#------------------------------------------------------------------------------ #$Date: 2020-04-10 04:22:34 +0300 (Fri, 10 Apr 2020) $ #$Revision: 250577 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557761.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_1557761 loop_ _publ_author_name 'Dong, Zhaowen' 'Pezzato, Cristian' 'Sienkiewicz, Andrzej' 'Scopelliti, Rosario' 'Fadaei-Tirani, Farzaneh' 'Severin, Kay' _publ_section_title ; SET processes in Lewis acid--base reactions: the tritylation of N-heterocyclic carbenes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D0SC01278E _journal_year 2020 _chemical_formula_moiety 'C46 H51 N2, C24 B F20, C H2 Cl2' _chemical_formula_sum 'C71 H53 B Cl2 F20 N2' _chemical_formula_weight 1395.86 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2019-11-08 _audit_creation_method ; Olex2 1.3-alpha (compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962) ; _audit_update_record ; 2020-01-28 deposited with the CCDC. 2020-04-03 downloaded from the CCDC. ; _cell_angle_alpha 94.923(3) _cell_angle_beta 102.959(3) _cell_angle_gamma 114.918(4) _cell_formula_units_Z 2 _cell_length_a 13.2446(5) _cell_length_b 13.7731(5) _cell_length_c 20.2266(8) _cell_measurement_reflns_used 8509 _cell_measurement_temperature 140.00(10) _cell_measurement_theta_max 72.5760 _cell_measurement_theta_min 3.6280 _cell_volume 3192.4(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.62a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.62a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.62a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 140.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2817 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -46.00 -10.00 1.00 10.00 -- -40.85 125.00 0.00 36 2 \w -118.00 -4.00 1.00 10.00 -- -40.85 -19.00 -90.00 114 3 \w -115.00 -22.00 1.00 10.00 -- -40.85 -38.00-150.00 93 4 \w 28.00 92.00 1.00 10.00 -- 40.85-125.00-180.00 64 5 \w 28.00 53.00 1.00 10.00 -- 40.85-125.00-150.00 25 6 \w 51.00 93.00 1.00 10.00 -- 40.85-128.00 49.00 42 7 \w 34.00 133.00 1.00 40.00 -- 105.15 -30.00-120.00 99 8 \w 56.00 96.00 1.00 40.00 -- 105.15-111.00 -60.00 40 9 \w 98.00 125.00 1.00 40.00 -- 105.15 -30.00 60.00 27 10 \w 41.00 131.00 1.00 40.00 -- 105.15 -30.00 -30.00 90 11 \w 112.00 159.00 1.00 40.00 -- 105.15 45.00 -90.00 47 12 \w 31.00 104.00 1.00 40.00 -- 105.15 -94.00 120.00 73 13 \w 57.00 106.00 1.00 40.00 -- 105.15-111.00 90.00 49 14 \w 113.00 162.00 1.00 40.00 -- 105.15 77.00 -60.00 49 15 \w 83.00 109.00 1.00 40.00 -- 105.15-111.00 0.00 26 16 \w 61.00 109.00 1.00 40.00 -- 105.15-111.00-120.00 48 17 \w 115.00 147.00 1.00 40.00 -- 105.15 77.00 0.00 32 18 \w 40.00 121.00 1.00 40.00 -- 105.15 -45.00 120.00 81 19 \w 117.00 178.00 1.00 40.00 -- 105.15 77.00 30.00 61 20 \w 47.00 80.00 1.00 40.00 -- 105.15 -30.00 60.00 33 21 \w 48.00 119.00 1.00 40.00 -- 105.15 -77.00 -60.00 71 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1245148000 _diffrn_orient_matrix_UB_12 0.0842402000 _diffrn_orient_matrix_UB_13 0.0047002000 _diffrn_orient_matrix_UB_21 0.0335407000 _diffrn_orient_matrix_UB_22 0.0152984000 _diffrn_orient_matrix_UB_23 0.0795546000 _diffrn_orient_matrix_UB_31 0.0362007000 _diffrn_orient_matrix_UB_32 -0.0924190000 _diffrn_orient_matrix_UB_33 -0.0047485000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_unetI/netI 0.0386 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.967 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 22810 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.742 _diffrn_reflns_theta_min 3.615 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.832 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.62a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on Gaussian integration over a multifaceted crystal model. Empirical absorption correction using spherical harmonics as implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_crystal_colour 'clear intense yellow' _exptl_crystal_density_diffrn 1.452 _exptl_crystal_description plate _exptl_crystal_F_000 1424 _exptl_crystal_size_max 0.311 _exptl_crystal_size_mid 0.132 _exptl_crystal_size_min 0.052 _refine_diff_density_max 0.335 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 873 _refine_ls_number_reflns 12281 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0433 _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^)+(0.0578P)^2^+1.0365P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.1185 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10158 _reflns_number_total 12281 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01278e2.cif _cod_data_source_block dzw-112 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Gaussian' was changed to 'gaussian' 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_original_cell_volume 3192.5(2) _cod_database_code 1557761 _shelx_shelxl_version_number 2018/3 _audit_contact_author 'Farzaneh Fadaei Tirani' _chemical_oxdiff_formula 'C71 H54 B Cl2 F20 N2' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.911 _shelx_estimated_absorpt_t_min 0.600 _reflns_odcompleteness_completeness 99.65 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C4(H4), C29(H29), C32(H32), C41(H41), C44(H44) 2.b Secondary CH2 refined with riding coordinates: C71(H71A,H71B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C37(H37), C38(H38), C39(H39) 2.d Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B, H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A, H46B,H46C) ; _shelx_res_file ; TITL dzw-112.res in P-1 dzw-112.res created by SHELXL-2018/3 at 12:35:57 on 08-Nov-2019 CELL 1.54184 13.244622 13.773148 20.226553 94.9234 102.9585 114.9181 ZERR 2 0.000501 0.000518 0.000804 0.0032 0.0034 0.0037 LATT 1 SFAC C H B Cl F N UNIT 142 106 2 4 40 4 L.S. 10 PLAN 5 SIZE 0.311 0.132 0.052 TEMP -133.15 CONF BOND $H fmap 2 acta MORE -1 REM REM REM WGHT 0.057800 1.036500 FVAR 0.37561 CL1 4 -0.031933 0.145176 0.412288 11.00000 0.04960 0.05497 = 0.07194 0.00330 0.01045 0.02132 CL2 4 0.088214 0.012520 0.396368 11.00000 0.06620 0.04243 = 0.05425 0.00384 0.00874 0.02314 C71 1 0.019363 0.084863 0.356749 11.00000 0.07185 0.08237 = 0.06165 0.02988 0.02595 0.04492 AFIX 23 H71A 2 -0.046871 0.034479 0.316657 11.00000 -1.20000 H71B 2 0.074719 0.142774 0.338873 11.00000 -1.20000 AFIX 0 F1 5 0.802511 0.428009 0.264382 11.00000 0.03829 0.04018 = 0.04022 0.00158 0.00937 0.02751 F2 5 0.936077 0.531502 0.392826 11.00000 0.07338 0.05872 = 0.04441 -0.01396 0.00716 0.04375 F3 5 1.128670 0.504957 0.448852 11.00000 0.05735 0.05235 = 0.03419 -0.00946 -0.00564 0.02156 F4 5 1.186557 0.376880 0.370505 11.00000 0.02610 