#------------------------------------------------------------------------------ #$Date: 2026-05-22 23:51:24 +0100 (Fri, 22 May 2026) $ #$Revision: 306072 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721046.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_7721046 loop_ _publ_author_name 'Zuo, Jing' 'Zhang, Jun' 'Li, Hongxiu' 'Hu, Chaojie' 'Zhao, Mei-Xin' _publ_section_title ; Nickel Complexes Supported by a New Class of Fused Imidazonaphthyridine Tridentate N,N,N-Ligands for Ethylene Oligomerization and Isolation of a Key Ni-Al Intermediate ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00825A _journal_year 2026 _chemical_formula_moiety 'C24 H26 Cl2 N4 Ni' _chemical_formula_sum 'C24 H26 Cl2 N4 Ni' _chemical_formula_weight 500.10 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _audit_creation_date 2026-01-29 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2026-03-31 deposited with the CCDC. 2026-05-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.6615(2) _cell_length_b 15.7274(3) _cell_length_c 19.5070(3) _cell_measurement_reflns_used 9930 _cell_measurement_temperature 200.00 _cell_measurement_theta_max 74.428 _cell_measurement_theta_min 4.705 _cell_volume 4498.07(13) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 200.00 _diffrn_detector 'photon counting detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'PHOTON III detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture PHOTON III' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_unetI/netI 0.0281 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 39760 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.537 _diffrn_reflns_theta_min 4.705 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatec I\ms Diamond II' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 3.576 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.6557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0910 before and 0.0621 after correction. The Ratio of minimum to maximum transmission is 0.8699. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'light red' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.477 _exptl_crystal_description block _exptl_crystal_F_000 2080 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.015 _refine_diff_density_max 0.906 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 285 _refine_ls_number_reflns 4590 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0367 _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^)+(0.0473P)^2^+3.5322P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.0981 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3888 _reflns_number_total 4590 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00825a2.cif _cod_data_source_block cu_20251031_y82240206_1_a _cod_database_code 7721046 