#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:57:36 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294492 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572174.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_1572174 loop_ _publ_author_name 'Bhattacharya, Debkanta' 'Scherübl, Maximilian' 'Daniliuc, Constantin G.' 'Studer, Armido' _publ_section_title ; Intermolecular radical oxyalkylation of arynes with alkenes and TEMPO. ; _journal_issue 34 _journal_name_full 'Chemical science' _journal_page_first 13712 _journal_page_last 13716 _journal_paper_doi 10.1039/d4sc04369c _journal_volume 15 _journal_year 2024 _chemical_formula_sum 'C26 H42 Cl2 N2 O2' _chemical_formula_weight 485.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method 'APEX4 v2021.4-0' _audit_update_record ; 2024-06-25 deposited with the CCDC. 2024-07-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.006(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.3322(6) _cell_length_b 7.6032(3) _cell_length_c 22.4351(8) _cell_measurement_reflns_used 9162 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 66.5229 _cell_measurement_theta_min 2.8826 _cell_volume 2614.94(17) _computing_cell_refinement 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_data_collection 'Bruker APEX4 v2021.4-0 Photon III' _computing_data_reduction 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 1242)' _computing_publication_material 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device 'Bruker D8 Venture Photon III' _diffrn_measurement_device_type 'single crystal diffractometer' _diffrn_measurement_method 'phi/omega scans' _diffrn_radiation_monochromator 'MX mirror' _diffrn_radiation_probe 'single crystal' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_unetI/netI 0.0212 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 52082 _diffrn_reflns_theta_full 66.61 _diffrn_reflns_theta_max 66.61 _diffrn_reflns_theta_min 2.88 _diffrn_source 'Cu ImS' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'micro focus tube' _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 2.417 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015). "Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination" J. Appl. Cryst. 48, 3-10. doi:10.1107/S1600576714022985 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1048 _exptl_crystal_size_max 0.246 _exptl_crystal_size_mid 0.093 _exptl_crystal_size_min 0.063 _refine_diff_density_max 0.274 _refine_diff_density_min -0.310 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 297 _refine_ls_number_reflns 4587 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0307 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+1.4739P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.0777 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4213 _reflns_number_total 4587 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04369c2.cif _cod_data_source_block stu10240_4i _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas Adding full bibliography for 1572173--1572174.cif. ; _cod_database_code 1572174 _shelx_res_file ; TITL stu10240.res in P2(1)/c stu10240.res created by SHELXL-2018/3 at 07:54:55 on 26-Nov-2021 CELL 1.54178 15.3322 7.6032 22.4351 90.000 91.006 90.000 ZERR 4.000 0.0006 0.0003 0.0008 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H Cl N O UNIT 104 168 8 8 8 LIST 4 SIZE 0.063 0.093 0.246 TEMP -173.150 ACTA CONF OMIT 1 1 0 L.S. 20 BOND $H FMAP 2 PLAN 10 HTAB WGHT 0.034700 1.473900 FVAR 0.68293 CL1 3 0.295577 1.074611 0.386591 11.00000 0.02202 0.03631 = 0.04190 0.02242 -0.00201 -0.00297 CL2 3 0.418037 0.908637 0.468450 11.00000 0.01442 0.02632 = 0.02080 0.00298 -0.00113 -0.00488 N1 4 0.186549 0.567519 0.367542 11.00000 0.01545 0.02456 = 0.01417 -0.00548 0.00046 0.00092 N2 4 0.339199 0.589075 0.614800 11.00000 0.01475 0.01556 = 0.01067 0.00336 -0.00213 -0.00104 O1 5 0.194842 0.742907 0.393681 11.00000 0.01446 0.02216 = 0.01445 -0.00111 -0.00274 0.00096 O2 5 0.317854 0.656658 0.555000 11.00000 0.01544 0.01688 = 0.01110 0.00169 0.00060 0.00318 C1 1 0.261153 0.754501 0.439739 11.00000 0.01288 0.02205 = 0.01345 0.00112 -0.00127 0.00023 AFIX 13 H1 2 0.284500 0.634085 0.448199 11.00000 -1.20000 AFIX 0 C2 1 0.334646 0.869173 0.414644 11.00000 0.01541 0.02917 = 0.01809 0.00332 -0.00132 -0.00084 AFIX 13 H2 2 0.361077 0.803768 0.380767 11.00000 -1.20000 AFIX 0 C3 1 0.220899 0.827597 0.496038 11.00000 0.01304 0.01537 = 0.01631 -0.00045 0.00097 -0.00298 C4 1 0.249459 0.774465 0.553348 11.00000 0.01223 0.01135 = 0.01720 0.00008 0.00025 -0.00175 C5 1 0.207647 0.835747 0.603849 11.00000 0.01719 0.01624 = 0.01453 -0.00084 0.00024 -0.00278 AFIX 43 H5 2 0.227722 0.801084 0.642390 11.00000 -1.20000 AFIX 0 C6 1 0.136598 0.947551 0.597733 11.00000 0.01638 0.01730 = 0.01895 -0.00482 0.00376 -0.00172 AFIX 43 H6 2 0.107330 0.987039 0.632224 11.00000 -1.20000 AFIX 0 C7 1 0.107800 1.002358 0.541786 11.00000 0.01544 0.01640 = 0.02560 -0.00229 -0.00016 0.00206 AFIX 43 H7 2 0.059344 1.079612 0.537841 11.00000 -1.20000 