#------------------------------------------------------------------------------ #$Date: 2026-05-26 23:51:50 +0100 (Tue, 26 May 2026) $ #$Revision: 306097 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721055.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_7721055 loop_ _publ_author_name 'Killian, Lars' 'Olarte Loyo, Anne' 'De Ridder, Roy R.P.A.M.' 'Lutz, Martin' 'Thevenon, Arnaud' _publ_section_title ; Synthesis and Characterisation of Novel Dipyridine and Pyridinyl Benzoquinoline Complexes of Zinc and Nickel ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00659K _journal_year 2026 _chemical_formula_moiety 'C64 H68 Cl2 N4 Ni, 6(C H2 Cl2)' _chemical_formula_sum 'C70 H80 Cl14 N4 Ni' _chemical_formula_weight 1532.39 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2025-10-16 deposited with the CCDC. 2026-05-25 downloaded from the CCDC. ; _cell_angle_alpha 102.479(1) _cell_angle_beta 93.579(2) _cell_angle_gamma 108.074(1) _cell_formula_units_Z 1 _cell_length_a 9.0227(3) _cell_length_b 12.0364(4) _cell_length_c 18.7791(5) _cell_measurement_reflns_used 34858 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.55 _cell_measurement_theta_min 1.11 _cell_volume 1874.49(10) _computing_cell_refinement Peakref _computing_data_collection Apex3 _computing_data_reduction 'Eval15, Sadabs' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution SHELXT _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker Kappa ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_unetI/netI 0.0248 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 50304 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.503 _diffrn_reflns_theta_min 1.122 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_T_max 0.9598 _exptl_absorpt_correction_T_min 0.7563 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour 'light green' _exptl_crystal_density_diffrn 1.357 _exptl_crystal_description block _exptl_crystal_F_000 794 _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _refine_diff_density_max 1.172 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 447 _refine_ls_number_reflns 8627 _refine_ls_number_restraints 157 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0461 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+2.1783P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1249 _refine_ls_wR_factor_ref 0.1297 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7288 _reflns_number_total 8627 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00659k2.cif _cod_data_source_block l1347a _cod_original_cell_volume 1874.50(10) _cod_database_code 7721055 _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 l1347a l1347a.res created by SHELXL-2018/3 at 09:54:15 on 10-Nov-2023 CELL 0.71073 9.02274 12.03645 18.77910 102.479 93.579 108.074 ZERR 1 0.00031 0.00041 0.00046 0.001 0.002 0.001 LATT 1 SFAC C H Cl N Ni UNIT 70 80 14 4 1 TEMP -123 L.S. 15 FMAP 2 PLAN -20 ACTA CONF BOND $H SADI 0.01 C33 CL2 C33 CL3 = C34 CL4 C34 CL5A C34 CL5B = C35A CL6A C35A CL7A C35B CL6B C35B CL7B SADI 0.02 CL2 CL3 CL4 CL5A CL4 CL5B CL6A CL7A CL6B CL7B ISOR 0.01 CL2 > C35B RIGU CL2 > C35B WGHT 0.066300 2.178300 FVAR 0.53786 0.36236 0.75665 NI1 5 0.500000 0.500000 0.500000 10.50000 0.01289 0.01862 = 0.01209 0.00556 0.00218 0.00634 CL1 3 0.286721 0.413806 0.397163 11.00000 0.01542 0.02752 = 0.01578 0.00740 0.00144 0.00637 N1 4 0.544222 0.677087 0.487088 11.00000 0.01526 0.02147 = 0.01433 0.00436 0.00048 0.00734 N2 4 0.673214 0.491763 0.431026 11.00000 0.01502 0.01964 = 0.01456 0.00521 0.00091 0.00641 C1 1 0.544684 0.764283 0.546097 11.00000 0.02107 0.02623 = 0.01642 0.00356 0.00177 0.01024 AFIX 43 H1 2 0.516310 0.741797 0.590124 11.00000 -1.20000 