#------------------------------------------------------------------------------ #$Date: 2020-02-21 01:54:06 +0200 (Fri, 21 Feb 2020) $ #$Revision: 248347 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557353.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_1557353 loop_ _publ_author_name 'Huang, Yanjie' 'Li, Xian' 'Peng, Xing-Rong' 'Adegoke, Adelakum Tiwalade' 'Chen, Jian-Chao' 'Su, Hai-Guo' 'Hu, Gui-Lin' 'Wei, Gang' 'Qiu, Ming-Hua' _publ_section_title ; NMR-based Structural Classification, Identification, and Quantification of Triterpenoids from Edible Mushroom Ganoderma resinaceum. ; _journal_name_full 'Journal of agricultural and food chemistry' _journal_paper_doi 10.1021/acs.jafc.9b07791 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C30 H44 O7' _chemical_formula_sum 'C30 H44 O7' _chemical_formula_weight 516.65 _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 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7074(2) _cell_length_b 11.7878(3) _cell_length_c 26.4646(6) _cell_measurement_reflns_used 9958 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 72.3604 _cell_measurement_theta_min 3.3400 _cell_volume 2716.36(11) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 VENTURE 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 0.0779 _diffrn_reflns_av_unetI/netI 0.0473 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 25491 _diffrn_reflns_theta_full 72.35 _diffrn_reflns_theta_max 72.35 _diffrn_reflns_theta_min 3.34 _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'translucent light colourless' _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1120 _exptl_crystal_size_max 0.470 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.227 _refine_diff_density_min -0.244 _refine_ls_abs_structure_details ; Flack x determined using 1966 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.08(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 345 _refine_ls_number_reflns 5367 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.893 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0415 _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1126 _refine_ls_wR_factor_ref 0.1190 _reflns_number_gt 4873 _reflns_number_total 5367 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jf9b07791_si_003.cif _cod_data_source_block kgr355 _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 1557353 _shelx_res_file ; TITL kgr355_0m_a.res in P2(1)2(1)2(1) kgr355_0m.res created by SHELXL-2017/1 at 23:16:32 on 06-Jun-2019 CELL 1.54178 8.7074 11.7878 26.4646 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0003 0.0006 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 28 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.160 SIZE 0.020 0.150 0.470 ACTA EQIV $1 -x+1, y+1/2, -z+3/2 HTAB O1 O3_$1 EQIV $2 -x+1, y-1/2, -z+3/2 HTAB O3 O2_$2 EQIV $3 -x+2, y-1/2, -z+3/2 HTAB O3 O5_$3 HTAB O5 O4_$1 EQIV $4 x+1, y, z HTAB O6 O2_$4 HTAB C1 O5_$3 EQIV $5 x+1/2, -y+3/2, -z+1 HTAB C14 O2_$5 HTAB C28 O5 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.100000 FVAR 0.59312 O1 3 -0.005723 0.818763 0.540334 11.00000 0.02966 0.02966 = 0.02468 -0.00137 -0.00064 -0.00546 AFIX 147 H41 2 -0.046669 0.827975 0.568779 11.00000 -1.50000 AFIX 0 O2 3 -0.131973 0.654722 0.543127 11.00000 0.01677 0.03155 = 0.03336 0.00372 0.00393 -0.00154 O3 3 1.140616 0.322375 0.869703 11.00000 0.01677 0.02826 = 0.02245 0.00034 -0.00451 0.00399 AFIX 147 H42 2 1.184617 0.259102 0.871601 11.00000 -1.50000 AFIX 0 O4 3 0.459580 0.244579 0.762237 11.00000 0.01915 0.03171 = 0.02344 0.00476 -0.00018 -0.00596 O5 3 0.723059 0.621189 0.665070 11.00000 0.01748 0.01987 = 0.02153 0.00159 -0.00096 0.00164 AFIX 147 H43 2 0.678952 0.653721 0.689295 11.00000 -1.50000 AFIX 0 O6 3 0.791809 0.433107 0.560153 11.00000 0.01597 0.03115 = 0.02654 0.00134 0.00702 -0.00048 AFIX 147 H44 2 0.823473 0.493565 0.546971 11.00000 -1.50000 AFIX 0 O7 3 0.182123 0.560826 0.557269 11.00000 0.02615 0.03496 = 0.02837 -0.00572 -0.00713 0.00636 C1 1 1.033467 0.321413 0.828051 11.00000 0.01463 0.02239 = 0.01945 0.00032 -0.00166 0.00234 AFIX 13 H1 2 1.077775 0.272922 0.800687 11.00000 -1.20000 AFIX 0 C2 1 1.016223 0.441977 0.807249 11.00000 0.01085 0.02410 = 0.02222 0.00127 -0.00122 -0.00068 C3 1 0.894663 0.434364 0.763830 11.00000 0.01142 0.02160 = 0.01895 -0.00035 0.00032 0.00048 AFIX 13 H30 2 0.941003 0.381290 0.738601 11.00000 -1.20000 AFIX 0 C4 1 0.872710 0.545372 0.735011 11.00000 0.01508 0.02275 = 0.02326 0.00285 -0.00337 -0.00269 AFIX 23 H14 2 0.804361 0.596368 0.754445 11.00000 -1.20000 H13 2 0.973087 0.583688 0.730841 11.00000 -1.20000 AFIX 0 C5 1 0.802773 0.521942 0.683391 11.00000 0.01459 0.02014 = 0.02099 0.00173 -0.00026 0.00052 AFIX 13 H31 2 0.888102 0.504324 0.659348 11.00000 -1.20000 AFIX 0 C6 1 0.691642 0.422334 0.683340 11.00000 0.01166 0.02273 = 0.02122 0.00051 -0.00053 0.00309 C7 1 0.627032 0.382218 0.633095 11.00000 0.01294 0.02234 = 0.01988 0.00083 0.00214 0.00095 C8 1 0.449357 0.376335 0.637948 11.00000 0.01198 0.02228 = 0.02020 0.00060 0.00016 -0.00173 C9 1 0.400707 0.366665 0.582310 11.00000 0.01695 0.02320 = 0.01864 -0.00204 -0.00143 0.00218 C10 1 0.243504 0.324891 0.567730 11.00000 0.01729 0.02815 = 0.02258 -0.00070 -0.00116 -0.00330 AFIX 13 H9 2 0.170632 0.345457 0.595461 11.00000 -1.20000 AFIX 0 C11 1 0.183781 0.377326 0.518635 11.00000 0.02016 0.03068 = 0.02447 -0.00241 -0.00385 0.00159 AFIX 23 H38 2 0.259620 0.362492 0.491559 11.00000 -1.20000 H37 2 0.087283 0.338362 0.509141 11.00000 -1.20000 AFIX 0 C12 1 0.153238 0.503857 0.520678 11.00000 0.01539 0.03260 = 0.02336 -0.00179 -0.00098 0.00162 C13 1 0.079270 0.555392 0.473792 11.00000 0.02099 0.02964 = 0.02452 0.00001 -0.00305 0.00122 AFIX 23 H5 2 0.144398 0.538446 0.444073 11.00000 -1.20000 H4 2 -0.021873 0.519104 0.468251 11.00000 -1.20000 AFIX 0 C14 1 0.057051 0.683235 0.477542 11.00000 0.01618 0.02933 = 0.02510 0.00224 -0.00240 -0.00363 AFIX 13 H3 2 0.159980 0.720606 0.479505 11.00000 -1.20000 AFIX 0 C15 1 -0.029352 0.728981 0.431145 11.00000 0.03177 0.03619 = 0.02350 0.00447 -0.00394 0.00131 AFIX 137 H2 2 -0.128744 0.690539 0.428205 11.00000 -1.50000 H39 2 0.031514 0.714803 0.400643 11.00000 -1.50000 H40 2 -0.045890 0.810754 0.435017 11.00000 -1.50000 AFIX 0 C16 1 -0.034687 0.714335 0.523834 11.00000 0.01445 0.02542 = 0.02349 0.00395 -0.00710 0.00179 C17 1 0.243698 0.194466 0.562361 11.00000 0.02916 0.02922 = 0.02899 0.00176 -0.00672 -0.00649 AFIX 137 H8 2 0.305787 0.172773 0.533026 11.00000 -1.50000 H7 2 0.138168 0.167514 0.557717 11.00000 -1.50000 H6 2 0.287261 0.160328 0.592932 11.00000 -1.50000 AFIX 0 C18 1 0.701242 0.264680 0.622642 11.00000 0.02010 0.02448 = 0.02481 -0.00234 -0.00092 0.00357 AFIX 137 H12 2 0.812423 0.273746 0.618540 11.00000 -1.50000 H11 2 0.657538 0.232424 0.591689 11.00000 -1.50000 H10 2 0.680578 0.213728 0.651102 11.00000 -1.50000 AFIX 0 C19 1 0.979340 0.527909 0.849046 11.00000 0.01993 0.02559 = 0.02846 -0.00287 -0.00501 0.00269 AFIX 137 H17 2 0.897659 0.497704 0.870680 11.00000 -1.50000 H16 2 0.945256 0.599336 0.833772 11.00000 -1.50000 H15 2 1.071539 0.541588 0.869391 11.00000 -1.50000 AFIX 0 C20 1 0.881267 0.268999 0.844290 11.00000 0.01768 0.02592 = 0.02494 0.00598 -0.00180 -0.00225 AFIX 23 H18 2 0.836471 0.314700 0.871999 11.00000 -1.20000 H26 2 0.899777 0.191469 0.857319 11.00000 -1.20000 AFIX 0 C21 1 0.767123 0.263444 0.800255 11.00000 0.01753 0.02246 = 0.02535 0.00263 -0.00291 -0.00113 AFIX 23 H19 2 0.669258 0.230644 0.812467 11.00000 -1.20000 H20 2 0.808483 0.212380 0.773857 11.00000 -1.20000 AFIX 0 C22 1 0.735048 0.381159 0.776687 11.00000 0.01290 0.02222 = 0.02022 0.00003 0.00012 -0.00105 C23 1 0.633350 0.452066 0.812208 11.00000 0.01427 0.02992 = 0.02587 -0.00336 0.00075 0.00136 AFIX 137 H22 2 0.619889 0.528252 0.798062 11.00000 -1.50000 H21 2 0.682500 0.457654 0.845428 11.00000 -1.50000 H23 2 0.532876 0.415465 0.815762 11.00000 -1.50000 AFIX 0 C24 1 0.648786 0.367355 0.726132 11.00000 0.01416 0.02060 = 0.02016 -0.00090 -0.00119 0.00077 C25 1 0.507639 0.293700 0.724710 11.00000 0.01451 0.02115 = 0.02202 0.00043 -0.00062 -0.00010 C26 1 0.412763 0.282910 0.675884 11.00000 0.01570 0.02604 = 0.02051 0.00087 -0.00117 -0.00444 AFIX 23 H24 2 0.433603 0.208253 0.660181 11.00000 -1.20000 H25 2 0.302148 0.285970 0.684426 11.00000 -1.20000 AFIX 0 C27 1 1.172783 0.474757 0.784226 11.00000 0.01390 0.03783 = 0.02772 0.00915 -0.00277 -0.00388 AFIX 137 H27 2 1.253962 0.462557 0.809292 11.00000 -1.50000 H28 2 1.171052 0.554862 0.774333 11.00000 -1.50000 H29 2 1.192808 0.427680 0.754424 11.00000 -1.50000 AFIX 0 C28 1 0.646885 0.453042 0.583981 11.00000 0.01639 0.02485 = 0.01847 0.00027 0.00176 -0.00089 AFIX 13 H32 2 0.635354 0.535618 0.591765 11.00000 -1.20000 AFIX 0 C29 1 0.509883 0.412145 0.553879 11.00000 0.01791 0.02563 = 0.02005 -0.00058 -0.00034 0.00069 AFIX 43 H33 2 0.502822 0.418438 0.518167 11.00000 -1.20000 AFIX 0 C30 1 0.379619 0.488260 0.658061 11.00000 0.01505 0.02434 = 0.02142 -0.00088 -0.00006 0.00048 AFIX 137 H36 2 0.267588 0.485704 0.654703 11.00000 -1.50000 H35 2 0.420050 0.552217 0.638497 11.00000 -1.50000 H34 2 0.407036 0.497769 0.693725 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM kgr355_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0415 for 4873 Fo > 4sig(Fo) and 0.0479 for all 5367 data REM 345 parameters refined using 0 restraints END WGHT 0.0618 0.1813 REM Instructions for potential hydrogen bonds HTAB O1 O3_$1 HTAB O3 O2_$2 HTAB O3 O5_$3 HTAB O5 O4_$1 HTAB O6 O2_$4 HTAB C1 O5_$3 HTAB C14 O2_$5 HTAB C28 O5 REM Highest difference peak 0.227, deepest hole -0.244, 1-sigma level 0.050 Q1 1 0.6607 0.4162 0.6561 11.00000 0.05 0.23 Q2 1 0.4783 0.2810 0.6985 11.00000 0.05 0.22 Q3 1 0.6525 0.4174 0.6099 11.00000 0.05 0.22 Q4 1 0.4129 0.3693 0.6087 11.00000 0.05 0.22 Q5 1 0.6417 0.4169 0.7077 11.00000 0.05 0.22 ; _shelx_res_checksum 48780 _shelx_hkl_file ; 1 0 0 -2.20 2.10 1 0 0 1.40 2.70 1 0 0 2.50 3.00 -1 0 0 1.90 1.70 -1 0 0 -1.30 1.60 -1 0 0 -1.10 1.70 -2 0 0 32.80 7.90 -2 0 0 31.60 6.70 -2 0 0 40.40 8.00 -3 0 0 -2.10 4.80 -3 0 0 9.20 5.40 -3 0 0 -2.60 3.80 -4 0 0 24.10 8.70 -4 0 0 7.60 7.10 -4 0 0 22.20 10.00 -5 0 0 -2.00 6.30 -5 0 0 2.70 8.40 -5 0 0 8.20 11.40 -6 0 0 742.63 30.70 -6 0 0 670.43 35.50 -6 0 0 726.43 32.00 -6 0 0 811.02 59.09 -6 0 0 711.03 32.10 -6 0 0 728.43 32.00 -7 0 0 2.10 2.60 -7 0 0 0.90 3.20 -7 0 0 -2.50 1.90 -7 0 0 -12.90 26.10 -7 0 0 -4.30 3.40 -7 0 0 -3.10 2.10 -8 0 0 438.86 22.50 -8 0 0 417.86 21.90 -8 0 0 375.66 20.60 -8 0 0 408.16 22.10 -8 0 0 398.96 22.10 -9 0 0 0.10 2.20 -9 0 0 0.60 1.90 -9 0 0 2.70 2.60 -9 0 0 -3.00 1.50 -10 0 0 -2.70 1.30 0 1 0 -1.60 2.30 0 1 0 1.10 1.40 0 -1 0 1.80 1.80 -1 1 0 1819.02 62.69 -1 1 0 1799.92 67.09 -1 1 0 1788.42 62.19 -1 1 0 1785.42 62.69 -1 -1 0 1864.01 60.19 -1 1 0 1782.72 65.89 1 1 0 1756.42 70.49 -2 1 0 482.35 28.90 -2 1 0 462.65 26.90 -2 -1 0 462.65 23.70 -2 1 0 477.75 24.90 -3 -1 0 498.85 30.10 -3 1 0 522.55 34.30 -3 1 0 505.65 30.30 -3 1 0 511.65 31.70 -4 1 0 813.22 45.90 -4 1 0 805.02 50.79 -4 1 0 801.12 45.80 -4 -1 0 808.62 46.00 -5 1 0 45.10 12.90 -5 1 0 41.40 14.30 -5 -1 0 71.99 15.90 -5 1 0 41.30 16.20 -6 1 0 73.29 8.40 -6 1 0 58.69 8.50 -6 1 0 54.69 20.10 -6 1 0 72.59 8.80 -6 1 0 59.89 18.20 -6 -1 0 63.49 8.00 -6 -1 0 51.69 8.80 -6 -1 0 67.19 7.30 -6 -1 0 67.89 21.60 -6 -1 0 63.59 8.00 -6 1 0 72.69 8.40 -6 -1 0 64.79 7.80 -6 1 0 58.59 8.70 -6 1 0 84.99 21.40 -6 1 0 85.89 7.50 -6 -1 0 62.89 7.40 -7 -1 0 125.79 11.80 -7 -1 0 121.39 10.50 -7 1 0 146.49 12.40 -7 1 0 144.49 32.90 -7 -1 0 133.39 11.20 -7 -1 0 134.19 10.80 -7 1 0 136.09 13.80 -7 1 0 139.39 10.40 -7 -1 0 137.19 11.80 -7 1 0 147.19 12.30 -8 1 0 672.63 28.20 -8 1 0 661.73 30.90 -8 -1 0 690.73 29.80 -8 1 0 680.13 31.10 -8 1 0 620.44 30.90 -8 1 0 616.64 30.40 -8 -1 0 633.64 28.10 -8 -1 0 690.73 30.50 -8 -1 0 642.44 29.90 -8 1 0 682.03 31.60 -9 1 0 102.59 7.70 -9 1 0 101.49 8.70 -9 1 0 112.09 9.80 -9 -1 0 93.69 8.10 -9 1 0 111.69 9.60 -9 1 0 103.79 9.20 -9 -1 0 96.39 8.20 -10 -1 0 161.48 8.70 -10 1 0 155.28 8.00 0 2 0 20.10 7.00 0 2 0 28.30 5.60 -1 2 0 3678.23 117.49 1 2 0 3157.58 130.79 -1 2 0 3388.76 123.99 -1 2 0 3505.45 123.29 -1 2 0 3547.45 125.39 -2 2 0 1677.83 61.79 -2 2 0 1642.34 69.89 -2 2 0 1672.83 71.39 -2 2 0 1593.94 60.59 -2 -2 0 1572.84 61.99 -2 2 0 1664.13 64.59 -3 2 0 174.78 19.80 -3 -2 0 143.29 15.50 -3 2 0 153.38 20.70 -3 2 0 148.49 17.40 -4 2 0 1983.80 90.89 -4 2 0 2006.30 87.29 -4 2 0 2021.70 95.69 -4 -2 0 1938.31 81.89 -5 2 0 500.85 40.70 -5 2 0 499.75 44.90 -5 2 0 498.55 40.90 -5 -2 0 473.35 57.89 -6 2 0 332.27 37.20 -6 -2 0 291.57 16.40 -6 2 0 327.87 43.10 -6 -2 0 295.37 17.00 -6 2 0 302.97 38.00 -6 2 0 304.27 17.90 -6 2 0 312.47 18.10 -6 2 0 289.87 18.80 -6 -2 0 271.17 17.70 -6 2 0 300.57 15.20 -6 2 0 306.77 18.70 -6 -2 0 281.97 15.80 -6 2 0 305.97 18.20 -6 -2 0 265.47 16.00 -6 -2 0 290.77 16.60 -7 2 0 86.69 7.50 -7 2 0 83.29 10.40 -7 2 0 81.59 9.50 -7 2 0 97.09 10.50 -7 -2 0 74.79 9.40 -7 -2 0 81.09 8.80 -7 -2 0 85.59 8.40 -7 2 0 77.39 9.50 -7 -2 0 74.89 7.70 -7 2 0 52.59 32.50 -7 2 0 73.49 9.50 -8 2 0 23.60 6.00 -8 2 0 26.60 4.50 -8 -2 0 22.00 4.80 -8 2 0 24.90 6.20 -8 -2 0 16.70 4.30 -8 2 0 21.40 5.90 -8 -2 0 24.10 5.70 -8 2 0 23.10 6.20 -8 2 0 18.90 5.90 -9 2 0 21.40 5.00 -9 -2 0 25.10 5.10 -9 2 0 25.10 3.90 -9 2 0 19.50 4.60 -9 2 0 25.70 5.80 -9 2 0 22.60 5.10 -9 2 0 17.60 4.50 -10 2 0 90.09 5.30 -10 -2 0 89.29 6.30 0 3 0 -3.90 3.80 -1 3 0 169.28 18.90 -1 3 0 169.18 19.20 1 3 0 165.68 20.50 -1 3 0 162.18 13.90 -1 3 0 155.48 17.20 -1 3 0 153.68 16.10 -2 3 0 522.95 35.10 -2 3 0 567.54 30.50 -2 3 0 546.65 36.00 -2 3 0 527.45 32.30 -2 3 0 504.05 31.80 -2 -3 0 542.55 29.40 -3 3 0 606.64 37.00 -3 -3 0 546.55 28.30 -3 3 0 592.74 26.80 -3 3 0 614.74 41.60 -3 3 0 571.14 26.90 -3 3 0 583.14 41.30 -4 3 0 -2.00 8.60 -4 3 0 3.00 9.70 -4 -3 0 -0.10 9.40 -5 -3 0 122.39 10.00 -5 3 0 135.89 27.70 -5 3 0 133.09 25.50 -5 3 0 114.19 11.50 -5 3 0 134.59 26.50 -5 3 0 110.29 11.00 -5 3 0 135.29 11.10 -6 3 0 228.88 16.80 -6 -3 0 213.78 13.40 -6 3 0 208.08 35.80 -6 3 0 226.78 16.20 -6 3 0 198.78 39.60 -6 3 0 209.28 15.80 -6 -3 0 242.18 15.20 -6 3 0 235.18 12.40 -6 3 0 216.38 38.10 -6 3 0 229.88 15.80 -6 3 0 236.78 16.20 -7 3 0 49.99 9.10 -7 -3 0 42.60 6.90 -7 3 0 37.00 7.60 -7 -3 0 39.50 5.60 -7 3 0 31.00 26.80 -7 3 0 40.10 7.80 -7 3 0 50.09 7.50 -7 3 0 18.30 25.70 -7 3 0 18.90 22.50 -7 3 0 45.70 7.80 -7 3 0 36.20 4.90 -8 3 0 208.28 15.50 -8 3 0 213.98 11.60 -8 3 0 223.68 15.50 -8 3 0 224.38 16.10 -8 3 0 207.18 15.80 -8 -3 0 230.98 15.00 -8 3 0 207.68 15.30 -9 3 0 47.00 6.30 -9 3 0 45.90 7.10 -9 -3 0 47.40 6.30 -9 3 0 51.29 6.50 -9 3 0 43.60 7.30 -9 3 0 42.80 4.40 -9 3 0 38.70 6.00 -10 -3 0 33.10 4.10 0 4 0 757.92 40.60 0 4 0 696.73 49.70 -1 4 0 1003.60 45.10 -1 4 0 894.01 55.29 -1 4 0 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3.10 1 -5 27 67.99 8.30 -1 -5 -27 74.59 9.60 -1 5 27 50.59 6.90 1 -5 -27 61.79 7.20 1 5 27 71.29 6.70 -1 -5 27 56.79 7.10 -2 5 27 5.80 2.90 -2 -5 -27 5.20 4.10 2 -5 27 11.60 5.50 2 5 27 9.00 3.10 -2 5 -27 11.60 6.90 2 -5 -27 12.10 5.30 3 -5 27 125.69 10.30 -3 5 27 105.69 9.10 -3 -5 -27 105.49 10.00 3 5 27 131.59 8.70 -3 5 -27 128.19 11.00 3 -5 -27 132.49 9.80 4 -5 27 4.50 2.50 -4 5 27 6.20 2.60 -4 -5 -27 5.00 3.20 4 -5 -27 4.00 2.30 -4 5 -27 8.00 4.90 0 -6 -27 30.30 5.20 0 -6 27 20.90 4.80 0 6 27 17.10 4.00 -1 -6 -27 71.79 7.00 1 -6 27 82.79 8.00 -1 6 27 62.99 7.00 1 -6 -27 71.69 7.10 1 6 27 74.09 5.80 -1 6 -27 75.29 8.50 -2 6 27 7.60 3.20 2 -6 27 7.40 2.90 2 -6 -27 7.90 2.80 2 6 27 6.90 2.50 -2 6 -27 8.20 3.90 -3 6 27 23.40 4.90 -3 -6 -27 18.30 4.00 3 -6 27 30.80 5.50 -3 6 -27 25.00 5.00 3 -6 -27 25.80 6.00 3 6 27 24.20 4.30 -4 6 27 31.00 3.80 4 -6 27 33.00 4.70 4 -6 -27 28.20 4.20 -4 6 -27 34.40 5.40 4 6 27 35.00 3.90 0 -7 27 17.40 3.90 0 7 27 16.50 3.40 0 7 -27 20.30 4.50 -1 7 27 11.20 3.20 1 7 -27 5.40 2.80 -1 -7 -27 11.00 3.60 -1 7 -27 10.00 4.00 1 -7 -27 10.20 3.00 1 7 27 5.00 2.60 2 7 -27 45.70 6.00 -2 7 27 64.09 6.00 -2 -7 -27 52.49 5.70 2 -7 27 70.19 7.40 2 -7 -27 66.49 6.60 -2 7 -27 54.29 6.50 2 7 27 69.09 5.00 3 -7 27 5.70 2.30 -3 7 27 1.00 2.00 3 -7 -27 2.20 2.10 -3 7 -27 2.70 2.30 3 7 27 6.30 2.00 0 -8 -27 11.90 2.40 0 -8 27 20.90 4.10 0 8 27 6.60 3.00 0 8 -27 14.50 4.20 1 -8 27 36.40 4.10 -1 8 27 32.30 4.40 1 8 27 28.50 3.90 -1 8 -27 23.40 4.20 0 0 -28 504.25 25.60 0 0 28 528.95 