AFIX 0 C8 1 0.150614 0.942996 0.491662 11.00000 0.01587 0.01771 = 0.01831 0.00100 -0.00259 -0.00099 AFIX 43 H8 2 0.131476 0.982097 0.453400 11.00000 -1.20000 AFIX 0 C9 1 0.195359 0.591826 0.301518 11.00000 0.02000 0.04241 = 0.01259 -0.00369 0.00146 0.00491 C10 1 0.178577 0.411503 0.272924 11.00000 0.02742 0.04800 = 0.01918 -0.01275 -0.00424 0.01289 AFIX 23 H10A 2 0.181047 0.423708 0.229053 11.00000 -1.20000 H10B 2 0.225716 0.330005 0.285611 11.00000 -1.20000 AFIX 0 C11 1 0.091611 0.331870 0.288959 11.00000 0.03114 0.03742 = 0.03255 -0.01647 -0.01056 0.00573 AFIX 23 H11A 2 0.085522 0.213983 0.270616 11.00000 -1.20000 H11B 2 0.043511 0.407059 0.273627 11.00000 -1.20000 AFIX 0 C12 1 0.086860 0.316961 0.356432 11.00000 0.02581 0.03006 = 0.03389 -0.00776 -0.00650 -0.00210 AFIX 23 H12A 2 0.130938 0.230601 0.370509 11.00000 -1.20000 H12B 2 0.028673 0.271192 0.366952 11.00000 -1.20000 AFIX 0 C13 1 0.102343 0.491817 0.389200 11.00000 0.01532 0.02701 = 0.02154 -0.00370 -0.00038 -0.00222 C14 1 0.136340 0.734176 0.273556 11.00000 0.03313 0.04500 = 0.01693 0.00263 -0.00086 0.00461 AFIX 137 H14A 2 0.076296 0.690396 0.270669 11.00000 -1.50000 H14B 2 0.156964 0.762996 0.233628 11.00000 -1.50000 H14C 2 0.138140 0.839870 0.298548 11.00000 -1.50000 AFIX 0 C15 1 0.290181 0.642305 0.289842 11.00000 0.02516 0.07078 = 0.01771 -0.00625 0.00785 -0.00193 AFIX 137 H15A 2 0.299176 0.766604 0.299740 11.00000 -1.50000 H15B 2 0.302900 0.623024 0.247688 11.00000 -1.50000 H15C 2 0.329177 0.569608 0.314623 11.00000 -1.50000 AFIX 0 C16 1 0.022309 0.612706 0.382371 11.00000 0.01370 0.03883 = 0.02916 -0.00725 0.00143 0.00127 AFIX 137 H16A 2 0.038408 0.732791 0.394003 11.00000 -1.50000 H16B 2 -0.024302 0.570257 0.408018 11.00000 -1.50000 H16C 2 0.001846 0.612064 0.340743 11.00000 -1.50000 AFIX 0 C17 1 0.116006 0.450753 0.455363 11.00000 0.02729 0.02964 = 0.02248 0.00045 0.00202 -0.00905 AFIX 137 H17A 2 0.170143 0.383817 0.461020 11.00000 -1.50000 H17B 2 0.066749 0.381181 0.469584 11.00000 -1.50000 H17C 2 0.119889 0.560919 0.477929 11.00000 -1.50000 AFIX 0 C18 1 0.311555 0.400283 0.614845 11.00000 0.01768 0.01326 = 0.01976 0.00116 0.00104 -0.00156 C19 1 0.343277 0.321934 0.674601 11.00000 0.02565 0.01826 = 0.02378 0.00616 0.00176 0.00013 AFIX 23 H19A 2 0.309609 0.375530 0.707183 11.00000 -1.20000 H19B 2 0.331118 0.194055 0.674572 11.00000 -1.20000 AFIX 0 C20 1 0.439993 0.350436 0.687237 11.00000 0.02688 0.02638 = 0.02296 0.00713 -0.00371 0.00434 AFIX 23 H20A 2 0.474893 0.289929 0.656703 11.00000 -1.20000 H20B 2 0.456192 0.301420 0.726786 11.00000 -1.20000 AFIX 0 C21 1 0.458346 0.546917 0.686048 11.00000 0.01781 0.02676 = 0.01724 -0.00060 -0.00298 0.00176 AFIX 23 H21A 2 0.521291 0.566468 0.694113 11.00000 -1.20000 H21B 2 0.425630 0.604375 0.718341 11.00000 -1.20000 AFIX 0 C22 1 0.433122 0.633840 0.626435 11.00000 0.01300 0.01776 = 0.01617 -0.00070 -0.00024 -0.00070 C23 1 0.342611 0.288991 0.562119 11.00000 0.02208 0.01613 = 0.02650 -0.00381 0.00112 -0.00002 AFIX 137 H23A 2 0.332567 0.353803 0.524870 11.00000 -1.50000 H23B 2 0.310046 0.178113 0.560743 11.00000 -1.50000 H23C 2 0.405025 0.264088 0.567123 11.00000 -1.50000 AFIX 0 C24 1 0.211668 0.400403 0.614468 11.00000 0.01877 0.01724 = 0.02518 0.00026 0.00188 -0.00396 AFIX 137 H24A 2 0.190963 0.473203 0.647374 11.00000 -1.50000 H24B 2 0.190411 0.279759 0.619256 11.00000 -1.50000 H24C 2 0.189708 0.448323 0.576532 11.00000 -1.50000 AFIX 0 C25 1 0.496921 0.579839 0.577577 11.00000 0.01562 0.02166 = 0.02080 -0.00209 0.00232 0.00066 AFIX 137 H25A 2 0.503768 0.451687 0.577675 11.00000 -1.50000 H25B 2 0.553685 0.635388 0.585278 11.00000 -1.50000 H25C 2 0.473970 0.618026 0.538641 11.00000 -1.50000 AFIX 0 C26 1 0.437285 0.834030 0.634293 11.00000 0.01708 0.01972 = 0.01971 -0.00391 0.00249 -0.00325 AFIX 137 H26A 2 0.421042 0.891424 0.596594 11.00000 -1.50000 H26B 2 0.496734 0.868553 0.646011 11.00000 -1.50000 H26C 2 0.396741 0.870051 0.665295 11.00000 -1.50000 AFIX 0 HKLF 4 REM stu10240.res in P2(1)/c REM wR2 = 0.077669, GooF = S = 1.02755, Restrained GooF = 1.02755 for all data REM R1 = 0.030738 for 4213 Fo > 4sig(Fo) and 0.033871 for all 4587 data REM 297 parameters refined using 0 restraints END WGHT 0.0347 1.4739 REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB C12 Cl1_$1 HTAB C25 Cl2 HTAB C26 Cl2 REM Highest difference peak 0.274, deepest hole -0.310, 1-sigma level 0.039 Q1 1 0.4426 0.5880 0.6560 11.00000 0.05 0.27 Q2 1 0.2370 0.7965 0.5221 11.00000 0.05 0.24 Q3 1 0.2638 0.3998 0.6138 11.00000 0.05 0.23 Q4 1 0.3300 0.3591 0.6438 11.00000 0.05 0.23 Q5 1 0.0917 0.4094 0.3727 11.00000 0.05 0.22 Q6 1 0.4626 0.6061 0.6033 11.00000 0.05 0.22 Q7 1 0.0666 0.5513 0.3818 11.00000 0.05 0.22 Q8 1 0.1916 0.5817 0.3336 11.00000 0.05 0.22 Q9 1 0.4347 0.7323 0.6267 11.00000 0.05 0.21 Q10 1 0.2995 0.8161 0.4284 11.00000 0.05 0.21 ; _shelx_res_checksum 24192 _shelx_hkl_file ; -1 0 0 1104.69 43.40 3 0 0 1800.02 70.29 3 0 0 1734.83 70.79 -3 0 0 1780.72 70.39 4 0 0 1128.19 48.30 4 0 0 1261.87 49.30 5 0 0 1409.06 60.19 5 0 0 1392.26 