#------------------------------------------------------------------------------ #$Date: 2024-04-06 04:30:45 +0300 (Sat, 06 Apr 2024) $ #$Revision: 291134 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/83/7248392.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_7248392 loop_ _publ_author_name 'Zhang, Xiao-Fang' 'Du, Jiao-Xian' 'Teng, Si-Qiong' 'Liu, Hui' 'He, Juan' 'Feng, Tao' 'Liu, Ji-Kai' _publ_section_title ; Carpesabrolide A, a novel meroterpenoid with anti-inflammatory activity from Carpesium abrotanoides ; _journal_issue 16 _journal_name_full 'RSC Advances' _journal_page_first 11002 _journal_page_last 11006 _journal_paper_doi 10.1039/D4RA00292J _journal_volume 14 _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_moiety 'C20 H22 O7' _chemical_formula_sum 'C20 H22 O7' _chemical_formula_weight 374.37 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_update_record ; 2023-12-04 deposited with the CCDC. 2024-03-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8989(3) _cell_length_b 11.3680(3) _cell_length_c 15.8912(5) _cell_measurement_reflns_used 9908 _cell_measurement_temperature 150.(2) _cell_measurement_theta_max 69.9806 _cell_measurement_theta_min 4.7829 _cell_volume 1788.25(9) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service vV6.2.15' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 882)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 150.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_unetI/netI 0.0386 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 16042 _diffrn_reflns_theta_full 70.04 _diffrn_reflns_theta_max 70.04 _diffrn_reflns_theta_min 4.78 _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.140 _refine_diff_density_max 0.183 _refine_diff_density_min -0.184 _refine_ls_abs_structure_details ; Flack x determined using 1356 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.08(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 247 _refine_ls_number_reflns 3367 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0295 _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^)+(0.0332P)^2^+0.2966P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.0731 _reflns_number_gt 3257 _reflns_number_total 3367 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ra00292j2.cif _cod_data_source_block lzca72 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 7248392 _shelx_res_file ; TITL lzca72_0m_a.res in P2(1)2(1)2(1) lzca72_0m.res created by SHELXL-2017/1 at 16:29:37 on 21-May-2023 CELL 1.54178 9.8989 11.3680 15.8912 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0003 0.0005 0.000 0.000 0.000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H O UNIT 80 88 28 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -123.150 SIZE 0.140 0.200 0.360 ACTA EQIV $1 -x+2, y-1/2, -z+3/2 HTAB C1 O3_$1 EQIV $2 x+1/2, -y+1/2, -z+1 HTAB C4 O4_$2 EQIV $3 x-1/2, -y+1/2, -z+1 HTAB C8 O5_$3 EQIV $4 x+1/2, -y+3/2, -z+1 HTAB C12 O2_$4 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.033200 0.296600 FVAR 0.94596 O1 3 0.890517 0.228478 0.693311 11.00000 0.02709 0.02087 = 0.03928 0.00226 -0.00993 0.00408 O2 3 0.016794 0.678116 0.409661 11.00000 0.02107 0.04426 = 0.03926 0.00040 -0.00459 0.01017 O3 3 0.937294 0.417403 0.716606 11.00000 0.04009 0.02431 = 0.07292 -0.00498 -0.03101 0.00366 O4 3 0.506225 0.344389 0.505721 11.00000 0.01594 0.02110 = 0.02971 -0.00444 -0.00233 0.00101 O5 3 0.591023 0.163594 0.518752 11.00000 0.02845 0.02242 = 0.06580 -0.01023 -0.01078 0.00292 O6 3 0.454336 0.418552 0.665617 11.00000 0.02435 0.02521 = 0.02615 0.00287 0.00717 0.00076 O7 3 0.143363 0.658862 0.525177 11.00000 0.01812 0.03113 = 0.02998 -0.00138 0.00122 0.00783 C1 1 1.014090 0.198342 0.736771 11.00000 0.03356 0.02667 = 0.04667 0.00333 -0.01291 0.00826 AFIX 137 H2 2 1.091310 0.231732 0.706460 11.00000 -1.50000 H3 2 1.023234 0.112575 0.739284 11.00000 -1.50000 H1 2 1.011480 0.230292 0.794025 11.00000 -1.50000 AFIX 0 C2 1 0.864920 0.343405 0.688154 11.00000 0.02511 0.02149 = 0.02552 0.00141 -0.00383 0.00422 C3 1 0.730608 0.365449 0.645611 11.00000 0.01917 0.02255 = 0.02456 0.00217 0.00003 -0.00007 AFIX 13 H4 2 0.659333 0.316998 0.673672 11.00000 -1.20000 AFIX 0 C4 1 0.732388 0.336746 0.548958 11.00000 0.01657 0.02249 = 0.02732 -0.00448 -0.00138 0.00267 AFIX 13 H5 2 0.818256 0.298344 0.530405 11.00000 -1.20000 AFIX 0 C5 1 0.709567 0.458006 0.507587 11.00000 0.01367 0.02704 = 0.02176 -0.00099 0.00067 0.00151 C6 1 0.552857 0.464498 0.519829 11.00000 0.01509 0.02031 = 0.02134 -0.00083 0.00078 -0.00010 C7 1 0.479305 0.543338 0.458205 11.00000 0.01617 0.02539 = 0.01814 0.00006 -0.00003 0.00248 AFIX 23 H16 2 0.497582 0.515434 0.400299 11.00000 -1.20000 