AFIX 0 C2 1 0.584392 0.884637 0.545622 11.00000 0.02917 0.02212 = 0.02126 -0.00071 -0.00018 0.01123 AFIX 43 H2 2 0.579374 0.942877 0.587695 11.00000 -1.20000 AFIX 0 C3 1 0.631728 0.918508 0.482362 11.00000 0.02590 0.01840 = 0.03061 0.00572 -0.00079 0.00780 AFIX 43 H3 2 0.661677 1.000745 0.480673 11.00000 -1.20000 AFIX 0 C4 1 0.634638 0.830982 0.421981 11.00000 0.02076 0.02035 = 0.01985 0.00725 0.00110 0.00510 AFIX 43 H4 2 0.668913 0.852733 0.378563 11.00000 -1.20000 AFIX 0 C5 1 0.586773 0.709658 0.424921 11.00000 0.01397 0.01910 = 0.01556 0.00493 0.00064 0.00629 C6 1 0.589036 0.614449 0.359363 11.00000 0.01594 0.01829 = 0.01562 0.00708 0.00434 0.00606 C7 1 0.688695 0.539830 0.372223 11.00000 0.01454 0.01773 = 0.01300 0.00280 0.00038 0.00387 C8 1 0.805506 0.531344 0.327687 11.00000 0.01750 0.02329 = 0.01638 0.00604 0.00358 0.00530 AFIX 43 H8 2 0.813117 0.564391 0.285928 11.00000 -1.20000 AFIX 0 C9 1 0.909623 0.474592 0.344876 11.00000 0.01606 0.02588 = 0.02151 0.00270 0.00584 0.00669 AFIX 43 H9 2 0.989173 0.467821 0.315040 11.00000 -1.20000 AFIX 0 C10 1 0.896235 0.427700 0.406304 11.00000 0.01560 0.02389 = 0.02368 0.00457 0.00074 0.00921 AFIX 43 H10 2 0.967207 0.389283 0.419823 11.00000 -1.20000 AFIX 0 C11 1 0.777128 0.438114 0.447497 11.00000 0.01908 0.02356 = 0.01791 0.00735 0.00154 0.00895 AFIX 43 H11 2 0.768113 0.405801 0.489545 11.00000 -1.20000 AFIX 0 C12 1 0.519408 0.606394 0.292002 11.00000 0.01694 0.02009 = 0.01585 0.00755 0.00414 0.00600 C13 1 0.422398 0.683388 0.279618 11.00000 0.02090 0.02125 = 0.01459 0.00538 -0.00001 0.00840 C14 1 0.286682 0.674629 0.312409 11.00000 0.02166 0.02525 = 0.02012 0.01134 0.00258 0.00829 AFIX 43 H14 2 0.260918 0.624999 0.345955 11.00000 -1.20000 AFIX 0 C15 1 0.187869 0.737778 0.296684 11.00000 0.02040 0.02940 = 0.02506 0.00966 0.00401 0.00962 AFIX 43 H15 2 0.095819 0.730168 0.319846 11.00000 -1.20000 AFIX 0 C16 1 0.220476 0.811660 0.247965 11.00000 0.02463 0.02370 = 0.02127 0.00645 -0.00169 0.01054 C17 1 0.359445 0.822737 0.217563 11.00000 0.03608 0.03614 = 0.02932 0.02199 0.00980 0.01744 AFIX 43 H17 2 0.386875 0.874507 0.185310 11.00000 -1.20000 AFIX 0 C18 1 0.459283 0.760970 0.232638 11.00000 0.03038 0.03881 = 0.02826 0.02022 0.01205 0.01805 AFIX 43 H18 2 0.553436 0.771316 0.210952 11.00000 -1.20000 AFIX 0 C19 1 0.510952 0.507888 0.225800 11.00000 0.01796 0.02484 = 0.01333 0.00560 -0.00018 0.00874 C20 1 0.432620 0.388637 0.225095 11.00000 0.04016 0.02551 = 0.01831 0.00805 0.00879 0.00913 AFIX 43 H20 2 0.393473 0.369599 0.268331 11.00000 -1.20000 AFIX 0 C21 1 0.410286 0.296148 0.162038 11.00000 0.04704 0.02311 = 0.02224 0.00728 0.00677 0.00817 AFIX 43 H21 2 0.355399 0.215375 0.163179 11.00000 -1.20000 AFIX 0 C22 1 0.466383 0.319098 0.097369 11.00000 0.03479 0.02656 = 0.01531 0.00361 0.00144 0.01386 C23 1 0.548667 0.438472 0.099159 11.00000 0.03869 0.03119 = 0.01574 0.00717 0.00806 0.01105 AFIX 43 H23 2 0.591285 0.457086 0.056497 11.00000 -1.20000 AFIX 0 C24 1 0.570451 0.531530 0.161622 11.00000 0.02984 0.02411 = 0.01777 0.00657 0.00408 0.00458 AFIX 43 H24 2 0.626475 0.612185 0.160663 11.00000 -1.20000 AFIX 0 C25 1 0.110650 0.878566 0.226622 11.00000 0.03025 0.03051 = 0.02990 0.01104 -0.00312 0.01574 C26 1 0.193013 1.014766 0.254649 11.00000 0.04166 0.03168 = 0.06154 0.01258 -0.00594 0.01740 AFIX 137 H26A 2 0.212386 1.036386 0.308598 11.00000 -1.50000 H26B 2 0.125954 1.057159 0.238049 11.00000 -1.50000 H26C 2 0.293475 1.038026 0.235260 11.00000 -1.50000 AFIX 0 C27 1 -0.043918 0.843797 0.258538 11.00000 0.03071 0.05134 = 0.07571 0.03210 0.00830 0.02444 AFIX 137 H27A 2 -0.100438 0.757323 0.238969 11.00000 -1.50000 H27B 2 -0.108838 0.889807 0.244810 11.00000 -1.50000 H27C 2 -0.021714 0.861937 0.312327 11.00000 -1.50000 AFIX 0 C28 1 0.071781 0.846763 0.142370 11.00000 0.07089 0.07127 = 0.03449 0.01044 -0.01257 0.04639 AFIX 137 H28A 2 0.168976 0.873308 0.120863 11.00000 -1.50000 H28B 2 -0.000316 0.887407 0.128609 11.00000 -1.50000 H28C 2 0.021881 0.759278 0.123875 11.00000 -1.50000 AFIX 0 C29 1 0.440597 0.219039 0.026893 11.00000 0.05641 0.02873 = 0.01726 0.00091 0.00103 0.01800 C30 1 0.598671 0.202777 0.011842 11.00000 0.10142 0.11107 = 0.05922 -0.03621 -0.00680 0.07384 AFIX 137 H30A 2 0.644707 0.183007 0.054090 11.00000 -1.50000 H30B 2 0.670412 0.277749 0.004103 11.00000 -1.50000 H30C 2 0.581904 0.137184 -0.032286 11.00000 -1.50000 AFIX 0 C31 1 0.330552 0.099571 0.032624 11.00000 0.20084 0.03368 = 0.04599 -0.01194 0.04857 -0.01679 AFIX 137 H31A 2 0.368174 0.079219 0.076573 11.00000 -1.50000 H31B 2 0.326891 0.036994 -0.011258 11.00000 -1.50000 H31C 2 0.224845 0.104612 0.036293 11.00000 -1.50000 AFIX 0 C32 1 0.379065 0.253369 -0.039024 11.00000 0.12512 0.05019 = 0.02633 -0.00816 -0.02755 0.04349 AFIX 137 H32A 2 0.359425 0.187031 -0.083020 11.00000 -1.50000 H32B 2 0.457191 0.325975 -0.046278 11.00000 -1.50000 H32C 2 0.280719 0.269338 -0.030472 11.00000 -1.50000 AFIX 0 CL2 3 0.972090 0.209814 0.527482 11.00000 0.05395 0.06522 = 0.04018 -0.00685 -0.00432 -0.00388 CL3 3 0.862774 0.108077 0.371408 11.00000 0.06243 0.03522 = 0.03531 0.00974 0.00578 0.00583 C33 1 1.024131 0.155811 0.441620 11.00000 0.03408 0.04419 = 0.05730 0.01999 0.01143 0.01091 AFIX 23 H33A 2 1.061813 0.087390 0.443532 11.00000 -1.20000 H33B 2 1.111227 0.220425 0.430336 11.00000 -1.20000 AFIX 0 CL4 3 -0.061421 0.483312 0.144186 11.00000 0.04861 0.05518 = 0.04040 0.01007 0.01395 0.01485 PART 1 CL5A 3 0.119052 0.412856 0.036491 21.00000 0.17269 0.21363 = 0.09722 0.00053 0.03829 0.15594 PART 2 CL5B 3 0.149762 0.458812 0.036796 -21.00000 0.07206 0.27083 = 0.04868 0.04679 0.02939 0.09829 PART 0 C34 1 0.129628 0.488994 0.127397 11.00000 0.03872 0.06740 = 0.05577 0.00945 -0.00037 0.01516 PART 1 AFIX 23 H34A 2 0.198784 0.573905 0.136069 21.00000 -1.20000 H34B 2 0.173897 0.450557 0.160961 21.00000 -1.20000 PART 2 AFIX 23 H34C 2 0.203791 0.570352 0.152080 -21.00000 -1.20000 H34D 2 0.159284 0.430165 0.149698 -21.00000 -1.20000 AFIX 0 PART 3 CL6A 3 0.664371 0.073697 0.202567 31.00000 0.09020 0.07824 = 0.09828 0.04386 -0.03077 -0.01817 CL7A 3 0.948816 0.166498 0.140376 31.00000 0.08845 0.08303 = 0.10204 0.02701 -0.01146 0.03951 C35A 1 0.823712 0.200425 0.202869 31.00000 0.09789 0.03771 = 0.05427 0.01054 -0.00479 -0.00415 AFIX 23 H35A 2 0.883839 0.233901 0.253016 31.00000 -1.20000 H35B 2 0.784457 0.262810 0.190025 31.00000 -1.20000 AFIX 0 PART 4 CL6B 3 0.679406 0.062960 0.193000 -31.00000 0.27408 0.02599 = 0.14459 -0.01636 -0.09287 0.00304 CL7B 3 0.980015 0.221881 0.191448 -31.00000 0.17957 0.18824 = 0.25366 0.12052 0.05580 0.12207 C35B 1 0.790830 0.214928 0.211505 -31.00000 0.08870 0.05868 = 0.07722 -0.00207 -0.00241 0.03619 AFIX 23 H35C 2 0.794995 0.254813 0.263901 -31.00000 -1.20000 H35D 2 0.744227 0.255824 0.180490 -31.00000 -1.20000 AFIX 0 HKLF 4 REM l1347a REM wR2 = 0.1297, GooF = S = 1.037, Restrained GooF = 1.073 for all data REM R1 = 0.0461 for 7288 Fo > 4sig(Fo) and 0.0557 for all 8627 data REM 447 parameters refined using 157 restraints END WGHT 0.0663 2.1777 REM Highest difference peak 1.172, deepest hole -0.639, 1-sigma level 0.073 Q1 1 0.5950 0.1693 0.2701 11.00000 0.05 1.17 Q2 1 0.9786 0.1605 0.5450 11.00000 0.05 0.78 Q3 1 0.8471 0.1097 0.1581 11.00000 0.05 0.75 Q4 1 0.8915 0.2200 0.5262 11.00000 0.05 0.69 Q5 1 0.1951 0.5453 0.0716 11.00000 0.05 0.55 Q6 1 0.0227 0.2810 0.0697 11.00000 0.05 0.42 Q7 1 0.6386 0.5794 0.3662 