#------------------------------------------------------------------------------ #$Date: 2019-05-25 07:29:27 +0300 (Sat, 25 May 2019) $ #$Revision: 215524 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/84/2108402.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2108402 loop_ _publ_author_name 'So, Hee-Soo' 'Matsumoto, Shinya' _publ_section_title ; Three differently coloured polymorphs of 3,6-bis(4-chlorophenyl)-2,5-dipropyl-2,5-dihydropyrrolo[3,4-c]pyrrole-1,4-dione ; _journal_coeditor_code BM5110SUP1 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520619004773 _journal_volume 75 _journal_year 2019 _chemical_formula_moiety 'C24 H22 Cl2 N2 O2' _chemical_formula_sum 'C24 H22 Cl2 N2 O2' _chemical_formula_weight 441.36 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 117.163(2) _cell_angle_gamma 90.0000 _cell_formula_units_Z 8 _cell_length_a 18.1075(2) _cell_length_b 14.16642(16) _cell_length_c 18.5436(3) _cell_measurement_reflns_used 6513 _cell_measurement_temperature 223 _cell_measurement_theta_max 73.94 _cell_measurement_theta_min 4.15 _cell_volume 4232.16(12) _computing_cell_refinement 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_molecular_graphics 'CrystalStructure 4.2' _computing_publication_material 'CrystalStructure 4.2 (Rigaku, 2017)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'SHELXT Version 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 223 _diffrn_detector_area_resol_mean 5.811 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku XtaLAB P200' _diffrn_measurement_method \w _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 10850 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 66.499 _diffrn_reflns_theta_max 66.499 _diffrn_reflns_theta_min 4.113 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.951 _exptl_absorpt_correction_T_max 0.753 _exptl_absorpt_correction_T_min 0.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour fluorescentlightr _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1840.00 _exptl_crystal_size_max 0.345 _exptl_crystal_size_mid 0.118 _exptl_crystal_size_min 0.096 _refine_diff_density_max 0.35 _refine_diff_density_min -0.25 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 271 _refine_ls_number_reflns 3726 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0459 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0730P)^2^+1.7848P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1354 _refine_ls_wR_factor_ref 0.1391 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3303 _reflns_number_total 3726 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file bm5110sup1.cif _cod_data_source_block I _cod_database_code 2108402 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL PR3R CELL 1.54187 18.10750 14.16642 18.54360 90.00000 117.16300 90.00000 ZERR 8 0.00020 0.00016 0.00030 0.00000 0.00200 0.00000 LATT 2 SYMM .50-X, +Y, -Z SFAC C H CL N O UNIT 192 176 16 16 16 SHEL 99999.000000 0.840660 L.S. 10 FMAP 2 PLAN 25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 23.0 ACTA SIZE 0.345 0.118 0.096 WGHT 0.073000 1.784800 FVAR 0.17594 CL2 3 1.099869 0.697151 0.375591 11.00000 0.04889 0.07180 = 0.12021 0.00290 0.05476 0.00629 CL1 3 0.289902 0.801354 0.406244 11.00000 0.05379 0.08182 = 0.13857 -0.00463 0.06454 0.00105 O2 5 0.613811 0.569974 0.405642 11.00000 0.04040 0.04339 = 0.07118 -0.00667 0.02937 -0.00627 O1 5 0.785860 0.920018 0.395838 11.00000 0.04461 0.04271 = 0.06706 0.00285 0.03337 -0.00025 N1 4 0.664618 0.887038 0.405713 11.00000 0.03894 0.03778 = 0.05236 0.00001 0.02635 0.00427 N2 4 0.738453 0.603031 0.401915 11.00000 0.03370 0.03619 = 0.05502 -0.00361 0.02085 0.00198 C13 1 0.732225 0.760257 0.390824 11.00000 0.03308 0.04159 = 0.04387 -0.00046 0.02041 0.00321 C1 1 0.659404 0.729740 0.394981 11.00000 0.03235 0.04175 = 0.04402 -0.00319 0.01912 0.00166 C3 1 0.736531 0.862053 0.396891 11.00000 0.03559 0.04331 = 0.04432 0.00294 0.02101 0.00522 C14 1 0.779851 