#------------------------------------------------------------------------------ #$Date: 2026-05-07 23:58:25 +0100 (Thu, 07 May 2026) $ #$Revision: 305891 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/09/7720992.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_7720992 loop_ _publ_author_name 'Liu, Wen-yang' 'Li, Honglei' 'Jia, Jiang-song' 'Zhao, Wen-ming' 'Sun, Jun' _publ_section_title ; Synthesis, Crystal Structures and Urease Inhibition of Ni(II) complexes Constructed from Schiff bases with 2,2’-bipyridine as co-ligands ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00460A _journal_year 2026 _chemical_formula_moiety 'C26 H21 Cl2 N3 Ni O4, 2(C H4 O)' _chemical_formula_sum 'C28 H29 Cl2 N3 Ni O6' _chemical_formula_weight 633.15 _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 difmap _atom_sites_solution_primary iterative _audit_creation_date 2026-01-22 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2026-01-22 deposited with the CCDC. 2026-04-28 downloaded from the CCDC. ; _cell_angle_alpha 86.307(2) _cell_angle_beta 81.250(2) _cell_angle_gamma 69.766(2) _cell_formula_units_Z 2 _cell_length_a 9.4508(6) _cell_length_b 11.9832(8) _cell_length_c 13.2510(7) _cell_measurement_reflns_used 4519 _cell_measurement_temperature 115.0 _cell_measurement_theta_max 27.252 _cell_measurement_theta_min 2.402 _cell_volume 1391.58(15) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.3 (Bourhis et al., 2015)' _diffrn_ambient_temperature 115.0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_unetI/netI 0.0642 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 27259 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.526 _diffrn_reflns_theta_min 2.403 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5397 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'clear greenish colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier greenish _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.511 _exptl_crystal_description block _exptl_crystal_F_000 656 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.457 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 477 _refine_ls_number_reflns 6363 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0434 _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^)+1.9928P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.0996 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5095 _reflns_number_total 6363 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00460a2.cif _cod_data_source_block 1_CCDC1 _cod_database_code 7720992 _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 ; ; _shelx_res_file ; TITL 1_a.res in P-1 1.res created by SHELXL-2018/3 at 17:13:46 on 08-Jul-2025 REM Old TITL 1 in P-1 REM SHELXT solution in P-1 REM R1 0.205, Rweak 0.008, Alpha 0.044, Orientation as input REM Formula found by SHELXT: C28 N4 O7 Ni CELL 0.71073 9.4508 11.9832 13.251 86.307 81.25 69.766 ZERR 2 0.0006 0.0008 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H Cl N Ni O UNIT 