0.04876 = 0.03944 0.00871 0.00168 0.01557 F5 5 1.058285 0.275475 0.243237 11.00000 0.02623 0.03962 = 0.03586 0.00269 0.00777 0.02019 F6 5 0.668508 0.384998 0.113705 11.00000 0.02718 0.03859 = 0.04668 0.01369 0.01754 0.02204 F7 5 0.725541 0.552331 0.051332 11.00000 0.04624 0.04512 = 0.05859 0.02197 0.01654 0.03372 F8 5 0.937224 0.645727 0.026984 11.00000 0.05103 0.03252 = 0.04318 0.01849 0.01554 0.01612 F9 5 1.095013 0.570265 0.073072 11.00000 0.02891 0.03364 = 0.04142 0.00802 0.01599 0.00589 F10 5 1.038342 0.398770 0.133894 11.00000 0.01933 0.03001 = 0.03834 0.00508 0.00746 0.01246 F11 5 0.841316 0.107675 0.233353 11.00000 0.04054 0.03106 = 0.03122 0.00960 0.01594 0.02187 F12 5 0.861821 -0.065209 0.182306 11.00000 0.05996 0.03556 = 0.03911 0.01206 0.01413 0.03356 F13 5 0.883298 -0.091404 0.051459 11.00000 0.06260 0.04110 = 0.03610 -0.00219 0.00652 0.03908 F14 5 0.877012 0.057515 -0.027006 11.00000 0.04791 0.04130 = 0.02601 0.00052 0.01003 0.02656 F15 5 0.855392 0.229848 0.022106 11.00000 0.03471 0.02801 = 0.02807 0.00642 0.01008 0.01549 F16 5 0.719303 0.208298 0.287624 11.00000 0.03975 0.03833 = 0.03798 0.01297 0.01928 0.02143 F17 5 0.501264 0.067704 0.270987 11.00000 0.05071 0.04950 = 0.07628 0.03304 0.04377 0.02512 F18 5 0.346110 -0.019283 0.141736 11.00000 0.02635 0.03800 = 0.10453 0.01814 0.02705 0.00624 F19 5 0.417112 0.042680 0.029391 11.00000 0.02483 0.04059 = 0.06328 -0.00636 -0.00047 0.01177 F20 5 0.636259 0.184794 0.044703 11.00000 0.02802 0.03721 = 0.03383 0.00301 0.00555 0.01400 C47 1 0.918070 0.341218 0.246988 11.00000 0.02288 0.02362 = 0.02909 0.00478 0.00812 0.01096 C48 1 0.897200 0.412089 0.288688 11.00000 0.03037 0.02859 = 0.03477 0.00497 0.00937 0.01635 C49 1 0.964855 0.467369 0.355202 11.00000 0.04664 0.03458 = 0.03593 -0.00085 0.01115 0.02178 C50 1 1.062717 0.454689 0.383697 11.00000 0.03916 0.03333 = 0.02886 -0.00145 0.00096 0.01250 C51 1 1.090535 0.389334 0.343778 11.00000 0.02399 0.03118 = 0.03576 0.00883 0.00513 0.01047 C52 1 1.020349 0.335777 0.277440 11.00000 0.02573 0.02645 = 0.03024 0.00542 0.01060 0.01224 C53 1 0.849802 0.379891 0.126119 11.00000 0.02236 0.02324 = 0.02602 0.00049 0.00709 0.01148 C54 1 0.775828 0.425728 0.104419 11.00000 0.02438 0.02722 = 0.02991 0.00401 0.01071 0.01443 C55 1 0.803614 0.514039 0.071768 11.00000 0.03422 0.02993 = 0.03399 0.00771 0.00885 0.02124 C56 1 0.910535 0.562945 0.060582 11.00000 0.03863 0.02238 = 0.02894 0.00832 0.01069 0.01240 C57 1 0.989305 0.523331 0.083071 11.00000 0.02453 0.02639 = 0.02722 0.00209 0.00933 0.00841 C58 1 0.957502 0.434856 0.114366 11.00000 0.02183 0.02398 = 0.02557 0.00086 0.00575 0.01124 C59 1 0.850718 0.180708 0.131776 11.00000 0.01824 0.02202 = 0.02715 0.00257 0.00626 0.00902 C60 1 0.850879 0.099260 0.168456 11.00000 0.02478 0.02729 = 0.02634 0.00499 0.00853 0.01406 C61 1 0.860619 0.008619 0.142712 11.00000 0.03232 0.02777 = 0.03032 0.00693 0.00641 0.01872 C62 1 0.869957 -0.005514 0.076830 11.00000 0.03136 0.02848 = 0.03064 -0.00165 0.00292 0.01907 C63 1 0.867159 0.070306 0.037345 11.00000 0.02626 0.03168 = 0.02236 -0.00186 0.00319 0.01496 C64 1 0.857247 0.160652 0.065066 11.00000 0.01943 0.02476 = 0.02824 0.00521 0.00502 0.00990 C65 1 0.690495 0.207635 0.166769 11.00000 0.02436 0.02329 = 0.03837 0.00689 0.01139 0.01469 C66 1 0.648956 0.173244 0.222139 11.00000 0.03003 0.02717 = 0.04265 0.01030 0.01631 0.01745 C67 1 0.534339 0.098214 0.214868 11.00000 0.03534 0.03198 = 0.06339 0.02163 0.03043 0.02121 C68 1 0.456493 0.053844 0.149963 11.00000 0.02291 0.02606 = 0.07550 0.01285 0.02085 0.01106 C69 1 0.492501 0.084479 0.093065 11.00000 0.02393 0.02702 = 0.05442 0.00205 0.00690 0.01317 C70 1 0.606679 0.159593 0.102768 11.00000 0.02484 0.02642 = 0.03979 0.00538 0.01084 0.01487 B1 3 0.827928 0.279138 0.168217 11.00000 0.02207 0.02411 = 0.02711 0.00302 0.00785 0.01301 N1 6 0.527193 0.585410 0.752690 11.00000 0.02018 0.01911 = 0.02510 0.00228 0.00832 0.01036 N2 6 0.443173 0.413343 0.752865 11.00000 0.02444 0.01868 = 0.03003 0.00326 0.01226 0.00932 C1 1 0.531486 0.490840 0.736608 11.00000 0.02050 0.02036 = 0.02329 0.00206 0.00617 0.00995 C2 1 0.434699 0.567425 0.778854 11.00000 0.02290 0.02672 = 0.03261 0.00164 0.01087 0.01408 AFIX 43 H2 2 0.412356 0.620704 0.793799 11.00000 -1.20000 AFIX 0 C3 1 0.382084 0.459940 0.779180 11.00000 0.02545 0.02757 = 0.03802 0.00254 0.01647 0.01148 AFIX 43 H3 2 0.315634 0.422987 0.794542 11.00000 -1.20000 AFIX 0 C4 1 0.624068 0.482264 0.707808 11.00000 0.02284 0.02353 = 0.03044 0.00370 0.01219 0.01328 AFIX 13 H4 2 0.666960 0.554720 0.695984 11.00000 -1.20000 AFIX 0 C5 1 0.712407 0.467039 0.761068 11.00000 0.02150 0.02420 = 0.02939 -0.00269 0.00595 0.01030 AFIX 43 H5 2 0.742925 0.511800 0.806130 11.00000 -1.20000 AFIX 0 C6 1 0.750066 0.393534 0.748053 11.00000 0.02237 0.02703 = 0.02832 0.00138 0.00418 0.01297 AFIX 43 H6 2 0.808305 0.390466 0.783815 11.00000 -1.20000 AFIX 0 C7 1 0.706227 0.317409 0.681500 11.00000 0.02601 0.02349 = 0.02782 0.00287 0.00879 0.01294 C8 1 0.616294 0.326671 0.629756 11.00000 0.02816 0.02636 = 0.02470 0.00098 0.00700 0.01414 AFIX 43 H8 2 0.584681 0.279162 0.585592 11.00000 -1.20000 AFIX 0 C9 1 0.576075 0.398818 0.641411 11.00000 0.02714 0.03093 = 0.02542 0.00437 0.00789 0.01709 AFIX 43 H9 2 0.514243 0.397319 0.606082 11.00000 -1.20000 AFIX 0 C10 1 0.746885 0.244048 0.669025 11.00000 0.03119 0.02638 = 0.03127 0.00579 0.01101 0.01701 C11 1 0.829847 0.227167 0.724023 11.00000 0.03291 0.02511 = 0.03048 0.00268 0.00810 0.01841 C12 1 0.933452 0.233591 0.714130 11.00000 0.04164 0.04713 = 0.03509 0.01020 0.01520 0.03044 AFIX 43 H12 2 0.950742 0.248500 0.671897 11.00000 -1.20000 AFIX 0 C13 1 1.011144 0.218363 0.765501 11.00000 0.03691 0.05375 = 0.04539 0.01030 0.01198 0.03218 AFIX 43 H13 2 1.081356 0.222993 0.758295 11.00000 -1.20000 AFIX 0 C14 1 0.987013 0.196531 0.827003 11.00000 0.04048 0.03563 = 0.03630 0.00462 0.00334 0.02481 AFIX 43 H14 2 1.041175 0.187672 0.862488 11.00000 -1.20000 AFIX 0 C15 1 0.883482 0.187569 0.836838 11.00000 0.04049 0.02784 = 0.03426 0.00753 0.01087 0.01616 AFIX 43 H15 2 0.865917 0.171202 0.878799 11.00000 -1.20000 AFIX 0 C16 1 0.805537 0.202457 0.785522 11.00000 0.03063 0.02899 = 0.03512 0.00463 0.01122 0.01587 AFIX 43 H16 2 0.734472 0.195661 0.792522 11.00000 -1.20000 AFIX 0 C17 1 0.712442 0.173621 0.599666 11.00000 0.04203 0.03890 = 0.03010 0.00362 0.00838 0.03131 C18 1 0.656892 0.060312 0.592017 11.00000 0.07258 0.03851 = 0.03677 0.00326 0.00497 0.03107 AFIX 43 H18 2 0.639131 0.029240 0.630604 11.00000 -1.20000 AFIX 0 C19 1 0.627321 -0.007388 0.529230 11.00000 0.10689 0.04443 = 0.04629 -0.00606 -0.00429 0.04618 