#------------------------------------------------------------------------------ #$Date: 2026-05-22 23:51:24 +0100 (Fri, 22 May 2026) $ #$Revision: 306072 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721044.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_7721044 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 'C33 H37 Cl2 N5 Ni O, 0.4[H2O]' _chemical_formula_sum 'C33 H37 Cl2 N5 Ni O' _chemical_formula_weight 649.28 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 100.2736(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.9309(2) _cell_length_b 13.2937(2) _cell_length_c 19.3267(4) _cell_measurement_reflns_used 46531 _cell_measurement_temperature 200.0 _cell_measurement_theta_max 74.456 _cell_measurement_theta_min 2.326 _cell_volume 3268.99(10) _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 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 200.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 41821 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.703 _diffrn_reflns_theta_min 3.474 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.619 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.6581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1053 before and 0.0530 after correction. The Ratio of minimum to maximum transmission is 0.8730. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.319 _exptl_crystal_description block _exptl_crystal_F_000 1360 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.527 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 386 _refine_ls_number_reflns 6654 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0420 _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^)+(0.0588P)^2^+2.6461P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1209 _refine_ls_wR_factor_ref 0.1233 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6081 _reflns_number_total 6654 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00825a2.cif _cod_data_source_block a_CCDC1 _cod_database_code 7721044 _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. ; _olex2_refinement_description ; 1. Others Fixed Uiso: H5(0.045) H11(0.045) H4(0.044) H10(0.048) H18(0.055) H1A(0.077) H1B(0.077) H1C(0.077) H9(0.046) H21(0.076) H22(0.082) H14(0.06) H23(0.075) H25(0.065) H17(0.068) H28(0.065) H30A(0.113) H30B(0.113) H30C(0.113) H16(0.076) H15(0.077) H26A(0.116) H26B(0.116) H26C(0.116) H29A(0.125) H29B(0.125) H29C(0.125) H27A(0.118) H27B(0.118) H27C(0.118) H31(0.048) H32A(0.142) H32B(0.142) H32C(0.142) H33A(0.167) H33B(0.167) H33C(0.167) Fixed X: H5(0.677638) H11(0.555644) H4(0.762918) H10(0.554581) H18(0.670854) H1A(0.799972) H1B(0.903292) H1C(0.901658) H9(0.599109) H21(1.122848) H22(1.037446) H14(0.567779) H23(0.861476) H25(0.690799) H17(0.645929) H28(0.99558) H30A(1.086165) H30B(1.159987) H30C(1.179326) H16(0.579613) H15(0.542548) H26A(0.680899) H26B(0.586341) H26C(0.683969) H29A(1.164282) H29B(1.141499) H29C(1.059964) H27A(0.726909) H27B(0.6189) H27C(0.724362) H31(0.851855) H32A(0.927349) H32B(1.052786) H32C(0.992365) H33A(1.053576) H33B(1.072808) H33C(1.132851) Fixed Y: H5(0.155737) H11(-0.189327) H4(0.296582) H10(-0.143411) H18(0.039038) H1A(0.454001) H1B(0.390674) H1C(0.46209) H9(-0.024039) H21(0.450282) H22(0.595035) H14(-0.240919) H23(0.617156) H25(0.443377) H17(0.00335) H28(0.238119) H30A(0.329447) H30B(0.240439) H30C(0.353302) H16(- 0.151673) H15(-0.273869) H26A(0.446261) H26B(0.507511) H26C(0.566575) H29A(0.281203) H29B(0.173324) H29C(0.220825) H27A(0.655953) H27B(0.606842) H27C(0.590125) H31(-0.001938) H32A(-0.150427) H32B(-0.141788) H32C(-0.196557) H33A(0.049318) H33B(-0.066614) H33C(-0.016435) Fixed Z: H5(-0.202875) H11(0.030394) H4(-0.147693) H10(-0.113925) H18(0.208244) H1A(-0.069735) H1B(-0.075641) H1C(-0.009185) H9(-0.187803) H21(0.192503) H22(0.217237) H14(0.147618) H23(0.176366) H25(0.068942) H17(0.322554) H28(0.094067) H30A(0.020426) H30B(0.056553) H30C(0.084701) H16(0.349155) H15(0.262182) H26A(0.191075) H26B(0.14506) H26C(0.189498) H29A(0.206908) H29B(0.170643) H29C(0.214837) H27A(0.079759) H27B(0.041195) H27C(0.010148) H31(0.154583) H32A(0.184665) H32B(0.198338) H32C(0.129039) H33A(0.068698) H33B(0.052626) H33C(0.123844) ; _smtbx_masks_special_details ; A solvent mask was calculated and 16 electrons were found in a volume of 110\%A^3^ in 1 void per unit cell. This is consistent with the presence of 0.4[H2O] per Asymmetric Unit which account for 16 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL A in P21/c #14 a.res created by SHELXL-2018/3 at 21:08:37 on 06-Nov-2025 REM reset to P21/c #14 CELL 1.54178 12.9309 13.2937 19.3267 90 100.2736 90 ZERR 4 0.0002 0.0002 0.0004 0 0.0009 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N Ni O UNIT 132 148 8 20 4 4 L.S. 20 PLAN 2 TEMP -73.15 CONF BOND fmap 2 MORE -1 BOND $H ACTA ABIN REM REM REM WGHT 0.058800 2.646100 FVAR 0.12864 NI1 5 0.757718 0.192865 0.097168 11.00000 0.03296 0.02959 = 0.02267 -0.00013 0.01096 0.00010 CL1 3 