#------------------------------------------------------------------------------ #$Date: 2020-04-20 23:37:32 +0300 (Mon, 20 Apr 2020) $ #$Revision: 250946 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557824.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_1557824 loop_ _publ_author_name 'Yang, Wei-Qun' 'Shao, Xue-Hua' 'Deng, Fang' 'Hu, Li-Jun' 'Xiong, Yu' 'Huang, Xiao-Jun' 'Fan, Chun-Lin' 'Jiang, Ren-Wang' 'Ye, Wen-Cai' 'Wang, Ying' _publ_section_title ; Unprecedented Quassinoids from Eurycoma longifolia: Biogenetic Evidence and Antifeedant Effects ; _journal_name_full 'Journal of Natural Products' _journal_paper_doi 10.1021/acs.jnatprod.0c00244 _journal_year 2020 _chemical_absolute_configuration unk _chemical_formula_moiety 'C20 H26 O10' _chemical_formula_sum 'C20 H26 O10' _chemical_formula_weight 426.41 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2019-06-17 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 103.943(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.3686(3) _cell_length_b 6.6338(2) _cell_length_c 13.6339(4) _cell_measurement_reflns_used 2622 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.2670 _cell_measurement_theta_min 3.3130 _cell_volume 910.15(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -65.00 12.00 1.00 2.00 -- -40.98 38.00-150.00 77 2 \w -113.00 -13.00 1.00 2.00 -- -40.98 -57.00-150.00 100 3 \w -79.00 -53.00 1.00 2.00 -- -40.98-158.00 -25.00 26 4 \w 54.00 178.00 1.00 8.00 -- 106.95 15.00-150.00 124 5 \w 125.00 164.00 1.00 8.00 -- 106.95 125.00-180.00 39 6 \w 119.00 145.00 1.00 8.00 -- 106.95 125.00 -90.00 26 7 \w 79.00 143.00 1.00 8.00 -- 106.95 61.00 90.00 64 8 \w 36.00 114.00 1.00 8.00 -- 106.95 -61.00 150.00 78 9 \w 43.00 105.00 1.00 8.00 -- 106.95 -95.00 120.00 62 10 \w -58.00 -21.00 1.00 2.00 -- -41.23 -77.00-150.00 37 11 \w -68.00 -14.00 1.00 2.00 -- -41.23 -57.00 120.00 54 12 \w -114.00 -88.00 1.00 2.00 -- -41.23 -77.00-150.00 26 13 \w 23.00 55.00 1.00 2.00 -- 41.23 38.00-180.00 32 14 \w 21.00 47.00 1.00 2.00 -- 41.23 38.00 -30.00 26 15 \w 28.00 93.00 1.00 2.00 -- 41.23-125.00 120.00 65 16 \w 22.00 49.00 1.00 2.00 -- 41.23 -99.00 0.00 27 17 \w 51.00 77.00 1.00 2.00 -- 41.23 38.00 -90.00 26 18 \w 75.00 101.00 1.00 8.00 -- 106.95 77.00-180.00 26 19 \w 79.00 105.00 1.00 8.00 -- 106.95 61.00 -60.00 26 20 \w 75.00 101.00 1.00 8.00 -- 106.95 77.00 -90.00 26 21 \w 78.00 103.00 1.00 8.00 -- 106.95 61.00-180.00 25 22 \w 81.00 107.00 1.00 8.00 -- 106.95 61.00-150.00 26 23 \w 83.00 109.00 1.00 8.00 -- 106.95 61.00 -90.00 26 24 \w 80.00 106.00 1.00 8.00 -- 106.95 61.00-120.00 26 25 \w 82.00 108.00 1.00 8.00 -- 106.95 45.00-150.00 26 26 \w 142.00 176.00 1.00 8.00 -- 106.95 77.00-150.00 34 27 \w 79.00 104.00 1.00 8.00 -- 106.95 61.00 150.00 25 28 \w 74.00 100.00 1.00 8.00 -- 106.95 77.00 150.00 26 29 \w 81.00 106.00 1.00 8.00 -- 106.95 45.00-180.00 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0693 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 6342 _diffrn_reflns_point_group_measured_fraction_full 0.896 _diffrn_reflns_point_group_measured_fraction_max 0.862 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.380 _diffrn_reflns_theta_min 3.340 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.556 _exptl_crystal_description block _exptl_crystal_F_000 452 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.414 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.064 _refine_ls_abs_structure_details ; Flack x determined using 979 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.3(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 279 _refine_ls_number_reflns 3151 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0471 _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^)+(0.0634P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1140 _refine_ls_wR_factor_ref 0.1179 _reflns_Friedel_coverage 0.617 _reflns_Friedel_fraction_full 0.771 _reflns_Friedel_fraction_max 