H17 2 0.515658 0.624176 0.463122 11.00000 -1.20000 AFIX 0 C8 1 0.326953 0.546878 0.472078 11.00000 0.01536 0.02087 = 0.02140 0.00009 -0.00021 -0.00039 AFIX 13 H15 2 0.295143 0.465363 0.484997 11.00000 -1.20000 AFIX 0 C9 1 0.242727 0.595058 0.401704 11.00000 0.01573 0.02097 = 0.02767 -0.00138 -0.00269 -0.00106 C10 1 0.120918 0.647615 0.441570 11.00000 0.02086 0.02080 = 0.03169 0.00159 -0.00019 0.00054 C11 1 0.607767 0.267718 0.523944 11.00000 0.01904 0.02353 = 0.03185 -0.00556 -0.00140 0.00363 C12 1 0.284790 0.627388 0.543984 11.00000 0.01584 0.02703 = 0.02486 -0.00198 -0.00061 0.00345 AFIX 13 H6 2 0.341907 0.699941 0.543477 11.00000 -1.20000 AFIX 0 C13 1 0.287025 0.573525 0.630426 11.00000 0.02355 0.04577 = 0.02356 0.00025 0.00473 0.00802 AFIX 23 H7 2 0.232988 0.500267 0.629137 11.00000 -1.20000 H8 2 0.242069 0.628367 0.669894 11.00000 -1.20000 AFIX 0 C14 1 0.427164 0.544418 0.665129 11.00000 0.02541 0.02427 = 0.02078 0.00081 0.00334 0.00443 C15 1 0.458925 0.608536 0.746146 11.00000 0.03169 0.03519 = 0.02214 -0.00472 0.00258 0.00562 AFIX 137 H9 2 0.379573 0.606962 0.783004 11.00000 -1.50000 H10 2 0.482864 0.690307 0.733537 11.00000 -1.50000 H11 2 0.534918 0.569883 0.774391 11.00000 -1.50000 AFIX 0 C16 1 0.541273 0.492505 0.616252 11.00000 0.02067 0.01963 = 0.01874 0.00091 0.00098 0.00089 C17 1 0.688079 0.495040 0.646922 11.00000 0.02165 0.02133 = 0.02047 -0.00127 -0.00333 0.00229 AFIX 13 H12 2 0.703222 0.536778 0.701507 11.00000 -1.20000 AFIX 0 C18 1 0.762904 0.546582 0.571425 11.00000 0.01846 0.02214 = 0.02753 0.00243 -0.00352 -0.00273 AFIX 23 H14 2 0.734615 0.628166 0.558602 11.00000 -1.20000 H13 2 0.862284 0.542755 0.577859 11.00000 -1.20000 AFIX 0 C19 1 0.762439 0.467330 0.418306 11.00000 0.02024 0.04982 = 0.02328 0.00068 0.00309 0.00107 AFIX 137 H19 2 0.742593 0.545807 0.395975 11.00000 -1.50000 H18 2 0.718576 0.407766 0.383079 11.00000 -1.50000 H20 2 0.860328 0.454446 0.418146 11.00000 -1.50000 AFIX 0 C20 1 0.262837 0.599087 0.319593 11.00000 0.02240 0.03667 = 0.02704 -0.00166 -0.00596 0.00114 AFIX 93 H21 2 0.198478 0.636360 0.284158 11.00000 -1.20000 H22 2 0.341661 0.564711 0.295966 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM lzca72_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0295 for 3257 Fo > 4sig(Fo) and 0.0310 for all 3367 data REM 247 parameters refined using 0 restraints END WGHT 0.0331 0.2988 REM Instructions for potential hydrogen bonds HTAB C1 O3_$1 HTAB C4 O4_$2 HTAB C8 O5_$3 HTAB C12 O2_$4 REM Highest difference peak 0.183, deepest hole -0.184, 1-sigma level 0.040 Q1 1 0.7354 0.3476 0.5992 11.00000 0.05 0.18 Q2 1 0.7274 0.3987 0.5240 11.00000 0.05 0.16 Q3 1 0.5413 0.4805 0.5662 11.00000 0.05 0.15 Q4 1 0.6760 0.3038 0.5364 11.00000 0.05 0.15 Q5 1 0.7310 0.4603 0.4630 11.00000 0.05 0.14 ; _shelx_res_checksum 38889 _shelx_hkl_file ; 1 0 0 0.80 0.30 1 0 0 0.10 0.50 -1 0 0 -1.50 1.60 -1 0 0 0.70 0.40 2 0 0 48.90 3.10 -2 0 0 45.70 3.40 -3 0 0 0.80 0.80 3 0 0 1.40 0.80 -3 0 0 0.40 4.00 -4 0 0 9251.07 467.15 5 0 0 0.50 1.40 -5 0 0 -2.30 6.40 6 0 0 708.23 36.40 -6 0 0 633.04 47.50 -7 0 0 1.80 1.40 -7 0 0 -3.80 13.60 7 0 0 1.10 3.70 7 0 0 2.80 2.20 -7 0 0 0.60 2.00 8 0 0 973.60 51.69 -8 0 0 977.60 52.59 -8 0 0 1039.20 55.49 -9 0 0 -2.60 2.80 -9 0 0 -6.00 25.30 9 0 0 -3.90 1.60 -9 0 0 0.00 1.10 -10 0 0 44.80 3.20 10 0 0 42.80 4.10 -10 0 0 45.80 6.20 11 0 0 -1.40 1.20 -11 0 0 3.90 3.50 -12 0 0 24.10 3.20 -1 -1 0 2.60 0.70 -1 1 0 2.80 0.70 -1 1 0 4.00 2.40 2 1 0 99.09 5.60 -2 1 0 105.29 10.70 -2 1 0 91.69 6.10 2 -1 0 105.29 5.90 -2 -1 0 95.99 7.40 3 1 0 1545.45 75.69 -3 -1 0 1451.15 79.09 -3 1 0 1381.06 76.59 -3 1 0 1582.74 83.09 3 -1 0 1588.94 76.19 -4 1 0 138.39 15.80 4 -1 0 128.59 8.10 -4 -1 0 113.79 12.20 4 1 0 124.89 7.70 -4 1 0 128.39 8.80 -5 1 0 290.37 18.30 -5 -1 0 263.97 23.10 -5 1 0 328.97 27.70 5 1 0 284.07 16.70 5 -1 0 332.37 17.40 6 -1 0 1569.14 79.89 -6 1 0 1603.44 94.59 -6 -1 0 1470.95 88.49 6 1 0 1561.14 79.39 7 1 0 7.30 4.30 -7 1 0 20.10 15.70 -7 -1 0 6.70 2.00 -7 -1 0 5.10 3.00 -7 -1 0 8.20 1.70 -7 1 0 3.20 3.00 -7 1 0 2.90 1.60 7 -1 0 7.60 4.00 -7 -1 0 2.80 2.60 7 -1 0 2.40 1.90 -7 -1 0 -0.10 11.60 8 1 0 659.23 34.60 -8 -1 0 728.23 38.90 -8 1 0 708.73 34.50 -8 -1 0 609.94 35.40 -8 1 0 487.05 63.09 -8 1 0 667.03 37.90 -8 -1 0 591.14 34.10 9 1 0 1.40 2.00 9 -1 0 0.20 1.50 -9 1 0 26.00 29.80 -9 1 0 0.90 2.80 -9 -1 0 2.50 1.10 -9 1 0 2.40 1.20 -9 -1 0 -3.50 2.30 -10 1 0 3.90 1.10 -10 1 0 3.40 2.80 10 1 0 2.60 1.90 -10 -1 0 4.60 2.70 10 -1 0 2.30 1.30 -11 -1 0 8.70 3.70 11 1 0 6.10 1.80 -11 1 0 8.30 3.10 11 -1 0 13.50 2.00 -12 -1 0 0.00 1.40 12 -1 0 1.20 0.90 0 -2 0 6566.94 328.67 -1 2 0 567.64 29.90 -1 -2 0 574.14 29.80 -1 2 0 581.44 