#------------------------------------------------------------------------------ #$Date: 2020-05-13 03:55:50 +0300 (Wed, 13 May 2020) $ #$Revision: 252003 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/65/7126530.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_7126530 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 'C36 H29 N4 Ni, 2(C H Cl3)' _chemical_formula_sum 'C38 H31 Cl6 N4 Ni' _chemical_formula_weight 815.08 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 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 90 _cell_angle_beta 102.422(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 35.3376(6) _cell_length_b 11.9482(2) _cell_length_c 17.8205(3) _cell_measurement_reflns_used 12161 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 30.5210 _cell_measurement_theta_min 2.2010 _cell_volume 7348.0(2) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 93(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Rigaku VariMax Saturn' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator Confocal _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_unetI/netI 0.0338 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 29922 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.498 _diffrn_reflns_theta_min 1.804 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.96155 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.474 _exptl_crystal_description prism _exptl_crystal_F_000 3336 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.010 _refine_diff_density_max 1.864 _refine_diff_density_min -1.388 _refine_diff_density_rms 0.153 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 479 _refine_ls_number_reflns 8360 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0901 _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^)+(0.1741P)^2^+40.2173P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2524 _refine_ls_wR_factor_ref 0.2828 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6075 _reflns_number_total 8360 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc02543g2.cif _cod_data_source_block v200127_22dimer9_a _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7126530 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.825 _shelx_estimated_absorpt_t_max 0.990 _shelx_res_file ; TITL v200127_22dimer9_a.res in C2/c v200127_22dimer9_a.res created by SHELXL-2018/3 at 10:57:16 on 09-Mar-2020 REM Yadorkari-X generated CELL 0.71073 35.3376 11.9482 17.8205 90.0000 102.4220 90.0000 ZERR 8.0 0.0006 0.0002 0.0003 0.0000 0.0020 0.0000 LATT 7 SYMM -X, +Y, 1/2-Z REM SPGR C2/c monoclinic SFAC C H N Ni Cl UNIT 304 248 32 8 48 SIZE 0.20 0.10 0.01 TEMP -180.0 L.S. 30 FMAP 2 PLAN -100 ACTA CONF HTAB LIST 4 BOND $H MERG 2 OMIT -10.000000 55.000000 OMIT -10 2 4 OMIT 0 2 6 OMIT 1 1 2 OMIT -2 0 4 OMIT -6 2 2 EQIV $2 1/2-X, 1/2-Y, 1-Z HTAB C7 Cl4^a_$2 WGHT 0.174100 40.217300 FVAR 0.11873 0.61766 C1 1 0.290493 0.236387 0.167752 11.00000 0.02164 0.03108 = 0.02711 -0.00004 0.00530 -0.00175 C2 1 0.255492 0.250999 0.193543 11.00000 0.02128 0.04015 = 0.03420 0.00041 0.00777 -0.00313 AFIX 43 H1 2 0.229928 0.240028 0.164282 11.00000 -1.20000 AFIX 0 C3 1 0.265926 0.284581 0.270166 11.00000 0.02087 0.03898 = 0.03511 -0.00064 0.01023 -0.00150 AFIX 43 H2 2 0.248593 0.301274 0.302647 11.00000 -1.20000 AFIX 0 C4 1 0.307494 0.289507 0.291376 11.00000 0.02295 0.03442 = 0.03021 -0.00055 0.01211 0.00060 C5 1 0.334288 0.316695 0.359962 11.00000 0.02173 0.02687 = 0.03009 -0.00255 0.01091 0.00059 C6 1 0.375676 0.314233 0.367230 11.00000 0.02234 0.03581 = 0.02736 -0.00358 0.00789 0.00041 C7 1 0.407715 0.340236 0.428240 11.00000 0.02689 0.03247 = 0.02693 -0.00521 0.00775 0.00168 AFIX 43 H3 2 0.406367 0.363076 0.478661 11.00000 -1.20000 AFIX 0 C8 1 0.441436 0.326042 0.400441 11.00000 0.02448 0.03424 = 0.03103 -0.00224 0.00499 -0.00067 AFIX 43 H4 2 0.467227 0.337631 0.428381 11.00000 -1.20000 AFIX 0 C9 1 0.430128 0.291248 0.323058 11.00000 0.02259 0.03690 = 0.02799 -0.00362 0.00941 -0.00065 C10 1 0.445220 0.262701 0.253012 11.00000 0.02124 0.03972 = 0.02652 0.00034 0.00512 -0.00003 C11 1 0.480429 0.245071 0.226795 11.00000 0.01973 0.03762 = 0.03073 0.00422 0.00852 0.00010 C12 1 0.469442 0.216545 0.149277 11.00000 0.02295 0.04171 = 0.02527 0.00023 0.00870 0.00076 AFIX 43 H5 2 0.486598 0.200173 0.116375 11.00000 -1.20000 AFIX 0 C13 1 0.428069 0.216029 0.127543 11.00000 