0.800262 0.209875 0.216374 11.00000 0.05541 0.04463 = 0.02358 -0.00280 0.01006 -0.00026 CL2 3 0.590257 0.268429 0.083500 11.00000 0.03902 0.03741 = 0.06047 -0.00458 0.01838 0.00140 N4 4 0.608153 -0.067271 -0.022606 11.00000 0.03255 0.03384 = 0.03365 -0.00361 0.00976 -0.00171 N2 4 0.732793 0.175066 -0.007901 11.00000 0.03079 0.02971 = 0.02546 0.00004 0.00982 0.00204 N1 4 0.832575 0.321760 0.062001 11.00000 0.03952 0.02919 = 0.02982 0.00037 0.01353 -0.00362 C7 1 0.684580 0.093962 -0.038994 11.00000 0.02767 0.03310 = 0.02543 -0.00171 0.00880 0.00419 N3 4 0.666890 0.020260 0.075602 11.00000 0.02950 0.03357 = 0.02754 0.00196 0.00877 0.00184 C8 1 0.655211 0.018915 0.006266 11.00000 0.02849 0.03128 = 0.02840 -0.00368 0.00841 0.00075 C6 1 0.662578 0.080584 -0.112397 11.00000 0.03029 0.04252 = 0.02649 -0.00535 0.00902 0.00336 C3 1 0.762653 0.248395 -0.046908 11.00000 0.03557 0.03240 = 0.02739 0.00249 0.01118 0.00271 C2 1 0.819798 0.331188 -0.004898 11.00000 0.04083 0.03221 = 0.03161 0.00310 0.01457 -0.00277 C12 1 0.625158 -0.070197 0.092744 11.00000 0.02885 0.03535 = 0.03717 0.00444 0.00926 0.00231 C5 1 0.692191 0.159742 -0.153005 11.00000 0.04187 0.04956 = 0.02372 0.00134 0.01070 0.00434 AFIX 43 H5 2 0.677638 0.155737 -0.202875 11.00000 -1.20000 AFIX 0 C11 1 0.588175 -0.125035 0.032913 11.00000 0.03674 0.03393 = 0.04309 0.00057 0.01109 -0.00305 AFIX 43 H11 2 0.555644 -0.189327 0.030394 11.00000 -1.20000 AFIX 0 C13 1 0.619461 -0.095874 0.166028 11.00000 0.03088 0.04538 = 0.03738 0.01146 0.00824 0.00232 C4 1 0.742327 0.243136 -0.120469 11.00000 0.04340 0.04105 = 0.02754 0.00505 0.01331 0.00255 AFIX 43 H4 2 0.762918 0.296582 -0.147693 11.00000 -1.20000 AFIX 0 C10 1 0.587280 -0.082861 -0.095254 11.00000 0.04076 0.04401 = 0.03507 -0.01308 0.00922 -0.00512 AFIX 43 H10 2 0.554581 -0.143411 -0.113925 11.00000 -1.20000 AFIX 0 C19 1 0.889338 0.398082 0.106311 11.00000 0.05458 0.03547 = 0.03234 0.00051 0.01375 -0.01653 C18 1 0.643939 -0.024621 0.218631 11.00000 0.04209 0.06073 = 0.03585 0.00774 0.00945 -0.01062 AFIX 43 H18 2 0.670854 0.039038 0.208244 11.00000 -1.20000 AFIX 0 C1 1 0.859628 0.416908 -0.043178 11.00000 0.07397 0.04520 = 0.03767 0.00890 0.01684 -0.01800 AFIX 137 H1A 2 0.799972 0.454001 -0.069735 11.00000 -1.50000 H1B 2 0.903292 0.390674 -0.075641 11.00000 -1.50000 H1C 2 0.901658 0.462090 -0.009185 11.00000 -1.50000 AFIX 0 C9 1 0.613406 -0.012384 -0.138522 11.00000 0.03840 0.04975 = 0.02909 -0.01029 0.01000 -0.00264 AFIX 43 H9 2 0.599109 -0.024039 -0.187803 11.00000 -1.20000 AFIX 0 C21 1 1.050044 0.458150 0.174346 11.00000 0.06820 0.07037 = 0.04722 0.01181 0.00073 -0.03085 AFIX 43 H21 2 1.122848 0.450282 0.192503 11.00000 -1.20000 AFIX 0 C22 1 0.999082 0.544035 0.189256 11.00000 0.10429 0.05249 = 0.04723 -0.00723 0.01355 -0.03148 AFIX 43 H22 2 1.037446 0.595035 0.217237 11.00000 -1.20000 AFIX 0 C14 1 0.582714 -0.190443 0.182778 11.00000 0.05068 0.04847 = 0.05299 0.01610 0.01286 0.00050 AFIX 43 H14 2 0.567779 -0.240919 0.147618 11.00000 -1.20000 AFIX 0 C23 1 0.894675 0.557334 0.164666 11.00000 0.09258 0.04647 = 0.05122 -0.01062 0.02107 -0.02063 AFIX 43 H23 2 0.861476 0.617156 0.176366 11.00000 -1.20000 AFIX 0 C20 1 0.995205 0.381272 0.132215 11.00000 0.05899 0.04783 = 0.03771 0.00911 0.00825 -0.01821 C25 1 0.719138 0.502279 0.098548 11.00000 0.07312 0.03530 = 0.06180 -0.00497 0.03534 -0.00255 AFIX 13 H25 2 0.690799 0.443377 0.068942 11.00000 -1.20000 AFIX 0 C17 1 0.629200 -0.046036 0.286780 11.00000 0.05238 0.08518 = 0.03367 0.00707 0.00948 -0.01260 AFIX 43 H17 2 0.645929 0.003350 0.322554 11.00000 -1.20000 AFIX 0 C28 1 1.050700 0.286340 0.116777 11.00000 0.03941 0.06211 = 0.05777 0.01856 0.00246 -0.01403 AFIX 13 H28 2 0.995580 0.238119 0.094067 11.00000 -1.20000 AFIX 0 C24 1 0.835227 0.485254 0.122698 11.00000 0.08161 0.03336 = 0.03800 -0.00347 0.02227 -0.01599 C30 1 1.125816 0.303971 0.064941 11.00000 0.08001 0.07401 = 0.07641 0.01135 0.02716 -0.00578 AFIX 137 H30A 2 1.086165 0.329447 0.020426 11.00000 -1.50000 H30B 2 1.159987 0.240439 0.056553 11.00000 -1.50000 H30C 2 1.179326 0.353302 0.084701 11.00000 -1.50000 AFIX 0 C16 1 0.590665 -0.137978 0.302782 11.00000 0.05398 0.09364 = 0.04268 0.02810 0.01261 -0.00741 AFIX 43 H16 2 0.579613 -0.151673 0.349155 11.00000 -1.20000 AFIX 0 C15 1 0.568233 -0.210018 0.251057 11.00000 0.06062 0.06915 = 0.06374 0.03480 0.01287 -0.00663 AFIX 43 H15 2 0.542548 -0.273869 0.262182 11.00000 -1.20000 AFIX 0 C26 1 0.662476 0.505991 0.161745 11.00000 0.10166 0.06241 = 0.08492 -0.01205 0.06012 -0.01296 AFIX 137 H26A 2 0.680899 0.446261 0.191075 11.00000 -1.50000 H26B 2 0.586341 0.507511 0.145060 11.00000 -1.50000 H26C 2 0.683969 0.566575 0.189498 11.00000 -1.50000 AFIX 0 C29 1 1.109354 0.235916 0.183231 11.00000 0.07457 0.09562 = 0.07550 0.03394 0.00324 0.00952 AFIX 137 H29A 2 1.164282 0.281203 0.206908 11.00000 -1.50000 H29B 2 1.141499 0.173324 0.170643 11.00000 -1.50000 H29C 2 1.059964 0.220825 0.214837 11.00000 -1.50000 AFIX 0 C27 