#------------------------------------------------------------------------------ #$Date: 2021-11-10 01:16:51 +0200 (Wed, 10 Nov 2021) $ #$Revision: 270546 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/51/1565148.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_1565148 loop_ _publ_author_name 'Wang, Lele' 'Han, Hua-Bin' 'Gu, Lijie' 'Zhang, Wenjing' 'Zhao, Junwei' 'Wang, Qi-Lin' _publ_section_title ; Skeletal remodeling of chalcone-based pyridinium salts to access isoindoline polycycles and their bridged derivatives ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC05741C _journal_year 2021 _chemical_formula_moiety 'C25 H24 N2 O5' _chemical_formula_sum 'C25 H24 N2 O5' _chemical_formula_weight 432.46 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens geom _audit_update_record ; 2021-05-28 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 25.4779(15) _cell_length_b 11.8085(6) _cell_length_c 13.8705(7) _cell_measurement_reflns_used 9961 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 72.4255 _cell_measurement_theta_min 3.4695 _cell_volume 4173.0(4) _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_molecular_graphics 'shelXle (C.B. Huebschle, rev 882)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.1556 _diffrn_reflns_av_unetI/netI 0.0586 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 45327 _diffrn_reflns_theta_full 72.73 _diffrn_reflns_theta_max 72.73 _diffrn_reflns_theta_min 3.47 _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1824 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.330 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.430 _refine_diff_density_min -0.462 _refine_ls_extinction_coef 0.0008(3) _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 291 _refine_ls_number_reflns 4147 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0766 _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^)+(0.1569P)^2^+0.5614P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2010 _refine_ls_wR_factor_ref 0.2225 _reflns_number_gt 3183 _reflns_number_total 4147 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc05741c2.cif _cod_data_source_block hd_wql32 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 1565148 _shelx_res_file ; TITL hd_wql32_0m_a.res in Pbcn hd_wql32_0m.res created by SHELXL-2017/1 at 13:00:23 on 15-Oct-2020 CELL 1.54178 25.4779 11.8085 13.8705 90.000 90.000 90.000 ZERR 8.00 0.0015 0.0006 0.0007 0.000 0.000 0.000 LATT 1 SYMM x+1/2, -y+1/2, -z SYMM -x, y, -z+1/2 SYMM -x+1/2, -y+1/2, z+1/2 SFAC C H N O UNIT 200 192 16 40 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.190 SIZE 0.010 0.330 0.350 ACTA EQIV $1 -x+3/2, -y+3/2, z+1/2 HTAB C7 O4_$1 EQIV $2 -x+3/2, y-1/2, z HTAB C19 O3_$2 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.156900 0.561400 EXTI 0.000842 FVAR 0.36266 O1 4 0.516210 0.869364 0.576942 11.00000 0.03485 0.02732 = 0.03398 -0.00413 0.00027 0.00258 O2 4 0.524993 0.764662 0.442141 11.00000 0.03944 0.03414 = 0.03652 -0.00763 -0.00232 0.00153 O3 4 0.816789 0.792477 0.322225 11.00000 0.05216 0.03529 = 0.04680 -0.01200 0.01618 -0.01740 O4 4 0.799646 0.627341 0.258975 11.00000 0.04094 0.03212 = 0.03039 -0.00633 0.00471 -0.00017 O5 4 0.730133 0.537451 0.585335 11.00000 0.04347 0.01866 = 0.04004 0.00162 -0.00592 -0.00200 N1 3 0.668480 0.602145 0.419857 11.00000 0.03415 0.01628 = 0.02772 -0.00271 0.00055 -0.00055 N2 3 0.788964 0.704821 0.317350 11.00000 0.03910 0.02702 = 0.02645 -0.00232 0.00269 -0.00227 C1 1 0.437722 0.897543 0.666587 11.00000 0.04162 0.04104 = 0.03658 0.00132 0.00204 0.00480 AFIX 137 H1 2 0.454784 0.872121 0.726095 11.00000 -1.50000 H4 2 0.400072 0.881008 0.669927 11.00000 -1.50000 H3 2 0.442908 0.979281 0.658916 11.00000 -1.50000 AFIX 0 C2 1 0.461315 0.836601 0.582058 11.00000 0.03235 0.03551 = 0.04081 -0.00288 -0.00110 0.00128 AFIX 23 H23 2 0.458203 0.753666 0.590796 11.00000 -1.20000 H24 2 0.442922 0.858007 0.521885 11.00000 -1.20000 AFIX 0 C3 1 0.543582 0.825911 0.502348 11.00000 0.03790 0.02036 = 0.02857 -0.00131 -0.00145 0.00228 C4 1 0.599508 0.867924 0.504892 11.00000 0.03616 0.01905 = 0.02944 -0.00244 -0.00160 0.00073 AFIX 23 H21 2 0.611932 0.867113 0.572516 11.00000 -1.20000 H22 2 0.600182 0.947458 0.482352 11.00000 -1.20000 AFIX 0 C5 1 0.637389 0.798860 0.443631 11.00000 0.03540 0.01776 = 0.02705 0.00044 -0.00021 0.00235 AFIX 13 H5 2 0.619530 0.776897 0.382214 11.00000 -1.20000 AFIX 0 C6 1 0.657648 0.688724 0.495735 11.00000 0.03297 0.02018 = 0.02630 -0.00255 0.00043 0.00370 C7 1 0.709736 0.727609 0.539859 11.00000 0.03237 0.01487 = 0.02818 -0.00212 -0.00160 -0.00062 AFIX 13 H11 2 0.702087 0.785814 0.590306 11.00000 -1.20000 AFIX 0 C8 1 0.743730 0.636637 0.584045 11.00000 0.03607 0.01892 = 0.02432 -0.00013 0.00046 0.00038 C9 1 0.796049 0.671447 0.622843 11.00000 0.03561 0.02035 = 0.02440 0.00157 0.00095 -0.00079 C10 1 0.833905 0.588125 0.637979 11.00000 0.03953 0.01874 = 0.02585 0.00099 0.00160 0.00146 AFIX 43 H14 2 0.825403 0.510731 0.627696 11.00000 -1.20000 AFIX 0 C11 1 0.884025 0.617950 0.668054 11.00000 0.03804 0.02908 = 0.02681 0.00395 -0.00123 0.00125 AFIX 43 H15 2 0.909971 0.561088 0.676776 11.00000 -1.20000 AFIX 0 C12 1 0.896290 0.730596 0.685393 11.00000 0.03472 0.03093 = 0.02965 0.00135 -0.00073 -0.00156 AFIX 43 H2 2 0.930712 0.750999 0.705180 11.00000 -1.20000 AFIX 0 C13 1 0.618089 0.627278 0.556240 11.00000 0.03365 0.01868 = 0.02706 0.00423 -0.00041 0.00035 C14 1 0.599949 0.656199 0.647441 11.00000 0.03418 0.02122 = 0.02792 -0.00132 -0.00106 -0.00173 AFIX 43 H20 2 0.614592 0.718318 0.681657 11.00000 -1.20000 AFIX 0 C15 1 0.559687 0.591550 0.687303 11.00000 0.03284 0.02737 = 0.02948 0.00453 0.00112 0.00041 AFIX 43 H6 2 0.546641 0.609841 0.749546 11.00000 -1.20000 AFIX 0 C16 1 0.538351 0.500569 0.637119 11.00000 0.03246 0.02533 = 0.03795 0.00489 0.00214 0.00060 AFIX 43 H7 2 0.509955 0.459282 0.664231 11.00000 -1.20000 AFIX 0 C17 1 0.558272 0.469509 0.547469 11.00000 0.03319 0.01883 = 0.03565 -0.00038 -0.00340 -0.00123 AFIX 43 H8 2 0.544477 0.406035 0.513870 11.00000 -1.20000 AFIX 0 