#------------------------------------------------------------------------------ #$Date: 2024-08-05 20:59:41 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293748 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/18/1571817.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_1571817 loop_ _publ_author_name 'Wang, Han' 'Xun, Shan-Shan' 'Yu, Chang-Bin' 'Zhou, Yong-Gui' _publ_section_title ; Palladium-catalyzed asymmetric hydrogenation of lactones under base-free conditions. ; _journal_issue 28 _journal_name_full 'Chemical science' _journal_page_first 11038 _journal_page_last 11042 _journal_paper_doi 10.1039/d4sc01890g _journal_volume 15 _journal_year 2024 _chemical_formula_sum 'C19 H18 O4' _chemical_formula_weight 310.33 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2023-03-09 deposited with the CCDC. 2024-06-11 downloaded from the CCDC. ; _cell_angle_alpha 82.2410(10) _cell_angle_beta 70.296(2) _cell_angle_gamma 66.5120(10) _cell_formula_units_Z 2 _cell_length_a 8.2353(3) _cell_length_b 9.8484(4) _cell_length_c 11.7427(5) _cell_measurement_reflns_used 9914 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 140.167 _cell_measurement_theta_min 7.997 _cell_volume 822.33(6) _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-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.964 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_unetI/netI 0.0303 _diffrn_reflns_Laue_measured_fraction_full 0.964 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 28232 _diffrn_reflns_point_group_measured_fraction_full 0.964 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 67.492 _diffrn_reflns_theta_min 3.999 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.253 _exptl_crystal_description prismatic _exptl_crystal_F_000 328 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.209 _refine_diff_density_min -0.127 _refine_diff_density_rms 0.028 _refine_ls_extinction_coef 0.059(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 2856 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0489 _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^)+(0.0724P)^2^+0.1431P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1336 _refine_ls_wR_factor_ref 0.1352 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2706 _reflns_number_total 2856 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01890g2.cif _cod_data_source_block cu_d8v23127_0m _cod_depositor_comments 'Adding full bibliography for 1571816--1571817.cif.' _cod_database_code 1571817 _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 0.870 _shelx_estimated_absorpt_t_max 0.919 _shelxl_version_number 2013-4 _shelx_res_file ; TITL cu_d8v23127_0m_a.res in P-1 CELL 1.54178 8.2353 9.8484 11.7427 82.241 70.296 66.512 ZERR 2 0.0003 0.0004 0.0005 0.001 0.002 0.001 LATT 1 SFAC C H O UNIT 38 36 8 OMIT -1 3 1 OMIT 1 2 1 OMIT -2 -4 1 OMIT -3.00 135.00 L.S. 8 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 HTAB C6 O2_$1 EQIV $1 -x+1, -y+1, -z+1 conf htab mpla wpdb -1 size 0.20 0.15 0.12 TEMP 20 WGHT 0.072400 0.143100 EXTI 0.059233 FVAR 2.99804 O1 3 0.161911 0.357915 0.531141 11.00000 0.07328 0.08579 = 0.03826 0.00134 -0.01513 -0.02467 O2 3 0.301223 0.508441 0.438015 11.00000 0.07499 0.07613 = 0.04292 -0.00571 -0.02472 -0.02800 O3 3 0.528805 0.221188 0.152231 11.00000 0.06543 0.09552 = 0.04721 -0.01376 -0.01015 -0.01751 O4 3 0.530664 0.177856 0.343238 11.00000 0.06122 0.07498 = 0.05432 0.00104 -0.02060 -0.00537 C1 1 0.233692 0.404277 0.435871 11.00000 0.05363 0.06424 = 0.04088 -0.00313 -0.01828 -0.01256 C2 1 0.253690 0.355285 0.312145 11.00000 0.05233 0.05958 = 0.03700 -0.00261 -0.01609 -0.01742 C3 1 0.217578 0.490168 0.228726 11.00000 0.05764 0.06225 = 0.04011 -0.00066 -0.02105 -0.02041 AFIX 23 H3A 2 0.243669 0.458436 0.147566 11.00000 -1.20000 H3B 2 0.087689 0.555953 0.257371 11.00000 -1.20000 AFIX 0 C4 1 0.339191 0.570588 0.226543 11.00000 0.05382 0.05238 = 0.04673 -0.00476 -0.01980 -0.01428 C5 1 0.379903 0.573561 0.330963 11.00000 0.05936 0.05606 = 0.04723 -0.00514 -0.02141 -0.01540 C6 1 0.492392 0.642703 0.337455 11.00000 0.07761 0.06764 = 0.07017 -0.00819 -0.04016 -0.02322 AFIX 43 H6 2 0.516275 0.643578 0.409262 11.00000 -1.20000 AFIX 0 C7 1 0.569211 0.710963 0.234529 11.00000 0.07582 0.06488 = 0.09063 -0.00190 -0.03438 -0.03240 AFIX 43 H7 2 0.646305 0.757802 0.236819 11.00000 -1.20000 AFIX 0 C8 1 0.532148 0.709925 0.128752 11.00000 0.07396 0.06044 = 0.07211 0.00406 -0.02479 -0.02843 AFIX 43 H8 2 0.584217 0.755973 0.059938 11.00000 -1.20000 AFIX 0 C9 1 0.418350 0.640937 0.124813 11.00000 0.06724 0.05591 = 0.05258 0.00132 -0.02323 -0.02132 AFIX 43 H9 2 0.393712 0.641169 0.053088 11.00000 -1.20000 AFIX 0 C10 1 0.117471 0.275550 0.330601 11.00000 0.05806 0.06859 = 0.04648 -0.00117 -0.01309 -0.02494 AFIX 23 H10A 2 0.159912 0.183716 0.373777 11.00000 -1.20000 H10B 2 -0.004389 0.337158 0.381539 11.00000 -1.20000 AFIX 0 C11 1 0.096900 0.240709 0.216527 11.00000 0.04904 0.05340 = 0.05141 -0.00185 -0.01496 -0.01976 C12 1 -0.033669 0.343398 0.166944 11.00000 0.06183 0.05785 = 0.08039 -0.00351 -0.03324 -0.01736 AFIX 43 H12 2 -0.107140 0.435157 0.204005 11.00000 -1.20000 AFIX 0 C13 1 -0.057198 0.312701 0.063938 11.00000 0.08926 0.08756 = 0.08897 0.01495 -0.05613 -0.04233 AFIX 43 H13 2 -0.145096 0.383816 0.031860 11.00000 -1.20000 AFIX 0 C14 1 0.047862 0.178487 0.008847 11.00000 0.09827 0.10918 = 0.06345 -0.00493 -0.02986 -0.06153 AFIX 43 H14 2 0.031386 0.157828 -0.060535 11.00000 -1.20000 AFIX 0 C15 1 0.177542 0.074266 0.055791 11.00000 0.07858 0.07741 = 0.07812 -0.02669 -0.00955 -0.03601 AFIX 43 H15 2 0.249308 -0.017356 0.018199 11.00000 -1.20000 AFIX 0 C16 1 0.202514 0.104603 0.159226 11.00000 0.05836 0.05513 = 0.07181 -0.00564 -0.01914 -0.01745 AFIX 43 H16 2 0.291003 0.032962 0.190544 11.00000 -1.20000 AFIX 0 C17 1 0.453659 0.245122 0.258100 11.00000 0.05542 0.06058 = 0.04357 -0.00461 -0.01549 -0.02079 C18 1 0.719950 0.067382 0.303452 11.00000 0.06200 0.07645 = 0.09160 -0.00349 -0.02289 -0.00593 AFIX 23 H18A 2 0.799348 0.107805 0.239925 11.00000 -1.20000 H18B 2 0.720498 -0.019020 0.272023 11.00000 -1.20000 AFIX 0 C19 1 0.788045 0.026603 0.408070 11.00000 0.08558 0.14785 = 0.11257 0.04179 -0.04236 -0.00775 AFIX 137 H19A 2 0.916610 -0.039105 0.382899 11.00000 -1.50000 H19B 2 0.715990 -0.022013 0.467127 11.00000 -1.50000 H19C 2 0.776256 0.114144 0.442890 11.00000 -1.50000 AFIX 0 HKLF 4 REM cu_d8v23127_0m_a.res in P-1 REM R1 = 0.0489 for 2706 Fo > 4sig(Fo) and 0.0505 for all 2856 data REM 210 parameters refined using 0 restraints END WGHT 0.0724 0.1433 REM Instructions for potential hydrogen bonds HTAB C6 O2_$1 REM Highest difference peak 0.209, deepest hole -0.127, 1-sigma level 0.028 Q1 1 0.6497 -0.0075 0.3455 11.00000 0.05 0.21 Q2 1 0.2456 0.3835 0.3673 11.00000 0.05 0.18 Q3 1 0.4511 0.1278 0.3724 11.00000 0.05 0.17 Q4 1 0.1133 0.2553 0.2661 11.00000 0.05 0.14 Q5 1 0.3353 0.5943 0.2824 11.00000 0.05 0.13 Q6 1 0.3303 0.3101 0.2932 11.00000 0.05 0.13 Q7 1 0.6923 0.0485 0.5073 11.00000 0.05 0.13 Q8 1 0.3730 0.5659 0.2744 11.00000 0.05 0.12 Q9 1 0.1691 0.2020 0.1885 11.00000 0.05 0.12 Q10 1 0.4985 0.7460 0.1942 11.00000 0.05 0.11 Q11 1 -0.0815 0.3052 0.1378 11.00000 0.05 0.11 Q12 1 -0.1741 0.4274 0.2773 11.00000 0.05 0.11 Q13 1 0.4973 0.1558 0.1954 11.00000 0.05 0.11 Q14 1 0.0818 0.3008 0.1840 11.00000 0.05 0.10 Q15 1 0.2044 0.3137 0.3202 11.00000 0.05 0.10 Q16 1 0.7227 