#------------------------------------------------------------------------------ #$Date: 2016-01-01 10:18:01 +0200 (Fri, 01 Jan 2016) $ #$Revision: 171863 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/07/1540747.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_1540747 loop_ _publ_author_name 'Wicht, Richard' 'Bahnm\"uller, Stefanie' 'Brandhorst, Kai' 'Schweyen, Peter' 'Br\"oring, Martin' _publ_section_title ; Cationic nickel porphyrinoids with unexpected reactivity ; _journal_issue 1 _journal_name_full 'Chem. Sci.' _journal_page_first 583 _journal_paper_doi 10.1039/C5SC03663A _journal_volume 7 _journal_year 2016 _chemical_formula_moiety ; C72 H92 N8 Ni2, 2(B F4), 3.657(C H Cl3) ; _chemical_formula_sum 'C75.66 H95.66 B2 Cl10.97 F8 N8 Ni2' _chemical_formula_weight 1797.07 _chemical_name_systematic ; ? ; _chemical_properties_physical Moisture-sensitive _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _audit_update_record ; 2015-03-30 deposited with the CCDC. 2015-10-16 downloaded from the CCDC. ; _cell_angle_alpha 90.00 _cell_angle_beta 104.352(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.0884(11) _cell_length_b 31.4527(15) _cell_length_c 18.2241(14) _cell_measurement_reflns_used 18138 _cell_measurement_temperature 100.0(3) _cell_measurement_theta_max 75.2300 _cell_measurement_theta_min 3.6610 _cell_volume 8378.7(10) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_molecular_graphics ; ORTEP3 for Windows (L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.) ; _computing_publication_material ; WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.) ; _computing_structure_refinement ; SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 122-122)' ; _computing_structure_solution ; SHELXS-97 (G. M. Sheldrick, Z. Dauter, K. S, Wilson, H. Hope, L. C. Sieker, Acta Cryst. (1993), D49, 18) ; _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.3543 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Oxford Diffraction, Xcalibur, Atlas, Nova' _diffrn_measurement_method \w-scan _diffrn_radiation_monochromator mirror _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0904 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 95426 _diffrn_reflns_theta_full 74.99 _diffrn_reflns_theta_max 74.99 _diffrn_reflns_theta_min 3.33 _exptl_absorpt_coefficient_mu 4.311 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.62546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 3720.4 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: chloroform, n-hexane' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.564 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1039 _refine_ls_number_reflns 17132 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0660 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+8.0765P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1650 _refine_ls_wR_factor_ref 0.1844 _reflns_number_gt 12109 _reflns_number_total 17132 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL rwyybb in P2(1)/c CELL 1.54184 15.0884 31.4527 18.2241 90.000 104.352 90.000 ZERR 4.00 0.0011 0.0015 0.0014 0.000 0.007 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N CL NI B F UNIT 303 383 32 44 8 8 32 MERG 2 OMIT -2.00 150.00 OMIT -12 2 20 OMIT 0 2 2 OMIT 3 3 1 OMIT -2 2 1 OMIT -9 25 16 EADP C76 C76A EADP C75 C75A EADP CL10 CL15 EADP CL11 CL13 EADP CL12 CL14 FMAP 2 PLAN 10 ACTA BOND BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.093400 8.076499 FVAR 0.96901 0.92921 0.89091 0.79439 0.09927 0.86920 0.07470 C1 1 0.133380 0.097715 0.372393 11.00000 0.03172 0.02381 = 0.02548 0.00147 0.01023 -0.00395 C2 1 0.156880 0.053251 0.375945 11.00000 0.04526 0.01981 = 0.03250 0.00102 0.01038 -0.00367 C3 1 0.239458 0.050222 0.356119 11.00000 0.03768 0.02229 = 0.03775 0.00289 0.00990 -0.00222 C4 1 0.266470 0.092479 0.342494 11.00000 0.02842 0.02015 = 0.03051 0.00058 0.00647 0.00157 C5 1 0.345492 0.107576 0.322785 11.00000 0.03185 0.01976 = 0.02770 -0.00086 0.00756 0.00363 AFIX 43 H5 2 0.389180 0.087178 0.315935 11.00000 -1.20000 AFIX 0 C6 1 0.363814 0.149611 0.312791 11.00000 0.02284 0.02136 = 0.02265 0.00000 0.00809 0.00284 C7 1 0.444409 0.167294 0.294672 11.00000 0.02167 0.02848 = 0.02043 0.00049 0.00660 0.00234 C8 1 0.431033 0.210333 0.285935 11.00000 0.02313 0.02597 = 0.01920 0.00082 0.00690 0.00080 C9 1 0.339180 0.218247 0.293222 11.00000 0.02186 0.02039 = 0.01970 -0.00235 0.00531 -0.00248 C10 1 0.285373 0.258892 0.277177 11.00000 0.02033 0.02018 = 0.01985 0.00140 0.00892 -0.00202 AFIX 13 H10 2 0.330198 0.281860 0.274256 11.00000 -1.20000 AFIX 0 C11 1 0.245830 0.269688 0.346686 11.00000 0.02213 0.01659 = 0.02064 0.00145 0.00797 -0.00120 C12 1 0.194596 0.311051 0.343810 11.00000 0.02647 0.02002 = 0.01632 -0.00038 0.00636 0.00014 C13 1 0.113212 0.303131 0.360207 11.00000 0.02694 0.02359 = 0.01860 -0.00028 0.01000 0.00147 C14 1 0.105457 0.257345 0.366289 11.00000 0.02415 0.02418 = 0.01790 0.00231 0.00821 0.00061 C15 1 0.026962 0.236360 0.383182 11.00000 0.02061 0.02730 = 0.02264 0.00148 0.00851 -0.00102 AFIX 43 H15 2 -0.022260 0.253290 0.390543 11.00000 -1.20000 AFIX 0 C16 1 0.021482 0.193670 0.388788 11.00000 0.02286 0.02980 = 0.01764 0.00178 0.00897 -0.00137 C17 1 -0.050319 0.166401 0.406377 11.00000 0.02660 0.03340 = 0.02304 0.00294 0.01218 -0.00467 C18 1 -0.022751 0.125267 0.404512 11.00000 0.03272 0.03070 = 0.02252 0.00186 0.01057 -0.01009 C19 1 0.065728 0.126429 0.385305 11.00000 0.03062 0.02522 = 0.02320 0.00358 0.00918 -0.00325 C20 1 0.105269 0.016986 0.400672 11.00000 0.04279 0.02186 = 0.05430 0.00441 0.01757 -0.00600 AFIX 23 H20A 2 0.119882 -0.009713 0.377396 11.00000 -1.20000 H20B 2 0.038761 0.022154 0.381946 11.00000 -1.20000 AFIX 0 C21 1 0.128389 0.011599 0.486463 11.00000 0.05585 0.03661 = 0.06103 0.01838 0.01826 -0.01063 AFIX 137 H21A 2 0.194527 0.007652 0.505620 11.00000 -1.50000 H21B 2 0.096297 -0.013326 0.499335 11.00000 -1.50000 H21C 2 0.109205 0.037007 0.509581 11.00000 -1.50000 AFIX 0 C22 1 0.296574 0.011455 0.353903 11.00000 0.04692 0.02011 = 0.05976 0.00487 0.01036 0.00417 AFIX 23 H22A 2 0.321693 0.012874 0.308668 11.00000 -1.20000 H22B 2 0.257240 -0.014102 0.349008 11.00000 -1.20000 AFIX 0 C23 1 0.374364 0.007131 0.423600 11.00000 0.05224 0.03516 = 0.06903 0.00882 0.01070 0.00566 AFIX 137 H23A 2 0.414275 0.032079 0.428179 11.00000 -1.50000 H23B 2 0.409566 -0.018556 0.419461 11.00000 -1.50000 H23C 2 0.349846 0.005058 0.468490 11.00000 -1.50000 AFIX 0 C24 1 0.526095 0.141739 0.287119 11.00000 0.02631 0.03074 = 0.03003 -0.00016 0.01035 0.00775 AFIX 23 H24A 2 0.564601 0.159694 0.262821 11.00000 -1.20000 H24B 2 0.504444 0.117299 0.253174 11.00000 -1.20000 AFIX 0 C25 1 0.585173 0.124982 0.362335 11.00000 0.03264 0.04018 = 0.03534 0.00542 0.00760 0.01245 AFIX 137 H25A 2 0.605887 0.148860 0.396875 11.00000 -1.50000 H25B 2 0.638376 0.109992 0.353220 11.00000 -1.50000 H25C 2 0.549058 0.105371 0.385041 11.00000 -1.50000 AFIX 0 C26 1 0.501382 0.243465 0.281783 11.00000 0.02208 0.02775 = 0.02572 0.00039 0.00847 -0.00143 AFIX 23 H26A 2 0.470517 0.269615 0.258092 11.00000 -1.20000 H26B 2 0.541253 0.232917 0.250004 11.00000 -1.20000 AFIX 0 C27 1 0.559907 0.253725 0.362004 11.00000 0.02537 0.03570 = 0.02934 0.00063 0.00498 -0.00132 AFIX 137 H27A 2 0.521107 0.266431 0.392018 11.00000 -1.50000 H27B 2 0.608391 0.273774 0.358460 11.00000 -1.50000 H27C 2 0.587393 0.227484 0.386480 11.00000 -1.50000 AFIX 0 C28 1 0.324593 0.270112 0.419149 11.00000 0.02641 0.02305 = 0.02098 0.00075 0.00918 0.00090 AFIX 137 H28A 2 0.300426 0.277459 0.462720 11.00000 -1.50000 H28B 2 0.370356 0.291224 0.413820 11.00000 -1.50000 H28C 2 