#------------------------------------------------------------------------------ #$Date: 2020-04-22 23:31:52 +0300 (Wed, 22 Apr 2020) $ #$Revision: 251051 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557857.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_1557857 loop_ _publ_author_name 'Wang, Meng' 'Du, Jiao-Xian' 'Hui-Xiang, Yang' 'Dai, Quan' 'Liu, Ya-Pei' 'He, Juan' 'Wang, Yi' 'Li, Zheng-Hui' 'Feng, Tao' 'Liu, Ji-Kai' _publ_section_title ; Sesquiterpenoids from Cultures of the Basidiomycetes Irpex lacteus. ; _journal_name_full 'Journal of natural products' _journal_paper_doi 10.1021/acs.jnatprod.9b01177 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_sum 'C15 H22 O3' _chemical_formula_weight 250.32 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.4807(2) _cell_length_b 11.5246(3) _cell_length_c 31.2716(9) _cell_measurement_reflns_used 9831 _cell_measurement_temperature 150.(2) _cell_measurement_theta_max 78.9771 _cell_measurement_theta_min 4.0882 _cell_volume 2695.99(13) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 833)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _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 0.968 _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 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 33015 _diffrn_reflns_theta_full 79.36 _diffrn_reflns_theta_max 79.36 _diffrn_reflns_theta_min 2.83 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'light colourless' _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Platelet _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.249 _exptl_crystal_size_mid 0.138 _exptl_crystal_size_min 0.077 _refine_diff_density_max 0.444 _refine_diff_density_min -0.374 _refine_ls_abs_structure_details ; Flack x determined using 2168 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 5551 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0558 _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^)+6.1056P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1491 _refine_ls_wR_factor_ref 0.1498 _reflns_number_gt 5362 _reflns_number_total 5551 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np9b01177_si_002.cif _cod_data_source_block LML74 _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/ACS/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 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 1557857 _shelx_res_file ; TITL LML74_0m_a.res in P2(1)2(1)2(1) LML74_0m.res created by SHELXL-2016/6 at 09:38:45 on 09-May-2019 CELL 1.54178 7.4807 11.5246 31.2716 90.000 90.000 90.000 ZERR 8 0.0002 0.0003 0.0009 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 120 176 24 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -123.140 SIZE 0.077 0.138 0.249 ACTA L.S. 15 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF OMIT 7 0 18 OMIT 7 0 19 OMIT 7 1 16 OMIT -8 1 15 OMIT -7 1 17 OMIT 7 1 15 OMIT -7 2 14 OMIT -8 1 16 OMIT -8 2 14 OMIT -7 2 20 OMIT -8 1 12 OMIT 7 0 17 OMIT 6 1 19 WGHT 0.000000 6.105600 FVAR 0.60609 O1 3 0.053358 0.438661 0.219760 11.00000 0.02504 0.03348 = 0.02933 -0.00249 -0.00221 -0.00253 H6O 2 0.126270 0.012851 0.321157 11.00000 0.03998 C1 1 0.122099 0.596557 0.364212 11.00000 0.01709 0.02346 = 0.02856 0.00042 -0.00252 0.00336 AFIX 13 H1 2 0.232078 0.645822 0.363313 11.00000 -1.20000 AFIX 0 O2 3 0.150604 0.263710 0.353883 11.00000 0.02060 0.02117 = 0.05262 0.00189 0.00661 -0.00127 AFIX 148 H2 2 0.171957 0.201307 0.347438 11.00000 -1.50000 AFIX 0 C2 1 0.071426 0.568436 0.319125 11.00000 0.01278 0.02302 = 0.03062 0.00430 -0.00551 0.00002 O3 3 -0.064848 0.592360 0.252836 11.00000 0.02627 0.03099 = 0.02903 0.00102 -0.00682 0.00539 C3 1 0.130160 0.482735 0.293887 11.00000 0.01650 0.02365 = 0.02781 0.00251 -0.00133 -0.00284 O4 3 0.490280 0.148172 0.219736 11.00000 0.02554 0.03875 = 0.02649 0.00131 -0.00372 0.00386 C4 1 0.272438 0.391438 0.299363 11.00000 0.01865 0.02680 = 0.03016 -0.00321 -0.00105 0.00372 AFIX 23 H4A 2 0.387926 0.426162 0.290689 11.00000 -1.20000 H4B 2 0.246378 0.328029 0.278935 11.00000 -1.20000 AFIX 0 O5 3 0.685634 0.248660 0.259440 11.00000 0.02207 0.02957 = 0.02803 0.00401 -0.00098 -0.00234 C5 1 0.298408 0.336684 0.343555 11.00000 0.00999 0.02305 = 0.03487 0.00258 0.00379 0.00187 AFIX 13 H5 2 0.406103 0.285545 0.341630 11.00000 -1.20000 AFIX 0 O6 3 0.203778 0.026261 0.341229 11.00000 0.01832 0.02761 = 0.03083 -0.00441 -0.00285 0.00240 C6 1 0.329856 0.419793 0.381084 11.00000 0.02167 0.02456 = 0.02819 0.00437 -0.00267 0.00490 AFIX 13 H6 2 0.355956 0.370033 0.406526 11.00000 -1.20000 AFIX 0 C7 1 0.162508 0.490776 0.392420 11.00000 0.02436 0.02589 = 0.02687 0.00265 -0.00216 0.00615 AFIX 13 H7 2 0.057196 0.437512 0.390799 11.00000 -1.20000 AFIX 0 C11 1 -0.054959 0.643586 0.294927 11.00000 0.02347 0.02889 = 0.02974 0.00073 -0.00629 0.00576 AFIX 23 H11A 2 -0.174054 0.644259 0.308731 11.00000 -1.20000 H11B 2 -0.009668 0.724183 0.293310 11.00000 -1.20000 AFIX 0 C10 1 -0.020957 0.662810 0.389782 11.00000 0.03213 0.03551 = 0.03172 -0.00145 -0.00136 0.01401 AFIX 23 H10A 2 -0.142118 0.636846 0.381378 11.00000 -1.20000 H10B 2 -0.011249 0.747241 0.384428 11.00000 -1.20000 AFIX 0 C9 1 0.013936 0.635608 0.437829 11.00000 0.04059 0.03167 = 0.02900 -0.00511 -0.00425 0.00981 C8 1 0.164795 0.544647 0.437333 11.00000 0.04060 0.04582 = 0.02793 -0.00098 -0.00324 0.01627 AFIX 23 H8A 2 0.281663 0.581821 0.443074 11.00000 -1.20000 H8B 2 0.143298 0.484479 0.459335 11.00000 -1.20000 AFIX 0 C13 1 0.496260 0.494754 0.373943 11.00000 0.01419 0.03198 = 0.03908 -0.00149 -0.00585 0.00142 AFIX 137 H13A 2 0.601298 0.444618 0.370886 11.00000 -1.50000 H13B 2 0.512975 0.546572 0.398467 11.00000 -1.50000 