0.0240 0.2164 11.00000 0.05 0.10 Q17 1 -0.2347 0.4204 0.0791 11.00000 0.05 0.10 Q18 1 0.4724 0.7160 0.2987 11.00000 0.05 0.10 Q19 1 0.1846 0.4124 0.5999 11.00000 0.05 0.09 Q20 1 0.9255 -0.0911 0.3458 11.00000 0.05 0.09 ; _shelx_res_checksum 72069 _shelx_hkl_file ; -2 0 0 282.37 23.70 -2 0 0 303.67 23.50 -2 0 0 353.76 24.20 -2 0 0 324.37 24.00 2 0 0 316.27 23.80 2 0 0 322.87 23.70 -3 0 0 8122.69 589.54 -4 0 0 3542.45 228.08 -4 0 0 2720.53 229.28 -4 0 0 3217.18 229.48 -4 0 0 3226.58 229.08 -4 0 0 3468.15 228.58 -4 0 0 3328.87 228.68 -4 0 0 3209.48 229.38 4 0 0 2972.00 228.88 4 0 0 2823.42 227.48 4 0 0 2834.72 228.48 -5 0 0 72.19 9.70 -5 0 0 90.99 9.40 -5 0 0 110.79 8.80 -5 0 0 98.09 9.20 -5 0 0 85.99 9.30 -5 0 0 86.59 8.50 -5 0 0 103.09 9.30 5 0 0 95.29 9.70 5 0 0 85.69 7.20 -6 0 0 5.90 2.10 -6 0 0 5.70 2.70 -6 0 0 11.70 2.90 -6 0 0 6.80 3.70 -6 0 0 9.10 2.40 -6 0 0 9.60 6.80 -6 0 0 9.00 3.20 -6 0 0 6.60 2.40 -6 0 0 8.30 2.40 -6 0 0 6.20 2.70 6 0 0 2.30 2.50 -7 0 0 52.99 6.10 -7 0 0 66.39 6.30 -7 0 0 53.99 6.50 -7 0 0 59.99 6.50 -7 0 0 67.99 7.10 -7 0 0 55.19 6.00 -7 0 0 68.19 7.60 -7 0 0 49.70 6.70 7 0 0 53.99 5.20 7 0 0 57.69 5.00 7 0 0 56.19 6.30 7 0 0 50.39 5.60 -8 0 0 2.30 1.90 -8 0 0 3.90 2.30 -8 0 0 2.70 1.50 -8 0 0 1.60 1.50 -8 0 0 0.60 1.30 -8 0 0 2.00 3.10 -8 0 0 2.80 2.00 8 0 0 3.60 1.60 8 0 0 1.00 0.80 8 0 0 1.90 0.70 8 -1 0 50.69 4.40 8 -1 0 49.70 5.80 8 -1 0 48.30 4.20 -8 1 0 50.29 5.20 -8 1 0 62.39 5.50 -8 1 0 47.60 5.40 -8 1 0 50.99 5.00 7 -1 0 57.79 6.40 7 -1 0 59.19 5.00 7 -1 0 58.79 6.10 7 -1 0 59.59 5.50 7 -1 0 59.49 5.30 -7 1 0 58.89 6.00 -7 1 0 59.19 6.30 -7 1 0 57.59 6.80 -7 1 0 57.69 7.20 -7 1 0 58.69 6.30 -7 1 0 55.29 6.40 -7 1 0 50.09 6.90 6 -1 0 7.10 2.10 6 -1 0 8.70 3.10 6 -1 0 10.20 1.80 6 -1 0 5.80 1.40 6 -1 0 6.90 1.40 -6 1 0 8.60 2.60 -6 1 0 14.30 3.70 -6 1 0 10.80 3.00 -6 1 0 5.00 2.60 -6 1 0 10.50 3.60 -6 1 0 7.50 3.70 -6 1 0 11.50 2.50 -6 1 0 7.80 2.30 -6 1 0 8.30 2.40 -6 1 0 11.10 2.80 -6 1 0 2.90 1.80 5 -1 0 41.40 4.90 5 -1 0 50.89 6.30 5 -1 0 44.40 4.30 5 -1 0 45.50 4.00 -5 1 0 46.70 6.00 -5 1 0 44.90 5.20 -5 1 0 48.10 5.70 -5 1 0 48.70 6.20 -5 1 0 44.90 5.00 -5 1 0 38.40 5.90 4 -1 0 57.39 6.20 4 -1 0 55.59 6.80 4 -1 0 55.69 5.10 -4 1 0 58.59 6.90 -4 1 0 68.99 6.30 -4 1 0 60.59 6.70 -4 1 0 60.89 6.10 -4 1 0 69.89 6.50 -4 1 0 62.09 6.00 3 -1 0 1880.51 147.69 3 -1 0 1991.20 148.59 -3 1 0 2224.68 149.49 -3 1 0 1834.62 148.39 -3 1 0 2236.58 149.19 -3 -1 0 1359.06 94.79 -3 -1 0 1197.78 95.09 -3 -1 0 1300.97 94.79 -3 -1 0 1182.38 95.19 -3 -1 0 1366.06 95.19 3 1 0 1359.26 94.89 -4 -1 0 1525.65 126.19 -4 -1 0 1777.72 125.09 -4 -1 0 2005.50 125.89 -4 -1 0 1804.62 124.89 -4 -1 0 1790.32 125.09 -4 -1 0 1730.73 125.59 -4 -1 0 1609.54 125.39 4 1 0 1553.54 125.09 4 1 0 1552.64 124.79 -5 -1 0 89.49 8.40 -5 -1 0 73.09 7.30 -5 -1 0 68.39 7.30 -5 -1 0 79.09 8.00 -5 -1 0 66.89 8.10 -5 -1 0 89.99 7.90 -5 -1 0 81.89 8.00 -5 -1 0 84.69 7.20 5 1 0 70.69 8.00 5 1 0 72.79 6.30 5 1 0 69.39 7.60 -6 -1 0 137.79 13.00 -6 -1 0 140.39 12.60 -6 -1 0 134.49 12.40 -6 -1 0 137.59 13.70 -6 -1 0 137.49 13.10 -6 -1 0 166.28 12.70 -6 -1 0 157.68 13.00 -6 -1 0 126.89 12.30 -6 -1 0 156.28 12.70 6 1 0 137.39 11.30 6 1 0 131.99 13.20 6 1 0 123.19 10.80 -7 -1 0 139.59 14.50 -7 -1 0 171.48 16.20 -7 -1 0 165.58 15.50 -7 -1 0 164.38 14.20 -7 -1 0 179.48 14.80 -7 -1 0 167.18 14.20 -7 -1 0 149.88 14.40 -7 -1 0 177.68 15.10 -7 -1 0 186.38 14.30 7 1 0 131.69 13.70 7 1 0 156.08 13.00 7 1 0 156.88 12.90 7 1 0 170.18 15.60 -8 -1 0 3.00 2.10 -8 -1 0 5.80 1.90 -8 -1 0 4.10 1.50 -8 -1 0 0.30 1.60 -8 -1 0 4.70 1.60 -8 -1 0 4.50 1.80 -8 -1 0 2.10 1.80 8 1 0 3.10 0.70 -9 -1 0 0.20 0.80 -9 -1 0 -0.80 0.80 8 -2 0 1.40 0.40 8 -2 0 2.60 0.80 -8 2 0 3.60 1.30 -8 2 0 1.60 1.60 -8 2 0 1.70 1.00 7 -2 0 1.30 1.30 7 -2 0 1.40 0.60 7 -2 0 0.50 0.60 7 -2 0 0.30 1.40 7 -2 0 1.00 0.80 -7 2 0 3.00 1.40 -7 2 0 1.40 1.70 -7 2 0 1.90 1.70 -7 2 0 3.30 1.90 -7 2 0 1.80 2.00 -7 2 0 -1.20 1.60 -7 2 0 -0.10 1.50 6 -2 0 583.54 43.70 6 -2 0 587.64 43.50 6 -2 0 645.94 46.80 6 -2 0 548.95 46.30 6 -2 0 593.34 44.10 6 -2 0 630.14 45.10 -6 2 0 593.44 45.60 -6 2 0 555.14 46.80 -6 2 0 620.74 48.10 -6 2 0 590.64 45.30 -6 2 0 557.84 46.20 -6 2 0 573.24 44.70 -6 2 0 568.64 46.20 -6 2 0 606.34 47.60 -6 2 0 595.94 45.10 -6 2 0 545.45 46.10 5 -2 0 34.70 3.50 5 -2 0 36.50 5.40 5 -2 0 33.20 3.70 5 -2 0 38.00 4.00 5 -2 0 44.40 4.90 -5 2 0 36.70 5.60 -5 2 0 35.20 4.70 -5 2 0 35.30 5.30 -5 2 0 46.60 5.10 -5 2 0 30.30 5.70 -5 2 0 36.60 6.30 -5 2 0 37.00 5.10 -5 2 0 40.70 4.70 -5 2 0 33.50 6.10 -5 2 0 49.10 5.10 -5 2 0 49.90 7.60 4 -2 0 744.63 49.90 4 -2 0 636.24 51.49 4 -2 0 614.04 50.69 -4 2 0 708.13 51.19 -4 2 0 593.24 52.39 -4 2 0 758.02 51.89 -4 2 0 730.73 52.19 -4 2 0 674.73 51.69 -4 2 0 656.63 50.89 1 -2 0 592.34 44.50 1 -2 0 605.54 44.30 -1 2 0 539.15 43.90 -1 2 0 652.63 44.60 -1 2 0 558.54 44.60 -1 2 0 660.83 44.40 -3 -2 0 18.20 2.30 -3 -2 0 24.20 2.50 -3 -2 0 22.00 2.60 -3 -2 0 19.00 2.70 -3 -2 0 19.80 2.50 -3 -2 0 17.40 2.60 -3 -2 0 23.60 2.80 3 2 0 19.80 2.30 3 2 0 25.10 2.40 -4 -2 0 1917.31 128.59 -4 -2 0 1824.42 128.59 -4 -2 0 1739.93 128.39 -4 -2 0 1774.42 128.39 -4 -2 0 1569.74 128.69 4 2 0 1695.93 128.09 4 2 0 1730.13 128.39 -5 -2 0 2460.95 158.98 -5 -2 0 2332.57 158.58 -5 -2 0 2118.69 158.48 -5 -2 0 1923.41 158.18 -5 -2 0 1980.00 158.38 -5 -2 0 2268.47 159.28 -5 -2 0 1933.41 159.08 -5 -2 0 2433.06 158.48 5 2 0 1980.70 158.28 5 2 0 2446.06 159.08 5 2 0 1873.41 156.78 -6 -2 0 690.83 47.60 -6 -2 0 661.13 47.20 -6 -2 0 714.13 47.60 -6 -2 0 583.14 47.30 -6 -2 0 566.74 48.50 -6 -2 0 638.74 47.00 -6 -2 0 561.14 47.30 6 2 0 657.33 46.10 6 2 0 584.24 48.00 6 2 0 539.55 47.50 -7 -2 0 233.58 18.20 -7 -2 0 229.28 19.90 -7 -2 0 233.58 18.70 -7 -2 0 197.68 17.70 -7 -2 0 225.88 18.40 -7 -2 0 225.08 18.60 -7 -2 0 255.47 18.60 -7 -2 0 195.98 17.90 -7 -2 0 186.48 17.70 -7 -2 0 246.58 18.40 7 2 0 193.78 18.90 7 2 0 203.18 16.80 7 2 0 184.08 16.40 -8 -2 0 25.80 3.60 -8 -2 0 20.20 4.50 -8 -2 0 29.90 5.40 -8 -2 0 27.70 4.70 -8 -2 0 19.90 4.50 -8 -2 0 21.90 4.00 -8 -2 0 20.70 3.50 -8 -2 0 25.20 3.80 8 2 0 16.60 2.20 8 2 0 17.80 2.30 8 2 0 15.50 3.30 -9 -2 0 8.30 2.20 -9 -2 0 3.30 1.80 -9 -2 0 6.80 1.80 7 -3 0 71.09 6.00 7 -3 0 60.29 6.10 7 -3 0 60.89 6.00 7 -3 0 68.59 5.30 -7 3 0 52.89 7.00 -7 3 0 61.19 7.60 -7 3 0 56.69 7.90 -7 3 0 77.49 8.10 -7 3 0 58.79 8.50 -7 3 0 57.99 6.90 6 -3 0 19.40 3.20 6 -3 0 17.80 2.20 6 -3 0 18.90 2.90 6 -3 0 15.40 2.60 6 -3 0 16.10 2.30 6 -3 0 16.70 3.10 -6 3 0 24.70 4.70 -6 3 0 18.70 4.50 -6 3 0 14.20 3.20 -6 3 0 15.70 3.30 -6 3 0 21.00 4.60 -6 3 0 12.40 3.60 -6 3 0 10.60 2.60 -6 3 0 12.90 2.90 -6 3 0 13.70 3.30 5 -3 0 190.08 15.20 5 -3 0 198.28 15.90 5 -3 0 190.18 15.60 5 -3 0 193.98 14.60 5 -3 0 212.48 17.70 5 -3 0 178.28 14.70 -5 3 0 188.68 17.20 -5 3 0 177.98 17.00 -5 3 0 191.78 15.60 -5 3 0 175.68 16.30 -5 3 0 188.18 15.80 -5 3 0 174.28 17.10 -5 3 0 183.98 15.80 -5 3 0 192.38 19.30 -5 3 0 174.68 17.80 -5 3 0 187.18 18.10 -5 3 0 175.98 16.90 -5 3 0 174.88 16.10 -5 3 0 228.38 20.20 4 -3 0 663.33 47.10 4 -3 0 589.64 44.70 4 -3 0 544.05 44.80 4 -3 0 583.74 45.70 4 -3 0 579.14 45.60 4 -3 0 584.64 45.30 -4 3 0 610.34 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93.29 9.70 -6 -6 0 84.39 9.00 -6 -6 0 88.49 12.10 -6 -6 0 97.89 9.30 -6 -6 0 90.99 9.90 -6 -6 0 79.99 9.10 -6 -6 0 78.49 9.10 -6 -6 0 99.39 10.30 -6 -6 0 73.59 9.60 -6 -6 0 102.09 9.40 6 6 0 92.09 8.30 