34.70 1 -2 0 602.24 29.90 2 -2 0 3075.39 154.48 -2 2 0 3180.68 154.78 -2 2 0 3009.80 160.78 3 -2 0 695.53 38.50 -3 -2 0 730.23 39.10 3 2 0 742.93 38.00 -3 2 0 830.72 47.80 -4 2 0 5578.34 270.57 4 -2 0 5201.78 258.67 -4 -2 0 4911.21 261.77 4 2 0 5036.70 257.77 -5 -2 0 807.32 47.50 5 -2 0 884.91 44.30 -5 2 0 823.52 45.50 5 2 0 785.72 43.20 -5 2 0 888.61 57.59 -6 2 0 282.27 19.20 -6 -2 0 292.67 18.80 -6 2 0 283.67 16.40 -6 2 0 325.57 33.60 6 -2 0 297.57 17.70 -6 -2 0 304.57 19.60 -6 -2 0 248.18 21.80 6 2 0 282.57 16.80 7 -2 0 1051.49 58.09 -7 2 0 1090.79 56.49 -7 2 0 1111.89 59.09 -7 -2 0 1176.18 60.29 -7 -2 0 970.30 59.39 -7 -2 0 1091.99 57.09 -7 2 0 1187.78 79.99 7 2 0 1157.98 57.49 -7 -2 0 1057.69 59.39 7 -2 0 1069.29 56.39 -8 -2 0 1483.45 76.29 -8 -2 0 1331.67 75.29 -8 2 0 1393.26 74.99 -8 2 0 1347.87 71.89 -8 -2 0 1386.66 72.29 8 -2 0 1414.36 71.89 -8 2 0 1495.75 100.19 9 -2 0 300.37 17.50 -9 2 0 311.07 17.50 -9 -2 0 325.77 21.30 -9 2 0 298.87 20.40 -9 2 0 265.57 49.50 -10 2 0 512.25 28.30 -10 2 0 558.14 31.50 10 -2 0 576.34 28.90 -10 -2 0 504.95 32.00 -11 -2 0 48.00 7.30 11 -2 0 49.60 3.70 -11 2 0 44.20 3.00 -11 2 0 36.90 5.30 0 -3 0 2.90 4.70 0 3 0 3.70 1.00 1 3 0 4268.67 215.78 -1 3 0 4083.89 216.28 -1 -3 0 4392.76 217.58 1 -3 0 4603.74 216.58 2 -3 0 487.75 25.00 -2 3 0 439.36 25.10 -2 3 0 477.65 33.00 3 -3 0 728.73 39.00 -3 3 0 778.22 49.30 -3 3 0 735.73 39.50 4 3 0 1213.68 65.19 4 -3 0 1274.67 66.19 -4 3 0 1333.47 79.19 -4 3 0 1330.77 67.19 -5 3 0 59.99 16.00 -5 3 0 66.09 7.10 5 -3 0 77.89 6.60 5 3 0 74.69 5.60 -6 -3 0 530.35 33.40 6 3 0 546.45 30.50 -6 3 0 593.54 51.59 -6 3 0 539.35 30.80 6 -3 0 599.74 34.40 -6 -3 0 597.84 33.40 -7 3 0 3.20 3.80 -7 -3 0 5.10 1.80 -7 -3 0 3.10 3.20 -7 -3 0 -2.30 4.70 7 -3 0 3.40 1.40 -7 -3 0 0.90 2.80 -7 3 0 -9.40 21.50 7 -3 0 5.70 4.30 -7 3 0 2.80 3.60 -7 3 0 5.80 1.90 -8 -3 0 175.78 14.30 -8 -3 0 194.28 14.90 -8 3 0 152.78 13.60 8 -3 0 196.18 11.50 -8 3 0 181.78 45.20 -8 3 0 185.18 11.70 -8 -3 0 188.98 12.10 -9 -3 0 1.40 1.40 -9 3 0 -45.40 42.80 -9 3 0 -1.10 3.30 9 -3 0 -0.20 1.20 -9 -3 0 3.30 2.90 -9 3 0 1.10 1.20 10 -3 0 75.19 5.50 -10 -3 0 78.89 8.10 -10 3 0 75.59 7.90 -10 3 0 64.29 5.20 11 -3 0 30.50 2.70 -11 3 0 27.60 2.40 -11 -3 0 25.20 3.90 0 -4 0 2501.65 135.99 0 4 0 2686.73 130.29 -1 4 0 5860.91 307.17 -1 -4 0 6068.59 300.77 -1 4 0 5927.01 297.87 1 4 0 6033.20 297.27 2 4 0 182.58 10.60 -2 4 0 193.58 11.80 2 -4 0 187.08 11.70 -2 4 0 201.98 21.00 -3 4 0 236.38 14.80 3 -4 0 239.48 14.60 -3 4 0 249.18 28.60 -4 4 0 701.93 40.10 4 -4 0 769.62 39.80 4 4 0 687.43 38.60 -4 4 0 823.72 56.69 -5 4 0 684.03 43.00 5 4 0 796.52 40.90 -5 4 0 821.22 60.39 5 -4 0 841.32 42.80 5 -4 0 792.32 40.70 -5 -4 0 770.32 42.40 -6 4 0 37.90 25.10 -6 4 0 23.30 5.40 -6 4 0 22.90 3.60 6 -4 0 20.10 4.10 -6 -4 0 32.00 5.50 6 -4 0 25.20 4.80 6 -4 0 20.70 3.00 -6 -4 0 26.60 4.30 -6 -4 0 26.60 5.60 -6 4 0 19.60 2.70 6 4 0 32.90 5.00 -7 -4 0 608.74 31.60 -7 4 0 551.34 61.99 -7 -4 0 527.65 32.40 -7 -4 0 563.64 36.10 7 -4 0 526.75 30.70 -7 4 0 493.25 33.50 -7 -4 0 584.44 33.10 -7 4 0 533.75 31.60 7 -4 0 489.25 32.10 -8 -4 0 527.95 27.90 8 -4 0 473.65 28.60 -8 4 0 503.85 27.30 -8 -4 0 484.95 30.40 8 -4 0 503.55 26.80 -8 4 0 494.25 68.69 -8 4 0 445.16 28.90 -8 -4 0 502.95 30.30 9 -4 0 238.68 14.80 -9 4 0 306.17 90.89 -9 -4 0 254.87 15.50 -9 4 0 251.17 17.20 -9 4 0 251.47 15.30 -9 -4 0 261.47 18.50 -9 -4 0 286.97 18.60 10 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47.20 3.70 6 -2 -16 50.59 3.40 0 3 16 5.20 2.20 0 -3 -16 10.60 1.90 0 -3 16 5.40 1.90 0 -3 16 8.00 3.00 0 3 -16 6.80 1.80 1 3 -16 0.20 1.00 1 -3 16 1.60 1.40 -1 -3 -16 -3.70 3.10 -1 3 16 1.60 1.70 1 -3 16 -3.70 2.40 -1 -3 16 1.00 1.30 -1 3 -16 1.20 1.10 1 -3 -16 1.30 1.10 1 3 16 0.20 2.70 -1 -3 16 0.90 2.20 2 -3 16 82.39 6.50 2 3 -16 76.09 5.60 -2 3 16 84.89 6.30 -2 -3 -16 77.59 8.90 2 -3 16 74.39 8.00 -2 3 -16 70.29 5.50 -2 -3 16 64.59 5.70 2 3 16 76.59 7.60 2 -3 -16 81.49 5.30 -2 -3 16 69.79 8.20 -3 -3 -16 80.39 8.70 3 -3 16 78.69 8.60 3 -3 16 91.89 7.00 -3 3 16 96.29 6.50 3 3 -16 88.39 6.00 3 -3 -16 84.59 5.60 -3 -3 16 76.19 8.20 -3 -3 16 81.99 6.10 -3 3 -16 79.79 5.90 -4 -3 -16 14.40 5.10 -4 3 16 25.10 3.70 4 -3 16 18.40 3.00 -4 3 -16 19.80 2.50 -4 -3 16 17.00 3.80 -4 -3 16 15.00 2.50 -5 3 16 26.60 2.80 5 3 -16 29.50 2.80 -5 3 16 41.40 6.00 5 -3 16 18.00 3.80 5 -3 -16 28.10 2.40 -5 -3 16 36.90 4.90 -5 -3 16 29.50 2.50 -6 3 16 57.59 4.00 6 -3 16 51.89 4.40 6 3 -16 54.39 3.80 6 -3 -16 52.09 3.50 -6 -3 16 55.79 5.40 0 4 -16 18.60 2.70 0 4 16 20.40 4.90 0 -4 16 22.20 3.00 0 -4 16 16.60 4.00 0 -4 -16 19.70 5.10 1 4 -16 40.00 3.90 -1 4 16 46.30 4.70 1 -4 16 43.30 6.30 -1 -4 -16 33.40 6.40 1 -4 16 40.90 4.20 