#------------------------------------------------------------------------------ #$Date: 2019-12-14 02:52:24 +0200 (Sat, 14 Dec 2019) $ #$Revision: 245132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556572.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_1556572 loop_ _publ_author_name 'Zheng, Guijuan' 'Zhou, Junfei' 'Huang, Lang' 'Zhang, Hao' 'Sun, Na' 'Zhang, Hanqi' 'Jin, Pengfei' 'Yue, Mingbo' 'Meng, Lingkui' 'Yao, Guangmin' _publ_section_title ; Antinociceptive Grayanane Diterpenoids from the Leaves of Pieris japonica. ; _journal_name_full 'Journal of natural products' _journal_paper_doi 10.1021/acs.jnatprod.9b00569 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_moiety ' C20 H32 O4, H2 O' _chemical_formula_sum 'C20 H34 O5' _chemical_formula_weight 354.47 _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 mixed _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 6.4945(3) _cell_length_b 11.4293(5) _cell_length_c 24.7998(11) _cell_measurement_reflns_used 8507 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 66.69 _cell_measurement_theta_min 3.56 _cell_volume 1840.83(14) _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 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_unetI/netI 0.0258 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 15631 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 66.716 _diffrn_reflns_theta_max 66.716 _diffrn_reflns_theta_min 3.564 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.279 _exptl_crystal_description block _exptl_crystal_F_000 648 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.145 _refine_diff_density_min -0.154 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.0(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 241 _refine_ls_number_reflns 3259 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0313 _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^)+(0.0387P)^2^+0.3381P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.0769 _reflns_Friedel_coverage 0.711 _reflns_Friedel_fraction_full 1.001 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 3010 _reflns_number_total 3259 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np9b00569_si_003.cif _cod_data_source_block a _cod_original_formula_sum ' C20 H34 O5' _cod_database_code 1556572 _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_res_file ; a.res created by SHELXL-2014/7 TITL 170615YGM_ZGJ_0ma_a.res in New: P212121 CELL 1.54178 6.4945 11.4293 24.7998 90.000 90.000 90.000 ZERR 4 0.0003 0.0005 0.0011 0.000 0.000 0.000 LATT -1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H N O UNIT 76 0 0 24 L.S. 22 ACTA BOND $H FMAP 2 PLAN 5 CONF TWIN WGHT 0.038700 0.338100 BASF 0.04332 FVAR 0.95062 C1 1 0.683777 0.224398 0.150057 11.00000 0.02578 0.02223 = 0.02577 -0.00058 -0.00026 0.00199 AFIX 13 H1 2 0.787000 0.220862 0.121279 11.00000 -1.20000 AFIX 0 C2 1 0.663388 0.099233 0.173371 11.00000 0.03089 0.02380 = 0.03240 0.00158 -0.00404 0.00263 AFIX 23 H2A 2 0.786702 0.054088 0.166015 11.00000 -1.20000 H2B 2 0.642306 0.102073 0.212070 11.00000 -1.20000 AFIX 0 C3 1 0.476161 0.044206 0.145292 11.00000 0.02696 0.02021 = 0.03026 -0.00016 0.00204 0.00247 AFIX 13 H3 2 0.359734 0.045126 0.170427 11.00000 -1.20000 AFIX 0 C4 1 0.424462 0.124807 0.097056 11.00000 0.02475 0.02269 = 0.02784 0.00056 -0.00192 -0.00062 C5 1 0.471970 0.245808 0.122559 11.00000 0.02384 0.02390 = 0.02654 0.00015 -0.00053 0.00048 C6 1 0.465332 0.350723 0.083812 11.00000 0.03050 0.02536 = 0.03302 0.00276 -0.00963 -0.00195 AFIX 23 H6A 2 0.406634 0.323846 0.050046 11.00000 -1.20000 H6B 2 0.370669 0.407805 0.098753 11.00000 -1.20000 AFIX 0 C7 1 0.667050 0.414295 0.070752 11.00000 0.03265 0.02383 = 0.02333 0.00204 -0.00163 -0.00167 AFIX 23 H7A 2 0.642628 0.464957 0.040030 11.00000 -1.20000 H7B 2 0.767367 0.356176 0.059695 11.00000 -1.20000 AFIX 0 C8 1 0.763864 0.488626 0.115969 11.00000 0.02297 0.02194 = 0.02481 -0.00147 0.00040 -0.00059 C9 1 0.879013 0.416322 0.160248 11.00000 0.02404 0.02239 = 0.02672 -0.00246 -0.00139 0.00212 AFIX 13 H9 2 0.988403 0.373586 0.141460 11.00000 -1.20000 AFIX 0 C10 1 0.744763 0.323863 0.186930 11.00000 0.02275 0.02414 = 0.02696 0.00202 -0.00568 0.00441 C11 1 0.988844 0.499902 0.199904 11.00000 0.03010 0.02833 = 0.03256 0.00089 -0.00719 -0.00274 AFIX 23 H11A 