0.02236 0.04359 = 0.02826 -0.00343 0.01086 0.00105 C14 1 0.401194 0.185647 0.059618 11.00000 0.02486 0.03399 = 0.02175 -0.00096 0.00864 -0.00018 C15 1 0.360054 0.185774 0.052347 11.00000 0.02397 0.03210 = 0.02672 0.00009 0.00632 -0.00002 C16 1 0.328018 0.151272 -0.006415 11.00000 0.03043 0.02618 = 0.02661 -0.00133 0.00637 -0.00179 AFIX 43 H6 2 0.329381 0.124461 -0.055951 11.00000 -1.20000 AFIX 0 C17 1 0.294107 0.163968 0.021950 11.00000 0.02409 0.03113 = 0.02761 -0.00113 0.00281 -0.00417 AFIX 43 H7 2 0.268416 0.147332 -0.004570 11.00000 -1.20000 AFIX 0 C18 1 0.305562 0.206218 0.097464 11.00000 0.02232 0.02750 = 0.02951 0.00119 0.00712 0.00035 N1 3 0.320173 0.260372 0.226540 11.00000 0.02008 0.03848 = 0.02555 -0.00376 0.00673 -0.00091 N2 3 0.390910 0.285383 0.306036 11.00000 0.02092 0.04373 = 0.02509 -0.00352 0.00950 -0.00024 PART 1 N3 3 0.415546 0.245499 0.193024 11.00000 0.02271 0.05134 = 0.02307 -0.00452 0.00638 -0.00190 PART 0 N4 3 0.344480 0.218960 0.113027 11.00000 0.02067 0.03669 = 0.02826 -0.00159 0.00773 -0.00070 NI1 4 0.367797 0.254130 0.209288 11.00000 0.01685 0.04322 = 0.02394 -0.00488 0.00669 -0.00066 C19 1 0.320061 0.354120 0.429144 11.00000 0.02179 0.03147 = 0.02915 -0.00185 0.00983 0.00183 C20 1 0.318139 0.468921 0.443946 11.00000 0.02500 0.03243 = 0.03177 -0.00152 0.01171 0.00368 C21 1 0.307952 0.503273 0.512441 11.00000 0.03182 0.03365 = 0.03972 -0.00715 0.01336 0.00430 AFIX 43 H8 2 0.307090 0.580948 0.523334 11.00000 -1.20000 AFIX 0 C22 1 0.299079 0.426012 0.564793 11.00000 0.03529 0.04254 = 0.03331 -0.00464 0.01523 0.00424 C23 1 0.299777 0.313891 0.547020 11.00000 0.04149 0.03548 = 0.03557 0.00101 0.02164 0.00159 AFIX 43 H9 2 0.292856 0.260961 0.581522 11.00000 -1.20000 AFIX 0 C24 1 0.310236 0.274689 0.480373 11.00000 0.03558 0.03146 = 0.03347 -0.00255 0.01842 0.00117 C25 1 0.326077 0.554233 0.387346 11.00000 0.04494 0.03061 = 0.03854 0.00032 0.01576 0.00296 AFIX 33 H10 2 0.323399 0.629588 0.407290 11.00000 -1.50000 H11 2 0.352481 0.544182 0.379526 11.00000 -1.50000 H12 2 0.307529 0.544581 0.338298 11.00000 -1.50000 AFIX 0 C26 1 0.289741 0.466347 0.639219 11.00000 0.05839 0.03909 = 0.03991 -0.00595 0.02729 0.00416 AFIX 33 H13 2 0.290731 0.548293 0.640980 11.00000 -1.50000 H14 2 0.263717 0.441094 0.642180 11.00000 -1.50000 H15 2 0.308725 0.435782 0.682710 11.00000 -1.50000 AFIX 0 C27 1 0.310401 0.150842 0.464074 11.00000 0.05420 0.02951 = 0.04581 -0.00536 0.02734 -0.00183 AFIX 33 H16 2 0.318383 0.138386 0.415368 11.00000 -1.50000 H17 2 0.328605 0.113227 0.505683 11.00000 -1.50000 H18 2 0.284322 0.120442 0.460580 11.00000 -1.50000 AFIX 0 C28 1 0.417570 0.147464 -0.006875 11.00000 0.02040 0.04158 = 0.02103 0.00196 0.00378 0.00497 C29 1 0.429218 0.226644 -0.055495 11.00000 0.02692 0.04197 = 0.03148 0.00379 0.00935 0.00298 C30 1 0.444294 0.187078 -0.116637 11.00000 0.03509 0.05781 = 0.03277 0.01014 0.01899 0.00516 AFIX 43 H19 2 0.451778 0.239762 -0.150648 11.00000 -1.20000 AFIX 0 C31 1 0.448771 0.074965 -0.129721 11.00000 0.04666 0.05407 = 0.03462 0.00316 0.01989 0.01566 C32 1 0.437744 -0.000878 -0.080313 11.00000 0.05497 0.04321 = 0.03557 -0.00002 0.01870 0.01371 AFIX 43 H20 2 0.440648 -0.078549 -0.088989 11.00000 -1.20000 AFIX 0 C33 1 0.422427 0.032619 -0.017844 11.00000 0.03639 0.03853 = 0.02900 0.00215 0.00907 0.00789 C34 1 0.426963 0.349696 -0.041687 11.00000 0.04755 0.04040 = 0.04998 0.00290 0.02446 -0.00007 AFIX 33 H21 2 0.415713 0.362502 0.003272 11.00000 -1.50000 H22 2 0.453047 0.381999 -0.032442 11.00000 -1.50000 H23 2 0.410650 0.385214 -0.086845 11.00000 -1.50000 AFIX 0 C35 1 0.464872 0.034808 -0.197552 11.00000 0.09537 0.07396 = 0.05242 0.00618 0.04891 0.02715 AFIX 33 H24 2 0.465913 -0.047157 -0.197393 11.00000 -1.50000 H25 2 0.448062 0.060701 -0.245503 11.00000 -1.50000 H26 2 0.491022 0.064991 -0.193488 11.00000 -1.50000 AFIX 0 C36 1 0.413181 -0.052055 0.038037 11.00000 0.06264 0.04044 = 0.03629 0.00421 0.02031 0.00567 AFIX 33 H27 2 0.402765 -0.013701 0.077820 11.00000 -1.50000 H28 2 0.393921 -0.105171 0.010722 11.00000 -1.50000 H29 2 0.436834 -0.092469 0.061980 11.00000 -1.50000 AFIX 0 C37 1 0.149177 0.414706 0.229100 11.00000 0.07571 0.06532 = 0.06897 0.00438 0.02987 0.02397 AFIX 13 H30 2 0.126802 0.432877 0.186044 11.00000 -1.20000 AFIX 0 CL1 5 0.136400 0.454150 0.313738 11.00000 0.23773 0.08130 = 0.12698 -0.01985 0.13688 -0.00123 CL2 5 