56 58 4 6 2 12 EQIV $1 1-X,1-Y,2-Z EQIV $2 1+X,+Y,+Z L.S. 20 PLAN 1 TEMP -158.15 CONF HTAB O2 O4_$1 HTAB O2 O5_$2 HTAB O5 O6 HTAB O6 O3 list 4 fmap 2 MORE -1 BOND $H ACTA REM REM REM WGHT 0.000000 1.992800 FVAR 0.81481 NI1 5 0.471816 0.727837 0.839484 11.00000 0.01802 0.01568 = 0.01435 0.00008 -0.00183 -0.00503 CL1 3 0.713105 0.744417 0.288201 11.00000 0.03296 0.03442 = 0.01528 0.00173 0.00010 -0.01265 CL2 3 0.685309 0.990186 0.621095 11.00000 0.03797 0.02477 = 0.02439 0.00050 -0.00439 -0.01793 O1 6 0.579124 0.811293 0.733242 11.00000 0.02508 0.01970 = 0.01405 0.00082 -0.00124 -0.01059 O2 6 0.683161 0.631352 0.883781 11.00000 0.01909 0.02266 = 0.02157 0.00394 -0.00368 -0.00624 O3 6 0.364066 0.621783 0.929129 11.00000 0.02206 0.01808 = 0.01679 -0.00112 0.00093 -0.00850 O4 6 0.307579 0.455473 0.925122 11.00000 0.02633 0.02308 = 0.01817 0.00146 -0.00037 -0.01268 N1 4 0.501318 0.599917 0.738498 11.00000 0.01759 0.01343 = 0.01761 0.00018 -0.00248 -0.00153 N2 4 0.412623 0.850165 0.956554 11.00000 0.02070 0.01621 = 0.01595 -0.00078 -0.00345 -0.00583 N3 4 0.265251 0.850316 0.802110 11.00000 0.01564 0.01666 = 0.01683 -0.00242 -0.00192 -0.00389 C1 1 0.604370 0.792880 0.636421 11.00000 0.01790 0.01655 = 0.01797 0.00149 -0.00402 -0.00566 C2 1 0.656886 0.872229 0.567682 11.00000 0.02242 0.01570 = 0.02112 0.00182 -0.00370 -0.00729 C3 1 0.686738 0.860402 0.463737 11.00000 0.02269 0.02513 = 0.01847 0.00647 -0.00105 -0.00942 C4 1 0.669328 0.764245 0.420099 11.00000 0.02023 0.02538 = 0.01292 -0.00055 -0.00065 -0.00487 C5 1 0.620696 0.684040 0.480051 11.00000 0.01884 0.01686 = 0.01915 -0.00232 -0.00334 -0.00323 C6 1 0.586677 0.696130 0.587011 11.00000 0.01694 0.01902 = 0.01666 0.00383 -0.00500 -0.00634 C7 1 0.540362 0.603643 0.642109 11.00000 0.01738 0.01692 = 0.01912 -0.00049 -0.00379 -0.00457 C8 1 0.372426 0.526209 0.887760 11.00000 0.01798 0.01644 = 0.01630 0.00119 -0.00232 -0.00332 C12 1 0.471227 0.494618 0.784063 11.00000 0.02396 0.01521 = 0.01708 -0.00176 0.00107 -0.00889 C13 1 0.622056 0.394977 0.801906 11.00000 0.02753 0.01568 = 0.01991 0.00194 -0.00278 -0.00569 C14 1 0.725442 0.351992 0.703664 11.00000 0.01810 0.01335 = 0.02113 0.00100 -0.00461 -0.00035 C15 1 0.844071 0.394844 0.670217 11.00000 0.02146 0.02578 = 0.02405 -0.00037 -0.00524 -0.00847 C16 1 0.936709 0.358694 0.577955 11.00000 0.02215 0.03090 = 0.03803 0.00393 0.00060 -0.00982 C17 1 0.910272 0.278998 0.518258 11.00000 0.03078 0.02918 = 0.02434 -0.00204 0.00300 -0.00431 C18 1 0.792329 0.236594 0.549745 11.00000 0.03172 0.02416 = 0.02025 0.00019 -0.00332 -0.00932 C19 1 0.700139 0.272651 0.642719 11.00000 0.01874 0.01671 = 0.02451 0.00173 -0.00364 -0.00277 C20 1 0.202666 0.849377 0.718532 11.00000 0.02128 0.02006 = 0.02187 -0.00262 -0.00314 -0.00307 C21 1 0.078395 0.942020 0.691352 11.00000 0.02460 0.02699 = 0.02452 -0.00197 -0.00758 -0.00615 C22 1 0.016382 1.040020 0.753061 11.00000 0.02526 0.02167 = 0.02916 0.00095 -0.01073 0.00043 C23 1 0.079073 1.042669 0.840126 11.00000 0.02518 0.02052 = 