#------------------------------------------------------------------------------ #$Date: 2024-12-06 18:25:34 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296365 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572705.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_1572705 loop_ _publ_author_name 'Jin, Ke' 'Xiao, Zuo' 'Xie, Huidong' 'Shen, Xingxing' 'Wang, Jizheng' 'Chen, Xiangyu' 'Wang, Zhijie' 'Zhao, Zujin' 'Yan, Keyou' 'Ding, Yong' 'Ding, Liming' _publ_section_title ; Tether-entangled conjugated helices. ; _journal_issue 41 _journal_name_full 'Chemical science' _journal_page_first 17128 _journal_page_last 17149 _journal_paper_doi 10.1039/d4sc04796f _journal_volume 15 _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_moiety '3(C0.5 H Cl), C46 H44 F2 N4, 0.5(C1 H2 Cl1)' _chemical_formula_sum 'C48 H48 Cl3.5 F2 N4' _chemical_formula_weight 842.98 _space_group_crystal_system tetragonal _space_group_IT_number 96 _space_group_name_Hall 'P 4nw 2abw' _space_group_name_H-M_alt 'P 43 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2022-08-25 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-05-11 deposited with the CCDC. 2024-09-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 15.9463(3) _cell_length_b 15.9463(3) _cell_length_c 35.1878(11) _cell_measurement_reflns_used 9786 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 24.92 _cell_measurement_theta_min 2.51 _cell_volume 8947.7(4) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _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 170.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_unetI/netI 0.0240 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_number 123102 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.125 _diffrn_reflns_theta_min 1.897 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.280 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.7066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1136 before and 0.0608 after correction. The Ratio of minimum to maximum transmission is 0.9478. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.252 _exptl_crystal_description block _exptl_crystal_F_000 3532 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _refine_diff_density_max 1.223 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.098 _refine_ls_abs_structure_details ; Flack x determined using 3171 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.034(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 570 _refine_ls_number_reflns 9906 _refine_ls_number_restraints 89 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0757 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1650P)^2^+3.1716P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2198 _refine_ls_wR_factor_ref 0.2383 _reflns_Friedel_coverage 0.759 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 8353 _reflns_number_total 9906 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04796f2.cif _cod_data_source_block mo_220824_c8f_0m _cod_depositor_comments 'Adding full bibliography for 1572702--1572708.cif.' _cod_original_formula_sum 'C48 H48 Cl3.50 F2 N4' _cod_database_code 1572705 _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. ; _shelx_estimated_absorpt_t_max 0.916 _shelx_estimated_absorpt_t_min 0.877 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances H41A-H50D 2 with sigma of 0.001 Cl2-C47 \\sim Cl2A-C47A with sigma of 0.02 Cl1-C47 \\sim Cl1A-C47A with sigma of 0.02 Cl2-Cl1 \\sim Cl2A-Cl1A with sigma of 0.04 Cl5-C50 \\sim Cl5A-C50A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Cl1 \\sim Cl2 \\sim C47 \\sim Cl1A \\sim Cl2A \\sim C47A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 Cl5 \\sim C50 \\sim Cl5A \\sim C50A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(C47) = Uanis(C47A) Uanis(C50) = Uanis(C50A) 4. Others Sof(Cl1A)=Sof(Cl2A)=Sof(C47A)=Sof(H47C)=Sof(H47D)=0.5*(1-FVAR(2)) Sof(Cl1)=Sof(Cl2)=Sof(C47)=Sof(H47A)=Sof(H47B)=0.5*FVAR(2) Sof(Cl5A)=Sof(C50A)=Sof(H50C)=Sof(H50D)=0.5*(1-FVAR(3)) Sof(Cl5)=Sof(C50)=Sof(H50A)=Sof(H50B)=0.5*FVAR(3) Fixed Sof: H48A(0.5) H48B(0.5) H49B(0.5) H49A(0.5) Fixed X: C50A(0.55148) Fixed Y: C50A(0.56099) Fixed Z: C50A(0.5298) 5.a Secondary CH2 refined with riding coordinates: C48(H48A,H48B), C49(H49B,H49A), C31(H31A,H31B), C32(H32A,H32B), C33(H33A, H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A, H47B), C50(H50A,H50B), C47A(H47C,H47D), C50A(H50C,H50D) 5.b Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C4(H4), C9(H9), C12(H12), C15(H15), C18(H18), C21(H21), C24(H24), C27(H27), C29(H29), C30(H30) ; _shelx_res_file ; TITL mo_220824_c8f_0m_a.res in P4(3)2(1)2 mo_220824_c8f_0m.res created by SHELXL-2018/3 at 20:40:37 on 25-Aug-2022 REM Old TITL mo_220824_C8F_0m in P4(3)2(1)2 REM SHELXT solution in P4(3)2(1)2: R1 0.209, Rweak 0.040, Alpha 0.008 REM 1.082 for 39 systematic absences, Orientation as input REM Flack x = -2.632 ( 0.158 ) from 3105 Parsons' quotients REM Formula found by SHELXT: C47 F3 N6 O2 CELL 0.71073 15.9463 15.9463 35.1878 90 90 90 ZERR 8 0.0003 0.0003 0.0011 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5-Y,0.5+X,0.75+Z SYMM 0.5+Y,0.5-X,0.25+Z SYMM 0.5-X,0.5+Y,0.75-Z SYMM 0.5+X,0.5-Y,0.25-Z SYMM +Y,+X,-Z SYMM -Y,-X,0.5-Z SFAC C H Cl F N UNIT 384 384 28 16 32 DFIX 2 0.001 H41a H50d SADI Cl2 C47 Cl2A C47A SADI Cl1 C47 Cl1A C47A SADI 0.04 Cl2 Cl1 Cl2A Cl1A SADI Cl5 C50 Cl5A C50A SIMU 0.02 0.04 2 Cl1 Cl2 C47 Cl1A > C47A SIMU 