2 1.021078 0.456719 0.232501 11.00000 -1.20000 H11B 2 1.118236 0.524126 0.183872 11.00000 -1.20000 AFIX 0 C12 1 0.867020 0.610365 0.215734 11.00000 0.03906 0.02713 = 0.02631 -0.00266 -0.00256 -0.00186 AFIX 23 H12A 2 0.769891 0.590483 0.243999 11.00000 -1.20000 H12B 2 0.961653 0.668135 0.230117 11.00000 -1.20000 AFIX 0 C13 1 0.749379 0.664084 0.168108 11.00000 0.02840 0.02231 = 0.02756 -0.00235 0.00374 0.00228 AFIX 13 H13 2 0.669114 0.732046 0.179885 11.00000 -1.20000 AFIX 0 C14 1 0.608349 0.570260 0.144247 11.00000 0.02276 0.02456 = 0.02575 0.00252 0.00273 0.00153 AFIX 23 H14A 2 0.511710 0.603644 0.118700 11.00000 -1.20000 H14B 2 0.532794 0.529327 0.172220 11.00000 -1.20000 AFIX 0 C15 1 0.920138 0.577135 0.090812 11.00000 0.02470 0.02402 = 0.02669 -0.00283 0.00255 -0.00137 AFIX 23 H15A 2 1.060296 0.550647 0.096610 11.00000 -1.20000 H15B 2 0.896914 0.584529 0.052326 11.00000 -1.20000 AFIX 0 C16 1 0.884224 0.695541 0.119141 11.00000 0.02638 0.02225 = 0.02649 -0.00049 0.00005 -0.00008 C17 1 1.077112 0.763868 0.134186 11.00000 0.02976 0.02731 = 0.03450 -0.00180 -0.00012 -0.00322 AFIX 23 H17A 2 1.038411 0.828654 0.157331 11.00000 -1.20000 H17B 2 1.168118 0.713237 0.154616 11.00000 -1.20000 AFIX 0 C18 1 0.198276 0.113245 0.080316 11.00000 0.02869 0.02738 = 0.03781 0.00176 -0.00586 -0.00354 AFIX 137 H18A 2 0.168397 0.168576 0.052263 11.00000 -1.50000 H18B 2 0.111510 0.128515 0.110856 11.00000 -1.50000 H18C 2 0.173206 0.035401 0.067343 11.00000 -1.50000 AFIX 0 C19 1 0.564201 0.097851 0.048922 11.00000 0.03480 0.03477 = 0.02959 -0.00421 0.00215 -0.00356 AFIX 137 H19A 2 0.525729 0.023974 0.033502 11.00000 -1.50000 H19B 2 0.704786 0.094396 0.060775 11.00000 -1.50000 H19C 2 0.549718 0.158277 0.022303 11.00000 -1.50000 AFIX 0 C20 1 0.681166 0.329241 0.237956 11.00000 0.03916 0.02665 = 0.02887 -0.00009 -0.00357 -0.00261 AFIX 93 H20A 2 0.596827 0.270745 0.251801 11.00000 -1.20000 H20B 2 0.721121 0.391490 0.259722 11.00000 -1.20000 AFIX 0 O1 4 0.519064 -0.074294 0.131069 11.00000 0.03111 0.02142 = 0.04527 -0.00302 -0.00358 0.00158 AFIX 147 H1A 2 0.416568 -0.103703 0.117317 11.00000 -1.50000 AFIX 0 O2 4 0.318094 0.260473 0.163837 11.00000 0.02610 0.02919 = 0.03330 -0.00424 0.00277 0.00291 AFIX 147 H2 2 0.356019 0.310717 0.185250 11.00000 -1.50000 AFIX 0 O3 4 0.765474 0.765543 0.081737 11.00000 0.02880 0.02496 = 0.03036 0.00128 0.00169 0.00240 AFIX 147 H3A 2 0.711481 0.820026 0.097951 11.00000 -1.50000 AFIX 0 O4 4 1.186075 0.808429 0.088835 11.00000 0.03217 0.03274 = 0.04737 0.00055 0.00612 -0.00778 AFIX 147 H4 2 1.238553 0.754075 0.072193 11.00000 -1.50000 AFIX 0 O1W 4 0.411553 0.671928 0.022252 11.00000 0.04327 0.05187 = 0.03510 0.00560 -0.00272 -0.00146 H2W 2 0.538967 0.696508 0.025615 11.00000 0.06466 H1W 2 0.392406 0.680371 -0.011860 11.00000 0.06726 HKLF 4 REM 170615YGM_ZGJ_0ma_a.res in New: P212121 REM R1 = 0.0313 for 3010 Fo > 4sig(Fo) and 0.0355 for all 3259 data REM 241 parameters refined using 0 restraints END WGHT 0.0385 0.3392 REM Highest difference peak 0.145, deepest hole -0.154, 1-sigma level 0.035 Q1 1 0.6898 0.5340 0.1271 11.00000 0.05 0.15 Q2 1 1.3468 0.6995 0.1030 11.00000 0.05 0.13 Q3 1 0.5691 0.3833 0.0822 11.00000 0.05 0.13 Q4 1 0.6597 0.6256 0.1562 11.00000 0.05 0.13 Q5 1 0.8413 0.5315 0.1038 11.00000 0.05 0.12 ; _shelx_res_checksum 95212 _shelx_hkl_file ; 0 1 0 -0.20 0.60 0 -1 0 3.90 0.80 0 -1 0 0.30 0.60 0 1 0 1.40 1.00 0 2 0 3960.90 85.59 0 -2 0 3674.33 85.49 0 -2 0 3703.23 85.89 0 3 0 1.10 1.70 0 -3 0 -0.10 1.80 0 -4 0 222.98 8.70 0 4 0 222.48 8.20 0 -5 0 2.10 2.60 0 -6 0 2392.36 59.39 0 7 0 -5.80 6.40 0 -7 0 7.20 11.80 0 -7 0 0.40 3.70 0 -8 0 5.60 5.10 0 8 0 3.20 6.40 0 -8 0 8.30 9.50 0 -9 0 -5.30 8.20 0 -9 0 6.90 6.30 0 -9 0 8.40 8.40 0 9 0 -1.70 6.50 0 -10 0 52.39 9.40 0 -10 0 58.09 10.60 0 10 0 47.00 7.70 0 -10 0 37.60 10.10 0 11 0 -4.80 6.90 0 -11 0 -6.90 8.10 0 -11 0 0.40 7.20 0 -11 0 -14.30 13.20 0 12 0 1146.59 31.50 0 -12 0 1170.28 35.80 0 -12 0 1143.99 34.10 0 -13 0 5.90 8.00 0 -13 0 -6.40 4.90 1 0 0 2.60 1.80 1 0 0 -0.70 1.00 -1 0 0 1.60 1.30 1 1 0 9882.81 221.58 1 -1 0 9999.00 221.58 -1 -1 0 9750.52 221.58 1 2 0 116.89 4.80 1 -2 0 116.69 5.20 -1 -2 0 121.89 5.30 1 -3 0 1229.98 30.30 -1 3 0 1237.08 28.20 -1 -3 0 1174.58 30.10 1 -4 0 23.90 3.30 -1 -4 0 25.80 3.50 -1 4 0 22.90 2.60 1 -5 0 14.20 