25.00 1 0 -28 4.60 3.60 1 0 28 1.90 2.70 2 0 -28 12.10 4.60 2 0 28 5.70 3.60 -2 0 -28 10.60 4.90 3 0 28 117.49 10.00 -3 0 -28 116.49 11.00 -3 0 -28 93.69 10.40 3 0 -28 111.99 10.80 -4 0 -28 51.19 7.90 -4 0 -28 33.80 5.80 4 0 28 46.50 6.60 -5 0 -28 36.00 5.80 5 0 28 30.10 5.10 0 1 28 4.40 3.60 0 -1 28 5.30 3.20 0 -1 -28 2.30 3.10 1 1 -28 45.50 7.80 -1 -1 -28 51.49 7.60 1 -1 28 42.30 7.10 -1 1 28 51.89 8.00 -1 -1 28 45.60 6.90 1 -1 -28 40.60 7.20 1 1 28 46.80 6.80 2 1 -28 1.00 3.30 2 -1 28 2.50 3.10 -2 -1 -28 6.70 5.10 -2 1 -28 7.50 4.50 2 -1 -28 8.50 4.00 2 1 28 5.50 3.10 -3 -1 -28 1.70 3.00 3 -1 28 0.70 2.40 3 1 28 -1.20 2.60 -3 1 -28 -0.40 3.20 3 -1 -28 5.40 3.60 4 -1 28 79.59 8.10 -4 -1 -28 63.89 8.60 4 1 28 91.79 8.20 4 -1 -28 83.19 8.80 -4 1 -28 77.09 8.80 -4 1 -28 68.79 7.80 -5 -1 -28 27.70 5.10 5 -1 28 31.70 5.10 5 1 28 37.10 5.00 -5 1 -28 27.50 4.90 0 -2 -28 18.00 5.00 0 2 28 36.50 6.40 0 -2 28 22.90 5.50 -1 -2 -28 3.90 3.60 1 -2 28 -0.10 2.30 -1 2 28 -6.40 3.50 1 2 28 5.20 3.20 1 -2 -28 4.90 3.30 1 2 28 0.00 3.30 -1 2 -28 5.10 4.40 -2 2 28 44.00 7.00 2 -2 28 33.30 6.50 2 2 28 47.80 6.70 -2 2 -28 49.70 8.40 2 -2 -28 52.89 7.40 -3 -2 -28 57.69 8.10 3 -2 28 60.29 7.70 -3 2 28 43.10 6.90 -3 2 -28 53.19 8.40 3 -2 -28 70.19 9.90 3 2 28 52.59 7.00 -3 2 -28 52.79 8.20 4 -2 28 91.69 8.80 -4 -2 -28 95.59 9.80 -4 2 -28 90.09 9.90 -4 2 -28 99.99 9.40 4 -2 -28 112.69 9.50 4 2 28 104.49 8.50 5 -2 28 8.50 3.60 -5 -2 -28 10.50 3.90 5 2 28 10.90 3.10 -5 2 -28 15.90 4.10 -5 2 -28 11.80 3.30 0 3 28 33.30 6.60 0 -3 -28 46.40 7.00 0 -3 28 39.90 6.80 -1 3 28 20.30 4.40 -1 -3 -28 24.90 4.80 1 -3 28 32.00 6.00 1 3 28 24.70 4.90 -1 3 -28 29.80 6.60 1 -3 -28 32.40 6.20 -1 -3 28 22.50 4.40 2 -3 28 9.90 3.80 -2 3 28 9.20 3.90 2 3 28 7.90 3.20 -2 3 -28 9.70 4.20 -2 3 -28 14.40 4.70 2 -3 -28 5.70 3.80 -3 -3 -28 29.40 5.90 3 -3 28 32.20 6.10 -3 3 28 31.60 6.90 -3 3 -28 31.50 7.70 3 -3 -28 33.80 6.00 3 3 28 44.10 5.80 -3 3 -28 34.30 7.40 -4 3 28 53.89 6.00 -4 -3 -28 65.99 8.00 4 -3 28 71.09 7.40 4 -3 -28 78.99 8.00 -4 3 -28 72.19 10.50 4 3 28 84.29 7.20 5 -3 28 51.39 5.50 -5 -3 -28 35.80 5.20 5 3 28 53.19 5.10 -5 3 -28 45.60 5.60 0 -4 28 4.20 3.80 0 4 28 6.40 5.30 0 -4 -28 2.00 2.90 0 4 28 7.10 2.80 -1 -4 -28 37.50 6.00 1 -4 28 23.40 5.00 -1 4 28 24.60 5.10 1 -4 -28 36.20 5.90 1 4 28 43.20 5.70 -1 -4 28 29.10 5.00 -2 4 28 35.10 5.80 2 -4 28 55.19 10.40 2 -4 -28 45.90 9.70 2 4 28 52.19 6.10 -2 4 -28 37.70 7.30 -3 -4 -28 129.19 10.60 3 -4 28 132.99 10.30 -3 4 28 124.39 10.40 -3 4 -28 113.99 11.40 3 -4 -28 126.29 10.00 3 4 28 130.79 9.00 -3 4 -28 118.59 10.70 -4 4 28 59.09 5.30 4 -4 28 72.59 7.30 -4 -4 -28 64.19 7.00 4 4 28 70.59 6.80 -4 4 -28 49.70 7.00 4 -4 -28 66.19 6.70 0 -5 28 78.39 7.90 0 -5 -28 85.39 7.80 0 5 28 70.19 6.70 -1 5 28 4.60 3.00 -1 -5 -28 -0.70 2.40 1 -5 -28 6.20 2.90 -1 5 -28 3.50 3.30 -2 5 28 49.99 6.10 2 -5 28 51.29 6.90 2 -5 -28 51.39 6.30 2 5 28 59.29 5.80 -2 5 -28 42.70 7.20 3 -5 28 16.90 4.20 -3 5 28 16.00 3.60 -3 -5 -28 19.90 5.30 -3 5 -28 25.80 5.10 3 5 28 17.00 5.60 3 -5 -28 23.80 4.70 -4 5 28 32.50 4.10 4 -5 28 35.40 5.00 -4 -5 -28 22.50 4.40 -4 5 -28 32.70 5.10 4 5 28 32.00 4.20 4 -5 -28 41.10 5.00 0 -6 -28 108.39 8.00 0 6 28 90.99 7.50 0 -6 28 101.19 8.40 0 6 -28 96.39 9.00 -1 -6 -28 12.70 5.00 1 -6 28 9.90 3.20 -1 6 28 10.20 3.10 1 6 28 7.60 3.00 1 -6 -28 7.40 2.70 -1 6 -28 3.70 3.50 -2 -6 -28 5.20 3.00 -2 6 28 0.40 2.40 -2 6 -28 -0.30 3.10 2 -6 -28 -1.00 2.40 2 6 28 0.40 1.70 -3 -6 -28 15.00 3.80 3 -6 28 27.80 5.40 -3 6 28 14.40 3.00 3 6 28 21.80 3.50 -3 6 -28 22.10 4.60 0 7 -28 6.10 2.40 0 -7 28 1.50 2.10 0 7 28 0.20 2.10 0 -7 -28 0.80 2.00 -1 7 28 26.60 4.80 1 -7 28 29.70 4.40 1 7 -28 17.10 3.70 -1 7 -28 22.30 4.10 1 -7 -28 28.80 4.70 2 -7 28 1.90 2.00 -2 7 28 4.90 2.10 -2 7 -28 3.10 2.30 2 7 28 4.30 1.90 2 -7 -28 3.80 2.10 0 0 -29 -1.70 3.00 0 0 29 3.90 4.20 1 0 29 -3.70 3.00 1 0 -29 4.40 3.30 2 0 29 78.09 8.20 2 0 -29 77.69 8.80 -2 0 -29 76.29 8.50 3 0 29 80.69 8.10 -3 0 -29 70.49 7.30 3 0 -29 100.29 9.60 -3 0 -29 88.29 9.30 -4 0 -29 4.60 3.90 4 0 29 3.40 2.50 0 -1 29 61.39 11.00 0 1 29 60.49 7.10 0 -1 -29 54.79 7.70 1 -1 29 4.30 3.00 -1 1 -29 4.00 5.00 1 1 29 3.00 2.90 1 -1 -29 -1.40 2.80 -2 -1 -29 41.30 6.40 2 -1 29 52.89 7.30 -2 -1 -29 53.39 9.00 -2 1 -29 57.39 7.70 2 -1 -29 50.79 7.60 2 1 29 55.29 8.20 -2 1 -29 47.00 7.90 -3 -1 -29 27.30 6.80 -3 -1 -29 19.10 5.40 3 -1 29 19.60 4.40 3 1 29 12.00 4.00 3 -1 -29 17.20 4.60 -3 1 -29 8.20 4.40 4 -1 29 21.60 4.60 -4 -1 -29 27.10 6.20 -4 1 -29 18.30 4.60 4 1 29 20.40 4.20 -4 1 -29 35.60 5.40 0 -2 -29 6.50 3.40 0 2 -29 4.00 4.40 0 2 29 7.20 3.40 0 2 29 -0.50 3.90 1 2 -29 3.80 5.80 1 -2 29 1.60 2.50 -1 2 29 -1.20 4.10 -1 -2 -29 3.70 3.20 1 -2 -29 5.00 3.30 1 2 29 6.20 4.00 -1 2 -29 7.20 3.90 1 2 29 3.50 3.60 -2 2 29 30.30 5.30 2 -2 29 56.09 9.80 -2 -2 -29 38.60 10.20 -2 2 -29 40.10 6.80 -2 2 -29 45.90 7.60 2 2 29 28.40 4.40 -3 -2 -29 4.90 3.10 3 -2 29 0.30 2.20 -3 2 -29 -0.70 3.30 3 2 29 8.20 2.80 3 -2 -29 3.80 3.20 -4 -2 -29 66.09 9.90 4 -2 29 72.39 7.90 4 2 29 63.29 8.70 4 -2 -29 55.39 6.50 -4 2 -29 52.69 8.60 -4 2 -29 49.40 6.40 0 -3 29 0.40 2.80 0 3 29 1.30 3.70 0 -3 -29 2.70 2.60 0 3 29 -0.70 3.10 1 -3 29 38.30 6.30 -1 -3 -29 45.70 6.30 1 3 29 35.10 5.90 1 3 29 46.30 5.90 2 -3 29 132.59 10.30 2 -3 -29 138.19 10.40 -2 3 -29 126.69 10.90 2 3 29 136.79 9.50 3 -3 29 46.00 6.10 -3 3 29 29.50 5.20 -3 -3 -29 39.10 6.50 3 3 29 44.20 5.40 -3 3 -29 37.90 6.40 3 -3 -29 45.50 