0.02 0.04 2 Cl5 C50 Cl5A C50A EADP C47 C47A EADP C50 C50A L.S. 4 0 0 PLAN 20 SIZE 0.32 0.38 0.48 TEMP -103.15 BOND $h htab conf list 4 fmap 2 53 acta OMIT 1 1 10 OMIT -1 2 3 OMIT 1 2 3 OMIT 3 3 0 REM REM REM WGHT 0.165000 3.171600 FVAR 0.30305 0.51156 0.79038 CL3 3 1.022661 0.051849 0.540217 11.00000 0.11844 0.11706 = 0.15916 -0.00113 -0.00869 -0.00728 C48 1 0.993338 -0.006662 0.500000 10.50000 0.19601 0.19601 = 0.23997 0.08045 -0.08045 -0.13546 AFIX 23 H48A 2 0.932940 0.002115 0.494845 10.50000 -1.20000 H48B 2 1.002116 -0.067060 0.505155 10.50000 -1.20000 AFIX 0 CL4 3 0.430528 0.310299 0.513905 11.00000 0.05523 0.09414 = 0.12488 0.03408 -0.01931 0.00735 C49 1 0.327890 0.327890 0.500000 10.50000 0.05754 0.05754 = 0.11231 0.02329 -0.02329 -0.00142 AFIX 23 H49B 2 0.314071 0.289986 0.478616 10.50000 -1.20000 H49A 2 0.289985 0.314070 0.521384 10.50000 -1.20000 AFIX 0 F1 4 0.664617 0.077971 0.251543 11.00000 0.10628 0.14415 = 0.03331 -0.01271 -0.00089 -0.02473 F2 4 0.778860 0.479202 0.801544 11.00000 0.07219 0.05397 = 0.03893 -0.01684 0.01493 -0.00830 N1 5 0.516404 0.182827 0.382774 11.00000 0.04212 0.05702 = 0.04244 0.00150 -0.01297 -0.01748 N2 5 0.795093 0.151313 0.471340 11.00000 0.03531 0.04968 = 0.02951 -0.00080 -0.00019 0.00615 N3 5 0.641340 0.253706 0.604876 11.00000 0.02872 0.04152 = 0.03418 -0.00029 0.00289 -0.00565 N4 5 0.929284 0.369211 0.670947 11.00000 0.03162 0.03941 = 0.02984 0.00024 -0.00269 -0.00039 C1 1 0.668413 0.096420 0.317657 11.00000 0.07769 0.07458 = 0.03297 -0.00133 -0.00308 -0.02353 AFIX 43 H1 2 0.720849 0.068392 0.319359 11.00000 -1.20000 AFIX 0 C2 1 0.627420 0.108808 0.282935 11.00000 0.08719 0.09042 = 0.03170 -0.00094 -0.00441 -0.03773 C3 1 0.551873 0.151460 0.279515 11.00000 0.08151 0.08443 = 0.04008 0.01145 -0.01986 -0.03950 AFIX 43 H3 2 0.528437 0.160939 0.255069 11.00000 -1.20000 AFIX 0 C4 1 0.511266 0.179736 0.311010 11.00000 0.06266 0.06587 = 0.04537 0.01460 -0.01936 -0.02723 AFIX 43 H4 2 0.459155 0.208243 0.308938 11.00000 -1.20000 AFIX 0 C5 1 0.548407 0.165694 0.346773 11.00000 0.05291 0.05722 = 0.03854 0.00382 -0.01005 -0.02561 C6 1 0.626960 0.128141 0.349840 11.00000 0.05871 0.05910 = 0.03427 0.00176 -0.00873 -0.02351 C7 1 0.649203 0.128831 0.389539 11.00000 0.05080 0.04758 = 0.03065 0.00054 -0.00237 -0.01242 C8 1 0.577224 0.159564 0.409090 11.00000 0.04027 0.04286 = 0.04141 0.00418 -0.00818 -0.01146 C9 1 0.574491 0.166970 0.448352 11.00000 0.03957 0.04704 = 0.03879 -0.00039 -0.00265 -0.01057 AFIX 43 H9 2 0.523594 0.177990 0.461464 11.00000 -1.20000 AFIX 0 C10 1 0.649701 0.157474 0.467389 11.00000 0.03873 0.04144 = 0.03161 -0.00099 -0.00063 -0.00350 C11 1 0.725050 0.139100 0.447316 11.00000 0.04292 0.04039 = 0.03311 -0.00178 -0.00351 0.00276 C12 1 0.724676 0.118451 0.409063 11.00000 0.04776 0.04874 = 0.03642 -0.00477 -0.00150 0.00057 AFIX 43 H12 2 0.773578 0.098149 0.396689 11.00000 -1.20000 AFIX 0 C13 1 0.763073 0.175084 0.507001 11.00000 0.03383 0.04140 = 0.02886 0.00021 0.00115 0.00537 C14 1 0.674026 0.177582 0.506063 11.00000 0.03594 0.03616 = 0.03131 0.00100 -0.00164 0.00033 C15 1 0.627108 0.202468 0.537908 11.00000 0.03029 0.03822 = 0.03210 0.00008 0.00039 -0.00276 AFIX 43 H15 2 0.567548 0.203509 0.537510 11.00000 -1.20000 AFIX 0 C16 1 0.671993 0.225338 0.569818 11.00000 0.02985 0.03640 = 0.03408 0.00146 0.00218 -0.00013 C17 1 0.760963 0.222353 0.570709 11.00000 0.03054 0.03413 = 0.02778 0.00109 0.00061 -0.00064 C18 1 0.807616 0.196763 0.539187 11.00000 0.02990 0.04534 = 0.02904 -0.00197 -0.00142 0.00720 AFIX 43 H18 2 0.867125 0.194384 0.539855 11.00000 -1.20000 AFIX 0 C19 1 0.785298 0.254323 0.607393 11.00000 0.03163 0.03247 = 0.02903 0.00033 0.00093 0.00163 C20 1 0.711394 0.271125 0.627930 11.00000 0.03009 0.03393 = 0.03298 0.00182 0.00173 -0.00224 C21 1 0.712921 0.303108 0.664674 11.00000 0.03139 0.03513 = 0.03126 0.00102 0.00579 -0.00319 AFIX 43 H21 2 0.663734 0.306214 0.679841 11.00000 -1.20000 AFIX 0 C22 1 0.790737 0.330438 0.678088 11.00000 0.03554 0.03136 = 0.02825 0.00228 0.00506 0.00209 C23 1 0.862994 0.322897 0.655042 11.00000 0.02948 0.03248 = 0.02967 0.00380 0.00024 0.00020 C24 1 0.863395 0.279985 0.620877 11.00000 0.02809 0.03800 = 0.02853 0.00273 0.00128 0.00465 AFIX 43 H24 2 0.913801 0.268695 0.607426 11.00000 -1.20000 AFIX 0 C25 1 0.899042 0.403476 0.704747 11.00000 0.03819 0.03676 = 0.02863 0.00060 -0.00155 0.00214 C26 1 0.815592 0.378659 0.710853 11.00000 0.03999 0.02824 = 0.02863 0.00341 0.00199 -0.00104 C27 1 0.774042 0.405629 0.743730 11.00000 0.04590 0.03463 = 0.03285 0.00271 0.00471 -0.00324 AFIX 43 H27 2 0.717180 0.391041 0.748332 11.00000 -1.20000 AFIX 0 C28 1 0.817756 0.453276 0.768765 11.00000 0.05512 0.03990 = 0.03093 -0.00307 0.00963 -0.00219 C29 1 0.900966 0.478455 0.763156 11.00000 0.05444 0.04348 = 0.03863 -0.00602 -0.00575 -0.00997 AFIX 43 H29 2 0.928440 0.512130 0.781622 11.00000 -1.20000 AFIX 0 C30 1 0.942562 0.454257 0.730881 11.00000 0.04178 0.04561 = 0.03818 -0.00414 -0.00220 -0.00695 AFIX 43 H30 2 0.998790 0.471154 0.726301 11.00000 -1.20000 AFIX 0 C31 1 0.455631 0.248711 0.390196 11.00000 0.03758 0.08103 = 0.06073 -0.00088 -0.01881 0.00059 AFIX 23 H31A 2 0.433589 0.241140 0.416273 11.00000 -1.20000 H31B 2 0.408043 0.241634 0.372414 11.00000 -1.20000 AFIX 0 C32 1 0.488062 0.337226 0.386522 11.00000 0.05907 0.06736 = 0.09935 0.00463 -0.03192 0.01234 AFIX 23 H32A 2 0.439934 0.376032 0.389089 11.00000 -1.20000 H32B 2 0.510840 0.344283 