#------------------------------------------------------------------------------ #$Date: 2026-04-29 01:35:00 +0100 (Wed, 29 Apr 2026) $ #$Revision: 305650 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/43/7064387.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_7064387 loop_ _publ_author_name 'Devaraj , Karthickram' 'Bhuvanesh, Nattamai' 'Sundaravel, Karuppasamy' _publ_section_title ; Nickel(II)-Flavonolate Complexes of Tetradentate 4N Donor Ligands as Enzyme-Substrate Models of Quercetin-2,4-Dioxygenase: Role of Ligand Steric and Electronic Properties on Dioxygenolysis ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ00257A _journal_year 2026 _chemical_formula_moiety 'C34 H35 N4 Ni O3, Cl O4, 0.5(H2 O)' _chemical_formula_sum 'C34 H36 Cl N4 Ni O7.5' _chemical_formula_weight 714.83 _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 mixed _atom_sites_solution_primary dual _audit_creation_date 2024-04-11 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2026-01-22 deposited with the CCDC. 2026-04-28 downloaded from the CCDC. ; _cell_angle_alpha 85.014(3) _cell_angle_beta 79.917(3) _cell_angle_gamma 87.367(3) _cell_formula_units_Z 2 _cell_length_a 8.7243(3) _cell_length_b 13.6695(4) _cell_length_c 13.6886(5) _cell_measurement_reflns_used 18274 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 77.6040 _cell_measurement_theta_min 3.2360 _cell_volume 1600.38(9) _computing_cell_refinement 'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro system (CCD 43.103a 64-bit (release 20-12-2023))' _computing_data_reduction 'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -117.00 -60.00 0.50 0.10 -- -44.97-144.00-114.00 114 2 \w -100.00 -23.00 0.50 0.10 -- -44.97 144.00 -61.00 154 3 \w -88.00 -14.00 0.50 0.10 -- -44.97 127.00 129.00 148 4 \w 36.00 93.00 0.50 0.10 -- 44.97-127.00 54.00 114 5 \w 45.00 103.00 0.50 0.10 -- 44.97-144.00-114.00 116 6 \w -87.00 -17.00 0.50 1.00 -- -87.75 127.00 129.00 140 7 \w -158.00 -72.00 0.50 1.00 -- -87.75-127.00 54.00 172 8 \w -153.00 -60.00 0.50 1.00 -- -87.75-144.00-114.00 186 9 \w 94.00 178.00 0.50 1.00 -- 109.25 127.00 129.00 168 10 \w 82.00 170.00 0.50 1.00 -- 109.25 144.00 -61.00 176 11 \w 39.00 113.00 0.50 1.00 -- 109.25-127.00 54.00 148 12 \w 45.00 125.00 0.50 1.00 -- 109.25-144.00-114.00 160 13 \w -13.00 31.00 0.50 0.10 -- -44.97 19.00 0.00 88 14 \w -13.00 31.00 0.50 0.10 -- -44.97 19.00 90.00 88 15 \w -13.00 31.00 0.50 0.10 -- -44.97 19.00 -30.00 88 16 \w -13.00 31.00 0.50 0.10 -- -44.97 19.00 120.00 88 17 \w -13.00 31.00 0.50 0.10 -- -44.97 19.00 30.00 88 18 \w -13.00 31.00 0.50 0.10 -- -44.97 19.00 60.00 88 19 \w -13.00 31.00 0.50 0.10 -- -44.97 19.00 150.00 88 20 \w -29.00 12.00 0.50 0.10 -- 44.97 -19.00 150.00 82 21 \w -29.00 12.00 0.50 0.10 -- 44.97 -19.00 120.00 82 22 \w -160.00 -81.00 0.50 1.00 -- -87.75 -47.00 108.02 158 23 \w -160.00 -81.00 0.50 1.00 -- -87.75 -47.00 108.02 158 24 \w 97.00 178.00 0.50 1.00 -- 109.25 45.00-120.00 162 25 \w 37.00 75.00 0.50 1.00 -- 109.25 -61.00 60.00 76 26 \w 37.00 106.00 0.50 1.00 -- 109.25 -95.00 -90.00 138 27 \w 97.00 178.00 0.50 1.00 -- 109.25 45.00-120.00 162 28 \w 110.00 178.00 0.50 1.00 -- 109.25 77.00-180.00 136 29 \w 37.00 75.00 0.50 1.00 -- 109.25 -61.00-180.00 76 30 \w 37.00 75.00 0.50 1.00 -- 109.25 -61.00-120.00 76 31 \w 37.00 106.00 0.50 1.00 -- 109.25 -95.00-150.00 138 32 \w 37.00 75.00 0.50 1.00 -- 109.25 -61.00 -90.00 76 33 \w 37.00 106.00 0.50 1.00 -- 109.25 -95.00-120.00 138 34 \w 40.00 111.00 0.50 1.00 -- 109.25-125.00 150.00 142 35 \w 134.00 176.00 0.50 1.00 -- 109.25 125.00-150.00 84 36 \w 41.00 95.00 0.50 1.00 -- 109.25-125.00 60.00 108 37 \w 61.00 106.00 0.50 1.00 -- 109.25 -95.00 -60.00 90 38 \w 45.00 75.00 0.50 1.00 -- 109.25 -61.00 120.00 60 39 \w 97.00 152.00 0.50 1.00 -- 109.25 45.00 90.00 110 40 \w 48.00 74.00 0.50 1.00 -- 109.25 -61.00 -30.00 52 41 \w 97.00 176.00 0.50 1.00 -- 109.25 45.00 -60.00 158 42 \w 47.00 73.00 0.50 1.00 -- 109.25-125.00-150.00 52 43 \w 148.00 175.00 0.50 1.00 -- 109.25 61.00 -90.00 54 44 \w 78.00 109.00 0.50 1.00 -- 109.25-125.00 30.00 62 45 \w 109.00 177.00 0.50 1.00 -- 109.25 30.00 -30.00 136 46 \w 60.00 124.00 0.50 1.00 -- 109.25 -77.00 30.00 128 47 \w 41.00 73.00 0.50 1.00 -- 109.25-125.00 30.00 64 48 \w 108.00 143.00 0.50 1.00 -- 109.25 61.00 -90.00 70 49 \w 148.00 178.00 0.50 