C18 1 0.598596 0.533125 0.508409 11.00000 0.03447 0.01721 = 0.02910 0.00314 -0.00222 0.00099 C19 1 0.627765 0.514427 0.415236 11.00000 0.03864 0.02020 = 0.03319 -0.00434 0.00108 -0.00620 AFIX 23 H10 2 0.643342 0.437687 0.412520 11.00000 -1.20000 H9 2 0.604544 0.525424 0.358779 11.00000 -1.20000 AFIX 0 C20 1 0.711514 0.607227 0.366477 11.00000 0.03485 0.02136 = 0.02507 -0.00291 -0.00141 0.00009 AFIX 43 H19 2 0.718711 0.549700 0.320460 11.00000 -1.20000 AFIX 0 C21 1 0.745776 0.696435 0.378087 11.00000 0.03584 0.02217 = 0.02600 -0.00115 0.00191 -0.00210 C22 1 0.734171 0.788192 0.450909 11.00000 0.03888 0.01953 = 0.02486 0.00102 -0.00205 0.00009 AFIX 13 H16 2 0.766267 0.832446 0.468302 11.00000 -1.20000 AFIX 0 C23 1 0.808234 0.784993 0.641806 11.00000 0.03652 0.02206 = 0.02628 0.00085 0.00006 -0.00103 AFIX 43 H12 2 0.782466 0.842178 0.632834 11.00000 -1.20000 AFIX 0 C24 1 0.858117 0.813491 0.673751 11.00000 0.04253 0.02104 = 0.02667 -0.00024 0.00038 -0.00332 AFIX 43 H13 2 0.866232 0.890267 0.687770 11.00000 -1.20000 AFIX 0 C25 1 0.688710 0.865212 0.419156 11.00000 0.03865 0.01944 = 0.02704 0.00309 0.00028 -0.00078 AFIX 23 H17 2 0.690778 0.880884 0.349143 11.00000 -1.20000 H18 2 0.689785 0.938051 0.454442 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM hd_wql32_0m_a.res in Pbcn REM R1 = 0.0766 for 3183 Fo > 4sig(Fo) and 0.0928 for all 4147 data REM 291 parameters refined using 0 restraints END WGHT 0.1569 0.5614 REM Instructions for potential hydrogen bonds HTAB C7 O4_$1 HTAB C19 O3_$2 REM Highest difference peak 0.430, deepest hole -0.462, 1-sigma level 0.089 Q1 1 0.6489 0.7487 0.4742 11.00000 0.05 0.36 Q2 1 0.7360 0.7464 0.4171 11.00000 0.05 0.34 Q3 1 0.6129 0.4646 0.3583 11.00000 0.05 0.33 Q4 1 0.7101 0.7875 0.5561 11.00000 0.05 0.32 Q5 1 0.7318 0.4499 0.5779 11.00000 0.05 0.29 ; _shelx_res_checksum 90990 _shelx_hkl_file ; 0 -1 0 -0.70 0.60 0 1 0 -0.10 1.10 0 -1 0 0.60 1.90 0 -2 0 5028.70 463.45 0 -2 0 5566.24 460.85 0 -3 0 -3.50 3.90 0 -3 0 2.40 3.40 0 -3 0 2.80 2.70 0 -4 0 1360.66 117.89 0 -4 0 1209.98 122.29 0 -5 0 0.10 4.50 0 -5 0 5.60 6.70 0 -6 0 335.87 44.10 0 -7 0 6.50 9.20 0 -7 0 -6.30 7.40 0 -8 0 569.94 55.29 0 -8 0 523.95 56.29 0 -9 0 19.50 19.10 0 -9 0 32.00 23.30 0 -10 0 432.16 47.10 0 -10 0 561.54 67.99 0 -10 0 481.85 81.09 0 -10 0 429.16 45.90 0 -11 0 25.70 40.40 0 -11 0 41.90 25.10 0 -11 0 8.70 5.20 0 11 0 2.50 3.60 0 -12 0 763.52 73.69 0 12 0 772.32 72.79 0 -13 0 -6.10 4.40 0 13 0 2.20 3.20 0 14 0 4.70 4.00 0 -14 0 6.50 3.90 0 0 1 0.90 1.70 0 0 -1 0.00 0.40 0 0 1 -1.50 2.20 0 0 -1 1.50 1.50 0 -1 -1 -0.40 2.10 0 -1 -1 -0.30 1.00 0 1 1 0.00 1.50 0 -2 1 27.50 9.40 0 -2 -1 24.00 6.00 0 -2 -1 29.00 5.60 0 -2 -1 30.90 7.60 0 -3 -1 2.70 2.10 0 -3 -1 3.90 4.00 0 -3 -1 4.40 4.50 0 -3 1 -2.50 5.50 0 -4 1 15.00 7.20 0 -4 -1 15.20 8.90 0 -4 1 19.40 8.70 0 -4 -1 10.90 6.30 0 -4 -1 8.60 6.50 0 -5 -1 0.70 2.90 0 -5 1 4.00 6.80 0 -5 -1 3.30 6.50 0 -5 1 4.20 7.80 0 -6 -1 118.09 19.00 0 -6 1 132.89 24.90 0 -6 -1 123.09 22.10 0 -6 1 103.59 29.40 0 -6 -1 166.68 27.90 0 -7 -1 12.00 8.60 0 -7 -1 1.70 8.40 0 -7 1 -10.10 6.90 0 -7 1 8.30 8.70 0 -8 1 13.10 11.90 0 8 -1 1.00 4.30 0 -8 1 -6.40 3.40 0 -8 -1 0.60 3.90 0 -8 -1 -5.10 5.60 0 -8 -1 -2.30 10.50 0 9 1 3.00 5.60 0 -9 1 -9.10 17.40 0 -9 -1 0.30 17.80 0 -9 -1 1.30 3.80 0 -9 1 2.00 18.50 0 -9 -1 17.10 22.30 0 -10 1 -6.40 5.10 0 -10 -1 5.80 29.60 0 -10 1 -3.10 30.10 0 -10 1 -1.00 3.80 0 -10 -1 5.50 18.60 0 -10 -1 4.30 4.10 0 10 -1 2.80 3.60 0 -10 -1 -0.50 5.70 0 -10 1 15.00 26.30 0 -11 1 42.80 44.70 0 -11 1 -12.00 30.30 0 -11 1 11.90 6.50 0 11 1 6.00 4.40 0 -11 1 -1.00 3.20 0 11 -1 1.30 3.20 0 -11 -1 4.40 4.00 0 -11 -1 -40.80 35.10 0 12 1 176.68 22.50 0 -12 1 180.18 22.60 0 -12 -1 191.58 23.60 0 -12 1 206.38 23.80 0 12 -1 219.08 23.60 0 13 -1 -1.00 2.30 0 -13 -1 1.50 3.00 0 13 1 -0.50 3.60 0 -14 -1 129.19 14.10 0 14 1 91.99 12.30 0 14 -1 92.69 12.60 0 -1 -2 -2.10 4.80 0 -1 -2 0.50 1.50 0 -1 2 7.70 6.00 0 -1 -2 -0.20 1.50 0 -2 -2 7.00 4.70 0 -2 2 7.60 6.30 0 3 2 0.60 0.90 0 -3 -2 -0.60 4.50 0 -3 -2 4.30 2.90 0 -3 -2 4.80 2.50 0 -3 2 -4.60 6.20 0 4 2 226.18 19.50 0 -4 2 181.08 29.30 0 4 2 208.18 19.40 0 -4 -2 207.98 24.30 0 -4 -2 218.68 23.80 0 -5 2 0.60 3.00 0 -5 -2 0.70 5.90 0 -5 2 0.60 1.30 0 -5 -2 2.00 5.60 0 -5 -2 3.00 3.30 0 -5 2 1.40 1.60 0 -5 2 -6.50 6.80 0 -6 2 404.16 60.79 0 -6 -2 471.15 53.79 0 -6 -2 632.84 68.69 0 -6 2 551.34 61.69 0 -6 -2 543.25 54.69 0 -7 -2 3.70 7.90 0 -7 -2 7.60 13.20 0 -7 2 3.00 9.90 0 -7 2 23.30 16.10 0 -7 -2 -0.30 6.80 0 -8 -2 45.40 19.60 0 -8 2 8.50 14.40 0 -8 2 5.50 6.20 0 -8 2 15.40 6.10 0 -8 -2 17.10 7.50 0 -8 -2 13.20 6.40 0 -9 -2 2.60 3.40 0 -9 2 19.20 22.10 0 -9 2 -2.40 4.90 0 -9 2 4.40 4.90 0 -9 -2 10.30 6.90 0 -9 -2 -7.60 19.70 0 -9 2 -1.90 15.90 0 -10 2 214.98 25.00 0 -10 2 140.59 54.09 0 -10 2 227.78 51.09 0 -10 -2 177.48 24.90 0 -10 2 188.88 25.60 0 10 -2 208.38 23.70 0 10 2 242.48 24.50 0 -11 2 9.10 34.60 0 -11 2 1.00 4.90 0 -11 -2 65.19 53.19 0 -11 2 -7.50 41.40 0 11 2 0.50 4.40 0 -11 2 10.40 5.10 0 12 -2 67.29 11.70 0 -12 2 84.89 14.40 0 -12 -2 79.59 13.20 0 -12 2 105.39 13.40 0 12 2 84.79 13.10 0 13 -2 -1.40 2.80 0 -13 -2 3.20 3.70 0 -13 2 -1.90 6.80 0 -13 2 4.10 4.70 0 13 2 1.40 3.80 0 14 -2 6.40 3.60 0 14 2 8.40 4.70 0 0 -3 -0.30 1.00 0 -1 -3 4.70 3.10 0 -1 -3 -1.20 1.40 0 -1 -3 -5.40 4.50 0 -2 3 495.55 55.69 0 -2 -3 501.55 47.20 0 -3 3 1.00 7.60 0 -3 -3 -6.60 5.00 0 -3 -3 -2.10 2.80 0 -4 -3 251.37 27.90 0 -4 -3 248.48 36.80 0 -4 3 234.78 36.60 0 -5 3 7.70 9.80 0 -5 -3 3.60 3.60 0 5 3 3.30 1.50 0 -5 3 -0.40 1.70 0 -5 -3 -2.40 8.40 0 -6 3 87.99 19.40 0 -6 -3 60.59 18.20 0 -6 -3 71.59 14.50 0 -6 3 68.09 24.70 0 -7 -3 8.40 7.00 0 -7 -3 3.40 4.90 0 -7 -3 -2.60 3.60 0 -7 3 0.70 6.30 0 -7 -3 3.30 13.00 0 -7 3 -7.40 5.10 0 -7 3 1.30 14.00 0 -8 3 25.80 7.20 0 -8 3 27.60 21.20 0 -8 3 13.50 14.10 0 -8 -3 29.70 8.50 0 -8 -3 17.70 6.90 0 -8 -3 25.10 21.40 0 8 -3 12.50 5.30 0 -8 3 25.20 9.00 0 -9 -3 8.10 25.90 0 -9 3 11.10 17.40 0 -9 3 27.80 26.20 0 -10 -3 78.69 40.00 0 10 -3 107.69 14.90 0 -10 -3 105.89 16.60 0 -10 3 125.49 16.00 0 -10 3 61.89 37.30 0 -10 3 104.89 18.20 0 -10 3 106.49 36.00 0 11 3 2.50 6.10 0 -11 3 -0.50 5.40 0 -11 3 10.80 6.40 0 -11 3 38.40 35.40 0 -12 3 344.87 35.40 0 12 -3 277.77 33.20 0 -12 3 372.56 36.40 0 12 3 334.37 34.60 0 -12 -3 302.47 34.90 0 -13 3 -3.10 4.00 0 13 3 -3.80 4.10 0 13 -3 2.60 3.20 0 -13 -3 3.00 3.90 0 14 -3 53.29 7.90 0 -14 -3 75.19 9.50 0 0 -4 3760.02 330.67 0 0 -4 3845.32 338.77 0 -1 -4 1.30 7.20 0 -1 4 3.20 11.20 0 1 -4 1.90 1.30 0 -1 -4 0.50 4.30 0 -1 -4 -1.50 1.90 0 -2 4 97.29 23.30 0 -2 -4 76.49 10.60 0 -3 -4 14.10 10.90 0 -3 4 5.70 8.10 0 4 4 25.20 5.40 0 -4 -4 27.20 8.20 0 -4 -4 6.90 11.30 0 -4 4 18.00 5.00 0 -4 4 12.50 13.50 0 5 4 -1.00 2.00 0 -5 4 9.70 11.30 0 -5 4 3.60 2.30 0 -5 -4 6.60 4.80 0 -5 -4 -6.30 9.00 0 -6 4 31.70 19.10 0 -6 -4 11.90 6.80 0 -6 4 8.10 3.90 0 -6 -4 2.70 13.20 0 -7 -4 -11.00 14.50 0 -7 -4 6.00 6.10 0 -7 4 2.20 8.80 0 -7 -4 -6.10 3.50 0 -7 4 -0.70 6.00 0 -7 4 -8.40 8.00 0 7 -4 -1.90 2.20 0 -7 4 0.40 3.40 0 -7 -4 0.10 6.20 0 -8 4 -3.00 12.20 0 -8 -4 6.50 7.10 0 -8 -4 6.00 3.80 0 -8 4 2.80 4.90 0 8 -4 8.10 3.40 0 -8 4 3.90 20.10 0 -8 -4 -19.80 19.30 0 -9 4 17.50 24.20 0 -9 -4 -2.70 3.30 0 9 -4 -1.70 2.60 0 -9 -4 0.10 31.40 0 -9 4 8.90 6.30 0 -9 4 -2.50 4.90 0 -10 4 182.48 25.30 0 -10 4 165.18 45.00 0 -10 4 153.58 54.19 0 -10 -4 164.38 23.00 0 10 -4 213.18 22.50 0 -11 -4 -8.90 4.60 0 -11 4 -40.90 48.40 0 11 -4 2.80 4.30 0 12 -4 60.89 10.20 0 -12 4 74.69 13.40 0 -12 -4 56.79 11.30 0 12 4 55.49 11.50 0 -13 -4 -2.70 2.20 0 13 -4 -0.70 3.00 0 13 4 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0 10 -5 147.09 24.50 0 -10 5 45.20 49.40 0 -10 5 98.59 19.20 0 -11 5 35.80 64.89 0 -12 -5 13.90 5.70 0 -12 5 17.70 5.90 0 12 -5 10.90 4.60 0 -13 5 -6.80 3.90 0 -13 -5 -1.20 2.50 0 13 5 -1.80 5.40 0 13 -5 -3.00 2.10 0 0 -6 192.98 20.90 0 0 -6 213.18 32.10 0 1 -6 29.40 16.90 0 -1 -6 5.20 3.40 0 -1 -6 11.00 7.90 0 -2 6 518.95 71.59 0 2 -6 601.44 52.89 0 -3 -6 8.00 5.30 0 -3 6 17.70 21.20 0 -4 -6 167.28 38.30 0 4 6 257.07 27.60 0 -4 6 311.57 47.30 0 -4 6 189.58 24.80 0 -5 6 -32.60 19.40 0 5 6 -1.90 4.40 0 -6 -6 9.30 10.20 0 -6 -6 26.10 19.10 0 -6 -6 25.50 13.10 0 -6 6 41.00 30.80 0 -6 6 22.80 7.70 0 6 -6 27.50 5.60 0 6 -6 17.20 6.30 0 -6 6 21.90 10.10 0 -6 -6 16.70 5.70 0 6 6 8.20 7.10 0 -6 6 12.20 4.60 0 -7 6 5.90 6.30 0 7 -6 6.70 4.50 0 -7 6 1.00 3.30 0 -7 -6 14.10 14.40 0 -7 6 8.70 3.50 0 -7 -6 -20.50 26.00 0 7 -6 -0.20 2.60 0 -7 -6 2.90 8.00 0 -7 -6 -1.20 6.40 0 -7 6 -8.90 9.80 0 8 -6 674.73 73.59 0 -8 6 739.23 69.59 0 -8 6 815.12 110.59 0 -8 6 813.72 107.59 0 8 -6 705.13 72.89 0 -9 -6 0.10 6.30 0 -9 -6 1.60 3.80 0 9 -6 3.10 5.50 0 -9 -6 -31.10 42.30 0 -9 6 -4.60 3.00 0 -9 6 1.50 5.40 0 9 -6 1.40 2.80 0 10 -6 410.16 40.00 0 -10 6 576.84 101.69 0 -10 6 279.37 79.79 0 -10 6 435.56 45.50 0 -10 6 349.47 44.40 0 -10 -6 374.86 42.20 0 11 -6 -3.10 2.40 0 11 -6 -4.50 8.00 0 -11 -6 -0.30 3.20 0 -11 6 -6.10 4.30 0 12 -6 63.59 8.80 0 -12 -6 61.79 11.30 0 -13 -6 1.30 2.30 0 -13 6 0.60 3.90 0 13 -6 -3.00 2.40 0 0 -7 6.60 3.70 0 -1 -7 9.60 8.90 0 -1 -7 6.60 4.10 0 1 -7 1.80 3.20 0 -2 -7 481.15 46.90 0 2 7 429.86 48.20 0 2 -7 464.65 43.00 0 3 -7 4.00 3.30 0 -3 7 44.40 30.90 0 3 7 4.40 4.50 0 -4 -7 90.99 29.50 0 4 7 167.88 22.70 0 -4 7 250.37 57.19 0 -4 -7 171.28 22.80 0 -4 7 132.59 19.40 0 -5 -7 11.90 22.50 0 -5 7 2.20 3.70 0 5 -7 -1.00 4.10 0 -5 7 0.30 3.80 0 5 7 2.10 6.20 0 -5 -7 5.90 8.00 0 -5 -7 8.10 7.00 0 -6 -7 -5.70 8.60 0 -6 -7 0.60 5.60 0 -6 -7 2.70 22.20 0 -6 7 0.00 7.10 0 -6 7 1.40 2.70 0 -6 -7 3.70 5.80 0 6 -7 -3.00 3.70 0 -6 7 1.30 6.50 0 6 -7 2.10 3.20 0 -6 7 1.60 3.60 0 -6 -7 12.00 5.10 0 6 7 17.10 10.30 0 -7 7 0.40 3.20 0 -7 -7 -11.10 8.70 0 -7 7 -3.50 32.60 0 -7 7 4.60 5.10 0 7 -7 -0.10 2.40 0 -7 -7 -2.00 6.70 0 -7 7 10.90 14.60 0 -7 -7 -40.50 27.70 0 -7 -7 -0.70 4.00 0 -7 7 1.10 3.70 0 8 -7 517.75 56.99 0 -8 7 687.13 150.98 0 -8 7 576.74 82.69 0 -8 -7 552.54 55.69 0 -8 7 583.04 59.89 0 8 -7 546.35 52.29 0 -8 7 520.75 53.69 0 -9 7 5.10 5.90 0 -9 7 0.90 3.30 0 9 -7 -7.30 4.80 0 9 -7 2.40 2.90 0 -9 -7 3.60 3.80 0 -9 7 -33.50 55.39 0 -9 -7 8.50 6.30 0 -9 -7 -92.39 83.09 0 -10 7 346.37 33.50 0 -10 7 318.27 123.29 0 -10 7 353.56 38.70 0 -10 -7 296.67 35.00 0 10 -7 283.07 32.00 0 10 -7 338.37 38.60 0 11 -7 1.40 2.70 0 11 -7 -4.60 5.80 0 -11 -7 2.50 2.80 0 12 -7 43.10 6.70 0 -12 -7 39.50 8.20 0 -12 7 49.30 12.40 0 -13 -7 1.90 2.70 0 -13 7 1.30 4.00 0 0 -8 974.70 80.89 0 0 8 757.12 84.59 0 1 8 3.80 4.20 0 -1 8 0.70 3.50 0 1 -8 33.90 37.10 0 1 -8 7.50 5.30 0 -1 -8 -3.40 5.50 0 -1 -8 5.50 14.00 0 2 8 383.76 42.80 0 -2 8 319.07 46.70 0 2 -8 347.07 34.70 0 -2 -8 413.96 40.00 0 3 -8 4.90 3.40 0 -3 -8 6.70 7.20 0 -3 -8 -10.30 8.00 0 3 8 10.10 9.80 0 -3 -8 7.30 3.70 0 -4 8 186.68 24.40 0 -4 -8 235.38 36.40 0 4 8 186.68 27.20 0 -4 8 143.69 23.40 0 -4 -8 174.18 23.10 0 -4 8 136.39 24.70 0 -4 -8 222.18 27.40 0 -5 -8 8.80 24.70 0 -5 -8 3.90 4.20 0 -5 8 11.30 8.20 0 -5 8 0.50 3.30 0 -5 -8 12.20 5.60 0 5 -8 4.60 3.00 0 -5 8 10.40 4.10 0 -5 -8 -8.10 7.40 0 -5 8 15.70 9.10 0 5 8 -0.10 10.40 0 -5 -8 3.80 9.60 0 -6 8 473.55 44.40 0 6 -8 395.46 44.60 0 -6 8 382.66 41.60 0 -6 8 333.27 46.60 0 6 -8 473.55 40.30 0 -6 8 424.06 48.90 0 -6 -8 393.36 43.50 0 -6 8 560.04 91.99 0 -6 -8 503.45 45.20 0 -7 -8 -3.70 4.20 0 -7 8 -93.59 55.19 0 -7 8 -0.90 3.20 0 7 -8 -0.30 4.70 0 -7 8 5.40 3.70 0 -7 8 -0.60 6.40 0 -7 -8 2.70 5.60 0 -7 -8 11.30 16.00 0 -7 -8 1.00 5.80 0 -8 8 90.29 13.00 0 -8 8 55.99 10.20 0 -8 8 -7.30 88.09 0 -8 8 62.99 14.60 0 -8 -8 26.60 56.99 0 -8 8 55.29 25.50 0 8 -8 109.59 19.40 0 8 -8 82.39 10.40 0 -9 8 3.00 3.50 0 9 -8 2.70 3.60 0 -9 -8 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21.50 10 11 -7 28.80 9.70 10 -11 7 41.90 14.00 10 -11 -7 45.20 7.80 10 11 7 30.30 9.00 -10 -12 -7 8.10 5.10 -10 -12 7 13.40 8.60 10 0 8 104.09 13.70 -10 0 8 127.99 15.60 10 0 8 82.99 13.70 -10 0 -8 122.79 16.00 10 0 -8 91.59 15.40 10 0 8 140.99 21.00 -10 0 -8 101.99 21.30 -10 0 8 93.19 17.20 10 0 -8 134.09 20.10 10 -1 8 32.60 14.70 -10 -1 -8 24.70 9.80 10 1 -8 -0.80 8.00 -10 -1 -8 38.60 20.40 10 -1 8 23.60 8.00 10 -1 8 21.20 5.80 -10 -1 -8 32.80 13.80 10 1 8 19.40 8.30 -10 1 -8 11.70 8.70 -10 -1 8 15.40 9.80 10 -1 -8 9.00 7.10 10 -1 -8 17.60 6.30 10 1 8 10.10 6.70 10 -2 8 209.78 28.80 -10 -2 -8 215.78 25.50 -10 -2 -8 261.37 30.60 -10 -2 -8 208.28 39.90 10 2 -8 240.48 33.80 10 -2 8 245.78 24.20 10 -2 8 193.88 24.20 10 2 -8 207.08 26.90 10 -2 8 216.18 33.50 -10 -2 -8 208.08 33.90 -10 -2 8 226.38 25.80 -10 2 -8 211.08 30.20 10 2 8 235.98 30.70 -10 -2 8 224.28 27.30 10 -2 -8 246.98 29.60 -10 -3 -8 10.10 12.20 -10 -3 -8 9.00 8.00 10 -3 8 12.30 17.30 -10 -3 -8 23.80 6.70 10 -3 8 31.50 7.00 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2.50 4.10 12 5 -5 55.79 13.10 12 -5 5 64.39 7.40 12 -5 5 58.49 9.10 12 -5 5 45.40 12.40 -12 -5 -5 40.00 11.80 12 -5 5 29.20 31.30 -12 -5 -5 56.09 20.60 12 -5 5 35.70 19.20 12 5 -5 60.79 9.80 -12 -5 -5 40.70 23.20 -12 -5 -5 27.50 47.00 12 5 -5 51.69 13.70 -12 -5 -5 50.99 11.00 12 -5 5 46.40 9.90 12 -5 -5 30.70 22.10 -12 -5 5 42.20 10.00 12 5 5 37.60 12.30 12 -5 -5 41.20 8.70 12 -5 -5 55.59 14.80 -12 -5 5 167.58 54.09 -12 -5 5 61.39 15.00 12 5 5 34.10 12.60 -12 -5 5 63.89 10.30 12 5 5 58.09 9.30 12 -6 5 -41.80 36.00 12 6 -5 2.40 3.90 -12 -6 -5 8.40 6.20 12 -6 5 9.10 3.40 -12 -6 -5 30.10 20.90 12 -6 5 12.20 12.80 12 -6 5 13.70 8.10 12 6 -5 11.80 7.70 -12 -6 -5 8.10 8.40 -12 -6 -5 18.70 16.00 -12 -6 -5 5.90 8.00 12 -6 5 16.70 33.30 -12 -6 -5 3.10 36.40 12 6 -5 17.70 7.50 12 -6 5 4.30 3.50 -12 -6 5 -1.10 8.40 -12 -6 5 8.20 4.70 12 6 5 8.10 5.30 12 -6 -5 40.80 29.50 12 -6 -5 11.70 4.20 -12 -6 5 5.60 4.80 12 -6 -5 3.20 6.80 -12 6 -5 6.30 3.00 -12 -6 5 31.20 49.00 12 -6 -5 8.90 6.10 -12 -7 -5 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38.90 23.20 12 -6 6 55.49 40.20 -12 -6 -6 27.20 9.00 12 -6 6 26.20 6.40 -12 -6 -6 34.30 12.80 -12 -6 -6 30.70 10.00 -12 -6 6 24.30 8.40 -12 -6 6 46.70 17.60 12 -6 -6 30.70 11.30 -12 -6 6 -51.89 62.29 12 -6 -6 30.30 11.10 -12 6 -6 40.10 6.80 12 -6 -6 -10.10 26.90 12 -7 6 112.49 13.00 -12 -7 -6 89.59 30.20 12 7 -6 84.39 13.00 12 -7 6 47.00 36.50 12 7 -6 108.39 17.80 -12 -7 -6 92.49 17.20 -12 -7 -6 61.29 15.20 12 -7 6 66.19 14.70 12 7 -6 90.39 18.00 -12 7 -6 109.29 11.40 -12 -7 6 104.09 93.09 12 -7 -6 86.59 17.10 -12 -7 6 67.59 15.60 12 7 6 90.89 12.50 -12 -7 6 89.89 15.20 12 -7 -6 13.90 34.40 12 -8 6 3.90 3.30 -12 -8 -6 -0.10 5.40 12 8 -6 -0.30 6.70 12 -8 6 9.60 39.20 12 8 -6 7.20 3.50 -12 -8 -6 50.79 31.20 12 8 -6 16.10 8.90 12 -8 6 2.30 5.10 12 -8 6 17.70 53.49 -12 -8 -6 4.70 6.50 12 8 6 8.20 5.30 12 -8 -6 -11.40 40.60 12 -8 -6 9.40 6.40 12 -8 -6 -1.20 4.00 -12 -8 6 111.39 101.59 -12 -8 6 9.80 44.70 -12 -8 6 -2.50 7.50 -12 -8 6 -3.00 4.50 -12 8 -6 1.60 2.50 -12 9 6 42.30 9.90 12 -9 6 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54.49 10.90 -15 -3 7 41.10 10.80 15 3 7 63.09 8.70 -15 -4 -7 43.80 25.00 15 4 -7 52.49 13.20 15 4 -7 89.59 17.40 -15 -4 -7 59.59 35.50 15 -4 7 100.69 12.60 -15 -4 -7 92.29 15.60 -15 4 7 61.99 10.70 15 -4 7 88.79 9.80 15 -4 7 95.49 17.70 -15 -4 -7 71.49 13.80 -15 4 -7 39.00 14.20 15 4 7 48.30 11.00 -15 -4 7 75.29 15.70 15 -4 -7 64.89 11.90 15 -4 -7 65.79 15.30 15 4 7 67.79 9.90 15 4 7 37.80 28.50 -15 -4 7 75.89 12.60 -15 -5 -7 18.80 17.40 -15 5 7 55.69 10.00 15 5 -7 78.29 18.10 -15 -5 -7 61.99 13.90 15 5 -7 59.29 14.60 15 -5 7 70.69 14.60 -15 -5 -7 43.00 11.20 -15 -5 -7 75.99 13.90 15 -5 7 62.59 7.70 15 5 7 48.60 11.30 -15 -5 7 64.49 14.10 15 5 7 55.49 9.40 15 -5 -7 76.89 16.80 -15 5 -7 59.99 18.80 -15 -5 7 49.10 10.00 -15 -5 7 61.09 18.20 15 6 -7 16.10 10.10 15 -6 7 11.50 7.10 15 -6 7 22.30 4.10 15 6 -7 26.10 8.80 -15 -6 -7 15.40 8.90 -15 6 7 6.80 5.70 -15 -6 -7 27.30 30.00 15 -6 7 24.80 5.80 -15 -6 -7 21.50 8.70 -15 -6 7 19.80 7.00 -15 6 -7 7.10 11.90 15 6 7 16.30 8.40 15 6 7 24.30 5.80 15 -6 -7 52.09 45.40 -15 -6 7 13.50 5.20 -15 -6 7 27.20 12.30 15 -6 -7 13.80 8.20 -15 -7 -7 14.40 8.40 15 7 -7 13.40 8.60 15 -7 7 6.40 6.60 -15 7 7 14.40 5.50 -15 -7 -7 5.30 7.00 15 7 -7 14.70 9.50 15 -7 7 14.50 4.60 -15 -7 7 7.80 9.50 -15 -7 7 11.60 5.70 15 7 7 14.40 5.20 15 -7 -7 7.70 6.00 -15 -8 -7 2.10 4.90 -15 8 7 3.80 4.00 15 8 -7 4.40 5.80 15 -8 7 4.00 3.10 -15 -8 7 6.50 8.70 -15 -8 7 -7.40 4.00 15 -8 -7 0.50 4.60 15 -9 7 1.70 3.80 15 9 -7 -1.10 9.20 15 -9 7 2.50 4.20 -15 -9 -7 0.10 4.90 -15 9 7 6.70 3.80 15 -9 -7 -7.20 4.60 -15 -9 7 -2.70 4.10 -15 -9 7 8.00 7.80 15 9 7 -5.30 3.40 15 10 -7 4.50 6.20 -15 10 7 0.50 3.80 15 -10 7 6.30 4.30 -15 -10 -7 -0.10 3.40 -15 -10 7 -0.50 4.30 15 10 7 2.00 3.90 15 -11 7 7.10 3.20 -15 -11 -7 4.60 4.00 -15 -11 7 4.30 5.40 15 11 7 1.00 3.40 15 0 8 224.68 23.00 -15 0 8 222.58 25.00 15 0 -8 232.48 31.20 -15 0 8 246.08 30.70 -15 0 -8 189.28 34.20 15 0 -8 193.38 27.10 15 0 8 213.08 24.30 15 0 8 197.58 31.70 15 -1 8 61.19 10.50 15 -1 8 70.39 24.30 15 1 -8 63.49 15.10 -15 -1 -8 32.00 12.50 15 1 -8 55.69 13.30 -15 1 8 60.79 10.90 -15 1 8 62.89 16.50 15 -1 8 57.09 8.10 -15 -1 -8 57.79 19.90 -15 -1 -8 100.79 36.70 15 1 8 35.10 7.40 -15 1 -8 39.50 17.30 -15 -1 8 28.70 9.60 15 -1 -8 46.50 10.70 -15 1 -8 13.20 38.00 -15 -1 8 46.70 9.50 15 -1 -8 53.09 16.10 15 1 8 52.79 10.70 15 1 8 44.20 17.60 -15 1 -8 49.10 12.30 15 -2 8 15.00 4.40 -15 -2 -8 20.30 16.20 -15 2 8 21.80 6.60 15 2 -8 12.00 8.80 -15 -2 -8 16.60 29.80 15 -2 8 11.90 4.60 15 2 -8 13.00 8.30 -15 -2 -8 15.10 8.90 15 -2 -8 20.30 6.00 15 2 8 10.00 4.30 -15 -2 8 11.40 5.70 15 2 8 20.10 6.00 -15 -2 8 11.10 6.10 -15 2 -8 5.10 6.40 -15 2 -8 14.40 11.50 15 -2 -8 16.50 8.00 -15 2 -8 -33.80 37.30 15 -3 8 2.20 3.30 15 -3 8 3.60 2.80 -15 3 8 2.30 3.60 -15 -3 -8 4.10 20.00 15 -3 8 2.80 9.40 -15 -3 -8 1.70 7.80 -15 -3 -8 -6.70 6.20 15 3 -8 8.10 9.40 15 -3 -8 4.30 5.10 -15 -3 8 -0.80 3.60 -15 3 -8 -17.10 9.30 -15 -3 8 -1.40 4.80 15 3 8 2.70 3.20 15 -3 -8 -3.70 4.90 15 3 8 6.00 4.90 -15 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22.70 15 2 -9 127.79 23.70 -15 -2 -9 99.39 30.50 -15 2 9 149.29 23.10 -15 -2 -9 156.08 24.20 -15 -2 -9 119.69 21.60 -15 2 9 156.98 20.40 15 -2 9 157.88 17.90 -15 -2 -9 85.09 42.70 15 2 -9 186.98 24.60 15 -2 9 189.08 20.40 15 2 9 188.18 21.40 15 -2 -9 144.19 19.40 -15 2 -9 161.08 22.10 -15 -2 9 173.18 21.50 15 2 9 166.68 18.40 -15 -2 9 172.68 23.60 15 -2 -9 186.38 26.90 -15 2 -9 172.68 58.69 15 3 -9 -5.20 7.90 15 3 -9 27.50 11.50 -15 -3 -9 12.70 40.30 -15 -3 -9 22.80 8.40 -15 3 9 11.50 6.10 -15 3 9 14.60 9.00 -15 -3 -9 18.30 23.50 15 -3 9 18.50 4.50 -15 -3 -9 12.30 6.40 -15 -3 -9 37.80 27.10 -15 -3 -9 10.20 9.30 15 -3 9 1.20 12.10 15 -3 9 18.80 5.90 15 3 9 9.30 6.60 -15 3 -9 10.30 6.20 15 -3 -9 16.60 6.10 -15 -3 9 16.10 6.20 15 -3 -9 24.00 9.30 15 3 9 10.20 5.00 -15 3 -9 9.00 16.80 -15 -3 9 19.50 6.50 -15 3 -9 3.10 48.60 -15 4 9 1.30 5.40 15 -4 9 3.80 3.70 -15 -4 -9 6.20 6.20 15 4 -9 -4.90 4.80 -15 -4 -9 -33.40 26.80 -15 -4 -9 4.10 8.20 15 -4 9 -0.30 1.90 -15 -4 9 -4.90 2.70 15 4 9 18.00 7.30 15 -4 -9 -1.30 4.80 -15 -4 9 13.80 14.80 -15 -4 9 0.90 3.50 -15 4 -9 5.60 16.50 15 4 9 -4.20 3.20 -15 5 9 7.90 4.70 -15 -5 -9 -7.00 7.10 15 -5 9 1.70 6.90 -15 -5 -9 -9.40 5.40 15 5 -9 -1.50 8.70 15 -5 9 -1.10 3.10 15 -5 9 -3.20 2.00 -15 -5 9 5.50 11.80 -15 -5 9 -2.30 2.60 15 5 9 -2.90 3.60 15 -5 -9 3.20 6.90 15 5 9 -9.50 7.30 -15 -6 -9 95.29 15.30 -15 -6 -9 68.39 14.80 15 -6 9 96.49 9.70 -15 6 9 87.39 14.50 15 6 -9 98.49 18.10 15 -6 9 71.39 16.30 -15 -6 9 67.49 11.30 -15 -6 9 107.39 17.00 15 6 9 91.19 12.40 -15 -6 9 106.89 23.20 15 -6 -9 83.29 16.20 -15 -7 -9 13.50 6.90 -15 7 9 -2.90 6.00 15 -7 9 3.70 7.40 15 -7 9 17.10 4.30 -15 -7 -9 14.90 7.20 15 7 -9 9.40 7.30 -15 -7 9 7.90 9.90 15 -7 -9 5.20 5.20 15 7 9 12.50 5.40 -15 -7 9 9.00 4.90 -15 8 9 -4.90 5.50 -15 -8 -9 4.90 6.30 15 -8 9 2.90 2.70 15 8 -9 2.60 5.10 -15 -8 9 -1.00 3.40 -15 -8 9 19.10 9.00 15 8 9 -6.80 4.00 -15 9 9 11.50 5.80 15 -9 9 25.20 4.90 -15 -9 -9 24.30 6.00 15 -9 9 19.40 5.80 -15 -9 9 11.80 4.30 15 9 9 15.90 5.40 -15 -9 9 22.10 8.70 15 -9 -9 15.60 6.90 15 -10 9 6.80 6.60 15 10 -9 7.10 4.00 -15 -10 -9 4.60 3.80 -15 10 -9 3.90 4.20 -15 -10 9 12.70 5.60 15 0 10 6.30 5.40 -15 0 -10 4.30 7.70 15 0 -10 8.00 5.10 -15 0 -10 -8.70 21.20 -15 0 10 2.00 4.30 15 0 10 1.10 2.90 15 0 -10 2.30 6.20 -15 0 -10 12.70 38.70 -15 0 10 5.50 5.50 15 -1 10 2.40 2.70 -15 -1 -10 14.70 17.00 15 -1 10 1.60 3.20 -15 1 10 -0.30 3.70 -15 1 10 9.60 6.90 -15 -1 -10 4.10 32.40 -15 -1 -10 50.39 28.40 -15 -1 -10 -8.10 6.80 -15 1 -10 7.00 41.60 -15 1 -10 7.20 5.70 15 1 10 1.90 2.90 -15 -1 10 8.80 5.10 15 -1 -10 8.20 4.90 -15 1 -10 5.30 23.00 15 1 10 -1.30 4.00 -15 -2 -10 26.30 8.30 15 2 -10 25.40 8.50 -15 -2 -10 38.00 26.80 -15 2 10 11.30 6.40 -15 2 10 27.50 8.50 -15 -2 -10 31.30 12.90 -15 -2 -10 62.29 33.30 15 -2 10 23.30 5.30 15 -2 10 23.80 6.30 15 2 -10 20.60 8.60 -15 -2 -10 34.80 9.80 15 -2 -10 23.30 6.90 15 -2 -10 9.50 7.60 -15 -2 10 17.00 7.60 15 2 10 12.50 7.10 -15 2 -10 22.40 8.90 -15 2 -10 -10.70 39.10 15 2 10 12.90 4.80 -15 2 -10 -11.70 26.40 -15 -2 10 23.60 6.80 15 3 -10 40.00 11.10 -15 -3 -10 17.20 12.20 -15 3 10 43.60 9.40 15 3 -10 37.70 10.60 -15 3 10 30.50 7.70 15 -3 10 39.10 8.20 15 -3 10 44.10 6.90 15 3 10 36.60 7.20 15 -3 -10 36.10 11.90 15 3 10 19.60 9.10 -15 -3 10 35.30 8.70 -15 3 -10 94.69 41.30 -15 -3 10 21.50 8.00 -15 4 10 3.70 4.80 15 4 -10 4.00 5.30 15 -4 10 -6.10 9.50 -15 -4 -10 15.30 9.00 15 -4 10 2.50 2.70 -15 -4 -10 9.30 7.00 15 -4 10 6.10 2.70 -15 -4 10 7.70 4.30 15 -4 -10 0.70 6.30 -15 -4 10 4.00 5.60 -15 4 -10 -5.90 59.09 15 4 10 12.80 6.20 -15 4 -10 5.90 5.30 15 4 10 -0.20 3.40 -15 -5 -10 17.80 7.80 15 5 -10 22.40 8.90 15 -5 10 17.40 5.10 15 -5 10 16.60 3.70 -15 5 10 16.60 6.00 15 -5 10 15.30 9.60 -15 -5 -10 29.20 9.40 -15 -5 10 9.40 4.20 -15 -5 10 4.00 15.80 -15 -5 10 14.60 6.80 -15 5 -10 28.50 8.90 15 5 10 20.40 5.60 15 -5 -10 19.20 8.60 -15 -6 -10 6.60 6.00 15 -6 10 13.70 4.50 15 6 -10 9.80 6.00 -15 6 10 22.10 6.20 15 -6 10 9.90 2.90 -15 -6 -10 14.00 7.20 15 -6 10 9.80 7.80 -15 -6 10 14.60 6.20 15 6 10 -2.50 4.50 -15 -6 10 5.20 3.30 -15 6 -10 9.90 5.10 15 -6 -10 5.10 4.90 -15 -7 -10 144.19 18.80 15 7 -10 161.58 21.60 15 -7 10 154.68 16.60 15 -7 10 145.99 19.00 -15 -7 -10 135.99 18.90 15 7 10 147.39 17.00 -15 -7 10 145.29 18.60 -15 -7 10 134.29 24.90 -15 7 -10 125.79 17.90 15 -7 -10 105.29 17.80 15 8 -10 4.80 3.90 15 -8 10 5.80 5.50 15 -8 10 3.20 2.50 -15 -8 -10 4.20 4.30 15 8 10 6.60 4.30 15 -8 -10 1.00 3.00 -15 -8 10 -1.60 2.30 -15 8 -10 5.70 4.60 15 -9 10 4.00 4.90 -15 -9 -10 4.30 4.10 -15 -9 10 11.40 6.40 -15 -9 10 4.60 3.20 -15 9 -10 -0.60 4.00 15 -9 -10 6.40 4.50 -15 0 11 6.80 5.40 15 0 11 -2.00 4.30 -15 0 11 -5.00 3.10 -15 0 -11 -0.30 5.80 15 0 11 3.10 2.60 -15 0 -11 -62.29 42.20 15 0 -11 -6.00 3.50 15 0 -11 -1.10 5.10 15 1 -11 2.60 5.10 15 -1 11 -2.10 2.10 -15 -1 -11 -0.30 6.40 -15 -1 -11 -0.70 7.50 -15 1 11 -0.90 4.80 15 1 -11 1.50 5.10 15 1 11 -0.40 2.30 -15 1 -11 -3.30 44.70 -15 -1 11 0.90 2.90 -15 -1 11 1.40 5.00 -15 1 -11 2.10 6.50 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2.60 15 -6 11 49.90 7.60 -15 6 11 33.20 8.90 -15 -6 -11 34.80 9.60 15 6 -11 61.69 11.80 15 -6 11 49.30 14.20 -15 -6 -11 36.70 8.50 -15 -6 11 23.50 5.70 -15 -6 11 49.20 9.80 -15 -6 11 47.40 18.00 15 -6 -11 30.60 8.50 15 6 11 43.00 7.60 -15 6 -11 37.00 8.50 15 -7 11 49.40 7.60 15 -7 11 64.39 12.20 -15 -7 -11 41.50 10.60 15 7 -11 62.59 11.50 -15 7 -11 61.39 9.00 15 7 11 39.60 7.70 -15 -7 11 56.49 9.00 15 8 -11 5.10 4.20 15 -8 11 2.60 4.50 -15 8 -11 0.20 3.90 15 -8 -11 -2.30 2.80 -15 -8 11 -1.00 2.70 -15 -8 11 12.60 8.10 15 0 12 48.20 6.90 -15 0 12 35.40 8.50 15 0 -12 28.40 9.30 -15 0 12 36.50 9.00 15 0 12 45.60 9.40 15 1 -12 75.29 14.30 15 1 -12 84.59 12.70 15 -1 12 89.39 13.10 -15 -1 -12 67.79 15.00 15 -1 12 88.09 11.00 -15 1 12 85.19 12.80 -15 -1 12 79.39 13.90 15 1 12 90.29 11.10 15 -1 -12 83.89 17.60 -15 1 -12 68.59 14.70 -15 -1 12 100.99 13.70 15 1 12 102.49 13.30 -15 -2 -12 -9.30 5.50 -15 2 12 -10.50 6.60 -15 2 12 6.60 4.20 15 -2 12 -4.40 2.90 15 -2 12 -1.20 1.70 15 2 -12 -1.80 3.90 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249.58 32.20 -25 -3 2 254.77 28.70 -25 -4 -2 26.20 8.90 -25 4 2 16.50 4.90 25 4 -2 49.10 11.70 25 -4 2 24.70 5.90 25 4 -2 23.50 7.20 25 -4 2 8.80 5.80 -25 -4 2 29.80 8.50 25 4 2 