0.360545 11.00000 -1.20000 AFIX 0 C33 1 0.556410 0.364468 0.415167 11.00000 0.05044 0.05560 = 0.10824 -0.01233 -0.02185 0.00869 AFIX 23 H33A 2 0.549040 0.424932 0.420609 11.00000 -1.20000 H33B 2 0.547369 0.333678 0.439252 11.00000 -1.20000 AFIX 0 C34 1 0.647852 0.349863 0.402169 11.00000 0.05865 0.05207 = 0.08344 0.01480 -0.01874 -0.00812 AFIX 23 H34A 2 0.650515 0.296311 0.387987 11.00000 -1.20000 H34B 2 0.663855 0.395294 0.384418 11.00000 -1.20000 AFIX 0 C35 1 0.712151 0.346893 0.434611 11.00000 0.04715 0.05558 = 0.07063 0.00859 -0.00961 -0.00995 AFIX 23 H35A 2 0.715060 0.402745 0.446825 11.00000 -1.20000 H35B 2 0.693009 0.306148 0.453985 11.00000 -1.20000 AFIX 0 C36 1 0.800066 0.321909 0.420994 11.00000 0.04947 0.06809 = 0.05902 0.01521 -0.00577 -0.01392 AFIX 23 H36A 2 0.826120 0.370936 0.408404 11.00000 -1.20000 H36B 2 0.794391 0.277097 0.401693 11.00000 -1.20000 AFIX 0 C37 1 0.859496 0.290830 0.452544 11.00000 0.03703 0.08253 = 0.04293 0.00513 -0.00061 -0.01630 AFIX 23 H37A 2 0.915648 0.315228 0.447877 11.00000 -1.20000 H37B 2 0.839212 0.313430 0.477083 11.00000 -1.20000 AFIX 0 C38 1 0.869545 0.195906 0.456745 11.00000 0.03245 0.08163 = 0.03228 -0.00301 -0.00006 0.00693 AFIX 23 H38A 2 0.884218 0.172175 0.431611 11.00000 -1.20000 H38B 2 0.917180 0.184814 0.474074 11.00000 -1.20000 AFIX 0 C39 1 0.567399 0.307682 0.606440 11.00000 0.02577 0.04957 = 0.04175 -0.00581 0.00589 -0.00364 AFIX 23 H39A 2 0.552884 0.317227 0.633451 11.00000 -1.20000 H39B 2 0.519867 0.277479 0.594598 11.00000 -1.20000 AFIX 0 C40 1 0.576450 0.393740 0.586779 11.00000 0.02838 0.05263 = 0.05705 0.00150 0.00128 0.00218 AFIX 23 H40A 2 0.520557 0.420664 0.585725 11.00000 -1.20000 H40B 2 0.595222 0.384517 0.560289 11.00000 -1.20000 AFIX 0 C41 1 0.639158 0.455588 0.606532 11.00000 0.03221 0.04053 = 0.06185 -0.00456 0.00328 0.00446 AFIX 23 H41A 2 0.615284 0.512875 0.605789 11.00000 -1.20000 H41B 2 0.645228 0.439346 0.633547 11.00000 -1.20000 AFIX 0 C42 1 0.726879 0.456966 0.587848 11.00000 0.03611 0.04060 = 0.04506 0.00352 0.00316 -0.00024 AFIX 23 H42A 2 0.743127 0.398990 0.580989 11.00000 -1.20000 H42B 2 0.724209 0.490253 0.564130 11.00000 -1.20000 AFIX 0 C43 1 0.793507 0.494116 0.613795 11.00000 0.03627 0.03684 = 0.04341 0.00587 0.00333 0.00095 AFIX 23 H43A 2 0.789864 0.466703 0.638984 11.00000 -1.20000 H43B 2 0.781833 0.554576 0.617381 11.00000 -1.20000 AFIX 0 C44 1 0.883146 0.483748 0.598290 11.00000 0.03340 0.04050 = 0.03729 0.00654 0.00173 -0.00315 AFIX 23 H44A 2 0.891836 0.525131 0.577690 11.00000 -1.20000 H44B 2 0.888315 0.427152 0.586964 11.00000 -1.20000 AFIX 0 C45 1 0.953957 0.495028 0.628285 11.00000 0.03466 0.04461 = 0.04143 0.00490 0.00107 -0.00519 AFIX 23 H45A 2 1.001146 0.525003 0.616049 11.00000 -1.20000 H45B 2 0.932428 0.531478 0.648865 11.00000 -1.20000 AFIX 0 C46 1 0.988581 0.414018 0.646458 11.00000 0.03062 0.04348 = 0.03548 0.00155 0.00073 -0.00165 AFIX 23 H46A 2 1.006760 0.375736 0.625897 11.00000 -1.20000 H46B 2 1.038799 0.428478 0.661647 11.00000 -1.20000 AFIX 0 PART 1 CL1 3 0.713885 -0.226092 0.433778 20.50000 0.12063 0.05920 = 0.06106 0.00607 0.03380 0.03661 CL2 3 0.809548 -0.066647 0.457820 20.50000 0.05851 0.05264 = 0.03407 -0.00877 0.00098 0.00750 C47 1 0.813185 -0.179746 0.455144 20.50000 0.05074 0.05327 = 0.02876 -0.01065 0.00759 0.00883 AFIX 23 H47A 2 0.821288 -0.202831 0.481002 20.50000 -1.20000 H47B 2 0.861920 -0.196743 0.439508 20.50000 -1.20000 AFIX 0 CL5 3 0.557736 0.609994 0.535908 30.50000 0.22896 0.06914 = 0.15316 0.02385 0.13067 0.00581 C50 1 0.541071 0.541071 0.500000 30.50000 0.14576 0.14576 = 0.13458 0.00861 -0.00861 0.02374 AFIX 23 H50A 2 0.483089 0.547499 0.490375 30.50000 -1.20000 H50B 2 0.547499 0.483089 0.509625 30.50000 -1.20000 AFIX 0 PART 0 PART 2 CL1A 3 0.701869 -0.202570 0.434939 -20.50000 0.05799 0.08617 = 0.06828 -0.00583 0.00100 0.02046 CL2A 3 0.815963 -0.074024 0.447211 -20.50000 0.14609 0.06974 = 0.02567 -0.02351 0.00192 0.00483 C47A 1 0.709317 -0.076020 0.426054 -20.50000 0.05074 0.05327 = 0.02876 -0.01065 0.00759 0.00883 AFIX 23 H47C 2 0.708199 -0.060102 0.398865 -20.50000 -1.20000 H47D 2 0.667493 -0.043411 0.440681 -20.50000 -1.20000 AFIX 0 CL5A 3 0.618170 0.628781 0.503462 -30.50000 0.16284 0.09444 = 0.08382 -0.00006 0.03768 0.01644 C50A 1 10.551480 10.560990 10.529800 -30.50000 0.14576 0.14576 = 0.13458 0.00861 -0.00861 0.02374 AFIX 23 H50C 2 0.492078 0.553547 0.522350 -30.50000 -1.20000 H50D 2 0.571638 0.534151 0.553468 -30.50000 -1.20000 AFIX 0 HKLF 4 REM mo_220824_c8f_0m_a.res in P4(3)2(1)2 REM wR2 = 0.2383, GooF = S = 1.072, Restrained GooF = 1.081 for all data REM R1 = 0.0757 for 8353 Fo > 4sig(Fo) and 0.0889 for all 9906 data REM 570 parameters refined using 89 restraints END WGHT 0.1650 3.1711 REM Instructions for potential hydrogen bonds HTAB C48 Cl2 HTAB C48 Cl2A EQIV $1 y+1, x-1, -z+1 HTAB C48 Cl2_$1 HTAB C48 Cl2A_$1 EQIV $3 -y+3/2, x-1/2, z-1/4 HTAB C1 Cl5_$3 EQIV $4 -y+1/2, x-1/2, z-1/4 HTAB C3 Cl2_$4 HTAB C15 Cl4 HTAB C24 F2_$3 HTAB C47 Cl2_$1 REM Highest difference peak 1.223, deepest hole -0.477, 1-sigma level 0.098 Q1 1 0.6370 0.6363 0.5409 11.00000 0.05 1.22 Q2 1 0.8041 -0.1791 0.4754 11.00000 0.05 1.13 Q3 1 0.5258 0.6336 0.5192 11.00000 0.05 0.88 Q4 1 0.7194 -0.1238 0.4310 11.00000 0.05 0.84 Q5 1 0.5593 0.5823 0.5240 11.00000 0.05 0.57 Q6 1 0.3937 0.2805 0.4861 11.00000 0.05 0.49 Q7 1 0.8148 -0.1082 0.4565 11.00000 0.05 0.47 Q8 1 0.7791 -0.0792 0.4490 11.00000 0.05 0.47 