0.682573 0.395040 11.00000 0.03166 0.04157 = 0.04035 -0.00140 0.01571 0.00179 C2 1 0.618423 0.807487 0.403538 11.00000 0.03473 0.04242 = 0.03999 -0.00078 0.01856 0.00316 C15 1 0.661582 0.627883 0.401374 11.00000 0.03391 0.04431 = 0.04565 -0.00514 0.01885 0.00057 C16 1 0.859336 0.681868 0.391774 11.00000 0.03275 0.03957 = 0.04709 -0.00552 0.01928 0.00228 C4 1 0.539066 0.809112 0.407027 11.00000 0.03618 0.04064 = 0.04854 0.00309 0.02285 0.00566 C21 1 0.867797 0.742383 0.336818 11.00000 0.03570 0.04671 = 0.04937 -0.00161 0.01951 0.00393 AFIX 43 H21 2 0.823411 0.780396 0.303435 11.00000 -1.20000 AFIX 0 C5 1 0.525697 0.861054 0.463748 11.00000 0.04254 0.04552 = 0.05312 -0.00114 0.02633 0.00357 AFIX 43 H5 2 0.568174 0.897909 0.501674 11.00000 -1.20000 AFIX 0 C6 1 0.449162 0.857945 0.463808 11.00000 0.05354 0.04911 = 0.06702 0.00193 0.04019 0.00943 AFIX 43 H6 2 0.440280 0.892261 0.501902 11.00000 -1.20000 AFIX 0 C17 1 0.927216 0.627226 0.443135 11.00000 0.03753 0.04519 = 0.06217 0.00387 0.02355 0.00519 AFIX 43 H17 2 0.922877 0.587590 0.481002 11.00000 -1.20000 AFIX 0 C18 1 1.001040 0.631849 0.437880 11.00000 0.03560 0.04722 = 0.07503 0.00325 0.02330 0.00861 AFIX 43 H18 2 1.046220 0.595284 0.471956 11.00000 -1.20000 AFIX 0 C20 1 0.941423 0.746726 0.331199 11.00000 0.04427 0.05161 = 0.05641 -0.00203 0.02888 -0.00063 AFIX 43 H20 2 0.946541 0.786590 0.293883 11.00000 -1.20000 AFIX 0 C9 1 0.474981 0.753194 0.351695 11.00000 0.04370 0.05035 = 0.05944 -0.00832 0.02857 -0.00078 AFIX 43 H9 2 0.483850 0.716951 0.314549 11.00000 -1.20000 AFIX 0 C19 1 1.007019 0.690828 0.381979 11.00000 0.03819 0.04741 = 0.07002 -0.00985 0.03054 0.00010 C10 1 0.643170 0.986293 0.408124 11.00000 0.05743 0.03812 = 0.07169 -0.00142 0.04240 0.00596 AFIX 23 H10A 2 0.690780 1.025123 0.417292 11.00000 -1.20000 H10B 2 0.631262 0.995499 0.453607 11.00000 -1.20000 AFIX 0 C8 1 0.398468 0.750719 0.351122 11.00000 0.04163 0.05688 = 0.07407 -0.00698 0.02832 -0.00519 AFIX 43 H8 2 0.355755 0.713839 0.313524 11.00000 -1.20000 AFIX 0 C7 1 0.386446 0.803737 0.407116 11.00000 0.04345 0.04983 = 0.07861 0.00902 0.03804 0.00747 C22 1 0.758014 0.503889 0.395788 11.00000 0.03967 0.03671 = 0.08911 -0.00266 0.02742 0.00387 AFIX 23 H22A 2 0.722673 0.463950 0.409402 11.00000 -1.20000 H22B 2 0.815145 0.491597 0.434839 11.00000 -1.20000 AFIX 0 C11 1 0.570414 1.018824 0.332633 11.00000 0.05337 0.05103 = 0.10389 0.01384 0.03941 0.01515 AFIX 23 H11A 2 0.557993 1.083664 0.339982 11.00000 -1.20000 H11B 2 0.522576 0.980685 0.323958 11.00000 -1.20000 AFIX 0 C12 1 0.583723 1.013218 0.258412 11.00000 0.08229 0.06514 = 0.07428 0.01229 0.02035 0.01911 AFIX 33 H12A 2 0.534850 1.035052 0.212149 11.00000 -1.20000 H12B 2 0.630129 1.052041 0.265871 11.00000 -1.20000 H12C 2 0.594685 0.948983 0.249834 11.00000 -1.20000 AFIX 0 C23 1 0.746158 0.478485 0.312112 11.00000 0.08138 0.05422 = 0.13900 -0.03410 0.07842 -0.01140 AFIX 23 H23A 2 0.783579 0.516517 0.299895 11.00000 -1.20000 H23B 2 0.761466 0.412859 0.312167 11.00000 -1.20000 AFIX 0 C24 1 0.659030 0.492574 0.246072 11.00000 0.10260 0.06961 = 0.07931 -0.02051 0.05133 -0.02020 AFIX 33 H24A 2 0.656210 0.475079 0.194860 11.00000 -1.20000 H24B 2 0.621579 0.453924 0.256757 11.00000 -1.20000 H24C 2 0.643719 0.557707 0.244470 11.00000 -1.20000 AFIX 0 HKLF 4 REM PR3R REM R1 = 0.0459 for 3303 Fo > 4sig(Fo) and 0.0492 for all 3726 data REM 271 parameters refined using 0 restraints END WGHT 0.0730 1.7847 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.351, deepest hole -0.254, 1-sigma level 0.051 Q1 1 0.6204 1.0409 0.3211 11.00000 0.05 0.35 Q2 1 1.1068 0.6973 0.4307 11.00000 0.05 0.35 Q3 1 1.1029 0.7011 0.3093 11.00000 0.05 0.24 Q4 1 0.2991 0.8082 0.3557 11.00000 0.05 0.23 Q5 1 0.2853 0.8060 0.4682 11.00000 0.05 0.21 Q6 1 1.0125 0.6888 0.4279 11.00000 0.05 0.20 Q7 1 0.5347 0.8049 0.4613 11.00000 0.05 0.19 Q8 1 0.3054 0.7473 0.4280 11.00000 0.05 0.18 Q9 1 0.5313 0.8506 0.4257 11.00000 0.05 