#------------------------------------------------------------------------------ #$Date: 2017-12-23 02:06:04 +0200 (Sat, 23 Dec 2017) $ #$Revision: 204488 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/85/1548536.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_1548536 loop_ _publ_author_name 'Zhou, Junfei' 'Liu, Tingting' 'Zhang, Hanqi' 'Zheng, Guijuan' 'Qiu, Yue' 'Deng, Mengyi' 'Zhang, Chun' 'Yao, Guangmin' _publ_section_title ; Anti-inflammatory Grayanane Diterpenoids from the Leaves of Rhododendron molle ; _journal_name_full 'Journal of Natural Products' _journal_paper_doi 10.1021/acs.jnatprod.7b00799 _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_moiety 'C20 H34 O7, C2 H5 O' _chemical_formula_sum 'C22 H39 O8' _chemical_formula_weight 431.53 _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' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M '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 10.3826(3) _cell_length_b 10.5016(3) _cell_length_c 19.1653(6) _cell_measurement_reflns_used 9869 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 68.25 _cell_measurement_theta_min 4.61 _cell_volume 2089.67(11) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'D8 VENTURE CMOS photon 100' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_unetI/netI 0.0161 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 18724 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.261 _diffrn_reflns_theta_min 4.614 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.372 _exptl_crystal_description block _exptl_crystal_F_000 940 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.481 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.058 _refine_ls_abs_structure_details ; Flack x determined using 1581 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 301 _refine_ls_number_reflns 3822 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0369 _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^)+(0.0725P)^2^+1.1123P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1048 _refine_ls_wR_factor_ref 0.1059 _reflns_Friedel_coverage 0.747 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 3748 _reflns_number_total 3822 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np7b00799_si_009.cif _cod_data_source_block t_a _cod_database_code 1548536 _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 0.849 _shelx_estimated_absorpt_t_max 0.849 _shelx_res_file ; t_a.res created by SHELXL-2014/7 TITL t_a.res in P2(1)2(1)2(1) REM Old TITL t in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.097, Rweak 0.028, Alpha 0.002, Orientation as input REM Flack x = -0.007 ( 0.032 ) from Parsons' quotients REM Formula found by SHELXT: C20 O9 CELL 1.54178 10.3826 10.5016 19.1653 90.000 90.000 90.000 ZERR 4.000 0.0003 0.0003 0.0006 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H O UNIT 88 156 32 TEMP -100.150 L.S. 50 ACTA SIZE 0.20 0.20 0.20 CONF BOND $H LIST 6 FMAP 2 PLAN 20 REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### REM ##### WGHT 0.072500 1.112300 FVAR 0.99165 O1 3 1.002978 0.772311 0.720642 11.00000 0.01506 0.02296 = 0.02653 -0.00980 -0.00375 -0.00094 C1 1 0.817367 0.671206 0.665392 11.00000 0.01426 0.01208 = 0.01217 -0.00050 -0.00099 0.00027 AFIX 13 H1 2 0.888556 0.677029 0.630392 11.00000 -1.20000 AFIX 0 O2 3 0.670246 0.823478 0.779418 11.00000 0.02034 0.02138 = 0.01445 0.00331 0.00225 0.00281 AFIX 148 H2A 2 0.687381 0.774253 0.807248 11.00000 -1.50000 AFIX 0 C23 1 0.264152 0.636028 0.634820 11.00000 0.38057 0.30003 = 0.12617 0.05149 0.03390 0.23740 AFIX 23 H23A 2 0.294966 0.694094 0.597707 11.00000 -1.20000 H23B 2 0.264702 0.688490 0.677737 11.00000 -1.20000 AFIX 0 C22 1 0.374366 0.557306 0.645396 11.00000 0.02449 0.02934 = 0.04849 0.00611 -0.00762 -0.00766 AFIX 93 H22A 2 0.366529 0.467317 0.642635 11.00000 -1.20000 H22B 2 0.455617 0.594857 0.655204 11.00000 -1.20000 AFIX 0 C2 1 0.870255 0.739290 0.731823 11.00000 0.01602 0.01555 = 0.01430 -0.00138 -0.00199 0.00205 AFIX 13 H2 2 0.862048 0.682228 0.773358 11.00000 -1.20000 AFIX 0 O3 3 0.582166 0.719495 0.658602 11.00000 0.01356 0.01856 = 0.01788 -0.00068 0.00141 -0.00107 C3 1 0.784295 0.856930 0.740684 11.00000 