0.723 _reflns_number_gt 2881 _reflns_number_total 3151 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np0c00244_si_006.cif _cod_data_source_block dg_2 _cod_database_code 1557824 _shelx_shelxl_version_number 2017/1 _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_max 0.910 _shelx_estimated_absorpt_t_min 0.883 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Ternary CH refined with riding coordinates: C1(H1), C2(H2), C5(H5), C7(H7), C9(H9), C12(H12), C15(H15) 2.b Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C18(H18A,H18B), C30(H30A,H30B) 2.c Aromatic/amide H refined with riding coordinates: C3(H3) 2.d Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C29(H29A,H29B,H29C) 2.e Idealised tetrahedral OH refined as rotating group: O1(H1A), O2(H2A), O5(H5A), O6(H6), O8(H8), O9(H9A) ; _shelx_res_file ; TITL dg_2_a.res in P2(1) dg_2.res created by SHELXL-2017/1 at 22:50:11 on 16-Jun-2019 REM Old TITL dg_2 in P2(1) REM SHELXT solution in P2(1): R1 0.086, Rweak 0.042, Alpha 0.002 REM 0.815 for 4 systematic absences, Orientation as input REM Flack x = -0.359 ( 0.223 ) from 910 Parsons' quotients REM Formula found by SHELXT: C30 O10 CELL 1.54184 10.368647 6.633773 13.633854 90 103.9428 90 ZERR 2 0.00032 0.000224 0.000427 0 0.0031 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O UNIT 40 52 20 L.S. 30 PLAN 20 SIZE 0.09 0.11 0.12 BOND list 4 fmap 2 acta REM REM REM WGHT 0.063400 FVAR 11.50439 C1 1 0.959633 0.329461 0.813841 11.00000 0.01124 0.01616 = 0.01362 -0.00091 -0.00277 -0.00347 AFIX 13 H1 2 0.903177 0.228204 0.835164 11.00000 -1.20000 AFIX 0 C2 1 1.063656 0.222298 0.772260 11.00000 0.01172 0.01949 = 0.02137 -0.00240 -0.00130 0.00054 AFIX 13 H2 2 1.136423 0.316856 0.772741 11.00000 -1.20000 AFIX 0 C3 1 1.011965 0.147521 0.666322 11.00000 0.01250 0.01570 = 0.02210 -0.00341 0.00471 0.00099 AFIX 43 H3 2 1.065510 0.061292 0.639655 11.00000 -1.20000 AFIX 0 C4 1 0.893903 0.197494 0.608324 11.00000 0.01380 0.01802 = 0.01405 -0.00042 0.00643 -0.00354 C5 1 0.798420 0.330023 0.647809 11.00000 0.00965 0.01502 = 0.01295 0.00013 0.00169 -0.00190 AFIX 13 H5 2 0.743166 0.238585 0.676723 11.00000 -1.20000 AFIX 0 C6 1 0.702830 0.451930 0.566671 11.00000 0.01433 0.01799 = 0.01188 0.00110 0.00079 -0.00121 AFIX 23 H6A 2 0.748830 0.567183 0.547457 11.00000 -1.20000 H6B 2 0.670787 0.369065 0.507163 11.00000 -1.20000 AFIX 0 C7 1 0.585957 0.523601 0.607098 11.00000 0.01610 0.01307 = 0.01132 -0.00021 0.00191 -0.00102 AFIX 13 H7 2 0.535241 0.620612 0.558594 11.00000 -1.20000 AFIX 0 C8 1 0.628845 0.629709 0.709855 11.00000 0.01335 0.01179 = 0.01326 -0.00206 0.00207 -0.00107 C9 1 0.759529 0.556505 0.784084 11.00000 0.01100 0.01222 = 0.01312 -0.00076 0.00187 -0.00278 AFIX 13 H9 2 0.735002 0.448791 0.825330 11.00000 -1.20000 AFIX 0 C10 1 0.870882 0.470570 0.736008 11.00000 0.01386 0.01105 = 0.01328 -0.00015 0.00428 -0.00219 C11 1 0.785742 0.747889 0.850783 11.00000 0.01310 0.01338 = 0.01319 0.00010 0.00143 -0.00290 C12 1 0.689378 0.744766 0.921560 11.00000 0.01560 0.01261 = 0.01280 -0.00104 0.00365 -0.00121 AFIX 13 H12 2 0.705925 0.862764 0.966080 11.00000 -1.20000 AFIX 0 C13 1 0.545954 0.745943 0.861651 11.00000 0.01477 0.01646 = 0.01415 -0.00085 0.00127 0.00324 C14 1 0.510894 0.623619 0.762811 11.00000 0.01146 0.01766 = 0.01310 0.00011 -0.00041 0.00373 C15 1 0.481291 0.400688 0.779073 11.00000 0.01213 0.01662 = 0.01533 -0.00025 0.00352 0.00032 AFIX 13 H15 2 0.563406 0.335761 0.816376 11.00000 -1.20000 AFIX 0 C16 1 0.435896 0.298591 0.675971 11.00000 0.01075 0.01576 = 0.01723 -0.00102 0.00178 0.00311 C18 1 0.442447 0.793382 0.913873 11.00000 0.01775 0.02535 = 0.02022 -0.00551 0.00289 0.00607 AFIX 23 H18A 2 0.355512 0.733319 0.888434 11.00000 -1.20000 H18B 2 0.468697 0.810716 0.986619 11.00000 -1.20000 AFIX 0 C19 1 0.955895 0.629696 0.699392 11.00000 0.01538 0.01863 = 0.01622 -0.00054 0.00398 -0.00310 AFIX 137 H19A 2 1.021245 0.681388 0.756075 11.00000 -1.50000 H19B 2 