6.40 -3 3 -29 39.00 6.70 -4 -3 -29 121.79 9.40 4 -3 29 129.79 9.00 4 -3 -29 118.29 10.50 -4 3 -29 109.09 9.60 4 3 29 136.29 8.40 -4 3 -29 120.19 9.00 0 4 29 2.60 2.40 0 -4 -29 1.60 2.50 0 -4 29 -2.90 2.10 -1 4 29 -1.20 3.30 1 -4 29 -0.90 2.40 -1 -4 -29 3.00 3.40 1 -4 -29 -0.20 2.60 -1 4 -29 3.70 2.70 1 4 29 -2.10 3.40 2 -4 29 68.19 7.10 -2 4 29 48.30 6.10 2 -4 -29 64.89 7.10 -2 4 -29 57.29 7.80 2 4 29 63.19 6.00 -3 4 29 8.20 2.80 -3 -4 -29 8.90 3.90 -3 4 -29 7.10 3.10 3 4 29 7.70 2.50 3 -4 -29 5.10 3.60 -4 -4 -29 71.89 6.80 -4 4 -29 79.79 6.90 0 -5 29 11.40 3.00 0 -5 -29 8.40 3.30 0 5 29 8.80 3.20 1 -5 29 16.60 3.80 -1 5 29 28.00 4.40 -1 -5 -29 21.80 3.80 -1 5 -29 19.10 4.80 1 5 29 16.90 3.20 -2 5 29 -7.00 3.80 -2 -5 -29 -4.30 2.50 2 5 29 -1.60 1.70 -2 5 -29 -3.10 5.00 -3 5 29 124.79 7.60 -3 -5 -29 122.69 8.90 3 5 29 139.99 7.60 -3 5 -29 128.89 10.10 0 -6 -29 0.60 2.30 0 -6 29 2.70 2.30 0 6 -29 4.50 2.80 0 6 29 -2.70 2.20 -1 6 29 48.30 5.10 1 6 -29 58.09 6.60 1 -6 29 62.99 8.40 -1 6 -29 51.89 6.10 1 6 29 54.99 5.20 1 -6 -29 61.09 5.70 -2 6 29 0.80 2.00 2 -6 29 1.30 2.10 2 6 -29 3.90 2.60 -2 -6 -29 2.00 2.70 2 -6 -29 2.60 2.00 2 6 29 -1.70 1.60 -2 6 -29 1.70 2.30 0 0 30 6.90 2.70 1 0 30 -1.10 2.20 -1 0 -30 2.60 3.20 -2 0 -30 5.00 3.20 2 0 30 2.10 2.50 -2 0 -30 6.70 3.80 3 0 30 25.70 5.00 -3 0 -30 29.70 5.00 -3 0 -30 12.60 5.60 4 0 30 26.10 4.70 -4 0 -30 25.10 5.00 0 1 -30 9.80 4.20 0 -1 30 11.60 3.50 0 -1 -30 16.60 4.20 1 1 -30 17.00 5.00 1 -1 30 4.70 2.90 -1 1 -30 7.10 3.60 1 1 30 12.10 3.60 1 -1 -30 7.70 3.30 2 -1 30 13.80 3.70 -2 -1 -30 15.20 4.20 -2 -1 -30 17.00 4.80 -2 1 -30 18.60 5.00 -2 1 -30 14.30 4.10 2 1 30 12.70 3.40 2 -1 -30 19.00 4.40 -3 -1 -30 0.00 3.20 3 -1 30 1.20 2.50 3 1 30 3.00 2.20 -3 1 -30 3.00 3.20 -3 1 -30 0.30 3.00 3 -1 -30 1.20 2.90 -4 -1 -30 26.50 7.20 4 1 30 23.70 5.50 -4 1 -30 20.40 4.20 0 -2 -30 264.27 14.40 0 2 -30 237.08 13.80 0 -2 30 252.07 13.80 1 -2 30 67.59 7.20 1 -2 -30 67.49 7.70 1 2 30 58.39 6.60 -1 2 -30 49.00 9.10 2 -2 30 12.70 3.60 -2 -2 -30 18.30 4.80 -2 2 -30 10.20 3.70 2 -2 -30 11.00 3.90 2 2 30 12.90 3.60 3 -2 30 12.70 5.80 -3 -2 -30 8.80 4.50 -3 2 -30 8.40 3.60 3 2 30 8.10 3.40 -4 -2 -30 162.98 10.70 4 -2 30 168.58 10.10 4 2 30 168.98 9.70 0 3 30 5.20 3.30 0 -3 -30 10.90 3.40 0 -3 30 14.10 4.20 1 -3 30 37.60 5.70 -1 3 30 27.40 4.60 1 3 30 37.10 4.80 -1 3 -30 26.40 5.20 1 -3 -30 38.60 5.50 1 3 30 25.30 4.70 2 -3 30 133.19 9.50 -2 -3 -30 108.59 9.80 2 3 30 120.89 8.80 2 -3 -30 129.79 9.50 -2 3 -30 104.99 9.50 -3 -3 -30 9.10 3.40 3 -3 30 6.70 2.50 3 -3 -30 7.60 2.90 3 3 30 5.50 2.00 -3 3 -30 9.90 4.90 0 -4 -30 25.00 4.50 0 4 30 13.80 3.00 1 -4 30 4.80 2.50 -1 4 30 9.60 3.20 -1 4 -30 7.10 3.40 1 4 30 4.60 3.00 1 -4 -30 3.60 3.40 2 -4 30 102.99 7.90 -2 -4 -30 91.39 8.00 -2 4 -30 88.29 8.20 2 -4 -30 89.69 7.50 2 4 30 88.89 6.20 3 -4 30 44.40 5.20 -3 -4 -30 40.40 5.30 3 -4 -30 37.50 4.80 3 4 30 27.60 3.90 -3 4 -30 27.00 4.60 0 5 -30 4.40 2.80 0 -5 -30 6.80 2.40 0 5 30 4.40 2.30 1 -5 30 86.19 6.40 -1 5 30 69.79 5.90 1 5 30 70.49 5.70 -1 5 -30 77.09 7.20 1 -5 -30 86.99 7.80 -2 5 30 100.89 9.20 -2 -5 -30 130.69 8.70 2 -5 30 150.48 8.50 -2 5 -30 135.99 9.00 2 -5 -30 142.19 8.50 2 5 30 103.39 7.50 0 0 -31 -3.30 2.60 1 0 31 13.10 3.20 -1 0 -31 9.60 4.00 -1 0 -31 6.50 3.00 -2 0 -31 -4.20 2.70 -2 0 -31 0.90 3.30 2 0 31 -2.10 2.00 3 0 31 0.60 2.10 -3 0 -31 -1.40 2.80 0 1 -31 5.90 3.80 1 -1 31 29.40 4.80 -1 -1 -31 36.80 7.70 -1 -1 -31 20.30 4.70 -1 1 -31 16.40 7.10 -1 1 -31 27.00 6.10 -2 -1 -31 33.90 5.30 2 -1 31 35.60 5.10 -2 1 -31 24.80 5.20 -2 1 -31 24.60 5.00 2 1 31 39.40 5.20 -3 -1 -31 15.60 3.90 -3 1 -31 5.50 6.20 3 1 31 6.60 3.70 -3 1 -31 7.80 3.00 0 -2 31 4.10 2.80 -1 -2 -31 36.60 8.80 1 -2 31 24.10 4.50 1 2 31 26.20 4.30 -1 2 -31 18.80 6.40 1 -2 -31 19.90 4.90 2 -2 31 79.39 6.70 -2 -2 -31 74.19 7.30 2 -2 -31 82.19 6.90 -2 2 -31 76.59 9.90 -3 -2 -31 87.69 7.60 3 -2 31 104.39 7.30 -3 2 -31 77.29 7.00 3 2 31 96.39 6.60 0 -3 -31 44.10 5.10 -1 -3 -31 27.50 5.20 1 -3 31 18.90 4.60 1 -3 -31 27.20 4.50 -1 3 -31 26.70 5.20 -2 -3 -31 35.30 5.40 2 -3 31 33.10 6.10 2 -3 -31 39.70 5.50 2 3 31 44.90 4.90 -2 3 -31 32.30 6.40 0 4 -31 127.99 9.30 1 -4 31 42.80 4.70 -1 -4 -31 49.99 8.50 1 -4 -31 40.60 4.50 0 0 -32 18.10 4.00 -1 0 -32 -3.00 3.00 -1 0 -32 0.70 3.10 -2 0 -32 123.09 8.40 2 0 32 131.99 7.60 0 -1 -32 31.40 4.80 0 -1 -32 27.10 7.60 -1 -1 -32 26.10 4.40 1 -1 32 19.30 3.60 -1 1 -32 19.30 4.10 1 -1 -32 25.20 4.10 2 -1 32 17.20 3.10 -2 -1 -32 17.10 3.70 -2 1 -32 7.70 4.10 2 1 32 16.00 3.00 0 2 -32 36.10 6.90 0 -2 -32 38.60 5.10 1 -2 32 -0.40 3.60 -1 -2 -32 -3.30 2.50 -1 2 -32 3.40 2.40 0 3 -32 4.00 2.60 0 -3 -32 7.70 2.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 62362 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 -0.0057(2) 0.81876(18) 0.54033(8) 0.0280(4) Uani d . . . 1 . . H H41 -0.046669 0.827975 0.568779 0.042 Uiso calc U . R 1 . . O O2 -0.1320(2) 0.65472(18) 0.54313(8) 0.0272(4) Uani d . . . 1 . . O O3 1.1406(2) 0.32237(17) 0.86970(7) 0.0225(4) Uani d . . . 1 . . H H42 1.184617 0.259102 0.871601 0.034 Uiso calc U . R 1 . . O O4 0.4596(2) 0.24458(17) 0.76224(8) 0.0248(4) Uani d . . . 1 . . O O5 0.72306(19) 0.62119(15) 0.66507(7) 0.0196(4) Uani d . . . 1 . . H H43 0.678952 0.653721 0.689295 0.029 Uiso calc U . R 1 . . O O6 0.7918(2) 0.43311(18) 0.56015(8) 0.0246(4) Uani d . . . 1 . . H H44 0.823473 0.493565 0.546971 0.037 Uiso calc U . R 1 . . O O7 0.1821(2) 0.56083(19) 0.55727(8) 0.0298(4) Uani d . . . 