1 -4 -16 51.89 3.70 -1 -4 16 42.00 6.10 -1 4 -16 35.70 3.70 1 4 16 35.10 5.10 -1 -4 16 38.50 3.90 2 -4 16 48.70 7.20 2 -4 16 53.29 5.10 -2 4 16 61.69 5.20 -2 -4 -16 56.69 7.40 2 4 -16 64.89 4.80 -2 4 -16 54.09 4.60 -2 -4 16 54.39 4.60 2 -4 -16 61.99 4.90 -2 -4 16 54.89 6.70 -3 4 16 43.10 4.40 -3 -4 -16 34.50 5.70 3 4 -16 35.80 3.40 3 -4 16 33.30 3.80 -3 4 -16 30.00 3.30 -3 -4 16 29.20 3.70 3 -4 -16 35.60 2.90 -3 -4 16 31.70 5.50 -4 4 16 20.60 5.60 4 -4 16 19.90 2.50 4 4 -16 17.10 2.40 -4 4 16 23.20 2.70 -4 -4 -16 18.10 3.80 4 -4 16 22.70 3.00 -4 -4 16 22.50 2.30 4 -4 -16 23.00 2.20 -4 -4 16 19.80 3.90 -4 4 -16 27.40 2.70 5 4 -16 63.79 4.40 -5 4 16 63.29 4.60 5 -4 16 63.29 4.10 5 -4 16 62.69 5.10 5 -4 -16 66.79 4.10 -5 -4 16 58.29 6.20 0 -5 -16 1.70 2.40 0 -5 16 2.70 1.20 0 5 -16 1.20 1.20 0 5 16 7.50 3.60 -1 5 16 35.20 4.50 -1 -5 -16 32.00 5.80 1 -5 16 34.80 5.70 1 5 -16 34.40 3.30 1 -5 16 31.80 3.50 -1 5 -16 32.50 3.30 -1 -5 16 32.10 5.50 -1 -5 16 24.60 3.20 1 -5 -16 32.60 6.00 -2 -5 -16 73.29 7.60 2 -5 16 56.69 5.00 2 5 -16 74.49 6.50 -2 5 16 68.99 5.40 -2 -5 16 59.09 4.70 -2 5 -16 57.79 4.70 -2 -5 16 52.09 7.40 -3 5 16 31.50 3.30 -3 -5 -16 20.30 3.90 3 5 -16 28.10 2.80 3 -5 16 25.00 3.20 -3 -5 16 27.70 4.60 -3 -5 16 26.50 2.50 3 -5 -16 19.70 3.10 -3 5 -16 24.30 2.70 4 -5 16 39.80 3.80 -4 5 16 53.89 6.70 4 5 -16 43.20 3.50 -4 5 -16 40.70 4.10 4 -5 -16 43.80 3.10 -4 -5 16 39.30 5.20 5 5 -16 22.40 2.60 -5 5 16 35.20 3.60 -5 -5 16 33.10 4.20 0 -6 16 9.10 1.70 0 -6 16 12.70 3.00 0 6 -16 9.70 1.70 0 -6 -16 4.60 2.70 -1 -6 -16 31.30 5.30 1 6 -16 37.50 3.40 -1 6 16 30.20 4.40 1 -6 16 31.60 3.30 -1 -6 16 36.70 3.10 -1 6 -16 35.30 3.30 -1 -6 16 30.10 5.00 1 -6 -16 34.60 5.40 2 6 -16 115.69 7.10 2 -6 16 100.19 7.20 -2 -6 -16 119.69 9.40 2 -6 -16 107.19 9.70 -2 -6 16 115.59 9.10 -2 -6 16 114.79 6.40 -2 6 -16 104.69 7.10 -3 6 16 71.89 5.50 3 6 -16 80.99 5.10 -3 -6 -16 91.99 9.40 3 -6 16 70.89 5.30 3 -6 -16 73.99 7.30 -3 6 -16 66.89 4.90 -3 -6 16 68.19 6.60 4 6 -16 -0.60 1.10 -4 6 16 2.30 1.40 4 -6 16 3.00 1.20 -4 -6 -16 1.50 1.90 -4 -6 16 2.70 2.20 4 -6 -16 1.20 1.90 -4 6 -16 0.90 3.30 -4 6 -16 3.50 1.20 0 -7 16 1.60 2.80 0 -7 16 3.10 1.10 0 7 -16 5.80 1.30 0 -7 -16 2.50 2.20 1 -7 16 44.20 4.40 1 7 -16 46.80 3.80 -1 -7 -16 49.40 5.50 -1 7 -16 49.70 3.80 1 -7 -16 44.30 5.40 2 7 -16 13.90 2.70 -2 -7 -16 14.30 2.90 2 -7 16 18.30 2.10 2 -7 -16 21.40 4.20 -2 -7 16 12.70 2.90 -2 7 -16 19.10 2.90 -3 -7 -16 43.20 4.70 3 -7 16 48.30 3.90 -3 -7 16 50.19 5.80 -3 7 -16 50.09 3.90 0 0 17 1.70 1.30 0 0 -17 0.70 1.10 -1 0 17 3.90 1.90 1 0 17 4.30 1.80 1 0 -17 2.90 1.30 -1 0 -17 5.90 1.50 -2 0 17 19.30 2.90 2 0 17 16.10 3.00 2 0 -17 20.00 2.30 3 0 -17 117.39 7.50 -3 0 17 111.69 7.90 -3 0 17 124.89 10.30 3 0 17 132.19 8.80 -4 0 17 3.40 1.10 -4 0 17 2.70 2.20 4 0 17 2.30 2.50 5 0 -17 40.60 3.10 -5 0 -17 44.50 5.20 -5 0 17 43.30 3.40 0 -1 -17 16.20 2.40 0 1 17 13.00 2.40 0 1 -17 12.10 2.10 0 -1 17 14.70 2.90 1 -1 17 85.09 6.40 -1 -1 -17 82.89 5.70 1 1 -17 66.69 5.30 -1 -1 -17 51.09 8.90 -1 1 17 76.99 6.10 1 -1 -17 75.19 5.30 -1 1 -17 67.59 5.30 -1 -1 17 71.29 5.90 1 1 17 79.29 6.40 2 -1 17 104.29 7.70 2 1 -17 94.39 6.50 -2 1 17 107.99 7.30 -2 -1 -17 100.59 7.00 -2 -1 17 94.09 9.00 -2 -1 17 94.09 7.00 -2 1 -17 102.69 7.00 2 1 17 113.49 7.90 2 -1 -17 92.09 6.30 -3 1 17 322.47 21.90 3 1 -17 300.57 17.00 3 -1 17 316.97 18.20 -3 1 17 307.67 17.70 -3 1 -17 329.57 16.80 -3 -1 17 291.87 17.50 -3 -1 17 317.97 20.30 3 -1 -17 307.57 17.00 3 1 17 330.07 19.40 -4 1 17 60.89 6.20 4 -1 17 56.49 4.90 -4 1 17 46.60 4.10 4 1 -17 48.10 3.80 -4 -1 17 44.50 5.80 -4 -1 17 52.39 4.10 4 -1 -17 48.40 3.60 5 -1 17 11.10 2.80 -5 1 17 17.50 2.10 -5 1 17 19.80 3.60 5 1 -17 19.10 2.00 -5 -1 17 18.90 3.50 -5 -1 17 18.40 2.40 5 -1 -17 15.90 1.80 0 -2 17 96.09 8.90 0 -2 -17 97.59 10.10 0 2 -17 91.19 6.40 0 -2 17 92.19 7.10 0 2 17 100.59 7.40 -1 -2 -17 41.90 6.90 -1 -2 -17 27.80 3.30 1 -2 17 37.00 4.00 1 -2 17 36.40 5.50 1 2 -17 29.30 3.00 -1 2 17 33.30 3.90 -1 -2 17 30.30 5.20 -1 2 -17 28.00 3.10 1 2 17 38.50 4.40 1 -2 -17 32.40 3.10 -1 -2 17 28.30 3.50 -2 -2 -17 15.80 4.50 2 2 -17 14.60 2.10 2 -2 17 13.30 2.50 2 -2 17 14.20 3.40 -2 2 17 13.00 2.30 -2 -2 17 14.60 2.40 -2 -2 17 11.40 3.20 2 2 17 12.60 3.10 2 -2 -17 15.90 2.10 -2 2 -17 16.80 2.40 -3 2 17 13.10 2.30 3 -2 17 14.10 2.60 3 -2 17 11.60 3.70 -3 2 -17 14.30 2.20 3 -2 -17 14.80 1.90 3 2 17 8.10 3.90 -3 -2 17 11.90 4.80 4 2 -17 49.90 3.80 4 -2 17 34.20 6.20 -4 2 17 52.19 4.20 -4 2 17 56.69 6.00 -4 -2 17 53.19 4.00 -4 -2 17 56.79 6.20 4 -2 -17 47.90 3.50 5 2 -17 29.70 2.60 -5 2 17 26.90 3.80 -5 2 17 32.80 5.20 -5 -2 17 35.00 2.60 5 -2 -17 32.30 2.50 -5 -2 17 35.40 4.70 0 -3 17 3.60 