60.99 -5 0 0 1619.74 61.39 -5 0 0 1519.15 60.59 6 0 0 518.35 24.70 6 0 0 579.84 26.10 -6 0 0 585.14 25.50 -6 0 0 554.54 25.20 7 0 0 1391.56 57.19 -7 0 0 1385.36 56.19 -7 0 0 1242.08 55.19 -8 0 0 6521.35 263.87 -8 0 0 6954.80 265.77 -8 0 0 6307.87 264.27 8 0 0 6622.84 266.47 8 0 0 7143.79 264.77 -9 0 0 3438.96 144.89 -9 0 0 3660.43 146.49 -9 0 0 3809.12 146.59 -9 0 0 3521.65 144.29 9 0 0 3646.24 145.19 10 0 0 2296.17 91.69 -10 0 0 2233.48 92.99 -10 0 0 2092.09 91.09 -10 0 0 2235.68 92.89 -10 0 0 2266.07 94.99 10 0 0 2178.88 89.89 -10 0 0 2181.38 90.59 -11 0 0 181.78 13.90 -11 0 0 190.38 12.40 11 0 0 213.18 13.50 11 0 0 186.58 12.30 -11 0 0 223.18 16.90 11 0 0 197.48 12.30 -11 0 0 169.48 12.80 12 0 0 96.09 9.20 -12 0 0 94.79 12.10 -12 0 0 104.19 13.50 12 0 0 98.29 11.30 -12 0 0 104.69 10.40 -12 0 0 97.59 10.90 -12 0 0 99.29 9.90 12 0 0 93.99 9.50 -13 0 0 1415.16 64.19 13 0 0 1572.14 63.19 -13 0 0 1387.46 67.19 13 0 0 1455.65 59.89 -13 0 0 1365.06 64.79 -13 0 0 1385.26 61.89 13 0 0 1277.57 59.59 14 0 0 306.07 19.40 -14 0 0 283.57 22.50 -14 0 0 259.07 17.80 -14 0 0 306.37 18.40 -14 0 0 270.17 21.40 14 0 0 275.57 16.40 -14 0 0 218.98 21.00 15 0 0 68.99 9.90 -15 0 0 62.49 15.60 15 0 0 79.49 7.50 -15 0 0 77.49 9.80 -15 0 0 89.39 13.90 -15 0 0 80.49 12.00 -15 0 0 77.49 13.70 -16 0 0 0.90 8.70 -16 0 0 0.50 4.60 -17 0 0 6.30 4.80 -17 0 0 -0.70 9.60 17 0 0 4.50 4.10 18 0 0 287.77 15.30 0 -1 0 0.00 1.10 0 1 0 1.20 0.90 0 1 0 0.30 0.30 0 1 0 0.70 0.30 0 1 0 0.00 0.60 -1 -1 0 60.59 3.70 2 -1 0 77.99 6.50 -2 -1 0 77.99 4.70 -2 -1 0 79.49 4.80 -2 1 0 76.49 3.90 -2 1 0 73.89 3.10 -2 1 0 72.39 3.10 2 1 0 75.39 4.90 -3 -1 0 1032.00 41.80 3 -1 0 1024.90 43.30 3 1 0 1043.90 42.50 3 1 0 1021.30 41.80 -3 1 0 999.10 40.70 -3 1 0 1004.20 40.60 -4 1 0 6038.20 236.78 -5 -1 0 703.23 31.30 -5 1 0 709.93 30.40 5 1 0 690.33 31.20 -5 1 0 741.23 30.50 5 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260.87 13.80 -3 -5 0 272.07 15.50 3 -5 0 290.97 22.10 3 -5 0 252.77 17.40 -3 -5 0 290.57 21.10 3 -5 0 261.77 15.30 3 -5 0 263.77 16.70 -3 -5 0 265.07 17.20 3 -5 0 220.98 16.90 -3 -5 0 286.57 15.90 3 5 0 298.57 16.50 3 5 0 264.67 14.40 3 5 0 263.17 16.20 -3 5 0 284.07 12.80 4 -5 0 1034.70 52.39 -4 -5 0 1005.50 42.90 -4 -5 0 1001.10 44.60 4 -5 0 1011.90 45.30 -4 -5 0 1005.90 45.60 4 -5 0 1001.40 44.70 4 -5 0 993.80 44.40 4 -5 0 976.40 45.80 -4 -5 0 1051.29 45.00 -4 -5 0 1087.19 52.79 -4 -5 0 1043.00 45.20 4 -5 0 948.91 45.90 4 5 0 998.60 45.70 -4 5 0 995.10 41.30 4 5 0 944.61 43.40 4 5 0 1003.70 44.30 4 5 0 1063.99 46.20 -4 5 0 987.60 41.90 4 5 0 948.41 43.30 -5 -5 0 5.10 6.90 5 -5 0 6.60 3.30 5 -5 0 10.00 7.10 5 -5 0 12.80 6.50 -5 -5 0 15.80 5.50 5 -5 0 20.50 6.50 5 -5 0 11.80 5.90 -5 -5 0 16.10 7.60 5 -5 0 13.10 8.30 5 -5 0 3.00 6.70 -5 -5 0 14.90 4.30 -5 -5 0 16.70 4.70 5 -5 0 9.70 5.40 -5 -5 0 8.50 6.20 5 5 0 12.60 4.50 5 5 0 10.50 5.10 5 5 0 16.00 4.80 5 5 0 8.40 4.90 5 5 0 5.30 4.00 6 -5 0 68.19 8.50 -6 -5 0 70.99 9.20 6 -5 0 68.79 13.10 -6 -5 0 65.69 9.10 6 -5 0 73.39 8.70 -6 -5 0 70.79 12.50 6 -5 0 82.69 11.10 6 -5 0 45.60 9.30 6 -5 0 58.59 8.20 6 -5 0 63.49 6.90 6 -5 0 59.39 9.40 -6 -5 0 68.89 6.80 -6 -5 0 56.19 8.10 -6 -5 0 58.89 12.10 6 5 0 64.79 9.20 -6 5 0 53.99 6.70 -6 5 0 71.59 5.40 6 5 0 69.99 8.00 6 5 0 77.39 8.10 6 5 0 75.99 8.70 6 5 0 70.99 9.90 -7 -5 0 130.59 17.00 7 -5 0 117.89 11.40 -7 -5 0 141.99 17.90 7 -5 0 126.19 13.50 -7 -5 0 161.88 12.10 7 -5 0 128.49 9.20 -7 -5 0 120.09 9.40 7 -5 0 149.79 12.40 7 -5 0 119.79 11.50 7 -5 0 107.79 13.70 7 -5 0 100.09 14.90 -7 5 0 127.89 10.40 7 5 0 125.59 12.30 7 5 0 125.89 10.80 7 5 0 132.39 12.50 -7 5 0 134.49 8.30 7 5 0 118.79 11.00 7 5 0 136.19 10.80 -8 -5 0 -2.40 5.50 -8 -5 0 0.80 6.60 -8 -5 0 -1.40 3.70 8 -5 0 2.00 7.80 -8 -5 0 -0.70 3.20 8 -5 0 -7.30 4.70 8 -5 0 -5.00 5.10 -8 -5 0 7.40 5.60 8 -5 0 12.60 6.80 8 -5 0 2.70 4.20 8 -5 0 0.90 6.60 8 5 0 -5.50 6.20 8 5 0 1.00 5.40 -8 5 0 4.40 3.20 -8 5 0 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494.45 25.70 -11 5 0 430.36 24.00 12 -5 0 12.80 7.50 -12 -5 0 16.30 4.40 12 -5 0 19.00 5.80 -12 -5 0 15.40 5.70 12 -5 0 8.90 5.10 12 -5 0 15.10 4.60 -12 5 0 22.60 6.10 -12 5 0 19.90 6.90 12 5 0 16.30 5.20 -13 -5 0 154.08 12.10 13 -5 0 154.78 12.30 -13 -5 0 147.49 11.30 13 -5 0 151.58 12.50 13 -5 0 146.19 10.90 13 -5 0 162.98 12.90 -13 5 0 142.39 12.40 13 5 0 155.98 12.60 14 -5 0 199.68 15.40 -14 -5 0 200.48 14.20 -14 -5 0 248.78 13.60 14 -5 0 254.77 13.40 14 -5 0 258.57 14.80 -14 5 0 240.88 14.40 14 5 0 216.58 13.80 15 -5 0 0.10 3.40 15 -5 0 -4.10 3.20 15 -5 0 0.50 3.50 15 5 0 3.90 4.40 -15 5 0 6.90 5.90 0 -6 0 1398.66 62.69 0 -6 0 1536.65 71.29 0 -6 0 1401.36 60.69 0 -6 0 1489.15 60.99 0 -6 0 1283.07 61.59 0 6 0 1323.27 58.79 0 6 0 1459.35 59.79 0 6 0 1324.27 59.49 -1 -6 0 199.58 16.20 -1 -6 0 175.98 17.70 1 -6 0 217.38 20.10 1 -6 0 205.38 14.80 1 -6 0 191.38 13.30 -1 -6 0 192.48 14.20 -1 -6 0 173.38 14.00 1 -6 0 159.08 16.90 -1 -6 0 195.38 18.90 1 -6 0 185.68 14.50 1 -6 0 150.98 15.80 -1 6 0 181.98 11.30 1 6 0 178.78 13.20 1 6 0 177.18 12.10 -1 6 0 166.38 12.10 1 6 0 200.28 12.90 2 -6 0 345.67 20.60 -2 -6 0 370.66 21.00 -2 -6 0 395.86 28.00 2 -6 0 347.57 21.70 2 -6 0 382.46 21.20 2 -6 0 332.97 20.50 -2 -6 0 373.06 22.10 2 -6 0 384.56 27.60 -2 -6 0 347.87 20.70 2 -6 0 348.17 22.20 2 6 0 347.37 20.30 -2 6 0 323.97 18.40 -2 6 0 364.66 17.90 2 6 0 325.57 18.80 2 6 0 393.26 19.70 2 6 0 343.47 20.40 -3 -6 0 41.40 7.20 3 -6 0 19.30 7.30 3 -6 0 45.20 8.80 3 -6 0 27.90 7.50 3 -6 0 29.20 10.30 -3 -6 0 31.00 8.50 -3 -6 0 45.90 8.10 -3 -6 0 33.30 9.70 3 -6 0 20.80 6.30 3 -6 0 28.60 7.40 3 -6 0 35.40 6.20 -3 -6 0 42.60 7.00 3 6 0 34.90 7.50 -3 6 0 33.40 4.50 3 6 0 31.40 5.80 -3 6 0 27.20 5.80 3 6 0 39.20 7.00 3 6 0 31.30 5.40 -4 -6 0 191.58 13.20 4 -6 0 168.88 13.90 -4 -6 0 166.18 13.40 4 -6 0 184.78 15.50 4 -6 0 163.78 12.70 4 -6 0 166.88 15.30 -4 -6 0 184.88 15.70 -4 -6 0 163.28 10.70 4 -6 0 181.18 13.80 -4 -6 0 152.78 14.40 4 -6 0 183.18 13.20 4 -6 0 146.19 11.50 -4 -6 0 191.68 21.90 4 -6 0 156.58 20.10 4 6 0 177.68 14.40 -4 6 0 168.98 9.20 4 6 0 165.48 13.60 4 6 0 154.48 12.00 -4 6 0 155.28 11.00 -5 -6 0 281.97 14.60 5 -6 0 273.77 16.70 5 -6 0 281.77 24.90 5 -6 0 241.48 18.00 5 -6 0 283.87 18.10 5 -6 0 258.57 17.70 -5 -6 0 287.17 18.60 -5 -6 0 264.97 17.40 5 -6 0 257.17 14.30 -5 -6 0 244.28 19.20 5 -6 0 301.77 18.80 5 -6 0 294.97 17.50 -5 -6 0 270.77 18.50 5 6 0 285.27 17.20 5 6 0 249.28 18.00 -5 6 0 256.57 11.80 5 6 0 269.47 16.10 5 6 0 207.88 19.30 6 -6 0 161.28 15.50 -6 -6 0 182.08 14.50 -6 -6 0 149.99 13.40 -6 -6 0 180.08 11.20 6 -6 0 155.88 15.00 -6 -6 0 176.38 22.10 6 -6 0 170.18 12.40 6 -6 0 185.68 15.40 6 -6 0 156.18 11.40 -6 -6 0 168.08 14.20 6 -6 0 188.58 20.70 6 -6 0 182.58 13.90 -6 -6 0 161.28 13.70 6 -6 0 126.89 14.60 -6 -6 0 172.58 17.80 6 6 0 160.58 14.30 6 6 0 148.59 12.40 6 6 0 182.78 13.50 6 6 0 148.49 10.80 6 6 0 154.38 14.10 7 -6 0 558.44 27.70 -7 -6 0 520.95 28.30 -7 -6 0 598.64 30.70 -7 -6 0 593.44 26.70 7 -6 0 497.95 27.60 7 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15.10 11 -6 0 155.48 12.70 -11 -6 0 159.08 16.50 11 -6 0 159.08 13.30 -11 -6 0 154.48 12.60 11 -6 0 150.08 15.20 -11 -6 0 158.88 11.00 11 6 0 178.68 14.50 -11 6 0 150.68 12.20 -12 -6 0 10.10 6.50 -12 -6 0 13.10 7.60 12 -6 0 14.80 5.80 12 -6 0 5.40 6.00 12 -6 0 14.30 8.00 12 6 0 10.80 7.10 -13 -6 0 235.88 12.30 13 -6 0 217.78 11.80 13 -6 0 233.58 14.10 0 -7 0 -6.00 7.30 0 -7 0 1.20 7.10 0 -7 0 -0.60 5.50 0 -7 0 6.20 6.40 0 -7 0 4.20 3.70 0 -7 0 -3.20 5.40 0 7 0 0.20 5.90 0 7 0 -1.60 4.20 0 7 0 -11.70 6.80 0 7 0 5.70 4.80 -1 -7 0 31.50 8.90 -1 -7 0 55.19 12.80 1 -7 0 32.80 8.30 1 -7 0 47.90 8.00 -1 -7 0 38.80 7.20 1 -7 0 48.20 9.10 -1 -7 0 46.90 8.60 1 -7 0 46.00 8.20 1 -7 0 66.49 14.00 1 -7 0 64.59 8.70 -1 -7 0 44.70 7.80 -1 -7 0 61.89 9.70 -1 7 0 45.70 7.90 -1 7 0 48.30 7.90 1 7 0 33.70 7.10 1 7 0 42.10 7.30 -1 7 0 57.19 7.70 1 7 0 46.50 7.80 1 7 0 27.50 7.20 -2 -7 0 62.39 10.60 2 -7 0 55.19 9.00 -2 -7 0 60.79 11.00 2 -7 0 67.29 8.80 -2 -7 0 62.29 8.70 -2 -7 0 82.89 10.10 2 -7 0 60.69 9.20 -2 -7 0 71.19 8.60 2 -7 0 73.99 11.20 -2 -7 0 51.99 13.10 2 -7 0 30.20 13.60 2 7 0 53.29 8.00 2 7 0 59.19 9.20 -2 7 0 75.29 9.30 -2 7 0 54.79 7.20 2 7 0 48.90 7.90 2 7 0 76.99 9.70 3 -7 0 441.76 33.10 3 -7 0 360.56 31.60 -3 -7 0 466.45 35.90 -3 -7 0 411.16 24.70 3 -7 0 439.76 23.70 3 -7 0 512.85 35.40 -3 7 0 397.86 21.20 3 7 0 435.36 22.60 3 7 0 358.26 21.50 3 7 0 396.66 24.50 3 7 0 405.16 23.90 -4 -7 0 12.30 6.00 4 -7 0 6.30 7.50 4 -7 0 -8.40 6.30 -4 -7 0 7.20 7.40 -4 -7 0 11.60 6.50 -4 -7 0 6.30 7.50 4 -7 0 5.80 4.90 4 -7 0 2.10 6.20 4 -7 0 4.60 10.90 -4 -7 0 8.80 6.10 4 -7 0 16.20 6.10 4 -7 0 16.70 7.00 -4 -7 0 20.00 10.80 4 7 0 19.20 5.70 4 7 0 4.90 5.40 4 7 0 3.40 7.00 4 7 0 4.80 6.80 4 7 0 11.50 6.00 -5 -7 0 6.80 5.30 5 -7 0 10.30 7.20 5 -7 0 16.90 20.00 5 -7 0 15.20 6.90 5 -7 0 9.30 4.60 5 -7 0 -7.90 7.70 -5 -7 0 24.10 12.10 -5 -7 0 16.20 15.50 5 -7 0 7.10 6.70 -5 -7 0 10.90 6.20 -5 -7 0 10.20 5.50 5 -7 0 16.60 4.90 -5 -7 0 3.10 5.40 5 7 0 7.30 5.10 5 7 0 12.00 6.20 5 7 0 24.80 10.20 5 7 0 13.80 5.40 -6 -7 0 12.40 3.50 -6 -7 0 10.90 5.40 6 -7 0 6.30 5.80 -6 -7 0 16.70 7.80 6 -7 0 11.20 6.30 6 -7 0 19.40 6.10 6 -7 0 12.90 7.40 6 -7 0 9.40 5.90 -6 -7 0 12.50 16.20 6 -7 0 17.00 6.80 6 7 0 12.40 5.00 6 7 0 17.60 5.90 6 7 0 7.90 6.20 6 7 0 7.60 7.40 -7 -7 0 193.88 15.70 7 -7 0 182.38 15.80 7 -7 0 188.78 12.70 7 -7 0 177.88 12.30 -7 -7 0 186.38 10.30 -7 -7 0 164.58 18.30 7 -7 0 188.08 13.60 -7 -7 0 179.18 18.50 7 7 0 212.18 14.80 7 7 0 184.28 11.80 8 -7 0 3.20 3.70 -8 -7 0 2.50 5.70 -8 -7 0 0.70 2.90 8 -7 0 0.00 4.30 -8 -7 0 8.30 8.30 8 -7 0 5.20 4.80 -8 -7 0 4.90 6.60 8 -7 0 -3.70 4.40 8 -7 0 4.50 5.00 8 7 0 10.30 6.10 8 7 0 3.00 4.60 8 7 0 8.70 5.00 9 -7 0 24.40 5.70 9 -7 0 25.20 5.00 -9 -7 0 12.90 5.30 9 -7 0 18.10 6.80 -9 -7 0 14.90 6.30 -9 -7 0 23.00 3.90 9 -7 0 5.80 6.40 -9 -7 0 16.10 6.10 9 -7 0 9.90 4.90 9 7 0 17.80 6.10 10 -7 0 19.00 7.30 -10 -7 0 8.40 5.40 10 -7 0 8.60 5.30 -10 -7 0 11.20 3.20 10 -7 0 12.50 4.90 10 -7 0 17.90 4.90 10 7 0 15.20 3.60 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548.15 