0.353047 0.241923 0.426955 11.00000 -1.50000 AFIX 0 C29 1 0.235776 0.353470 0.334417 11.00000 0.03112 0.01885 = 0.02777 -0.00090 0.01035 0.00047 AFIX 23 H29A 2 0.189418 0.370865 0.299075 11.00000 -1.20000 H29B 2 0.287644 0.349100 0.310955 11.00000 -1.20000 AFIX 0 C30 1 0.270067 0.378343 0.408424 11.00000 0.04154 0.02628 = 0.03806 -0.00481 0.00942 -0.00482 AFIX 137 H30A 2 0.219235 0.382989 0.432126 11.00000 -1.50000 H30B 2 0.294528 0.405841 0.397493 11.00000 -1.50000 H30C 2 0.318345 0.362091 0.442937 11.00000 -1.50000 AFIX 0 C31 1 0.043720 0.334375 0.372383 11.00000 0.02802 0.02505 = 0.02725 0.00199 0.01289 0.00557 AFIX 23 H31A 2 -0.018143 0.324161 0.346340 11.00000 -1.20000 H31B 2 0.053741 0.361968 0.349566 11.00000 -1.20000 AFIX 0 C32 1 0.048516 0.340950 0.456839 11.00000 0.03322 0.03284 = 0.03206 -0.00369 0.01393 0.00481 AFIX 137 H32A 2 0.035213 0.314038 0.479023 11.00000 -1.50000 H32B 2 0.003439 0.362372 0.462338 11.00000 -1.50000 H32C 2 0.109955 0.350631 0.483014 11.00000 -1.50000 AFIX 0 C33 1 -0.137473 0.182857 0.420229 11.00000 0.02868 0.03727 = 0.03534 -0.00179 0.01704 -0.00637 AFIX 23 H33A 2 -0.124895 0.209425 0.450137 11.00000 -1.20000 H33B 2 -0.162126 0.161770 0.450320 11.00000 -1.20000 AFIX 0 C34 1 -0.209032 0.191668 0.346318 11.00000 0.02838 0.04964 = 0.04592 -0.00025 0.00950 0.00009 AFIX 137 H34A 2 -0.184438 0.212129 0.315932 11.00000 -1.50000 H34B 2 -0.264260 0.203421 0.357741 11.00000 -1.50000 H34C 2 -0.224283 0.165103 0.317889 11.00000 -1.50000 AFIX 0 C35 1 -0.073951 0.086131 0.417295 11.00000 0.04140 0.02879 = 0.04077 -0.00194 0.02156 -0.01100 AFIX 23 H35A 2 -0.113338 0.093206 0.451685 11.00000 -1.20000 H35B 2 -0.029562 0.064258 0.442478 11.00000 -1.20000 AFIX 0 C36 1 -0.133295 0.067813 0.343790 11.00000 0.05149 0.04086 = 0.05608 -0.00416 0.01008 -0.01852 AFIX 137 H36A 2 -0.182966 0.087695 0.322329 11.00000 -1.50000 H36B 2 -0.159191 0.040580 0.354328 11.00000 -1.50000 H36C 2 -0.095801 0.063411 0.307559 11.00000 -1.50000 AFIX 0 C37 1 0.440153 0.133731 0.089175 11.00000 0.03177 0.02514 = 0.02196 -0.00078 0.00569 0.00484 C38 1 0.530447 0.134591 0.071917 11.00000 0.03009 0.03276 = 0.02287 -0.00039 0.00955 0.00963 C39 1 0.553634 0.176331 0.070353 11.00000 0.02791 0.03363 = 0.02109 -0.00193 0.00925 0.00554 C40 1 0.478870 0.201664 0.086489 11.00000 0.02487 0.02897 = 0.01952 -0.00059 0.00772 0.00020 C41 1 0.469596 0.244233 0.092962 11.00000 0.02329 0.02950 = 0.02077 -0.00024 0.00932 -0.00280 AFIX 43 H41 2 0.517310 0.262290 0.085977 11.00000 -1.20000 AFIX 0 C42 1 0.389570 0.263281 0.110155 11.00000 0.02395 0.02361 = 0.01801 -0.00190 0.00753 -0.00101 C43 1 0.379046 0.309060 0.118641 11.00000 0.02737 0.01930 = 0.02117 0.00058 0.00765 -0.00416 C44 1 0.297723 0.315146 0.135310 11.00000 0.02523 0.02046 = 0.01848 0.00077 0.00529 -0.00187 C45 1 0.249109 0.272832 0.130306 11.00000 0.02120 0.01813 = 0.01892 -0.00082 0.00824 0.00047 C46 1 0.210048 0.259665 0.199087 11.00000 0.01797 0.01969 = 0.01958 0.00018 0.00824 -0.00117 AFIX 13 H46 2 0.164441 0.281902 0.203864 11.00000 -1.20000 AFIX 0 C47 1 0.158201 0.218777 0.180370 11.00000 0.02025 0.02123 = 0.01864 0.00168 0.00775 -0.00124 C48 1 0.066449 0.209031 0.186984 11.00000 0.02245 0.03168 = 0.01807 0.00067 0.00581 -0.00396 C49 1 0.055893 0.166205 0.177675 11.00000 0.02746 0.03126 = 0.02106 -0.00017 0.00971 -0.00782 C50 1 0.138218 0.149988 0.159402 11.00000 0.02688 0.02536 = 0.02235 0.00207 0.00682 -0.00703 C51 1 0.161334 0.108359 0.150386 11.00000 0.03641 0.02249 = 0.02908 0.00083 0.00949 -0.00749 AFIX 43 H51 2 0.119503 0.086947 0.156837 11.00000 -1.20000 AFIX 0 C52 1 0.242743 0.095170 0.132239 11.00000 0.03781 0.02048 = 0.02904 0.00094 0.00903 -0.00260 C53 1 0.276315 0.053376 0.120557 11.00000 0.05360 0.01807 = 0.03768 0.00100 0.01219 -0.00046 C54 1 0.358272 0.058642 0.100276 11.00000 0.04524 0.02026 = 0.03457 -0.00178 0.00870 0.00521 C55 1 0.374896 0.103565 0.101701 11.00000 0.03199 0.02308 = 0.02468 -0.00130 0.00612 0.00429 C56 1 0.587566 0.097042 0.062303 11.00000 0.03698 0.03717 = 0.03626 0.00181 0.01888 0.01432 AFIX 23 H56A 2 0.629215 0.105330 0.030471 11.00000 -1.20000 H56B 2 0.547110 0.074162 0.035597 11.00000 -1.20000 AFIX 0 C57 1 0.644046 0.080077 0.137986 11.00000 0.04314 0.04211 = 0.04645 0.00517 0.00768 0.01539 AFIX 137 H57A 2 0.682797 0.102874 0.165371 11.00000 -1.50000 H57B 2 0.682635 0.056574 0.128925 11.00000 -1.50000 H57C 2 0.602964 0.069893 0.168245 11.00000 -1.50000 AFIX 0 C58 1 0.640760 0.195212 0.059521 11.00000 0.02877 0.04318 = 0.03299 0.00123 0.01420 0.00724 AFIX 23 H58A 2 0.626650 0.221712 0.029585 11.00000 -1.20000 H58B 2 0.669469 0.175068 0.030597 11.00000 -1.20000 AFIX 0 C59 1 0.707925 0.205073 0.135073 11.00000 0.03449 0.05686 = 0.04897 -0.00174 0.00822 -0.00743 AFIX 137 H59A 2 0.679819 0.225137 0.163718 11.00000 -1.50000 H59B 2 0.763587 0.217668 0.125860 11.00000 -1.50000 H59C 2 0.723515 0.178747 0.164176 11.00000 -1.50000 AFIX 0 C60 1 0.448089 0.341365 0.108372 11.00000 0.02979 0.02456 = 0.03076 -0.00096 0.01441 -0.00800 AFIX 23 H60A 2 0.510185 0.331185 0.133826 11.00000 -1.20000 H60B 2 0.437392 0.368332 0.132848 11.00000 -1.20000 AFIX 0 C61 1 0.443218 0.349775 0.024387 11.00000 0.03592 0.03505 = 0.03485 0.00177 0.01825 -0.00634 AFIX 137 H61A 2 0.456255 0.323405 0.000394 11.00000 -1.50000 H61B 2 0.488453 0.371423 0.020280 11.00000 -1.50000 H61C 2 0.381841 0.359857 -0.001065 11.00000 -1.50000 AFIX 0 C62 1 0.254938 0.356774 0.147361 11.00000 0.03130 0.02001 = 0.02561 0.00113 0.01272 0.00169 AFIX 23 H62A 2 0.301327 0.374417 0.182169 11.00000 -1.20000 H62B 2 0.204740 0.351305 0.172284 11.00000 -1.20000 AFIX 0 C63 1 0.216604 0.381955 0.074227 11.00000 0.04700 0.02494 = 0.03508 0.00551 0.01218 0.00471 AFIX 137 H63A 2 0.265895 0.387821 0.049327 11.00000 -1.50000 H63B 2 0.190758 0.408848 0.086463 11.00000 -1.50000 H63C 2 0.168684 0.365273 0.040197 11.00000 -1.50000 AFIX 0 C64 1 0.170299 0.273930 0.057682 11.00000 0.02500 0.02430 = 0.02161 0.00047 0.00738 -0.00145 AFIX 137 H64A 2 0.194205 0.282748 0.014709 11.00000 -1.50000 H64B 2 0.123563 0.294192 0.064325 11.00000 -1.50000 H64C 2 0.143136 0.245546 0.047943 11.00000 -1.50000 AFIX 0 C65 1 -0.004726 0.241266 0.193427 11.00000 0.02106 0.03236 = 0.02802 -0.00182 0.00962 -0.00159 AFIX 23 H65A 2 0.025573 0.266364 0.221649 11.00000 -1.20000 H65B 2 -0.046036 0.228852 0.222286 11.00000 -1.20000 AFIX 0 C66 1 -0.061065 0.255323 0.115024 11.00000 0.02839 0.04454 = 0.03141 0.00237 0.00956 0.00115 AFIX 137 H66A 2 -0.020307 0.267767 0.086487 11.00000 -1.50000 H66B 2 -0.106347 0.276533 0.120979 11.00000 -1.50000 H66C 2 -0.092501 0.230641 0.087564 11.00000 -1.50000 AFIX 0 C67 1 -0.023893 0.139036 0.184769 11.00000 0.03286 0.03535 = 0.03264 0.00148 0.00978 -0.01296 AFIX 23 H67A 2 -0.062426 0.155643 0.211128 11.00000 -1.20000 H67B 2 -0.000179 0.114091 0.216762 11.00000 -1.20000 AFIX 0 C68 1 -0.084068 0.123226 0.108963 11.00000 0.03785 0.05591 = 0.04050 0.00239 0.00677 -0.02517 AFIX 137 H68A 2 -0.108610 0.147655 0.076968 11.00000 -1.50000 H68B 2 -0.134700 0.106277 0.118236 11.00000 -1.50000 H68C 2 -0.047293 0.105658 0.083308 11.00000 -1.50000 AFIX 0 C69 1 0.228124 0.012357 0.128050 11.00000 0.07154 0.02102 = 0.06014 -0.00175 0.02452 -0.00588 AFIX 23 H69A 2 0.274328 -0.010423 0.143175 11.00000 -1.20000 H69B 2 0.195922 0.015428 0.168937 11.00000 -1.20000 AFIX 0 C70 1 0.161248 -0.000640 0.057633 11.00000 0.13161 0.07119 = 0.07078 -0.00325 0.01515 -0.05499 AFIX 137 H70A 2 0.117426 0.022458 0.040449 11.00000 -1.50000 H70B 2 0.128525 -0.026090 0.067456 11.00000 -1.50000 H70C 2 0.193507 -0.006894 0.018366 11.00000 -1.50000 AFIX 0 C71 1 0.411092 0.023894 