H13C 2 0.480984 0.541036 0.347909 11.00000 -1.50000 AFIX 0 C12 1 0.041843 0.496658 0.252111 11.00000 0.01349 0.02831 = 0.03069 0.00334 -0.00139 -0.00319 C16 1 0.701544 0.100690 0.366734 11.00000 0.01581 0.02451 = 0.02407 0.00005 -0.00229 -0.00058 AFIX 13 H16 2 0.794518 0.038380 0.365955 11.00000 -1.20000 AFIX 0 C15 1 -0.155143 0.580961 0.457808 11.00000 0.04069 0.05888 = 0.04525 0.00239 0.00020 0.00955 AFIX 137 H15A 2 -0.256190 0.634348 0.454535 11.00000 -1.50000 H15B 2 -0.134271 0.566203 0.488264 11.00000 -1.50000 H15C 2 -0.182222 0.507668 0.443297 11.00000 -1.50000 AFIX 0 C14 1 0.062392 0.742985 0.463241 11.00000 0.07146 0.04303 = 0.05839 -0.01242 -0.01888 0.00464 AFIX 137 H14A 2 0.169644 0.778683 0.450963 11.00000 -1.50000 H14B 2 0.085745 0.721335 0.493028 11.00000 -1.50000 H14C 2 -0.036863 0.798409 0.462175 11.00000 -1.50000 AFIX 0 C17 1 0.664301 0.138695 0.321804 11.00000 0.01314 0.02399 = 0.02604 0.00009 0.00234 0.00302 C18 1 0.557562 0.089274 0.292778 11.00000 0.01606 0.02386 = 0.02487 -0.00199 0.00172 0.00278 C19 1 0.453371 -0.022131 0.293498 11.00000 0.02621 0.02455 = 0.02703 -0.00421 -0.00123 -0.00129 AFIX 23 H19A 2 0.537830 -0.086234 0.287503 11.00000 -1.20000 H19B 2 0.366983 -0.019765 0.269531 11.00000 -1.20000 AFIX 0 C20 1 0.350115 -0.053411 0.333955 11.00000 0.02094 0.02036 = 0.02976 -0.00191 -0.00037 0.00143 AFIX 13 H20 2 0.295582 -0.131419 0.328862 11.00000 -1.20000 AFIX 0 C21 1 0.457214 -0.062531 0.375607 11.00000 0.02333 0.02295 = 0.02894 0.00270 -0.00006 -0.00244 AFIX 13 H21 2 0.370922 -0.087553 0.398223 11.00000 -1.20000 AFIX 0 C22 1 0.536524 0.053708 0.390675 11.00000 0.01536 0.02498 = 0.02538 0.00171 -0.00171 0.00050 AFIX 13 H22 2 0.440129 0.113321 0.387812 11.00000 -1.20000 AFIX 0 C23 1 0.596686 0.054143 0.438160 11.00000 0.02658 0.03706 = 0.02568 0.00369 -0.00290 -0.00660 AFIX 23 H23A 2 0.633886 -0.024704 0.447032 11.00000 -1.20000 H23B 2 0.497196 0.079583 0.456812 11.00000 -1.20000 AFIX 0 C25 1 0.765071 0.196440 0.397164 11.00000 0.02031 0.02828 = 0.02529 -0.00052 -0.00145 -0.00477 AFIX 23 H25A 2 0.685430 0.264916 0.395603 11.00000 -1.20000 H25B 2 0.888562 0.220824 0.390179 11.00000 -1.20000 AFIX 0 C24 1 0.756869 0.140096 0.441794 11.00000 0.02517 0.02853 = 0.02474 -0.00149 -0.00051 0.00005 C26 1 0.754275 0.242019 0.302264 11.00000 0.01734 0.03002 = 0.02615 0.00191 0.00091 -0.00299 AFIX 23 H26A 2 0.725218 0.313415 0.318439 11.00000 -1.20000 H26B 2 0.885647 0.231666 0.302002 11.00000 -1.20000 AFIX 0 C28 1 0.596344 -0.159353 0.371829 11.00000 0.03223 0.02476 = 0.05064 0.00116 -0.01125 0.00466 AFIX 137 H28A 2 0.537397 -0.231370 0.362950 11.00000 -1.50000 H28B 2 0.654342 -0.171093 0.399594 11.00000 -1.50000 H28C 2 0.686384 -0.137595 0.350525 11.00000 -1.50000 AFIX 0 C29 1 0.931894 0.074923 0.450725 11.00000 0.03294 0.04313 = 0.03473 -0.00040 -0.01136 0.00753 AFIX 137 H29A 2 0.952237 0.017287 0.428203 11.00000 -1.50000 H29B 2 0.923708 0.035716 0.478464 11.00000 -1.50000 H29C 2 1.031476 0.130160 0.451209 11.00000 -1.50000 AFIX 0 C30 1 0.727059 0.231899 0.476248 11.00000 0.04128 0.03569 = 0.02825 -0.00337 0.00233 -0.00033 AFIX 137 H30A 2 0.824843 0.288444 0.475426 11.00000 -1.50000 H30B 2 0.723912 0.194580 0.504397 11.00000 -1.50000 H30C 2 0.613284 0.271614 0.471042 11.00000 -1.50000 AFIX 0 C27 1 0.567290 0.159597 0.253351 11.00000 0.01970 0.02695 = 0.02677 -0.00129 0.00063 0.00410 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM LML74_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0558 for 5362 Fo > 4sig(Fo) and 0.0575 for all 5551 data REM 337 parameters refined using 0 restraints END WGHT 0.0344 2.8683 REM Instructions for potential hydrogen bonds EQIV $1 -x, y-1/2, -z+1/2 HTAB O6 O1_$1 HTAB O6 O3_$1 HTAB O2 O6 EQIV $2 -x, y+1/2, -z+1/2 HTAB C11 O4_$2 HTAB C11 O1_$2 EQIV $3 x+1, y, z HTAB C26 O2_$3 REM Highest difference peak 0.444, deepest hole -0.374, 1-sigma level 0.075 Q1 1 0.1732 0.7409 0.4466 11.00000 0.05 0.44 Q2 1 0.6691 0.2008 0.3190 11.00000 0.05 0.32 Q3 1 0.5987 0.2887 0.3997 11.00000 0.05 0.31 Q4 1 0.5489 0.1330 0.3145 11.00000 0.05 0.31 Q5 1 0.3758 0.4890 0.3698 11.00000 0.05 0.29 ; _shelx_res_checksum 56342 _shelx_hkl_file ; 1 0 0 0.80 0.40 -1 0 0 -0.10 0.40 2 0 0 951.70 46.60 3 0 0 1.70 1.20 4 0 0 454.35 27.50 5 0 0 4.10 2.80 -6 0 0 21.30 3.80 -6 0 0 18.60 3.20 -6 0 0 13.20 3.20 -6 0 0 21.50 4.50 -6 0 0 25.20 6.30 -6 0 0 16.00 2.30 -6 0 0 16.20 4.20 -6 0 0 17.20 4.70 -7 0 0 0.60 1.80 -7 0 0 -0.30 1.30 -7 0 0 0.20 1.30 -7 0 0 -0.40 2.10 -7 0 0 0.40 1.40 -8 0 0 165.08 12.20 -8 0 0 204.58 14.90 -8 0 0 181.38 12.50 -8 0 0 178.98 14.80 0 1 0 0.10 0.40 0 1 0 -0.30 0.30 1 -1 0 8939.11 384.26 -1 1 0 8579.24 382.26 1 1 0 7198.48 376.96 2 -1 0 1509.45 80.29 2 1 0 1259.57 65.09 2 -1 0 1277.77 64.39 3 -1 0 579.24 31.50 3 1 0 574.74 32.20 4 1 0 21.20 5.10 4 -1 0 24.20 4.30 5 -1 0 52.49 7.80 5 1 0 52.09 8.40 -5 -1 0 83.89 10.00 -5 -1 0 54.79 7.10 -5 -1 0 80.59 8.70 -5 1 0 68.99 7.10 -6 -1 0 51.79 5.20 -6 1 0 50.09 5.20 -6 -1 0 62.99 7.30 -6 -1 0 62.29 9.50 -6 -1 0 59.49 7.40 -6 1 0 65.09 7.40 -6 1 0 67.09 6.60 -6 1 0 70.19 9.60 -6 -1 0 55.59 6.30 -6 1 0 70.59 7.10 -6 1 0 62.39 5.40 -7 1 0 4.30 3.10 -7 -1 0 1.50 1.50 -7 1 0 2.20 1.70 -7 1 0 5.90 2.00 -7 -1 0 2.30 2.70 -7 1 0 3.00 2.70 -7 -1 0 3.00 2.10 -7 -1 0 6.80 4.00 -7 -1 0 2.10 1.60 -8 1 0 164.18 12.00 -8 1 0 175.08 13.20 -8 -1 0 152.38 11.40 -8 -1 0 163.98 11.40 -8 1 0 163.68 11.20 -8 1 0 146.79 13.10 -8 -1 0 156.88 13.80 -9 1 0 5.10 1.70 0 2 0 4656.33 217.08 0 2 0 4673.93 219.38 -1 2 0 2865.61 134.69 1 -2 0 2736.83 134.49 1 2 0 2646.94 130.09 2 -2 0 4207.68 202.58 2 2 0 3787.92 187.68 3 -2 0 722.53 39.00 3 2 0 702.93 40.10 4 -2 0 264.17 