1 0.695153 0.597424 0.053312 11.00000 0.08202 0.05804 = 0.10411 0.02338 0.04129 0.01247 AFIX 137 H27A 2 0.726909 0.655953 0.079759 11.00000 -1.50000 H27B 2 0.618900 0.606842 0.041195 11.00000 -1.50000 H27C 2 0.724362 0.590125 0.010148 11.00000 -1.50000 AFIX 0 O1 6 0.889397 0.097269 0.094920 11.00000 0.03336 0.03861 = 0.03996 0.00180 0.01224 0.00548 C31 1 0.902304 0.016605 0.126685 11.00000 0.04030 0.04416 = 0.03639 -0.00131 0.00824 0.00836 AFIX 43 H31 2 0.851855 -0.001938 0.154583 11.00000 -1.20000 AFIX 0 N5 4 0.980973 -0.045914 0.124830 11.00000 0.06232 0.06062 = 0.05026 0.00379 0.01371 0.03146 C32 1 0.989028 -0.141492 0.162283 11.00000 0.13040 0.07385 = 0.08342 0.02301 0.02986 0.05841 AFIX 137 H32A 2 0.927349 -0.150427 0.184665 11.00000 -1.50000 H32B 2 1.052786 -0.141788 0.198338 11.00000 -1.50000 H32C 2 0.992365 -0.196557 0.129039 11.00000 -1.50000 AFIX 0 C33 1 1.067068 -0.017604 0.089631 11.00000 0.08699 0.12029 = 0.14245 0.02332 0.06412 0.05644 AFIX 137 H33A 2 1.053576 0.049318 0.068698 11.00000 -1.50000 H33B 2 1.072808 -0.066614 0.052626 11.00000 -1.50000 H33C 2 1.132851 -0.016435 0.123844 11.00000 -1.50000 AFIX 0 HKLF 4 REM A in P21/c #14 REM wR2 = 0.1233, GooF = S = 1.082, Restrained GooF = 1.082 for all data REM R1 = 0.0420 for 6081 Fo > 4sig(Fo) and 0.0453 for all 6654 data REM 386 parameters refined using 0 restraints END WGHT 0.0588 2.6461 REM Highest difference peak 0.527, deepest hole -0.518, 1-sigma level 0.070 Q1 1 1.1044 0.4083 0.1708 11.00000 0.05 0.53 Q2 1 0.6491 0.2687 0.1227 11.00000 0.05 0.39 ; _shelx_res_checksum 66595 _shelx_fab_file ; -15 0 2 0.1101 0.1195 -15 0 4 -0.0385 0.0615 -15 0 6 -0.0605 -0.0197 -15 0 8 -0.0962 -0.0367 -15 0 10 -0.1641 -0.0024 -15 0 12 -0.1571 0.0431 -15 1 1 -0.1443 -0.0951 -15 1 2 0.1529 0.0127 -15 1 3 -0.0258 -0.0767 -15 1 4 0.1116 0.0343 -15 1 5 0.0551 -0.0053 -15 1 6 0.0496 0.0162 -15 1 7 0.0863 0.0323 -15 1 8 0.0568 0.0098 -15 1 9 0.1298 0.0114 -15 1 10 0.0215 0.0005 -15 1 11 0.1325 -0.0222 -15 1 12 -0.0421 -0.0176 -15 2 1 -0.2056 -0.0056 -15 2 2 0.0548 0.0304 -15 2 3 -0.2422 -0.0539 -15 2 4 0.0165 0.0085 -15 2 5 -0.1352 -0.0444 -15 2 6 -0.0525 -0.0098 -15 2 7 -0.0706 -0.0127 -15 2 8 -0.1025 -0.0054 -15 2 9 -0.0156 -0.0093 -15 2 10 -0.0710 0.0181 -15 2 11 0.0553 0.0003 -15 2 12 -0.0754 0.0083 -15 3 1 0.0130 0.0152 -15 3 2 0.2238 0.0407 -15 3 3 -0.0715 0.0216 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0.0340 10 5 7 -0.0644 -0.0197 10 5 8 0.3167 0.0274 10 5 9 0.2489 -0.0206 10 5 10 0.2115 0.0397 10 5 11 0.1845 -0.0082 10 5 12 0.0845 0.0595 10 5 13 0.0809 0.0134 10 5 14 -0.0547 0.0545 10 6 0 0.1064 -0.0160 10 6 1 -0.7362 -0.0194 10 6 2 0.2934 -0.0135 10 6 3 -0.7860 -0.0281 10 6 4 0.4154 -0.0054 10 6 5 -0.7306 -0.0313 10 6 6 0.2598 0.0006 10 6 7 -0.6796 -0.0192 10 6 8 -0.0373 0.0044 10 6 9 -0.4656 -0.0225 10 6 10 -0.0884 0.0010 10 6 11 -0.2314 -0.0529 10 6 12 0.0626 -0.0084 10 6 13 -0.0878 -0.0578 10 7 0 0.1887 0.0141 10 7 1 0.4406 -0.0006 10 7 2 0.4034 0.0271 10 7 3 0.0098 0.0084 10 7 4 0.4946 0.0272 10 7 5 -0.1809 0.0128 10 7 6 0.6348 0.0112 10 7 7 -0.1369 0.0135 10 7 8 0.5669 -0.0013 10 7 9 -0.0882 0.0235 10 7 10 0.2736 0.0185 10 7 11 -0.1595 0.0273 10 7 12 0.0823 0.0318 10 7 13 -0.2379 0.0073 10 8 0 -0.8813 0.0120 10 8 1 0.1851 -0.0194 10 8 2 -0.5204 0.0092 10 8 3 0.1704 -0.0338 10 8 4 -0.1931 -0.0024 10 8 5 -0.0672 -0.0216 10 8 6 -0.0035 -0.0107 10 8 7 -0.2937 -0.0017 10 8 8 0.1556 -0.0297 10 8 9 -0.2151 0.0018 10 8 10 0.2475 -0.0436 10 8 11 -0.0150 0.0015 10 8 12 0.2755 -0.0264 10 9 0 -0.2532 -0.0031 10 9 1 0.4459 -0.0121 10 9 2 -0.5608 0.0272 10 9 3 0.3760 -0.0076 10 9 4 -0.5360 0.0339 10 9 5 0.3095 -0.0025 10 9 6 -0.2649 0.0239 10 9 7 0.0773 0.0108 10 9 8 -0.0643 0.0110 10 9 9 -0.1862 0.0286 10 9 10 -0.0661 -0.0089 10 10 0 0.1644 0.0160 10 10 1 0.3311 -0.0199 10 10 2 -0.0096 0.0069 10 10 3 0.5526 -0.0296 10 10 4 -0.2741 0.0048 10 10 5 0.5372 -0.0309 10 10 6 -0.3133 0.0064 10 10 7 0.3843 -0.0278 10 10 8 -0.0627 0.0041 10 10 9 0.2144 -0.0073 10 11 0 -0.0207 0.0394 10 11 1 -0.4454 -0.0234 10 11 2 -0.1481 0.0312 10 11 3 -0.1098 -0.0123 10 11 4 -0.2671 0.0203 10 11 5 0.1862 -0.0119 10 11 6 -0.3526 0.0205 10 11 7 0.1929 -0.0235 10 12 0 0.4635 0.0450 10 12 1 -0.0606 -0.0442 10 12 2 0.3109 0.0419 10 12 3 -0.0679 -0.0179 10 12 4 0.0762 0.0268 11 0 0 0.4158 0.1669 11 0 2 0.3480 0.1355 11 0 4 0.5841 0.0527 11 0 6 0.6704 0.0309 11 0 8 0.3225 0.0388 11 0 10 0.0725 0.0407 11 0 12 0.0145 0.0376 11 0 14 -0.1140 0.0297 11 1 0 -0.0025 -0.0472 11 1 1 -0.2316 -0.1376 11 1 2 0.0084 0.0050 11 1 3 -0.2993 -0.0841 11 1 4 0.0538 0.0083 11 1 5 -0.5066 -0.0423 11 1 6 0.3198 -0.0030 11 1 7 -0.4111 -0.0317 11 1 8 0.4363 -0.0001 11 1 9 -0.1558 -0.0325 11 1 10 0.2993 -0.0147 11 1 11 -0.0818 -0.0238 11 1 12 0.2085 -0.0425 11 1 13 -0.0101 0.0074 11 1 14 0.1375 -0.0338 11 2 0 -0.1225 0.0619 11 2 1 -0.0156 0.0284 11 2 2 -0.0803 0.0559 11 2 3 0.0023 0.0013 11 2 4 0.0227 0.0368 11 2 5 -0.2413 0.0056 11 2 6 0.1298 0.0201 11 2 