(5) C1 0.0210(9) 0.0141(8) 0.0594(13) 0.0039(8) 0.0139(9) 0.0026(7) C2 0.0298(10) 0.0142(8) 0.0420(11) -0.0076(8) 0.0153(9) -0.0035(8) C3 0.0229(8) 0.0173(8) 0.0245(9) -0.0036(7) 0.0065(7) -0.0049(7) C4 0.0159(7) 0.0134(7) 0.0201(8) 0.0009(6) 0.0033(6) -0.0011(6) C5 0.0184(8) 0.0139(7) 0.0138(7) -0.0002(6) 0.0004(6) -0.0023(6) C6 0.0136(7) 0.0126(7) 0.0184(8) -0.0016(6) -0.0022(6) 0.0024(6) C7 0.0167(7) 0.0135(7) 0.0172(8) -0.0005(6) -0.0016(6) 0.0038(6) C8 0.0160(7) 0.0135(7) 0.0188(8) 0.0003(6) 0.0001(6) -0.0010(6) C9 0.0159(8) 0.0182(8) 0.0229(9) 0.0002(7) 0.0031(7) -0.0014(6) C10 0.0139(7) 0.0223(8) 0.0179(8) -0.0002(7) 0.0005(6) -0.0029(7) C11 0.0176(8) 0.0225(8) 0.0216(9) 0.0001(7) -0.0007(7) 0.0008(7) C12 0.0214(9) 0.0237(9) 0.0299(9) 0.0020(7) -0.0025(7) 0.0023(7) C13 0.0221(9) 0.0252(9) 0.0446(11) 0.0103(8) -0.0017(8) 0.0050(8) C14 0.0213(8) 0.0191(8) 0.0269(9) -0.0009(7) -0.0025(7) 0.0019(7) C15 0.0444(12) 0.0372(11) 0.0239(10) -0.0048(8) -0.0021(8) 0.0191(10) C16 0.0146(7) 0.0113(7) 0.0189(8) -0.0014(6) -0.0007(6) 0.0012(6) C17 0.0140(7) 0.0138(7) 0.0167(8) -0.0028(6) 0.0004(6) -0.0006(6) C18 0.0116(7) 0.0122(7) 0.0199(8) 0.0005(6) -0.0022(6) 0.0011(6) C19 0.0289(9) 0.0175(8) 0.0139(8) -0.0013(6) -0.0009(7) -0.0060(7) C20 0.0208(8) 0.0159(8) 0.0166(8) -0.0011(6) -0.0009(6) -0.0026(7) C21 0.0284(9) 0.0192(8) 0.0163(8) -0.0042(6) 0.0010(7) -0.0040(7) C22 0.0230(8) 0.0204(8) 0.0201(9) -0.0055(7) 0.0054(7) -0.0017(7) C23 0.0148(7) 0.0162(7) 0.0211(8) -0.0038(6) 0.0025(6) 0.0010(6) C24 0.0164(8) 0.0210(8) 0.0261(9) -0.0034(7) -0.0013(7) 0.0025(7) C25 0.0230(8) 0.0147(8) 0.0261(9) -0.0042(7) 0.0027(7) 0.0022(7) C26 0.0247(9) 0.0290(9) 0.0252(9) -0.0034(8) 0.0085(7) -0.0064(8) C27 0.0347(10) 0.0225(9) 0.0213(9) -0.0035(7) 0.0070(8) -0.0102(8) C28 0.0392(10) 0.0166(8) 0.0221(9) 0.0019(7) -0.0045(8) -0.0029(8) C29 0.0201(8) 0.0149(8) 0.0193(8) 0.0017(6) 0.0003(7) -0.0003(7) C30 0.0215(8) 0.0165(8) 0.0219(9) -0.0016(6) 0.0023(7) 0.0016(7) C31 0.0169(7) 0.0166(8) 0.0286(9) -0.0002(7) 0.0036(7) 0.0025(7) C32 0.0495(13) 0.0287(10) 0.0269(10) 0.0034(8) 0.0058(9) -0.0098(10) C33 0.0252(9) 0.0176(8) 0.0346(10) -0.0008(7) 0.0059(8) -0.0025(7) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 O4 C19 109.89(12) . . ? C13 C1 C2 