11.00000 0.05 0.40 Q8 1 1.0078 0.2377 0.5296 11.00000 0.05 0.39 Q9 1 0.1687 0.8478 0.2383 11.00000 0.05 0.38 Q10 1 0.5927 0.7665 0.4203 11.00000 0.05 0.37 Q11 1 0.4739 0.6450 0.2829 11.00000 0.05 0.37 Q12 1 0.5018 0.1410 0.0349 11.00000 0.05 0.37 Q13 1 0.3692 0.1088 0.0371 11.00000 0.05 0.36 Q14 1 0.2400 0.7001 0.2996 11.00000 0.05 0.35 Q15 1 0.5498 0.7214 0.5108 11.00000 0.05 0.33 Q16 1 0.2238 0.1434 0.0281 11.00000 0.05 0.33 Q17 1 0.5646 0.8245 0.5380 11.00000 0.05 0.33 Q18 1 0.3552 0.6710 0.2945 11.00000 0.05 0.32 Q19 1 0.5056 0.5530 0.2612 11.00000 0.05 0.32 Q20 1 0.4583 0.2704 0.0672 11.00000 0.05 0.32 ; _shelx_res_checksum 56779 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 0.500000 0.500000 0.500000 0.01397(10) Uani 1 2 d S . P . . Cl1 Cl 0.28672(6) 0.41381(5) 0.39716(3) 0.01946(12) Uani 1 1 d . . . . . N1 N 0.5442(2) 0.67709(16) 0.48709(9) 0.0168(3) Uani 1 1 d . . . . . N2 N 0.6732(2) 0.49176(16) 0.43103(9) 0.0161(3) Uani 1 1 d . . . . . C1 C 0.5447(3) 0.7643(2) 0.54610(12) 0.0210(4) Uani 1 1 d . . . . . H1 H 0.516310 0.741797 0.590124 0.025 Uiso 1 1 calc R U . . . C2 C 0.5844(3) 0.8846(2) 0.54562(13) 0.0247(5) Uani 1 1 d . . . . . H2 H 0.579374 0.942877 0.587695 0.030 Uiso 1 1 calc R U . . . C3 C 0.6317(3) 0.9185(2) 0.48236(13) 0.0251(5) Uani 1 1 d . . . . . H3 H 0.661677 1.000745 0.480673 0.030 Uiso 1 1 calc R U . . . C4 C 0.6346(3) 0.83098(19) 0.42198(12) 0.0204(4) Uani 1 1 d . . . . . H4 H 0.668913 0.852733 0.378563 0.025 Uiso 1 1 calc R U . . . C5 C 0.5868(2) 0.70966(18) 0.42492(11) 0.0160(4) Uani 1 1 d . . . . . C6 C 0.5890(2) 0.61445(18) 0.35936(11) 0.0160(4) Uani 1 1 d . . . . . C7 C 0.6887(2) 0.53983(18) 0.37222(11) 0.0157(4) Uani 1 1 d . . . . . C8 C 0.8055(2) 0.53134(19) 0.32769(12) 0.0192(4) Uani 1 1 d . . . . . H8 H 0.813117 0.564391 0.285928 0.023 Uiso 1 1 calc R U . . . C9 C 0.9096(2) 0.4746(2) 0.34488(12) 0.0216(4) Uani 1 1 d . . . . . H9 H 0.989173 0.467821 0.315040 0.026 Uiso 1 1 calc R U . . . C10 C 0.8962(2) 0.4277(2) 0.40630(12) 0.0207(4) Uani 1 1 d . . . . . H10 H 0.967207 0.389283 0.419823 0.025 Uiso 1 1 calc R U . . . C11 C 0.7771(2) 0.43811(19) 0.44750(12) 0.0194(4) Uani 1 1 d . . . . . H11 H 0.768113 0.405801 0.489545 0.023 Uiso 1 1 calc R U . . . C12 C 0.5194(2) 0.60639(19) 0.29200(11) 0.0171(4) Uani 1 1 d . . . . . C13 C 0.4224(3) 0.68339(19) 0.27962(11) 0.0185(4) Uani 1 1 d . . . . . C14 C 0.2867(3) 0.6746(2) 0.31241(12) 0.0213(4) Uani 1 1 d . . . . . H14 H 0.260918 0.624999 0.345955 0.026 Uiso 1 1 calc R U . . . C15 C 0.1879(3) 0.7378(2) 0.29668(13) 0.0241(5) Uani 1 1 d . . . . . H15 H 0.095819 0.730168 0.319846 0.029 Uiso 1 1 calc R U . . . C16 C 0.2205(3) 0.8117(2) 0.24796(13) 0.0227(4) Uani 1 1 d . . . . . C17 C 0.3594(3) 0.8227(2) 0.21756(14) 0.0301(5) Uani 1 1 d . . . . . H17 H 0.386875 0.874507 0.185310 0.036 Uiso 1 1 calc R U . . . C18 C 0.4593(3) 0.7610(2) 0.23264(14) 0.0286(5) Uani 1 1 d . . . . . H18 H 0.553436 0.771316 0.210952 0.034 Uiso 1 1 calc R U . . . C19 C 0.5110(2) 0.5079(2) 0.22580(11) 0.0183(4) Uani 1 1 d . . . . . C20 C 0.4326(3) 0.3886(2) 0.22510(13) 0.0278(5) Uani 1 1 d . . . . . H20 H 0.393473 0.369599 0.268331 0.033 Uiso 1 1 calc R U . . . C21 C 0.4103(3) 0.2961(2) 0.16204(13) 0.0313(5) Uani 1 1 d . . . . . H21 H 0.355399 0.215375 0.163179 0.038 Uiso 1 1 calc R U . . . C22 C 0.4664(3) 0.3191(2) 0.09737(12) 0.0250(5) Uani 1 1 d . . . . . C23 C 0.5487(3) 0.4385(2) 0.09916(13) 0.0283(5) Uani 1 1 d . . . . . H23 H 0.591285 0.457086 0.056497 0.034 Uiso 1 1 calc R U . . . C24 C 0.5705(3) 0.5315(2) 0.16162(12) 0.0247(5) Uani 1 1 d . . . . . H24 H 0.626475 0.612185 0.160663 0.030 Uiso 1 1 calc R U . . . C25 C 0.1106(3) 0.8786(2) 0.22662(14) 0.0286(5) Uani 