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.948 _shelx_estimated_absorpt_t_min 0.870 _olex2_refinement_description ; 1. Others Fixed Uiso: H2(0.05) H3(0.049) H4(0.051) H5(0.049) H8(0.041) H9(0.037) H12A(0.045) H12B(0.045) H12C(0.045) H15(0.036) H16(0.038) H17(0.034) H19(0.035) H20A(0.071) H20B(0.071) H20C(0.071) H21(0.03) H22A(0.054) H22B(0.054) H22C(0.054) H23A(0.055) H23B(0.055) H23C(0.055) H24A(0.056) H24B(0.056) H24C(0.056) Fixed X: H2(0.298859) H3(0.279686) H4(0.355175) H5(0.449269) H8(0.558802) H9(0.63171) H12A(0.70769) H12B(0.659241) H12C(0.730106) H15(0.761717) H16(0.713292) H17(0.595642) H19(0.6628) H20A(0.846496) H20B(0.793247) H20C(0.817401) H21(0.484211) H22A(0.489281) H22B(0.592497) H22C(0.545008) H23A(0.761481) H23B(0.733874) H23C(0.656438) H24A(0.395467) H24B(0.368522) H24C(0.431636) Fixed Y: H2(1.033863) H3(1.089519) H4(1.033815) H5(0.936395) H8(0.808165) H9(0.715653) H12A(0.616524) H12B(0.599533) H12C(0.676287) H15(0.666166) H16(0.526724) H17(0.470937) H19(0.814125) H20A(0.758296) H20B(0.756105) H20C(0.845288) H21(0.577688) H22A(0.435859) H22B(0.46684) H22C(0.410174) H23A(0.806359) H23B(0.892228) H23C(0.832855) H24A(0.569091) H24B(0.494244) H24C(0.474504) Fixed Z: H2(0.404755) H3(0.521927) H4(0.64871) H5(0.697164) H8(0.681487) H9(0.605084) H12A(0.445065) H12B(0.517292) H12C(0.50929) H15(0.230117) H16(0.213991) H17(0.279896) H19(0.349251) H20A(0.330278) H20B(0.401871) H20C(0.366789) H21(0.420366) H22A(0.453102) H22B(0.443713) H22C(0.385669) H23A(0.22293) H23B(0.261749) H23C(0.229322) H24A(0.319452) H24B(0.371208) H24C(0.306194) ; _shelx_res_file ; TITL cu_20251031_Y82240206_1_a.res in Pbca cu_20251031_y82240206_1_a.res created by SHELXL-2018/3 at 09:26:32 on 01-Nov-2025 REM Old TITL cu_20251031_Y82240206_1 in Pbca REM SHELXT solution in Pbca: R1 0.122, Rweak 0.004, Alpha 0.017 REM 0.915 for 520 systematic absences, Orientation as input REM Formula found by SHELXT: C24 Cl2 N4 Ni CELL 1.54178 14.6615 15.7274 19.507 90 90 90 ZERR 8 0.0002 0.0003 0.0003 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl N Ni UNIT 192 208 16 32 8 L.S. 10 PLAN 2 SIZE 0.015 0.03 0.04 TEMP -73.15 CONF BOND LIST 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.047300 3.532200 FVAR 0.20431 NI1 5 0.463073 0.793662 0.397847 11.00000 0.01936 0.02789 = 0.02461 -0.00041 -0.00135 0.00240 CL1 3 0.472311 0.828979 0.288883 11.00000 0.03656 0.05091 = 0.02903 0.00881 0.00021 0.01335 CL2 3 0.341834 0.712835 0.427904 11.00000 0.02358 0.03409 = 0.05188 -0.00611 0.00645 -0.00306 N1 4 0.383928 0.940720 0.443774 11.00000 0.02849 0.03535 = 0.03733 0.00157 0.00129 -0.00185 N2 4 0.367789 0.991090 0.550720 11.00000 0.02968 0.02362 = 0.04663 -0.00724 0.00990 -0.00270 N3 4 0.505169 0.813670 0.494487 11.00000 0.02284 0.02205 = 0.02394 -0.00337 0.00091 -0.00074 N4 4 0.571229 0.708415 