120.32(17) . . ? C13 C1 H1 119.8 . . ? C2 C1 H1 119.8 . . ? C3 C2 C1 119.95(18) . . ? C3 C2 H38 120.0 . . ? C1 C2 H38 120.0 . . ? C2 C3 C4 120.08(18) . . ? C2 C3 H37 120.0 . . ? C4 C3 H37 120.0 . . ? C14 C4 C3 119.11(16) . . ? C14 C4 C5 121.29(15) . . ? C3 C4 C5 119.59(15) . . ? O1 C5 C4 121.87(14) . . ? O1 C5 C6 120.35(14) . . ? C4 C5 C6 117.75(14) . . ? C18 C6 C7 120.75(15) . . ? C18 C6 C5 123.29(15) . . ? C7 C6 C5 115.59(14) . . ? O2 C7 C6 120.81(15) . . ? O2 C7 C8 119.21(15) . . ? C6 C7 C8 119.90(14) . . ? C16 C8 C7 114.88(13) . . ? C16 C8 C9 108.12(13) . . ? C7 C8 C9 108.40(13) . . ? C16 C8 C29 111.33(13) . . ? C7 C8 C29 104.81(13) . . ? C9 C8 C29 109.15(13) . . ? C10 C9 C8 114.39(14) . . ? C10 C9 H9 108.7 . . ? C8 C9 H9 108.7 . . ? C10 C9 H10 108.7 . . ? C8 C9 H10 108.7 . . ? H9 C9 H10 107.6 . . ? C11 C10 C9 127.71(15) . . ? C11 C10 H8 116.1 . . ? C9 C10 H8 116.1 . . ? C10 C11 C15 124.80(16) . . ? C10 C11 C12 121.30(16) . . ? C15 C11 C12 113.88(16) . . ? C11 C12 H4 109.5 . . ? C11 C12 H3 109.5 . . ? H4 C12 H3 109.5 . . ? C11 C12 H2 109.5 . . ? H4 C12 H2 109.5 . . ? H3 C12 H2 109.5 . . ? C1 C13 C14 119.57(18) . . ? C1 C13 H40 120.2 . . ? C14 C13 H40 120.2 . . ? C13 C14 C4 120.82(17) . . ? C13 C14 H39 119.6 . . ? C4 C14 H39 119.6 . . ? C11 C15 H5 109.5 . . ? C11 C15 H7 109.5 . . ? H5 C15 H7 109.5 . . ? C11 C15 H6 109.5 . . ? H5 C15 H6 109.5 . . ? H7 C15 H6 109.5 . . ? O3 C16 C17 119.44(15) . . ? O3 C16 C8 120.02(14) . . ? C17 C16 C8 120.54(13) . . ? C18 C17 C16 110.44(13) . . ? C18 C17 C20 101.79(13) . . ? C16 C17 C20 114.31(13) . . ? C18 C17 C23 113.82(13) . . ? C16 C17 C23 112.29(13) . . ? C20 C17 C23 103.67(13) . . ? O4 C18 C6 121.66(15) . . ? O4 C18 C17 111.15(13) . . ? C6 C18 C17 127.15(15) . . ? O4 C19 C28 106.75(13) . . ? O4 C19 C27 106.87(14) . . ? C28 C19 C27 110.96(15) . . ? O4 C19 C20 105.11(12) . . ? C28 C19 C20 113.29(15) . . ? C27 C19 C20 113.25(14) . . ? C21 C20 C19 110.99(14) . . ? C21 C20 C17 105.22(13) . . ? C19 C20 C17 103.64(12) . . ? C21 C20 H11 112.2 . . ? C19 C20 H11 112.2 . . ? C17 C20 H11 112.2 . . ? C20 C21 C22 100.38(13) . . ? C20 C21 H24 111.7 . . ? C22 C21 H24 111.7 . . ? C20 C21 H23 111.7 . . ? C22 C21 H23 111.7 . . ? H24 C21 H23 109.5 . . ? C21 C22 C26 109.08(15) . . ? C21 C22 C23 102.85(13) . . ? C26 