AFIX 43 H19 2 0.588029 -0.084431 0.524846 11.00000 -1.20000 AFIX 0 C20 1 0.653956 0.035188 0.473112 11.00000 0.10501 0.07275 = 0.03490 -0.00943 0.00269 0.07014 AFIX 43 H20 2 0.633162 -0.011880 0.429961 11.00000 -1.20000 AFIX 0 C21 1 0.711372 0.147286 0.479924 11.00000 0.09030 0.08959 = 0.03787 0.01473 0.02640 0.06563 AFIX 43 H21 2 0.731880 0.177508 0.441599 11.00000 -1.20000 AFIX 0 C22 1 0.739319 0.216209 0.542845 11.00000 0.06432 0.05073 = 0.04318 0.01080 0.02348 0.03735 AFIX 43 H22 2 0.777214 0.293224 0.546759 11.00000 -1.20000 AFIX 0 C23 1 0.605537 0.691882 0.744209 11.00000 0.02335 0.01809 = 0.02978 0.00376 0.01132 0.01184 C24 1 0.584249 0.718776 0.679410 11.00000 0.03294 0.02527 = 0.03028 0.00623 0.01185 0.01666 C25 1 0.659246 0.823685 0.674094 11.00000 0.04590 0.02928 = 0.03985 0.01481 0.01937 0.01882 AFIX 43 H25 2 0.649777 0.845045 0.630593 11.00000 -1.20000 AFIX 0 C26 1 0.746902 0.896803 0.731061 11.00000 0.04353 0.02225 = 0.05016 0.01067 0.01920 0.01129 AFIX 43 H26 2 0.795078 0.968585 0.726584 11.00000 -1.20000 AFIX 0 C27 1 0.765509 0.867122 0.794352 11.00000 0.03018 0.02111 = 0.04264 0.00072 0.00720 0.00773 AFIX 43 H27 2 0.826670 0.918607 0.832797 11.00000 -1.20000 AFIX 0 C28 1 0.695743 0.762415 0.802813 11.00000 0.02396 0.02219 = 0.03342 0.00188 0.00946 0.01296 C29 1 0.483399 0.639497 0.618156 11.00000 0.04320 0.03166 = 0.02766 0.00453 0.00641 0.01992 AFIX 13 H29 2 0.457696 0.564703 0.628874 11.00000 -1.20000 AFIX 0 C30 1 0.517429 0.636445 0.552000 11.00000 0.08197 0.06053 = 0.03391 -0.00072 0.02021 0.02303 AFIX 137 H30A 2 0.536074 0.706711 0.537674 11.00000 -1.50000 H30B 2 0.452699 0.577823 0.515607 11.00000 -1.50000 H30C 2 0.585636 0.622816 0.559707 11.00000 -1.50000 AFIX 0 C31 1 0.381429 0.665880 0.609631 11.00000 0.05442 0.09847 = 0.06174 -0.02534 -0.01657 0.04930 AFIX 137 H31A 2 0.316010 0.612534 0.571099 11.00000 -1.50000 H31B 2 0.404345 0.739483 0.599894 11.00000 -1.50000 H31C 2 0.358119 0.662651 0.652399 11.00000 -1.50000 AFIX 0 C32 1 0.716950 0.727612 0.871394 11.00000 0.02887 0.02610 = 0.02975 0.00145 0.00463 0.01503 AFIX 13 H32 2 0.679078 0.645866 0.861986 11.00000 -1.20000 AFIX 0 C33 1 0.846434 0.768430 0.905997 11.00000 0.03331 0.04666 = 0.03702 -0.00142 0.00295 0.02603 AFIX 137 H33A 2 0.881317 0.746925 0.873196 11.00000 -1.50000 H33B 2 0.856735 0.736273 0.946840 11.00000 -1.50000 H33C 2 0.884405 0.848305 0.920176 11.00000 -1.50000 AFIX 0 C34 1 0.661480 0.766002 0.920115 11.00000 0.03205 0.04308 = 0.03400 0.00278 0.00840 0.01933 AFIX 137 H34A 2 0.695352 0.845980 0.929043 11.00000 -1.50000 H34B 2 0.676191 0.742018 0.963955 11.00000 -1.50000 H34C 2 0.577458 0.734533 0.898472 11.00000 -1.50000 AFIX 0 C35 1 0.406336 0.296027 0.738982 11.00000 0.02872 0.01916 = 0.03547 0.00417 0.01662 0.01004 C36 1 0.328190 0.236375 0.674451 11.00000 0.02858 0.02336 = 0.03724 0.00371 0.01619 0.00933 C37 1 0.292011 0.123927 0.662141 11.00000 0.03873 0.02352 = 0.04199 -0.00067 0.01619 0.00892 AFIX 43 H37 2 0.239014 0.079639 0.618883 11.00000 -1.20000 AFIX 0 C38 1 0.332525 0.076084 0.712326 11.00000 0.04970 0.02077 = 0.05446 0.00904 0.02482 0.01357 AFIX 43 H38 2 0.308435 -0.000366 0.702557 11.00000 -1.20000 AFIX 0 C39 1 0.406977 0.137547 0.775967 11.00000 0.05166 0.02967 = 0.04816 0.01587 0.02613 0.02083 AFIX 43 H39 2 0.432180 0.102547 0.809824 11.00000 -1.20000 AFIX 0 C40 1 0.446480 0.250816 0.791935 11.00000 0.03408 0.02893 = 0.03782 0.00917 0.01817 0.01612 C41 1 0.281270 0.288016 0.620070 11.00000 0.02933 0.02779 = 0.03778 0.00289 0.00877 0.00864 AFIX 13 H41 2 0.338557 0.366972 0.629137 11.00000 -1.20000 AFIX 0 C42 1 0.267015 0.236278 0.546426 11.00000 0.04832 0.04871 = 0.03684 0.00163 0.00603 0.01837 AFIX 137 H42A 2 0.338724 0.232750 0.544566 11.00000 -1.50000 H42B 2 0.250949 0.280692 0.514195 11.00000 -1.50000 H42C 2 0.202242 0.162249 0.533342 11.00000 -1.50000 AFIX 0 C43 1 0.165078 0.282265 0.625400 11.00000 0.03501 0.04774 = 0.05994 0.00952 0.01326 0.01902 AFIX 137 H43A 2 0.108509 0.205714 0.619592 11.00000 -1.50000 H43B 2 0.135932 0.314560 0.589071 11.00000 -1.50000 H43C 2 0.176660 0.322850 0.670939 11.00000 -1.50000 AFIX 0 C44 1 0.521122 0.316534 0.863948 11.00000 0.03980 0.03638 = 0.03590 0.00985 0.01574 0.01813 AFIX 13 H44 2 0.557834 0.395454 0.861025 11.00000 -1.20000 AFIX 0 C45 1 0.618609 0.286897 0.894105 11.00000 0.04789 0.06133 = 0.04326 0.01581 0.01468 0.03046 AFIX 137 H45A 2 0.584798 0.210700 0.899584 11.00000 -1.50000 H45B 2 0.666416 0.335004 0.939365 11.00000 -1.50000 H45C 2 0.667076 0.295997 0.862688 11.00000 -1.50000 AFIX 0 C46 1 0.444652 0.302678 0.912905 11.00000 0.05413 0.08111 = 0.04109 0.00682 0.02147 0.03370 AFIX 137 H46A 2 0.386384 0.327538 0.895250 11.00000 -1.50000 H46B 2 0.493345 0.346244 0.959232 11.00000 -1.50000 H46C 2 0.405467 0.225415 0.915448 11.00000 -1.50000 AFIX 0 HKLF 4 REM dzw-112.res in P-1 REM wR2 = 0.1185, GooF = S = 1.025, Restrained GooF = 1.025 for all data REM R1 = 0.0433 for 10158 Fo > 4sig(Fo) and 0.0542 for all 12281 data REM 873 parameters refined using 0 restraints END WGHT 0.0578 1.0415 REM Highest difference peak 0.335, deepest hole -0.494, 1-sigma level 0.050 Q1 1 0.8813 0.3140 0.2035 11.00000 0.05 0.33 Q2 1 0.8383 0.2297 0.1496 11.00000 0.05 0.31 Q3 1 0.0377 0.0081 0.4205 11.00000 0.05 0.27 Q4 1 0.9403 0.5237 0.0488 11.00000 0.05 0.26 Q5 1 0.6389 0.7318 0.7766 11.00000 0.05 0.24 ; _shelx_res_checksum 94361 _olex2_date_sample_data_collection 2019-11-07 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 1.844 _oxdiff_exptl_absorpt_empirical_full_min 0.696 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.03193(6) 0.14518(6) 0.41229(4) 0.06164(18) Uani 1 1 d . . . . . Cl2 Cl 0.08821(6) 0.01252(5) 0.39637(4) 0.05680(17) Uani 1 1 d . . . . . C71 C 0.0194(3) 0.0849(3) 0.35675(17) 0.0661(8) Uani 1 1 d . . . . . H71A H -0.046871 0.034479 0.316657 0.079 Uiso 1 1 calc R U . . . H71B H 0.074719 0.142774 0.338873 0.079 Uiso 1 1 calc R U . . . F1 F 0.80251(11) 0.42801(10) 0.26438(6) 0.0368(3) Uani 1 1 d . . . . . F2 F 0.93608(15) 0.53150(13) 0.39283(8) 0.0572(4) Uani 1 1 d . . . . . F3 F 1.12867(14) 0.50496(12) 0.44885(7) 0.0538(4) Uani 1 1 d . . . . . F4 F 1.18656(10) 0.37688(10) 0.37050(7) 0.0400(3) Uani 1 1 d . . . . . F5 F 1.05828(9) 0.27548(9) 0.24324(6) 0.0325(2) Uani 1 1 d . . . . . F6 F 0.66851(10) 0.38500(9) 0.11371(6) 0.0333(2) Uani 1 1 d . . . . . F7 F 0.72554(12) 0.55233(11) 0.05133(8) 0.0442(3) Uani 1 1 d . . . . . F8 F 0.93722(12) 0.64573(10) 0.02698(7) 0.0422(3) Uani 1 1 d . . . . . F9 F 1.09501(10) 0.57026(9) 0.07307(6) 0.0366(3) Uani 1 1 d . . . . . F10 F 1.03834(9) 0.39877(8) 0.13389(6) 0.0290(2) Uani 