7 -0.5859 -0.0008 11 2 8 0.1485 0.0118 11 2 9 -0.5168 -0.0048 11 2 10 0.1437 0.0115 11 2 11 -0.3213 0.0055 11 2 12 0.1404 -0.0089 11 2 13 -0.2852 0.0223 11 2 14 0.0663 -0.0346 11 3 0 -0.1363 -0.0346 11 3 1 0.5186 -0.0094 11 3 2 -0.0814 -0.0240 11 3 3 0.3956 -0.0064 11 3 4 -0.0085 -0.0271 11 3 5 0.3217 0.0025 11 3 6 0.3100 -0.0139 11 3 7 0.1020 0.0113 11 3 8 0.4364 0.0007 11 3 9 -0.1172 0.0123 11 3 10 0.2543 0.0051 11 3 11 -0.1598 0.0100 11 3 12 0.2063 -0.0024 11 3 13 -0.1515 0.0106 11 4 0 -0.8647 0.0048 11 4 1 0.2610 0.0124 11 4 2 -0.6602 0.0014 11 4 3 0.2661 0.0363 11 4 4 -0.5832 -0.0137 11 4 5 0.1118 0.0382 11 4 6 -0.4182 -0.0249 11 4 7 -0.0639 0.0196 11 4 8 -0.0345 -0.0277 11 4 9 -0.0324 0.0094 11 4 10 0.1379 -0.0262 11 4 11 0.0398 0.0127 11 4 12 0.0858 -0.0043 11 4 13 -0.0687 0.0306 11 5 0 -0.2163 0.0072 11 5 1 0.6077 -0.0181 11 5 2 -0.4527 -0.0156 11 5 3 0.5551 -0.0092 11 5 4 -0.4254 -0.0374 11 5 5 0.5312 0.0116 11 5 6 -0.3413 -0.0349 11 5 7 0.2299 0.0204 11 5 8 -0.2859 -0.0186 11 5 9 -0.0975 0.0261 11 5 10 -0.2573 -0.0241 11 5 11 -0.0672 0.0143 11 5 12 -0.1951 -0.0466 11 6 0 -0.0204 0.0109 11 6 1 0.2821 0.0070 11 6 2 -0.1540 0.0216 11 6 3 0.4466 0.0219 11 6 4 -0.3196 0.0161 11 6 5 0.4816 0.0310 11 6 6 -0.2782 0.0025 11 6 7 0.5254 0.0170 11 6 8 -0.0022 -0.0051 11 6 9 0.4264 0.0114 11 6 10 0.1031 -0.0022 11 6 11 0.2876 0.0412 11 6 12 -0.0588 0.0116 11 7 0 0.1047 -0.0028 11 7 1 -0.4707 -0.0022 11 7 2 -0.1117 -0.0223 11 7 3 -0.1694 -0.0137 11 7 4 -0.2098 -0.0292 11 7 5 0.0328 -0.0149 11 7 6 -0.4102 -0.0182 11 7 7 0.0167 -0.0102 11 7 8 -0.4761 -0.0007 11 7 9 -0.0622 -0.0200 11 7 10 -0.2831 -0.0141 11 7 11 0.0066 -0.0285 11 8 0 0.6680 -0.0030 11 8 1 -0.1589 0.0104 11 8 2 0.5211 -0.0065 11 8 3 -0.2200 0.0362 11 8 4 0.3239 0.0019 11 8 5 -0.0574 0.0325 11 8 6 0.1977 0.0051 11 8 7 0.2091 0.0148 11 8 8 0.0720 0.0199 11 8 9 0.2089 0.0069 11 8 10 -0.0228 0.0392 11 9 0 0.0017 0.0182 11 9 1 -0.2913 0.0064 11 9 2 0.3018 -0.0246 11 9 3 -0.3196 0.0089 11 9 4 0.3981 -0.0437 11 9 5 -0.3728 0.0075 11 9 6 0.2233 -0.0387 11 9 7 -0.2408 -0.0013 11 9 8 0.0397 -0.0277 11 10 0 -0.2097 -0.0108 11 10 1 -0.0443 0.0129 11 10 2 -0.1144 -0.0068 11 10 3 -0.2696 0.0370 11 10 4 0.1577 -0.0092 11 10 5 -0.3430 0.0452 11 10 6 0.2947 -0.0114 11 10 7 -0.2769 0.0444 11 11 0 -0.0528 -0.0308 11 11 1 0.4291 0.0202 11 11 2 0.0062 -0.0365 11 11 3 0.2206 0.0136 11 11 4 0.0993 -0.0358 11 12 0 -0.3478 -0.0336 12 0 0 -0.2460 -0.0761 12 0 2 -0.1959 -0.0989 12 0 4 -0.4148 -0.0350 12 0 6 -0.5419 -0.0085 12 0 8 -0.2665 -0.0240 12 0 10 -0.0908 -0.0367 12 0 12 -0.1197 -0.0361 12 1 0 0.0832 0.0770 12 1 1 0.1146 0.0847 12 1 2 0.0759 0.0255 12 1 3 0.1585 0.0594 12 1 4 0.0476 0.0061 12 1 5 0.3639 0.0232 12 1 6 -0.1934 0.0140 12 1 7 0.3237 0.0174 12 1 8 -0.3064 0.0084 12 1 9 0.1280 0.0266 12 1 10 -0.1711 0.0092 12 1 11 0.1228 0.0253 12 1 12 -0.1025 0.0331 12 2 0 0.1228 -0.0292 12 2 1 -0.0901 -0.0601 12 2 2 0.1377 -0.0299 12 2 3 -0.1205 -0.0227 12 2 4 0.0784 -0.0198 12 2 5 0.0687 -0.0226 12 2 6 -0.0358 -0.0113 12 2 7 0.3875 -0.0179 12 2 8 -0.0866 -0.0057 12 2 9 0.3247 -0.0020 12 2 10 -0.1093 -0.0071 12 2 11 0.1349 0.0031 12 2 12 -0.1502 0.0069 12 3 0 0.1469 0.0418 12 3 1 -0.4424 -0.0003 12 3 2 0.1109 0.0285 12 3 3 -0.4086 -0.0024 12 3 4 0.1030 0.0353 12 3 5 -0.3766 -0.0031 12 3 6 -0.1475 0.0294 12 3 7 -0.1752 -0.0113 12 3 8 -0.2775 0.0085 12 3 9 0.0380 -0.0188 12 3 10 -0.0984 -0.0106 12 3 11 0.0845 -0.0170 12 3 12 -0.0415 -0.0136 12 4 0 0.6371 -0.0006 12 4 1 -0.1079 0.0035 12 4 2 0.5663 -0.0022 12 4 3 -0.1737 -0.0235 12 4 4 0.5576 0.0045 12 4 5 -0.1209 -0.0390 12 4 6 0.4628 0.0164 12 4 7 0.0216 -0.0217 12 4 8 0.1318 0.0281 12 4 9 -0.0004 -0.0013 12 4 10 -0.0369 0.0342 12 4 11 -0.1161 0.0047 12 5 0 -0.0727 -0.0216 12 5 1 -0.4666 0.0128 12 5 2 0.1566 -0.0070 12 5 3 -0.4570 0.0197 12 5 4 0.2207 0.0232 12 5 5 -0.5006 0.0019 12 5 6 0.2070 0.0289 12 5 7 -0.3009 -0.0151 12 5 8 0.1751 0.0089 12 5 9 0.0072 -0.0284 12 5 10 0.1968 0.0057 12 5 11 0.0167 -0.0233 12 6 0 0.0284 0.0016 12 6 1 0.0504 0.0096 12 6 2 0.1044 -0.0215 12 6 3 -0.1243 -0.0050 12 6 4 0.2420 -0.0256 12 6 5 -0.2008 -0.0212 12 6 6 0.2715 -0.0080 12 6 7 -0.2924 -0.0120 12 6 8 0.0432 0.0064 12 6 9 -0.2739 0.0005 12 6 10 -0.1179 0.0092 12 7 0 -0.2508 -0.0121 12 7 1 0.3052 -0.0011 12 7 2 -0.0908 0.0082 12 7 3 0.1483 0.0153 12 7 4 -0.0273 0.0198 12 7 5 0.0004 0.0178 12 7 6 0.1594 0.0175 12 7 7 0.0128 0.0066 12 7 8 0.2989 0.0006 12 7 9 0.1345 0.0095 12 8 0 -0.3524 -0.0024 12 8 1 0.1311 0.0066 12 8 2 -0.3220 0.0052 12 8 3 0.2133 -0.0256 12 8 4 -0.2480 -0.0028 12 8 5 0.1342 -0.0308 12 8 6 -0.2108 -0.0025 12 8 7 -0.1109 -0.0192 12 9 0 0.0747 -0.0348 12 9 1 0.1020 -0.0005 12 9 2 -0.1190 0.0097 12 9 3 0.1506 -0.0070 12 9 4 -0.2391 0.0385 12 9 5 0.2723 -0.0077 12 9 6 -0.1427 0.0395 12 10 0 0.1633 0.0051 12 10 1 -0.0606 0.0040 12 10 2 0.1673 0.0020 12 10 3 0.0776 -0.0284 13 0 0 0.1798 -0.0105 13 0 2 0.1160 0.0426 13 0 4 0.2873 0.0005 13 0 6 0.4237 -0.0242 13 0 8 0.1936 -0.0006 13 0 10 0.0370 0.0248 13 1 0 -0.1086 -0.0804 13 1 1 -0.0828 -0.0280 13 1 2 -0.1096 -0.0417 13 1 3 -0.0806 -0.0219 13 1 4 -0.0983 -0.0163 13 1 5 -0.2505 0.0067 13 1 6 0.1189 -0.0228 13 1 7 -0.2403 0.0058 13 1 8 0.2372 -0.0172 13 1 9 -0.0740 -0.0132 13 1 10 0.1073 -0.0053 13 2 0 -0.0450 0.0033 13 2 1 0.1277 0.0651 13 2 2 -0.1118 0.0056 13 2 3 0.1642 0.0268 13 2 4 -0.1197 -0.0005 13 2 5 0.0230 0.0276 13 2 6 -0.0275 -0.0016 13 2 7 -0.2710 0.0296 13 2 8 0.0433 -0.0023 13 2 9 -0.2296 0.0090 13 2 10 0.0737 0.0019 13 3 0 -0.1490 -0.0366 13 3 1 0.2871 0.0054 13 3 2 -0.1009 -0.0164 13 3 3 0.3382 0.0075 13 3 4 -0.1257 -0.0254 13 3 5 0.3667 0.0022 13 3 6 0.0563 -0.0315 13 3 7 0.1941 0.0074 13 3 8 0.1904 -0.0134 13 3 9 -0.0135 0.0190 13 4 0 -0.3837 -0.0064 13 4 1 0.0315 -0.0181 13 4 2 -0.4046 0.0017 13 4 3 0.0825 -0.0002 13 4 4 -0.4575 0.0053 13 4 5 0.0975 0.0257 13 4 6 -0.4264 -0.0032 13 4 7 -0.0038 0.0171 13 4 8 -0.1540 -0.0196 13 4 9 -0.0168 -0.0058 13 5 0 0.1395 0.0226 13 5 1 0.3116 0.0005 13 5 2 0.0082 0.0261 13 5 3 0.3337 -0.0228 13 5 4 -0.0677 -0.0018 13 5 5 0.4108 -0.0148 13 5 6 -0.0991 -0.0162 13 5 7 0.3044 0.0045 13 5 8 -0.0666 0.0003 13 6 0 -0.0221 -0.0188 13 6 1 -0.1649 -0.0175 13 6 2 -0.0919 0.0108 13 6 3 -0.0533 -0.0120 13 6 4 -0.1901 0.0284 13 6 5 0.0121 0.0059 13 6 6 -0.2576 0.0144 13 6 7 0.0995 0.0051 13 7 0 0.2553 0.0185 13 7 1 -0.1407 0.0112 13 7 2 0.1633 0.0048 13 7 3 -0.0498 -0.0093 13 7 4 0.1448 -0.0051 13 7 5 0.0475 -0.0190 13 7 6 0.0174 -0.0103 13 8 0 0.1601 0.0004 13 8 1 -0.1273 -0.0205 13 8 2 0.1212 -0.0089 13 8 3 -0.1848 0.0093 13 8 4 0.0907 0.0021 13 9 0 -0.0114 0.0424 13 9 1 -0.0128 -0.0001 13 9 2 0.0679 0.0086 14 0 0 -0.1633 0.0638 14 0 2 -0.0734 0.0037 14 0 4 -0.1809 0.0306 14 0 6 -0.3213 0.0530 14 1 0 0.1023 0.0644 14 1 1 0.0852 -0.0100 14 1 2 0.1081 0.0411 14 1 3 0.0341 -0.0070 14 1 4 0.1214 0.0180 14 1 5 0.1553 -0.0312 14 1 6 -0.0596 0.0264 14 1 7 0.1778 -0.0269 14 2 0 -0.0245 0.0115 14 2 1 -0.1246 -0.0514 14 2 2 0.0606 0.0078 14 2 3 -0.1657 -0.0157 14 2 4 0.1289 0.0131 14 2 5 -0.0801 -0.0193 14 2 6 0.0730 0.0107 14 2 7 0.1761 -0.0310 14 3 0 0.1510 0.0292 14 3 1 -0.1460 -0.0092 14 3 2 0.0848 -0.0009 14 3 3 -0.2400 -0.0088 14 3 4 0.1231 0.0046 14 3 5 -0.3254 0.0008 14 3 6 0.0149 0.0210 14 4 0 0.1903 0.0189 14 4 1 -0.0252 0.0206 14 4 2 0.2441 0.0049 14 4 3 -0.0340 0.0204 14 4 4 0.3316 -0.0099 14 4 5 -0.0875 -0.0065 14 5 0 -0.0910 -0.0084 14 5 1 -0.1639 -0.0204 14 5 2 -0.0464 -0.0296 14 5 3 -0.2057 0.0143 14 5 4 0.0047 -0.0143 14 5 5 -0.2891 0.0197 14 6 0 -0.0471 0.0350 14 6 1 0.1438 0.0104 14 6 2 0.0493 0.0079 14 6 3 0.0932 0.0179 14 6 4 0.1238 -0.0207 14 7 0 -0.2037 -0.0119 14 7 1 0.0989 -0.0232 14 7 2 -0.1542 -0.0077 15 0 0 0.1775 -0.0758 15 0 2 0.0598 -0.0238 15 1 0 -0.0830 -0.0426 15 1 1 -0.1050 0.0220 15 1 2 -0.0776 -0.0298 15 1 3 -0.0046 0.0165 15 2 0 0.0654 -0.0161 15 2 1 0.0912 0.0334 15 2 2 -0.0133 -0.0099 15 2 3 0.1226 -0.0005 15 3 0 -0.1306 -0.0265 15 3 1 0.0564 0.0148 15 3 2 -0.0461 0.0115 15 4 0 -0.0780 -0.0337 15 4 1 0.0173 -0.0103 15 4 2 -0.1276 -0.0182 15 5 0 0.0604 -0.0110 15 5 1 0.0525 0.0405 0 0 0 0.0 0.0 ; _shelx_fab_checksum 31074 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.75772(3) 0.19286(3) 0.09717(2) 0.02767(11) Uani 1 1 d . . . . . Cl1 Cl 0.80026(5) 0.20987(4) 0.21637(3) 0.04084(15) Uani 1 1 d . . . . . Cl2 Cl 0.59026(5) 0.26843(4) 0.08350(3) 0.04447(15) Uani 1 1 d . . . . . N4 N 0.60815(14) -0.06727(14) -0.02261(9) 0.0329(4) Uani 1 1 d . . . . . N2 N 0.73279(13) 0.17507(13) -0.00790(9) 0.0281(3) Uani 1 1 d . . . . . N1 N 0.83257(14) 0.32176(13) 0.06200(9) 0.0319(4) Uani 1 1 d . . . . . C12 C 0.68458(15) 0.09396(15) -0.03899(10) 0.0282(4) Uani 1 1 d . . . . . N3 N 0.66689(13) 0.02026(13) 0.07560(9) 0.0298(4) Uani 1 1 d . . . . . C11 C 0.65521(15) 0.01891(16) 0.00627(10) 0.0290(4) Uani 1 1 d . . . . . C6 C 0.66258(16) 0.08058(17) -0.11240(11) 0.0326(4) Uani 1 1 d . . . . . C3 C 0.76265(17) 0.24839(16) -0.04691(11) 0.0311(4) Uani 1 1 d . . . . . C2 C 0.81980(18) 0.33119(16) -0.00490(11) 0.0339(4) Uani 1 1 d . . . . . C10 C 0.62516(16) -0.07020(17) 0.09274(11) 0.0334(4) Uani 1 1 d . . . . . C5 C 0.69219(18) 0.15974(19) -0.15300(11) 0.0378(5) Uani 1 1 d . . . . . H5 H 0.677638 0.155737 -0.202875 0.045 Uiso 1 1 calc R U . . . C9 C 0.58818(18) -0.12503(18) 0.03291(12) 0.0374(5) Uani 1 1 d . . . . . H11 H 0.555644 -0.189327 0.030394 0.045 Uiso 1 1 calc R U . . . C25 C 0.61946(17) -0.09587(18) 0.16603(12) 0.0376(5) Uani 1 1 d . . . . . C4 C 0.74233(18) 0.24314(18) -0.12047(11) 0.0365(5) Uani 1 1 d . . . . . H4 H 0.762918 0.296582 -0.147693 0.044 Uiso 1 1 calc R U . . . C8 C 0.58728(18) -0.08286(19) -0.09525(12) 0.0396(5) Uani 1 1 d . . . . . H10 H 0.554581 -0.143411 -0.113925 0.048 Uiso 1 1 calc R U . . . C13 C 0.8893(2) 0.39808(17) 0.10631(12) 0.0401(5) Uani 1 1 d . . . . . C30 C 0.6439(2) -0.0246(2) 0.21863(13) 0.0459(6) Uani 1 1 d . . . . . H18 H 0.670854 0.039038 0.208244 0.055 Uiso 1 1 calc R