18.80 4 2 0 252.57 19.60 -5 -2 0 -1.20 2.00 -5 -2 0 0.50 1.10 -5 -2 0 0.60 2.00 -5 2 0 0.50 1.80 5 -2 0 0.20 2.80 -5 2 0 0.30 1.40 -5 2 0 1.50 1.10 -5 2 0 -1.10 1.30 -5 -2 0 -0.40 1.50 5 2 0 5.00 3.40 -6 -2 0 42.10 4.70 -6 2 0 37.70 7.10 -6 2 0 24.70 6.10 -6 -2 0 50.19 8.60 -6 2 0 36.80 2.90 -6 2 0 42.60 5.90 -6 -2 0 37.60 5.30 -6 -2 0 43.20 7.00 -6 2 0 34.40 5.40 -6 2 0 35.90 4.00 -6 -2 0 44.40 6.50 -7 -2 0 40.60 6.40 -7 2 0 46.20 6.40 -7 -2 0 28.30 3.90 -7 -2 0 35.80 5.40 -7 -2 0 41.70 7.60 -7 2 0 38.20 6.90 -8 2 0 90.49 7.50 -8 -2 0 102.29 8.40 -8 2 0 106.89 9.60 -8 -2 0 96.89 10.30 -8 -2 0 83.49 6.30 -8 -2 0 98.39 8.70 -8 2 0 84.09 9.20 -9 -2 0 26.00 6.50 -9 -2 0 27.30 5.50 0 3 0 0.90 1.20 0 3 0 1.80 1.60 1 -3 0 1973.20 101.39 -1 3 0 2120.39 100.99 -1 3 0 2031.40 106.49 1 3 0 2026.00 100.39 2 -3 0 482.55 35.80 2 3 0 453.45 28.90 3 3 0 1541.15 80.09 3 -3 0 1507.25 78.09 4 3 0 1455.75 78.49 4 -3 0 1424.96 75.69 -5 -3 0 24.50 6.30 5 3 0 13.20 6.60 -5 3 0 19.10 2.00 -5 3 0 23.50 4.40 -5 -3 0 30.50 6.60 5 -3 0 23.40 6.80 -5 -3 0 29.80 3.80 -6 3 0 203.08 14.10 6 3 0 157.58 21.30 -6 3 0 223.08 11.50 -6 3 0 263.17 19.40 -6 3 0 217.38 17.60 -6 -3 0 243.98 13.90 -6 3 0 217.98 12.50 -6 3 0 204.08 15.00 -7 -3 0 63.69 5.80 -7 3 0 72.69 8.00 -7 -3 0 83.09 8.40 -7 3 0 55.99 8.10 -7 3 0 54.49 6.40 -7 -3 0 71.99 7.30 -7 3 0 64.79 6.20 -7 -3 0 81.89 9.90 -8 3 0 36.80 5.60 -8 3 0 33.20 6.80 -8 -3 0 32.50 6.10 -8 -3 0 33.00 5.00 -8 -3 0 38.00 6.00 -8 3 0 43.30 4.90 -9 -3 0 73.69 8.30 -9 -3 0 59.99 6.60 0 4 0 66.39 8.80 0 4 0 73.99 11.10 -1 4 0 153.88 18.90 1 -4 0 183.98 16.30 1 4 0 158.38 14.80 -1 4 0 161.48 15.10 1 4 0 189.08 19.80 2 -4 0 469.15 33.40 2 4 0 479.15 41.60 2 4 0 498.95 32.60 -2 4 0 507.05 34.40 3 4 0 629.34 40.80 4 -4 0 139.19 14.30 4 4 0 138.29 16.00 5 -4 0 -4.00 3.80 -5 4 0 5.70 2.50 -5 4 0 6.40 1.70 -5 4 0 8.30 2.60 5 4 0 24.20 13.20 -6 4 0 106.49 7.50 6 4 0 118.39 17.90 -6 4 0 94.19 8.60 -6 -4 0 122.39 9.80 -6 -4 0 120.89 8.90 -6 4 0 104.69 6.60 -6 4 0 125.99 10.60 -6 -4 0 123.29 10.60 -6 -4 0 137.19 13.80 -7 -4 0 37.70 7.50 -7 4 0 27.80 4.60 -7 -4 0 38.30 7.10 -7 -4 0 39.20 8.50 -7 4 0 34.90 4.60 -7 4 0 37.60 6.10 -7 -4 0 29.80 4.10 -8 4 0 17.40 4.00 -8 -4 0 20.60 4.40 -8 4 0 9.90 4.40 -8 -4 0 13.50 2.30 -8 -4 0 20.00 5.20 -8 4 0 15.50 3.60 -9 -4 0 82.89 7.50 0 5 0 2.50 2.30 0 5 0 6.20 6.70 -1 5 0 -0.20 1.80 1 5 0 4.50 5.30 1 5 0 1.20 2.30 -1 5 0 2.00 5.20 2 5 0 1237.08 68.09 -2 5 0 1031.50 65.49 2 5 0 1262.97 81.79 3 5 0 68.99 11.50 3 5 0 60.89 18.70 -4 -5 0 144.59 10.70 -4 -5 0 142.79 9.40 4 5 0 113.99 33.00 4 5 0 139.09 17.00 4 -5 0 127.09 15.30 -4 5 0 153.48 11.00 -4 5 0 126.29 7.50 -5 -5 0 8.20 1.60 -5 -5 0 10.30 2.90 -5 5 0 7.90 1.60 5 5 0 7.10 1.20 -5 -5 0 8.30 4.20 5 5 0 4.50 6.30 -5 -5 0 7.70 2.60 5 -5 0 15.00 5.70 -6 5 0 69.29 7.30 6 5 0 75.79 5.00 -6 5 0 96.99 9.10 -6 -5 0 99.39 8.70 -6 5 0 86.99 5.50 -6 -5 0 99.99 9.50 -6 -5 0 93.59 7.60 -6 5 0 84.59 6.30 -6 -5 0 100.29 11.30 -7 5 0 9.70 2.50 -7 -5 0 5.40 2.20 -7 5 0 4.00 1.80 -7 -5 0 7.40 3.60 -7 -5 0 7.60 2.80 -7 -5 0 4.90 1.90 -7 5 0 8.20 3.20 -7 5 0 -0.30 3.10 0 6 0 740.53 57.49 0 6 0 764.72 49.90 1 6 0 8.40 4.40 1 6 0 6.70 4.90 -1 6 0 9.00 9.00 -1 6 0 3.70 2.60 -2 6 0 146.39 18.10 2 6 0 100.09 15.10 2 6 0 110.09 20.30 3 6 0 97.79 14.80 3 6 0 101.39 29.00 -4 -6 0 302.47 16.60 4 -6 0 292.67 26.40 -4 -6 0 286.17 14.90 -4 -6 0 310.17 17.70 -4 6 0 264.67 14.90 4 6 0 324.17 30.60 -4 6 0 293.97 14.40 4 -6 0 269.67 13.90 4 6 0 305.57 47.50 4 6 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276.87 13.20 5 -7 0 305.37 28.80 -5 -7 0 238.68 13.20 -5 -7 0 255.97 15.90 -5 7 0 287.87 17.60 -5 7 0 220.18 12.40 -5 -7 0 229.38 17.90 6 7 0 0.70 0.60 -6 -7 0 -0.10 1.40 -6 7 0 0.00 1.70 -6 7 0 -0.90 1.10 -6 -7 0 3.80 4.50 -6 -7 0 -1.00 1.30 -8 -7 0 8.60 2.00 -8 -7 0 6.20 1.50 -8 7 0 9.70 2.30 0 8 0 257.77 12.90 0 -8 0 256.47 12.60 0 8 0 260.67 28.20 0 8 0 166.88 42.00 0 8 0 253.87 12.70 1 8 0 20.80 2.00 1 8 0 6.00 8.50 1 8 0 17.90 1.90 -1 8 0 16.00 2.00 -1 -8 0 22.30 1.90 1 -8 0 19.80 1.80 -1 8 0 23.10 2.00 -2 8 0 229.68 12.00 -2 8 0 228.58 12.00 2 8 0 237.68 12.20 2 8 0 224.18 12.00 2 8 0 217.38 42.70 2 8 0 258.77 30.90 2 -8 0 227.98 11.90 -2 8 0 266.97 16.10 3 8 0 38.60 13.90 -3 8 0 43.40 3.20 -3 -8 0 48.70 6.50 3 -8 0 41.30 2.90 3 8 0 44.30 3.30 -3 8 0 40.00 3.20 -3 8 0 48.40 6.00 -3 -8 0 45.50 3.00 -3 8 0 38.10 4.00 4 -8 0 67.49 4.30 -4 -8 0 78.39 5.40 -4 -8 0 90.99 7.40 4 8 0 40.90 15.00 4 -8 0 72.99 15.10 4 8 0 76.79 4.80 -4 8 0 71.99 4.70 -4 8 0 69.29 5.30 -4 8 0 64.49 4.60 -4 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137.69 8.30 1 0 -28 133.19 7.20 -1 0 -28 135.99 7.20 -1 0 -28 120.59 7.90 1 0 -28 131.69 7.00 -1 0 -28 144.09 7.50 -1 0 -28 131.09 6.90 1 0 -28 135.89 6.80 -1 0 28 129.19 8.10 -2 0 -28 397.66 19.80 -2 0 -28 412.66 19.60 -2 0 28 420.26 20.70 -2 0 -28 376.16 18.90 -2 0 -28 410.76 20.90 2 0 -28 413.06 19.40 2 0 -28 395.96 19.60 -2 0 -28 411.86 20.70 -3 0 -28 74.59 5.60 3 0 -28 75.29 4.50 3 0 -28 70.59 4.40 -3 0 -28 71.19 4.50 -3 0 -28 69.49 4.60 -3 0 -28 70.89 5.30 -3 0 -28 70.79 4.30 -3 0 28 74.29 5.30 -4 0 -28 32.20 2.60 -4 0 -28 38.80 3.70 -4 0 -28 36.00 3.30 -4 0 -28 34.70 3.10 4 0 -28 36.50 2.60 4 0 -28 35.00 2.60 -4 0 -28 37.50 2.60 -4 0 28 38.40 3.30 -5 0 -28 28.30 2.20 5 0 -28 34.40 2.40 -5 0 -28 29.90 2.20 -5 0 28 37.10 4.70 -5 0 -28 38.00 3.20 -5 0 -28 37.90 3.50 -5 0 -28 32.50 2.80 -5 0 28 37.00 2.90 5 0 -28 34.90 2.40 -6 0 -28 12.00 1.00 6 0 -28 13.50 1.20 -6 0 28 16.00 3.70 -6 0 -28 14.90 1.90 -6 0 -28 13.50 1.60 0 1 -28 6.20 1.00 0 -1 -28 7.30 1.20 0 -1 -28 7.00 1.70 0 -1 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36.90 