Q9 1 0.4444 0.3448 0.4861 11.00000 0.05 0.47 Q10 1 0.7200 -0.2160 0.4402 11.00000 0.05 0.40 Q11 1 0.7486 -0.2307 0.4386 11.00000 0.05 0.38 Q12 1 0.4559 0.3588 0.4956 11.00000 0.05 0.35 Q13 1 0.3443 0.3592 0.5371 11.00000 0.05 0.33 Q14 1 0.6841 0.3213 0.7294 11.00000 0.05 0.30 Q15 1 0.8635 0.5992 0.7943 11.00000 0.05 0.27 Q16 1 0.6355 0.4599 0.5975 11.00000 0.05 0.27 Q17 1 0.3998 0.3884 0.5110 11.00000 0.05 0.27 Q18 1 0.8222 0.4191 0.4742 11.00000 0.05 0.27 Q19 1 1.0067 0.0061 0.5574 11.00000 0.05 0.26 Q20 1 0.7108 0.3838 0.7637 11.00000 0.05 0.26 ; _shelx_res_checksum 82441 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl3 Cl 1.0227(2) 0.0518(2) 0.54022(12) 0.1316(11) Uani 1 1 d . . . . . C48 C 0.9933(8) -0.0067(8) 0.500000 0.211(14) Uani 1 2 d S T P . . H48A H 0.932940 0.002115 0.494845 0.253 Uiso 0.5 1 calc R . . . . H48B H 1.002116 -0.067060 0.505155 0.253 Uiso 0.5 1 calc R . . . . Cl4 Cl 0.43053(12) 0.31030(15) 0.51391(7) 0.0914(7) Uani 1 1 d . . . . . C49 C 0.3279(4) 0.3279(4) 0.500000 0.076(3) Uani 1 2 d S T P . . H49B H 0.314071 0.289986 0.478616 0.091 Uiso 0.5 1 calc R . . . . H49A H 0.289985 0.314070 0.521384 0.091 Uiso 0.5 1 calc R . . . . F1 F 0.6646(3) 0.0780(4) 0.25154(9) 0.0946(15) Uani 1 1 d . . . . . F2 F 0.7789(2) 0.4792(2) 0.80154(8) 0.0550(8) Uani 1 1 d . . . . . N1 N 0.5164(3) 0.1828(3) 0.38277(12) 0.0472(10) Uani 1 1 d . . . . . N2 N 0.7951(2) 0.1513(3) 0.47134(10) 0.0382(8) Uani 1 1 d . . . . . N3 N 0.6413(2) 0.2537(2) 0.60488(10) 0.0348(8) Uani 1 1 d . . . . . N4 N 0.9293(2) 0.3692(2) 0.67095(9) 0.0336(7) Uani 1 1 d . . . . . C1 C 0.6684(5) 0.0964(4) 0.31766(14) 0.0617(16) Uani 1 1 d . . . . . H1 H 0.720849 0.068392 0.319359 0.074 Uiso 1 1 calc R . . . . C2 C 0.6274(5) 0.1088(5) 0.28294(15) 0.070(2) Uani 1 1 d . . . . . C3 C 0.5519(5) 0.1515(5) 0.27952(16) 0.0687(19) Uani 1 1 d . . . . . H3 H 0.528437 0.160939 0.255069 0.082 Uiso 1 1 calc R . . . . C4 C 0.5113(4) 0.1797(4) 0.31101(15) 0.0580(15) Uani 1 1 d . . . . . H4 H 0.459155 0.208243 0.308938 0.070 Uiso 1 1 calc R . . . . C5 C 0.5484(3) 0.1657(4) 0.34677(13) 0.0496(13) Uani 1 1 d . . . . . C6 C 0.6270(4) 0.1281(4) 0.34984(13) 0.0507(13) Uani 1 1 d . . . . . C7 C 0.6492(3) 0.1288(3) 0.38954(12) 0.0430(10) Uani 1 1 d . . . . . C8 C 0.5772(3) 0.1596(3) 0.40909(13) 0.0415(10) Uani 1 1 d . . . . . C9 C 0.5745(3) 0.1670(3) 0.44835(13) 0.0418(10) Uani 1 1 d . . . . . H9 H 0.523594 0.177990 0.461464 0.050 Uiso 1 1 calc R . . . . C10 C 0.6497(3) 0.1575(3) 0.46739(12) 0.0373(9) Uani 1 1 d . . . . . C11 C 0.7251(3) 0.1391(3) 0.44732(12) 0.0388(9) Uani 1 1 d . . . . . C12 C 0.7247(3) 0.1185(3) 0.40906(13) 0.0443(10) Uani 1 1 d . . . . . H12 H 0.773578 0.098149 0.396689 0.053 Uiso 1 1 calc R . . . . C13 C 0.7631(3) 0.1751(3) 0.50700(11) 0.0347(9) Uani 1 1 d . . . . . C14 C 0.6740(3) 0.1776(3) 0.50606(11) 0.0345(8) Uani 1 1 d . . . . . C15 C 0.6271(3) 0.2025(3) 0.53791(11) 0.0335(8) Uani 1 1 d . . . . . H15 H 0.567548 0.203509 0.537510 0.040 Uiso 1 1 calc R . . . . C16 C 0.6720(3) 0.2253(3) 0.56982(12) 0.0334(8) Uani 1 1 d . . . . . C17 C 0.7610(3) 0.2224(3) 0.57071(11) 0.0308(8) Uani 1 1 d . . . . . C18 C 0.8076(3) 0.1968(3) 0.53919(11) 0.0348(9) Uani 1 1 d . . . . . H18 H 0.867125 0.194384 0.539855 0.042 Uiso 1 1 calc R . . . . C19 C 0.7853(3) 0.2543(3) 0.60739(11) 0.0310(8) Uani 1 1 d . . . . . C20 C 0.7114(3) 0.2711(3) 0.62793(11) 0.0323(8) Uani 1 1 d . . . . . C21 C 0.7129(3) 0.3031(3) 0.66467(11) 0.0326(8) Uani 1 1 d . . . . . H21 H 0.663734 0.306214 0.679841 0.039 Uiso 1 1 calc R . . . . C22 C 0.7907(3) 0.3304(3) 0.67809(11) 0.0317(8) Uani 1 1 d . . . . . C23 C 0.8630(3) 0.3229(3) 0.65504(11) 0.0305(8) Uani 1 1 d . . . . . C24 C 0.8634(2) 0.2800(3) 0.62088(11) 0.0315(8) Uani 1 1 d . . . . . H24 H 0.913801 0.268695 0.607426 0.038 Uiso 1 1 calc R . . . . C25 C 0.8990(3) 0.4035(3) 0.70475(11) 0.0345(9) Uani 1 1 d . . . . . C26 C 0.8156(3) 0.3787(2) 0.71085(11) 0.0323(8) Uani 1 1 d . . . . . C27 C 0.7740(3) 0.4056(3) 0.74373(12) 0.0378(9) Uani 1 1 d . . . . . H27 H 0.717180 0.391041 0.748332 0.045 Uiso 1 1 calc R . . . . C28 C 0.8178(3) 0.4533(3) 0.76877(12) 0.0420(10) Uani 1 1 d . . . . . C29 C 0.9010(3) 0.4785(3) 0.76316(14) 0.0455(11) Uani 1 1 d . . . . . H29 H 0.928440 0.512130 0.781622 0.055 Uiso 1 1 calc R . . . . C30 C 0.9426(3) 0.4543(3) 0.73088(13) 0.0419(10) Uani 1 1 d . . . . . H30 H 0.998790 0.471154 0.726301 0.050 Uiso 1 1 calc R . . . . C31 C 0.4556(4) 0.2487(4) 0.39020(18) 0.0598(15) Uani 1 1 d . . . . . H31A H 0.433589 0.241140 0.416273 0.072 Uiso 1 1 calc R . . . . H31B H 0.408043 0.241634 0.372414 0.072 Uiso 1 1 calc R . . . . C32 C 0.4881(5) 0.3372(4) 0.3865(2) 0.075(2) Uani 1 1 d . . . . . H32A H 0.439934 0.376032 0.389089 0.090 Uiso 1 1 calc R . . . . H32B H 0.510840 0.344283 0.360545 0.090 Uiso 1 1 calc R . . . . C33 C 0.5564(4) 0.3645(4) 0.4152(2) 0.0714(19) Uani 1 1 d . . . . . H33A H 0.549040 0.424932 0.420609 0.086 Uiso 1 1 calc R . . . . H33B H 0.547369 0.333678 0.439252 0.086 Uiso 1 1 calc R . . . . C34 C 0.6479(4) 0.3499(4) 0.4022(2) 0.0647(16) Uani 1 1 d . . . . . H34A H 0.650515 0.296311 0.387987 0.078 Uiso 1 1 calc R . . . . H34B H 0.663855 0.395294 0.384418 0.078 Uiso 1 1 calc R . . . . C35 C 0.7122(4) 0.3469(4) 0.43461(18) 0.0578(14) Uani 1 1 d . . . . . H35A H 0.715060 0.402745 0.446825 0.069 Uiso 1 1 calc R . . . . H35B H 0.693009 0.306148 0.453985 0.069 Uiso 1 1 calc R . . . . C36 C 0.8001(4) 0.3219(4) 