0.074193 11.00000 0.05555 0.02344 = 0.04574 -0.00043 0.01498 0.01214 AFIX 23 H71A 2 0.397164 -0.003607 0.095282 11.00000 -1.20000 H71B 2 0.477446 0.029376 0.093187 11.00000 -1.20000 AFIX 0 C72 1 0.386576 0.021276 -0.012872 11.00000 0.05559 0.03739 = 0.04303 -0.00946 0.00985 0.01645 AFIX 137 H72A 2 0.320148 0.018469 -0.031925 11.00000 -1.50000 H72B 2 0.416752 -0.003483 -0.028586 11.00000 -1.50000 H72C 2 0.407222 0.047175 -0.033525 11.00000 -1.50000 AFIX 0 N1 3 0.201604 0.120119 0.352472 11.00000 0.02627 0.02176 = 0.02538 0.00291 0.00895 -0.00422 N2 3 0.301883 0.183045 0.314479 11.00000 0.02625 0.01676 = 0.01861 0.00133 0.00779 0.00323 N3 3 0.178048 0.237234 0.355614 11.00000 0.02068 0.02136 = 0.02015 0.00111 0.00839 -0.00187 N4 3 0.089140 0.167487 0.377263 11.00000 0.02783 0.02190 = 0.02402 0.00224 0.01100 -0.00254 N5 3 0.412508 0.173980 0.096315 11.00000 0.02602 0.02157 = 0.02377 -0.00329 0.00881 0.00078 N6 3 0.318110 0.241716 0.119828 11.00000 0.02238 0.01907 = 0.02064 -0.00173 0.00873 0.00074 N7 3 0.197324 0.184466 0.158079 11.00000 0.02572 0.01772 = 0.01896 -0.00006 0.00710 -0.00304 N8 3 0.303757 0.124271 0.121409 11.00000 0.03032 0.02176 = 0.02284 -0.00186 0.00954 0.00048 NI1 5 0.194429 0.178676 0.347931 11.00000 0.02341 0.01727 = 0.02318 0.00210 0.01016 -0.00110 NI2 5 0.305699 0.182787 0.125619 11.00000 0.02404 0.01719 = 0.02293 -0.00098 0.01007 -0.00030 B1 6 0.514576 0.374732 0.340088 11.00000 0.03391 0.03659 = 0.04139 -0.00170 0.01385 0.00295 B2 6 -0.003231 0.379376 0.157129 11.00000 0.03959 0.05328 = 0.04219 0.00096 0.01908 0.00422 F1 7 0.449004 0.343813 0.317121 11.00000 0.03426 0.05029 = 0.13010 -0.00797 0.01054 -0.00278 F2 7 0.587182 0.359195 0.396244 11.00000 0.05853 0.05629 = 0.04240 -0.00004 0.00687 0.01003 F3 7 0.548121 0.386363 0.278462 11.00000 0.07411 0.09710 = 0.04670 0.01003 0.02899 0.00970 F4 7 0.477572 0.410435 0.364975 11.00000 0.08230 0.04965 = 0.07025 -0.00449 0.03294 0.01957 F5 7 0.048012 0.344131 0.183404 11.00000 0.04777 0.06015 = 0.08180 0.01215 0.00613 0.00552 F6 7 0.055771 0.413252 0.164617 11.00000 0.10812 0.05648 = 0.25937 -0.03564 0.11865 -0.01633 F7 7 -0.062289 0.389120 0.201761 11.00000 0.04797 0.14152 = 0.05655 -0.01474 0.02093 0.00534 F8 7 -0.052427 0.373110 0.085566 11.00000 0.12521 0.15409 = 0.03904 -0.00166 0.00320 0.07141 C73 1 0.735104 0.123936 0.601666 21.00000 0.03381 0.03385 = 0.03466 0.00147 0.00995 0.00239 AFIX 13 H73 2 0.798962 0.125683 0.634224 21.00000 -1.20000 AFIX 0 CL1 4 0.701397 0.175676 0.563744 21.00000 0.04323 0.03109 = 0.04356 -0.00042 0.01378 -0.00245 CL2 4 0.733513 0.087816 0.527564 21.00000 0.04908 0.03217 = 0.03810 -0.00089 0.01663 0.00149 CL3 4 0.662986 0.106558 0.657485 21.00000 0.03689 0.03366 = 0.04419 0.00225 0.01730 0.00270 C74 1 0.570132 -0.028807 0.286667 31.00000 0.04768 0.03233 = 0.04298 -0.00270 0.01448 -0.00103 AFIX 13 H74 2 0.535212 -0.052958 0.257385 31.00000 -1.20000 AFIX 0 CL4 4 0.503224 0.017246 0.264636 31.00000 0.07642 0.05469 = 0.04891 0.01738 0.02761 0.02973 CL5 4 0.674599 -0.024043 0.260406 31.00000 0.04783 0.06176 = 0.10586 0.00868 0.02689 0.00154 CL6 4 0.590189 -0.040899 0.383025 31.00000 0.10850 0.04901 = 0.05061 0.01547 0.01445 0.01720 PART 1 C76 1 -0.048309 -0.028259 0.189929 41.00000 0.05001 0.02870 = 0.04975 0.00283 0.01146 -0.00561 AFIX 13 H76 2 -0.034457 -0.048636 0.233400 41.00000 -1.20000 AFIX 0 CL10 4 0.024146 0.016064 0.212301 41.00000 0.08216 0.06565 = 0.05755 -0.01780 0.03471 -0.04512 CL11 4 -0.030505 -0.053397 0.109662 41.00000 0.10997 0.03469 = 0.07317 -0.01237 0.03435 0.00109 CL12 4 -0.160416 -0.011631 0.174280 41.00000 0.03861 0.15792 = 0.10315 -0.05895 0.00726 0.00144 PART 2 SAME C76 CL10 CL11 CL12 C76A 1 -0.036215 -0.026419 0.215754 51.00000 0.05001 0.02870 = 0.04975 0.00283 0.01146 -0.00561 AFIX 13 H76A 2 -0.041147 -0.029316 0.269243 51.00000 -1.20000 AFIX 0 CL13 4 0.058512 -0.055354 0.203131 51.00000 0.10997 0.03469 = 0.07317 -0.01237 0.03435 0.00109 CL14 4 -0.135759 -0.044723 0.154018 51.00000 0.03861 0.15792 = 0.10315 -0.05895 0.00726 0.00144 CL15 4 -0.025936 0.026299 0.194536 51.00000 0.08216 0.06565 = 0.05755 -0.01780 0.03471 -0.04512 PART 1 C75 1 0.761863 0.164830 0.845973 61.00000 0.02854 0.03838 = 0.04347 0.00647 0.00968 -0.00033 AFIX 13 H75 2 0.695203 0.159401 0.840315 61.00000 -1.20000 AFIX 0 CL7 4 0.819076 0.116213 0.850547 61.00000 0.03879 0.03569 = 0.07875 0.00246 0.00472 0.00230 CL8 4 0.776153 0.194327 0.766999 61.00000 0.09094 0.03934 = 0.03753 0.00013 0.01540 -0.01127 CL9 4 0.805125 0.195392 0.929140 61.00000 0.03594 0.04763 = 0.03495 0.00218 0.01086 0.00206 PART 3 SAME C75 CL7 CL8 CL9 C75A 1 0.761686 0.124419 0.882789 71.00000 0.02854 0.03838 = 0.04347 0.00647 0.00968 -0.00033 AFIX 13 H75A 2 0.697649 0.125875 0.850505 71.00000 -1.20000 AFIX 0 CL16 4 0.764481 0.089460 0.956475 71.00000 0.06647 0.05269 = 0.07144 -0.00547 0.00227 0.01395 CL17 4 0.795833 0.176237 0.917635 71.00000 0.01922 0.03004 = 0.05263 -0.00887 0.01829 -0.00499 CL18 4 0.833042 0.103021 0.828182 71.00000 0.05005 0.04218 = 0.14145 0.04868 0.02750 0.01079 HKLF 4 REM rwyybb in P2(1)/c REM R1 = 0.0660 for 12109 Fo > 4sig(Fo) and 0.0946 for all 17132 data REM 1039 parameters refined using 12 restraints END WGHT 0.0934 8.0759 REM Highest difference peak 1.564, deepest hole -0.602, 1-sigma level 0.090 Q1 1 -0.1722 -0.0254 0.2212 11.00000 0.05 1.56 Q2 1 0.7132 0.1898 0.7104 11.00000 0.05 1.17 Q3 1 0.6677 -0.0068 0.3045 11.00000 0.05 1.11 Q4 1 -0.0902 -0.0426 0.0791 11.00000 0.05 1.03 Q5 1 0.6921 0.1974 0.5484 11.00000 0.05 1.01 Q6 1 0.6750 0.1132 0.6156 11.00000 0.05 0.94 Q7 1 0.7141 0.1926 0.7454 11.00000 0.05 0.94 Q8 1 0.5184 -0.0444 0.3740 11.00000 0.05 0.92 Q9 1 -0.1590 -0.0017 0.1709 11.00000 0.05 0.88 Q10 1 -0.0923 -0.0488 0.1273 11.00000 0.05 0.79 ; _cod_data_source_file c5sc03663a2.cif _cod_data_source_block rw100bb_(sb) _cod_original_sg_symbol_H-M P21/c _cod_database_code 1540747 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1334(3) 0.09772(11) 0.3724(2) 0.0264(7) Uani 1 1 d . . . C2 C 0.1569(3) 0.05325(11) 0.3759(2) 0.0324(8) Uani 1 1 d . . . C3 C 0.2395(3) 0.05022(11) 0.3561(2) 0.0325(8) Uani 1 1 d . . . C4 C 0.2665(3) 0.09248(11) 0.3425(2) 0.0265(7) Uani 1 1 d . . . C5 C 0.3455(3) 0.10758(11) 0.3228(2) 0.0264(7) Uani 1 1 d . . . H5 H 0.3892 0.0872 0.3159 0.032 Uiso 1 1 calc R . . C6 C 0.3638(2) 0.14961(10) 0.31279(19) 0.0219(7) Uani 1 1 d . . . C7 C 0.4444(2) 0.16729(11) 0.29467(19) 0.0233(7) Uani 1 1 d . . . C8 C 0.4310(2) 0.21033(11) 0.28593(19) 0.0225(7) Uani 1 1 d . . . C9 C 0.3392(2) 0.21825(10) 0.29322(18) 0.0206(6) Uani 1 1 d . . . C10 C 0.2854(2) 0.25889(10) 0.27718(18) 0.0194(6) Uani 1 1 d . . . H10 H 0.3302 0.2819 0.2743 0.023 Uiso 1 1 calc R . . C11 C 0.2458(2) 0.26969(10) 0.34669(18) 0.0193(6) Uani 1 1 d . . . C12 C 0.1946(2) 0.31105(10) 0.34381(18) 0.0207(6) Uani 1 1 d . . . C13 C 0.1132(2) 0.30313(11) 0.36021(18) 0.0223(7) Uani 1 1 d . . . C14 C 0.1055(2) 0.25734(10) 0.36629(18) 0.0215(7) Uani 1 1 d . . . C15 C 0.0270(2) 0.23636(11) 0.38318(19) 0.0230(7) Uani 1 1 d . . . H15 H -0.0223 0.2533 0.3905 0.028 Uiso 1 1 calc R . . C16 C 0.0215(2) 0.19367(11) 0.38879(18) 0.0227(7) Uani 1 1 d . . . C17 C -0.0503(3) 0.16640(12) 0.4064(2) 0.0266(7) Uani 1 1 d . . . C18 C -0.0228(3) 0.12527(12) 0.4045(2) 0.0280(8) Uani 1 1 d . . . C19 C 0.0657(3) 0.12643(11) 0.3853(2) 0.0259(7) Uani 1 1 d . . . C20 C 0.1053(3) 0.01699(12) 0.4007(3) 0.0387(10) Uani 1 1 d . . . H20A H 0.1199 -0.0097 0.3774 0.046 Uiso 1 1 calc R . . H20B H 0.0388 0.0222 0.3819 0.046 Uiso 1 1 calc R . . C21 C 0.1284(4) 0.01160(15) 0.4865(3) 0.0505(12) Uani 1 1 d . . . H21A H 0.1945 0.0077 