2.70 -3 1 -28 37.20 3.60 -4 1 28 1.10 1.00 -4 -1 -28 2.00 0.70 -4 -1 -28 2.40 1.00 -4 -1 -28 1.90 0.80 -4 -1 -28 1.90 0.90 4 1 -28 1.70 0.70 4 1 -28 2.10 0.70 -4 -1 -28 1.30 1.10 4 -1 -28 1.80 0.70 -4 1 -28 1.70 0.60 4 -1 -28 1.20 0.60 -4 1 -28 2.80 1.80 -4 1 -28 2.80 1.30 -4 1 -28 2.00 1.10 -4 1 -28 2.90 0.90 -4 -1 28 2.80 0.90 -5 -1 -28 6.30 1.40 5 1 -28 5.80 1.10 -5 -1 -28 5.50 0.90 -5 -1 -28 5.90 1.60 -5 -1 -28 5.60 1.40 -5 1 28 4.10 1.90 -5 1 28 1.60 3.00 5 1 -28 5.20 0.90 -5 1 28 6.50 1.40 -5 1 -28 6.10 1.50 -5 -1 28 2.80 3.30 5 -1 -28 7.70 1.10 5 -1 -28 4.10 0.80 -5 1 -28 11.00 2.10 -5 1 -28 4.80 0.80 -5 1 -28 4.50 0.90 -5 -1 28 5.80 1.30 -5 1 -28 4.90 1.50 -6 1 28 1.00 2.00 -6 -1 -28 4.40 0.60 -6 -1 -28 8.30 1.80 -6 1 28 3.30 1.30 6 1 -28 5.10 0.70 -6 -1 -28 4.00 1.00 -6 -1 28 1.70 2.40 -6 1 -28 4.20 0.70 -6 1 -28 5.90 1.20 -6 1 -28 4.90 1.20 6 -1 -28 3.50 0.60 0 -2 -28 -0.90 0.70 0 -2 -28 0.10 0.40 0 2 -28 0.00 0.90 0 2 -28 0.30 0.60 0 2 -28 0.20 0.60 0 2 -28 0.70 0.50 0 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1.20 -3 2 -28 9.90 1.90 -3 2 -28 10.20 2.30 -3 2 -28 9.40 1.60 3 -2 -28 7.60 1.20 4 2 -28 7.10 1.10 -4 -2 -28 7.20 1.30 -4 -2 -28 6.40 1.00 4 2 -28 6.40 1.00 -4 -2 -28 5.90 1.60 -4 -2 -28 7.30 1.60 -4 -2 -28 6.20 1.10 -4 2 28 6.50 1.40 -4 2 -28 5.50 1.40 4 -2 -28 5.40 1.00 -4 2 -28 6.90 1.20 4 -2 -28 5.90 0.90 -4 2 -28 5.70 1.40 -4 2 -28 5.80 1.10 -4 -2 28 5.20 1.40 -5 -2 -28 25.10 2.70 5 2 -28 23.20 1.90 5 2 -28 29.70 2.40 -5 2 28 28.50 2.70 -5 -2 -28 25.80 2.70 -5 2 28 20.20 5.70 -5 -2 -28 25.70 2.20 -5 2 28 27.30 4.80 -5 -2 -28 23.80 1.70 -5 2 -28 28.50 3.80 5 -2 -28 23.20 1.80 -5 2 -28 23.40 1.90 -5 2 -28 30.00 2.40 -5 2 -28 23.50 2.40 -6 -2 -28 28.70 2.30 -6 -2 -28 30.20 2.30 -6 2 28 19.40 3.90 -6 -2 -28 26.20 2.10 6 2 -28 22.40 1.70 -6 2 28 30.90 2.00 -6 2 28 29.60 3.60 -6 -2 -28 24.30 1.60 -6 2 -28 23.70 1.60 6 -2 -28 31.70 1.80 -6 2 -28 23.90 1.60 -6 2 -28 27.70 2.40 0 3 -28 111.09 7.10 0 3 -28 112.69 6.50 0 -3 -28 111.39 7.40 0 3 -28 112.79 6.10 0 3 -28 111.09 6.00 0 -3 -28 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1.80 -3 3 -35 15.80 1.70 4 3 -35 1.20 0.40 -4 -3 -35 0.50 0.30 4 -3 -35 1.30 0.90 4 -3 -35 0.80 0.40 -4 3 -35 2.10 0.40 -4 3 -35 1.50 0.40 0 -4 -35 5.70 1.10 0 -4 -35 7.20 0.70 0 4 -35 5.40 0.60 0 4 -35 7.00 1.10 0 -4 -35 5.10 0.80 0 -4 -35 5.50 1.30 0 -4 -35 5.50 0.80 -1 -4 -35 18.50 2.10 1 4 -35 17.30 1.30 -1 -4 -35 15.70 1.60 -1 -4 -35 15.20 1.40 1 4 -35 15.60 1.40 -1 -4 -35 15.10 1.30 1 -4 -35 16.40 1.20 -1 4 -35 17.10 1.50 1 -4 -35 17.40 2.10 1 -4 -35 17.90 1.50 1 -4 -35 18.70 1.30 -2 4 35 -1.40 0.80 -2 -4 -35 0.20 0.60 -2 -4 -35 0.30 0.80 -2 -4 -35 0.20 0.40 2 4 -35 0.60 0.40 -2 4 -35 -0.60 0.80 2 -4 -35 0.40 0.80 2 -4 -35 0.40 0.40 -2 4 -35 0.60 0.50 -2 4 -35 -0.20 0.40 -3 -4 -35 33.80 2.40 -3 -4 -35 39.10 2.20 3 4 -35 42.40 2.30 -3 -4 -35 40.10 2.70 -3 4 35 35.00 2.40 -3 4 -35 37.70 2.10 3 -4 -35 46.30 2.80 -3 4 -35 38.20 2.30 3 -4 -35 42.80 2.20 0 -5 -35 27.80 1.70 0 -5 -35 22.30 1.90 0 -5 -35 29.20 2.40 0 5 -35 26.00 1.70 0 -5 -35 29.90 1.60 0 -5 -35 27.90 1.80 1 5 -35 15.30 1.30 -1 -5 -35 16.70 1.20 -1 -5 -35 14.10 1.40 -1 -5 -35 17.20 1.90 1 -5 -35 13.60 1.10 1 -5 -35 16.40 1.30 -1 5 -35 14.60 1.20 1 -5 -35 17.40 1.20 1 -5 -35 16.90 2.00 -2 -5 -35 41.90 2.40 -2 -5 -35 40.40 3.30 2 5 -35 45.60 2.40 2 -5 -35 45.60 2.40 -2 5 -35 40.20 2.50 2 -5 -35 46.10 3.00 -3 -5 -35 46.70 2.50 3 -5 -35 51.19 2.70 3 -5 -35 47.70 3.20 -3 5 -35 49.80 2.60 3 -5 -35 55.09 2.60 0 -6 -35 2.20 0.40 -1 -6 -35 17.90 1.20 -1 -6 -35 14.20 1.40 1 -6 -35 19.00 1.10 1 -6 -35 16.80 1.30 1 -6 -35 14.30 1.70 -2 -6 -35 3.80 0.60 2 6 -35 3.80 0.50 2 -6 -35 3.80 0.50 0 0 -36 16.20 1.50 0 0 -36 16.10 1.20 0 0 -36 18.60 2.30 0 0 -36 14.80 1.30 1 0 -36 55.99 3.10 -1 0 -36 58.59 4.00 -1 0 -36 52.29 3.00 1 0 -36 52.79 3.30 1 0 -36 58.59 3.90 -1 0 -36 50.19 3.30 -2 0 -36 0.40 0.80 -2 0 -36 0.40 0.40 2 0 -36 0.40 0.50 2 0 -36 -0.10 0.80 2 0 -36 0.20 0.40 -2 0 -36 0.40 0.50 3 0 -36 3.30 0.60 -3 0 -36 4.60 0.70 3 0 -36 3.40 0.60 -3 0 -36 4.00 1.00 -3 0 -36 3.80 0.60 -4 0 -36 29.90 1.80 -4 0 -36 40.10 2.30 0 -1 -36 36.40 2.10 0 1 -36 41.10 3.10 0 1 -36 37.00 2.50 0 1 -36 37.00 2.10 0 -1 -36 35.90 2.50 0 -1 -36 34.40 2.20 0 -1 -36 39.90 3.20 0 1 -36 33.40 2.00 1 1 -36 4.50 0.70 1 1 -36 5.40 0.90 -1 -1 -36 3.50 1.20 -1 -1 -36 4.90 0.80 1 1 -36 4.20 1.10 -1 -1 -36 5.20 0.90 -1 1 -36 4.00 0.70 -1 1 -36 3.80 0.80 1 -1 -36 3.80 0.70 1 -1 -36 4.20 0.90 1 -1 -36 3.90 1.20 -1 1 -36 5.00 1.30 -2 -1 -36 22.20 1.60 2 1 -36 20.80 2.10 2 1 -36 26.00 1.70 2 1 -36 22.70 1.70 -2 -1 -36 27.10 2.50 -2 -1 -36 21.10 1.70 2 -1 -36 24.70 1.80 -2 1 -36 22.40 1.60 2 -1 -36 25.30 2.40 -2 1 -36 22.50 1.70 -2 1 -36 25.40 2.40 2 -1 -36 23.60 1.60 -3 -1 -36 15.60 1.30 -3 -1 -36 17.70 2.80 3 1 -36 17.10 1.20 -3 -1 -36 15.10 1.20 3 1 -36 16.10 1.40 -3 1 -36 17.70 1.20 -3 1 -36 15.10 1.30 3 -1 -36 19.50 1.40 3 -1 -36 17.70 1.30 3 -1 -36 21.20 1.80 -3 1 -36 18.20 1.90 -4 -1 -36 8.80 0.70 -4 -1 -36 11.20 1.50 -4 1 -36 8.90 0.70 -4 1 -36 7.20 1.20 0 -2 -36 3.00 0.70 0 2 -36 3.60 0.50 0 2 -36 1.80 0.60 0 -2 -36 2.60 0.60 0 -2 -36 3.40 1.30 0 -2 -36 3.40 0.60 -1 -2 -36 31.90 2.20 -1 -2 -36 31.90 2.10 1 2 -36 31.70 2.60 1 2 -36 35.00 2.10 -1 -2 -36 33.40 2.90 1 2 -36 33.10 2.20 -1 2 -36 30.20 1.90 1 -2 -36 28.60 1.90 1 -2 -36 37.00 3.00 1 -2 -36 34.60 2.10 -1 2 -36 34.40 2.30 1 -2 -36 34.10 2.30 -1 2 -36 36.70 2.90 -2 -2 -36 5.10 1.10 -2 -2 -36 4.20 1.20 2 2 -36 3.50 0.60 -2 -2 -36 3.20 0.60 2 2 -36 4.60 0.70 -2 2 36 3.00 1.30 -2 -2 -36 3.80 0.80 2 -2 -36 3.20 1.10 2 -2 -36 4.20 0.80 -2 2 -36 4.10 1.10 2 -2 -36 5.30 0.80 -2 2 -36 3.10 