0.900031 0.737862 0.667066 11.00000 -1.50000 H19C 2 0.999618 0.569433 0.652116 11.00000 -1.50000 AFIX 0 C29 1 0.846212 0.107698 0.503942 11.00000 0.01683 0.02656 = 0.01399 -0.00082 0.00320 0.00158 AFIX 137 H29A 2 0.836009 0.212815 0.454268 11.00000 -1.50000 H29B 2 0.762308 0.042079 0.498734 11.00000 -1.50000 H29C 2 0.910034 0.011179 0.492542 11.00000 -1.50000 AFIX 0 C30 1 0.661631 0.849394 0.692538 11.00000 0.01948 0.01405 = 0.01294 0.00109 0.00025 0.00045 AFIX 23 H30A 2 0.702022 0.860161 0.635553 11.00000 -1.20000 H30B 2 0.581589 0.930841 0.678860 11.00000 -1.20000 AFIX 0 O1 3 1.026654 0.444666 0.901358 11.00000 0.01710 0.01708 = 0.01229 0.00103 -0.00197 -0.00191 AFIX 147 H1A 2 1.040811 0.372299 0.951579 11.00000 -1.50000 AFIX 0 O2 3 1.115535 0.056164 0.839809 11.00000 0.02235 0.01871 = 0.02382 -0.00291 -0.00572 0.00515 AFIX 147 H2A 2 1.055321 -0.023096 0.841216 11.00000 -1.50000 AFIX 0 O3 3 0.502564 0.343888 0.605621 11.00000 0.01214 0.01910 = 0.01652 -0.00366 0.00337 -0.00216 O4 3 0.351407 0.172003 0.658639 11.00000 0.01510 0.01955 = 0.02143 -0.00249 0.00249 -0.00405 O5 3 0.384356 0.378301 0.834594 11.00000 0.01405 0.02339 = 0.01969 -0.00285 0.00703 -0.00258 AFIX 147 H5A 2 0.358954 0.260884 0.831319 11.00000 -1.50000 AFIX 0 O6 3 0.394337 0.701883 0.697043 11.00000 0.01390 0.02120 = 0.01628 -0.00262 -0.00271 0.00743 AFIX 147 H6 2 0.380176 0.815838 0.715276 11.00000 -1.50000 AFIX 0 O7 3 0.486208 0.944490 0.851297 11.00000 0.02645 0.01886 = 0.02160 -0.00293 0.00079 0.00805 O8 3 0.708735 0.566745 0.980853 11.00000 0.01752 0.01947 = 0.01137 0.00265 -0.00004 -0.00251 AFIX 147 H8 2 0.772550 0.581760 1.029226 11.00000 -1.50000 AFIX 0 O9 3 0.915367 0.779941 0.908553 11.00000 0.01325 0.01927 = 0.01481 -0.00207 -0.00107 -0.00251 AFIX 147 H9A 2 0.957584 0.674469 0.912721 11.00000 -1.50000 AFIX 0 O10 3 0.752948 0.916002 0.783868 11.00000 0.02330 0.01258 = 0.01168 0.00204 0.00090 -0.00458 HKLF 4 REM dg_2_a.res in P2(1) REM R1 = 0.0471 for 2881 Fo > 4sig(Fo) and 0.0521 for all 3151 data REM 279 parameters refined using 1 restraints END WGHT 0.0634 0.0000 REM Highest difference peak 0.414, deepest hole -0.307, 1-sigma level 0.064 Q1 1 1.1732 0.1292 0.8164 11.00000 0.05 0.41 Q2 1 0.5002 0.6931 0.9091 11.00000 0.05 0.26 Q3 1 0.8276 1.0399 0.7964 11.00000 0.05 0.25 Q4 1 0.8807 0.1559 0.5589 11.00000 0.05 0.24 Q5 1 0.5215 1.0742 0.8058 11.00000 0.05 0.22 Q6 1 0.8408 0.3828 0.6939 11.00000 0.05 0.22 Q7 1 0.3247 0.4802 0.8392 11.00000 0.05 0.21 Q8 1 0.5315 0.4958 0.7784 11.00000 0.05 0.21 Q9 1 0.7331 0.7600 0.8825 11.00000 0.05 0.21 Q10 1 0.8217 0.5156 0.7703 11.00000 0.05 0.21 Q11 1 0.2714 0.3400 0.7899 11.00000 0.05 0.19 Q12 1 0.9796 0.2565 0.6187 11.00000 0.05 0.19 Q13 1 0.8613 0.2828 0.6376 11.00000 0.05 0.18 Q14 1 1.0014 0.2968 0.7875 11.00000 0.05 0.18 Q15 1 0.4326 0.4344 0.6167 11.00000 0.05 0.18 Q16 1 1.0196 -0.1148 0.5191 11.00000 0.05 0.18 Q17 1 1.1172 -0.1112 0.9214 11.00000 0.05 0.18 Q18 1 0.9399 0.1225 0.6572 11.00000 0.05 0.18 Q19 1 0.3182 0.6043 0.6791 11.00000 0.05 0.17 Q20 1 0.7885 0.6318 0.8248 11.00000 0.05 0.17 ; _shelx_res_checksum 28509 _shelx_hkl_file ; 0 -7 -6 4650.26 703.888 18 0 -7 -7 15893.8 1234.38 18 0 -6 -8 3302.33 767.507 25 0 -6 -9 11189.8 1192.50 21 0 -6 -9 10974.7 1207.77 25 0 -6 -9 13853.3 1324.23 18 0 -6 -10 719.019 350.030 25 0 -6 -10 953.052 424.318 18 0 -6 -10 1563.97 519.068 21 0 -6 -11 13196.2 1127.39 22 0 -6 -11 16464.6 1168.49 18 0 -5 -1 26788.4 4200.26 10 0 -5 -1 19246.8 3302.76 11 0 -5 -2 19117.5 3535.70 11 0 -5 -2 19950.0 3745.95 10 0 -5 -3 46907.0 5712.81 11 0 -5 -3 47206.5 5628.33 10 0 -5 -4 3735.72 1412.00 10 0 -5 -4 5824.87 2198.81 11 0 -5 -5 47755.4 5767.83 10 0 -5 -5 53219.6 6544.10 11 0 -5 -8 3520.49 946.033 21 0 -5 -8 2641.16 720.741 28 0 -5 -9 8419.27 1282.76 21 0 -5 -9 9227.50 1238.54 28 0 -5 -10-204.666 479.515 28 0 -5 -10-58.6944 538.823 21 0 -5 -11 677.279 605.509 21 0 -5 -11 1159.49 559.815 18 0 -5 -11 1460.85 