26.50 7.00 -25 -4 2 14.90 7.00 25 4 2 46.20 18.20 25 4 2 22.60 5.20 25 -4 -2 26.10 6.50 -25 4 -2 29.90 11.10 -25 -5 -2 74.79 14.60 -25 -5 -2 82.69 14.40 25 -5 2 77.49 11.60 25 5 -2 83.09 17.60 25 -5 -2 70.19 10.70 -25 5 -2 104.39 18.70 -25 -5 2 80.59 16.70 -25 -5 2 45.70 11.50 25 5 2 59.59 9.00 -25 6 2 0.10 1.70 25 6 -2 -1.60 7.80 25 -6 2 -0.70 2.70 25 6 -2 5.20 3.80 -25 -6 -2 6.50 4.80 -25 -6 -2 -1.20 5.00 25 -6 -2 5.90 3.20 -25 6 -2 0.50 2.00 25 -6 -2 0.10 3.70 -25 -6 2 -0.40 6.40 25 6 2 1.00 3.50 25 6 2 0.80 2.10 -25 -6 2 -5.00 5.00 25 7 -2 4.90 4.10 -25 7 2 11.80 3.00 -25 -7 -2 13.90 6.80 -25 -7 -2 6.00 4.90 25 -7 2 11.30 4.10 25 7 -2 12.90 12.00 -25 -7 2 17.80 7.80 25 7 2 4.70 4.50 25 -7 -2 11.50 3.60 25 -7 -2 10.40 4.50 -25 -7 2 12.30 6.20 25 7 2 7.60 2.90 25 -8 2 -1.30 2.20 -25 8 2 0.30 1.60 -25 -8 -2 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-1 -4.70 4.60 30 0 -1 1.00 4.20 -30 0 1 -2.00 2.40 -30 -1 -1 10.40 6.70 30 1 -1 2.50 3.50 30 -1 1 9.40 6.30 30 1 -1 -8.90 5.50 -30 1 1 3.30 6.50 30 -1 -1 0.10 2.90 30 1 1 -3.70 3.90 -30 1 -1 -4.10 3.10 -30 1 -1 -7.10 4.80 30 -1 -1 0.20 2.80 -30 -1 1 0.20 3.70 -30 -1 1 0.50 4.10 30 1 1 -6.60 3.00 -30 2 1 3.60 2.90 30 -2 1 4.10 3.50 -30 -2 -1 4.70 6.50 -30 2 1 -7.90 9.80 30 2 -1 2.90 4.10 30 2 1 -3.20 2.90 30 -2 -1 -1.10 3.00 -30 -2 1 -6.90 4.90 30 2 1 -8.40 4.80 30 -2 -1 -1.40 2.80 -30 2 -1 1.10 2.40 -30 2 -1 4.30 5.60 30 3 -1 6.30 4.80 -30 -3 -1 -0.80 3.00 30 -3 1 3.00 2.70 30 3 -1 -2.20 3.30 -30 -3 -1 0.80 4.10 -30 3 1 -0.40 1.80 30 -3 -1 2.10 3.20 -30 3 -1 -2.20 5.70 30 -3 -1 -2.10 2.90 -30 -3 1 -4.60 3.00 30 3 1 4.70 11.70 -30 3 -1 0.70 2.70 30 3 1 -0.30 3.00 -30 4 1 3.10 2.80 30 4 -1 8.00 6.60 -30 -4 -1 3.50 3.10 30 4 -1 6.00 3.20 30 -4 1 2.70 3.00 -30 -4 -1 -5.70 4.70 30 -4 -1 1.40 2.60 -30 -4 1 5.90 4.90 30 -4 -1 3.10 4.00 30 4 1 -0.90 2.50 30 0 2 4.50 4.00 30 0 -2 11.90 4.70 -30 0 -2 11.60 6.60 30 0 -2 -2.20 3.40 30 0 2 6.70 5.40 -30 0 2 -2.60 7.00 30 1 -2 8.70 5.30 -30 -1 -2 12.00 5.30 30 -1 2 5.80 4.10 -30 1 2 8.10 3.80 -30 1 2 -0.70 7.70 30 -1 -2 4.10 3.30 30 -1 -2 0.10 3.40 -30 -1 2 7.10 3.10 -30 -1 2 18.00 6.90 30 1 2 12.30 6.00 30 1 2 1.70 3.50 -30 1 -2 0.30 4.30 -30 2 2 -1.40 3.00 30 -2 2 1.30 3.70 -30 -2 -2 5.90 5.30 30 2 2 8.60 6.70 -30 2 -2 0.50 2.80 30 -2 -2 0.10 3.10 -30 2 -2 -6.20 3.60 30 2 2 0.10 3.20 -30 -2 2 5.30 3.20 30 -2 -2 -0.40 2.50 -30 -2 2 3.70 7.20 -30 -3 -2 5.90 4.30 30 -3 2 5.90 3.80 30 3 -2 13.20 5.50 -30 3 2 -1.80 2.40 -30 -3 -2 1.30 2.60 30 -3 -2 2.30 3.10 30 3 2 -1.40 2.70 30 -3 -2 3.40 3.20 -30 3 -2 3.70 2.30 -30 3 -2 -0.40 4.70 -30 4 2 30.50 5.70 30 4 -2 25.60 7.80 -30 -4 -2 38.20 7.20 -30 -4 -2 35.70 7.50 30 -4 2 28.50 6.30 -30 -4 2 20.60 6.40 30 4 2 17.90 5.00 30 0 3 -6.50 4.40 30 0 -3 2.70 4.70 -30 0 3 0.40 2.30 -30 0 -3 -6.20 3.90 30 0 -3 0.70 3.60 -30 0 3 5.20 8.90 30 0 3 1.70 3.00 -30 -1 -3 6.70 3.70 30 -1 3 8.00 4.70 30 -1 3 8.60 3.50 -30 1 3 5.20 3.10 -30 -1 3 20.90 7.00 30 1 3 6.50 3.50 -30 1 -3 8.00 4.00 30 -1 -3 3.90 3.40 30 -1 -3 9.50 4.50 -30 -1 3 6.70 3.80 30 1 3 5.60 6.50 30 2 -3 12.70 3.60 30 -2 3 7.10 4.50 -30 -2 -3 8.80 4.00 -30 2 3 7.60 3.60 30 2 3 11.60 4.00 30 -2 -3 3.00 3.50 -30 2 -3 10.90 5.50 -30 -2 3 26.20 7.40 30 -2 -3 9.00 3.90 30 -3 3 1.50 3.20 -30 -3 -3 3.90 3.10 30 3 -3 12.20 4.40 -30 3 3 1.90 3.10 -30 -3 -3 5.30 4.10 -30 3 -3 -0.30 3.90 30 -3 -3 1.80 3.70 -30 -3 3 2.00 4.60 30 3 3 4.30 3.80 -30 0 4 2.40 2.60 30 0 4 -0.70 2.80 30 0 -4 0.80 3.40 30 0 4 -3.00 8.10 -30 0 -4 -4.10 3.30 30 -1 4 -2.80 2.60 30 1 -4 0.20 2.50 -30 1 4 -1.70 1.90 -30 -1 -4 0.60 2.80 30 -1 -4 -3.80 2.20 30 1 4 -3.50 2.70 -30 1 -4 1.70 3.60 30 -1 -4 -0.50 2.30 -30 -1 4 -2.70 2.20 -30 2 4 0.30 2.20 -30 -2 -4 -0.80 2.90 30 2 -4 3.40 3.50 -30 -2 -4 6.10 4.20 30 -2 4 3.50 3.30 30 -2 -4 0.30 2.30 -30 2 -4 5.00 3.50 -30 -2 4 2.80 2.40 30 -2 -4 -1.50 2.30 30 3 4 2.10 3.30 -30 0 -5 1.70 3.20 30 0 -5 -0.70 2.90 30 0 5 -1.70 2.10 -30 0 5 1.50 1.90 30 1 -5 7.50 3.20 -30 -1 -5 9.60 3.90 30 -1 5 5.60 3.20 -30 -1 -5 6.30 3.40 -30 -1 5 6.90 2.80 -30 1 -5 9.20 3.60 30 -1 -5 15.60 3.80 30 1 5 10.10 3.60 -31 0 0 -6.10 3.70 31 0 0 -3.50 3.10 31 0 0 1.10 3.30 31 -1 0 8.70 6.10 -31 -1 0 14.70 5.50 -31 1 0 12.80 6.00 31 1 0 19.00 5.80 31 -1 0 11.30 4.40 31 2 0 -5.50 3.60 31 -2 0 3.20 2.70 31 -2 0 -3.70 2.90 -31 -2 0 2.80 4.30 -31 -2 0 3.60 3.00 -31 2 0 0.40 2.30 -31 0 1 -4.70 4.40 31 0 1 0.10 3.80 31 0 1 0.30 4.20 -31 0 1 -1.50 2.70 31 0 -1 4.40 3.20 -31 0 -1 -4.10 4.10 31 -1 1 2.60 2.80 -31 1 1 0.30 1.90 31 1 -1 -1.30 3.50 -31 -1 -1 3.40 3.40 31 -1 1 4.40 3.80 31 -1 -1 -1.30 2.60 -31 -1 1 3.40 5.70 31 -1 -1 4.30 5.00 31 1 1 -2.60 4.80 -31 1 -1 4.30 4.60 31 2 -1 3.00 4.00 -31 -2 -1 1.10 3.80 -31 2 1 -2.10 1.90 -31 -2 -1 -1.90 2.80 31 -2 1 -4.00 3.20 -31 2 -1 6.20 7.10 -31 -2 1 4.40 4.30 31 -2 -1 -1.50 2.20 -31 -2 1 -5.20 3.50 31 -2 -1 -2.40 2.60 31 2 1 -1.50 3.00 31 2 1 -2.40 7.10 -31 0 2 10.70 9.40 31 0 2 26.30 5.50 -31 0 -2 32.60 7.10 -31 0 2 18.10 3.80 31 0 -2 20.50 5.90 -31 1 2 3.20 2.40 -31 -1 -2 2.10 3.90 31 -1 2 4.30 4.20 31 1 -2 3.70 3.70 -31 1 -2 7.10 4.10 31 1 2 11.70 7.00 31 1 2 0.90 2.90 -31 -1 2 -2.60 5.40 31 -1 -2 5.20 3.00 31 -1 -2 0.90 3.30 -31 2 2 -0.30 2.10 -31 -2 -2 0.80 2.50 31 2 2 -0.80 2.50 -31 0 3 -1.50 1.90 -31 0 -3 -2.20 3.30 31 0 -3 1.30 3.70 31 1 3 7.30 3.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 93390 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' 'x-1/2, y-1/2, -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 0.51621(7) 0.86936(16) 0.57694(13) 0.0320(4) Uani d . . . 1 . . O O2 0.52499(8) 0.76466(18) 0.44214(14) 0.0367(5) Uani d . . . 1 . . O O3 0.81679(9) 0.79248(18) 0.32222(16) 0.0448(6) Uani d . . . 1 . . O O4 0.79965(8) 0.62734(17) 0.25898(13) 0.0345(5) Uani d . . . 1 . . O O5 0.73013(8) 0.53745(15) 0.58533(14) 0.0341(5) Uani d . . . 1 . . N N1 0.66848(8) 0.60215(17) 0.41986(15) 0.0260(5) Uani d . . . 1 . . N N2 0.78896(9) 0.70482(19) 0.31735(15) 0.0309(5) Uani d . . . 1 . . C C1 0.43772(12) 0.8975(3) 0.6666(2) 0.0397(7) Uani d . . . 