0.42099(17) 0.0589(14) Uani 1 1 d . . . . . H36A H 0.826120 0.370936 0.408404 0.071 Uiso 1 1 calc R . . . . H36B H 0.794391 0.277097 0.401693 0.071 Uiso 1 1 calc R . . . . C37 C 0.8595(3) 0.2908(4) 0.45254(14) 0.0542(13) Uani 1 1 d . . . . . H37A H 0.915648 0.315228 0.447877 0.065 Uiso 1 1 calc R . . . . H37B H 0.839212 0.313430 0.477083 0.065 Uiso 1 1 calc R . . . . C38 C 0.8695(3) 0.1959(4) 0.45674(13) 0.0488(12) Uani 1 1 d . . . . . H38A H 0.884218 0.172175 0.431611 0.059 Uiso 1 1 calc R . . . . H38B H 0.917180 0.184814 0.474074 0.059 Uiso 1 1 calc R . . . . C39 C 0.5674(3) 0.3077(3) 0.60644(13) 0.0390(9) Uani 1 1 d . . . . . H39A H 0.552884 0.317227 0.633451 0.047 Uiso 1 1 calc R . . . . H39B H 0.519867 0.277479 0.594598 0.047 Uiso 1 1 calc R . . . . C40 C 0.5765(3) 0.3937(3) 0.58678(15) 0.0460(11) Uani 1 1 d . . . . . H40A H 0.520557 0.420664 0.585725 0.055 Uiso 1 1 calc R . . . . H40B H 0.595222 0.384517 0.560289 0.055 Uiso 1 1 calc R . . . . C41 C 0.6392(3) 0.4556(3) 0.60653(6) 0.0449(11) Uani 1 1 d . . . . . H41A H 0.615284 0.512875 0.605789 0.054 Uiso 1 1 calc DR . . . . H41B H 0.645228 0.439346 0.633547 0.054 Uiso 1 1 calc R . . . . C42 C 0.7269(3) 0.4570(3) 0.58785(13) 0.0406(9) Uani 1 1 d . . . . . H42A H 0.743127 0.398990 0.580989 0.049 Uiso 1 1 calc R . . . . H42B H 0.724209 0.490253 0.564130 0.049 Uiso 1 1 calc R . . . . C43 C 0.7935(3) 0.4941(3) 0.61379(13) 0.0388(9) Uani 1 1 d . . . . . H43A H 0.789864 0.466703 0.638984 0.047 Uiso 1 1 calc R . . . . H43B H 0.781833 0.554576 0.617381 0.047 Uiso 1 1 calc R . . . . C44 C 0.8831(3) 0.4837(3) 0.59829(12) 0.0371(9) Uani 1 1 d . . . . . H44A H 0.891836 0.525131 0.577690 0.044 Uiso 1 1 calc R . . . . H44B H 0.888315 0.427152 0.586964 0.044 Uiso 1 1 calc R . . . . C45 C 0.9540(3) 0.4950(3) 0.62829(13) 0.0402(9) Uani 1 1 d . . . . . H45A H 1.001146 0.525003 0.616049 0.048 Uiso 1 1 calc R . . . . H45B H 0.932428 0.531478 0.648865 0.048 Uiso 1 1 calc R . . . . C46 C 0.9886(3) 0.4140(3) 0.64646(12) 0.0365(9) Uani 1 1 d . . . . . H46A H 1.006760 0.375736 0.625897 0.044 Uiso 1 1 calc R . . . . H46B H 1.038799 0.428478 0.661647 0.044 Uiso 1 1 calc R . . . . Cl1 Cl 0.7139(10) -0.2261(8) 0.4338(4) 0.080(4) Uani 0.256(9) 1 d D U . A 1 Cl2 Cl 0.8095(5) -0.0666(7) 0.4578(3) 0.0484(18) Uani 0.256(9) 1 d D U . A 1 C47 C 0.8132(12) -0.1797(11) 0.4551(5) 0.044(3) Uani 0.256(9) 1 d D U . A 1 H47A H 0.821288 -0.202831 0.481002 0.053 Uiso 0.256(9) 1 calc R . . A 1 H47B H 0.861920 -0.196743 0.439508 0.053 Uiso 0.256(9) 1 calc R . . A 1 Cl5 Cl 0.5577(7) 0.6100(4) 0.5359(2) 0.150(4) Uani 0.395(6) 1 d D U . B 1 C50 C 0.5411(12) 0.5411(12) 0.500000 0.142(6) Uani 0.790(11) 2 d DS TU P B 1 H50A H 0.483089 0.547499 0.490375 0.170 Uiso 0.395(6) 1 calc R . . B 1 H50B H 0.547499 0.483089 0.509625 0.170 Uiso 0.395(6) 1 calc R . . B 1 Cl1A Cl 0.7019(8) -0.2026(9) 0.4349(5) 0.071(3) Uani 0.244(9) 1 d D U . A 2 Cl2A Cl 0.8160(11) -0.0740(10) 0.4472(3) 0.080(4) Uani 0.244(9) 1 d D U . A 2 C47A C 0.7093(12) -0.0760(12) 0.4261(5) 0.044(3) Uani 0.244(9) 1 d D U . A 2 H47C H 0.708199 -0.060102 0.398865 0.053 Uiso 0.244(9) 1 calc R . . A 2 H47D H 0.667493 -0.043411 0.440681 0.053 Uiso 0.244(9) 1 calc R . . A 2 Cl5A Cl 0.618(4) 0.629(3) 0.5035(14) 0.114(8) Uani 0.105(6) 1 d D U . B 2 C50A C 0.551480 0.560990 0.529800 0.142(6) Uani 0.105(6) 1 d D U . B 2 H50C H 0.492078 0.553547 0.522350 0.170 Uiso 0.105(6) 1 calc R . . B 2 H50D H 0.571638 0.534151 0.553468 0.170 Uiso 0.105(6) 1 calc DR . . B 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 Cl3 0.118(2) 0.117(2) 0.159(3) -0.001(2) -0.009(2) -0.0073(18) C48 0.196(18) 0.196(18) 0.24(3) 0.08(2) -0.08(2) -0.14(2) Cl4 0.0552(9) 0.0941(14) 0.1249(17) 0.0341(12) -0.0193(10) 0.0073(9) C49 0.058(3) 0.058(3) 0.112(8) 0.023(4) -0.023(4) -0.001(4) F1 0.106(3) 0.144(4) 0.0333(16) -0.013(2) -0.0009(18) -0.025(3) F2 0.072(2) 0.0540(17) 0.0389(13) -0.0168(12) 0.0149(14) -0.0083(15) N1 0.042(2) 0.057(3) 0.042(2) 0.0015(18) -0.0130(17) -0.0175(19) N2 0.0353(18) 0.050(2) 0.0295(16) -0.0008(15) -0.0002(14) 0.0061(16) N3 0.0287(17) 0.0415(19) 0.0342(17) -0.0003(14) 0.0029(13) -0.0057(14) N4 0.0316(17) 0.0394(19) 0.0298(15) 0.0002(14) -0.0027(13) -0.0004(14) C1 0.078(4) 0.075(4) 0.033(2) -0.001(2) -0.003(2) -0.024(3) C2 0.087(5) 0.090(5) 0.032(2) -0.001(3) -0.004(3) -0.038(4) C3 0.082(5) 0.084(4) 0.040(3) 0.011(3) -0.020(3) -0.040(4) C4 0.063(3) 0.066(3) 0.045(3) 0.015(2) -0.019(2) -0.027(3) C5 0.053(3) 0.057(3) 0.039(2) 0.004(2) -0.010(2) -0.026(2) C6 0.059(3) 0.059(3) 0.034(2) 0.002(2) -0.009(2) -0.024(2) C7 0.051(3) 0.048(3) 0.0307(19) 0.0005(18) -0.0024(18) -0.012(2) C8 0.040(2) 0.043(2) 0.041(2) 0.0042(18) -0.0082(18) -0.0115(19) C9 0.040(2) 0.047(3) 0.039(2) -0.0004(19) -0.0027(18) -0.0106(19) C10 0.039(2) 0.041(2) 0.0316(19) -0.0010(16) -0.0006(16) -0.0035(18) C11 0.043(2) 0.040(2) 0.0331(19) -0.0018(16) -0.0035(18) 0.0028(18) C12 0.048(3) 0.049(3) 0.036(2) -0.0048(19) -0.0015(19) 0.001(2) C13 0.034(2) 0.041(2) 0.0289(18) 0.0002(16) 0.0012(15) 0.0054(16) C14 0.036(2) 0.036(2) 0.0313(19) 0.0010(16) -0.0016(16) 0.0003(16) C15 0.0303(19) 0.038(2) 0.0321(18) 0.0001(16) 0.0004(15) -0.0028(16) C16 0.0298(19) 0.036(2) 0.0341(19) 0.0015(16) 0.0022(15) -0.0001(16) C17 0.0305(18) 0.034(2) 0.0278(17) 0.0011(15) 0.0006(14) -0.0006(15) C18 0.0299(19) 0.045(2) 0.0290(18) -0.0020(16) -0.0014(15) 0.0072(16) C19 0.0316(19) 0.0325(19) 0.0290(17) 0.0003(14) 0.0009(15) 0.0016(15) C20 