0.18 Q10 1 0.6395 0.7550 0.4072 11.00000 0.05 0.18 Q11 1 0.3972 0.7463 0.4047 11.00000 0.05 0.18 Q12 1 0.7589 0.7378 0.3936 11.00000 0.05 0.18 Q13 1 0.7973 0.9355 0.3387 11.00000 0.05 0.17 Q14 1 0.7518 0.5601 0.4068 11.00000 0.05 0.17 Q15 1 0.7413 0.6126 0.4560 11.00000 0.05 0.16 Q16 1 0.6140 0.5589 0.4698 11.00000 0.05 0.16 Q17 1 0.7493 0.8040 0.4102 11.00000 0.05 0.16 Q18 1 0.8644 0.6943 0.3458 11.00000 0.05 0.15 Q19 1 0.9355 0.7607 0.2613 11.00000 0.05 0.15 Q20 1 0.6933 0.4572 0.3077 11.00000 0.05 0.15 Q21 1 0.7500 0.4983 0.5000 10.50000 0.05 0.15 Q22 1 0.3893 0.7954 0.3654 11.00000 0.05 0.15 Q23 1 0.6627 0.8668 0.4452 11.00000 0.05 0.14 Q24 1 0.7383 0.7592 0.4544 11.00000 0.05 0.14 Q25 1 0.6454 0.6149 0.4514 11.00000 0.05 0.14 ; _shelx_res_checksum 92239 _shelx_hkl_file ; 0 0 2 933.10 48.92 0 0 4 9999.00 523.07 0 0 4 9990.03 522.99 0 0 6 3879.92 200.29 0 0 6 3741.53 200.43 0 0 8 418.60 21.57 0 0 8 382.48 21.73 0 0 10 675.57 37.57 0 0 10 719.75 37.30 0 0 -12 96.48 5.32 0 0 -14 334.64 17.82 0 0 -16 92.16 5.10 0 0 -16 86.36 5.08 0 0 -16 94.04 5.07 0 0 -18 7.02 0.64 0 0 -18 9.50 0.69 0 1 -1 0.08 0.05 0 -1 1 0.07 0.02 0 -1 1 0.07 0.05 0 1 3 49.91 2.85 0 -1 3 50.83 2.75 0 1 5 39.17 2.35 0 -1 5 38.26 2.23 0 1 7 0.18 0.15 0 -1 7 0.06 0.10 0 -1 7 0.04 0.13 0 1 9 -0.04 0.13 0 1 9 -0.05 0.16 0 -1 9 0.20 0.21 0 -1 9 0.11 0.11 0 1 -11 1.25 0.23 0 1 -13 5.80 0.55 0 1 -15 17.82 1.23 0 1 -15 16.72 1.21 0 1 -15 16.93 1.20 0 1 -17 3.11 0.39 0 1 -17 3.38 0.40 0 1 -17 3.02 0.40 0 -1 -17 2.83 0.36 0 -1 -17 3.53 0.40 0 1 -19 1.23 0.21 0 1 -19 1.74 0.25 0 -1 -19 1.07 0.20 0 2 0 2029.25 110.08 0 -2 0 2173.35 110.08 0 2 2 564.59 28.99 0 2 -2 549.55 29.10 0 -2 2 533.18 29.07 0 2 4 3525.39 158.50 0 -2 4 3639.48 158.24 0 -2 4 3313.38 158.51 0 2 6 34.95 2.27 0 2 6 35.87 1.98 0 -2 6 35.36 2.05 0 2 8 84.14 5.12 0 2 8 86.12 5.09 0 -2 8 88.66 4.85 0 -2 8 85.93 5.19 0 2 10 26.64 1.98 0 2 10 24.94 2.03 0 -2 10 25.59 2.10 0 2 -12 15.62 1.09 0 2 -14 3.59 0.44 0 2 -14 3.52 0.44 0 2 -14 3.65 0.44 0 2 -16 9.78 0.78 0 2 -16 8.98 0.78 0 2 -16 8.70 0.76 0 -2 -16 8.71 0.72 0 2 -18 9.11 0.74 0 2 -18 10.19 0.76 0 2 -18 9.26 0.72 0 -2 -18 8.97 0.70 0 2 -20 0.22 0.10 0 3 -1 17.12 0.97 0 3 1 16.92 1.00 0 3 -1 16.15 1.06 0 -3 1 16.66 1.05 0 -3 -1 16.31 1.01 0 3 3 321.73 17.65 0 3 -3 334.83 17.70 0 3 3 335.77 17.54 0 -3 3 330.91 17.65 0 3 5 1.42 0.24 0 -3 5 1.26 0.13 0 -3 5 1.27 0.11 0 -3 5 1.74 0.33 0 3 7 148.72 8.28 0 -3 7 146.02 8.34 0 3 9 0.38 0.23 0 3 9 0.24 0.20 0 3 -11 65.26 3.85 0 3 -11 71.70 3.87 0 3 -13 0.26 0.16 0 3 -13 0.46 0.19 0 3 -13 0.28 0.18 0 3 -13 0.10 0.17 0 3 -15 10.35 0.86 0 3 -15 10.71 0.86 0 3 -15 10.73 0.88 0 3 -17 27.29 1.83 0 3 -17 31.35 1.87 0 3 -17 30.55 1.88 0 3 -19 0.24 0.13 0 3 -19 0.52 0.17 0 4 0 954.19 50.56 0 4 0 934.64 50.59 0 -4 0 997.64 50.57 0 4 2 2127.73 113.94 0 4 -2 2252.20 113.96 0 4 2 2204.63 114.09 0 4 -2 2246.73 114.12 0 -4 -2 2051.22 113.95 0 -4 2 2239.85 114.06 0 -4 -2 2179.57 113.88 0 4 4 225.31 12.09 0 4 4 224.67 12.27 0 -4 4 229.05 12.27 0 4 6 219.05 11.76 0 -4 6 215.42 11.98 0 4 8 55.95 3.36 0 4 8 46.10 3.18 0 -4 8 51.94 3.39 0 4 -10 28.66 1.78 0 -4 -10 29.15 1.79 0 4 -12 33.76 2.24 0 4 -12 39.92 2.26 0 4 -12 37.25 2.22 0 4 -14 0.39 0.21 0 4 -14 0.29 0.19 0 4 -14 0.26 0.22 0 4 -14 0.73 0.25 0 4 -14 0.44 0.21 0 4 -16 2.35 0.38 0 4 -16 1.72 0.32 0 4 -16 2.11 0.35 0 4 -18 0.12 0.14 0 4 -18 0.17 0.17 0 4 -18 0.15 0.16 0 5 1 29.34 1.81 0 5 1 30.54 1.89 0 5 -1 30.13 1.76 0 5 -1 28.37 1.89 0 5 -1 31.28 1.89 0 -5 1 32.67 1.86 0 -5 -1 30.31 1.82 0 5 3 151.66 8.29 0 5 3 147.32 8.07 0 5 -3 156.94 8.36 0 -5 3 147.85 8.22 0 5 5 21.17 1.55 0 -5 5 19.22 1.50 0 -5 7 416.58 22.53 0 5 -9 43.17 2.39 0 5 -9 40.07 2.40 0 5 -9 40.49 2.37 0 5 -9 40.10 2.37 0 5 -11 62.85 3.78 0 5 -11 70.02 3.77 0 5 -11 67.97 3.77 0 -5 -11 63.48 3.77 0 5 -13 59.13 3.84 0 5 -13 75.68 3.89 0 5 -15 6.23 0.61 0 5 -15 6.19 0.57 0 5 -15 6.50 0.60 0 5 -17 8.13 0.69 0 5 -17 8.76 0.71 0 5 -19 0.24 0.15 0 