#------------------------------------------------------------------------------ #$Date: 2026-04-29 01:35:00 +0100 (Wed, 29 Apr 2026) $ #$Revision: 305650 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/43/7064388.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_7064388 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 H33 Br2 N4 Ni O3, Cl O4' _chemical_formula_sum 'C34 H33 Br2 Cl N4 Ni O7' _chemical_formula_weight 863.62 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-09-09 _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 90 _cell_angle_beta 105.9340(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.63340(10) _cell_length_b 30.0080(2) _cell_length_c 12.03790(10) _cell_measurement_reflns_used 44719 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 79.4560 _cell_measurement_theta_min 2.9010 _cell_volume 3346.20(5) _computing_cell_refinement 'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro system (CCD 43.128a 64-bit (release 20-06-2024))' _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 -64.00 25.00 0.50 0.30 -- -47.48 61.00 157.00 178 2 \w -120.00 -31.00 0.50 0.30 -- -47.48 -61.00 19.00 178 3 \w -64.00 25.00 0.50 0.30 -- -47.48 61.00 157.00 178 4 \w -120.00 -31.00 0.50 0.30 -- -47.48 -61.00 19.00 178 5 \w -75.00 -19.00 0.50 1.50 -- -91.75 61.00 157.00 112 6 \w -163.00 -75.00 0.50 1.50 -- -91.75 -61.00 19.00 176 7 \w 42.00 75.00 0.50 1.50 -- 113.25 -61.00 19.00 66 8 \w 97.00 178.00 0.50 1.50 -- 113.25 61.00 157.00 162 9 \w -12.00 28.00 0.50 0.30 -- -47.48 19.00 150.00 80 10 \w -62.00 25.00 0.50 0.30 -- -47.48 57.00 30.00 174 11 \w 35.00 120.00 0.50 0.30 -- 47.48 46.00 -15.21 170 12 \w 34.00 93.00 0.50 0.30 -- 47.48-125.00-120.00 118 13 \w 31.00 120.00 0.50 0.30 -- 47.48 61.00 157.00 178 14 \w 35.00 119.00 0.50 0.30 -- 47.48 45.00 -78.28 168 15 \w -24.00 64.00 0.50 0.30 -- 47.48 -61.00 19.00 176 16 \w -163.00 -81.00 0.50 1.50 -- -91.75 -47.00-158.31 164 17 \w -49.00 -20.00 0.50 1.50 -- -91.75 45.00 0.00 58 18 \w -163.00 -79.00 0.50 1.50 -- -91.75 -46.00-104.06 168 19 \w -108.00 -83.00 0.50 1.50 -- -91.75 -47.00-136.86 50 20 \w -49.00 -22.00 0.50 1.50 -- -91.75 45.00 -30.00 54 21 \w -165.00-139.00 0.50 1.50 -- -91.75 -35.00 -85.44 52 22 \w -49.00 -20.00 0.50 1.50 -- -91.75 45.00 150.00 58 23 \w -118.00 -92.00 0.50 1.50 -- -91.75 -35.00 -85.44 52 24 \w -112.00 -87.00 0.50 1.50 -- -91.75 -48.00 -87.06 50 25 \w -114.00 -80.00 0.50 1.50 -- -91.75 -45.00-120.00 68 26 \w 109.00 177.00 0.50 1.50 -- 113.25 45.00-150.00 136 27 \w 102.00 136.00 0.50 1.50 -- 113.25 45.00 30.00 68 28 \w 106.00 177.00 0.50 1.50 -- 113.25 61.00 60.00 142 29 \w 42.00 70.00 0.50 1.50 -- 113.25 -61.00 150.00 56 30 \w 51.00 104.00 0.50 1.50 -- 113.25 -95.00 -90.00 106 31 \w 149.00 176.00 0.50 1.50 -- 113.25 15.00 60.00 54 32 \w 131.00 156.00 0.50 1.50 -- 113.25 125.00-120.00 50 33 \w 43.00 72.00 0.50 1.50 -- 113.25 -61.00-180.00 58 34 \w 42.00 103.00 0.50 1.50 -- 113.25 -95.00 120.00 122 35 \w 42.00 74.00 0.50 1.50 -- 113.25 -61.00 -30.00 64 36 \w 143.00 178.00 0.50 1.50 -- 113.25 45.00 30.00 70 37 \w 102.00 132.00 0.50 1.50 -- 113.25 45.00 -90.00 60 38 \w 135.00 178.00 0.50 1.50 -- 113.25 77.00-150.00 86 39 \w 146.00 174.00 0.50 1.50 -- 113.25 30.00 -30.00 56 40 \w 105.00 131.00 0.50 1.50 -- 113.25 30.00 -30.00 52 41 \w 111.00 152.00 0.50 1.50 -- 113.25 30.00 -60.00 82 42 \w 151.00 177.00 0.50 1.50 -- 113.25 45.00-120.00 52 43 \w 106.00 151.00 0.50 1.50 -- 113.25 61.00-120.00 90 44 \w 105.00 145.00 0.50 1.50 -- 113.25 45.00-120.00 80 45 \w 42.00 75.00 0.50 1.50 -- 113.25 -61.00 -90.00 66 46 \w 111.00 136.00 0.50 1.50 -- 113.25 -77.00 -60.00 50 47 \w 47.00 73.00 0.50 1.50 -- 113.25 -61.00 0.00 52 48 \w 101.00 143.00 0.50 1.50 -- 113.25 45.00 -30.00 84 49 \w 140.00 165.00 0.50 1.50 -- 113.25 77.00 90.00 50 50 \w 106.00 132.00 0.50 1.50 -- 113.25 61.00 -90.00 52 51 \w 148.00 174.00 0.50 1.50 -- 113.25 61.00 -90.00 52 52 \w 66.00 97.00 0.50 1.50 -- 113.25 -77.00 -60.00 62 53 \w 117.00 150.00 0.50 1.50 -- 113.25 77.00-180.00 66 54 \w 106.00 176.00 0.50 1.50 -- 113.25 61.00 -60.00 140 55 \w 129.00 175.00 0.50 1.50 -- 113.25 45.00 90.00 92 56 \w 78.00 109.00 0.50 1.50 -- 113.25-125.00 150.00 62 57 \w 108.00 134.00 0.50 1.50 -- 113.25 45.00 -60.00 52 58 \w 58.00 104.00 0.50 1.50 -- 113.25 -95.00 90.00 92 59 \w 43.00 69.00 0.50 1.50 -- 113.25 -77.00 120.00 52 60 \w 106.00 132.00 0.50 1.50 -- 113.25 -77.00 120.00 52 61 \w 42.00 73.00 0.50 1.50 -- 113.25 -61.00 60.00 62 62 \w 101.00 177.00 0.50 1.50 -- 113.25 45.00 150.00 152 63 \w 46.00 74.00 0.50 1.50 -- 113.25 -61.00 -60.00 56 64 \w 44.00 71.00 0.50 1.50 -- 113.25-125.00 150.00 54 ; _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 -0.1188513000 _diffrn_orient_matrix_UB_12 0.0009060000 _diffrn_orient_matrix_UB_13 -0.1156160000 _diffrn_orient_matrix_UB_21 0.0824733000 _diffrn_orient_matrix_UB_22 0.0368542000 _diffrn_orient_matrix_UB_23 -0.0444585000 _diffrn_orient_matrix_UB_31 0.0820144000 _diffrn_orient_matrix_UB_32 -0.0357145000 _diffrn_orient_matrix_UB_33 -0.0487654000 _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 0.0244 _diffrn_reflns_av_unetI/netI 0.0105 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 68828 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.498 _diffrn_reflns_theta_min 2.945 _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 4.841 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.529 _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 blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.714 _exptl_crystal_description block _exptl_crystal_F_000 1744 _exptl_crystal_size_max 0.177 _exptl_crystal_size_mid 0.143 _exptl_crystal_size_min 0.034 _refine_diff_density_max 1.273 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 824 _refine_ls_number_reflns 6828 _refine_ls_number_restraints 2434 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0653 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+11.2321P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1585 _refine_ls_wR_factor_ref 0.1592 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6605 _reflns_number_total 6828 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj00257a2.cif _cod_data_source_block kskr30a _cod_database_code 7064388 _shelx_shelxl_version_number 2019/1 _chemical_oxdiff_formula C34H33Br2N4ClNiO7 _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 0.853 _shelx_estimated_absorpt_t_min 0.481 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances C25-C24 \\sim C26-C25 \\sim C24-C23 \\sim C23-C22 \\sim C27-C22 \\sim C27-C26 with sigma of 0.01 Ni1-N2A \\sim Ni1-N2 with sigma of 0.01 Ni1-N3A \\sim Ni1-N3 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints Ni1 \\sim Br1 \\sim Br2 \\sim N1 \\sim N2 \\sim N3 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim N4 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim O1 \\sim O2 \\sim O3 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim Br1A \\sim Br2A \\sim N1A \\sim N2A \\sim N3A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim N4A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim O1A \\sim O2A \\sim O3A \\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Uanis(C17A) = Uanis(C17) 4. Rigid body (RIGU) restrains Ni1, Br1, Br2, N1, N2, N3, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, N4, C13, C14, C15, C16, C17, C18, C19, O1, O2, O3, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, Br1A, Br2A, N1A, N2A, N3A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A, N4A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, O1A, O2A, O3A, C20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Same fragment restrains {O1, O2, O3, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34} sigma for 1-2: 0.01, 1-3: 0.04 as in {O1A, O2A, O3A, C20A, C21A, C22A, C23A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A} {N4, C13, C14, C15, C16, C17, C18, C19} sigma for 1-2: 0.01, 1-3: 0.04 as in {N4A, C13A, C14A, C15A, C16A, C17A, C18A, C19A} {Br1, Br2, N1, N2, N3, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12} sigma for 1-2: 0.01, 1-3: 0.04 as in {Br1A, Br2A, N1A, N2A, N3A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A} 6. Others Sof(Br1A)=Sof(Br2A)=Sof(N1A)=Sof(N2A)=Sof(N3A)=Sof(C1A)=Sof(C2A)=Sof(H2A)= Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)= Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)= Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(N4A)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)= Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)= Sof(H16D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18C)=Sof(H18D)= Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(C20A)=Sof(C21A)= Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)= Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(C28A)=Sof(C29A)=Sof(C30A)=Sof(H30A)= Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)= Sof(H34A)=1-FVAR(1) Sof(Br1)=Sof(Br2)=Sof(N1)=Sof(N2)=Sof(N3)=Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)= Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)= Sof(H7B)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)= Sof(N4)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)= Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)= Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(O1)=Sof(O2)= Sof(O3)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)= Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)= Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)= Sof(H34)=FVAR(1) 7.a 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), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C13A(H13C,H13D), C14A(H14C,H14D), C15A(H15C,H15D), C16A(H16C, H16D), C17A(H17C,H17D), C18A(H18C,H18D), C19A(H19C,H19D) 7.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C2A(H2A), C3A(H3A), C4A(H4A), C9A(H9A), C10A(H10A), C11A(H11A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A) ; _shelx_res_file ; TITL kskr30a_a.res in P2(1)/n kskr30a.res created by SHELXL-2019/1 at 15:19:04 on 09-Sep-2024 REM Old TITL KSKR30A in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.311, Rweak 0.060, Alpha 0.082 REM 1.495 for 156 systematic absences, Orientation as input REM Formula found by SHELXT: C36 N8 O7 Cl Ni Br2 CELL 1.54184 9.6334 30.008 12.0379 90 105.934 90 ZERR 4 0.0001 0.0002 0.0001 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Br Cl N Ni O UNIT 136 132 8 4 16 4 28 SADI 0.01 C25 C24 C26 C25 C24 C23 C23 C22 C27 C22 C27 C26 EADP C17A C17 SADI 0.01 Ni1 N2A Ni1 N2 SADI 0.01 Ni1 N3A Ni1 N3 RIGU 0.01 0.01 Ni1 > C34A SIMU 0.01 0.02 2 Ni1 > C34A L.S. 8 0 0 PLAN 10 SIZE 0.034 0.143 0.177 TEMP -173.15(10) CONF BOND list 4 MORE -1 BOND $H wpdb -1 fmap 2 53 acta OMIT 3 1 1 OMIT 4 0 2 REM REM REM WGHT 0.061300 11.232100 FVAR 0.25749 0.61037 NI1 6 0.358117 0.649437 0.337622 11.00000 0.01911 0.03647 = 0.05788 -0.00197 0.00361 0.00291 PART 1 BR1 3 0.279684 0.529287 0.271521 21.00000 0.05809 0.04706 = 0.07985 -0.02015 -0.00063 0.00003 BR2 3 0.203357 0.627005 0.039503 21.00000 0.14399 0.10617 = 0.04435 -0.02508 0.03465 -0.01594 N1 5 0.313195 0.590232 0.446461 21.00000 0.02598 0.03693 = 0.05311 0.00577 0.00293 -0.00259 N2 5 0.273911 0.676073 0.464052 21.00000 0.04089 0.03937 = 0.03131 0.00740 -0.00133 -0.00191 N3 5 0.136267 0.650828 0.241533 21.00000 0.02611 0.03456 = 0.03326 -0.00141 -0.00039 -0.00200 C1 1 0.316838 0.546899 0.427840 21.00000 0.03082 0.04118 = 0.05796 0.00121 0.00823 -0.00249 C2 1 0.342696 0.514313 0.512273 21.00000 0.03375 0.04000 = 0.05964 0.00728 0.00609 -0.00177 AFIX 43 H2 2 0.340364 0.483513 0.493598 21.00000 -1.20000 AFIX 0 C3 1 0.372115 0.528908 0.625272 21.00000 0.03607 0.04590 = 0.06183 0.01388 0.01006 -0.00083 AFIX 43 H3 2 0.394435 0.507953 0.686782 21.00000 -1.20000 AFIX 0 C4 1 0.369148 0.573854 0.648979 21.00000 0.03992 0.04533 = 0.05284 0.01278 -0.00085 -0.00289 AFIX 43 H4 2 0.388219 0.584189 0.726306 21.00000 -1.20000 AFIX 0 C5 1 0.337532 0.603672 0.556828 21.00000 0.03470 0.04381 = 0.04602 0.01007 0.00033 -0.00180 C6 1 0.329054 0.652864 0.577027 21.00000 0.04711 0.04269 = 0.03700 0.00980 -0.00484 0.00091 AFIX 23 H6A 2 0.263669 0.658568 0.626143 21.00000 -1.20000 H6B 2 0.425960 0.664421 0.617626 21.00000 -1.20000 AFIX 0 C7 1 0.114143 0.673057 0.429379 21.00000 0.03427 0.03993 = 0.03960 0.01069 0.01233 0.00844 AFIX 23 H7A 2 0.074514 0.700545 0.454412 21.00000 -1.20000 H7B 2 0.085048 0.647681 0.470533 21.00000 -1.20000 AFIX 0 C8 1 0.048204 0.667055 0.301875 21.00000 0.02279 0.03499 = 0.04103 0.00628 0.00441 0.00304 C9 1 -0.096403 0.675007 0.248776 21.00000 0.02352 0.04192 = 0.04789 0.00535 -0.00352 0.00355 AFIX 43 H9 2 -0.156978 0.685412 0.293628 21.00000 -1.20000 AFIX 0 C10 1 -0.153498 0.668146 0.132941 21.00000 0.03366 0.04717 = 0.04638 0.00674 -0.01601 -0.00232 AFIX 43 H10 2 -0.252873 0.673647 0.097245 21.00000 -1.20000 AFIX 0 C11 1 -0.065764 0.653336 0.069777 21.00000 0.04766 0.04586 = 0.03866 0.00245 -0.01175 -0.01502 AFIX 43 H11 2 -0.101634 0.648613 -0.011094 21.00000 -1.20000 AFIX 0 C12 1 0.079645 0.645214 0.127692 21.00000 0.04731 0.04318 = 0.03597 -0.00248 -0.00303 -0.01087 N4 5 0.407326 0.715894 0.306397 21.00000 0.02379 0.03740 = 0.04104 -0.00181 0.00486 0.00211 C13 1 0.305729 0.724389 0.474549 21.00000 0.04201 0.03813 = 0.02902 0.00264 0.00133 -0.00046 AFIX 23 H13A 2 0.329677 0.733550 0.556637 21.00000 -1.20000 H13B 2 0.220429 0.741593 0.430996 21.00000 -1.20000 AFIX 0 C14 1 0.435852 0.733586 0.424840 21.00000 0.04778 0.04672 = 0.04853 0.00030 0.00051 -0.00144 AFIX 23 H14A 2 0.453280 0.766087 0.424208 21.00000 -1.20000 H14B 2 0.523667 0.719382 0.474846 21.00000 -1.20000 AFIX 0 C15 1 0.294130 0.740094 0.219674 21.00000 0.04513 0.04760 = 0.05034 0.00509 0.00518 -0.00093 AFIX 23 H15A 2 0.205792 0.741628 0.246398 21.00000 -1.20000 H15B 2 0.270354 0.723302 0.146065 21.00000 -1.20000 AFIX 0 C16 1 0.340148 0.787386 0.198118 21.00000 0.06788 0.05004 = 0.06416 0.00853 0.01641 -0.00632 AFIX 23 H16A 2 0.334074 0.807074 0.262610 21.00000 -1.20000 H16B 2 0.274594 0.799267 0.125909 21.00000 -1.20000 AFIX 0 C17 1 0.501534 0.786613 0.187901 21.00000 0.09084 0.05467 = 0.07553 -0.00028 0.06274 -0.02486 AFIX 23 H17A 2 0.512193 0.764239 0.130366 21.00000 -1.20000 H17B 2 0.529422 0.816214 0.164734 21.00000 -1.20000 AFIX 0 C18 1 0.591530 0.774508 0.305484 21.00000 0.04930 0.05196 = 0.09851 0.00583 0.03672 -0.00622 AFIX 23 H18A 2 0.555339 0.786820 0.368568 21.00000 -1.20000 H18B 2 0.695511 0.781046 0.318553 21.00000 -1.20000 AFIX 0 C19 1 0.546922 0.718357 0.274797 21.00000 0.04018 0.05043 = 0.08411 0.00233 0.02357 -0.00113 AFIX 23 H19A 2 0.533856 0.711426 0.192153 21.00000 -1.20000 H19B 2 0.620519 0.698174 0.322980 21.00000 -1.20000 AFIX 0 O1 7 0.563736 0.636292 0.427265 21.00000 0.02107 0.03283 = 0.03109 -0.00377 0.00412 0.00524 O2 7 0.440945 0.622376 0.204864 21.00000 0.02241 0.04453 = 0.03462 -0.00994 -0.00104 0.00955 O3 7 0.837618 0.570269 0.347073 21.00000 0.02769 0.03592 = 0.04553 -0.00142 0.00799 0.01071 C20 1 0.636328 0.612939 0.371583 21.00000 0.02066 0.03161 = 0.03751 -0.00077 0.00267 0.00096 C21 1 0.567724 0.607254 0.248245 21.00000 0.02226 0.03198 = 0.03850 -0.00673 0.00563 0.00603 C22 1 0.644774 0.584273 0.178730 21.00000 0.03174 0.03472 = 0.04384 -0.00459 0.00921 0.00729 C23 1 0.590860 0.580049 0.058748 21.00000 0.05344 0.04510 = 0.04656 -0.01155 0.01555 0.01675 AFIX 43 H23 2 0.498652 0.591925 0.020686 21.00000 -1.20000 AFIX 0 C24 1 0.670964 0.558692 -0.004791 21.00000 0.05234 0.05862 = 0.05662 -0.00875 0.02032 0.02855 AFIX 43 H24 2 0.632474 0.556036 -0.086095 21.00000 -1.20000 AFIX 0 C25 1 0.805431 0.541182 