1.00 -- 109.25 45.00 30.00 60 50 \w 39.00 104.00 0.50 1.00 -- 109.25 -95.00-180.00 130 51 \w 40.00 68.00 0.50 1.00 -- 109.25-125.00-180.00 56 52 \w 113.00 139.00 0.50 1.00 -- 109.25 45.00 30.00 52 53 \w 38.00 106.00 0.50 1.00 -- 109.25 -95.00 60.00 136 54 \w 38.00 83.00 0.50 1.00 -- 109.25 -77.00 -30.00 90 55 \w 38.00 64.00 0.50 1.00 -- 109.25 -61.00 -60.00 52 56 \w 39.00 93.00 0.50 1.00 -- 109.25 -95.00 150.00 108 57 \w 112.00 164.00 0.50 1.00 -- 109.25 61.00-150.00 104 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0355168000 _diffrn_orient_matrix_UB_12 0.0038449000 _diffrn_orient_matrix_UB_13 0.1139023000 _diffrn_orient_matrix_UB_21 0.0140207000 _diffrn_orient_matrix_UB_22 -0.1129495000 _diffrn_orient_matrix_UB_23 0.0131931000 _diffrn_orient_matrix_UB_31 0.1753320000 _diffrn_orient_matrix_UB_32 0.0061822000 _diffrn_orient_matrix_UB_33 0.0018406000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_unetI/netI 0.0204 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 23177 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.070 _diffrn_reflns_theta_min 3.247 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_current '1 mA' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _diffrn_source_voltage '50 kV' _exptl_absorpt_coefficient_mu 2.131 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.425 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.483 _exptl_crystal_description block _exptl_crystal_F_000 746 _exptl_crystal_size_max 0.698 _exptl_crystal_size_mid 0.348 _exptl_crystal_size_min 0.207 _refine_diff_density_max 0.798 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 436 _refine_ls_number_reflns 5941 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.118 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0697 _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^)+(0.0642P)^2^+4.5113P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1689 _refine_ls_wR_factor_ref 0.1768 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5287 _reflns_number_total 5941 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj00257a2.cif _cod_data_source_block kskr31 _cod_original_formula_sum 'C34 H36 Cl N4 Ni O7.50' _cod_database_code 7064387 _shelx_shelxl_version_number 2019/1 _chemical_oxdiff_formula CHNOClNi _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 0.667 _shelx_estimated_absorpt_t_min 0.318 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Others Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5) 3.a Free rotating group: O1W(H1WA,H1WB) 3.b Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B) 3.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33) ; _shelx_res_file ; TITL kskr31_a.res in P-1 kskr31.res created by SHELXL-2019/1 at 14:25:59 on 11-Apr-2024 REM Old TITL KSKR31 in P-1 REM SHELXT solution in P-1: R1 0.138, Rweak 0.009, Alpha 0.032 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C38 N5 O3 Cl Ni CELL 1.54184 8.7243 13.6695 13.6886 85.014 79.917 87.367 ZERR 2 0.0003 0.0004 0.0005 0.003 0.003 0.003 LATT 1 SFAC C H Cl N Ni O UNIT 68 72 2 8 2 15 L.S. 8 PLAN 20 SIZE 0.207 0.348 0.698 TEMP -173.15(10) CONF BOND list 4 fmap 2 53 MORE -1 BOND $H acta wpdb -1 SHEL 999 0.82 OMIT 7 1 9 OMIT 7 1 13 OMIT 9 0 4 OMIT 10 0 3 REM REM REM WGHT 0.064200 4.511300 FVAR 0.53001 NI1 5 0.190826 0.305018 0.735817 11.00000 0.03411 0.02961 = 0.02938 -0.00171 -0.00428 -0.00046 O1 6 0.403183 0.226800 0.691715 11.00000 0.03328 0.03620 = 0.03296 -0.00417 -0.00558 0.00281 O2 6 0.168716 0.287650 0.595514 11.00000 0.03311 0.03357 = 0.03125 -0.00443 -0.00567 0.00241 O3 6 0.426888 0.161714 0.405774 11.00000 0.03514 0.03396 = 0.03192 -0.00248 -0.00385 0.00128 N1 4 0.316079 0.431476 0.710059 11.00000 0.03017 0.03373 = 0.03322 -0.00040 -0.00309 0.00039 N2 4 0.234510 0.309379 0.880204 11.00000 0.03217 0.03392 = 0.03085 -0.00311 -0.00393 -0.00180 N3 4 0.112835 0.166738 0.797256 11.00000 0.03652 0.03015 = 0.03337 -0.00311 -0.00403 0.00009 N4 4 -0.023444 0.393923 0.789539 11.00000 0.03306 0.02749 = 0.03392 0.00011 -0.00347 -0.00064 C1 1 0.342390 0.491361 0.626019 11.00000 0.02996 0.03878 = 0.03612 0.00130 -0.00322 0.00266 AFIX 43 H1 2 0.306848 0.473350 0.568517 11.00000 -1.20000 AFIX 0 C2 1 0.418992 0.577736 0.620613 11.00000 0.03881 0.03320 = 0.04995 0.00572 -0.00425 0.00028 AFIX 43 H2 2 0.439915 0.617131 0.559399 11.00000 -1.20000 AFIX 0 C3 1 0.465549 0.607052 0.704957 11.00000 0.04079 0.03100 = 0.05824 0.00008 -0.00793 -0.00316 AFIX 43 H3 2 0.513064 0.668414 0.703654 11.00000 -1.20000 AFIX 0 C4 1 0.441248 0.544909 0.791113 11.00000 0.04165 0.03674 = 0.04911 -0.00772 -0.01212 -0.00097 AFIX 43 H4 2 0.472481 0.562756 0.850074 11.00000 -1.20000 AFIX 0 C5 1 0.370849 0.456402 0.790305 11.00000 0.03232 0.03306 = 0.03692 -0.00371 -0.00473 0.00049 C6 1 0.357881 0.380504 0.878996 11.00000 0.04005 0.03715 = 0.03451 -0.00271 -0.00872 -0.00101 AFIX 23 H6A 2 0.459047 0.344303 0.877702 11.00000 -1.20000 H6B 2 0.335642 0.414677 0.941040 11.00000 -1.20000 AFIX 0 C7 1 0.282590 0.207553 0.911216 11.00000 0.03971 0.03866 = 0.03411 0.00200 -0.00569 -0.00091 AFIX 23 H7A 2 0.269436 0.198609 0.984725 11.00000 -1.20000 H7B 2 0.393988 0.195669 0.883806 11.00000 -1.20000 AFIX 0 C8 1 0.184711 0.134437 0.873944 11.00000 0.03830 0.03499 = 0.03503 -0.00083 -0.00521 0.00261 C9 1 0.175900 0.038051 0.914333 11.00000 0.05225 0.03635 = 0.04103 0.00350 -0.00866 0.00283 AFIX 43 H9 2 0.226815 0.017073 0.968799 11.00000 -1.20000 AFIX 0 C10 1 0.092811 -0.026988 0.874897 11.00000 0.05295 0.02945 = 0.04967 0.00478 -0.00421 -0.00034 AFIX 43 H10 2 0.087394 -0.093691 0.900973 11.00000 -1.20000 AFIX 0 C11 1 0.016580 0.005818 0.796300 11.00000 0.04523 0.03411 = 0.04839 -0.00490 -0.00495 -0.00373 AFIX 43 H11 2 -0.044089 -0.037212 0.768955 11.00000 -1.20000 AFIX 0 C12 1 0.031866 0.102766 0.759343 11.00000 0.04001 0.03583 = 0.03992 -0.00519 -0.00709 0.00160 AFIX 43 H12 2 -0.017291 0.125190 0.704482 11.00000 -1.20000 AFIX 0 C13 1 0.085237 0.338533 0.941713 11.00000 0.04170 0.03864 = 0.02821 -0.00506 -0.00422 -0.00048 AFIX 23 H13A 2 0.105006 0.359916 1.005531 11.00000 -1.20000 H13B 2 0.016766 0.281441 0.956745 11.00000 -1.20000 AFIX 0 C14 1 0.005007 0.421438 0.887374 11.00000 0.03743 0.03552 = 0.03739 -0.00626 -0.00182 0.00130 AFIX 23 H14A 2 -0.095597 0.438942 0.928876 11.00000 -1.20000 H14B 2 0.070479 0.479958 0.876905 11.00000 -1.20000 AFIX 0 C15 1 -0.167169 0.335315 0.805725 11.00000 0.03033 0.03619 = 0.03647 -0.00326 0.00001 0.00032 AFIX 23 H15A 2 -0.254893 0.373167 0.842433 11.00000 -1.20000 H15B 2 -0.150835 0.273768 0.846873 11.00000 -1.20000 AFIX 0 C16 1 -0.208630 0.310386 0.706987 11.00000 0.03475 0.03849 = 0.04418 -0.00705 -0.00810 -0.00009 AFIX 23 H16A 2 -0.124678 0.267800 0.673024 11.00000 -1.20000 H16B 2 -0.305882 0.273251 0.720324 11.00000 -1.20000 AFIX 0 C17 1 -0.230499 0.402260 0.638737 11.00000 0.04100 0.04779 = 0.04331 -0.00399 -0.01353 0.00878 AFIX 23 H17A 2 -0.242421 0.383236 0.572382 11.00000 -1.20000 H17B 2 -0.326250 0.439099 0.666605 11.00000 -1.20000 AFIX 0 C18 1 -0.090494 0.467283 0.628394 11.00000 0.04484 0.03458 = 0.03897 0.00135 -0.00421 0.01057 AFIX 23 H18A 2 0.001300 0.434927 0.589453 11.00000 -1.20000 H18B 2 -0.112021 0.530556 0.591551 11.00000 -1.20000 AFIX 0 C19 1 -0.054044 0.486736 0.729273 11.00000 0.04104 0.02854 = 0.04223 -0.00046 -0.00324 0.00331 AFIX 23 H19A 2 0.038468 0.528099 0.719579 11.00000 -1.20000 H19B 2 -0.142906 0.523553 0.766122 11.00000 -1.20000 AFIX 0 C20 1 0.410798 0.203872 0.604114 11.00000 0.02972 0.02650 = 0.03402 0.00006 -0.00051 -0.00381 C21 1 0.287959 0.236719 0.549259 11.00000 0.02825 0.02764 = 0.03661 0.00004 -0.00255 -0.00366 C22 1 0.298403 0.210951 0.452692 11.00000 0.02867 0.02800 = 0.03636 -0.00001 -0.00134 -0.00061 C23 1 0.181318 0.229409 0.387457 11.00000 0.03696 0.02471 = 0.03599 -0.00198 -0.00598 -0.00435 C24 1 0.220817 0.220033 0.284828 11.00000 0.03968 0.03369 = 0.03645 -0.00155 -0.00472 -0.00475 AFIX 43 H24 2 0.325076 0.203297 0.256552 11.00000 -1.20000 AFIX 0 C25 1 0.108481 0.235062 0.224417 11.00000 0.05538 0.03660 = 0.03227 -0.00149 -0.00952 -0.00602 AFIX 43 H25 2 0.137492 0.230420 0.154732 11.00000 -1.20000 AFIX 0 C26 1 -0.045522 0.256760 0.264009 11.00000 0.04613 0.03441 = 0.04381 -0.00089 -0.01786 -0.00212 AFIX 43 H26 2 -0.122043 0.265995 0.222207 11.00000 -1.20000 AFIX 0 C27 1 -0.085621 0.264685 0.364857 11.00000 0.03623 0.03415 = 0.04682 -0.00312 -0.01229 0.00058 AFIX 43 H27 2 -0.191117 0.278587 0.392751 11.00000 -1.20000 AFIX 0 C28 1 0.025495 0.252709 0.426526 11.00000 0.03938 0.03177 = 0.03674 -0.00223 -0.00553 -0.00165 AFIX 43 H28 2 -0.004127 0.260336 0.495669 11.00000 -1.20000 AFIX 0 C29 1 0.537595 0.144151 0.555801 11.00000 