#------------------------------------------------------------------------------ #$Date: 2021-11-09 01:14:31 +0200 (Tue, 09 Nov 2021) $ #$Revision: 270530 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/51/1565135.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_1565135 loop_ _publ_author_name 'Zhu, Zhaoyang' 'Zhang, Xue' 'Guo, Xing' 'Wu, Qinghua' 'Li, Zhongxin' 'Yu, Changjiang' 'Hao, Erhong' 'Jiao, Lijuan' 'Zhao, Jianzhang' _publ_section_title ; Orthogonally aligned cyclic BODIPY arrays with long-lived triplet excited states as efficient heavy-atom-free photosensitizers ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC04893G _journal_year 2021 _chemical_formula_moiety '0.05(C72 H60 B3 Cl3 N6 O3)' _chemical_formula_sum 'C H B Cl N O0.02' _chemical_formula_weight 73.65 _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 _audit_block_doi 10.5517/ccdc.csd.cc2299wl _audit_creation_date 2018-12-22 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-05-13 deposited with the CCDC. 2021-10-28 downloaded from the CCDC. ; _cell_angle_alpha 102.574(2) _cell_angle_beta 90.075(2) _cell_angle_gamma 90.745(2) _cell_formula_units_Z 44 _cell_length_a 12.2187(5) _cell_length_b 13.6971(5) _cell_length_c 20.7232(8) _cell_measurement_reflns_used 9737 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 27.43 _cell_measurement_theta_min 3.02 _cell_volume 3384.8(2) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_unetI/netI 0.0356 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 140792 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.562 _diffrn_reflns_theta_min 2.778 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.590 _exptl_crystal_F_000 1592 _refine_diff_density_max 2.991 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.141 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.715 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 803 _refine_ls_number_reflns 15543 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.715 _refine_ls_R_factor_all 0.1697 _refine_ls_R_factor_gt 0.1224 _refine_ls_shift/su_max 1.230 _refine_ls_shift/su_mean 0.169 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1059P)^2^+2.5699P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3463 _refine_ls_wR_factor_ref 0.3693 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9541 _reflns_number_total 15543 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc04893g2.cif _cod_data_source_block 20181221a _cod_database_code 1565135 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(H55)=Sof(Cl0A)=1-FVAR(1) Sof(H57)=Sof(Cl3)=FVAR(1) 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C18(H18), C20(H20), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C37(H37), C38(H38), C42(H42), C44(H44), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C61(H61), C62(H62), C66(H66), C68(H68) 3.b Idealised Me refined as rotating group: C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C46(H46A,H46B, H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C70(H70A,H70B,H70C), C71(H71A, H71B,H71C), C72(H72A,H72B,H72C) ; _shelx_res_file ; TITL 20181221a_a.res in P-1 20181221a.res created by SHELXL-2018/3 at 10:11:39 on 22-Dec-2018 REM Old TITL 20181221a in P-1 REM SHELXT solution in P-1: R1 0.215, Rweak 0.029, Alpha 0.067 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C77 B3 N9 Cl3 CELL 0.71073 12.2187 13.6971 20.7232 102.574 90.075 90.745 ZERR 44 0.0005 0.0005 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H B N Cl O UNIT 44 44 44 44 44 1 L.S. 2 PLAN 2 TEMP 0 BOND list 4 fmap 2 53 ACTA REM REM REM WGHT 0.105900 2.569900 FVAR 0.57311 0.90842 CL1 5 -0.039947 0.089159 0.764829 11.00000 0.06990 0.11314 = 0.07436 0.04711 0.00750 -0.01342 CL2 5 0.549368 0.125411 0.580756 11.00000 0.10185 0.05208 = 0.06706 0.00108 0.01561 0.00229 O1 6 0.159092 0.239771 0.750447 11.00000 0.05667 0.03964 = 0.03855 0.00461 -0.00220 -0.00030 O2 6 0.368340 0.254054 0.681778 11.00000 0.04536 0.04721 = 0.04459 0.01395 -0.00436 -0.00573 O3 6 0.356450 0.360957 0.829663 11.00000 0.05446 0.04471 = 0.04176 0.01212 0.00728 0.00011 N1 4 0.024894 0.162535 0.661053 11.00000 0.04939 0.04967 = 0.04139 0.00745 -0.00137 -0.01073 N2 4 0.200209 0.234838 0.632817 11.00000 0.04355 0.04199 = 0.03840 0.00682 -0.00349 -0.00731 N3 4 0.545779 0.317853 0.643918 11.00000 0.04194 0.04607 = 0.04010 0.00658 -0.00214 0.00167 N4 4 0.457476 0.407934 0.747490 11.00000 0.04109 0.04408 = 0.03912 0.00976 0.00125 -0.00022 N5 4 0.253805 0.466989 0.926483 11.00000 0.04904 0.04470 = 0.03351 0.00775 0.00148 -0.00757 N6 4 0.159433 0.392631 0.821635 11.00000 0.05359 0.03967 = 0.03255 0.00537 0.00256 -0.00242 C1 1 0.209276 0.073347 0.679392 11.00000 0.05535 0.04093 = 0.05214 0.00830 -0.00112 -0.01021 C2 1 0.227543 0.035877 