615.742 25 0 -5 -12 4579.35 719.154 21 0 -5 -12 4934.77 799.900 25 0 -5 -12 5699.51 777.598 18 0 -5 -13 1753.66 369.838 18 0 -5 -13 1599.32 416.777 25 0 -4 0 12697.0 2531.33 2 0 -4 1 63042.5 6034.06 2 0 -4 -1 67796.4 6063.84 2 0 -4 -2 85647.2 6923.28 10 0 -4 -2 81193.0 6749.53 2 0 -4 -3 18810.5 3149.56 2 0 -4 -3 18526.3 3021.49 10 0 -4 -4 53795.1 5671.93 2 0 -4 -4 58385.0 5545.81 10 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10 -3 -3 17568.8 2010.36 7 -10 -3 2 7012.53 1070.30 23 10 -3 -2 6495.30 1447.62 7 -10 -3 1 19417.2 1700.72 23 -10 -3 0 2054.60 883.174 4 -10 -3 0 1873.19 637.288 23 -10 -3 -1 34756.0 2754.80 4 -10 -3 -2 4178.74 851.784 4 -10 -3 -3 6091.15 945.291 4 -10 -3 -4 5390.92 849.556 4 10 -2 -12 1020.05 641.273 4 10 -2 -11 3162.13 952.344 4 10 -2 -11 1847.74 507.700 27 10 -2 -10 6763.17 1073.93 7 -10 -2 9 1468.24 558.357 19 10 -2 -9 2174.32 816.911 7 -10 -2 8 12170.1 1377.13 19 10 -2 -8 17235.5 1859.85 7 10 -2 -7 6734.99 1282.29 7 -10 -2 6 4574.60 986.957 23 -10 -2 6 4214.43 903.931 20 10 -2 -6 6055.88 1283.45 7 -10 -2 5 4079.18 951.219 23 -10 -2 5 3169.80 796.133 20 10 -2 -5 3989.28 1145.87 7 -10 -2 4 15585.8 1701.42 23 -10 -2 4 13692.7 1525.23 20 -10 -2 3 22978.2 2043.73 23 10 -2 -3 27948.7 2725.90 7 -10 -2 2 7338.03 1134.90 23 -10 -2 1 2555.20 720.420 23 -10 -2 1 2182.33 840.737 4 -10 -2 0 976.659 652.000 4 -10 -2 -1 44721.1 3522.13 4 -10 -2 -2 6116.45 1263.53 4 -10 -2 -3 6877.08 1233.47 4 -10 -2 -4 1245.09 684.709 4 -10 -2 -5 246.774 409.089 4 -10 -2 -6 2612.48 579.365 4 10 -1 -13 2612.00 686.698 4 10 -1 -12 2273.34 801.724 4 10 -1 -12 1845.48 635.473 7 10 -1 -11-23.0676 550.314 7 10 -1 -10 7555.51 1236.02 7 10 -1 -9 10793.8 1568.05 7 10 -1 -8 1945.57 850.783 7 10 -1 -7 1176.30 834.252 7 10 -1 -6 18827.5 2253.14 7 10 -1 -5 18736.9 2187.82 7 -10 -1 4 20441.9 1974.91 23 10 -1 -4 21809.1 2407.03 7 -10 -1 3 25581.1 2225.90 23 10 -1 -3 34243.9 3025.37 7 -10 -1 2 2041.67 1093.38 4 10 -1 -2 4069.97 1300.92 7 -10 -1 1 7626.22 1494.12 4 -10 -1 0 1789.29 819.796 4 -10 -1 -1 3306.94 955.414 4 -10 -1 -2 30602.6 2792.38 4 -10 -1 -3-208.812 623.130 4 -10 -1 -4-918.760 693.469 4 -10 -1 -5 16495.2 1640.60 4 -10 -1 -6 15279.8 1570.61 4 10 0 -13 372.760 460.619 4 10 0 -12 2260.92 708.731 7 10 0 -11 945.092 679.079 7 10 0 -10 12469.3 1610.05 7 10 0 -9 5144.22 1214.06 7 10 0 -8 31365.4 2803.32 7 10 0 -7 20614.8 2328.39 7 -10 0 6 1127.21 554.343 26 10 0 -6-483.749 747.829 7 -10 0 5 14210.2 1745.36 26 10 0 -5 13579.1 1856.11 7 10 0 -4 117590. 6748.89 7 10 0 -3 2212.59 908.042 7 10 0 -2 13855.0 1891.21 7 -10 0 1 6591.16 1235.42 4 10 0 -1 8796.88 1548.36 7 -10 0 0 7414.41 1399.28 4 10 0 0 6993.62 1332.28 7 -10 0 -1 11272.5 1687.70 4 10 0 1 8424.91 1316.25 7 -10 0 -2 12717.1 1733.75 4 10 0 2 10990.3 1437.54 7 -10 0 -3 35935.8 2932.35 4 -10 0 -4-335.336 534.156 4 -10 0 -5 13734.2 1508.88 4 -10 0 -6 16792.9 1479.79 4 -10 0 -7 8068.58 927.641 5 10 1 -12 1112.46 549.710 4 10 1 -12 1892.37 607.539 7 10 1 -11 752.115 621.052 7 10 1 -10 7825.83 1316.25 7 10 1 -9 9550.38 1479.49 7 10 1 -8 912.295 658.080 7 -10 1 7 1510.46 736.812 26 10 1 -7 591.269 738.353 7 -10 1 6 15629.8 1915.10 26 10 1 -6 15486.8 1950.75 7 -10 1 5 13860.8 1824.28 26 10 1 -5 19082.2 2127.33 7 -10 1 4 21301.2 2281.67 26 10 1 -4 20321.2 2205.13 7 -10 1 3 32868.1 2925.47 26 10 1 -3 25331.8 2456.82 7 10 1 -2 2071.69 867.681 7 10 1 -1 5761.62 1155.24 7 -10 1 0 2516.68 1041.72 4 -10 1 -1 3901.60 900.076 4 -10 1 -2 28763.5 2612.39 4 -10 1 -3 215.254 560.573 4 -10 1 -4-168.537 489.048 4 -10 1 -5 13330.3 1359.47 4 -10 1 -5 14846.5 1391.56 26 -10 1 -6 13090.2 1429.38 5 10 2 -11 4541.78 914.974 7 10 2 -10 7576.06 1194.45 7 10 2 -9 2991.98 880.686 7 10 2 -8 15915.3 1845.94 7 -10 2 7 6633.69 1225.97 26 10 2 -7 7039.97 1248.27 7 -10 2 6 5509.83 1198.67 26 10 2 -6 6256.54 1195.76 7 -10 2 5 5639.41 1256.25 26 10 2 -5 4098.22 1014.75 7 -10 2 4 16924.0 2110.48 26 10 2 -4 13702.1 1637.96 7 -10 2 3 20601.9 2366.98 26 -10 2 2 7495.71 1407.21 5 -10 2 2 10587.2 1647.87 26 -10 2 1 2121.36 825.277 5 -10 2 1 2211.23 893.376 26 -10 2 0 1172.78 927.357 5 -10 2 0 984.342 763.015 26 -10 2 -1 44382.2 3756.24 5 -10 2 -1 45559.6 3466.80 26 -10 2 -2 6241.41 1410.95 5 -10 2 -2 6570.84 1270.92 26 -10 2 -3 4205.38 1102.84 5 -10 2 -3 5278.50 1030.39 26 -10 2 -4 1227.83 599.490 5 -10 2 -4 1135.32 547.010 26 -10 2 -5 1018.60 616.090 5 -10 2 -6 2575.10 619.995 5 -10 3 10 7114.86 970.843 9 -10 3 9 13207.6 1473.63 9 -10 3 8 5414.04 1054.09 9 10 3 -8 3339.42 798.889 7 -10 3 6 4512.09 1041.34 26 -10 3 5 249.244 772.550 26 -10 3 4 19635.4 2203.56 26 -10 3 3 13762.6 1920.40 26 -10 3 2 5115.33 1150.04 5 -10 3 2 5846.40 1264.99 26 -10 3 1 21944.9 2349.49 5 -10 3 1 23918.0 2415.76 26 -10 3 0 2198.17 967.192 5 -10 3 0 1916.72 951.891 26 -10 3 -1 38127.8 3194.80 5 -10 3 -1 39773.7 2999.15 26 -10 3 -2 5513.61 1202.80 5 -10 3 -2 6831.53 1108.33 26 -10 3 -3 7511.24 1255.94 5 -10 3 -3 5422.40 814.056 26 -10 3 -4 7223.05 1135.98 5 -10 3 -5 5176.74 830.183 5 -10 4 9 433.978 404.221 9 -10 4 8 5043.25 973.241 9 -10 4 7 3869.90 882.637 9 -10 4 6 1277.20 778.871 9 -10 4 5 4273.66 1018.05 9 -10 4 4 483.713 695.782 9 -10 4 3 5792.37 1127.70 9 -10 4 2 1279.87 604.270 5 -10 4 2 1486.32 713.550 9 -10 4 2 451.735 660.413 26 -10 4 1 614.238 621.403 5 -10 4 1 1052.63 700.641 26 -10 4 0 1302.92 625.380 5 -10 4 0 574.435 481.754 26 -10 4 -1 9413.73 1351.06 5 -10 4 -2 8434.97 1213.06 5 -10 4 -3 2036.70 661.440 5 -10 5 5 5384.91 789.705 9 -10 5 4 38063.7 2331.37 9 -11 -4 4 16741.6 1292.24 23 -11 -4 3 3833.24 604.153 23 11 -3 -7 3114.03 718.004 7 11 -3 -6 8697.50 1152.10 7 -11 -3 5 16247.8 1483.80 23 11 -3 -5 16795.8 1668.19 7 -11 -3 4 141.879 413.483 23 11 -3 -4-623.934 570.130 7 -11 -3 3 13335.4 1280.07 23 11 -3 -3 17353.1 1778.21 7 -11 -3 2 1453.57 517.845 23 11 -3 -2 1216.72 547.020 7 11 -3 -1 2456.02 768.956 7 11 -3 0 13176.1 1418.90 7 11 -3 1 9794.57 1156.99 7 11 -3 2 3184.51 659.071 7 11 -2 -10 261.838 449.716 7 11 -2 -9 781.605 508.300 7 11 -2 -8 320.733 507.536 7 11 -2 -7 2600.93 851.730 7 11 -2 -6 6793.63 1186.69 7 11 -2 -5 26541.3 2434.11 7 11 -2 -4 23597.0 2300.99 7 -11 -2 3 939.544 390.010 23 11 -2 -3 290.598 694.482 7 11 -2 -2 13609.0 1708.68 7 11 -2 -1 23963.5 2243.81 7 11 -2 0 12569.5 1564.54 7 11 -2 1 31389.7 2414.53 7 -11 -2 -2 16994.2 1677.36 4 11 -2 2 17487.5 1600.00 7 -11 -2 -3 4610.16 769.557 4 11 -2 3 4912.52 778.004 7 11 -1 -11 119.040 395.408 7 11 -1 -10 4046.88 827.229 7 11 -1 -9 6969.97 1138.22 7 11 -1 -8 1931.96 880.707 7 11 -1 -7 14972.8 1804.94 7 11 -1 -6 19844.3 2105.38 7 11 -1 -5 5142.18 1086.70 7 -11 -1 4 11621.9 1502.93 26 11 -1 -4 12748.8 1671.59 7 11 -1 -3 41103.0 3262.38 7 11 -1 -2 793.703 771.596 7 11 -1 -1 26576.7 2406.28 7 11 -1 0 14408.0 1690.38 7 -11 -1 -1 27231.9 2372.11 4 11 -1 1 25820.9 2182.02 7 -11 -1 -2 31771.4 2462.04 4 11 -1 2 28299.4 2149.57 7 -11 -1 -3 4945.00 897.193 4 11 -1 3 4118.36 705.444 7 -11 -1 -4 2586.74 604.822 4 11 0 -11 1324.29 613.163 7 11 0 -10 3337.46 860.914 7 11 0 -9 38550.3 2855.01 7 11 0 -8 744.729 661.065 7 11 0 -7 2792.41 888.911 7 11 0 -6 22387.5 2276.48 7 -11 0 5 815.204 680.839 26 11 0 -5 1333.10 817.285 7 -11 0 4 241.969 613.170 26 11 0 -4-221.744 670.050 7 -11 0 3 23449.4 2269.06 26 11 0 -3 23509.2 2291.40 7 11 0 -2 6508.77 1208.47 7 11 0 -1 996.013 699.865 7 11 0 0 10300.3 1272.92 7 11 0 1 4273.49 829.144 7 -11 0 -2 48953.7 3279.89 4 -11 0 -3-338.323 476.217 4 -11 0 -4 13047.9 1243.54 26 -11 0 -5 20720.3 1649.98 5 11 1 -11 41.5801 436.542 7 11 1 -10 4194.47 825.369 7 11 1 -9 6832.69 1153.52 7 11 1 -8 208.159 617.693 7 -11 1 7 8879.42 1216.52 26 11 1 -7 12818.4 1624.59 7 -11 1 6 17517.9 1835.51 26 11 1 -6 21127.0 2090.77 7 -11 1 5 3546.03 893.537 26 11 1 -5 4307.43 979.900 7 -11 1 4 11524.5 1557.70 26 11 1 -4 10809.1 1482.58 7 -11 1 3 37740.2 2984.79 26 11 1 -3 35310.0 2690.92 7 -11 1 2 993.521 795.115 26 11 1 -2 2054.07 726.311 7 -11 1 1 28739.0 