3.50 -1 -5 0 12.60 3.70 1 -6 0 75.59 7.00 -1 -6 0 94.19 7.80 1 -7 0 212.18 14.20 1 -7 0 190.28 10.90 1 7 0 162.08 15.60 -1 -7 0 179.88 11.40 -1 7 0 193.28 11.70 1 8 0 -2.90 8.20 1 -8 0 5.60 7.00 1 -8 0 1.50 5.10 -1 -8 0 -2.50 5.80 -1 8 0 0.80 5.30 -1 -8 0 8.50 9.40 -1 -8 0 14.20 14.60 1 -9 0 303.67 19.40 1 -9 0 302.47 17.10 1 9 0 285.27 17.40 1 -9 0 324.57 15.70 -1 -9 0 292.87 20.00 -1 -9 0 245.88 25.20 -1 9 0 302.87 14.40 -1 -9 0 287.57 19.10 1 -10 0 183.98 17.60 1 -10 0 159.18 13.10 1 -10 0 181.78 16.70 1 10 0 176.88 16.70 1 10 0 164.08 15.40 -1 -10 0 221.18 21.50 -1 10 0 173.38 12.10 -1 -10 0 161.48 23.10 -1 -10 0 180.28 16.70 1 -11 0 723.93 31.50 1 -11 0 733.33 25.30 1 -11 0 723.83 28.00 -1 -11 0 682.73 31.90 -1 11 0 754.82 23.90 -1 -11 0 784.52 45.00 -1 -11 0 736.23 28.40 1 -12 0 -7.30 5.30 1 -12 0 12.20 6.40 -1 -12 0 -7.40 5.90 -1 12 0 8.60 4.90 1 -13 0 73.79 9.20 1 -13 0 69.69 8.40 -1 -13 0 67.39 8.30 2 0 0 219.38 7.80 -2 0 0 222.28 8.20 2 -1 0 285.47 9.50 2 1 0 298.47 9.50 -2 1 0 301.27 9.80 -2 -1 0 302.17 10.20 2 -2 0 5401.86 125.39 2 2 0 5505.05 125.19 -2 -2 0 5541.25 125.99 2 3 0 1307.77 32.60 2 -3 0 1303.37 32.90 -2 -3 0 1258.67 33.40 -2 3 0 1296.77 30.20 2 4 0 320.47 12.00 2 -4 0 312.57 12.00 -2 4 0 324.47 9.00 -2 -4 0 324.47 13.00 2 5 0 1105.49 30.90 2 -5 0 1171.68 31.50 -2 -5 0 1202.68 33.00 2 -6 0 141.29 9.20 2 -6 0 123.79 11.70 2 6 0 137.79 9.20 -2 6 0 145.89 10.10 -2 -6 0 120.89 17.50 -2 -6 0 136.59 10.80 2 -7 0 3.70 5.20 2 -7 0 7.10 4.50 2 7 0 14.70 4.80 2 7 0 17.40 13.60 -2 -7 0 0.10 6.10 -2 -7 0 9.10 12.10 -2 7 0 3.20 4.70 2 -8 0 26.30 6.10 2 -8 0 35.50 11.00 2 8 0 20.10 12.80 2 8 0 28.50 6.40 2 -8 0 22.20 6.10 -2 -8 0 26.30 8.30 -2 -8 0 36.50 10.90 -2 8 0 23.10 6.00 2 -9 0 389.36 22.30 2 -9 0 373.66 16.30 2 -9 0 392.56 19.70 -2 9 0 399.06 15.90 -2 -9 0 405.26 22.80 2 10 0 97.69 14.10 2 -10 0 115.79 15.70 2 -10 0 113.69 17.50 2 -10 0 112.19 10.40 -2 -10 0 107.69 16.30 -2 10 0 123.99 10.20 2 -11 0 208.08 17.60 -2 11 0 188.88 11.90 2 -12 0 -1.80 4.40 2 -12 0 15.90 6.70 -2 12 0 5.50 4.00 -2 -12 0 1.30 6.30 2 -13 0 58.99 7.20 2 -13 0 68.29 8.90 -2 -13 0 69.09 9.80 -2 13 0 61.89 9.00 3 0 0 -2.40 2.70 -3 0 0 -5.40 3.30 3 -1 0 5.60 2.90 3 1 0 12.70 3.30 -3 -1 0 7.20 3.80 -3 1 0 9.40 3.50 3 -2 0 25.50 3.90 3 2 0 29.80 4.10 -3 -2 0 31.70 5.10 3 3 0 435.96 14.90 3 -3 0 454.15 14.90 -3 -3 0 472.05 17.50 -3 3 0 460.95 13.20 3 -4 0 -2.00 3.00 3 4 0 2.60 3.60 3 -4 0 3.90 5.90 -3 -4 0 6.30 6.10 -3 4 0 1.00 7.50 3 5 0 309.27 12.40 3 -5 0 291.47 12.70 3 -5 0 302.97 13.90 -3 5 0 282.67 13.20 -3 -5 0 285.27 16.50 3 6 0 40.70 5.90 3 -6 0 32.30 5.50 3 -6 0 33.90 5.80 -3 6 0 33.80 5.40 -3 -6 0 46.10 8.70 3 -7 0 1141.49 32.00 3 7 0 1153.58 32.90 3 -7 0 1097.19 42.50 3 -7 0 1125.89 33.70 -3 7 0 1144.89 31.00 -3 -7 0 1139.19 38.50 -3 -7 0 1110.59 45.20 3 -8 0 58.09 13.50 3 -8 0 65.99 8.80 3 -8 0 47.00 7.80 3 8 0 61.69 9.90 -3 8 0 53.29 7.80 -3 -8 0 45.00 14.10 -3 -8 0 57.69 14.30 3 -9 0 355.66 20.30 3 -9 0 370.86 23.30 3 -9 0 349.87 15.10 -3 -9 0 365.86 33.90 -3 -9 0 315.07 24.20 -3 9 0 357.26 14.90 3 -10 0 102.79 15.90 3 -10 0 113.39 9.70 -3 10 0 109.09 9.50 -3 -10 0 101.89 16.00 3 -11 0 354.26 13.30 3 -11 0 328.57 17.80 -3 11 0 353.86 13.00 -3 -11 0 351.56 19.60 3 -12 0 73.59 10.20 3 -12 0 58.69 5.90 -3 12 0 49.60 5.80 4 0 0 215.98 9.40 4 0 0 199.28 19.50 4 0 0 197.08 14.00 -4 0 0 211.18 12.50 4 1 0 259.57 10.20 4 1 0 258.27 15.20 4 -1 0 260.47 10.20 4 1 0 251.47 22.50 4 -1 0 223.88 14.00 -4 -1 0 254.47 17.70 -4 1 0 207.28 21.30 4 -2 0 2.40 3.50 4 2 0 0.50 3.70 4 -2 0 -1.60 5.60 4 2 0 1.50 7.60 -4 -2 0 -12.60 15.00 -4 -2 0 3.40 6.30 -4 2 0 15.00 9.00 4 -3 0 420.56 14.80 4 -3 0 423.36 16.10 4 3 0 413.66 13.90 4 3 0 389.96 19.10 -4 3 0 384.16 17.40 -4 -3 0 395.36 19.60 -4 3 0 403.96 15.10 -4 -3 0 359.46 29.50 4 -4 0 858.51 25.60 4 4 0 822.32 23.80 4 -4 0 877.31 25.50 4 4 0 869.41 28.90 -4 -4 0 876.21 34.80 -4 -4 0 873.11 31.60 -4 4 0 825.72 25.70 4 5 0 8.40 6.40 4 -5 0 13.00 5.30 4 -5 0 11.00 5.00 4 5 0 13.30 8.00 -4 -5 0 17.40 12.00 -4 -5 0 11.50 11.60 -4 5 0 16.60 5.30 4 -6 0 383.16 17.00 4 6 0 375.96 19.00 4 -6 0 379.66 15.00 -4 -6 0 354.86 30.00 -4 6 0 353.46 13.70 4 -7 0 269.17 12.40 4 7 0 260.17 16.90 4 -7 0 263.07 17.20 -4 7 0 252.57 11.80 -4 -7 0 325.57 36.50 4 -8 0 192.38 19.60 4 -8 0 186.78 10.50 4 8 0 162.08 