1 1 d . . . . . F11 F 0.84132(10) 0.10767(9) 0.23335(6) 0.0310(2) Uani 1 1 d . . . . . F12 F 0.86182(12) -0.06521(10) 0.18231(7) 0.0403(3) Uani 1 1 d . . . . . F13 F 0.88330(13) -0.09140(10) 0.05146(7) 0.0430(3) Uani 1 1 d . . . . . F14 F 0.87701(11) 0.05751(10) -0.02701(6) 0.0366(3) Uani 1 1 d . . . . . F15 F 0.85539(10) 0.22985(8) 0.02211(6) 0.0296(2) Uani 1 1 d . . . . . F16 F 0.71930(11) 0.20830(9) 0.28762(6) 0.0355(3) Uani 1 1 d . . . . . F17 F 0.50126(13) 0.06770(12) 0.27099(9) 0.0520(4) Uani 1 1 d . . . . . F18 F 0.34611(11) -0.01928(11) 0.14174(10) 0.0576(4) Uani 1 1 d . . . . . F19 F 0.41711(11) 0.04268(10) 0.02939(8) 0.0475(3) Uani 1 1 d . . . . . F20 F 0.63626(10) 0.18479(9) 0.04470(6) 0.0342(3) Uani 1 1 d . . . . . C47 C 0.91807(15) 0.34122(14) 0.24699(10) 0.0250(4) Uani 1 1 d . . . . . C48 C 0.89720(17) 0.41209(15) 0.28869(11) 0.0303(4) Uani 1 1 d . . . . . C49 C 0.9649(2) 0.46737(17) 0.35520(12) 0.0385(5) Uani 1 1 d . . . . . C50 C 1.06272(19) 0.45469(17) 0.38370(11) 0.0373(5) Uani 1 1 d . . . . . C51 C 1.09053(17) 0.38933(16) 0.34378(11) 0.0315(4) Uani 1 1 d . . . . . C52 C 1.02035(16) 0.33578(15) 0.27744(10) 0.0269(4) Uani 1 1 d . . . . . C53 C 0.84980(15) 0.37989(14) 0.12612(9) 0.0237(3) Uani 1 1 d . . . . . C54 C 0.77583(16) 0.42573(15) 0.10442(10) 0.0258(4) Uani 1 1 d . . . . . C55 C 0.80361(18) 0.51404(15) 0.07177(11) 0.0304(4) Uani 1 1 d . . . . . C56 C 0.91053(18) 0.56294(15) 0.06058(10) 0.0301(4) Uani 1 1 d . . . . . C57 C 0.98930(16) 0.52333(14) 0.08307(10) 0.0271(4) Uani 1 1 d . . . . . C58 C 0.95750(15) 0.43486(14) 0.11437(9) 0.0240(3) Uani 1 1 d . . . . . C59 C 0.85072(14) 0.18071(13) 0.13178(9) 0.0227(3) Uani 1 1 d . . . . . C60 C 0.85088(15) 0.09926(14) 0.16846(10) 0.0251(4) Uani 1 1 d . . . . . C61 C 0.86062(17) 0.00862(15) 0.14271(10) 0.0287(4) Uani 1 1 d . . . . . C62 C 0.86996(17) -0.00551(15) 0.07683(10) 0.0298(4) Uani 1 1 d . . . . . C63 C 0.86716(16) 0.07031(15) 0.03735(9) 0.0273(4) Uani 1 1 d . . . . . C64 C 0.85725(15) 0.16065(14) 0.06507(10) 0.0245(3) Uani 1 1 d . . . . . C65 C 0.69050(16) 0.20763(14) 0.16677(10) 0.0268(4) Uani 1 1 d . . . . . C66 C 0.64896(17) 0.17324(15) 0.22214(11) 0.0304(4) Uani 1 1 d . . . . . C67 C 0.53434(19) 0.09821(17) 0.21487(13) 0.0377(5) Uani 1 1 d . . . . . C68 C 0.45649(17) 0.05384(16) 0.14996(14) 0.0401(5) Uani 1 1 d . . . . . C69 C 0.49250(17) 0.08448(16) 0.09307(13) 0.0358(5) Uani 1 1 d . . . . . C70 C 0.60668(16) 0.15959(15) 0.10277(11) 0.0290(4) Uani 1 1 d . . . . . B1 B 0.82793(17) 0.27914(16) 0.16822(11) 0.0235(4) Uani 1 1 d . . . . . N1 N 0.52719(12) 0.58541(11) 0.75269(8) 0.0208(3) Uani 1 1 d . . . . . N2 N 0.44317(13) 0.41334(11) 0.75286(8) 0.0239(3) Uani 1 1 d . . . . . C1 C 0.53149(15) 0.49084(13) 0.73661(9) 0.0213(3) Uani 1 1 d . . . . . C2 C 0.43470(15) 0.56742(14) 0.77885(10) 0.0262(4) Uani 1 1 d . . . . . H2 H 0.412356 0.620704 0.793799 0.031 Uiso 1 1 calc R U . . . C3 C 0.38208(16) 0.45994(15) 0.77918(11) 0.0295(4) Uani 1 1 d . . . . . H3 H 0.315634 0.422987 0.794542 0.035 Uiso 1 1 calc R U . . . C4 C 0.62407(15) 0.48226(14) 0.70781(10) 0.0239(3) Uani 1 1 d . . . . . H4 H 0.666960 0.554720 0.695984 0.029 Uiso 1 1 calc R U . . . C5 C 0.71241(15) 0.46704(14) 0.76107(10) 0.0259(4) Uani 1 1 d . . . . . H5 H 0.742925 0.511800 0.806130 0.031 Uiso 1 1 calc R U . . . C6 C 0.75007(16) 0.39353(14) 0.74805(10) 0.0261(4) Uani 1 1 d . . . . . H6 H 0.808305 0.390466 0.783815 0.031 Uiso 1 1 calc R U . . . C7 C 0.70623(16) 0.31741(14) 0.68150(10) 0.0251(4) Uani 1 1 d . . . . . C8 C 0.61629(16) 0.32667(14) 0.62976(10) 0.0262(4) Uani 1 1 d . . . . . H8 H 0.584681 0.279162 0.585592 0.031 Uiso 1 1 calc R U . . . C9 C 0.57608(16) 0.39882(15) 0.64141(10) 0.0264(4) Uani 1 1 d . . . . . H9 H 0.514243 0.397319 0.606082 0.032 Uiso 1 1 calc R U . . . C10 C 0.74688(17) 0.24405(15) 0.66903(10) 0.0278(4) Uani 1 1 d . . . . . C11 C 0.82985(17) 0.22717(15) 0.72402(10) 0.0280(4) Uani 1 1 d . . . . . C12 C 0.93345(19) 0.23359(18) 0.71413(11) 0.0367(4) Uani 1 1 d . . . . . H12 H 0.950742 0.248500 0.671897 0.044 Uiso 1 1 calc R U . . . C13 C 1.0111(2) 0.2184(2) 0.76550(12) 0.0411(5) Uani 1 1 d . . . . . H13 H 1.081356 0.222993 0.758295 0.049 Uiso 1 1 calc R U . . . C14 C 0.98701(19) 0.19653(17) 0.82700(11) 0.0363(4) Uani 1 1 d . . . . . H14 H 1.041175 0.187672 0.862488 0.044 Uiso 1 1 calc R U . . . C15 C 0.88348(19) 0.18757(16) 0.83684(11) 0.0339(4) Uani 1 1 d . . . . . H15 H 0.865917 0.171202 0.878799 0.041 Uiso 1 1 calc R U . . . C16 C 0.80554(17) 0.20246(15) 0.78552(11) 0.0305(4) Uani 1 1 d . . . . . H16 H 0.734472 0.195661 0.792522 0.037 Uiso 1 1 calc R U . . . C17 C 0.71244(19) 0.17362(17) 0.59967(11) 0.0329(4) Uani 1 1 d . . . . . C18 C 0.6569(3) 0.06031(19) 0.59202(13) 0.0494(6) Uani 1 1 d . . . . . H18 H 0.639131 0.029240 0.630604 0.059 Uiso 1 1 calc R U . . . C19 C 0.6273(3) -0.0074(2) 0.52923(15) 0.0673(9) Uani 1 1 d . . . . . H19 H 0.588029 -0.084431 0.524846 0.081 Uiso 1 1 calc R U . . . C20 C 0.6540(3) 0.0352(3) 0.47311(14) 0.0646(9) Uani 1 1 d . . . . . H20 H 0.633162 -0.011880 0.429961 0.077 Uiso 1 1 calc R U . . . C21 C 0.7114(3) 0.1473(3) 0.47992(14) 0.0620(8) Uani 1 1 d . . . . . H21 H 0.731880 0.177508 0.441599 0.074 Uiso 1 1 calc R U . . . C22 C 0.7393(2) 0.2162(2) 0.54285(13) 0.0471(6) Uani 1 1 d . . . . . H22 H 0.777214 0.293224 0.546759 0.057 Uiso 1 1 calc R U . . . C23 C 0.60554(15) 0.69188(13) 0.74421(9) 0.0223(3) Uani 1 1 d . . . . . C24 C 0.58425(17) 0.71878(15) 0.67941(10) 0.0277(4) Uani 1 1 d . . . . . C25 C 0.6592(2) 0.82368(16) 0.67409(12) 0.0359(4) Uani 1 1 d . . . . . H25 H 0.649777 0.845045 0.630593 0.043 Uiso 1 1 calc R U . . . C26 C 0.7469(2) 0.89680(16) 0.73106(12) 0.0387(5) Uani 1 1 d . . . . . H26 H 0.795078 0.968585 0.726584 0.046 Uiso 1 1 calc R U . . . C27 C 0.76551(18) 0.86712(15) 0.79435(11) 0.0337(4) Uani 1 1 d . . . . . H27 H 0.826670 0.918607 0.832797 0.040 Uiso 1 1 calc R U . . . C28 C 0.69574(16) 0.76242(14) 0.80281(10) 0.0257(4) Uani 1 1 d . . . . . C29 C 0.48340(19) 0.63950(16) 0.61816(10) 0.0339(4) Uani 1 1 d . . . . . H29 H 0.457696 0.564703 0.628874 0.041 Uiso 1 1 calc R U . . . C30 C 0.5174(3) 0.6364(2) 0.55200(14) 0.0623(8) Uani 1 1 d . . . . . H30A H 0.536074 0.706711 0.537674 0.093 Uiso 1 1 calc R U . . . H30B H 0.452699 0.577823 0.515607 0.093 Uiso 1 1 calc R U . . . H30C H 0.585636 0.622816 0.559707 0.093 Uiso 1 1 calc R U . . . C31 C 0.3814(3) 0.6659(3) 0.60963(17) 0.0750(11) Uani 1 1 d . . . . . H31A H 0.316010 0.612534 0.571099 0.113 Uiso 1 1 calc R U . . . H31B H 0.404345 0.739483 0.599894 0.113 Uiso 1 1 calc R U . . . H31C H 0.358119 0.662651 0.652399 0.113 