2.40 0 -3 -17 3.50 3.30 0 3 -17 1.00 1.00 0 3 17 1.30 2.00 0 -3 17 -0.10 1.10 -1 -3 -17 72.99 7.70 -1 3 17 64.49 5.40 1 -3 17 54.59 6.80 1 -3 17 55.39 5.10 1 3 -17 59.39 4.70 -1 -3 17 55.89 4.90 -1 3 -17 57.29 4.70 1 -3 -17 63.19 4.40 1 3 17 67.79 6.20 -1 -3 17 61.99 6.90 2 3 -17 19.90 2.50 -2 -3 -17 22.00 4.40 -2 3 17 20.00 2.90 2 -3 17 13.20 3.40 2 -3 17 16.00 3.60 -2 -3 17 16.60 3.90 2 -3 -17 22.70 2.40 -2 3 -17 16.30 3.10 -2 -3 17 15.90 2.40 3 3 -17 4.90 1.30 -3 -3 -17 2.70 4.20 3 -3 17 5.50 1.60 -3 3 17 5.00 1.40 -3 3 -17 7.50 1.40 3 -3 -17 6.30 1.20 -3 -3 17 3.50 1.30 4 -3 17 65.69 5.90 4 3 -17 66.39 4.60 -4 3 17 66.79 4.90 -4 3 17 71.29 7.50 -4 -3 17 66.39 4.40 -4 -3 17 58.89 6.40 -4 3 -17 64.39 4.30 5 3 -17 171.68 9.30 5 -3 17 157.28 8.70 -5 3 17 156.28 9.20 5 -3 17 135.19 9.30 -5 -3 17 193.48 14.90 5 -3 -17 156.48 8.80 0 4 17 54.09 5.80 0 -4 17 50.99 6.30 0 -4 -17 61.89 7.30 -1 -4 -17 6.10 3.10 -1 4 17 10.80 2.10 1 -4 17 6.50 1.90 1 4 -17 9.00 2.10 1 -4 17 4.40 2.70 -1 4 -17 6.40 1.80 1 4 17 7.80 3.40 1 -4 -17 0.90 2.50 -1 -4 17 9.20 2.10 -1 -4 17 8.20 2.70 2 4 -17 4.40 1.20 -2 4 17 7.00 1.70 2 -4 17 4.60 1.40 2 -4 17 -0.10 4.20 -2 -4 -17 5.60 2.70 -2 -4 17 3.20 1.20 -2 4 -17 3.10 1.20 -2 -4 17 0.50 2.20 2 -4 -17 4.10 1.70 -3 4 17 31.00 3.70 3 -4 17 34.00 3.30 -3 -4 -17 31.20 5.50 3 4 -17 28.50 2.90 3 -4 -17 31.60 2.80 -3 4 -17 30.90 2.80 -3 -4 17 26.50 4.50 -3 -4 17 29.50 3.70 4 -4 17 95.79 6.50 4 4 -17 109.29 6.10 -4 4 17 98.79 6.30 -4 4 17 100.49 9.80 -4 -4 17 84.39 8.60 4 -4 -17 95.89 5.50 -4 4 -17 87.59 5.60 0 5 -17 16.80 2.20 0 -5 17 17.50 2.30 0 5 17 7.40 3.50 0 -5 17 18.70 4.80 0 -5 -17 15.10 3.70 1 -5 17 6.60 3.60 -1 -5 -17 17.80 3.70 1 5 -17 11.40 1.90 1 -5 17 14.60 2.10 1 -5 -17 13.60 3.60 -1 -5 17 9.10 1.70 -1 -5 17 12.50 3.00 -1 5 -17 11.50 1.90 2 -5 17 25.90 3.10 -2 5 17 25.00 3.50 -2 -5 -17 35.80 4.90 2 5 -17 36.10 3.00 2 -5 -17 30.10 4.90 -2 -5 17 34.00 2.90 -2 5 -17 30.20 2.80 -2 -5 17 31.00 4.70 3 -5 17 49.00 4.60 -3 5 17 59.59 4.50 -3 -5 -17 46.80 5.30 3 5 -17 64.19 4.10 -3 5 -17 56.69 4.00 -3 -5 17 63.69 7.80 0 -6 17 11.70 2.80 0 -6 17 9.00 1.50 -1 -6 -17 10.70 3.30 1 -6 17 13.40 1.80 1 6 -17 12.90 1.90 -1 -6 17 6.70 3.00 -1 -6 17 14.70 1.70 -1 6 -17 10.10 2.40 1 -6 -17 16.10 4.40 2 -6 17 43.90 3.50 -2 -6 -17 53.69 5.90 -2 -6 17 49.90 7.60 -2 6 -17 43.30 3.40 2 -6 -17 50.49 5.50 0 0 18 119.19 7.90 0 0 -18 112.79 7.10 -1 0 -18 6.20 1.40 -1 0 18 2.10 1.30 1 0 18 6.00 2.00 1 0 -18 -6.40 4.00 1 0 -18 4.90 1.30 -2 0 18 126.99 10.10 -2 0 -18 126.69 7.60 2 0 18 137.59 8.80 2 0 -18 129.79 7.80 -2 0 18 131.19 8.30 3 0 -18 27.50 2.50 -3 0 18 33.80 4.60 3 0 18 28.20 4.00 -3 0 18 28.90 3.00 3 0 18 26.20 5.30 -4 0 18 41.00 3.30 -4 0 18 52.19 5.40 4 0 -18 42.70 3.20 0 -1 18 97.79 7.40 0 1 -18 105.69 6.80 0 1 18 114.79 7.70 0 -1 -18 117.69 6.70 0 -1 18 111.49 9.10 -1 -1 -18 1.10 2.70 1 -1 18 4.70 1.50 1 -1 18 4.30 2.40 -1 1 18 4.90 1.50 1 1 -18 5.20 1.30 1 -1 -18 6.20 1.30 -1 -1 18 6.90 1.60 1 1 18 5.40 1.80 -1 -1 18 4.50 2.20 -1 1 -18 4.80 1.30 2 -1 18 70.59 5.50 2 -1 18 71.39 7.30 2 1 -18 62.69 4.60 -2 1 18 70.39 5.20 -2 -1 18 69.99 5.20 -2 -1 18 64.39 6.80 2 1 18 70.59 5.70 2 -1 -18 69.79 4.60 -2 1 -18 70.29 4.50 -3 1 18 -0.60 1.80 3 1 -18 2.40 0.90 -3 1 18 -0.60 0.90 3 -1 18 -3.40 3.00 3 -1 18 -1.50 1.50 -3 -1 18 0.80 1.00 3 -1 -18 0.50 0.80 -3 -1 18 -1.10 1.70 3 1 18 -4.30 2.30 -4 1 18 68.89 4.80 -4 1 18 76.99 6.40 4 1 -18 68.49 4.50 4 -1 -18 68.99 4.40 -4 -1 18 67.49 4.60 -4 -1 18 76.59 6.60 0 -2 18 24.30 2.90 0 -2 18 26.10 4.40 0 -2 -18 18.50 5.60 0 2 -18 20.30 2.40 0 -2 -18 18.70 2.80 0 2 18 24.80 3.30 -1 2 18 44.00 4.10 1 -2 18 48.80 4.20 1 2 -18 43.50 3.60 1 -2 18 41.10 5.40 1 -2 -18 46.10 6.40 1 2 18 48.80 4.70 -1 -2 18 40.90 5.50 1 -2 -18 49.00 3.50 -1 2 -18 42.10 3.50 -1 -2 18 42.40 3.90 2 -2 18 149.88 9.40 2 2 -18 149.49 8.80 -2 2 18 160.88 9.40 2 -2 18 135.39 10.50 -2 -2 18 138.69 10.90 -2 2 -18 149.69 9.90 2 -2 -18 154.98 9.50 -2 -2 18 148.89 9.10 3 -2 18 3.50 1.50 3 2 -18 1.10 0.90 -3 2 18 1.70 1.50 -3 2 18 2.40 2.10 -3 -2 18 2.50 1.10 -3 -2 18 3.40 2.10 3 -2 -18 1.50 0.90 -4 2 18 82.69 5.50 4 -2 18 74.69 5.70 -4 2 18 97.19 6.80 4 2 -18 83.79 5.20 4 -2 -18 82.79 5.00 -4 -2 18 79.49 5.00 -4 -2 18 87.09 7.80 0 -3 18 83.79 7.60 0 -3 -18 108.19 10.90 0 -3 18 81.29 6.10 0 3 -18 89.69 5.90 0 3 18 96.39 6.80 1 -3 18 4.80 1.50 -1 3 18 7.30 1.90 1 3 -18 4.90 1.30 1 -3 18 8.70 2.60 1 3 18 3.20 2.50 -1 3 -18 6.60 1.30 -1 -3 18 6.50 1.40 -1 -3 18 8.60 2.50 1 -3 -18 5.90 3.00 2 -3 18 56.89 4.60 2 3 -18 52.29 4.10 -2 3 18 58.79 4.60 -2 -3 18 62.39 6.10 -2 3 -18 53.69 4.00 -2 -3 18 52.49 4.10 2 -3 -18 63.89 4.90 -3 3 18 5.70 3.00 3 -3 18 3.30 1.40 3 3 -18 3.60 0.90 -3 3 18 3.80 1.20 -3 3 -18 -0.30 1.20 -3 -3 18 3.60 1.10 3 -3 -18 1.40 1.10 -3 -3 18 3.30 2.00 0 -4 -18 19.60 3.80 0 -4 18 13.70 2.90 0 4 18 13.40 2.90 0 4 -18 17.50 2.10 0 -4 18 16.50 2.10 1 4 -18 8.20 1.60 -1 4 18 7.10 1.90 1 -4 18 3.60 2.70 1 -4 18 8.20 1.70 -1 -4 -18 9.80 4.20 1 -4 -18 5.50 2.80 -1 -4 18 6.40 2.50 2 4 -18 60.89 4.30 -2 4 18 59.19 4.70 -2 -4 -18 50.39 6.10 2 -4 18 63.99 4.60 2 -4 -18 65.69 6.50 -2 -4 18 59.89 4.40 -2 4 -18 65.29 4.20 -2 -4 18 65.39 6.00 0 -5 18 9.00 2.00 0 5 -18 7.20 1.30 0 -5 -18 7.10 2.50 0 -5 18 6.80 2.50 -1 -5 -18 1.20 2.10 1 -5 18 1.10 1.30 1 5 -18 -0.40 0.90 -1 5 -18 0.50 1.10 1 -5 -18 -2.80 2.80 -1 -5 18 0.40 0.90 -1 -5 18 2.00 2.00 0 0 19 -1.20 1.00 0 0 19 -1.40 1.80 0 0 -19 1.10 1.10 1 0 19 181.08 11.60 -1 0 19 168.88 10.40 -1 0 19 185.38 12.20 1 0 -19 175.88 10.50 2 0 -19 5.20 1.10 -2 0 19 3.50 1.90 -2 0 19 6.40 1.40 2 0 19 5.90 1.60 2 0 19 9.10 2.20 0 1 -19 2.20 1.10 0 -1 19 1.60 2.00 0 -1 19 3.50 1.30 -1 1 19 50.89 4.00 1 -1 19 44.50 6.80 -1 1 19 46.50 5.00 1 -1 19 47.70 4.00 1 1 -19 49.20 3.40 1 -1 -19 45.90 3.30 -1 1 -19 44.10 3.30 -1 -1 19 52.99 5.40 1 1 19 45.00 4.20 -1 -1 19 46.50 3.80 2 -1 19 15.60 2.50 2 1 -19 20.40 2.30 2 -1 19 16.00 3.60 -2 1 19 14.90 2.80 -2 1 19 18.20 3.10 2 1 19 20.60 3.60 2 -1 -19 22.20 1.90 2 1 19 8.80 3.00 -2 -1 19 17.60 2.10 -2 -1 19 13.30 2.70 0 2 19 0.60 1.40 0 -2 19 1.20 1.10 1 -2 19 68.59 5.90 1 2 -19 69.09 4.50 1 -2 19 66.09 4.90 -1 2 19 74.49 5.10 -1 2 -19 72.49 4.30 1 -2 -19 49.70 7.80 -1 -2 19 70.09 6.20 -1 -2 19 66.99 4.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 37799 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.89052(14) 0.22848(13) 0.69331(10) 0.0291(3) Uani d . . . 1 . . O O2 0.01679(14) 0.67812(15) 0.40966(10) 0.0349(4) Uani d . . . 1 . . O O3 0.93729(17) 0.41740(15) 0.71661(13) 0.0458(5) Uani d . . . 1 . . O O4 0.50622(12) 0.34439(12) 0.50572(8) 0.0222(3) Uani d . . . 1 . . O O5 0.59102(15) 0.16359(14) 0.51875(12) 0.0389(4) Uani d . . . 1 . . O O6 0.45434(14) 0.41855(13) 0.66562(8) 0.0252(3) Uani d . . . 1 . . O O7 0.14336(12) 0.65886(13) 0.52518(9) 0.0264(3) Uani d . . . 1 . . C C1 1.0141(2) 0.1983(2) 0.73677(16) 0.0356(5) Uani d . . . 1 . . H H2 1.09131 0.231732 0.70646 0.053 Uiso calc U . R 1 . . H H3 1.023234 0.112575 0.739284 0.053 Uiso calc U . R 1 . . H H1 1.01148 0.230292 0.794025 0.053 Uiso calc U . R 1 . . C C2 0.86492(19) 0.34340(18) 0.68815(12) 0.0240(4) Uani d . . . 1 . . C C3 0.73061(18) 0.36545(18) 0.64561(12) 0.0221(4) Uani d . . . 1 . . H H4 0.659333 0.316998 0.673672 0.027 Uiso calc U . R 1 . . C C4 0.73239(18) 0.33675(17) 0.54896(12) 0.0221(4) Uani d . . . 1 . . H H5 0.818256 0.298344 0.530405 0.027 Uiso calc U . R 1 . . C C5 0.70957(17) 0.45801(17) 0.50759(11) 0.0208(4) Uani d . . . 1 . . C C6 0.55286(17) 0.46450(16) 0.51983(11) 0.0189(4) Uani d . . . 1 . . C C7 0.47930(17) 0.54334(17) 0.45820(11) 0.0199(4) Uani d . . . 1 . . H H16 0.497582 0.515434 0.400299 0.024 Uiso calc U . R 1 . . H H17 0.515658 0.624176 0.463122 0.024 Uiso calc U . R 1 . . C C8 0.32695(17) 0.54688(17) 0.47208(11) 0.0192(4) Uani d . . . 1 . . H H15 0.295143 0.465363 0.484997 0.023 Uiso calc U . R 1 . . C C9 0.24273(17) 0.59506(16) 0.40170(12) 0.0215(4) Uani d . . . 1 . . C C10 0.12092(18) 0.64761(17) 0.44157(13) 0.0245(4) Uani d . . . 1 . . C C11 0.60777(19) 0.26772(18) 0.52394(13) 0.0248(4) Uani d . . . 1 . . C C12 0.28479(18) 0.62739(17) 0.54398(12) 0.0226(4) Uani d . . . 1 . . H H6 0.341907 0.699941 0.543477 0.027 Uiso calc U . R 1 . . C C13 0.2870(2) 0.5735(2) 0.63043(12) 0.0310(5) Uani d . . . 1 . . H H7 0.232988 0.500267 0.629137 0.037 Uiso calc U . R 1 . . H H8 0.242069 0.628367 0.669894 0.037 Uiso calc U . R 1 . . C C14 0.42716(19) 0.54442(18) 0.66513(11) 0.0235(4) Uani d . . . 1 . . C C15 0.4589(2) 0.6085(2) 0.74615(12) 0.0297(5) Uani d . . . 1 . . H H9 0.379573 0.606962 0.783004 0.045 Uiso calc U . R 1 . . H H10 0.482864 0.690307 0.733537 0.045 Uiso calc U . R 1 . . H H11 0.534918 0.569883 0.774391 0.045 Uiso calc U . R 1 . . C C16 0.54127(18) 0.49251(16) 0.61625(11) 0.0197(4) Uani d . . . 1 . . C C17 0.68808(19) 0.49504(17) 0.64692(12) 0.0212(4) Uani d . . . 1 . . H H12 0.703222 0.536778 0.701507 0.025 Uiso calc U . R 1 . . C C18 0.76290(18) 0.54658(17) 0.57143(12) 0.0227(4) Uani d . . . 1 . . H H14 0.734615 0.628166 0.558602 0.027 Uiso calc U . R 1 . . H H13 0.862284 0.542755 0.577859 0.027 Uiso calc U . R 1 . . C C19 0.7624(2) 0.4673(2) 0.41831(13) 0.0311(5) Uani d . . . 1 . . H H19 0.742593 0.545807 0.395975 0.047 Uiso calc U . R 1 . . H H18 0.718576 0.407766 0.383079 0.047 Uiso calc U . R 1 . . H H20 0.860328 0.454446 0.418146 0.047 Uiso calc U . R 1 . . C C20 0.2628(2) 0.59909(19) 0.31959(13) 0.0287(4) Uani d . . . 