0.047341 21.00000 0.05556 0.06185 = 0.05823 -0.00285 0.01854 0.02899 AFIX 43 H25 2 0.858980 0.526113 0.003258 21.00000 -1.20000 AFIX 0 C26 1 0.860343 0.546158 0.165757 21.00000 0.05827 0.04869 = 0.05356 -0.00368 0.02414 0.02028 AFIX 43 H26 2 0.953904 0.534972 0.202652 21.00000 -1.20000 AFIX 0 C27 1 0.781426 0.567223 0.232148 21.00000 0.03203 0.03475 = 0.05078 -0.00108 0.01473 0.01039 C28 1 0.767212 0.592145 0.418870 21.00000 0.02326 0.02855 = 0.04639 -0.00131 0.00589 0.00338 C29 1 0.841958 0.587858 0.541168 21.00000 0.02504 0.02993 = 0.04998 -0.00027 0.00366 0.00263 C30 1 0.974161 0.561450 0.570737 21.00000 0.02785 0.03837 = 0.06137 0.00551 0.00498 -0.00099 AFIX 43 H30 2 1.013942 0.549128 0.513543 21.00000 -1.20000 AFIX 0 C31 1 1.037178 0.555602 0.686631 21.00000 0.02966 0.04329 = 0.06133 0.00674 0.00544 0.00611 AFIX 43 H31 2 1.126185 0.539925 0.709266 21.00000 -1.20000 AFIX 0 C32 1 0.978647 0.571288 0.773960 21.00000 0.03424 0.03822 = 0.05785 0.00810 -0.00660 0.00218 AFIX 43 H32 2 1.026163 0.565945 0.853055 21.00000 -1.20000 AFIX 0 C33 1 0.848815 0.594950 0.741777 21.00000 0.03731 0.04017 = 0.05252 -0.00554 -0.00926 0.01114 AFIX 43 H33 2 0.805298 0.605507 0.798655 21.00000 -1.20000 AFIX 0 C34 1 0.784949 0.602720 0.626238 21.00000 0.03514 0.03743 = 0.04739 -0.00547 -0.00467 0.00809 AFIX 43 H34 2 0.697339 0.619155 0.604912 21.00000 -1.20000 AFIX 0 SAME 0.01 0.04 Br1 > C12 PART 2 BR1A 3 0.265360 0.534015 0.216840 -21.00000 0.06670 0.05815 = 0.07421 -0.02869 0.01507 -0.02093 BR2A 3 0.164188 0.642982 0.013734 -21.00000 0.02759 0.08276 = 0.03056 -0.00834 -0.01125 0.01779 N1A 5 0.319135 0.588531 0.409951 -21.00000 0.02547 0.04000 = 0.04696 0.00503 0.01121 -0.00011 N2A 5 0.285428 0.674706 0.470315 -21.00000 0.03815 0.04023 = 0.03282 0.00567 0.00218 -0.00121 N3A 5 0.137853 0.657769 0.236645 -21.00000 0.02743 0.03383 = 0.03608 0.00008 0.00322 -0.00360 C1A 1 0.303174 0.546303 0.377305 -21.00000 0.03205 0.03889 = 0.05052 -0.00171 0.01397 -0.00225 C2A 1 0.317483 0.510383 0.451798 -21.00000 0.03744 0.04044 = 0.05900 0.00298 0.01728 -0.00331 AFIX 43 H2A 2 0.305388 0.480666 0.423567 -21.00000 -1.20000 AFIX 0 C3A 1 0.349947 0.519335 0.568519 -21.00000 0.03500 0.04077 = 0.05273 0.00862 0.01201 -0.00154 AFIX 43 H3A 2 0.364873 0.495655 0.622902 -21.00000 -1.20000 AFIX 0 C4A 1 0.360488 0.562963 0.605363 -21.00000 0.03571 0.04402 = 0.04982 0.00941 0.01154 0.00273 AFIX 43 H4A 2 0.377109 0.569836 0.684980 -21.00000 -1.20000 AFIX 0 C5A 1 0.346354 0.596886 0.523832 -21.00000 0.02876 0.03991 = 0.04540 0.00700 0.01079 0.00355 C6A 1 0.366664 0.644639 0.563273 -21.00000 0.02479 0.04114 = 0.03317 0.00545 0.00977 0.01198 AFIX 23 H6AA 2 0.332100 0.648576 0.632879 -21.00000 -1.20000 H6AB 2 0.470564 0.652319 0.583934 -21.00000 -1.20000 AFIX 0 C7A 1 0.129108 0.665301 0.441085 -21.00000 0.03314 0.03930 = 0.03732 0.00940 0.00921 0.01131 AFIX 23 H7AA 2 0.081772 0.687735 0.478742 -21.00000 -1.20000 H7AB 2 0.113892 0.635625 0.471708 -21.00000 -1.20000 AFIX 0 C8A 1 0.060074 0.666167 0.312842 -21.00000 0.02250 0.03514 = 0.04285 0.00596 0.00499 0.00418 C9A 1 -0.085837 0.676779 0.283361 -21.00000 0.02238 0.03987 = 0.03802 0.00229 -0.00461 0.00139 AFIX 43 H9A 2 -0.131524 0.686253 0.339914 -21.00000 -1.20000 AFIX 0 C10A 1 -0.160559 0.673038 0.170141 -21.00000 0.03099 0.04274 = 0.04086 -0.00283 -0.00302 0.00264 AFIX 43 H10A 2 -0.261094 0.679259 0.146472 -21.00000 -1.20000 AFIX 0 C11A 1 -0.091455 0.660404 0.090867 -21.00000 0.03534 0.03777 = 0.03740 -0.00691 -0.00540 0.00365 AFIX 43 H11A 2 -0.145030 0.655583 0.012886 -21.00000 -1.20000 AFIX 0 C12A 1 0.060094 0.654405 0.124117 -21.00000 0.03613 0.03837 = 0.03856 -0.00337 -0.00093 -0.00210 SAME 0.01 0.04 N4 > C19 N4A 5 0.400869 0.719146 0.302790 -21.00000 0.02749 0.03754 = 0.04338 -0.00152 0.01001 -0.00006 C13A 1 0.345238 0.721297 0.488362 -21.00000 0.03996 0.03941 = 0.03458 0.00190 0.00351 -0.00187 AFIX 23 H13C 2 0.450244 0.720414 0.526578 -21.00000 -1.20000 H13D 2 0.297667 0.738314 0.538112 -21.00000 -1.20000 AFIX 0 C14A 1 0.316203 0.743960 0.367811 -21.00000 0.02833 0.02774 = 0.02462 -0.00024 0.01184 0.00031 AFIX 23 H14C 2 0.212058 0.742747 0.326714 -21.00000 -1.20000 H14D 2 0.346706 0.775568 0.376503 -21.00000 -1.20000 AFIX 0 C15A 1 0.355837 0.728562 0.177586 -21.00000 0.03499 0.04149 = 0.03782 -0.00569 0.02576 0.00048 AFIX 23 H15C 2 0.251185 0.722430 0.147909 -21.00000 -1.20000 H15D 2 0.406918 0.707710 0.138642 -21.00000 -1.20000 AFIX 0 C16A 1 0.384253 0.775989 0.144326 -21.00000 0.06549 0.04744 = 0.04163 -0.00400 0.03641 0.00224 AFIX 23 H16C 2 0.323836 0.795931 0.177212 -21.00000 -1.20000 H16D 2 0.346892 0.778125 0.059250 -21.00000 -1.20000 AFIX 0 C17A 1 0.537213 0.795732 0.177148 -21.00000 0.09084 0.05467 = 0.07553 -0.00028 0.06274 -0.02486 AFIX 23 H17C 2 0.576609 0.798763 0.109728 -21.00000 -1.20000 H17D 2 0.542470 0.824702 0.217440 -21.00000 -1.20000 AFIX 0 C18A 1 0.602351 0.761964 0.250130 -21.00000 0.05160 0.05089 = 0.07685 -0.01900 0.04930 -0.00756 AFIX 23 H18C 2 0.695014 0.775425 0.294006 -21.00000 -1.20000 H18D 2 0.628399 0.740234 0.197307 -21.00000 -1.20000 AFIX 0 C19A 1 0.557495 0.728677 0.350535 -21.00000 0.02804 0.03917 = 0.05525 -0.00390 0.01475 -0.00349 AFIX 23 H19C 2 0.614211 0.700720 0.361657 -21.00000 -1.20000 H19D 2 0.576004 0.744241 0.425703 -21.00000 -1.20000 AFIX 0 SAME 0.01 0.04 O1 > C34 O1A 7 0.488997 0.620255 0.271236 -21.00000 0.03211 0.04528 = 0.04843 -0.00401 0.00460 0.00462 O2A 7 0.549640 0.645313 0.491362 -21.00000 0.02815 0.04450 = 0.04823 -0.00019 -0.00160 0.00297 O3A 7 0.845838 0.571494 0.394651 -21.00000 0.03082 0.04033 = 0.05464 -0.00037 0.01034 0.00460 C20A 1 0.612021 0.608328 0.343623 -21.00000 0.02548 0.03649 = 0.04374 -0.00087 0.00756 0.00329 C21A 1 0.640616 0.620649 0.464070 -21.00000 0.02662 0.03872 = 0.04848 -0.00084 0.00464 -0.00051 C22A 1 0.765797 0.603955 0.549672 -21.00000 0.03201 0.03905 = 0.05368 -0.00033 0.00433 0.00096 C23A 1 0.791645 0.609544 0.667672 -21.00000 0.03669 0.04194 = 0.05424 -0.00329 0.00054 0.00806 AFIX 43 H23A 2 0.723215 0.625341 0.696278 -21.00000 -1.20000 AFIX 0 C24A 1 0.914658 0.592742 0.745480 -21.00000 0.03865 0.04595 = 0.05644 -0.00264 -0.00619 0.00591 AFIX 43 H24A 2 0.927210 0.597046 0.825824 -21.00000 -1.20000 AFIX 0 C25A 1 1.020184 0.569794 0.709543 -21.00000 0.03817 0.04209 = 0.06179 -0.00343 -0.00346 0.00325 AFIX 43 H25A 2 1.104278 0.557534 0.761280 -21.00000 -1.20000 AFIX 0 C26A 1 0.989773 0.566682 0.590234 -21.00000 0.02809 0.03809 = 0.06205 0.00312 0.00419 0.00023 AFIX 43 H26A 2 1.063063 0.554086 0.560932 -21.00000 -1.20000 AFIX 0 C27A 1 0.864514 0.579884 0.509028 -21.00000 0.02881 0.03609 = 0.05445 0.00223 0.00747 -0.00003 C28A 1 0.716924 0.583134 0.314816 -21.00000 0.03583 0.03977 = 0.05052 -0.00049 0.01200 0.00498 C29A 1 0.717324 0.568628 0.200740 -21.00000 0.04988 0.04553 = 0.05052 0.00001 0.01728 0.01132 C30A 1 0.850758 0.547636 0.191442 -21.00000 0.05921 0.05386 = 0.05470 -0.00185 0.02003 0.01665 AFIX 43 H30A 2 0.931408 0.541762 0.255657 -21.00000 -1.20000 AFIX 0 C31A 1 0.846163 0.537517 0.080637 -21.00000 0.06469 0.06434 = 0.06152 -0.00305 0.01717 0.02464 AFIX 43 H31A 2 0.930392 0.524482 0.067979 -21.00000 -1.20000 AFIX 0 C32A 1 0.730147 0.544363 -0.016284 -21.00000 0.07423 0.07259 = 0.06640 -0.00099 0.01867 0.02465 AFIX 43 H32A 2 0.735495 0.535652 -0.090868 -21.00000 -1.20000 AFIX 0 C33A 1 0.606867 0.564160 -0.001352 -21.00000 0.06808 0.06632 = 0.06146 -0.00105 0.01382 0.02584 AFIX 43 H33A 2 0.525807 0.569380 -0.065720 -21.00000 -1.20000 AFIX 0 C34A 1 0.603461 0.576084 0.107302 -21.00000 0.05567 0.05229 = 0.05577 -0.00233 0.01523 0.01700 AFIX 43 H34A 2 0.519281 0.589946 0.117754 -21.00000 -1.20000 AFIX 0 PART 0 CL1 4 0.000112 0.815954 0.366390 11.00000 0.02618 0.04949 = 0.03734 -0.00128 -0.00271 -0.00095 O4 7 0.030705 0.798033 