0.188694 0.488857 0.213456 11.00000 0.09434 0.05980 = 0.06970 -0.00190 0.03622 0.00603 CL3 5 0.156577 0.269953 0.227487 11.00000 0.05580 0.06141 = 0.06727 -0.01064 0.01949 0.00401 PART 1 CL4 5 0.105192 0.036675 0.380480 21.00000 0.10297 0.10482 = 0.11683 -0.03812 0.07389 -0.02547 CL5 5 0.025912 0.095943 0.387268 21.00000 0.12560 0.21569 = 0.06895 -0.01486 0.00825 0.10927 CL6 5 0.044433 0.053358 0.240321 21.00000 0.38903 0.07985 = 0.05692 0.01795 0.06210 0.05693 C38 1 0.052723 0.033174 0.333633 21.00000 0.12629 0.13587 = 0.03504 -0.00023 0.00688 0.03463 AFIX 13 H31 2 0.045957 -0.047562 0.337608 21.00000 -1.20000 PART 2 AFIX 0 CL7 5 0.097938 0.047164 0.245665 -21.00000 0.19499 0.08362 = 0.12589 -0.02323 0.10211 -0.02002 CL8 5 0.067574 0.220658 0.334959 -21.00000 0.36280 0.04957 = 0.08495 0.00115 0.09246 0.01718 CL9 5 0.074590 -0.004486 0.381226 -21.00000 0.33823 0.08615 = 0.13398 -0.03647 0.13825 -0.05250 C39 1 0.095033 0.101675 0.341790 -21.00000 0.04179 0.05569 = 0.06538 0.02545 0.01557 -0.01754 AFIX 13 H32 2 0.121662 0.116753 0.372833 -21.00000 -1.20000 PART 0 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM v200127_22dimer9_a.res in C2/c REM wR2 = 0.2828, GooF = S = 1.018, Restrained GooF = 1.018 for all data REM R1 = 0.0901 for 6075 Fo > 4sig(Fo) and 0.1156 for all 8360 data REM 479 parameters refined using 0 restraints END WGHT 0.1738 35.4967 REM Instructions for potential hydrogen bonds HTAB C7 Cl4_$2 HTAB C7 Cl9_$2 REM Highest difference peak 1.864, deepest hole -1.388, 1-sigma level 0.153 Q1 1 0.1847 0.4351 0.3487 11.00000 0.05 1.71 Q2 1 0.1584 0.4254 0.2903 11.00000 0.05 0.98 Q3 1 0.4540 -0.3317 0.1407 11.00000 0.05 0.87 Q4 1 0.4818 -0.4810 0.1348 11.00000 0.05 0.86 Q5 1 0.4126 -0.4712 0.1625 11.00000 0.05 0.74 Q6 1 0.1445 0.3086 0.2822 11.00000 0.05 0.74 Q7 1 0.1591 0.4803 0.1982 11.00000 0.05 0.71 Q8 1 0.3144 0.3259 0.4488 11.00000 0.05 0.64 Q9 1 0.2926 0.2341 0.1442 11.00000 0.05 0.61 Q10 1 0.2608 0.2560 0.2296 11.00000 0.05 0.61 Q11 1 0.3049 0.4581 0.5413 11.00000 0.05 0.60 Q12 1 0.4749 0.2473 0.1806 11.00000 0.05 0.59 Q13 1 0.4224 0.2350 0.1549 11.00000 0.05 0.58 Q14 1 0.3030 0.1039 0.5009 11.00000 0.05 0.58 Q15 1 0.4228 0.1835 -0.0360 11.00000 0.05 0.57 Q16 1 0.3907 0.2647 0.2948 11.00000 0.05 0.56 Q17 1 0.4531 -0.4088 0.1865 11.00000 0.05 0.56 Q18 1 0.3815 0.3040 0.3371 11.00000 0.05 0.56 Q19 1 0.3118 0.4846 0.4782 11.00000 0.05 0.56 Q20 1 0.2905 0.1313 0.4176 11.00000 0.05 0.55 Q21 1 0.3306 0.1368 0.4513 11.00000 0.05 0.54 Q22 1 0.4303 -0.0369 0.0890 11.00000 0.05 0.53 Q23 1 0.4095 0.3584 -0.0311 11.00000 0.05 0.53 Q24 1 0.3214 0.4985 0.4179 11.00000 0.05 0.51 Q25 1 0.4506 -0.0195 -0.2212 11.00000 0.05 0.51 Q26 1 0.4318 -0.0350 -0.0872 11.00000 0.05 0.50 Q27 1 0.2864 0.4173 0.6569 11.00000 0.05 0.49 Q28 1 0.4213 -0.1342 0.0213 11.00000 0.05 0.49 Q29 1 0.4676 0.0976 -0.2282 11.00000 0.05 0.49 Q30 1 0.4360 0.3168 0.3569 11.00000 0.05 0.48 Q31 1 0.3159 0.4235 0.4273 11.00000 0.05 0.48 Q32 1 0.4371 0.0437 -0.1133 11.00000 0.05 0.47 Q33 1 0.3031 0.2998 0.5110 11.00000 0.05 0.47 Q34 1 0.4404 0.0917 -0.1418 11.00000 0.05 0.47 Q35 1 0.3078 0.2049 0.4682 11.00000 0.05 0.46 Q36 1 0.3796 -0.0454 0.0442 11.00000 0.05 0.46 Q37 1 0.4089 0.1740 0.0272 11.00000 0.05 0.46 Q38 1 0.4145 -0.4438 0.2000 11.00000 0.05 0.45 Q39 1 0.4514 0.0360 -0.1872 11.00000 0.05 0.45 Q40 1 0.2940 0.4392 0.5929 11.00000 0.05 0.44 Q41 1 0.3288 0.3278 0.3875 11.00000 0.05 0.44 Q42 1 0.3017 0.1805 0.0561 11.00000 0.05 0.44 Q43 1 0.4223 0.3138 0.4255 11.00000 0.05 0.43 Q44 1 0.4418 -0.4454 0.2575 11.00000 0.05 0.43 Q45 1 0.3081 0.1604 0.0123 11.00000 0.05 0.42 Q46 1 0.2648 0.5226 0.6174 11.00000 0.05 0.42 Q47 1 0.4433 -0.3120 0.2011 11.00000 0.05 0.42 Q48 1 0.4473 0.3733 0.0087 11.00000 0.05 0.42 Q49 1 0.4261 0.2497 0.3091 11.00000 0.05 0.39 Q50 1 0.4458 -0.4248 0.1315 11.00000 0.05 0.39 Q51 1 0.4340 0.3871 -0.0832 11.00000 0.05 0.38 Q52 1 0.4460 0.2176 0.1332 11.00000 0.05 0.38 Q53 1 0.3094 0.5034 0.6735 11.00000 0.05 0.38 Q54 1 0.4237 0.0231 -0.0445 11.00000 0.05 0.38 Q55 1 0.3901 0.3293 0.3938 11.00000 0.05 0.37 Q56 1 0.4890 0.0010 -0.1819 11.00000 0.05 0.33 Q57 1 0.4127 -0.3556 0.1847 11.00000 0.05 0.31 Q58 1 0.3826 0.1870 0.0612 11.00000 0.05 0.31 Q59 1 0.4631 0.0956 -0.1026 11.00000 0.05 0.29 Q60 1 0.1807 0.2683 0.2810 11.00000 0.05 0.29 Q61 1 0.3999 0.2268 -0.1308 11.00000 0.05 0.27 Q62 1 