Uiso 1 1 calc R U . . . C32 C 0.71695(16) 0.72761(15) 0.87139(10) 0.0283(4) Uani 1 1 d . . . . . H32 H 0.679078 0.645866 0.861986 0.034 Uiso 1 1 calc R U . . . C33 C 0.84643(19) 0.76843(18) 0.90600(12) 0.0381(5) Uani 1 1 d . . . . . H33A H 0.881317 0.746925 0.873196 0.057 Uiso 1 1 calc R U . . . H33B H 0.856735 0.736273 0.946840 0.057 Uiso 1 1 calc R U . . . H33C H 0.884405 0.848305 0.920176 0.057 Uiso 1 1 calc R U . . . C34 C 0.66148(18) 0.76600(18) 0.92011(11) 0.0361(4) Uani 1 1 d . . . . . H34A H 0.695352 0.845980 0.929043 0.054 Uiso 1 1 calc R U . . . H34B H 0.676191 0.742018 0.963955 0.054 Uiso 1 1 calc R U . . . H34C H 0.577458 0.734533 0.898472 0.054 Uiso 1 1 calc R U . . . C35 C 0.40634(16) 0.29603(14) 0.73898(10) 0.0268(4) Uani 1 1 d . . . . . C36 C 0.32819(17) 0.23637(15) 0.67445(11) 0.0296(4) Uani 1 1 d . . . . . C37 C 0.29201(19) 0.12393(16) 0.66214(12) 0.0363(5) Uani 1 1 d . . . . . H37 H 0.239014 0.079639 0.618883 0.044 Uiso 1 1 calc R U . . . C38 C 0.3325(2) 0.07608(16) 0.71233(13) 0.0407(5) Uani 1 1 d . . . . . H38 H 0.308435 -0.000366 0.702557 0.049 Uiso 1 1 calc R U . . . C39 C 0.4070(2) 0.13755(17) 0.77597(13) 0.0396(5) Uani 1 1 d . . . . . H39 H 0.432180 0.102547 0.809824 0.048 Uiso 1 1 calc R U . . . C40 C 0.44648(18) 0.25082(16) 0.79194(11) 0.0314(4) Uani 1 1 d . . . . . C41 C 0.28127(17) 0.28802(16) 0.62007(11) 0.0336(4) Uani 1 1 d . . . . . H41 H 0.338557 0.366972 0.629137 0.040 Uiso 1 1 calc R U . . . C42 C 0.2670(2) 0.2363(2) 0.54643(12) 0.0476(6) Uani 1 1 d . . . . . H42A H 0.338724 0.232750 0.544566 0.071 Uiso 1 1 calc R U . . . H42B H 0.250949 0.280692 0.514195 0.071 Uiso 1 1 calc R U . . . H42C H 0.202242 0.162249 0.533342 0.071 Uiso 1 1 calc R U . . . C43 C 0.1651(2) 0.2823(2) 0.62540(14) 0.0476(6) Uani 1 1 d . . . . . H43A H 0.108509 0.205714 0.619592 0.071 Uiso 1 1 calc R U . . . H43B H 0.135932 0.314560 0.589071 0.071 Uiso 1 1 calc R U . . . H43C H 0.176660 0.322850 0.670939 0.071 Uiso 1 1 calc R U . . . C44 C 0.52112(19) 0.31653(17) 0.86395(11) 0.0360(4) Uani 1 1 d . . . . . H44 H 0.557834 0.395454 0.861025 0.043 Uiso 1 1 calc R U . . . C45 C 0.6186(2) 0.2869(2) 0.89411(13) 0.0481(6) Uani 1 1 d . . . . . H45A H 0.584798 0.210700 0.899584 0.072 Uiso 1 1 calc R U . . . H45B H 0.666416 0.335004 0.939365 0.072 Uiso 1 1 calc R U . . . H45C H 0.667076 0.295997 0.862688 0.072 Uiso 1 1 calc R U . . . C46 C 0.4447(3) 0.3027(3) 0.91290(14) 0.0567(7) Uani 1 1 d . . . . . H46A H 0.386384 0.327538 0.895250 0.085 Uiso 1 1 calc R U . . . H46B H 0.493345 0.346244 0.959232 0.085 Uiso 1 1 calc R U . . . H46C H 0.405467 0.225415 0.915448 0.085 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 Cl1 0.0496(4) 0.0550(4) 0.0719(4) 0.0033(3) 0.0104(3) 0.0213(3) Cl2 0.0662(4) 0.0424(3) 0.0542(4) 0.0038(3) 0.0087(3) 0.0231(3) C71 0.072(2) 0.082(2) 0.0616(18) 0.0299(16) 0.0259(15) 0.0449(17) F1 0.0383(6) 0.0402(6) 0.0402(7) 0.0016(5) 0.0094(5) 0.0275(5) F2 0.0734(10) 0.0587(9) 0.0444(8) -0.0140(6) 0.0072(7) 0.0438(8) F3 0.0573(9) 0.0524(8) 0.0342(7) -0.0095(6) -0.0056(6) 0.0216(7) F4 0.0261(6) 0.0488(7) 0.0394(7) 0.0087(5) 0.0017(5) 0.0156(5) F5 0.0262(5) 0.0396(6) 0.0359(6) 0.0027(5) 0.0078(5) 0.0202(5) F6 0.0272(5) 0.0386(6) 0.0467(7) 0.0137(5) 0.0175(5) 0.0220(5) F7 0.0462(7) 0.0451(7) 0.0586(8) 0.0220(6) 0.0165(6) 0.0337(6) F8 0.0510(8) 0.0325(6) 0.0432(7) 0.0185(5) 0.0155(6) 0.0161(5) F9 0.0289(6) 0.0336(6) 0.0414(7) 0.0080(5) 0.0160(5) 0.0059(5) F10 0.0193(5) 0.0300(5) 0.0383(6) 0.0051(4) 0.0075(4) 0.0125(4) F11 0.0405(6) 0.0311(5) 0.0312(6) 0.0096(4) 0.0159(5) 0.0219(5) F12 0.0600(8) 0.0356(6) 0.0391(7) 0.0121(5) 0.0141(6) 0.0336(6) F13 0.0626(8) 0.0411(6) 0.0361(7) -0.0022(5) 0.0065(6) 0.0391(6) F14 0.0479(7) 0.0413(6) 0.0260(6) 0.0005(5) 0.0100(5) 0.0266(5) F15 0.0347(6) 0.0280(5) 0.0281(5) 0.0064(4) 0.0101(4) 0.0155(4) F16 0.0397(6) 0.0383(6) 0.0380(6) 0.0130(5) 0.0193(5) 0.0214(5) F17 0.0507(8) 0.0495(7) 0.0763(10) 0.0330(7) 0.0438(8) 0.0251(6) F18 0.0264(6) 0.0380(7) 0.1045(13) 0.0181(7) 0.0271(7) 0.0062(5) F19 0.0248(6) 0.0406(7) 0.0633(9) -0.0064(6) -0.0005(6) 0.0118(5) F20 0.0280(6) 0.0372(6) 0.0338(6) 0.0030(5) 0.0056(5) 0.0140(5) C47 0.0229(8) 0.0236(8) 0.0291(9) 0.0048(7) 0.0081(7) 0.0110(7) C48 0.0304(10) 0.0286(9) 0.0348(10) 0.0050(8) 0.0094(8) 0.0164(8) C49 0.0466(12) 0.0346(10) 0.0359(11) -0.0008(8) 0.0111(9) 0.0218(9) C50 0.0392(11) 0.0333(10) 0.0289(10) -0.0015(8) 0.0010(8) 0.0125(8) C51 0.0240(9) 0.0312(9) 0.0358(10) 0.0088(8) 0.0051(8) 0.0105(7) C52 0.0257(9) 0.0265(8) 0.0302(9) 0.0054(7) 0.0106(7) 0.0122(7) C53 0.0224(8) 0.0232(8) 0.0260(9) 0.0005(7) 0.0071(7) 0.0115(7) C54 0.0244(9) 0.0272(8) 0.0299(9) 0.0040(7) 0.0107(7) 0.0144(7) C55 0.0342(10) 0.0299(9) 0.0340(10) 0.0077(8) 0.0088(8) 0.0212(8) C56 0.0386(10) 0.0224(8) 0.0289(9) 0.0083(7) 0.0107(8) 0.0124(7) C57 0.0245(9) 0.0264(8) 0.0272(9) 0.0021(7) 0.0093(7) 0.0084(7) C58 0.0218(8) 0.0240(8) 0.0256(9) 0.0009(6) 0.0057(7) 0.0112(7) C59 0.0182(8) 0.0220(8) 0.0272(9) 0.0026(6) 0.0063(6) 0.0090(6) C60 0.0248(9) 0.0273(8) 0.0263(9) 0.0050(7) 0.0085(7) 0.0141(7) C61 0.0323(10) 0.0278(9) 0.0303(10) 0.0069(7) 0.0064(8) 0.0187(8) C62 0.0314(10) 0.0285(9) 0.0306(10) -0.0017(7) 0.0029(8) 0.0191(8) C63 0.0263(9) 0.0317(9) 0.0224(9) -0.0019(7) 0.0032(7) 0.0150(7) C64 0.0194(8) 0.0248(8) 0.0282(9) 0.0052(7) 0.0050(7) 0.0099(6) C65 0.0244(9) 0.0233(8) 0.0384(10) 0.0069(7) 0.0114(7) 0.0147(7) C66 0.0300(10) 0.0272(9) 0.0426(11) 0.0103(8) 0.0163(8) 0.0175(8) C67 0.0353(11) 0.0320(10) 0.0634(15) 0.0216(10) 0.0304(10) 0.0212(9) C68 0.0229(9) 0.0261(9) 0.0755(17) 0.0129(10) 0.0208(10) 0.0111(8) C69 0.0239(9) 0.0270(9) 0.0544(13) 0.0020(8) 0.0069(9) 0.0132(8) C70 0.0248(9) 0.0264(9) 0.0398(11) 0.0054(7) 0.0108(8) 0.0149(7) B1 0.0221(9) 0.0241(9) 0.0271(10) 0.0030(7) 0.0078(8) 0.0130(7) N1 0.0202(7) 0.0191(6) 0.0251(7) 0.0023(5) 0.0083(6) 0.0104(5) N2 0.0244(7) 0.0187(7) 0.0300(8) 0.0033(6) 0.0123(6) 0.0093(6) C1 0.0205(8) 0.0204(7) 0.0233(8) 0.0021(6) 0.0062(6) 0.0099(6) C2 0.0229(8) 0.0267(8) 0.0326(10) 0.0016(7) 0.0109(7) 0.0141(7) C3 0.0254(9) 0.0276(9) 0.0380(10) 0.0025(7) 0.0165(8) 0.0115(7) C4 0.0228(8) 0.0235(8) 0.0304(9) 0.0037(7) 0.0122(7) 0.0133(7) C5 0.0215(8) 0.0242(8) 0.0294(9) -0.0027(7) 0.0060(7) 0.0103(7) C6 0.0224(8) 0.0270(8) 0.0283(9) 0.0014(7) 0.0042(7) 0.0130(7) C7 0.0260(9) 0.0235(8) 0.0278(9) 0.0029(7) 0.0088(7) 0.0129(7) C8 0.0282(9) 0.0264(8) 0.0247(9) 0.0010(7) 0.0070(7) 0.0141(7) C9 0.0271(9) 0.0309(9) 0.0254(9) 0.0044(7) 0.0079(7) 0.0171(7) C10 0.0312(9) 0.0264(8) 0.0313(10) 0.0058(7) 0.0110(8) 0.0170(7) C11 0.0329(10) 0.0251(8) 0.0305(9) 0.0027(7) 0.0081(8) 0.0184(7) C12 