1 . . C C1 1.0335(3) 0.3214(2) 0.82805(9) 0.0188(5) Uani d . . . 1 . . H H1 1.077775 0.272922 0.800687 0.023 Uiso calc U . R 1 . . C C2 1.0162(2) 0.4420(2) 0.80725(9) 0.0191(5) Uani d . . . 1 . . C C3 0.8947(2) 0.4344(2) 0.76383(9) 0.0173(5) Uani d . . . 1 . . H H30 0.941003 0.38129 0.738601 0.021 Uiso calc U . R 1 . . C C4 0.8727(3) 0.5454(2) 0.73501(10) 0.0204(5) Uani d . . . 1 . . H H14 0.804361 0.596368 0.754445 0.024 Uiso calc U . R 1 . . H H13 0.973087 0.583688 0.730841 0.024 Uiso calc U . R 1 . . C C5 0.8028(3) 0.5219(2) 0.68339(10) 0.0186(5) Uani d . . . 1 . . H H31 0.888102 0.504324 0.659348 0.022 Uiso calc U . R 1 . . C C6 0.6916(2) 0.4223(2) 0.68334(10) 0.0185(5) Uani d . . . 1 . . C C7 0.6270(3) 0.3822(2) 0.63309(10) 0.0184(5) Uani d . . . 1 . . C C8 0.4494(3) 0.3763(2) 0.63795(10) 0.0182(5) Uani d . . . 1 . . C C9 0.4007(3) 0.3667(2) 0.58231(10) 0.0196(5) Uani d . . . 1 . . C C10 0.2435(3) 0.3249(2) 0.56773(10) 0.0227(5) Uani d . . . 1 . . H H9 0.170632 0.345457 0.595461 0.027 Uiso calc U . R 1 . . C C11 0.1838(3) 0.3773(2) 0.51863(11) 0.0251(5) Uani d . . . 1 . . H H38 0.25962 0.362492 0.491559 0.03 Uiso calc U . R 1 . . H H37 0.087283 0.338362 0.509141 0.03 Uiso calc U . R 1 . . C C12 0.1532(3) 0.5039(2) 0.52068(11) 0.0238(5) Uani d . . . 1 . . C C13 0.0793(3) 0.5554(3) 0.47379(11) 0.0250(5) Uani d . . . 1 . . H H5 0.144398 0.538446 0.444073 0.03 Uiso calc U . R 1 . . H H4 -0.021873 0.519104 0.468251 0.03 Uiso calc U . R 1 . . C C14 0.0571(3) 0.6832(2) 0.47754(11) 0.0235(5) Uani d . . . 1 . . H H3 0.15998 0.720606 0.479505 0.028 Uiso calc U . R 1 . . C C15 -0.0294(4) 0.7290(3) 0.43114(11) 0.0305(6) Uani d . . . 1 . . H H2 -0.128744 0.690539 0.428205 0.046 Uiso calc U . R 1 . . H H39 0.031514 0.714803 0.400643 0.046 Uiso calc U . R 1 . . H H40 -0.04589 0.810754 0.435017 0.046 Uiso calc U . R 1 . . C C16 -0.0347(3) 0.7143(2) 0.52383(10) 0.0211(5) Uani d . . . 1 . . C C17 0.2437(3) 0.1945(3) 0.56236(12) 0.0291(6) Uani d . . . 1 . . H H8 0.305787 0.172773 0.533026 0.044 Uiso calc U . R 1 . . H H7 0.138168 0.167514 0.557717 0.044 Uiso calc U . R 1 . . H H6 0.287261 0.160328 0.592932 0.044 Uiso calc U . R 1 . . C C18 0.7012(3) 0.2647(2) 0.62264(10) 0.0231(5) Uani d . . . 1 . . H H12 0.812423 0.273746 0.61854 0.035 Uiso calc U . R 1 . . H H11 0.657538 0.232424 0.591689 0.035 Uiso calc U . R 1 . . H H10 0.680578 0.213728 0.651102 0.035 Uiso calc U . R 1 . . C C19 0.9793(3) 0.5279(2) 0.84905(11) 0.0247(5) Uani d . . . 1 . . H H17 0.897659 0.497704 0.87068 0.037 Uiso calc U . R 1 . . H H16 0.945256 0.599336 0.833772 0.037 Uiso calc U . R 1 . . H H15 1.071539 0.541588 0.869391 0.037 Uiso calc U . R 1 . . C C20 0.8813(3) 0.2690(2) 0.84429(11) 0.0228(5) Uani d . . . 1 . . H H18 0.836471 0.3147 0.871999 0.027 Uiso calc U . R 1 . . H H26 0.899777 0.191469 0.857319 0.027 Uiso calc U . R 1 . . C C21 0.7671(3) 0.2634(2) 0.80026(10) 0.0218(5) Uani d . . . 1 . . H H19 0.669258 0.230644 0.812467 0.026 Uiso calc U . R 1 . . H H20 0.808483 0.21238 0.773857 0.026 Uiso calc U . R 1 . . C C22 0.7350(3) 0.3812(2) 0.77669(10) 0.0184(5) Uani d . . . 1 . . C C23 0.6334(3) 0.4521(2) 0.81221(10) 0.0234(5) Uani d . . . 1 . . H H22 0.619889 0.528252 0.798062 0.035 Uiso calc U . R 1 . . H H21 0.6825 0.457654 0.845428 0.035 Uiso calc U . R 1 . . H H23 0.532876 0.415465 0.815762 0.035 Uiso calc U . R 1 . . C C24 0.6488(3) 0.3674(2) 0.72613(10) 0.0183(5) Uani d . . . 1 . . C C25 0.5076(3) 0.2937(2) 0.72471(10) 0.0192(5) Uani d . . . 1 . . C C26 0.4128(3) 0.2829(2) 0.67588(10) 0.0208(5) Uani d . . . 1 . . H H24 0.433603 0.208253 0.660181 0.025 Uiso calc U . R 1 . . H H25 0.302148 0.28597 0.684426 0.025 Uiso calc U . R 1 . . C C27 1.1728(3) 0.4748(3) 0.78423(11) 0.0265(6) Uani d . . . 1 . . H H27 1.253962 0.462557 0.809292 0.04 Uiso calc U . R 1 . . H H28 1.171052 0.554862 0.774333 0.04 Uiso calc U . R 1 . . H H29 1.192808 0.42768 0.754424 0.04 Uiso calc U . R 1 . . C C28 0.6469(3) 0.4530(2) 0.58398(10) 0.0199(5) Uani d . . . 1 . . H H32 0.635354 0.535618 0.591765 0.024 Uiso calc U . R 1 . . C C29 0.5099(3) 0.4121(2) 0.55388(10) 0.0212(5) Uani d . . . 1 . . H H33 0.502822 0.418438 0.518167 0.025 Uiso calc U . R 1 . . C C30 0.3796(3) 0.4883(2) 0.65806(10) 0.0203(5) Uani d . . . 1 . . H H36 0.267588 0.485704 0.654703 0.03 Uiso calc U . R 1 . . H H35 0.42005 0.552217 0.638497 0.03 Uiso calc U . R 1 . . H H34 0.407036 0.497769 0.693725 0.03 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 0.0297(9) 0.0297(10) 0.0247(9) -0.0055(8) -0.0006(8) -0.0014(8) O2 0.0168(8) 0.0316(10) 0.0334(10) -0.0015(7) 0.0039(8) 0.0037(8) O3 0.0168(8) 0.0283(9) 0.0224(9) 0.0040(7) -0.0045(7) 0.0003(7) O4 0.0191(8) 0.0317(10) 0.0234(9) -0.0060(7) -0.0002(7) 0.0048(8) O5 0.0175(8) 0.0199(8) 0.0215(9) 0.0016(7) -0.0010(7) 0.0016(7) O6 0.0160(8) 0.0312(10) 0.0265(9) -0.0005(7) 0.0070(7) 0.0013(8) O7 0.0261(9) 0.0350(11) 0.0284(10) 0.0064(8) -0.0071(8) -0.0057(9) C1 0.0146(9) 0.0224(11) 0.0195(11) 0.0023(9) -0.0017(9) 0.0003(9) C2 0.0109(9) 0.0241(12) 0.0222(11) -0.0007(9) -0.0012(9) 0.0013(10) C3 0.0114(9) 0.0216(11) 0.0189(11) 0.0005(9) 0.0003(9) -0.0003(9) C4 0.0151(10) 0.0227(12) 0.0233(12) -0.0027(9) -0.0034(9) 0.0029(10) C5 0.0146(9) 0.0201(11) 0.0210(12) 0.0005(9) -0.0003(9) 0.0017(9) C6 0.0117(9) 0.0227(12) 0.0212(12) 0.0031(9) -0.0005(9) 0.0005(9) C7 0.0129(9) 0.0223(12) 0.0199(12) 0.0010(9) 0.0021(9) 0.0008(9) C8 0.0120(10) 0.0223(12) 