6 6 0 89.99 8.00 6 6 0 89.29 10.20 6 6 0 83.99 9.30 6 6 0 94.89 8.90 -7 -6 0 61.09 9.00 -7 -6 0 58.89 6.40 -7 -6 0 54.99 6.70 -7 -6 0 52.09 6.90 -7 -6 0 59.89 7.00 -7 -6 0 38.00 8.50 -7 -6 0 58.29 8.70 -7 -6 0 54.39 6.50 -7 -6 0 54.39 9.10 -7 -6 0 47.20 7.90 7 6 0 53.99 6.20 7 6 0 56.49 5.70 7 6 0 56.79 7.50 -8 -6 0 83.29 8.90 -8 -6 0 93.79 8.20 -8 -6 0 73.99 9.70 -8 -6 0 87.49 8.80 -8 -6 0 64.69 9.80 -8 -6 0 75.59 9.90 8 6 0 82.49 7.20 8 6 0 84.79 7.60 8 6 0 84.19 7.70 -9 -6 0 55.39 7.10 -9 -6 0 57.19 5.70 -9 -6 0 56.59 5.70 -9 -6 0 53.09 6.70 -9 -6 0 63.39 5.40 9 6 0 57.79 5.20 4 -7 0 95.69 9.40 4 -7 0 80.59 6.40 4 -7 0 86.29 7.60 4 -7 0 75.69 7.30 4 -7 0 70.59 8.90 -4 7 0 76.99 7.30 -4 7 0 78.99 7.20 -4 7 0 78.59 9.80 -4 7 0 55.49 9.90 -4 7 0 85.49 8.70 -4 7 0 76.59 9.80 3 -7 0 14.60 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403.26 29.60 5 8 0 373.76 29.20 -6 -8 0 13.00 3.40 -6 -8 0 15.20 3.70 -6 -8 0 12.50 4.20 -6 -8 0 23.30 4.20 -6 -8 0 18.90 4.60 -6 -8 0 21.20 3.50 -6 -8 0 14.30 3.50 -6 -8 0 17.50 5.20 -6 -8 0 11.90 3.60 -6 -8 0 20.10 5.70 6 8 0 11.50 2.80 6 8 0 18.70 3.00 6 8 0 15.30 2.60 6 8 0 15.90 5.70 -7 -8 0 5.40 2.40 -7 -8 0 3.50 1.90 -7 -8 0 1.90 3.70 -7 -8 0 0.50 2.00 -7 -8 0 -1.40 1.40 -7 -8 0 0.70 1.80 -7 -8 0 0.80 3.30 -7 -8 0 1.90 2.00 -7 -8 0 2.10 1.50 7 8 0 -1.80 1.90 7 8 0 1.50 1.00 7 8 0 1.30 1.40 7 8 0 0.80 1.10 7 8 0 0.50 1.10 -8 -8 0 2.60 1.70 -8 -8 0 1.80 1.00 -8 -8 0 -0.60 1.10 -8 -8 0 -1.10 1.30 -8 -8 0 1.40 1.40 -8 -8 0 2.80 1.70 8 8 0 1.50 0.90 8 8 0 1.90 1.10 8 8 0 0.90 1.00 -3 9 0 18.70 3.40 2 -9 0 5.80 2.10 2 -9 0 7.70 1.80 2 -9 0 9.20 3.40 2 -9 0 9.20 2.20 -2 9 0 6.70 2.50 -2 9 0 2.80 2.40 -2 9 0 4.80 2.60 1 -9 0 70.29 6.90 1 -9 0 54.39 8.20 1 -9 0 71.39 7.50 1 -9 0 48.10 8.90 1 -9 0 90.29 8.90 -1 9 0 79.29 12.70 -1 9 0 79.59 8.40 -1 9 0 75.89 8.40 -1 9 0 65.19 9.60 0 -9 0 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48.30 7.30 3 11 0 59.99 6.80 -4 -11 0 6.60 2.10 -4 -11 0 10.50 2.20 -4 -11 0 5.20 2.30 -4 -11 0 8.30 2.60 -4 -11 0 5.90 1.60 4 11 0 3.80 2.00 4 11 0 4.30 2.50 -5 -11 0 -2.00 1.60 -5 -11 0 -1.40 0.90 -5 -11 0 -2.60 1.40 -5 -11 0 1.50 1.20 -5 -11 0 -0.40 1.10 -5 -11 0 0.30 1.40 5 11 0 0.90 0.50 -6 -11 0 8.90 2.90 -6 -11 0 10.40 2.30 -6 -11 0 13.70 2.10 -6 -11 0 11.10 2.50 -6 -11 0 10.50 2.20 6 11 0 16.10 2.90 6 11 0 9.00 1.40 6 11 -1 11.70 1.60 6 11 -1 11.00 2.40 -6 -11 1 8.60 1.70 -6 -11 1 14.60 1.70 -6 -11 1 11.10 2.10 -6 -11 1 9.70 2.10 5 11 -1 26.80 4.90 5 11 -1 26.50 2.60 -5 -11 1 30.40 3.60 -5 -11 1 25.20 4.60 -5 -11 1 28.60 3.70 -5 -11 1 22.40 3.60 -5 -11 1 32.30 3.50 4 11 -1 4.10 1.80 4 11 -1 2.00 1.90 -4 -11 1 5.80 1.50 -4 -11 1 1.70 2.50 -4 -11 1 0.70 1.50 -4 -11 1 7.00 2.30 -4 -11 1 4.30 1.50 3 11 -1 26.70 3.70 -3 -11 1 24.10 3.10 -3 -11 1 17.00 4.90 -3 -11 1 23.60 3.70 -3 -11 1 18.30 4.00 -3 -11 1 25.30 3.20 2 11 -1 26.10 4.40 2 11 -1 17.80 4.30 -2 -11 1 28.70 4.70 -2 -11 1 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-0.30 1.10 6 0 13 -0.60 0.80 0 -1 -13 24.50 2.30 0 -1 -13 22.70 2.50 0 1 13 24.50 3.30 0 1 13 19.10 3.30 0 1 13 18.50 3.20 0 1 13 25.30 3.40 0 1 13 20.30 3.10 -1 -1 -13 118.39 9.40 -1 -1 -13 119.59 9.50 1 1 13 126.49 11.10 1 1 13 109.79 9.90 1 1 13 121.19 12.00 -2 -1 -13 1.60 0.80 -2 -1 -13 0.20 1.40 -2 -1 -13 6.60 2.10 2 1 13 0.70 1.40 2 1 13 2.10 1.80 2 1 13 4.40 2.00 2 1 13 2.80 1.40 -3 -1 -13 84.19 8.50 -3 -1 -13 105.89 10.80 3 1 13 83.59 8.50 3 1 13 65.39 8.60 3 1 13 85.29 8.30 -4 -1 -13 7.40 2.40 -4 -1 -13 9.40 3.00 4 1 13 11.70 2.60 4 1 13 6.80 2.50 -5 -1 -13 38.40 4.80 5 1 13 37.20 4.40 5 1 13 33.60 6.20 -6 -1 -13 1.60 1.70 -6 -1 -13 -1.90 1.40 6 1 13 0.00 1.00 0 -2 -13 6.70 1.10 0 -2 -13 8.50 1.50 0 2 13 6.60 