0.0416(11) 0.0471(11) 0.0351(11) 0.0102(9) 0.0152(9) 0.0304(10) C13 0.0369(11) 0.0538(13) 0.0454(13) 0.0103(10) 0.0120(9) 0.0322(10) C14 0.0405(11) 0.0356(10) 0.0363(11) 0.0046(8) 0.0033(9) 0.0248(9) C15 0.0405(11) 0.0278(9) 0.0343(10) 0.0075(8) 0.0109(9) 0.0162(8) C16 0.0306(10) 0.0290(9) 0.0351(10) 0.0046(7) 0.0112(8) 0.0159(7) C17 0.0420(11) 0.0389(10) 0.0301(10) 0.0036(8) 0.0084(8) 0.0313(9) C18 0.0726(17) 0.0385(12) 0.0368(12) 0.0033(9) 0.0050(11) 0.0311(12) C19 0.107(3) 0.0444(14) 0.0463(15) -0.0061(11) -0.0043(15) 0.0462(16) C20 0.105(2) 0.0728(18) 0.0349(13) -0.0094(12) 0.0027(14) 0.0701(19) C21 0.090(2) 0.090(2) 0.0379(14) 0.0147(13) 0.0264(14) 0.0656(19) C22 0.0643(16) 0.0507(13) 0.0432(13) 0.0108(10) 0.0235(11) 0.0373(12) C23 0.0234(8) 0.0181(7) 0.0298(9) 0.0038(6) 0.0113(7) 0.0118(6) C24 0.0329(10) 0.0253(8) 0.0303(10) 0.0062(7) 0.0118(8) 0.0167(7) C25 0.0459(12) 0.0293(9) 0.0398(11) 0.0148(8) 0.0194(9) 0.0188(9) C26 0.0435(12) 0.0223(9) 0.0502(13) 0.0107(8) 0.0192(10) 0.0113(8) C27 0.0302(10) 0.0211(8) 0.0426(11) 0.0007(8) 0.0072(8) 0.0077(7) C28 0.0240(8) 0.0222(8) 0.0334(10) 0.0019(7) 0.0095(7) 0.0130(7) C29 0.0432(11) 0.0317(9) 0.0277(10) 0.0045(8) 0.0064(8) 0.0199(9) C30 0.082(2) 0.0605(16) 0.0339(13) -0.0007(11) 0.0202(13) 0.0230(14) C31 0.0544(17) 0.098(2) 0.0617(19) -0.0253(17) -0.0166(14) 0.0493(17) C32 0.0289(9) 0.0261(8) 0.0298(10) 0.0015(7) 0.0046(7) 0.0150(7) C33 0.0333(11) 0.0467(12) 0.0370(11) -0.0014(9) 0.0029(9) 0.0260(9) C34 0.0320(10) 0.0431(11) 0.0340(11) 0.0028(8) 0.0084(8) 0.0193(9) C35 0.0287(9) 0.0192(8) 0.0355(10) 0.0042(7) 0.0166(8) 0.0100(7) C36 0.0286(9) 0.0234(8) 0.0372(10) 0.0037(7) 0.0162(8) 0.0093(7) C37 0.0387(11) 0.0235(9) 0.0420(12) -0.0007(8) 0.0162(9) 0.0089(8) C38 0.0497(13) 0.0208(9) 0.0545(14) 0.0090(9) 0.0248(11) 0.0136(8) C39 0.0517(13) 0.0297(10) 0.0482(13) 0.0159(9) 0.0261(10) 0.0208(9) C40 0.0341(10) 0.0289(9) 0.0378(11) 0.0092(8) 0.0182(8) 0.0161(8) C41 0.0293(10) 0.0278(9) 0.0378(11) 0.0029(8) 0.0088(8) 0.0086(7) C42 0.0483(14) 0.0487(13) 0.0368(12) 0.0016(10) 0.0060(10) 0.0184(11) C43 0.0350(12) 0.0477(13) 0.0599(15) 0.0095(11) 0.0133(11) 0.0190(10) C44 0.0398(11) 0.0364(10) 0.0359(11) 0.0098(8) 0.0157(9) 0.0181(9) C45 0.0479(14) 0.0613(15) 0.0433(13) 0.0158(11) 0.0147(11) 0.0305(12) C46 0.0541(15) 0.0811(19) 0.0411(14) 0.0068(12) 0.0215(12) 0.0337(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 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' B B 0.0090 0.0039 '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' F F 0.0727 0.0534 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 1 0.0757 1 0 -1 0.0342 0 0 1 0.0181 0 0 -1 0.0342 0 -2 1 0.1133 0 2 -1 0.1184 -1 1 -2 0.1211 1 1 -2 0.0568 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 C71 H71A 108.9 . . ? Cl1 C71 H71B 108.9 . . ? Cl2 C71 Cl1 113.53(18) . . ? Cl2 C71 H71A 108.9 . . ? Cl2 C71 H71B 108.9 . . ? H71A C71 H71B 107.7 . . ? C48 C47 C52 113.06(17) . . ? C48 C47 B1 119.51(16) . . ? C52 C47 B1 127.35(16) . . ? F1 C48 C47 119.22(17) . . ? F1 C48 C49 115.85(17) . . ? C49 C48 C47 124.91(18) . . ? F2 C49 C48 121.0(2) . . ? F2 C49 C50 119.82(19) . . ? C48 C49 C50 119.15(19) . . ? F3 C50 C49 120.7(2) . . ? F3 C50 C51 120.8(2) . . ? C51 C50 C49 118.52(19) . . ? F4 C51 C50 119.36(18) . . ? F4 C51 C52 120.37(18) . . ? C50 C51 C52 120.27(18) . . ? F5 C52 C47 121.59(16) . . ? F5 C52 C51 114.46(16) . . ? C51 C52 C47 123.95(17) . . ? C54 C53 C58 112.92(17) . . ? C54 C53 B1 127.84(16) . . ? C58 C53 B1 119.02(15) . . ? F6 C54 C53 121.13(16) . . ? F6 C54 C55 114.93(16) . . ? C55 C54 C53 123.94(17) . . ? F7 C55 C54 120.01(18) . . ? F7 C55 C56 119.96(18) . . ? C56 C55 C54 120.02(17) . . ? F8 C56 C55 120.77(18) . . ? F8 C56 C57 120.49(18) . . ? C55 C56 C57 118.72(17) . . ? F9 C57 C56 119.88(17) . . ? F9 C57 C58 120.87(17) . . ? C58 C57 C56 119.23(17) . . ? F10 C58 C53 118.77(16) . . ? F10 C58 C57 116.12(16) . . ? C57 C58 C53 125.10(17) . . ? C60 C59 B1 117.91(16) . . ? C64 C59 C60 113.67(15) . . ? C64 C59 B1 128.00(16) . . ? F11 C60 C59 119.37(15) . . ? F11 C60 C61 116.36(16) . . ? C61 C60 C59 124.26(17) . . ? F12 C61 C60 120.23(17) . . ? F12 C61 C62 120.29(16) . . ? C62 C61 C60 119.48(18) . . ? F13 C62 C61 120.51(18) . . ? F13 C62 C63 120.41(18) . . ? C61 C62 C63 119.07(16) . . ? F14 C63 C62 119.47(16) . . ? F14 C63 C64 120.71(17) . . ? C62 C63 C64 119.80(17) . . ? F15 C64 C59 121.31(15) . . ? F15 C64 C63 115.02(16) . . ? C59 C64 C63 123.67(17) . . ? C66 C65 C70 113.50(18) . . ? C66 C65 B1 127.18(17) . . ? C70 C65 B1 118.38(17) . . ? F16 C66 C65 121.48(17) . . ? F16 C66 C67 114.82(19) . . ? C65 C66 C67 123.7(2) . . ? F17 C67 C66 120.1(2) . . ? F17 C67 C68 120.32(19) . . ? C68 C67 C66 119.6(2) . . ? F18 C68 C67 120.5(2) . . ? F18 C68 C69 120.0(2) . . ? C67 C68 C69 119.49(19) . . ? F19 C69 C68 120.15(19) . . ? F19 C69 C70 120.9(2) . . ? C68 C69 C70 119.0(2) . . ? F20 C70 C65 119.42(17) . . ? F20 C70 C69 115.74(18) . . ? C69 C70 C65 124.8(2) . . ? C53 B1 C47 103.34(14) . . ? C53 B1 C59 113.40(15) . . ? C53 B1 C65 113.76(14) . . ? C59 B1 C47 112.95(14) . . ? C65 B1 C47 113.97(15) . . ? C65 B1 C59 99.90(13) . . ? C1 N1 C2 109.88(14) . . ? C1 N1 C23 126.66(14) . . ? C2 N1 C23 123.46(14) . . ? C1 N2 C3 109.45(14) . . ? C1 N2 C35 126.78(15) . . ? C3 N2 C35 123.46(15) . . ? N1 C1 C4 123.37(15) . . ? N2 C1 N1 106.72(15) . . ? N2 C1 C4 129.88(15) . . ? N1 C2 H2 126.6 . . ? C3 C2 N1 106.89(15) . . ? C3 C2 H2 126.6 . . ? N2 C3 H3 126.5 . . ? C2 C3 N2 107.06(16) . . ? C2 C3 H3 126.5 . . ? C1 C4 H4 106.0 . . ? C5 C4 C1 112.14(15) . . ? C5 C4 H4 106.0 . . ? C5 C4 C9 112.13(14) . . ? C9 C4 C1 113.73(15) . . ? C9 C4 H4 106.0 . . ? C4 C5 H5 118.5 . . ? C6 C5 C4 123.05(16) . . ? C6 C5 H5 118.5 . . ? C5 C6 H6 118.3 . . ? C5 C6 C7 123.36(17) . . ? C7 C6 H6 118.3 . . ? C8 C7 C6 114.86(15) . . ? C10 C7 C6 122.42(17) . . ? C10 C7 C8 122.72(17) . . ? C7 C8 H8 118.4 . . ? C9 C8 C7 123.18(17) . . ? C9 C8 H8 118.4 . . ? C4 C9 H9 118.4 . . ? C8 C9 C4 123.15(17) . . ? C8 C9 H9 118.4 . . ? C7 C10 C11 122.47(17) . . ? C7 C10 C17 123.36(17) . . ? C11 C10 C17 114.17(15) . . ? C12 C11 C10 120.42(18) . . ? C16 C11 C10 121.11(17) . . ? C16 C11 C12 118.45(18) . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.8 . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.3(2) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 120.1 . . ? C13 C14 C15 119.74(19) . . ? C15 C14 H14 120.1 . . ? C14 C15 H15 120.0 . . ? C14 C15 C16 120.0(2) . . ? C16 C15 H15 120.0 . . ? C11 C16 H16 119.5 . . ? C15 C16 C11 120.91(19) . . ? C15 C16 H16 119.5 . . ? C18 C17 C10 119.3(2) . . ? C22 C17 C10 122.5(2) . . ? C22 C17 C18 118.1(2) . . ? C17 C18 H18 119.5 . . ? C19 C18 C17 120.9(3) . . ? C19 C18 H18 119.5 . . ? C18 C19 H19 119.6 . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19 119.6 . . ? C19 C20 H20 120.3 . . ? C19 C20 C21 119.3(2) . . ? C21 C20 H20 120.3 . . ? C20 C21 H21 119.9 . . ? C20 C21 C22 120.2(3) . . ? C22 C21 H21 119.9 . . ? C17 C22 C21 120.7(3) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 N1 118.17(16) . . ? C24 C23 C28 124.43(17) . . ? C28 C23 N1 117.37(16) . . ? C23 C24 C25 116.36(18) . . ? C23 C24 C29 121.97(17) . . ? C25 C24 C29 121.66(18) . . ? C24 C25 H25 119.5 . . ? C26 C25 C24 121.0(2) . . ? C26 C25 H25 119.5 . . ? C25 C26 H26 119.5 . . ? C27 C26 C25 120.92(19) . . ? C27 C26 H26 119.5 . . ? C26 C27 H27 119.5 . . ? C26 C27 C28 120.99(19) . . ? C28 C27 H27 119.5 . . ? C23 C28 C32 122.13(16) . . ? C27 C28 C23 116.22(18) . . ? C27 C28 C32 121.64(17) . . ? C24 C29 H29 107.5 . . ? C30 C29 C24 112.6(2) . . ? C30 C29 H29 107.5 . . ? C30 C29 C31 111.3(2) . . ? C31 C29 C24 110.28(18) . . ? C31 C29 H29 107.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32 107.8 . . ? C28 C32 C33 111.54(18) . . ? C28 C32 C34 111.24(15) . . ? C33 C32 H32 107.8 . . ? C33 C32 C34 110.61(16) . . ? C34 C32 H32 107.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N2 116.82(17) . . ? C36 C35 C40 124.86(17) . . ? C40 C35 N2 118.23(17) . . ? C35 C36 C37 116.35(19) . . ? C35 C36 C41 123.08(16) . . ? C37 C36 C41 120.55(19) . . ? C36 C37 H37 119.6 . . ? C38 C37 C36 120.7(2) . . ? C38 C37 H37 119.6 . . ? C37 C38 H38 119.5 . . ? C39 C38 C37 120.99(19) . . ? C39 C38 H38 119.5 . . ? C38 C39 H39 119.4 . . ? C38 C39 C40 121.3(2) . . ? C40 C39 H39 119.4 . . ? C35 C40 C39 115.7(2) . . ? C35 C40 C44 123.29(17) . . ? C39 C40 C44 120.9(2) . . ? C36 C41 H41 107.7 . . ? C36 C41 C42 112.50(17) . . ? C36 C41 C43 111.21(19) . . ? C42 C41 H41 107.7 . . ? C42 C41 C43 109.77(19) . . ? C43 C41 H41 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 H44 107.8 . . ? C40 C44 C45 113.40(18) . . ? C40 C44 C46 109.91(19) . . ? C45 C44 H44 107.8 . . ? C45 C44 C46 109.9(2) . . ? C46 C44 H44 107.8 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C71 1.753(3) . ? Cl2 C71 1.744(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? F1 C48 1.355(2) . ? F2 C49 1.343(2) . ? F3 C50 1.340(2) . ? F4 C51 1.353(2) . ? F5 C52 1.353(2) . ? F6 C54 1.355(2) . ? F7 C55 1.350(2) . ? F8 C56 1.337(2) . ? F9 C57 1.344(2) . ? F10 C58 1.357(2) . ? F11 C60 1.347(2) . ? F12 C61 1.350(2) . ? F13 C62 1.344(2) . ? F14 C63 1.341(2) . ? F15 C64 1.348(2) . ? F16 C66 1.347(2) . ? F17 C67 1.344(3) . ? F18 C68 1.342(2) . ? F19 C69 1.341(3) . ? F20 C70 1.347(2) . ? C47 C48 1.390(3) . ? C47 C52 1.393(3) . ? C47 B1 1.658(3) . ? C48 C49 1.379(3) . ? C49 C50 1.384(3) . ? C50 C51 1.373(3) . ? C51 C52 1.379(3) . ? C53 C54 1.388(2) . ? C53 C58 1.392(3) . ? C53 B1 1.646(3) . ? C54 C55 1.386(3) . ? C55 C56 1.370(3) . ? C56 C57 1.379(3) . ? C57 C58 1.372(3) . ? C59 C60 1.398(3) . ? C59 C64 1.383(3) . ? C59 B1 1.657(2) . ? C60 C61 1.379(3) . ? C61 C62 1.371(3) . ? C62 C63 1.376(3) . ? C63 C64 1.390(3) . ? C65 C66 1.389(3) . ? C65 C70 1.391(3) . ? C65 B1 1.657(3) . ? C66 C67 1.395(3) . ? C67 C68 1.373(4) . ? C68 C69 1.375(4) . ? C69 C70 1.382(3) . ? N1 C1 1.343(2) . ? N1 C2 1.378(2) . ? N1 C23 1.448(2) . ? N2 C1 1.340(2) . ? N2 C3 1.386(2) . ? N2 C35 1.457(2) . ? C1 C4 1.512(2) . ? C2 H2 0.9500 . ? C2 C3 1.346(3) . ? C3 H3 0.9500 . ? C4 H4 1.0000 . ? C4 C5 1.501(3) . ? C4 C9 1.505(2) . ? C5 H5 0.9500 . ? C5 C6 1.335(3) . ? C6 H6 0.9500 . ? C6 C7 1.464(2) . ? C7 C8 1.457(3) . ? C7 C10 1.360(3) . ? C8 H8 0.9500 . ? C8 C9 1.337(3) . ? C9 H9 0.9500 . ? C10 C11 1.487(3) . ? C10 C17 1.491(3) . ? C11 C12 1.398(3) . ? C11 C16 1.388(3) . ? C12 H12 0.9500 . ? C12 C13 1.386(3) . ? C13 H13 0.9500 . ? C13 C14 1.379(3) . ? C14 H14 0.9500 . ? C14 C15 1.385(3) . ? C15 H15 0.9500 . ? C15 C16 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.393(3) . ? C17 C22 1.384(3) . ? C18 H18 0.9500 . ? C18 C19 1.379(4) . ? C19 H19 0.9500 . ? C19 C20 1.370(5) . ? C20 H20 0.9500 . ? C20 C21 1.381(5) . ? C21 H21 0.9500 . ? C21 C22 1.394(4) . ? C22 H22 0.9500 . ? C23 C24 1.393(3) . ? C23 C28 1.402(3) . ? C24 C25 1.397(3) . ? C24 C29 1.519(3) . ? C25 H25 0.9500 . ? C25 C26 1.380(3) . ? C26 H26 0.9500 . ? C26 C27 1.378(3) . ? C27 H27 0.9500 . ? C27 C28 1.398(3) . ? C28 C32 1.512(3) . ? C29 H29 1.0000 . ? C29 C30 1.507(3) . ? C29 C31 1.518(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32 1.0000 . ? C32 C33 1.526(3) . ? C32 C34 1.534(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.394(3) . ? C35 C40 1.398(3) . ? C36 C37 1.395(3) . ? C36 C41 1.517(3) . ? C37 H37 0.9500 . ? C37 C38 1.386(3) . ? C38 H38 0.9500 . ? C38 C39 1.373(4) . ? C39 H39 0.9500 . ? C39 C40 1.401(3) . ? C40 C44 1.514(3) . ? C41 H41 1.0000 . ? C41 C42 1.530(3) . ? C41 C43 1.536(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44 1.0000 . ? C44 C45 1.530(3) . ? C44 C46 1.537(3) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 C48 C49 F2 0.8(3) . . . . ? F1 C48 C49 C50 179.7(2) . . . . ? F2 C49 C50 F3 0.7(4) . . . . ? F2 C49 C50 C51 -179.4(2) . . . . ? F3 C50 C51 F4 -0.8(3) . . . . ? F3 C50 C51 C52 178.31(19) . . . . ? F4 C51 C52 F5 -1.9(3) . . . . ? F4 C51 C52 C47 177.72(17) . . . . ? F6 C54 C55 F7 -0.6(3) . . . . ? F6 C54 C55 C56 179.01(17) . . . . ? F7 C55 C56 F8 -2.8(3) . . . . ? F7 C55 C56 C57 178.89(17) . . . . ? F8 C56 C57 F9 2.0(3) . . . . ? F8 C56 C57 C58 -176.80(16) . . . . ? F9 C57 C58 F10 -0.2(2) . . . . ? F9 C57 C58 C53 -179.08(16) . . . . ? F11 C60 C61 F12 -0.9(3) . . . . ? F11 C60 C61 C62 179.61(17) . . . . ? F12 C61 C62 F13 -1.7(3) . . . . ? F12 C61 C62 C63 179.27(17) . . . . ? F13 C62 C63 F14 0.5(3) . . . . ? F13 C62 C63 C64 -177.84(17) . . . . ? F14 C63 C64 F15 1.7(2) . . . . ? F14 C63 C64 C59 -177.76(16) . . . . ? F16 C66 C67 F17 1.1(3) . . . . ? F16 C66 C67 C68 -177.35(16) . . . . ? F17 C67 C68 F18 0.9(3) . . . . ? F17 C67 C68 C69 -178.75(17) . . . . ? F18 C68 C69 F19 1.0(3) . . . . ? F18 C68 C69 C70 -179.76(17) . . . . ? F19 C69 C70 F20 -1.6(3) . . . . ? F19 C69 C70 C65 179.58(17) . . . . ? C47 C48 C49 F2 -177.7(2) . . . . ? C47 C48 C49 C50 1.2(3) . . . . ? C48 C47 C52 F5 -176.52(17) . . . . ? C48 C47 C52 C51 3.9(3) . . . . ? C48 C47 B1 C53 68.1(2) . . . . ? C48 C47 B1 C59 -168.96(17) . . . . ? C48 C47 B1 C65 -55.8(2) . . . . ? C48 C49 C50 F3 -178.2(2) . . . . ? C48 C49 C50 C51 1.6(3) . . . . ? C49 C50 C51 F4 179.31(19) . . . . ? C49 C50 C51 C52 -1.6(3) . . . . ? C50 C51 C52 F5 179.00(18) . . . . ? C50 C51 C52 C47 -1.4(3) . . . . ? C52 C47 C48 F1 177.78(17) . . . . ? C52 