0.0202(12) -0.0017(9) 0.0002(9) 0.0006(9) C9 0.0169(11) 0.0232(11) 0.0186(12) 0.0022(9) -0.0014(9) -0.0020(9) C10 0.0173(11) 0.0282(13) 0.0226(12) -0.0033(10) -0.0012(10) -0.0007(10) C11 0.0202(11) 0.0307(14) 0.0245(13) 0.0016(10) -0.0039(10) -0.0024(11) C12 0.0154(10) 0.0326(14) 0.0234(13) 0.0016(10) -0.0010(9) -0.0018(11) C13 0.0210(11) 0.0296(13) 0.0245(13) 0.0012(10) -0.0030(10) 0.0000(11) C14 0.0162(10) 0.0293(13) 0.0251(13) -0.0036(10) -0.0024(10) 0.0022(11) C15 0.0318(13) 0.0362(14) 0.0235(13) 0.0013(12) -0.0039(11) 0.0045(11) C16 0.0145(9) 0.0254(12) 0.0235(12) 0.0018(9) -0.0071(10) 0.0040(10) C17 0.0292(13) 0.0292(13) 0.0290(14) -0.0065(11) -0.0067(12) 0.0018(11) C18 0.0201(11) 0.0245(13) 0.0248(13) 0.0036(10) -0.0009(10) -0.0023(10) C19 0.0199(11) 0.0256(12) 0.0285(13) 0.0027(10) -0.0050(10) -0.0029(10) C20 0.0177(10) 0.0259(12) 0.0249(12) -0.0023(10) -0.0018(10) 0.0060(10) C21 0.0175(10) 0.0225(12) 0.0253(12) -0.0011(9) -0.0029(10) 0.0026(10) C22 0.0129(10) 0.0222(11) 0.0202(11) -0.0010(9) 0.0001(9) 0.0000(9) C23 0.0143(10) 0.0299(13) 0.0259(12) 0.0014(10) 0.0007(9) -0.0034(11) C24 0.0142(10) 0.0206(11) 0.0202(12) 0.0008(9) -0.0012(9) -0.0009(9) C25 0.0145(10) 0.0211(11) 0.0220(12) -0.0001(9) -0.0006(9) 0.0004(9) C26 0.0157(10) 0.0260(12) 0.0205(12) -0.0044(9) -0.0012(9) 0.0009(10) C27 0.0139(10) 0.0378(15) 0.0277(14) -0.0039(10) -0.0028(10) 0.0091(11) C28 0.0164(10) 0.0248(12) 0.0185(11) -0.0009(9) 0.0018(9) 0.0003(10) C29 0.0179(11) 0.0256(12) 0.0200(12) 0.0007(9) -0.0003(9) -0.0006(9) C30 0.0151(9) 0.0243(12) 0.0214(11) 0.0005(9) -0.0001(9) -0.0009(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C16 O1 H41 . . 109.5 ? C1 O3 H42 . . 109.5 ? C5 O5 H43 . . 109.5 ? C28 O6 H44 . . 109.5 ? O3 C1 C20 . . 110.5(2) ? O3 C1 C2 . . 109.3(2) ? C20 C1 C2 . . 113.1(2) ? O3 C1 H1 . . 107.9 ? C20 C1 H1 . . 107.9 ? C2 C1 H1 . . 107.9 ? C1 C2 C19 . . 112.0(2) ? C1 C2 C27 . . 106.7(2) ? C19 C2 C27 . . 107.7(2) ? C1 C2 C3 . . 106.1(2) ? C19 C2 C3 . . 115.2(2) ? C27 C2 C3 . . 108.8(2) ? C4 C3 C22 . . 109.97(18) ? C4 C3 C2 . . 113.7(2) ? C22 C3 C2 . . 117.7(2) ? C4 C3 H30 . . 104.7 ? C22 C3 H30 . . 104.7 ? C2 C3 H30 . . 104.7 ? C5 C4 C3 . . 110.1(2) ? C5 C4 H14 . . 109.6 ? C3 C4 H14 . . 109.6 ? C5 C4 H13 . . 109.6 ? C3 C4 H13 . . 109.6 ? H14 C4 H13 . . 108.2 ? O5 C5 C4 . . 110.3(2) ? O5 C5 C6 . . 108.61(18) ? C4 C5 C6 . . 113.3(2) ? O5 C5 H31 . . 108.2 ? C4 C5 H31 . . 108.2 ? C6 C5 H31 . . 108.2 ? C24 C6 C7 . . 118.7(2) ? C24 C6 C5 . . 122.9(2) ? C7 C6 C5 . . 118.5(2) ? C6 C7 C18 . . 106.2(2) ? C6 C7 C8 . . 108.1(2) ? C18 C7 C8 . . 112.9(2) ? C6 C7 C28 . . 121.6(2) ? C18 C7 C28 . . 106.5(2) ? C8 C7 C28 . . 101.76(19) ? C26 C8 C9 . . 121.3(2) ? C26 C8 C30 . . 107.9(2) ? C9 C8 C30 . . 106.5(2) ? C26 C8 C7 . . 107.1(2) ? C9 C8 C7 . . 101.46(19) ? C30 C8 C7 . . 112.4(2) ? C29 C9 C10 . . 129.7(2) ? C29 C9 C8 . . 108.4(2) ? C10 C9 C8 . . 121.4(2) ? C9 C10 C11 . . 113.2(2) ? C9 C10 C17 . . 110.4(2) ? C11 C10 C17 . . 108.9(2) ? C9 C10 H9 . . 108.0 ? C11 C10 H9 . . 108.0 ? C17 C10 H9 . . 108.0 ? C12 C11 C10 . . 115.3(2) ? C12 C11 H38 . . 108.5 ? C10 C11 H38 . . 108.5 ? C12 C11 H37 . . 108.5 ? C10 C11 H37 . . 108.5 ? H38 C11 H37 . . 107.5 ? O7 C12 C11 . . 122.7(3) ? O7 C12 C13 . . 121.4(3) ? C11 C12 C13 . . 115.9(2) ? C14 C13 C12 . . 113.3(2) ? C14 C13 H5 . . 108.9 ? C12 C13 H5 . . 108.9 ? C14 C13 H4 . . 108.9 ? C12 C13 H4 . . 108.9 ? H5 C13 H4 . . 107.7 ? C16 C14 C13 . . 111.2(2) ? C16 C14 C15 . . 107.7(2) ? C13 C14 C15 . . 110.9(2) ? C16 C14 H3 . . 109.0 ? C13 C14 H3 . . 109.0 ? C15 C14 H3 . . 109.0 ? C14 C15 H2 . . 109.5 ? C14 C15 H39 . . 109.5 ? H2 C15 H39 . . 109.5 ? C14 C15 H40 . . 109.5 ? H2 C15 H40 . . 109.5 ? H39 C15 H40 . . 109.5 ? O2 C16 O1 . . 122.0(3) ? O2 C16 C14 . . 124.8(3) ? O1 C16 C14 . . 113.0(2) ? C10 C17 H8 . . 109.5 ? C10 C17 H7 . . 109.5 ? H8 C17 H7 . . 109.5 ? C10 C17 H6 . . 109.5 ? H8 C17 H6 . . 109.5 ? H7 C17 H6 . . 109.5 ? C7 C18 H12 . . 109.5 ? C7 C18 H11 . . 109.5 ? H12 C18 H11 . . 109.5 ? C7 C18 H10 . . 109.5 ? H12 C18 H10 . . 109.5 ? H11 C18 H10 . . 109.5 ? C2 C19 H17 . . 109.5 ? C2 C19 H16 . . 109.5 ? H17 C19 H16 . . 109.5 ? C2 C19 H15 . . 109.5 ? H17 C19 H15 . . 109.5 ? H16 C19 H15 . . 109.5 ? C1 C20 C21 . . 111.5(2) ? C1 C20 H18 . . 109.3 ? C21 C20 H18 . . 109.3 ? C1 C20 H26 . . 109.3 ? C21 C20 H26 . . 109.3 ? H18 C20 H26 . . 108.0 ? C20 C21 C22 . . 112.7(2) ? C20 C21 H19 . . 109.1 ? C22 C21 H19 . . 109.1 ? C20 C21 H20 . . 109.1 ? C22 C21 H20 . . 109.1 ? H19 C21 H20 . . 107.8 ? C23 C22 C24 . . 107.88(19) ? C23 C22 C21 . . 110.2(2) ? C24 C22 C21 . . 110.1(2) ? C23 C22 C3 . . 115.3(2) ? C24 C22 C3 . . 106.65(19) ? C21 C22 C3 . . 106.70(18) ? C22 C23 H22 . . 109.5 ? C22 C23 H21 . . 109.5 ? H22 C23 H21 . . 109.5 ? C22 C23 H23 . . 109.5 ? H22 C23 H23 . . 109.5 ? H21 C23 H23 . . 109.5 ? C6 C24 C25 . . 118.6(2) ? C6 C24 C22 . . 122.6(2) ? C25 C24 C22 . . 118.7(2) ? O4 C25 C24 . . 122.1(2) ? O4 C25 C26 . . 117.3(2) ? C24 C25 C26 . . 120.5(2) ? C8 C26 C25 . . 112.41(19) ? C8 C26 H24 . . 109.1 ? C25 C26 H24 . . 109.1 ? C8 C26 H25 . . 109.1 ? C25 C26 H25 . . 109.1 ? H24 C26 H25 . . 107.9 ? C2 C27 H27 . . 109.5 ? C2 C27 H28 . . 109.5 ? H27 C27 H28 . . 109.5 ? C2 C27 H29 . . 109.5 ? H27 C27 H29 . . 109.5 ? H28 C27 H29 . . 109.5 ? O6 C28 C29 . . 114.3(2) ? O6 C28 C7 . . 112.2(2) ? C29 C28 C7 . . 100.5(2) ? O6 C28 H32 . . 109.8 ? C29 C28 H32 . . 109.8 ? C7 C28 H32 . . 109.8 ? C9 C29 C28 . . 113.3(2) ? C9 C29 H33 . . 