0.480889 11.00000 0.05264 0.08884 = 0.04749 0.02088 0.00037 -0.00086 O5 7 -0.116248 0.847440 0.349477 11.00000 0.03695 0.06729 = 0.04312 -0.00768 0.00268 0.01323 O6 7 0.126032 0.837982 0.352080 11.00000 0.03655 0.05859 = 0.06323 -0.00521 0.01363 -0.00878 O7 7 -0.039439 0.780540 0.282907 11.00000 0.04018 0.05243 = 0.06447 -0.01702 -0.00819 0.00145 HKLF 4 REM kskr30a_a.res in P2(1)/n REM wR2 = 0.1592, GooF = S = 1.054, Restrained GooF = 1.004 for all data REM R1 = 0.0653 for 6605 Fo > 4sig(Fo) and 0.0665 for all 6828 data REM 824 parameters refined using 2434 restraints END WGHT 0.0613 11.2312 REM Highest difference peak 1.273, deepest hole -1.168, 1-sigma level 0.085 Q1 1 0.5756 0.7789 0.2149 11.00000 0.05 1.27 Q2 1 0.1321 0.6198 0.0395 11.00000 0.05 1.12 Q3 1 0.1966 0.5406 0.2448 11.00000 0.05 1.07 Q4 1 0.4398 0.7847 0.1441 11.00000 0.05 1.07 Q5 1 0.6032 0.7798 0.3450 11.00000 0.05 0.99 Q6 1 0.2440 0.6184 0.0582 11.00000 0.05 0.72 Q7 1 0.1158 0.6643 -0.0087 11.00000 0.05 0.50 Q8 1 0.6554 0.7645 0.1932 11.00000 0.05 0.39 Q9 1 0.6482 0.5344 -0.0550 11.00000 0.05 0.34 Q10 1 0.6533 0.5259 -0.0383 11.00000 0.05 0.32 ; _shelx_res_checksum 5935 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder' _olex2_submission_original_sample_id KSB_240906_SDc_KSKR30a _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 1.348 _oxdiff_exptl_absorpt_empirical_full_min 0.769 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 0.35812(6) 0.64944(2) 0.33762(6) 0.03920(19) Uani 1 1 d D U . . . Br1 Br 0.27968(18) 0.52929(5) 0.27152(17) 0.0655(4) Uani 0.610(3) 1 d D U P A 1 Br2 Br 0.2034(3) 0.62701(7) 0.03950(15) 0.0964(6) Uani 0.610(3) 1 d D U P A 1 N1 N 0.3132(11) 0.5902(2) 0.4465(7) 0.0402(18) Uani 0.610(3) 1 d D U P A 1 N2 N 0.2739(11) 0.6761(3) 0.4641(6) 0.0394(15) Uani 0.610(3) 1 d D U P A 1 N3 N 0.1363(6) 0.6508(4) 0.2415(6) 0.0330(19) Uani 0.610(3) 1 d D U P A 1 C1 C 0.3168(9) 0.5469(2) 0.4278(8) 0.0441(16) Uani 0.610(3) 1 d D U P A 1 C2 C 0.3427(9) 0.5143(3) 0.5123(9) 0.0458(18) Uani 0.610(3) 1 d D U P A 1 H2 H 0.340364 0.483513 0.493598 0.055 Uiso 0.610(3) 1 calc R U P A 1 C3 C 0.3721(9) 0.5289(3) 0.6253(9) 0.0486(17) Uani 0.610(3) 1 d D U P A 1 H3 H 0.394435 0.507953 0.686782 0.058 Uiso 0.610(3) 1 calc R U P A 1 C4 C 0.3691(10) 0.5739(3) 0.6490(8) 0.0487(18) Uani 0.610(3) 1 d D U P A 1 H4 H 0.388219 0.584189 0.726306 0.058 Uiso 0.610(3) 1 calc R U P A 1 C5 C 0.3375(12) 0.6037(3) 0.5568(7) 0.0436(18) Uani 0.610(3) 1 d D U P A 1 C6 C 0.3291(10) 0.6529(3) 0.5770(7) 0.0455(19) Uani 0.610(3) 1 d D U P A 1 H6A H 0.263669 0.658568 0.626143 0.055 Uiso 0.610(3) 1 calc R U P A 1 H6B H 0.425960 0.664421 0.617626 0.055 Uiso 0.610(3) 1 calc R U P A 1 C7 C 0.1141(11) 0.6731(4) 0.4294(8) 0.0375(19) Uani 0.610(3) 1 d D U P A 1 H7A H 0.074514 0.700545 0.454412 0.045 Uiso 0.610(3) 1 calc R U P A 1 H7B H 0.085048 0.647681 0.470533 0.045 Uiso 0.610(3) 1 calc R U P A 1 C8 C 0.0482(11) 0.6671(10) 0.3019(8) 0.0338(15) Uani 0.610(3) 1 d D U P A 1 C9 C -0.0964(10) 0.6750(5) 0.2488(8) 0.0404(19) Uani 0.610(3) 1 d D U P A 1 H9 H -0.156978 0.685412 0.293628 0.048 Uiso 0.610(3) 1 calc R U P A 1 C10 C -0.1535(10) 0.6681(4) 0.1329(8) 0.048(2) Uani 0.610(3) 1 d D U P A 1 H10 H -0.252873 0.673647 0.097245 0.057 Uiso 0.610(3) 1 calc R U P A 1 C11 C -0.0658(10) 0.6533(4) 0.0698(8) 0.049(2) Uani 0.610(3) 1 d D U P A 1 H11 H -0.101634 0.648613 -0.011094 0.058 Uiso 0.610(3) 1 calc R U P A 1 C12 C 0.0796(9) 0.6452(4) 0.1277(6) 0.045(2) Uani 0.610(3) 1 d D U P A 1 N4 N 0.4073(7) 0.7159(3) 0.3064(5) 0.0349(14) Uani 0.610(3) 1 d D U P A 1 C13 C 0.3057(9) 0.7244(4) 0.4745(7) 0.0381(18) Uani 0.610(3) 1 d D U P A 1 H13A H 0.329677 0.733550 0.556637 0.046 Uiso 0.610(3) 1 calc R U P A 1 H13B H 0.220429 0.741593 0.430996 0.046 Uiso 0.610(3) 1 calc R U P A 1 C14 C 0.4359(8) 0.7336(3) 0.4248(6) 0.0502(15) Uani 0.610(3) 1 d D U P A 1 H14A H 0.453280 0.766087 0.424208 0.060 Uiso 0.610(3) 1 calc R U P A 1 H14B H 0.523667 0.719382 0.474846 0.060 Uiso 0.610(3) 1 calc R U P A 1 C15 C 0.2941(8) 0.7401(2) 0.2197(7) 0.0493(15) Uani 0.610(3) 1 d D U P A 1 H15A H 0.205792 0.741628 0.246398 0.059 Uiso 0.610(3) 1 calc R U P A 1 H15B H 0.270354 0.723302 0.146065 0.059 Uiso 0.610(3) 1 calc R U P A 1 C16 C 0.3401(9) 0.7874(3) 0.1981(8) 0.0610(17) Uani 0.610(3) 1 d D U P A 1 H16A H 0.334074 0.807074 0.262610 0.073 Uiso 0.610(3) 1 calc R U P A 1 H16B H 0.274594 0.799267 0.125909 0.073 Uiso 0.610(3) 1 calc R U P A 1 C17 C 0.5015(10) 0.7866(3) 0.1879(8) 0.0658(15) Uani 0.610(3) 1 d D U P A 1 H17A H 0.512193 0.764239 0.130366 0.079 Uiso 0.610(3) 1 calc R U P A 1 H17B H 0.529422 0.816214 0.164734 0.079 Uiso 0.610(3) 1 calc R U P A 1 C18 C 0.5915(9) 0.7745(3) 0.3055(9) 0.0633(17) Uani 0.610(3) 1 d D U P A 1 H18A H 0.555339 0.786820 0.368568 0.076 Uiso 0.610(3) 1 calc R U P A 1 H18B H 0.695511 0.781046 0.318553 0.076 Uiso 0.610(3) 1 calc R U P A 1 C19 C 0.5469(8) 0.7184(2) 0.2748(9) 0.0570(15) Uani 0.610(3) 1 d D U P A 1 H19A H 0.533856 0.711426 0.192153 0.068 Uiso 0.610(3) 1 calc R U P A 1 H19B H 0.620519 0.698174 0.322980 0.068 Uiso 0.610(3) 1 calc R U P A 1 O1 O 0.5637(4) 0.63629(14) 0.4273(4) 0.0289(8) Uani 0.610(3) 1 d D U P A 1 O2 O 0.4409(4) 0.62238(15) 0.2049(4) 0.0356(10) Uani 0.610(3) 1 d D U P A 1 O3 O 0.8376(6) 0.5703(2) 0.3471(4) 0.0368(11) Uani 0.610(3) 1 d D U P A 1 C20 C 0.6363(7) 0.6129(3) 0.3716(7) 0.0310(14) Uani 0.610(3) 1 d D U P A 1 C21 C 0.5677(6) 0.60725(19) 0.2482(5) 0.0315(11) Uani 0.610(3) 1 d D U P A 1 C22 C 0.6448(7) 0.5843(2) 0.1787(5) 0.0370(12) Uani 0.610(3) 1 d D U P A 1 C23 C 0.5909(9) 0.5800(3) 0.0587(6) 0.0480(17) Uani 0.610(3) 1 d D U P A 1 H23 H 0.498652 0.591925 0.020686 0.058 Uiso 0.610(3) 1 calc R U P A 1 C24 C 0.6710(9) 0.5587(3) -0.0048(7) 0.0548(17) Uani 0.610(3) 1 d D U P A 1 H24 H 0.632474 0.556036 -0.086095 0.066 Uiso 0.610(3) 1 calc R U P A 1 C25 C 0.8054(10) 0.5412(4) 0.0473(8) 0.0580(19) Uani 0.610(3) 1 d D U P A 1 H25 H 0.858980 0.526113 0.003258 0.070 Uiso 0.610(3) 1 calc R U P A 1 C26 C 0.8603(14) 0.5462(5) 0.1658(8) 0.0518(19) Uani 0.610(3) 1 d D U P A 1 H26 H 0.953904 0.534972 0.202652 0.062 Uiso 0.610(3) 1 calc R U P A 1 C27 C 0.7814(7) 0.5672(2) 0.2321(6) 0.0385(13) Uani 0.610(3) 1 d D U P A 1 C28 C 0.7672(6) 0.59215(19) 0.4189(5) 0.0335(11) Uani 0.610(3) 1 d D U P A 1 C29 C 0.8420(8) 0.5879(3) 0.5412(6) 0.0363(14) Uani 0.610(3) 1 d D U P A 1 C30 C 0.9742(12) 0.5615(5) 0.5707(9) 0.0440(19) Uani 0.610(3) 1 d D U P A 1 H30 H 1.013942 0.549128 0.513543 0.053 Uiso 0.610(3) 1 calc R U P A 1 C31 C 1.0372(9) 0.5556(3) 0.6866(8) 0.0462(17) Uani 0.610(3) 1 d D U P A 1 H31 H 1.126185 0.539925 0.709266 0.055 Uiso 0.610(3) 1 calc R U P A 1 C32 C 0.9786(8) 0.5713(2) 0.7740(7) 0.0472(15) Uani 0.610(3) 1 d D U P A 1 H32 H 1.026163 0.565945 0.853055 0.057 Uiso 0.610(3) 1 calc R U P A 1 C33 C 0.8488(9) 0.5950(3) 0.7418(7) 0.0476(16) Uani 0.610(3) 1 d D U P A 1 H33 H 0.805298 0.605507 0.798655 0.057 Uiso 0.610(3) 1 calc R U P A 1 C34 C 0.7849(9) 0.6027(3) 0.6262(8) 0.0432(16) Uani 0.610(3) 1 d D U P A 1 H34 H 0.697339 0.619155 0.604912 0.052 Uiso 0.610(3) 1 calc R U P A 1 Br1A Br 0.2654(3) 0.53401(9) 0.2168(3) 0.0672(6) Uani 0.390(3) 1 d D U P A 2 Br2A Br 0.16419(16) 0.64298(8) 0.01373(16) 0.0508(5) Uani 0.390(3) 1 d D U P A 2 N1A N 0.3191(18) 0.5885(4) 0.4100(10) 0.037(2) Uani 0.390(3) 1 d D U P A 2 N2A N 0.2854(17) 0.6747(5) 0.4703(9) 0.039(2) Uani 0.390(3) 1 d D U P A 2 N3A N 0.1379(9) 0.6578(8) 0.2366(10) 0.034(2) Uani 0.390(3) 1 d D U P A 2 C1A C 0.3032(15) 0.5463(3) 0.3773(10) 0.040(2) Uani 0.390(3) 1 d D U P A 2 C2A C 0.3175(14) 0.5104(4) 0.4518(13) 0.045(2) Uani 0.390(3) 1 d D U P A 2 H2A H 0.305388 0.480666 0.423567 0.054 Uiso 0.390(3) 1 calc R U P A 2 C3A C 0.3499(15) 0.5193(4) 0.5685(13) 0.043(2) Uani 0.390(3) 1 d D U P A 2 H3A H 0.364873 0.495655 