0.0301(19) 0.034(2) 0.0330(18) 0.0018(15) 0.0017(15) -0.0022(15) C21 0.0314(19) 0.035(2) 0.0313(17) 0.0010(15) 0.0058(15) -0.0032(16) C22 0.036(2) 0.0314(19) 0.0282(17) 0.0023(15) 0.0051(15) 0.0021(16) C23 0.0295(19) 0.0325(19) 0.0297(17) 0.0038(15) 0.0002(14) 0.0002(15) C24 0.0281(18) 0.038(2) 0.0285(16) 0.0027(15) 0.0013(14) 0.0046(16) C25 0.038(2) 0.037(2) 0.0286(18) 0.0006(16) -0.0016(16) 0.0021(17) C26 0.040(2) 0.0282(18) 0.0286(17) 0.0034(15) 0.0020(15) -0.0010(16) C27 0.046(2) 0.035(2) 0.0329(19) 0.0027(16) 0.0047(17) -0.0032(17) C28 0.055(3) 0.040(2) 0.031(2) -0.0031(17) 0.0096(19) -0.002(2) C29 0.054(3) 0.043(2) 0.039(2) -0.0060(19) -0.006(2) -0.010(2) C30 0.042(2) 0.046(2) 0.038(2) -0.0041(19) -0.0022(18) -0.0070(19) C31 0.038(3) 0.081(4) 0.061(3) -0.001(3) -0.019(2) 0.001(3) C32 0.059(4) 0.067(4) 0.099(5) 0.005(4) -0.032(4) 0.012(3) C33 0.050(3) 0.056(3) 0.108(5) -0.012(3) -0.022(3) 0.009(3) C34 0.059(3) 0.052(3) 0.083(4) 0.015(3) -0.019(3) -0.008(3) C35 0.047(3) 0.056(3) 0.071(4) 0.009(3) -0.010(3) -0.010(2) C36 0.049(3) 0.068(4) 0.059(3) 0.015(3) -0.006(2) -0.014(3) C37 0.037(2) 0.083(4) 0.043(2) 0.005(2) -0.0006(19) -0.016(3) C38 0.032(2) 0.082(4) 0.032(2) -0.003(2) -0.0001(17) 0.007(2) C39 0.0258(19) 0.050(3) 0.042(2) -0.0058(18) 0.0059(16) -0.0036(17) C40 0.028(2) 0.053(3) 0.057(3) 0.001(2) 0.001(2) 0.002(2) C41 0.032(2) 0.041(2) 0.062(3) -0.005(2) 0.003(2) 0.0045(18) C42 0.036(2) 0.041(2) 0.045(2) 0.0035(18) 0.0032(18) -0.0002(18) C43 0.036(2) 0.037(2) 0.043(2) 0.0059(18) 0.0033(18) 0.0010(17) C44 0.033(2) 0.041(2) 0.037(2) 0.0065(17) 0.0017(17) -0.0032(17) C45 0.035(2) 0.045(2) 0.041(2) 0.0049(18) 0.0011(18) -0.0052(18) C46 0.031(2) 0.043(2) 0.0355(19) 0.0015(17) 0.0007(16) -0.0016(17) Cl1 0.121(10) 0.059(5) 0.061(4) 0.006(4) 0.034(5) 0.037(5) Cl2 0.059(3) 0.053(4) 0.034(5) -0.009(4) 0.001(3) 0.008(2) C47 0.051(7) 0.053(7) 0.029(5) -0.011(5) 0.008(5) 0.009(6) Cl5 0.229(9) 0.069(3) 0.153(6) 0.024(4) 0.131(7) 0.006(4) C50 0.146(9) 0.146(9) 0.135(12) 0.009(8) -0.009(8) 0.024(11) Cl1A 0.058(4) 0.086(9) 0.068(5) -0.006(6) 0.001(4) 0.020(6) Cl2A 0.146(10) 0.070(5) 0.026(5) -0.024(4) 0.002(4) 0.005(5) C47A 0.051(7) 0.053(7) 0.029(5) -0.011(5) 0.008(5) 0.009(6) Cl5A 0.163(17) 0.094(14) 0.084(15) 0.000(13) 0.038(13) 0.016(13) C50A 0.146(9) 0.146(9) 0.135(12) 0.009(8) -0.009(8) 0.024(11) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 Cl3 C48 Cl3 111.4(10) . 7_646 ? Cl3 C48 H48A 109.3 7_646 . ? Cl3 C48 H48A 109.3 . . ? Cl3 C48 H48B 109.3 7_646 . ? Cl3 C48 H48B 109.3 . . ? H48A C48 H48B 108.0 . . ? Cl4 C49 Cl4 112.7(6) 7_556 . ? Cl4 C49 H49B 109.0 . . ? Cl4 C49 H49B 109.0 7_556 . ? Cl4 C49 H49A 109.0 7_556 . ? Cl4 C49 H49A 109.0 . . ? H49B C49 H49A 107.8 . . ? C5 N1 C31 123.3(5) . . ? C8 N1 C5 107.3(5) . . ? C8 N1 C31 122.6(4) . . ? C11 N2 C38 119.6(4) . . ? C13 N2 C11 106.5(3) . . ? C13 N2 C38 118.2(4) . . ? C16 N3 C20 107.1(3) . . ? C16 N3 C39 120.3(4) . . ? C20 N3 C39 120.2(4) . . ? C23 N4 C46 120.5(3) . . ? C25 N4 C23 106.6(3) . . ? C25 N4 C46 122.2(4) . . ? C2 C1 H1 122.2 . . ? C2 C1 C6 115.7(7) . . ? C6 C1 H1 122.2 . . ? F1 C2 C1 117.3(7) . . ? F1 C2 C3 119.3(5) . . ? C3 C2 C1 123.4(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.3(5) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 120.8 . . ? C3 C4 C5 118.4(6) . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 128.8(6) . . ? C6 C5 N1 110.1(4) . . ? C6 C5 C4 121.0(5) . . ? C1 C6 C7 131.9(6) . . ? C5 C6 C1 121.0(5) . . ? C5 C6 C7 107.0(5) . . ? C8 C7 C6 105.8(5) . . ? C12 C7 C6 133.5(5) . . ? C12 C7 C8 119.8(4) . . ? N1 C8 C7 109.4(4) . . ? C9 C8 N1 128.2(5) . . ? C9 C8 C7 122.4(4) . . ? C8 C9 H9 121.8 . . ? C10 C9 C8 116.5(5) . . ? C10 C9 H9 121.8 . . ? C9 C10 C11 120.9(4) . . ? C9 C10 C14 131.5(4) . . ? C11 C10 C14 106.6(4) . . ? N2 C11 C10 110.0(4) . . ? C12 C11 N2 128.1(4) . . ? C12 C11 C10 121.8(4) . . ? C7 C12 H12 121.5 . . ? C11 C12 C7 117.0(5) . . ? C11 C12 H12 121.5 . . ? N2 C13 C14 110.5(4) . . ? C18 C13 N2 127.8(4) . . ? C18 C13 C14 121.7(4) . . ? C13 C14 C10 106.4(4) . . ? C15 C14 C10 131.9(4) . . ? C15 C14 C13 121.4(4) . . ? C14 C15 H15 121.7 . . ? C16 C15 C14 116.6(4) . . ? C16 C15 H15 121.7 . . ? N3 C16 C17 109.9(4) . . ? C15 C16 N3 128.3(4) . . ? C15 C16 C17 121.8(4) . . ? C16 C17 C19 106.1(4) . . ? C18 C17 C16 121.6(4) . . ? C18 C17 C19 132.2(4) . . ? C13 C18 C17 116.8(4) . . ? C13 C18 H18 121.6 . . ? C17 C18 H18 121.6 . . ? C20 C19 C17 107.6(3) . . ? C24 C19 C17 130.5(4) . . ? C24 C19 C20 121.1(4) . . ? C19 C20 N3 109.3(3) . . ? C21 C20 N3 128.5(4) . . ? C21 C20 C19 122.2(4) . . ? C20 C21 H21 121.8 . . ? C20 C21 C22 116.4(4) . . ? C22 C21 H21 121.8 . . ? C21 C22 C23 120.2(4) . . ? C21 C22 C26 132.9(4) . . ? C23 C22 C26 106.3(4) . . ? N4 C23 C22 109.9(3) . . ? C24 C23 N4 127.0(4) . . ? C24 C23 C22 123.0(4) . . ? C19 C24 H24 122.0 . . ? C23 C24 C19 115.9(4) . . ? C23 C24 H24 122.0 . . ? N4 C25 C26 110.3(4) . . ? N4 C25 C30 127.7(4) . . ? C26 C25 C30 121.9(4) . . ? C25 C26 C22 106.8(3) . . ? C27 C26 C22 134.0(4) . . ? C27 C26 C25 119.2(4) . . ? C26 C27 H27 121.1 . . ? C28 C27 C26 117.7(4) . . ? C28 C27 H27 121.1 . . ? F2 C28 C29 117.4(4) . . ? C27 C28 F2 118.8(4) . . ? C27 C28 C29 123.8(4) . . ? C28 C29 H29 120.2 . . ? C30 C29 C28 119.6(4) . . ? C30 C29 H29 120.2 . . ? C25 C30 H30 121.2 . . ? C29 C30 C25 117.7(4) . . ? C29 C30 H30 121.2 . . ? N1 C31 H31A 108.4 . . ? N1 C31 H31B 108.4 . . ? N1 C31 C32 115.6(5) . . ? H31A