0.736097 11.00000 0.07202 0.05077 = 0.07352 0.02189 0.00375 -0.00115 AFIX 43 H2 2 0.200506 0.070247 0.776499 11.00000 -1.20000 AFIX 0 C3 1 0.285448 -0.051915 0.733181 11.00000 0.09183 0.06013 = 0.10602 0.03950 0.00107 -0.00168 AFIX 43 H3 2 0.295125 -0.076232 0.771317 11.00000 -1.20000 AFIX 0 C4 1 0.328411 -0.102890 0.674307 11.00000 0.11333 0.04707 = 0.14413 0.02132 0.00811 0.01204 AFIX 43 H4 2 0.367451 -0.161267 0.672441 11.00000 -1.20000 AFIX 0 C5 1 0.312920 -0.066505 0.618440 11.00000 0.12100 0.06088 = 0.10901 -0.01265 0.01912 0.02002 AFIX 43 H5 2 0.342930 -0.099904 0.578639 11.00000 -1.20000 AFIX 0 C6 1 0.253004 0.019582 0.620450 11.00000 0.09061 0.05343 = 0.06537 -0.00801 0.00337 0.00429 AFIX 43 H6 2 0.241854 0.041780 0.581646 11.00000 -1.20000 AFIX 0 C7 1 -0.059585 0.128578 0.693349 11.00000 0.05873 0.05710 = 0.05031 0.00796 0.00114 -0.01311 C8 1 -0.156995 0.130717 0.660851 11.00000 0.05079 0.07353 = 0.06586 0.01250 0.00392 -0.01781 AFIX 43 H8 2 -0.225418 0.111457 0.673700 11.00000 -1.20000 AFIX 0 C9 1 -0.133610 0.166831 0.605715 11.00000 0.04600 0.06834 = 0.06102 0.01021 -0.00820 -0.01250 AFIX 43 H9 2 -0.183681 0.175829 0.573744 11.00000 -1.20000 AFIX 0 C10 1 -0.022007 0.187684 0.605880 11.00000 0.05092 0.05103 = 0.04438 0.00458 -0.00542 -0.00890 C11 1 0.041414 0.235402 0.563802 11.00000 0.05145 0.05221 = 0.04101 0.00445 -0.00556 -0.01143 C12 1 0.148807 0.258251 0.577794 11.00000 0.04811 0.05106 = 0.03645 0.00574 -0.00611 -0.00669 C13 1 0.227463 0.309748 0.546340 11.00000 0.05725 0.06297 = 0.04913 0.02270 -0.00731 -0.00840 AFIX 43 H13 2 0.215997 0.333690 0.508221 11.00000 -1.20000 AFIX 0 C14 1 0.321244 0.317736 0.581369 11.00000 0.04713 0.06219 = 0.05408 0.02180 -0.00564 -0.01323 AFIX 43 H14 2 0.385705 0.348792 0.572148 11.00000 -1.20000 AFIX 0 C15 1 0.303691 0.269683 0.635451 11.00000 0.04518 0.04049 = 0.04171 0.00523 -0.00042 -0.00468 C16 1 -0.013051 0.263783 0.505479 11.00000 0.04648 0.06853 = 0.04863 0.01716 -0.00753 -0.01459 C17 1 -0.013682 0.194050 0.444634 11.00000 0.07073 0.09029 = 0.04596 0.00782 -0.01362 -0.01927 C18 1 -0.057699 0.225171 0.390284 11.00000 0.09389 0.12723 = 0.04798 0.00993 -0.02118 -0.02795 AFIX 43 H18 2 -0.057226 0.180829 0.349329 11.00000 -1.20000 AFIX 0 C19 1 -0.101753 0.318396 0.394482 11.00000 0.08114 0.11301 = 0.06522 0.04244 -0.02137 -0.03080 C20 1 -0.103942 0.381200 0.455621 11.00000 0.07147 0.08958 = 0.08058 0.04154 -0.01883 -0.02107 AFIX 43 H20 2 -0.136031 0.443472 0.459914 11.00000 -1.20000 AFIX 0 C21 1 -0.060043 0.355650 0.511724 11.00000 0.05553 0.06944 = 0.06116 0.02679 -0.00841 -0.01566 C22 1 0.027115 0.090724 0.438059 11.00000 0.12961 0.09321 = 0.06044 -0.01282 -0.01714 0.00374 AFIX 137 H22A 2 0.091611 0.092146 0.464771 11.00000 -1.50000 H22B 2 0.044456 0.063100 0.392638 11.00000 -1.50000 H22C 2 -0.028346 0.050120 0.452518 11.00000 -1.50000 AFIX 0 C23 1 -0.143628 0.349161 0.333905 11.00000 0.13345 0.20233 = 0.09312 0.08554 -0.04509 -0.05113 AFIX 137 H23A 2 -0.084403 0.350027 0.303632 11.00000 -1.50000 H23B 2 -0.174282 0.414749 0.346204 11.00000 -1.50000 H23C 2 -0.199004 0.302400 0.313105 11.00000 -1.50000 AFIX 0 C24 1 -0.065697 0.428448 0.578079 11.00000 0.08166 0.06552 = 0.07787 0.02087 -0.00422 -0.00255 AFIX 137 H24A 2 -0.113659 0.401834 0.606843 11.00000 -1.50000 H24B 2 -0.093176 0.491225 0.572073 11.00000 -1.50000 H24C 2 0.006163 0.438416 0.597371 11.00000 -1.50000 AFIX 0 C25 1 0.539356 0.232953 0.745583 11.00000 0.05054 0.05283 = 0.04121 0.01023 0.00375 0.00907 C26 1 0.633809 0.270561 0.780558 11.00000 0.06756 0.06944 = 0.06149 0.01072 -0.01727 0.00846 AFIX 43 H26 2 0.658858 0.334419 0.779025 11.00000 -1.20000 AFIX 0 C27 1 0.691108 0.215591 0.817378 11.00000 0.08302 0.10366 = 0.07598 0.01695 -0.02238 0.02585 AFIX 43 H27 2 0.753008 0.243089 0.841001 11.00000 -1.20000 AFIX 0 C28 1 0.657464 0.121756 0.819207 11.00000 0.11377 0.12211 = 0.08265 0.04709 0.00350 0.05618 AFIX 43 H28 2 0.696351 0.084681 0.843924 11.00000 -1.20000 AFIX 0 C29 1 0.563727 0.080385 0.783730 11.00000 0.10361 0.08272 = 0.12481 0.05592 0.01014 0.02219 AFIX 43 H29 2 0.540022 0.015923 0.784691 11.00000 -1.20000 AFIX 0 C30 1 0.507296 0.136883 0.747397 11.00000 0.07234 0.06493 = 0.09471 0.03767 -0.00445 0.00479 AFIX 43 H30 2 0.445786 0.109186 0.723438 11.00000 -1.20000 AFIX 0 C31 1 0.581353 0.249319 0.590611 11.00000 0.05180 0.05301 = 0.04424 0.00704 -0.00057 0.00715 C32 1 0.638404 0.293032 0.547879 11.00000 0.06430 0.06770 = 0.04193 0.00807 0.00857 0.00694 AFIX 43 H32 2 0.669395 0.261094 0.508018 11.00000 -1.20000 AFIX 0 C33 1 0.641091 0.394211 0.575499 11.00000 0.05647 0.06295 = 0.05155 0.01806 0.01227 0.00003 AFIX 43 H33 2 0.675414 0.443240 0.557651 11.00000 -1.20000 AFIX 0 C34 1 0.584146 0.410046 0.634082 11.00000 0.04054 0.05214 = 0.04434 0.01280 -0.00076 -0.00378 C35 1 0.559287 0.499871 0.679903 11.00000 0.03899 0.05209 = 0.04659 0.01232 -0.00085 -0.00445 C36 1 0.498791 0.497096 0.734675 11.00000 0.04110 0.04418 = 0.05140 0.01027 0.00084 -0.00365 C37 1 0.469118 0.576227 0.788388 11.00000 0.06588 0.04309 = 0.06115 0.00296 0.01339 -0.00536 AFIX 43 H37 2 0.486455 0.643664 0.792715 11.00000 -1.20000 AFIX 0 C38 1 0.411553 0.536048 0.831741 11.00000 0.06854 0.04765 = 0.05759 -0.00024 0.02081 -0.00314 AFIX 43 H38 2 0.382556 0.570567 0.871549 11.00000 -1.20000 AFIX 0 C39 1 0.403082 0.430760 0.805510 11.00000 0.04572 0.04487 = 0.04152 0.00582 0.00068 -0.00015 C40 1 0.596979 0.597901 0.665920 11.00000 0.05895 0.04819 = 0.07127 0.00950 0.02335 -0.00556 C41 1 0.530661 0.641746 0.624186 11.00000 0.09005 0.06592 = 0.08557 0.03744 0.02238 0.01310 C42 1 0.561430 0.732306 0.611985 11.00000 0.12997 0.07475 = 0.13595 0.05292 0.04340 0.00915 AFIX 43 H42 2 0.516208 0.761577 0.585621 11.00000 -1.20000 AFIX 0 C43 1 0.652278 0.780311 0.635811 11.00000 0.13752 0.06753 = 0.18177 0.03987 0.07455 0.00609 C44 1 0.720748 0.738172 0.676902 11.00000 0.08818 0.07736 = 0.19738 -0.00270 0.05058 -0.03290 AFIX 43 H44 2 0.784025 0.772128 0.694661 11.00000 -1.20000 AFIX 0 C45 1 0.693135 0.642157 0.691668 11.00000 0.05666 0.06849 = 0.12500 0.00350 0.00854 -0.01769 C46 1 0.425348 0.590490 0.594652 11.00000 0.10674 0.11743 = 0.12525 0.05997 -0.02661 0.00695 AFIX 137 H46A 2 0.442555 0.530724 0.562701 11.00000 -1.50000 H46B 2 0.385521 0.634861 0.573493 11.00000 -1.50000 H46C 2 0.381458 0.573515 0.629109 11.00000 -1.50000 AFIX 0 C47 1 0.690921 0.882755 0.627668 11.00000 0.28455 0.07386 = 0.40623 0.07860 0.20075 -0.00911 AFIX 137 H47A 2 0.736498 0.875376 0.589256 11.00000 -1.50000 H47B 2 0.731991 0.915142 0.666077 11.00000 -1.50000 H47C 2 0.628700 0.922504 0.622524 11.00000 -1.50000 AFIX 0 C48 1 0.763257 0.596601 0.734130 11.00000 0.08807 0.11078 = 0.18814 -0.00807 -0.05130 -0.02484 AFIX 137 H48A 2 0.721281 0.583773 0.770599 11.00000 -1.50000 H48B 2 0.822987 0.641377 0.750571 11.00000 -1.50000 H48C 2 0.791426 0.534817 0.709028 11.00000 -1.50000 AFIX 0 C49 1 0.228586 0.270632 0.892051 11.00000 0.07174 0.04864 = 0.03477 0.01165 -0.00333 -0.00811 C50 1 0.125876 0.251317 0.914852 11.00000 0.08765 0.07800 = 0.05750 0.02022 0.00133 -0.02669 AFIX 43 H50 2 0.071710 0.299091 0.917516 11.00000 -1.20000 AFIX 0 C51 1 0.101729 0.162073 0.933893 11.00000 0.14342 0.10018 = 0.07891 0.04259 -0.00275 -0.05519 AFIX 43 H51 2 0.031481 0.151230 0.948321 11.00000 -1.20000 AFIX 0 C52 1 0.176153 0.092408 0.931969 11.00000 0.22615 0.07618 = 0.06841 0.04007 -0.03151 -0.06221 AFIX 43 H52 2 0.158722 0.033557 0.945343 11.00000 -1.20000 AFIX 0 C53 1 0.281856 0.108261 0.909500 11.00000 0.17779 0.05741 = 0.07897 0.02961 -0.02973 -0.00162 AFIX 43 H53 2 0.334882 0.059659 0.907723 11.00000 -1.20000 AFIX 0 C54 1 0.307408 0.197462 0.889738 11.00000 0.10132 0.06039 = 0.06059 0.02021 -0.00908 0.00419 AFIX 43 H54 2 0.377555 0.207830 0.874970 11.00000 -1.20000 AFIX 0 C55 1 0.318512 0.484911 0.980854 11.00000 0.05265 0.05375 = 0.04198 0.00971 0.00277 -0.00894 PART 2 AFIX 43 H55 2 0.367798 0.439417 0.991226 -21.00000 -1.20000 AFIX 0 PART 0 C56 1 0.301946 0.579496 1.018984 11.00000 0.06529 0.06217 = 0.04048 -0.00125 -0.00310 -0.01166 AFIX 43 H56 2 0.336942 0.608316 1.058556 11.00000 -1.20000 AFIX 0 C57 1 0.223759 0.622688 0.987097 11.00000 0.06822 0.04705 = 0.04519 -0.00244 0.00506 -0.00451 PART 1 AFIX 43 H57 2 0.195875 0.686613 1.001237 21.00000 -1.20000 AFIX 0 PART 0 C58 1 0.193608 0.553788 0.929814 11.00000 0.05384 0.04301 = 0.03566 0.00769 0.00684 -0.00260 C59 1 0.119432 0.562378 0.878951 11.00000 0.05758 0.04185 = 0.03884 0.00927 0.00824 -0.00412 C60 1 0.104447 0.484106 0.826475 11.00000 0.05748 0.04648 = 0.03658 0.01032 0.00265 0.00414 C61 1 0.032251 0.472587 0.771829 11.00000 0.07522 0.05274 = 0.04357 0.00803 -0.00750 0.01099 AFIX 43 H61 2 -0.013508 0.521547 0.762552 11.00000 -1.20000 AFIX 0 C62 1 0.041080 0.378072 0.735274 11.00000 0.07268 0.05650 = 0.04267 0.00365 -0.01391 0.00598 AFIX 43 H62 2 0.002094 0.350022 0.697010 11.00000 -1.20000 AFIX 0 C63 1 0.121972 0.329789 0.766929 11.00000 0.05443 0.04307 = 0.03589 0.00508 0.00353 -0.00319 C64 1 0.054914 0.655378 0.881431 11.00000 0.06917 0.04114 = 0.03894 0.00517 0.00496 0.00002 C65 1 -0.053886 0.658466 0.901119 11.00000 0.07309 0.05396 = 0.05553 0.01460 0.01328 0.00757 C66 1 -0.114795 0.743290 0.899660 11.00000 0.08224 0.07313 = 0.07734 0.01835 0.01729 0.02480 AFIX 43 H66 2 -0.187979 0.745213 0.912090 11.00000 -1.20000 AFIX 0 C67 1 -0.068343 0.824423 0.880092 11.00000 0.11711 0.05705 = 0.07552 0.01995 0.00650 0.02542 C68 1 0.039654 0.821021 0.861640 11.00000 0.11726 0.04653 = 0.07433 0.02584 0.01019 0.00568 AFIX 43 H68 2 0.070750 