0.70 -2 2 -36 4.40 0.60 -3 -2 -36 18.00 1.70 -3 -2 -36 17.80 1.20 -3 2 36 18.10 1.50 3 2 -36 17.80 1.30 3 -2 -36 18.00 1.80 -3 2 -36 16.80 1.20 3 -2 -36 15.20 1.30 -3 2 -36 20.70 1.80 -3 2 -36 16.40 1.30 3 -2 -36 18.60 1.30 0 3 -36 5.80 0.60 0 -3 -36 5.80 0.90 0 3 -36 6.30 1.00 0 -3 -36 6.20 0.80 0 -3 -36 5.50 0.60 0 -3 -36 4.80 1.20 0 3 -36 5.10 1.10 1 3 -36 12.60 1.00 -1 -3 -36 11.20 1.80 -1 -3 -36 11.30 1.10 1 3 -36 11.30 1.10 -1 -3 -36 8.80 1.30 -1 -3 -36 10.90 1.10 1 -3 -36 9.80 1.10 1 -3 -36 13.40 1.90 1 -3 -36 12.80 1.00 -1 3 -36 12.50 1.60 -1 3 -36 11.50 1.20 1 -3 -36 11.00 0.90 -2 -3 -36 14.40 1.80 -2 -3 -36 10.40 1.00 2 3 -36 14.00 1.20 -2 -3 -36 13.30 1.10 2 3 -36 13.10 1.10 -2 -3 -36 10.70 1.30 -2 3 -36 13.40 1.20 -2 3 -36 15.90 1.70 -2 3 -36 13.40 1.00 2 -3 -36 13.80 1.10 2 -3 -36 15.70 1.90 2 -3 -36 13.30 1.20 -3 -3 -36 39.60 2.30 -3 -3 -36 44.80 2.70 3 3 -36 43.10 2.30 -3 3 -36 39.10 2.20 -3 3 -36 35.70 2.30 3 -3 -36 45.10 2.30 3 -3 -36 43.00 2.40 3 -3 -36 46.60 2.80 0 -4 -36 4.30 0.70 0 -4 -36 5.30 1.20 0 -4 -36 5.90 0.60 0 4 -36 5.60 0.80 0 -4 -36 4.10 0.70 1 4 -36 5.20 0.80 -1 -4 -36 4.60 0.70 -1 -4 -36 6.00 1.40 -1 -4 -36 4.70 0.90 -1 -4 -36 4.50 0.60 1 4 -36 5.40 0.60 1 -4 -36 6.00 0.70 -1 4 -36 2.90 0.70 1 -4 -36 6.40 1.00 1 -4 -36 5.40 1.20 1 -4 -36 4.40 0.60 -2 -4 -36 36.30 2.10 -2 -4 -36 35.60 2.50 2 4 -36 37.80 2.10 2 -4 -36 38.30 2.10 2 -4 -36 39.30 2.70 -2 4 -36 32.40 2.10 2 -4 -36 34.70 2.20 3 4 -36 15.20 1.00 -3 -4 -36 12.30 0.90 3 -4 -36 13.80 1.00 3 -4 -36 15.70 1.80 3 -4 -36 15.20 1.00 -3 4 -36 13.50 1.00 0 -5 -36 1.00 0.70 0 -5 -36 0.70 0.30 1 5 -36 4.50 0.60 -1 -5 -36 7.00 0.70 -1 -5 -36 7.50 1.30 1 -5 -36 6.30 0.70 -1 5 -36 5.10 0.80 1 -5 -36 8.00 1.00 1 -5 -36 7.00 1.30 1 -5 -36 7.50 0.60 2 5 -36 2.30 0.50 -2 -5 -36 2.20 0.50 -2 5 -36 2.10 0.50 2 -5 -36 1.60 0.40 2 -5 -36 1.20 0.70 2 -5 -36 2.90 0.40 0 -6 -36 1.40 0.30 -1 -6 -36 75.49 3.70 0 0 -37 -0.90 0.50 0 0 -37 -0.30 0.20 0 0 -37 0.00 0.40 0 0 -37 -0.10 0.80 -1 0 -37 32.30 2.30 -1 0 -37 39.20 3.00 1 0 -37 38.40 2.10 -1 0 -37 30.80 2.00 1 0 -37 38.10 2.90 1 0 -37 35.40 2.30 2 0 -37 13.30 1.60 -2 0 -37 12.20 1.30 2 0 -37 13.60 1.10 -2 0 -37 13.40 1.00 -2 0 -37 14.70 1.80 3 0 -37 13.30 0.90 -3 0 -37 11.70 0.90 3 0 -37 10.90 1.00 -3 0 -37 14.80 1.60 -3 0 -37 14.40 0.90 0 -1 -37 2.80 0.80 0 -1 -37 2.80 0.50 0 -1 -37 4.60 1.30 0 1 -37 3.30 0.40 0 1 -37 3.00 0.70 0 1 -37 2.80 1.00 0 -1 -37 4.40 0.50 -1 -1 -37 2.50 0.60 1 1 -37 4.70 0.80 1 1 -37 3.30 0.50 -1 -1 -37 2.20 0.60 1 1 -37 2.20 0.90 -1 -1 -37 2.80 1.10 1 -1 -37 3.60 0.60 -1 1 -37 3.30 0.70 -1 1 -37 3.00 0.50 1 -1 -37 3.90 0.80 1 -1 -37 3.00 1.00 -1 1 -37 3.50 1.10 2 1 -37 5.20 1.20 2 1 -37 6.30 0.70 2 1 -37 6.80 0.80 -2 -1 -37 6.20 0.80 -2 -1 -37 7.70 1.50 -2 -1 -37 6.60 0.70 2 -1 -37 8.60 1.50 -2 1 -37 7.80 1.40 2 -1 -37 7.10 0.90 2 -1 -37 7.60 0.80 -2 1 -37 6.50 0.90 -2 1 -37 5.90 0.60 -3 -1 -37 5.30 0.60 3 1 -37 6.90 0.70 -3 -1 -37 6.30 1.10 -3 1 -37 5.10 0.60 3 -1 -37 5.30 0.70 3 -1 -37 5.70 0.60 -3 1 -37 5.10 0.60 -3 1 -37 7.10 1.20 0 2 -37 11.30 1.60 0 -2 -37 8.10 0.60 0 2 -37 6.90 0.90 0 -2 -37 7.60 1.00 0 -2 -37 9.00 1.60 0 -2 -37 6.40 0.70 -1 -2 -37 2.70 1.00 1 2 -37 3.20 0.60 -1 -2 -37 3.20 0.70 1 2 -37 3.70 1.10 -1 -2 -37 3.00 0.60 1 2 -37 3.60 0.80 1 -2 -37 3.30 1.00 1 -2 -37 2.80 0.50 1 -2 -37 2.60 0.60 -1 2 -37 2.60 0.60 -1 2 -37 2.30 0.90 -2 -2 -37 28.90 2.40 -2 -2 -37 20.50 1.50 -2 -2 -37 24.10 1.50 2 2 -37 25.10 1.50 2 2 -37 21.60 1.50 -2 2 -37 20.20 1.60 -2 2 -37 23.50 1.60 2 -2 -37 24.60 1.50 -2 2 -37 25.00 2.00 2 -2 -37 25.70 2.20 2 -2 -37 25.00 1.70 3 2 -37 86.59 4.10 -3 -2 -37 75.49 4.00 3 -2 -37 90.79 4.10 3 -2 -37 73.69 4.20 -3 2 -37 78.49 4.20 3 -2 -37 89.79 4.80 0 -3 -37 12.00 1.10 0 -3 -37 9.70 0.90 0 3 -37 11.40 1.10 0 -3 -37 11.70 1.70 -1 -3 -37 2.90 0.50 -1 -3 -37 1.30 0.50 1 3 -37 1.10 0.40 -1 -3 -37 1.70 1.10 1 3 -37 2.30 0.40 -1 3 -37 1.70 0.60 1 -3 -37 1.40 0.90 1 -3 -37 1.20 0.60 1 -3 -37 1.90 0.40 2 3 -37 12.30 0.90 -2 -3 -37 12.70 1.50 -2 -3 -37 12.30 1.00 2 -3 -37 14.40 1.00 -2 3 -37 11.20 1.00 2 -3 -37 11.80 1.50 2 -3 -37 12.30 1.00 0 -4 -37 23.70 1.50 0 -4 -37 30.20 2.20 0 -4 -37 25.50 1.60 0 4 -37 23.40 1.60 -1 -4 -37 15.60 1.60 -1 -4 -37 13.40 1.00 1 -4 -37 13.40 1.10 -1 4 -37 12.20 1.00 1 -4 -37 15.00 1.60 1 -4 -37 14.20 0.90 2 4 -37 2.60 0.40 -2 -4 -37 3.00 0.50 -2 4 -37 1.30 0.50 2 -4 -37 2.60 0.80 2 -4 -37 3.10 0.40 -1 -5 -37 1.70 0.30 0 0 -38 9.30 1.50 0 0 -38 8.30 1.00 -1 0 -38 0.60 0.40 1 0 -38 0.50 0.70 1 0 -38 1.10 0.30 -1 0 -38 1.40 0.80 -1 0 -38 1.20 0.60 1 0 -38 1.30 0.50 -2 0 -38 25.90 1.70 -2 0 -38 32.40 2.20 2 0 -38 33.20 1.70 2 0 -38 29.80 1.80 -2 0 -38 24.10 1.60 0 -1 -38 0.30 0.50 0 1 -38 -0.70 0.70 0 1 -38 -0.10 0.40 0 -1 -38 -1.00 1.30 1 1 -38 18.70 1.10 -1 -1 -38 18.90 1.90 -1 -1 -38 17.60 1.40 -1 -1 -38 16.60 1.20 1 1 -38 22.60 2.10 1 1 -38 18.40 1.40 -1 1 -38 20.30 1.50 1 -1 -38 20.10 1.20 -1 1 -38 20.30 1.90 1 -1 -38 21.10 1.90 1 -1 -38 18.10 1.50 2 1 -38 13.30 1.00 2 1 -38 15.80 1.00 -2 -1 -38 12.90 1.10 -2 -1 -38 14.90 1.00 -2 -1 -38 14.00 1.60 2 -1 -38 16.20 1.00 2 -1 -38 17.60 2.00 -2 1 -38 18.60 1.60 2 -1 -38 14.70 1.10 -2 1 -38 13.70 1.10 0 -2 -38 1.40 0.50 0 -2 -38 0.40 0.70 0 2 -38 0.60 0.40 -1 -2 -38 1.70 0.80 -1 -2 -38 0.90 0.40 1 2 -38 1.40 0.50 1 2 -38 1.40 0.40 -1 -2 -38 2.70 0.40 -1 2 -38 1.50 0.90 1 -2 -38 1.80 0.30 1 -2 -38 1.80 0.50 -1 2 -38 2.10 0.60 1 -2 -38 1.40 0.80 -2 -2 -38 13.80 1.50 2 2 -38 16.00 1.00 -2 -2 -38 12.80 1.00 2 -2 -38 12.10 1.00 2 -2 -38 12.20 1.50 2 -2 -38 14.00 0.90 -2 2 -38 13.20 1.10 0 -3 -38 23.50 2.00 0 3 -38 20.30 1.40 0 -3 -38 21.00 1.40 -1 -3 -38 29.50 2.20 -1 -3 -38 24.10 1.60 1 -3 -38 26.60 1.70 -1 3 -38 24.60 1.60 1 -3 -38 29.10 2.20 2 -3 -38 12.70 0.90 -2 3 -38 12.20 0.90 2 -3 -38 12.70 1.30 0 -4 -38 6.10 1.10 1 -4 -38 12.70 1.30 0 0 -39 0.20 0.70 0 0 -39 -0.30 0.30 -1 0 -39 0.00 0.60 1 0 -39 0.20 0.40 -1 0 -39 0.00 0.50 0 1 -39 43.00 2.50 0 -1 -39 46.40 2.60 0 -1 -39 48.90 3.00 -1 -1 -39 17.40 1.60 1 1 -39 14.20 1.20 -1 -1 -39 14.80 1.20 -1 1 -39 15.90 1.20 1 -1 -39 16.20 1.60 1 -1 -39 15.70 1.10 0 -2 -39 72.09 3.90 0 -2 -39 68.59 3.60 0 2 -39 57.79 3.50 -1 -2 -39 20.10 2.30 1 -2 -39 16.80 1.40 1 -2 -39 13.80 1.10 -1 2 -39 15.60 1.10 0 -3 -39 34.80 2.