0.03193 0.02702 = 0.03642 -0.00084 -0.00254 -0.00398 C30 1 0.654089 0.099364 0.605750 11.00000 0.03772 0.03294 = 0.04055 -0.00276 -0.00799 -0.00317 AFIX 43 H30 2 0.652792 0.109428 0.673695 11.00000 -1.20000 AFIX 0 C31 1 0.769489 0.041162 0.556149 11.00000 0.03253 0.03199 = 0.05145 -0.00361 -0.00990 0.00115 AFIX 43 H31 2 0.846795 0.010082 0.590237 11.00000 -1.20000 AFIX 0 C32 1 0.773481 0.027499 0.455288 11.00000 0.03328 0.03292 = 0.05083 -0.00820 0.00244 0.00166 AFIX 43 H32 2 0.855385 -0.011414 0.421222 11.00000 -1.20000 AFIX 0 C33 1 0.660238 0.069739 0.404906 11.00000 0.03488 0.03355 = 0.04230 -0.00648 -0.00269 -0.00389 AFIX 43 H33 2 0.663176 0.060378 0.336635 11.00000 -1.20000 AFIX 0 C34 1 0.541785 0.126302 0.456425 11.00000 0.02858 0.02842 = 0.04061 -0.00053 -0.00173 -0.00273 CL1C 3 0.616353 0.226644 1.067566 11.00000 0.04057 0.05441 = 0.03659 0.00380 -0.00651 0.00059 O2C 6 0.479490 0.289578 1.067236 11.00000 0.05416 0.05001 = 0.05534 -0.00588 -0.02406 0.00267 O3C 6 0.749313 0.283392 1.064027 11.00000 0.05182 0.10786 = 0.04421 -0.01026 -0.00566 -0.01801 O4C 6 0.595288 0.162997 1.157511 11.00000 0.06434 0.09152 = 0.05237 0.02970 0.00625 0.02432 O5C 6 0.639392 0.169570 0.982925 11.00000 0.06562 0.05616 = 0.05457 -0.00721 -0.00252 0.00335 AFIX 6 O1W 6 0.637558 -0.000153 0.863191 10.50000 0.05515 0.08755 = 0.08463 -0.03382 0.00396 -0.01946 H1WA 2 0.609220 0.058086 0.882053 10.50000 -1.50000 H1WB 2 0.551117 -0.026571 0.857360 10.50000 -1.50000 AFIX 0 HKLF 4 REM kskr31_a.res in P-1 REM wR2 = 0.1768, GooF = S = 1.118, Restrained GooF = 1.118 for all data REM R1 = 0.0697 for 5287 Fo > 4sig(Fo) and 0.0781 for all 5941 data REM 436 parameters refined using 0 restraints END WGHT 0.0642 4.5115 REM Highest difference peak 0.798, deepest hole -0.414, 1-sigma level 0.093 Q1 1 0.2020 0.2926 0.6633 11.00000 0.05 0.80 Q2 1 0.0783 0.2809 0.7359 11.00000 0.05 0.62 Q3 1 0.1692 0.3242 0.8045 11.00000 0.05 0.62 Q4 1 0.2763 0.3542 0.7194 11.00000 0.05 0.61 Q5 1 0.6390 0.2191 0.9980 11.00000 0.05 0.56 Q6 1 0.6243 0.2934 1.0589 11.00000 0.05 0.55 Q7 1 0.5910 0.2336 1.1450 11.00000 0.05 0.52 Q8 1 0.2930 0.2644 0.7060 11.00000 0.05 0.49 Q9 1 0.1404 0.2378 0.7529 11.00000 0.05 0.47 Q10 1 0.0763 0.3532 0.7604 11.00000 0.05 0.47 Q11 1 0.2881 0.2894 0.7660 11.00000 0.05 0.45 Q12 1 0.0851 0.3122 0.5845 11.00000 0.05 0.45 Q13 1 0.7295 0.3433 1.0535 11.00000 0.05 0.44 Q14 1 0.2534 0.2846 0.7928 11.00000 0.05 0.43 Q15 1 0.3118 0.3192 0.8851 11.00000 0.05 0.41 Q16 1 0.7126 0.1883 1.0197 11.00000 0.05 0.40 Q17 1 0.4054 0.4361 0.7361 11.00000 0.05 0.39 Q18 1 0.3357 0.2151 0.5821 11.00000 0.05 0.38 Q19 1 0.7218 0.2598 1.0797 11.00000 0.05 0.37 Q20 1 0.5596 0.1545 1.0190 11.00000 0.05 0.37 ; _shelx_res_checksum 50561 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder' _olex2_submission_original_sample_id KSB_240411_SDc_KSKR31 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.035 _oxdiff_exptl_absorpt_empirical_full_min 0.617 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 0.19083(7) 0.30502(4) 0.73582(4) 0.03123(19) Uani 1 1 d . . . . . O1 O 0.4032(3) 0.22680(19) 0.69171(19) 0.0342(6) Uani 1 1 d . . . . . O2 O 0.1687(3) 0.28765(18) 0.59551(18) 0.0326(6) Uani 1 1 d . . . . . O3 O 0.4269(3) 0.16171(19) 0.40577(19) 0.0340(6) Uani 1 1 d . . . . . N1 N 0.3161(4) 0.4315(2) 0.7101(2) 0.0328(7) Uani 1 1 d . . . . . N2 N 0.2345(4) 0.3094(2) 0.8802(2) 0.0324(7) Uani 1 1 d . . . . . N3 N 0.1128(4) 0.1667(2) 0.7973(2) 0.0336(7) Uani 1 1 d . . . . . N4 N -0.0234(4) 0.3939(2) 0.7895(2) 0.0319(7) Uani 1 1 d . . . . . C1 C 0.3424(4) 0.4914(3) 0.6260(3) 0.0356(8) Uani 1 1 d . . . . . H1 H 0.306848 0.473350 0.568517 0.043 Uiso 1 1 calc R U . . . C2 C 0.4190(5) 0.5777(3) 0.6206(3) 0.0416(9) Uani 1 1 d . . . . . H2 H 0.439915 0.617131 0.559399 0.050 Uiso 1 1 calc R U . . . C3 C 0.4655(5) 0.6071(3) 0.7050(3) 0.0436(10) Uani 1 1 d . . . . . H3 H 0.513064 0.668414 0.703654 0.052 Uiso 1 1 calc R U . . . C4 C 0.4412(5) 0.5449(3) 0.7911(3) 0.0417(9) Uani 1 1 d . . . . . H4 H 0.472481 0.562756 0.850074 0.050 Uiso 1 1 calc R U . . . C5 C 0.3708(4) 0.4564(3) 0.7903(3) 0.0342(8) Uani 1 1 d . . . . . C6 C 0.3579(5) 0.3805(3) 0.8790(3) 0.0370(8) Uani 1 1 d . . . . . H6A H 0.459047 0.344303 0.877702 0.044 Uiso 1 1 calc R U . . . H6B H 0.335642 0.414677 0.941040 0.044 Uiso 1 1 calc R U . . . C7 