14.20 -4 8 0 161.08 10.10 4 -9 0 104.69 9.10 4 9 0 95.59 12.40 -4 9 0 107.79 9.00 -4 -9 0 120.49 14.60 4 10 0 199.98 11.00 4 -10 0 199.68 9.30 -4 -10 0 213.48 12.80 -4 10 0 201.18 9.50 4 11 0 5.60 4.10 4 -11 0 5.70 2.80 -4 -11 0 5.90 4.80 -4 11 0 6.40 3.00 5 0 0 3.30 5.50 5 -1 0 -4.30 5.00 5 1 0 -3.60 5.50 -5 -1 0 -13.00 10.70 -5 1 0 7.10 8.00 5 -2 0 257.47 12.70 5 2 0 248.08 14.40 5 -2 0 248.98 13.30 -5 -2 0 227.58 21.70 -5 2 0 277.17 15.30 -5 -2 0 253.87 23.70 5 3 0 56.39 8.10 5 -3 0 46.10 6.30 5 -3 0 42.20 7.20 -5 3 0 69.19 8.20 -5 -3 0 54.79 12.50 5 4 0 101.99 12.00 5 -4 0 96.09 9.50 5 -4 0 97.69 9.00 -5 4 0 95.79 10.00 -5 -4 0 86.49 13.70 5 -5 0 190.48 10.90 5 -5 0 217.88 18.70 5 5 0 184.88 14.10 -5 5 0 210.78 10.70 -5 -5 0 178.78 20.30 5 -6 0 190.38 10.50 5 6 0 209.08 14.20 -5 6 0 194.08 10.00 -5 -6 0 177.98 19.60 5 -7 0 89.79 8.40 5 7 0 86.79 11.70 -5 7 0 83.49 7.70 -5 -7 0 87.69 12.60 5 -8 0 -2.00 3.20 5 8 0 -9.30 5.00 -5 -8 0 -6.20 7.40 -5 8 0 -2.00 3.20 5 -9 0 9.40 2.90 5 9 0 26.30 4.60 -5 -9 0 15.30 6.20 -5 9 0 14.10 3.40 5 -10 0 101.29 5.70 -5 10 0 100.39 5.80 -5 -10 0 93.49 9.00 6 0 0 -6.10 4.50 -6 0 0 2.90 7.10 6 1 0 126.19 9.60 6 -1 0 119.59 9.10 -6 -1 0 111.79 14.60 -6 1 0 113.09 12.00 6 2 0 18.80 5.10 6 -2 0 17.70 4.70 -6 2 0 16.40 6.00 -6 -2 0 21.10 8.90 6 -3 0 71.29 7.90 6 3 0 87.29 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4 25 44.10 5.60 0 5 25 11.70 4.10 0 5 25 1.90 6.20 0 5 25 8.10 4.70 0 6 25 225.08 10.30 0 6 25 223.88 20.40 0 6 25 208.58 10.10 0 7 25 27.00 5.00 0 7 25 35.90 4.50 -1 -7 25 24.60 6.20 -1 -6 25 14.30 4.40 1 -5 25 73.49 10.80 -1 -5 25 74.99 7.80 1 -4 25 123.79 10.40 -1 -4 25 134.19 9.50 1 -3 25 24.40 5.50 -1 -3 25 25.30 5.20 1 -2 25 21.10 8.90 1 -2 25 23.10 5.50 -1 -2 25 19.60 5.30 -1 -2 25 22.70 6.20 1 -1 25 142.89 12.10 1 -1 25 166.28 14.60 -1 -1 25 140.19 15.30 -1 -1 25 144.49 10.00 1 0 25 10.60 5.60 -1 0 25 12.60 4.80 1 1 25 182.28 15.20 1 1 25 127.59 18.60 1 1 25 155.18 10.90 1 -1 -25 126.99 18.10 -1 1 25 157.18 11.40 -1 1 25 158.38 9.60 1 2 25 17.80 5.70 1 2 25 21.60 5.10 1 -2 -25 48.90 11.80 1 2 25 18.30 7.10 -1 2 25 22.80 5.90 -1 2 25 10.20 8.80 -1 2 25 20.10 4.30 1 3 25 18.20 4.70 1 3 25 22.50 6.20 1 3 25 23.40 5.90 -1 3 25 24.40 6.00 -1 3 25 18.10 4.30 -1 3 25 23.80 6.70 1 4 25 121.49 10.00 1 4 25 128.99 9.20 1 4 25 124.69 10.70 -1 4 25 110.29 12.10 -1 4 25 119.29 8.70 -1 4 25 116.19 9.80 1 5 25 46.20 6.60 1 5 25 65.49 7.50 1 5 25 55.09 8.20 -1 5 25 89.09 7.90 -1 5 25 80.49 7.10 -1 5 25 67.09 9.10 1 6 25 8.60 4.10 1 6 25 6.30 5.50 1 6 25 -0.20 4.00 -1 6 25 5.60 3.60 -1 6 25 -2.10 3.90 1 7 25 23.50 4.60 1 7 25 20.00 4.10 -1 7 25 27.30 4.00 -2 -6 25 109.19 8.10 -2 -5 25 152.28 8.80 2 -4 25 124.99 12.20 -2 -4 25 141.39 8.80 2 -3 25 77.69 10.20 -2 -3 25 77.19 7.60 2 -2 25 65.89 7.60 -2 -2 25 64.29 7.90 -2 -2 25 69.59 6.60 2 -1 25 248.28 14.20 2 1 -25 260.17 15.50 2 -1 25 241.98 13.90 -2 -1 25 262.47 12.60 -2 -1 25 257.77 11.20 2 0 -25 10.80 6.90 2 0 25 6.60 5.70 2 0 25 4.00 5.30 -2 0 25 3.40 4.30 -2 0 25 12.20 4.30 2 1 25 272.47 14.40 2 1 25 294.97 14.90 2 1 25 265.17 13.30 2 -1 -25 234.08 16.50 -2 1 25 248.08 11.00 -2 1 25 249.68 12.80 2 2 25 61.49 9.30 2 -2 -25 54.59 9.40 2 2 25 70.59 9.10 2 2 25 70.79 7.60 -2 2 25 63.09 9.20 -2 2 25 56.59 6.30 2 3 25 79.49 9.10 2 3 25 62.09 9.10 2 3 25 74.39 9.00 -2 3 25 53.39 6.00 -2 3 25 71.29 8.10 -2 3 25 74.99 10.50 2 4 25 127.19 10.00 2 4 25 124.89 9.60 2 4 25 127.69 9.10 -2 4 25 115.79 15.40 -2 4 25 129.69 10.00 -2 4 25 134.69 7.90 2 5 25 140.19 9.50 2 5 25 132.99 8.80 2 5 25 143.99 9.20 -2 5 25 134.29 7.60 -2 5 25 146.39 9.20 2 6 25 104.79 7.50 2 6 25 91.29 7.50 2 6 25 103.59 8.70 -2 6 25 90.09 7.40 -2 6 25 111.09 7.00 3 4 -25 78.09 8.90 -3 -4 25 89.49 6.50 3 3 -25 33.80 5.90 -3 -3 25 27.20 4.20 3 2 -25 25.00 5.80 3 -2 25 20.10 5.90 -3 -2 25 31.70 5.10 -3 -2 25 18.40 3.90 3 1 -25 33.00 6.60 3 -1 25 27.20 7.80 3 -1 25 29.20 5.50 -3 -1 25 28.40 4.30 -3 -1 25 27.30 4.80 3 0 25 139.49 10.80 3 0 -25 147.49 12.20 3 0 25 132.29 11.00 -3 0 25 143.99 7.80 -3 0 25 127.39 9.00 3 1 25 37.50 5.60 3 -1 -25 44.60 7.20 3 1 25 41.80 6.40 3 1 25 29.30 5.20 -3 1 25 31.50 4.10 -3 1 25 25.20 5.40 3 -2 -25 26.90 7.10 3 2 25 22.20 4.70 3 2 25 23.10 5.10 3 2 25 30.40 5.50 -3 2 25 26.10 6.40 -3 2 25 28.50 3.70 3 3 25 31.10 5.20 3 3 25 17.90 4.70 