2542.89 26 -11 1 0 13381.5 1653.77 26 -11 1 -1 32114.7 2644.26 26 -11 1 -2 35171.3 2619.93 26 -11 1 -3 5234.41 1057.81 5 -11 1 -3 4940.23 838.730 26 -11 1 -4 4043.82 801.177 5 -11 1 -4 2441.67 523.164 26 -11 2 10 962.617 432.040 9 11 2 -10 2111.80 626.808 7 11 2 -9 1994.60 681.877 7 11 2 -8 1018.08 567.471 7 11 2 -7 2813.88 802.395 7 -11 2 6 5773.88 1074.21 26 11 2 -6 5539.02 977.320 7 -11 2 5 21757.1 2046.87 26 11 2 -5 17257.8 1650.25 7 -11 2 4 21283.9 2119.76 26 -11 2 3 1122.68 734.123 26 -11 2 2 11697.2 1604.06 26 -11 2 1 18319.8 1932.96 5 -11 2 1 21689.5 2100.97 26 -11 2 0 9964.87 1479.17 5 -11 2 0 11196.6 1481.00 26 -11 2 -1 32439.1 2618.88 5 -11 2 -1 31189.1 2445.15 26 -11 2 -2 19405.8 1878.52 5 -11 2 -2 17811.3 1636.40 26 -11 2 -3 5580.25 929.201 5 -11 2 -3 4811.20 737.687 26 -11 2 -4 1176.91 434.349 5 -11 3 9-831.751 456.515 9 -11 3 8 737.896 607.650 9 -11 3 7 2352.12 816.137 9 -11 3 6 9589.55 1350.55 9 -11 3 5 15089.0 1603.22 26 -11 3 4-549.808 644.477 26 -11 3 3 17528.5 1817.16 26 -11 3 2 1073.30 583.014 26 -11 3 2 427.492 520.836 9 -11 3 1 1945.19 708.334 5 -11 3 1 2713.13 791.301 26 -11 3 0 10396.2 1315.08 5 -11 3 0 10887.5 1299.05 26 -11 3 -1 8075.92 1126.47 5 -11 3 -1 6987.52 945.282 26 -11 3 -2 4504.42 802.275 5 -11 4 6 1422.51 532.987 9 -11 4 5 17330.1 1494.72 9 -11 4 4 14109.5 1288.89 9 12 -2 -7 27915.5 2002.53 7 12 -2 -6 3501.80 736.416 7 12 -2 -5 10586.3 1254.59 7 12 -2 -4 542.887 582.139 7 12 -2 -3 2311.83 684.620 7 -12 -2 2 875.026 418.064 26 12 -2 -2 1172.39 556.425 7 -12 -2 1 7613.77 890.539 26 12 -2 -1 7921.55 995.781 7 12 -2 0 588.580 394.167 7 12 -1 -9 6223.73 894.646 7 12 -1 -8 2058.73 687.060 7 12 -1 -7 12852.9 1420.24 7 12 -1 -6 9711.65 1286.61 7 12 -1 -5 27037.1 2210.42 7 -12 -1 4 5593.56 869.084 26 12 -1 -4 8241.14 1108.06 7 -12 -1 3 16436.2 1549.22 26 12 -1 -3 15923.7 1608.98 7 -12 -1 2 1297.89 593.622 26 12 -1 -2 2965.98 692.520 7 -12 -1 1 15550.6 1467.86 26 12 -1 -1 13476.2 1352.02 7 -12 -1 0 313.129 385.457 26 12 -1 0 461.755 394.969 7 -12 -1 -1 14566.5 1289.59 26 12 0 -9 14737.7 1414.93 7 12 0 -8 34469.8 2436.30 7 12 0 -7 43296.0 2899.41 7 12 0 -6 10160.6 1286.67 7 -12 0 5 301.791 372.945 26 12 0 -5 1809.05 659.400 7 -12 0 4 6162.88 976.132 26 12 0 -4 6108.34 1084.11 7 -12 0 3 3983.15 845.964 26 12 0 -3 3936.80 767.412 7 -12 0 2 883.391 524.075 26 12 0 -2-509.608 442.551 7 -12 0 1 14016.1 1401.92 26 12 0 -1 8355.12 1010.10 7 -12 0 0 4058.93 780.049 5 -12 0 0 4855.85 842.230 26 -12 0 -1 6350.81 907.827 5 -12 0 -1 4282.59 735.063 26 -12 0 -2 514.600 328.057 26 12 1 -9 4466.60 727.626 7 12 1 -8 1975.93 595.998 7 12 1 -7 11713.1 1265.38 7 -12 1 6 5211.08 790.317 26 12 1 -6 7698.66 1047.17 7 -12 1 5 19959.7 1707.38 26 12 1 -5 18441.0 1634.21 7 -12 1 4 7681.06 1074.18 26 12 1 -4 6466.27 929.243 7 -12 1 3 16111.5 1620.95 26 -12 1 2 1816.26 597.714 26 -12 1 1 15218.8 1504.20 26 -12 1 0-15.1624 369.282 5 -12 1 0 252.497 385.751 26 -12 1 -1 14357.8 1290.37 26 -12 2 8 2592.86 614.821 9 -12 2 5 7298.15 969.312 26 -12 2 4 775.567 478.076 26 -12 2 3 2576.03 686.355 26 -12 2 2 812.573 463.999 26 -12 2 1 8374.69 1044.25 26 -12 2 0-10.1204 355.700 26 0 0 0 0.00 0.00 0 TITL dg_2 in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 10.368647 6.633773 13.633854 90.0000 103.9428 90.0000 ZERR 4.00 0.000320 0.000224 0.000427 0.0000 0.0031 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 44.00 40.00 4.