C 0.2826(5) 0.2076(3) 0.9112(3) 0.0379(9) Uani 1 1 d . . . . . H7A H 0.269436 0.198609 0.984725 0.045 Uiso 1 1 calc R U . . . H7B H 0.393988 0.195669 0.883806 0.045 Uiso 1 1 calc R U . . . C8 C 0.1847(5) 0.1344(3) 0.8739(3) 0.0365(8) Uani 1 1 d . . . . . C9 C 0.1759(5) 0.0381(3) 0.9143(3) 0.0437(10) Uani 1 1 d . . . . . H9 H 0.226815 0.017073 0.968799 0.052 Uiso 1 1 calc R U . . . C10 C 0.0928(5) -0.0270(3) 0.8749(3) 0.0451(10) Uani 1 1 d . . . . . H10 H 0.087394 -0.093691 0.900973 0.054 Uiso 1 1 calc R U . . . C11 C 0.0166(5) 0.0058(3) 0.7963(3) 0.0428(9) Uani 1 1 d . . . . . H11 H -0.044089 -0.037212 0.768955 0.051 Uiso 1 1 calc R U . . . C12 C 0.0319(5) 0.1028(3) 0.7593(3) 0.0385(9) Uani 1 1 d . . . . . H12 H -0.017291 0.125190 0.704482 0.046 Uiso 1 1 calc R U . . . C13 C 0.0852(5) 0.3385(3) 0.9417(3) 0.0363(8) Uani 1 1 d . . . . . H13A H 0.105006 0.359916 1.005531 0.044 Uiso 1 1 calc R U . . . H13B H 0.016766 0.281441 0.956745 0.044 Uiso 1 1 calc R U . . . C14 C 0.0050(5) 0.4214(3) 0.8874(3) 0.0372(8) Uani 1 1 d . . . . . H14A H -0.095597 0.438942 0.928876 0.045 Uiso 1 1 calc R U . . . H14B H 0.070479 0.479958 0.876905 0.045 Uiso 1 1 calc R U . . . C15 C -0.1672(4) 0.3353(3) 0.8057(3) 0.0350(8) Uani 1 1 d . . . . . H15A H -0.254893 0.373167 0.842433 0.042 Uiso 1 1 calc R U . . . H15B H -0.150835 0.273768 0.846873 0.042 Uiso 1 1 calc R U . . . C16 C -0.2086(5) 0.3104(3) 0.7070(3) 0.0388(9) Uani 1 1 d . . . . . H16A H -0.124678 0.267800 0.673024 0.047 Uiso 1 1 calc R U . . . H16B H -0.305882 0.273251 0.720324 0.047 Uiso 1 1 calc R U . . . C17 C -0.2305(5) 0.4023(3) 0.6387(3) 0.0436(10) Uani 1 1 d . . . . . H17A H -0.242421 0.383236 0.572382 0.052 Uiso 1 1 calc R U . . . H17B H -0.326250 0.439099 0.666605 0.052 Uiso 1 1 calc R U . . . C18 C -0.0905(5) 0.4673(3) 0.6284(3) 0.0404(9) Uani 1 1 d . . . . . H18A H 0.001300 0.434927 0.589453 0.049 Uiso 1 1 calc R U . . . H18B H -0.112021 0.530556 0.591551 0.049 Uiso 1 1 calc R U . . . C19 C -0.0540(5) 0.4867(3) 0.7293(3) 0.0380(9) Uani 1 1 d . . . . . H19A H 0.038468 0.528099 0.719579 0.046 Uiso 1 1 calc R U . . . H19B H -0.142906 0.523553 0.766122 0.046 Uiso 1 1 calc R U . . . C20 C 0.4108(4) 0.2039(3) 0.6041(3) 0.0307(8) Uani 1 1 d . . . . . C21 C 0.2880(4) 0.2367(3) 0.5493(3) 0.0313(8) Uani 1 1 d . . . . . C22 C 0.2984(4) 0.2110(3) 0.4527(3) 0.0317(8) Uani 1 1 d . . . . . C23 C 0.1813(4) 0.2294(3) 0.3875(3) 0.0325(8) Uani 1 1 d . . . . . C24 C 0.2208(5) 0.2200(3) 0.2848(3) 0.0368(8) Uani 1 1 d . . . . . H24 H 0.325076 0.203297 0.256552 0.044 Uiso 1 1 calc R U . . . C25 C 0.1085(5) 0.2351(3) 0.2244(3) 0.0411(9) Uani 1 1 d . . . . . H25 H 0.137492 0.230420 0.154732 0.049 Uiso 1 1 calc R U . . . C26 C -0.0455(5) 0.2568(3) 0.2640(3) 0.0403(9) Uani 1 1 d . . . . . H26 H -0.122043 0.265995 0.222207 0.048 Uiso 1 1 calc R U . . . C27 C -0.0856(5) 0.2647(3) 0.3649(3) 0.0385(9) Uani 1 1 d . . . . . H27 H -0.191117 0.278587 0.392751 0.046 Uiso 1 1 calc R U . . . C28 C 0.0255(5) 0.2527(3) 0.4265(3) 0.0361(8) Uani 1 1 d . . . . . H28 H -0.004127 0.260336 0.495669 0.043 Uiso 1 1 calc R U . . . C29 C 0.5376(4) 0.1442(3) 0.5558(3) 0.0322(8) Uani 1 1 d . . . . . C30 C 0.6541(5) 0.0994(3) 0.6057(3) 0.0369(8) Uani 1 1 d . . . . . H30 H 0.652792 0.109428 0.673695 0.044 Uiso 1 1 calc R U . . . C31 C 0.7695(5) 0.0412(3) 0.5561(3) 0.0384(9) Uani 1 1 d . . . . . H31 H 0.846795 0.010082 0.590237 0.046 Uiso 1 1 calc R U . . . C32 C 0.7735(5) 0.0275(3) 0.4553(3) 0.0400(9) Uani 1 1 d . . . . . H32 H 0.855385 -0.011414 0.421222 0.048 Uiso 1 1 calc R U . . . C33 C 0.6602(5) 0.0697(3) 0.4049(3) 0.0371(8) Uani 1 1 d . . . . . H33 H 0.663176 0.060378 0.336635 0.045 Uiso 1 1 calc R U . . . C34 C 0.5418(4) 0.1263(3) 0.4564(3) 0.0331(8) Uani 1 1 d . . . . . Cl1C Cl 0.61635(12) 0.22664(8) 1.06757(7) 0.0444(3) Uani 1 1 d . . . . . O2C O 0.4795(4) 0.2896(2) 1.0672(2) 0.0514(8) Uani 1 1 d . . . . . O3C O 0.7493(4) 0.2834(3) 1.0640(3) 0.0675(10) Uani 1 1 d . . . . . O4C O 0.5953(4) 0.1630(3) 1.1575(3) 0.0743(12) Uani 1 1 d . . . . . O5C O 0.6394(4) 0.1696(3) 0.9829(3) 0.0597(9) Uani 1 1 d . . . . . O1W O 0.6376(9) -0.0002(7) 0.8632(7) 0.076(2) Uani 0.5 1 d G . P . . H1WA H 0.609220 0.058086 0.882053 0.113 Uiso 0.5 1 d G U P . . H1WB H 0.551117 -0.026571 0.857360 0.113 Uiso 0.5 1 d G U P . . 