0.622902 0.051 Uiso 0.390(3) 1 calc R U P A 2 C4A C 0.3605(16) 0.5630(4) 0.6054(11) 0.043(2) Uani 0.390(3) 1 d D U P A 2 H4A H 0.377109 0.569836 0.684980 0.052 Uiso 0.390(3) 1 calc R U P A 2 C5A C 0.3464(18) 0.5969(4) 0.5238(11) 0.038(2) Uani 0.390(3) 1 d D U P A 2 C6A C 0.3667(12) 0.6446(4) 0.5633(11) 0.033(2) Uani 0.390(3) 1 d D U P A 2 H6AA H 0.332100 0.648576 0.632879 0.039 Uiso 0.390(3) 1 calc R U P A 2 H6AB H 0.470564 0.652319 0.583934 0.039 Uiso 0.390(3) 1 calc R U P A 2 C7A C 0.1291(18) 0.6653(7) 0.4411(12) 0.037(2) Uani 0.390(3) 1 d D U P A 2 H7AA H 0.081772 0.687735 0.478742 0.044 Uiso 0.390(3) 1 calc R U P A 2 H7AB H 0.113892 0.635625 0.471708 0.044 Uiso 0.390(3) 1 calc R U P A 2 C8A C 0.0601(17) 0.6662(16) 0.3128(13) 0.034(2) Uani 0.390(3) 1 d D U P A 2 C9A C -0.0858(15) 0.6768(7) 0.2834(12) 0.036(2) Uani 0.390(3) 1 d D U P A 2 H9A H -0.131524 0.686253 0.339914 0.043 Uiso 0.390(3) 1 calc R U P A 2 C10A C -0.1606(15) 0.6730(6) 0.1701(12) 0.041(2) Uani 0.390(3) 1 d D U P A 2 H10A H -0.261094 0.679259 0.146472 0.049 Uiso 0.390(3) 1 calc R U P A 2 C11A C -0.0915(13) 0.6604(6) 0.0909(12) 0.040(2) Uani 0.390(3) 1 d D U P A 2 H11A H -0.145030 0.655583 0.012886 0.048 Uiso 0.390(3) 1 calc R U P A 2 C12A C 0.0601(12) 0.6544(7) 0.1241(9) 0.040(2) Uani 0.390(3) 1 d D U P A 2 N4A N 0.4009(11) 0.7191(5) 0.3028(8) 0.036(2) Uani 0.390(3) 1 d D U P A 2 C13A C 0.3452(17) 0.7213(6) 0.4884(11) 0.039(2) Uani 0.390(3) 1 d D U P A 2 H13C H 0.450244 0.720414 0.526578 0.047 Uiso 0.390(3) 1 calc R U P A 2 H13D H 0.297667 0.738314 0.538112 0.047 Uiso 0.390(3) 1 calc R U P A 2 C14A C 0.3162(9) 0.7440(3) 0.3678(7) 0.0260(14) Uani 0.390(3) 1 d D U P A 2 H14C H 0.212058 0.742747 0.326714 0.031 Uiso 0.390(3) 1 calc R U P A 2 H14D H 0.346706 0.775568 0.376503 0.031 Uiso 0.390(3) 1 calc R U P A 2 C15A C 0.3558(10) 0.7286(3) 0.1776(8) 0.0350(15) Uani 0.390(3) 1 d D U P A 2 H15C H 0.251185 0.722430 0.147909 0.042 Uiso 0.390(3) 1 calc R U P A 2 H15D H 0.406918 0.707710 0.138642 0.042 Uiso 0.390(3) 1 calc R U P A 2 C16A C 0.3843(12) 0.7760(3) 0.1443(10) 0.0472(18) Uani 0.390(3) 1 d D U P A 2 H16C H 0.323836 0.795931 0.177212 0.057 Uiso 0.390(3) 1 calc R U P A 2 H16D H 0.346892 0.778125 0.059250 0.057 Uiso 0.390(3) 1 calc R U P A 2 C17A C 0.5372(14) 0.7957(5) 0.1771(14) 0.0658(15) Uani 0.390(3) 1 d D U P A 2 H17C H 0.576609 0.798763 0.109728 0.079 Uiso 0.390(3) 1 calc R U P A 2 H17D H 0.542470 0.824702 0.217440 0.079 Uiso 0.390(3) 1 calc R U P A 2 C18A C 0.6024(13) 0.7620(4) 0.2501(11) 0.0535(19) Uani 0.390(3) 1 d D U P A 2 H18C H 0.695014 0.775425 0.294006 0.064 Uiso 0.390(3) 1 calc R U P A 2 H18D H 0.628399 0.740234 0.197307 0.064 Uiso 0.390(3) 1 calc R U P A 2 C19A C 0.5575(10) 0.7287(3) 0.3505(9) 0.0402(17) Uani 0.390(3) 1 d D U P A 2 H19C H 0.614211 0.700720 0.361657 0.048 Uiso 0.390(3) 1 calc R U P A 2 H19D H 0.576004 0.744241 0.425703 0.048 Uiso 0.390(3) 1 calc R U P A 2 O1A O 0.4890(8) 0.6203(3) 0.2712(7) 0.0432(15) Uani 0.390(3) 1 d D U P A 2 O2A O 0.5496(7) 0.6453(3) 0.4914(7) 0.0427(16) Uani 0.390(3) 1 d D U P A 2 O3A O 0.8458(10) 0.5715(4) 0.3947(7) 0.0422(18) Uani 0.390(3) 1 d D U P A 2 C20A C 0.6120(11) 0.6083(5) 0.3436(11) 0.036(2) Uani 0.390(3) 1 d D U P A 2 C21A C 0.6406(10) 0.6206(3) 0.4641(8) 0.0391(17) Uani 0.390(3) 1 d D U P A 2 C22A C 0.7658(10) 0.6040(4) 0.5497(8) 0.0431(18) Uani 0.390(3) 1 d D U P A 2 C23A C 0.7916(15) 0.6095(5) 0.6677(9) 0.047(2) Uani 0.390(3) 1 d D U P A 2 H23A H 0.723215 0.625341 0.696278 0.056 Uiso 0.390(3) 1 calc R U P A 2 C24A C 0.9147(12) 0.5927(5) 0.7455(11) 0.051(2) Uani 0.390(3) 1 d D U P A 2 H24A H 0.927210 0.597046 0.825824 0.061 Uiso 0.390(3) 1 calc R U P A 2 C25A C 1.0202(14) 0.5698(5) 0.7095(12) 0.051(2) Uani 0.390(3) 1 d D U P A 2 H25A H 1.104278 0.557534 0.761280 0.061 Uiso 0.390(3) 1 calc R U P A 2 C26A C 0.9898(19) 0.5667(8) 0.5902(12) 0.044(3) Uani 0.390(3) 1 d D U P A 2 H26A H 1.063063 0.554086 0.560932 0.053 Uiso 0.390(3) 1 calc R U P A 2 C27A C 0.8645(12) 0.5799(4) 0.5090(9) 0.0406(19) Uani 0.390(3) 1 d D U P A 2 C28A C 0.7169(10) 0.5831(3) 0.3148(8) 0.0420(16) Uani 0.390(3) 1 d D U P A 2 C29A C 0.7173(15) 0.5686(5) 0.2007(9) 0.0479(19) Uani 0.390(3) 1 d D U P A 2 C30A C 0.851(2) 0.5476(9) 0.1914(15) 0.055(2) Uani 0.390(3) 1 d D U P A 2 H30A H 0.931408 0.541762 0.255657 0.066 Uiso 0.390(3) 1 calc R U P A 2 C31A C 0.8462(18) 0.5375(7) 0.0806(13) 0.064(3) Uani 0.390(3) 1 d D U P A 2 H31A H 0.930392 0.524482 0.067979 0.076 Uiso 0.390(3) 1 calc R U P A 2 C32A C 0.7301(17) 0.5444(6) -0.0163(13) 0.071(3) Uani 0.390(3) 1 d D U P A 2 H32A H 0.735495 0.535652 -0.090868 0.085 Uiso 0.390(3) 1 calc R U P A 2 C33A C 0.6069(16) 0.5642(6) -0.0014(13) 0.066(3) Uani 0.390(3) 1 d D U P A 2 H33A H 0.525807 0.569380 -0.065720 0.079 Uiso 0.390(3) 1 calc R U P A 2 C34A C 0.6035(16) 0.5761(6) 0.1073(12) 0.055(2) Uani 0.390(3) 1 d D U P A 2 H34A H 0.519281 0.589946 0.117754 0.066 Uiso 0.390(3) 1 calc R U P A 2 Cl1 Cl 0.00011(9) 0.81595(3) 0.36639(8) 0.0399(2) Uani 1 1 d . . . . . O4 O 0.0307(4) 0.79803(14) 0.4809(3) 0.0656(10) Uani 1 1 d . . . . . O5 O -0.1162(3) 0.84744(11) 0.3495(3) 0.0508(8) Uani 1 1 d . . . . . O6 O 0.1260(3) 0.83798(11) 0.3521(3) 0.0528(8) Uani 1 1 d . . . . . O7 O -0.0394(3) 0.78054(11) 0.2829(3) 0.0568(9) Uani 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 0.0191(3) 0.0365(4) 0.0579(4) -0.0020(3) 0.0036(3) 0.0029(2) Br1 0.0581(6) 0.0471(6) 0.0798(10) -0.0202(7) -0.0006(8) 0.0000(4) Br2 0.1440(18) 0.1062(14) 0.0443(8) -0.0251(8) 0.0347(10) -0.0159(11) N1 0.026(3) 0.037(3) 0.053(4) 0.006(3) 0.003(4) -0.003(2) N2 0.041(3) 0.039(3) 0.031(3) 0.007(2) -0.001(2) -0.002(2) N3 0.026(3) 0.035(4) 0.033(3) -0.001(2) 0.000(2) -0.002(2) C1 0.031(3) 0.041(3) 0.058(4) 0.001(3) 0.008(3) -0.002(2) C2 0.034(3) 0.040(3) 0.060(4) 0.007(4) 0.006(4) -0.002(2) C3 0.036(3) 0.046(4) 0.062(4) 0.014(3) 0.010(3) -0.001(3) C4 0.040(3) 0.045(3) 0.053(4) 0.013(3) -0.001(3) -0.003(3) C5 0.035(3) 0.044(3) 0.046(4) 0.010(3) 0.000(3) -0.002(3) C6 0.047(4) 0.043(3) 0.037(3) 0.010(3) -0.005(3) 0.001(3) C7 0.034(3) 0.040(4) 0.040(3) 0.011(3) 0.012(3) 0.008(3) C8 0.023(3) 0.035(3) 0.041(3) 0.006(3) 0.004(2) 0.003(3) C9 0.024(3) 0.042(3) 0.048(4) 0.005(4) -0.004(3) 0.004(2) C10 0.034(3) 0.047(4) 0.046(5) 0.007(4) -0.016(3) -0.002(3) C11 0.048(4) 0.046(4) 0.039(4) 0.002(3) -0.012(3) -0.015(3) C12 0.047(3) 0.043(5) 0.036(3) -0.002(3) -0.003(3) -0.011(3) N4 0.024(2) 0.037(3) 0.041(3) -0.002(2) 0.005(2) 0.002(2) C13 0.042(4) 0.038(3) 0.029(3) 0.003(2) 0.001(3) 0.000(3) C14 0.048(3) 0.047(3) 0.049(3) 0.000(3) 0.001(3) -0.001(3) C15 0.045(3) 0.048(3) 0.050(3) 0.005(3) 0.005(3) -0.001(3) C16 0.068(4) 0.050(3) 0.064(4) 0.009(3) 0.016(3) -0.006(3) C17 0.091(3) 0.055(3) 0.076(3) 0.000(3) 0.063(3) -0.025(3) C18 0.049(3) 0.052(4) 0.099(4) 0.006(3) 0.037(3) -0.006(3) C19 0.040(3) 0.050(3) 0.084(4) 0.002(3) 0.024(3) -0.001(3) O1 0.0211(18) 0.033(2) 0.031(2) -0.0038(17) 0.0041(16) 0.0052(15) O2 0.022(2) 0.045(2) 0.035(2) -0.0099(19) -0.0010(17) 0.0095(17) O3 0.028(2) 0.036(2) 0.046(3) -0.001(2) 0.008(2) 0.0107(17) C20 0.021(2) 0.032(3) 0.038(3) -0.001(2) 0.003(2) 0.001(2) C21 0.022(2) 0.032(2) 0.039(3) -0.007(2) 0.006(2) 0.006(2) C22 0.032(3) 0.035(3) 0.044(3) -0.005(2) 0.009(2) 0.007(2) C23 0.053(3) 0.045(3) 0.047(4) -0.012(3) 0.016(3) 0.017(3) C24 0.052(4) 0.059(3) 0.057(3) -0.009(3) 0.020(3) 0.029(3) C25 0.056(4) 0.062(3) 0.058(4) -0.003(4) 0.019(3) 0.029(3) C26 0.058(3) 0.049(3) 0.054(4) -0.004(4) 0.024(3) 0.020(3) C27 0.032(3) 0.035(2) 0.051(3) -0.001(2) 0.015(2) 0.010(2) C28 0.023(2) 0.029(2) 0.046(2) -0.001(2) 0.0059(19) 0.0034(19) C29 0.025(3) 0.030(3) 0.050(3) 0.000(2) 0.004(2) 0.003(2) C30 0.028(3) 0.038(4) 0.061(4) 0.006(3) 0.005(3) -0.001(3) C31 0.030(3) 0.043(4) 0.061(4) 0.007(3) 0.005(3) 0.006(3) C32 0.034(3) 0.038(3) 