0.5056 0.076 Uiso 1 1 calc R . . H21B H 0.0963 -0.0133 0.4993 0.076 Uiso 1 1 calc R . . H21C H 0.1092 0.0370 0.5096 0.076 Uiso 1 1 calc R . . C22 C 0.2966(3) 0.01145(12) 0.3539(3) 0.0428(10) Uani 1 1 d . . . H22A H 0.3217 0.0129 0.3087 0.051 Uiso 1 1 calc R . . H22B H 0.2572 -0.0141 0.3490 0.051 Uiso 1 1 calc R . . C23 C 0.3744(4) 0.00713(15) 0.4236(3) 0.0529(12) Uani 1 1 d . . . H23A H 0.4143 0.0321 0.4282 0.079 Uiso 1 1 calc R . . H23B H 0.4096 -0.0186 0.4195 0.079 Uiso 1 1 calc R . . H23C H 0.3498 0.0051 0.4685 0.079 Uiso 1 1 calc R . . C24 C 0.5261(3) 0.14174(12) 0.2871(2) 0.0284(8) Uani 1 1 d . . . H24A H 0.5646 0.1597 0.2628 0.034 Uiso 1 1 calc R . . H24B H 0.5044 0.1173 0.2532 0.034 Uiso 1 1 calc R . . C25 C 0.5852(3) 0.12498(13) 0.3623(2) 0.0362(9) Uani 1 1 d . . . H25A H 0.6059 0.1489 0.3969 0.054 Uiso 1 1 calc R . . H25B H 0.6384 0.1100 0.3532 0.054 Uiso 1 1 calc R . . H25C H 0.5491 0.1054 0.3850 0.054 Uiso 1 1 calc R . . C26 C 0.5014(2) 0.24347(11) 0.2818(2) 0.0247(7) Uani 1 1 d . . . H26A H 0.4705 0.2696 0.2581 0.030 Uiso 1 1 calc R . . H26B H 0.5413 0.2329 0.2500 0.030 Uiso 1 1 calc R . . C27 C 0.5599(3) 0.25372(12) 0.3620(2) 0.0305(8) Uani 1 1 d . . . H27A H 0.5211 0.2664 0.3920 0.046 Uiso 1 1 calc R . . H27B H 0.6084 0.2738 0.3585 0.046 Uiso 1 1 calc R . . H27C H 0.5874 0.2275 0.3865 0.046 Uiso 1 1 calc R . . C28 C 0.3246(2) 0.27011(10) 0.41915(19) 0.0229(7) Uani 1 1 d . . . H28A H 0.3004 0.2775 0.4627 0.034 Uiso 1 1 calc R . . H28B H 0.3704 0.2912 0.4138 0.034 Uiso 1 1 calc R . . H28C H 0.3530 0.2419 0.4270 0.034 Uiso 1 1 calc R . . C29 C 0.2358(3) 0.35347(10) 0.3344(2) 0.0254(7) Uani 1 1 d . . . H29A H 0.1894 0.3709 0.2991 0.030 Uiso 1 1 calc R . . H29B H 0.2876 0.3491 0.3110 0.030 Uiso 1 1 calc R . . C30 C 0.2701(3) 0.37834(12) 0.4084(2) 0.0354(9) Uani 1 1 d . . . H30A H 0.2192 0.3830 0.4321 0.053 Uiso 1 1 calc R . . H30B H 0.2945 0.4058 0.3975 0.053 Uiso 1 1 calc R . . H30C H 0.3183 0.3621 0.4429 0.053 Uiso 1 1 calc R . . C31 C 0.0437(3) 0.33438(11) 0.3724(2) 0.0257(7) Uani 1 1 d . . . H31A H -0.0181 0.3242 0.3463 0.031 Uiso 1 1 calc R . . H31B H 0.0537 0.3620 0.3496 0.031 Uiso 1 1 calc R . . C32 C 0.0485(3) 0.34095(12) 0.4568(2) 0.0317(8) Uani 1 1 d . . . H32A H 0.0352 0.3140 0.4790 0.048 Uiso 1 1 calc R . . H32B H 0.0034 0.3624 0.4623 0.048 Uiso 1 1 calc R . . H32C H 0.1100 0.3506 0.4830 0.048 Uiso 1 1 calc R . . C33 C -0.1375(3) 0.18286(13) 0.4202(2) 0.0322(8) Uani 1 1 d . . . H33A H -0.1249 0.2094 0.4501 0.039 Uiso 1 1 calc R . . H33B H -0.1621 0.1618 0.4503 0.039 Uiso 1 1 calc R . . C34 C -0.2090(3) 0.19167(15) 0.3463(3) 0.0413(10) Uani 1 1 d . . . H34A H -0.1844 0.2121 0.3159 0.062 Uiso 1 1 calc R . . H34B H -0.2643 0.2034 0.3577 0.062 Uiso 1 1 calc R . . H34C H -0.2243 0.1651 0.3179 0.062 Uiso 1 1 calc R . . C35 C -0.0740(3) 0.08613(12) 0.4173(2) 0.0350(9) Uani 1 1 d . . . H35A H -0.1133 0.0932 0.4517 0.042 Uiso 1 1 calc R . . H35B H -0.0296 0.0643 0.4425 0.042 Uiso 1 1 calc R . . C36 C -0.1333(4) 0.06781(15) 0.3438(3) 0.0500(12) Uani 1 1 d . . . H36A H -0.1830 0.0877 0.3223 0.075 Uiso 1 1 calc R . . H36B H -0.1592 0.0406 0.3543 0.075 Uiso 1 1 calc R . . H36C H -0.0958 0.0634 0.3076 0.075 Uiso 1 1 calc R . . C37 C 0.4402(3) 0.13373(11) 0.0892(2) 0.0265(7) Uani 1 1 d . . . C38 C 0.5304(3) 0.13459(12) 0.0719(2) 0.0280(8) Uani 1 1 d . . . C39 C 0.5536(3) 0.17633(12) 0.0704(2) 0.0270(7) Uani 1 1 d . . . C40 C 0.4789(2) 0.20166(11) 0.08649(19) 0.0241(7) Uani 1 1 d . . . C41 C 0.4696(2) 0.24423(11) 0.09296(19) 0.0238(7) Uani 1 1 d . . . H41 H 0.5173 0.2623 0.0860 0.029 Uiso 1 1 calc R . . C42 C 0.3896(2) 0.26328(10) 0.11016(18) 0.0214(7) Uani 1 1 d . . . C43 C 0.3790(2) 0.30906(10) 0.11864(19) 0.0223(7) Uani 1 1 d . . . C44 C 0.2977(2) 0.31515(10) 0.13531(18) 0.0214(7) Uani 1 1 d . . . C45 C 0.2491(2) 0.27283(10) 0.13031(18) 0.0188(6) Uani 1 1 d . . . C46 C 0.2100(2) 0.25966(10) 0.19909(18) 0.0184(6) Uani 1 1 d . . . H46 H 0.1644 0.2819 0.2039 0.022 Uiso 1 1 calc R . . C47 C 0.1582(2) 0.21878(10) 0.18037(18) 0.0195(6) Uani 1 1 d . . . C48 C 0.0664(2) 0.20903(11) 0.18698(19) 0.0239(7) Uani 1 1 d . . . C49 C 0.0559(3) 0.16621(12) 0.1777(2) 0.0259(7) Uani 1 1 d . . . C50 C 0.1382(3) 0.14999(11) 0.15940(19) 0.0247(7) Uani 1 1 d . . . C51 C 0.1613(3) 0.10836(11) 0.1504(2) 0.0291(8) Uani 1 1 d . . . H51 H 0.1195 0.0869 0.1568 0.035 Uiso 1 1 calc R . . C52 C 0.2427(3) 0.09517(11) 0.1322(2) 0.0290(8) Uani 1 1 d . . . C53 C 0.2763(3) 0.05338(11) 0.1206(2) 0.0363(9) Uani 1 1 d . . . C54 C 0.3583(3) 0.05864(11) 0.1003(2) 0.0336(9) Uani 1 1 d . . . C55 C 0.3749(3) 0.10357(11) 0.1017(2) 0.0267(7) Uani 1 1 d . . . C56 C 0.5876(3) 0.09704(13) 0.0623(2) 0.0351(9) Uani 1 1 d . . . H56A H 0.6292 0.1053 0.0305 0.042 Uiso 1 1 calc R . . H56B H 0.5471 0.0742 0.0356 0.042 Uiso 1 1 calc R . . C57 C 0.6440(3) 0.08008(15) 0.1380(3) 0.0445(10) Uani 1 1 d . . . H57A H 0.6828 0.1029 0.1654 0.067 Uiso 1 1 calc R . . H57B H 0.6826 0.0566 0.1289 0.067 Uiso 1 1 calc R . . H57C H 0.6030 0.0699 0.1682 0.067 Uiso 1 1 calc R . . C58 C 0.6408(3) 0.19521(13) 0.0595(2) 0.0338(8) Uani 1 1 d . . . H58A H 0.6267 0.2217 0.0296 0.041 Uiso 1 1 calc R . . H58B H 0.6695 0.1751 0.0306 0.041 Uiso 1 1 calc R . . C59 C 0.7079(3) 0.20507(16) 0.1351(3) 0.0471(11) Uani 1 1 d . . . H59A H 0.6798 0.2251 0.1637 0.071 Uiso 1 1 calc R . . H59B H 0.7636 0.2177 0.1259 0.071 Uiso 1 1 calc R . . H59C H 0.7235 0.1787 0.1642 0.071 Uiso 1 1 calc R . . C60 C 0.4481(3) 0.34137(11) 0.1084(2) 0.0272(7) Uani 1 1 d . . . H60A H 0.5102 0.3312 0.1338 0.033 Uiso 1 1 calc R . . H60B H 0.4374 0.3683 0.1328 0.033 Uiso 1 1 calc R . . C61 C 0.4432(3) 0.34977(13) 0.0244(2) 0.0336(8) Uani 1 1 d . . . H61A H 0.4563 0.3234 0.0004 0.050 Uiso 1 1 calc R . . H61B H 0.4885 0.3714 0.0203 0.050 Uiso 1 1 calc R . . H61C H 0.3818 0.3599 -0.0011 0.050 Uiso 1 1 calc R . . C62 C 0.2549(3) 0.35677(10) 0.1474(2) 0.0246(7) Uani 1 1 d . . . H62A H 0.3013 0.3744 0.1822 0.030 Uiso 1 1 calc R . . H62B H 0.2047 0.3513 0.1723 0.030 Uiso 1 1 calc R . . C63 C 0.2166(3) 0.38196(12) 0.0742(2) 0.0353(9) Uani 1 1 d . . . H63A H 0.2659 0.3878 0.0493 0.053 Uiso 1 1 calc R . . H63B H 0.1908 0.4088 0.0865 0.053 Uiso 1 1 calc R . . H63C H 0.1687 0.3653 0.0402 0.053 Uiso 1 1 calc R . . C64 C 0.1703(2) 0.27393(11) 0.05768(19) 0.0234(7) Uani 1 1 d . . . H64A H 0.1942 0.2827 0.0147 0.035 Uiso 1 1 calc R . . H64B H 0.1236 0.2942 0.0643 0.035 Uiso 1 1 calc R . . H64C H 0.1431 0.2455 0.0479 0.035 Uiso 1 1 calc R . . C65 C -0.0047(2) 0.24127(12) 0.1934(2) 0.0265(7) Uani 1 1 d . . . H65A H 0.0256 0.2664 0.2216 0.032 Uiso 1 1 calc R . . H65B H -0.0460 0.2289 0.2223 0.032 Uiso 1 1 calc R . . C66 C -0.0611(3) 0.25532(13) 0.1150(2) 0.0344(8) Uani 1 1 d . . . H66A H -0.0203 0.2678 0.0865 0.052 Uiso 1 1 calc R . . H66B H -0.1063 0.2765 0.1210 0.052 Uiso 1 1 calc R . . H66C H -0.0925 0.2306 0.0876 0.052 Uiso 1 1 calc R . . C67 C -0.0239(3) 0.13904(13) 0.1848(2) 0.0333(8) Uani 1 1 d . . . H67A H -0.0624 0.1556 0.2111 0.040 Uiso 1 1 calc R . . H67B H -0.0002 0.1141 0.2168 0.040 Uiso 1 1 calc R . . C68 C -0.0841(3) 0.12323(16) 0.1090(3) 0.0453(11) Uani 1 1 d . . . H68A H -0.1086 0.1477 0.0770 0.068 Uiso 1 1 calc R . . H68B H -0.1347 0.1063 0.1182 0.068 Uiso 1 1 calc R . . H68C H -0.0473 0.1057 0.0833 0.068 Uiso 1 1 calc R . . C69 C 0.2281(4) 0.01236(13) 0.1280(3) 0.0495(12) Uani 1 1 d . . . H69A H 0.2743 -0.0104 0.1432 0.059 Uiso 1 1 calc R . . H69B H 0.1959 0.0154 0.1689 0.059 Uiso 1 1 calc R . . C70 C 0.1612(6) -0.0006(2) 0.0576(4) 0.093(3) Uani 1 1 d . . . H70A H 0.1174 0.0225 0.0404 0.139 Uiso 1 1 calc R . . H70B H 0.1285 -0.0261 0.0675 0.139 Uiso 1 1 