#------------------------------------------------------------------------------ #$Date: 2020-05-13 03:55:50 +0300 (Wed, 13 May 2020) $ #$Revision: 252003 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/65/7126529.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_7126529 loop_ _publ_author_name 'Liu, Si-Yu' 'Kawashima, Hiroyuki' 'Fukui, Norihito' 'Shinokubo, Hiroshi' _publ_section_title ; A 2-to-2' 18-to-18' doubly linked Ni(II) norcorrole dimer: An effectively conjugated antiaromatic dyad ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D0CC02543G _journal_year 2020 _chemical_formula_moiety 'C72 H58 N8 Ni2, 2(C2 H4 Cl2)' _chemical_formula_sum 'C76 H66 Cl4 N8 Ni2' _chemical_formula_weight 1350.58 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-03-21 deposited with the CCDC. 2020-05-12 downloaded from the CCDC. ; _cell_angle_alpha 72.164(4) _cell_angle_beta 77.709(3) _cell_angle_gamma 86.387(3) _cell_formula_units_Z 2 _cell_length_a 12.0197(3) _cell_length_b 15.4760(7) _cell_length_c 18.5471(7) _cell_measurement_reflns_used 5651 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 28.0050 _cell_measurement_theta_min 2.2850 _cell_volume 3209.0(2) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.957 _diffrn_measured_fraction_theta_max 0.750 _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_unetI/netI 0.0759 _diffrn_reflns_Laue_measured_fraction_full 0.957 _diffrn_reflns_Laue_measured_fraction_max 0.750 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 24753 _diffrn_reflns_point_group_measured_fraction_full 0.957 _diffrn_reflns_point_group_measured_fraction_max 0.750 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.736 _diffrn_reflns_theta_min 1.887 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.93239 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.398 _exptl_crystal_description prism _exptl_crystal_F_000 1404 _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.070 _refine_diff_density_max 1.264 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 846 _refine_ls_number_reflns 12476 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_gt 0.0638 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+6.7417P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1392 _refine_ls_wR_factor_ref 0.1612 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8509 _reflns_number_total 12476 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc02543g2.cif _cod_data_source_block 151030HK_a _cod_database_code 7126529 _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_res_file ; TITL 151030HK_a.res in P-1 151030HK_a.res created by SHELXL-2018/3 at 12:46:31 on 09-Mar-2020 REM Yadorkari-X generated CELL 0.71073 12.0197 15.4760 18.5471 72.1640 77.7090 86.3870 ZERR 2.0 0.0003 0.0007 0.0007 0.0040 0.0030 0.0030 LATT 1 REM SPGR P-1 triclinic SFAC C H N Ni Cl UNIT 152 132 16 4 8 L.S. 10 FMAP 2 PLAN -20 ACTA CONF LIST 4 MERG 2 OMIT -10.000000 60.000000 OMIT -1 1 1 DFIX 1.76 0.03 C75 Cl3 WGHT 0.064000 6.741700 FVAR 0.30267 0.46758 NI1 4 0.543627 -0.168179 0.401991 11.00000 0.01500 0.02055 = 0.03192 -0.01262 0.00358 -0.00375 NI2 4 0.778698 0.442451 0.202645 11.00000 0.01466 0.02044 = 0.03586 -0.00632 -0.00107 -0.00255 N1 3 0.756083 0.323925 0.252289 11.00000 0.01189 0.02217 = 0.03332 -0.00788 -0.00179 0.00027 N2 3 0.576839 -0.052706 0.391892 11.00000 0.01753 0.01960 = 0.02929 -0.01100 0.00518 -0.00375 N3 3 0.404570 -0.144717 0.449531 11.00000 0.01283 0.02519 = 0.02931 -0.01328 0.00347 -0.00257 N4 3 0.504725 -0.278266 0.400940 11.00000 0.01808 0.02059 = 0.03594 -0.01538 0.00316 -0.00297 N5 3 0.800888 0.559999 0.152095 11.00000 0.01858 0.02364 = 0.03440 -0.00637 -0.00319 -0.00021 N6 3 0.634054 0.466131 0.198632 11.00000 0.01768 0.02203 = 0.03649 -0.00421 -0.00110 -0.00068 N7 3 0.924704 0.419287 0.205437 11.00000 0.01783 0.02389 = 0.03266 -0.00978 0.00041 -0.00361 N8 3 0.676909 -0.188428 0.346131 11.00000 0.01484 0.02507 = 0.02968 -0.01190 0.00522 -0.00180 C1 1 0.669179 0.002233 0.348633 11.00000 0.01602 0.02148 = 0.02593 -0.00922 -0.00073 -0.00414 C2 1 0.658460 0.272035 0.281045 11.00000 0.01959 0.02459 = 0.02722 -0.00991 -0.00065 -0.00294 C3 1 0.399840 -0.319696 0.422251 11.00000 0.01883 0.02331 = 0.03605 -0.01396 0.00051 -0.00808 C4 1 0.698067 0.179475 0.316867 11.00000 0.01896 0.01972 = 0.02428 -0.00911 -0.00058 -0.00286 C5 1 0.815707 0.184652 0.308684 11.00000 0.01691 0.01865 = 0.02897 -0.00837 -0.00383 -0.00034 AFIX 43 H1 2 0.863440 0.136975 0.326980 11.00000 -1.20000 AFIX 0 C6 1 1.111740 0.624836 0.100877 11.00000 0.01812 0.02151 = 0.03039 -0.00971 0.00167 -0.00254 C7 1 0.541495 0.410342 0.230905 11.00000 0.01483 0.02666 = 0.03066 -0.00895 -0.00030 -0.00205 C8 1 1.006382 0.567490 0.133059 11.00000 0.02024 0.03216 = 0.02729 -0.01689 0.00170 -0.00723 C9 1 0.223659 0.193910 0.375646 11.00000 0.01635 0.02441 = 0.03046 -0.00251 -0.00334 -0.00018 C10 1 0.489487 -0.004032 0.417095 11.00000 0.01918 0.02614 = 0.02497 -0.01362 -0.00143 -0.00102 C11 1 0.216733 -0.132462 0.490218 11.00000 0.01794 0.02569 = 0.02822 -0.01171 0.00349 -0.00390 AFIX 43 H2 2 0.139654 -0.146352 0.508006 11.00000 -1.20000 AFIX 0 C12 1 0.551979 0.316838 0.271428 11.00000 0.01656 0.02758 = 0.02490 -0.01200 -0.00189 0.00005 C13 1 1.307930 0.732581 0.043725 11.00000 0.01690 0.02240 = 0.04103 -0.00730 -0.00149 -0.00055 C14 1 0.444843 0.467995 0.215107 11.00000 0.01775 0.03433 = 0.03017 -0.01145 -0.00381 0.00085 AFIX 43 H3 2 0.369037 0.449636 0.229358 11.00000 -1.20000 AFIX 0 C15 1 0.439342 0.270752 0.308029 11.00000 0.01638 0.02112 = 0.02852 -0.00720 -0.00334 0.00126 C16 1 0.484449 0.555530 0.175000 11.00000 0.02245 0.02854 = 0.03681 -0.01027 -0.00431 0.00292 AFIX 43 H4 2 0.440395 0.606215 0.157637 11.00000 -1.20000 AFIX 0 C17 1 0.953756 0.333005 0.236722 11.00000 0.01922 0.02247 = 0.02955 -0.00734 -0.00341 -0.00401 C18 1 0.380866 0.283863 0.377224 11.00000 0.01832 0.02141 = 0.03359 -0.00991 -0.00536 0.00508 C19 1 0.266246 -0.050162 0.479148 11.00000 0.01876 0.02283 = 0.02613 -0.00993 0.00163 -0.00005 AFIX 43 H5 2 0.229103 0.001436 0.487724 11.00000 -1.20000 AFIX 0 C20 1 0.304247 -0.192860 0.469652 11.00000 0.01876 0.02706 = 0.02610 -0.00800 0.00175 -0.00580 C21 1 0.633764 0.094650 0.351716 11.00000 0.01791 0.02498 = 0.02390 -0.00871 -0.00398 -0.00305 C22 1 0.849425 0.275160 0.267679 11.00000 0.01701 