1.80 0 2 13 5.90 1.70 0 2 13 5.80 1.90 0 2 13 6.30 1.70 -1 -2 -13 79.59 6.80 -1 -2 -13 89.29 6.80 -1 -2 -13 79.39 7.40 1 2 13 78.79 7.80 1 2 13 88.99 8.90 1 2 13 76.49 7.40 1 2 13 74.89 7.80 -2 -2 -13 8.50 2.60 -2 -2 -13 8.10 2.20 -2 -2 -13 5.50 1.10 -2 -2 -13 10.80 3.70 2 2 13 9.50 2.40 2 2 13 4.70 1.80 2 2 13 9.80 2.50 -3 -2 -13 22.40 3.80 -3 -2 -13 16.00 4.10 -3 -2 -13 25.30 3.90 3 2 13 21.10 3.80 3 2 13 17.40 3.80 3 2 13 23.70 4.10 3 2 13 21.30 3.20 -4 -2 -13 37.10 4.90 -4 -2 -13 39.00 6.10 4 2 13 32.50 4.60 4 2 13 30.30 5.20 -5 -2 -13 11.80 2.80 -5 -2 -13 12.10 2.60 5 2 13 6.40 3.90 5 2 13 16.30 3.10 -6 -2 -13 85.39 7.70 6 2 13 65.29 7.80 6 2 13 79.79 7.20 -1 -3 -13 37.40 3.20 -1 -3 -13 33.30 4.20 1 3 13 37.60 4.50 1 3 13 30.80 4.10 1 3 13 39.10 4.40 1 3 13 37.50 4.30 -2 -3 -13 6.20 1.00 -2 -3 -13 6.40 2.10 2 3 13 8.00 2.90 2 3 13 7.20 2.20 -3 -3 -13 10.80 2.60 3 3 13 10.70 2.80 3 3 13 14.40 2.70 3 3 13 10.10 3.60 -4 -3 -13 5.20 2.10 -4 -3 -13 5.90 2.30 -4 -3 -13 1.60 1.80 4 3 13 4.80 2.10 -5 -3 -13 21.80 4.80 -5 -3 -13 21.60 3.70 5 3 13 15.30 3.30 -6 -3 -13 144.79 12.40 6 3 13 138.79 11.90 7 3 13 29.00 4.30 -1 -4 -13 46.50 4.00 1 4 13 58.09 5.60 1 4 13 52.69 5.20 1 4 13 47.00 5.10 1 4 13 49.00 6.60 -2 -4 -13 72.89 5.00 -2 -4 -13 62.99 6.40 2 4 13 57.49 6.20 2 4 13 53.69 6.10 2 4 13 64.89 6.40 -3 -4 -13 43.10 4.60 -3 -4 -13 32.10 4.30 3 4 13 35.60 4.60 3 4 13 32.70 4.50 -4 -4 -13 361.46 29.90 4 4 13 406.06 29.60 4 4 13 358.66 28.70 -5 -4 -13 -0.50 1.30 5 4 13 0.20 1.20 -6 -4 -13 23.90 3.60 6 4 13 22.80 3.30 7 4 13 33.80 4.70 -2 -5 -13 41.80 4.40 2 5 13 37.30 4.50 2 5 13 39.80 4.20 -3 -5 -13 123.39 11.10 3 5 13 132.29 11.10 3 5 13 126.19 11.00 -4 -5 -13 203.98 16.00 4 5 13 157.88 16.30 4 5 13 202.48 15.80 -5 -5 -13 18.80 3.30 5 5 13 18.70 3.00 -6 -5 -13 46.50 5.10 6 5 13 45.30 5.00 3 6 13 32.00 4.30 3 6 13 33.80 4.30 -4 -6 -13 2.10 1.20 4 6 13 3.50 1.10 4 6 13 5.50 1.90 -5 -6 -13 7.30 2.10 5 6 13 7.30 1.80 -2 0 -14 19.70 2.90 2 0 14 14.50 2.70 2 0 14 13.30 2.90 -3 0 -14 422.56 32.00 3 0 14 407.86 33.30 -4 0 -14 4.50 1.50 4 0 14 2.00 1.40 4 0 14 3.90 1.80 -2 -1 -14 56.89 5.70 2 1 14 54.79 5.60 2 1 14 53.49 5.50 -3 -1 -14 213.18 16.90 3 1 14 200.48 16.60 4 1 14 94.09 9.90 -2 -2 -14 102.29 10.80 2 2 14 104.89 8.60 -3 -2 -14 10.60 2.00 3 2 14 9.10 2.10 -4 -2 -14 46.50 4.70 -4 -2 -14 47.00 5.10 4 2 14 40.70 4.70 -5 -2 -14 23.30 3.20 5 2 14 22.70 3.40 -3 -3 -14 39.10 4.00 -3 -3 -14 33.10 3.80 3 3 14 33.00 4.00 4 3 14 10.40 2.20 -5 -3 -14 23.70 3.50 5 3 14 25.00 4.30 -4 -4 -14 42.70 5.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87237 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.16191(16) 0.35791(14) 0.53114(9) 0.0683(4) Uani 1 1 d . . . . . O2 O 0.30122(16) 0.50844(13) 0.43802(9) 0.0625(3) Uani 1 1 d . . . . . O3 O 0.52880(16) 0.22119(15) 0.15223(9) 0.0743(4) Uani 1 1 d . . . . . O4 O 0.53066(15) 0.17786(13) 0.34324(10) 0.0697(4) Uani 1 1 d . . . . . C1 C 0.2337(2) 0.40428(17) 0.43587(12) 0.0549(4) Uani 1 1 d . . . . . C2 C 0.25369(19) 0.35529(16) 0.31214(11) 0.0500(4) Uani 1 1 d . . . . . C3 C 0.2176(2) 0.49017(16) 0.22873(12) 0.0524(4) Uani 1 1 d . . . . . H3A H 0.2437 0.4584 0.1476 0.063 Uiso 1 1 calc R U . . . H3B H 0.0877 0.5560 0.2574 0.063 Uiso 1 1 calc R U . . . C4 C 0.33919(19) 0.57059(15) 0.22654(12) 0.0513(4) Uani 1 1 d . . . . . C5 C 0.3799(2) 0.57356(16) 0.33096(13) 0.0545(4) Uani 1 1 d . . . . . C6 C 0.4924(2) 0.64270(19) 0.33746(16) 0.0677(5) Uani 1 1 d . . . . . H6 H 0.5163 0.6436 0.4093 0.081 Uiso 1 1 calc R U . . . C7 C 0.5692(3) 0.71096(19) 0.23453(18) 0.0727(5) Uani 1 1 d . . . . . H7 H 0.6463 0.7578 0.2368 0.087 Uiso 1 1 calc R U . . . C8 C 0.5321(3) 0.70992(18) 0.12875(16) 