24.80 -4 -2 23 542.55 27.10 4 -2 -23 497.55 23.10 -4 2 23 495.95 25.90 4 2 -23 550.84 25.40 -4 2 23 539.05 25.60 -4 2 23 528.95 24.30 4 2 -23 519.75 25.60 -3 -2 23 41.30 7.50 -3 -2 23 30.80 5.30 -3 -2 23 45.20 6.20 3 -2 -23 34.50 6.90 -3 2 23 32.00 7.30 -3 2 23 34.20 5.60 3 2 -23 34.40 6.20 -3 2 23 64.29 11.50 3 2 -23 18.00 10.70 3 2 -23 53.29 9.10 -2 -2 23 452.05 24.30 2 -2 -23 493.55 22.30 2 -2 -23 461.35 24.00 -2 -2 23 483.45 22.60 2 2 -23 417.96 27.30 2 2 -23 491.25 23.50 -2 2 23 455.95 24.70 2 2 -23 481.75 24.30 -2 2 23 452.95 22.20 -2 2 23 463.85 23.50 1 -2 -23 663.73 33.30 -1 -2 23 708.03 31.20 1 -2 -23 705.23 30.90 -1 -2 23 637.14 30.20 -1 -2 23 736.83 34.30 1 2 -23 647.74 34.80 -1 2 23 675.73 33.30 1 2 -23 703.83 33.10 1 2 -23 725.13 31.70 -1 2 23 701.03 31.00 -1 2 23 679.73 32.60 0 -2 -23 17.50 6.90 0 -2 23 20.40 4.90 0 -2 23 18.10 7.50 0 -2 23 30.90 4.30 0 -2 -23 22.10 5.30 0 -2 23 29.90 6.30 0 2 -23 19.80 4.50 0 2 23 17.00 4.80 0 2 23 24.80 5.60 0 2 -23 29.90 8.00 0 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384.96 22.20 2 1 -25 345.47 17.30 -2 1 25 344.97 18.50 -1 -1 25 54.09 6.10 1 -1 -25 70.19 8.10 1 -1 -25 62.29 6.30 -1 -1 25 60.39 7.60 -1 1 25 47.60 7.80 1 1 -25 71.29 6.60 -1 1 25 56.79 6.80 -1 1 25 55.89 5.90 0 -1 25 -0.40 2.50 0 -1 -25 -0.80 6.40 0 -1 -25 -4.30 2.80 0 1 -25 9.40 5.50 0 1 25 3.50 3.40 0 1 25 -2.60 5.70 0 1 -25 -9.40 9.80 0 1 25 -2.70 3.60 -1 -1 -25 227.88 13.10 1 -1 25 239.58 12.80 -1 -1 -25 230.78 14.30 -1 1 -25 211.38 13.90 -1 1 -25 215.38 12.70 1 1 25 234.38 14.00 -2 -1 -25 186.88 10.70 2 -1 25 187.48 11.40 -2 1 -25 183.18 11.20 -2 1 -25 167.38 12.40 -3 -1 -25 -2.20 2.70 -3 -1 -25 -8.20 4.70 3 -1 25 -0.80 3.10 -3 1 -25 4.70 4.00 -3 1 -25 0.30 4.20 -3 1 -25 1.50 5.90 4 -1 25 7.90 4.60 -4 -1 -25 2.00 5.00 -4 -1 -25 1.00 2.80 -4 1 -25 -7.10 5.10 4 1 25 5.60 4.70 -4 1 -25 2.30 3.00 -4 1 -25 -0.60 5.90 5 -1 25 186.38 11.20 -5 -1 -25 224.28 11.90 -5 1 -25 202.48 12.20 -5 1 -25 217.18 11.50 -5 -2 25 148.39 10.10 -5 2 25 151.78 8.50 5 2 -25 170.38 10.40 4 -2 -25 43.90 6.20 -4 -2 25 29.20 5.40 -4 -2 25 50.09 5.90 -4 2 25 37.30 6.30 4 2 -25 39.80 5.10 -4 2 25 33.20 8.40 -3 -2 25 4.50 4.10 -3 -2 25 1.10 3.60 3 -2 -25 7.10 4.00 -3 2 25 12.10 4.30 -3 2 25 3.70 3.80 3 2 -25 2.10 4.20 -3 2 25 4.10 2.70 2 -2 -25 205.88 12.80 -2 -2 25 214.68 11.80 2 -2 -25 195.18 10.00 2 2 -25 221.58 12.40 -2 2 25 202.18 13.80 -2 2 25 170.18 13.00 -2 2 25 209.48 10.70 1 -2 -25 33.90 5.90 -1 -2 25 21.60 4.30 1 -2 -25 29.40 5.30 1 2 -25 26.50 6.40 -1 2 25 26.20 4.80 -1 2 25 35.40 4.50 1 2 -25 34.90 4.70 -1 2 25 31.50 5.70 0 -2 25 2.30 3.60 0 -2 -25 3.30 5.60 0 -2 -25 3.90 2.90 0 2 25 7.60 4.20 0 2 -25 1.70 4.30 0 2 25 1.40 3.50 0 2 -25 8.40 4.20 1 -2 25 157.58 9.40 -1 -2 -25 149.99 12.30 -1 2 -25 151.88 10.60 -1 2 -25 153.78 10.40 -2 -2 -25 65.59 7.40 -2 -2 -25 83.59 12.10 2 -2 25 67.59 6.90 -2 2 -25 63.79 6.40 2 2 25 62.39 6.70 -2 2 -25 55.99 8.50 -3 -2 -25 65.39 7.10 -3 -2 -25 77.49 7.60 3 -2 25 64.49 6.70 -3 2 -25 71.39 6.60 -4 -2 -25 9.10 2.80 -4 -2 -25 5.30 4.40 4 -2 25 12.70 4.20 -4 2 -25 18.90 3.90 -4 2 -25 15.00 4.00 -2 -3 25 -0.10 3.30 -2 -3 25 -1.50 3.30 2 3 -25 4.40 4.00 2 3 -25 3.60 3.00 -2 3 25 3.10 4.10 -1 -3 25 8.60 5.20 1 -3 -25 6.10 3.70 -1 3 25 8.10 3.40 1 3 -25 13.70 6.80 1 3 -25 13.10 4.10 0 -3 -25 8.50 5.60 0 -3 25 4.90 3.10 0 3 -25 5.50 3.20 0 3 -25 4.40 5.30 0 3 25 5.70 3.40 1 -3 25 0.90 3.00 -1 -3 -25 6.60 8.00 -1 3 -25 9.50 4.00 -1 3 -25 7.00 4.10 1 3 25 5.00 2.40 -4 0 26 8.80 5.10 -4 0 26 6.00 3.90 4 0 -26 14.20 3.00 4 0 -26 10.30 6.00 -3 0 26 21.60 4.00 3 0 -26 21.10 3.70 -3 0 26 17.10 4.70 3 0 -26 3.10 6.50 2 0 -26 -0.40 3.90 -2 0 26 1.60 5.10 2 0 -26 -0.80 5.00 -2 0 26 1.20 3.00 -1 0 26 0.80 2.80 1 0 -26 1.00 3.90 1 0 -26 8.60 5.50 -1 0 26 3.70 3.80 0 0 -26 230.98 14.90 0 0 26 252.67 13.70 -1 0 -26 6.70 9.20 -1 0 -26 24.30 3.90 1 0 26 17.60 4.40 -2 0 -26 158.48 9.40 -3 0 -26 247.58 12.70 -3 -1 26 148.59 10.60 -3 -1 26 162.98 9.90 3 -1 -26 148.99 8.60 -3 1 26 147.39 10.50 3 1 -26 161.28 9.20 -3 1 26 155.28 9.80 2 -1 -26 2.10 2.60 -2 -1 26 -1.10 3.50 -2 -1 26 5.60 2.80 2 -1 -26 7.80 5.60 2 1 -26 0.30 2.70 -2 1 26 10.20 5.70 -2 1 26 0.40 3.30 -1 -1 26 4.80 3.70 1 -1 -26 4.90 4.30 1 -1 -26 2.60 4.20 -1 1 26 5.00 4.10 1 1 -26 6.20 2.90 -1 1 26 11.50 4.80 0 -1 -26 40.20 6.10 0 -1 -26 38.60 5.00 0 -1 26 54.29 6.20 0 1 26 53.79 6.00 0 1 -26 45.20 5.40 1 -1 26 312.97 15.00 -1 1 -26 302.07 15.20 2 -1 26 43.00 7.00 -2 -1 -26 59.09 7.40 -2 -1 -26 37.00 5.60 -2 1 -26 44.30 5.20 -3 1 -26 123.79 8.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 4814 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Cl Cl1 0.29558(2) 1.07461(5) 0.38659(2) 0.03344(12) Uani d . . . 1 . . Cl Cl2 0.41804(2) 0.90864(4) 0.46845(2) 0.02053(10) Uani d . . . 1 . . N N1 0.18655(7) 0.56752(16) 0.36754(5) 0.0181(3) Uani d . . . 1 . . N N2 0.33920(7) 0.58907(14) 0.61480(5) 0.0137(2) Uani d . . . 1 . . O O1 0.19484(6) 0.74291(12) 0.39368(4) 0.0171(2) Uani d . . . 