C31 H31B 107.4 . . ? C32 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? C31 C32 H32A 108.1 . . ? C31 C32 H32B 108.1 . . ? C31 C32 C33 116.6(6) . . ? H32A C32 H32B 107.3 . . ? C33 C32 H32A 108.1 . . ? C33 C32 H32B 108.1 . . ? C32 C33 H33A 108.4 . . ? C32 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C34 C33 C32 115.4(7) . . ? C34 C33 H33A 108.4 . . ? C34 C33 H33B 108.4 . . ? C33 C34 H34A 108.6 . . ? C33 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C35 C34 C33 114.5(6) . . ? C35 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C34 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C36 C35 C34 112.7(6) . . ? C36 C35 H35A 109.0 . . ? C36 C35 H35B 109.0 . . ? C35 C36 H36A 108.6 . . ? C35 C36 H36B 108.6 . . ? C35 C36 C37 114.9(5) . . ? H36A C36 H36B 107.5 . . ? C37 C36 H36A 108.6 . . ? C37 C36 H36B 108.6 . . ? C36 C37 H37A 108.1 . . ? C36 C37 H37B 108.1 . . ? H37A C37 H37B 107.3 . . ? C38 C37 C36 116.9(5) . . ? C38 C37 H37A 108.1 . . ? C38 C37 H37B 108.1 . . ? N2 C38 C37 115.2(4) . . ? N2 C38 H38A 108.5 . . ? N2 C38 H38B 108.5 . . ? C37 C38 H38A 108.5 . . ? C37 C38 H38B 108.5 . . ? H38A C38 H38B 107.5 . . ? N3 C39 H39A 108.4 . . ? N3 C39 H39B 108.4 . . ? N3 C39 C40 115.6(4) . . ? H39A C39 H39B 107.5 . . ? C40 C39 H39A 108.4 . . ? C40 C39 H39B 108.4 . . ? C39 C40 H40A 108.6 . . ? C39 C40 H40B 108.6 . . ? C39 C40 C41 114.9(4) . . ? H40A C40 H40B 107.5 . . ? C41 C40 H40A 108.6 . . ? C41 C40 H40B 108.6 . . ? C40 C41 H41A 108.9 . . ? C40 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C42 C41 C40 113.4(4) . . ? C42 C41 H41A 108.9 . . ? C42 C41 H41B 108.9 . . ? C41 C42 H42A 109.1 . . ? C41 C42 H42B 109.1 . . ? H42A C42 H42B 107.8 . . ? C43 C42 C41 112.5(4) . . ? C43 C42 H42A 109.1 . . ? C43 C42 H42B 109.1 . . ? C42 C43 H43A 108.9 . . ? C42 C43 H43B 108.9 . . ? C42 C43 C44 113.2(4) . . ? H43A C43 H43B 107.7 . . ? C44 C43 H43A 108.9 . . ? C44 C43 H43B 108.9 . . ? C43 C44 H44A 108.5 . . ? C43 C44 H44B 108.5 . . ? C43 C44 C45 114.9(4) . . ? H44A C44 H44B 107.5 . . ? C45 C44 H44A 108.5 . . ? C45 C44 H44B 108.5 . . ? C44 C45 H45A 108.2 . . ? C44 C45 H45B 108.2 . . ? H45A C45 H45B 107.4 . . ? C46 C45 C44 116.3(4) . . ? C46 C45 H45A 108.2 . . ? C46 C45 H45B 108.2 . . ? N4 C46 C45 114.9(4) . . ? N4 C46 H46A 108.5 . . ? N4 C46 H46B 108.5 . . ? C45 C46 H46A 108.5 . . ? C45 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? Cl1 C47 H47A 109.1 . . ? Cl1 C47 H47B 109.1 . . ? Cl2 C47 Cl1 112.4(11) . . ? Cl2 C47 H47A 109.1 . . ? Cl2 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? Cl5 C50 Cl5 110.6(16) . 7_556 ? Cl5 C50 H50A 109.5 . . ? Cl5 C50 H50A 109.5 7_556 . ? Cl5 C50 H50B 109.5 7_556 . ? Cl5 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? Cl1A C47A H47C 113.6 . . ? Cl1A C47A H47D 113.6 . . ? Cl2A C47A Cl1A 90.5(10) . . ? Cl2A C47A H47C 113.6 . . ? Cl2A C47A H47D 113.6 . . ? H47C C47A H47D 110.8 . . ? Cl5A Cl5A C50A 59(8) 7_556 7_556 ? Cl5A Cl5A C50A 112(9) 7_556 . ? C50A Cl5A C50A 69.2(11) . 7_556 ? Cl5A C50A H50A 97.9(16) 7_556 7_556 ? Cl5A C50A H50A 107.2(15) . 7_556 ? Cl5A C50A Cl5A 9(3) . 7_556 ? Cl5A C50A H50C 120.5 . . ? Cl5A C50A H50C 120.5 7_556 . ? Cl5A C50A H50D 120.5 7_556 . ? Cl5A C50A H50D 120.5 . . ? H50C C50A H50A 73.9 . 7_556 ? H50C C50A H50D 118.8 . . ? H50D C50A H50A 93.2 . 7_556 ? 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 Cl3 C48 1.758(11) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? Cl4 C49 1.731(6) . ? C49 H49B 0.9900 . ? C49 H49A 0.9900 . ? F1 C2 1.347(8) . ? F2 C28 1.373(5) . ? N1 C5 1.393(7) . ? N1 C8 1.391(6) . ? N1 C31 1.453(8) . ? N2 C11 1.414(6) . ? N2 C13 1.407(5) . ? N2 C38 1.476(7) . ? N3 C16 1.402(5) . ? N3 C20 1.408(5) . ? N3 C39 1.461(6) . ? N4 C23 1.406(5) . ? N4 C25 1.395(5) . ? N4 C46 1.465(6) . ? C1 H1 0.9500 . ? C1 C2 1.400(8) . ? C1 C6 1.405(9) . ? C2 C3 1.389(12) . ? C3 H3 0.9500 . ? C3 C4 1.360(10) . ? C4 H4 0.9500 . ? C4 C5 1.409(7) . ? C5 C6 1.393(9) . ? C6 C7 1.441(6) . ? C7 C8 1.425(8) . ? C7 C12 1.396(7) . ? C8 C9 1.387(6) . ? C9 H9 0.9500 . ? C9 C10 1.382(7) . ? C10 C11 1.424(7) . ? C10 C14 1.451(6) . ? C11 C12 1.386(6) . ? C12 H12 0.9500 . ? C13 C14 1.421(6) . ? C13 C18 1.381(6) . ? C14 C15 1.405(6) . ? C15 H15 0.9500 . ? C15 C16 1.381(6) . ? C16 C17 1.420(6) . ? C17 C18 1.397(6) . ? C17 C19 1.441(5) . ? C18 H18 0.9500 . ? C19 C20 1.408(6) . ? C19 C24 1.394(6) . ? C20 C21 1.390(6) . ? C21 H21 0.9500 . ? C21 C22 1.397(6) . ? C22 C23 1.414(6) . ? C22 C26 1.441(6) . ? C23 C24 1.383(6) . ? C24 H24 0.9500 . ? C25 C26 1.405(6) . ? C25 C30 1.408(6) . ? C26 C27 1.401(6) . ? C27 H27 0.9500 . ? C27 C28 1.356(7) . ? C28 C29 1.400(7) . ? C29 H29 0.9500 . ? C29 C30 1.371(7) . ? C30 H30 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.509(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C33 1.547(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.546(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 C35 1.535(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.534(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36 C37 1.542(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.529(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 C40 1.544(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C41 1.567(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 C42 1.546(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 C43 1.521(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.539(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.556(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.544(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? Cl1 C47 1.90(2) . ? Cl2 C47 1.81(2) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? Cl5 C50 1.696(17) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? Cl1A C47A 2.05(2) . ? Cl2A C47A 1.86(2) . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? Cl5A Cl5A 0.34(9) 7_556 ? Cl5A C50A 1.78(2) . ? Cl5A C50A 1.93(5) 7_556 ? C50A H50C 0.9900 . ? C50A H50D 0.9900 . ? 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 C2 C3 C4 176.9(6) . . . . ? F2 C28 C29 C30 -180.0(5) . . . . ? N1 C5 C6 C1 173.0(5) . . . . ? N1 C5 C6 C7 -5.6(6) . . . . ? N1 C8 C9 C10 -165.5(5) . . . . ? N1 C31 C32 C33 -64.8(9) . . . . ? N2 C11 C12 C7 -165.5(5) . . . . ? N2 C13 C14 C10 -2.3(5) . . . . ? N2 C13 C14 C15 -177.8(4) . . . . ? N2 C13 C18 C17 176.7(4) . . . . ? N3 C16 C17 C18 -179.5(4) . . . . ? N3 C16 C17 C19 -2.9(5) . . . . ? N3 C20 C21 C22 -167.3(4) . . . . ? N3 C39 C40 C41 -67.8(5) . . . . ? N4 C23 C24 C19 -166.6(4) . . . . ? N4 C25 C26 C22 -3.5(5) . . . . ? N4 C25 C26 C27 179.1(4) . . . . ? N4 C25 C30 C29 -177.6(4) . . . . ? C1 C2 C3 C4 -3.7(10) . . . . ? C1 C6 C7 C8 -172.3(6) . . . . ? C1 C6 C7 C12 18.6(10) . . . . ? C2 C1 C6 C5 2.9(8) . . . . ? C2 C1 C6 C7 -178.9(6) . . . . ? C2 C3 C4 C5 0.9(9) . . . . ? C3 C4 C5 N1 -174.7(6) . . . . ? C3 C4 C5 C6 3.6(8) . . . . ? C4 C5 C6 C1 -5.6(8) . . . . ? C4 C5 C6 C7 175.7(5) . . . . ? C5 N1 C8 C7 1.1(5) . . . . ? C5 N1 C8 C9 178.2(5) . . . . ? C5 N1 C31 C32 -70.0(7) . . . . ? C5 C6 C7 C8 6.1(6) . . . . ? C5 C6 C7 C12 -163.0(6) . . . . ? C6 C1 C2 F1 -178.9(6) . . . . ? C6 C1 C2 C3 1.8(9) . . . . ? C6 C7 C8 N1 -4.5(6) . . . . ? C6 C7 C8 C9 178.3(5) . . . . ? C6 C7 C12 C11 167.9(6) . . . . ? C7 C8 C9 C10 11.2(7) . . . . ? C8 N1 C5 C4 -178.6(5) . . . . ? C8 N1 C5 C6 2.9(6) . . . . ? C8 N1 C31 C32 77.4(7) . . . . ? C8 C7 C12 C11 0.1(7) . . . . ? C8 C9 C10 C11 -1.4(7) . . . . ? C8 C9 C10 C14 165.4(5) . . . . ? C9 C10 C11 N2 166.7(4) . . . . ? C9 C10 C11 C12 -9.2(7) . . . . ? C9 C10 C14 C13 -165.0(5) . . . . ? C9 C10 C14 C15 9.8(9) . . . . ? C10 C11 C12 C7 9.6(7) . . . . ? C10 C14 C15 C16 -173.3(5) . . . . ? C11 N2 C13 C14 0.4(5) . . . . ? C11 N2 C13 C18 -177.4(4) . . . . ? C11 N2 C38 C37 74.2(5) . . . . ? C11 C10 C14 C13 3.2(5) . . . . ? C11 C10 C14 C15 178.1(5) . . . . ? C12 C7 C8 N1 166.4(4) . . . . ? C12 C7 C8 C9 -10.9(7) . . . . ? C13 N2 C11 C10 1.7(5) . . . . ? C13 N2 C11 C12 177.3(5) . . . . ? C13 N2 C38 C37 -58.2(5) . . . . ? C13 C14 C15 C16 0.9(6) . . . . ? C14 C10 C11 N2 -3.1(5) . . . . ? C14 C10 C11 C12 -179.0(4) . . . . ? C14 C13 C18 C17 -0.8(6) . . . . ? C14 C15 C16 N3 178.9(4) . . . . ? C14 C15 C16 C17 -1.2(6) . . . . ? C15 C16 C17 C18 0.6(7) . . . . ? C15 C16 C17 C19 177.2(4) . . . . ? C16 N3 C20 C19 0.4(5) . . . . ? C16 N3 C20 C21 177.9(4) . . . . ? C16 N3 C39 C40 -62.6(5) . . . . ? C16 C17 C18 C13 0.5(6) . . . . ? C16 C17 C19 C20 3.0(5) . . . . ? C16 C17 C19 C24 -166.4(4) . . . . ? C17 C19 C20 N3 -2.1(5) . . . . ? C17 C19 C20 C21 -179.8(4) . . . . ? C17 C19 C24 C23 167.7(4) . . . . ? C18 C13 C14 C10 175.6(4) . . . . ? C18 C13 C14 C15 0.1(7) . . . . ? C18 C17 C19 C20 179.1(4) . . . . ? C18 C17 C19 C24 9.7(8) . . . . ? C19 C17 C18 C13 -175.1(4) . . . . ? C19 C20 C21 C22 9.9(6) . . . . ? C20 N3 C16 C15 -178.4(4) . . . . ? C20 N3 C16 C17 1.6(5) . . . . ? C20 N3 C39 C40 74.5(5) . . . . ? C20 C19 C24 C23 -0.5(6) . . . . ? C20 C21 C22 C23 -1.6(6) . . . . ? C20 C21 C22 C26 168.1(4) . . . . ? C21 C22 C23 N4 168.1(4) . . . . ? C21 C22 C23 C24 -8.1(6) . . . . ? C21 C22 C26 C25 -166.2(4) . . . . ? C21 C22 C26 C27 10.7(8) . . . . ? C22 C23 C24 C19 8.9(6) . . . . ? C22 C26 C27 C28 -178.2(5) . . . . ? C23 N4 C25 C26 1.0(5) . . . . ? C23 N4 C25 C30 179.5(4) . . . . ? C23 N4 C46 C45 74.6(5) . . . . ? C23 C22 C26 C25 4.5(4) . . . . ? C23 C22 C26 C27 -178.6(4) . . . . ? C24 C19 C20 N3 168.5(4) . . . . ? C24 C19 C20 C21 -9.2(6) . . . . ? C25 N4 C23 C22 2.0(4) . . . . ? C25 N4 C23 C24 178.0(4) . . . . ? C25 N4 C46 C45 -65.1(5) . . . . ? C25 C26 C27 C28 -1.6(6) . . . . ? C26 C22 C23 N4 -4.1(4) . . . . ? C26 C22 C23 C24 179.8(4) . . . . ? C26 C25 C30 C29 0.7(7) . . . . ? C26 C27 C28 F2 -178.8(4) . . . . ? C26 C27 C28 C29 1.6(7) . . . . ? C27 C28 C29 C30 -0.3(8) . . . . ? C28 C29 C30 C25 -0.8(7) . . . . ? C30 C25 C26 C22 177.9(4) . . . . ? C30 C25 C26 C27 0.5(6) . . . . ? C31 N1 C5 C4 -27.0(8) . . . . ? C31 N1 C5 C6 154.5(5) . . . . ? C31 N1 C8 C7 -150.8(5) . . . . ? C31 N1 C8 C9 26.3(8) . . . . ? C31 C32 C33 C34 91.1(9) . . . . ? C32 C33 C34 C35 -159.2(6) . . . . ? C33 C34 C35 C36 173.1(5) . . . . ? C34 C35 C36 C37 -161.5(5) . . . . ? C35 C36 C37 C38 99.4(6) . . . . ? C36 C37 C38 N2 -69.6(6) . . . . ? C38 N2 C11 C10 -135.5(5) . . . . ? C38 N2 C11 C12 40.0(7) . . . . ? C38 N2 C13 C14 138.4(4) . . . . ? C38 N2 C13 C18 -39.4(7) . . . . ? C39 N3 C16 C15 -36.4(7) . . . . ? C39 N3 C16 C17 143.6(4) . . . . ? C39 N3 C20 C19 -141.7(4) . . . . ? C39 N3 C20 C21 35.7(6) . . . . ? C39 C40 C41 C42 98.3(4) . . . . ? C40 C41 C42 C43 -161.7(4) . . . . ? C41 C42 C43 C44 171.2(4) . . . . ? C42 C43 C44 C45 -162.1(4) . . . . ? C43 C44 C45 C46 96.2(5) . . . . ? C44 C45 C46 N4 -67.4(5) . . . . ? C46 N4 C23 C22 -143.2(4) . . . . ? C46 N4 C23 C24 32.8(6) . . . . ? C46 N4 C25 C26 145.4(4) . . . . ? C46 N4 C25 C30 -36.1(6) . . . . ? C50A Cl5A C50A Cl5A 42(22) 7_556 . . 7_556 ?