0.406101 11.00000 0.01822 0.01938 = 0.02394 -0.00197 0.00154 -0.00031 C1 1 0.407114 0.931218 0.508466 11.00000 0.02503 0.02453 = 0.03471 -0.00496 0.00629 -0.00374 C2 1 0.326913 1.010630 0.444458 11.00000 0.02950 0.03756 = 0.05747 0.01143 0.00005 -0.00158 AFIX 43 H2 2 0.298859 1.033863 0.404755 11.00000 -1.20000 AFIX 0 C3 1 0.315803 1.042129 0.508699 11.00000 0.02951 0.02850 = 0.06500 0.00211 0.00942 0.00204 AFIX 43 H3 2 0.279686 1.089519 0.521927 11.00000 -1.20000 AFIX 0 C4 1 0.383892 0.992194 0.620785 11.00000 0.04777 0.03384 = 0.04544 -0.01722 0.01440 -0.00217 AFIX 43 H4 2 0.355175 1.033815 0.648710 11.00000 -1.20000 AFIX 0 C5 1 0.439441 0.935141 0.649038 11.00000 0.04906 0.04338 = 0.03041 -0.01435 0.00781 -0.00417 AFIX 43 H5 2 0.449269 0.936395 0.697164 11.00000 -1.20000 AFIX 0 C6 1 0.485111 0.871409 0.608308 11.00000 0.03241 0.02956 = 0.02924 -0.00704 0.00432 -0.00738 C7 1 0.467561 0.870157 0.537547 11.00000 0.02349 0.02416 = 0.02887 -0.00574 0.00433 -0.00406 C8 1 0.546177 0.811030 0.633776 11.00000 0.03731 0.04001 = 0.02602 -0.00265 -0.00248 -0.00748 AFIX 43 H8 2 0.558802 0.808165 0.681487 11.00000 -1.20000 AFIX 0 C9 1 0.588076 0.755440 0.588738 11.00000 0.03156 0.03195 = 0.02914 0.00033 -0.00480 -0.00313 AFIX 43 H9 2 0.631710 0.715653 0.605084 11.00000 -1.20000 AFIX 0 C10 1 0.566037 0.758052 0.519409 11.00000 0.02197 0.02272 = 0.02618 -0.00071 -0.00135 -0.00298 C11 1 0.606171 0.701363 0.466162 11.00000 0.01958 0.02032 = 0.02638 -0.00066 -0.00165 -0.00302 C12 1 0.682346 0.643452 0.486171 11.00000 0.02548 0.03031 = 0.03518 0.00127 -0.00622 0.00485 AFIX 137 H12A 2 0.707690 0.616524 0.445065 11.00000 -1.50000 H12B 2 0.659241 0.599533 0.517292 11.00000 -1.50000 H12C 2 0.730106 0.676287 0.509290 11.00000 -1.50000 AFIX 0 C13 1 0.608676 0.657727 0.350654 11.00000 0.01722 0.02115 = 0.02408 -0.00193 -0.00085 0.00476 C14 1 0.675989 0.693952 0.309214 11.00000 0.01947 0.02216 = 0.02923 0.00130 -0.00053 0.00200 C15 1 0.714776 0.643547 0.258304 11.00000 0.02686 0.03073 = 0.03160 0.00392 0.00774 0.00417 AFIX 43 H15 2 0.761717 0.666166 0.230117 11.00000 -1.20000 AFIX 0 C16 1 0.685559 0.560781 0.248390 11.00000 0.03628 0.02959 = 0.02992 -0.00323 0.00849 0.00797 AFIX 43 H16 2 0.713292 0.526724 0.213991 11.00000 -1.20000 AFIX 0 C17 1 0.616202 0.527275 0.288251 11.00000 0.03336 0.02031 = 0.03192 -0.00403 0.00113 0.00311 AFIX 43 H17 2 0.595642 0.470937 0.279896 11.00000 -1.20000 AFIX 0 C18 1 0.576001 0.574876 0.340487 11.00000 0.02087 0.02214 = 0.02631 0.00004 -0.00017 0.00071 C19 1 0.708866 0.784457 0.319976 11.00000 0.02543 0.02489 = 0.03821 -0.00151 0.00478 -0.00404 AFIX 13 H19 2 0.662800 0.814125 0.349251 11.00000 -1.20000 AFIX 0 C20 1 0.799607 0.786192 0.358137 11.00000 0.03482 0.05484 = 0.05322 0.00330 -0.00665 -0.01783 AFIX 137 H20A 2 0.846496 0.758296 0.330278 11.00000 -1.50000 H20B 2 0.793247 0.756105 0.401871 11.00000 -1.50000 H20C 2 0.817401 0.845288 0.366789 11.00000 -1.50000 AFIX 0 C21 1 0.501440 0.535620 0.384173 11.00000 0.02302 0.02025 = 0.03124 -0.00196 0.00180 -0.00075 AFIX 13 H21 2 0.484211 0.577688 0.420366 11.00000 -1.20000 AFIX 0 C22 1 0.535080 0.454865 0.419873 11.00000 0.03408 0.02798 = 0.04544 0.00874 0.00527 0.00151 AFIX 137 H22A 2 0.489281 0.435859 0.453102 11.00000 -1.50000 H22B 2 0.592497 0.466840 0.443713 11.00000 -1.50000 H22C 2 0.545008 0.410174 0.385669 11.00000 -1.50000 AFIX 0 C23 1 0.715786 0.833365 0.252430 11.00000 0.03324 0.02771 = 0.04808 0.00546 0.00523 -0.00484 AFIX 137 H23A 2 0.761481 0.806359 0.222930 11.00000 -1.50000 H23B 2 0.733874 0.892228 0.261749 11.00000 -1.50000 H23C 2 0.656438 0.832855 0.229322 11.00000 -1.50000 AFIX 0 C24 1 0.416687 0.516670 0.341435 11.00000 0.02546 0.04515 = 0.04235 -0.00021 -0.00139 -0.00592 AFIX 137 H24A 2 0.395467 0.569091 0.319452 11.00000 -1.50000 H24B 2 0.368522 0.494244 0.371208 11.00000 -1.50000 H24C 2 0.431636 0.474504 0.306194 11.00000 -1.50000 AFIX 0 HKLF 4 REM cu_20251031_Y82240206_1_a.res in Pbca REM wR2 = 0.0981, GooF = S = 1.030, Restrained GooF = 1.030 for all data REM R1 = 0.0367 for 3888 Fo > 4sig(Fo) and 0.0446 for all 4590 data REM 285 parameters refined using 0 restraints END WGHT 0.0471 3.5440 REM Highest difference peak 0.906, deepest hole -0.311, 1-sigma level 0.060 Q1 1 0.4638 0.8068 0.3426 11.00000 0.05 0.91 Q2 1 0.4666 0.8020 0.4547 11.00000 0.05 0.61 ; _shelx_res_checksum 14310 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 0.46307(2) 0.79366(2) 0.39785(2) 0.02395(11) Uani 1 1 d . . . . . Cl2 Cl 0.47231(4) 0.82898(4) 0.28888(3) 0.03883(15) Uani 1 1 d . . . . . Cl1 Cl 0.34183(3) 0.71284(3) 0.42790(3) 0.03652(14) Uani 1 1 d . . . . . N3 N 0.38393(13) 0.94072(13) 0.44377(10) 0.0337(4) Uani 1 1 d . . . . . N4 N 0.36779(13) 0.99109(12) 0.55072(10) 0.0333(4) Uani 1 1 d . . . . . N2 N 0.50517(11) 0.81367(10) 0.49449(9) 0.0229(3) Uani 1 1 d . . . . . N1 N 0.57123(11) 0.70842(10) 0.40610(8) 0.0205(3) Uani 1 1 d . . . . . C11 C 0.40711(14) 0.93122(13) 0.50847(11) 0.0281(4) Uani 1 1 d . . . . . C10 C 0.32691(16) 1.01063(16) 0.44446(14) 0.0415(6) Uani 1 1 d . . . . . H2 H 0.298859 1.033863 0.404755 0.050 Uiso 1 1 calc R U . . . C9 C 0.31580(16) 1.04213(15) 0.50870(14) 0.0410(6) Uani 1 1 d . . . . . H3 H 0.279686 1.089519 0.521927 0.049 Uiso 1 1 calc R U . . . C8 C 0.38389(18) 0.99219(16) 0.62078(13) 0.0424(6) Uani 1 1 d . . . . . H4 H 0.355175 1.033815 0.648710 0.051 Uiso 1 1 calc R U . . . C7 C 0.43944(18) 0.93514(17) 0.64904(12) 0.0410(6) Uani 1 1 d . . . . . H5 H 0.449269 0.936395 0.697164 0.049 Uiso 1 1 calc R U . . . C6 C 0.48511(15) 0.87141(14) 0.60831(11) 0.0304(4) Uani 1 1 d . . . . . C12 C 0.46756(13) 0.87016(13) 0.53755(11) 