0.02435 = 0.02491 -0.00930 -0.00033 -0.00220 C23 1 0.522548 0.086612 0.395383 11.00000 0.01865 0.02115 = 0.02276 -0.00890 -0.00213 -0.00075 AFIX 43 H6 2 0.478342 0.133567 0.407778 11.00000 -1.20000 AFIX 0 C24 1 0.863346 0.073951 0.183829 11.00000 0.02191 0.02552 = 0.02992 -0.01278 -0.00298 -0.00394 C25 1 0.605110 0.553073 0.165474 11.00000 0.02332 0.02509 = 0.03253 -0.00777 -0.00363 0.00145 C26 1 0.761095 -0.036386 0.307224 11.00000 0.01765 0.02349 = 0.02510 -0.00706 -0.00257 -0.00157 C27 1 0.688052 -0.265859 0.325319 11.00000 0.01980 0.02103 = 0.03172 -0.01338 0.00085 0.00157 C28 1 0.392223 0.218379 0.272352 11.00000 0.02031 0.02646 = 0.02720 -0.00749 -0.00428 -0.00042 C29 1 0.273894 0.243895 0.410469 11.00000 0.01899 0.02589 = 0.02904 -0.00727 0.00175 0.00245 AFIX 43 H15 2 0.235287 0.251068 0.457362 11.00000 -1.20000 AFIX 0 C30 1 0.709754 0.610670 0.134823 11.00000 0.02449 0.02425 = 0.03200 -0.00958 -0.00097 -0.00085 C31 1 1.113997 0.416411 0.185211 11.00000 0.01782 0.03176 = 0.03232 -0.00725 -0.00197 -0.00753 AFIX 43 H7 2 1.190060 0.434101 0.169683 11.00000 -1.20000 AFIX 0 C32 1 0.581442 -0.319893 0.359008 11.00000 0.02366 0.02694 = 0.03060 -0.01351 -0.00019 0.00069 C33 1 0.414629 -0.395931 0.392750 11.00000 0.02353 0.02627 = 0.04381 -0.01776 0.00380 -0.00847 AFIX 43 H8 2 0.358884 -0.437981 0.398608 11.00000 -1.20000 AFIX 0 C34 1 0.384087 -0.059264 0.452309 11.00000 0.01883 0.02019 = 0.02399 -0.00892 -0.00140 -0.00260 C35 1 0.864571 0.016189 0.258043 11.00000 0.01796 0.02359 = 0.02565 -0.01222 0.00349 -0.00300 C36 1 0.302348 -0.278780 0.457007 11.00000 0.01935 0.02804 = 0.02838 -0.01166 0.00013 -0.00301 C37 1 1.063020 0.047987 0.240135 11.00000 0.01812 0.03998 = 0.03214 -0.01623 -0.00117 -0.00567 AFIX 43 H16 2 1.130261 0.038174 0.258647 11.00000 -1.20000 AFIX 0 C38 1 0.285130 0.180281 0.307521 11.00000 0.01889 0.03000 = 0.03426 -0.01111 -0.00923 -0.00056 AFIX 43 H17 2 0.253613 0.144552 0.284762 11.00000 -1.20000 AFIX 0 C39 1 0.764012 -0.128992 0.304776 11.00000 0.01529 0.02895 = 0.03073 -0.01106 -0.00054 -0.00154 C40 1 1.256354 0.709597 0.121251 11.00000 0.02307 0.02810 = 0.04287 -0.01740 -0.00764 0.00061 AFIX 43 H18 2 1.287402 0.731474 0.154124 11.00000 -1.20000 AFIX 0 C41 1 1.074096 0.329355 0.224962 11.00000 0.01821 0.02827 = 0.03570 -0.00825 -0.00377 -0.00106 AFIX 43 H9 2 1.117965 0.278102 0.240953 11.00000 -1.20000 AFIX 0 C42 1 0.188765 -0.322663 0.476783 11.00000 0.01994 0.02424 = 0.03736 -0.01851 0.00656 -0.00397 C43 1 0.965313 0.003551 0.287206 11.00000 0.01860 0.02465 = 0.03119 -0.01334 0.00121 -0.00462 C44 1 0.899950 0.609485 0.123053 11.00000 0.02435 0.02525 = 0.02948 -0.01182 0.00237 -0.00467 C45 1 1.159914 0.655052 0.151780 11.00000 0.02029 0.02807 = 0.03144 -0.01248 -0.00001 -0.00307 C46 1 1.161928 0.646868 0.022630 11.00000 0.02686 0.02392 = 0.02985 -0.00901 0.00089 -0.00382 C47 1 1.018451 0.474644 0.172022 11.00000 0.01414 0.02851 = 0.02917 -0.01064 0.00019 -0.00163 C48 1 0.103736 0.159146 0.409088 11.00000 0.01957 0.03598 = 0.03877 -0.00505 -0.00150 -0.00467 AFIX 137 H19 2 0.089998 0.143386 0.464481 11.00000 -1.50000 H20 2 0.093543 0.106436 0.394205 11.00000 -1.50000 H21 2 0.051165 0.205440 0.389913 11.00000 -1.50000 AFIX 0 C49 1 0.156503 -0.389443 0.548826 11.00000 0.02722 0.03308 = 0.03974 -0.02096 0.00856 -0.00728 C50 1 0.113555 -0.294295 0.425664 11.00000 0.02342 0.02795 = 0.05105 -0.02557 -0.00289 0.00180 C51 1 1.259716 0.699320 -0.004631 11.00000 0.02655 0.02887 = 0.02842 -0.00619 0.00239 -0.00355 AFIX 43 H22 2 1.294334 0.712811 -0.056674 11.00000 -1.20000 AFIX 0 C52 1 0.433019 0.337001 0.417974 11.00000 0.02462 0.02886 = 0.03626 -0.01580 0.00051 0.00076 AFIX 137 H23 2 0.440498 0.399572 0.387253 11.00000 -1.50000 H24 2 0.506778 0.312750 0.425064 11.00000 -1.50000 H25 2 0.384881 0.332407 0.467469 11.00000 -1.50000 AFIX 0 C53 1 0.838015 -0.174487 0.257470 11.00000 0.02052 0.03053 = 0.02841 -0.01290 0.00400 -0.00034 AFIX 43 H10 2 0.906033 -0.151829 0.223883 11.00000 -1.20000 AFIX 0 C54 1 0.963327 0.119081 0.139272 11.00000 0.03257 0.03121 = 0.02207 -0.00814 0.00104 -0.00840 AFIX 43 H26 2 0.962395 0.158529 0.090178 11.00000 -1.20000 AFIX 0 C55 1 0.964654 -0.052399 0.369412 11.00000 0.02308 0.03297 = 0.03366 -0.01010 -0.00316 -0.00245 AFIX 137 H27 2 1.039629 -0.052841 0.379798 11.00000 -1.50000 H28 2 0.941881 -0.113416 0.376949 11.00000 -1.50000 H29 2 0.912032 -0.026655 0.403967 11.00000 -1.50000 AFIX 0 C56 1 0.749242 0.700242 0.091621 11.00000 0.02888 0.02476 = 0.03476 -0.00655 -0.00290 0.00270 AFIX 43 H11 2 0.705019 0.749761 0.071729 11.00000 -1.20000 AFIX 0 C57 1 0.865984 0.699289 0.084999 11.00000 0.03116 0.02568 = 0.03023 -0.00991 0.00211 -0.00779 AFIX 43 H12 2 0.914425 0.748800 0.059965 11.00000 -1.20000 AFIX 0 C58 1 0.526341 -0.395961 0.354052 11.00000 0.02942 0.02582 = 0.04623 -0.02151 0.00144 -0.00270 AFIX 43 H13 2 0.559454 -0.437997 0.329300 11.00000 -1.20000 AFIX 0 C59 1 1.064744 0.106658 0.166353 11.00000 0.02606 0.04173 = 0.03194 -0.01692 0.00625 -0.01464 C60 1 0.456187 0.201594 0.198999 11.00000 0.02497 0.04546 = 0.03549 -0.01862 -0.00020 -0.00531 AFIX 137 H30 2 0.487553 0.257746 0.163015 11.00000 -1.50000 H31 2 0.405233 0.177015 0.176815 11.00000 -1.50000 H32 2 0.516663 0.159292 0.210277 11.00000 -1.50000 AFIX 0 C61 1 0.790182 -0.259420 0.270504 11.00000 0.02113 0.02946 = 0.03516 -0.01685 0.00305 0.00201 AFIX 43 H14 2 0.820405 -0.303426 0.247200 11.00000 -1.20000 AFIX 0 C62 1 0.756739 0.089281 0.151937 11.00000 0.02799 0.03990 = 0.03197 -0.00784 -0.00397 -0.00611 AFIX 137 H33 2 0.708656 0.131309 0.172985 11.00000 -1.50000 H34 2 0.717223 0.032678 0.165785 11.00000 -1.50000 H35 2 0.776059 0.113674 0.096614 11.00000 -1.50000 AFIX 0 C63 1 -0.029847 -0.395992 0.519984 11.00000 0.02036 0.03279 = 0.06931 -0.03326 0.00900 0.00073 C64 1 1.413980 0.791093 0.012417 11.00000 0.02475 0.03689 = 0.05223 -0.00464 -0.00180 -0.01187 AFIX 137 H36 2 1.410209 0.835480 0.039407 11.00000 -1.50000 H37 2 1.419124 0.821277 -0.041768 11.00000 -1.50000 H38 2 1.479880 0.753639 0.019750 11.00000 -1.50000 AFIX 0 C65 1 0.004346 -0.332692 0.448618 11.00000 0.02437 0.03368 = 0.06200 -0.02814 -0.00441 0.00292 AFIX 43 H39 2 -0.046135 -0.315178 0.415093 11.00000 -1.20000 AFIX 0 C66 1 1.113567 0.611932 -0.032530 11.00000 0.04109 0.04727 = 0.03050 -0.01481 0.00091 -0.01573 AFIX 137 H40 2 