1 . . H H21 0.198478 0.63636 0.284158 0.034 Uiso calc U . R 1 . . H H22 0.341661 0.564711 0.295966 0.034 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0271(7) 0.0209(7) 0.0393(8) 0.0041(6) -0.0099(6) 0.0023(6) O2 0.0211(7) 0.0443(10) 0.0393(8) 0.0102(6) -0.0046(6) 0.0004(7) O3 0.0401(9) 0.0243(8) 0.0729(12) 0.0037(7) -0.0310(9) -0.0050(8) O4 0.0159(6) 0.0211(7) 0.0297(6) 0.0010(5) -0.0023(5) -0.0044(5) O5 0.0285(7) 0.0224(8) 0.0658(11) 0.0029(6) -0.0108(7) -0.0102(8) O6 0.0243(6) 0.0252(7) 0.0261(7) 0.0008(5) 0.0072(5) 0.0029(5) O7 0.0181(6) 0.0311(8) 0.0300(7) 0.0078(5) 0.0012(5) -0.0014(6) C1 0.0336(12) 0.0267(12) 0.0467(13) 0.0083(8) -0.0129(10) 0.0033(9) C2 0.0251(9) 0.0215(10) 0.0255(9) 0.0042(8) -0.0038(7) 0.0014(8) C3 0.0192(9) 0.0225(10) 0.0246(9) -0.0001(7) 0.0000(7) 0.0022(7) C4 0.0166(8) 0.0225(10) 0.0273(9) 0.0027(7) -0.0014(7) -0.0045(8) C5 0.0137(8) 0.0270(10) 0.0218(9) 0.0015(7) 0.0007(6) -0.0010(7) C6 0.0151(8) 0.0203(9) 0.0213(8) -0.0001(7) 0.0008(7) -0.0008(7) C7 0.0162(8) 0.0254(10) 0.0181(7) 0.0025(7) 0.0000(6) 0.0001(7) C8 0.0154(8) 0.0209(9) 0.0214(8) -0.0004(6) -0.0002(6) 0.0001(7) C9 0.0157(8) 0.0210(10) 0.0277(9) -0.0011(7) -0.0027(7) -0.0014(7) C10 0.0209(9) 0.0208(10) 0.0317(10) 0.0005(7) -0.0002(7) 0.0016(8) C11 0.0190(9) 0.0235(11) 0.0319(10) 0.0036(7) -0.0014(8) -0.0056(8) C12 0.0158(8) 0.0270(10) 0.0249(9) 0.0034(7) -0.0006(7) -0.0020(8) C13 0.0235(10) 0.0458(13) 0.0236(10) 0.0080(9) 0.0047(8) 0.0002(9) C14 0.0254(9) 0.0243(10) 0.0208(9) 0.0044(7) 0.0033(7) 0.0008(8) C15 0.0317(10) 0.0352(12) 0.0221(9) 0.0056(9) 0.0026(8) -0.0047(8) C16 0.0207(9) 0.0196(9) 0.0187(8) 0.0009(7) 0.0010(7) 0.0009(7) C17 0.0217(9) 0.0213(10) 0.0205(8) 0.0023(7) -0.0033(7) -0.0013(7) C18 0.0185(8) 0.0221(10) 0.0275(9) -0.0027(7) -0.0035(7) 0.0024(7) C19 0.0202(9) 0.0498(14) 0.0233(9) 0.0011(9) 0.0031(8) 0.0007(9) C20 0.0224(9) 0.0367(12) 0.0270(9) 0.0011(8) -0.0060(8) -0.0017(8) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 O1 C1 . . 114.98(16) ? C11 O4 C6 . . 109.44(13) ? C16 O6 C14 . . 62.13(11) ? C10 O7 C12 . . 109.38(14) ? O1 C1 H2 . . 109.5 ? O1 C1 H3 . . 109.5 ? H2 C1 H3 . . 109.5 ? O1 C1 H1 . . 109.5 ? H2 C1 H1 . . 109.5 ? H3 C1 H1 . . 109.5 ? O3 C2 O1 . . 123.58(17) ? O3 C2 C3 . . 125.45(19) ? O1 C2 C3 . . 110.91(16) ? C2 C3 C17 . . 113.25(16) ? C2 C3 C4 . . 113.14(15) ? C17 C3 C4 . . 102.48(15) ? C2 C3 H4 . . 109.2 ? C17 C3 H4 . . 109.2 ? C4 C3 H4 . . 109.2 ? C11 C4 C5 . . 103.39(14) ? C11 C4 C3 . . 110.80(16) ? C5 C4 C3 . . 103.26(15) ? C11 C4 H5 . . 112.9 ? C5 C4 H5 . . 112.9 ? C3 C4 H5 . . 112.9 ? C19 C5 C18 . . 117.21(16) ? C19 C5 C4 . . 114.23(16) ? C18 C5 C4 . . 104.82(14) ? C19 C5 C6 . . 117.08(15) ? C18 C5 C6 . . 103.27(14) ? C4 C5 C6 . . 97.71(14) ? O4 C6 C7 . . 107.61(14) ? O4 C6 C5 . . 104.50(14) ? C7 C6 C5 . . 115.10(15) ? O4 C6 C16 . . 108.47(14) ? C7 C6 C16 . . 118.45(15) ? C5 C6 C16 . . 101.73(14) ? C6 C7 C8 . . 113.44(15) ? C6 C7 H16 . . 108.9 ? C8 C7 H16 . . 108.9 ? C6 C7 H17 . . 108.9 ? C8 C7 H17 . . 108.9 ? H16 C7 H17 . . 107.7 ? C9 C8 C12 . . 100.83(14) ? C9 C8 C7 . . 116.88(15) ? C12 C8 C7 . . 113.30(15) ? C9 C8 H15 . . 108.5 ? C12 C8 H15 . . 108.5 ? C7 C8 H15 . . 108.5 ? C20 C9 C10 . . 121.94(17) ? C20 C9 C8 . . 131.77(17) ? C10 C9 C8 . . 106.26(16) ? O2 C10 O7 . . 121.92(18) ? O2 C10 C9 . . 129.23(18) ? O7 C10 C9 . . 108.85(16) ? O5 C11 O4 . . 121.04(17) ? O5 C11 C4 . . 129.97(18) ? O4 C11 C4 . . 108.99(16) ? O7 C12 C13 . . 107.32(15) ? O7 C12 C8 . . 104.71(14) ? C13 C12 C8 . . 115.90(17) ? O7 C12 H6 . . 109.6 ? C13 C12 H6 . . 109.6 ? C8 C12 H6 . . 109.6 ? C12 C13 C14 . . 115.52(16) ? C12 C13 H7 . . 108.4 ? C14 C13 H7 . . 108.4 ? C12 C13 H8 . . 108.4 ? C14 C13 H8 . . 108.4 ? H7 C13 H8 . . 107.5 ? O6 C14 C16 . . 58.29(11) ? O6 C14 C15 . . 115.51(16) ? C16 C14 C15 . . 118.44(17) ? O6 C14 C13 . . 112.47(17) ? C16 C14 C13 . . 125.77(16) ? C15 C14 C13 . . 113.04(17) ? C14 C15 H9 . . 109.5 ? C14 C15 H10 . . 109.5 ? H9 C15 H10 . . 109.5 ? C14 C15 H11 . . 109.5 ? H9 C15 H11 . . 109.5 ? H10 C15 H11 . . 109.5 ? O6 C16 C14 . . 59.58(12) ? O6 C16 C17 . . 113.91(15) ? C14 C16 C17 . . 122.99(16) ? O6 C16 C6 . . 117.28(15) ? C14 C16 C6 . . 130.07(15) ? C17 C16 C6 . . 104.18(14) ? C18 C17 C3 . . 103.00(15) ? C18 C17 C16 . . 102.55(14) ? C3 C17 C16 . . 103.77(15) ? C18 C17 H12 . . 115.3 ? C3 C17 H12 . . 115.3 ? C16 C17 H12 . . 115.3 ? C5 C18 C17 . . 95.82(14) ? C5 C18 H14 . . 112.6 ? C17 C18 H14 . . 112.6 ? C5 C18 H13 . . 112.6 ? C17 C18 H13 . . 112.6 ? H14 C18 H13 . . 110.1 ? C5 C19 H19 . . 109.5 ? C5 C19 H18 . . 109.5 ? H19 C19 H18 . . 109.5 ? C5 C19 H20 . . 109.5 ? H19 C19 H20 . . 