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 0.0341(4) 0.0296(3) 0.0294(3) -0.0017(2) -0.0043(3) -0.0005(3) O1 0.0333(14) 0.0362(14) 0.0330(14) -0.0042(11) -0.0056(11) 0.0028(11) O2 0.0331(14) 0.0336(13) 0.0313(13) -0.0044(10) -0.0057(10) 0.0024(10) O3 0.0351(14) 0.0340(13) 0.0319(13) -0.0025(10) -0.0038(11) 0.0013(11) N1 0.0302(16) 0.0337(16) 0.0332(16) -0.0004(13) -0.0031(12) 0.0004(12) N2 0.0322(16) 0.0339(16) 0.0309(16) -0.0031(12) -0.0039(12) -0.0018(13) N3 0.0365(17) 0.0301(16) 0.0334(16) -0.0031(13) -0.0040(13) 0.0001(13) N4 0.0331(16) 0.0275(15) 0.0339(16) 0.0001(12) -0.0035(13) -0.0006(12) C1 0.0300(19) 0.039(2) 0.036(2) 0.0013(16) -0.0032(15) 0.0027(15) C2 0.039(2) 0.033(2) 0.050(2) 0.0057(17) -0.0043(18) 0.0003(16) C3 0.041(2) 0.031(2) 0.058(3) 0.0001(18) -0.0079(19) -0.0032(17) C4 0.042(2) 0.037(2) 0.049(2) -0.0077(18) -0.0121(18) -0.0010(17) C5 0.0323(19) 0.0331(19) 0.037(2) -0.0037(15) -0.0047(15) 0.0005(15) C6 0.040(2) 0.037(2) 0.035(2) -0.0027(16) -0.0087(16) -0.0010(16) C7 0.040(2) 0.039(2) 0.034(2) 0.0020(16) -0.0057(16) -0.0009(17) C8 0.038(2) 0.035(2) 0.035(2) -0.0008(15) -0.0052(16) 0.0026(16) C9 0.052(3) 0.036(2) 0.041(2) 0.0035(17) -0.0087(19) 0.0028(18) C10 0.053(3) 0.029(2) 0.050(2) 0.0048(17) -0.004(2) -0.0003(18) C11 0.045(2) 0.034(2) 0.048(2) -0.0049(17) -0.0049(19) -0.0037(17) C12 0.040(2) 0.036(2) 0.040(2) -0.0052(16) -0.0071(17) 0.0016(16) C13 0.042(2) 0.039(2) 0.0282(18) -0.0051(15) -0.0042(16) -0.0005(17) C14 0.037(2) 0.036(2) 0.037(2) -0.0063(16) -0.0018(16) 0.0013(16) C15 0.0303(19) 0.036(2) 0.036(2) -0.0033(16) 0.0000(15) 0.0003(15) C16 0.035(2) 0.038(2) 0.044(2) -0.0071(17) -0.0081(17) -0.0001(16) C17 0.041(2) 0.048(2) 0.043(2) -0.0040(18) -0.0135(18) 0.0088(18) C18 0.045(2) 0.035(2) 0.039(2) 0.0013(16) -0.0042(17) 0.0106(17) C19 0.041(2) 0.0285(19) 0.042(2) -0.0005(16) -0.0032(17) 0.0033(16) C20 0.0297(18) 0.0265(17) 0.0340(19) 0.0001(14) -0.0005(14) -0.0038(14) C21 0.0283(18) 0.0276(17) 0.037(2) 0.0000(14) -0.0025(15) -0.0037(14) C22 0.0287(18) 0.0280(18) 0.036(2) 0.0000(14) -0.0013(15) -0.0006(14) C23 0.037(2) 0.0247(17) 0.036(2) -0.0020(14) -0.0060(15) -0.0043(14) C24 0.040(2) 0.034(2) 0.036(2) -0.0015(16) -0.0047(16) -0.0048(16) C25 0.055(3) 0.037(2) 0.032(2) -0.0015(16) -0.0095(18) -0.0060(18) C26 0.046(2) 0.034(2) 0.044(2) -0.0009(17) -0.0179(18) -0.0021(17) C27 0.036(2) 0.034(2) 0.047(2) -0.0031(17) -0.0123(17) 0.0006(16) C28 0.039(2) 0.0318(19) 0.037(2) -0.0022(15) -0.0055(16) -0.0017(16) C29 0.0319(19) 0.0270(17) 0.036(2) -0.0008(14) -0.0025(15) -0.0040(14) C30 0.038(2) 0.0329(19) 0.041(2) -0.0028(16) -0.0080(16) -0.0032(16) C31 0.033(2) 0.0320(19) 0.051(2) -0.0036(17) -0.0099(17) 0.0012(15) C32 0.033(2) 0.033(2) 0.051(2) -0.0082(17) 0.0024(17) 0.0017(16) C33 0.035(2) 0.034(2) 0.042(2) -0.0065(16) -0.0027(16) -0.0039(16) C34 0.0286(19) 0.0284(18) 0.041(2) -0.0005(15) -0.0017(15) -0.0027(14) Cl1C 0.0406(5) 0.0544(6) 0.0366(5) 0.0038(4) -0.0065(4) 0.0006(4) O2C 0.0542(19) 0.0500(18) 0.0553(19) -0.0059(14) -0.0241(15) 0.0027(14) O3C 0.052(2) 0.108(3) 0.0442(19) -0.0103(19) -0.0057(15) -0.018(2) O4C 0.064(2) 0.092(3) 0.052(2) 0.0297(19) 0.0063(17) 0.024(2) O5C 0.066(2) 0.056(2) 0.055(2) -0.0072(16) -0.0025(16) 0.0033(16) O1W 0.055(4) 0.088(6) 0.085(6) -0.034(5) 0.004(4) -0.019(4) 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.1360 0 -1 0 0.1420 0 1 1 0.1051 0 -1 -1 0.1017 1 0 0 0.3064 -1 0 0 0.3374 0 0 -1 0.1059 0 0 1 0.1272 -1 -1 1 0.2337 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 N4 175.58(11) . . ? O2 Ni1 O1 81.39(10) . . ? O2 Ni1 N1 98.50(12) . . ? O2 Ni1 N2 173.01(12) . . ? O2 Ni1 N3 97.03(12) . . ? O2 Ni1 N4 102.23(11) . . ? N1 Ni1 O1 87.44(11) . . ? N1 Ni1 N2 83.23(12) . . ? N1 Ni1 N3 160.71(13) . . ? N1 Ni1 N4 89.49(12) . . ? N2 Ni1 O1 91.96(11) . . ? N2 Ni1 N3 80.03(12) . . ? N2 Ni1 N4 84.51(12) . . ? N3 Ni1 O1 83.64(11) . . ? N3 Ni1 N4 98.34(12) . . ? C20 O1 Ni1 109.4(2) . . ? C21 O2 Ni1 111.7(2) . . ? C34 O3 C22 120.9(3) . . ? C1 N1 Ni1 127.9(3) . . ? C1 N1 C5 118.4(3) . . ? C5 N1 Ni1 113.7(2) . . ? C6 N2 Ni1 108.8(2) . . ? C6 N2 C7 112.6(3) . . ? C7 N2 Ni1 105.6(2) . . ? C13 N2 Ni1 106.5(2) . . ? C13 N2 C6 112.4(3) . . ? C13 N2 C7 110.7(3) . . ? C8 N3 Ni1 111.0(3) . . ? C12 N3 Ni1 129.0(3) . . ? C12 N3 C8 118.4(3) . . ? C14 N4 Ni1 102.5(2) . . ? C14 N4 C15 108.9(3) . . ? C14 N4 C19 107.4(3) . . ? C15 N4 Ni1 112.4(2) . . ? C19 N4 Ni1 117.6(2) . . ? C19 N4 C15 107.7(3) . . ? N1 C1 H1 118.9 . . ? N1 C1 C2 122.1(4) . . ? C2 C1 H1 118.9 . . ? C1 C2 H2 120.2 . . ? C1 C2 C3 119.6(4) . . ? C3 C2 H2 120.2 . . ? C2 C3 H3 120.8 . . ? C4 C3 C2 118.4(4) . . ? C4 C3 H3 120.8 . . ? C3 C4 H4 120.4 . . ? C3 C4 C5 119.1(4) . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 122.0(4) . . ? N1 C5 C6 116.7(3) . . ? C4 C5 C6 121.2(4) . . ? N2 C6 C5 112.9(3) . . ? N2 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? N2 C7 C8 110.1(3) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? N3 C8 C7 116.9(3) . . ? N3 C8 C9 121.8(4) . . ? C9 C8 C7 121.2(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 C8 119.4(4) . . ? C10 C9 H9 120.3 . . ? C9 C10 H10 120.3 . . ? C9 C10 C11 119.4(4) . . ? C11 C10 H10 120.3 . . ? C10 C11 H11 121.0 . . ? C12 C11 C10 118.0(4) . . ? C12 C11 H11 121.0 . . ? N3 C12 C11 123.1(4) . . ? N3 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? N2 C13 H13A 109.6 . . ? N2 C13 H13B 109.6 . . ? N2 C13 C14 110.4(3) . . ? H13A C13 H13B 108.1 . . ? C14 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? N4 C14 C13 111.7(3) . . ? N4 C14 H14A 109.3 . . ? N4 C14 H14B 109.3 . . ? C13 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? N4 C15 H15A 109.4 . . ? N4 C15 H15B 109.4 . . ? N4 C15 C16 111.3(3) . . ? H15A C15 H15B 108.0 . . ? C16 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C15 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C17 C16 C15 111.9(3) . . ? C17 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? C16 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C18 C17 C16 110.0(3) . . ? C18 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? C17 C18 H18A 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? C19 C18 C17 111.5(3) . . ? C19 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? N4 C19 C18 112.0(3) . . ? N4 C19 H19A 109.2 . . ? N4 C19 H19B 109.2 . . ? C18 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? O1 C20 C21 119.5(3) . . ? O1 C20 C29 122.3(3) . . ? C29 C20 C21 118.2(3) . . ? O2 C21 C20 117.9(3) . . ? O2 C21 C22 123.3(3) . . ? C22 C21 C20 118.8(3) . . ? O3 C22 C21 121.6(3) . . ? O3 C22 C23 110.9(3) . . ? C21 C22 C23 127.4(3) . . ? C24 C23 C22 120.8(3) . . ? C24 C23 C28 118.1(4) . . ? C28 C23 C22 121.1(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 119.8 . . ? C24 C25 H25 119.4 . . ? C24 C25 C26 121.1(4) . . ? C26 C25 H25 119.4 . . ? C25 C26 H26 120.6 . . ? C27 C26 C25 118.9(4) . . ? C27 C26 H26 120.6 . . ? C26 C27 H27 119.4 . . ? C26 C27 C28 121.1(4) . . ? C28 C27 H27 119.4 . . ? C23 C28 H28 119.8 . . ? C27 C28 C23 120.5(4) . . ? C27 C28 H28 119.8 . . ? C30 C29 C20 122.9(4) . . ? C34 C29 C20 118.7(3) . . ? C34 C29 C30 118.4(3) . . ? C29 C30 H30 120.0 . . ? C31 C30 C29 120.0(4) . . ? C31 C30 H30 120.0 . . ? C30 C31 H31 119.9 . . ? C30 C31 C32 120.2(4) . . ? C32 C31 H31 119.9 . . ? C31 C32 H32 119.5 . . ? C33 C32 C31 121.0(4) . . ? C33 C32 H32 119.5 . . ? C32 C33 H33 120.8 . . ? C32 C33 C34 118.4(4) . . ? C34 C33 H33 120.8 . . ? O3 C34 C29 121.4(3) . . ? O3 C34 C33 116.6(3) . . ? C33 C34 C29 122.0(4) . . ? O3C Cl1C O2C 110.3(2) . . ? O3C Cl1C O4C 109.0(3) . . ? O3C Cl1C O5C 109.0(2) . . ? O4C Cl1C O2C 108.6(2) . . ? O5C Cl1C O2C 109.8(2) . . ? O5C Cl1C O4C 110.0(2) . . ? H1WA O1W H1WB 104.5 . . ? 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 O1 2.116(3) . ? Ni1 O2 1.999(3) . ? Ni1 N1 2.059(3) . ? Ni1 N2 2.084(3) . ? Ni1 N3 2.094(3) . ? Ni1 N4 2.231(3) . ? O1 C20 1.255(5) . ? O2 C21 1.322(4) . ? O3 C22 1.370(4) . ? O3 C34 1.364(5) . ? N1 C1 1.344(5) . ? N1 C5 1.347(5) . ? N2 C6 1.480(5) . ? N2 C7 1.483(5) . ? N2 C13 1.480(5) . ? N3 C8 1.347(5) . ? N3 C12 1.341(5) . ? N4 C14 1.486(5) . ? N4 C15 1.492(5) . ? N4 C19 1.492(5) . ? C1 H1 0.9500 . ? C1 C2 1.373(6) . ? C2 H2 0.9500 . ? C2 C3 1.385(6) . ? C3 H3 0.9500 . ? C3 C4 1.383(6) . ? C4 H4 0.9500 . ? C4 C5 1.383(6) . ? C5 C6 1.519(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.519(6) . ? C8 C9 1.384(6) . ? C9 H9 0.9500 . ? C9 C10 1.374(6) . ? C10 H10 0.9500 . ? C10 C11 1.393(6) . ? C11 H11 0.9500 . ? C11 C12 1.381(6) . ? C12 H12 