0.01604 0.01459 = 0.01484 -0.00171 -0.00097 0.00059 AFIX 13 H3 2 0.832026 0.928332 0.763556 11.00000 -1.20000 AFIX 0 O4 3 0.629411 0.851609 0.529410 11.00000 0.02492 0.01695 = 0.01341 0.00199 -0.00385 0.00748 AFIX 148 H4 2 0.626169 0.847181 0.490749 11.00000 -1.50000 AFIX 0 C4 1 0.741957 0.892791 0.666299 11.00000 0.01709 0.01345 = 0.01442 0.00006 -0.00156 0.00073 O7 3 0.800559 0.346201 0.386719 11.00000 0.03356 0.01974 = 0.01341 -0.00206 0.00007 0.00034 C7 1 0.658904 0.624867 0.526140 11.00000 0.01362 0.01651 = 0.01439 -0.00072 -0.00251 0.00271 AFIX 23 H7A 2 0.650232 0.636356 0.475085 11.00000 -1.20000 H7B 2 0.570967 0.611767 0.544776 11.00000 -1.20000 AFIX 0 O6 3 0.880771 0.566479 0.446276 11.00000 0.01805 0.02041 = 0.01439 0.00424 0.00203 -0.00311 C6 1 0.708431 0.750491 0.555980 11.00000 0.01431 0.01344 = 0.01210 0.00143 -0.00111 0.00262 AFIX 13 H6 2 0.798666 0.763932 0.539288 11.00000 -1.20000 AFIX 0 O5 3 0.923515 0.477050 0.691780 11.00000 0.01651 0.01566 = 0.01893 0.00266 -0.00432 0.00307 H5 2 0.574954 0.747247 0.704825 11.00000 0.05793 C5 1 0.707618 0.757792 0.635754 11.00000 0.01275 0.01357 = 0.01155 0.00057 -0.00002 -0.00096 C8 1 0.733757 0.500637 0.537965 11.00000 0.01298 0.01212 = 0.01187 -0.00114 -0.00292 -0.00068 O8 3 0.132101 0.629738 0.620032 11.00000 0.02713 0.03405 = 0.02465 -0.00097 0.00114 0.00536 AFIX 148 H8A 2 0.089684 0.684040 0.647504 11.00000 -1.50000 AFIX 0 H8 2 1.024877 0.831986 0.747416 11.00000 0.03406 C9 1 0.730272 0.450922 0.614530 11.00000 0.01199 0.01345 = 0.01415 -0.00082 0.00081 -0.00023 AFIX 13 H9 2 0.636844 0.445913 0.626911 11.00000 -1.20000 AFIX 0 C10 1 0.795198 0.526727 0.676167 11.00000 0.01521 0.01417 = 0.01329 0.00130 -0.00256 0.00241 H10 2 0.951183 0.598731 0.446820 11.00000 0.01434 C11 1 0.779268 0.311770 0.616412 11.00000 0.01856 0.01214 = 0.01525 0.00140 -0.00013 -0.00119 AFIX 23 H11A 2 0.795818 0.287207 0.665471 11.00000 -1.20000 H11B 2 0.711115 0.255017 0.598025 11.00000 -1.20000 AFIX 0 H11 2 0.829856 0.419368 0.386272 11.00000 0.04643 C12 1 0.903119 0.291731 0.573634 11.00000 0.01879 0.01398 = 0.01589 0.00087 -0.00081 0.00481 AFIX 23 H12A 2 0.977229 0.326013 0.600160 11.00000 -1.20000 H12B 2 0.917339 0.199281 0.567097 11.00000 -1.20000 AFIX 0 H12 2 0.981937 0.518382 0.669319 11.00000 0.03567 C13 1 0.897999 0.356323 0.502020 11.00000 0.01391 0.01632 = 0.01373 -0.00110 0.00139 0.00253 AFIX 13 H13 2 0.979316 0.340875 0.475370 11.00000 -1.20000 AFIX 0 C14 1 0.873993 0.499567 0.511514 11.00000 0.01304 0.01474 = 0.01168 0.00210 0.00034 0.00010 AFIX 13 H14 2 0.934090 0.537064 0.546733 11.00000 -1.20000 AFIX 0 C15 1 0.669915 0.397492 0.489575 11.00000 0.01497 0.01452 = 0.01666 -0.00265 -0.00252 -0.00107 AFIX 23 H15A 2 0.609076 0.344486 0.516750 11.00000 -1.20000 H15B 2 0.621889 0.439125 0.451221 11.00000 -1.20000 AFIX 0 C16 1 0.779860 0.313845 0.459612 11.00000 0.02103 0.01563 = 0.01264 -0.00082 -0.00152 0.00105 C17 1 0.755145 0.170767 0.458648 11.00000 0.02574 0.01526 = 0.02168 -0.00284 -0.00109 0.00001 AFIX 137 H17A 2 0.689332 0.151106 0.423613 11.00000 -1.50000 H17B 2 0.725112 0.143246 0.504720 11.00000 -1.50000 H17C 2 0.835102 0.125968 0.446993 11.00000 -1.50000 AFIX 0 C18 1 0.855323 0.954644 0.627411 11.00000 0.02185 0.01516 = 0.01996 0.00131 0.00082 -0.00462 AFIX 137 H18A 2 0.926340 0.893522 0.623826 11.00000 -1.50000 H18B 2 0.884334 1.030066 0.653096 11.00000 -1.50000 H18C 2 0.827572 0.979779 0.580517 11.00000 -1.50000 AFIX 0 C19 1 0.630675 0.988493 0.668149 11.00000 0.02257 0.01442 = 0.02064 0.00023 -0.00162 0.00492 AFIX 137 H19A 2 0.613414 1.019332 0.620802 11.00000 -1.50000 H19B 2 0.653993 1.060475 0.698139 11.00000 -1.50000 H19C 2 0.553421 0.946901 0.686689 11.00000 -1.50000 AFIX 0 C20 1 0.717744 0.493871 0.741992 11.00000 0.02634 0.01581 = 0.01583 0.00094 0.00488 -0.00193 AFIX 137 H20A 2 0.635829 0.540223 0.741395 11.00000 -1.50000 H20B 2 0.767129 0.518334 0.783456 11.00000 -1.50000 H20C 2 0.700836 0.402086 0.743142 11.00000 -1.50000 AFIX 0 HKLF 4 REM t_a.res in P2(1)2(1)2(1) REM R1 = 0.0369 for 3748 Fo > 4sig(Fo) and 0.0377 for all 3822 data REM 301 parameters refined using 0 restraints END WGHT 0.0611 0.9972 REM Highest difference peak 0.481, deepest