0.2631 0.2628 0.5373 11.00000 0.05 0.24 Q63 1 0.1904 0.4359 0.1581 11.00000 0.05 0.24 Q64 1 0.4161 -0.5085 0.1129 11.00000 0.05 0.24 Q65 1 0.4592 -0.1616 0.1312 11.00000 0.05 0.23 Q66 1 0.3115 0.4940 0.2896 11.00000 0.05 0.23 Q67 1 0.1649 0.3570 0.2618 11.00000 0.05 0.22 Q68 1 0.1746 0.5831 0.2212 11.00000 0.05 0.22 Q69 1 0.2004 0.4991 0.2803 11.00000 0.05 0.22 Q70 1 0.3068 0.5539 0.3737 11.00000 0.05 0.22 Q71 1 0.2185 0.2987 0.1530 11.00000 0.05 0.21 Q72 1 0.4862 -0.2957 0.1273 11.00000 0.05 0.21 Q73 1 0.3656 -0.4611 0.1843 11.00000 0.05 0.21 Q74 1 0.2100 0.5590 0.2486 11.00000 0.05 0.21 Q75 1 0.4375 -0.1340 -0.0951 11.00000 0.05 0.21 Q76 1 0.3000 0.6170 0.5225 11.00000 0.05 0.21 Q77 1 0.4869 0.2277 0.0941 11.00000 0.05 0.21 Q78 1 0.3971 -0.3666 0.1032 11.00000 0.05 0.21 Q79 1 0.4919 0.2985 0.3340 11.00000 0.05 0.20 Q80 1 0.3177 0.0843 -0.0502 11.00000 0.05 0.20 Q81 1 0.4779 -0.0938 0.0989 11.00000 0.05 0.20 Q82 1 0.2490 0.5512 0.6481 11.00000 0.05 0.19 Q83 1 0.5019 -0.2642 0.1419 11.00000 0.05 0.19 Q84 1 0.4727 -0.0347 -0.0541 11.00000 0.05 0.19 Q85 1 0.4421 0.4402 -0.1264 11.00000 0.05 0.19 Q86 1 0.2507 0.3200 0.3170 11.00000 0.05 0.19 Q87 1 0.2948 0.5627 0.3398 11.00000 0.05 0.19 Q88 1 0.4623 -0.0660 -0.0742 11.00000 0.05 0.19 Q89 1 0.5195 0.0570 -0.1975 11.00000 0.05 0.18 Q90 1 0.4146 0.0213 -0.1863 11.00000 0.05 0.18 Q91 1 0.1913 0.2866 0.2372 11.00000 0.05 0.18 Q92 1 0.4459 0.5017 -0.1311 11.00000 0.05 0.18 Q93 1 0.4168 -0.4171 0.0948 11.00000 0.05 0.18 Q94 1 0.3017 0.0239 0.0054 11.00000 0.05 0.18 Q95 1 0.4845 -0.5069 0.0582 11.00000 0.05 0.18 Q96 1 0.3188 0.0273 0.0545 11.00000 0.05 0.18 Q97 1 0.1721 0.3488 0.3200 11.00000 0.05 0.17 Q98 1 0.3948 -0.3184 0.1271 11.00000 0.05 0.17 Q99 1 0.4987 0.2668 0.1534 11.00000 0.05 0.17 Q100 1 0.1907 0.2214 0.1648 11.00000 0.05 0.17 ; _shelx_res_checksum 71380 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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_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 C1 C 0.29049(12) 0.2364(4) 0.1678(3) 0.0266(9) Uani 1 1 d . . . . . C2 C 0.25549(13) 0.2510(4) 0.1935(3) 0.0316(10) Uani 1 1 d . . . . . H1 H 0.229928 0.240028 0.164282 0.038 Uiso 1 1 calc R U . . . C3 C 0.26593(12) 0.2846(4) 0.2702(3) 0.0310(9) Uani 1 1 d . . . . . H2 H 0.248593 0.301274 0.302647 0.037 Uiso 1 1 calc R U . . . C4 C 0.30749(12) 0.2895(4) 0.2914(3) 0.0282(9) Uani 1 1 d . . . . . C5 C 0.33429(12) 0.3167(3) 0.3600(2) 0.0254(8) Uani 1 1 d . . . . . C6 C 0.37568(12) 0.3142(4) 0.3672(2) 0.0281(9) Uani 1 1 d . . . . . C7 C 0.40772(12) 0.3402(4) 0.4282(3) 0.0285(9) Uani 1 1 d . . . . . H3 H 0.406367 0.363076 0.478661 0.034 Uiso 1 1 calc R U . . . C8 C 0.44144(13) 0.3260(4) 0.4004(3) 0.0301(9) Uani 1 1 d . . . . . H4 H 0.467227 0.337631 0.428381 0.036 Uiso 1 1 calc R U . . . C9 C 0.43013(12) 0.2912(4) 0.3231(3) 0.0286(9) Uani 1 1 d . . . . . C10 C 0.44522(12) 0.2627(4) 0.2530(3) 0.0292(9) Uani 1 1 d . . . . . C11 C 0.48043(12) 0.2451(4) 0.2268(3) 0.0289(9) Uani 1 1 d . . . . . C12 C 0.46944(12) 0.2165(4) 0.1493(3) 0.0294(9) Uani 1 1 d . . . . . H5 H 0.486598 0.200173 0.116375 0.035 Uiso 1 1 calc R U . . . C13 C 0.42807(12) 0.2160(4) 0.1275(3) 0.0306(9) Uani 1 1 d . . . . . C14 C 0.40119(12) 0.1856(4) 0.0596(2) 0.0263(8) Uani 1 1 d . . . . . C15 C 0.36005(12) 0.1858(4) 0.0523(2) 0.0275(9) Uani 1 1 d . . . . . C16 C 0.32802(13) 0.1513(3) -0.0064(2) 0.0277(9) Uani 1 1 d . . . . . H6 H 0.329381 0.124461 -0.055951 0.033 Uiso 1 1 calc R U . . . C17 C 0.29411(12) 0.1640(4) 0.0219(2) 0.0280(9) Uani 1 1 d . . . . . H7 H 0.268416 0.147332 -0.004570 0.034 Uiso 1 1 calc R U . . . C18 C 0.30556(12) 0.2062(4) 0.0975(2) 0.0262(8) Uani 1 1 d . . . . . N1 N 0.32017(10) 0.2604(3) 0.2265(2) 0.0278(8) Uani 1 1 d . . . . . N2 N 0.39091(10) 0.2854(3) 0.3060(2) 0.0292(8) Uani 1 1 d . . . . . N3 N 0.41555(11) 0.2455(3) 0.1930(2) 0.0322(9) Uani 1 1 d . . . A 1 N4 N 0.34448(10) 0.2190(3) 0.1130(2) 0.0282(8) Uani 1 1 d . . . . . Ni1 Ni 0.36780(2) 0.25413(5) 0.20929(3) 0.0277(2) Uani 1 1 d . . . . . C19 C 0.32006(12) 0.3541(4) 0.4291(2) 0.0268(9) Uani 1 1 d . . . . . C20 C 0.31814(12) 0.4689(4) 0.4439(3) 0.0289(9) Uani 1 1 d . . . . . C21 C 0.30795(13) 0.5033(4) 0.5124(3) 0.0342(10) Uani 1 1 d . . . . . H8 H 0.307090 0.580948 0.523334 0.041 Uiso 1 1 calc R U . . . C22 C 0.29908(14) 0.4260(4) 0.5648(3) 0.0359(10) Uani 1 1 d . . . . . C23 