C47 C48 C49 -3.8(3) . . . . ? C52 C47 B1 C53 -108.4(2) . . . . ? C52 C47 B1 C59 14.6(3) . . . . ? C52 C47 B1 C65 127.69(19) . . . . ? C53 C54 C55 F7 178.90(17) . . . . ? C53 C54 C55 C56 -1.5(3) . . . . ? C54 C53 C58 F10 179.38(15) . . . . ? C54 C53 C58 C57 -1.7(3) . . . . ? C54 C53 B1 C47 -108.3(2) . . . . ? C54 C53 B1 C59 129.09(18) . . . . ? C54 C53 B1 C65 15.8(3) . . . . ? C54 C55 C56 F8 177.62(17) . . . . ? C54 C55 C56 C57 -0.7(3) . . . . ? C55 C56 C57 F9 -179.63(17) . . . . ? C55 C56 C57 C58 1.5(3) . . . . ? C56 C57 C58 F10 178.66(16) . . . . ? C56 C57 C58 C53 -0.3(3) . . . . ? C58 C53 C54 F6 -177.95(15) . . . . ? C58 C53 C54 C55 2.6(3) . . . . ? C58 C53 B1 C47 65.86(19) . . . . ? C58 C53 B1 C59 -56.8(2) . . . . ? C58 C53 B1 C65 -170.04(15) . . . . ? C59 C60 C61 F12 178.95(17) . . . . ? C59 C60 C61 C62 -0.6(3) . . . . ? C60 C59 C64 F15 178.49(15) . . . . ? C60 C59 C64 C63 -2.1(3) . . . . ? C60 C59 B1 C47 53.9(2) . . . . ? C60 C59 B1 C53 171.01(15) . . . . ? C60 C59 B1 C65 -67.58(19) . . . . ? C60 C61 C62 F13 177.85(17) . . . . ? C60 C61 C62 C63 -1.2(3) . . . . ? C61 C62 C63 F14 179.56(17) . . . . ? C61 C62 C63 C64 1.2(3) . . . . ? C62 C63 C64 F15 179.95(16) . . . . ? C62 C63 C64 C59 0.5(3) . . . . ? C64 C59 C60 F11 -178.01(15) . . . . ? C64 C59 C60 C61 2.2(3) . . . . ? C64 C59 B1 C47 -134.08(18) . . . . ? C64 C59 B1 C53 -16.9(2) . . . . ? C64 C59 B1 C65 104.5(2) . . . . ? C65 C66 C67 F17 178.94(17) . . . . ? C65 C66 C67 C68 0.5(3) . . . . ? C66 C65 C70 F20 -179.00(15) . . . . ? C66 C65 C70 C69 -0.2(3) . . . . ? C66 C65 B1 C47 -16.9(2) . . . . ? C66 C65 B1 C53 -135.06(18) . . . . ? C66 C65 B1 C59 103.80(19) . . . . ? C66 C67 C68 F18 179.34(17) . . . . ? C66 C67 C68 C69 -0.4(3) . . . . ? C67 C68 C69 F19 -179.30(17) . . . . ? C67 C68 C69 C70 -0.1(3) . . . . ? C68 C69 C70 F20 179.21(16) . . . . ? C68 C69 C70 C65 0.3(3) . . . . ? C70 C65 C66 F16 177.48(15) . . . . ? C70 C65 C66 C67 -0.3(3) . . . . ? C70 C65 B1 C47 174.98(15) . . . . ? C70 C65 B1 C53 56.8(2) . . . . ? C70 C65 B1 C59 -64.31(19) . . . . ? B1 C47 C48 F1 0.8(3) . . . . ? B1 C47 C48 C49 179.2(2) . . . . ? B1 C47 C52 F5 0.1(3) . . . . ? B1 C47 C52 C51 -179.43(18) . . . . ? B1 C53 C54 F6 -3.5(3) . . . . ? B1 C53 C54 C55 177.03(17) . . . . ? B1 C53 C58 F10 4.4(2) . . . . ? B1 C53 C58 C57 -176.70(16) . . . . ? B1 C59 C60 F11 -4.9(2) . . . . ? B1 C59 C60 C61 175.32(17) . . . . ? B1 C59 C64 F15 6.2(3) . . . . ? B1 C59 C64 C63 -174.46(17) . . . . ? B1 C65 C66 F16 8.9(3) . . . . ? B1 C65 C66 C67 -168.87(17) . . . . ? B1 C65 C70 F20 -9.3(2) . . . . ? B1 C65 C70 C69 169.52(17) . . . . ? N1 C1 C4 C5 105.04(19) . . . . ? N1 C1 C4 C9 -126.43(18) . . . . ? N1 C2 C3 N2 -0.2(2) . . . . ? N1 C23 C24 C25 177.70(16) . . . . ? N1 C23 C24 C29 -0.9(3) . . . . ? N1 C23 C28 C27 -176.01(15) . . . . ? N1 C23 C28 C32 4.1(2) . . . . ? N2 C1 C4 C5 -72.9(2) . . . . ? N2 C1 C4 C9 55.6(3) . . . . ? N2 C35 C36 C37 -178.96(17) . . . . ? N2 C35 C36 C41 -0.3(3) . . . . ? N2 C35 C40 C39 179.15(17) . . . . ? N2 C35 C40 C44 3.2(3) . . . . ? C1 N1 C2 C3 0.4(2) . . . . ? C1 N1 C23 C24 83.4(2) . . . . ? C1 N1 C23 C28 -98.7(2) . . . . ? C1 N2 C3 C2 -0.1(2) . . . . ? C1 N2 C35 C36 -86.6(2) . . . . ? C1 N2 C35 C40 96.7(2) . . . . ? C1 C4 C5 C6 134.66(19) . . . . ? C1 C4 C9 C8 -134.41(19) . . . . ? C2 N1 C1 N2 -0.5(2) . . . . ? C2 N1 C1 C4 -178.88(16) . . . . ? C2 N1 C23 C24 -96.1(2) . . . . ? C2 N1 C23 C28 81.8(2) . . . . ? C3 N2 C1 N1 0.4(2) . . . . ? C3 N2 C1 C4 178.61(18) . . . . ? C3 N2 C35 C36 86.3(2) . . . . ? C3 N2 C35 C40 -90.4(2) . . . . ? C4 C5 C6 C7 -2.4(3) . . . . ? C5 C4 C9 C8 -5.9(3) . . . . ? C5 C6 C7 C8 -0.6(3) . . . . ? C5 C6 C7 C10 179.14(19) . . . . ? C6 C7 C8 C9 0.0(3) . . . . ? C6 C7 C10 C11 6.6(3) . . . . ? C6 C7 C10 C17 -173.59(19) . . . . ? C7 C8 C9 C4 3.5(3) . . . . ? C7 C10 C11 C12 -127.0(2) . . . . ? C7 C10 C11 C16 54.4(3) . . . . ? C7 C10 C17 C18 -119.5(2) . . . . ? C7 C10 C17 C22 64.2(3) . . . . ? C8 C7 C10 C11 -173.68(18) . . . . ? C8 C7 C10 C17 6.1(3) . . . . ? C9 C4 C5 C6 5.3(3) . . . . ? C10 C7 C8 C9 -179.7(2) . . . . ? C10 C11 C12 C13 179.70(19) . . . . ? C10 C11 C16 C15 -179.53(17) . . . . ? C10 C17 C18 C19 -177.8(3) . . . . ? C10 C17 C22 C21 176.3(2) . . . . ? C11 C10 C17 C18 60.3(3) . . . . ? C11 C10 C17 C22 -115.9(2) . . . . ? C11 C12 C13 C14 0.1(3) . . . . ? C12 C11 C16 C15 1.8(3) . . . . ? C12 C13 C14 C15 1.3(3) . . . . ? C13 C14 C15 C16 -1.2(3) . . . . ? C14 C15 C16 C11 -0.4(3) . . . . ? C16 C11 C12 C13 -1.7(3) . . . . ? C17 C10 C11 C12 53.1(3) . . . . ? C17 C10 C11 C16 -125.5(2) . . . . ? C17 C18 C19 C20 1.3(5) . . . . ? C18 C17 C22 C21 0.0(4) . . . . ? C18 C19 C20 C21 0.2(5) . . . . ? C19 C20 C21 C22 -1.5(5) . . . . ? C20 C21 C22 C17 1.4(4) . . . . ? C22 C17 C18 C19 -1.4(4) . . . . ? C23 N1 C1 N2 179.94(16) . . . . ? C23 N1 C1 C4 1.6(3) . . . . ? C23 N1 C2 C3 -179.98(17) . . . . ? C23 C24 C25 C26 -2.0(3) . . . . ? C23 C24 C29 C30 -136.6(2) . . . . ? C23 C24 C29 C31 98.4(3) . . . . ? C23 C28 C32 C33 138.55(17) . . . . ? C23 C28 C32 C34 -97.4(2) . . . . ? C24 C23 C28 C27 1.8(3) . . . . ? C24 C23 C28 C32 -178.14(17) . . . . ? C24 C25 C26 C27 2.3(3) . . . . ? C25 C24 C29 C30 44.8(3) . . . . ? C25 C24 C29 C31 -80.2(3) . . . . ? C25 C26 C27 C28 -0.4(3) . . . . ? C26 C27 C28 C23 -1.5(3) . . . . ? C26 C27 C28 C32 178.39(19) . . . . ? C27 C28 C32 C33 -41.3(2) . . . . ? C27 C28 C32 C34 82.7(2) . . . . ? C28 C23 C24 C25 0.0(3) . . . . ? C28 C23 C24 C29 -178.70(17) . . . . ? C29 C24 C25 C26 176.7(2) . . . . ? C35 N2 C1 N1 174.11(17) . . . . ? C35 N2 C1 C4 -7.6(3) . . . . ? C35 N2 C3 C2 -174.10(18) . . . . ? C35 C36 C37 C38 0.2(3) . . . . ? C35 C36 C41 C42 142.9(2) . . . . ? C35 C36 C41 C43 -93.4(2) . . . . ? C35 C40 C44 C45 -139.4(2) . . . . ? C35 C40 C44 C46 97.2(2) . . . . ? C36 C35 C40 C39 2.7(3) . . . . ? C36 C35 C40 C44 -173.21(18) . . . . ? C36 C37 C38 C39 1.6(3) . . . . ? C37 C36 C41 C42 -38.5(3) . . . . ? C37 C36 C41 C43 85.1(2) . . . . ? C37 C38 C39 C40 -1.3(4) . . . . ? C38 C39 C40 C35 -0.7(3) . . . . ? C38 C39 C40 C44 175.3(2) . . . . ? C39 C40 C44 C45 44.9(3) . . . . ? C39 C40 C44 C46 -78.5(3) . . . . ? C40 C35 C36 C37 -2.5(3) . . . . ? C40 C35 C36 C41 176.16(18) . . . . ? C41 C36 C37 C38 -178.4(2) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.0002 0.0006 1.0001 -0.1198 0.0460 -0.0410 1.0002 -0.0006 -1.0001 0.1198 -0.0460 0.0410 0.0005 -0.0004 1.0000 0.0047 0.0796 -0.0047 -0.0005 0.0004 -1.0000 -0.0047 -0.0796 0.0047 -0.0012 -1.9989 0.9997 -0.1638 0.0489 0.1799 0.0012 1.9989 -0.9997 0.1638 -0.0489 -0.1799 -1.0010 1.0010 -1.9997 -0.0497 -0.1773 -0.1193 1.0006 0.9990 -1.9999 0.1993 -0.1103 -0.0466