109.5 ? H18 C19 H20 . . 109.5 ? C9 C20 H21 . . 120.0 ? C9 C20 H22 . . 120.0 ? H21 C20 H22 . . 120.0 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C2 . 1.333(3) ? O1 C1 . 1.446(2) ? O2 C10 . 1.200(2) ? O3 C2 . 1.194(3) ? O4 C11 . 1.362(2) ? O4 C6 . 1.459(2) ? O5 C11 . 1.198(3) ? O6 C16 . 1.436(2) ? O6 C14 . 1.456(3) ? O7 C10 . 1.353(2) ? O7 C12 . 1.476(2) ? C1 H2 . 0.98 ? C1 H3 . 0.98 ? C1 H1 . 0.98 ? C2 C3 . 1.512(2) ? C3 C17 . 1.532(3) ? C3 C4 . 1.570(3) ? C3 H4 . 1.0 ? C4 C11 . 1.515(3) ? C4 C5 . 1.544(3) ? C4 H5 . 1.0 ? C5 C19 . 1.516(3) ? C5 C18 . 1.524(3) ? C5 C6 . 1.565(2) ? C6 C7 . 1.514(2) ? C6 C16 . 1.569(2) ? C7 C8 . 1.525(2) ? C7 H16 . 0.99 ? C7 H17 . 0.99 ? C8 C9 . 1.499(2) ? C8 C12 . 1.522(3) ? C8 H15 . 1.0 ? C9 C20 . 1.321(3) ? C9 C10 . 1.487(3) ? C12 C13 . 1.504(3) ? C12 H6 . 1.0 ? C13 C14 . 1.529(3) ? C13 H7 . 0.99 ? C13 H8 . 0.99 ? C14 C16 . 1.492(3) ? C14 C15 . 1.513(3) ? C15 H9 . 0.98 ? C15 H10 . 0.98 ? C15 H11 . 0.98 ? C16 C17 . 1.533(3) ? C17 C18 . 1.527(3) ? C17 H12 . 1.0 ? C18 H14 . 0.99 ? C18 H13 . 0.99 ? C19 H19 . 0.98 ? C19 H18 . 0.98 ? C19 H20 . 0.98 ? C20 H21 . 0.95 ? C20 H22 . 0.95 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C1 H3 O3 3_746 0.98 2.36 3.314(3) 164.4 ? C4 H5 O4 2_556 1.00 2.53 3.513(2) 166.0 ? C8 H15 O5 2_456 1.00 2.50 3.347(2) 142.6 ? C12 H6 O2 2_566 1.00 2.34 3.272(2) 154.8 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C1 O1 C2 O3 . . . . 0.2(3) ? C1 O1 C2 C3 . . . . -177.17(17) ? O3 C2 C3 C17 . . . . -3.9(3) ? O1 C2 C3 C17 . . . . 173.37(16) ? O3 C2 C3 C4 . . . . 112.1(2) ? O1 C2 C3 C4 . . . . -70.6(2) ? C2 C3 C4 C11 . . . . 134.98(17) ? C17 C3 C4 C11 . . . . -102.73(17) ? C2 C3 C4 C5 . . . . -114.90(17) ? C17 C3 C4 C5 . . . . 7.40(17) ? C11 C4 C5 C19 . . . . -88.50(18) ? C3 C4 C5 C19 . . . . 155.97(15) ? C11 C4 C5 C18 . . . . 141.87(15) ? C3 C4 C5 C18 . . . . 26.34(17) ? C11 C4 C5 C6 . . . . 35.89(16) ? C3 C4 C5 C6 . . . . -79.65(15) ? C11 O4 C6 C7 . . . . 149.05(15) ? C11 O4 C6 C5 . . . . 26.25(18) ? C11 O4 C6 C16 . . . . -81.68(17) ? C19 C5 C6 O4 . . . . 84.5(2) ? C18 C5 C6 O4 . . . . -145.13(14) ? C4 C5 C6 O4 . . . . -37.84(16) ? C19 C5 C6 C7 . . . . -33.3(2) ? C18 C5 C6 C7 . . . . 97.08(18) ? C4 C5 C6 C7 . . . . -155.63(15) ? C19 C5 C6 C16 . . . . -162.70(17) ? C18 C5 C6 C16 . . . . -32.30(17) ? C4 C5 C6 C16 . . . . 74.99(15) ? O4 C6 C7 C8 . . . . 63.78(19) ? C5 C6 C7 C8 . . . . 179.80(15) ? C16 C6 C7 C8 . . . . -59.6(2) ? C6 C7 C8 C9 . . . . -164.02(16) ? C6 C7 C8 C12 . . . . 79.4(2) ? C12 C8 C9 C20 . . . . 150.4(2) ? C7 C8 C9 C20 . . . . 27.1(3) ? C12 C8 C9 C10 . . . . -27.54(19) ? C7 C8 C9 C10 . . . . -150.80(16) ? C12 O7 C10 O2 . . . . -173.31(19) ? C12 O7 C10 C9 . . . . 6.2(2) ? C20 C9 C10 O2 . . . . 15.7(3) ? C8 C9 C10 O2 . . . . -166.1(2) ? C20 C9 C10 O7 . . . . -163.78(18) ? C8 C9 C10 O7 . . . . 14.4(2) ? C6 O4 C11 O5 . . . . 178.21(19) ? C6 O4 C11 C4 . . . . -2.0(2) ? C5 C4 C11 O5 . . . . 156.5(2) ? C3 C4 C11 O5 . . . . -93.4(3) ? C5 C4 C11 O4 . . . . -23.2(2) ? C3 C4 C11 O4 . . . . 86.84(19) ? C10 O7 C12 C13 . . . . -147.78(17) ? C10 O7 C12 C8 . . . . -24.1(2) ? C9 C8 C12 O7 . . . . 30.88(18) ? C7 C8 C12 O7 . . . . 156.58(15) ? C9 C8 C12 C13 . . . . 148.88(16) ? C7 C8 C12 C13 . . . . -85.4(2) ? O7 C12 C13 C14 . . . . -174.86(17) ? C8 C12 C13 C14 . . . . 68.6(2) ? C16 O6 C14 C15 . . . . -108.99(18) ? C16 O6 C14 C13 . . . . 119.21(17) ? C12 C13 C14 O6 . . . . -106.9(2) ? C12 C13 C14 C16 . . . . -40.7(3) ? C12 C13 C14 C15 . . . . 120.0(2) ? C14 O6 C16 C17 . . . . 115.49(18) ? C14 O6 C16 C6 . . . . -122.49(18) ? C15 C14 C16 O6 . . . . 103.95(19) ? C13 C14 C16 O6 . . . . -96.2(2) ? O6 C14 C16 C17 . . . . -100.33(19) ? C15 C14 C16 C17 . . . . 3.6(3) ? C13 C14 C16 C17 . . . . 163.44(19) ? O6 C14 C16 C6 . . . . 101.6(2) ? C15 C14 C16 C6 . . . . -154.47(19) ? C13 C14 C16 C6 . . . . 5.3(3) ? O4 C6 C16 O6 . . . . -18.6(2) ? C7 C6 C16 O6 . . . . 104.32(18) ? C5 C6 C16 O6 . . . . -128.44(16) ? O4 C6 C16 C14 . . . . -90.5(2) ? C7 C6 C16 C14 . . . . 32.4(3) ? C5 C6 C16 C14 . . . . 159.66(19) ? O4 C6 C16 C17 . . . . 108.30(15) ? C7 C6 C16 C17 . . . . -128.76(16) ? C5 C6 C16 C17 . . . . -1.51(18) ? C2 C3 C17 C18 . . . . 83.56(18) ? C4 C3 C17 C18 . . . . -38.66(17) ? C2 C3 C17 C16 . . . . -169.81(15) ? C4 C3 C17 C16 . . . . 67.97(16) ? O6 C16 C17 C18 . . . . 163.69(15) ? C14 C16 C17 C18 . . . . -128.18(18) ? C6 C16 C17 C18 . . . . 34.70(18) ? O6 C16 C17 C3 . . . . 56.72(18) ? C14 C16 C17 C3 . . . . 124.85(18) ? C6 C16 C17 C3 . . . . -72.27(17) ? C19 C5 C18 C17 . . . . -176.74(16) ? C4 C5 C18 C17 . . . . -48.90(16) ? C6 C5 C18 C17 . . . . 52.93(17) ? C3 C17 C18 C5 . . . . 53.84(16) ? C16 C17 C18 C5 . . . . -53.72(16) ?