U . . . C1 C 0.8596(2) 0.4169(2) -0.04318(13) 0.0514(7) Uani 1 1 d . . . . . H1A H 0.799972 0.454001 -0.069735 0.077 Uiso 1 1 calc R U . . . H1B H 0.903292 0.390674 -0.075641 0.077 Uiso 1 1 calc R U . . . H1C H 0.901658 0.462090 -0.009185 0.077 Uiso 1 1 calc R U . . . C7 C 0.61341(18) -0.01238(19) -0.13852(12) 0.0386(5) Uani 1 1 d . . . . . H9 H 0.599109 -0.024039 -0.187803 0.046 Uiso 1 1 calc R U . . . C15 C 1.0500(3) 0.4581(3) 0.17435(15) 0.0631(8) Uani 1 1 d . . . . . H21 H 1.122848 0.450282 0.192503 0.076 Uiso 1 1 calc R U . . . C16 C 0.9991(3) 0.5440(2) 0.18926(16) 0.0680(9) Uani 1 1 d . . . . . H22 H 1.037446 0.595035 0.217237 0.082 Uiso 1 1 calc R U . . . C26 C 0.5827(2) -0.1904(2) 0.18278(15) 0.0503(6) Uani 1 1 d . . . . . H14 H 0.567779 -0.240919 0.147618 0.060 Uiso 1 1 calc R U . . . C17 C 0.8947(3) 0.5573(2) 0.16467(16) 0.0624(8) Uani 1 1 d . . . . . H23 H 0.861476 0.617156 0.176366 0.075 Uiso 1 1 calc R U . . . C14 C 0.9952(2) 0.3813(2) 0.13221(13) 0.0482(6) Uani 1 1 d . . . . . C22 C 0.7191(3) 0.5023(2) 0.09855(16) 0.0539(7) Uani 1 1 d . . . . . H25 H 0.690799 0.443377 0.068942 0.065 Uiso 1 1 calc R U . . . C29 C 0.6292(2) -0.0460(3) 0.28678(14) 0.0569(7) Uani 1 1 d . . . . . H17 H 0.645929 0.003350 0.322554 0.068 Uiso 1 1 calc R U . . . C19 C 1.0507(2) 0.2863(2) 0.11678(16) 0.0539(7) Uani 1 1 d . . . . . H28 H 0.995580 0.238119 0.094067 0.065 Uiso 1 1 calc R U . . . C18 C 0.8352(2) 0.48525(19) 0.12270(13) 0.0496(6) Uani 1 1 d . . . . . C21 C 1.1258(3) 0.3040(3) 0.0649(2) 0.0752(10) Uani 1 1 d . . . . . H30A H 1.086165 0.329447 0.020426 0.113 Uiso 1 1 calc R U . . . H30B H 1.159987 0.240439 0.056553 0.113 Uiso 1 1 calc R U . . . H30C H 1.179326 0.353302 0.084701 0.113 Uiso 1 1 calc R U . . . C28 C 0.5907(2) -0.1380(3) 0.30278(15) 0.0629(8) Uani 1 1 d . . . . . H16 H 0.579613 -0.151673 0.349155 0.076 Uiso 1 1 calc R U . . . C27 C 0.5682(3) -0.2100(3) 0.25106(17) 0.0643(9) Uani 1 1 d . . . . . H15 H 0.542548 -0.273869 0.262182 0.077 Uiso 1 1 calc R U . . . C23 C 0.6625(3) 0.5060(3) 0.1617(2) 0.0777(11) Uani 1 1 d . . . . . H26A H 0.680899 0.446261 0.191075 0.116 Uiso 1 1 calc R U . . . H26B H 0.586341 0.507511 0.145060 0.116 Uiso 1 1 calc R U . . . H26C H 0.683969 0.566575 0.189498 0.116 Uiso 1 1 calc R U . . . C20 C 1.1094(3) 0.2359(3) 0.1832(2) 0.0831(11) Uani 1 1 d . . . . . H29A H 1.164282 0.281203 0.206908 0.125 Uiso 1 1 calc R U . . . H29B H 1.141499 0.173324 0.170643 0.125 Uiso 1 1 calc R U . . . H29C H 1.059964 0.220825 0.214837 0.125 Uiso 1 1 calc R U . . . C24 C 0.6952(3) 0.5974(3) 0.0533(2) 0.0784(10) Uani 1 1 d . . . . . H27A H 0.726909 0.655953 0.079759 0.118 Uiso 1 1 calc R U . . . H27B H 0.618900 0.606842 0.041195 0.118 Uiso 1 1 calc R U . . . H27C H 0.724362 0.590125 0.010148 0.118 Uiso 1 1 calc R U . . . O1 O 0.88940(12) 0.09727(12) 0.09492(8) 0.0366(3) Uani 1 1 d . . . . . C31 C 0.90230(19) 0.01660(19) 0.12669(12) 0.0401(5) Uani 1 1 d . . . . . H31 H 0.851855 -0.001938 0.154583 0.048 Uiso 1 1 calc R U . . . N5 N 0.9810(2) -0.04591(19) 0.12483(12) 0.0573(6) Uani 1 1 d . . . . . C32 C 0.9890(4) -0.1415(3) 0.1623(2) 0.0946(14) Uani 1 1 d . . . . . H32A H 0.927349 -0.150427 0.184665 0.142 Uiso 1 1 calc R U . . . H32B H 1.052786 -0.141788 0.198338 0.142 Uiso 1 1 calc R U . . . H32C H 0.992365 -0.196557 0.129039 0.142 Uiso 1 1 calc R U . . . C33 C 1.0671(4) -0.0176(4) 0.0896(3) 0.1112(18) Uani 1 1 d . . . . . H33A H 1.053576 0.049318 0.068698 0.167 Uiso 1 1 calc R U . . . H33B H 1.072808 -0.066614 0.052626 0.167 Uiso 1 1 calc R U . . . H33C H 1.132851 -0.016435 0.123844 0.167 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 0.0330(2) 0.0296(2) 0.02267(18) -0.00013(13) 0.01096(14) 0.00010(14) Cl1 0.0554(3) 0.0446(3) 0.0236(2) -0.0028(2) 0.0101(2) -0.0003(2) Cl2 0.0390(3) 0.0374(3) 0.0605(4) -0.0046(2) 0.0184(3) 0.0014(2) N4 0.0325(9) 0.0338(9) 0.0336(9) -0.0036(7) 0.0098(7) -0.0017(7) N2 0.0308(8) 0.0297(8) 0.0255(8) 0.0000(6) 0.0098(6) 0.0020(7) N1 0.0395(10) 0.0292(9) 0.0298(9) 0.0004(7) 0.0135(7) -0.0036(7) C12 0.0277(9) 0.0331(10) 0.0254(9) -0.0017(8) 0.0088(7) 0.0042(8) N3 0.0295(8) 0.0336(9) 0.0275(8) 0.0020(7) 0.0088(7) 0.0018(7) C11 0.0285(10) 0.0313(10) 0.0284(9) -0.0037(8) 0.0084(8) 0.0007(8) C6 0.0303(10) 0.0425(12) 0.0265(10) -0.0054(8) 0.0090(8) 0.0034(9) C3 0.0356(11) 0.0324(10) 0.0274(10) 0.0025(8) 0.0112(8) 0.0027(8) C2 0.0408(11) 0.0322(11) 0.0316(10) 0.0031(8) 0.0146(9) -0.0028(9) C10 0.0289(10) 0.0354(11) 0.0372(11) 0.0044(9) 0.0093(8) 0.0023(8) C5 0.0419(12) 0.0496(13) 0.0237(10) 0.0013(9) 0.0107(8) 0.0043(10) C9 0.0367(11) 0.0339(11) 0.0431(12) 0.0006(9) 0.0111(9) -0.0030(9) C25 0.0309(10) 0.0454(13) 0.0374(11) 0.0115(10) 0.0082(9) 0.0023(9) C4 0.0434(12) 0.0411(12) 0.0275(10) 0.0051(9) 0.0133(9) 0.0026(10) C8 0.0408(12) 0.0440(13) 0.0351(11) -0.0131(10) 0.0092(9) -0.0051(10) C13 0.0546(14) 0.0355(12) 0.0323(11) 0.0005(9) 0.0137(10) -0.0165(10) C30 0.0421(13) 0.0607(16) 0.0358(12) 0.0077(11) 0.0094(10) -0.0106(11) C1 