1.157954 0.635243 -0.083965 11.00000 -1.50000 H41 2 1.036114 0.631674 -0.031818 11.00000 -1.50000 H42 2 1.116076 0.546807 -0.016657 11.00000 -1.50000 AFIX 0 C67 1 0.045958 -0.423776 0.569179 11.00000 0.03194 0.03369 = 0.04867 -0.02042 0.01359 -0.00883 AFIX 43 H43 2 0.022551 -0.466534 0.617151 11.00000 -1.20000 AFIX 0 C68 1 0.151040 -0.226369 0.347462 11.00000 0.03679 0.03719 = 0.04883 -0.01992 -0.01339 0.00346 AFIX 137 H44 2 0.089406 -0.214684 0.320297 11.00000 -1.50000 H45 2 0.214751 -0.250146 0.318456 11.00000 -1.50000 H46 2 0.172906 -0.170892 0.353686 11.00000 -1.50000 AFIX 0 C69 1 0.239667 -0.423606 0.600800 11.00000 0.04410 0.04760 = 0.03554 -0.00734 0.00296 -0.01658 AFIX 137 H47 2 0.300606 -0.454657 0.576300 11.00000 -1.50000 H48 2 0.201810 -0.464731 0.648799 11.00000 -1.50000 H49 2 0.269935 -0.373347 0.610642 11.00000 -1.50000 AFIX 0 C70 1 -0.148949 -0.437501 0.545273 11.00000 0.02257 0.03990 = 0.10808 -0.04285 0.01376 -0.00971 AFIX 137 H50 2 -0.143179 -0.502259 0.556663 11.00000 -1.50000 H51 2 -0.190188 -0.413737 0.504409 11.00000 -1.50000 H52 2 -0.188426 -0.422628 0.590659 11.00000 -1.50000 AFIX 0 C71 1 1.172831 0.154094 0.115977 11.00000 0.03141 0.06997 = 0.03560 -0.01113 0.00480 -0.02460 AFIX 137 H53 2 1.204766 0.122991 0.078808 11.00000 -1.50000 H54 2 1.226544 0.153806 0.147657 11.00000 -1.50000 H55 2 1.155858 0.215624 0.089460 11.00000 -1.50000 AFIX 0 C72 1 1.108397 0.629768 0.237278 11.00000 0.04250 0.05896 = 0.03993 -0.02580 0.00015 -0.01869 AFIX 137 H56 2 1.042190 0.666286 0.245705 11.00000 -1.50000 H57 2 1.163177 0.640135 0.264613 11.00000 -1.50000 H58 2 1.087096 0.566818 0.255832 11.00000 -1.50000 AFIX 0 CL2 5 0.367317 0.399784 0.038939 11.00000 0.07094 0.08063 = 0.04910 -0.02498 0.00388 -0.01242 CL3 5 0.088901 0.890298 0.065534 11.00000 0.10536 0.07327 = 0.05995 -0.02490 -0.02398 0.04409 C73 1 0.440222 0.509351 -0.001169 11.00000 0.07647 0.07590 = 0.05519 -0.03302 -0.01815 0.03224 AFIX 23 H59 2 0.431096 0.537905 -0.053971 11.00000 -1.20000 H60 2 0.409546 0.549462 0.029416 11.00000 -1.20000 AFIX 0 C75 1 0.051641 1.017947 -0.013199 11.00000 0.12049 0.16200 = 0.15659 -0.13636 0.07917 -0.08481 AFIX 23 H61 2 0.063306 1.071286 0.001345 11.00000 -1.20000 H62 2 0.082696 1.025379 -0.067489 11.00000 -1.20000 AFIX 0 CL4 5 0.599088 0.935444 0.077829 11.00000 0.08895 0.05054 = 0.06987 -0.01217 -0.03204 -0.01005 C76 1 0.556613 0.866062 0.176454 11.00000 0.05241 0.05192 = 0.06636 -0.00964 -0.02002 0.00445 PART 1 AFIX 23 H63 2 0.578618 0.804342 0.177600 21.00000 0.43043 H64 2 0.603030 0.884609 0.206008 21.00000 0.03705 PART 2 AFIX 23 H65 2 0.524023 0.809375 0.178519 -21.00000 0.03472 H66 2 0.621747 0.852432 0.201198 -21.00000 0.08555 PART 1 AFIX 0 C77 1 0.435494 0.861844 0.220777 21.00000 0.05169 0.05308 = 0.06394 -0.01376 -0.02515 -0.00337 AFIX 23 H67 2 0.426646 0.811687 0.268248 21.00000 -1.20000 H68 2 0.384265 0.852038 0.190058 21.00000 -1.20000 AFIX 0 CL6 5 0.400876 0.967782 0.243135 21.00000 0.08914 0.06029 = 0.07857 -0.03482 -0.03076 0.02004 PART 2 C78 1 0.472177 0.917655 0.215380 -21.00000 0.07548 0.07662 = 0.06949 -0.02902 -0.02871 0.01583 AFIX 23 H69 2 0.505225 0.975426 0.210059 -21.00000 -1.20000 H70 2 0.453406 0.884758 0.270110 -21.00000 -1.20000 AFIX 0 CL5 5 0.343987 0.938227 0.178223 -21.00000 0.04305 0.09366 = 0.07262 -0.00642 -0.01285 0.01122 PART 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 151030HK_a.res in P-1 REM wR2 = 0.1612, GooF = S = 1.029, Restrained GooF = 1.036 for all data REM R1 = 0.0638 for 8509 Fo > 4sig(Fo) and 0.1075 for all 12476 data REM 846 parameters refined using 1 restraints END WGHT 0.0639 6.7608 REM Highest difference peak 1.264, deepest hole -1.142, 1-sigma level 0.087 Q1 1 0.4785 0.7788 0.2082 11.00000 0.05 1.26 Q2 1 -0.0207 0.9479 0.0415 11.00000 0.05 0.63 Q3 1 0.6450 0.9613 -0.0150 11.00000 0.05 0.63 Q4 1 0.6618 0.9595 -0.0031 11.00000 0.05 0.61 Q5 1 0.9512 -0.1416 0.1885 11.00000 0.05 0.59 Q6 1 0.1612 0.9360 0.0414 11.00000 0.05 0.58 Q7 1 0.3122 0.9738 0.2275 11.00000 0.05 0.56 Q8 1 0.7689 0.4968 0.2126 11.00000 0.05 0.46 Q9 1 0.4970 0.4392 0.0195 11.00000 0.05 0.38 Q10 1 0.1430 0.8994 0.1513 11.00000 0.05 0.38 Q11 1 0.4769 0.8230 0.1542 11.00000 0.05 0.38 Q12 1 0.5739 -0.0832 0.3421 11.00000 0.05 0.36 Q13 1 1.0572 0.5881 0.1155 11.00000 0.05 0.36 Q14 1 0.3081 0.4648 0.2540 11.00000 0.05 0.35 Q15 1 0.9009 0.4480 0.2343 11.00000 0.05 0.35 Q16 1 0.3569 0.9867 0.0830 11.00000 0.05 0.34 Q17 1 0.1252 0.9410 0.0869 11.00000 0.05 0.34 Q18 1 1.2409 0.4339 0.1489 11.00000 0.05 0.33 Q19 1 0.2654 0.9591 0.0894 11.00000 0.05 0.32 Q20 1 1.1826 0.2063 0.1294 11.00000 0.05 0.31 ; _shelx_res_checksum 47517 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.54363(4) -0.16818(3) 0.40199(3) 0.02253(15) Uani 1 1 d . . . . . Ni2 Ni 0.77870(4) 0.44245(3) 0.20264(3) 0.02466(15) Uani 1 1 d . . . . . N1 N 0.7561(3) 0.3239(2) 0.25229(19) 0.0230(8) Uani 1 1 d . . . . . N2 N 0.5768(3) -0.0527(2) 0.39189(19) 0.0227(8) Uani 1 1 d . . . . . N3 N 0.4046(3) -0.1447(2) 0.44953(19) 0.0224(7) Uani 1 1 d . . . . . N4 N 0.5047(3) -0.2783(2) 0.4009(2) 0.0245(8) Uani 1 1 d . . . . . N5 N 0.8009(3) 0.5600(2) 0.1521(2) 0.0264(8) Uani 1 1 d . . . . . N6 N 0.6341(3) 0.4661(2) 0.1986(2) 0.0271(8) Uani 1 1 d . . . . . N7 N 0.9247(3) 0.4193(2) 0.2054(2) 0.0252(8) Uani 1 1 d . . . . . N8 N 0.6769(3) -0.1884(2) 0.34613(19) 0.0238(8) Uani 1 1 d . . . . . C1 C 0.6692(3) 0.0022(3) 0.3486(2) 0.0210(9) Uani 1 1 d . . . . . C2 C 0.6585(3) 0.2720(3) 0.2810(2) 0.0238(9) Uani 1 1 d . . . . . C3 C 0.3998(3) -0.3197(3) 0.4223(2) 0.0255(9) Uani 1 1 d . . . . . C4 C 0.6981(3) 0.1795(3) 0.3169(2) 0.0209(9) Uani 1 1 d . . . . . C5 C 0.8157(3) 0.1847(3) 0.3087(2) 0.0213(9) Uani 1 1 d . . . . . H1 H 0.863440 0.136975 0.326980 0.026 Uiso 1 1 calc R U . . . C6 C 1.1117(3) 0.6248(3) 0.1009(2) 0.0238(9) Uani 1 1 d . . . . . C7 C 0.5415(3) 0.4103(3) 0.2309(2) 0.0246(9) Uani 1 1 d . . . . . C8 C 1.0064(3) 0.5675(3) 0.1331(2) 0.0254(9) Uani 1 1 d . . . . . C9 C 0.2237(3) 0.1939(3) 0.3756(2) 0.0253(9) Uani 1 1 d . . . . . C10 C 0.4895(3) -0.0040(3) 0.4171(2) 0.0225(9) Uani 1 1 d . . . . . C11 C 0.2167(3) -0.1325(3) 0.4902(2) 0.0242(9) Uani 1 1 d . . . . . H2 H 0.139654 -0.146352 0.508006 0.029 Uiso 1 1 calc R U . . . C12 C 0.5520(3) 0.3168(3) 0.2714(2) 0.0224(9) Uani 1 1 d . . . . . C13 C 1.3079(3) 0.7326(3) 