1 . . O O2 0.31785(6) 0.65666(12) 0.55500(4) 0.0145(2) Uani d . . . 1 . . C C1 0.26115(8) 0.75450(18) 0.43974(6) 0.0161(3) Uani d . . . 1 . . H H1 0.284500 0.634085 0.448199 0.019000 Uiso calc U . R 1 . . C C2 0.33465(9) 0.8692(2) 0.41464(6) 0.0209(3) Uani d . . . 1 . . H H2 0.361077 0.803768 0.380767 0.025000 Uiso calc U . R 1 . . C C3 0.22090(8) 0.82760(17) 0.49604(6) 0.0149(3) Uani d . . . 1 . . C C4 0.24946(8) 0.77446(16) 0.55335(6) 0.0136(3) Uani d . . . 1 . . C C5 0.20765(8) 0.83575(17) 0.60385(6) 0.0160(3) Uani d . . . 1 . . H H5 0.227722 0.801084 0.642390 0.019000 Uiso calc U . R 1 . . C C6 0.13660(9) 0.94755(18) 0.59773(6) 0.0175(3) Uani d . . . 1 . . H H6 0.107330 0.987039 0.632224 0.021000 Uiso calc U . R 1 . . C C7 0.10780(9) 1.00236(18) 0.54179(6) 0.0192(3) Uani d . . . 1 . . H H7 0.059344 1.079612 0.537841 0.023000 Uiso calc U . R 1 . . C C8 0.15061(9) 0.94300(18) 0.49166(6) 0.0173(3) Uani d . . . 1 . . H H8 0.131476 0.982097 0.453400 0.021000 Uiso calc U . R 1 . . C C9 0.19536(10) 0.5918(2) 0.30152(6) 0.0250(3) Uani d . . . 1 . . C C10 0.17858(10) 0.4115(2) 0.27292(7) 0.0316(4) Uani d . . . 1 . . H H10A 0.181047 0.423708 0.229053 0.038000 Uiso calc U . R 1 . . H H10B 0.225716 0.330005 0.285611 0.038000 Uiso calc U . R 1 . . C C11 0.09161(11) 0.3319(2) 0.28896(7) 0.0338(4) Uani d . . . 1 . . H H11A 0.085522 0.213983 0.270616 0.041000 Uiso calc U . R 1 . . H H11B 0.043511 0.407059 0.273627 0.041000 Uiso calc U . R 1 . . C C12 0.08686(10) 0.3170(2) 0.35643(7) 0.0300(4) Uani d . . . 1 . . H H12A 0.130938 0.230601 0.370509 0.036000 Uiso calc U . R 1 . . H H12B 0.028673 0.271192 0.366952 0.036000 Uiso calc U . R 1 . . C C13 0.10234(9) 0.4918(2) 0.38920(6) 0.0213(3) Uani d . . . 1 . . C C14 0.13634(11) 0.7342(2) 0.27356(7) 0.0317(4) Uani d . . . 1 . . H H14A 0.076296 0.690396 0.270669 0.048000 Uiso calc U . R 1 . . H H14B 0.156964 0.762996 0.233628 0.048000 Uiso calc U . R 1 . . H H14C 0.138140 0.839870 0.298548 0.048000 Uiso calc U . R 1 . . C C15 0.29018(11) 0.6423(3) 0.28984(7) 0.0378(4) Uani d . . . 1 . . H H15A 0.299176 0.766604 0.299740 0.057000 Uiso calc U . R 1 . . H H15B 0.302900 0.623024 0.247688 0.057000 Uiso calc U . R 1 . . H H15C 0.329177 0.569608 0.314623 0.057000 Uiso calc U . R 1 . . C C16 0.02231(9) 0.6127(2) 0.38237(7) 0.0272(3) Uani d . . . 1 . . H H16A 0.038408 0.732791 0.394003 0.041000 Uiso calc U . R 1 . . H H16B -0.024302 0.570257 0.408018 0.041000 Uiso calc U . R 1 . . H H16C 0.001846 0.612064 0.340743 0.041000 Uiso calc U . R 1 . . C C17 0.11601(10) 0.4508(2) 0.45536(7) 0.0264(3) Uani d . . . 1 . . H H17A 0.170143 0.383817 0.461020 0.040000 Uiso calc U . R 1 . . H H17B 0.066749 0.381181 0.469584 0.040000 Uiso calc U . R 1 . . H H17C 0.119889 0.560919 0.477929 0.040000 Uiso calc U . R 1 . . C C18 0.31155(9) 0.40028(17) 0.61484(6) 0.0169(3) Uani d . . . 1 . . C C19 0.34328(10) 0.32193(19) 0.67460(6) 0.0225(3) Uani d . . . 1 . . H H19A 0.309609 0.375530 0.707183 0.027000 Uiso calc U . R 1 . . H H19B 0.331118 0.194055 0.674572 0.027000 Uiso calc U . R 1 . . C C20 0.43999(10) 0.3504(2) 0.68724(7) 0.0255(3) Uani d . . . 1 . . H H20A 0.474893 0.289929 0.656703 0.031000 Uiso calc U . R 1 . . H H20B 0.456192 0.301420 0.726786 0.031000 Uiso calc U . R 1 . . C C21 0.45835(9) 0.54692(19) 0.68605(6) 0.0206(3) Uani d . . . 1 . . H H21A 0.521291 0.566468 0.694113 0.025000 Uiso calc U . R 1 . . H H21B 0.425630 0.604375 0.718341 0.025000 Uiso calc U . R 1 . . C C22 0.43312(8) 0.63384(18) 0.62644(6) 0.0157(3) Uani d . . . 1 . . C C23 0.34261(9) 0.28899(18) 0.56212(6) 0.0216(3) Uani d . . . 1 . . H H23A 0.332567 0.353803 0.524870 0.032000 Uiso calc U . R 1 . . H H23B 0.310046 0.178113 0.560743 0.032000 Uiso calc U . R 1 . . H H23C 0.405025 0.264088 0.567123 0.032000 Uiso calc U . R 1 . . C C24 0.21167(9) 0.40040(18) 0.61447(6) 0.0204(3) Uani d . . . 1 . . H H24A 0.190963 0.473203 0.647374 0.031000 Uiso calc U . R 1 . . H H24B 0.190411 0.279759 0.619256 0.031000 Uiso calc U . R 1 . . H H24C 0.189708 0.448323 0.576532 0.031000 Uiso calc U . R 1 . . C C25 0.49692(9) 0.57984(18) 0.57758(6) 0.0193(3) Uani d . . . 1 . . H H25A 0.503768 0.451687 0.577675 0.029000 Uiso calc U . R 1 . . H H25B 0.553685 0.635388 0.585278 0.029000 Uiso calc U . R 1 . . H H25C 0.473970 0.618026 0.538641 0.029000 Uiso calc U . R 1 . . C C26 0.43729(9) 0.83403(18) 0.63429(6) 0.0188(3) Uani d . . . 