0.058(4) 0.008(3) -0.007(3) 0.002(3) C33 0.037(3) 0.040(3) 0.053(3) -0.006(3) -0.009(3) 0.011(3) C34 0.035(3) 0.037(3) 0.047(4) -0.005(3) -0.005(3) 0.008(2) Br1A 0.0667(12) 0.0581(11) 0.0742(14) -0.0287(12) 0.0151(13) -0.0209(9) Br2A 0.0276(6) 0.0828(13) 0.0306(7) -0.0083(7) -0.0112(5) 0.0178(6) N1A 0.025(3) 0.040(3) 0.047(5) 0.005(3) 0.011(4) 0.000(3) N2A 0.038(3) 0.040(3) 0.033(3) 0.006(3) 0.002(3) -0.001(3) N3A 0.027(4) 0.034(5) 0.036(4) 0.000(3) 0.003(3) -0.004(3) C1A 0.032(4) 0.039(3) 0.051(5) -0.002(4) 0.014(4) -0.002(3) C2A 0.037(4) 0.040(4) 0.059(5) 0.003(4) 0.017(4) -0.003(3) C3A 0.035(4) 0.041(4) 0.053(5) 0.009(4) 0.012(4) -0.002(3) C4A 0.036(3) 0.044(4) 0.050(5) 0.009(4) 0.012(4) 0.003(3) C5A 0.029(3) 0.040(3) 0.045(4) 0.007(3) 0.011(3) 0.004(3) C6A 0.025(4) 0.041(4) 0.033(4) 0.005(3) 0.010(3) 0.012(3) C7A 0.033(4) 0.039(5) 0.037(4) 0.009(4) 0.009(3) 0.011(4) C8A 0.022(3) 0.035(4) 0.043(4) 0.006(4) 0.005(3) 0.004(3) C9A 0.022(3) 0.040(4) 0.038(5) 0.002(5) -0.005(4) 0.001(3) C10A 0.031(4) 0.043(4) 0.041(5) -0.003(4) -0.003(4) 0.003(3) C11A 0.035(4) 0.038(4) 0.037(4) -0.007(4) -0.005(3) 0.004(3) C12A 0.036(4) 0.038(5) 0.039(4) -0.003(3) -0.001(3) -0.002(3) N4A 0.027(3) 0.038(3) 0.043(3) -0.002(3) 0.010(3) 0.000(3) C13A 0.040(4) 0.039(4) 0.035(4) 0.002(3) 0.004(4) -0.002(4) C14A 0.028(3) 0.028(3) 0.025(3) 0.000(3) 0.012(2) 0.000(3) C15A 0.035(3) 0.041(3) 0.038(3) -0.006(3) 0.026(3) 0.000(3) C16A 0.065(4) 0.047(4) 0.042(4) -0.004(3) 0.036(3) 0.002(4) C17A 0.091(3) 0.055(3) 0.076(3) 0.000(3) 0.063(3) -0.025(3) C18A 0.052(4) 0.051(4) 0.077(4) -0.019(4) 0.049(3) -0.008(3) C19A 0.028(3) 0.039(3) 0.055(4) -0.004(3) 0.015(3) -0.003(3) O1A 0.032(3) 0.045(3) 0.048(3) -0.004(3) 0.005(3) 0.005(3) O2A 0.028(3) 0.044(4) 0.048(4) 0.000(3) -0.002(3) 0.003(3) O3A 0.031(3) 0.040(3) 0.055(4) 0.000(4) 0.010(3) 0.005(3) C20A 0.025(3) 0.036(3) 0.044(4) -0.001(3) 0.008(3) 0.003(3) C21A 0.027(3) 0.039(3) 0.048(4) -0.001(3) 0.005(3) -0.001(3) C22A 0.032(3) 0.039(3) 0.054(4) 0.000(3) 0.004(3) 0.001(3) C23A 0.037(4) 0.042(4) 0.054(5) -0.003(4) 0.001(4) 0.008(4) C24A 0.039(4) 0.046(4) 0.056(4) -0.003(3) -0.006(4) 0.006(4) C25A 0.038(4) 0.042(4) 0.062(4) -0.003(4) -0.003(4) 0.003(4) C26A 0.028(4) 0.038(5) 0.062(4) 0.003(4) 0.004(4) 0.000(4) C27A 0.029(3) 0.036(3) 0.054(4) 0.002(3) 0.007(3) 0.000(3) C28A 0.036(3) 0.040(3) 0.051(3) 0.000(3) 0.012(3) 0.005(3) C29A 0.050(4) 0.046(3) 0.051(4) 0.000(3) 0.017(3) 0.011(3) C30A 0.059(4) 0.054(4) 0.055(5) -0.002(4) 0.020(4) 0.017(4) C31A 0.065(5) 0.064(4) 0.062(5) -0.003(4) 0.017(4) 0.025(4) C32A 0.074(6) 0.073(5) 0.066(5) -0.001(5) 0.019(5) 0.025(5) C33A 0.068(5) 0.066(5) 0.061(4) -0.001(4) 0.014(5) 0.026(5) C34A 0.056(4) 0.052(4) 0.056(4) -0.002(4) 0.015(4) 0.017(3) Cl1 0.0262(4) 0.0495(5) 0.0373(5) -0.0013(4) -0.0027(3) -0.0010(4) O4 0.053(2) 0.089(3) 0.0475(19) 0.0209(18) 0.0004(15) -0.0009(18) O5 0.0369(15) 0.067(2) 0.0431(16) -0.0077(14) 0.0027(12) 0.0132(14) O6 0.0366(15) 0.0586(19) 0.063(2) -0.0052(16) 0.0136(14) -0.0088(14) O7 0.0402(16) 0.0524(18) 0.064(2) -0.0170(15) -0.0082(14) 0.0014(14) 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' Br Br -0.6763 1.2805 '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 -1 0.0092 0 1 1 0.0251 1 0 -1 0.0725 -2 1 2 0.0579 0 -1 0 0.0592 0 1 0 0.0622 -1 2 0 0.0911 1 -2 0 0.1044 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 73.1(3) . . ? N2 Ni1 N3 81.6(4) . . ? N2 Ni1 N4 85.3(4) . . ? N2 Ni1 O2 178.8(3) . . ? N3 Ni1 N1 90.4(4) . . ? N3 Ni1 O2 97.3(3) . . ? N4 Ni1 N1 155.8(3) . . ? N4 Ni1 N3 97.2(4) . . ? N4 Ni1 O2 94.5(2) . . ? O1 Ni1 N1 81.7(3) . . ? O1 Ni1 N2 102.0(3) . . ? O1 Ni1 N3 169.8(4) . . ? O1 Ni1 N4 92.6(2) . . ? O1 Ni1 O2 79.17(18) . . ? O2 Ni1 N1 107.3(2) . . ? N1A Ni1 N3A 94.3(7) . . ? N1A Ni1 N4A 166.4(4) . . ? N1A Ni1 O2A 79.0(5) . . ? N2A Ni1 N1A 82.0(5) . . ? N2A Ni1 N3A 84.4(5) . . ? N2A Ni1 N4A 85.3(5) . . ? N2A Ni1 O2A 75.9(5) . . ? N3A Ni1 N4A 89.4(7) . . ? N3A Ni1 O2A 159.9(4) . . ? N4A Ni1 O2A 93.2(3) . . ? O1A Ni1 N1A 89.3(5) . . ? O1A Ni1 N2A 155.6(5) . . ? O1A Ni1 N3A 119.1(4) . . ? O1A Ni1 N4A 100.3(4) . . ? O1A Ni1 O2A 80.1(3) . . ? C1 N1 Ni1 129.8(7) . . ? C1 N1 C5 117.2(7) . . ? C5 N1 Ni1 108.6(5) . . ? C6 N2 Ni1 112.1(6) . . ? C7 N2 Ni1 110.8(6) . . ? C7 N2 C6 108.1(7) . . ? C13 N2 Ni1 109.1(6) . . ? C13 N2 C6 111.5(7) . . ? C13 N2 C7 105.0(7) . . ? C8 N3 Ni1 113.5(6) . . ? C12 N3 Ni1 128.2(6) . . ? C12 N3 C8 117.2(6) . . ? N1 C1 Br1 115.9(6) . . ? N1 C1 C2 125.4(9) . . ? C2 C1 Br1 118.7(6) . . ? C1 C2 H2 121.8 . . ? C3 C2 C1 116.5(7) . . ? C3 C2 H2 121.8 . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.2(7) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 120.8 . . ? C3 C4 C5 118.4(9) . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 122.3(8) . . ? N1 C5 C6 116.9(6) . . ? C4 C5 C6 120.8(8) . . ? N2 C6 C5 109.5(7) . . ? N2 C6 H6A 109.8 . . ? N2 C6 H6B 109.8 . . ? C5 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N2 C7 H7A 108.7 . . ? N2 C7 H7B 108.7 . . ? N2 C7 C8 114.2(8) . . ? H7A C7 H7B 107.6 . . ? C8 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? N3 C8 C7 116.2(7) . . ? N3 C8 C9 121.0(8) . . ? C9 C8 C7 122.7(7) . . ? C8 C9 H9 119.4 . . ? C10 C9 C8 121.1(8) . . ? C10 C9 H9 119.4 . . ? C9 C10 H10 120.6 . . ? C11 C10 C9 118.9(7) . . ? C11 C10 H10 120.6 . . ? C10 C11 H11 121.0 . . ? C10 C11 C12 117.9(7) . . ? C12 C11 H11 121.0 . . ? N3 C12 Br2 118.1(6) . . ? N3 C12 C11 123.8(7) . . ? C11 C12 Br2 118.1(6) . . ? C14 N4 Ni1 99.2(5) . . ? C14 N4 C15 114.3(7) . . ? C14 N4 C19 106.6(7) . . ? C15 N4 Ni1 115.6(5) . . ? C15 N4 C19 109.7(7) . . ? C19 N4 Ni1 110.7(5) . . ? N2 C13 H13A 110.1 . . ? N2 C13 H13B 110.1 . . ? N2 C13 C14 108.1(8) . . ? H13A C13 H13B 108.4 . . ? C14 C13 H13A 110.1 . . ? C14 C13 H13B 110.1 . . ? N4 C14 C13 110.6(6) . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N4 C15 H15A 109.1 . . ? N4 C15 H15B 109.1 . . ? N4 C15 C16 112.6(7) . . ? H15A C15 H15B 107.8 . . ? C16 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C15 C16 H16A 109.8 . . ? C15 C16 H16B 109.8 . . ? C15 C16 C17 109.5(7) . . ? H16A C16 H16B 108.2 . . ? C17 C16 H16A 109.8 . . ? C17 C16 H16B 109.8 . . ? C16 C17 H17A 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? C18 C17 C16 104.8(7) . . ? C18 C17 H17A 110.8 . . ? C18 C17 H17B 110.8 . . ? C17 C18 H18A 113.7 . . ? C17 C18 H18B 113.7 . . ? C17 C18 C19 89.4(7) . . ? H18A C18 H18B 111.0 . . ? C19 C18 H18A 113.8 . . ? C19 C18 H18B 113.8 . . ? N4 C19 C18 100.3(6) . . ? N4 C19 H19A 111.7 . . ? N4 C19 H19B 111.7 . . ? C18 C19 H19A 111.7 . . ? C18 C19 H19B 111.7 . . ? H19A C19 H19B 109.5 . . ? C20 O1 Ni1 114.7(4) . . ? C21 O2 Ni1 110.0(4) . . ? C27 O3 C28 122.8(5) . . ? O1 C20 C21 115.5(5) . . ? O1 C20 C28 126.2(7) . . ? C28 C20 C21 118.2(6) . . ? O2 C21 C20 119.4(5) . . ? O2 C21 C22 121.5(5) . . ? C22 C21 C20 119.1(5) . . ? C23 C22 C21 122.6(6) . . ? C27 C22 C21 118.7(6) . . ? C27 C22 C23 118.6(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 C22 120.5(7) . . ? C24 C23 H23 119.8 . . ? C23 C24 H24 119.3 . . ? C25 C24 C23 121.4(8) . . ? C25 C24 H24 119.3 . . ? C24 C25 H25 120.9 . . ? C24 C25 C26 118.2(9) . . ? C26 C25 H25 120.9 . . ? C25 C26 H26 119.2 . . ? C25 C26 C27 121.6(10) . . ? C27 C26 H26 119.2 . . ? O3 C27 C22 120.8(6) . . ? O3 C27 C26 119.4(7) . . ? C22 C27 C26 119.7(8) . . ? O3 C28 C29 113.2(5) . . ? C20 C28 O3 120.0(6) . . ? C20 C28 C29 126.8(6) . . ? C28 C29 C30 116.8(7) . . ? C34 C29 C28 122.8(7) . . ? C34 C29 C30 120.0(8) . . ? C29 C30 H30 122.2 . . ? C31 C30 C29 115.5(11) . . ? C31 C30 H30 122.2 . . ? C30 C31 H31 117.9 . . ? C30 C31 C32 124.2(9) . . ? C32 C31 H31 117.9 . . ? C31 C32 H32 120.8 . . ? C33 C32 C31 118.4(7) . . ? C33 C32 H32 120.8 . . ? C32 C33 H33 120.5 . . ? C34 C33 C32 118.9(8) . . ? C34 C33 H33 120.5 . . ? C29 