0.0437(3) 0.0280(10) Uani 1 1 d . . . . . C14 C 0.4448(4) 0.4680(3) 0.2151(2) 0.0272(10) Uani 1 1 d . . . . . H3 H 0.369037 0.449636 0.229358 0.033 Uiso 1 1 calc R U . . . C15 C 0.4393(3) 0.2708(3) 0.3080(2) 0.0223(9) Uani 1 1 d . . . . . C16 C 0.4844(4) 0.5555(3) 0.1750(2) 0.0296(10) Uani 1 1 d . . . . . H4 H 0.440395 0.606215 0.157637 0.035 Uiso 1 1 calc R U . . . C17 C 0.9538(3) 0.3330(3) 0.2367(2) 0.0239(9) Uani 1 1 d . . . . . C18 C 0.3809(3) 0.2839(3) 0.3772(2) 0.0243(9) Uani 1 1 d . . . . . C19 C 0.2662(3) -0.0502(3) 0.4791(2) 0.0229(9) Uani 1 1 d . . . . . H5 H 0.229103 0.001436 0.487724 0.028 Uiso 1 1 calc R U . . . C20 C 0.3042(3) -0.1929(3) 0.4697(2) 0.0247(9) Uani 1 1 d . . . . . C21 C 0.6338(3) 0.0946(3) 0.3517(2) 0.0219(9) Uani 1 1 d . . . . . C22 C 0.8494(3) 0.2752(3) 0.2677(2) 0.0222(9) Uani 1 1 d . . . . . C23 C 0.5225(3) 0.0866(3) 0.3954(2) 0.0206(9) Uani 1 1 d . . . . . H6 H 0.478342 0.133567 0.407778 0.025 Uiso 1 1 calc R U . . . C24 C 0.8633(3) 0.0740(3) 0.1838(2) 0.0249(9) Uani 1 1 d . . . . . C25 C 0.6051(4) 0.5531(3) 0.1655(2) 0.0276(10) Uani 1 1 d . . . . . C26 C 0.7611(3) -0.0364(3) 0.3072(2) 0.0223(9) Uani 1 1 d . . . . . C27 C 0.6881(3) -0.2659(3) 0.3253(2) 0.0239(9) Uani 1 1 d . . . . . C28 C 0.3922(3) 0.2184(3) 0.2724(2) 0.0249(9) Uani 1 1 d . . . . . C29 C 0.2739(3) 0.2439(3) 0.4105(2) 0.0260(9) Uani 1 1 d . . . . . H15 H 0.235287 0.251068 0.457362 0.031 Uiso 1 1 calc R U . . . C30 C 0.7098(4) 0.6107(3) 0.1348(2) 0.0274(10) Uani 1 1 d . . . . . C31 C 1.1140(4) 0.4164(3) 0.1852(2) 0.0280(10) Uani 1 1 d . . . . . H7 H 1.190060 0.434101 0.169683 0.034 Uiso 1 1 calc R U . . . C32 C 0.5814(4) -0.3199(3) 0.3590(2) 0.0268(10) Uani 1 1 d . . . . . C33 C 0.4146(4) -0.3959(3) 0.3927(3) 0.0308(10) Uani 1 1 d . . . . . H8 H 0.358884 -0.437981 0.398608 0.037 Uiso 1 1 calc R U . . . C34 C 0.3841(3) -0.0593(3) 0.4523(2) 0.0208(9) Uani 1 1 d . . . . . C35 C 0.8646(3) 0.0162(3) 0.2580(2) 0.0224(9) Uani 1 1 d . . . . . C36 C 0.3023(3) -0.2788(3) 0.4570(2) 0.0252(9) Uani 1 1 d . . . . . C37 C 1.0630(4) 0.0480(3) 0.2401(2) 0.0292(10) Uani 1 1 d . . . . . H16 H 1.130261 0.038174 0.258647 0.035 Uiso 1 1 calc R U . . . C38 C 0.2851(3) 0.1803(3) 0.3075(2) 0.0268(9) Uani 1 1 d . . . . . H17 H 0.253613 0.144552 0.284762 0.032 Uiso 1 1 calc R U . . . C39 C 0.7640(3) -0.1290(3) 0.3048(2) 0.0251(9) Uani 1 1 d . . . . . C40 C 1.2564(4) 0.7096(3) 0.1213(3) 0.0297(10) Uani 1 1 d . . . . . H18 H 1.287402 0.731474 0.154124 0.036 Uiso 1 1 calc R U . . . C41 C 1.0741(3) 0.3294(3) 0.2250(2) 0.0279(10) Uani 1 1 d . . . . . H9 H 1.117965 0.278102 0.240953 0.034 Uiso 1 1 calc R U . . . C42 C 0.1888(3) -0.3227(3) 0.4768(2) 0.0268(10) Uani 1 1 d . . . . . C43 C 0.9653(3) 0.0036(3) 0.2872(2) 0.0244(9) Uani 1 1 d . . . . . C44 C 0.8999(4) 0.6095(3) 0.1231(2) 0.0265(10) Uani 1 1 d . . . . . C45 C 1.1599(3) 0.6551(3) 0.1518(2) 0.0265(9) Uani 1 1 d . . . . . C46 C 1.1619(4) 0.6469(3) 0.0226(2) 0.0275(10) Uani 1 1 d . . . . . C47 C 1.0185(3) 0.4746(3) 0.1720(2) 0.0241(9) Uani 1 1 d . . . . . C48 C 0.1037(4) 0.1591(3) 0.4091(3) 0.0333(11) Uani 1 1 d . . . . . H19 H 0.089998 0.143386 0.464481 0.050 Uiso 1 1 calc R U . . . H20 H 0.093543 0.106436 0.394205 0.050 Uiso 1 1 calc R U . . . H21 H 0.051165 0.205440 0.389913 0.050 Uiso 1 1 calc R U . . . C49 C 0.1565(4) -0.3894(3) 0.5488(3) 0.0331(11) Uani 1 1 d . . . . . C50 C 0.1136(4) -0.2943(3) 0.4257(3) 0.0318(11) Uani 1 1 d . . . . . C51 C 1.2597(4) 0.6993(3) -0.0046(3) 0.0296(10) Uani 1 1 d . . . . . H22 H 1.294334 0.712811 -0.056674 0.035 Uiso 1 1 calc R U . . . C52 C 0.4330(4) 0.3370(3) 0.4180(3) 0.0296(10) Uani 1 1 d . . . . . H23 H 0.440498 0.399572 0.387253 0.044 Uiso 1 1 calc R U . . . H24 H 0.506778 0.312750 0.425064 0.044 Uiso 1 1 calc R U . . . H25 H 0.384881 0.332407 0.467469 0.044 Uiso 1 1 calc R U . . . C53 C 0.8380(3) -0.1745(3) 0.2575(2) 0.0269(10) Uani 1 1 d . . . . . H10 H 0.906033 -0.151829 0.223883 0.032 Uiso 1 1 calc R U . . . C54 C 0.9633(4) 0.1191(3) 0.1393(2) 0.0292(10) Uani 1 1 d . . . . . H26 H 0.962395 0.158529 0.090178 0.035 Uiso 1 1 calc R U . . . C55 C 0.9647(4) -0.0524(3) 0.3694(2) 0.0302(10) Uani 1 1 d . . . . . H27 H 1.039629 -0.052841 0.379798 0.045 Uiso 1 1 calc R U . . . H28 H 0.941881 -0.113416 0.376949 0.045 Uiso 1 1 calc R U . . . H29 H 0.912032 -0.026655 0.403967 0.045 Uiso 1 1 calc R U . . . C56 C 0.7492(4) 0.7002(3) 0.0916(3) 0.0307(10) Uani 1 1 d . . . . . H11 H 0.705019 0.749761 0.071729 0.037 Uiso 1 1 calc R U . . . C57 C 0.8660(4) 0.6993(3) 0.0850(2) 0.0296(10) Uani 1 1 d . . . . . H12 H 0.914425 0.748800 0.059965 0.036 Uiso 1 1 calc R U . . . C58 C 0.5263(4) -0.3960(3) 0.3541(3) 0.0327(11) Uani 1 1 d . . . . . H13 H 0.559454 -0.437997 0.329300 0.039 Uiso 1 1 calc R U . . . C59 C 1.0647(4) 0.1067(3) 0.1664(3) 0.0331(11) Uani 1 1 d . . . . . C60 C 0.4562(4) 0.2016(3) 0.1990(3) 0.0345(11) Uani 1 1 d . . . . . H30 H 0.487553 0.257746 0.163015 0.052 Uiso 1 1 calc R U . . . H31 H 0.405233 0.177015 0.176815 0.052 Uiso 1 1 calc R U . . . H32 H 0.516663 0.159292 0.210277 0.052 Uiso 1 1 calc R U . . . C61 C 0.7902(3) -0.2594(3) 0.2705(2) 0.0284(10) Uani 1 1 d . . . . . H14 H 0.820405 -0.303426 0.247200 0.034 Uiso 1 1 calc R U . . . C62 C 0.7567(4) 0.0893(3) 0.1519(3) 0.0340(11) Uani 1 1 d . . . . . H33 H 0.708656 0.131309 0.172985 0.051 Uiso 1 1 calc R U . . . H34 H 0.717223 0.032678 0.165785 0.051 Uiso 1 1 calc R U . . . H35 H 0.776059 0.113674 0.096614 0.051 Uiso 1 1 calc R U . . . C63 C -0.0298(4) -0.3960(3) 0.5200(3) 0.0395(13) Uani 1 1 d . . . . . C64 C 1.4140(4) 0.7911(3) 0.0124(3) 0.0404(12) Uani 1 1 d . . . . . H36 H 1.410209 0.835480 0.039407 0.061 Uiso 1 1 calc R U . . . H37 H 1.419124 0.821277 -0.041768 0.061 Uiso 1 1 calc R U . . . H38 H 1.479880 0.753639 0.019750 0.061 Uiso 1 1 calc R U . . . C65 C 0.0043(4) -0.3327(3) 0.4486(3) 0.0377(12) Uani 1 1 d . . . . . H39 H -0.046135 -0.315178 0.415093 0.045 Uiso 1 1 calc R U . . . C66 C 1.1136(4) 0.6119(3) -0.0325(3) 0.0395(12) Uani 1 1 d . . . . . H40 H 1.157954 0.635243 -0.083965 0.059 Uiso 1 1 calc R U . . . H41 H 1.036114 0.631674 -0.031818 0.059 Uiso 1 1 calc R U . . . H42 H 1.116076 0.546807 -0.016657 0.059 Uiso 1 1 calc R U . . . C67 C 0.0460(4) -0.4238(3) 0.5692(3) 0.0392(12) Uani 1 1 d . . . . . H43 H 0.022551 -0.466534 0.617151 0.047 Uiso 1 1 calc R U . . . C68 C 0.1510(4) -0.2264(3) 0.3475(3) 0.0387(11) Uani 1 1 d . . . . . H44 H 0.089406 -0.214684 0.320297 0.058 Uiso 1 1 calc R U . . . H45 H 0.214751 -0.250146 0.318456 0.058 Uiso 1 1 calc R U . . . H46 H 0.172906 -0.170892 0.353686 0.058 Uiso 1 1 calc R U . . . C69 C 0.2397(4) -0.4236(3) 0.6008(3) 0.0446(13) Uani 1 1 d . . . . . H47 H 0.300606 -0.454657 0.576300 0.067 Uiso 1 1 calc R U . . . H48 H 0.201810 -0.464731 0.648799 0.067 Uiso 1 1 calc R U . . . H49 H 0.269935 -0.373347 0.610642 0.067 Uiso 1 1 calc R U . . . C70 C -0.1489(4) -0.4375(3) 0.5453(4) 0.0559(17) Uani 1 1 d . . . . . H50 H -0.143179 -0.502259 0.556663 0.084 Uiso 1 1 calc R U . . . H51 H -0.190188 -0.413737 0.504409 0.084 Uiso 1 1 calc R U . . . H52 H -0.188426 -0.422628 0.590659 0.084 Uiso 1 1 calc R U . . . C71 C 1.1728(4) 0.1541(4) 0.1160(3) 0.0474(14) Uani 1 1 d . . . . . H53 H 1.204766 0.122991 0.078808 0.071 Uiso 1 1 calc R U . . . H54 H 1.226544 0.153806 0.147657 0.071 Uiso 1 1 calc R U . . . H55 H 1.155858 0.215624 0.089460 0.071 Uiso 1 1 calc R U . . . C72 C 1.1084(4) 0.6298(4) 0.2373(3) 0.0451(13) Uani 1 1 d . . . . . H56 H 1.042190 0.666286 0.245705 0.068 Uiso 1 1 calc R U . . . H57 H 1.163177 0.640135 0.264613 0.068 Uiso 1 1 calc R U . . . H58 H 1.087096 0.566818 0.255832 0.068 Uiso 1 1 calc R U . . . Cl2 Cl 0.36732(14) 0.39978(12) 0.03894(9) 0.0676(4) Uani 1 1 d . . . . . Cl3 Cl 0.08890(17) 0.89030(12) 0.06553(10) 0.0793(5) Uani 1 1 d D . . . . C73 C 0.4402(5) 0.5094(4) -0.0012(4) 0.0668(18) Uani 1 1 d . . . . . H59 H 0.431096 0.537905 -0.053971 0.080 Uiso 1 1 calc R U . . . H60 H 0.409546 0.549462 0.029416 0.080 Uiso 1 1 calc R U . . . C75 C 0.0516(7) 1.0179(6) -0.0132(5) 0.139(5) Uani 1 1 d D . . . . H61 H 0.063306 1.071286 0.001345 0.167 Uiso 1 1 calc R U . . . H62 H 0.082696 1.025379 -0.067489 0.167 Uiso 1 1 calc R U . . . Cl4 Cl 0.59909(15) 0.93544(10) 0.07783(9) 0.0682(5) Uani 1 1 d . . . . . C76 C 0.5566(5) 0.8661(4) 0.1765(3) 0.0577(15) Uani 1 1 d . . . . . H63 H 0.578618 0.804342 0.177600 0.4(3) Uiso 0.468(4) 1 calc R . P A 1 H64 H 0.603030 0.884609 0.206008 0.04(3) Uiso 0.468(4) 1 calc R . P A 1 H65 H 0.524023 0.809375 0.178519 0.03(2) Uiso 0.532(4) 1 calc R . P A 2 H66 H 0.621747 0.852432 0.201198 0.09(4) Uiso 0.532(4) 1 calc R . P A 2 C77 C 0.4355(11) 0.8618(10) 0.2208(8) 0.055(3) Uani 0.468(4) 1 d . . P A 1 H67 H 0.426646 0.811687 0.268248 0.066 Uiso 0.468(4) 1 calc R U P A 1 H68 H 0.384265 0.852038 0.190058 0.066 Uiso 0.468(4) 1 calc R U P A 1 Cl6 Cl 0.4009(3) 0.9678(2) 0.2431(2) 0.0715(13) Uani 0.468(4) 1 d . . P A 1 C78 C 0.4722(12) 0.9177(11) 0.2154(8) 0.071(4) Uani 0.532(4) 1 d . . P A 2 H69 H 0.505225 0.975426 0.210059 0.085 Uiso 0.532(4) 1 calc R U P A 2 H70 H 0.453406 0.884758 0.270110 0.085 Uiso 0.532(4) 1 calc R U P A 2 Cl5 Cl 0.3440(2) 0.9382(2) 0.17822(19) 0.0744(12) Uani 0.532(4) 1 d . . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0150(3) 0.0205(3) 0.0319(3) -0.0126(2) 0.0036(2) -0.0037(2) Ni2 0.0147(3) 0.0204(3) 0.0359(3) -0.0063(2) -0.0011(2) -0.0026(2) N1 0.0119(17) 0.0222(17) 0.033(2) -0.0079(15) -0.0018(14) 0.0003(14) N2 0.0175(17) 0.0196(17) 0.0293(19) -0.0110(14) 0.0052(14) -0.0037(14) N3 0.0128(16) 0.0252(18) 0.0293(19) -0.0133(15) 0.0035(14) -0.0026(14) N4 0.0181(18) 0.0206(17) 0.036(2) -0.0154(15) 0.0032(15) -0.0030(15) N5 0.0186(18) 0.0236(18) 0.034(2) -0.0064(15) -0.0032(15) -0.0002(16) N6 0.0177(18) 0.0220(18) 0.036(2) -0.0042(15) -0.0011(15) -0.0007(15) N7 0.0178(18) 0.0239(18) 0.033(2) -0.0098(15) 0.0004(15) -0.0036(15) N8 0.0148(17) 0.0251(18) 0.0297(19) -0.0119(15) 0.0052(14) -0.0018(15) C1 0.016(2) 0.021(2) 0.026(2) -0.0092(17) -0.0007(16) -0.0041(17) C2 0.020(2) 0.025(2) 0.027(2) -0.0099(18) -0.0006(17) -0.0029(18) C3 0.019(2) 0.023(2) 0.036(2) -0.0140(18) 0.0005(18) -0.0081(18) C4 0.019(2) 0.020(2) 0.024(2) -0.0091(16) -0.0006(16) -0.0029(17) C5 0.017(2) 0.019(2) 0.029(2) -0.0084(17) -0.0038(17) -0.0003(17) C6 0.018(2) 0.022(2) 0.030(2) -0.0097(18) 0.0017(17) -0.0025(17) C7 0.015(2) 0.027(2) 0.031(2) -0.0089(18) -0.0003(17) -0.0021(18) C8 0.020(2) 0.032(2) 0.027(2) -0.0169(19) 0.0017(17) -0.0072(19) C9 0.016(2) 0.024(2) 0.030(2) -0.0025(18) -0.0033(17) -0.0002(18) C10 0.019(2) 0.026(2) 0.025(2) -0.0136(17) -0.0014(17) -0.0010(18) C11 0.018(2) 0.026(2) 0.028(2) -0.0117(18) 0.0035(17) -0.0039(18) C12 0.017(2) 0.028(2) 0.025(2) -0.0120(17) -0.0019(17) 0.0000(18) C13 0.017(2) 0.022(2) 0.041(3) -0.0073(19) -0.0015(19) -0.0005(18) C14 0.018(2) 0.034(2) 0.030(2) -0.0114(19) -0.0038(18) 0.0009(19) C15 0.016(2) 0.021(2) 0.029(2) -0.0072(17) -0.0033(17) 0.0013(17) C16 0.022(2) 0.029(2) 0.037(3) -0.0103(19) -0.0043(19) 0.0029(19) C17 0.019(2) 0.022(2) 0.030(2) -0.0073(17) -0.0034(17) -0.0040(18) C18 0.018(2) 0.021(2) 0.034(2) -0.0099(18) -0.0054(18) 0.0051(17) C19 0.019(2) 0.023(2) 0.026(2) -0.0099(17) 0.0016(17) -0.0001(17) C20 0.019(2) 0.027(2) 0.026(2) -0.0080(18) 0.0018(17) -0.0058(18) C21 0.018(2) 0.025(2) 0.024(2) -0.0087(17) -0.0040(17) -0.0031(17) C22 0.017(2) 0.024(2) 0.025(2) -0.0093(17) -0.0003(17) -0.0022(18) C23 0.019(2) 0.021(2) 0.023(2) -0.0089(16) -0.0021(16) -0.0008(17) C24 0.022(2) 0.026(2) 0.030(2) -0.0128(18) -0.0030(18) -0.0039(18) C25 0.023(2) 0.025(2) 0.033(2) -0.0078(18) -0.0036(18) 0.0015(19) C26 0.018(2) 0.023(2) 0.025(2) -0.0071(17) -0.0026(17) -0.0016(17) C27 0.020(2) 0.021(2) 0.032(2) -0.0134(18) 0.0008(18) 0.0016(17) C28 0.020(2) 0.026(2) 0.027(2) -0.0075(18) -0.0043(17) -0.0004(18) C29 0.019(2) 0.026(2) 0.029(2) -0.0073(18) 0.0017(18) 0.0025(18) C30 0.024(2) 0.024(2) 0.032(2) -0.0096(18) -0.0010(19) -0.0009(19) C31 0.018(2) 0.032(2) 0.032(2) -0.0073(19) -0.0020(18) -0.0075(19) C32 0.024(2) 0.027(2) 0.031(2) -0.0135(18) -0.0002(18) 0.0007(19) C33 0.024(2) 0.026(2) 0.044(3) -0.018(2) 0.004(2) -0.0085(19) C34 0.019(2) 0.020(2) 0.024(2) -0.0089(17) -0.0014(16) -0.0026(17) C35 0.018(2) 0.024(2) 0.026(2) -0.0122(17) 0.0035(17) -0.0030(17) C36 0.019(2) 0.028(2) 0.028(2) -0.0117(18) 0.0001(17) -0.0030(18) C37 0.018(2) 0.040(3) 0.032(2) -0.016(2) -0.0012(18) -0.006(2) C38 0.019(2) 0.030(2) 0.034(2) -0.0111(19) -0.0092(18) -0.0006(18) C39 0.015(2) 0.029(2) 0.031(2) -0.0111(18) -0.0005(17) -0.0015(18) C40 0.023(2) 0.028(2) 0.043(3) -0.017(2) -0.008(2) 0.0006(19) C41 0.018(2) 0.028(2) 0.036(3) -0.0082(19) -0.0038(18) -0.0011(18) C42 0.020(2) 