0.0255(4) Uani 1 1 d . . . . . C5 C 0.54618(16) 0.81103(15) 0.63378(12) 0.0344(5) Uani 1 1 d . . . . . H8 H 0.558802 0.808165 0.681487 0.041 Uiso 1 1 calc R U . . . C4 C 0.58808(15) 0.75544(14) 0.58874(11) 0.0309(4) Uani 1 1 d . . . . . H9 H 0.631710 0.715653 0.605084 0.037 Uiso 1 1 calc R U . . . C3 C 0.56604(13) 0.75805(13) 0.51941(10) 0.0236(4) Uani 1 1 d . . . . . C2 C 0.60617(13) 0.70136(12) 0.46616(10) 0.0221(4) Uani 1 1 d . . . . . C1 C 0.68235(14) 0.64345(14) 0.48617(11) 0.0303(4) Uani 1 1 d . . . . . H12A H 0.707690 0.616524 0.445065 0.045 Uiso 1 1 calc R U . . . H12B H 0.659241 0.599533 0.517292 0.045 Uiso 1 1 calc R U . . . H12C H 0.730106 0.676287 0.509290 0.045 Uiso 1 1 calc R U . . . C13 C 0.60868(12) 0.65773(12) 0.35065(10) 0.0208(4) Uani 1 1 d . . . . . C14 C 0.67599(13) 0.69395(12) 0.30921(10) 0.0236(4) Uani 1 1 d . . . . . C15 C 0.71478(14) 0.64355(14) 0.25830(11) 0.0297(4) Uani 1 1 d . . . . . H15 H 0.761717 0.666166 0.230117 0.036 Uiso 1 1 calc R U . . . C16 C 0.68556(16) 0.56078(14) 0.24839(11) 0.0319(5) Uani 1 1 d . . . . . H16 H 0.713292 0.526724 0.213991 0.038 Uiso 1 1 calc R U . . . C17 C 0.61620(15) 0.52727(13) 0.28825(11) 0.0285(4) Uani 1 1 d . . . . . H17 H 0.595642 0.470937 0.279896 0.034 Uiso 1 1 calc R U . . . C18 C 0.57600(13) 0.57488(12) 0.34049(10) 0.0231(4) Uani 1 1 d . . . . . C19 C 0.70887(14) 0.78446(13) 0.31998(12) 0.0295(4) Uani 1 1 d . . . . . H19 H 0.662800 0.814125 0.349251 0.035 Uiso 1 1 calc R U . . . C20 C 0.79961(18) 0.78619(19) 0.35814(15) 0.0476(6) Uani 1 1 d . . . . . H20A H 0.846496 0.758296 0.330278 0.071 Uiso 1 1 calc R U . . . H20B H 0.793247 0.756105 0.401871 0.071 Uiso 1 1 calc R U . . . H20C H 0.817401 0.845288 0.366789 0.071 Uiso 1 1 calc R U . . . C22 C 0.50144(13) 0.53562(13) 0.38417(11) 0.0248(4) Uani 1 1 d . . . . . H21 H 0.484211 0.577688 0.420366 0.030 Uiso 1 1 calc R U . . . C24 C 0.53508(16) 0.45486(14) 0.41987(13) 0.0358(5) Uani 1 1 d . . . . . H22A H 0.489281 0.435859 0.453102 0.054 Uiso 1 1 calc R U . . . H22B H 0.592497 0.466840 0.443713 0.054 Uiso 1 1 calc R U . . . H22C H 0.545008 0.410174 0.385669 0.054 Uiso 1 1 calc R U . . . C21 C 0.71579(16) 0.83337(14) 0.25243(13) 0.0363(5) Uani 1 1 d . . . . . H23A H 0.761481 0.806359 0.222930 0.055 Uiso 1 1 calc R U . . . H23B H 0.733874 0.892228 0.261749 0.055 Uiso 1 1 calc R U . . . H23C H 0.656438 0.832855 0.229322 0.055 Uiso 1 1 calc R U . . . C23 C 0.41669(15) 0.51667(17) 0.34143(12) 0.0377(5) Uani 1 1 d . . . . . H24A H 0.395467 0.569091 0.319452 0.056 Uiso 1 1 calc R U . . . H24B H 0.368522 0.494244 0.371208 0.056 Uiso 1 1 calc R U . . . H24C H 0.431636 0.474504 0.306194 0.056 Uiso 1 1 calc R U . . . 