0.875860 0.848484 11.00000 -1.20000 AFIX 0 C69 1 0.103705 0.738532 0.862003 11.00000 0.08357 0.05438 = 0.04893 0.01778 0.00083 -0.00203 C70 1 -0.108015 0.570342 0.923414 11.00000 0.08298 0.07222 = 0.09345 0.02503 0.03276 0.00188 AFIX 137 H70A 2 -0.132180 0.521454 0.885368 11.00000 -1.50000 H70B 2 -0.169700 0.593488 0.950893 11.00000 -1.50000 H70C 2 -0.056202 0.540671 0.948002 11.00000 -1.50000 AFIX 0 C71 1 -0.141072 0.914644 0.878065 11.00000 0.18943 0.09481 = 0.16097 0.05216 0.03045 0.07764 AFIX 137 H71A 2 -0.174637 0.905726 0.835231 11.00000 -1.50000 H71B 2 -0.097074 0.974687 0.886536 11.00000 -1.50000 H71C 2 -0.196863 0.919783 0.911165 11.00000 -1.50000 AFIX 0 C72 1 0.220798 0.738226 0.842377 11.00000 0.08436 0.08715 = 0.08976 0.04482 0.00364 -0.01584 AFIX 137 H72A 2 0.266293 0.738874 0.880275 11.00000 -1.50000 H72B 2 0.236687 0.796438 0.825122 11.00000 -1.50000 H72C 2 0.234971 0.679169 0.809070 11.00000 -1.50000 AFIX 0 B1 3 0.148491 0.176311 0.681991 11.00000 0.04862 0.04392 = 0.03703 0.00459 -0.00090 -0.00755 B2 3 0.476907 0.300468 0.703847 11.00000 0.04066 0.04228 = 0.03862 0.00665 -0.00215 -0.00145 B3 3 0.251177 0.371566 0.868366 11.00000 0.05306 0.04655 = 0.03700 0.00976 0.00438 -0.00138 PART 1 CL3 5 0.406778 0.398489 0.997674 21.00000 0.06027 0.06288 = 0.06309 0.01153 -0.01812 -0.00196 PART 0 PART 2 CL0A 5 0.171365 0.740100 1.018517 -21.00000 0.06269 0.03941 = 0.02789 -0.01881 -0.01400 0.01737 HKLF 4 REM 20181221a_a.res in P-1 REM wR2 = 0.3693, GooF = S = 1.715, Restrained GooF = 1.715 for all data REM R1 = 0.1224 for 9541 Fo > 4sig(Fo) and 0.1697 for all 15543 data REM 803 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 2.991, deepest hole -0.479, 1-sigma level 0.141 Q1 1 0.5331 0.8523 0.8682 11.00000 0.05 2.99 Q2 1 0.4446 0.8209 0.9860 11.00000 0.05 2.59 ; _shelx_res_checksum 84222 _olex2_submission_special_instructions 'No special instructions were received' 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 -0.03995(13) 0.08916(15) 0.76483(8) 0.0819(5) Uani 1 1 d . . . . . Cl2 Cl 0.54937(15) 0.12541(11) 0.58076(8) 0.0755(5) Uani 1 1 d . . . . . O1 O 0.1591(3) 0.2398(2) 0.75045(15) 0.0456(7) Uani 1 1 d . . . . . O2 O 0.3683(3) 0.2541(2) 0.68178(15) 0.0452(7) Uani 1 1 d . . . . . O3 O 0.3564(3) 0.3610(2) 0.82966(15) 0.0466(8) Uani 1 1 d . . . . . N1 N 0.0249(3) 0.1625(3) 0.66105(19) 0.0473(9) Uani 1 1 d . . . . . N2 N 0.2002(3) 0.2348(3) 0.63282(18) 0.0417(8) Uani 1 1 d . . . . . N3 N 0.5458(3) 0.3179(3) 0.64392(18) 0.0431(9) Uani 1 1 d . . . . . N4 N 0.4575(3) 0.4079(3) 0.74749(18) 0.0413(8) Uani 1 1 d . . . . . N5 N 0.2538(3) 0.4670(3) 0.92648(18) 0.0426(9) Uani 1 1 d . . . . . N6 N 0.1594(3) 0.3926(3) 0.82163(17) 0.0423(8) Uani 1 1 d . . . . . C1 C 0.2093(4) 0.0733(4) 0.6794(3) 0.0499(11) Uani 1 1 d . . . . . C2 C 0.2275(5) 0.0359(4) 0.7361(3) 0.0642(14) Uani 1 1 d . . . . . H2 H 0.200506 0.070247 0.776499 0.077 Uiso 1 1 calc R . . . . C3 C 0.2854(6) -0.0519(5) 0.7332(4) 0.083(2) Uani 1 1 d . . . . . H3 H 0.295125 -0.076232 0.771317 0.099 Uiso 1 1 calc R . . . . C4 C 0.3284(7) -0.1029(5) 0.6743(5) 0.101(3) Uani 1 1 d . . . . . H4 H 0.367451 -0.161267 0.672441 0.122 Uiso 1 1 calc R . . . . C5 C 0.3129(7) -0.0665(6) 0.6184(5) 0.102(3) Uani 1 1 d . . . . . H5 H 0.342930 -0.099904 0.578639 0.122 Uiso 1 1 calc R . . . . C6 C 0.2530(6) 0.0196(4) 0.6205(3) 0.0730(17) Uani 1 1 d . . . . . H6 H 0.241854 0.041780 0.581646 0.088 Uiso 1 1 calc R . . . . C7 C -0.0596(4) 0.1286(4) 0.6933(3) 0.0561(13) Uani 1 1 d . . . . . C8 C -0.1570(5) 0.1307(5) 0.6609(3) 0.0640(15) Uani 1 1 d . . . . . H8 H -0.225418 0.111457 0.673700 0.077 Uiso 1 1 calc R . . . . C9 C -0.1336(4) 0.1668(4) 0.6057(3) 0.0592(13) Uani 1 1 d . . . . . H9 H -0.183681 0.175829 0.573744 0.071 Uiso 1 1 calc R . . . . C10 C -0.0220(4) 0.1877(4) 0.6059(2) 0.0497(11) Uani 1 1 d . . . . . C11 C 0.0414(4) 0.2354(4) 0.5638(2) 0.0492(11) Uani 1 1 d . . . . . C12 C 0.1488(4) 0.2583(4) 0.5778(2) 0.0459(10) Uani 1 1 d . . . . . C13 C 0.2275(4) 0.3097(4) 0.5463(3) 0.0549(12) Uani 1 1 d . . . . . H13 H 0.215997 0.333690 0.508221 0.066 Uiso 1 1 calc R . . . . C14 C 0.3212(4) 0.3177(4) 0.5814(3) 0.0532(12) Uani 1 1 d . . . . . H14 H 0.385705 0.348792 0.572148 0.064 Uiso 1 1 calc R . . . . C15 C 0.3037(4) 0.2697(3) 0.6355(2) 0.0431(10) Uani 1 1 d . . . . . C16 C -0.0131(4) 0.2638(4) 0.5055(3) 0.0540(12) Uani 1 1 d . . . . . C17 C -0.0137(5) 0.1940(5) 0.4446(3) 0.0703(16) Uani 1 1 d . . . . . C18 C -0.0577(6) 0.2252(7) 0.3903(3) 0.091(2) Uani 1 1 d . . . . . H18 H -0.057226 0.180829 0.349329 0.110 Uiso 1 1 calc R . . . . C19 C -0.1018(6) 0.3184(7) 0.3945(3) 0.083(2) Uani 1 1 d . . . . . C20 C -0.1039(5) 0.3812(6) 0.4556(4) 0.0773(18) Uani 1 1 d . . . . . H20 H -0.136031 0.443472 0.459914 0.093 Uiso 1 1 calc R . . . . C21 C -0.0600(5) 0.3556(4) 0.5117(3) 0.0603(14) Uani 1 1 d . . . . . C22 C 0.0271(8) 0.0907(6) 0.4381(4) 0.099(2) Uani 1 1 d . . . . . H22A H 0.091611 0.092146 0.464771 0.148 Uiso 1 1 calc GR . . . . H22B H 0.044456 0.063100 0.392638 0.148 Uiso 1 1 calc GR . . . . H22C H -0.028346 0.050120 0.452518 0.148 Uiso 1 1 calc GR . . . . C23 C -0.1436(9) 0.3492(9) 0.3339(5) 0.135(4) Uani 1 1 d . . . . . H23A H -0.084403 0.350027 0.303632 0.203 Uiso 1 1 calc GR . . . . H23B H -0.174282 0.414749 0.346204 0.203 Uiso 1 1 calc GR . . . . H23C H -0.199004 0.302400 0.313105 0.203 Uiso 1 1 calc GR . . . . C24 C -0.0657(6) 0.4284(5) 0.5781(3) 0.0743(17) Uani 1 1 d . . . . . H24A H -0.113659 0.401834 0.606843 0.111 Uiso 1 1 calc GR . . . . H24B H -0.093176 0.491225 0.572073 0.111 Uiso 1 1 calc GR . . . . H24C H 0.006163 0.438416 0.597371 0.111 Uiso 1 1 calc GR . . . . C25 C 0.5394(4) 0.2330(4) 0.7456(2) 0.0481(11) Uani 1 1 d . . . . . C26 C 0.6338(5) 0.2706(5) 0.7806(3) 0.0666(15) Uani 1 1 d . . . . . H26 H 0.658858 0.334419 0.779025 0.080 Uiso 1 1 calc R . . . . C27 C 0.6911(6) 0.2156(7) 0.8174(4) 0.088(2) Uani 1 1 d . . . . . H27 H 0.753008 0.243089 0.841001 0.105 Uiso 1 1 calc R . . . . C28 C 0.6575(8) 0.1218(7) 0.8192(4) 0.102(3) Uani 1 1 d . . . . . H28 H 0.696351 0.084681 0.843924 0.122 Uiso 1 1 calc R . . . . C29 C 0.5637(7) 0.0804(6) 0.7837(5) 0.098(2) Uani 1 1 d . . . . . H29 H 0.540022 0.015923 0.784691 0.118 Uiso 1 1 calc R . . . . C30 C 0.5073(6) 0.1369(5) 0.7474(4) 0.0742(17) Uani 1 1 d . . . . . H30 H 0.445786 0.109186 0.723438 0.089 Uiso 1 1 calc R . . . . C31 C 0.5814(4) 0.2493(4) 0.5906(2) 0.0502(11) Uani 1 1 d . . . . . C32 C 0.6384(5) 0.2930(4) 0.5479(3) 0.0585(13) Uani 1 1 d . . . . . H32 H 0.669395 0.261094 0.508018 0.070 Uiso 1 1 calc R . . . . C33 C 0.6411(4) 0.3942(4) 0.5755(3) 0.0561(13) Uani 1 1 d . . . . . H33 H 0.675414 0.443240 0.557651 0.067 Uiso 1 1 calc R . . . . C34 C 0.5841(4) 0.4100(4) 0.6341(2) 0.0454(10) Uani 1 1 d . . . . . C35 C 0.5593(4) 0.4999(4) 0.6799(2) 0.0457(10) Uani 1 1 d . . . . . C36 C 0.4988(4) 0.4971(3) 0.7347(2) 0.0456(10) Uani 1 1 d . . . . . C37 C 0.4691(4) 0.5762(4) 0.7884(3) 0.0580(13) Uani 1 1 d . . . . . H37 H 0.486455 0.643664 0.792715 0.070 Uiso 1 1 calc R . . . . C38 C 0.4116(5) 0.5360(4) 0.8317(3) 0.0597(14) Uani 1 1 d . . . . . H38 H 0.382556 0.570567 0.871549 0.072 Uiso 1 1 calc R . . . . C39 C 0.4031(4) 0.4308(3) 0.8055(2) 0.0446(10) Uani 1 1 d . . . . . C40 C 0.5970(5) 0.5979(4) 0.6659(3) 0.0600(14) Uani 1 1 d . . . . . C41 C 0.5307(6) 0.6417(5) 0.6242(4) 0.0772(18) Uani 1 1 d . . . . . C42 C 0.5614(9) 0.7323(6) 0.6120(5) 0.109(3) Uani 1 1 d . . . . . H42 H 0.516208 0.761577 0.585621 0.131 Uiso 1 1 calc R . . . . C43 C 0.6523(11) 0.7803(7) 0.6358(7) 0.127(4) Uani 1 1 d . . . . . C44 C 0.7207(8) 0.7382(7) 0.6769(6) 0.126(4) Uani 1 1 d . . . . . H44 H 0.784025 0.772128 0.694661 0.151 Uiso 1 1 calc R . . . . C45 C 0.6931(5) 0.6422(5) 0.6917(4) 0.086(2) Uani 1 1 d . . . . . C46 C 0.4253(7) 0.5905(7) 0.5947(5) 0.111(3) Uani 1 1 d . . . . . H46A H 0.442555 0.530724 0.562701 0.167 Uiso 1 1 calc GR . . . . H46B H 0.385521 0.634861 0.573493 0.167 Uiso 1 1 calc GR . . . . H46C H 0.381458 0.573515 0.629109 0.167 Uiso 1 1 calc GR . . . . C47 C 0.6909(15) 0.8828(8) 0.6277(10) 0.251(11) Uani 1 1 d . . . . . H47A H 0.736498 0.875376 0.589256 0.376 Uiso 1 1 calc GR . . . . H47B H 0.731991 0.915142 0.666077 0.376 Uiso 1 1 calc GR . . . . H47C H 0.628700 0.922504 0.622524 0.376 Uiso 1 1 calc GR . . . . C48 C 0.7633(7) 0.5966(7) 0.7341(6) 0.135(4) Uani 1 1 d . . . . . H48A H 0.721281 0.583773 0.770599 0.203 Uiso 1 1 calc GR . . . . H48B H 0.822987 0.641377 0.750571 0.203 Uiso 1 1 calc GR . . . . H48C H 0.791426 0.534817 0.709028 0.203 Uiso 1 1 calc GR . . . . C49 C 0.2286(5) 0.2706(4) 0.8921(2) 0.0514(12) Uani 1 1 d . . . . . C50 C 0.1259(6) 0.2513(5) 0.9149(3) 0.0738(17) Uani 1 1 d . . . . . H50 H 0.071710 0.299091 0.917516 0.089 Uiso 1 1 calc R . . . . C51 C 0.1017(9) 0.1621(7) 0.9339(4) 0.104(3) Uani 1 1 d . . . . . H51 H 0.031481 0.151230 0.948321 0.125 Uiso 1 1 calc R . . . . C52 C 0.1762(12) 0.0924(7) 0.9320(4) 0.120(4) Uani 1 1 d . . . . . H52 H 0.158722 0.033557 0.945343 0.145 Uiso 1 1 calc R . . . . C53 C 0.2819(10) 0.1083(5) 0.9095(4) 0.103(3) Uani 1 1 d . . . . . H53 H 0.334882 0.059659 0.907723 0.123 Uiso 1 1 calc R . . . . C54 C 0.3074(6) 0.1975(5) 0.8897(3) 0.0730(17) Uani 1 1 d . . . . . H54 H 0.377555 0.207830 0.874970 0.088 Uiso 1 1 calc R . . . . C55 C 0.3185(4) 0.4849(4) 0.9809(2) 0.0497(11) Uani 1 1 d . . . . . H55 H 0.367798 0.439417 0.991226 0.060 Uiso 0.092(4) 1 calc R . P A 2 C56 C 0.3019(5) 0.5795(4) 1.0190(3) 0.0580(13) Uani 1 1 d . . . . . H56 H 0.336942 0.608316 1.058556 0.070 Uiso 1 1 calc R . . . . C57 