C 0.29978(14) 0.3139(4) 0.5470(3) 0.0355(10) Uani 1 1 d . . . . . H9 H 0.292856 0.260961 0.581522 0.043 Uiso 1 1 calc R U . . . C24 C 0.31024(14) 0.2747(4) 0.4804(3) 0.0319(10) Uani 1 1 d . . . . . C25 C 0.32608(15) 0.5542(4) 0.3873(3) 0.0370(10) Uani 1 1 d . . . . . H10 H 0.323399 0.629588 0.407290 0.056 Uiso 1 1 calc R U . . . H11 H 0.352481 0.544182 0.379526 0.056 Uiso 1 1 calc R U . . . H12 H 0.307529 0.544581 0.338298 0.056 Uiso 1 1 calc R U . . . C26 C 0.28974(17) 0.4663(4) 0.6392(3) 0.0433(12) Uani 1 1 d . . . . . H13 H 0.290731 0.548293 0.640980 0.065 Uiso 1 1 calc R U . . . H14 H 0.263717 0.441094 0.642180 0.065 Uiso 1 1 calc R U . . . H15 H 0.308725 0.435782 0.682710 0.065 Uiso 1 1 calc R U . . . C27 C 0.31040(16) 0.1508(4) 0.4641(3) 0.0407(12) Uani 1 1 d . . . . . H16 H 0.318383 0.138386 0.415368 0.061 Uiso 1 1 calc R U . . . H17 H 0.328605 0.113227 0.505683 0.061 Uiso 1 1 calc R U . . . H18 H 0.284322 0.120442 0.460580 0.061 Uiso 1 1 calc R U . . . C28 C 0.41757(12) 0.1475(4) -0.0069(2) 0.0278(9) Uani 1 1 d . . . . . C29 C 0.42922(13) 0.2266(4) -0.0555(3) 0.0330(10) Uani 1 1 d . . . . . C30 C 0.44429(14) 0.1871(5) -0.1166(3) 0.0401(11) Uani 1 1 d . . . . . H19 H 0.451778 0.239762 -0.150648 0.048 Uiso 1 1 calc R U . . . C31 C 0.44877(16) 0.0750(5) -0.1297(3) 0.0434(12) Uani 1 1 d . . . . . C32 C 0.43774(16) -0.0009(5) -0.0803(3) 0.0432(12) Uani 1 1 d . . . . . H20 H 0.440648 -0.078549 -0.088989 0.052 Uiso 1 1 calc R U . . . C33 C 0.42243(14) 0.0326(4) -0.0178(3) 0.0343(10) Uani 1 1 d . . . . . C34 C 0.42696(16) 0.3497(4) -0.0417(3) 0.0439(12) Uani 1 1 d . . . . . H21 H 0.415713 0.362502 0.003272 0.066 Uiso 1 1 calc R U . . . H22 H 0.453047 0.381999 -0.032442 0.066 Uiso 1 1 calc R U . . . H23 H 0.410650 0.385214 -0.086845 0.066 Uiso 1 1 calc R U . . . C35 C 0.4649(2) 0.0348(6) -0.1976(4) 0.069(2) Uani 1 1 d . . . . . H24 H 0.465913 -0.047157 -0.197393 0.103 Uiso 1 1 calc R U . . . H25 H 0.448062 0.060701 -0.245503 0.103 Uiso 1 1 calc R U . . . H26 H 0.491022 0.064991 -0.193488 0.103 Uiso 1 1 calc R U . . . C36 C 0.41318(18) -0.0521(5) 0.0380(3) 0.0450(12) Uani 1 1 d . . . . . H27 H 0.402765 -0.013701 0.077820 0.068 Uiso 1 1 calc R U . . . H28 H 0.393921 -0.105171 0.010722 0.068 Uiso 1 1 calc R U . . . H29 H 0.436834 -0.092469 0.061980 0.068 Uiso 1 1 calc R U . . . C37 C 0.1492(2) 0.4147(6) 0.2291(4) 0.0678(19) Uani 1 1 d . . . . . H30 H 0.126802 0.432877 0.186044 0.081 Uiso 1 1 calc R U . . . Cl1 Cl 0.13640(12) 0.4541(2) 0.31374(18) 0.1340(14) Uani 1 1 d . . . . . Cl2 Cl 0.18869(6) 0.48886(15) 0.21346(11) 0.0718(5) Uani 1 1 d . . . . . Cl3 Cl 0.15658(5) 0.26995(14) 0.22749(11) 0.0606(4) Uani 1 1 d . . . . . Cl4 Cl 0.10519(13) 0.0367(4) 0.3805(3) 0.1006(16) Uani 0.618(5) 1 d . . P B 1 Cl5 Cl 0.02591(15) 0.0959(5) 0.3873(2) 0.139(3) Uani 0.618(5) 1 d . . P B 1 Cl6 Cl 0.0444(3) 0.0534(4) 0.2403(2) 0.173(4) Uani 0.618(5) 1 d . . P B 1 C38 C 0.0527(5) 0.0332(18) 0.3336(8) 0.101(6) Uani 0.618(5) 1 d . . P B 1 H31 H 0.045957 -0.047562 0.337608 0.121 Uiso 0.618(5) 1 calc R U P B 1 Cl7 Cl 0.0979(3) 0.0472(6) 0.2457(5) 0.125(3) Uani 0.382(5) 1 d . . P B 2 Cl8 Cl 0.0676(4) 0.2207(5) 0.3350(4) 0.159(5) Uani 0.382(5) 1 d . . P B 2 Cl9 Cl 0.0746(5) -0.0045(7) 0.3812(7) 0.173(7) Uani 0.382(5) 1 d . . P B 2 C39 C 0.0950(5) 0.1017(15) 0.3418(11) 0.054(4) Uani 0.382(5) 1 d . . P B 2 H32 H 0.121662 0.116753 0.372833 0.064 Uiso 0.382(5) 1 calc R U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0216(19) 0.031(2) 0.027(2) 0.0000(16) 0.0053(16) -0.0017(15) C2 0.021(2) 0.040(2) 0.034(2) 0.0004(18) 0.0078(17) -0.0031(17) C3 0.021(2) 0.039(2) 0.035(2) -0.0006(19) 0.0102(17) -0.0015(17) C4 0.023(2) 0.034(2) 0.030(2) -0.0005(18) 0.0121(17) 0.0006(17) C5 0.0217(19) 0.027(2) 0.030(2) -0.0025(16) 0.0109(16) 0.0006(15) C6 0.022(2) 0.036(2) 0.027(2) -0.0036(17) 0.0079(16) 0.0004(16) C7 0.027(2) 0.032(2) 0.027(2) -0.0052(17) 0.0078(17) 0.0017(17) C8 0.024(2) 0.034(2) 0.031(2) -0.0022(18) 0.0050(17) -0.0007(17) C9 0.023(2) 0.037(2) 0.028(2) -0.0036(18) 0.0094(16) -0.0007(17) C10 0.021(2) 0.040(2) 0.027(2) 0.0003(18) 0.0051(17) 0.0000(16) C11 0.020(2) 0.038(2) 0.031(2) 0.0042(17) 0.0085(18) 0.0001(16) C12 0.023(2) 0.042(2) 0.025(2) 0.0002(18) 0.0087(16) 0.0008(17) C13 0.022(2) 0.044(2) 0.028(2) -0.0034(19) 0.0109(17) 0.0011(18) C14 0.025(2) 0.034(2) 0.022(2) -0.0010(16) 0.0086(16) -0.0002(16) C15 