C22 C23 115.96(14) . . ? C21 C22 H18 109.6 . . ? C26 C22 H18 109.6 . . ? C23 C22 H18 109.6 . . ? C24 C23 C25 108.06(14) . . ? C24 C23 C22 114.42(14) . . ? C25 C23 C22 106.18(13) . . ? C24 C23 C17 112.83(13) . . ? C25 C23 C17 112.02(13) . . ? C22 C23 C17 103.17(13) . . ? C23 C24 H13 109.5 . . ? C23 C24 H14 109.5 . . ? H13 C24 H14 109.5 . . ? C23 C24 H12 109.5 . . ? H13 C24 H12 109.5 . . ? H14 C24 H12 109.5 . . ? C23 C25 H17 109.5 . . ? C23 C25 H15 109.5 . . ? H17 C25 H15 109.5 . . ? C23 C25 H16 109.5 . . ? H17 C25 H16 109.5 . . ? H15 C25 H16 109.5 . . ? C27 C26 C22 112.93(15) . . ? C27 C26 H19 109.0 . . ? C22 C26 H19 109.0 . . ? C27 C26 H20 109.0 . . ? C22 C26 H20 109.0 . . ? H19 C26 H20 107.8 . . ? C19 C27 C26 113.83(15) . . ? C19 C27 H22 108.8 . . ? C26 C27 H22 108.8 . . ? C19 C27 H21 108.8 . . ? C26 C27 H21 108.8 . . ? H22 C27 H21 107.7 . . ? C19 C28 H25 109.5 . . ? C19 C28 H26 109.5 . . ? H25 C28 H26 109.5 . . ? C19 C28 H27 109.5 . . ? H25 C28 H27 109.5 . . ? H26 C28 H27 109.5 . . ? C30 C29 C8 116.40(14) . . ? C30 C29 H35 108.2 . . ? C8 C29 H35 108.2 . . ? C30 C29 H36 108.2 . . ? C8 C29 H36 108.2 . . ? H35 C29 H36 107.3 . . ? C31 C30 C29 125.12(16) . . ? C31 C30 H34 117.4 . . ? C29 C30 H34 117.4 . . ? C30 C31 C33 121.96(17) . . ? C30 C31 C32 124.52(16) . . ? C33 C31 C32 113.52(16) . . ? C31 C32 H29 109.5 . . ? C31 C32 H28 109.5 . . ? H29 C32 H28 109.5 . . ? C31 C32 H30 109.5 . . ? H29 C32 H30 109.5 . . ? H28 C32 H30 109.5 . . ? C31 C33 H31 109.5 . . ? C31 C33 H33 109.5 . . ? H31 C33 H33 109.5 . . ? C31 C33 H32 109.5 . . ? H31 C33 H32 109.5 . . ? H33 C33 H32 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.212(2) . ? O2 C7 1.223(2) . ? O3 C16 1.212(2) . ? O4 C18 1.340(2) . ? O4 C19 1.4929(19) . ? C1 C13 1.382(3) . ? C1 C2 1.388(3) . ? C1 H1 0.9500 . ? C2 C3 1.386(3) . ? C2 H38 0.9500 . ? C3 C4 1.396(2) . ? C3 H37 0.9500 . ? C4 C14 1.388(2) . ? C4 C5 1.491(2) . ? C5 C6 1.511(2) . ? C6 C18 1.341(2) . ? C6 C7 1.454(2) . ? C7 C8 1.539(2) . ? C8 C16 1.538(2) . ? C8 C9 1.554(2) . ? C8 C29 1.565(2) . ? C9 C10 1.508(2) . ? C9 H9 0.9900 . ? C9 H10 0.9900 . ? C10 C11 1.332(2) . ? C10 H8 0.9500 . ? C11 C15 1.497(3) . ? C11 C12 1.505(2) . ? C12 H4 0.9800 . ? C12 H3 0.9800 . ? C12 H2 0.9800 . ? C13 C14 1.386(3) . ? C13 H40 0.9500 . ? C14 H39 0.9500 . ? C15 H5 0.9800 . ? C15 H7 0.9800 . ? C15 H6 0.9800 . ? C16 C17 1.527(2) . ? C17 C18 1.495(2) . ? C17 C20 1.556(2) . ? C17 C23 1.621(2) . ? C19 C28 1.517(2) . ? C19 C27 1.517(3) . ? C19 C20 1.555(2) . ? C20 C21 1.528(2) . ? C20 H11 1.0000 . ? C21 C22 1.534(2) . ? C21 H24 0.9900 . ? C21 H23 0.9900 . ? C22 C26 1.545(2) . ? C22 C23 1.563(2) . ? C22 H18 1.0000 . ? C23 C24 1.525(2) . ? C23 C25 1.538(2) . ? C24 H13 0.9800 . ? C24 H14 0.9800 . ? C24 H12 0.9800 . ? C25 H17 0.9800 . ? C25 H15 0.9800 . ? C25 H16 0.9800 . ? C26 C27 1.528(3) . ? C26 H19 0.9900 . ? C26 H20 0.9900 . ? C27 H22 0.9900 . ? C27 H21 0.9900 . ? C28 H25 0.9800 . ? C28 H26 0.9800 . ? C28 H27 0.9800 . ? C29 C30 1.501(2) . ? C29 H35 0.9900 . ? C29 H36 0.9900 . ? C30 C31 1.330(2) . ? C30 H34 0.9500 . ? C31 C33 1.504(2) . ? C31 C32 1.508(3) . ? C32 H29 0.9800 . ? C32 H28 0.9800 . ? C32 H30 0.9800 . ? C33 H31 0.9800 . ? C33 H33 0.9800 . ? C33 H32 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 C1 C2 C3 -2.7(3) . . . . ? C1 C2 C3 C4 3.6(3) . . . . ? C2 C3 C4 C14 -1.0(3) . . . . ? C2 C3 C4 C5 179.96(15) . . . . ? C14 C4 C5 O1 -158.08(17) . . . . ? C3 C4 C5 O1 21.0(2) . . . . ? C14 C4 C5 C6 23.7(2) . . . . ? C3 C4 C5 C6 -157.23(15) . . . . ? O1 C5 C6 C18 95.0(2) . . . . ? C4 C5 C6 C18 -86.76(19) . . . . ? O1 C5 C6 C7 -91.94(19) . . . . ? C4 C5 C6 C7 86.31(18) . . . . ? C18 C6 C7 O2 178.36(15) . . . . ? C5 C6 C7 O2 5.1(2) . . . . ? C18 C6 C7 C8 1.7(2) . . . . ? C5 C6 C7 C8 -171.52(13) . . . . ? O2 C7 C8 C16 -173.96(14) . . . . ? C6 C7 C8 C16 2.7(2) . . . . ? O2 C7 C8 C9 -52.92(19) . . . . ? C6 C7 C8 C9 123.74(15) . . . . ? O2 C7 C8 C29 63.54(18) . . . . ? C6 C7 C8 C29 -119.80(15) . . . . ? C16 C8 C9 C10 53.82(18) . . . . ? C7 C8 C9 C10 -71.31(18) . . . . ? C29 C8 C9 C10 175.07(13) . . . . ? C8 C9 C10 C11 109.9(2) . . . . ? C9 C10 C11 C15 -3.2(3) . . . . ? C9 C10 C11 C12 175.55(16) . . . . ? C2 C1 C13 C14 -0.8(3) . . . . ? C1 C13 C14 C4 3.5(3) . . . . ? C3 C4 C14 C13 -2.6(3) . . . . ? C5 C4 C14 C13 176.49(16) . . . . ? C7 C8 C16 O3 160.30(15) . . . . ? C9 C8 C16 O3 39.1(2) . . . . ? C29 C8 C16 O3 -80.78(18) . . . . ? C7 C8 C16 C17 -19.3(2) . . . . ? C9 C8 C16 C17 -140.49(15) . . . . ? C29 C8 C16 C17 99.61(17) . . . . ? O3 C16 C17 C18 -150.67(15) . . . . ? C8 