calc R . . H70C H 0.1935 -0.0069 0.0184 0.139 Uiso 1 1 calc R . . C71 C 0.4111(3) 0.02389(12) 0.0742(3) 0.0411(10) Uani 1 1 d . . . H71A H 0.3972 -0.0036 0.0953 0.049 Uiso 1 1 calc R . . H71B H 0.4774 0.0294 0.0932 0.049 Uiso 1 1 calc R . . C72 C 0.3866(4) 0.02128(14) -0.0129(3) 0.0458(11) Uani 1 1 d . . . H72A H 0.3201 0.0185 -0.0319 0.069 Uiso 1 1 calc R . . H72B H 0.4168 -0.0035 -0.0286 0.069 Uiso 1 1 calc R . . H72C H 0.4072 0.0472 -0.0335 0.069 Uiso 1 1 calc R . . N1 N 0.2016(2) 0.12012(9) 0.35247(17) 0.0240(6) Uani 1 1 d . . . N2 N 0.3019(2) 0.18304(8) 0.31448(15) 0.0201(6) Uani 1 1 d . . . N3 N 0.17805(19) 0.23723(8) 0.35561(15) 0.0201(5) Uani 1 1 d . . . N4 N 0.0891(2) 0.16749(9) 0.37726(16) 0.0238(6) Uani 1 1 d . . . N5 N 0.4125(2) 0.17398(9) 0.09631(16) 0.0233(6) Uani 1 1 d . . . N6 N 0.3181(2) 0.24172(8) 0.11983(15) 0.0201(6) Uani 1 1 d . . . N7 N 0.1973(2) 0.18447(8) 0.15808(15) 0.0205(6) Uani 1 1 d . . . N8 N 0.3038(2) 0.12427(9) 0.12141(16) 0.0245(6) Uani 1 1 d . . . Ni1 Ni 0.19443(4) 0.178676(17) 0.34793(3) 0.02051(15) Uani 1 1 d . . . Ni2 Ni 0.30570(4) 0.182787(17) 0.12562(3) 0.02064(15) Uani 1 1 d . . . B1 B 0.5146(3) 0.37473(15) 0.3401(3) 0.0365(10) Uani 1 1 d . . . B2 B -0.0032(4) 0.37938(18) 0.1571(3) 0.0434(12) Uani 1 1 d . . . F1 F 0.4490(2) 0.34381(10) 0.3171(2) 0.0733(10) Uani 1 1 d . . . F2 F 0.5872(2) 0.35919(9) 0.39624(16) 0.0534(7) Uani 1 1 d . . . F3 F 0.5481(3) 0.38636(12) 0.27846(18) 0.0702(9) Uani 1 1 d . . . F4 F 0.4776(2) 0.41043(10) 0.36497(19) 0.0649(9) Uani 1 1 d . . . F5 F 0.0480(2) 0.34413(10) 0.1834(2) 0.0650(8) Uani 1 1 d . . . F6 F 0.0558(3) 0.41325(12) 0.1646(4) 0.128(2) Uani 1 1 d . . . F7 F -0.0623(2) 0.38912(15) 0.2018(2) 0.0806(11) Uani 1 1 d . . . F8 F -0.0524(3) 0.37311(17) 0.0856(2) 0.1091(18) Uani 1 1 d . . . C73 C 0.7351(3) 0.12394(13) 0.6017(2) 0.0338(9) Uani 0.929(3) 1 d P . . H73 H 0.7990 0.1257 0.6342 0.041 Uiso 0.929(3) 1 calc PR . . Cl1 Cl 0.70140(8) 0.17568(3) 0.56374(6) 0.0388(3) Uani 0.929(3) 1 d P . . Cl2 Cl 0.73351(8) 0.08782(3) 0.52756(6) 0.0388(3) Uani 0.929(3) 1 d P . . Cl3 Cl 0.66299(8) 0.10656(3) 0.65749(6) 0.0370(3) Uani 0.929(3) 1 d P . . C74 C 0.5701(4) -0.02881(15) 0.2867(3) 0.0404(11) Uani 0.891(3) 1 d P . . H74 H 0.5352 -0.0530 0.2574 0.049 Uiso 0.891(3) 1 calc PR . . Cl4 Cl 0.50322(12) 0.01725(5) 0.26464(8) 0.0579(4) Uani 0.891(3) 1 d P . . Cl5 Cl 0.67460(11) -0.02404(5) 0.26041(12) 0.0704(5) Uani 0.891(3) 1 d P . . Cl6 Cl 0.59019(14) -0.04090(5) 0.38303(9) 0.0703(5) Uani 0.891(3) 1 d P . . C76 C -0.0483(4) -0.02826(17) 0.1899(3) 0.0430(14) Uani 0.794(3) 1 d PD A 1 H76 H -0.0345 -0.0486 0.2334 0.052 Uiso 0.794(3) 1 calc PR A 1 Cl10 Cl 0.02415(16) 0.01606(6) 0.21230(11) 0.0654(6) Uani 0.794(3) 1 d PD A 1 Cl11 Cl -0.03050(16) -0.05340(5) 0.10966(11) 0.0706(6) Uani 0.794(3) 1 d PD A 1 Cl12 Cl -0.1604(2) -0.0116(1) 0.1742(2) 0.1017(10) Uani 0.794(3) 1 d PD A 1 C76A C -0.0362(16) -0.0264(7) 0.216(2) 0.0430(14) Uani 0.099(2) 1 d PD B 2 H76A H -0.0411 -0.0293 0.2692 0.052 Uiso 0.099(2) 1 calc PR B 2 Cl13 Cl 0.0585(12) -0.0554(4) 0.2031(9) 0.0706(6) Uani 0.099(2) 1 d PD B 2 Cl14 Cl -0.1358(10) -0.0447(7) 0.1540(12) 0.1017(10) Uani 0.099(2) 1 d PD B 2 Cl15 Cl -0.0259(13) 0.0263(5) 0.1945(10) 0.0654(6) Uani 0.099(2) 1 d PD B 2 C75 C 0.7619(3) 0.16483(15) 0.8460(3) 0.0367(10) Uani 0.869(4) 1 d PD C 1 H75 H 0.6952 0.1594 0.8403 0.044 Uiso 0.869(4) 1 calc PR C 1 Cl7 Cl 0.81908(15) 0.11621(6) 0.85055(14) 0.0528(5) Uani 0.869(4) 1 d PD C 1 Cl8 Cl 0.77615(12) 0.19433(4) 0.76700(8) 0.0560(5) Uani 0.869(4) 1 d PD C 1 Cl9 Cl 0.80512(11) 0.19539(6) 0.92914(8) 0.0391(4) Uani 0.869(4) 1 d PD C 1 C75A C 0.762(3) 0.1244(7) 0.8828(17) 0.0367(10) Uani 0.075(4) 1 d PD D 3 H75A H 0.6976 0.1259 0.8505 0.044 Uiso 0.075(4) 1 calc PR D 3 Cl16 Cl 0.7645(14) 0.0895(5) 0.9565(11) 0.066(6) Uani 0.075(4) 1 d PD D 3 Cl17 Cl 0.7958(10) 0.1762(5) 0.9176(10) 0.032(4) Uani 0.075(4) 1 d PD D 3 Cl18 Cl 0.833(2) 0.1030(8) 0.8282(17) 0.077(10) Uani 0.075(4) 1 d PD D 3 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 C1 0.032(2) 0.0238(17) 0.0255(18) 0.0015(13) 0.0102(15) -0.0040(14) C2 0.045(2) 0.0198(17) 0.033(2) 0.0010(14) 0.0104(17) -0.0037(15) C3 0.038(2) 0.0223(17) 0.038(2) 0.0029(15) 0.0099(17) -0.0022(15) C4 0.0284(19) 0.0201(16) 0.0305(19) 0.0006(13) 0.0065(15) 0.0016(13) C5 0.0318(19) 0.0198(16) 0.0277(18) -0.0009(13) 0.0076(15) 0.0036(13) C6 0.0228(17) 0.0214(15) 0.0227(16) 0.0000(12) 0.0081(13) 0.0028(12) C7 0.0217(17) 0.0285(17) 0.0204(16) 0.0005(13) 0.0066(13) 0.0023(13) C8 0.0231(17) 0.0260(16) 0.0192(16) 0.0008(12) 0.0069(13) 0.0008(13) C9 0.0219(17) 0.0204(15) 0.0197(15) -0.0023(12) 0.0053(12) -0.0025(12) C10 0.0203(16) 0.0202(15) 0.0198(16) 0.0014(12) 0.0089(12) -0.0020(12) C11 0.0221(16) 0.0166(14) 0.0206(16) 0.0014(11) 0.0080(13) -0.0012(12) C12 0.0265(17) 0.0200(15) 0.0163(15) -0.0004(11) 0.0064(13) 0.0001(13) C13 0.0269(18) 0.0236(16) 0.0186(16) -0.0003(12) 0.0100(13) 0.0015(13) C14 0.0241(17) 0.0242(16) 0.0179(15) 0.0023(12) 0.0082(13) 0.0006(13) C15 0.0206(17) 0.0273(17) 0.0226(17) 0.0015(13) 0.0085(13) -0.0010(13) C16 0.0229(17) 0.0298(17) 0.0176(15) 0.0018(12) 0.0090(13) -0.0014(13) C17 0.0266(19) 0.0334(18) 0.0230(17) 0.0029(14) 0.0122(14) -0.0047(14) C18 0.033(2) 0.0307(18) 0.0225(17) 0.0019(14) 0.0106(15) -0.0101(15) C19 0.0306(19) 0.0252(17) 0.0232(17) 0.0036(13) 0.0092(14) -0.0032(14) C20 0.043(2) 0.0219(17) 0.054(3) 0.0044(17) 0.018(2) -0.0060(16) C21 0.056(3) 0.037(2) 0.061(3) 0.018(2) 0.018(2) -0.011(2) C22 0.047(3) 0.0201(18) 0.060(3) 0.0049(17) 0.010(2) 0.0042(17) C23 0.052(3) 0.035(2) 0.069(3) 0.009(2) 0.011(3) 0.006(2) C24 0.0263(19) 0.0307(18) 0.0300(19) -0.0002(14) 0.0103(15) 0.0077(14) C25 0.033(2) 0.040(2) 0.035(2) 0.0054(17) 0.0076(17) 0.0124(17) C26 0.0221(17) 0.0278(17) 0.0257(17) 0.0004(13) 0.0085(14) -0.0014(13) C27 0.0254(19) 0.0357(19) 0.0293(19) 0.0006(15) 0.0050(15) -0.0013(15) C28 0.0264(18) 0.0230(16) 0.0210(16) 0.0008(12) 0.0092(14) 0.0009(13) C29 0.0311(19) 0.0189(15) 0.0278(18) -0.0009(13) 0.0103(15) 0.0005(13) C30 0.042(2) 0.0263(18) 0.038(2) -0.0048(15) 0.0094(18) -0.0048(16) C31 0.0280(19) 0.0251(16) 0.0272(18) 0.0020(13) 0.0129(15) 0.0056(14) C32 0.033(2) 0.0328(19) 0.032(2) -0.0037(15) 0.0139(16) 0.0048(15) C33 0.029(2) 0.037(2) 0.035(2) -0.0018(16) 0.0170(16) -0.0064(16) C34 0.028(2) 0.050(2) 0.046(2) -0.0003(19) 0.0095(18) 0.0001(18) C35 0.041(2) 0.0288(18) 0.041(2) -0.0019(16) 0.0216(19) -0.0110(16) C36 0.051(3) 0.041(2) 0.056(3) -0.004(2) 0.010(2) -0.019(2) C37 0.032(2) 0.0251(17) 0.0220(17) -0.0008(13) 0.0057(14) 0.0048(14) C38 0.030(2) 0.0328(18) 0.0229(17) -0.0004(14) 0.0095(15) 0.0096(15) C39 0.0279(19) 0.0336(18) 0.0211(17) -0.0019(13) 0.0092(14) 0.0055(14) C40 0.0249(18) 0.0290(17) 0.0195(16) -0.0006(13) 0.0077(13) 0.0002(14) C41 0.0233(17) 0.0295(17) 0.0208(16) -0.0002(13) 0.0093(13) -0.0028(13) C42 0.0239(17) 0.0236(16) 0.0180(15) -0.0019(12) 0.0075(13) -0.0010(13) C43 0.0274(18) 0.0193(15) 0.0212(16) 0.0006(12) 0.0077(13) -0.0042(13) C44 0.0252(17) 0.0205(15) 0.0185(15) 0.0008(12) 0.0053(13) -0.0019(13) C45 0.0212(16) 0.0181(14) 0.0189(15) -0.0008(11) 0.0082(13) 0.0005(12) C46 0.0180(16) 0.0197(14) 0.0196(15) 0.0002(12) 0.0082(12) -0.0012(12) C47 0.0202(16) 0.0212(15) 0.0186(15) 0.0017(12) 0.0077(12) -0.0012(12) C48 0.0224(18) 0.0317(18) 0.0181(16) 0.0007(13) 0.0058(13) -0.0040(14) C49 0.0275(19) 0.0313(17) 0.0211(17) -0.0002(13) 0.0097(14) -0.0078(14) C50 0.0269(18) 0.0254(16) 0.0224(17) 0.0021(13) 0.0068(14) -0.0070(13) C51 0.036(2) 0.0225(17) 0.0291(19) 0.0008(13) 0.0095(16) -0.0075(14) C52 0.038(2) 0.0205(16) 0.0290(19) 0.0009(13) 