1 1 d . . . . . C26 C 0.1930(4) 1.0148(3) 0.25465(19) 0.0442(7) Uani 1 1 d . . . . . H26A H 0.212386 1.036386 0.308598 0.066 Uiso 1 1 calc R U . . . H26B H 0.125954 1.057159 0.238049 0.066 Uiso 1 1 calc R U . . . H26C H 0.293475 1.038026 0.235260 0.066 Uiso 1 1 calc R U . . . C27 C -0.0439(3) 0.8438(3) 0.2585(2) 0.0473(8) Uani 1 1 d . . . . . H27A H -0.100438 0.757323 0.238969 0.071 Uiso 1 1 calc R U . . . H27B H -0.108838 0.889807 0.244810 0.071 Uiso 1 1 calc R U . . . H27C H -0.021714 0.861937 0.312327 0.071 Uiso 1 1 calc R U . . . C28 C 0.0718(5) 0.8468(4) 0.14237(17) 0.0548(9) Uani 1 1 d . . . . . H28A H 0.168976 0.873308 0.120863 0.082 Uiso 1 1 calc R U . . . H28B H -0.000316 0.887407 0.128609 0.082 Uiso 1 1 calc R U . . . H28C H 0.021881 0.759278 0.123875 0.082 Uiso 1 1 calc R U . . . C29 C 0.4406(4) 0.2190(2) 0.02689(13) 0.0342(6) Uani 1 1 d . . . . . C30 C 0.5987(6) 0.2028(5) 0.0118(2) 0.0915(17) Uani 1 1 d . . . . . H30A H 0.644707 0.183007 0.054090 0.137 Uiso 1 1 calc R U . . . H30B H 0.670412 0.277749 0.004103 0.137 Uiso 1 1 calc R U . . . H30C H 0.581904 0.137184 -0.032286 0.137 Uiso 1 1 calc R U . . . C31 C 0.3306(8) 0.0996(3) 0.0326(2) 0.109(2) Uani 1 1 d . . . . . H31A H 0.368174 0.079219 0.076573 0.163 Uiso 1 1 calc R U . . . H31B H 0.326891 0.036994 -0.011258 0.163 Uiso 1 1 calc R U . . . H31C H 0.224845 0.104612 0.036293 0.163 Uiso 1 1 calc R U . . . C32 C 0.3791(6) 0.2534(3) -0.03902(18) 0.0684(12) Uani 1 1 d . . . . . H32A H 0.359425 0.187031 -0.083020 0.103 Uiso 1 1 calc R U . . . H32B H 0.457191 0.325975 -0.046278 0.103 Uiso 1 1 calc R U . . . H32C H 0.280719 0.269338 -0.030472 0.103 Uiso 1 1 calc R U . . . Cl2 Cl 0.97209(11) 0.20981(9) 0.52748(5) 0.0625(3) Uani 1 1 d D U . . . Cl3 Cl 0.86277(10) 0.10808(7) 0.37141(4) 0.04669(19) Uani 1 1 d D U . . . C33 C 1.0241(3) 0.1558(3) 0.44162(16) 0.0443(7) Uani 1 1 d D U . . . H33A H 1.061813 0.087390 0.443532 0.053 Uiso 1 1 calc R U . . . H33B H 1.111227 0.220425 0.430336 0.053 Uiso 1 1 calc R U . . . Cl4 Cl -0.06142(10) 0.48331(8) 0.14419(4) 0.04857(19) Uani 1 1 d D U . . . Cl5A Cl 0.1191(18) 0.4129(17) 0.0365(4) 0.145(4) Uani 0.36(2) 1 d D U P A 1 Cl5B Cl 0.1498(6) 0.4588(10) 0.03680(16) 0.119(2) Uani 0.64(2) 1 d D U P A 2 C34 C 0.1296(4) 0.4890(4) 0.12740(18) 0.0558(9) Uani 1 1 d D U . . . H34A H 0.198784 0.573905 0.136069 0.067 Uiso 0.36(2) 1 calc R U P A 1 H34B H 0.173897 0.450557 0.160961 0.067 Uiso 0.36(2) 1 calc R U P A 1 H34C H 0.203791 0.570352 0.152080 0.067 Uiso 0.64(2) 1 calc R U P A 2 H34D H 0.159284 0.430165 0.149698 0.067 Uiso 0.64(2) 1 calc R U P A 2 Cl6A Cl 0.6644(3) 0.0737(3) 0.2026(2) 0.0984(11) Uani 0.757(9) 1 d D U P B 3 Cl7A Cl 0.9488(3) 0.1665(2) 0.14038(16) 0.0890(9) Uani 0.757(9) 1 d D U P B 3 C35A C 0.8237(9) 0.2004(5) 0.2029(5) 0.070(2) Uani 0.757(9) 1 d D U P B 3 H35A H 0.883839 0.233901 0.253016 0.085 Uiso 0.757(9) 1 calc R U P B 3 H35B H 0.784457 0.262810 0.190025 0.085 Uiso 0.757(9) 1 calc R U P B 3 Cl6B Cl 0.6794(19) 0.0630(9) 0.1930(9) 0.171(6) Uani 0.243(9) 1 d D U P B 4 Cl7B Cl 0.9800(17) 0.2219(17) 0.1914(14) 0.181(7) Uani 0.243(9) 1 d D U P B 4 C35B C 0.791(2) 0.2149(11) 0.212(3) 0.076(8) Uani 0.243(9) 1 d D U P B 4 H35C H 0.794995 0.254813 0.263901 0.091 Uiso 0.243(9) 1 calc R U P B 4 H35D H 0.744227 0.255824 0.180490 0.091 Uiso 0.243(9) 1 calc R U P B 4 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 0.01289(17) 0.01862(19) 0.01209(18) 0.00556(14) 0.00218(13) 0.00634(14) Cl1 0.0154(2) 0.0275(3) 0.0158(2) 0.00740(19) 0.00144(17) 0.00637(19) N1 0.0153(8) 0.0215(9) 0.0143(8) 0.0044(7) 0.0005(6) 0.0073(7) N2 0.0150(8) 0.0196(8) 0.0146(8) 0.0052(7) 0.0009(6) 0.0064(7) C1 0.0211(10) 0.0262(11) 0.0164(10) 0.0036(8) 