0.024(2) 0.037(3) -0.0185(19) 0.0066(19) -0.0040(18) C43 0.019(2) 0.025(2) 0.031(2) -0.0133(18) 0.0012(18) -0.0046(18) C44 0.024(2) 0.025(2) 0.029(2) -0.0118(18) 0.0024(18) -0.0047(19) C45 0.020(2) 0.028(2) 0.031(2) -0.0125(19) 0.0000(18) -0.0031(18) C46 0.027(2) 0.024(2) 0.030(2) -0.0090(18) 0.0009(19) -0.0038(19) C47 0.014(2) 0.029(2) 0.029(2) -0.0106(18) 0.0002(17) -0.0016(18) C48 0.020(2) 0.036(3) 0.039(3) -0.005(2) -0.0015(19) -0.005(2) C49 0.027(2) 0.033(2) 0.040(3) -0.021(2) 0.009(2) -0.007(2) C50 0.023(2) 0.028(2) 0.051(3) -0.026(2) -0.003(2) 0.0018(19) C51 0.027(2) 0.029(2) 0.028(2) -0.0062(19) 0.0024(19) -0.004(2) C52 0.025(2) 0.029(2) 0.036(3) -0.0158(19) 0.0005(19) 0.0008(19) C53 0.021(2) 0.031(2) 0.028(2) -0.0129(18) 0.0040(18) -0.0003(19) C54 0.033(3) 0.031(2) 0.022(2) -0.0081(18) 0.0010(18) -0.008(2) C55 0.023(2) 0.033(2) 0.034(2) -0.010(2) -0.0032(19) -0.002(2) C56 0.029(2) 0.025(2) 0.035(3) -0.0066(19) -0.0029(19) 0.0027(19) C57 0.031(3) 0.026(2) 0.030(2) -0.0099(19) 0.0021(19) -0.008(2) C58 0.029(2) 0.026(2) 0.046(3) -0.022(2) 0.001(2) -0.003(2) C59 0.026(2) 0.042(3) 0.032(3) -0.017(2) 0.0063(19) -0.015(2) C60 0.025(2) 0.045(3) 0.035(3) -0.019(2) 0.000(2) -0.005(2) C61 0.021(2) 0.029(2) 0.035(2) -0.0168(19) 0.0031(18) 0.0020(19) C62 0.028(2) 0.040(3) 0.032(3) -0.008(2) -0.004(2) -0.006(2) C63 0.020(2) 0.033(3) 0.069(4) -0.033(3) 0.009(2) 0.001(2) C64 0.025(2) 0.037(3) 0.052(3) -0.005(2) -0.002(2) -0.012(2) C65 0.024(2) 0.034(3) 0.062(3) -0.028(2) -0.004(2) 0.003(2) C66 0.041(3) 0.047(3) 0.030(3) -0.015(2) 0.001(2) -0.016(2) C67 0.032(3) 0.034(3) 0.049(3) -0.020(2) 0.014(2) -0.009(2) C68 0.037(3) 0.037(3) 0.049(3) -0.020(2) -0.013(2) 0.003(2) C69 0.044(3) 0.048(3) 0.036(3) -0.007(2) 0.003(2) -0.017(3) C70 0.023(3) 0.040(3) 0.108(5) -0.043(3) 0.014(3) -0.010(2) C71 0.031(3) 0.070(4) 0.036(3) -0.011(3) 0.005(2) -0.025(3) C72 0.043(3) 0.059(3) 0.040(3) -0.026(3) 0.000(2) -0.019(3) Cl2 0.0709(10) 0.0806(11) 0.0491(9) -0.0250(8) 0.0039(7) -0.0124(9) Cl3 0.1054(14) 0.0733(11) 0.0600(10) -0.0249(8) -0.0240(9) 0.0441(10) C73 0.076(4) 0.076(4) 0.055(4) -0.033(3) -0.018(3) 0.032(4) C75 0.120(7) 0.162(9) 0.157(8) -0.136(8) 0.079(6) -0.085(6) Cl4 0.0889(12) 0.0505(8) 0.0699(10) -0.0122(7) -0.0320(9) -0.0100(8) C76 0.052(4) 0.052(4) 0.066(4) -0.010(3) -0.020(3) 0.004(3) C77 0.052(8) 0.053(8) 0.064(9) -0.014(7) -0.025(7) -0.003(7) Cl6 0.089(3) 0.060(2) 0.079(3) -0.0348(19) -0.031(2) 0.0200(19) C78 0.075(10) 0.077(10) 0.069(9) -0.029(8) -0.029(7) 0.016(9) Cl5 0.0431(17) 0.094(3) 0.073(2) -0.0064(17) -0.0128(14) 0.0112(16) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' 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 N8 Ni1 N3 174.39(16) . . ? N8 Ni1 N2 94.56(14) . . ? N3 Ni1 N2 85.71(14) . . ? N8 Ni1 N4 84.97(14) . . ? N3 Ni1 N4 94.07(14) . . ? N2 Ni1 N4 172.94(16) . . ? N6 Ni2 N7 179.30(17) . . ? N6 Ni2 N5 84.97(15) . . ? N7 Ni2 N5 94.59(15) . . ? N6 Ni2 N1 94.80(15) . . ? N7 Ni2 N1 85.63(15) . . ? N5 Ni2 N1 179.20(16) . . ? C22 N1 C2 112.1(3) . . ? C22 N1 Ni2 116.0(3) . . ? C2 N1 Ni2 131.8(3) . . ? C10 N2 C1 111.4(3) . . ? C10 N2 Ni1 115.4(3) . . ? C1 N2 Ni1 131.7(3) . . ? C34 N3 C20 110.6(3) . . ? C34 N3 Ni1 117.0(3) . . ? C20 N3 Ni1 130.7(3) . . ? C32 N4 C3 111.7(3) . . ? C32 N4 Ni1 116.7(3) . . ? C3 N4 Ni1 130.0(3) . . ? C30 N5 C44 111.8(3) . . ? C30 N5 Ni2 117.9(3) . . ? C44 N5 Ni2 130.2(3) . . ? C25 N6 C7 112.5(3) . . ? C25 N6 Ni2 118.0(3) . . ? C7 N6 Ni2 129.2(3) . . ? C17 N7 C47 111.9(3) . . ? C17 N7 Ni2 117.6(3) . . ? C47 N7 Ni2 130.0(3) . . ? C27 N8 C39 111.2(3) . . ? C27 N8 Ni1 117.7(3) . . ? C39 N8 Ni1 129.3(3) . . ? N2 C1 C26 118.2(3) . . ? N2 C1 C21 104.8(3) . . ? C26 C1 C21 136.4(3) . . ? N1 C2 C12 117.7(3) . . ? N1 C2 C4 104.8(3) . . ? C12 C2 C4 137.5(4) . . ? N4 C3 C36 120.8(3) . . ? N4 C3 C33 105.6(3) . . ? C36 C3 C33 133.1(4) . . ? C5 C4 C21 123.4(4) . . ? C5 C4 C2 106.9(3) . . ? C21 C4 C2 129.6(4) . . ? C4 C5 C22 107.8(4) . . ? C46 C6 C45 120.6(4) . . ? C46 C6 C8 120.9(4) . . ? C45 C6 C8 118.5(4) . . ? N6 C7 C12 121.9(4) . . ? N6 C7 C14 105.0(3) . . ? C12 C7 C14 133.0(4) . . ? C47 C8 C44 123.6(4) . . ? C47 C8 C6 118.1(4) . . ? C44 C8 C6 118.3(4) . . ? C29 C9 C38 118.2(4) . . ? C29 C9 C48 120.5(4) . . ? C38 C9 C48 121.3(4) . . ? N2 C10 C23 109.2(3) . . ? N2 C10 C34 112.0(3) . . ? C23 C10 C34 138.4(4) . . ? C19 C11 C20 108.3(3) . . ? C7 C12 C2 124.2(3) . . ? C7 C12 C15 112.8(3) . . ? C2 C12 C15 122.9(4) . . ? C40 C13 C51 117.9(4) . . ? C40 C13 C64 121.1(4) . . ? C51 C13 C64 121.0(4) . . ? C16 C14 C7 108.3(4) . . ? C18 C15 C28 120.9(4) . . ? C18 C15 C12 118.2(3) . . ? C28 C15 C12 120.9(4) . . ? C14 C16 C25 107.1(4) . . ? N7 C17 C41 107.6(3) . . ? N7 C17 C22 109.6(3) . . ? C41 C17 C22 142.7(4) . . ? C15 C18 C29 118.7(4) . . ? C15 C18 C52 121.4(4) . . ? C29 C18 C52 119.9(4) . . ? C11 C19 C34 106.8(3) . . ? N3 C20 C36 120.4(4) . . ? N3 C20 C11 105.6(3) . . ? C36 C20 C11 133.2(4) . . ? C23 C21 C4 124.9(4) . . ? C23 C21 C1 106.4(3) . . ? C4 C21 C1 128.7(3) . . ? N1 C22 C5 108.4(3) . . ? N1 C22 C17 111.1(3) . . ? C5 C22 C17 140.5(4) . . ? C10 C23 C21 108.1(3) . . ? C54 C24 C35 118.9(4) . . ? C54 C24 C62 119.7(4) . . ? C35 C24 C62 121.3(4) . . ? N6 C25 C16 107.1(3) . . ? N6 C25 C30 109.5(4) . . ? C16 C25 C30 143.4(4) . . ? C1 C26 C39 124.5(3) . . ? C1 C26 C35 123.1(3) . . ? C39 C26 C35 112.4(3) . . ? N8 C27 C61 107.6(3) . . ? N8 C27 C32 109.5(3) . . ? C61 C27 C32 142.0(4) . . ? C38 C28 C15 118.3(4) . . ? C38 C28 C60 120.4(4) . . ? C15 C28 C60 121.3(4) . . ? C9 C29 C18 121.8(4) . . ? N5 C30 C56 107.6(4) . . ? N5 C30 C25 109.6(3) . . ? C56 C30 C25 142.8(4) . . ? C41 C31 C47 108.4(4) . . ? N4 C32 C58 107.3(3) . . ? N4 C32 C27 111.0(3) . . ? C58 C32 C27 141.0(4) . . ? C58 C33 C3 107.9(4) . . ? N3 C34 C19 108.5(3) . . ? N3 C34 C10 109.7(3) . . ? C19 C34 C10 141.1(4) . . ? C24 C35 C43 120.4(4) . . ? C24 C35 C26 121.2(4) . . ? C43 C35 C26 118.3(4) . . ? C20 C36 C3 123.7(3) . . ? C20 C36 C42 116.1(4) . . ? C3 C36 C42 120.1(3) . . ? C43 C37 C59 122.6(4) . . ? C28 C38 C9 122.1(4) . . ? N8 C39 C53 106.1(3) . . ? N8 C39 C26 121.4(4) . . ? C53 C39 C26 132.1(4) . . ? C13 C40 C45 122.4(4) . . ? C31 C41 C17 107.0(4) . . ? C50 C42 C49 121.1(4) . . ? C50 C42 C36 119.9(4) . . ? C49 C42 C36 118.9(4) . . ? C37 C43 C35 118.5(4) . . ? C37 C43 C55 120.8(4) . . ? C35 C43 C55 120.5(3) . . ? N5 