0.0090(16) -0.0026(14) C53 0.054(3) 0.0181(17) 0.038(2) 0.0010(14) 0.0122(19) -0.0005(16) C54 0.045(2) 0.0203(17) 0.035(2) -0.0018(14) 0.0087(17) 0.0052(15) C55 0.032(2) 0.0231(16) 0.0247(17) -0.0013(13) 0.0061(14) 0.0043(14) C56 0.037(2) 0.037(2) 0.036(2) 0.0018(16) 0.0189(18) 0.0143(17) C57 0.043(3) 0.042(2) 0.046(3) 0.0052(19) 0.008(2) 0.0154(19) C58 0.029(2) 0.043(2) 0.033(2) 0.0012(16) 0.0142(16) 0.0072(16) C59 0.034(2) 0.057(3) 0.049(3) -0.002(2) 0.008(2) -0.007(2) C60 0.0298(19) 0.0246(17) 0.0308(19) -0.0010(14) 0.0144(15) -0.0080(14) C61 0.036(2) 0.035(2) 0.035(2) 0.0018(16) 0.0182(17) -0.0063(16) C62 0.0313(19) 0.0200(15) 0.0256(17) 0.0011(13) 0.0127(15) 0.0017(13) C63 0.047(2) 0.0249(18) 0.035(2) 0.0055(15) 0.0122(18) 0.0047(16) C64 0.0250(18) 0.0243(16) 0.0216(16) 0.0005(12) 0.0074(14) -0.0015(13) C65 0.0211(17) 0.0324(18) 0.0280(18) -0.0018(14) 0.0096(14) -0.0016(14) C66 0.028(2) 0.045(2) 0.031(2) 0.0024(16) 0.0096(16) 0.0012(16) C67 0.033(2) 0.035(2) 0.033(2) 0.0015(15) 0.0098(16) -0.0130(16) C68 0.038(2) 0.056(3) 0.041(2) 0.002(2) 0.0068(19) -0.025(2) C69 0.072(3) 0.0210(19) 0.060(3) -0.0018(18) 0.025(3) -0.006(2) C70 0.132(7) 0.071(4) 0.071(4) -0.003(3) 0.015(4) -0.055(4) C71 0.056(3) 0.0234(18) 0.046(2) -0.0004(16) 0.015(2) 0.0121(18) C72 0.056(3) 0.037(2) 0.043(2) -0.0095(18) 0.010(2) 0.016(2) N1 0.0263(16) 0.0218(13) 0.0254(15) 0.0029(11) 0.0089(12) -0.0042(11) N2 0.0263(15) 0.0168(12) 0.0186(13) 0.0013(10) 0.0078(11) 0.0032(11) N3 0.0207(14) 0.0214(13) 0.0201(13) 0.0011(10) 0.0084(11) -0.0019(11) N4 0.0278(16) 0.0219(13) 0.0240(15) 0.0022(11) 0.0110(12) -0.0025(11) N5 0.0260(15) 0.0216(14) 0.0238(14) -0.0033(11) 0.0088(12) 0.0008(11) N6 0.0224(14) 0.0191(13) 0.0206(14) -0.0017(10) 0.0087(11) 0.0007(10) N7 0.0257(15) 0.0177(12) 0.0190(13) -0.0001(10) 0.0071(11) -0.0030(11) N8 0.0303(16) 0.0218(14) 0.0228(14) -0.0019(11) 0.0095(12) 0.0005(12) Ni1 0.0234(3) 0.0173(3) 0.0232(3) 0.0021(2) 0.0102(2) -0.0011(2) Ni2 0.0240(3) 0.0172(3) 0.0229(3) -0.0010(2) 0.0101(2) -0.0003(2) B1 0.034(2) 0.037(2) 0.041(3) -0.0017(19) 0.014(2) 0.0029(19) B2 0.040(3) 0.053(3) 0.042(3) 0.001(2) 0.019(2) 0.004(2) F1 0.0343(16) 0.0503(17) 0.130(3) -0.0080(18) 0.0105(18) -0.0028(13) F2 0.0585(18) 0.0563(16) 0.0424(15) 0.0000(12) 0.0069(13) 0.0100(13) F3 0.074(2) 0.097(3) 0.0467(17) 0.0100(16) 0.0290(17) 0.0097(19) F4 0.082(2) 0.0496(17) 0.070(2) -0.0045(14) 0.0329(18) 0.0196(16) F5 0.0478(18) 0.0602(19) 0.082(2) 0.0122(16) 0.0061(16) 0.0055(14) F6 0.108(4) 0.056(2) 0.259(7) -0.036(3) 0.119(4) -0.016(2) F7 0.0480(19) 0.142(4) 0.057(2) -0.015(2) 0.0209(16) 0.005(2) F8 0.125(4) 0.154(4) 0.0390(18) -0.002(2) 0.003(2) 0.071(3) C73 0.034(2) 0.034(2) 0.035(2) 0.0015(17) 0.0099(18) 0.0024(17) Cl1 0.0432(6) 0.0311(5) 0.0436(6) -0.0004(4) 0.0138(5) -0.0024(4) Cl2 0.0491(7) 0.0322(5) 0.0381(6) -0.0009(4) 0.0166(5) 0.0015(4) Cl3 0.0369(6) 0.0337(5) 0.0442(6) 0.0023(4) 0.0173(5) 0.0027(4) C74 0.048(3) 0.032(2) 0.043(3) -0.0027(19) 0.014(2) -0.001(2) Cl4 0.0764(10) 0.0547(8) 0.0489(8) 0.0174(6) 0.0276(7) 0.0297(7) Cl5 0.0478(9) 0.0618(9) 0.1059(14) 0.0087(9) 0.0269(9) 0.0015(7) Cl6 0.1085(15) 0.0490(8) 0.0506(8) 0.0155(6) 0.0144(8) 0.0172(8) C76 0.050(3) 0.029(2) 0.050(4) 0.003(2) 0.011(3) -0.006(2) Cl10 0.0822(14) 0.0657(11) 0.0575(11) -0.0178(8) 0.0347(11) -0.0451(11) Cl11 0.1100(17) 0.0347(8) 0.0732(12) -0.0124(7) 0.0344(11) 0.0011(8) Cl12 0.0386(10) 0.158(2) 0.1032(18) -0.0589(17) 0.0073(10) 0.0014(12) C76A 0.050(3) 0.029(2) 0.050(4) 0.003(2) 0.011(3) -0.006(2) Cl13 0.1100(17) 0.0347(8) 0.0732(12) -0.0124(7) 0.0344(11) 0.0011(8) Cl14 0.0386(10) 0.158(2) 0.1032(18) -0.0589(17) 0.0073(10) 0.0014(12) Cl15 0.0822(14) 0.0657(11) 0.0575(11) -0.0178(8) 0.0347(11) -0.0451(11) C75 0.029(2) 0.038(2) 0.043(3) 0.006(2) 0.010(2) -0.0003(18) Cl7 0.0388(10) 0.0357(10) 0.0787(11) 0.0025(8) 0.0047(8) 0.0023(7) Cl8 0.0909(12) 0.0393(7) 0.0375(7) 0.0001(5) 0.0154(7) -0.0113(7) Cl9 0.0359(7) 0.0476(10) 0.0350(7) 0.0022(7) 0.0109(5) 0.0021(7) C75A 0.029(2) 0.038(2) 0.043(3) 0.006(2) 0.010(2) -0.0003(18) Cl16 0.066(12) 0.053(10) 0.071(12) -0.005(8) 0.002(9) 0.014(8) Cl17 0.019(6) 0.030(8) 0.053(9) -0.009(7) 0.018(6) -0.005(6) Cl18 0.050(12) 0.042(14) 0.14(3) 0.049(16) 0.028(15) 0.011(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' N N 0.0311 0.0180 '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' Ni Ni -3.0029 0.5091 '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' F F 0.0727 0.0534 '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 N1 C1 C19 109.5(3) N1 C1 C2 108.6(3) C19 C1 C2 141.8(3) C3 C2 C1 106.4(3) C3 C2 C20 126.1(3) C1 C2 C20 127.4(4) C2 C3 C4 107.2(3) C2 C3 C22 128.6(4) C4 C3 C22 124.1(4) N1 C4 C5 120.2(3) N1 C4 C3 109.1(3) C5 C4 C3 130.7(3) C6 C5 C4 124.7(3) C6 C5 H5 117.7 C4 C5 H5 117.7 C5 C6 N2 124.0(3) C5 C6 C7 127.5(3) N2 C6 C7 108.5(3) C8 C7 C6 107.3(3) C8 C7 C24 128.0(3) C6 C7 C24 124.6(3) C7 C8 C9 106.0(3) C7 C8 C26 127.2(3) C9 C8 C26 126.2(3) N2 C9 C8 111.4(3) N2 C9 C10 120.8(3) C8 C9 C10 127.7(3) C9 C10 C11 108.8(3) C9 C10 C46 114.8(3) C11 C10 C46 113.0(3) C9 C10 H10 106.5 C11 C10 H10 106.5 C46 C10 H10 106.5 N3 C11 C12 103.7(3) N3 C11 C28 108.6(3) C12 C11 C28 107.6(3) N3 C11 C10 110.6(3) C12 C11 C10 117.0(3) C28 C11 C10 109.1(3) C13 C12 C29 127.7(3) C13 C12 C11 108.6(3) C29 C12 C11 123.3(3) C12 C13 C14 107.1(3) C12 C13 C31 128.2(3) C14 C13 C31 124.7(3) N3 C14 C13 112.2(3) N3 C14 C15 124.2(3) C13 C14 C15 123.5(3) C16 C15 C14 122.4(3) C16 C15 H15 118.8 C14 C15 H15 118.8 C15 C16 N4 121.7(3) C15 C16 C17 130.9(3) N4 C16 C17 107.4(3) C18 C17 C16 107.5(3) C18 C17 C33 128.4(3) C16 C17 C33 124.0(3) C17 C18 C19 106.5(3) C17 C18 C35 127.1(4) C19 C18 C35 126.4(3) N4 C19 C1 111.7(3) N4 C19 C18 109.1(3) C1 C19 C18 139.2(3) C2 C20 C21 112.7(4) C2 C20 H20A 109.1 C21 C20 H20A 109.1 C2 C20 H20B 109.1 C21 C20 H20B 109.1 H20A C20 H20B 107.8 C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C3 C22 C23 112.6(4) C3 C22 H22A 109.1 C23 C22 H22A 109.1 C3 C22 H22B 109.1 C23 C22 H22B 109.1 H22A C22 H22B 107.8 C22 C23 H23A 109.5 C22 C23 H23B 109.5 H23A C23 H23B 109.5 C22 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C7 C24 C25 114.2(3) C7 C24 H24A 108.7 C25 C24 H24A 108.7 C7 C24 H24B 108.7 C25 C24 H24B 108.7 H24A C24 H24B 107.6 C24 C25 H25A 109.5 C24 C25 H25B 109.5 H25A C25 H25B 109.5 C24 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C8 C26 C27 110.0(3) C8 C26 H26A 109.7 C27 C26 H26A 109.7 C8 C26 H26B 109.7 C27 C26 H26B 109.7 H26A C26 H26B 108.2 C26 C27 H27A 109.5 C26 C27 H27B 109.5 H27A C27 H27B 109.5 C26 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C11 C28 H28A 109.5 C11 C28 H28B 109.5 H28A C28 H28B 109.5 C11 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C12 C29 C30 114.4(3) C12 C29 H29A 108.7 C30 C29 H29A 108.7 C12 C29 H29B 108.7 C30 C29 H29B 108.7 H29A C29 H29B 107.6 C29 C30 H30A 109.5 C29 C30 H30B 109.5 H30A C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C13 C31 C32 112.1(3) C13 C31 H31A 109.2 C32 C31 H31A 109.2 C13 C31 H31B 109.2 C32 C31 H31B 109.2 H31A C31 H31B 107.9 C31 C32 H32A 109.5 C31 C32 H32B 109.5 H32A C32 H32B 109.5 C31 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C17 C33 C34 111.9(3) C17 C33 H33A 109.2 C34 C33 H33A 109.2 C17 C33 H33B 109.2 C34 C33 H33B 109.2 H33A C33 H33B 107.9 C33 C34 H34A 109.5 C33 C34 H34B 109.5 H34A C34 H34B 109.5 C33 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 C18 C35 C36 112.7(3) C18 C35 H35A 109.1 C36 C35 H35A 109.1 C18 C35 H35B 109.1 C36 C35 H35B 109.1 H35A C35 H35B 107.8 C35 C36 H36A 109.5 C35 C36 H36B 109.5 H36A C36 H36B 109.5 C35 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 