123.4 ? C28 C29 H33 . . 123.4 ? C8 C30 H36 . . 109.5 ? C8 C30 H35 . . 109.5 ? H36 C30 H35 . . 109.5 ? C8 C30 H34 . . 109.5 ? H36 C30 H34 . . 109.5 ? H35 C30 H34 . . 109.5 ? 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 C16 . 1.330(3) ? O1 H41 . 0.84 ? O2 C16 . 1.213(3) ? O3 C1 . 1.444(3) ? O3 H42 . 0.84 ? O4 C25 . 1.223(3) ? O5 C5 . 1.444(3) ? O5 H43 . 0.84 ? O6 C28 . 1.430(3) ? O6 H44 . 0.84 ? O7 C12 . 1.205(4) ? C1 C20 . 1.524(3) ? C1 C2 . 1.531(3) ? C1 H1 . 1.0 ? C2 C19 . 1.534(4) ? C2 C27 . 1.542(3) ? C2 C3 . 1.565(3) ? C3 C4 . 1.527(3) ? C3 C22 . 1.562(3) ? C3 H30 . 1.0 ? C4 C5 . 1.521(3) ? C4 H14 . 0.99 ? C4 H13 . 0.99 ? C5 C6 . 1.522(3) ? C5 H31 . 1.0 ? C6 C24 . 1.357(4) ? C6 C7 . 1.519(3) ? C7 C18 . 1.554(3) ? C7 C8 . 1.554(3) ? C7 C28 . 1.554(3) ? C8 C26 . 1.524(3) ? C8 C9 . 1.536(4) ? C8 C30 . 1.547(3) ? C9 C29 . 1.326(4) ? C9 C10 . 1.505(3) ? C10 C11 . 1.530(4) ? C10 C17 . 1.544(4) ? C10 H9 . 1.0 ? C11 C12 . 1.516(4) ? C11 H38 . 0.99 ? C11 H37 . 0.99 ? C12 C13 . 1.524(4) ? C13 C14 . 1.523(4) ? C13 H5 . 0.99 ? C13 H4 . 0.99 ? C14 C16 . 1.508(4) ? C14 C15 . 1.538(4) ? C14 H3 . 1.0 ? C15 H2 . 0.98 ? C15 H39 . 0.98 ? C15 H40 . 0.98 ? C17 H8 . 0.98 ? C17 H7 . 0.98 ? C17 H6 . 0.98 ? C18 H12 . 0.98 ? C18 H11 . 0.98 ? C18 H10 . 0.98 ? C19 H17 . 0.98 ? C19 H16 . 0.98 ? C19 H15 . 0.98 ? C20 C21 . 1.533(4) ? C20 H18 . 0.99 ? C20 H26 . 0.99 ? C21 C22 . 1.547(3) ? C21 H19 . 0.99 ? C21 H20 . 0.99 ? C22 C23 . 1.538(3) ? C22 C24 . 1.543(3) ? C23 H22 . 0.98 ? C23 H21 . 0.98 ? C23 H23 . 0.98 ? C24 C25 . 1.505(3) ? C25 C26 . 1.539(3) ? C26 H24 . 0.99 ? C26 H25 . 0.99 ? C27 H27 . 0.98 ? C27 H28 . 0.98 ? C27 H29 . 0.98 ? C28 C29 . 1.513(3) ? C28 H32 . 1.0 ? C29 H33 . 0.95 ? C30 H36 . 0.98 ? C30 H35 . 0.98 ? C30 H34 . 0.98 ? 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 O1 H41 O3 3_656 0.84 1.82 2.655(3) 170.4 ? O3 H42 O2 3_646 0.84 2.61 3.039(3) 113.0 ? O3 H42 O5 3_746 0.84 2.06 2.807(3) 148.4 ? O5 H43 O4 3_656 0.84 2.06 2.889(3) 168.5 ? O6 H44 O2 1_655 0.84 1.94 2.733(3) 156.6 ? C1 H1 O5 3_746 1.00 2.65 3.178(3) 113.0 ? C14 H3 O2 2_566 1.00 2.41 3.359(3) 158.4 ? C28 H32 O5 . 1.00 2.32 2.996(3) 124.3 ? 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 O3 C1 C2 C19 . . . . -51.6(3) ? C20 C1 C2 C19 . . . . 71.9(3) ? O3 C1 C2 C27 . . . . 66.1(2) ? C20 C1 C2 C27 . . . . -170.4(2) ? O3 C1 C2 C3 . . . . -178.03(18) ? C20 C1 C2 C3 . . . . -54.5(3) ? C1 C2 C3 C4 . . . . -174.7(2) ? C19 C2 C3 C4 . . . . 60.9(3) ? C27 C2 C3 C4 . . . . -60.2(3) ? C1 C2 C3 C22 . . . . 54.6(3) ? C19 C2 C3 C22 . . . . -69.8(3) ? C27 C2 C3 C22 . . . . 169.1(2) ? C22 C3 C4 C5 . . . . -66.6(2) ? C2 C3 C4 C5 . . . . 158.98(19) ? C3 C4 C5 O5 . . . . 155.76(19) ? C3 C4 C5 C6 . . . . 33.8(3) ? O5 C5 C6 C24 . . . . -117.0(2) ? C4 C5 C6 C24 . . . . 5.9(3) ? O5 C5 C6 C7 . . . . 63.5(3) ? C4 C5 C6 C7 . . . . -173.6(2) ? C24 C6 C7 C18 . . . . -69.4(3) ? C5 C6 C7 C18 . . . . 110.1(2) ? C24 C6 C7 C8 . . . . 52.1(3) ? C5 C6 C7 C8 . . . . -128.4(2) ? C24 C6 C7 C28 . . . . 168.9(2) ? C5 C6 C7 C28 . . . . -11.6(3) ? C6 C7 C8 C26 . . . . -66.3(3) ? C18 C7 C8 C26 . . . . 50.9(3) ? C28 C7 C8 C26 . . . . 164.7(2) ? C6 C7 C8 C9 . . . . 165.6(2) ? C18 C7 C8 C9 . . . . -77.2(2) ? C28 C7 C8 C9 . . . . 36.5(2) ? C6 C7 C8 C30 . . . . 52.1(3) ? C18 C7 C8 C30 . . . . 169.3(2) ? C28 C7 C8 C30 . . . . -76.9(2) ? C26 C8 C9 C29 . . . . -143.5(2) ? C30 C8 C9 C29 . . . . 92.6(2) ? C7 C8 C9 C29 . . . . -25.1(3) ? C26 C8 C9 C10 . . . . 43.5(3) ? C30 C8 C9 C10 . . . . -80.3(3) ? C7 C8 C9 C10 . . . . 161.9(2) ? C29 C9 C10 C11 . . . . -22.3(4) ? C8 C9 C10 C11 . . . . 149.0(2) ? C29 C9 C10 C17 . . . . 100.2(3) ? C8 C9 C10 C17 . . . . -88.6(3) ? C9 C10 C11 C12 . . . . -65.8(3) ? C17 C10 C11 C12 . . . . 170.9(2) ? C10 C11 C12 O7 . . . . 4.2(4) ? C10 C11 C12 C13 . . . . -174.3(2) ? O7 C12 C13 C14 . . . . 3.6(3) ? C11 C12 C13 C14 . . . . -177.9(2) ? C12 C13 C14 C16 . . . . -55.7(3) ? C12 C13 C14 C15 . . . . -175.5(2) ? C13 C14 C16 O2 . . . . -30.0(3) ? C15 C14 C16 O2 . . . . 91.7(3) ? C13 C14 C16 O1 . . . . 154.1(2) ? C15 C14 C16 O1 . . . . -84.2(3) ? O3 C1 C20 C21 . . . . -178.2(2) ? C2 C1 C20 C21 . . . . 59.0(3) ? C1 C20 C21 C22 . . . . -57.5(3) ? C20 C21 C22 C23 . . . . -73.4(3) ? C20 C21 C22 C24 . . . . 167.8(2) ? C20 C21 C22 C3 . . . . 52.4(3) ? C4 C3 C22 C23 . . . . -63.6(3) ? C2 C3 C22 C23 . . . . 68.8(3) ? C4 C3 C22 C24 . . . . 56.1(3) ? C2 C3 C22 C24 . . . . -171.5(2) ? C4 C3 C22 C21 . . . . 173.8(2) ? C2 C3 C22 C21 . . . . -53.8(3) ? C7 C6 C24 C25 . . . . -17.7(3) ? C5 C6 C24 C25 . . . . 162.8(2) ? C7 C6 C24 C22 . . . . 164.9(2) ? C5 C6 C24 C22 . . . . -14.6(4) ? C23 C22 C24 C6 . . . . 107.7(3) ? C21 C22 C24 C6 . . . . -132.1(2) ? C3 C22 C24 C6 . . . . -16.7(3) ? C23 C22 C24 C25 . . . . -69.8(3) ? C21 C22 C24 C25 . . . . 50.5(3) ? C3 C22 C24 C25 . . . . 165.8(2) ? C6 C24 C25 O4 . . . . -177.6(2) ? C22 C24 C25 O4 . . . . -0.1(4) ? C6 C24 C25 C26 . . . . -1.0(4) ? C22 C24 C25 C26 . . . . 176.5(2) ? C9 C8 C26 C25 . . . . 164.4(2) ? C30 C8 C26 C25 . . . . -72.4(2) ? C7 C8 C26 C25 . . . . 48.9(3) ? O4 C25 C26 C8 . . . . 160.3(2) ? C24 C25 C26 C8 . . . . -16.4(3) ? C6 C7 C28 O6 . . . . 83.6(3) ? C18 C7 C28 O6 . . . . -38.0(3) ? C8 C7 C28 O6 . . . . -156.4(2) ? C6 C7 C28 C29 . . . . -154.6(2) ? C18 C7 C28 C29 . . . . 83.8(2) ? C8 C7 C28 C29 . . . . -34.6(2) ? C10 C9 C29 C28 . . . . 174.7(3) ? C8 C9 C29 C28 . . . . 2.6(3) ? O6 C28 C29 C9 . . . . 141.4(2) ? C7 C28 C29 C9 . . . . 21.0(3) ?