C34 C33 122.9(8) . . ? C29 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C1A N1A Ni1 136.8(9) . . ? C1A N1A C5A 117.1(10) . . ? C5A N1A Ni1 104.6(7) . . ? C6A N2A Ni1 98.1(7) . . ? C6A N2A C13A 110.8(11) . . ? C7A N2A Ni1 106.7(10) . . ? C7A N2A C6A 110.9(11) . . ? C7A N2A C13A 122.5(12) . . ? C13A N2A Ni1 104.8(9) . . ? C8A N3A Ni1 106.4(7) . . ? C8A N3A C12A 115.6(9) . . ? C12A N3A Ni1 137.9(9) . . ? N1A C1A Br1A 117.5(8) . . ? N1A C1A C2A 124.8(11) . . ? C2A C1A Br1A 117.7(8) . . ? C1A C2A H2A 121.2 . . ? C3A C2A C1A 117.5(11) . . ? C3A C2A H2A 121.2 . . ? C2A C3A H3A 120.4 . . ? C4A C3A C2A 119.3(11) . . ? C4A C3A H3A 120.4 . . ? C3A C4A H4A 120.6 . . ? C3A C4A C5A 118.9(12) . . ? C5A C4A H4A 120.6 . . ? N1A C5A C4A 122.3(10) . . ? N1A C5A C6A 118.1(9) . . ? C4A C5A C6A 119.6(11) . . ? N2A C6A C5A 110.2(10) . . ? N2A C6A H6AA 109.6 . . ? N2A C6A H6AB 109.6 . . ? C5A C6A H6AA 109.6 . . ? C5A C6A H6AB 109.6 . . ? H6AA C6A H6AB 108.1 . . ? N2A C7A H7AA 109.2 . . ? N2A C7A H7AB 109.2 . . ? N2A C7A C8A 112.1(13) . . ? H7AA C7A H7AB 107.9 . . ? C8A C7A H7AA 109.2 . . ? C8A C7A H7AB 109.2 . . ? N3A C8A C7A 121.3(11) . . ? N3A C8A C9A 125.3(12) . . ? C9A C8A C7A 113.4(10) . . ? C8A C9A H9A 121.4 . . ? C10A C9A C8A 117.2(12) . . ? C10A C9A H9A 121.4 . . ? C9A C10A H10A 120.0 . . ? C11A C10A C9A 120.0(11) . . ? C11A C10A H10A 120.0 . . ? C10A C11A H11A 119.9 . . ? C10A C11A C12A 120.2(11) . . ? C12A C11A H11A 119.9 . . ? N3A C12A Br2A 117.2(9) . . ? N3A C12A C11A 121.0(9) . . ? C11A C12A Br2A 121.7(8) . . ? C14A N4A Ni1 102.7(7) . . ? C14A N4A C19A 110.3(9) . . ? C15A N4A Ni1 111.1(8) . . ? C15A N4A C14A 113.2(9) . . ? C15A N4A C19A 109.9(9) . . ? C19A N4A Ni1 109.5(7) . . ? N2A C13A H13C 110.1 . . ? N2A C13A H13D 110.1 . . ? N2A C13A C14A 107.9(11) . . ? H13C C13A H13D 108.4 . . ? C14A C13A H13C 110.1 . . ? C14A C13A H13D 110.1 . . ? N4A C14A C13A 106.8(9) . . ? N4A C14A H14C 110.4 . . ? N4A C14A H14D 110.4 . . ? C13A C14A H14C 110.4 . . ? C13A C14A H14D 110.4 . . ? H14C C14A H14D 108.6 . . ? N4A C15A H15C 108.5 . . ? N4A C15A H15D 108.5 . . ? N4A C15A C16A 115.0(9) . . ? H15C C15A H15D 107.5 . . ? C16A C15A H15C 108.5 . . ? C16A C15A H15D 108.5 . . ? C15A C16A H16C 107.0 . . ? C15A C16A H16D 107.0 . . ? C15A C16A C17A 121.4(9) . . ? H16C C16A H16D 106.7 . . ? C17A C16A H16C 107.0 . . ? C17A C16A H16D 107.0 . . ? C16A C17A H17C 112.4 . . ? C16A C17A H17D 112.4 . . ? H17C C17A H17D 110.0 . . ? C18A C17A C16A 96.7(10) . . ? C18A C17A H17C 112.4 . . ? C18A C17A H17D 112.4 . . ? C17A C18A H18C 103.1 . . ? C17A C18A H18D 103.1 . . ? C17A C18A C19A 136.2(10) . . ? H18C C18A H18D 105.1 . . ? C19A C18A H18C 103.1 . . ? C19A C18A H18D 103.1 . . ? N4A C19A C18A 105.4(8) . . ? N4A C19A H19C 110.7 . . ? N4A C19A H19D 110.7 . . ? C18A C19A H19C 110.7 . . ? C18A C19A H19D 110.7 . . ? H19C C19A H19D 108.8 . . ? C20A O1A Ni1 115.6(7) . . ? C21A O2A Ni1 107.0(6) . . ? C27A O3A C28A 119.8(8) . . ? O1A C20A C21A 118.9(8) . . ? O1A C20A C28A 124.9(10) . . ? C28A C20A C21A 116.1(8) . . ? O2A C21A C20A 117.2(8) . . ? O2A C21A C22A 121.5(8) . . ? C22A C21A C20A 121.2(8) . . ? C23A C22A C21A 124.8(9) . . ? C23A C22A C27A 118.6(9) . . ? C27A C22A C21A 116.6(9) . . ? C22A C23A H23A 119.0 . . ? C22A C23A C24A 121.9(11) . . ? C24A C23A H23A 119.0 . . ? C23A C24A H24A 119.0 . . ? C23A C24A C25A 122.1(12) . . ? C25A C24A H24A 119.0 . . ? C24A C25A H25A 123.5 . . ? C26A C25A C24A 113.0(13) . . ? C26A C25A H25A 123.5 . . ? C25A C26A H26A 116.3 . . ? C27A C26A C25A 127.3(15) . . ? C27A C26A H26A 116.3 . . ? O3A C27A C22A 122.7(9) . . ? O3A C27A C26A 120.5(10) . . ? C26A C27A C22A 116.7(12) . . ? O3A C28A C29A 110.3(8) . . ? C20A C28A O3A 122.7(9) . . ? C20A C28A C29A 126.7(9) . . ? C28A C29A C30A 115.8(11) . . ? C34A C29A C28A 121.8(12) . . ? C34A C29A C30A 122.3(12) . . ? C29A C30A H30A 123.9 . . ? C31A C30A C29A 112.3(15) . . ? C31A C30A H30A 123.9 . . ? C30A C31A H31A 116.8 . . ? C30A C31A C32A 126.4(16) . . ? C32A C31A H31A 116.8 . . ? C31A C32A H32A 120.8 . . ? C33A C32A C31A 118.4(14) . . ? C33A C32A H32A 120.8 . . ? C32A C33A H33A 120.5 . . ? C34A C33A C32A 119.0(14) . . ? C34A C33A H33A 120.5 . . ? C29A C34A C33A 121.6(13) . . ? C29A C34A H34A 119.2 . . ? C33A C34A H34A 119.2 . . ? O4 Cl1 O5 109.2(2) . . ? O4 Cl1 O6 109.4(2) . . ? O4 Cl1 O7 109.8(2) . . ? O5 Cl1 O7 109.85(18) . . ? O6 Cl1 O5 109.4(2) . . ? O6 Cl1 O7 109.1(2) . . ? 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 N1 2.318(8) . ? Ni1 N2 2.071(6) . ? Ni1 N3 2.133(5) . ? Ni1 N4 2.107(9) . ? Ni1 O1 2.017(4) . ? Ni1 O2 2.133(4) . ? Ni1 N1A 2.102(12) . ? Ni1 N2A 2.057(7) . ? Ni1 N3A 2.151(7) . ? Ni1 N4A 2.195(14) . ? Ni1 O1A 1.884(8) . ? Ni1 O2A 2.229(7) . ? Br1 C1 1.892(9) . ? Br2 C12 1.882(7) . ? N1 C1 1.322(8) . ? N1 C5 1.346(9) . ? N2 C6 1.490(7) . ? N2 C7 1.483(7) . ? N2 C13 1.480(15) . ? N3 C8 1.350(8) . ? N3 C12 1.339(7) . ? C1 C2 1.383(11) . ? C2 H2 0.9500 . ? C2 C3 1.382(12) . ? C3 H3 0.9500 . ? C3 C4 1.381(11) . ? C4 H4 0.9500 . ? C4 C5 1.392(8) . ? C5 C6 1.502(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.502(8) . ? C8 C9 1.385(7) . ? C9 H9 0.9500 . ? C9 C10 1.367(10) . ? C10 H10 0.9500 . ? C10 C11 1.358(11) . ? C11 H11 0.9500 . ? C11 C12 1.404(9) . ? N4 C14 1.475(8) . ? N4 C15 1.477(8) . ? N4 C19 1.496(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.555(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.530(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.593(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.488(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.753(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? O1 C20 1.299(8) . ? O2 C21 1.273(7) . ? O3 C27 1.343(8) . ? O3 C28 1.400(7) . ? C20 C21 1.460(9) . ? C20 C28 1.382(7) . ? C21 C22 1.438(8) . ? C22 C23 1.400(6) . ? C22 C27 1.394(6) . ? C23 H23 0.9500 . ? C23 C24 1.384(7) . ? C24 H24 0.9500 . ? C24 C25 1.379(7) . ? C25 H25 0.9500 . ? C25 C26 1.386(7) . ? C26 H26 0.9500 . ? C26 C27 1.396(7) . ? C28 C29 1.456(9) . ? C29 C30 1.459(12) . ? C29 C34 1.363(11) . ? C30 H30 0.9500 . ? C30 C31 1.371(12) . ? C31 H31 0.9500 . ? C31 C32 1.404(11) . ? C32 H32 0.9500 . ? C32 C33 1.397(9) . ? C33 H33 0.9500 . ? C33 C34 1.378(11) . ? C34 H34 0.9500 . ? Br1A C1A 1.901(11) . ? Br2A C12A 1.903(9) . ? N1A C1A 1.323(10) . ? N1A C5A 1.347(11) . ? N2A C6A 1.483(9) . ? N2A C7A 1.477(9) . ? N2A C13A 1.51(3) . ? N3A C8A 1.358(9) . ? N3A C12A 1.360(8) . ? C1A C2A 1.385(12) . ? C2A H2A 0.9500 . ? C2A C3A 1.379(13) . ? C3A H3A 0.9500 . ? C3A C4A 1.377(13) . ? C4A H4A 0.9500 . ? C4A C5A 1.394(10) . ? C5A C6A 1.505(11) . ? C6A H6AA 0.9900 . ? C6A H6AB 0.9900 . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C7A C8A 1.504(9) . ? C8A C9A 1.389(9) . ? C9A H9A 0.9500 . ? C9A C10A 1.360(12) . ? C10A H10A 0.9500 . ? C10A C11A 1.359(12) . ? C11A H11A 0.9500 . ? C11A C12A 1.415(11) . ? N4A C14A 1.477(10) . ? N4A C15A 1.477(9) . ? N4A C19A 1.487(9) . ? C13A H13C 0.9900 . ? C13A H13D 0.9900 . ? C13A C14A 1.557(10) . ? C14A H14C 0.9900 . ? C14A H14D 0.9900 . ? C15A H15C 0.9900 . ? C15A H15D 0.9900 . ? C15A C16A 1.523(10) . ? C16A H16C 0.9900 . ? C16A H16D 0.9900 . ? C16A C17A 1.536(12) . ? C17A H17C 0.9900 . ? C17A H17D 0.9900 . ? C17A C18A 1.375(12) . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C18A C19A 1.712(10) . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? O1A C20A 1.313(10) . ? O2A C21A 1.258(9) . ? O3A C27A 1.362(10) . ? O3A C28A 1.390(9) . ? C20A C21A 1.448(11) . ? C20A C28A 1.380(9) . ? C21A C22A 1.444(10) . ? C22A C23A 1.383(7) . ? C22A C27A 1.386(7) . ? C23A H23A 0.9500 . ? C23A C24A 1.388(8) . ? C24A H24A 0.9500 . ? C24A C25A 1.391(8) . ? C25A H25A 0.9500 . ? C25A C26A 1.388(8) . ? C26A H26A 0.9500 . ? C26A C27A 1.386(8) . ? C28A C29A 1.442(11) . ? C29A C30A 1.463(15) . ? C29A C34A 1.357(13) . ? C30A H30A 0.9500 . ? C30A C31A 1.357(14) . ? C31A H31A 0.9500 . ? C31A C32A 1.392(13) . ? C32A H32A 0.9500 . ? C32A C33A 1.383(12) . ? C33A H33A 0.9500 . ? C33A C34A 1.365(13) . ? C34A H34A 0.9500 . ? Cl1 O4 1.433(3) . ? Cl1 O5 1.437(3) . ? Cl1 O6 1.433(3) . ? Cl1 O7 1.440(3) . ? 