N5 C37 C55 111.5(3) N5 C37 C38 109.1(3) C55 C37 C38 139.3(3) C39 C38 C37 106.2(3) C39 C38 C56 126.9(4) C37 C38 C56 126.9(3) C38 C39 C40 107.8(3) C38 C39 C58 128.6(3) C40 C39 C58 123.6(3) C41 C40 N5 121.4(3) C41 C40 C39 130.9(3) N5 C40 C39 107.7(3) C40 C41 C42 122.5(3) C40 C41 H41 118.8 C42 C41 H41 118.8 N6 C42 C41 124.6(3) N6 C42 C43 112.2(3) C41 C42 C43 123.2(3) C44 C43 C42 107.0(3) C44 C43 C60 129.1(3) C42 C43 C60 123.9(3) C43 C44 C62 127.3(3) C43 C44 C45 108.4(3) C62 C44 C45 123.9(3) N6 C45 C44 104.1(3) N6 C45 C64 108.8(3) C44 C45 C64 106.9(3) N6 C45 C46 110.2(3) C44 C45 C46 117.2(3) C64 C45 C46 109.2(3) C47 C46 C45 108.8(3) C47 C46 C10 114.1(3) C45 C46 C10 113.2(3) C47 C46 H46 106.7 C45 C46 H46 106.7 C10 C46 H46 106.7 N7 C47 C48 110.8(3) N7 C47 C46 121.0(3) C48 C47 C46 128.1(3) C49 C48 C47 106.4(3) C49 C48 C65 127.8(3) C47 C48 C65 125.4(3) C48 C49 C50 107.2(3) C48 C49 C67 128.4(4) C50 C49 C67 124.5(3) C51 C50 N7 123.4(3) C51 C50 C49 128.1(3) N7 C50 C49 108.3(3) C50 C51 C52 124.7(3) C50 C51 H51 117.7 C52 C51 H51 117.7 N8 C52 C51 120.1(3) N8 C52 C53 108.6(3) C51 C52 C53 131.3(4) C54 C53 C52 107.4(3) C54 C53 C69 127.6(4) C52 C53 C69 124.9(4) C53 C54 C55 106.1(3) C53 C54 C71 125.3(4) C55 C54 C71 128.3(4) N8 C55 C37 109.9(3) N8 C55 C54 109.1(3) C37 C55 C54 141.0(4) C38 C56 C57 112.2(3) C38 C56 H56A 109.2 C57 C56 H56A 109.2 C38 C56 H56B 109.2 C57 C56 H56B 109.2 H56A C56 H56B 107.9 C56 C57 H57A 109.5 C56 C57 H57B 109.5 H57A C57 H57B 109.5 C56 C57 H57C 109.5 H57A C57 H57C 109.5 H57B C57 H57C 109.5 C39 C58 C59 111.7(3) C39 C58 H58A 109.3 C59 C58 H58A 109.3 C39 C58 H58B 109.3 C59 C58 H58B 109.3 H58A C58 H58B 107.9 C58 C59 H59A 109.5 C58 C59 H59B 109.5 H59A C59 H59B 109.5 C58 C59 H59C 109.5 H59A C59 H59C 109.5 H59B C59 H59C 109.5 C43 C60 C61 112.2(3) C43 C60 H60A 109.2 C61 C60 H60A 109.2 C43 C60 H60B 109.2 C61 C60 H60B 109.2 H60A C60 H60B 107.9 C60 C61 H61A 109.5 C60 C61 H61B 109.5 H61A C61 H61B 109.5 C60 C61 H61C 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 C44 C62 C63 114.0(3) C44 C62 H62A 108.8 C63 C62 H62A 108.8 C44 C62 H62B 108.8 C63 C62 H62B 108.8 H62A C62 H62B 107.7 C62 C63 H63A 109.5 C62 C63 H63B 109.5 H63A C63 H63B 109.5 C62 C63 H63C 109.5 H63A C63 H63C 109.5 H63B C63 H63C 109.5 C45 C64 H64A 109.5 C45 C64 H64B 109.5 H64A C64 H64B 109.5 C45 C64 H64C 109.5 H64A C64 H64C 109.5 H64B C64 H64C 109.5 C48 C65 C66 111.3(3) C48 C65 H65A 109.4 C66 C65 H65A 109.4 C48 C65 H65B 109.4 C66 C65 H65B 109.4 H65A C65 H65B 108.0 C65 C66 H66A 109.5 C65 C66 H66B 109.5 H66A C66 H66B 109.5 C65 C66 H66C 109.5 H66A C66 H66C 109.5 H66B C66 H66C 109.5 C49 C67 C68 114.4(3) C49 C67 H67A 108.7 C68 C67 H67A 108.7 C49 C67 H67B 108.7 C68 C67 H67B 108.7 H67A C67 H67B 107.6 C67 C68 H68A 109.5 C67 C68 H68B 109.5 H68A C68 H68B 109.5 C67 C68 H68C 109.5 H68A C68 H68C 109.5 H68B C68 H68C 109.5 C70 C69 C53 113.5(4) C70 C69 H69A 108.9 C53 C69 H69A 108.9 C70 C69 H69B 108.9 C53 C69 H69B 108.9 H69A C69 H69B 107.7 C69 C70 H70A 109.5 C69 C70 H70B 109.5 H70A C70 H70B 109.5 C69 C70 H70C 109.5 H70A C70 H70C 109.5 H70B C70 H70C 109.5 C54 C71 C72 110.8(3) C54 C71 H71A 109.5 C72 C71 H71A 109.5 C54 C71 H71B 109.5 C72 C71 H71B 109.5 H71A C71 H71B 108.1 C71 C72 H72A 109.5 C71 C72 H72B 109.5 H72A C72 H72B 109.5 C71 C72 H72C 109.5 H72A C72 H72C 109.5 H72B C72 H72C 109.5 C4 N1 C1 108.7(3) C4 N1 Ni1 132.1(2) C1 N1 Ni1 119.1(2) C9 N2 C6 106.3(3) C9 N2 Ni1 127.8(2) C6 N2 Ni1 125.7(2) C14 N3 C11 107.8(3) C14 N3 Ni1 127.8(2) C11 N3 Ni1 124.3(2) C19 N4 C16 109.4(3) C19 N4 Ni1 118.8(2) C16 N4 Ni1 131.6(2) C37 N5 C40 109.3(3) C37 N5 Ni2 118.9(2) C40 N5 Ni2 131.5(2) C42 N6 C45 107.6(3) C42 N6 Ni2 127.8(2) C45 N6 Ni2 124.5(2) C47 N7 C50 106.6(3) C47 N7 Ni2 127.1(2) C50 N7 Ni2 126.2(2) C52 N8 C55 108.8(3) C52 N8 Ni2 132.6(3) C55 N8 Ni2 118.6(2) N4 Ni1 N1 80.83(13) N4 Ni1 N3 91.55(12) N1 Ni1 N3 171.06(13) N4 Ni1 N2 172.93(12) N1 Ni1 N2 92.40(12) N3 Ni1 N2 95.36(12) N5 Ni2 N8 81.00(13) N5 Ni2 N6 91.47(12) N8 Ni2 N6 171.71(13) N5 Ni2 N7 172.84(12) N8 Ni2 N7 92.02(13) N6 Ni2 N7 95.59(12) F1 B1 F4 110.9(4) F1 B1 F2 110.6(4) F4 B1 F2 110.7(4) F1 B1 F3 108.6(4) F4 B1 F3 108.0(4) F2 B1 F3 108.0(4) F8 B2 F5 110.4(5) F8 B2 F6 113.5(5) F5 B2 F6 107.3(5) F8 B2 F7 108.8(5) F5 B2 F7 111.4(4) F6 B2 F7 105.4(5) Cl3 C73 Cl2 110.6(2) Cl3 C73 Cl1 110.5(2) Cl2 C73 Cl1 110.0(2) Cl3 C73 H73 108.6 Cl2 C73 H73 108.6 Cl1 C73 H73 108.6 Cl6 C74 Cl4 110.9(3) Cl6 C74 Cl5 110.3(3) Cl4 C74 Cl5 111.7(3) Cl6 C74 H74 107.9 Cl4 C74 H74 107.9 Cl5 C74 H74 107.9 Cl12 C76 Cl11 110.4(4) Cl12 C76 Cl10 109.0(3) Cl11 C76 Cl10 109.8(3) Cl12 C76 H76 109.2 Cl11 C76 H76 109.2 Cl10 C76 H76 109.2 Cl15 C76A Cl14 106.6(17) Cl15 C76A Cl13 110.4(17) Cl14 C76A Cl13 110.2(17) Cl15 C76A H76A 109.9 Cl14 C76A H76A 109.9 Cl13 C76A H76A 109.9 Cl7 C75 Cl8 109.8(3) Cl7 C75 Cl9 111.1(3) Cl8 C75 Cl9 108.5(3) Cl7 C75 H75 109.1 Cl8 C75 H75 109.1 Cl9 C75 H75 109.1 Cl16 C75A Cl18 107.1(18) Cl16 C75A Cl17 110.9(17) Cl18 C75A Cl17 112.7(18) Cl16 C75A H75A 108.7 Cl18 C75A H75A 108.7 Cl17 C75A H75A 108.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.369(4) C1 C19 1.425(5) C1 C2 1.440(5) C2 C3 1.384(6) C2 C20 1.511(5) C3 C4 1.430(5) C3 C22 1.499(5) C4 N1 1.355(5) C4 C5 1.410(5) C5 C6 1.372(5) C5 H5 0.9500 C6 N2 1.412(4) C6 C7 1.448(5) C7 C8 1.372(5) C7 C24 1.506(5) C8 C9 1.446(5) C8 C26 1.503(5) C9 N2 1.342(4) C9 C10 1.504(4) C10 C11 1.565(4) C10 C46 1.586(4) C10 H10 1.0000 C11 N3 1.482(4) C11 C12 1.508(4) C11 C28 1.542(5) C12 C13 1.357(5) C12 C29 1.499(4) C13 C14 1.451(5) C13 C31 1.493(5) C14 N3 1.320(4) C14 C15 1.454(5) C15 C16 1.351(5) C15 H15 0.9500 C16 N4 1.368(5) C16 C17 1.478(5) C17 C18 1.362(5) C17 C33 1.492(5) C18 C19 1.462(5) C18 C35 1.502(5) C19 N4 1.356(4) C20 C21 1.525(7) C20 H20A 0.9900 C20 H20B 0.9900 C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 C23 1.507(7) C22 H22A 0.9900 C22 H22B 0.9900 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 C25 1.532(5) C24 H24A 0.9900 C24 H24B 0.9900 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 C27 1.543(5) C26 H26A 0.9900 C26 H26B 0.9900 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 C30 1.534(5) C29 H29A 0.9900 C29 H29B 0.9900 C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C31 C32 1.537(5) C31 H31A 0.9900 C31 H31B 0.9900 C32 H32A 0.9800 C32 H32B 0.9800 C32 H32C 0.9800 C33 C34 1.528(6) C33 H33A 0.9900 C33 H33B 0.9900 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C35 C36 1.528(6) C35 H35A 0.9900 C35 H35B 0.9900 C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C37 N5 1.349(4) C37 C55 1.426(5) C37 C38 1.472(5) C38 C39 1.361(5) C38 C56 1.498(5) C39 C40 1.469(5) C39 C58 1.499(5) C40 C41 1.354(5) C40 N5 1.372(5) C41 C42 1.450(5) C41 H41 0.9500 C42 N6 1.322(4) C42 C43 1.461(4) C43 C44 1.349(5) C43 C60 1.500(5) C44 C62 1.500(4) C44 C45 1.511(4) C45 N6 1.475(4) C45 C64 1.545(5) C45 C46 1.567(4) C46 C47 1.500(4) C46 H46 1.0000 C47 N7 1.341(4) C47 C48 1.452(5) C48 C49 1.362(5) C48 C65 1.503(5) C49 C50 1.456(5) C49 C67 1.508(5) C50 C51 1.375(5) C50 N7 1.408(4) C51 C52 1.411(6) C51 H51 0.9500 C52 N8 1.347(5) C52 C53 1.443(5) C53 C54 1.386(6) C53 C69 1.504(6) C54 C55 1.434(5) C54 C71 1.498(5) C55 N8 1.377(5) C56 C57 1.527(6) C56 H56A 0.9900 C56 H56B 0.9900 C57 H57A 0.9800 C57 H57B 0.9800 C57 H57C 0.9800 C58 C59 1.526(6) C58 H58A 0.9900 C58 H58B 0.9900 C59 H59A 0.9800 C59 H59B 0.9800 C59 H59C 0.9800 C60 C61 1.537(5) C60 H60A 0.9900 C60 H60B 0.9900 C61 H61A 0.9800 C61 H61B 0.9800 C61 H61C 0.9800 C62 C63 1.535(5) C62 H62A 0.9900 C62 H62B 0.9900 C63 H63A 0.9800 C63 H63B 0.9800 C63 H63C 0.9800 C64 H64A 0.9800 C64 H64B 0.9800 C64 H64C 0.9800 C65 C66 1.535(5) C65 H65A 0.9900 C65 H65B 0.9900 C66 