0.024(2) 0.032(2) 0.027(2) 0.0001(17) 0.0063(16) 0.0000(16) C16 0.030(2) 0.026(2) 0.027(2) -0.0013(16) 0.0064(17) -0.0018(16) C17 0.024(2) 0.031(2) 0.028(2) -0.0011(17) 0.0028(16) -0.0042(16) C18 0.0223(19) 0.027(2) 0.030(2) 0.0012(17) 0.0071(16) 0.0003(16) N1 0.0201(17) 0.038(2) 0.0255(18) -0.0038(15) 0.0067(14) -0.0009(14) N2 0.0209(17) 0.044(2) 0.0251(18) -0.0035(16) 0.0095(14) -0.0002(15) N3 0.0227(18) 0.051(2) 0.0231(19) -0.0045(16) 0.0064(14) -0.0019(15) N4 0.0207(17) 0.0367(19) 0.0283(19) -0.0016(15) 0.0077(14) -0.0007(14) Ni1 0.0169(3) 0.0432(4) 0.0239(3) -0.0049(2) 0.0067(2) -0.0007(2) C19 0.0218(19) 0.031(2) 0.029(2) -0.0019(17) 0.0098(16) 0.0018(16) C20 0.025(2) 0.032(2) 0.032(2) -0.0015(18) 0.0117(17) 0.0037(16) C21 0.032(2) 0.034(2) 0.040(3) -0.0071(19) 0.0134(19) 0.0043(18) C22 0.035(2) 0.043(3) 0.033(2) -0.005(2) 0.0152(19) 0.004(2) C23 0.041(3) 0.035(2) 0.036(3) 0.0010(19) 0.022(2) 0.0016(19) C24 0.036(2) 0.031(2) 0.033(2) -0.0026(18) 0.0184(19) 0.0012(18) C25 0.045(3) 0.031(2) 0.039(3) 0.0003(19) 0.016(2) 0.0030(19) C26 0.058(3) 0.039(3) 0.040(3) -0.006(2) 0.027(2) 0.004(2) C27 0.054(3) 0.030(2) 0.046(3) -0.005(2) 0.027(2) -0.002(2) C28 0.0204(19) 0.042(2) 0.021(2) 0.0020(17) 0.0038(15) 0.0050(17) C29 0.027(2) 0.042(3) 0.031(2) 0.0038(19) 0.0094(18) 0.0030(18) C30 0.035(2) 0.058(3) 0.033(3) 0.010(2) 0.019(2) 0.005(2) C31 0.047(3) 0.054(3) 0.035(3) 0.003(2) 0.020(2) 0.016(2) C32 0.055(3) 0.043(3) 0.036(3) 0.000(2) 0.019(2) 0.014(2) C33 0.036(2) 0.039(2) 0.029(2) 0.0021(19) 0.0091(19) 0.0079(19) C34 0.048(3) 0.040(3) 0.050(3) 0.003(2) 0.024(2) 0.000(2) C35 0.095(5) 0.074(4) 0.052(4) 0.006(3) 0.049(4) 0.027(4) C36 0.063(3) 0.040(3) 0.036(3) 0.004(2) 0.020(2) 0.006(2) C37 0.076(5) 0.065(4) 0.069(4) 0.004(3) 0.030(4) 0.024(4) Cl1 0.238(4) 0.0813(15) 0.127(2) -0.0198(15) 0.137(3) -0.0012(18) Cl2 0.0943(14) 0.0598(10) 0.0697(11) -0.0019(8) 0.0362(10) 0.0060(9) Cl3 0.0558(9) 0.0614(9) 0.0673(10) -0.0106(7) 0.0195(8) 0.0040(7) Cl4 0.103(3) 0.105(3) 0.117(3) -0.038(3) 0.074(3) -0.025(2) Cl5 0.126(4) 0.216(6) 0.069(2) -0.015(3) 0.008(2) 0.109(4) Cl6 0.389(11) 0.080(3) 0.057(2) 0.0180(19) 0.062(4) 0.057(4) C38 0.126(14) 0.136(15) 0.035(7) 0.000(8) 0.007(7) 0.035(11) Cl7 0.195(9) 0.084(4) 0.126(6) -0.023(4) 0.102(6) -0.020(5) Cl8 0.363(16) 0.050(3) 0.085(5) 0.001(3) 0.092(7) 0.017(5) Cl9 0.34(2) 0.086(5) 0.134(8) -0.036(5) 0.138(11) -0.053(8) C39 0.042(8) 0.056(9) 0.065(10) 0.025(8) 0.016(7) -0.018(7) 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 N1 C1 C2 108.0(4) . . ? N1 C1 C18 110.1(4) . . ? C2 C1 C18 141.9(4) . . ? C3 C2 C1 106.7(4) . . ? C3 C2 H1 126.7 . . ? C1 C2 H1 126.7 . . ? C2 C3 C4 108.0(4) . . ? C2 C3 H2 126.0 . . ? C4 C3 H2 126.0 . . ? N1 C4 C5 120.5(4) . . ? N1 C4 C3 105.6(4) . . ? C5 C4 C3 133.9(4) . . ? C4 C5 C6 123.5(4) . . ? C4 C5 C19 120.0(4) . . ? C6 C5 C19 116.5(4) . . ? N2 C6 C7 106.3(4) . . ? N2 C6 C5 120.2(4) . . ? C7 C6 C5 133.5(4) . . ? C8 C7 C6 107.6(4) . . ? C8 C7 H3 126.2 . . ? C6 C7 H3 126.2 . . ? C7 C8 C9 107.4(4) . . ? C7 C8 H4 126.3 . . ? C9 C8 H4 126.3 . . ? N2 C9 C8 107.1(4) . . ? N2 C9 C10 109.4(4) . . ? C8 C9 C10 143.4(4) . . ? N3 C10 C11 107.6(4) . . ? N3 C10 C9 109.9(4) . . ? C11 C10 C9 142.5(4) . . ? C12 C11 C10 106.4(4) . . ? C12 C11 C11 126.4(5) . 2_655 ? C10 C11 C11 127.0(5) . 2_655 ? C11 C12 C13 108.7(4) . . ? C11 C12 H5 125.7 . . ? C13 C12 H5 125.7 . . ? N3 C13 C14 120.7(4) . . ? N3 C13 C12 105.4(4) . . ? C14 C13 C12 133.8(4) . . ? C13 C14 C15 124.0(4) . . ? C13 C14 C28 116.9(4) . . ? C15 C14 C28 119.1(4) . . ? N4 C15 C16 105.8(4) . . ? N4 C15 C14 120.0(4) . . ? C16 C15 C14 134.1(4) . . ? C17 C16 C15 107.9(4) . . ? C17 C16 H6 126.0 . . ? C15 C16 H6 126.0 . . ? C16 C17 C18 106.8(4) . . ? C16 C17 H7 126.6 . . ? C18 C17 H7 126.6 . . ? N4 C18 C17 107.8(4) . . ? N4 C18 C1 109.2(4) . . ? C17 C18 C1 142.9(4) . . ? C1 N1 C4 111.7(4) . . ? C1 N1 Ni1 117.8(3) . . ? C4 N1 Ni1 130.5(3) . . ? C9 N2 C6 111.7(4) . . ? C9 N2 Ni1 117.5(3) . . ? C6 N2 Ni1 130.6(3) . . ? C10 N3 C13 112.0(4) . . ? C10 N3 Ni1 117.9(3) . . ? C13 N3 Ni1 129.9(3) . . ? C18 N4 C15 111.6(4) . . ? C18 N4 Ni1 117.5(3) . . ? C15 N4 Ni1 130.1(3) . . ? N3 Ni1 N1 178.93(18) . . ? N3 Ni1 N2 85.19(17) . . ? N1 Ni1 N2 94.47(16) . . ? N3 Ni1 N4 95.04(17) . . ? N1 Ni1 N4 85.27(17) . . ? N2 Ni1 N4 178.45(18) . . ? C20 C19 C24 120.5(4) . . ? C20 C19 C5 119.1(4) . . ? C24 