5 -19 0.37 0.13 0 6 0 130.20 7.48 0 6 0 135.44 7.43 0 -6 0 144.00 7.47 0 6 2 9.57 0.80 0 6 -2 7.58 0.50 0 6 -2 7.72 0.76 0 6 2 8.24 0.65 0 6 -2 6.87 0.49 0 6 -2 8.58 0.69 0 -6 -2 9.18 0.62 0 -6 -2 7.18 0.62 0 -6 2 9.65 0.75 0 6 4 59.55 3.60 0 -6 4 57.22 3.52 0 6 6 224.65 12.33 0 -6 6 219.89 12.29 0 6 -8 3.25 0.35 0 -6 8 3.97 0.66 0 6 -10 4.07 0.41 0 6 -10 3.36 0.38 0 6 -10 3.20 0.38 0 6 -10 3.12 0.40 0 -6 -10 3.06 0.38 0 6 -12 8.18 0.73 0 6 -12 8.75 0.78 0 6 -12 8.65 0.73 0 6 -12 9.19 0.75 0 6 -14 9.38 0.77 0 6 -14 10.05 0.79 0 6 -16 3.80 0.45 0 6 -16 3.13 0.38 0 6 -18 2.33 0.29 0 7 1 6.97 0.68 0 7 -1 7.18 0.72 0 -7 -1 7.19 0.64 0 -7 1 7.27 0.67 0 7 3 7.71 0.79 0 -7 3 7.41 0.74 0 7 5 32.87 2.29 0 -7 5 30.69 2.18 0 7 -7 67.48 3.97 0 7 -7 72.81 4.02 0 7 -9 0.27 0.13 0 7 -9 0.55 0.20 0 7 -9 0.27 0.14 0 7 -9 0.35 0.15 0 7 -11 21.98 1.40 0 7 -11 20.86 1.46 0 7 -11 21.76 1.41 0 7 -11 19.37 1.39 0 7 -13 4.23 0.48 0 7 -13 3.78 0.47 0 7 -13 3.91 0.51 0 7 -13 4.86 0.50 0 7 -15 2.57 0.40 0 7 -15 3.02 0.40 0 7 -15 4.17 0.47 0 7 -15 3.18 0.40 0 7 -17 -0.03 0.14 0 7 -17 -0.18 0.19 0 8 0 75.59 4.57 0 8 2 19.57 1.50 0 8 4 188.60 10.53 0 -8 4 187.14 10.40 0 8 -6 92.26 4.92 0 8 -6 81.19 4.85 0 8 -8 54.79 3.27 0 8 -8 59.40 3.23 0 8 -8 49.42 3.18 0 8 -8 63.55 3.22 0 8 -10 121.90 6.73 0 8 -10 123.26 6.71 0 8 -12 7.33 0.67 0 8 -12 7.57 0.72 0 8 -12 7.21 0.65 0 8 -14 0.63 0.23 0 8 -14 0.45 0.20 0 8 -14 0.15 0.17 0 8 -16 0.43 0.17 0 8 -16 0.41 0.20 0 8 -16 0.68 0.20 0 8 -18 0.59 0.15 0 8 -18 0.41 0.12 0 9 1 0.02 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0.59 0.17 19 -3 -12 0.57 0.20 -19 -3 12 0.93 0.21 -19 3 10 26.44 1.66 19 3 -10 27.69 1.73 -19 -3 10 24.83 1.66 -19 3 8 4.10 0.42 -19 -3 8 5.16 0.44 19 -3 -8 5.39 0.50 -19 -3 8 4.14 0.43 -19 3 6 9.34 0.72 -19 -3 6 10.38 0.69 19 -3 -6 9.93 0.76 -19 -3 6 10.02 0.76 -19 3 4 3.98 0.37 19 -3 -4 3.26 0.35 -19 -3 4 3.38 0.38 -19 3 2 0.24 0.13 19 -3 -2 0.19 0.09 -19 -3 2 0.17 0.13 -19 3 0 0.52 0.13 -19 3 0 0.52 0.12 -19 -3 0 0.39 0.10 -19 -3 0 0.60 0.12 19 4 -17 0.26 0.16 -19 -4 17 0.23 0.10 19 -4 -15 2.13 0.27 -19 4 13 4.48 0.39 -19 -4 13 5.55 0.44 -19 4 11 34.76 2.09 19 4 -11 36.70 2.13 -19 -4 11 33.17 2.09 -19 4 9 13.49 0.91 19 -4 -9 13.39 0.97 -19 -4 9 15.39 0.95 -19 -4 9 12.08 0.91 -19 4 7 67.45 3.83 -19 -4 7 70.28 3.80 19 -4 -7 70.21 3.89 -19 -4 7 68.54 3.88 19 -4 -5 0.49 0.15 -19 -4 5 0.23 0.13 -19 4 3 41.03 2.15 -19 -4 3 33.26 2.14 19 -4 -3 37.12 2.10 -19 4 1 4.74 0.39 -19 4 1 4.99 0.40 -19 -4 1 5.11 0.40 -19 -4 1 5.19 0.42 -19 4 -1 3.00 0.27 -19 -4 -1 4.29 0.29 -19 -5 18 0.95 0.12 19 5 -16 -0.09 0.15 19 -5 -16 0.02 0.08 -19 -5 16 0.08 0.09 -19 -5 14 1.07 0.17 19 -5 -14 0.76 0.19 -19 5 12 0.02 0.08 -19 -5 12 0.14 0.11 -19 -5 12 -0.03 0.09 19 5 -10 0.79 0.17 -19 5 10 0.74 0.16 -19 -5 10 0.98 0.19 -19 -5 10 0.41 0.14 -19 5 8 0.73 0.17 19 -5 -8 0.81 0.19 -19 -5 8 0.72 0.15 -19 -5 8 0.60 0.17 -19 5 6 -0.08 0.13 19 -5 -6 0.01 0.11 -19 -5 6 -0.08 0.12 19 -5 -4 1.28 0.18 -19 5 2 0.01 0.08 -19 5 2 0.01 0.09 -19 -5 2 0.02 0.10 -19 5 0 0.36 0.10 -19 5 0 0.34 0.08 -19 -5 0 0.49 0.10 -19 -6 17 2.41 0.21 -19 -6 15 -0.03 0.08 19 -6 -15 0.04 0.11 -19 -6 13 1.42 0.19 19 -6 -13 1.18 0.21 -19 6 11 1.43 0.18 -19 -6 11 1.48 0.20 -19 -6 11 1.12 0.19 -19 6 9 1.63 0.22 19 6 -9 1.97 0.24 -19 -6 9 1.71 0.21 -19 -6 9 1.57 0.24 -19 6 7 21.94 1.35 -19 -6 7 22.81 1.39 -19 6 5 0.21 0.12 -19 -6 3 26.19 1.54 -19 6 1 0.35 0.10 -19 -6 1 0.37 0.10 -19 -6 1 0.41 0.10 -19 -7 16 2.51 0.21 -19 -7 14 16.23 0.99 19 -7 -14 18.10 1.07 -19 -7 12 -0.04 0.09 -19 -7 12 0.03 0.08 -19 7 10 11.54 0.76 -19 -7 10 12.36 0.81 19 -7 -10 13.34 0.85 -19 7 8 1.66 0.20 -19 -7 8 1.47 0.22 -19 7 6 4.13 0.35 -19 -7 6 4.03 0.36 19 -7 -6 3.51 0.32 -19 7 4 4.47 0.37 -19 -7 4 4.66 0.39 -19 -7 2 -0.01 0.06 19 -8 -13 0.70 0.15 19 -8 -11 12.70 0.74 -19 -8 11 9.21 0.66 -19 8 9 2.53 0.23 -19 -8 9 2.98 0.28 19 -8 -9 2.78 0.28 -19 8 7 9.56 0.61 19 -8 -7 8.30 0.61 -19 8 5 -0.02 0.07 -19 -8 5 -0.03 0.08 -19 8 3 1.36 0.15 19 -9 -12 0.05 0.07 19 -9 -10 11.83 0.67 -19 -9 10 8.97 0.63 -19 -9 8 0.89 0.14 -19 -9 6 3.14 0.26 -20 0 16 16.97 1.03 -20 0 14 13.11 0.86 20 0 -12 0.82 0.20 -20 0 12 0.63 0.17 20 0 -10 0.16 0.13 -20 0 10 0.12 0.12 -20 0 8 -0.01 0.11 -20 0 8 0.08 0.10 -20 0 6 4.47 0.39 20 0 -6 5.11 0.46 -20 0 6 4.19 0.41 -20 0 4 2.08 0.23 20 0 -4 2.47 0.28 20 0 -2 4.23 0.35 -20 0 0 2.87 0.24 -20 1 17 13.55 0.88 -20 -1 17 18.46 0.94 -20 1 15 0.33 0.12 -20 -1 15 0.37 0.14 20 1 -13 41.24 2.46 -20 1 13 42.13 2.42 20 -1 -13 43.48 2.49 -20 -1 13 44.51 2.45 -20 1 11 8.82 0.65 20 1 -11 8.94 0.70 20 -1 -11 9.84 0.73 -20 -1 11 9.00 0.66 -20 1 9 11.51 0.80 20 1 -9 13.52 0.90 -20 -1 9 12.64 0.82 -20 -1 9 10.76 0.79 -20 1 7 54.88 2.98 -20 -1 7 53.78 2.96 20 -1 -7 56.70 3.05 -20 -1 7 47.79 2.98 -20 1 5 2.42 0.26 20 1 -5 2.12 0.28 20 -1 -5 1.98 0.27 -20 -1 5 1.92 0.23 -20 -1 5 2.23 0.27 -20 1 3 36.31 2.04 20 1 -3 37.83 2.09 20 -1 -3 34.76 2.06 20 1 -1 0.40 0.09 -20 -1 1 0.44 0.11 -20 -2 18 1.96 0.19 -20 2 16 7.90 0.57 -20 -2 16 12.11 0.68 -20 2 14 19.34 1.16 -20 2 12 0.54 0.14 20 2 -12 0.56 0.16 20 -2 -12 0.79 0.20 -20 -2 12 0.70 0.18 -20 2 10 12.62 0.82 20 2 -10 12.89 0.88 -20 -2 10 12.92 0.83 -20 -2 10 10.50 0.79 20 2 -8 0.12 0.14 20 -2 -8 -0.07 0.13 -20 -2 8 0.11 0.11 -20 -2 8 0.01 0.12 -20 2 6 0.52 0.16 20 -2 -6 0.57 0.17 -20 -2 6 0.53 0.13 -20 -2 6 0.55 0.17 -20 2 4 0.46 0.13 20 -2 -4 0.31 0.12 -20 -2 4 0.41 0.14 20 2 -2 5.09 0.39 -20 2 2 5.10 0.37 -20 2 2 4.90 0.39 -20 -2 2 4.36 0.34 -20 -3 17 18.91 1.12 -20 3 15 2.99 0.25 -20 3 13 36.96 2.33 -20 -3 13 52.62 2.47 20 3 -11 37.80 2.16 -20 -3 11 41.67 2.15 -20 3 9 54.00 3.06 20 3 -9 55.94 3.12 20 -3 -9 58.70 3.14 -20 -3 9 56.71 3.05 -20 -3 9 50.68 3.06 -20 -3 7 36.96 2.08 20 -3 -7 38.61 2.17 -20 -3 7 35.44 2.14 -20 3 5 8.17 0.59 -20 -3 5 8.08 0.61 20 -3 -5 8.53 0.60 -20 3 3 25.34 1.43 -20 -3 3 23.24 1.39 20 -3 -3 22.25 1.39 -20 3 1 0.31 0.08 20 3 -1 0.22 0.08 20 -4 -16 3.80 0.31 -20 4 14 0.79 0.13 -20 -4 14 1.45 0.20 -20 4 12 0.42 0.12 -20 -4 12 0.56 0.17 -20 4 10 0.21 0.11 20 4 -10 0.25 0.13 20 -4 -10 0.24 0.15 -20 -4 10 0.32 0.12 -20 -4 10 0.05 0.08 20 4 -8 0.73 0.17 -20 4 8 0.89 0.17 20 -4 -8 0.81 0.18 -20 -4 8 0.77 0.14 -20 -4 8 0.59 0.15 20 -4 -6 0.29 0.13 -20 -4 6 0.31 0.13 -20 4 4 0.05 0.08 -20 4 4 0.02 0.09 20 -4 -4 0.07 0.06 -20 4 2 0.13 0.07 -20 4 2 0.05 0.07 -20 -4 2 0.06 0.07 -20 -5 15 0.83 0.14 20 -5 -15 0.63 0.14 -20 5 13 79.19 4.88 -20 -5 13 121.64 5.01 -20 5 11 29.16 1.76 -20 -5 11 28.72 1.76 -20 5 9 43.29 2.51 20 5 -9 49.63 2.56 -20 -5 9 45.88 2.48 -20 -5 9 42.04 2.53 -20 5 7 108.67 5.82 -20 -5 7 107.39 5.85 -20 5 5 4.64 0.37 -20 -5 5 6.09 0.44 -20 5 3 64.39 3.30 -20 -5 3 62.72 3.31 -20 -5 3 55.90 3.28 -20 -6 14 2.85 0.26 20 -6 -14 2.56 0.27 -20 6 12 1.75 0.18 20 -6 -12 2.22 0.26 -20 -6 12 2.27 0.21 -20 6 10 0.13 0.08 -20 -6 10 0.05 0.06 -20 -6 10 -0.02 0.08 -20 6 8 0.22 0.10 20 6 -8 0.09 0.09 -20 -6 8 0.27 0.12 -20 6 6 0.42 0.11 -20 -6 6 0.41 0.12 -20 -6 4 0.92 0.14 20 -7 -13 23.53 1.37 20 -7 -11 12.34 0.71 -20 -7 11 9.21 0.63 -20 7 9 22.79 1.38 -20 -7 9 25.25 1.42 20 -7 -9 26.17 1.43 -20 7 7 18.39 0.99 -20 -7 7 21.14 1.04 -20 7 5 1.52 0.16 -20 -7 5 1.43 0.17 20 -8 -10 7.87 0.52 -20 -8 8 0.04 0.06 -21 0 15 0.04 0.07 21 0 -13 -0.02 0.10 -21 0 13 0.02 0.08 21 0 -11 -0.01 0.10 -21 0 11 -0.02 0.10 21 0 -9 0.16 0.13 -21 0 9 0.06 0.10 21 0 -7 0.04 0.10 -21 0 7 -0.03 0.09 21 0 -5 0.02 0.09 -21 0 5 0.01 0.06 -21 0 3 -0.01 0.06 21 0 -3 0.03 0.06 -21 1 16 0.03 0.05 -21 -1 16 0.08 0.07 -21 1 14 0.18 0.09 -21 -1 14 0.16 0.10 -21 1 12 1.88 0.22 21 1 -12 2.30 0.26 21 -1 -12 2.14 0.27 -21 -1 12 2.26 0.23 21 1 -10 15.94 1.04 21 -1 -10 17.20 1.06 -21 -1 10 15.26 0.98 -21 1 8 0.97 0.16 21 1 -8 1.06 0.19 21 -1 -8 0.99 0.19 -21 -1 8 0.79 0.14 -21 1 6 55.88 2.99 21 1 -6 58.47 3.05 21 -1 -6 55.19 3.03 -21 -1 6 50.55 2.96 -21 1 4 5.95 0.41 21 1 -4 6.01 0.44 21 -1 -4 5.97 0.43 -21 2 15 0.01 0.06 -21 -2 15 -0.03 0.08 