0.02563 -0.00365 -0.00423 -0.00401 C24 1 0.204036 0.946499 0.862832 11.00000 0.01658 0.01875 = 0.01976 0.00200 -0.00081 -0.00780 C25 1 0.282144 0.942977 0.952612 11.00000 0.02085 0.01558 = 0.01747 0.00078 -0.00101 -0.00730 C26 1 0.224922 1.029245 1.028003 11.00000 0.02457 0.01988 = 0.02289 -0.00237 -0.00252 -0.00460 C27 1 0.306199 1.020145 1.109028 11.00000 0.03346 0.02064 = 0.01683 -0.00424 -0.00071 -0.01043 C28 1 0.438481 0.925065 1.113524 11.00000 0.03219 0.02395 = 0.01632 0.00059 -0.00737 -0.00978 C29 1 0.487751 0.842307 1.035888 11.00000 0.02145 0.01814 = 0.02048 0.00245 -0.00337 -0.00642 O5 6 -0.062530 0.696217 0.826280 11.00000 0.03128 0.04252 = 0.04017 0.00052 -0.00890 -0.01518 C30 1 0.038860 0.609334 0.757099 11.00000 0.05085 0.05058 = 0.03392 0.00082 0.00029 -0.03160 O6 6 0.061792 0.720899 0.994193 11.00000 0.02172 0.02679 = 0.03057 -0.00156 -0.00004 -0.00452 C31 1 0.002614 0.651649 1.068501 11.00000 0.03101 0.03464 = 0.03524 0.00257 -0.00023 -0.00809 H3 2 0.717000 0.913060 0.422891 11.00000 0.00566 H13A 2 0.672275 0.423507 0.848453 11.00000 0.01352 H15 2 0.863299 0.446279 0.714754 11.00000 0.01115 H27 2 0.273999 1.076037 1.158890 11.00000 0.01185 H23 2 0.040642 1.107946 0.885277 11.00000 0.02092 H12 2 0.419282 0.460525 0.740328 11.00000 0.01506 H19 2 0.620394 0.243532 0.661994 11.00000 0.03239 H28 2 0.494728 0.916402 1.167322 11.00000 0.02295 H20 2 0.246072 0.783068 0.679386 11.00000 0.02381 H16 2 1.016734 0.387656 0.555621 11.00000 0.02700 H7 2 0.538431 0.536697 0.599490 11.00000 0.01986 H5 2 0.608002 0.618276 0.451633 11.00000 0.01619 H13B 2 0.586973 0.331715 0.833924 11.00000 0.02542 H22 2 -0.069881 1.107270 0.737433 11.00000 0.02921 H29 2 0.576812 0.774180 1.036956 11.00000 0.01950 H26 2 0.132339 1.095548 1.023766 11.00000 0.03336 H21 2 0.041725 0.934545 0.629000 11.00000 0.03401 H17 2 0.970231 0.259114 0.456312 11.00000 0.03990 H30A 2 -0.020476 0.607305 0.700501 11.00000 0.05756 H18 2 0.771016 0.180929 0.506904 11.00000 0.04789 H5A 2 -0.013734 0.706752 0.879401 11.00000 0.07186 H6 2 0.156842 0.690159 0.985209 11.00000 0.04333 H30B 2 0.073406 0.525158 0.793993 11.00000 0.06703 H31A 2 -0.108895 0.683067 1.070469 11.00000 0.05692 H31B 2 0.041369 0.568176 1.061945 11.00000 0.06808 H2A 2 0.755472 0.663504 0.870148 11.00000 0.06108 H30C 2 0.128888 0.631707 0.724074 11.00000 0.05627 H2B 2 0.694400 0.593743 0.940678 11.00000 0.05072 H31C 2 0.027615 0.657938 1.141903 11.00000 0.07441 HKLF 4 REM 1_a.res in P-1 REM wR2 = 0.0996, GooF = S = 1.075, Restrained GooF = 1.075 for all data REM R1 = 0.0434 for 5095 Fo > 4sig(Fo) and 0.0600 for all 6363 data REM 477 parameters refined using 0 restraints END WGHT 0.0000 1.9928 REM Highest difference peak 0.457, deepest hole -0.604, 1-sigma level 0.087 Q1 1 0.3537 0.8011 0.8112 11.00000 0.05 0.46 ; _shelx_res_checksum 70931 _olex2_submission_special_instructions 'No special instructions were received' 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 0.47182(4) 0.72784(3) 0.83948(2) 0.01626(10) Uani 