1 . . H H26A 0.421042 0.891424 0.596594 0.028000 Uiso calc U . R 1 . . H H26B 0.496734 0.868553 0.646011 0.028000 Uiso calc U . R 1 . . H H26C 0.396741 0.870051 0.665295 0.028000 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 Cl1 0.02202(19) 0.0363(2) 0.0419(2) -0.00297(15) -0.00201(15) 0.02242(17) Cl2 0.01442(17) 0.02632(19) 0.02080(17) -0.00488(12) -0.00113(12) 0.00298(13) N1 0.0154(6) 0.0246(6) 0.0142(6) 0.0009(5) 0.0005(4) -0.0055(5) N2 0.0148(6) 0.0156(6) 0.0107(5) -0.0010(4) -0.0021(4) 0.0034(4) O1 0.0145(5) 0.0222(5) 0.0145(4) 0.0010(4) -0.0027(3) -0.0011(4) O2 0.0154(5) 0.0169(5) 0.0111(4) 0.0032(4) 0.0006(3) 0.0017(3) C1 0.0129(6) 0.0220(7) 0.0135(6) 0.0002(5) -0.0013(5) 0.0011(5) C2 0.0154(7) 0.0292(8) 0.0181(7) -0.0008(6) -0.0013(5) 0.0033(6) C3 0.0130(6) 0.0154(6) 0.0163(6) -0.0030(5) 0.0010(5) -0.0005(5) C4 0.0122(6) 0.0114(6) 0.0172(6) -0.0017(5) 0.0002(5) 0.0001(5) C5 0.0172(7) 0.0162(7) 0.0145(6) -0.0028(5) 0.0002(5) -0.0008(5) C6 0.0164(7) 0.0173(7) 0.0190(7) -0.0017(5) 0.0038(5) -0.0048(5) C7 0.0154(6) 0.0164(7) 0.0256(7) 0.0021(5) -0.0002(5) -0.0023(6) C8 0.0159(7) 0.0177(7) 0.0183(7) -0.0010(5) -0.0026(5) 0.0010(5) C9 0.0200(7) 0.0424(9) 0.0126(7) 0.0049(6) 0.0015(5) -0.0037(6) C10 0.0274(8) 0.0480(10) 0.0192(7) 0.0129(7) -0.0042(6) -0.0128(7) C11 0.0311(9) 0.0374(9) 0.0325(9) 0.0057(7) -0.0106(7) -0.0165(7) C12 0.0258(8) 0.0301(9) 0.0339(9) -0.0021(7) -0.0065(6) -0.0078(7) C13 0.0153(7) 0.0270(8) 0.0215(7) -0.0022(6) -0.0004(5) -0.0037(6) C14 0.0331(9) 0.0450(10) 0.0169(7) 0.0046(7) -0.0009(6) 0.0026(7) C15 0.0252(8) 0.0708(13) 0.0177(7) -0.0019(8) 0.0078(6) -0.0063(8) C16 0.0137(7) 0.0388(9) 0.0292(8) 0.0013(6) 0.0014(6) -0.0073(7) C17 0.0273(8) 0.0296(8) 0.0225(8) -0.0091(6) 0.0020(6) 0.0004(6) C18 0.0177(7) 0.0133(7) 0.0198(7) -0.0016(5) 0.0010(5) 0.0012(5) C19 0.0256(8) 0.0183(7) 0.0238(7) 0.0001(6) 0.0018(6) 0.0062(6) C20 0.0269(8) 0.0264(8) 0.0230(7) 0.0043(6) -0.0037(6) 0.0071(6) C21 0.0178(7) 0.0268(8) 0.0172(7) 0.0018(6) -0.0030(5) -0.0006(6) C22 0.0130(6) 0.0178(7) 0.0162(6) -0.0007(5) -0.0002(5) -0.0007(5) C23 0.0221(7) 0.0161(7) 0.0265(7) 0.0000(6) 0.0011(6) -0.0038(6) C24 0.0188(7) 0.0172(7) 0.0252(7) -0.0040(5) 0.0019(6) 0.0003(5) C25 0.0156(7) 0.0217(7) 0.0208(7) 0.0007(5) 0.0023(5) -0.0021(5) C26 0.0171(7) 0.0197(7) 0.0197(7) -0.0033(5) 0.0025(5) -0.0039(5) 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' Cl Cl 0.3639 0.7018 '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 O1 N1 C9 . . 105.96(10) ? O1 N1 C13 . . 106.80(9) ? C9 N1 C13 . . 117.33(11) ? O2 N2 C18 . . 106.12(9) ? O2 N2 C22 . . 106.13(9) ? C18 N2 C22 . . 119.28(10) ? C1 O1 N1 . . 113.53(9) ? C4 O2 N2 . . 114.14(9) ? O1 C1 C3 . . 109.07(10) ? O1 C1 C2 . . 106.53(10) ? C3 C1 C2 . . 114.03(11) ? O1 C1 H1 . . 109.000000 ? C3 C1 H1 . . 109.000000 ? C2 C1 H1 . . 109.000000 ? C1 C2 Cl2 . . 111.81(9) ? C1 C2 Cl1 . . 112.44(10) ? Cl2 C2 Cl1 . . 109.06(8) ? C1 C2 H2 . . 107.800000 ? Cl2 C2 H2 . . 107.800000 ? Cl1 C2 H2 . . 107.800000 ? C8 C3 C4 . . 118.20(12) ? C8 C3 C1 . . 119.79(12) ? C4 C3 C1 . . 121.91(12) ? O2 C4 C5 . . 123.81(11) ? O2 C4 C3 . . 115.75(11) ? C5 C4 C3 . . 120.41(12) ? C6 C5 C4 . . 119.80(12) ? C6 C5 H5 . . 120.100000 ? C4 C5 H5 . . 120.100000 ? C5 C6 C7 . . 120.71(12) ? C5 C6 H6 . . 119.600000 ? C7 C6 H6 . . 119.600000 ? C6 C7 C8 . . 119.21(13) ? C6 C7 H7 . . 120.400000 ? C8 C7 H7 . . 120.400000 ? C7 C8 C3 . . 121.64(12) ? C7 C8 H8 . . 119.200000 ? C3 C8 H8 . . 119.200000 ? N1 C9 C15 . . 107.57(11) ? N1 C9 C10 . . 106.58(12) ? C15 C9 C10 . . 107.79(13) ? N1 C9 C14 . . 115.26(12) ? C15 C9 C14 . . 107.92(14) ? C10 C9 C14 . . 111.44(12) ? C11 C10 C9 . . 113.59(13) ? C11 C10 H10A . . 108.800000 ? C9 C10 H10A . . 108.800000 ? C11 C10 H10B . . 108.800000 ? C9 C10 H10B . . 108.800000 ? H10A C10 H10B . . 107.700000 ? C10 C11 C12 . . 108.91(13) ? C10 C11 H11A . . 109.900000 ? C12 C11 H11A . . 109.900000 ? C10 C11 H11B . . 109.900000 ? C12 C11 H11B . . 109.900000 ? H11A C11 H11B . . 108.300000 ? C11 C12 C13 . . 113.72(14) ? C11 C12 H12A . . 108.800000 ? C13 C12 H12A . . 108.800000 ? C11 C12 H12B . . 108.800000 ? C13 C12 H12B . . 108.800000 ? H12A C12 H12B . . 107.700000 ? N1 C13 C17 . . 106.78(11) ? N1 C13 C12 . . 107.66(11) ? C17 C13 C12 . . 107.80(13) ? N1 C13 C16 . . 115.30(12) ? C17 C13 C16 . . 108.32(12) ? C12 C13 C16 . . 110.68(12) ? C9 C14 H14A . . 109.500000 ? C9 C14 H14B . . 109.500000 ? H14A C14 H14B . . 109.500000 ? C9 C14 H14C . . 109.500000 ? H14A C14 H14C . . 109.500000 ? H14B C14 H14C . . 109.500000 ? C9 C15 H15A . . 109.500000 ? C9 C15 H15B . . 109.500000 ? H15A C15 H15B . . 109.500000 ? C9 C15 H15C . . 109.500000 ? H15A C15 H15C . . 109.500000 ? H15B C15 H15C . . 109.500000 ? C13 C16 H16A . . 109.500000 ? C13 C16 H16B . . 109.500000 ? H16A C16 H16B . . 109.500000 ? C13 C16 H16C . . 109.500000 ? H16A C16 H16C . . 109.500000 ? H16B C16 H16C . . 109.500000 ? C13 C17 H17A . . 109.500000 ? C13 C17 H17B . . 109.500000 ? H17A C17 H17B . . 109.500000 ? C13 C17 H17C . . 109.500000 ? H17A C17 H17C . . 109.500000 ? H17B C17 H17C . . 109.500000 ? N2 C18 C24 . . 106.42(10) ? N2 C18 C23 . . 115.85(11) ? C24 C18 C23 . . 108.63(11) ? N2 C18 C19 . . 106.67(11) ? C24 C18 C19 . . 107.82(11) ? C23 C18 C19 . . 111.11(11) ? C20 C19 C18 . . 113.56(12) ? C20 C19 H19A . . 108.900000 ? C18 C19 H19A . . 108.900000 ? C20 C19 H19B . . 108.900000 ? C18 C19 H19B . . 108.900000 ? H19A C19 H19B . . 107.700000 ? C19 C20 C21 . . 108.48(12) ? C19 C20 H20A . . 110.000000 ? C21 C20 H20A . . 110.000000 ? C19 C20 H20B . . 110.000000 ? C21 C20 H20B . . 110.000000 ? H20A C20 H20B . . 108.400000 ? C20 C21 C22 . . 113.23(12) ? C20 C21 H21A . . 108.900000 ? C22 C21 H21A . . 108.900000 ? C20 C21 H21B . . 