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 37130 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 C1 C 0.9596(3) 0.3295(6) 0.8138(3) 0.0147(7) Uani 1 1 d . . . . . H1 H 0.903177 0.228204 0.835164 0.018 Uiso 1 1 calc R . . . . C2 C 1.0637(3) 0.2223(6) 0.7723(3) 0.0184(8) Uani 1 1 d . . . . . H2 H 1.136423 0.316856 0.772741 0.022 Uiso 1 1 calc R . . . . C3 C 1.0120(4) 0.1475(6) 0.6663(3) 0.0167(7) Uani 1 1 d . . . . . H3 H 1.065510 0.061292 0.639655 0.020 Uiso 1 1 calc R . . . . C4 C 0.8939(3) 0.1975(6) 0.6083(3) 0.0148(7) Uani 1 1 d . . . . . C5 C 0.7984(3) 0.3300(6) 0.6478(3) 0.0127(7) Uani 1 1 d . . . . . H5 H 0.743166 0.238585 0.676723 0.015 Uiso 1 1 calc R . . . . C6 C 0.7028(4) 0.4519(6) 0.5667(3) 0.0151(7) Uani 1 1 d . . . . . H6A H 0.748830 0.567183 0.547457 0.018 Uiso 1 1 calc R . . . . H6B H 0.670787 0.369065 0.507163 0.018 Uiso 1 1 calc R . . . . C7 C 0.5860(4) 0.5236(5) 0.6071(3) 0.0137(7) Uani 1 1 d . . . . . H7 H 0.535241 0.620612 0.558594 0.016 Uiso 1 1 calc R . . . . C8 C 0.6288(3) 0.6297(5) 0.7099(3) 0.0130(7) Uani 1 1 d . . . . . C9 C 0.7595(3) 0.5565(6) 0.7841(3) 0.0123(7) Uani 1 1 d . . . . . H9 H 0.735002 0.448791 0.825330 0.015 Uiso 1 1 calc R . . . . C10 C 0.8709(3) 0.4706(5) 0.7360(3) 0.0126(7) Uani 1 1 d . . . . . C11 C 0.7857(3) 0.7479(6) 0.8508(3) 0.0135(7) Uani 1 1 d . . . . . C12 C 0.6894(3) 0.7448(5) 0.9216(3) 0.0136(7) Uani 1 1 d . . . . . H12 H 0.705925 0.862764 0.966080 0.016 Uiso 1 1 calc R . . . . C13 C 0.5460(4) 0.7459(6) 0.8617(3) 0.0155(7) Uani 1 1 d . . . . . C14 C 0.5109(4) 0.6236(6) 0.7628(3) 0.0146(7) Uani 1 1 d . . . . . C15 C 0.4813(3) 0.4007(6) 0.7791(3) 0.0147(7) Uani 1 1 d . . . . . H15 H 0.563406 0.335761 0.816376 0.018 Uiso 1 1 calc R . . . . C16 C 0.4359(3) 0.2986(6) 0.6760(3) 0.0149(7) Uani 1 1 d . . . . . C18 C 0.4424(4) 0.7934(7) 0.9139(3) 0.0214(8) Uani 1 1 d . . . . . H18A H 0.355512 0.733319 0.888434 0.026 Uiso 1 1 calc R . . . . H18B H 0.468697 0.810716 0.986619 0.026 Uiso 1 1 calc R . . . . C19 C 0.9559(4) 0.6297(6) 0.6994(3) 0.0167(7) Uani 1 1 d . . . . . H19A H 1.021245 0.681388 0.756075 0.025 Uiso 1 1 calc GR . . . . H19B H 0.900031 0.737862 0.667066 0.025 Uiso 1 1 calc GR . . . . H19C H 0.999618 0.569433 0.652116 0.025 Uiso 1 1 calc GR . . . . C29 C 0.8462(4) 0.1077(7) 0.5039(3) 0.0192(8) Uani 1 1 d . . . . . H29A H 0.836009 0.212815 0.454268 0.029 Uiso 1 1 calc GR . . . . H29B H 0.762308 0.042079 0.498734 0.029 Uiso 1 1 calc GR . . . . H29C H 0.910034 0.011179 0.492542 0.029 Uiso 1 1 calc GR . . . . C30 C 0.6616(4) 0.8494(6) 0.6925(3) 0.0161(7) Uani 1 1 d . . . . . H30A H 0.702022 0.860161 0.635553 0.019 Uiso 1 1 calc R . . . . H30B H 0.581589 0.930841 0.678860 0.019 Uiso 1 1 calc R . . . . O1 O 1.0267(3) 0.4447(4) 0.90136(19) 0.0164(5) Uani 1 1 d . . . . . H1A H 1.040811 0.372299 0.951579 0.025 Uiso 1 1 calc GR . . . . O2 O 1.1155(3) 0.0562(4) 0.8398(2) 0.0236(6) Uani 1 1 d . . . . . H2A H 1.055321 -0.023096 0.841216 0.035 Uiso 1 1 calc GR . . . . O3 O 0.5026(2) 0.3439(4) 0.60562(19) 0.0159(5) Uani 1 1 d . . . . . O4 O 0.3514(3) 0.1720(4) 0.6586(2) 0.0190(6) Uani 1 1 d . . . . . O5 O 0.3844(2) 0.3783(4) 0.8346(2) 0.0185(6) Uani 1 1 d . . . . . H5A H 0.358954 0.260884 0.831319 0.028 Uiso 1 1 calc GR . . . . O6 O 0.3943(3) 0.7019(4) 0.6970(2) 0.0182(6) Uani 1 1 d . . . . . H6 H 0.380176 0.815838 0.715276 0.027 Uiso 1 1 calc GR . . . . O7 O 0.4862(3) 0.9445(5) 0.8513(2) 0.0232(6) Uani 1 1 d . . . . . O8 O 0.7087(3) 0.5667(4) 0.98085(18) 0.0167(5) Uani 1 1 d . . . . . H8 H 0.772550 0.581760 1.029226 0.025 Uiso 1 1 calc GR . . . . O9 O 0.9154(2) 0.7799(4) 0.90855(19) 0.0165(5) Uani 1 1 d . . . . . H9A H 0.957584 0.674469 0.912721 0.025 Uiso 1 1 calc GR . . . . O10 O 0.7529(3) 0.9160(4) 0.78387(18) 0.0164(6) Uani 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 0.0112(15) 0.016(2) 0.0136(16) -0.0009(13) -0.0028(13) -0.0035(13) C2 0.0117(17) 0.019(2) 0.0214(19) -0.0024(14) -0.0013(14) 0.0005(14) C3 0.0125(16) 0.0157(19) 0.0221(19) -0.0034(14) 0.0047(14) 0.0010(13) C4 0.0138(16) 0.0180(19) 0.0140(17) -0.0004(13) 0.0064(13) -0.0035(13) C5 0.0096(15) 0.0150(19) 0.0130(16) 0.0001(13) 0.0017(13) -0.0019(13) C6 0.0143(16) 0.0180(19) 0.0119(16) 0.0011(13) 0.0008(13) -0.0012(14) C7 0.0161(17) 0.0131(18) 0.0113(15) -0.0002(12) 0.0019(13) -0.0010(13) C8 0.0134(16) 0.0118(18) 0.0133(17) -0.0021(12) 0.0021(13) -0.0011(13) C9 0.0110(16) 0.0122(19) 0.0131(16) -0.0008(12) 0.0019(13) -0.0028(12) C10 0.0139(16) 0.0110(19) 