1 1 d . . . . . Cl1 Cl 0.71311(8) 0.74442(7) 0.28820(5) 0.02772(17) Uani 1 1 d . . . . . Cl2 Cl 0.68531(9) 0.99019(6) 0.62109(5) 0.02716(17) Uani 1 1 d . . . . . O1 O 0.5791(2) 0.81129(16) 0.73324(13) 0.0190(4) Uani 1 1 d . . . . . O2 O 0.6832(2) 0.63135(18) 0.88378(16) 0.0214(4) Uani 1 1 d . . . . . O3 O 0.3641(2) 0.62178(16) 0.92913(13) 0.0189(4) Uani 1 1 d . . . . . O4 O 0.3076(2) 0.45547(16) 0.92512(14) 0.0218(4) Uani 1 1 d . . . . . N1 N 0.5013(2) 0.59992(18) 0.73850(16) 0.0172(4) Uani 1 1 d . . . . . N2 N 0.4126(2) 0.85016(19) 0.95655(16) 0.0176(4) Uani 1 1 d . . . . . N3 N 0.2653(2) 0.85032(19) 0.80211(16) 0.0167(4) Uani 1 1 d . . . . . C1 C 0.6044(3) 0.7929(2) 0.63642(19) 0.0174(5) Uani 1 1 d . . . . . C2 C 0.6569(3) 0.8722(2) 0.5677(2) 0.0196(5) Uani 1 1 d . . . . . C3 C 0.6867(3) 0.8604(3) 0.4637(2) 0.0223(6) Uani 1 1 d . . . . . C4 C 0.6693(3) 0.7642(2) 0.42010(19) 0.0204(6) Uani 1 1 d . . . . . C5 C 0.6207(3) 0.6840(2) 0.4801(2) 0.0189(5) Uani 1 1 d . . . . . C6 C 0.5867(3) 0.6961(2) 0.58701(19) 0.0174(5) Uani 1 1 d . . . . . C7 C 0.5404(3) 0.6036(2) 0.6421(2) 0.0180(5) Uani 1 1 d . . . . . C8 C 0.3724(3) 0.5262(2) 0.88776(19) 0.0176(5) Uani 1 1 d . . . . . C12 C 0.4712(3) 0.4946(2) 0.7841(2) 0.0185(5) Uani 1 1 d . . . . . C13 C 0.6221(3) 0.3950(2) 0.8019(2) 0.0216(6) Uani 1 1 d . . . . . C14 C 0.7254(3) 0.3520(2) 0.7037(2) 0.0187(5) Uani 1 1 d . . . . . C15 C 0.8441(3) 0.3948(3) 0.6702(2) 0.0234(6) Uani 1 1 d . . . . . C16 C 0.9367(3) 0.3587(3) 0.5780(2) 0.0309(7) Uani 1 1 d . . . . . C17 C 0.9103(4) 0.2790(3) 0.5183(2) 0.0303(7) Uani 1 1 d . . . . . C18 C 0.7923(3) 0.2366(3) 0.5497(2) 0.0255(6) Uani 1 1 d . . . . . C19 C 0.7001(3) 0.2727(2) 0.6427(2) 0.0209(6) Uani 1 1 d . . . . . C20 C 0.2027(3) 0.8494(3) 0.7185(2) 0.0220(6) Uani 1 1 d . . . . . C21 C 0.0784(3) 0.9420(3) 0.6914(2) 0.0255(6) Uani 1 1 d . . . . . C22 C 0.0164(3) 1.0400(3) 0.7531(2) 0.0269(6) Uani 1 1 d . . . . . C23 C 0.0791(3) 1.0427(3) 0.8401(2) 0.0245(6) Uani 1 1 d . . . . . C24 C 0.2040(3) 0.9465(2) 0.8628(2) 0.0182(5) Uani 1 1 d . . . . . C25 C 0.2821(3) 0.9430(2) 0.95261(19) 0.0179(5) Uani 1 1 d . . . . . C26 C 0.2249(3) 1.0292(3) 1.0280(2) 0.0232(6) Uani 1 1 d . . . . . C27 C 0.3062(3) 1.0201(3) 1.1090(2) 0.0234(6) Uani 1 1 d . . . . . C28 C 0.4385(3) 0.9251(3) 1.1135(2) 0.0237(6) Uani 1 1 d . . . . . C29 C 0.4878(3) 0.8423(2) 1.0359(2) 0.0202(5) Uani 1 1 d . . . . . O5 O -0.0625(3) 0.6962(2) 0.82628(19) 0.0369(5) Uani 1 1 d . . . . . C30 C 0.0389(5) 0.6093(4) 0.7571(3) 0.0421(9) Uani 1 1 d . . . . . O6 O 0.0618(2) 0.72090(19) 0.99419(16) 0.0277(5) Uani 1 1 d . . . . . C31 C 0.0026(4) 0.6516(3) 1.0685(3) 0.0351(7) Uani 1 1 d . . . . . H3 H 0.717(3) 0.913(2) 0.4229(19) 0.006(6) Uiso 1 1 d . . . . . H13A H 0.672(3) 0.424(2) 0.848(2) 0.014(7) Uiso 1 1 d . . . . . H15 H 0.863(3) 0.446(2) 0.715(2) 0.011(7) Uiso 1 1 d . . . . . H27 H 0.274(3) 1.076(2) 1.159(2) 0.012(7) Uiso 1 1 d . . . . . H23 H 0.041(3) 1.108(3) 0.885(2) 0.021(8) Uiso 1 1 d . . . . . H12 H 0.419(3) 