H66A 0.9800 C66 H66B 0.9800 C66 H66C 0.9800 C67 C68 1.536(6) C67 H67A 0.9900 C67 H67B 0.9900 C68 H68A 0.9800 C68 H68B 0.9800 C68 H68C 0.9800 C69 C70 1.480(8) C69 H69A 0.9900 C69 H69B 0.9900 C70 H70A 0.9800 C70 H70B 0.9800 C70 H70C 0.9800 C71 C72 1.540(6) C71 H71A 0.9900 C71 H71B 0.9900 C72 H72A 0.9800 C72 H72B 0.9800 C72 H72C 0.9800 N1 Ni1 1.846(3) N2 Ni1 1.873(3) N3 Ni1 1.868(3) N4 Ni1 1.832(3) N5 Ni2 1.840(3) N6 Ni2 1.868(3) N7 Ni2 1.872(3) N8 Ni2 1.842(3) B1 F1 1.376(6) B1 F4 1.380(5) B1 F2 1.389(6) B1 F3 1.390(6) B2 F8 1.346(7) B2 F5 1.368(6) B2 F6 1.373(7) B2 F7 1.382(6) C73 Cl3 1.751(4) C73 Cl2 1.760(4) C73 Cl1 1.792(4) C73 H73 1.0000 C74 Cl6 1.748(5) C74 Cl4 1.754(5) C74 Cl5 1.764(5) C74 H74 1.0000 C76 Cl12 1.725(7) C76 Cl11 1.741(6) C76 Cl10 1.756(6) C76 H76 1.0000 C76A Cl15 1.72(2) C76A Cl14 1.74(2) C76A Cl13 1.76(2) C76A H76A 1.0000 C75 Cl7 1.748(5) C75 Cl8 1.770(5) C75 Cl9 1.777(5) C75 H75 1.0000 C75A Cl16 1.73(2) C75A Cl18 1.77(2) C75A Cl17 1.78(2) C75A H75A 1.0000 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 N1 C1 C2 C3 -1.2(4) C19 C1 C2 C3 -177.7(5) N1 C1 C2 C20 175.6(4) C19 C1 C2 C20 -1.0(8) C1 C2 C3 C4 1.3(4) C20 C2 C3 C4 -175.5(4) C1 C2 C3 C22 177.1(4) C20 C2 C3 C22 0.3(7) C2 C3 C4 N1 -1.0(4) C22 C3 C4 N1 -177.0(4) C2 C3 C4 C5 178.1(4) C22 C3 C4 C5 2.1(7) N1 C4 C5 C6 0.4(6) C3 C4 C5 C6 -178.6(4) C4 C5 C6 N2 -5.8(6) C4 C5 C6 C7 178.2(3) C5 C6 C7 C8 176.7(4) N2 C6 C7 C8 0.2(4) C5 C6 C7 C24 -3.1(6) N2 C6 C7 C24 -179.6(3) C6 C7 C8 C9 -4.2(4) C24 C7 C8 C9 175.6(3) C6 C7 C8 C26 167.2(3) C24 C7 C8 C26 -13.0(6) C7 C8 C9 N2 7.2(4) C26 C8 C9 N2 -164.3(3) C7 C8 C9 C10 -170.3(3) C26 C8 C9 C10 18.2(5) N2 C9 C10 C11 52.8(4) C8 C9 C10 C11 -129.9(3) N2 C9 C10 C46 -75.0(4) C8 C9 C10 C46 102.3(4) C9 C10 C11 N3 -65.6(3) C46 C10 C11 N3 63.2(3) C9 C10 C11 C12 176.1(3) C46 C10 C11 C12 -55.1(4) C9 C10 C11 C28 53.7(3) C46 C10 C11 C28 -177.5(2) N3 C11 C12 C13 7.9(3) C28 C11 C12 C13 -107.0(3) C10 C11 C12 C13 129.8(3) N3 C11 C12 C29 -179.5(3) C28 C11 C12 C29 65.6(4) C10 C11 C12 C29 -57.5(4) C29 C12 C13 C14 -177.8(3) C11 C12 C13 C14 -5.6(4) C29 C12 C13 C31 0.6(6) C11 C12 C13 C31 172.8(3) C12 C13 C14 N3 0.9(4) C31 C13 C14 N3 -177.6(3) C12 C13 C14 C15 -179.8(3) C31 C13 C14 C15 1.7(5) N3 C14 C15 C16 -0.6(5) C13 C14 C15 C16 -179.8(3) C14 C15 C16 N4 -1.4(5) C14 C15 C16 C17 178.9(3) C15 C16 C17 C18 179.6(4) N4 C16 C17 C18 -0.1(4) C15 C16 C17 C33 1.7(6) N4 C16 C17 C33 -178.0(3) C16 C17 C18 C19 -0.4(4) C33 C17 C18 C19 177.4(4) C16 C17 C18 C35 -178.7(4) C33 C17 C18 C35 -1.0(6) N1 C1 C19 N4 -2.4(4) C2 C1 C19 N4 174.2(5) N1 C1 C19 C18 177.3(4) C2 C1 C19 C18 -6.2(9) C17 C18 C19 N4 0.8(4) C35 C18 C19 N4 179.1(3) C17 C18 C19 C1 -178.8(4) C35 C18 C19 C1 -0.5(7) C3 C2 C20 C21 93.1(5) C1 C2 C20 C21 -83.0(5) C2 C3 C22 C23 -98.8(5) C4 C3 C22 C23 76.3(6) C8 C7 C24 C25 108.4(4) C6 C7 C24 C25 -71.8(5) C7 C8 C26 C27 -78.9(4) C9 C8 C26 C27 90.8(4) C13 C12 C29 C30 71.7(5) C11 C12 C29 C30 -99.4(4) C12 C13 C31 C32 -101.3(4) C14 C13 C31 C32 76.9(4) C18 C17 C33 C34 -95.7(5) C16 C17 C33 C34 81.8(5) C17 C18 C35 C36 92.5(5) C19 C18 C35 C36 -85.6(5) N5 C37 C38 C39 0.7(4) C55 C37 C38 C39 -177.9(4) N5 C37 C38 C56 177.6(3) C55 C37 C38 C56 -1.0(7) C37 C38 C39 C40 0.0(4) C56 C38 C39 C40 -176.9(4) C37 C38 C39 C58 176.4(4) C56 C38 C39 C58 -0.6(6) C38 C39 C40 C41 178.4(4) C58 C39 C40 C41 1.9(6) C38 C39 C40 N5 -0.7(4) C58 C39 C40 N5 -177.3(3) N5 C40 C41 C42 -0.3(5) C39 C40 C41 C42 -179.4(3) C40 C41 C42 N6 -1.2(5) C40 C41 C42 C43 178.9(3) N6 C42 C43 C44 0.9(4) C41 C42 C43 C44 -179.2(3) N6 C42 C43 C60 -178.1(3) C41 C42 C43 C60 1.8(5) C42 C43 C44 C62 -178.3(3) C60 C43 C44 C62 0.5(6) C42 C43 C44 C45 -5.5(4) C60 C43 C44 C45 173.4(3) C43 C44 C45 N6 7.9(3) C62 C44 C45 N6 -179.0(3) C43 C44 C45 C64 -107.2(3) C62 C44 C45 C64 65.9(4) C43 C44 C45 C46 129.9(3) C62 C44 C45 C46 -57.0(4) N6 C45 C46 C47 -65.7(3) C44 C45 C46 C47 175.4(3) C64 C45 C46 C47 53.7(3) N6 C45 C46 C10 62.2(3) C44 C45 C46 C10 -56.6(4) C64 C45 C46 C10 -178.3(2) C9 C10 C46 C47 40.5(4) C11 C10 C46 C47 -85.1(3) C9 C10 C46 C45 -84.7(3) C11 C10 C46 C45 149.7(3) C45 C46 C47 N7 54.0(4) C10 C46 C47 N7 -73.5(4) C45 C46 C47 C48 -129.9(3) C10 C46 C47 C48 102.6(4) N7 C47 C48 C49 7.9(4) C46 C47 C48 C49 -168.5(3) N7 C47 C48 C65 -165.5(3) C46 C47 C48 C65 18.1(5) C47 C48 C49 C50 -4.4(4) C65 C48 C49 C50 168.8(3) C47 C48 C49 C67 175.2(4) C65 C48 C49 C67 -11.6(6) C48 C49 C50 C51 175.0(4) C67 C49 C50 C51 -4.6(6) C48 C49 C50 N7 -0.1(4) C67 C49 C50 N7 -179.7(3) N7 C50 C51 C52 -5.8(6) C49 C50 C51 C52 179.7(4) C50 C51 C52 N8 -1.0(6) C50 C51 C52 C53 -179.6(4) N8 C52 C53 C54 -1.7(5) C51 C52 C53 C54 177.1(4) N8 C52 C53 C69 179.5(4) C51 C52 C53 C69 -1.8(7) C52 C53 C54 C55 1.4(4) C69 C53 C54 C55 -179.7(4) C52 C53 C54 C71 -172.5(4) C69 C53 C54 C71 6.3(7) N5 C37 C55 N8 -3.0(4) C38 C37 C55 N8 175.5(4) N5 C37 C55 C54 176.6(5) C38 C37 C55 C54 -4.9(9) C53 C54 C55 N8 -0.8(4) C71 C54 C55 N8 172.9(4) C53 C54 C55 C37 179.7(5) C71 C54 C55 C37 -6.7(8) C39 C38 C56 C57 93.1(5) C37 C38 C56 C57 -83.2(5) C38 C39 C58 C59 -95.0(5) C40 C39 C58 C59 80.8(5) C44 C43 C60 C61 -101.2(4) C42 C43 C60 C61 77.5(4) C43 C44 C62 C63 74.0(5) C45 C44 C62 C63 -97.8(4) C49 C48 C65 C66 -84.2(4) C47 C48 C65 C66 87.8(4) C48 C49 C67 C68 106.3(5) C50 C49 C67 C68 -74.1(5) C54 C53 C69 C70 -91.6(7) C52 C53 C69 C70 87.1(6) C53 C54 C71 C72 94.6(5) C55 C54 C71 C72 -78.0(6) C5 C4 N1 C1 -179.0(3) C3 C4 N1 C1 0.3(4) C5 C4 N1 Ni1 -2.0(5) C3 C4 N1 Ni1 177.2(3) C19 C1 N1 C4 178.3(3) C2 C1 N1 C4 0.6(4) C19 C1 N1 Ni1 0.9(4) C2 C1 N1 Ni1 -176.9(2) C8 C9 N2 C6 -7.0(4) C10 C9 N2 C6 170.7(3) C8 C9 N2 Ni1 168.2(2) C10 C9 N2 Ni1 -14.1(4) C5 C6 N2 C9 -172.4(3) C7 C6 N2 C9 4.3(4) C5 C6 N2 Ni1 12.2(5) C7 C6 N2 Ni1 -171.2(2) C13 C14 N3 C11 4.2(4) C15 C14 N3 C11 -175.0(3) C13 C14 N3 Ni1 -173.1(2) C15 C14 N3 Ni1 7.7(5) C12 C11 N3 C14 -7.2(3) C28 C11 N3 C14 107.0(3) C10 C11 N3 C14 -133.4(3) C12 C11 N3 Ni1 170.2(2) C28 C11 N3 Ni1 -75.6(3) C10 C11 N3 Ni1 44.0(3) C1 C19 N4 C16 178.9(3) C18 C19 N4 C16 -0.9(4) C1 C19 N4 Ni1 3.1(4) C18 C19 N4 Ni1 -176.7(2) C15 C16 N4 C19 -179.2(3) C17 C16 N4 C19 0.6(4) C15 C16 N4 Ni1 -4.0(5) C17 C16 N4 Ni1 175.7(3) C55 C37 N5 C40 177.8(3) C38 C37 N5 C40 -1.2(4) C55 C37 N5 Ni2 3.9(4) C38 C37 N5 Ni2 -175.1(2) C41 C40 N5 C37 -178.1(3) C39 C40 N5 C37 1.2(4) C41 C40 N5 Ni2 -5.2(5) C39 C40 N5 Ni2 174.1(2) C41 C42 N6 C45 -175.7(3) C43 C42 N6 C45 4.2(4) C41 C42 N6 Ni2 7.8(5) C43 C42 N6 Ni2 -172.3(2) C44 C45 N6 C42 -7.2(3) C64 C45 N6 C42 106.5(3) C46 C45 N6 C42 -133.8(3) C44 C45 N6 Ni2 169.5(2) C64 C45 N6 Ni2 -76.8(3) C46 C45 N6 Ni2 42.9(3) C48 C47 N7 C50 -7.9(4) C46 C47 N7 C50 168.9(3) C48 C47 N7 Ni2 168.7(2) C46 C47 N7 Ni2 -14.6(4) C51 C50 N7 C47 -170.5(3) C49 C50 N7 C47 5.0(4) C51 C50 N7 Ni2 12.9(5) C49 C50 N7 Ni2 -171.6(2) C51 C52 N8 C55 -177.7(3) C53 C52 N8 C55 1.2(4) C51 C52 N8 Ni2 0.3(6) C53 C52 N8 Ni2 179.2(3) C37 C55 N8 C52 179.4(3) C54 C55 N8 C52 -0.3(4) C37 C55 N8 Ni2 1.1(4) C54 C55 N8 Ni2 -178.6(2) C19 N4 Ni1 N1 -2.1(3) C16 N4 Ni1 N1 -176.8(3) C19 N4 Ni1 N3 -177.4(3) C16 N4 Ni1 N3 7.9(3) C4 N1 Ni1 N4 -176.2(4) C1 N1 Ni1 N4 0.6(3) C4 N1 Ni1 N2 5.9(3) C1 N1 Ni1 N2 -177.4(3) C14 N3 Ni1 N4 -9.4(3) C11 N3 Ni1 N4 173.7(3) C14 N3 Ni1 N2 169.1(3) C11 N3 Ni1 N2 -7.8(3) C9 N2 Ni1 N1 175.2(3) C6 N2 Ni1 N1 -10.4(3) C9 N2 Ni1 N3 -9.2(3) C6 N2 Ni1 N3 165.2(3) C37 N5 Ni2 N8 -2.7(3) C40 N5 Ni2 N8 -175.0(3) C37 N5 Ni2 N6 -179.2(3) C40 N5 Ni2 N6 8.5(3) C52 N8 Ni2 N5 -177.1(4) C55 N8 Ni2 N5 0.7(3) C52 N8 Ni2 N7 4.5(4) C55 N8 Ni2 N7 -177.7(3) C42 N6 Ni2 N5 -9.5(3) C45 N6 Ni2 N5 174.5(3) C42 N6 Ni2 N7 169.3(3) C45 N6 Ni2 N7 -6.7(3) C47 N7 Ni2 N8 173.5(3) C50 N7 Ni2 N8 -10.5(3) C47 N7 Ni2 N6 -9.8(3) C50 N7 Ni2 N6 166.2(3)