C19 C5 120.3(4) . . ? C19 C20 C21 118.8(4) . . ? C19 C20 C25 120.9(4) . . ? C21 C20 C25 120.3(4) . . ? C22 C21 C20 121.6(4) . . ? C22 C21 H8 119.2 . . ? C20 C21 H8 119.2 . . ? C23 C22 C21 118.2(4) . . ? C23 C22 C26 122.0(5) . . ? C21 C22 C26 119.9(4) . . ? C22 C23 C24 122.8(4) . . ? C22 C23 H9 118.6 . . ? C24 C23 H9 118.6 . . ? C23 C24 C19 118.1(4) . . ? C23 C24 C27 120.3(4) . . ? C19 C24 C27 121.6(4) . . ? C20 C25 H10 109.5 . . ? C20 C25 H11 109.5 . . ? H10 C25 H11 109.5 . . ? C20 C25 H12 109.5 . . ? H10 C25 H12 109.5 . . ? H11 C25 H12 109.5 . . ? C22 C26 H13 109.5 . . ? C22 C26 H14 109.5 . . ? H13 C26 H14 109.5 . . ? C22 C26 H15 109.5 . . ? H13 C26 H15 109.5 . . ? H14 C26 H15 109.5 . . ? C24 C27 H16 109.5 . . ? C24 C27 H17 109.5 . . ? H16 C27 H17 109.5 . . ? C24 C27 H18 109.5 . . ? H16 C27 H18 109.5 . . ? H17 C27 H18 109.5 . . ? C33 C28 C29 120.9(4) . . ? C33 C28 C14 119.2(4) . . ? C29 C28 C14 119.9(4) . . ? C30 C29 C28 117.8(5) . . ? C30 C29 C34 120.3(5) . . ? C28 C29 C34 121.9(4) . . ? C31 C30 C29 122.7(5) . . ? C31 C30 H19 118.7 . . ? C29 C30 H19 118.7 . . ? C30 C31 C32 118.3(4) . . ? C30 C31 C35 121.3(5) . . ? C32 C31 C35 120.4(5) . . ? C31 C32 C33 122.2(5) . . ? C31 C32 H20 118.9 . . ? C33 C32 H20 118.9 . . ? C32 C33 C28 118.1(4) . . ? C32 C33 C36 120.8(5) . . ? C28 C33 C36 121.0(4) . . ? C29 C34 H21 109.5 . . ? C29 C34 H22 109.5 . . ? H21 C34 H22 109.5 . . ? C29 C34 H23 109.5 . . ? H21 C34 H23 109.5 . . ? H22 C34 H23 109.5 . . ? C31 C35 H24 109.5 . . ? C31 C35 H25 109.5 . . ? H24 C35 H25 109.5 . . ? C31 C35 H26 109.5 . . ? H24 C35 H26 109.5 . . ? H25 C35 H26 109.5 . . ? C33 C36 H27 109.5 . . ? C33 C36 H28 109.5 . . ? H27 C36 H28 109.5 . . ? C33 C36 H29 109.5 . . ? H27 C36 H29 109.5 . . ? H28 C36 H29 109.5 . . ? Cl2 C37 Cl1 111.9(5) . . ? Cl2 C37 Cl3 112.1(4) . . ? Cl1 C37 Cl3 110.6(4) . . ? Cl2 C37 H30 107.3 . . ? Cl1 C37 H30 107.3 . . ? Cl3 C37 H30 107.3 . . ? Cl6 C38 Cl5 121.1(10) . . ? Cl6 C38 Cl4 113.2(12) . . ? Cl5 C38 Cl4 111.6(8) . . ? Cl6 C38 H31 102.7 . . ? Cl5 C38 H31 102.7 . . ? Cl4 C38 H31 102.7 . . ? Cl9 C39 Cl8 111.6(11) . . ? Cl9 C39 Cl7 103.6(10) . . ? Cl8 C39 Cl7 111.7(10) . . ? Cl9 C39 H32 110.0 . . ? Cl8 C39 H32 110.0 . . ? Cl7 C39 H32 110.0 . . ? 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 C1 N1 1.344(6) . ? C1 C2 1.420(6) . ? C1 C18 1.506(6) . ? C2 C3 1.395(7) . ? C2 H1 0.9500 . ? C3 C4 1.437(6) . ? C3 H2 0.9500 . ? C4 N1 1.371(6) . ? C4 C5 1.414(6) . ? C5 C6 1.441(6) . ? C5 C19 1.496(6) . ? C6 N2 1.360(5) . ? C6 C7 1.425(6) . ? C7 C8 1.396(6) . ? C7 H3 0.9500 . ? C8 C9 1.413(6) . ? C8 H4 0.9500 . ? C9 N2 1.355(5) . ? C9 C10 1.498(6) . ? C10 N3 1.343(6) . ? C10 C11 1.436(6) . ? C11 C12 1.394(6) . ? C11 C11 1.451(8) 2_655 ? C12 C13 1.430(6) . ? C12 H5 0.9500 . ? C13 N3 1.380(6) . ? C13 C14 1.416(6) . ? C14 C15 1.432(6) . ? C14 C28 1.497(6) . ? C15 N4 1.373(6) . ? C15 C16 1.428(6) . ? C16 C17 1.405(6) . ? C16 H6 0.9500 . ? C17 C18 1.413(6) . ? C17 H7 0.9500 . ? C18 N4 1.352(5) . ? N1 Ni1 1.776(4) . ? N2 Ni1 1.781(4) . ? N3 Ni1 1.775(4) . ? N4 Ni1 1.786(4) . ? C19 C20 1.401(6) . ? C19 C24 1.411(6) . ? C20 C21 1.406(6) . ? C20 C25 1.502(6) . ? C21 C22 1.395(7) . ? C21 H8 0.9500 . ? C22 C23 1.378(7) . ? C22 C26 1.513(6) . ? C23 C24 1.398(6) . ? C23 H9 0.9500 . ? C24 C27 1.508(6) . ? C25 H10 0.9800 . ? C25 H11 0.9800 . ? C25 H12 0.9800 . ? C26 H13 0.9800 . ? C26 H14 0.9800 . ? C26 H15 0.9800 . ? C27 H16 0.9800 . ? C27 H17 0.9800 . ? C27 H18 0.9800 . ? C28 C33 1.402(7) . ? C28 C29 1.403(6) . ? C29 C30 1.394(7) . ? C29 C34 1.496(7) . ? C30 C31 1.375(8) . ? C30 H19 0.9500 . ? C31 C32 1.377(8) . ? C31 C35 1.520(7) . ? C32 C33 1.397(7) . ? C32 H20 0.9500 . ? C33 C36 1.504(7) . ? C34 H21 0.9800 . ? C34 H22 0.9800 . ? C34 H23 0.9800 . ? C35 H24 0.9800 . ? C35 H25 0.9800 . ? C35 H26 0.9800 . ? C36 H27 0.9800 . ? C36 H28 0.9800 . ? C36 H29 0.9800 . ? C37 Cl2 1.726(8) . ? C37 Cl1 1.730(7) . ? C37 Cl3 1.750(7) . ? C37 H30 1.0000 . ? Cl4 C38 1.863(19) . ? Cl5 C38 1.662(17) . ? Cl6 C38 1.643(14) . ? C38 H31 1.0000 . ? Cl7 C39 1.86(2) . ? Cl8 C39 1.71(2) . ? Cl9 C39 1.686(16) . ? C39 H32 1.0000 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C7 H3 Cl4^a 0.95 2.89 3.829(6) 170.5 7_556 yes 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 N1 C1 C2 C3 0.0(5) . . . . ? C18 C1 C2 C3 -178.1(5) . . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? C2 C3 C4 N1 0.8(5) . . . . ? C2 C3 C4 C5 -179.4(5) . . . . ? N1 C4 C5 C6 -1.0(7) . . . . ? C3 C4 C5 C6 179.3(5) . . . . ? N1 C4 C5 C19 176.8(4) . . . . ? C3 C4 C5 C19 -2.9(8) . . . . ? C4 C5 C6 N2 0.5(7) . . . . ? C19 C5 C6 N2 -177.4(4) . . . . ? C4 C5 C6 C7 178.1(5) . . . . ? C19 C5 C6 C7 0.2(7) . . . . ? N2 C6 C7 C8 0.2(5) . . . . ? C5 C6 C7 C8 -177.7(5) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 N2 0.1(5) . . . . ? C7 C8 C9 C10 177.0(6) . . . . ? N2 C9 C10 N3 3.2(5) . . . . ? C8 C9 C10 N3 -173.7(6) . . . . ? N2 C9 C10 C11 -175.3(6) . . . . ? C8 C9 C10 C11 7.8(12) . . . . ? N3 C10 C11 C12 -0.3(5) . . . . ? C9 C10 C11 C12 178.3(6) . . . . ? N3 C10 C11 C11 -174.3(3) . . . 2_655 ? C9 C10 C11 C11 4.2(8) . . . 2_655 ? C10 C11 C12 C13 -0.2(5) . . . . ? C11 C11 C12 C13 173.9(3) 2_655 . . . ? C11 C12 C13 N3 0.6(5) . . . . ? C11 C12 C13 C14 -174.3(5) . . . . ? N3 C13 C14 C15 1.8(7) . . . . ? C12 C13 C14 C15 176.0(5) . . . . ? N3 C13 C14 C28 -176.0(4) . . . . ? C12 C13 C14 C28 -1.7(8) . . . . ? C13 C14 C15 N4 1.4(7) . . . . ? C28 C14 C15 N4 179.1(4) . . . . ? C13 C14 C15 C16 -174.3(5) . . . . ? C28 C14 C15 C16 3.4(8) . . . . ? N4 C15 C16 C17 -0.7(5) . . . . ? C14 C15 C16 C17 175.4(5) . . . . ? C15 C16 C17 C18 0.1(5) . . . . ? C16 C17 C18 N4 0.5(5) . . . . ? C16 C17 C18 C1 -175.1(6) . . . . ? N1 C1 C18 N4 -3.8(5) . . . . ? C2 C1 C18 N4 174.2(6) . . . . ? N1 C1 C18 C17 171.7(6) . . . . ? C2 C1 C18 C17 -10.3(11) . . . . ? C2 C1 N1 C4 0.6(5) . . . . ? C18 C1 N1 C4 179.3(4) . . . . ? C2 C1 N1 Ni1 -177.7(3) . . . . ? C18 C1 N1 Ni1 1.0(5) . . . . ? C5 C4 N1 C1 179.3(4) . . . . ? C3 C4 N1 C1 -0.9(5) . . . . ? C5 C4 N1 Ni1 -2.7(7) . . . . ? C3 C4 N1 Ni1 177.1(3) . . . . ? C8 C9 N2 C6 0.1(5) . . . . ? C10 C9 N2 C6 -178.0(4) . . . . ? C8 C9 N2 Ni1 175.1(3) . . . . ? C10 C9 N2 Ni1 -3.0(5) . . . . ? C7 C6 N2 C9 -0.2(5) . . . . ? C5 C6 N2 C9 178.0(4) . . . . ? C7 C6 N2 Ni1 -174.4(3) . . . . ? C5 C6 N2 Ni1 3.9(7) . . . . ? C11 C10 N3 C13 0.7(5) . . . . ? C9 C10 N3 C13 -178.4(4) . . . . ? C11 C10 N3 Ni1 176.7(3) . . . . ? C9 C10 N3 Ni1 -2.3(5) . . . . ? C14 C13 N3 C10 174.9(4) . . . . ? C12 C13 N3 C10 -0.8(5) . . . . ? C14 C13 N3 Ni1 -0.5(7) . . . . ? C12 C13 N3 Ni1 -176.2(3) . . . . ? C17 C18 N4 C15 -1.0(5) . . . . ? C1 C18 N4 C15 176.2(4) . . . . ? C17 C18 N4 Ni1 -172.0(3) . . . . ? C1 C18 N4 Ni1 5.1(5) . . . . ? C16 C15 N4 C18 1.1(5) . . . . ? C14 C15 N4 C18 -175.7(4) . . . . ? C16 C15 N4 Ni1 170.7(3) . . . . ? C14 C15 N4 Ni1 -6.1(6) . . . . ? C10 N3 Ni1 N2 0.7(4) . . . . ? C13 N3 Ni1 N2 175.9(5) . . . . ? C10 N3 Ni1 N4 -177.8(4) . . . . ? C13 N3 Ni1 N4 -2.6(5) . . . . ? C1 N1 Ni1 N2 -177.1(3) . . . . ? C4 N1 Ni1 N2 5.0(4) . . . . ? C1 N1 Ni1 N4 1.4(3) . . . . ? C4 N1 Ni1 N4 -176.5(4) . . . . ? C9 N2 Ni1 N3 1.5(4) . . . . ? C6 N2 Ni1 N3 175.4(5) . . . . ? C9 N2 Ni1 N1 -179.5(4) . . . . ? C6 N2 Ni1 N1 -5.6(5) . . . . ? C18 N4 Ni1 N3 175.1(3) . . . . ? C15 N4 Ni1 N3 6.0(4) . . . . ? C18 N4 Ni1 N1 -3.9(3) . . . . ? C15 N4 Ni1 N1 -173.0(4) . . . . ? C4 C5 C19 C20 -97.2(5) . . . . ? C6 C5 C19 C20 80.8(5) . . . . ? C4 C5 C19 C24 85.4(5) . . . . ? C6 C5 C19 C24 -96.6(5) . . . . ? C24 C19 C20 C21 2.9(7) . . . . ? C5 C19 C20 C21 -174.6(4) . . . . ? C24 C19 C20 C25 -176.1(4) . . . . ? C5 C19 C20 C25 6.5(6) . . . . ? C19 C20 C21 C22 -1.2(7) . . . . ? C25 C20 C21 C22 177.7(5) . . . . ? C20 C21 C22 C23 -1.3(7) . . . . ? C20 C21 C22 C26 177.7(5) . . . . ? C21 C22 C23 C24 2.2(8) . . . . ? C26 C22 C23 C24 -176.7(5) . . . . ? C22 C23 C24 C19 -0.7(8) . . . . ? C22 C23 C24 C27 -179.9(5) . . . . ? C20 C19 C24 C23 -1.9(7) . . . . ? C5 C19 C24 C23 175.5(4) . . . . ? C20 C19 C24 C27 177.3(4) . . . . ? C5 C19 C24 C27 -5.3(7) . . . . ? C13 C14 C28 C33 95.1(5) . . . . ? C15 C14 C28 C33 -82.7(5) . . . . ? C13 C14 C28 C29 -82.4(5) . . . . ? C15 C14 C28 C29 99.7(5) . . . . ? C33 C28 C29 C30 2.5(7) . . . . ? C14 C28 C29 C30 180.0(4) . . . . ? C33 C28 C29 C34 -175.6(5) . . . . ? C14 C28 C29 C34 1.9(7) . . . . ? C28 C29 C30 C31 -1.3(8) . . . . ? C34 C29 C30 C31 176.8(5) . . . . ? C29 C30 C31 C32 0.2(8) . . . . ? C29 C30 C31 C35 179.3(6) . . . . ? C30 C31 C32 C33 -0.2(9) . . . . ? C35 C31 C32 C33 -179.3(6) . . . . ? C31 C32 C33 C28 1.3(8) . . . . ? C31 C32 C33 C36 -175.9(5) . . . . ? C29 C28 C33 C32 -2.5(7) . . . . ? C14 C28 C33 C32 180.0(4) . . . . ? C29 C28 C33 C36 174.7(5) . . . . ? C14 C28 C33 C36 -2.8(7) . . . . ?