21 -2 -15 -0.02 0.07 -21 2 13 17.12 1.02 21 2 -13 15.90 1.03 -21 -2 13 18.37 1.04 -21 2 11 0.72 0.14 21 2 -11 0.81 0.17 21 -2 -11 0.76 0.18 -21 -2 11 0.65 0.13 21 2 -9 8.61 0.61 21 -2 -9 9.06 0.62 -21 -2 9 8.33 0.55 21 2 -7 1.65 0.22 -21 2 7 1.40 0.18 21 -2 -7 1.14 0.20 -21 -2 7 1.07 0.15 -21 -2 7 1.22 0.18 -21 2 5 2.22 0.21 21 2 -5 2.02 0.23 21 -2 -5 1.65 0.20 21 2 -3 0.04 0.06 -21 -3 16 7.76 0.50 -21 3 14 0.07 0.07 -21 -3 14 0.17 0.09 -21 3 12 8.19 0.56 21 3 -12 8.16 0.57 -21 -3 12 9.22 0.58 -21 3 10 15.14 0.93 21 3 -10 16.30 0.97 21 -3 -10 17.31 1.01 -21 -3 10 15.94 0.92 21 3 -8 0.63 0.15 21 -3 -8 0.62 0.15 -21 -3 8 0.46 0.10 -21 -3 8 0.65 0.13 21 3 -6 34.15 1.89 -21 3 6 32.56 1.85 21 -3 -6 34.38 1.87 -21 -3 6 30.36 1.86 21 3 -4 10.47 0.57 -21 3 4 8.75 0.53 -21 -4 15 2.08 0.19 -21 4 13 64.79 3.81 -21 -4 13 80.13 3.85 -21 4 11 4.66 0.36 21 4 -11 4.47 0.35 -21 -4 11 4.77 0.34 -21 4 9 52.93 2.79 21 4 -9 54.42 2.81 -21 -4 9 48.09 2.73 -21 -4 9 48.64 2.78 21 4 -7 13.72 0.85 -21 -4 7 12.80 0.83 21 4 -5 7.08 0.48 -21 4 5 6.46 0.45 -21 -4 5 6.52 0.46 -21 -5 14 4.03 0.29 21 -5 -14 4.03 0.32 -21 5 12 0.37 0.08 -21 -5 12 0.32 0.08 21 -5 -12 0.30 0.11 -21 5 10 2.47 0.22 -21 -5 10 2.18 0.21 -21 5 8 1.01 0.14 21 5 -8 0.96 0.14 -21 -5 8 0.95 0.14 21 5 -6 5.25 0.38 -21 5 6 5.03 0.37 -21 -5 6 4.98 0.37 21 -6 -11 3.96 0.32 -21 6 9 14.42 0.78 21 -6 -9 11.50 0.78 -22 0 14 22.01 1.24 -22 0 10 67.90 3.78 22 0 -10 73.67 3.84 -22 0 8 52.03 2.82 22 0 -6 77.04 4.14 -22 1 13 4.60 0.33 22 1 -11 0.11 0.09 22 -1 -11 -0.02 0.10 -22 -1 11 0.09 0.08 -22 1 9 3.38 0.27 22 1 -9 4.02 0.32 -22 -1 9 3.02 0.26 -22 1 7 0.79 0.11 22 -1 -7 0.67 0.12 -22 -2 14 1.24 0.13 -22 2 12 14.93 0.90 -22 -2 12 15.81 0.90 22 2 -10 24.87 1.34 -22 -2 10 21.85 1.29 -22 2 8 11.07 0.69 22 2 -8 12.03 0.73 22 -2 -8 11.20 0.72 -22 3 11 -0.04 0.06 -22 -3 11 0.01 0.05 22 3 -9 1.20 0.15 -22 3 9 1.40 0.15 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 27192 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Cl2 Cl 1.09987(3) 0.69715(4) 0.37559(4) 0.0741(2) Uani 1 1 d . . Cl1 Cl 0.28990(4) 0.80135(5) 0.40624(5) 0.0835(3) Uani 1 1 d . . O2 O 0.61381(7) 0.56997(9) 0.40564(8) 0.0502(3) Uani 1 1 d . . O1 O 0.78586(7) 0.92002(9) 0.39584(8) 0.0484(3) Uani 1 1 d . . N1 N 0.66462(8) 0.88704(10) 0.40571(9) 0.0409(3) Uani 1 1 d . . N2 N 0.73845(8) 0.60303(10) 0.40191(9) 0.0414(3) Uani 1 1 d . . C13 C 0.73222(10) 0.76026(12) 0.39082(10) 0.0384(4) Uani 1 1 d . . C1 C 0.65940(10) 0.72974(12) 0.39498(10) 0.0387(4) Uani 1 1 d . . C3 C 0.73653(10) 0.86205(12) 0.39689(10) 0.0400(4) Uani 1 1 d . . C14 C 0.77985(10) 0.68257(12) 0.39504(10) 0.0381(4) Uani 1 1 d . . C2 C 0.61842(10) 0.80749(12) 0.40354(10) 0.0385(4) Uani 1 1 d . . C15 C 0.66158(10) 0.62788(12) 0.40137(10) 0.0410(4) Uani 1 1 d . . C16 C 0.85934(10) 0.68187(12) 0.39177(10) 0.0394(4) Uani 1 1 d . . C4 C 0.53907(10) 0.80911(12) 0.40703(10) 0.0404(4) Uani 1 1 d . . C21 C 0.86780(10) 0.74238(13) 0.33682(11) 0.0439(4) Uani 1 1 d . . H21 H 0.8234 0.7804 0.3034 0.053 Uiso 1 1 calc R U C5 C 0.52570(11) 0.86105(13) 0.46375(11) 0.0453(4) Uani 1 1 d . . H5 H 0.5682 0.8979 0.5017 0.054 Uiso 1 1 calc R U C6 C 0.44916(12) 0.85795(13) 0.46381(12) 0.0517(5) Uani 1 1 d . . H6 H 0.4403 0.8923 0.5019 0.062 Uiso 1 1 calc R U C17 C 0.92722(11) 0.62723(13) 0.44313(12) 0.0480(4) Uani 1 1 d . . H17 H 0.9229 0.5876 0.4810 0.058 Uiso 1 1 calc R U C18 C 1.00104(11) 0.63185(13) 0.43788(13) 0.0534(5) Uani 1 1 d . . H18 H 1.0462 0.5953 0.4720 0.064 Uiso 1 1 calc R U C20 C 0.94142(11) 0.74673(14) 0.33120(12) 0.0485(4) Uani 1 1 d . . H20 H 0.9465 0.7866 0.2939 0.058 Uiso 1 1 calc R U C9 C 0.47498(11) 0.75319(14) 0.35170(12) 0.0492(4) Uani 1 1 d . . H9 H 0.4839 0.7170 0.3145 0.059 Uiso 1 1 calc R U C19 C 1.00702(11) 0.69083(13) 0.38198(13) 0.0496(5) Uani 1 1 d . . C10 C 0.64317(12) 0.98629(13) 0.40812(12) 0.0508(4) Uani 1 1 d . . H10A H 0.6908 1.0251 0.4173 0.061 Uiso 1 1 calc R U H10B H 0.6313 0.9955 