0.0133(16) -0.0002(12) 0.0043(13) -0.0022(13) C11 0.0131(15) 0.0134(18) 0.0132(16) 0.0001(12) 0.0014(13) -0.0029(12) C12 0.0156(16) 0.0126(18) 0.0128(16) -0.0010(12) 0.0036(13) -0.0012(13) C13 0.0148(17) 0.016(2) 0.0141(17) -0.0009(13) 0.0013(13) 0.0032(13) C14 0.0115(16) 0.018(2) 0.0131(17) 0.0001(13) -0.0004(13) 0.0037(13) C15 0.0121(16) 0.0166(19) 0.0153(16) -0.0002(13) 0.0035(13) 0.0003(13) C16 0.0107(15) 0.0158(19) 0.0172(17) -0.0010(13) 0.0018(13) 0.0031(14) C18 0.0177(17) 0.025(2) 0.0202(19) -0.0055(15) 0.0029(15) 0.0061(16) C19 0.0154(17) 0.019(2) 0.0162(17) -0.0005(13) 0.0040(13) -0.0031(14) C29 0.0168(17) 0.027(2) 0.0140(18) -0.0008(14) 0.0032(14) 0.0016(14) C30 0.0195(17) 0.0140(19) 0.0129(16) 0.0011(12) 0.0003(14) 0.0005(14) O1 0.0171(12) 0.0171(14) 0.0123(12) 0.0010(9) -0.0020(10) -0.0019(10) O2 0.0224(14) 0.0187(16) 0.0238(14) -0.0029(11) -0.0057(11) 0.0052(11) O3 0.0121(11) 0.0191(14) 0.0165(12) -0.0037(10) 0.0034(10) -0.0022(9) O4 0.0151(12) 0.0195(15) 0.0214(13) -0.0025(10) 0.0025(10) -0.0041(10) O5 0.0140(12) 0.0234(15) 0.0197(13) -0.0029(10) 0.0070(10) -0.0026(10) O6 0.0139(12) 0.0212(15) 0.0163(12) -0.0026(10) -0.0027(10) 0.0074(10) O7 0.0264(14) 0.0189(15) 0.0216(13) -0.0029(11) 0.0008(11) 0.0080(11) O8 0.0175(12) 0.0195(15) 0.0114(12) 0.0026(9) 0.0000(10) -0.0025(10) O9 0.0133(12) 0.0193(14) 0.0148(12) -0.0021(10) -0.0011(9) -0.0025(10) O10 0.0233(13) 0.0126(14) 0.0117(12) 0.0020(9) 0.0009(10) -0.0046(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' 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 C2 C1 C10 112.9(3) . . ? O1 C1 C2 108.3(3) . . ? O1 C1 C10 109.6(3) . . ? C3 C2 C1 113.3(3) . . ? O2 C2 C1 107.9(3) . . ? O2 C2 C3 110.6(3) . . ? C4 C3 C2 123.7(3) . . ? C3 C4 C5 121.3(3) . . ? C3 C4 C29 120.5(3) . . ? C29 C4 C5 118.0(3) . . ? C4 C5 C6 114.5(3) . . ? C4 C5 C10 112.6(3) . . ? C6 C5 C10 110.4(3) . . ? C7 C6 C5 109.7(3) . . ? C6 C7 C8 113.1(3) . . ? O3 C7 C6 105.0(3) . . ? O3 C7 C8 115.1(3) . . ? C7 C8 C9 117.7(3) . . ? C7 C8 C14 108.8(3) . . ? C9 C8 C14 110.2(3) . . ? C30 C8 C7 108.8(3) . . ? C30 C8 C9 101.9(3) . . ? C30 C8 C14 108.9(3) . . ? C8 C9 C10 117.0(3) . . ? C11 C9 C8 97.3(3) . . ? C11 C9 C10 120.1(3) . . ? C1 C10 C5 105.3(3) . . ? C1 C10 C9 108.1(3) . . ? C5 C10 C9 105.8(3) . . ? C19 C10 C1 110.3(3) . . ? C19 C10 C5 111.6(3) . . ? C19 C10 C9 115.2(3) . . ? C9 C11 C12 107.9(3) . . ? O9 C11 C9 117.6(3) . . ? O9 C11 C12 109.1(3) . . ? O9 C11 O10 106.8(3) . . ? O10 C11 C9 106.5(3) . . ? O10 C11 C12 108.6(3) . . ? C13 C12 C11 111.2(3) . . ? O8 C12 C11 110.0(3) . . ? O8 C12 C13 107.3(3) . . ? C12 C13 C14 117.6(3) . . ? C18 C13 C12 118.7(3) . . ? C18 C13 C14 119.7(3) . . ? O7 C13 C12 113.5(3) . . ? O7 C13 C14 112.9(3) . . ? O7 C13 C18 60.2(3) . . ? C13 C14 C8 110.2(3) . . ? C15 C14 C8 107.3(3) . . ? C15 C14 C13 113.2(3) . . ? O6 C14 C8 109.9(3) . . ? O6 C14 C13 110.2(3) . . ? O6 C14 C15 105.9(3) . . ? C16 C15 C14 108.8(3) . . ? O5 C15 C14 111.9(3) . . ? O5 C15 C16 110.3(3) . . ? O3 C16 C15 117.4(3) . . ? O4 C16 C15 122.8(3) . . ? O4 C16 O3 119.6(3) . . ? O7 C18 C13 59.5(2) . . ? O10 C30 C8 106.5(3) . . ? C16 O3 C7 125.0(3) . . ? C13 O7 C18 60.2(2) . . ? C11 O10 C30 108.6(3) . . ? 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 C1 C2 1.512(5) . ? C1 C10 1.542(5) . ? C1 O1 1.446(4) . ? C2 C3 1.499(5) . ? C2 O2 1.454(5) . ? C3 C4 1.329(5) . ? C4 C5 1.516(5) . ? C4 C29 1.512(5) . ? C5 C6 1.527(5) . ? C5 C10 1.563(5) . ? C6 C7 1.523(5) . ? C7 C8 1.535(5) . ? C7 O3 1.470(4) . ? C8 C9 1.561(5) . ? C8 C14 1.563(5) . ? C8 C30 1.528(5) . ? C9 C10 1.566(5) . ? C9 C11 1.547(5) . ? C10 C19 1.534(5) . ? C11 C12 1.547(5) . ? C11 O9 1.401(4) . ? C11 O10 1.429(4) . ? C12 C13 1.514(5) . ? C12 O8 1.418(4) . ? C13 C14 1.540(5) . ? C13 C18 1.458(5) . ? C13 O7 1.448(5) . ? C14 C15 1.537(5) . ? C14 O6 1.418(4) . ? C15 C16 1.529(5) . ? C15 O5 1.404(4) . ? C16 O3 1.344(5) . ? C16 O4 1.195(5) . ? C18 O7 1.458(5) . ? C30 O10 1.440(4) . ?