0.0018(8) 0.0102(9) C2 0.0292(12) 0.0221(11) 0.0213(11) -0.0007(9) -0.0002(9) 0.0112(9) C3 0.0259(11) 0.0184(10) 0.0306(12) 0.0057(9) -0.0008(9) 0.0078(9) C4 0.0208(10) 0.0203(10) 0.0198(10) 0.0072(8) 0.0011(8) 0.0051(8) C5 0.0140(9) 0.0191(10) 0.0156(9) 0.0049(8) 0.0006(7) 0.0063(7) C6 0.0159(9) 0.0183(9) 0.0156(9) 0.0071(8) 0.0043(7) 0.0061(8) C7 0.0145(9) 0.0177(9) 0.0130(9) 0.0028(7) 0.0004(7) 0.0039(7) C8 0.0175(10) 0.0233(10) 0.0164(10) 0.0060(8) 0.0036(8) 0.0053(8) C9 0.0161(10) 0.0259(11) 0.0215(11) 0.0027(9) 0.0058(8) 0.0067(8) C10 0.0156(9) 0.0239(11) 0.0237(11) 0.0046(9) 0.0007(8) 0.0092(8) C11 0.0191(10) 0.0236(10) 0.0179(10) 0.0074(8) 0.0015(8) 0.0089(8) C12 0.0169(9) 0.0201(10) 0.0159(10) 0.0075(8) 0.0041(8) 0.0060(8) C13 0.0209(10) 0.0212(10) 0.0146(10) 0.0054(8) 0.0000(8) 0.0084(8) C14 0.0217(10) 0.0252(11) 0.0201(11) 0.0113(9) 0.0026(8) 0.0083(9) C15 0.0204(10) 0.0294(12) 0.0251(11) 0.0097(9) 0.0040(9) 0.0096(9) C16 0.0246(11) 0.0237(11) 0.0213(11) 0.0064(9) -0.0017(8) 0.0105(9) C17 0.0361(13) 0.0361(13) 0.0293(13) 0.0220(11) 0.0098(10) 0.0174(11) C18 0.0304(12) 0.0388(14) 0.0283(12) 0.0202(11) 0.0121(10) 0.0180(11) C19 0.0180(10) 0.0248(11) 0.0133(9) 0.0056(8) -0.0002(7) 0.0087(8) C20 0.0402(14) 0.0255(11) 0.0183(11) 0.0081(9) 0.0088(10) 0.0091(10) C21 0.0470(15) 0.0231(11) 0.0222(12) 0.0073(9) 0.0068(11) 0.0082(11) C22 0.0348(12) 0.0266(11) 0.0153(10) 0.0036(9) 0.0014(9) 0.0139(10) C23 0.0387(13) 0.0312(12) 0.0157(11) 0.0072(9) 0.0081(9) 0.0110(10) C24 0.0298(12) 0.0241(11) 0.0178(11) 0.0066(9) 0.0041(9) 0.0046(9) C25 0.0302(12) 0.0305(12) 0.0299(13) 0.0110(10) -0.0031(10) 0.0157(10) C26 0.0417(16) 0.0317(14) 0.062(2) 0.0126(13) -0.0059(14) 0.0174(12) C27 0.0307(14) 0.0513(18) 0.076(2) 0.0321(17) 0.0083(14) 0.0244(13) C28 0.071(2) 0.071(2) 0.0345(16) 0.0104(15) -0.0126(15) 0.046(2) C29 0.0564(17) 0.0287(13) 0.0173(11) 0.0009(10) 0.0010(11) 0.0180(12) C30 0.101(4) 0.111(4) 0.059(3) -0.036(3) -0.007(2) 0.074(3) C31 0.201(6) 0.0337(19) 0.046(2) -0.0119(16) 0.049(3) -0.017(3) C32 0.125(4) 0.050(2) 0.0263(15) -0.0082(14) -0.0276(19) 0.043(2) Cl2 0.0539(5) 0.0652(5) 0.0402(4) -0.0069(4) -0.0043(4) -0.0039(4) Cl3 0.0624(5) 0.0352(4) 0.0353(4) 0.0097(3) 0.0058(3) 0.0058(3) C33 0.0341(14) 0.0442(16) 0.0573(19) 0.0200(14) 0.0114(13) 0.0109(12) Cl4 0.0486(4) 0.0552(5) 0.0404(4) 0.0101(3) 0.0140(3) 0.0149(4) Cl5A 0.173(8) 0.214(9) 0.097(5) 0.001(4) 0.038(4) 0.156(7) Cl5B 0.072(2) 0.271(6) 0.0487(16) 0.047(2) 0.0294(11) 0.098(3) C34 0.0387(17) 0.067(2) 0.056(2) 0.0094(17) -0.0004(14) 0.0152(16) Cl6A 0.0902(16) 0.078(2) 0.0983(19) 0.0439(16) -0.0308(12) -0.0182(12) Cl7A 0.0884(13) 0.0830(14) 0.1020(18) 0.0270(11) -0.0115(10) 0.0395(10) C35A 0.098(5) 0.038(3) 0.054(4) 0.011(3) -0.005(4) -0.004(3) Cl6B 0.274(13) 0.026(3) 0.145(9) -0.016(4) -0.093(8) 0.003(5) Cl7B 0.180(9) 0.188(11) 0.254(17) 0.121(12) 0.056(10) 0.122(8) C35B 0.089(10) 0.059(10) 0.077(11) -0.002(7) -0.002(8) 0.036(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _diffrn_orient_matrix_type _diffrn_orient_matrix_UB_11 _diffrn_orient_matrix_UB_12 _diffrn_orient_matrix_UB_13 _diffrn_orient_matrix_UB_21 _diffrn_orient_matrix_UB_22 _diffrn_orient_matrix_UB_23 _diffrn_orient_matrix_UB_31 _diffrn_orient_matrix_UB_32 _diffrn_orient_matrix_UB_33 'Nonius RMAT' -0.0103470 0.0808365 0.0200686 0.0414836 0.0269510 -0.0437874 -0.1096758 -0.0295927 -0.0267060 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 N2 Ni1 N2 180.0 . 2_666 ? N2 Ni1 N1 94.54(7) . 2_666 ? N2 Ni1 N1 85.46(7) 2_666 2_666 ? N2 Ni1 N1 85.45(7) . . ? N2 Ni1 N1 94.55(7) 2_666 . ? N1 Ni1 N1 180.0 2_666 . ? N2 Ni1 Cl1 87.11(5) . 2_666 ? N2 Ni1 Cl1 92.89(5) 2_666 2_666 ? N1 Ni1 Cl1 92.85(5) 2_666 2_666 ? N1 Ni1 Cl1 87.15(5) . 