0.4536 0.061 Uiso 1 1 calc R U C8 C 0.39847(12) 0.75072(15) 0.35112(14) 0.0568(5) Uani 1 1 d . . H8 H 0.3558 0.7138 0.3135 0.068 Uiso 1 1 calc R U C7 C 0.38645(12) 0.80374(13) 0.40712(14) 0.0534(5) Uani 1 1 d . . C22 C 0.75801(11) 0.50389(13) 0.39579(14) 0.0559(5) Uani 1 1 d . . H22A H 0.7227 0.4640 0.4094 0.067 Uiso 1 1 calc R U H22B H 0.8151 0.4916 0.4348 0.067 Uiso 1 1 calc R U C11 C 0.57041(13) 1.01882(16) 0.33263(16) 0.0681(6) Uani 1 1 d . . H11A H 0.5580 1.0837 0.3400 0.082 Uiso 1 1 calc R U H11B H 0.5226 0.9807 0.3240 0.082 Uiso 1 1 calc R U C12 C 0.58372(17) 1.01322(18) 0.25841(15) 0.0798(7) Uani 1 1 d . . H12A H 0.5349 1.0351 0.2121 0.096 Uiso 1 1 calc R U H12B H 0.6301 1.0520 0.2659 0.096 Uiso 1 1 calc R U H12C H 0.5947 0.9490 0.2498 0.096 Uiso 1 1 calc R U C23 C 0.74616(16) 0.47849(17) 0.31211(19) 0.0807(8) Uani 1 1 d . . H23A H 0.7836 0.5165 0.2999 0.097 Uiso 1 1 calc R U H23B H 0.7615 0.4129 0.3122 0.097 Uiso 1 1 calc R U C24 C 0.65903(17) 0.4926(2) 0.24607(16) 0.0801(7) Uani 1 1 d . . H24A H 0.6562 0.4751 0.1949 0.096 Uiso 1 1 calc R U H24B H 0.6216 0.4539 0.2568 0.096 Uiso 1 1 calc R U H24C H 0.6437 0.5577 0.2445 0.096 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl2 0.0489(3) 0.0718(4) 0.1202(5) 0.0029(3) 0.0548(3) 0.0063(2) Cl1 0.0538(4) 0.0818(5) 0.1386(6) -0.0046(4) 0.0645(4) 0.0011(3) O2 0.0404(7) 0.0434(7) 0.0712(8) -0.0067(6) 0.0294(6) -0.0063(5) O1 0.0446(7) 0.0427(7) 0.0671(8) 0.0028(6) 0.0334(6) -0.0002(5) N1 0.0389(7) 0.0378(7) 0.0524(8) 0.0000(6) 0.0263(6) 0.0043(6) N2 0.0337(7) 0.0362(7) 0.0550(8) -0.0036(6) 0.0208(6) 0.0020(5) C13 0.0331(8) 0.0416(9) 0.0439(8) -0.0005(7) 0.0204(7) 0.0032(7) C1 0.0324(8) 0.0417(9) 0.0440(8) -0.0032(7) 0.0191(7) 0.0017(7) C3 0.0356(8) 0.0433(9) 0.0443(8) 0.0029(7) 0.0210(7) 0.0052(7) C14 0.0317(8) 0.0416(9) 0.0403(8) -0.0014(6) 0.0157(6) 0.0018(6) C2 0.0347(8) 0.0424(9) 0.0400(8) -0.0008(6) 0.0186(7) 0.0032(6) C15 0.0339(8) 0.0443(9) 0.0457(9) -0.0051(7) 0.0188(7) 0.0006(7) C16 0.0328(8) 0.0396(9) 0.0471(9) -0.0055(7) 0.0193(7) 0.0023(6) C4 0.0362(9) 0.0406(9) 0.0485(9) 0.0031(7) 0.0228(7) 0.0057(6) C21 0.0357(8) 0.0467(10) 0.0494(9) -0.0016(7) 0.0195(7) 0.0039(7) C5 0.0425(9) 0.0455(10) 0.0531(9) -0.0011(7) 0.0263(8) 0.0036(7) C6 0.0535(10) 0.0491(10) 0.0670(11) 0.0019(9) 0.0402(9) 0.0094(8) C17 0.0375(8) 0.0452(10) 0.0622(11) 0.0039(8) 0.0235(8) 0.0052(7) C18 0.0356(9) 0.0472(10) 0.0750(12) 0.0033(9) 0.0233(8) 0.0086(7) C20 0.0443(9) 0.0516(11) 0.0564(10) -0.0020(8) 0.0289(8) -0.0006(8) C9 0.0437(9) 0.0503(10) 0.0594(11) -0.0083(8) 0.0286(8) -0.0008(8) C19 0.0382(9) 0.0474(10) 0.0700(12) -0.0098(8) 0.0305(9) 0.0001(7) C10 0.0574(11) 0.0381(9) 0.0717(12) -0.0014(8) 0.0424(10) 0.0060(8) C8 0.0416(10) 0.0569(12) 0.0741(13) -0.0070(10) 0.0283(9) -0.0052(8) C7 0.0435(10) 0.0498(11) 0.0786(13) 0.0090(9) 0.0380(10) 0.0075(8) C22 0.0397(9) 0.0367(9) 0.0891(14) -0.0027(9) 0.0274(9) 0.0039(7) C11 0.0534(12) 0.0510(12) 0.1039(18) 0.0138(11) 0.0394(12) 0.0152(9) C12 0.0823(16) 0.0651(15) 0.0743(15) 0.0123(12) 0.0203(12) 0.0191(13) C23 0.0814(16) 0.0542(13) 0.139(2) -0.0341(14) 0.0784(17) -0.0114(12) C24 0.103(2) 0.0696(16) 0.0793(15) -0.0205(12) 0.0513(15) -0.0202(14) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; Cl Cl 0.3639 0.7018 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0492 0.0322 ; International Tables for Crystallography (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 C2 N1 C3 111.27(13) C2 N1 C10 127.83(14) C3 N1 C10 120.62(14) C14 N2 C15 111.29(13) C14 N2 C22 127.57(14) C15 N2 C22 120.26(14) C14 C13 C1 109.01(15) C14 C13 C3 141.44(16) C1 C13 C3 108.50(14) C2 C1 C13 108.95(16) C2 C1 C15 141.64(16) C13 C1 C15 108.43(14) O1 C3 N1 123.17(15) O1 C3 C13 133.15(15) N1 C3 C13 103.67(13) C13 C14 N2 107.61(14) C13 C14 C16 127.09(15) N2 C14 C16 125.29(14) C1 C2 N1 107.60(15) C1 C2 C4 127.41(15) N1 C2 C4 124.96(14) O2 C15 N2 123.36(16) O2 C15 C1 133.00(15) N2 C15 C1 103.65(14) C21 