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 0.01936(18) 0.0279(2) 0.02461(19) -0.00041(13) -0.00135(13) 0.00240(13) Cl2 0.0366(3) 0.0509(3) 0.0290(3) 0.0088(2) 0.0002(2) 0.0134(2) Cl1 0.0236(2) 0.0341(3) 0.0519(3) -0.0061(2) 0.0064(2) -0.0031(2) N3 0.0285(9) 0.0353(10) 0.0373(10) 0.0016(8) 0.0013(8) -0.0018(8) N4 0.0297(9) 0.0236(9) 0.0466(11) -0.0072(8) 0.0099(8) -0.0027(7) N2 0.0228(8) 0.0221(8) 0.0239(8) -0.0034(6) 0.0009(6) -0.0007(6) N1 0.0182(7) 0.0194(8) 0.0239(8) -0.0020(6) 0.0015(6) -0.0003(6) C11 0.0250(9) 0.0245(10) 0.0347(11) -0.0050(8) 0.0063(8) -0.0037(8) C10 0.0295(11) 0.0376(13) 0.0575(16) 0.0114(11) 0.0000(11) -0.0016(10) C9 0.0295(11) 0.0285(11) 0.0650(17) 0.0021(11) 0.0094(11) 0.0020(9) C8 0.0478(14) 0.0338(12) 0.0454(14) -0.0172(11) 0.0144(11) -0.0022(11) C7 0.0491(14) 0.0434(14) 0.0304(12) -0.0144(10) 0.0078(10) -0.0042(11) C6 0.0324(10) 0.0296(11) 0.0292(10) -0.0070(8) 0.0043(9) -0.0074(9) C12 0.0235(9) 0.0242(10) 0.0289(10) -0.0057(8) 0.0043(8) -0.0041(8) C5 0.0373(12) 0.0400(12) 0.0260(11) -0.0027(9) -0.0025(9) -0.0075(10) C4 0.0316(11) 0.0320(11) 0.0291(11) 0.0003(9) -0.0048(8) -0.0031(9) C3 0.0220(9) 0.0227(9) 0.0262(10) -0.0007(8) -0.0014(7) -0.0030(7) C2 0.0196(8) 0.0203(9) 0.0264(10) -0.0007(7) -0.0017(7) -0.0030(7) C1 0.0255(10) 0.0303(11) 0.0352(11) 0.0013(9) -0.0062(8) 0.0048(8) C13 0.0172(8) 0.0211(9) 0.0241(9) -0.0019(7) -0.0008(7) 0.0048(7) C14 0.0195(8) 0.0222(9) 0.0292(10) 0.0013(8) -0.0005(7) 0.0020(7) C15 0.0269(10) 0.0307(11) 0.0316(11) 0.0039(9) 0.0077(8) 0.0042(8) C16 0.0363(11) 0.0296(11) 0.0299(11) -0.0032(8) 0.0085(9) 0.0080(9) C17 0.0334(11) 0.0203(10) 0.0319(11) -0.0040(8) 0.0011(8) 0.0031(8) C18 0.0209(9) 0.0221(9) 0.0263(10) 0.0000(8) -0.0002(7) 0.0007(7) C19 0.0254(10) 0.0249(10) 0.0382(12) -0.0015(8) 0.0048(9) -0.0040(8) C20 0.0348(13) 0.0548(16) 0.0532(15) 0.0033(12) -0.0066(11) -0.0178(12) C22 0.0230(9) 0.0203(9) 0.0312(10) -0.0020(8) 0.0018(8) -0.0008(7) C24 0.0341(12) 0.0280(11) 0.0454(13) 0.0087(10) 0.0053(10) 0.0015(9) C21 0.0332(11) 0.0277(11) 0.0481(14) 0.0055(9) 0.0052(10) -0.0048(9) C23 0.0255(10) 0.0452(14) 0.0424(13) -0.0002(10) -0.0014(9) -0.0059(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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 Cl2 Ni1 Cl1 116.13(3) . . ? N2 Ni1 Cl2 147.99(5) . . ? N2 Ni1 Cl1 94.95(5) . . ? N2 Ni1 N1 78.13(7) . . ? N1 Ni1 Cl2 100.97(5) . . ? N1 Ni1 Cl1 102.50(5) . . ? C11 N3 C10 103.7(2) . . ? C11 N4 C8 121.8(2) . . ? C9 N4 C11 105.9(2) . . ? C9 N4 C8 132.3(2) . . ? C12 N2 Ni1 124.42(14) . . ? C3 N2 Ni1 116.27(13) . . ? C3 N2 C12 118.60(18) . . ? C2 N1 Ni1 115.47(13) . . ? C2 N1 C13 118.80(16) . . ? C13 N1 Ni1 125.73(12) . . ? N3 C11 N4 112.8(2) . . ? N3 C11 C12 128.27(19) . . ? N4 C11 C12 118.87(19) . . ? N3 C10 H2 124.1 . . ? C9 C10 N3 111.8(2) . . ? C9 C10 H2 124.1 . . ? N4 C9 H3 127.2 . . ? C10 C9 N4 105.7(2) . . ? C10 C9 H3 127.2 . . ? N4 C8 H4 119.9 . . ? C7 C8 N4 