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 65647 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 0.0534(4) 0.4387(3) 0.21976(10) 0.0293(7) Uani d . . . 1 . . H H6O 0.126(8) 0.013(5) 0.3212(19) 0.040(16) Uiso d . . . 1 . . C C1 0.1221(6) 0.5966(4) 0.36421(13) 0.0230(8) Uani d . . . 1 . . H H1 0.232078 0.645822 0.363313 0.028 Uiso calc U . R 1 . . O O2 0.1506(4) 0.2637(3) 0.35388(12) 0.0315(8) Uani d . . . 1 . . H H2 0.172(4) 0.201(5) 0.347(2) 0.047 Uiso calc U . R 1 . . C C2 0.0714(5) 0.5684(4) 0.31913(14) 0.0221(8) Uani d . . . 1 . . O O3 -0.0648(4) 0.5924(3) 0.25284(10) 0.0288(7) Uani d . . . 1 . . C C3 0.1302(6) 0.4827(4) 0.29389(13) 0.0226(8) Uani d . . . 1 . . O O4 0.4903(4) 0.1482(3) 0.21974(10) 0.0303(7) Uani d . . . 1 . . C C4 0.2724(6) 0.3914(4) 0.29936(14) 0.0252(9) Uani d . . . 1 . . H H4A 0.387926 0.426162 0.290689 0.03 Uiso calc U . R 1 . . H H4B 0.246378 0.328029 0.278935 0.03 Uiso calc U . R 1 . . O O5 0.6856(4) 0.2487(3) 0.25944(9) 0.0266(7) Uani d . . . 1 . . C C5 0.2984(5) 0.3367(4) 0.34355(14) 0.0226(8) Uani d . . . 1 . . H H5 0.406103 0.285545 0.34163 0.027 Uiso calc U . R 1 . . O O6 0.2038(4) 0.0263(3) 0.34123(10) 0.0256(6) Uani d . . . 1 . . C C6 0.3299(6) 0.4198(4) 0.38108(14) 0.0248(9) Uani d . . . 1 . . H H6 0.355956 0.370033 0.406526 0.03 Uiso calc U . R 1 . . C C7 0.1625(6) 0.4908(4) 0.39242(14) 0.0257(9) Uani d . . . 1 . . H H7 0.057196 0.437512 0.390799 0.031 Uiso calc U . R 1 . . C C11 -0.0550(6) 0.6436(4) 0.29493(14) 0.0274(9) Uani d . . . 1 . . H H11A -0.174054 0.644259 0.308731 0.033 Uiso calc U . R 1 . . H H11B -0.009668 0.724183 0.29331 0.033 Uiso calc U . R 1 . . C C10 -0.0210(7) 0.6628(4) 0.38978(15) 0.0331(10) Uani d . . . 1 . . H H10A -0.142118 0.636846 0.381378 0.04 Uiso calc U . R 1 . . H H10B -0.011249 0.747241 0.384428 0.04 Uiso calc U . R 1 . . C C9 0.0139(7) 0.6356(4) 0.43783(15) 0.0338(11) Uani d . . . 1 . . C C8 0.1648(8) 0.5446(5) 0.43733(15) 0.0381(12) Uani d . . . 1 . . H H8A 0.281663 0.581821 0.443074 0.046 Uiso calc U . R 1 . . H H8B 0.143298 0.484479 0.459335 0.046 Uiso calc U . R 1 . . C C13 0.4963(6) 0.4948(4) 0.37394(15) 0.0284(9) Uani d . . . 1 . . H H13A 0.601298 0.444618 0.370886 0.043 Uiso calc U . R 1 . . H H13B 0.512975 0.546572 0.398467 0.043 Uiso calc U . R 1 . . H H13C 0.480984 0.541036 0.347909 0.043 Uiso calc U . R 1 . . C C12 0.0418(6) 0.4967(4) 0.25211(14) 0.0242(9) Uani d . . . 1 . . C C16 0.7015(5) 0.1007(4) 0.36673(13) 0.0215(8) Uani d . . . 1 . . H H16 0.794518 0.03838 0.365955 0.026 Uiso calc U . R 1 . . C C15 -0.1551(8) 0.5810(6) 0.45781(19) 0.0483(14) Uani d . . . 1 . . H H15A -0.25619 0.634348 0.454535 0.072 Uiso calc U . R 1 . . H H15B -0.134271 0.566203 0.488264 0.072 Uiso calc U . R 1 . . H H15C -0.182222 0.507668 0.443297 0.072 Uiso calc U . R 1 . . C C14 0.0624(10) 0.7430(5) 0.4632(2) 0.0576(17) Uani d . . . 1 . . H H14A 0.169644 0.778683 0.450963 0.086 Uiso calc U . R 1 . . H H14B 0.085745 0.721335 0.493028 0.086 Uiso calc U . R 1 . . H H14C -0.036863 0.798409 0.462175 0.086 Uiso calc U . R 1 . . C C17 0.6643(6) 0.1387(4) 0.32180(13) 0.0211(8) Uani d . . . 1 . . C C18 0.5576(6) 0.0893(3) 0.29278(13) 0.0216(8) Uani d . . . 1 . . C C19 0.4534(6) -0.0221(4) 0.29350(13) 0.0259(9) Uani d . . . 1 . . H H19A 0.53783 -0.086234 0.287503 0.031 Uiso calc U . R 1 . . H H19B 0.366983 -0.019765 0.269531 0.031 Uiso calc U . R 1 . . C C20 0.3501(6) -0.0534(4) 0.33395(13) 0.0237(9) Uani d . . . 1 . . H H20 0.295582 -0.131419 0.328862 0.028 Uiso calc U . R 1 . . C C21 0.4572(6) -0.0625(4) 0.37561(14) 0.0251(9) Uani d . . . 1 . . H H21 0.370922 -0.087553 0.398223 0.03 Uiso calc U . R 1 . . C C22 0.5365(6) 0.0537(4) 0.39068(13) 0.0219(8) Uani d . . . 1 . . H H22 0.440129 0.113321 0.387812 0.026 Uiso calc U . R 1 . . C C23 0.5967(6) 0.0541(4) 0.43816(14) 0.0298(10) Uani d . . . 1 . . H H23A 0.633886 -0.024704 0.447032 0.036 Uiso calc U . R 1 . . H H23B 0.497196 0.079583 0.456812 0.036 Uiso calc U . R 1 . . C C25 0.7651(6) 0.1964(4) 0.39716(13) 0.0246(9) Uani d . . . 1 . . H H25A 0.68543 0.264916 0.395603 0.03 Uiso calc U . R 1 . . H H25B 0.888562 0.220824 0.390179 0.03 Uiso calc U . R 1 . . C C24 0.7569(6) 0.1401(4) 0.44179(14) 0.0261(9) Uani d . . . 1 . . C C26 0.7543(6) 0.2420(4) 0.30226(13) 0.0245(9) Uani d . . . 1 . . H H26A 0.725218 0.313415 0.318439 0.029 Uiso calc U . R 1 . . H H26B 0.885647 0.231666 0.302002 0.029 Uiso calc U . R 1 . . C C28 0.5963(7) -0.1594(4) 0.37183(17) 0.0359(11) Uani d . . . 1 . . H H28A 0.537397 -0.23137 0.36295 0.054 Uiso calc U . R 1 . . H H28B 0.654342 -0.171093 0.399594 0.054 Uiso calc U . R 1 . . H H28C 0.686384 -0.137595 0.350525 0.054 Uiso calc U . R 1 . . C C29 0.9319(7) 0.0749(5) 0.45072(16) 0.0369(11) Uani d . . . 1 . . H H29A 0.952237 0.017287 0.428203 0.055 Uiso calc U . R 1 . . H H29B 0.923708 0.035716 0.478464 0.055 Uiso calc U . R 1 . . H H29C 1.031476 0.13016 0.451209 0.055 Uiso calc U . R 1 . . C C30 0.7271(8) 0.2319(4) 0.47625(14) 0.0351(11) Uani d . . . 