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.513(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.528(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.524(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.523(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.518(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.447(5) . ? C20 C29 1.443(5) . ? C21 C22 1.384(5) . ? C22 C23 1.470(5) . ? C23 C24 1.402(5) . ? C23 C28 1.404(6) . ? C24 H24 0.9500 . ? C24 C25 1.386(6) . ? C25 H25 0.9500 . ? C25 C26 1.387(6) . ? C26 H26 0.9500 . ? C26 C27 1.376(6) . ? C27 H27 0.9500 . ? C27 C28 1.388(6) . ? C28 H28 0.9500 . ? C29 C30 1.410(5) . ? C29 C34 1.397(5) . ? C30 H30 0.9500 . ? C30 C31 1.374(6) . ? C31 H31 0.9500 . ? C31 C32 1.403(6) . ? C32 H32 0.9500 . ? C32 C33 1.379(6) . ? C33 H33 0.9500 . ? C33 C34 1.389(5) . ? Cl1C O2C 1.440(3) . ? Cl1C O3C 1.416(4) . ? Cl1C O4C 1.434(3) . ? Cl1C O5C 1.433(4) . ? O1W H1WA 0.8700 . ? O1W H1WB 0.8698 . ? 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 C20 C21 3.4(4) . . . . ? Ni1 O1 C20 C29 -175.7(3) . . . . ? Ni1 O2 C21 C20 -0.6(4) . . . . ? Ni1 O2 C21 C22 177.3(3) . . . . ? Ni1 N1 C1 C2 175.2(3) . . . . ? Ni1 N1 C5 C4 -172.0(3) . . . . ? Ni1 N1 C5 C6 10.5(4) . . . . ? Ni1 N2 C6 C5 22.9(4) . . . . ? Ni1 N2 C7 C8 -39.5(3) . . . . ? Ni1 N2 C13 C14 -43.3(3) . . . . ? Ni1 N3 C8 C7 9.8(4) . . . . ? Ni1 N3 C8 C9 -167.4(3) . . . . ? Ni1 N3 C12 C11 165.3(3) . . . . ? Ni1 N4 C14 C13 -37.8(3) . . . . ? Ni1 N4 C15 C16 -70.8(3) . . . . ? Ni1 N4 C19 C18 67.2(4) . . . . ? O1 C20 C21 O2 -2.1(5) . . . . ? O1 C20 C21 C22 179.9(3) . . . . ? O1 C20 C29 C30 6.2(6) . . . . ? O1 C20 C29 C34 -176.6(3) . . . . ? O2 C21 C22 O3 177.2(3) . . . . ? O2 C21 C22 C23 -3.4(6) . . . . ? O3 C22 C23 C24 -15.5(5) . . . . ? O3 C22 C23 C28 161.7(3) . . . . ? N1 C1 C2 C3 -2.8(6) . . . . ? N1 C5 C6 N2 -23.0(5) . . . . ? N2 C7 C8 N3 20.6(5) . . . . ? N2 C7 C8 C9 -162.2(4) . . . . ? N2 C13 C14 N4 57.7(4) . . . . ? N3 C8 C9 C10 0.6(6) . . . . ? N4 C15 C16 C17 -57.3(4) . . . . ? C1 N1 C5 C4 5.4(6) . . . . ? C1 N1 C5 C6 -172.0(3) . . . . ? C1 C2 C3 C4 3.8(6) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C3 C4 C5 N1 -4.3(6) . . . . ? C3 C4 C5 C6 173.0(4) . . . . ? C4 C5 C6 N2 159.5(4) . . . . ? C5 N1 C1 C2 -1.8(6) . . . . ? C6 N2 C7 C8 -158.0(3) . . . . ? C6 N2 C13 C14 75.7(4) . . . . ? C7 N2 C6 C5 139.6(3) . . . . ? C7 N2 C13 C14 -157.5(3) . . . . ? C7 C8 C9 C10 -176.5(4) . . . . ? C8 N3 C12 C11 1.1(6) . . . . ? C8 C9 C10 C11 -1.2(7) . . . . ? C9 C10 C11 C12 1.8(6) . . . . ? C10 C11 C12 N3 -1.8(6) . . . . ? C12 N3 C8 C7 176.7(3) . . . . ? C12 N3 C8 C9 -0.5(6) . . . . ? C13 N2 C6 C5 -94.7(4) . . . . ? C13 N2 C7 C8 75.3(4) . . . . ? C14 N4 C15 C16 176.3(3) . . . . ? C14 N4 C19 C18 -178.0(3) . . . . ? C15 N4 C14 C13 81.5(4) . . . . ? C15 N4 C19 C18 -60.9(4) . . . . ? C15 C16 C17 C18 51.4(5) . . . . ? C16 C17 C18 C19 -51.4(4) . . . . ? C17 C18 C19 N4 57.9(4) . . . . ? C19 N4 C14 C13 -162.3(3) . . . . ? C19 N4 C15 C16 60.2(4) . . . . ? C20 C21 C22 O3 -4.9(5) . . . . ? C20 C21 C22 C23 174.5(3) . . . . ? C20 C29 C30 C31 178.2(3) . . . . ? C20 C29 C34 O3 -1.9(5) . . . . ? C20 C29 C34 C33 179.9(3) . . . . ? C21 C20 C29 C30 -172.9(3) . . . . ? C21 C20 C29 C34 4.3(5) . . . . ? C21 C22 C23 C24 165.0(4) . . . . ? C21 C22 C23 C28 -17.8(6) . . . . ? C22 O3 C34 C29 -4.1(5) . . . . ? C22 O3 C34 C33 174.3(3) . . . . ? C22 C23 C24 C25 178.3(3) . . . . ? C22 C23 C28 C27 -176.5(3) . . . . ? C23 C24 C25 C26 -1.9(6) . . . . ? C24 C23 C28 C27 0.8(5) . . . . ? C24 C25 C26 C27 0.9(6) . . . . ? C25 C26 C27 C28 0.9(6) . . . . ? C26 C27 C28 C23 -1.8(6) . . . . ? C28 C23 C24 C25 1.0(5) . . . . ? C29 C20 C21 O2 177.0(3) . . . . ? C29 C20 C21 C22 -1.0(5) . . . . ? C29 C30 C31 C32 1.1(6) . . . . ? C30 C29 C34 O3 175.4(3) . . . . ? C30 C29 C34 C33 -2.9(5) . . . . ? C30 C31 C32 C33 -1.7(6) . . . . ? C31 C32 C33 C34 0.0(6) . . . . ? C32 C33 C34 O3 -176.0(3) . . . . ? C32 C33 C34 C29 2.3(6) . . . . ? C34 O3 C22 C21 7.6(5) . . . . ? C34 O3 C22 C23 -171.9(3) . . . . ? C34 C29 C30 C31 1.1(5) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0000 1.0000 -0.0000 0.0038 -0.1129 0.0062 0.0000 -1.0000 0.0000 -0.0038 0.1129 -0.0062 -0.0000 1.0000 1.0000 0.1177 -0.0998 0.0080 0.0000 -1.0000 -1.0000 -0.1177 0.0998 -0.0080 1.0000 0.0000 0.0001 -0.0355 0.0140 0.1753 -1.0000 -0.0000 -0.0001 0.0355 -0.0140 -0.1753 0.0000 0.0000 -1.0000 -0.1139 -0.0132 -0.0018 -0.0000 -0.0000 1.0000 0.1139 0.0132 0.0018 -1.0001 -1.0000 0.9999 0.1456 0.1121 -0.1797