120.2(2) . . ? C7 C8 H4 119.9 . . ? C8 C7 H5 119.2 . . ? C8 C7 C6 121.6(2) . . ? C6 C7 H5 119.2 . . ? C12 C6 C7 117.8(2) . . ? C5 C6 C7 125.0(2) . . ? C5 C6 C12 117.2(2) . . ? N2 C12 C11 116.93(18) . . ? N2 C12 C6 123.3(2) . . ? C6 C12 C11 119.73(19) . . ? C6 C5 H8 120.4 . . ? C4 C5 C6 119.2(2) . . ? C4 C5 H8 120.4 . . ? C5 C4 H9 120.1 . . ? C5 C4 C3 119.7(2) . . ? C3 C4 H9 120.1 . . ? N2 C3 C4 121.76(19) . . ? N2 C3 C2 113.61(17) . . ? C4 C3 C2 124.64(19) . . ? N1 C2 C3 115.28(17) . . ? N1 C2 C1 126.15(18) . . ? C3 C2 C1 118.57(17) . . ? C2 C1 H12A 109.5 . . ? C2 C1 H12B 109.5 . . ? C2 C1 H12C 109.5 . . ? H12A C1 H12B 109.5 . . ? H12A C1 H12C 109.5 . . ? H12B C1 H12C 109.5 . . ? C14 C13 N1 118.32(17) . . ? C14 C13 C18 122.57(18) . . ? C18 C13 N1 119.11(17) . . ? C13 C14 C19 121.79(18) . . ? C15 C14 C13 117.98(18) . . ? C15 C14 C19 120.21(18) . . ? C14 C15 H15 119.7 . . ? C16 C15 C14 120.59(19) . . ? C16 C15 H15 119.7 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.46(19) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 119.5 . . ? C16 C17 C18 121.1(2) . . ? C18 C17 H17 119.5 . . ? C13 C18 C22 123.01(17) . . ? C17 C18 C13 117.23(18) . . ? C17 C18 C22 119.75(18) . . ? C14 C19 H19 107.6 . . ? C14 C19 C20 111.19(19) . . ? C14 C19 C21 111.95(18) . . ? C20 C19 H19 107.6 . . ? C20 C19 C21 110.72(19) . . ? C21 C19 H19 107.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C22 H21 108.0 . . ? C18 C22 C24 111.17(17) . . ? C18 C22 C23 111.06(17) . . ? C24 C22 H21 108.0 . . ? C23 C22 H21 108.0 . . ? C23 C22 C24 110.43(18) . . ? C22 C24 H22A 109.5 . . ? C22 C24 H22B 109.5 . . ? C22 C24 H22C 109.5 . . ? H22A C24 H22B 109.5 . . ? H22A C24 H22C 109.5 . . ? H22B C24 H22C 109.5 . . ? C19 C21 H23A 109.5 . . ? C19 C21 H23B 109.5 . . ? C19 C21 H23C 109.5 . . ? H23A C21 H23B 109.5 . . ? H23A C21 H23C 109.5 . . ? H23B C21 H23C 109.5 . . ? C22 C23 H24A 109.5 . . ? C22 C23 H24B 109.5 . . ? C22 C23 H24C 109.5 . . ? H24A C23 H24B 109.5 . . ? H24A C23 H24C 109.5 . . ? H24B C23 H24C 109.5 . . ? 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 Cl2 2.2011(6) . ? Ni1 Cl1 2.2626(6) . ? Ni1 N2 2.0084(17) . ? Ni1 N1 2.0828(16) . ? N3 C11 1.315(3) . ? N3 C10 1.381(3) . ? N4 C11 1.378(3) . ? N4 C9 1.377(3) . ? N4 C8 1.387(3) . ? N2 C12 1.341(3) . ? N2 C3 1.341(3) . ? N1 C2 1.284(3) . ? N1 C13 1.451(2) . ? C11 C12 1.425(3) . ? C10 H2 0.9500 . ? C10 C9 1.357(4) . ? C9 H3 0.9500 . ? C8 H4 0.9500 . ? C8 C7 1.331(4) . ? C7 H5 0.9500 . ? C7 C6 1.444(3) . ? C6 C12 1.404(3) . ? C6 C5 1.396(3) . ? C5 H8 0.9500 . ? C5 C4 1.383(3) . ? C4 H9 0.9500 . ? C4 C3 1.391(3) . ? C3 C2 1.490(3) . ? C2 C1 1.493(3) . ? C1 H12A 0.9800 . ? C1 H12B 0.9800 . ? C1 H12C 0.9800 . ? C13 C14 1.397(3) . ? C13 C18 1.402(3) . ? C14 C15 1.392(3) . ? C14 C19 1.517(3) . ? C15 H15 0.9500 . ? C15 C16 1.384(3) . ? C16 H16 