1 . . H H30A 0.824843 0.288444 0.475426 0.053 Uiso calc U . R 1 . . H H30B 0.723912 0.19458 0.504397 0.053 Uiso calc U . R 1 . . H H30C 0.613284 0.271614 0.471042 0.053 Uiso calc U . R 1 . . C C27 0.5673(6) 0.1596(4) 0.25335(13) 0.0245(8) Uani d . . . 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 0.0250(17) 0.0335(16) 0.0293(15) -0.0025(14) -0.0022(13) -0.0025(13) C1 0.017(2) 0.0235(19) 0.029(2) 0.0034(16) -0.0025(17) 0.0004(16) O2 0.0206(16) 0.0212(15) 0.053(2) -0.0013(13) 0.0066(15) 0.0019(14) C2 0.0128(19) 0.0230(19) 0.031(2) 0.0000(16) -0.0055(17) 0.0043(16) O3 0.0263(16) 0.0310(15) 0.0290(15) 0.0054(13) -0.0068(13) 0.0010(12) C3 0.016(2) 0.0236(19) 0.028(2) -0.0028(16) -0.0013(16) 0.0025(16) O4 0.0255(17) 0.0388(17) 0.0265(15) 0.0039(14) -0.0037(13) 0.0013(13) C4 0.019(2) 0.027(2) 0.030(2) 0.0037(17) -0.0011(17) -0.0032(17) O5 0.0221(16) 0.0296(15) 0.0280(14) -0.0023(13) -0.0010(12) 0.0040(12) C5 0.0100(19) 0.0230(19) 0.035(2) 0.0019(15) 0.0038(17) 0.0026(17) O6 0.0183(15) 0.0276(15) 0.0308(15) 0.0024(12) -0.0028(13) -0.0044(12) C6 0.022(2) 0.025(2) 0.028(2) 0.0049(17) -0.0027(17) 0.0044(16) C7 0.024(2) 0.026(2) 0.027(2) 0.0061(18) -0.0022(18) 0.0026(17) C11 0.023(2) 0.029(2) 0.030(2) 0.0058(18) -0.0063(18) 0.0007(17) C10 0.032(3) 0.036(2) 0.032(2) 0.014(2) -0.001(2) -0.0014(19) C9 0.041(3) 0.032(2) 0.029(2) 0.010(2) -0.004(2) -0.0051(18) C8 0.041(3) 0.046(3) 0.028(2) 0.016(2) -0.003(2) -0.001(2) C13 0.014(2) 0.032(2) 0.039(2) 0.0014(17) -0.0058(18) -0.0015(18) C12 0.013(2) 0.028(2) 0.031(2) -0.0032(16) -0.0014(17) 0.0033(17) C16 0.016(2) 0.0245(19) 0.0241(19) -0.0006(16) -0.0023(16) 0.0000(15) C15 0.041(3) 0.059(4) 0.045(3) 0.010(3) 0.000(3) 0.002(3) C14 0.071(5) 0.043(3) 0.058(4) 0.005(3) -0.019(4) -0.012(3) C17 0.0131(19) 0.0240(19) 0.0260(19) 0.0030(15) 0.0023(16) 0.0001(15) C18 0.0161(19) 0.0239(19) 0.0249(18) 0.0028(16) 0.0017(16) -0.0020(15) C19 0.026(2) 0.0246(19) 0.027(2) -0.0013(18) -0.0012(18) -0.0042(16) C20 0.021(2) 0.0204(19) 0.030(2) 0.0014(16) -0.0004(17) -0.0019(16) C21 0.023(2) 0.0230(19) 0.029(2) -0.0024(17) -0.0001(18) 0.0027(16) C22 0.015(2) 0.0250(19) 0.0254(18) 0.0005(16) -0.0017(16) 0.0017(15) C23 0.027(2) 0.037(2) 0.026(2) -0.0066(19) -0.0029(18) 0.0037(18) C25 0.020(2) 0.028(2) 0.025(2) -0.0048(17) -0.0015(17) -0.0005(16) C24 0.025(2) 0.029(2) 0.025(2) 0.0001(18) -0.0005(18) -0.0015(17) C26 0.017(2) 0.030(2) 0.026(2) -0.0030(18) 0.0009(16) 0.0019(17) C28 0.032(3) 0.025(2) 0.051(3) 0.005(2) -0.011(2) 0.001(2) C29 0.033(3) 0.043(3) 0.035(2) 0.008(2) -0.011(2) 0.000(2) C30 0.041(3) 0.036(2) 0.028(2) 0.000(2) 0.002(2) -0.0034(19) C27 0.020(2) 0.027(2) 0.027(2) 0.0041(17) 0.0006(17) -0.0013(16) 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 C1 C7 . . 114.8(4) ? C2 C1 C10 . . 114.9(4) ? C7 C1 C10 . . 103.4(4) ? C2 C1 H1 . . 107.8 ? C7 C1 H1 . . 107.8 ? C10 C1 H1 . . 107.8 ? C5 O2 H2 . . 109.5 ? C3 C2 C11 . . 109.8(4) ? C3 C2 C1 . . 129.2(4) ? C11 C2 C1 . . 120.9(4) ? C12 O3 C11 . . 108.4(3) ? C2 C3 C12 . . 107.2(4) ? C2 C3 C4 . . 132.9(4) ? C12 C3 C4 . . 119.6(4) ? C3 C4 C5 . . 118.7(4) ? C3 C4 H4A . . 107.6 ? C5 C4 H4A . . 107.6 ? C3 C4 H4B . . 107.6 ? C5 C4 H4B . . 107.6 ? H4A C4 H4B . . 107.1 ? C27 O5 C26 . . 108.7(3) ? O2 C5 C4 . . 110.4(4) ? O2 C5 C6 . . 108.3(4) ? C4 C5 C6 . . 116.9(3) ? O2 C5 H5 . . 106.9 ? C4 C5 H5 . . 106.9 ? C6 C5 H5 . . 106.9 ? C20 O6 H6O . . 106.(4) ? C13 C6 C5 . . 111.4(4) ? C13 C6 C7 . . 113.3(4) ? C5 C6 C7 . . 112.6(4) ? C13 C6 H6 . . 106.3 ? C5 C6 H6 . . 106.3 ? C7 C6 H6 . . 106.3 ? C6 C7 C1 . . 116.8(4) ? C6 C7 C8 . . 114.6(4) ? C1 C7 C8 . . 101.9(4) ? C6 C7 H7 . . 107.7 ? C1 C7 H7 . . 107.7 ? C8 C7 H7 . . 107.7 ? O3 C11 C2 . . 104.9(3) ? O3 C11 H11A . . 110.8 ? C2 C11 H11A . . 110.8 ? O3 C11 H11B . . 110.8 ? C2 C11 H11B . . 110.8 ? H11A C11 H11B . . 108.8 ? C1 C10 C9 . . 106.6(4) ? C1 C10 H10A . . 110.4 ? C9 C10 H10A . . 110.4 ? C1 C10 H10B . . 110.4 ? C9 C10 H10B . . 110.4 ? H10A C10 H10B . . 108.6 ? C14 C9 C8 . . 112.7(5) ? C14 C9 C15 . . 108.5(5) ? C8 C9 C15 . . 109.1(4) ? C14 C9 C10 . . 112.5(4) ? C8 C9 C10 . . 104.5(4) ? C15 C9 C10 . . 109.6(4) ? C7 C8 C9 . . 106.0(4) ? C7 C8 H8A . . 110.5 ? C9 C8 H8A . . 110.5 ? C7 C8 H8B . . 110.5 ? C9 C8 H8B . . 110.5 ? H8A C8 H8B . . 108.7 ? C6 C13 H13A . . 109.5 ? C6 C13 H13B . . 109.5 ? H13A C13 H13B . . 109.5 ? C6 C13 H13C . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? O1 C12 O3 . . 120.1(4) ? O1 C12 C3 . . 130.3(4) ? O3 C12 C3 . . 109.7(4) ? C17 C16 C25 . . 115.4(4) ? C17 C16 C22 . . 114.2(3) ? C25 C16 C22 . . 101.5(3) ? C17 C16 H16 . . 108.5 ? C25 C16 H16 . . 108.5 ? C22 C16 H16 . . 108.5 ? C9 C15 H15A . . 109.5 ? C9 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C9 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? C9 C14 H14A . . 109.5 ? C9 C14 H14B . . 109.5 ? H14A C14 H14B . . 109.5 ? C9 C14 H14C . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 109.5 ? C18 C17 C16 . . 128.6(4) ? C18 C17 C26 . . 109.3(4) ? C16 C17 C26 . . 122.1(4) ? C17 C18 C27 . . 107.7(4) ? C17 C18 C19 . . 131.6(4) ? C27 C18 C19 . . 120.5(4) ? C18 C19 C20 . . 118.5(3) ? C18 C19 H19A . . 107.7 ? C20 C19 H19A . . 107.7 ? C18 C19 H19B . . 107.7 ? C20 C19 H19B . . 107.7 ? H19A C19 H19B . . 107.1 ? O6 C20 C19 . . 111.3(3) ? O6 C20 C21 . . 107.8(3) ? C19 C20 C21 . . 117.1(4) ? O6 C20 H20 . . 106.7 ? C19 C20 H20 . . 106.7 ? C21 C20 H20 . . 106.7 ? C28 C21 C20 . . 109.9(4) ? C28 C21 C22 . . 113.3(4) ? C20 C21 C22 . . 113.7(3) ? C28 C21 H21 . . 106.5 ? C20 C21 H21 . . 106.5 ? C22 C21 H21 . . 106.5 ? C21 C22 C16 . . 117.8(3) ? C21 C22 C23 . . 114.1(3) ? C16 C22 C23 . . 103.4(3) ? C21 C22 H22 . . 107.0 ? C16 C22 H22 . . 107.0 ? C23 C22 H22 . . 107.0 ? C22 C23 C24 . . 