hole -0.635, 1-sigma level 0.058 Q1 1 0.7650 0.8743 0.7014 11.00000 0.05 0.22 Q2 1 0.7376 0.4824 0.5749 11.00000 0.05 0.21 Q3 1 0.7950 0.6015 0.6683 11.00000 0.05 0.21 Q4 1 0.7041 0.5628 0.5341 11.00000 0.05 0.20 Q5 1 0.7705 0.2428 0.4594 11.00000 0.05 0.20 Q6 1 0.7295 0.8288 0.6491 11.00000 0.05 0.20 Q7 1 0.7035 0.7571 0.5972 11.00000 0.05 0.20 Q8 1 0.8373 0.3269 0.4816 11.00000 0.05 0.19 Q9 1 0.7907 0.3194 0.4302 11.00000 0.05 0.17 Q10 1 0.6502 0.0428 0.5253 11.00000 0.05 0.17 Q11 1 0.7022 0.1176 0.5249 11.00000 0.05 0.16 Q12 1 0.7573 0.7025 0.6524 11.00000 0.05 0.16 Q13 1 0.5824 0.3052 0.7616 11.00000 0.05 0.16 Q14 1 0.8043 0.5000 0.5291 11.00000 0.05 0.16 Q15 1 0.8910 0.4260 0.5006 11.00000 0.05 0.16 Q16 1 0.6933 0.0937 0.4794 11.00000 0.05 0.15 Q17 1 0.8924 1.0959 0.7101 11.00000 0.05 0.15 Q18 1 0.6939 0.4040 0.8163 11.00000 0.05 0.15 Q19 1 0.7884 0.4615 0.8021 11.00000 0.05 0.15 Q20 1 0.7438 0.0069 0.5149 11.00000 0.05 0.15 ; _shelx_res_checksum 35396 _shelx_hkl_file ; 1 0 0 0.60 0.20 -1 0 0 0.30 0.20 3 0 0 0.20 0.80 -3 0 0 0.60 0.40 3 0 0 0.90 1.10 4 0 0 4270.07 110.19 -4 0 0 4371.56 104.89 4 0 0 4486.55 105.79 5 0 0 2.00 2.60 5 0 0 1.60 2.00 6 0 0 191.18 7.10 -6 0 0 212.68 8.40 6 0 0 198.78 12.80 -7 0 0 4.60 3.00 8 0 0 1549.84 39.10 -8 0 0 1526.85 40.10 9 0 0 0.90 2.10 -9 0 0 -1.80 3.00 10 0 0 438.46 12.70 -10 0 0 443.26 13.80 -11 0 0 1.80 2.80 11 0 0 1.60 1.50 12 0 0 193.18 6.00 12 0 0 189.08 6.40 0 -1 0 0.60 0.30 0 -1 0 0.60 0.30 0 1 0 1.20 0.30 0 1 0 1.00 0.30 0 1 0 0.20 0.30 -3 -1 0 187.58 5.90 3 1 0 183.48 7.50 3 1 0 181.28 6.80 -4 -1 0 40.30 2.50 4 1 0 39.70 4.40 4 1 0 38.10 4.60 -5 -1 0 2299.47 57.69 -5 -1 0 2519.65 60.29 5 -1 0 2292.27 64.69 5 1 0 2247.38 59.59 5 1 0 2322.17 62.69 -5 1 0 2332.57 59.69 6 -1 0 509.95 22.60 6 -1 0 501.95 14.30 -6 -1 0 503.35 15.20 -6 1 0 516.55 16.40 6 1 0 504.35 20.30 -6 1 0 491.75 15.40 6 1 0 505.15 14.00 -7 -1 0 3.80 2.70 -7 1 0 -0.30 3.10 7 1 0 0.40 1.90 -8 -1 0 850.71 24.60 8 -1 0 886.11 23.70 -8 1 0 902.31 24.70 8 1 0 887.51 23.40 9 -1 0 1088.69 28.60 -9 -1 0 1067.49 29.70 9 1 0 1080.99 28.20 -9 1 0 1100.19 29.60 -10 -1 0 2.70 2.30 10 -1 0 4.60 1.80 -10 1 0 6.40 3.20 10 1 0 2.60 1.60 10 1 0 6.50 5.80 11 -1 0 43.00 3.00 -11 -1 0 37.50 4.20 11 1 0 44.10 3.50 11 1 0 40.50 2.90 12 -1 0 -0.10 1.40 -12 -1 0 0.10 2.80 12 -1 0 1.30 1.40 12 1 0 -0.70 1.40 12 1 0 0.60 1.60 0 -2 0 395.26 10.30 0 -2 0 349.67 10.00 0 2 0 378.06 10.00 0 2 0 381.66 10.50 0 2 0 378.76 10.40 1 -2 0 23.50 1.30 -1 -2 0 25.80 2.10 -1 -2 0 23.80 1.80 1 2 0 21.40 2.50 1 2 0 23.50 1.50 1 2 0 22.10 1.60 -1 2 0 23.80 1.80 -1 2 0 18.90 2.40 -2 -2 0 41.20 2.40 -2 -2 0 38.90 3.60 2 2 0 33.90 2.00 2 2 0 37.50 2.30 -3 -2 0 1559.14 44.10 -3 -2 0 1685.63 41.50 3 2 0 1686.43 42.80 3 2 0 1683.03 42.50 -4 -2 0 2116.39 52.79 4 2 0 2149.58 54.89 4 2 0 2082.59 54.89 -5 -2 0 406.66 12.40 -5 -2 0 374.06 12.30 -5 2 0 387.06 13.90 5 2 0 382.76 16.90 5 2 0 419.96 15.10 5 2 0 387.36 11.10 6 -2 0 382.46 20.80 -6 -2 0 433.16 13.60 -6 -2 0 428.56 13.20 6 -2 0 419.86 12.50 -6 2 0 400.36 14.00 6 2 0 418.96 11.80 -6 2 0 425.46 14.80 6 2 0 419.26 17.20 -7 -2 0 1650.93 42.40 7 -2 0 1618.44 41.40 -7 2 0 1599.64 42.00 -7 2 0 1649.13 43.80 7 2 0 1670.13 40.80 -8 -2 0 435.76 14.30 8 -2 0 436.16 13.40 8 2 0 432.56 12.60 8 2 0 442.46 15.30 9 -2 0 138.89 6.70 -9 -2 0 143.69 7.80 9 2 0 143.19 5.90 9 2 0 125.99 9.40 -10 -2 0 838.42 23.50 10 2 0 832.22 21.90 10 2 0 851.01 23.30 -11 -2 0 49.90 4.10 11 -2 0 58.39 3.30 11 2 0 41.10 3.40 11 2 0 53.29 3.00 12 -2 0 86.99 3.60 -12 -2 0 89.19 4.50 12 2 0 70.59 4.20 12 2 0 89.39 3.70 0 -3 0 3.10 0.90 0 3 0 0.80 1.10 0 3 0 4.80 1.20 -1 -3 0 2339.27 58.39 1 -3 0 2273.77 59.09 1 -3 0 2339.57 57.39 -1 -3 0 2345.27 58.09 1 3 0 2447.46 57.39 1 3 0 2417.26 59.19 1 3 0 2379.76 58.29 -1 3 0 2394.76 58.59 -1 3 0 2352.16 58.09 -2 -3 0 3312.97 82.19 -2 -3 0 3478.85 88.29 -2 3 0 3427.16 83.09 2 3 0 3252.27 80.89 -2 3 0 3421.76 81.19 2 3 0 3312.07 81.99 2 3 0 3334.07 83.49 -3 -3 0 1848.72 49.80 -3 -3 0 1887.01 46.60 3 3 0 1841.92 45.30 3 3 0 1816.12 46.60 3 3 0 1807.92 48.60 -4 -3 0 653.73 19.10 4 3 0 702.23 18.20 4 3 0 618.44 22.70 4 3 0 686.43 19.80 -5 -3 0 742.63 21.30 -5 -3 0 709.93 20.30 5 -3 0 700.23 19.60 5 3 0 737.23 20.30 5 3 0 726.23 18.80 -5 3 0 740.73 22.00 5 3 0 758.62 22.70 6 -3 0 1101.19 28.60 -6 -3 0 1088.49 31.00 -6 -3 0 1101.59 29.50 6 3 0 1109.19 33.50 -6 3 0 1115.69 31.20 6 3 0 1103.39 27.90 6 3 0 1119.49 29.80 7 -3 0 536.05 15.80 -7 -3 0 543.05 16.70 -7 3 0 557.54 18.60 7 3 0 552.64 17.10 7 3 0 540.15 14.90 8 -3 0 883.11 24.20 -8 -3 0 897.51 25.20 8 3 0 896.21 26.10 8 3 0 885.81 24.60 8 3 0 893.41 23.30 9 -3 0 421.36 13.10 -9 -3 0 404.76 14.00 9 3 0 387.66 15.30 9 3 0 424.16 12.00 9 3 0 407.36 13.30 10 -3 0 55.49 4.00 -10 -3 0 60.49 4.40 10 3 0 68.69 5.10 10 3 0 59.49 3.30 -11 -3 0 22.20 3.50 11 -3 0 31.70 2.90 11 3 0 25.40 2.90 11 3 0 26.80 2.80 -12 -3 0 4.50 2.00 12 3 0 2.50 1.20 0 -4 0 1258.27 31.80 0 -4 0 1259.47 32.40 0 4 0 1231.68 32.10 0 4 0 1220.88 33.20 -1 -4 0 495.05 14.30 1 -4 0 494.35 13.50 1 -4 0 483.85 15.00 -1 -4 0 487.35 14.90 -1 4 0 488.55 15.00 1 4 0 479.35 16.20 -1 4 0 485.25 14.90 1 4 0 503.95 13.70 1 4 0 489.65 14.70 2 -4 0 908.81 27.90 -2 -4 0 999.50 26.50 -2 -4 0 997.30 28.30 -2 4 0 976.20 26.00 2 4 0 949.40 28.90 2 4 0 1009.00 25.10 2 4 0 1007.90 26.40 -2 4 0 995.10 27.50 -3 -4 0 263.47 14.00 -3 -4 0 262.07 9.60 3 4 0 271.67 9.40 3 4 0 277.77 8.40 -4 -4 0 555.94 15.40 -4 -4 0 566.54 16.70 -4 -4 0 581.74 17.70 4 4 0 576.24 19.00 4 4 0 599.64 16.00 -4 4 0 580.34 18.40 4 4 0 558.54 15.00 -5 -4 0 673.23 21.10 5 -4 0 647.44 18.20 -5 -4 0 666.03 17.80 -5 -4 0 712.23 19.30 -5 4 0 672.13 21.00 5 4 0 667.83 21.30 5 4 0 675.33 17.40 -6 -4 0 803.22 22.00 6 -4 0 794.12 21.10 -6 4 0 778.82 23.80 6 4 0 749.92 25.80 6 4 0 797.12 21.90 6 4 0 755.12 21.50 6 4 0 753.02 20.40 7 -4 0 1587.94 41.30 -7 -4 0 1605.94 42.20 7 4 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3 -4 490.75 15.00 6 3 -4 500.55 13.30 -5 -3 4 201.68 7.20 -5 -3 4 183.58 9.60 5 -3 -4 202.78 7.20 -5 -3 4 195.58 8.70 -5 3 4 184.78 9.80 5 3 -4 195.98 6.60 -3 -3 4 611.04 18.50 3 -3 -4 543.65 19.90 3 3 -4 603.34 14.90 3 3 -4 539.95 20.60 -3 3 4 616.84 15.90 3 3 -4 619.94 15.40 -3 3 4 586.14 18.80 2 -3 -4 1970.00 51.79 -2 -3 4 2001.20 51.49 -2 3 4 2052.19 49.50 2 3 -4 1933.31 52.59 -2 3 4 2037.80 51.49 1 -3 -4 6270.27 156.28 -1 -3 4 6480.45 156.38 -1 3 4 6304.97 154.78 -1 3 4 6607.84 155.78 1 3 -4 6546.95 157.18 0 -3 4 112.19 3.70 0 -3 4 108.39 5.30 0 -3 -4 118.39 5.80 0 3 4 119.29 5.30 0 3 -4 113.59 6.40 -1 -3 -4 6654.63 159.78 1 -3 4 6530.55 158.38 1 3 4 6488.75 158.38 2 -3 4 1989.90 49.60 -2 -3 -4 1985.90 53.29 2 3 4 2011.10 50.79 2 3 4 1972.60 50.69 2 3 4 1981.00 49.20 3 -3 4 583.54 15.30 -3 -3 -4 532.15 22.30 3 3 4 570.04 18.80 3 3 4 609.84 16.10 3 3 4 570.74 17.80 4 -3 4 375.56 16.90 -4 -3 -4 365.06 11.60 4 3 4 399.06 11.90 4 3 4 387.36 13.90 4 3 4 368.76 10.30 -4 3 -4 352.66 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184.88 7.80 3 5 -20 195.88 6.40 3 5 -20 185.58 6.10 -2 -5 20 219.48 7.70 2 -5 -20 227.28 8.80 2 5 -20 229.48 7.50 -1 -5 20 69.79 5.20 1 -5 -20 69.59 5.60 1 5 -20 69.19 3.90 -1 5 20 73.69 5.50 0 -5 20 90.29 6.20 0 -5 -20 89.59 5.70 0 5 -20 76.09 4.40 0 5 20 86.39 5.20 -1 -5 -20 68.79 5.30 1 5 20 67.49 4.50 -1 5 -20 70.19 4.20 -2 -5 -20 231.98 8.80 -2 5 -20 229.78 7.80 2 5 20 230.98 7.70 -3 -5 -20 184.98 10.70 -3 5 -20 203.08 6.80 3 5 20 210.08 7.00 1 -6 -20 26.90 3.10 -1 -6 20 37.30 4.90 1 6 -20 29.40 2.60 0 -6 -20 39.10 4.40 0 6 -20 44.50 3.00 -1 -6 -20 30.20 4.20 -1 6 -20 24.20 2.60 -5 0 21 3.20 2.70 -5 0 21 1.40 2.90 -4 0 21 352.36 10.70 -4 0 21 349.96 11.70 -3 0 21 61.09 5.30 -3 0 21 56.49 4.30 3 0 -21 59.69 5.00 2 0 -21 343.47 12.20 -2 0 21 350.16 11.20 2 0 -21 347.37 10.90 -1 0 21 34.00 4.10 1 0 -21 32.80 5.00 1 0 -21 28.70 4.30 0 0 -21 -3.10 2.60 0 0 21 5.30 2.50 0 0 -21 -3.70 3.20 -1 0 -21 21.70 3.10 1 0 21 29.20 4.20 -1 0 -21 25.00 3.50 2 0 21 344.37 10.80 -2 0 -21 338.07 11.70 -2 0 -21 340.87 11.30 -3 0 -21 47.70 4.20 3 0 21 54.69 4.60 -4 0 -21 345.97 10.70 4 0 21 332.17 10.30 -5 0 -21 5.50 2.00 -5 -1 21 154.98 6.60 -5 -1 21 159.38 6.10 -5 1 21 154.58 6.90 -4 -1 21 27.60 3.20 -4 -1 21 30.00 3.70 -4 1 21 31.00 4.10 -4 1 21 22.70 3.40 -3 -1 21 120.49 5.60 3 -1 -21 118.09 6.40 -3 -1 21 125.29 6.70 3 1 -21 109.89 5.40 -3 1 21 121.59 6.60 -3 1 21 127.99 5.70 2 -1 -21 77.39 5.70 -2 -1 21 87.79 4.90 2 1 -21 75.49 4.80 -2 1 21 77.49 4.90 -1 -1 21 91.29 5.20 1 -1 -21 88.39 6.20 1 -1 -21 81.79 5.50 1 1 -21 81.49 5.90 1 1 -21 83.59 5.10 -1 1 21 89.69 5.20 0 -1 -21 3.50 3.30 0 -1 -21 4.80 2.90 0 -1 21 3.30 2.60 0 1 21 3.60 2.40 0 1 -21 5.10 2.60 0 1 -21 10.50 3.10 -1 -1 -21 88.89 5.30 -1 -1 -21 86.19 6.30 1 -1 21 88.99 5.50 -1 1 -21 85.29 5.20 1 1 21 80.59 5.00 -2 -1 -21 71.59 6.10 -2 -1 -21 68.39 4.70 2 -1 21 71.59 6.60 -2 1 -21 75.69 4.70 2 1 21 85.29 4.70 -3 -1 -21 122.39 5.60 -3 -1 -21 104.99 7.70 3 -1 21 108.89 6.40 -3 1 -21 108.49 5.40 3 1 21 113.39 5.80 -4 -1 -21 24.70 3.20 4 -1 21 25.50 6.50 4 1 21 30.10 3.80 -4 1 -21 28.60 3.30 -5 -1 -21 155.98 5.80 5 1 21 157.58 5.90 -5 1 -21 152.28 5.80 -4 -2 21 44.50 3.80 4 -2 -21 43.30 4.60 -4 -2 21 39.70 4.70 -4 2 21 48.50 5.20 4 2 -21 41.20 3.70 -4 2 21 37.00 5.00 -3 -2 21 72.69 5.50 3 -2 -21 72.79 5.30 -3 2 21 78.99 4.70 3 2 -21 66.09 4.10 -3 2 21 70.09 5.40 -2 -2 21 122.29 5.80 2 -2 -21 119.69 6.60 -2 -2 21 126.59 6.80 2 2 -21 122.99 5.60 -2 2 21 121.49 5.80 1 -2 -21 73.19 5.70 -1 -2 21 76.69 5.00 1 2 -21 72.49 4.60 -1 2 21 73.89 4.70 0 -2 -21 55.29 5.50 0 -2 -21 67.69 5.50 0 -2 21 54.19 4.90 0 2 21 51.99 4.30 0 2 -21 51.19 4.30 -1 -2 -21 73.79 5.10 1 -2 21 48.70 6.00 -1 -2 -21 66.09 5.80 1 2 21 71.29 4.50 -1 2 -21 74.69 4.70 -2 -2 -21 116.19 5.70 2 -2 21 129.99 7.20 -2 -2 -21 118.09 6.70 2 2 21 126.49 5.40 -2 2 -21 120.39 5.70 -3 -2 -21 52.69 7.50 -3 -2 -21 67.39 4.40 -3 2 -21 70.49 4.40 3 2 21 70.59 4.20 -4 -2 -21 43.80 3.60 4 2 21 45.60 3.70 -4 2 -21 46.70 3.60 -4 -3 21 72.69 5.30 -4 -3 21 80.19 4.20 4 -3 -21 79.89 6.90 4 3 -21 76.99 3.80 3 -3 -21 98.59 5.90 -3 -3 21 107.19 5.00 -3 -3 21 97.39 6.20 -3 3 21 87.49 6.30 -3 3 21 96.89 5.50 3 3 -21 100.19 4.50 -2 -3 21 187.28 8.40 2 -3 -21 205.28 8.30 -2 -3 21 190.78 7.30 -2 3 21 202.48 7.20 2 3 -21 200.58 7.00 -1 -3 21 26.20 3.80 1 -3 -21 22.30 3.40 -1 -3 21 33.80 4.20 -1 3 21 31.80 3.70 1 3 -21 29.10 3.40 0 -3 -21 218.08 8.90 0 -3 21 201.48 8.20 0 3 -21 219.78 7.90 0 3 21 221.08 7.70 -1 -3 -21 28.40 3.60 1 -3 21 43.10 6.00 -1 3 -21 29.30 3.50 1 3 21 33.60 3.70 -2 -3 -21 193.08 7.40 -2 -3 -21 203.98 8.20 2 3 21 200.98 9.20 -2 3 -21 205.28 7.50 -3 -3 -21 95.69 5.10 -3 -3 -21 97.49 6.90 -3 3 -21 99.59 4.90 3 3 21 103.79 4.80 -4 -3 -21 65.19 4.90 -4 3 -21 74.89 4.00 4 3 21 80.59 4.00 3 -4 -21 55.59 4.60 -3 -4 21 56.09 3.80 3 4 -21 49.60 3.10 -2 -4 21 61.89 4.40 2 -4 -21 61.89 4.70 -2 -4 21 58.09 6.80 2 4 -21 60.19 3.60 -2 4 21 59.89 5.50 1 -4 -21 164.98 7.20 -1 -4 21 154.88 6.40 -1 -4 21 145.69 8.90 1 4 -21 154.78 5.90 -1 4 21 162.38 6.40 0 -4 21 182.38 7.60 0 -4 -21 210.98 8.20 0 4 21 198.58 7.20 0 4 -21 199.38 7.10 -1 -4 -21 154.08 7.10 -1 4 -21 153.18 6.10 1 4 21 161.88 6.30 -2 -4 -21 59.69 5.20 -2 4 -21 62.49 3.80 2 4 21 74.29 4.30 -3 -4 -21 61.89 5.80 3 4 21 50.49 4.00 -3 4 -21 61.59 3.60 -1 -5 21 74.99 5.70 1 -5 -21 71.39 4.80 1 5 -21 71.59 3.60 0 -5 -21 222.68 8.50 0 5 21 265.67 9.50 0 5 -21 226.38 7.40 -1 -5 -21 75.09 4.70 1 5 21 67.79 5.10 -1 5 -21 71.29 3.60 -3 0 22 12.10 2.90 -3 0 22 11.10 2.40 -2 0 22 16.30 2.40 2 0 -22 17.60 3.20 1 0 -22 24.60 3.90 1 0 -22 22.90 3.10 -1 0 22 20.40 3.50 0 0 -22 21.50 2.70 0 0 -22 25.20 3.20 0 0 22 30.30 4.10 1 0 22 21.30 2.70 -1 0 -22 22.20 2.70 -1 0 -22 29.40 4.60 -2 0 -22 17.00 2.40 2 0 22 21.10 3.00 -3 0 -22 11.30 2.00 3 0 22 12.80 2.70 -3 -1 22 92.19 4.70 3 -1 -22 92.99 5.10 -3 -1 22 83.09 5.50 -3 1 22 80.79 5.50 -3 1 22 84.49 4.60 -2 -1 22 258.57 8.50 -2 -1 22 253.37 9.70 2 -1 -22 246.08 9.00 -2 1 22 253.97 8.40 2 1 -22 235.28 9.20 -1 -1 22 46.20 4.20 1 -1 -22 54.39 4.70 -1 1 22 52.69 4.50 1 1 -22 50.89 3.90 0 -1 22 -3.10 2.50 0 -1 -22 4.20 2.90 0 -1 -22 1.60 2.70 0 1 -22 0.60 2.10 0 1 22 3.70 3.20 -1 -1 -22 59.69 5.00 -1 -1 -22 43.80 4.10 1 -1 22 54.59 4.80 1 1 22 55.89 4.20 -1 1 -22 53.89 3.90 -2 -1 -22 242.28 8.30 2 -1 22 251.77 8.60 -2 -1 -22 258.27 9.50 2 1 22 256.67 8.40 -2 1 -22 243.58 8.30 -3 -1 -22 83.29 4.30 -3 1 -22 87.49 4.30 3 1 22 86.79 4.70 -3 -2 22 126.49 6.10 3 -2 -22 129.49 5.90 -3 -2 22 125.59 5.30 -3 2 22 126.49 6.40 3 2 -22 109.29 4.80 -3 2 22 130.29 5.70 -2 -2 22 80.99 5.70 2 -2 -22 81.39 5.10 -2 -2 