0.461(2) 0.740(2) 0.015(7) Uiso 1 1 d . . . . . H19 H 0.620(4) 0.244(3) 0.662(2) 0.032(9) Uiso 1 1 d . . . . . H28 H 0.495(3) 0.916(3) 1.167(2) 0.023(8) Uiso 1 1 d . . . . . H20 H 0.246(3) 0.783(3) 0.679(2) 0.024(8) Uiso 1 1 d . . . . . H16 H 1.017(4) 0.388(3) 0.556(2) 0.027(8) Uiso 1 1 d . . . . . H7 H 0.538(3) 0.537(3) 0.599(2) 0.020(7) Uiso 1 1 d . . . . . H5 H 0.608(3) 0.618(3) 0.452(2) 0.016(7) Uiso 1 1 d . . . . . H13B H 0.587(3) 0.332(3) 0.834(2) 0.025(8) Uiso 1 1 d . . . . . H22 H -0.070(4) 1.107(3) 0.737(2) 0.029(8) Uiso 1 1 d . . . . . H29 H 0.577(3) 0.774(3) 1.037(2) 0.020(7) Uiso 1 1 d . . . . . H26 H 0.132(4) 1.096(3) 1.024(2) 0.033(9) Uiso 1 1 d . . . . . H21 H 0.042(4) 0.935(3) 0.629(3) 0.034(9) Uiso 1 1 d . . . . . H17 H 0.970(4) 0.259(3) 0.456(3) 0.040(10) Uiso 1 1 d . . . . . H30A H -0.020(4) 0.607(3) 0.701(3) 0.058(12) Uiso 1 1 d . . . . . H18 H 0.771(4) 0.181(3) 0.507(3) 0.048(10) Uiso 1 1 d . . . . . H5A H -0.014(5) 0.707(4) 0.879(3) 0.072(14) Uiso 1 1 d . . . . . H6 H 0.157(4) 0.690(3) 0.985(3) 0.043(11) Uiso 1 1 d . . . . . H30B H 0.073(5) 0.525(4) 0.794(3) 0.067(13) Uiso 1 1 d . . . . . H31A H -0.109(5) 0.683(4) 1.070(3) 0.057(12) Uiso 1 1 d . . . . . H31B H 0.041(5) 0.568(4) 1.062(3) 0.068(13) Uiso 1 1 d . . . . . H2A H 0.755(5) 0.664(4) 0.870(3) 0.061(13) Uiso 1 1 d . . . . . H30C H 0.129(5) 0.632(3) 0.724(3) 0.056(11) Uiso 1 1 d . . . . . H2B H 0.694(4) 0.594(3) 0.941(3) 0.051(12) Uiso 1 1 d . . . . . H31C H 0.028(5) 0.658(4) 1.142(4) 0.074(14) Uiso 1 1 d . . . . . 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 0.01802(18) 0.01568(18) 0.01435(17) 0.00008(12) -0.00183(12) -0.00503(14) Cl1 0.0330(4) 0.0344(4) 0.0153(3) 0.0017(3) 0.0001(3) -0.0127(3) Cl2 0.0380(4) 0.0248(4) 0.0244(3) 0.0005(3) -0.0044(3) -0.0179(3) O1 0.0251(10) 0.0197(9) 0.0140(9) 0.0008(7) -0.0012(7) -0.0106(8) O2 0.0191(10) 0.0227(10) 0.0216(10) 0.0039(8) -0.0037(8) -0.0062(8) O3 0.0221(10) 0.0181(9) 0.0168(9) -0.0011(7) 0.0009(7) -0.0085(8) O4 0.0263(10) 0.0231(10) 0.0182(9) 0.0015(8) -0.0004(8) -0.0127(8) N1 0.0176(11) 0.0134(11) 0.0176(11) 0.0002(8) -0.0025(8) -0.0015(9) N2 0.0207(11) 0.0162(11) 0.0159(11) -0.0008(8) -0.0035(8) -0.0058(9) N3 0.0156(11) 0.0167(11) 0.0168(11) -0.0024(8) -0.0019(8) -0.0039(9) C1 0.0179(13) 0.0165(13) 0.0180(13) 0.0015(10) -0.0040(10) -0.0057(10) C2 0.0224(14) 0.0157(13) 0.0211(13) 0.0018(10) -0.0037(10) -0.0073(11) C3 0.0227(14) 0.0251(15) 0.0185(13) 0.0065(11) -0.0010(11) -0.0094(12) C4 0.0202(14) 0.0254(14) 0.0129(12) -0.0005(10) -0.0006(10) -0.0049(11) C5 0.0188(13) 0.0169(13) 0.0192(13) -0.0023(10) -0.0033(10) -0.0032(11) C6 0.0169(13) 0.0190(13) 0.0167(13) 0.0038(10) -0.0050(10) -0.0063(11) C7 0.0174(13) 0.0169(13) 0.0191(13) -0.0005(10) -0.0038(10) -0.0046(11) C8 0.0180(13) 0.0164(13) 0.0163(12) 0.0012(10) -0.0023(10) -0.0033(10) C12 0.0240(14) 0.0152(13) 0.0171(13) -0.0018(10) 0.0011(10) -0.0089(11) C13 0.0275(15) 0.0157(13) 0.0199(14) 0.0019(11) -0.0028(11) -0.0057(12) C14 0.0181(13) 0.0134(12) 0.0211(13) 