1 . . H H1 0.454784 0.872121 0.726095 0.06 Uiso calc U . R 1 . . H H4 0.400072 0.881008 0.669927 0.06 Uiso calc U . R 1 . . H H3 0.442908 0.979281 0.658916 0.06 Uiso calc U . R 1 . . C C2 0.46131(11) 0.8366(3) 0.5821(2) 0.0362(6) Uani d . . . 1 . . H H23 0.458203 0.753666 0.590796 0.043 Uiso calc U . R 1 . . H H24 0.442922 0.858007 0.521885 0.043 Uiso calc U . R 1 . . C C3 0.54358(10) 0.8259(2) 0.50235(18) 0.0289(6) Uani d . . . 1 . . C C4 0.59951(10) 0.8679(2) 0.50489(18) 0.0282(5) Uani d . . . 1 . . H H21 0.611932 0.867113 0.572516 0.034 Uiso calc U . R 1 . . H H22 0.600182 0.947458 0.482352 0.034 Uiso calc U . R 1 . . C C5 0.63739(10) 0.7989(2) 0.44363(17) 0.0267(5) Uani d . . . 1 . . H H5 0.61953 0.776897 0.382214 0.032 Uiso calc U . R 1 . . C C6 0.65765(10) 0.6887(2) 0.49574(17) 0.0265(5) Uani d . . . 1 . . C C7 0.70974(10) 0.7276(2) 0.53986(18) 0.0251(5) Uani d . . . 1 . . H H11 0.702087 0.785814 0.590306 0.03 Uiso calc U . R 1 . . C C8 0.74373(10) 0.6366(2) 0.58405(17) 0.0264(5) Uani d . . . 1 . . C C9 0.79605(10) 0.6714(2) 0.62284(17) 0.0268(5) Uani d . . . 1 . . C C10 0.83391(10) 0.5881(2) 0.63798(17) 0.0280(5) Uani d . . . 1 . . H H14 0.825403 0.510731 0.627696 0.034 Uiso calc U . R 1 . . C C11 0.88402(11) 0.6180(2) 0.66805(18) 0.0313(6) Uani d . . . 1 . . H H15 0.909971 0.561088 0.676776 0.038 Uiso calc U . R 1 . . C C12 0.89629(10) 0.7306(2) 0.68539(19) 0.0318(6) Uani d . . . 1 . . H H2 0.930712 0.750999 0.70518 0.038 Uiso calc U . R 1 . . C C13 0.61809(10) 0.6273(2) 0.55624(18) 0.0265(5) Uani d . . . 1 . . C C14 0.59995(10) 0.6562(2) 0.64744(19) 0.0278(5) Uani d . . . 1 . . H H20 0.614592 0.718318 0.681657 0.033 Uiso calc U . R 1 . . C C15 0.55969(10) 0.5916(2) 0.68730(19) 0.0299(6) Uani d . . . 1 . . H H6 0.546641 0.609841 0.749546 0.036 Uiso calc U . R 1 . . C C16 0.53835(10) 0.5006(2) 0.6371(2) 0.0319(6) Uani d . . . 1 . . H H7 0.509955 0.459282 0.664231 0.038 Uiso calc U . R 1 . . C C17 0.55827(10) 0.4695(2) 0.54747(19) 0.0292(5) Uani d . . . 1 . . H H8 0.544477 0.406035 0.51387 0.035 Uiso calc U . R 1 . . C C18 0.59860(10) 0.5331(2) 0.50841(18) 0.0269(5) Uani d . . . 1 . . C C19 0.62776(11) 0.5144(2) 0.41524(19) 0.0307(6) Uani d . . . 1 . . H H10 0.643342 0.437687 0.41252 0.037 Uiso calc U . R 1 . . H H9 0.604544 0.525424 0.358779 0.037 Uiso calc U . R 1 . . C C20 0.71151(10) 0.6072(2) 0.36648(17) 0.0271(5) Uani d . . . 1 . . H H19 0.718711 0.5497 0.32046 0.033 Uiso calc U . R 1 . . C C21 0.74578(10) 0.6964(2) 0.37809(17) 0.0280(5) Uani d . . . 1 . . C C22 0.73417(10) 0.7882(2) 0.45091(17) 0.0278(5) Uani d . . . 1 . . H H16 0.766267 0.832446 0.468302 0.033 Uiso calc U . R 1 . . C C23 0.80823(10) 0.7850(2) 0.64181(18) 0.0283(5) Uani d . . . 1 . . H H12 0.782466 0.842178 0.632834 0.034 Uiso calc U . R 1 . . C C24 0.85812(11) 0.8135(2) 0.67375(18) 0.0301(6) Uani d . . . 1 . . H H13 0.866232 0.890267 0.68777 0.036 Uiso calc U . R 1 . . C C25 0.68871(10) 0.8652(2) 0.41916(18) 0.0284(5) Uani d . . . 1 . . H H17 0.690778 0.880884 0.349143 0.034 Uiso calc U . R 1 . . H H18 0.689785 0.938051 0.454442 0.034 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0348(9) 0.0273(10) 0.0340(10) 0.0026(7) 0.0003(7) -0.0041(8) O2 0.0394(10) 0.0341(11) 0.0365(10) 0.0015(8) -0.0023(8) -0.0076(8) O3 0.0522(12) 0.0353(12) 0.0468(12) -0.0174(9) 0.0162(10) -0.0120(9) O4 0.0409(10) 0.0321(10) 0.0304(9) -0.0002(8) 0.0047(7) -0.0063(8) O5 0.0435(11) 0.0187(9) 0.0400(10) -0.0020(7) -0.0059(8) 0.0016(7) N1 0.0341(11) 0.0163(10) 0.0277(10) -0.0005(8) 0.0006(8) -0.0027(8) N2 0.0391(12) 0.0270(11) 0.0264(10) -0.0023(9) 0.0027(8) -0.0023(9) C1 0.0416(15) 0.0410(16) 0.0366(14) 0.0048(12) 0.0020(11) 0.0013(12) C2 0.0323(13) 0.0355(15) 0.0408(15) 0.0013(11) -0.0011(10) -0.0029(12) C3 0.0379(13) 0.0204(12) 0.0286(12) 0.0023(10) -0.0015(10) -0.0013(10) C4 0.0362(13) 0.0190(12) 0.0294(12) 0.0007(9) -0.0016(9) -0.0024(10) C5 0.0354(13) 0.0178(12) 0.0270(11) 0.0024(9) -0.0002(9) 0.0004(9) C6 0.0330(12) 0.0202(12) 0.0263(12) 0.0037(9) 0.0004(9) -0.0025(9) C7 0.0324(12) 0.0149(11) 0.0282(11) -0.0006(9) -0.0016(9) -0.0021(9) C8 0.0361(12) 0.0189(11) 0.0243(11) 0.0004(9) 0.0005(9) -0.0001(9) C9 0.0356(12) 0.0203(12) 0.0244(11) -0.0008(9) 0.0009(9) 0.0016(9) C10 0.0395(13) 0.0187(12) 0.0259(11) 0.0015(10) 0.0016(9) 0.0010(9) C11 0.0380(13) 0.0291(14) 0.0268(12) 0.0012(10) -0.0012(10) 0.0040(10) C12 0.0347(13) 0.0309(14) 0.0296(12) -0.0016(10) -0.0007(9) 0.0013(11) C13 0.0337(12) 0.0187(11) 0.0271(11) 0.0003(9) -0.0004(9) 0.0042(9) C14 0.0342(12) 0.0212(12) 0.0279(12) -0.0017(10) -0.0011(9) -0.0013(10) C15 0.0328(12) 0.0274(13) 0.0295(12) 0.0004(10) 0.0011(10) 0.0045(10) C16 0.0325(12) 0.0253(12) 0.0379(13) 0.0006(10) 0.0021(10) 0.0049(11) C17 0.0332(12) 0.0188(11) 0.0356(13) -0.0012(9) -0.0034(10) -0.0004(10) C18 0.0345(12) 0.0172(11) 0.0291(12) 0.0010(9) -0.0022(9) 0.0031(9) C19 0.0386(13) 0.0202(12) 0.0332(13) -0.0062(10) 0.0011(10) -0.0043(10) C20 0.0349(12) 0.0214(12) 0.0251(11) 0.0001(9) -0.0014(9) -0.0029(9) C21 0.0358(12) 0.0222(12) 0.0260(11) -0.0021(10) 0.0019(9) -0.0012(10) C22 0.0389(13) 0.0195(11) 0.0249(11) 0.0001(9) -0.0021(9) 0.0010(9) C23 0.0365(13) 0.0221(12) 0.0263(11) -0.0010(10) 0.0001(9) 0.0008(9) C24 0.0425(14) 0.0210(12) 0.0267(12) -0.0033(10) 0.0004(10) -0.0002(9) C25 0.0386(13) 0.0194(12) 0.0270(11) -0.0008(10) 0.0003(9) 0.0031(9) 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' N N 0.0311 0.0180 '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 C3 O1 C2 . . 115.7(2) ? C20 N1 C19 . . 126.4(2) ? C20 N1 C6 . . 121.1(2) ? C19 N1 C6 . . 112.6(2) ? O4 N2 O3 . . 121.0(2) ? O4 N2 C21 . . 120.8(2) ? O3 N2 C21 . . 118.2(2) ? C2 C1 H1 . . 109.5 ? C2 C1 H4 . . 109.5 ? H1 C1 H4 . . 109.5 ? C2 C1 H3 . . 109.5 ? H1 C1 H3 . . 109.5 ? H4 C1 H3 . . 109.5 ? O1 C2 C1 . . 107.2(2) ? O1 C2 H23 . . 110.3 ? C1 C2 H23 . . 110.3 ? O1 C2 H24 . . 110.3 ? C1 C2 H24 . . 110.3 ? H23 C2 H24 . . 108.5 ? O2 C3 O1 . . 123.9(2) ? O2 C3 C4 . . 125.9(2) ? O1 C3 C4 . . 110.2(2) ? C3 C4 C5 . . 114.2(2) ? C3 C4 H21 . . 108.7 ? C5 C4 H21 . . 108.7 ? C3 C4 H22 . . 108.7 ? C5 C4 H22 . . 108.7 ? H21 C4 H22 . . 