C 0.2238(5) 0.6227(4) 0.9871(2) 0.0554(13) Uani 1 1 d . . . . . H57 H 0.195875 0.686613 1.001237 0.067 Uiso 0.908(4) 1 calc R . P A 1 C58 C 0.1936(4) 0.5538(3) 0.9298(2) 0.0443(10) Uani 1 1 d . . . . . C59 C 0.1194(4) 0.5624(3) 0.8790(2) 0.0461(11) Uani 1 1 d . . . . . C60 C 0.1044(4) 0.4841(4) 0.8265(2) 0.0466(11) Uani 1 1 d . . . . . C61 C 0.0323(5) 0.4726(4) 0.7718(2) 0.0575(13) Uani 1 1 d . . . . . H61 H -0.013508 0.521547 0.762552 0.069 Uiso 1 1 calc R . . . . C62 C 0.0411(5) 0.3781(4) 0.7353(3) 0.0583(13) Uani 1 1 d . . . . . H62 H 0.002094 0.350022 0.697010 0.070 Uiso 1 1 calc R . . . . C63 C 0.1220(4) 0.3298(3) 0.7669(2) 0.0450(10) Uani 1 1 d . . . . . C64 C 0.0549(4) 0.6554(4) 0.8814(2) 0.0503(11) Uani 1 1 d . . . . . C65 C -0.0539(5) 0.6585(4) 0.9011(3) 0.0604(14) Uani 1 1 d . . . . . C66 C -0.1148(6) 0.7433(5) 0.8997(3) 0.0770(18) Uani 1 1 d . . . . . H66 H -0.187979 0.745213 0.912090 0.092 Uiso 1 1 calc R . . . . C67 C -0.0683(7) 0.8244(5) 0.8801(4) 0.082(2) Uani 1 1 d . . . . . C68 C 0.0397(7) 0.8210(4) 0.8616(3) 0.0774(19) Uani 1 1 d . . . . . H68 H 0.070750 0.875860 0.848484 0.093 Uiso 1 1 calc R . . . . C69 C 0.1037(5) 0.7385(4) 0.8620(3) 0.0613(14) Uani 1 1 d . . . . . C70 C -0.1080(6) 0.5703(5) 0.9234(4) 0.082(2) Uani 1 1 d . . . . . H70A H -0.132180 0.521454 0.885368 0.123 Uiso 1 1 calc GR . . . . H70B H -0.169700 0.593488 0.950893 0.123 Uiso 1 1 calc GR . . . . H70C H -0.056202 0.540671 0.948002 0.123 Uiso 1 1 calc GR . . . . C71 C -0.1411(10) 0.9146(7) 0.8781(6) 0.144(4) Uani 1 1 d . . . . . H71A H -0.174637 0.905726 0.835231 0.216 Uiso 1 1 calc GR . . . . H71B H -0.097074 0.974687 0.886536 0.216 Uiso 1 1 calc GR . . . . H71C H -0.196863 0.919783 0.911165 0.216 Uiso 1 1 calc GR . . . . C72 C 0.2208(6) 0.7382(6) 0.8424(4) 0.0833(19) Uani 1 1 d . . . . . H72A H 0.266293 0.738874 0.880275 0.125 Uiso 1 1 calc GR . . . . H72B H 0.236687 0.796438 0.825122 0.125 Uiso 1 1 calc GR . . . . H72C H 0.234971 0.679169 0.809070 0.125 Uiso 1 1 calc GR . . . . B1 B 0.1485(4) 0.1763(4) 0.6820(3) 0.0439(11) Uani 1 1 d . . . . . B2 B 0.4769(4) 0.3005(4) 0.7038(3) 0.0409(11) Uani 1 1 d . . . . . B3 B 0.2512(5) 0.3716(4) 0.8684(3) 0.0455(12) Uani 1 1 d . . . . . Cl3 Cl 0.40678(12) 0.39849(12) 0.99767(8) 0.0625(5) Uani 0.908(4) 1 d . . P A 1 Cl0A Cl 0.1714(11) 0.7401(9) 1.0185(5) 0.047(4) Uani 0.092(4) 1 d . . P A 2 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 0.0699(9) 0.1131(14) 0.0744(10) 0.0471(10) 0.0075(8) -0.0134(9) Cl2 0.1018(12) 0.0521(8) 0.0671(9) 0.0011(7) 0.0156(8) 0.0023(7) O1 0.0567(19) 0.0396(17) 0.0385(16) 0.0046(13) -0.0022(14) -0.0003(14) O2 0.0454(17) 0.0472(18) 0.0446(17) 0.0139(14) -0.0044(14) -0.0057(14) O3 0.0545(19) 0.0447(18) 0.0418(17) 0.0121(14) 0.0073(14) 0.0001(14) N1 0.049(2) 0.050(2) 0.041(2) 0.0074(17) -0.0014(17) -0.0107(17) N2 0.044(2) 0.042(2) 0.0384(19) 0.0068(16) -0.0035(15) -0.0073(16) N3 0.042(2) 0.046(2) 0.040(2) 0.0066(16) -0.0021(16) 0.0017(16) N4 0.0411(19) 0.044(2) 0.039(2) 0.0098(16) 0.0012(15) -0.0002(15) N5 0.049(2) 0.045(2) 0.0335(19) 0.0077(16) 0.0015(16) -0.0076(16) N6 0.054(2) 0.040(2) 0.0326(18) 0.0054(15) 0.0026(16) -0.0024(16) C1 0.055(3) 0.041(2) 0.052(3) 0.008(2) -0.001(2) -0.010(2) C2 0.072(4) 0.051(3) 0.074(4) 0.022(3) 0.004(3) -0.001(3) C3 0.092(5) 0.060(4) 0.106(6) 0.039(4) 0.001(4) -0.002(3) C4 0.113(6) 0.047(4) 0.144(8) 0.021(5) 0.008(6) 0.012(4) C5 0.121(6) 0.061(4) 0.109(6) -0.013(4) 0.019(5) 0.020(4) C6 0.091(4) 0.053(3) 0.065(4) -0.008(3) 0.003(3) 0.004(3) C7 0.059(3) 0.057(3) 0.050(3) 0.008(2) 0.001(2) -0.013(2) C8 0.051(3) 0.074(4) 0.066(3) 0.013(3) 0.004(3) -0.018(3) C9 0.046(3) 0.068(3) 0.061(3) 0.010(3) -0.008(2) -0.012(2) C10 0.051(3) 0.051(3) 0.044(3) 0.005(2) -0.005(2) -0.009(2) C11 0.051(3) 0.052(3) 0.041(2) 0.004(2) -0.006(2) -0.011(2) C12 0.048(3) 0.051(3) 0.036(2) 0.006(2) -0.0061(19) -0.007(2) C13 0.057(3) 0.063(3) 0.049(3) 0.023(2) -0.007(2) -0.008(2) C14 0.047(3) 0.062(3) 0.054(3) 0.022(2) -0.006(2) -0.013(2) C15 0.045(2) 0.040(2) 0.042(2) 0.0052(19) -0.0004(19) -0.0047(19) C16 0.046(3) 0.069(3) 0.049(3) 0.017(2) -0.008(2) -0.015(2) C17 0.071(4) 0.090(5) 0.046(3) 0.008(3) -0.014(3) -0.019(3) C18 0.094(5) 0.127(7) 0.048(3) 0.010(4) -0.021(3) -0.028(5) C19 0.081(4) 0.113(6) 0.065(4) 0.042(4) -0.021(3) -0.031(4) C20 0.071(4) 0.090(5) 0.081(5) 0.042(4) -0.019(3) -0.021(3) C21 0.056(3) 0.069(4) 0.061(3) 0.027(3) -0.008(2) -0.016(3) C22 0.130(7) 0.093(6) 0.060(4) -0.013(4) -0.017(4) 0.004(5) C23 0.133(8) 0.202(11) 0.093(6) 0.086(7) -0.045(6) -0.051(7) C24 0.082(4) 0.066(4) 0.078(4) 0.021(3) -0.004(3) -0.003(3) C25 0.051(3) 0.053(3) 0.041(2) 0.010(2) 0.004(2) 0.009(2) C26 0.068(4) 0.069(4) 0.061(3) 0.011(3) -0.017(3) 0.008(3) C27 0.083(5) 0.104(6) 0.076(4) 0.017(4) -0.022(4) 