0.0010(10) -0.0046(10) -0.0004(10) C15 0.0215(14) 0.0258(15) 0.0240(15) -0.0004(12) -0.0052(11) -0.0085(12) C16 0.0222(15) 0.0309(17) 0.0380(18) 0.0039(13) 0.0006(13) -0.0098(13) C17 0.0308(17) 0.0292(16) 0.0243(16) -0.0020(13) 0.0030(13) -0.0043(13) C18 0.0317(16) 0.0242(15) 0.0202(14) 0.0002(11) -0.0033(12) -0.0093(13) C19 0.0187(14) 0.0167(13) 0.0245(14) 0.0017(11) -0.0036(11) -0.0028(11) C20 0.0213(14) 0.0201(14) 0.0219(14) -0.0026(11) -0.0031(11) -0.0031(11) C21 0.0246(15) 0.0270(15) 0.0245(15) -0.0020(12) -0.0076(12) -0.0062(12) C22 0.0253(15) 0.0217(15) 0.0292(16) 0.0010(12) -0.0107(12) 0.0004(12) C23 0.0252(15) 0.0205(14) 0.0256(15) -0.0036(12) -0.0042(11) -0.0040(12) C24 0.0166(13) 0.0187(13) 0.0198(13) 0.0020(10) -0.0008(10) -0.0078(11) C25 0.0209(13) 0.0156(13) 0.0175(13) 0.0008(10) -0.0010(10) -0.0073(11) C26 0.0246(15) 0.0199(14) 0.0229(14) -0.0024(11) -0.0025(11) -0.0046(12) C27 0.0335(16) 0.0206(14) 0.0168(13) -0.0042(11) -0.0007(11) -0.0104(12) C28 0.0322(16) 0.0240(15) 0.0163(13) 0.0006(11) -0.0074(11) -0.0098(12) C29 0.0215(14) 0.0181(13) 0.0205(13) 0.0025(10) -0.0034(10) -0.0064(11) O5 0.0313(13) 0.0425(14) 0.0402(14) 0.0005(11) -0.0089(10) -0.0152(11) C30 0.051(2) 0.051(2) 0.0339(19) 0.0008(16) 0.0003(17) -0.0316(19) O6 0.0217(11) 0.0268(11) 0.0306(12) -0.0016(9) 0.0000(9) -0.0045(9) C31 0.0310(19) 0.0346(19) 0.0352(19) 0.0026(15) -0.0002(14) -0.0081(15) 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' O O 0.0106 0.0060 '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 O1 Ni1 O2 88.18(8) . . ? O1 Ni1 O3 170.15(7) . . ? O1 Ni1 N2 98.72(8) . . ? O1 Ni1 N3 87.29(8) . . ? O2 Ni1 O3 92.68(8) . . ? O2 Ni1 N3 170.44(8) . . ? O3 Ni1 N3 93.22(8) . . ? N1 Ni1 O1 90.29(8) . . ? N1 Ni1 O2 89.55(8) . . ? N1 Ni1 O3 79.90(8) . . ? N1 Ni1 N2 170.40(9) . . ? N1 Ni1 N3 98.89(8) . . ? N2 Ni1 O2 94.02(8) . . ? N2 Ni1 O3 91.01(8) . . ? N2 Ni1 N3 78.37(8) . . ? C1 O1 Ni1 125.70(16) . . ? Ni1 O2 H2A 117(3) . . ? Ni1 O2 H2B 124(3) . . ? H2A O2 H2B 108(4) . . ? C8 O3 Ni1 115.47(16) . . ? C7 N1 Ni1 126.85(18) . . ? C7 N1 C12 119.0(2) . . ? C12 N1 Ni1 114.19(16) . . ? C25 N2 Ni1 115.69(17) . . ? C29 N2 Ni1 126.18(18) . . ? C29 N2 C25 118.1(2) . . ? C20 N3 Ni1 126.30(18) . . ? C20 N3 C24 118.2(2) . . ? C24 N3 Ni1 114.83(17) . . ? O1 C1 C2 120.0(2) . . ? O1 C1 C6 126.0(2) . . ? C2 C1 C6 114.1(2) . . ? C1 C2 Cl2 117.2(2) . . ? C3 C2 Cl2 118.4(2) . . ? C3 C2 C1 124.4(2) . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3 121.9(16) . . ? C4 C3 H3 119.0(16) . . ? C3 C4 Cl1 119.9(2) . . ? C5 C4 Cl1 119.7(2) . . ? C5 C4 C3 120.3(2) . . ? C4 C5 C6 121.3(2) . . ? C4 C5 H5 121.4(17) . . ? C6 C5 H5 117.2(17) . . ? C1 C6 C7 123.2(2) . . ? C5 C6 C1 120.8(2) . . ? C5 C6 C7 116.0(2) . . ? N1 C7 C6 125.5(2) . . ? N1 C7 H7 118.1(16) . . ? C6 C7 H7 116.3(16) . . ? O3 C8 C12 117.6(2) . . ? O4 C8 O3 125.5(2) . . ? O4 C8 C12 117.0(2) . . ? N1 C12 C8 109.5(2) . . ? N1 C12 C13 110.5(2) . . ? N1 C12 H12 113.0(16) . . ? C8 C12 C13 107.7(2) . . ? C8 C12 H12 108.9(16) . . ? C13 C12 H12 107.0(16) . . ? C12 C13 H13A 109.1(16) . . ? C12 C13 H13B 102.7(18) . . ? C14 C13 C12 112.4(2) . . ? C14 C13 H13A 111.4(16) . . ? C14 C13 H13B 110.1(18) . . ? H13A C13 H13B 111(2) . . ? C15 C14 C13 120.6(2) . . ? C19 C14 C13 120.6(2) . . ? C19 C14 C15 118.8(2) . . ? C14 C15 H15 117.7(16) . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15 121.2(16) . . ? C15 C16 H16 120.7(19) . . ? C17 C16 C15 119.5(3) . . ? C17 C16 H16 119.7(19) . . ? C16 C17 H17 118(2) . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 122(2) . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 121(2) . . ? C19 C18 H18 119(2) . . ? C14 C19 C18 120.5(3) . . ? C14 C19 H19 121(2) . . ? C18 C19 H19 118(2) . . ? N3 C20 C21 123.1(3) . . ? N3 C20 H20 116.1(19) . . ? C21 C20 H20 120.7(19) . . ? C20 C21 H21 118(2) . . ? C22 C21 C20 118.6(3) . . ? C22 C21 H21 124(2) . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22 122.0(19) . . ? C23 C22 H22 118.8(19) . . ? C22 C23 C24 119.2(3) . . ? C22 C23 H23 122.6(18) . . ? C24 C23 H23 118.3(18) . . ? N3 C24 C23 121.7(3) . . ? N3 C24 C25 115.3(2) . . ? C23 C24 C25 123.0(2) . . ? N2 C25 C24 115.5(2) . . ? N2 C25 C26 122.1(2) . . ? C26 C25 C24 122.4(2) . . ? C25 C26 H26 121(2) . . ? C27 C26 C25 118.8(3) . . ? C27 C26 H26 120.0(19) . . ? C26 C27 H27 121.4(17) . . ? C28 C27 C26 119.1(3) . . ? C28 C27 H27 119.5(17) . . ? C27 C28 C29 118.8(3) . . ? C27 C28 H28 120.9(18) . . ? C29 C28 H28 120.3(18) . . ? N2 C29 C28 123.1(3) . . ? N2 C29 H29 115.3(17) . . ? C28 C29 H29 121.5(17) . . ? C30 O5 H5A 111(3) . . ? O5 C30 H30A 106(2) . . ? O5 C30 H30B 110(2) . . ? O5 C30 H30C 113(2) . . ? H30A C30 H30B 110(3) . . ? H30A C30 H30C 106(3) . . ? H30B C30 H30C 112(3) . . ? C31 O6 H6 108(3) . . ? O6 C31 H31A 106(2) . . ? O6 C31 H31B 118(3) . . ? O6 C31 H31C 113(2) . . ? H31A C31 H31B 112(3) . . ? H31A C31 H31C 108(3) . . ? H31B C31 H31C 99(3) . . ? 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 O1 2.0239(17) . ? Ni1 O2 2.084(2) . ? Ni1 O3 2.0966(17) . ? Ni1 N1 2.018(2) . ? Ni1 N2 2.081(2) . ? Ni1 N3 2.105(2) . ? Cl1 C4 1.746(3) . ? Cl2 C2 1.738(3) . ? O1 C1 1.288(3) . ? O2 H2A 0.89(4) . ? O2 H2B 0.85(4) . ? O3 C8 1.274(3) . ? O4 C8 1.246(3) . ? N1 C7 1.277(3) . ? N1 C12 1.461(3) . ? N2 C25 1.350(3) . ? N2 C29 1.336(3) . ? N3 C20 1.335(3) . ? N3 C24 1.352(3) . ? C1 C2 1.434(3) . ? C1 C6 1.437(4) . ? C2 C3 1.370(4) . ? C3 C4 1.391(4) . ? C3 H3 0.90(3) . ? C4 C5 1.365(4) . ? C5 C6 1.410(4) . ? C5 H5 0.95(3) . ? C6 C7 1.445(3) . ? C7 H7 1.02(3) . ? C8 C12 1.528(3) . ? C12 C13 1.550(4) . ? C12 H12 1.00(3) . ? C13 C14 1.505(4) . ? C13 H13A 0.98(3) . ? C13 H13B 0.98(3) . ? C14 C15 1.391(4) . ? C14 C19 1.389(4) . ? C15 C16 1.389(4) . ? C15 H15 0.96(3) . ? C16 C17 1.387(4) . ? C16 H16 0.94(3) . ? C17 C18 1.378(4) . ? C17 H17 0.92(3) . ? C18 C19 1.395(4) . ? C18 H18 0.99(4) . ? C19 H19 0.93(3) . ? C20 C21 1.384(4) . ? C20 H20 0.91(3) . ? C21 C22 1.376(4) . ? C21 H21 0.96(3) . ? C22 C23 1.382(4) . ? C22 H22 0.97(3) . ? C23 C24 