0.0677(4) Uani 1 1 d . . . . . H8 H 0.5842 0.7560 0.0599 0.081 Uiso 1 1 calc R U . . . C9 C 0.4184(2) 0.64094(17) 0.12481(14) 0.0581(4) Uani 1 1 d . . . . . H9 H 0.3937 0.6412 0.0531 0.070 Uiso 1 1 calc R U . . . C10 C 0.1175(2) 0.27555(18) 0.33060(13) 0.0581(4) Uani 1 1 d . . . . . H10A H 0.1599 0.1837 0.3738 0.070 Uiso 1 1 calc R U . . . H10B H -0.0044 0.3372 0.3815 0.070 Uiso 1 1 calc R U . . . C11 C 0.09690(19) 0.24071(15) 0.21653(12) 0.0512(4) Uani 1 1 d . . . . . C12 C -0.0337(2) 0.34340(18) 0.16694(16) 0.0651(4) Uani 1 1 d . . . . . H12 H -0.1071 0.4352 0.2040 0.078 Uiso 1 1 calc R U . . . C13 C -0.0572(3) 0.3127(2) 0.06394(19) 0.0795(5) Uani 1 1 d . . . . . H13 H -0.1451 0.3838 0.0319 0.095 Uiso 1 1 calc R U . . . C14 C 0.0479(3) 0.1785(3) 0.00885(17) 0.0811(6) Uani 1 1 d . . . . . H14 H 0.0314 0.1578 -0.0605 0.097 Uiso 1 1 calc R U . . . C15 C 0.1775(3) 0.0743(2) 0.05579(17) 0.0772(5) Uani 1 1 d . . . . . H15 H 0.2493 -0.0174 0.0182 0.093 Uiso 1 1 calc R U . . . C16 C 0.2025(2) 0.10460(17) 0.15923(15) 0.0628(4) Uani 1 1 d . . . . . H16 H 0.2910 0.0330 0.1905 0.075 Uiso 1 1 calc R U . . . C17 C 0.4537(2) 0.24512(16) 0.25810(12) 0.0531(4) Uani 1 1 d . . . . . C18 C 0.7199(3) 0.0674(2) 0.30345(19) 0.0834(6) Uani 1 1 d . . . . . H18A H 0.7993 0.1078 0.2399 0.100 Uiso 1 1 calc R U . . . H18B H 0.7205 -0.0190 0.2720 0.100 Uiso 1 1 calc R U . . . C19 C 0.7880(4) 0.0266(4) 0.4081(3) 0.1287(11) Uani 1 1 d . . . . . H19A H 0.9166 -0.0391 0.3829 0.193 Uiso 1 1 calc R U . . . H19B H 0.7160 -0.0220 0.4671 0.193 Uiso 1 1 calc R U . . . H19C H 0.7763 0.1141 0.4429 0.193 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 0.0733(7) 0.0858(8) 0.0383(6) 0.0013(5) -0.0151(5) -0.0247(6) O2 0.0750(7) 0.0761(7) 0.0429(6) -0.0057(5) -0.0247(5) -0.0280(6) O3 0.0654(7) 0.0955(9) 0.0472(6) -0.0138(5) -0.0102(5) -0.0175(6) O4 0.0612(7) 0.0750(7) 0.0543(6) 0.0010(5) -0.0206(5) -0.0054(5) C1 0.0536(8) 0.0642(9) 0.0409(7) -0.0031(6) -0.0183(6) -0.0126(7) C2 0.0523(8) 0.0596(8) 0.0370(7) -0.0026(5) -0.0161(5) -0.0174(6) C3 0.0576(8) 0.0623(8) 0.0401(7) -0.0007(6) -0.0210(6) -0.0204(6) C4 0.0538(8) 0.0524(7) 0.0467(7) -0.0048(6) -0.0198(6) -0.0143(6) C5 0.0594(8) 0.0561(8) 0.0472(7) -0.0051(6) -0.0214(6) -0.0154(6) C6 0.0776(10) 0.0676(10) 0.0702(10) -0.0082(8) -0.0402(9) -0.0232(8) C7 0.0758(11) 0.0649(10) 0.0906(12) -0.0019(9) -0.0344(9) -0.0324(8) C8 0.0740(10) 0.0604(9) 0.0721(10) 0.0041(7) -0.0248(8) -0.0284(8) C9 0.0672(9) 0.0559(8) 0.0526(8) 0.0013(6) -0.0232(7) -0.0213(7) C10 0.0581(8) 0.0686(9) 0.0465(8) -0.0012(6) -0.0131(6) -0.0249(7) C11 0.0490(7) 0.0534(8) 0.0514(8) -0.0018(6) -0.0150(6) -0.0198(6) C12 0.0618(9) 0.0578(9) 0.0804(11) -0.0035(7) -0.0332(8) -0.0174(7) C13 0.0893(13) 0.0876(13) 0.0890(13) 0.0150(10) -0.0561(11) -0.0423(10) C14 0.0983(14) 0.1092(15) 0.0635(10) -0.0049(10) -0.0299(10) -0.0615(13) C15 0.0786(11) 0.0774(11) 0.0781(11) -0.0267(9) -0.0096(9) -0.0360(9) C16 0.0584(9) 0.0551(8) 0.0718(10) -0.0056(7) -0.0191(7) -0.0174(7) C17 0.0554(8) 0.0606(8) 0.0436(7) -0.0046(6) -0.0155(6) -0.0208(6) C18 0.0620(10) 0.0764(11) 0.0916(13) -0.0035(10) -0.0229(9) -0.0059(9) C19 0.0856(15) 0.148(2) 0.1126(19) 0.0418(17) -0.0424(14) -0.0077(15) 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 C1 O2 C5 121.40(11) . . ? C17 O4 C18 116.98(13) . . ? O1 C1 O2 117.63(13) . . ? O1 C1 C2 124.93(14) . . ? O2 C1 C2 117.44(12) . . ? C1 C2 C3 109.28(12) . . ? C1 C2 C17 108.45(11) . . ? C3 C2 C17 108.89(11) . . ? C1 C2 C10 108.28(11) . . ? C3 C2 C10 113.05(11) . . ? C17 C2 C10 108.80(12) . . ? C4 C3 C2 109.86(11) . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? C2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C9 117.21(14) . . ? C5 C4 C3 118.49(13) . . ? C9 C4 C3 124.28(12) . . ? C6 C5 C4 122.81(14) . . ? C6 C5 O2 116.70(13) . . ? C4 C5 O2 120.46(13) . . ? C5 C6 C7 118.41(15) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C8 C7 C6 120.41(15) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 120.07(16) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C4 121.10(14) . . ? C8 C9 H9 119.5 . . ? C4 C9 H9 119.5 . . ? C11 C10 C2 115.37(11) . . ? C11 C10 H10A 108.4 . . ? C2 C10 H10A 108.4 . . ? C11 C10 H10B 108.4 . . ? C2 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C16 117.53(14) . . ? C12 C11 C10 120.50(14) . . ? C16 C11 C10 121.94(14) . . ? C13 C12 C11 121.44(16) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 120.22(18) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.84(16) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 120.26(17) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.71(16) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? O3 C17 O4 124.44(14) . . ? O3 C17 C2 123.89(13) . . ? O4 C17 C2 111.66(11) . . ? O4 C18 C19 107.66(17) . . ? O4 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? O4 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.2003(18) . ? O2 C1 1.3541(19) . ? O2 C5 1.4056(18) . ? O3 C17 1.1950(17) . ? O4 C17 1.3245(18) . ? O4 C18 1.458(2) . ? C1 C2 1.5282(18) . ? C2 C3 1.5306(19) . ? C2 C17 1.533(2) . ? C2 C10 1.554(2) . ? C3 C4 1.497(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.3826(19) . ? C4 C9 1.394(2) . ? C5 C6 1.376(2) . ? C6 C7 1.385(3) . ? C6 H6 0.9300 . ? C7 C8 1.378(2) . ? C7 H7 0.9300 . ? C8 C9 1.374(2) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.505(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.384(2) . ? C11 C16 1.388(2) . ? C12 C13 1.377(2) . ? C12 H12 0.9300 . ? C13 C14 1.362(3) . ? C13 H13 0.9300 . ? C14 C15 1.367(3) . ? C14 H14 0.9300 . ? C15 C16 1.386(2) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 C19 1.462(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C6 H6 O2 0.93 2.65 3.464(2) 146.8 2_666 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 O2 C1 O1 -177.12(12) . . . . ? C5 O2 C1 C2 2.53(19) . . . . ? O1 C1 C2 C3 140.31(15) . . . . ? O2 C1 C2 C3 -39.31(17) . . . . ? O1 C1 C2 C17 -101.12(16) . . . . ? O2 C1 C2 C17 79.26(15) . . . . ? O1 C1 C2 C10 16.78(19) . . . . ? O2 C1 C2 C10 -162.84(12) . . . . ? C1 C2 C3 C4 52.98(15) . . . . ? C17 C2 C3 C4 -65.31(14) . . . . ? C10 C2 C3 C4 173.64(11) . . . . ? C2 C3 C4 C5 -34.11(17) . . . . ? C2 C3 C4 C9 144.50(14) . . . . ? C9 C4 C5 C6 0.3(2) . . . . ? C3 C4 C5 C6 179.05(14) . . . . ? C9 C4 C5 O2 178.29(12) . . . . ? C3 C4 C5 O2 -3.0(2) . . . . ? C1 O2 C5 C6 -161.18(14) . . . . ? C1 O2 C5 C4 20.8(2) . . . . ? C4 C5 C6 C7 -0.6(2) . . . . ? O2 C5 C6 C7 -178.62(14) . . . . ? C5 C6 C7 C8 0.4(3) . . . . ? C6 C7 C8 C9 0.0(3) . . . . ? C7 C8 C9 C4 -0.3(2) . . . . ? C5 C4 C9 C8 0.1(2) . . . . ? C3 C4 C9 C8 -178.53(14) . . . . ? C1 C2 C10 C11 170.89(12) . . . . ? C3 C2 C10 C11 49.66(17) . . . . ? C17 C2 C10 C11 -71.44(15) . . . . ? C2 C10 C11 C12 -87.80(17) . . . . ? C2 C10 C11 C16 94.15(17) . . . . ? C16 C11 C12 C13 -0.6(2) . . . . ? C10 C11 C12 C13 -178.75(15) . . . . ? C11 C12 C13 C14 0.6(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C13 C14 C15 C16 0.0(3) . . . . ? C14 C15 C16 C11 -0.1(3) . . . . ? C12 C11 C16 C15 0.4(2) . . . . ? C10 C11 C16 C15 178.46(14) . . . . ? C18 O4 C17 O3 0.0(2) . . . . ? C18 O4 C17 C2 178.56(14) . . . . ? C1 C2 C17 O3 -156.64(15) . . . . ? C3 C2 C17 O3 -37.82(19) . . . . ? C10 C2 C17 O3 85.79(18) . . . . ? C1 C2 C17 O4 24.75(17) . . . . ? C3 C2 C17 O4 143.56(12) . . . . ? C10 C2 C17 O4 -92.82(14) . . . . ? C17 O4 C18 C19 170.5(2) . . . . ?