2_666 ? N2 Ni1 Cl1 92.89(5) . . ? N2 Ni1 Cl1 87.11(5) 2_666 . ? N1 Ni1 Cl1 87.15(5) 2_666 . ? N1 Ni1 Cl1 92.85(5) . . ? Cl1 Ni1 Cl1 180.0 2_666 . ? C1 N1 C5 118.19(18) . . ? C1 N1 Ni1 118.32(14) . . ? C5 N1 Ni1 123.18(14) . . ? C11 N2 C7 118.06(18) . . ? C11 N2 Ni1 118.25(14) . . ? C7 N2 Ni1 123.66(14) . . ? N1 C1 C2 123.3(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.5(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.22(19) . . ? N1 C5 C6 118.89(18) . . ? C4 C5 C6 119.84(18) . . ? C12 C6 C5 121.32(18) . . ? C12 C6 C7 122.76(19) . . ? C5 C6 C7 115.54(17) . . ? N2 C7 C8 121.51(19) . . ? N2 C7 C6 118.64(17) . . ? C8 C7 C6 119.55(18) . . ? C9 C8 C7 119.6(2) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.0(2) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 118.5(2) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? N2 C11 C10 123.4(2) . . ? N2 C11 H11 118.3 . . ? C10 C11 H11 118.3 . . ? C6 C12 C13 122.27(19) . . ? C6 C12 C19 122.88(19) . . ? C13 C12 C19 114.19(17) . . ? C14 C13 C18 117.8(2) . . ? C14 C13 C12 119.97(19) . . ? C18 C13 C12 122.14(19) . . ? C13 C14 C15 120.8(2) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 121.8(2) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C17 C16 C15 116.7(2) . . ? C17 C16 C25 120.0(2) . . ? C15 C16 C25 123.3(2) . . ? C18 C17 C16 122.3(2) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C17 C18 C13 120.5(2) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C20 C19 C24 117.5(2) . . ? C20 C19 C12 119.82(19) . . ? C24 C19 C12 122.5(2) . . ? C19 C20 C21 121.1(2) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 121.7(2) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C23 C22 C21 116.8(2) . . ? C23 C22 C29 120.6(2) . . ? C21 C22 C29 122.6(2) . . ? C22 C23 C24 121.9(2) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C23 C24 C19 120.9(2) . . ? C23 C24 H24 119.6 . . ? C19 C24 H24 119.6 . . ? C27 C25 C26 108.7(2) . . ? C27 C25 C28 108.1(3) . . ? C26 C25 C28 109.0(3) . . ? C27 C25 C16 112.1(2) . . ? C26 C25 C16 109.6(2) . . ? C28 C25 C16 109.2(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C32 109.6(4) . . ? C31 C29 C30 107.7(4) . . ? C32 C29 C30 106.7(3) . . ? C31 C29 C22 112.5(2) . . ? C32 C29 C22 110.8(2) . . ? C30 C29 C22 109.4(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl2 C33 Cl3 111.12(16) . . ? Cl2 C33 H33A 109.4 . . ? Cl3 C33 H33A 109.4 . . ? Cl2 C33 H33B 109.4 . . ? Cl3 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? Cl5B C34 Cl4 113.8(2) . . ? Cl5A C34 Cl4 108.1(5) . . ? Cl5A C34 H34A 110.1 . . ? Cl4 C34 H34A 110.1 . . ? Cl5A C34 H34B 110.1 . . ? Cl4 C34 H34B 110.1 . . ? H34A C34 H34B 108.4 . . ? Cl5B C34 H34C 108.8 . . ? Cl4 C34 H34C 108.8 . . ? Cl5B C34 H34D 108.8 . . ? Cl4 C34 H34D 108.8 . . ? H34C C34 H34D 107.7 . . ? Cl6A C35A Cl7A 111.9(4) . . ? Cl6A C35A H35A 109.2 . . ? Cl7A C35A H35A 109.2 . . ? Cl6A C35A H35B 109.2 . . ? Cl7A C35A H35B 109.2 . . ? H35A C35A H35B 107.9 . . ? Cl6B C35B Cl7B 106.7(9) . . ? Cl6B C35B H35C 110.4 . . ? Cl7B C35B H35C 110.4 . . ? Cl6B C35B H35D 110.4 . . ? Cl7B C35B H35D 110.4 . . ? H35C C35B H35D 108.6 . . ? 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 N2 2.1032(17) . ? Ni1 N2 2.1033(17) 2_666 ? Ni1 N1 2.1140(18) 2_666 ? Ni1 N1 2.1140(18) . ? Ni1 Cl1 2.4373(5) 2_666 ? Ni1 Cl1 2.4373(5) . ? N1 C1 1.350(3) . ? N1 C5 1.351(3) . ? N2 C11 1.348(3) . ? N2 C7 1.349(3) . ? C1 C2 1.382(3) . ? C1 H1 0.9500 . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 C4 1.379(3) . ? C3 H3 0.9500 . ? C4 C5 1.403(3) . ? C4 H4 0.9500 . ? C5 C6 1.496(3) . ? C6 C12 1.347(3) . ? C6 C7 1.497(3) . ? C7 C8 1.400(3) . ? C8 C9 1.382(3) . ? C8 H8 0.9500 . ? C9 C10 1.386(3) . ? C9 H9 0.9500 . ? C10 C11 1.384(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.500(3) . ? C12 C19 1.501(3) . ? C13 C14 1.390(3) . ? C13 C18 1.400(3) . ? C14 C15 1.394(3) . ? C14 H14 0.9500 . ? C15 C16 1.392(3) . ? C15 H15 0.9500 . ? C16 C17 1.391(3) . ? C16 C25 1.541(3) . ? C17 C18 1.385(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.386(3) . ? C19 C24 1.399(3) . ? C20 C21 1.394(3) . ? C20 H20 0.9500 . ? C21 C22 1.394(3) . ? C21 H21 0.9500 . ? C22 C23 1.390(3) . ? C22 C29 1.535(3) . ? C23 C24 1.391(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C27 1.526(4) . ? C25 C26 1.529(4) . ? C25 C28 1.536(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.503(5) . ? C29 C32 1.513(4) . ? C29 C30 1.534(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? Cl2 C33 1.753(3) . ? Cl3 C33 1.761(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? Cl4 C34 1.755(3) . ? Cl5A C34 1.736(6) . ? Cl5B C34 1.695(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 H34C 0.9900 . ? C34 H34D 0.9900 . ? Cl6A C35A 1.740(4) . ? Cl7A C35A 1.750(6) . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? Cl6B C35B 1.737(8) . ? Cl7B C35B 1.752(8) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 0.9(3) . . . . ? Ni1 N1 C1 C2 174.70(17) . . . . ? N1 C1 C2 C3 -2.4(3) . . . . ? C1 C2 C3 C4 1.2(3) . . . . ? C2 C3 C4 C5 1.4(3) . . . . ? C1 N1 C5 C4 1.8(3) . . . . ? Ni1 N1 C5 C4 -171.66(15) . . . . ? C1 N1 C5 C6 179.18(18) . . . . ? Ni1 N1 C5 C6 5.7(2) . . . . ? C3 C4 C5 N1 -3.0(3) . . . . ? C3 C4 C5 C6 179.7(2) . . . . ? N1 C5 C6 C12 131.2(2) . . . . ? C4 C5 C6 C12 -51.4(3) . . . . ? N1 C5 C6 C7 -55.7(2) . . . . ? C4 C5 C6 C7 121.7(2) . . . . ? C11 N2 C7 C8 2.1(3) . . . . ? Ni1 N2 C7 C8 -179.62(15) . . . . ? C11 N2 C7 C6 -171.58(18) . . . . ? Ni1 N2 C7 C6 6.7(3) . . . . ? C12 C6 C7 N2 -138.3(2) . . . . ? C5 C6 C7 N2 48.7(3) . . . . ? C12 C6 C7 C8 47.9(3) . . . . ? C5 C6 C7 C8 -125.1(2) . . . . ? N2 C7 C8 C9 -1.3(3) . . . . ? C6 C7 C8 C9 172.36(19) . . . . ? C7 C8 C9 C10 -0.3(3) . . . . ? C8 C9 C10 C11 0.9(3) . . . . ? C7 N2 C11 C10 -1.4(3) . . . . ? Ni1 N2 C11 C10 -179.81(17) . . . . ? C9 C10 C11 N2 -0.1(3) . . . . ? C5 C6 C12 C13 -6.2(3) . . . . ? C7 C6 C12 C13 -178.77(18) . . . . ? C5 C6 C12 C19 -176.32(18) . . . . ? C7 C6 C12 C19 11.1(3) . . . . ? C6 C12 C13 C14 -62.0(3) . . . . ? C19 C12 C13 C14 109.0(2) . . . . ? C6 C12 C13 C18 121.3(3) . . . . ? C19 C12 C13 C18 -67.8(3) . . . . ? C18 C13 C14 C15 2.3(3) . . . . ? C12 C13 C14 C15 -174.6(2) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C17 -2.1(4) . . . . ? C14 C15 C16 C25 177.3(2) . . . . ? C15 C16 C17 C18 2.0(4) . . . . ? C25 C16 C17 C18 -177.5(2) . . . . ? C16 C17 C18 C13 0.3(4) . . . . ? C14 C13 C18 C17 -2.5(4) . . . . ? C12 C13 C18 C17 174.3(2) . . . . ? C6 C12 C19 C20 61.3(3) . . . . ? C13 C12 C19 C20 -109.6(2) . . . . ? C6 C12 C19 C24 -123.1(2) . . . . ? C13 C12 C19 C24 66.0(3) . . . . ? C24 C19 C20 C21 -1.7(4) . . . . ? C12 C19 C20 C21 174.1(2) . . . . ? C19 C20 C21 C22 0.5(4) . . . . ? C20 C21 C22 C23 1.3(4) . . . . ? C20 C21 C22 C29 -178.9(2) . . . . ? C21 C22 C23 C24 -1.8(4) . . . . ? C29 C22 C23 C24 178.3(2) . . . . ? C22 C23 C24 C19 0.6(4) . . . . ? C20 C19 C24 C23 1.2(3) . . . . ? C12 C19 C24 C23 -174.5(2) . . . . ? C17 C16 C25 C27 173.4(3) . . . . ? C15 C16 C25 C27 -6.0(4) . . . . ? C17 C16 C25 C26 -65.8(3) . . . . ? C15 C16 C25 C26 114.8(3) . . . . ? C17 C16 C25 C28 53.6(3) . . . . ? C15 C16 C25 C28 -125.8(3) . . . . ? C23 C22 C29 C31 -172.0(4) . . . . ? C21 C22 C29 C31 8.2(5) . . . . ? C23 C22 C29 C32 -48.9(4) . . . . ? C21 C22 C29 C32 131.3(3) . . . . ? C23 C22 C29 C30 68.4(4) . . . . ? C21 C22 C29 C30 -111.4(4) . . . . ?