3 3 25 33.50 4.90 -3 3 25 26.00 3.70 3 4 25 90.29 7.60 3 4 25 75.19 7.40 3 4 25 78.89 7.50 -3 4 25 80.29 5.80 4 1 -25 16.40 4.70 -4 -1 25 20.30 4.30 4 0 25 3.90 6.20 4 0 -25 0.90 4.50 -4 0 25 -5.10 4.90 -4 0 25 2.00 3.00 4 1 25 24.20 4.40 4 -1 -25 25.80 5.80 -4 1 25 17.20 3.10 0 -6 26 29.90 6.70 0 -5 26 92.89 8.70 0 -4 26 197.88 10.60 0 -3 26 7.20 4.50 0 -2 26 14.00 8.00 0 -2 26 7.60 4.40 0 -1 26 0.10 4.40 0 -1 26 5.30 5.90 0 0 26 -1.30 4.60 0 0 26 -0.60 5.10 0 1 26 -3.70 4.50 0 -1 -26 -6.50 14.20 0 1 26 0.40 5.30 0 2 26 -13.80 8.50 0 2 26 3.00 4.20 0 2 26 11.90 5.10 0 3 26 12.50 6.30 0 3 26 11.00 5.00 0 3 26 17.20 4.40 0 4 26 213.08 11.10 0 4 26 203.78 10.20 0 4 26 205.98 12.30 0 5 26 73.29 7.80 0 5 26 80.89 7.70 0 5 26 82.99 7.00 0 6 26 18.40 3.90 0 6 26 24.70 4.40 1 -5 26 2.40 8.30 -1 -5 26 10.50 4.10 1 -4 26 97.19 9.30 -1 -4 26 88.09 8.00 1 -3 26 59.59 8.90 -1 -3 26 65.19 7.40 1 -2 26 31.80 5.60 -1 -2 26 31.90 5.60 -1 -2 26 38.00 6.90 1 -1 26 173.48 11.80 1 -1 26 166.08 12.40 -1 -1 26 197.08 11.20 -1 -1 26 182.88 10.70 1 0 26 8.50 5.30 1 0 -26 -1.60 8.10 1 0 26 -3.30 4.60 -1 0 26 9.30 4.60 -1 0 26 8.00 4.40 1 1 26 174.88 12.10 1 1 26 166.48 10.30 1 -1 -26 219.18 18.50 -1 1 26 157.58 10.90 -1 1 26 174.08 9.60 1 2 26 37.10 7.20 1 2 26 28.90 5.40 1 2 26 29.20 5.30 -1 2 26 22.20 5.70 -1 2 26 27.80 4.50 1 3 26 76.59 9.50 1 3 26 65.59 9.10 1 3 26 51.69 6.00 -1 3 26 46.70 6.70 -1 3 26 58.79 6.90 -1 3 26 50.59 7.70 1 4 26 115.09 9.80 1 4 26 107.09 8.50 1 4 26 113.89 9.30 -1 4 26 99.99 11.40 -1 4 26 94.29 9.90 -1 4 26 110.49 7.40 1 5 26 5.40 3.90 1 5 26 2.70 4.40 1 5 26 2.70 4.80 -1 5 26 1.10 3.50 -1 5 26 -2.40 4.50 -1 5 26 -3.10 10.90 1 6 26 39.90 4.80 1 6 26 41.10 4.80 1 6 26 42.10 6.30 -1 6 26 46.00 6.90 -1 6 26 38.30 4.60 2 5 -26 6.40 4.30 -2 -5 26 3.20 3.50 2 4 -26 41.00 6.00 -2 -4 26 37.20 4.80 2 -3 26 73.19 9.10 2 3 -26 70.69 9.60 -2 -3 26 78.99 7.20 2 2 -26 15.10 5.70 2 -2 26 22.00 5.50 -2 -2 26 14.10 5.70 -2 -2 26 12.10 4.10 2 -1 26 81.49 8.90 2 1 -26 78.29 11.30 2 -1 26 61.39 7.90 -2 -1 26 56.89 7.70 -2 -1 26 57.49 7.50 2 0 -26 168.38 14.20 2 0 26 167.78 10.90 2 0 26 174.98 11.10 -2 0 26 172.28 10.10 -2 0 26 164.98 9.00 2 1 26 40.40 6.10 2 1 26 60.19 8.50 2 1 26 70.39 8.60 2 -1 -26 66.69 8.40 -2 1 26 58.09 8.00 -2 1 26 58.79 6.30 2 2 26 12.80 4.70 2 2 26 8.00 4.80 2 2 26 10.30 6.10 2 -2 -26 9.50 9.90 -2 2 26 12.70 3.50 -2 2 26 12.70 5.20 2 3 26 96.49 9.30 2 3 26 87.09 7.70 2 3 26 84.69 8.70 -2 3 26 93.59 10.80 -2 3 26 74.39 8.70 2 4 26 31.70 5.20 2 4 26 38.70 5.10 2 4 26 29.80 4.90 -2 4 26 43.60 5.50 -2 4 26 42.20 7.40 2 5 26 4.10 3.90 2 5 26 8.20 4.30 2 5 26 4.20 3.90 -2 5 26 8.20 3.10 -2 5 26 0.90 5.70 3 3 -26 64.79 8.50 -3 -3 26 50.09 6.10 3 -2 26 53.09 6.30 3 2 -26 27.30 5.90 -3 -2 26 40.10 6.00 -3 -2 26 43.60 6.10 3 1 -26 20.70 5.60 3 -1 26 16.70 5.00 -3 -1 26 19.60 4.00 -3 -1 26 18.60 4.20 3 0 26 20.70 6.20 3 0 26 27.80 5.10 3 0 -26 22.50 6.20 -3 0 26 23.80 3.70 -3 0 26 27.40 4.70 3 -1 -26 16.00 6.50 3 1 26 26.90 4.70 3 1 26 25.80 4.90 -3 1 26 16.20 4.90 -3 1 26 24.30 3.70 3 2 26 34.40 5.80 3 2 26 52.79 7.40 3 2 26 33.70 4.90 -3 2 26 36.90 7.60 -3 2 26 46.90 4.90 3 3 26 56.39 6.70 3 3 26 56.99 7.60 3 3 26 55.69 6.80 -3 3 26 59.59 5.20 0 -5 27 -9.40 5.00 0 -4 27 5.70 4.10 0 -3 27 2.60 4.10 0 -2 27 132.69 9.40 0 -1 27 40.40 6.30 0 -1 27 31.60 5.10 0 0 27 3.10 4.90 0 0 27 -4.10 4.70 0 1 27 26.40 5.30 0 2 27 119.59 8.50 0 2 27 125.89 10.10 0 3 27 3.70 4.70 0 3 27 3.90 3.70 0 3 27 2.40 7.30 0 4 27 -0.90 5.60 0 4 27 1.30 3.70 0 4 27 1.80 5.00 0 5 27 -2.40 6.10 0 5 27 -2.50 3.40 0 5 27 -4.00 4.70 1 -5 27 117.99 13.80 -1 -5 27 168.88 8.40 1 -4 27 -7.70 5.00 -1 -4 27 2.70 3.60 1 -3 27 73.99 8.70 -1 -3 27 69.49 7.10 1 -2 27 118.99 9.10 -1 -2 27 93.09 8.60 -1 -2 27 99.99 8.10 1 -1 27 74.79 7.90 1 -1 27 89.39 9.10 -1 -1 27 70.69 9.00 -1 -1 27 94.89 8.20 1 0 -27 33.00 8.80 1 0 27 28.00 5.40 -1 0 27 32.80 4.80 -1 0 27 39.90 5.50 1 1 27 82.69 9.00 1 1 27 79.89 8.20 1 -1 -27 99.89 11.20 -1 1 27 87.49 8.60 -1 1 27 77.39 7.30 1 2 27 83.59 9.00 1 2 27 83.49 7.90 1 2 27 96.19 13.50 -1 2 27 87.79 8.90 -1 2 27 80.19 7.10 1 3 27 87.49 8.50 1 3 27 66.59 7.20 1 3 27 69.39 7.10 -1 3 27 88.09 9.40 -1 3 27 79.09 6.80 1 4 27 6.30 3.80 1 4 27 0.40 4.40 1 4 27 4.80 5.00 -1 4 27 1.30 6.20 -1 4 27 2.80 3.30 -1 4 27 8.80 6.80 1 5 27 