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 N1 C1 Br1 -27.2(11) . . . . ? Ni1 N1 C1 C2 154.0(8) . . . . ? Ni1 N1 C5 C4 -157.2(8) . . . . ? Ni1 N1 C5 C6 22.8(10) . . . . ? Ni1 N2 C6 C5 -39.5(10) . . . . ? Ni1 N2 C7 C8 -19.9(15) . . . . ? Ni1 N2 C13 C14 -21.5(7) . . . . ? Ni1 N3 C8 C7 -11(3) . . . . ? Ni1 N3 C8 C9 172.6(17) . . . . ? Ni1 N3 C12 Br2 8.1(14) . . . . ? Ni1 N3 C12 C11 -170.0(10) . . . . ? Ni1 N4 C14 C13 -54.4(7) . . . . ? Ni1 N4 C15 C16 -177.6(6) . . . . ? Ni1 N4 C19 C18 -159.6(5) . . . . ? Ni1 O1 C20 C21 11.0(10) . . . . ? Ni1 O1 C20 C28 -166.5(7) . . . . ? Ni1 O2 C21 C20 -3.9(8) . . . . ? Ni1 O2 C21 C22 175.5(5) . . . . ? Ni1 N1A C1A Br1A -16(2) . . . . ? Ni1 N1A C1A C2A 161.1(13) . . . . ? Ni1 N1A C5A C4A -167.1(12) . . . . ? Ni1 N1A C5A C6A 10.9(16) . . . . ? Ni1 N2A C6A C5A -49.6(11) . . . . ? Ni1 N2A C7A C8A -32(2) . . . . ? Ni1 N2A C13A C14A 46.8(12) . . . . ? Ni1 N3A C8A C7A -4(4) . . . . ? Ni1 N3A C8A C9A 175(3) . . . . ? Ni1 N3A C12A Br2A -5(3) . . . . ? Ni1 N3A C12A C11A 176.3(18) . . . . ? Ni1 N4A C14A C13A 44.8(10) . . . . ? Ni1 N4A C15A C16A -178.7(7) . . . . ? Ni1 N4A C19A C18A 140.3(6) . . . . ? Ni1 O1A C20A C21A -3.8(19) . . . . ? Ni1 O1A C20A C28A 173.8(13) . . . . ? Ni1 O2A C21A C20A 9.8(13) . . . . ? Ni1 O2A C21A C22A -168.0(8) . . . . ? Br1 C1 C2 C3 178.7(6) . . . . ? N1 C1 C2 C3 -2.5(14) . . . . ? N1 C5 C6 N2 7.8(12) . . . . ? N2 C7 C8 N3 21(3) . . . . ? N2 C7 C8 C9 -162.8(19) . . . . ? N2 C13 C14 N4 53.9(8) . . . . ? N3 C8 C9 C10 -2(3) . . . . ? C1 N1 C5 C4 1.7(15) . . . . ? C1 N1 C5 C6 -178.3(9) . . . . ? C1 C2 C3 C4 2.5(12) . . . . ? C2 C3 C4 C5 -0.7(13) . . . . ? C3 C4 C5 N1 -1.5(15) . . . . ? C3 C4 C5 C6 178.4(9) . . . . ? C4 C5 C6 N2 -172.1(9) . . . . ? C5 N1 C1 Br1 179.2(7) . . . . ? C5 N1 C1 C2 0.4(14) . . . . ? C6 N2 C7 C8 -143.2(14) . . . . ? C6 N2 C13 C14 102.9(8) . . . . ? C7 N2 C6 C5 82.9(10) . . . . ? C7 N2 C13 C14 -140.3(6) . . . . ? C7 C8 C9 C10 -178.4(17) . . . . ? C8 N3 C12 Br2 175.2(18) . . . . ? C8 N3 C12 C11 -3(2) . . . . ? C8 C9 C10 C11 0(2) . . . . ? C9 C10 C11 C12 0.9(16) . . . . ? C10 C11 C12 Br2 -177.5(9) . . . . ? C10 C11 C12 N3 0.6(16) . . . . ? C12 N3 C8 C7 180.0(15) . . . . ? C12 N3 C8 C9 4(3) . . . . ? N4 C15 C16 C17 43.9(10) . . . . ? C13 N2 C6 C5 -162.2(8) . . . . ? C13 N2 C7 C8 97.7(14) . . . . ? C14 N4 C15 C16 68.1(9) . . . . ? C14 N4 C19 C18 -52.7(8) . . . . ? C15 N4 C14 C13 69.2(9) . . . . ? C15 N4 C19 C18 71.5(8) . . . . ? C15 C16 C17 C18 -67.2(9) . . . . ? C16 C17 C18 C19 80.8(7) . . . . ? C17 C18 C19 N4 -85.7(7) . . . . ? C19 N4 C14 C13 -169.4(7) . . . . ? C19 N4 C15 C16 -51.6(10) . . . . ? O1 C20 C21 O2 -4.5(11) . . . . ? O1 C20 C21 C22 176.1(7) . . . . ? O1 C20 C28 O3 -176.1(8) . . . . ? O1 C20 C28 C29 7.5(14) . . . . ? O2 C21 C22 C23 5.0(11) . . . . ? O2 C21 C22 C27 -177.9(6) . . . . ? O3 C28 C29 C30 -1.1(11) . . . . ? O3 C28 C29 C34 -173.2(8) . . . . ? C20 C21 C22 C23 -175.6(8) . . . . ? C20 C21 C22 C27 1.5(10) . . . . ? C20 C28 C29 C30 175.5(10) . . . . ? C20 C28 C29 C34 3.4(13) . . . . ? C21 C20 C28 O3 6.5(12) . . . . ? C21 C20 C28 C29 -169.9(7) . . . . ? C21 C22 C23 C24 178.2(8) . . . . ? C21 C22 C27 O3 3.1(11) . . . . ? C21 C22 C27 C26 -177.8(10) . . . . ? C22 C23 C24 C25 -0.2(16) . . . . ? C23 C22 C27 O3 -179.7(8) . . . . ? C23 C22 C27 C26 -0.6(13) . . . . ? C23 C24 C25 C26 -1.1(18) . . . . ? C24 C25 C26 C27 2(2) . . . . ? C25 C26 C27 O3 178.3(12) . . . . ? C25 C26 C27 C22 -0.8(19) . . . . ? C27 O3 C28 C20 -2.0(11) . . . . ? C27 O3 C28 C29 174.8(7) . . . . ? C27 C22 C23 C24 1.1(13) . . . . ? C28 O3 C27 C22 -3.0(11) . . . . ? C28 O3 C27 C26 177.8(10) . . . . ? C28 C20 C21 O2 173.2(7) . . . . ? C28 C20 C21 C22 -6.3(12) . . . . ? C28 C29 C30 C31 -176.0(8) . . . . ? C28 C29 C34 C33 173.6(8) . . . . ? C29 C30 C31 C32 3.3(16) . . . . ? C30 C29 C34 C33 1.7(15) . . . . ? C30 C31 C32 C33 -0.9(13) . . . . ? C31 C32 C33 C34 -1.3(12) . . . . ? C32 C33 C34 C29 0.8(14) . . . . ? C34 C29 C30 C31 -3.6(16) . . . . ? Br1A C1A C2A C3A 177.8(11) . . . . ? N1A Ni1 O1A C20A -72.2(11) . . . . ? N1A C1A C2A C3A 0(2) . . . . ? N1A C5A C6A N2A 27.8(17) . . . . ? N2A Ni1 O1A C20A -3.5(18) . . . . ? N2A C7A C8A N3A 25(5) . . . . ? N2A C7A C8A C9A -154(3) . . . . ? N2A C13A C14A N4A -64.7(12) . . . . ? N3A Ni1 O1A C20A -166.7(12) . . . . ? N3A C8A C9A C10A 9(5) . . . . ? C1A N1A C5A C4A 1(2) . . . . ? C1A N1A C5A C6A 179.3(13) . . . . ? C1A C2A C3A C4A 3(2) . . . . ? C2A C3A C4A C5A -4(2) . . . . ? C3A C4A C5A N1A 2(2) . . . . ? C3A C4A C5A C6A -176.2(13) . . . . ? C4A C5A C6A N2A -154.1(13) . . . . ? C5A N1A C1A Br1A -179.8(12) . . . . ? C5A N1A C1A C2A -2(2) . . . . ? C6A N2A C7A C8A -138(2) . . . . ? C6A N2A C13A C14A 151.6(9) . . . . ? C7A N2A C6A C5A 61.7(13) . . . . ? C7A N2A C13A C14A -74.5(14) . . . . ? C7A C8A C9A C10A -172(2) . . . . ? C8A N3A C12A Br2A 180(3) . . . . ? C8A N3A C12A C11A 1(4) . . . . ? C8A C9A C10A C11A -2(3) . . . . ? C9A C10A C11A C12A -5(3) . . . . ? C10A C11A C12A Br2A -173.2(15) . . . . ? C10A C11A C12A N3A 5(3) . . . . ? C12A N3A C8A C7A 173(3) . . . . ? C12A N3A C8A C9A -8(6) . . . . ? N4A Ni1 O1A C20A 98.2(11) . . . . ? N4A C15A C16A C17A 58.7(14) . . . . ? C13A N2A C6A C5A -158.9(10) . . . . ? C13A N2A C7A C8A 88(2) . . . . ? C14A N4A C15A C16A 66.4(12) . . . . ? C14A N4A C19A C18A -107.4(10) . . . . ? C15A N4A C14A C13A 164.6(11) . . . . ? C15A N4A C19A C18A 18.1(12) . . . . ? C15A C16A C17A C18A -10.0(16) . . . . ? C16A C17A C18A C19A -38(2) . . . . ? C17A C18A C19A N4A 37(2) . . . . ? C19A N4A C14A C13A -71.8(12) . . . . ? C19A N4A C15A C16A -57.4(12) . . . . ? O1A C20A C21A O2A -5(2) . . . . ? O1A C20A C21A C22A 172.5(12) . . . . ? O1A C20A C28A O3A 179.8(14) . . . . ? O1A C20A C28A C29A 6(3) . . . . ? O2A Ni1 O1A C20A 6.7(11) . . . . ? O2A C21A C22A C23A 6.1(19) . . . . ? O2A C21A C22A C27A -175.2(11) . . . . ? O3A C28A C29A C30A -3(2) . . . . ? O3A C28A C29A C34A -179.9(14) . . . . ? C20A C21A C22A C23A -171.6(14) . . . . ? C20A C21A C22A C27A 7.0(18) . . . . ? C20A C28A C29A C30A 171.7(18) . . . . ? C20A C28A C29A C34A -5(2) . . . . ? C21A C20A C28A O3A -3(2) . . . . ? C21A C20A C28A C29A -176.7(12) . . . . ? C21A C22A C23A C24A -179.8(13) . . . . ? C21A C22A C27A O3A -0.8(19) . . . . ? C21A C22A C27A C26A 175.4(16) . . . . ? C22A C23A C24A C25A 1(2) . . . . ? C23A C22A C27A O3A 177.9(14) . . . . ? C23A C22A C27A C26A -6(2) . . . . ? C23A C24A C25A C26A 1(2) . . . . ? C24A C25A C26A C27A -6(3) . . . . ? C25A C26A C27A O3A -174.8(18) . . . . ? C25A C26A C27A C22A 9(3) . . . . ? C27A O3A C28A C20A 9(2) . . . . ? C27A O3A C28A C29A -176.3(13) . . . . ? C27A C22A C23A C24A 2(2) . . . . ? C28A O3A C27A C22A -7(2) . . . . ? C28A O3A C27A C26A 177.1(17) . . . . ? C28A C20A C21A O2A 176.8(12) . . . . ? C28A C20A C21A C22A -5(2) . . . . ? C28A C29A C30A C31A -176.0(18) . . . . ? C28A C29A C34A C33A 176.9(15) . . . . ? C29A C30A C31A C32A -2(4) . . . . ? C30A C29A C34A C33A 0(3) . . . . ? C30A C31A C32A C33A 1(3) . . . . ? C31A C32A C33A C34A 0(3) . . . . ? C32A C33A C34A C29A -1(3) . . . . ? C34A C29A C30A C31A 1(3) . . . . ? 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 0.0001 -1.0009 -1.0003 0.1147 0.0076 0.0845 -0.0001 1.0009 1.0003 -0.1147 -0.0076 -0.0845 0.9999 -0.0018 -1.0008 -0.0031 0.1269 0.1309 -1.9997 1.0033 2.0014 0.0072 -0.2169 -0.2974 -0.0002 -0.9997 0.0002 -0.0009 -0.0369 0.0357 0.0002 0.9997 -0.0002 0.0009 0.0369 -0.0357 -0.9994 2.0000 -0.0001 0.1206 -0.0087 -0.1534 0.9994 -2.0000 0.0001 -0.1206 0.0087 0.1534