0.026(4) C28 0.114(7) 0.122(7) 0.083(5) 0.047(5) 0.003(5) 0.056(6) C29 0.104(6) 0.083(5) 0.125(7) 0.056(5) 0.010(5) 0.022(4) C30 0.072(4) 0.065(4) 0.095(5) 0.038(3) -0.004(3) 0.005(3) C31 0.052(3) 0.053(3) 0.044(3) 0.007(2) -0.001(2) 0.007(2) C32 0.064(3) 0.068(4) 0.042(3) 0.008(2) 0.009(2) 0.007(3) C33 0.056(3) 0.063(3) 0.052(3) 0.018(2) 0.012(2) 0.000(2) C34 0.041(2) 0.052(3) 0.044(2) 0.013(2) -0.0008(19) -0.004(2) C35 0.039(2) 0.052(3) 0.047(3) 0.012(2) -0.0008(19) -0.0044(19) C36 0.041(2) 0.044(2) 0.051(3) 0.010(2) 0.001(2) -0.0037(19) C37 0.066(3) 0.043(3) 0.061(3) 0.003(2) 0.013(3) -0.005(2) C38 0.069(3) 0.048(3) 0.058(3) 0.000(2) 0.021(3) -0.003(2) C39 0.046(2) 0.045(3) 0.042(2) 0.006(2) 0.0007(19) -0.0001(19) C40 0.059(3) 0.048(3) 0.071(3) 0.010(3) 0.023(3) -0.006(2) C41 0.090(5) 0.066(4) 0.086(5) 0.037(3) 0.022(4) 0.013(3) C42 0.130(8) 0.075(5) 0.136(8) 0.053(5) 0.043(6) 0.009(5) C43 0.138(9) 0.068(5) 0.182(11) 0.040(6) 0.075(8) 0.006(6) C44 0.088(6) 0.077(5) 0.197(11) -0.003(6) 0.051(7) -0.033(5) C45 0.057(4) 0.068(4) 0.125(6) 0.003(4) 0.009(4) -0.018(3) C46 0.107(6) 0.117(7) 0.125(7) 0.060(6) -0.027(5) 0.007(5) C47 0.285(18) 0.074(7) 0.41(3) 0.079(11) 0.201(19) -0.009(9) C48 0.088(6) 0.111(7) 0.188(11) -0.008(7) -0.051(6) -0.025(5) C49 0.072(3) 0.049(3) 0.035(2) 0.012(2) -0.003(2) -0.008(2) C50 0.088(4) 0.078(4) 0.058(3) 0.020(3) 0.001(3) -0.027(3) C51 0.143(8) 0.100(6) 0.079(5) 0.043(5) -0.003(5) -0.055(6) C52 0.226(12) 0.076(5) 0.068(5) 0.040(4) -0.032(6) -0.062(7) C53 0.178(9) 0.057(4) 0.079(5) 0.030(4) -0.030(5) -0.002(5) C54 0.101(5) 0.060(3) 0.061(3) 0.020(3) -0.009(3) 0.004(3) C55 0.053(3) 0.054(3) 0.042(3) 0.010(2) 0.003(2) -0.009(2) C56 0.065(3) 0.062(3) 0.040(3) -0.001(2) -0.003(2) -0.012(3) C57 0.068(3) 0.047(3) 0.045(3) -0.002(2) 0.005(2) -0.005(2) C58 0.054(3) 0.043(2) 0.036(2) 0.0077(19) 0.0068(19) -0.003(2) C59 0.058(3) 0.042(2) 0.039(2) 0.0093(19) 0.008(2) -0.004(2) C60 0.057(3) 0.046(3) 0.037(2) 0.010(2) 0.003(2) 0.004(2) C61 0.075(4) 0.053(3) 0.044(3) 0.008(2) -0.007(2) 0.011(3) C62 0.073(3) 0.057(3) 0.043(3) 0.004(2) -0.014(2) 0.006(3) C63 0.054(3) 0.043(3) 0.036(2) 0.0051(19) 0.0035(19) -0.003(2) C64 0.069(3) 0.041(3) 0.039(2) 0.0052(19) 0.005(2) 0.000(2) C65 0.073(4) 0.054(3) 0.056(3) 0.015(2) 0.013(3) 0.008(3) C66 0.082(4) 0.073(4) 0.077(4) 0.018(3) 0.017(3) 0.025(3) C67 0.117(6) 0.057(4) 0.076(4) 0.020(3) 0.007(4) 0.025(4) C68 0.117(6) 0.047(3) 0.074(4) 0.026(3) 0.010(4) 0.006(3) C69 0.084(4) 0.054(3) 0.049(3) 0.018(2) 0.001(3) -0.002(3) C70 0.083(4) 0.072(4) 0.093(5) 0.025(4) 0.033(4) 0.002(3) C71 0.189(11) 0.095(6) 0.161(10) 0.052(7) 0.030(8) 0.078(7) C72 0.084(5) 0.087(5) 0.090(5) 0.045(4) 0.004(4) -0.016(4) B1 0.049(3) 0.044(3) 0.037(3) 0.005(2) -0.001(2) -0.008(2) B2 0.041(3) 0.042(3) 0.039(3) 0.007(2) -0.002(2) -0.001(2) B3 0.053(3) 0.047(3) 0.037(3) 0.010(2) 0.004(2) -0.001(2) Cl3 0.0603(9) 0.0629(9) 0.0631(9) 0.0115(7) -0.0181(7) -0.0020(7) Cl0A 0.063(8) 0.039(7) 0.028(6) -0.019(4) -0.014(5) 0.017(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C63 O1 B1 123.0(4) . . ? C15 O2 B2 129.6(4) . . ? C39 O3 B3 125.4(4) . . ? C7 N1 C10 105.3(4) . . ? C7 N1 B1 128.5(4) . . ? C10 N1 B1 126.1(4) . . ? C12 N2 B1 126.5(4) . . ? C15 N2 C12 108.2(4) . . ? C15 N2 B1 125.3(4) . . ? C31 N3 C34 105.1(4) . . ? C31 N3 B2 128.8(4) . . ? C34 N3 B2 126.2(4) . . ? C36 N4 B2 125.6(4) . . ? C39 N4 C36 107.5(4) . . ? C39 N4 B2 126.8(4) . . ? C55 N5 C58 105.9(4) . . ? C55 N5 B3 127.8(4) . . ? C58 N5 B3 126.2(4) . . ? C60 N6 B3 126.2(4) . . ? C63 N6 C60 107.1(4) . . ? C63 N6 B3 126.6(4) . . ? C2 C1 C6 116.9(5) . . ? C2 C1 B1 122.2(5) . . ? C6 C1 B1 120.8(5) . . ? C3 C2 C1 121.3(6) . . ? C4 C3 C2 120.5(7) . . ? C5 C4 C3 119.1(7) . . ? C4 C5 C6 120.9(7) . . ? C5 C6 C1 121.4(7) . . ? N1 C7 Cl1 121.8(4) . . ? N1 C7 C8 111.5(5) . . ? C8 C7 Cl1 126.7(4) . . ? C7 C8 C9 106.4(5) . . ? C8 C9 C10 108.1(5) . . ? N1 C10 C9 108.7(4) . . ? N1 C10 C11 120.7(4) . . ? C9 C10 C11 130.4(5) . . ? C10 C11 C16 119.1(4) . . ? C12 C11 C10 120.2(4) . . ? C12 C11 C16 120.7(4) . . ? N2 C12 C13 107.2(4) . . ? C11 C12 N2 121.6(4) . . ? C11 C12 C13 131.2(5) . . ? C14 C13 C12 108.2(4) . . ? C13 C14 C15 107.6(4) . . ? O2 C15 N2 119.2(4) . . ? O2 C15 C14 131.9(4) . . ? N2 C15 C14 108.9(4) . . ? C17 C16 C11 118.3(5) . . ? C21 C16 C11 120.5(5) . . ? C21 C16 C17 121.1(5) . . ? C16 C17 C22 122.1(6) . . ? C18 C17 C16 117.0(7) . . ? C18 C17 C22 120.9(6) . . ? C19 C18 C17 123.1(7) . . ? C18 C19 C23 120.7(8) . . ? C20 C19 C18 117.2(6) . . ? C20 C19 C23 122.0(9) . . ? C19 C20 C21 122.7(7) . . ? C16 C21 C24 121.3(5) . . ? C20 C21 C16 118.7(6) . . ? C20 C21 C24 120.0(6) . . ? C26 C25 B2 119.2(5) . . ? C30 C25 C26 117.2(5) . . ? C30 C25 B2 123.5(5) . . ? C27 C26 C25 121.7(7) . . ? C28 C27 C26 