C44 C8 120.5(4) . . ? N5 C44 C57 105.2(4) . . ? C8 C44 C57 134.2(4) . . ? C40 C45 C6 118.2(4) . . ? C40 C45 C72 120.5(4) . . ? C6 C45 C72 121.4(4) . . ? C51 C46 C6 119.0(4) . . ? C51 C46 C66 119.6(4) . . ? C6 C46 C66 121.3(4) . . ? N7 C47 C8 120.8(4) . . ? N7 C47 C31 105.1(3) . . ? C8 C47 C31 134.1(4) . . ? C67 C49 C42 118.0(5) . . ? C67 C49 C69 121.3(4) . . ? C42 C49 C69 120.7(4) . . ? C65 C50 C42 118.3(4) . . ? C65 C50 C68 121.2(4) . . ? C42 C50 C68 120.5(4) . . ? C46 C51 C13 121.9(4) . . ? C61 C53 C39 107.8(3) . . ? C24 C54 C59 121.8(4) . . ? C57 C56 C30 106.7(4) . . ? C56 C57 C44 108.7(4) . . ? C33 C58 C32 107.4(4) . . ? C37 C59 C54 117.7(4) . . ? C37 C59 C71 121.5(4) . . ? C54 C59 C71 120.8(4) . . ? C53 C61 C27 107.3(3) . . ? C65 C63 C67 119.4(4) . . ? C65 C63 C70 121.4(5) . . ? C67 C63 C70 119.1(5) . . ? C63 C65 C50 121.3(5) . . ? C63 C67 C49 121.8(5) . . ? C73 C73 Cl2 106.2(6) 2_665 . ? C75 C75 Cl3 79.7(9) 2_575 . ? C78 C76 Cl4 106.9(7) . . ? C77 C76 Cl4 122.5(6) . . ? C76 C77 Cl6 109.1(9) . . ? C76 C78 Cl5 113.4(9) . . ? 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 Ni1 N8 1.780(3) . ? Ni1 N3 1.788(3) . ? Ni1 N2 1.800(3) . ? Ni1 N4 1.802(3) . ? Ni2 N6 1.767(3) . ? Ni2 N7 1.777(3) . ? Ni2 N5 1.780(3) . ? Ni2 N1 1.791(3) . ? N1 C22 1.344(5) . ? N1 C2 1.377(5) . ? N2 C10 1.340(5) . ? N2 C1 1.386(5) . ? N3 C34 1.344(5) . ? N3 C20 1.378(5) . ? N4 C32 1.340(5) . ? N4 C3 1.375(5) . ? N5 C30 1.343(5) . ? N5 C44 1.372(5) . ? N6 C25 1.355(5) . ? N6 C7 1.365(5) . ? N7 C17 1.340(5) . ? N7 C47 1.374(5) . ? N8 C27 1.358(5) . ? N8 C39 1.370(5) . ? C1 C26 1.416(5) . ? C1 C21 1.481(5) . ? C2 C12 1.435(6) . ? C2 C4 1.478(6) . ? C3 C36 1.423(6) . ? C3 C33 1.432(6) . ? C4 C5 1.394(5) . ? C4 C21 1.461(5) . ? C5 C22 1.412(5) . ? C6 C46 1.392(6) . ? C6 C45 1.408(6) . ? C6 C8 1.498(5) . ? C7 C12 1.423(6) . ? C7 C14 1.444(6) . ? C8 C47 1.411(6) . ? C8 C44 1.420(6) . ? C9 C29 1.382(6) . ? C9 C38 1.390(6) . ? C9 C48 1.505(5) . ? C10 C23 1.394(5) . ? C10 C34 1.485(5) . ? C11 C19 1.379(5) . ? C11 C20 1.432(6) . ? C12 C15 1.495(5) . ? C13 C40 1.383(6) . ? C13 C51 1.395(6) . ? C13 C64 1.513(5) . ? C14 C16 1.389(6) . ? C15 C18 1.393(6) . ? C15 C28 1.401(6) . ? C16 C25 1.423(6) . ? C17 C41 1.416(6) . ? C17 C22 1.491(5) . ? C18 C29 1.395(5) . ? C18 C52 1.513(6) . ? C19 C34 1.411(5) . ? C20 C36 1.422(6) . ? C21 C23 1.399(5) . ? C24 C54 1.394(6) . ? C24 C35 1.395(6) . ? C24 C62 1.499(6) . ? C25 C30 1.492(6) . ? C26 C39 1.446(5) . ? C26 C35 1.494(5) . ? C27 C61 1.404(5) . ? C27 C32 1.485(5) . ? C28 C38 1.390(5) . ? C28 C60 1.502(6) . ? C30 C56 1.425(6) . ? C31 C41 1.382(6) . ? C31 C47 1.430(6) . ? C32 C58 1.422(6) . ? C33 C58 1.381(6) . ? C35 C43 1.408(6) . ? C36 C42 1.487(5) . ? C37 C43 1.383(5) . ? C37 C59 1.388(6) . ? C39 C53 1.423(6) . ? C40 C45 1.389(6) . ? C42 C50 1.403(6) . ? C42 C49 1.410(6) . ? C43 C55 1.504(6) . ? C44 C57 1.431(6) . ? C45 C72 1.511(6) . ? C46 C51 1.383(6) . ? C46 C66 1.519(6) . ? C49 C67 1.394(6) . ? C49 C69 1.496(7) . ? C50 C65 1.401(6) . ? C50 C68 1.503(6) . ? C53 C61 1.399(6) . ? C54 C59 1.395(6) . ? C56 C57 1.382(6) . ? C59 C71 1.511(6) . ? C63 C65 1.380(7) . ? C63 C67 1.383(7) . ? C63 C70 1.526(6) . ? Cl2 C73 1.826(7) . ? Cl3 C75 2.153(11) . ? C73 C73 1.455(12) 2_665 ? C75 C75 1.323(13) 2_575 ? Cl4 C76 1.797(6) . ? C76 C78 1.459(15) . ? C76 C77 1.506(14) . ? C77 Cl6 1.814(15) . ? C78 Cl5 1.791(14) . ? 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 N6 Ni2 N1 C22 179.2(3) . . . . ? N7 Ni2 N1 C22 -0.3(3) . . . . ? N6 Ni2 N1 C2 -3.6(4) . . . . ? N7 Ni2 N1 C2 177.0(4) . . . . ? N8 Ni1 N2 C10 170.4(3) . . . . ? N3 Ni1 N2 C10 -4.0(3) . . . . ? N8 Ni1 N2 C1 6.0(4) . . . . ? N3 Ni1 N2 C1 -168.3(4) . . . . ? N2 Ni1 N3 C34 4.1(3) . . . . ? N4 Ni1 N3 C34 -168.8(3) . . . . ? N2 Ni1 N3 C20 167.4(4) . . . . ? N4 Ni1 N3 C20 -5.5(4) . . . . ? N8 Ni1 N4 C32 -3.9(3) . . . . ? N3 Ni1 N4 C32 170.5(3) . . . . ? N8 Ni1 N4 C3 -168.0(4) . . . . ? N3 Ni1 N4 C3 6.4(4) . . . . ? N6 Ni2 N5 C30 0.3(3) . . . . ? N7 Ni2 N5 C30 179.8(3) . . . . ? N6 Ni2 N5 C44 -176.0(4) . . . . ? N7 Ni2 N5 C44 3.4(4) . . . . ? N5 Ni2 N6 C25 -2.0(3) . . . . ? N1 Ni2 N6 C25 178.7(3) . . . . ? N5 Ni2 N6 C7 -175.2(4) . . . . ? N1 Ni2 N6 C7 5.5(4) . . . . ? N5 Ni2 N7 C17 -176.8(3) . . . . ? N1 Ni2 N7 C17 2.4(3) . . . . ? N5 Ni2 N7 C47 -5.5(4) . . . . ? N1 Ni2 N7 C47 173.7(4) . . . . ? N2 Ni1 N8 C27 -169.4(3) . . . . ? N4 Ni1 N8 C27 3.6(3) . . . . ? N2 Ni1 N8 C39 -6.3(4) . . . . ? N4 Ni1 N8 C39 166.7(4) . . . . ? C10 N2 C1 C26 -169.7(4) . . . . ? Ni1 N2 C1 C26 -4.9(6) . . . . ? C10 N2 C1 C21 2.9(4) . . . . ? Ni1 N2 C1 C21 167.7(3) . . . . ? C22 N1 C2 C12 177.4(3) . . . . ? Ni2 N1 C2 C12 0.0(6) . . . . ? C22 N1 C2 C4 -1.5(4) . . . . ? Ni2 N1 C2 C4 -178.8(3) . . . . ? C32 N4 C3 C36 -170.6(4) . . . . ? Ni1 N4 C3 C36 -5.9(6) . . . . ? C32 N4 C3 C33 2.1(5) . . . . ? Ni1 N4 C3 C33 166.8(3) . . . . ? N1 C2 C4 C5 1.9(4) . . . . ? C12 C2 C4 C5 -176.6(5) . . . . ? N1 C2 C4 C21 -175.1(4) . . . . ? C12 C2 C4 C21 6.3(8) . . . . ? C21 C4 C5 C22 175.6(4) . . . . ? C2 C4 C5 C22 -1.7(4) . . . . ? C25 N6 C7 C12 -177.6(4) . . . . ? Ni2 N6 C7 C12 -4.1(6) . . . . ? C25 N6 C7 C14 1.1(5) . . . . ? Ni2 N6 C7 C14 174.6(3) . . . . ? C46 C6 C8 C47 100.3(5) . . . . ? C45 C6 C8 C47 -78.8(5) . . . . ? C46 C6 C8 C44 -80.0(5) . . . . ? C45 C6 C8 C44 100.9(5) . . . . ? C1 N2 C10 C23 -3.7(5) . . . . ? Ni1 N2 C10 C23 -171.2(3) . . . . ? C1 N2 C10 C34 170.6(3) . . . . ? Ni1 N2 C10 C34 3.1(4) . . . . ? N6 C7 C12 C2 -1.3(6) . . . . ? C14 C7 C12 C2 -179.5(4) . . . . ? N6 C7 C12 C15 174.8(4) . . . . ? C14 C7 C12 C15 -3.5(7) . . . . ? N1 C2 C12 C7 3.2(6) . . . . ? C4 C2 C12 C7 -178.5(4) . . . . ? N1 C2 C12 C15 -172.5(4) . . . . ? C4 C2 C12 C15 5.8(7) . . . . ? N6 C7 C14 C16 -0.7(5) . . . . ? C12 C7 C14 C16 177.8(4) . . . . ? C7 C12 C15 C18 -78.7(5) . . . . ? C2 C12 C15 C18 97.4(5) . . . . ? C7 C12 C15 C28 99.1(5) . . . . ? C2 C12 C15 C28 -84.7(5) . . . . ? C7 C14 C16 C25 0.1(5) . . . . ? C47 N7 C17 C41 0.8(5) . . . . ? Ni2 N7 C17 C41 173.6(3) . . . . ? C47 N7 C17 C22 -176.5(3) . . . . ? Ni2 N7 C17 C22 -3.7(4) . . . . ? C28 C15 C18 C29 -0.1(6) . . . . ? C12 C15 C18 C29 177.7(4) . . . . ? C28 C15 C18 C52 177.4(4) . . . . ? C12 C15 C18 C52 -4.7(6) . . . . ? C20 C11 C19 C34 -0.4(5) . . . . ? C34 N3 C20 C36 168.2(4) . . . . ? Ni1 N3 C20 C36 4.0(6) . . . . ? C34 N3 C20 