1.391(4) . ? C23 H23 0.95(3) . ? C24 C25 1.484(4) . ? C25 C26 1.393(4) . ? C26 C27 1.390(4) . ? C26 H26 0.96(3) . ? C27 C28 1.376(4) . ? C27 H27 0.91(3) . ? C28 C29 1.387(4) . ? C28 H28 0.93(3) . ? C29 H29 0.95(3) . ? O5 C30 1.417(4) . ? O5 H5A 0.94(5) . ? C30 H30A 1.01(4) . ? C30 H30B 1.06(4) . ? C30 H30C 1.01(4) . ? O6 C31 1.421(4) . ? O6 H6 0.84(4) . ? C31 H31A 0.99(4) . ? C31 H31B 0.94(5) . ? C31 H31C 1.05(5) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O5 H5A O6 0.94(5) 1.82(5) 2.746(3) 172(4) . yes O6 H6 O3 0.84(4) 1.89(4) 2.711(3) 165(4) . yes O2 H2A O5 0.89(4) 1.89(4) 2.760(3) 166(4) 1_655 yes O2 H2B O4 0.85(4) 1.84(4) 2.677(3) 167(4) 2_667 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni1 O1 C1 C2 168.86(18) . . . . ? Ni1 O1 C1 C6 -11.9(4) . . . . ? Ni1 O3 C8 O4 -174.8(2) . . . . ? Ni1 O3 C8 C12 5.8(3) . . . . ? Ni1 N1 C7 C6 6.8(4) . . . . ? Ni1 N1 C12 C8 20.1(3) . . . . ? Ni1 N1 C12 C13 -98.4(2) . . . . ? Ni1 N2 C25 C24 -2.5(3) . . . . ? Ni1 N2 C25 C26 177.3(2) . . . . ? Ni1 N2 C29 C28 -177.4(2) . . . . ? Ni1 N3 C20 C21 -170.2(2) . . . . ? Ni1 N3 C24 C23 171.4(2) . . . . ? Ni1 N3 C24 C25 -6.9(3) . . . . ? Cl1 C4 C5 C6 179.0(2) . . . . ? Cl2 C2 C3 C4 177.9(2) . . . . ? O1 C1 C2 Cl2 0.6(3) . . . . ? O1 C1 C2 C3 -179.9(3) . . . . ? O1 C1 C6 C5 -178.8(2) . . . . ? O1 C1 C6 C7 -1.5(4) . . . . ? O3 C8 C12 N1 -17.0(3) . . . . ? O3 C8 C12 C13 103.3(3) . . . . ? O4 C8 C12 N1 163.6(2) . . . . ? O4 C8 C12 C13 -76.2(3) . . . . ? N1 C12 C13 C14 -63.5(3) . . . . ? N2 C25 C26 C27 0.9(4) . . . . ? N3 C20 C21 C22 0.2(4) . . . . ? N3 C24 C25 N2 6.3(3) . . . . ? N3 C24 C25 C26 -173.5(2) . . . . ? C1 C2 C3 C4 -1.6(4) . . . . ? C1 C6 C7 N1 4.4(4) . . . . ? C2 C1 C6 C5 0.4(4) . . . . ? C2 C1 C6 C7 177.7(2) . . . . ? C2 C3 C4 Cl1 -177.8(2) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C4 C5 C6 C1 -0.9(4) . . . . ? C4 C5 C6 C7 -178.3(2) . . . . ? C5 C6 C7 N1 -178.2(2) . . . . ? C6 C1 C2 Cl2 -178.70(19) . . . . ? C6 C1 C2 C3 0.8(4) . . . . ? C7 N1 C12 C8 -159.0(2) . . . . ? C7 N1 C12 C13 82.5(3) . . . . ? C8 C12 C13 C14 176.9(2) . . . . ? C12 N1 C7 C6 -174.3(2) . . . . ? C12 C13 C14 C15 98.0(3) . . . . ? C12 C13 C14 C19 -79.3(3) . . . . ? C13 C14 C15 C16 -177.8(3) . . . . ? C13 C14 C19 C18 177.4(3) . . . . ? C14 C15 C16 C17 0.2(5) . . . . ? C15 C14 C19 C18 0.1(4) . . . . ? C15 C16 C17 C18 0.5(5) . . . . ? C16 C17 C18 C19 -0.8(5) . . . . ? C17 C18 C19 C14 0.6(4) . . . . ? C19 C14 C15 C16 -0.5(4) . . . . ? C20 N3 C24 C23 0.1(4) . . . . ? C20 N3 C24 C25 -178.3(2) . . . . ? C20 C21 C22 C23 -0.4(4) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C22 C23 C24 N3 -0.3(4) . . . . ? C22 C23 C24 C25 177.9(3) . . . . ? C23 C24 C25 N2 -172.0(2) . . . . ? C23 C24 C25 C26 8.2(4) . . . . ? C24 N3 C20 C21 0.0(4) . . . . ? C24 C25 C26 C27 -179.2(2) . . . . ? C25 N2 C29 C28 -0.4(4) . . . . ? C25 C26 C27 C28 -1.5(4) . . . . ? C26 C27 C28 C29 1.1(4) . . . . ? C27 C28 C29 N2 -0.1(4) . . . . ? C29 N2 C25 C24 -179.9(2) . . . . ? C29 N2 C25 C26 0.0(4) . . . . ?