22 81.79 4.80 2 2 -22 83.19 4.10 -2 2 22 71.89 4.70 1 -2 -22 236.38 8.80 -1 -2 22 219.88 8.00 -1 -2 22 223.28 9.10 -1 2 22 235.18 7.90 1 2 -22 240.68 7.80 0 -2 -22 3.10 2.80 0 -2 22 -1.10 2.70 0 2 -22 4.30 2.00 0 2 22 3.10 2.20 -1 -2 -22 220.38 7.80 -1 -2 -22 232.18 8.50 1 -2 22 208.68 8.10 1 2 22 239.38 7.90 -1 2 -22 227.68 7.80 -2 2 -22 83.49 4.30 2 2 22 80.69 4.70 -3 -2 -22 122.29 5.20 3 2 22 123.39 5.30 -3 2 -22 123.59 5.10 2 -3 -22 39.70 4.10 -2 -3 22 37.00 3.80 -2 -3 22 29.90 3.80 -2 3 22 31.80 4.50 -2 3 22 35.00 5.40 2 3 -22 36.20 3.80 -1 -3 22 172.38 6.70 1 -3 -22 189.88 7.40 -1 -3 22 180.28 8.10 1 3 -22 183.48 6.40 -1 3 22 178.38 6.70 0 -3 22 415.46 12.50 0 -3 22 416.56 13.80 0 -3 -22 432.56 13.20 0 3 22 432.16 12.40 0 3 -22 446.66 12.50 -1 -3 -22 190.48 7.50 1 3 22 195.98 6.90 -1 3 -22 185.48 6.70 -2 -3 -22 34.90 5.00 2 3 22 35.40 3.80 -2 3 -22 45.70 3.20 1 0 -23 48.10 4.40 -1 0 23 53.09 4.10 0 0 -23 0.30 2.30 0 0 23 3.30 2.30 -1 0 -23 48.60 3.60 1 0 23 57.99 4.40 0 -1 -23 62.69 5.90 0 -1 23 49.20 4.50 0 1 -23 53.29 3.50 0 1 23 55.99 4.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 30986 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -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 O1 O 1.00298(18) 0.7723(2) 0.72064(11) 0.0215(4) Uani 1 1 d . . C1 C 0.8174(2) 0.6712(2) 0.66539(13) 0.0128(5) Uani 1 1 d . . H1 H 0.8886 0.6770 0.6304 0.015 Uiso 1 1 calc R U O2 O 0.67025(18) 0.82348(19) 0.77942(10) 0.0187(4) Uani 1 1 d . . H2A H 0.6874(12) 0.774(4) 0.807(2) 0.028 Uiso 1 1 calc R U C23 C 0.2642(19) 0.6360(16) 0.6348(7) 0.269(11) Uani 1 1 d . . H23A H 0.2950 0.6941 0.5977 0.323 Uiso 1 1 calc R U H23B H 0.2647 0.6885 0.6777 0.323 Uiso 1 1 calc R U C22 C 0.3744(3) 0.5573(3) 0.64540(19) 0.0341(7) Uani 1 1 d . . H22A H 0.3665 0.4673 0.6426 0.041 Uiso 1 1 calc R U H22B H 0.4556 0.5949 0.6552 0.041 Uiso 1 1 calc R U C2 C 0.8703(2) 0.7393(2) 0.73182(13) 0.0153(5) Uani 1 1 d . . H2 H 0.8620 0.6822 0.7734 0.018 Uiso 1 1 calc R U O3 O 0.58217(17) 0.71950(18) 0.65860(10) 0.0167(4) Uani 1 1 d . . C3 C 0.7843(3) 0.8569(2) 0.74068(13) 0.0152(5) Uani 1 1 d . . H3 H 0.8320 0.9283 0.7636 0.018 Uiso 1 1 calc R U O4 O 0.62941(19) 0.85161(18) 0.52941(10) 0.0184(4) Uani 1 1 d . . H4 H 0.626(3) 0.847(2) 0.491(2) 0.028 Uiso 1 1 calc R U C4 C 0.7420(3) 0.8928(2) 0.66630(13) 0.0150(5) Uani 1 1 d . . O7 O 0.8006(2) 0.3462(2) 0.38672(10) 0.0222(4) Uani 1 1 d . . C7 C 0.6589(2) 0.6249(2) 0.52614(13) 0.0148(5) Uani 1 1 d . . H7A H 0.6502 0.6364 0.4751 0.018 Uiso 1 1 calc R U H7B H 0.5710 0.6118 0.5448 0.018 Uiso 1 1 calc R U O6 O 0.8808(2) 0.56648(18) 0.44628(10) 0.0176(4) Uani 1 1 d . . C6 C 0.7084(2) 0.7505(2) 0.55598(13) 0.0133(5) Uani 1 1 d . . H6 H 0.7987 0.7639 0.5393 0.016 Uiso 1 1 calc R U O5 O 0.92352(19) 0.47705(18) 0.69178(10) 0.0170(4) Uani 1 1 d . . H5 H 0.575(5) 0.747(5) 0.705(3) 0.058(14) Uiso 1 1 d . . C5 C 0.7076(2) 0.7578(2) 0.63575(13) 0.0126(5) Uani 1 1 d . . C8 C 0.7338(2) 0.5006(2) 0.53797(12) 0.0123(5) Uani 1 1 d . . O8 O 0.1321(2) 0.6297(2) 0.62003(11) 0.0286(5) Uani 1 1 d . . H8A H 0.090(2) 0.684(4) 0.648(2) 0.043 Uiso 1 1 calc R U H8 H 1.025(4) 0.832(4) 0.747(2) 0.034(10) Uiso 1 1 d . . C9 C 0.7303(2) 0.4509(2) 0.61453(13) 0.0132(5) Uani 1 1 d . . H9 H 0.6368 0.4459 0.6269 0.016 Uiso 1 1 calc R U C10 C 0.7952(2) 0.5267(2) 0.67617(13) 0.0142(5) Uani 1 1 d . . H10 H 0.951(4) 0.599(3) 0.4468(17) 0.014(8) Uiso 1 1 d . . C11 C 0.7793(2) 0.3118(2) 0.61641(14) 0.0153(5) Uani 1 1 d . . H11A H 0.7958 0.2872 0.6655 0.018 Uiso 1 1 calc R U H11B H 0.7111 0.2550 0.5980 0.018 Uiso 1 1 calc R U H11 H 0.830(5) 0.419(5) 0.386(2) 0.046(13) Uiso 1 1 d . . C12 C 0.9031(3) 0.2917(2) 0.57363(13) 0.0162(5) Uani 1 1 d . . H12A H 0.9772 0.3260 0.6002 0.019 Uiso 1 1 calc R U H12B H 0.9173 0.1993 0.5671 0.019 Uiso 1 1 calc R U H12 H 0.982(4) 0.518(4) 0.669(2) 0.036(11) Uiso 1 1 d . . C13 C 0.8980(2) 0.3563(2) 0.50202(13) 0.0147(5) Uani 1 1 d . . H13 H 0.9793 0.3409 0.4754 0.018 Uiso 1 1 calc R U C14 C 0.8740(2) 0.4996(2) 0.51151(12) 0.0132(5) Uani 1 1 d . . H14 H 0.9341 0.5371 0.5467 0.016 Uiso 1 1 calc R U C15 C 0.6699(2) 0.3975(2) 0.48957(13) 0.0154(5) Uani 1 1 d . . H15A H 0.6091 0.3445 0.5167 0.018 Uiso 