107.6 ? C4 C5 C25 . . 112.5(2) ? C4 C5 C6 . . 113.2(2) ? C25 C5 C6 . . 103.87(19) ? C4 C5 H5 . . 109.0 ? C25 C5 H5 . . 109.0 ? C6 C5 H5 . . 109.0 ? N1 C6 C13 . . 100.81(19) ? N1 C6 C7 . . 109.07(19) ? C13 C6 C7 . . 120.3(2) ? N1 C6 C5 . . 107.61(19) ? C13 C6 C5 . . 115.9(2) ? C7 C6 C5 . . 102.69(19) ? C8 C7 C6 . . 116.5(2) ? C8 C7 C22 . . 114.8(2) ? C6 C7 C22 . . 99.65(19) ? C8 C7 H11 . . 108.5 ? C6 C7 H11 . . 108.5 ? C22 C7 H11 . . 108.5 ? O5 C8 C9 . . 120.7(2) ? O5 C8 C7 . . 121.7(2) ? C9 C8 C7 . . 117.5(2) ? C10 C9 C23 . . 119.6(2) ? C10 C9 C8 . . 118.5(2) ? C23 C9 C8 . . 121.9(2) ? C11 C10 C9 . . 120.2(2) ? C11 C10 H14 . . 119.9 ? C9 C10 H14 . . 119.9 ? C12 C11 C10 . . 120.2(2) ? C12 C11 H15 . . 119.9 ? C10 C11 H15 . . 119.9 ? C11 C12 C24 . . 119.8(2) ? C11 C12 H2 . . 120.1 ? C24 C12 H2 . . 120.1 ? C18 C13 C14 . . 120.9(2) ? C18 C13 C6 . . 111.2(2) ? C14 C13 C6 . . 127.9(2) ? C13 C14 C15 . . 118.1(2) ? C13 C14 H20 . . 120.9 ? C15 C14 H20 . . 120.9 ? C16 C15 C14 . . 120.8(2) ? C16 C15 H6 . . 119.6 ? C14 C15 H6 . . 119.6 ? C15 C16 C17 . . 120.5(2) ? C15 C16 H7 . . 119.7 ? C17 C16 H7 . . 119.7 ? C18 C17 C16 . . 118.5(2) ? C18 C17 H8 . . 120.7 ? C16 C17 H8 . . 120.7 ? C17 C18 C13 . . 120.9(2) ? C17 C18 C19 . . 128.5(2) ? C13 C18 C19 . . 110.6(2) ? N1 C19 C18 . . 102.0(2) ? N1 C19 H10 . . 111.4 ? C18 C19 H10 . . 111.4 ? N1 C19 H9 . . 111.4 ? C18 C19 H9 . . 111.4 ? H10 C19 H9 . . 109.2 ? N1 C20 C21 . . 119.6(2) ? N1 C20 H19 . . 120.2 ? C21 C20 H19 . . 120.2 ? C20 C21 N2 . . 119.0(2) ? C20 C21 C22 . . 120.2(2) ? N2 C21 C22 . . 120.6(2) ? C21 C22 C25 . . 112.4(2) ? C21 C22 C7 . . 106.2(2) ? C25 C22 C7 . . 101.41(19) ? C21 C22 H16 . . 112.1 ? C25 C22 H16 . . 112.1 ? C7 C22 H16 . . 112.1 ? C24 C23 C9 . . 119.7(2) ? C24 C23 H12 . . 120.2 ? C9 C23 H12 . . 120.2 ? C23 C24 C12 . . 120.5(2) ? C23 C24 H13 . . 119.8 ? C12 C24 H13 . . 119.8 ? C22 C25 C5 . . 105.77(19) ? C22 C25 H17 . . 110.6 ? C5 C25 H17 . . 110.6 ? C22 C25 H18 . . 110.6 ? C5 C25 H18 . . 110.6 ? H17 C25 H18 . . 108.7 ? 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 C3 . 1.349(3) ? O1 C2 . 1.453(3) ? O2 C3 . 1.202(3) ? O3 N2 . 1.256(3) ? O4 N2 . 1.252(3) ? O5 C8 . 1.222(3) ? N1 C20 . 1.324(3) ? N1 C19 . 1.467(3) ? N1 C6 . 1.493(3) ? N2 C21 . 1.389(3) ? C1 C2 . 1.501(4) ? C1 H1 . 0.98 ? C1 H4 . 0.98 ? C1 H3 . 0.98 ? C2 H23 . 0.99 ? C2 H24 . 0.99 ? C3 C4 . 1.509(4) ? C4 C5 . 1.523(3) ? C4 H21 . 0.99 ? C4 H22 . 0.99 ? C5 C25 . 1.562(3) ? C5 C6 . 1.575(3) ? C5 H5 . 1.0 ? C6 C13 . 1.499(3) ? C6 C7 . 1.532(3) ? C7 C8 . 1.510(3) ? C7 C22 . 1.556(3) ? C7 H11 . 1.0 ? C8 C9 . 1.495(3) ? C9 C10 . 1.394(4) ? C9 C23 . 1.401(3) ? C10 C11 . 1.389(4) ? C10 H14 . 0.95 ? C11 C12 . 1.387(4) ? C11 H15 . 0.95 ? C12 C24 . 1.389(4) ? C12 H2 . 0.95 ? C13 C18 . 1.387(4) ? C13 C14 . 1.389(4) ? C14 C15 . 1.393(4) ? C14 H20 . 0.95 ? C15 C16 . 1.391(4) ? C15 H6 . 0.95 ? C16 C17 . 1.392(4) ? C16 H7 . 0.95 ? C17 C18 . 1.383(4) ? C17 H8 . 0.95 ? C18 C19 . 1.507(4) ? C19 H10 . 0.99 ? C19 H9 . 0.99 ? C20 C21 . 1.378(3) ? C20 H19 . 0.95 ? C21 C22 . 1.511(3) ? C22 C25 . 1.537(3) ? C22 H16 . 1.0 ? C23 C24 . 1.387(4) ? C23 H12 . 0.95 ? C24 H13 . 0.95 ? C25 H17 . 0.99 ? C25 H18 . 0.99 ? 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 C7 H11 O4 4_665 1.00 2.55 3.497(3) 156.9 ? C19 H10 O3 6_755 0.99 2.35 3.245(3) 149.3 ? 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 C3 O1 C2 C1 . . . . -177.5(2) ? C2 O1 C3 O2 . . . . 0.7(4) ? C2 O1 C3 C4 . . . . 179.2(2) ? O2 C3 C4 C5 . . . . -18.7(4) ? O1 C3 C4 C5 . . . . 162.8(2) ? C3 C4 C5 C25 . . . . 160.3(2) ? C3 C4 C5 C6 . . . . -82.3(3) ? C20 N1 C6 C13 . . . . -160.9(2) ? C19 N1 C6 C13 . . . . 17.6(3) ? C20 N1 C6 C7 . . . . -33.4(3) ? C19 N1 C6 C7 . . . . 145.1(2) ? C20 N1 C6 C5 . . . . 77.3(3) ? C19 N1 C6 C5 . . . . -104.1(2) ? C4 C5 C6 N1 . . . . 149.9(2) ? C25 C5 C6 N1 . . . . -87.7(2) ? C4 C5 C6 C13 . . . . 38.0(3) ? C25 C5 C6 C13 . . . . 160.4(2) ? C4 C5 C6 C7 . . . . -95.1(2) ? C25 C5 C6 C7 . . . . 27.3(2) ? N1 C6 C7 C8 . . . . -57.6(3) ? C13 C6 C7 C8 . . . . 57.9(3) ? C5 C6 C7 C8 . . . . -171.6(2) ? N1 C6 C7 C22 . . . . 66.4(2) ? C13 C6 C7 C22 . . . . -178.0(2) ? C5 C6 C7 C22 . . . . -47.5(2) ? C6 C7 C8 O5 . . . . -0.7(3) ? C22 C7 C8 O5 . . . . -116.6(3) ? C6 C7 C8 C9 . . . . 176.8(2) ? C22 C7 C8 C9 . . . . 60.9(3) ? O5 C8 C9 C10 . . . . 15.8(4) ? C7 C8 C9 C10 . . . . -161.7(2) ? O5 C8 C9 C23 . . . . -165.8(2) ? C7 C8 C9 C23 . . . . 16.7(3) ? C23 C9 C10 C11 . . . . -2.5(4) ? C8 C9 C10 C11 . . . . 175.9(2) ? C9 C10 C11 C12 . . . . 1.5(4) ? C10 C11 C12 C24 . . . . 0.8(4) ? N1 C6 C13 C18 . . . . -14.3(3) ? C7 C6 C13 C18 . . . . -134.0(2) ? C5 C6 C13 C18 . . . . 101.5(2) ? N1 C6 C13 C14 . . . . 167.4(2) ? C7 C6 C13 C14 . . . . 47.7(4) ? C5 C6 C13 C14 . . . . -76.8(3) ? C18 C13 C14 C15 . . . . -3.4(4) ? C6 C13 C14 C15 . . . . 174.8(2) ? C13 C14 C15 C16 . . . . 0.1(4) ? C14 C15 C16 C17 . . . . 2.6(4) ? C15 C16 C17 C18 . . . . -1.9(4) ? C16 C17 C18 C13 . . . . -1.4(4) ? C16 C17 C18 C19 . . . . 177.6(2) ? C14 C13 C18 C17 . . . . 4.1(4) ? C6 C13 C18 C17 . . . . -174.4(2) ? C14 C13 C18 C19 . . . . -175.1(2) ? C6 C13 C18 C19 . . . . 6.5(3) ? C20 N1 C19 C18 . . . . 164.2(2) ? C6 N1 C19 C18 . . . . -14.2(3) ? C17 C18 C19 N1 . . . . -174.5(2) ? C13 C18 C19 N1 . . . . 4.6(3) ? C19 N1 C20 C21 . . . . 178.9(2) ? C6 N1 C20 C21 . . . . -2.9(4) ? N1 C20 C21 N2 . . . . -175.8(2) ? N1 C20 C21 C22 . . . . -0.3(4) ? O4 N2 C21 C20 . . . . -6.8(4) ? O3 N2 C21 C20 . . . . 172.8(2) ? O4 N2 C21 C22 . . . . 177.8(2) ? O3 N2 C21 C22 . . . . -2.6(4) ? C20 C21 C22 C25 . . . . -71.8(3) ? N2 C21 C22 C25 . . . . 103.6(3) ? C20 C21 C22 C7 . . . . 38.2(3) ? N2 C21 C22 C7 . . . . -146.4(2) ? C8 C7 C22 C21 . . . . 57.5(3) ? C6 C7 C22 C21 . . . . -67.7(2) ? C8 C7 C22 C25 . . . . 175.1(2) ? C6 C7 C22 C25 . . . . 49.9(2) ? C10 C9 C23 C24 . . . . 1.2(4) ? C8 C9 C23 C24 . . . . -177.2(2) ? C9 C23 C24 C12 . . . . 1.2(4) ? C11 C12 C24 C23 . . . . -2.1(4) ? C21 C22 C25 C5 . . . . 80.0(2) ? C7 C22 C25 C5 . . . . -32.9(2) ? C4 C5 C25 C22 . . . . 126.6(2) ? C6 C5 C25 C22 . . . . 3.8(2) ?