157.28 9.90 1 5 27 157.68 8.40 1 5 27 146.29 9.00 -1 5 27 161.48 7.90 -1 5 27 155.08 10.40 2 4 -27 17.50 4.70 -2 -4 27 10.40 3.20 2 3 -27 0.50 4.90 2 -3 27 0.60 5.40 -2 -3 27 7.00 3.30 2 -2 27 -1.10 4.40 2 2 -27 4.70 5.10 -2 -2 27 -4.40 3.10 -2 -2 27 3.20 7.70 2 1 -27 67.49 8.20 2 -1 27 69.99 8.00 2 -1 27 60.79 15.80 -2 -1 27 77.69 7.90 -2 -1 27 60.09 6.90 2 0 -27 75.99 8.30 2 0 27 92.19 8.40 2 0 27 88.89 9.10 -2 0 27 72.19 6.90 -2 0 27 80.09 7.30 2 1 27 54.09 6.20 2 1 27 59.89 8.10 2 -1 -27 72.69 8.90 -2 1 27 60.89 8.00 -2 1 27 50.39 6.20 2 2 27 1.40 4.10 2 2 27 -6.40 4.10 -2 2 27 3.10 4.90 -2 2 27 0.70 3.40 2 3 27 9.40 4.20 2 3 27 4.50 3.80 2 3 27 0.50 5.40 -2 3 27 2.60 3.00 -2 3 27 -8.00 7.80 2 4 27 6.40 3.90 2 4 27 7.10 5.90 2 4 27 7.70 4.10 -2 4 27 6.20 3.10 3 1 -27 -3.10 5.20 -3 -1 27 -3.40 3.50 -3 -1 27 4.60 4.80 3 0 -27 99.09 11.10 3 0 27 79.49 7.50 3 0 27 96.59 7.70 -3 0 27 82.59 6.60 -3 0 27 90.99 7.80 3 1 27 -5.00 5.20 3 -1 -27 1.40 6.70 3 1 27 0.20 3.70 -3 1 27 -6.70 5.00 -3 1 27 -0.60 3.00 0 -4 28 17.90 4.40 0 -3 28 6.90 3.90 0 -2 28 121.29 8.80 0 -1 28 4.10 4.00 0 -1 28 -2.60 6.60 0 0 28 172.38 10.00 0 0 28 179.98 10.00 0 1 28 5.10 4.20 0 1 28 -0.50 3.90 0 2 28 125.49 8.10 0 2 28 125.39 8.90 0 3 28 3.80 3.50 0 3 28 8.60 4.50 0 4 28 19.10 3.60 0 4 28 23.50 6.30 0 4 28 40.90 7.10 1 -3 28 10.20 4.30 -1 -3 28 9.40 3.50 1 2 -28 44.50 7.30 1 -2 28 34.60 4.80 -1 -2 28 58.69 6.40 1 -1 28 14.10 4.50 1 1 -28 8.60 7.40 1 -1 28 -3.30 8.30 -1 -1 28 17.60 5.90 -1 -1 28 15.20 4.00 1 0 -28 109.59 15.30 1 0 28 108.59 8.50 1 0 28 91.39 9.50 -1 0 28 99.69 8.10 -1 0 28 112.59 8.20 1 1 28 14.30 4.30 1 1 28 15.20 4.80 -1 1 28 16.50 3.90 -1 1 28 16.10 4.40 1 2 28 51.79 7.20 1 2 28 46.20 5.20 -1 2 28 59.09 6.10 -1 2 28 72.29 8.00 1 3 28 22.60 7.50 1 3 28 -0.30 3.70 1 3 28 -0.90 4.00 -1 3 28 9.00 3.40 -1 3 28 8.80 5.10 2 -2 28 65.39 8.70 2 2 -28 63.49 7.10 -2 -2 28 80.49 6.00 2 -1 28 11.90 4.40 2 1 -28 13.60 6.40 -2 -1 28 23.20 6.00 -2 -1 28 17.60 3.50 2 0 28 23.10 6.70 2 0 -28 38.90 8.20 2 0 28 35.50 4.60 -2 0 28 32.90 4.40 -2 0 28 29.40 4.50 2 1 28 24.10 5.10 2 1 28 15.00 4.00 2 -1 -28 23.40 9.90 -2 1 28 21.40 3.70 -2 1 28 14.30 4.40 2 2 28 70.39 7.00 2 2 28 57.59 7.10 -2 2 28 59.99 5.90 -2 2 28 59.39 6.60 0 -2 29 23.40 3.80 0 2 -29 38.60 8.40 0 1 -29 12.00 10.80 0 0 29 -0.90 3.70 0 1 29 0.50 3.70 0 1 29 -10.70 4.10 0 2 29 24.30 4.10 0 2 29 31.10 4.70 1 -1 29 3.40 3.90 1 1 -29 6.10 7.70 -1 -1 29 1.60 3.60 -1 -1 29 -8.40 8.30 1 0 -29 12.40 11.60 1 0 29 12.70 6.40 1 0 29 14.90 4.00 -1 0 29 13.10 6.70 -1 0 29 10.60 3.80 1 1 29 8.20 6.40 1 1 29 2.50 3.60 -1 1 29 7.80 4.00 -1 1 29 4.10 4.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87773 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp C1 C 0.6838(3) 0.22440(17) 0.15006(8) 0.0246(5) Uani 1 1 d . . H1 H 0.7870 0.2209 0.1213 0.030 Uiso 1 1 calc R U C2 C 0.6634(4) 0.09923(19) 0.17337(9) 0.0290(5) Uani 1 1 d . . H2A H 0.7867 0.0541 0.1660 0.035 Uiso 1 1 calc R U H2B H 0.6423 0.1021 0.2121 0.035 Uiso 1 1 calc R U C3 C 0.4762(4) 0.04421(18) 0.14529(9) 0.0258(5) Uani 1 1 d . . H3 H 0.3597 0.0451 0.1704 0.031 Uiso 1 1 calc R U C4 C 0.4245(3) 0.12481(19) 0.09706(9) 0.0251(5) Uani 1 1 d . . C5 C 0.4720(3) 0.24581(19) 0.12256(8) 0.0248(5) Uani 1 1 d . . C6 C 0.4653(4) 0.35072(19) 0.08381(9) 0.0296(5) Uani 1 1 d . . H6A H 0.4066 0.3238 0.0500 0.036 Uiso 1 1 calc R U H6B H 0.3707 0.4078 0.0988 0.036 Uiso 1 1 calc R U C7 C 0.6671(4) 0.41430(19) 0.07075(8) 0.0266(5) Uani 1 1 d . . H7A H 0.6426 0.4650 0.0400 0.032 Uiso 1 1 calc R U H7B H 0.7674 0.3562 0.0597 0.032 Uiso 1 1 calc R U C8 C 0.7639(3) 0.48863(18) 0.11597(8) 0.0232(5) Uani 1 1 d . . C9 C 0.8790(3) 0.41632(18) 0.16025(8) 0.0244(5) Uani 1 1 d . . H9 H 0.9884 0.3736 0.1415 0.029 Uiso 1 1 calc R U C10 C 0.7448(3) 0.32386(19) 0.18693(8) 0.0246(5) Uani 1 1 d . . C11 C 0.9888(4) 0.4999(2) 0.19990(9) 0.0303(5) Uani 1 1 d . . H11A H 1.0211 0.4567 0.2325 0.036 Uiso 1 1 calc R U H11B H 1.1182 0.5241 0.1839 0.036 Uiso 1 1 calc R U C12 C 0.8670(4) 0.6104(2) 0.21573(9) 0.0308(5) Uani 1 1 d . . H12A H 0.7699 0.5905 0.2440 0.037 Uiso 1 1 calc R U H12B H 0.9617 0.6681 0.2301 0.037 Uiso 1 1 calc R U C13 C 0.7494(3) 0.66408(18) 0.16811(8) 0.0261(5) Uani 1 1 d . . H13 H 0.6691 0.7320 0.1799 0.031 Uiso 1 1 calc R U C14 C 0.6083(3) 0.57026(19) 