C16 C17 C18 28.9(2) . . . . ? O3 C16 C17 C20 -36.6(2) . . . . ? C8 C16 C17 C20 142.98(14) . . . . ? O3 C16 C17 C23 81.11(19) . . . . ? C8 C16 C17 C23 -99.29(16) . . . . ? C19 O4 C18 C6 155.93(15) . . . . ? C19 O4 C18 C17 -21.86(17) . . . . ? C7 C6 C18 O4 -166.11(14) . . . . ? C5 C6 C18 O4 6.6(2) . . . . ? C7 C6 C18 C17 11.3(3) . . . . ? C5 C6 C18 C17 -175.97(15) . . . . ? C16 C17 C18 O4 151.69(13) . . . . ? C20 C17 C18 O4 29.92(16) . . . . ? C23 C17 C18 O4 -80.93(16) . . . . ? C16 C17 C18 C6 -26.0(2) . . . . ? C20 C17 C18 C6 -147.72(16) . . . . ? C23 C17 C18 C6 101.43(19) . . . . ? C18 O4 C19 C28 -116.70(15) . . . . ? C18 O4 C19 C27 124.50(14) . . . . ? C18 O4 C19 C20 3.89(17) . . . . ? O4 C19 C20 C21 126.57(14) . . . . ? C28 C19 C20 C21 -117.25(16) . . . . ? C27 C19 C20 C21 10.3(2) . . . . ? O4 C19 C20 C17 14.09(16) . . . . ? C28 C19 C20 C17 130.27(15) . . . . ? C27 C19 C20 C17 -102.22(16) . . . . ? C18 C17 C20 C21 -141.71(13) . . . . ? C16 C17 C20 C21 99.24(15) . . . . ? C23 C17 C20 C21 -23.32(16) . . . . ? C18 C17 C20 C19 -25.10(16) . . . . ? C16 C17 C20 C19 -144.15(14) . . . . ? C23 C17 C20 C19 93.29(14) . . . . ? C19 C20 C21 C22 -66.38(16) . . . . ? C17 C20 C21 C22 45.09(15) . . . . ? C20 C21 C22 C26 74.44(16) . . . . ? C20 C21 C22 C23 -49.20(15) . . . . ? C21 C22 C23 C24 157.32(14) . . . . ? C26 C22 C23 C24 38.4(2) . . . . ? C21 C22 C23 C25 -83.59(15) . . . . ? C26 C22 C23 C25 157.46(15) . . . . ? C21 C22 C23 C17 34.37(15) . . . . ? C26 C22 C23 C17 -84.57(17) . . . . ? C18 C17 C23 C24 -21.1(2) . . . . ? C16 C17 C23 C24 105.27(16) . . . . ? C20 C17 C23 C24 -130.85(14) . . . . ? C18 C17 C23 C25 -143.36(14) . . . . ? C16 C17 C23 C25 -16.95(19) . . . . ? C20 C17 C23 C25 106.94(15) . . . . ? C18 C17 C23 C22 102.85(15) . . . . ? C16 C17 C23 C22 -130.74(14) . . . . ? C20 C17 C23 C22 -6.85(15) . . . . ? C21 C22 C26 C27 -24.8(2) . . . . ? C23 C22 C26 C27 90.69(19) . . . . ? O4 C19 C27 C26 -73.49(17) . . . . ? C28 C19 C27 C26 170.49(15) . . . . ? C20 C19 C27 C26 41.8(2) . . . . ? C22 C26 C27 C19 -34.0(2) . . . . ? C16 C8 C29 C30 66.53(18) . . . . ? C7 C8 C29 C30 -168.69(14) . . . . ? C9 C8 C29 C30 -52.75(19) . . . . ? C8 C29 C30 C31 128.94(18) . . . . ? C29 C30 C31 C33 176.45(16) . . . . ? C29 C30 C31 C32 -2.8(3) . . . . ?