0.9500 . ? C16 C17 1.384(3) . ? C17 H17 0.9500 . ? C17 C18 1.395(3) . ? C18 C22 1.517(3) . ? C19 H19 1.0000 . ? C19 C20 1.525(3) . ? C19 C21 1.529(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C22 H21 1.0000 . ? C22 C24 1.530(3) . ? C22 C23 1.526(3) . ? C24 H22A 0.9800 . ? C24 H22B 0.9800 . ? C24 H22C 0.9800 . ? C21 H23A 0.9800 . ? C21 H23B 0.9800 . ? C21 H23C 0.9800 . ? C23 H24A 0.9800 . ? C23 H24B 0.9800 . ? C23 H24C 0.9800 . ? 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 Ni1 N2 C12 C11 -13.4(3) . . . . ? Ni1 N2 C12 C6 166.63(15) . . . . ? Ni1 N2 C3 C4 -168.19(15) . . . . ? Ni1 N2 C3 C2 11.9(2) . . . . ? Ni1 N1 C2 C3 -2.4(2) . . . . ? Ni1 N1 C2 C1 178.38(16) . . . . ? Ni1 N1 C13 C14 86.3(2) . . . . ? Ni1 N1 C13 C18 -93.5(2) . . . . ? N3 C11 C12 N2 -1.2(3) . . . . ? N3 C11 C12 C6 178.7(2) . . . . ? N3 C10 C9 N4 0.3(3) . . . . ? N4 C11 C12 N2 -179.24(18) . . . . ? N4 C11 C12 C6 0.7(3) . . . . ? N4 C8 C7 C6 0.6(4) . . . . ? N2 C3 C2 N1 -6.0(3) . . . . ? N2 C3 C2 C1 173.20(18) . . . . ? N1 C13 C14 C15 176.89(18) . . . . ? N1 C13 C14 C19 -1.2(3) . . . . ? N1 C13 C18 C17 -177.69(17) . . . . ? N1 C13 C18 C22 1.2(3) . . . . ? C11 N3 C10 C9 -0.3(3) . . . . ? C11 N4 C9 C10 -0.2(2) . . . . ? C11 N4 C8 C7 0.8(4) . . . . ? C10 N3 C11 N4 0.2(2) . . . . ? C10 N3 C11 C12 -177.9(2) . . . . ? C9 N4 C11 N3 0.0(2) . . . . ? C9 N4 C11 C12 178.27(19) . . . . ? C9 N4 C8 C7 -178.9(2) . . . . ? C8 N4 C11 N3 -179.8(2) . . . . ? C8 N4 C11 C12 -1.5(3) . . . . ? C8 N4 C9 C10 179.5(2) . . . . ? C8 C7 C6 C12 -1.4(4) . . . . ? C8 C7 C6 C5 178.1(2) . . . . ? C7 C6 C12 N2 -179.4(2) . . . . ? C7 C6 C12 C11 0.7(3) . . . . ? C7 C6 C5 C4 -177.5(2) . . . . ? C6 C5 C4 C3 -2.7(3) . . . . ? C12 N2 C3 C4 2.6(3) . . . . ? C12 N2 C3 C2 -177.30(17) . . . . ? C12 C6 C5 C4 2.0(3) . . . . ? C5 C6 C12 N2 1.1(3) . . . . ? C5 C6 C12 C11 -178.88(19) . . . . ? C5 C4 C3 N2 0.4(3) . . . . ? C5 C4 C3 C2 -179.7(2) . . . . ? C4 C3 C2 N1 174.06(19) . . . . ? C4 C3 C2 C1 -6.7(3) . . . . ? C3 N2 C12 C11 176.58(17) . . . . ? C3 N2 C12 C6 -3.4(3) . . . . ? C2 N1 C13 C14 -93.9(2) . . . . ? C2 N1 C13 C18 86.3(2) . . . . ? C13 N1 C2 C3 177.75(16) . . . . ? C13 N1 C2 C1 -1.4(3) . . . . ? C13 C14 C15 C16 1.5(3) . . . . ? C13 C14 C19 C20 101.0(2) . . . . ? C13 C14 C19 C21 -134.6(2) . . . . ? C13 C18 C22 C24 -120.8(2) . . . . ? C13 C18 C22 C23 115.9(2) . . . . ? C14 C13 C18 C17 2.6(3) . . . . ? C14 C13 C18 C22 -178.59(18) . . . . ? C14 C15 C16 C17 1.1(3) . . . . ? C15 C14 C19 C20 -77.1(3) . . . . ? C15 C14 C19 C21 47.3(3) . . . . ? C15 C16 C17 C18 -1.9(3) . . . . ? C16 C17 C18 C13 0.1(3) . . . . ? C16 C17 C18 C22 -178.77(19) . . . . ? C17 C18 C22 C24 58.1(3) . . . . ? C17 C18 C22 C23 -65.3(2) . . . . ? C18 C13 C14 C15 -3.4(3) . . . . ? C18 C13 C14 C19 178.52(18) . . . . ? C19 C14 C15 C16 179.6(2) . . . . ?