C11 -3.3(5) . . . . ? Ni1 N3 C20 C11 -167.4(3) . . . . ? C19 C11 C20 N3 2.2(5) . . . . ? C19 C11 C20 C36 -167.7(4) . . . . ? C5 C4 C21 C23 146.5(4) . . . . ? C2 C4 C21 C23 -36.8(6) . . . . ? C5 C4 C21 C1 -33.9(6) . . . . ? C2 C4 C21 C1 142.7(4) . . . . ? N2 C1 C21 C23 -1.1(4) . . . . ? C26 C1 C21 C23 169.5(5) . . . . ? N2 C1 C21 C4 179.3(4) . . . . ? C26 C1 C21 C4 -10.1(8) . . . . ? C2 N1 C22 C5 0.4(5) . . . . ? Ni2 N1 C22 C5 178.2(3) . . . . ? C2 N1 C22 C17 -179.4(3) . . . . ? Ni2 N1 C22 C17 -1.6(4) . . . . ? C4 C5 C22 N1 0.9(4) . . . . ? C4 C5 C22 C17 -179.4(5) . . . . ? N7 C17 C22 N1 3.3(5) . . . . ? C41 C17 C22 N1 -172.5(5) . . . . ? N7 C17 C22 C5 -176.5(5) . . . . ? C41 C17 C22 C5 7.7(10) . . . . ? N2 C10 C23 C21 2.8(5) . . . . ? C34 C10 C23 C21 -169.2(5) . . . . ? C4 C21 C23 C10 178.6(4) . . . . ? C1 C21 C23 C10 -1.0(4) . . . . ? C7 N6 C25 C16 -1.1(5) . . . . ? Ni2 N6 C25 C16 -175.4(3) . . . . ? C7 N6 C25 C30 177.4(3) . . . . ? Ni2 N6 C25 C30 3.0(5) . . . . ? C14 C16 C25 N6 0.6(5) . . . . ? C14 C16 C25 C30 -176.9(6) . . . . ? N2 C1 C26 C39 2.1(6) . . . . ? C21 C1 C26 C39 -167.5(4) . . . . ? N2 C1 C26 C35 179.4(4) . . . . ? C21 C1 C26 C35 9.7(7) . . . . ? C39 N8 C27 C61 3.1(5) . . . . ? Ni1 N8 C27 C61 169.1(3) . . . . ? C39 N8 C27 C32 -168.5(4) . . . . ? Ni1 N8 C27 C32 -2.5(5) . . . . ? C18 C15 C28 C38 0.4(6) . . . . ? C12 C15 C28 C38 -177.4(4) . . . . ? C18 C15 C28 C60 -178.1(4) . . . . ? C12 C15 C28 C60 4.0(6) . . . . ? C38 C9 C29 C18 3.1(6) . . . . ? C48 C9 C29 C18 -174.2(4) . . . . ? C15 C18 C29 C9 -1.7(6) . . . . ? C52 C18 C29 C9 -179.3(4) . . . . ? C44 N5 C30 C56 -0.2(5) . . . . ? Ni2 N5 C30 C56 -177.2(3) . . . . ? C44 N5 C30 C25 178.2(3) . . . . ? Ni2 N5 C30 C25 1.2(5) . . . . ? N6 C25 C30 N5 -2.6(5) . . . . ? C16 C25 C30 N5 174.9(6) . . . . ? N6 C25 C30 C56 175.0(5) . . . . ? C16 C25 C30 C56 -7.6(11) . . . . ? C3 N4 C32 C58 -2.2(5) . . . . ? Ni1 N4 C32 C58 -169.2(3) . . . . ? C3 N4 C32 C27 170.4(4) . . . . ? Ni1 N4 C32 C27 3.4(5) . . . . ? N8 C27 C32 N4 -0.6(5) . . . . ? C61 C27 C32 N4 -167.5(6) . . . . ? N8 C27 C32 C58 168.1(6) . . . . ? C61 C27 C32 C58 1.2(11) . . . . ? N4 C3 C33 C58 -1.1(5) . . . . ? C36 C3 C33 C58 170.3(5) . . . . ? C20 N3 C34 C19 3.1(5) . . . . ? Ni1 N3 C34 C19 169.7(3) . . . . ? C20 N3 C34 C10 -169.8(3) . . . . ? Ni1 N3 C34 C10 -3.2(4) . . . . ? C11 C19 C34 N3 -1.6(5) . . . . ? C11 C19 C34 C10 167.7(5) . . . . ? N2 C10 C34 N3 0.0(5) . . . . ? C23 C10 C34 N3 171.9(5) . . . . ? N2 C10 C34 C19 -169.2(5) . . . . ? C23 C10 C34 C19 2.6(9) . . . . ? C54 C24 C35 C43 -0.2(6) . . . . ? C62 C24 C35 C43 -179.3(4) . . . . ? C54 C24 C35 C26 -177.8(4) . . . . ? C62 C24 C35 C26 3.2(6) . . . . ? C1 C26 C35 C24 -79.0(5) . . . . ? C39 C26 C35 C24 98.5(5) . . . . ? C1 C26 C35 C43 103.4(5) . . . . ? C39 C26 C35 C43 -79.1(5) . . . . ? N3 C20 C36 C3 -1.4(7) . . . . ? C11 C20 C36 C3 167.3(4) . . . . ? N3 C20 C36 C42 -176.8(4) . . . . ? C11 C20 C36 C42 -8.1(7) . . . . ? N4 C3 C36 C20 2.3(7) . . . . ? C33 C3 C36 C20 -168.0(5) . . . . ? N4 C3 C36 C42 177.5(4) . . . . ? C33 C3 C36 C42 7.2(8) . . . . ? C15 C28 C38 C9 1.1(6) . . . . ? C60 C28 C38 C9 179.7(4) . . . . ? C29 C9 C38 C28 -2.8(6) . . . . ? C48 C9 C38 C28 174.5(4) . . . . ? C27 N8 C39 C53 -3.1(5) . . . . ? Ni1 N8 C39 C53 -167.1(3) . . . . ? C27 N8 C39 C26 169.6(4) . . . . ? Ni1 N8 C39 C26 5.6(6) . . . . ? C1 C26 C39 N8 -2.6(6) . . . . ? C35 C26 C39 N8 179.9(4) . . . . ? C1 C26 C39 C53 168.0(4) . . . . ? C35 C26 C39 C53 -9.5(7) . . . . ? C51 C13 C40 C45 0.2(6) . . . . ? C64 C13 C40 C45 -179.1(4) . . . . ? C47 C31 C41 C17 0.0(5) . . . . ? N7 C17 C41 C31 -0.5(5) . . . . ? C22 C17 C41 C31 175.4(5) . . . . ? C20 C36 C42 C50 78.9(5) . . . . ? C3 C36 C42 C50 -96.7(5) . . . . ? C20 C36 C42 C49 -98.0(5) . . . . ? C3 C36 C42 C49 86.4(5) . . . . ? C59 C37 C43 C35 2.1(6) . . . . ? C59 C37 C43 C55 -174.1(4) . . . . ? C24 C35 C43 C37 -1.4(6) . . . . ? C26 C35 C43 C37 176.3(4) . . . . ? C24 C35 C43 C55 174.9(4) . . . . ? C26 C35 C43 C55 -7.5(6) . . . . ? C30 N5 C44 C8 -178.1(4) . . . . ? Ni2 N5 C44 C8 -1.6(6) . . . . ? C30 N5 C44 C57 0.6(5) . . . . ? Ni2 N5 C44 C57 177.1(3) . . . . ? C47 C8 C44 N5 0.3(6) . . . . ? C6 C8 C44 N5 -179.4(4) . . . . ? C47 C8 C44 C57 -177.9(4) . . . . ? C6 C8 C44 C57 2.4(7) . . . . ? C13 C40 C45 C6 -2.0(6) . . . . ? C13 C40 C45 C72 178.4(4) . . . . ? C46 C6 C45 C40 2.0(6) . . . . ? C8 C6 C45 C40 -178.8(4) . . . . ? C46 C6 C45 C72 -178.4(4) . . . . ? C8 C6 C45 C72 0.8(6) . . . . ? C45 C6 C46 C51 -0.3(6) . . . . ? C8 C6 C46 C51 -179.4(4) . . . . ? C45 C6 C46 C66 177.7(4) . . . . ? C8 C6 C46 C66 -1.4(6) . . . . ? C17 N7 C47 C8 177.4(4) . . . . ? Ni2 N7 C47 C8 5.7(6) . . . . ? C17 N7 C47 C31 -0.8(5) . . . . ? Ni2 N7 C47 C31 -172.5(3) . . . . ? C44 C8 C47 N7 -2.3(6) . . . . ? C6 C8 C47 N7 177.4(4) . . . . ? C44 C8 C47 C31 175.4(4) . . . . ? C6 C8 C47 C31 -5.0(7) . . . . ? C41 C31 C47 N7 0.5(5) . . . . ? C41 C31 C47 C8 -177.4(5) . . . . ? C50 C42 C49 C67 -2.6(6) . . . . ? C36 C42 C49 C67 174.3(4) . . . . ? C50 C42 C49 C69 176.1(4) . . . . ? C36 C42 C49 C69 -7.0(6) . . . . ? C49 C42 C50 C65 1.3(6) . . . . ? C36 C42 C50 C65 -175.6(4) . . . . ? C49 C42 C50 C68 -177.0(4) . . . . ? C36 C42 C50 C68 6.1(6) . . . . ? C6 C46 C51 C13 -1.6(7) . . . . ? C66 C46 C51 C13 -179.6(4) . . . . ? C40 C13 C51 C46 1.6(6) . . . . ? C64 C13 C51 C46 -179.0(4) . . . . ? N8 C39 C53 C61 1.9(5) . . . . ? C26 C39 C53 C61 -169.7(4) . . . . ? C35 C24 C54 C59 1.2(6) . . . . ? C62 C24 C54 C59 -179.7(4) . . . . ? N5 C30 C56 C57 -0.2(5) . . . . ? C25 C30 C56 C57 -177.8(5) . . . . ? C30 C56 C57 C44 0.6(5) . . . . ? N5 C44 C57 C56 -0.7(5) . . . . ? C8 C44 C57 C56 177.7(4) . . . . ? C3 C33 C58 C32 -0.2(5) . . . . ? N4 C32 C58 C33 1.4(5) . . . . ? C27 C32 C58 C33 -167.6(6) . . . . ? C43 C37 C59 C54 -1.1(7) . . . . ? C43 C37 C59 C71 -179.8(4) . . . . ? C24 C54 C59 C37 -0.6(7) . . . . ? C24 C54 C59 C71 178.1(4) . . . . ? C39 C53 C61 C27 -0.1(5) . . . . ? N8 C27 C61 C53 -1.8(5) . . . . ? C32 C27 C61 C53 165.3(6) . . . . ? C67 C63 C65 C50 -1.6(7) . . . . ? C70 C63 C65 C50 179.7(4) . . . . ? C42 C50 C65 C63 0.8(6) . . . . ? C68 C50 C65 C63 179.1(4) . . . . ? C65 C63 C67 C49 0.1(7) . . . . ? C70 C63 C67 C49 178.9(4) . . . . ? C42 C49 C67 C63 1.9(6) . . . . ? C69 C49 C67 C63 -176.7(4) . . . . ? Cl4 C76 C77 Cl6 -71.8(9) . . . . ? Cl4 C76 C78 Cl5 64.6(10) . . . . ?