C16 C17 118.94(16) C21 C16 C14 117.61(14) C17 C16 C14 123.38(16) C5 C4 C9 118.90(16) C5 C4 C2 123.57(15) C9 C4 C2 117.50(15) C20 C21 C16 120.90(16) C20 C21 H21 119.5 C16 C21 H21 119.5 C6 C5 C4 120.14(17) C6 C5 H5 119.9 C4 C5 H5 119.9 C7 C6 C5 119.56(17) C7 C6 H6 120.2 C5 C6 H6 120.2 C18 C17 C16 120.21(18) C18 C17 H17 119.9 C16 C17 H17 119.9 C19 C18 C17 119.52(17) C19 C18 H18 120.2 C17 C18 H18 120.2 C19 C20 C21 118.78(18) C19 C20 H20 120.6 C21 C20 H20 120.6 C8 C9 C4 121.04(17) C8 C9 H9 119.5 C4 C9 H9 119.5 C18 C19 C20 121.62(17) C18 C19 Cl2 119.60(14) C20 C19 Cl2 118.77(15) N1 C10 C11 113.63(17) N1 C10 H10A 108.8 C11 C10 H10A 108.8 N1 C10 H10B 108.8 C11 C10 H10B 108.8 H10A C10 H10B 107.7 C7 C8 C9 118.93(19) C7 C8 H8 120.5 C9 C8 H8 120.5 C6 C7 C8 121.40(17) C6 C7 Cl1 119.52(15) C8 C7 Cl1 119.09(16) N2 C22 C23 112.47(18) N2 C22 H22A 109.1 C23 C22 H22A 109.1 N2 C22 H22B 109.1 C23 C22 H22B 109.1 H22A C22 H22B 107.8 C10 C11 C12 113.63(18) C10 C11 H11A 108.8 C12 C11 H11A 108.8 C10 C11 H11B 108.8 C12 C11 H11B 108.8 H11A C11 H11B 107.7 C11 C12 H12A 109.5 C11 C12 H12B 109.5 H12A C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C24 C23 C22 114.15(18) C24 C23 H23A 108.7 C22 C23 H23A 108.7 C24 C23 H23B 108.7 C22 C23 H23B 108.7 H23A C23 H23B 107.6 C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl2 C19 1.7409(18) Cl1 C7 1.7412(19) O2 C15 1.221(2) O1 C3 1.220(2) N1 C2 1.393(2) N1 C3 1.429(2) N1 C10 1.465(2) N2 C14 1.391(2) N2 C15 1.431(2) N2 C22 1.465(2) C13 C14 1.378(2) C13 C1 1.423(2) C13 C3 1.446(2) C1 C2 1.377(2) C1 C15 1.447(2) C14 C16 1.468(2) C2 C4 1.468(2) C16 C21 1.393(3) C16 C17 1.396(2) C4 C5 1.392(2) C4 C9 1.393(3) C21 C20 1.385(2) C21 H21 0.9300 C5 C6 1.387(2) C5 H5 0.9300 C6 C7 1.376(3) C6 H6 0.9300 C17 C18 1.386(3) C17 H17 0.9300 C18 C19 1.374(3) C18 H18 0.9300 C20 C19 1.380(3) C20 H20 0.9300 C9 C8 1.381(3) C9 H9 0.9300 C10 C11 1.491(3) C10 H10A 0.9700 C10 H10B 0.9700 C8 C7 1.377(3) C8 H8 0.9300 C22 C23 1.510(3) C22 H22A 0.9700 C22 H22B 0.9700 C11 C12 1.504(4) C11 H11A 0.9700 C11 H11B 0.9700 C12 H12A 0.9600 C12 H12B 0.9600 C12 H12C 0.9600 C23 C24 1.505(4) C23 H23A 0.9700 C23 H23B 0.9700 C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 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 C14 C13 C1 C2 170.71(14) C3 C13 C1 C2 -0.16(19) C14 C13 C1 C15 -0.53(19) C3 C13 C1 C15 -171.39(14) C2 N1 C3 O1 178.98(16) C10 N1 C3 O1 4.5(2) C2 N1 C3 C13 -1.20(17) C10 N1 C3 C13 -175.67(15) C14 C13 C3 O1 14.5(4) C1 C13 C3 O1 -179.40(18) C14 C13 C3 N1 -165.3(2) C1 C13 C3 N1 0.81(17) C1 C13 C14 N2 -0.07(19) C3 C13 C14 N2 166.0(2) C1 C13 C14 C16 179.09(15) C3 C13 C14 C16 -14.9(3) C15 N2 C14 C13 0.66(19) C22 N2 C14 C13 169.80(17) C15 N2 C14 C16 -178.52(14) C22 N2 C14 C16 -9.4(3) C13 C1 C2 N1 -0.59(19) C15 C1 C2 N1 165.9(2) C13 C1 C2 C4 177.42(15) C15 C1 C2 C4 -16.1(3) C3 N1 C2 C1 1.15(19) C10 N1 C2 C1 175.12(16) C3 N1 C2 C4 -176.92(14) C10 N1 C2 C4 -3.0(3) C14 N2 C15 O2 179.04(16) C22 N2 C15 O2 9.0(3) C14 N2 C15 C1 -0.94(17) C22 N2 C15 C1 -171.00(16) C2 C1 C15 O2 14.3(4) C13 C1 C15 O2 -179.10(19) C2 C1 C15 N2 -165.7(2) C13 C1 C15 N2 0.87(17) C13 C14 C16 C21 -40.5(2) N2 C14 C16 C21 138.51(17) C13 C14 C16 C17 136.49(19) N2 C14 C16 C17 -44.5(2) C1 C2 C4 C5 134.32(19) N1 C2 C4 C5 -48.0(2) C1 C2 C4 C9 -43.8(2) N1 C2 C4 C9 133.91(18) C17 C16 C21 C20 1.8(3) C14 C16 C21 C20 178.96(16) C9 C4 C5 C6 -1.1(3) C2 C4 C5 C6 -179.14(16) C4 C5 C6 C7 -0.4(3) C21 C16 C17 C18 -1.5(3) C14 C16 C17 C18 -178.44(17) C16 C17 C18 C19 0.2(3) C16 C21 C20 C19 -0.9(3) C5 C4 C9 C8 1.7(3) C2 C4 C9 C8 179.91(18) C17 C18 C19 C20 0.7(3) C17 C18 C19 Cl2 179.71(15) C21 C20 C19 C18 -0.4(3) C21 C20 C19 Cl2 -179.38(14) C2 N1 C10 C11 -66.8(2) C3 N1 C10 C11 106.62(19) C4 C9 C8 C7 -0.8(3) C5 C6 C7 C8 1.4(3) C5 C6 C7 Cl1 -178.99(15) C9 C8 C7 C6 -0.7(3) C9 C8 C7 Cl1 179.64(16) C14 N2 C22 C23 -65.4(2) C15 N2 C22 C23 102.84(19) N1 C10 C11 C12 -61.9(2) N2 C22 C23 C24 -60.0(3) _cod_database_fobs_code 2108402