0.0740(18) 0.0452(14) 0.0377(12) 0.0089(11) 0.0168(12) -0.0180(13) C7 0.0384(11) 0.0498(13) 0.0291(10) -0.0103(9) 0.0100(9) -0.0026(10) C15 0.0682(19) 0.070(2) 0.0472(15) 0.0118(14) 0.0007(13) -0.0308(16) C16 0.104(3) 0.0525(17) 0.0472(16) -0.0072(13) 0.0136(16) -0.0315(18) C26 0.0507(15) 0.0485(15) 0.0530(15) 0.0161(12) 0.0129(12) 0.0005(12) C17 0.093(2) 0.0465(15) 0.0512(16) -0.0106(13) 0.0211(16) -0.0206(16) C14 0.0590(15) 0.0478(14) 0.0377(12) 0.0091(10) 0.0083(11) -0.0182(12) C22 0.0731(18) 0.0353(13) 0.0618(17) -0.0050(11) 0.0353(14) -0.0025(12) C29 0.0524(15) 0.085(2) 0.0337(12) 0.0071(13) 0.0095(11) -0.0126(15) C19 0.0394(13) 0.0621(17) 0.0578(16) 0.0186(13) 0.0025(12) -0.0140(12) C18 0.0816(19) 0.0334(12) 0.0380(12) -0.0035(10) 0.0223(12) -0.0160(12) C21 0.080(2) 0.074(2) 0.076(2) 0.0113(18) 0.0272(19) -0.0058(18) C28 0.0540(16) 0.094(2) 0.0427(14) 0.0281(16) 0.0126(12) -0.0074(16) C27 0.0606(18) 0.069(2) 0.0637(19) 0.0348(16) 0.0129(15) -0.0066(15) C23 0.102(3) 0.062(2) 0.085(2) -0.0121(17) 0.060(2) -0.0130(19) C20 0.075(2) 0.096(3) 0.076(2) 0.034(2) 0.0032(19) 0.010(2) C24 0.082(2) 0.0580(19) 0.104(3) 0.0234(19) 0.041(2) 0.0125(17) O1 0.0334(8) 0.0386(8) 0.0400(8) 0.0018(7) 0.0122(6) 0.0055(6) C31 0.0403(12) 0.0442(13) 0.0364(11) -0.0013(10) 0.0082(9) 0.0084(10) N5 0.0623(14) 0.0606(14) 0.0503(13) 0.0038(11) 0.0137(11) 0.0315(12) C32 0.130(4) 0.074(2) 0.083(3) 0.023(2) 0.030(2) 0.058(3) C33 0.087(3) 0.120(4) 0.142(4) 0.023(3) 0.064(3) 0.056(3) 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' O O 0.0492 0.0322 '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 Cl1 Ni1 Cl2 97.01(2) . . ? N2 Ni1 Cl1 175.25(5) . . ? N2 Ni1 Cl2 87.62(5) . . ? N2 Ni1 N1 76.91(7) . . ? N2 Ni1 O1 83.92(6) . . ? N1 Ni1 Cl1 101.55(5) . . ? N1 Ni1 Cl2 94.69(5) . . ? O1 Ni1 Cl1 91.72(5) . . ? O1 Ni1 Cl2 166.52(5) . . ? O1 Ni1 N1 93.60(7) . . ? C11 N4 C9 106.25(17) . . ? C11 N4 C8 121.74(19) . . ? C9 N4 C8 132.0(2) . . ? C12 N2 Ni1 121.84(13) . . ? C3 N2 Ni1 118.36(14) . . ? C3 N2 C12 119.76(17) . . ? C2 N1 Ni1 114.55(15) . . ? C2 N1 C13 119.44(18) . . ? C13 N1 Ni1 125.93(13) . . ? N2 C12 C11 116.40(17) . . ? N2 C12 C6 123.40(19) . . ? C6 C12 C11 120.20(19) . . ? C11 N3 C10 104.62(17) . . ? N4 C11 C12 118.98(18) . . ? N3 C11 N4 112.76(18) . . ? N3 C11 C12 128.26(19) . . ? C12 C6 C7 117.3(2) . . ? C5 C6 C12 116.2(2) . . ? C5 C6 C7 126.44(19) . . ? N2 C3 C2 113.56(17) . . ? N2 C3 C4 121.2(2) . . ? C4 C3 C2 125.26(19) . . ? N1 C2 C3 116.23(18) . . ? N1 C2 C1 125.4(2) . . ? C3 C2 C1 118.37(19) . . ? N3 C10 C25 121.4(2) . . ? C9 C10 N3 110.54(19) . . ? C9 C10 C25 128.0(2) . . ? C6 C5 H5 120.0 . . ? C4 C5 C6 120.01(19) . . ? C4 C5 H5 120.0 . . ? N4 C9 H11 127.1 . . ? C10 C9 N4 105.83(19) . . ? C10 C9 H11 127.1 . . ? C30 C25 C10 120.3(2) . . ? C30 C25 C26 119.1(2) . . ? C26 C25 C10 120.5(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4 120.3 . . ? N4 C8 H10 120.0 . . ? C7 C8 N4 119.9(2) . . ? C7 C8 H10 120.0 . . ? C14 C13 N1 117.7(2) . . ? C14 C13 C18 123.0(2) . . ? C18 C13 N1 119.2(2) . . ? C25 C30 H18 119.9 . . ? C25 C30 C29 120.2(3) . . ? C29 C30 H18 119.9 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C6 C7 H9 119.1 . . ? C8 C7 C6 121.8(2) . . ? C8 C7 H9 119.1 . . ? C16 C15 H21 119.6 . . ? C16 C15 C14 120.7(3) . . ? C14 C15 H21 119.6 . . ? C15 C16 H22 119.4 . . ? C17 C16 C15 121.2(3) . . ? C17 C16 H22 119.4 . . ? C25 C26 H14 120.1 . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H14 120.1 . . ? C16 C17 H23 119.2 . . ? C16 C17 C18 121.6(3) . . ? C18 C17 H23 119.2 . . ? C13 C14 C15 116.8(3) . . ? C13 C14 C19 122.4(2) . . ? C15 C14 C19 120.7(3) . . ? C18 C22 H25 107.6 . . ? C18 C22 C23 110.4(3) . . ? C18 C22 C24 112.9(3) . . ? C23 C22 H25 107.6 . . ? C23 C22 C24 110.5(3) . . ? C24 C22 H25 107.6 . . ? C30 C29 H17 119.7 . . ? C28 C29 C30 120.7(3) . . ? C28 C29 H17 119.7 . . ? C14 C19 H28 107.2 . . ? C14 C19 C21 112.4(2) . . ? C14 C19 C20 112.6(3) . . ? C21 C19 H28 107.2 . . ? C20 C19 H28 107.2 . . ? C20 C19 C21 109.9(3) . . ? C13 C18 C22 123.9(2) . . ? C17 C18 C13 116.7(3) . . ? C17 C18 C22 119.5(3) . . ? C19 C21 H30A 109.5 . . ? C19 C21 H30B 109.5 . . ? C19 C21 H30C 109.5 . . ? H30A C21 H30B 109.5 . . ? H30A C21 H30C 109.5 . . ? H30B C21 H30C 109.5 . . ? C29 C28 H16 120.3 . . ? C29 C28 C27 119.5(3) . . ? C27 C28 H16 120.3 . . ? C26 C27 H15 119.6 . . ? C28 C27 C26 120.8(3) . . ? C28 C27 H15 119.6 . . ? C22 C23 H26A 109.5 . . ? C22 C23 H26B 109.5 . . ? C22 C23 H26C 109.5 . . ? H26A C23 H26B 109.5 . . ? H26A C23 H26C 109.5 . . ? H26B C23 H26C 109.5 . . ? C19 C20 H29A 109.5 . . ? C19 C20 H29B 109.5 . . ? C19 C20 H29C 109.5 . . ? H29A C20 H29B 109.5 . . ? H29A C20 H29C 109.5 . . ? H29B C20 H29C 109.5 . . ? C22 C24 H27A 109.5 . . ? C22 C24 H27B 109.5 . . ? C22 C24 H27C 109.5 . . ? H27A C24 H27B 109.5 . . ? H27A C24 H27C 109.5 . . ? H27B C24 H27C 109.5 . . ? C31 O1 Ni1 123.13(15) . . ? O1 C31 H31 117.6 . . ? O1 C31 N5 124.8(2) . . ? N5 C31 H31 117.6 . . ? C31 N5 C32 121.5(3) . . ? C31 N5 C33 120.5(3) . . ? C33 N5 C32 117.7(3) . . ? N5 C32 H32A 109.5 . . ? N5 C32 H32B 109.5 . . ? N5 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 H33A 109.5 . . ? N5 C33 H33B 109.5 . . ? N5 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 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 Cl1 2.2824(6) . ? Ni1 Cl2 2.3588(7) . ? Ni1 N2 2.0124(17) . ? Ni1 N1 2.1377(17) . ? Ni1 O1 2.1313(15) . ? N4 C11 1.369(3) . ? N4 C9 1.381(3) . ? N4 C8 1.397(3) . ? N2 C12 1.334(3) . ? N2 C3 1.331(3) . ? N1 C2 1.280(3) . ? N1 C13 1.441(3) . ? C12 C11 1.422(3) . ? C12 C6 1.408(3) . ? N3 C11 1.322(3) . ? N3 C10 1.382(3) . ? C6 C5 1.406(3) . ? C6 C7 1.439(3) . ? C3 C2 1.484(3) . ? C3 C4 1.401(3) . ? C2 C1 1.499(3) . ? C10 C9 1.378(3) . ? C10 C25 1.471(3) . ? C5 H5 0.9500 . ? C5 C4 1.378(3) . ? C9 H11 0.9500 . ? C25 C30 1.384(4) . ? C25 C26 1.402(3) . ? C4 H4 0.9500 . ? C8 H10 0.9500 . ? C8 C7 1.339(3) . ? C13 C14 1.389(4) . ? C13 C18 1.418(4) . ? C30 H18 0.9500 . ? C30 C29 1.393(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C7 H9 0.9500 . ? C15 H21 0.9500 . ? C15 C16 1.374(5) . ? C15 C14 1.416(4) . ? C16 H22 0.9500 . ? C16 C17 1.360(5) . ? C26 H14 0.9500 . ? C26 C27 1.390(4) . ? C17 H23 0.9500 . ? C17 C18 1.394(4) . ? C14 C19 1.508(4) . ? C22 H25 1.0000 . ? C22 C18 1.508(4) . ? C22 C23 1.533(4) . ? C22 C24 1.537(4) . ? C29 H17 0.9500 . ? C29 C28 1.376(5) . ? C19 H28 1.0000 . ? C19 C21 1.533(4) . ? C19 C20 1.525(4) . ? C21 H30A 0.9800 . ? C21 H30B 0.9800 . ? C21 H30C 0.9800 . ? C28 H16 0.9500 . ? C28 C27 1.377(5) . ? C27 H15 0.9500 . ? C23 H26A 0.9800 . ? C23 H26B 0.9800 . ? C23 H26C 0.9800 . ? C20 H29A 0.9800 . ? C20 H29B 0.9800 . ? C20 H29C 0.9800 . ? C24 H27A 0.9800 . ? C24 H27B 0.9800 . ? C24 H27C 0.9800 . ? O1 C31 1.232(3) . ? C31 H31 0.9500 . ? C31 N5 1.319(3) . ? N5 C32 1.457(4) . ? N5 C33 1.454(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 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 -2.3(2) . . . . ? Ni1 N2 C12 C6 177.73(15) . . . . ? Ni1 N2 C3 C2 5.0(2) . . . . ? Ni1 N2 C3 C4 -176.43(16) . . . . ? Ni1 N1 C2 C3 -4.3(3) . . . . ? Ni1 N1 C2 C1 177.1(2) . . . . ? Ni1 N1 C13 C14 86.5(2) . . . . ? Ni1 N1 C13 C18 -92.3(2) . . . . ? Ni1 O1 C31 N5 177.8(2) . . . . ? N4 C8 C7 C6 -0.3(4) . . . . ? N2 C12 C11 N4 -178.17(17) . . . . ? N2 C12 C11 N3 2.1(3) . . . . ? N2 C12 C6 C5 -1.5(3) . . . . ? N2 C12 C6 C7 177.86(19) . . . . ? N2 C3 C2 N1 -0.1(3) . . . . ? N2 C3 C2 C1 178.5(2) . . . . ? N2 C3 C4 C5 -1.2(3) . . . . ? N1 C13 C14 C15 178.6(2) . . . . ? N1 C13 C14 C19 -1.3(3) . . . . ? N1 C13 C18 C17 -178.8(2) . . . . ? N1 C13 C18 C22 2.3(3) . . . . ? C12 N2 C3 C2 -177.16(18) . . . . ? C12 N2 C3 C4 1.4(3) . . . . ? C12 C6 C5 C4 1.7(3) . . . . ? C12 C6 C7 C8 1.4(3) . . . . ? N3 C10 C9 N4 0.4(2) . . . . ? N3 C10 C25 C30 8.0(3) . . . . ? N3 C10 C25 C26 -176.1(2) . . . . ? C11 N4 C9 C10 -0.3(2) . . . . ? C11 N4 C8 C7 -0.1(3) . . . . ? C11 C12 C6 C5 178.51(19) . . . . ? C11 C12 C6 C7 -2.1(3) . . . . ? C11 N3 C10 C9 -0.3(2) . . . . ? C11 N3 C10 C25 -177.49(19) . . . . ? C6 C12 C11 N4 1.8(3) . . . . ? C6 C12 C11 N3 -177.9(2) . . . . ? C6 C5 C4 C3 -0.4(3) . . . . ? C3 N2 C12 C11 179.95(18) . . . . ? C3 N2 C12 C6 0.0(3) . . . . ? C2 N1 C13 C14 -96.9(3) . . . . ? C2 N1 C13 C18 84.4(3) . . . . ? C2 C3 C4 C5 177.2(2) . . . . ? C10 N3 C11 N4 0.1(2) . . . . ? C10 N3 C11 C12 179.8(2) . . . . ? C10 C25 C30 C29 174.0(2) . . . . ? C10 C25 C26 C27 -173.8(2) . . . . ? C5 C6 C7 C8 -179.3(2) . . . . ? C9 N4 C11 C12 -179.61(18) . . . . ? C9 N4 C11 N3 0.2(2) . . . . ? C9 N4 C8 C7 178.5(2) . . . . ? C9 C10 C25 C30 -168.7(2) . . . . ? C9 C10 C25 C26 7.2(4) . . . . ? C25 C10 C9 N4 177.4(2) . . . . ? C25 C30 C29 C28 0.2(4) . . . . ? C25 C26 C27 C28 -0.7(5) . . . . ? C4 C3 C2 N1 -178.6(2) . . . . ? C4 C3 C2 C1 0.0(3) . . . . ? C8 N4 C11 C12 -0.7(3) . . . . ? C8 N4 C11 N3 179.07(19) . . . . ? C8 N4 C9 C10 -179.1(2) . . . . ? C13 N1 C2 C3 178.7(2) . . . . ? C13 N1 C2 C1 0.1(4) . . . . ? C13 C14 C19 C21 107.5(3) . . . . ? C13 C14 C19 C20 -127.9(3) . . . . ? C30 C25 C26 C27 2.1(4) . . . . ? C30 C29 C28 C27 1.1(5) . . . . ? C7 C6 C5 C4 -177.6(2) . . . . ? C15 C16 C17 C18 -0.8(5) . . . . ? C15 C14 C19 C21 -72.4(3) . . . . ? C15 C14 C19 C20 52.2(3) . . . . ? C16 C15 C14 C13 1.0(4) . . . . ? C16 C15 C14 C19 -179.0(3) . . . . ? C16 C17 C18 C13 -0.7(4) . . . . ? C16 C17 C18 C22 178.2(3) . . . . ? C26 C25 C30 C29 -1.8(4) . . . . ? C14 C13 C18 C17 2.5(4) . . . . ? C14 C13 C18 C22 -176.4(2) . . . . ? C14 C15 C16 C17 0.6(5) . . . . ? C29 C28 C27 C26 -0.9(5) . . . . ? C18 C13 C14 C15 -2.7(3) . . . . ? C18 C13 C14 C19 177.4(2) . . . . ? C23 C22 C18 C13 115.5(3) . . . . ? C23 C22 C18 C17 -63.4(3) . . . . ? C24 C22 C18 C13 -120.3(3) . . . . ? C24 C22 C18 C17 60.8(3) . . . . ? O1 C31 N5 C32 -178.1(3) . . . . ? O1 C31 N5 C33 6.8(5) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.500 0.500 0.000 54.9 8.3 '0.8 H2O' 2 0.500 0.000 0.500 54.9 8.3 '0.8 H2O'