0.14425(9) 0.0244(5) Uani 1 1 d . . H14A H 0.5117 0.6036 0.1187 0.029 Uiso 1 1 calc R U H14B H 0.5328 0.5293 0.1722 0.029 Uiso 1 1 calc R U C15 C 0.9201(3) 0.57714(18) 0.09081(8) 0.0251(5) Uani 1 1 d . . H15A H 1.0603 0.5506 0.0966 0.030 Uiso 1 1 calc R U H15B H 0.8969 0.5845 0.0523 0.030 Uiso 1 1 calc R U C16 C 0.8842(3) 0.69554(19) 0.11914(8) 0.0250(5) Uani 1 1 d . . C17 C 1.0771(4) 0.7639(2) 0.13419(9) 0.0305(5) Uani 1 1 d . . H17A H 1.0384 0.8287 0.1573 0.037 Uiso 1 1 calc R U H17B H 1.1681 0.7132 0.1546 0.037 Uiso 1 1 calc R U C18 C 0.1983(4) 0.1132(2) 0.08032(10) 0.0313(5) Uani 1 1 d . . H18A H 0.1684 0.1686 0.0523 0.047 Uiso 1 1 calc R U H18B H 0.1115 0.1285 0.1109 0.047 Uiso 1 1 calc R U H18C H 0.1732 0.0354 0.0673 0.047 Uiso 1 1 calc R U C19 C 0.5642(4) 0.0979(2) 0.04892(9) 0.0331(5) Uani 1 1 d . . H19A H 0.5257 0.0240 0.0335 0.050 Uiso 1 1 calc R U H19B H 0.7048 0.0944 0.0608 0.050 Uiso 1 1 calc R U H19C H 0.5497 0.1583 0.0223 0.050 Uiso 1 1 calc R U C20 C 0.6812(4) 0.3292(2) 0.23796(9) 0.0316(5) Uani 1 1 d . . H20A H 0.5968 0.2707 0.2518 0.038 Uiso 1 1 calc R U H20B H 0.7211 0.3915 0.2597 0.038 Uiso 1 1 calc R U O1 O 0.5191(3) -0.07429(13) 0.13107(7) 0.0326(4) Uani 1 1 d . . H1A H 0.4166 -0.1037 0.1173 0.049 Uiso 1 1 calc R U O2 O 0.3181(2) 0.26047(13) 0.16384(6) 0.0295(4) Uani 1 1 d . . H2 H 0.3560 0.3107 0.1852 0.044 Uiso 1 1 calc R U O3 O 0.7655(2) 0.76554(13) 0.08174(6) 0.0280(3) Uani 1 1 d . . H3A H 0.7115 0.8200 0.0980 0.042 Uiso 1 1 calc R U O4 O 1.1861(3) 0.80843(14) 0.08883(7) 0.0374(4) Uani 1 1 d . . H4 H 1.2386 0.7541 0.0722 0.056 Uiso 1 1 calc R U O1W O 0.4116(3) 0.67193(19) 0.02225(8) 0.0434(4) Uani 1 1 d . . H2W H 0.539(6) 0.697(3) 0.0256(14) 0.065(11) Uiso 1 1 d . . H1W H 0.392(6) 0.680(3) -0.0119(15) 0.067(11) Uiso 1 1 d . . 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 C1 0.0258(11) 0.0222(10) 0.0258(11) -0.0006(8) -0.0003(9) 0.0020(9) C2 0.0309(12) 0.0238(10) 0.0324(11) 0.0016(9) -0.0040(10) 0.0026(10) C3 0.0270(11) 0.0202(10) 0.0303(11) -0.0002(9) 0.0020(9) 0.0025(9) C4 0.0247(11) 0.0227(11) 0.0278(11) 0.0006(9) -0.0019(9) -0.0006(9) C5 0.0238(11) 0.0239(11) 0.0265(10) 0.0002(9) -0.0005(9) 0.0005(9) C6 0.0305(12) 0.0254(11) 0.0330(12) 0.0028(10) -0.0096(10) -0.0019(9) C7 0.0327(12) 0.0238(10) 0.0233(10) 0.0020(9) -0.0016(9) -0.0017(9) C8 0.0230(10) 0.0219(10) 0.0248(10) -0.0015(8) 0.0004(9) -0.0006(8) C9 0.0240(11) 0.0224(10) 0.0267(10) -0.0025(9) -0.0014(9) 0.0021(8) C10 0.0228(10) 0.0241(10) 0.0270(11) 0.0020(9) -0.0057(9) 0.0044(9) C11 0.0301(12) 0.0283(12) 0.0326(12) 0.0009(9) -0.0072(10) -0.0027(10) C12 0.0391(14) 0.0271(11) 0.0263(11) -0.0027(10) -0.0026(10) -0.0019(10) C13 0.0284(11) 0.0223(10) 0.0276(11) -0.0023(9) 0.0037(10) 0.0023(9) C14 0.0228(11) 0.0246(10) 0.0258(10) 0.0025(8) 0.0027(9) 0.0015(8) C15 0.0247(11) 0.0240(11) 0.0267(10) -0.0028(9) 0.0025(9) -0.0014(9) C16 0.0264(11) 0.0223(11) 0.0265(11) -0.0005(9) 0.0001(9) -0.0001(9) C17 0.0298(12) 0.0273(11) 0.0345(12) -0.0018(10) -0.0001(10) -0.0032(10) C18 0.0287(12) 0.0274(11) 0.0378(12) 0.0018(10) -0.0059(10) -0.0035(10) C19 0.0348(13) 0.0348(13) 0.0296(11) -0.0042(10) 0.0021(10) -0.0036(11) C20 0.0392(13) 0.0266(11) 0.0289(11) -0.0001(9) -0.0036(10) -0.0026(11) O1 0.0311(9) 0.0214(8) 0.0453(9) -0.0030(7) -0.0036(8) 0.0016(7) O2 0.0261(8) 0.0292(8) 0.0333(8) -0.0042(7) 0.0028(7) 0.0029(7) O3 0.0288(8) 0.0250(8) 0.0304(8) 0.0013(7) 0.0017(7) 0.0024(6) O4 0.0322(9) 0.0327(8) 0.0474(10) 0.0005(8) 0.0061(8) -0.0078(8) O1W 0.0433(11) 0.0519(12) 0.0351(10) 0.0056(9) -0.0027(9) -0.0015(10) 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' N N 0.0311 0.0180 '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 C10 C1 C2 119.42(18) C10 C1 C5 112.26(17) C2 C1 C5 103.50(18) C10 C1 H1 107.0 C2 C1 H1 107.0 C5 C1 H1 107.0 C3 C2 C1 106.06(17) C3 C2 H2A 110.5 C1 C2 H2A 110.5 C3 C2 H2B 110.5 C1 C2 H2B 110.5 H2A C2 H2B 108.7 O1 C3 C2 110.25(18) O1 C3 C4 114.61(18) C2 C3 C4 106.18(17) O1 C3 H3 108.5 C2 C3 H3 108.5 C4 C3 H3 108.5 C19 C4 C18 109.86(18) C19 C4 C3 110.76(19) C18 C4 C3 111.49(19) C19 C4 C5 112.29(18) C18 C4 C5 112.21(18) C3 C4 C5 99.93(16) O2 C5 C6 109.51(18) O2 C5 C4 104.80(17) C6 C5 C4 115.78(17) O2 C5 C1 108.69(15) C6 C5 C1 114.95(18) C4 C5 C1 102.38(17) C7 C6 C5 118.55(18) C7 C6 H6A 107.7 C5 C6 H6A 107.7 C7 