107.1(4) ? C22 C23 H23A . . 110.3 ? C24 C23 H23A . . 110.3 ? C22 C23 H23B . . 110.3 ? C24 C23 H23B . . 110.3 ? H23A C23 H23B . . 108.5 ? C16 C25 C24 . . 104.3(3) ? C16 C25 H25A . . 110.9 ? C24 C25 H25A . . 110.9 ? C16 C25 H25B . . 110.9 ? C24 C25 H25B . . 110.9 ? H25A C25 H25B . . 108.9 ? C30 C24 C29 . . 109.6(4) ? C30 C24 C25 . . 110.7(4) ? C29 C24 C25 . . 109.7(4) ? C30 C24 C23 . . 112.3(4) ? C29 C24 C23 . . 111.0(4) ? C25 C24 C23 . . 103.4(3) ? O5 C26 C17 . . 105.2(3) ? O5 C26 H26A . . 110.7 ? C17 C26 H26A . . 110.7 ? O5 C26 H26B . . 110.7 ? C17 C26 H26B . . 110.7 ? H26A C26 H26B . . 108.8 ? C21 C28 H28A . . 109.5 ? C21 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? C21 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? C24 C29 H29A . . 109.5 ? C24 C29 H29B . . 109.5 ? H29A C29 H29B . . 109.5 ? C24 C29 H29C . . 109.5 ? H29A C29 H29C . . 109.5 ? H29B C29 H29C . . 109.5 ? C24 C30 H30A . . 109.5 ? C24 C30 H30B . . 109.5 ? H30A C30 H30B . . 109.5 ? C24 C30 H30C . . 109.5 ? H30A C30 H30C . . 109.5 ? H30B C30 H30C . . 109.5 ? O4 C27 O5 . . 120.8(4) ? O4 C27 C18 . . 130.1(4) ? O5 C27 C18 . . 109.1(4) ? 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 C12 . 1.216(5) ? C1 C2 . 1.496(6) ? C1 C7 . 1.535(6) ? C1 C10 . 1.539(6) ? C1 H1 . 1.0 ? O2 C5 . 1.426(5) ? O2 H2 . 0.76(6) ? C2 C3 . 1.338(6) ? C2 C11 . 1.489(6) ? O3 C12 . 1.362(5) ? O3 C11 . 1.444(5) ? C3 C12 . 1.473(6) ? C3 C4 . 1.506(6) ? O4 C27 . 1.206(5) ? C4 C5 . 1.532(6) ? C4 H4A . 0.99 ? C4 H4B . 0.99 ? O5 C27 . 1.369(5) ? O5 C26 . 1.436(5) ? C5 C6 . 1.533(6) ? C5 H5 . 1.0 ? O6 C20 . 1.447(5) ? O6 H6O . 0.87(6) ? C6 C13 . 1.532(6) ? C6 C7 . 1.537(6) ? C6 H6 . 1.0 ? C7 C8 . 1.536(6) ? C7 H7 . 1.0 ? C11 H11A . 0.99 ? C11 H11B . 0.99 ? C10 C9 . 1.557(6) ? C10 H10A . 0.99 ? C10 H10B . 0.99 ? C9 C14 . 1.515(7) ? C9 C8 . 1.540(7) ? C9 C15 . 1.545(8) ? C8 H8A . 0.99 ? C8 H8B . 0.99 ? C13 H13A . 0.98 ? C13 H13B . 0.98 ? C13 H13C . 0.98 ? C16 C17 . 1.498(5) ? C16 C25 . 1.533(6) ? C16 C22 . 1.542(6) ? C16 H16 . 1.0 ? C15 H15A . 0.98 ? C15 H15B . 0.98 ? C15 H15C . 0.98 ? C14 H14A . 0.98 ? C14 H14B . 0.98 ? C14 H14C . 0.98 ? C17 C18 . 1.336(6) ? C17 C26 . 1.498(6) ? C18 C27 . 1.477(6) ? C18 C19 . 1.502(6) ? C19 C20 . 1.526(6) ? C19 H19A . 0.99 ? C19 H19B . 0.99 ? C20 C21 . 1.533(6) ? C20 H20 . 1.0 ? C21 C28 . 1.530(6) ? C21 C22 . 1.539(6) ? C21 H21 . 1.0 ? C22 C23 . 1.552(6) ? C22 H22 . 1.0 ? C23 C24 . 1.559(6) ? C23 H23A . 0.99 ? C23 H23B . 0.99 ? C25 C24 . 1.541(6) ? C25 H25A . 0.99 ? C25 H25B . 0.99 ? C24 C30 . 1.526(6) ? C24 C29 . 1.535(7) ? C26 H26A . 0.99 ? C26 H26B . 0.99 ? C28 H28A . 0.98 ? C28 H28B . 0.98 ? C28 H28C . 0.98 ? C29 H29A . 0.98 ? C29 H29B . 0.98 ? C29 H29C . 0.98 ? C30 H30A . 0.98 ? C30 H30B . 0.98 ? C30 H30C . 0.98 ? 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 C7 C1 C2 C3 . . . . -34.8(6) ? C10 C1 C2 C3 . . . . -154.6(5) ? C7 C1 C2 C11 . . . . 148.5(4) ? C10 C1 C2 C11 . . . . 28.7(6) ? C11 C2 C3 C12 . . . . -1.1(5) ? C1 C2 C3 C12 . . . . -178.1(4) ? C11 C2 C3 C4 . . . . 171.9(5) ? C1 C2 C3 C4 . . . . -5.2(8) ? C2 C3 C4 C5 . . . . 37.1(7) ? C12 C3 C4 C5 . . . . -150.7(4) ? C3 C4 C5 O2 . . . . 70.3(5) ? C3 C4 C5 C6 . . . . -54.1(5) ? O2 C5 C6 C13 . . . . 175.4(3) ? C4 C5 C6 C13 . . . . -59.1(5) ? O2 C5 C6 C7 . . . . -56.0(4) ? C4 C5 C6 C7 . . . . 69.5(5) ? C13 C6 C7 C1 . . . . 47.9(5) ? C5 C6 C7 C1 . . . . -79.7(5) ? C13 C6 C7 C8 . . . . -71.2(5) ? C5 C6 C7 C8 . . . . 161.2(4) ? C2 C1 C7 C6 . . . . 67.1(5) ? C10 C1 C7 C6 . . . . -166.9(4) ? C2 C1 C7 C8 . . . . -167.2(4) ? C10 C1 C7 C8 . . . . -41.2(5) ? C12 O3 C11 C2 . . . . 0.6(5) ? C3 C2 C11 O3 . . . . 0.3(5) ? C1 C2 C11 O3 . . . . 177.6(4) ? C2 C1 C10 C9 . . . . 155.1(4) ? C7 C1 C10 C9 . . . . 29.2(5) ? C1 C10 C9 C14 . . . . 117.0(5) ? C1 C10 C9 C8 . . . . -5.5(5) ? C1 C10 C9 C15 . . . . -122.2(5) ? C6 C7 C8 C9 . . . . 165.6(4) ? C1 C7 C8 C9 . . . . 38.5(5) ? C14 C9 C8 C7 . . . . -142.8(5) ? C15 C9 C8 C7 . . . . 96.7(5) ? C10 C9 C8 C7 . . . . -20.4(6) ? C11 O3 C12 O1 . . . . 179.4(4) ? C11 O3 C12 C3 . . . . -1.3(5) ? C2 C3 C12 O1 . . . . -179.3(5) ? C4 C3 C12 O1 . . . . 6.7(7) ? C2 C3 C12 O3 . . . . 1.5(5) ? C4 C3 C12 O3 . . . . -172.5(4) ? C25 C16 C17 C18 . . . . -156.2(4) ? C22 C16 C17 C18 . . . . -39.1(6) ? C25 C16 C17 C26 . . . . 26.2(6) ? C22 C16 C17 C26 . . . . 143.3(4) ? C16 C17 C18 C27 . . . . -179.7(4) ? C26 C17 C18 C27 . . . . -1.9(5) ? C16 C17 C18 C19 . . . . -5.6(8) ? C26 C17 C18 C19 . . . . 172.3(4) ? C17 C18 C19 C20 . . . . 43.5(7) ? C27 C18 C19 C20 . . . . -143.0(4) ? C18 C19 C20 O6 . . . . 66.9(5) ? C18 C19 C20 C21 . . . . -57.7(5) ? O6 C20 C21 C28 . . . . 171.5(4) ? C19 C20 C21 C28 . . . . -62.1(5) ? O6 C20 C21 C22 . . . . -60.3(5) ? C19 C20 C21 C22 . . . . 66.1(5) ? C28 C21 C22 C16 . . . . 51.1(5) ? C20 C21 C22 C16 . . . . -75.3(5) ? C28 C21 C22 C23 . . . . -70.3(5) ? C20 C21 C22 C23 . . . . 163.3(4) ? C17 C16 C22 C21 . . . . 68.6(5) ? C25 C16 C22 C21 . . . . -166.5(4) ? C17 C16 C22 C23 . . . . -164.7(4) ? C25 C16 C22 C23 . . . . -39.8(4) ? C21 C22 C23 C24 . . . . 149.5(4) ? C16 C22 C23 C24 . . . . 20.4(5) ? C17 C16 C25 C24 . . . . 169.2(4) ? C22 C16 C25 C24 . . . . 45.2(4) ? C16 C25 C24 C30 . . . . -152.6(4) ? C16 C25 C24 C29 . . . . 86.4(4) ? C16 C25 C24 C23 . . . . -32.1(4) ? C22 C23 C24 C30 . . . . 126.3(4) ? C22 C23 C24 C29 . . . . -110.6(4) ? C22 C23 C24 C25 . . . . 6.9(5) ? C27 O5 C26 C17 . . . . -0.1(4) ? C18 C17 C26 O5 . . . . 1.3(5) ? C16 C17 C26 O5 . . . . 179.3(4) ? C26 O5 C27 O4 . . . . 179.1(4) ? C26 O5 C27 C18 . . . . -1.0(5) ? C17 C18 C27 O4 . . . . -178.2(5) ? C19 C18 C27 O4 . . . . 6.8(7) ? C17 C18 C27 O5 . . . . 1.9(5) ? C19 C18 C27 O5 . . . . -173.1(4) ?