1 1 calc R U H15B H 0.6219 0.4391 0.4512 0.018 Uiso 1 1 calc R U C16 C 0.7799(3) 0.3138(2) 0.45961(13) 0.0164(5) Uani 1 1 d . . C17 C 0.7551(3) 0.1708(3) 0.45865(15) 0.0209(6) Uani 1 1 d . . H17A H 0.6893 0.1511 0.4236 0.031 Uiso 1 1 calc R U H17B H 0.7251 0.1432 0.5047 0.031 Uiso 1 1 calc R U H17C H 0.8351 0.1260 0.4470 0.031 Uiso 1 1 calc R U C18 C 0.8553(3) 0.9546(3) 0.62741(15) 0.0190(5) Uani 1 1 d . . H18A H 0.9263 0.8935 0.6238 0.028 Uiso 1 1 calc R U H18B H 0.8843 1.0301 0.6531 0.028 Uiso 1 1 calc R U H18C H 0.8276 0.9798 0.5805 0.028 Uiso 1 1 calc R U C19 C 0.6307(3) 0.9885(3) 0.66815(14) 0.0192(5) Uani 1 1 d . . H19A H 0.6134 1.0193 0.6208 0.029 Uiso 1 1 calc R U H19B H 0.6540 1.0605 0.6981 0.029 Uiso 1 1 calc R U H19C H 0.5534 0.9469 0.6867 0.029 Uiso 1 1 calc R U C20 C 0.7177(3) 0.4939(3) 0.74199(13) 0.0193(6) Uani 1 1 d . . H20A H 0.6358 0.5402 0.7414 0.029 Uiso 1 1 calc R U H20B H 0.7671 0.5183 0.7835 0.029 Uiso 1 1 calc R U H20C H 0.7008 0.4021 0.7431 0.029 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 0.0151(9) 0.0230(10) 0.0265(10) -0.0098(9) -0.0037(8) -0.0009(8) C1 0.0143(11) 0.0121(12) 0.0122(11) -0.0005(9) -0.0010(9) 0.0003(10) O2 0.0203(9) 0.0214(9) 0.0145(9) 0.0033(8) 0.0022(7) 0.0028(8) C23 0.38(2) 0.30(2) 0.126(10) 0.051(11) 0.034(13) 0.24(2) C22 0.0245(15) 0.0293(16) 0.048(2) 0.0061(15) -0.0076(14) -0.0077(13) C2 0.0160(12) 0.0156(12) 0.0143(11) -0.0014(9) -0.0020(10) 0.0020(10) O3 0.0136(8) 0.0186(9) 0.0179(9) -0.0007(7) 0.0014(7) -0.0011(7) C3 0.0160(12) 0.0146(12) 0.0148(12) -0.0017(10) -0.0010(10) 0.0006(10) O4 0.0249(10) 0.0170(9) 0.0134(8) 0.0020(7) -0.0038(8) 0.0075(8) C4 0.0171(12) 0.0134(12) 0.0144(12) 0.0001(9) -0.0016(10) 0.0007(10) O7 0.0336(11) 0.0197(10) 0.0134(9) -0.0021(8) 0.0001(8) 0.0003(9) C7 0.0136(11) 0.0165(12) 0.0144(12) -0.0007(9) -0.0025(9) 0.0027(10) O6 0.0180(10) 0.0204(9) 0.0144(8) 0.0042(7) 0.0020(7) -0.0031(8) C6 0.0143(11) 0.0134(12) 0.0121(11) 0.0014(9) -0.0011(9) 0.0026(9) O5 0.0165(9) 0.0157(9) 0.0189(9) 0.0027(7) -0.0043(7) 0.0031(8) C5 0.0127(11) 0.0136(12) 0.0116(12) 0.0006(9) 0.0000(9) -0.0010(9) C8 0.0130(11) 0.0121(11) 0.0119(11) -0.0011(9) -0.0029(9) -0.0007(9) O8 0.0271(11) 0.0340(12) 0.0247(11) -0.0010(9) 0.0011(9) 0.0054(9) C9 0.0120(11) 0.0134(12) 0.0141(12) -0.0008(10) 0.0008(9) -0.0002(9) C10 0.0152(12) 0.0142(12) 0.0133(11) 0.0013(9) -0.0026(10) 0.0024(10) C11 0.0186(12) 0.0121(12) 0.0153(12) 0.0014(9) -0.0001(10) -0.0012(10) C12 0.0188(13) 0.0140(12) 0.0159(12) 0.0009(10) -0.0008(10) 0.0048(10) C13 0.0139(12) 0.0163(13) 0.0137(12) -0.0011(10) 0.0014(9) 0.0025(9) C14 0.0130(11) 0.0147(12) 0.0117(11) 0.0021(9) 0.0003(9) 0.0001(10) C15 0.0150(12) 0.0145(12) 0.0167(12) -0.0027(10) -0.0025(10) -0.0011(10) C16 0.0210(13) 0.0156(13) 0.0126(12) -0.0008(9) -0.0015(10) 0.0011(10) C17 0.0257(14) 0.0153(12) 0.0217(13) -0.0028(10) -0.0011(11) 0.0000(11) C18 0.0219(13) 0.0152(12) 0.0200(12) 0.0013(10) 0.0008(11) -0.0046(10) C19 0.0226(13) 0.0144(12) 0.0206(13) 0.0002(10) -0.0016(11) 0.0049(11) C20 0.0263(14) 0.0158(12) 0.0158(12) 0.0009(10) 0.0049(11) -0.0019(12) 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 C2 O1 H8 110(3) C10 C1 C2 113.1(2) C10 C1 C5 120.6(2) C2 C1 C5 106.6(2) C10 C1 H1 105.0 C2 C1 H1 105.0 C5 C1 H1 105.0 C3 O2 H2A 109.5 C22 C23 O8 141.8(15) C22 C23 H23A 101.5 O8 C23 H23A 101.5 C22 C23 H23B 101.5 O8 C23 H23B 101.5 H23A C23 H23B 104.6 C23 C22 H22A 120.0 C23 C22 H22B 120.0 H22A C22 H22B 120.0 O1 C2 C3 112.3(2) O1 C2 C1 109.1(2) C3 C2 C1 104.8(2) O1 C2 H2 110.2 C3 C2 H2 110.2 C1 C2 H2 110.2 C5 O3 H5 106(3) O2 C3 C2 109.8(2) O2 C3 C4 107.6(2) C2 C3 C4 105.1(2) O2 C3 H3 111.4 C2 C3 H3 111.4 C4 C3 H3 111.4 C6 O4 H4 109.5 C19 C4 C18 108.2(2) C19 C4 C3 110.8(2) C18 C4 C3 109.5(2) C19 C4 C5 115.4(2) C18 C4 C5 111.9(2) C3 C4 C5 100.88(19) C16 O7 H11 106(3) C6 C7 C8 120.6(2) C6 C7 H7A 107.2 C8 C7 H7A 107.2 C6 C7 H7B 107.2 C8 C7 H7B 107.2 H7A C7 H7B 106.8 C14 O6 H10 104(2) O4 C6 C7 108.29(19) O4 C6 C5 108.31(19) C7 C6 C5 114.5(2) O4 C6 H6 108.5 C7 C6 H6 108.5 C5 C6 H6 108.5 C10 O5 H12 111(3) O3 C5 C6 107.24(19) O3 C5 C1 112.8(2) C6 C5 C1 109.24(19) O3 C5 C4 110.2(2) C6 C5 C4 114.5(2) C1 C5 C4 102.91(19) C7 C8 C14 115.8(2) C7 