C6 H6B 107.7 C5 C6 H6B 107.7 H6A C6 H6B 107.1 C6 C7 C8 117.15(18) C6 C7 H7A 108.0 C8 C7 H7A 108.0 C6 C7 H7B 108.0 C8 C7 H7B 108.0 H7A C7 H7B 107.3 C7 C8 C14 113.38(18) C7 C8 C15 109.35(17) C14 C8 C15 102.42(16) C7 C8 C9 114.49(17) C14 C8 C9 108.25(17) C15 C8 C9 108.16(17) C10 C9 C11 114.65(17) C10 C9 C8 113.47(17) C11 C9 C8 109.92(17) C10 C9 H9 106.0 C11 C9 H9 106.0 C8 C9 H9 106.0 C20 C10 C1 121.9(2) C20 C10 C9 124.0(2) C1 C10 C9 114.17(17) C12 C11 C9 115.57(19) C12 C11 H11A 108.4 C9 C11 H11A 108.4 C12 C11 H11B 108.4 C9 C11 H11B 108.4 H11A C11 H11B 107.4 C13 C12 C11 112.79(18) C13 C12 H12A 109.0 C11 C12 H12A 109.0 C13 C12 H12B 109.0 C11 C12 H12B 109.0 H12A C12 H12B 107.8 C14 C13 C12 108.38(18) C14 C13 C16 101.49(16) C12 C13 C16 114.66(18) C14 C13 H13 110.6 C12 C13 H13 110.6 C16 C13 H13 110.6 C13 C14 C8 101.99(17) C13 C14 H14A 111.4 C8 C14 H14A 111.4 C13 C14 H14B 111.4 C8 C14 H14B 111.4 H14A C14 H14B 109.2 C16 C15 C8 106.73(17) C16 C15 H15A 110.4 C8 C15 H15A 110.4 C16 C15 H15B 110.4 C8 C15 H15B 110.4 H15A C15 H15B 108.6 O3 C16 C17 108.17(17) O3 C16 C13 109.36(17) C17 C16 C13 113.23(18) O3 C16 C15 105.88(16) C17 C16 C15 115.92(19) C13 C16 C15 103.91(17) O4 C17 C16 113.52(18) O4 C17 H17A 108.9 C16 C17 H17A 108.9 O4 C17 H17B 108.9 C16 C17 H17B 108.9 H17A C17 H17B 107.7 C4 C18 H18A 109.5 C4 C18 H18B 109.5 H18A C18 H18B 109.5 C4 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C4 C19 H19A 109.5 C4 C19 H19B 109.5 H19A C19 H19B 109.5 C4 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C10 C20 H20A 120.0 C10 C20 H20B 120.0 H20A C20 H20B 120.0 C3 O1 H1A 109.5 C5 O2 H2 109.5 C16 O3 H3A 109.5 C17 O4 H4 109.5 H2W O1W H1W 101(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C10 1.512(3) C1 C2 1.549(3) C1 C5 1.555(3) C1 H1 0.9800 C2 C3 1.536(3) C2 H2A 0.9700 C2 H2B 0.9700 C3 O1 1.427(3) C3 C4 1.547(3) C3 H3 0.9800 C4 C19 1.531(3) C4 C18 1.532(3) C4 C5 1.552(3) C5 O2 1.440(3) C5 C6 1.537(3) C6 C7 1.533(3) C6 H6A 0.9700 C6 H6B 0.9700 C7 C8 1.541(3) C7 H7A 0.9700 C7 H7B 0.9700 C8 C14 1.544(3) C8 C15 1.563(3) C8 C9 1.565(3) C9 C10 1.521(3) C9 C11 1.545(3) C9 H9 0.9800 C10 C20 1.333(3) C11 C12 1.541(3) C11 H11A 0.9700 C11 H11B 0.9700 C12 C13 1.535(3) C12 H12A 0.9700 C12 H12B 0.9700 C13 C14 1.529(3) C13 C16 1.540(3) C13 H13 0.9800 C14 H14A 0.9700 C14 H14B 0.9700 C15 C16 1.543(3) C15 H15A 0.9700 C15 H15B 0.9700 C16 O3 1.448(3) C16 C17 1.523(3) C17 O4 1.423(3) C17 H17A 0.9700 C17 H17B 0.9700 C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 C20 H20A 0.9300 C20 H20B 0.9300 O1 H1A 0.8200 O2 H2 0.8200 O3 H3A 0.8200 O4 H4 0.8200 O1W H2W 0.88(4) O1W H1W 0.86(4) 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 C10 C1 C2 C3 141.3(2) C5 C1 C2 C3 15.7(2) C1 C2 C3 O1 138.19(18) C1 C2 C3 C4 13.5(2) O1 C3 C4 C19 -40.4(3) C2 C3 C4 C19 81.5(2) O1 C3 C4 C18 82.2(2) C2 C3 C4 C18 -155.80(19) O1 C3 C4 C5 -158.99(18) C2 C3 C4 C5 -37.0(2) C19 C4 C5 O2 175.67(17) C18 C4 C5 O2 51.3(2) C3 C4 C5 O2 -66.89(19) C19 C4 C5 C6 54.9(2) C18 C4 C5 C6 -69.4(2) C3 C4 C5 C6 172.36(19) C19 C4 C5 C1 -70.9(2) C18 C4 C5 C1 164.76(18) C3 C4 C5 C1 46.52(19) C10 C1 C5 O2 -58.6(2) C2 C1 C5 O2 71.5(2) C10 C1 C5 C6 64.5(2) C2 C1 C5 C6 -165.37(18) C10 C1 C5 C4 -169.09(17) C2 C1 C5 C4 -38.99(19) O2 C5 C6 C7 129.7(2) C4 C5 C6 C7 -112.2(2) C1 C5 C6 C7 7.0(3) C5 C6 C7 C8 -71.0(3) C6 C7 C8 C14 -47.7(2) C6 C7 C8 C15 -161.27(18) C6 C7 C8 C9 77.2(2) C7 C8 C9 C10 -56.1(2) C14 C8 C9 C10 71.4(2) C15 C8 C9 C10 -178.30(16) C7 C8 C9 C11 174.02(18) C14 C8 C9 C11 -58.4(2) C15 C8 C9 C11 51.8(2) C2 C1 C10 C20 -36.1(3) C5 C1 C10 C20 85.3(2) C2 C1 C10 C9 145.1(2) C5 C1 C10 C9 -93.5(2) C11 C9 C10 C20 16.5(3) C8 C9 C10 C20 -110.9(2) C11 C9 C10 C1 -164.72(18) C8 C9 C10 C1 67.8(2) C10 C9 C11 C12 -88.9(2) C8 C9 C11 C12 40.3(3) C9 C11 C12 C13 -39.8(3) C11 C12 C13 C14 56.1(2) C11 C12 C13 C16 -56.4(3) C12 C13 C14 C8 -72.2(2) C16 C13 C14 C8 48.85(19) C7 C8 C14 C13 -157.59(17) C15 C8 C14 C13 -39.9(2) C9 C8 C14 C13 74.23(19) C7 C8 C15 C16 136.74(18) C14 C8 C15 C16 16.2(2) C9 C8 C15 C16 -98.0(2) C14 C13 C16 O3 74.60(19) C12 C13 C16 O3 -168.82(17) C14 C13 C16 C17 -164.70(18) C12 C13 C16 C17 -48.1(2) C14 C13 C16 C15 -38.1(2) C12 C13 C16 C15 78.5(2) C8 C15 C16 O3 -101.83(18) C8 C15 C16 C17 138.25(19) C8 C15 C16 C13 13.3(2) O3 C16 C17 O4 -49.7(2) C13 C16 C17 O4 -171.04(18) C15 C16 C17 O4 69.0(2)