120.1(7) . . ? C29 C28 C27 119.9(7) . . ? C28 C29 C30 119.0(8) . . ? C25 C30 C29 122.0(7) . . ? N3 C31 Cl2 121.3(4) . . ? N3 C31 C32 111.9(5) . . ? C32 C31 Cl2 126.8(4) . . ? C31 C32 C33 106.3(5) . . ? C34 C33 C32 108.2(5) . . ? N3 C34 C35 120.6(4) . . ? C33 C34 N3 108.6(4) . . ? C33 C34 C35 130.8(5) . . ? C34 C35 C40 119.1(4) . . ? C36 C35 C34 120.2(4) . . ? C36 C35 C40 120.6(4) . . ? N4 C36 C37 107.9(4) . . ? C35 C36 N4 122.3(4) . . ? C35 C36 C37 129.8(5) . . ? C38 C37 C36 107.9(5) . . ? C37 C38 C39 107.6(4) . . ? O3 C39 N4 120.6(4) . . ? O3 C39 C38 130.2(4) . . ? N4 C39 C38 109.1(4) . . ? C41 C40 C35 117.6(5) . . ? C45 C40 C35 121.0(6) . . ? C45 C40 C41 121.3(6) . . ? C40 C41 C46 120.7(6) . . ? C42 C41 C40 118.9(8) . . ? C42 C41 C46 120.3(8) . . ? C43 C42 C41 123.2(10) . . ? C42 C43 C44 119.2(8) . . ? C42 C43 C47 127.2(14) . . ? C44 C43 C47 113.5(14) . . ? C43 C44 C45 120.4(8) . . ? C40 C45 C44 116.8(8) . . ? C40 C45 C48 121.7(7) . . ? C44 C45 C48 121.4(8) . . ? C50 C49 C54 117.2(6) . . ? C50 C49 B3 119.8(5) . . ? C54 C49 B3 123.0(5) . . ? C49 C50 C51 121.6(8) . . ? C52 C51 C50 121.6(9) . . ? C51 C52 C53 119.2(7) . . ? C52 C53 C54 119.9(8) . . ? C49 C54 C53 120.5(8) . . ? N5 C55 C56 111.2(5) . . ? N5 C55 Cl3 122.4(4) . . ? C56 C55 Cl3 126.4(4) . . ? C55 C56 C57 106.6(5) . . ? C56 C57 Cl0A 123.4(5) . . ? C58 C57 C56 107.8(5) . . ? C58 C57 Cl0A 128.7(6) . . ? N5 C58 C59 121.1(4) . . ? C57 C58 N5 108.5(4) . . ? C57 C58 C59 130.4(5) . . ? C58 C59 C64 121.8(4) . . ? C60 C59 C58 119.7(4) . . ? C60 C59 C64 118.5(4) . . ? N6 C60 C61 107.6(4) . . ? C59 C60 N6 121.9(4) . . ? C59 C60 C61 130.3(5) . . ? C62 C61 C60 108.4(5) . . ? C61 C62 C63 106.8(4) . . ? O1 C63 N6 120.1(4) . . ? O1 C63 C62 129.8(4) . . ? N6 C63 C62 110.0(4) . . ? C65 C64 C59 119.7(4) . . ? C65 C64 C69 120.2(5) . . ? C69 C64 C59 120.1(5) . . ? C64 C65 C70 121.2(5) . . ? C66 C65 C64 119.2(5) . . ? C66 C65 C70 119.6(6) . . ? C67 C66 C65 121.1(6) . . ? C66 C67 C68 119.2(6) . . ? C66 C67 C71 118.4(8) . . ? C68 C67 C71 122.4(7) . . ? C67 C68 C69 122.1(6) . . ? C64 C69 C72 121.3(5) . . ? C68 C69 C64 118.3(6) . . ? C68 C69 C72 120.4(6) . . ? O1 B1 N1 110.3(4) . . ? O1 B1 N2 108.3(4) . . ? O1 B1 C1 108.8(4) . . ? N1 B1 C1 113.4(4) . . ? N2 B1 N1 104.6(4) . . ? N2 B1 C1 111.4(4) . . ? O2 B2 N3 111.1(4) . . ? O2 B2 N4 108.4(4) . . ? O2 B2 C25 109.6(4) . . ? N3 B2 C25 112.1(4) . . ? N4 B2 N3 105.1(4) . . ? N4 B2 C25 110.4(4) . . ? O3 B3 N5 111.6(4) . . ? O3 B3 N6 107.3(4) . . ? O3 B3 C49 108.3(4) . . ? N5 B3 C49 113.5(4) . . ? N6 B3 N5 104.4(4) . . ? N6 B3 C49 111.6(4) . . ? 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 C7 1.701(6) . ? Cl2 C31 1.705(5) . ? O1 C63 1.294(6) . ? O1 B1 1.498(6) . ? O2 C15 1.297(5) . ? O2 B2 1.491(6) . ? O3 C39 1.298(6) . ? O3 B3 1.509(6) . ? N1 C7 1.362(6) . ? N1 C10 1.389(6) . ? N1 B1 1.568(7) . ? N2 C12 1.400(6) . ? N2 C15 1.343(6) . ? N2 B1 1.557(6) . ? N3 C31 1.360(6) . ? N3 C34 1.397(6) . ? N3 B2 1.560(6) . ? N4 C36 1.394(6) . ? N4 C39 1.352(6) . ? N4 B2 1.572(6) . ? N5 C55 1.352(6) . ? N5 C58 1.395(6) . ? N5 B3 1.573(6) . ? N6 C60 1.414(6) . ? N6 C63 1.341(6) . ? N6 B3 1.551(7) . ? C1 C2 1.400(8) . ? C1 C6 1.393(8) . ? C1 B1 1.593(8) . ? C2 C3 1.393(9) . ? C3 C4 1.375(12) . ? C4 C5 1.370(12) . ? C5 C6 1.389(10) . ? C7 C8 1.371(8) . ? C8 C9 1.369(8) . ? C9 C10 1.389(7) . ? C10 C11 1.423(7) . ? C11 C12 1.361(7) . ? C11 C16 1.505(7) . ? C12 C13 1.425(7) . ? C13 C14 1.346(7) . ? C14 C15 1.433(7) . ? C16 C17 1.406(8) . ? C16 C21 1.370(8) . ? C17 C18 1.397(9) . ? C17 C22 1.485(10) . ? C18 C19 1.377(11) . ? C19 C20 1.368(10) . ? C19 C23 1.500(10) . ? C20 C21 1.394(8) . ? C21 C24 1.515(9) . ? C25 C26 1.394(8) . ? C25 C30 1.376(8) . ? C25 B2 1.597(7) . ? C26 C27 1.379(9) . ? C27 C28 1.353(12) . ? C28 C29 1.405(13) . ? C29 C30 1.381(10) . ? C31 C32 1.360(7) . ? C32 C33 1.379(8) . ? C33 C34 1.377(7) . ? C34 C35 1.418(7) . ? C35 C36 1.363(7) . ? C35 C40 1.501(7) . ? C36 C37 1.425(7) . ? C37 C38 1.346(8) . ? C38 C39 1.429(7) . ? C40 C41 1.415(9) . ? C40 C45 1.368(9) . ? C41 C42 1.367(10) . ? C41 C46 1.520(11) . ? C42 C43 1.322(15) . ? C43 C44 1.408(16) . ? C43 C47 1.519(12) . ? C44 C45 1.449(12) . ? C45 C48 1.466(13) . ? C49 C50 1.384(8) . ? C49 C54 1.392(8) . ? C49 B3 1.586(7) . ? C50 C51 1.392(10) . ? C51 C52 1.321(14) . ? C52 C53 1.404(15) . ? C53 C54 1.402(10) . ? C55 C56 1.380(7) . ? C55 Cl3 1.702(5) . ? C56 C57 1.372(8) . ? C57 C58 1.392(7) . ? C57 Cl0A 1.730(12) . ? C58 C59 1.414(7) . ? C59 C60 1.361(7) . ? C59 C64 1.498(7) . ? C60 C61 1.415(7) . ? C61 C62 1.356(7) . ? C62 C63 1.431(7) . ? C64 C65 1.390(8) . ? C64 C69 1.413(7) . ? C65 C66 1.394(8) . ? C65 C70 1.527(8) . ? C66 C67 1.379(10) . ? C67 C68 1.373(10) . ? C67 C71 1.539(10) . ? C68 C69 1.384(8) . ? C69 C72 1.488(9) . ?