C8 C9 114.3(2) C14 C8 C9 109.22(19) C7 C8 C15 106.55(19) C14 C8 C15 101.49(19) C9 C8 C15 108.4(2) C23 O8 H8A 109.5 C11 C9 C8 109.3(2) C11 C9 C10 108.6(2) C8 C9 C10 121.8(2) C11 C9 H9 105.3 C8 C9 H9 105.3 C10 C9 H9 105.3 O5 C10 C20 103.2(2) O5 C10 C1 104.0(2) C20 C10 C1 114.1(2) O5 C10 C9 111.3(2) C20 C10 C9 106.2(2) C1 C10 C9 117.3(2) C12 C11 C9 113.0(2) C12 C11 H11A 109.0 C9 C11 H11A 109.0 C12 C11 H11B 109.0 C9 C11 H11B 109.0 H11A C11 H11B 107.8 C13 C12 C11 112.8(2) 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 C12 C13 C14 109.5(2) C12 C13 C16 111.9(2) C14 C13 C16 102.6(2) C12 C13 H13 110.9 C14 C13 H13 110.9 C16 C13 H13 110.9 O6 C14 C13 111.6(2) O6 C14 C8 109.21(19) C13 C14 C8 101.50(19) O6 C14 H14 111.4 C13 C14 H14 111.4 C8 C14 H14 111.4 C16 C15 C8 107.4(2) C16 C15 H15A 110.2 C8 C15 H15A 110.2 C16 C15 H15B 110.2 C8 C15 H15B 110.2 H15A C15 H15B 108.5 O7 C16 C17 104.1(2) O7 C16 C13 108.8(2) C17 C16 C13 115.3(2) O7 C16 C15 109.4(2) C17 C16 C15 116.0(2) C13 C16 C15 103.1(2) C16 C17 H17A 109.5 C16 C17 H17B 109.5 H17A C17 H17B 109.5 C16 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 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 109.5 C10 C20 H20B 109.5 H20A C20 H20B 109.5 C10 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C2 1.437(3) O1 H8 0.84(5) C1 C10 1.548(3) C1 C2 1.560(3) C1 C5 1.565(3) C1 H1 1.0000 O2 C3 1.441(3) O2 H2A 0.76(4) C23 C22 1.426(14) C23 O8 1.40(2) C23 H23A 0.9900 C23 H23B 0.9900 C22 H22A 0.9500 C22 H22B 0.9500 C2 C3 1.534(3) C2 H2 1.0000 O3 C5 1.432(3) O3 H5 0.94(5) C3 C4 1.539(3) C3 H3 1.0000 O4 C6 1.435(3) O4 H4 0.74(4) C4 C19 1.532(4) C4 C18 1.537(4) C4 C5 1.575(3) O7 C16 1.454(3) O7 H11 0.83(5) C7 C6 1.527(3) C7 C8 1.535(3) C7 H7A 0.9900 C7 H7B 0.9900 O6 C14 1.436(3) O6 H10 0.81(4) C6 C5 1.531(3) C6 H6 1.0000 O5 C10 1.462(3) O5 H12 0.86(5) C8 C14 1.542(3) C8 C9 1.558(3) C8 C15 1.573(3) O8 H8A 0.89(5) C9 C11 1.548(3) C9 C10 1.576(3) C9 H9 1.0000 C10 C20 1.535(4) C11 C12 1.539(4) C11 H11A 0.9900 C11 H11B 0.9900 C12 C13 1.532(3) C12 H12A 0.9900 C12 H12B 0.9900 C13 C14 1.536(3) C13 C16 1.538(3) C13 H13 1.0000 C14 H14 1.0000 C15 C16 1.551(4) C15 H15A 0.9900 C15 H15B 0.9900 C16 C17 1.524(4) C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 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 C10 C1 C2 O1 108.1(2) C5 C1 C2 O1 -117.0(2) C10 C1 C2 C3 -131.4(2) C5 C1 C2 C3 3.5(3) O1 C2 C3 O2 -156.0(2) C1 C2 C3 O2 85.8(2) O1 C2 C3 C4 88.6(2) C1 C2 C3 C4 -29.7(3) O2 C3 C4 C19 49.5(3) C2 C3 C4 C19 166.5(2) O2 C3 C4 C18 168.7(2) C2 C3 C4 C18 -74.3(2) O2 C3 C4 C5 -73.2(2) C2 C3 C4 C5 43.8(2) C8 C7 C6 O4 172.6(2) C8 C7 C6 C5 -66.4(3) O4 C6 C5 O3 70.9(2) C7 C6 C5 O3 -50.1(3) O4 C6 C5 C1 -166.5(2) C7 C6 C5 C1 72.5(3) O4 C6 C5 C4 -51.7(3) C7 C6 C5 C4 -172.7(2) C10 C1 C5 O3 35.0(3) C2 C1 C5 O3 -95.7(2) C10 C1 C5 C6 -84.1(3) C2 C1 C5 C6 145.1(2) C10 C1 C5 C4 153.8(2) C2 C1 C5 C4 23.0(2) C19 C4 C5 O3 -39.2(3) C18 C4 C5 O3 -163.5(2) C3 C4 C5 O3 80.2(2) C19 C4 C5 C6 81.8(3) C18 C4 C5 C6 -42.5(3) C3 C4 C5 C6 -158.8(2) C19 C4 C5 C1 -159.8(2) C18 C4 C5 C1 75.9(2) C3 C4 C5 C1 -40.4(2) C6 C7 C8 C14 -58.1(3) C6 C7 C8 C9 70.3(3) C6 C7 C8 C15 -170.1(2) C7 C8 C9 C11 166.4(2) C14 C8 C9 C11 -62.0(2) C15 C8 C9 C11 47.8(2) C7 C8 C9 C10 -65.7(3) C14 C8 C9 C10 65.9(3) C15 C8 C9 C10 175.7(2) C2 C1 C10 O5 -62.0(2) C5 C1 C10 O5 170.1(2) C2 C1 C10 C20 49.7(3) C5 C1 C10 C20 -78.2(3) C2 C1 C10 C9 174.7(2) C5 C1 C10 C9 46.8(3) C11 C9 C10 O5 31.0(3) C8 C9 C10 O5 -97.3(3) C11 C9 C10 C20 -80.6(2) C8 C9 C10 C20 151.1(2) C11 C9 C10 C1 150.5(2) C8 C9 C10 C1 22.3(3) C8 C9 C11 C12 45.9(3) C10 C9 C11 C12 -89.1(2) C9 C11 C12 C13 -44.8(3) C11 C12 C13 C14 57.9(3) C11 C12 C13 C16 -55.1(3) C12 C13 C14 O6 174.38(19) C16 C13 C14 O6 -66.7(2) C12 C13 C14 C8 -69.4(2) C16 C13 C14 C8 49.5(2) C7 C8 C14 O6 -38.8(3) C9 C8 C14 O6 -169.56(19) C15 C8 C14 O6 76.2(2) C7 C8 C14 C13 -156.7(2) C9 C8 C14 C13 72.5(2) C15 C8 C14 C13 -41.8(2) C7 C8 C15 C16 141.3(2) C14 C8 C15 C16 19.7(2) C9 C8 C15 C16 -95.2(2) C12 C13 C16 O7 -162.8(2) C14 C13 C16 O7 80.0(2) C12 C13 C16 C17 -46.4(3) C14 C13 C16 C17 -163.6(2) C12 C13 C16 C15 81.1(2) C14 C13 C16 C15 -36.1(2) C8 C15 C16 O7 -105.7(2) C8 C15 C16 C17 136.9(2) C8 C15 C16 C13 9.9(3)