108.900000 ? C22 C21 H21B . . 108.900000 ? H21A C21 H21B . . 107.700000 ? N2 C22 C26 . . 106.47(10) ? N2 C22 C21 . . 106.30(10) ? C26 C22 C21 . . 108.53(11) ? N2 C22 C25 . . 115.89(11) ? C26 C22 C25 . . 108.74(11) ? C21 C22 C25 . . 110.63(11) ? C18 C23 H23A . . 109.500000 ? C18 C23 H23B . . 109.500000 ? H23A C23 H23B . . 109.500000 ? C18 C23 H23C . . 109.500000 ? H23A C23 H23C . . 109.500000 ? H23B C23 H23C . . 109.500000 ? C18 C24 H24A . . 109.500000 ? C18 C24 H24B . . 109.500000 ? H24A C24 H24B . . 109.500000 ? C18 C24 H24C . . 109.500000 ? H24A C24 H24C . . 109.500000 ? H24B C24 H24C . . 109.500000 ? C22 C25 H25A . . 109.500000 ? C22 C25 H25B . . 109.500000 ? H25A C25 H25B . . 109.500000 ? C22 C25 H25C . . 109.500000 ? H25A C25 H25C . . 109.500000 ? H25B C25 H25C . . 109.500000 ? C22 C26 H26A . . 109.500000 ? C22 C26 H26B . . 109.500000 ? H26A C26 H26B . . 109.500000 ? C22 C26 H26C . . 109.500000 ? H26A C26 H26C . . 109.500000 ? H26B C26 H26C . . 109.500000 ? 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 Cl1 C2 . 1.7837(15) ? Cl2 C2 . 1.7686(14) ? N1 O1 . 1.4614(14) ? N1 C9 . 1.5012(17) ? N1 C13 . 1.5021(18) ? N2 O2 . 1.4682(13) ? N2 C18 . 1.4967(17) ? N2 C22 . 1.4982(16) ? O1 C1 . 1.4395(15) ? O2 C4 . 1.3791(15) ? C1 C3 . 1.5207(18) ? C1 C2 . 1.5392(19) ? C1 H1 . 1.000000 ? C2 H2 . 1.000000 ? C3 C8 . 1.3918(19) ? C3 C4 . 1.4101(18) ? C4 C5 . 1.3918(18) ? C5 C6 . 1.3867(19) ? C5 H5 . 0.950000 ? C6 C7 . 1.387(2) ? C6 H6 . 0.950000 ? C7 C8 . 1.387(2) ? C7 H7 . 0.950000 ? C8 H8 . 0.950000 ? C9 C15 . 1.531(2) ? C9 C10 . 1.534(2) ? C9 C14 . 1.537(2) ? C10 C11 . 1.514(2) ? C10 H10A . 0.990000 ? C10 H10B . 0.990000 ? C11 C12 . 1.521(2) ? C11 H11A . 0.990000 ? C11 H11B . 0.990000 ? C12 C13 . 1.536(2) ? C12 H12A . 0.990000 ? C12 H12B . 0.990000 ? C13 C17 . 1.528(2) ? C13 C16 . 1.539(2) ? C14 H14A . 0.980000 ? C14 H14B . 0.980000 ? C14 H14C . 0.980000 ? C15 H15A . 0.980000 ? C15 H15B . 0.980000 ? C15 H15C . 0.980000 ? C16 H16A . 0.980000 ? C16 H16B . 0.980000 ? C16 H16C . 0.980000 ? C17 H17A . 0.980000 ? C17 H17B . 0.980000 ? C17 H17C . 0.980000 ? C18 C24 . 1.5314(19) ? C18 C23 . 1.5368(19) ? C18 C19 . 1.5381(19) ? C19 C20 . 1.520(2) ? C19 H19A . 0.990000 ? C19 H19B . 0.990000 ? C20 C21 . 1.520(2) ? C20 H20A . 0.990000 ? C20 H20B . 0.990000 ? C21 C22 . 1.5352(18) ? C21 H21A . 0.990000 ? C21 H21B . 0.990000 ? C22 C26 . 1.5335(19) ? C22 C25 . 1.5377(18) ? C23 H23A . 0.980000 ? C23 H23B . 0.980000 ? C23 H23C . 0.980000 ? C24 H24A . 0.980000 ? C24 H24B . 0.980000 ? C24 H24C . 0.980000 ? C25 H25A . 0.980000 ? C25 H25B . 0.980000 ? C25 H25C . 0.980000 ? C26 H26A . 0.980000 ? C26 H26B . 0.980000 ? C26 H26C . 0.980000 ? 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 C9 N1 O1 C1 . . . . -125.85(11) ? C13 N1 O1 C1 . . . . 108.33(11) ? C18 N2 O2 C4 . . . . 109.60(11) ? C22 N2 O2 C4 . . . . -122.54(11) ? N1 O1 C1 C3 . . . . -125.45(11) ? N1 O1 C1 C2 . . . . 111.04(11) ? O1 C1 C2 Cl2 . . . . 175.79(9) ? C3 C1 C2 Cl2 . . . . 55.43(14) ? O1 C1 C2 Cl1 . . . . 52.71(13) ? C3 C1 C2 Cl1 . . . . -67.65(13) ? O1 C1 C3 C8 . . . . -29.96(16) ? C2 C1 C3 C8 . . . . 88.96(15) ? O1 C1 C3 C4 . . . . 146.42(12) ? C2 C1 C3 C4 . . . . -94.66(15) ? N2 O2 C4 C5 . . . . 4.56(16) ? N2 O2 C4 C3 . . . . -173.39(10) ? C8 C3 C4 O2 . . . . 178.42(11) ? C1 C3 C4 O2 . . . . 1.99(18) ? C8 C3 C4 C5 . . . . 0.40(19) ? C1 C3 C4 C5 . . . . -176.04(12) ? O2 C4 C5 C6 . . . . -176.84(12) ? C3 C4 C5 C6 . . . . 1.02(19) ? C4 C5 C6 C7 . . . . -1.4(2) ? C5 C6 C7 C8 . . . . 0.4(2) ? C6 C7 C8 C3 . . . . 1.0(2) ? C4 C3 C8 C7 . . . . -1.43(19) ? C1 C3 C8 C7 . . . . 175.08(12) ? O1 N1 C9 C15 . . . . 69.61(14) ? C13 N1 C9 C15 . . . . -171.30(13) ? O1 N1 C9 C10 . . . . -175.01(10) ? C13 N1 C9 C10 . . . . -55.92(15) ? O1 N1 C9 C14 . . . . -50.81(15) ? C13 N1 C9 C14 . . . . 68.29(17) ? N1 C9 C10 C11 . . . . 55.86(16) ? C15 C9 C10 C11 . . . . 171.10(14) ? C14 C9 C10 C11 . . . . -70.67(17) ? C9 C10 C11 C12 . . . . -57.26(18) ? C10 C11 C12 C13 . . . . 55.36(18) ? O1 N1 C13 C17 . . . . -71.14(13) ? C9 N1 C13 C17 . . . . 170.22(12) ? O1 N1 C13 C12 . . . . 173.33(10) ? C9 N1 C13 C12 . . . . 54.69(16) ? O1 N1 C13 C16 . . . . 49.24(14) ? C9 N1 C13 C16 . . . . -69.40(16) ? C11 C12 C13 N1 . . . . -52.67(16) ? C11 C12 C13 C17 . . . . -167.53(13) ? C11 C12 C13 C16 . . . . 74.17(16) ? O2 N2 C18 C24 . . . . -71.62(12) ? C22 N2 C18 C24 . . . . 168.80(10) ? O2 N2 C18 C23 . . . . 49.23(14) ? C22 N2 C18 C23 . . . . -70.35(15) ? O2 N2 C18 C19 . . . . 173.47(10) ? C22 N2 C18 C19 . . . . 53.89(14) ? N2 C18 C19 C20 . . . . -53.16(15) ? C24 C18 C19 C20 . . . . -167.12(12) ? C23 C18 C19 C20 . . . . 73.96(15) ? C18 C19 C20 C21 . . . . 57.53(16) ? C19 C20 C21 C22 . . . . -58.45(16) ? O2 N2 C22 C26 . . . . 70.14(12) ? C18 N2 C22 C26 . . . . -170.28(11) ? O2 N2 C22 C21 . . . . -174.28(10) ? C18 N2 C22 C21 . . . . -54.70(14) ? O2 N2 C22 C25 . . . . -50.91(14) ? C18 N2 C22 C25 . . . . 68.66(15) ? C20 C21 C22 N2 . . . . 54.80(15) ? C20 C21 C22 C26 . . . . 168.97(12) ? C20 C21 C22 C25 . . . . -71.80(15) ?