#------------------------------------------------------------------------------ #$Date: 2026-04-29 01:35:00 +0100 (Wed, 29 Apr 2026) $ #$Revision: 305650 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/43/7064389.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_7064389 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 'C36 H39 N4 Ni O3, Cl O4' _chemical_formula_sum 'C36 H39 Cl N4 Ni O7' _chemical_formula_weight 733.87 _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 2024-08-02 _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 105.9780(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.65110(10) _cell_length_b 29.7064(3) _cell_length_c 12.03790(10) _cell_measurement_reflns_used 26043 _cell_measurement_temperature 100.6(10) _cell_measurement_theta_max 79.4240 _cell_measurement_theta_min 2.9380 _cell_volume 3317.93(6) _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 100.6(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 0.999 _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 -26.00 11.00 0.50 0.10 -- 47.69 -19.00 120.00 74 2 \w 48.00 112.00 0.50 0.10 -- 47.69-152.00 66.00 128 3 \w 97.00 128.00 0.50 0.30 -- 113.25-152.00 66.00 62 4 \w 44.00 99.00 0.50 0.30 -- 113.25-125.00 60.00 110 5 \w -21.00 4.00 0.50 0.10 -- 47.69 -19.00 -60.00 50 6 \w -27.00 -2.00 0.50 0.10 -- 47.69 -19.00-180.00 50 7 \w 60.00 106.00 0.50 0.30 -- 113.25 -95.00 -60.00 92 8 \w 77.00 102.00 0.50 0.30 -- 113.25-122.00-132.00 50 9 \w 32.00 92.00 0.50 0.10 -- 47.69-122.00-132.00 120 10 \w 55.00 106.00 0.50 0.30 -- 113.25 -95.00 -90.00 102 11 \w 52.00 98.00 0.50 0.30 -- 113.25 -95.00-120.00 92 12 \w 42.00 104.00 0.50 0.30 -- 113.25 -95.00-150.00 124 13 \w 42.00 75.00 0.50 0.30 -- 113.25 -61.00 -90.00 66 14 \w 44.00 75.00 0.50 0.30 -- 113.25 -61.00-120.00 62 15 \w 48.00 74.00 0.50 0.30 -- 113.25 -61.00-150.00 52 16 \w 42.00 67.00 0.50 0.30 -- 113.25 -61.00 60.00 50 17 \w 107.00 173.00 0.50 0.30 -- 113.25 30.00 -90.00 132 18 \w 104.00 178.00 0.50 0.30 -- 113.25 45.00 -60.00 148 19 \w 106.00 177.00 0.50 0.30 -- 113.25 61.00-150.00 142 20 \w 97.00 178.00 0.50 0.30 -- 113.25 122.00 -51.00 162 21 \w 77.00 158.00 0.50 0.30 -- 113.25 152.00 109.00 162 22 \w 101.00 158.00 0.50 0.30 -- 113.25 125.00 150.00 114 23 \w -26.00 23.00 0.50 0.10 -- -47.69 38.00 90.00 98 24 \w -85.00 -11.00 0.50 0.10 -- -47.69 122.00 -51.00 148 25 \w -105.00 -27.00 0.50 0.10 -- -47.69 152.00 109.00 156 26 \w -10.00 27.00 0.50 0.10 -- -47.69 19.00 -30.00 74 27 \w -11.00 25.00 0.50 0.10 -- -47.69 19.00-150.00 72 28 \w -119.00 -55.00 0.50 0.10 -- -47.69-152.00 66.00 128 29 \w -161.00 -75.00 0.50 0.30 -- -91.75-122.00-132.00 172 30 \w -46.00 -21.00 0.50 0.30 -- -91.75 45.00-180.00 50 31 \w -49.00 -24.00 0.50 0.30 -- -91.75 45.00 120.00 50 32 \w -48.00 -22.00 0.50 0.30 -- -91.75 45.00 150.00 52 ; _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 -0.1007262000 _diffrn_orient_matrix_UB_12 -0.0015245000 _diffrn_orient_matrix_UB_13 -0.1239654000 _diffrn_orient_matrix_UB_21 0.0163384000 _diffrn_orient_matrix_UB_22 -0.0515477000 _diffrn_orient_matrix_UB_23 -0.0012941000 _diffrn_orient_matrix_UB_31 -0.1310306000 _diffrn_orient_matrix_UB_32 -0.0052073000 _diffrn_orient_matrix_UB_33 0.0486312000 _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 0.0278 _diffrn_reflns_av_unetI/netI 0.0175 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 34615 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.501 _diffrn_reflns_theta_min 2.975 _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 2.059 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.292 _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 1.469 _exptl_crystal_description block _exptl_crystal_F_000 1536 _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.413 _exptl_crystal_size_min 0.139 _refine_diff_density_max 0.608 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 702 _refine_ls_number_reflns 6767 _refine_ls_number_restraints 1325 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0413 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+2.9423P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1018 _refine_ls_wR_factor_ref 0.1023 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6555 _reflns_number_total 6767 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj00257a2.cif _cod_data_source_block kskr38 _cod_database_code 7064389 _shelx_shelxl_version_number 2019/1 _chemical_oxdiff_formula 'C36 H41 Cl1 N4 Ni1 O7 ' _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 0.763 _shelx_estimated_absorpt_t_min 0.403 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C16A-C15 \\sim C16-C15 with sigma of 0.01 N4-C16A \\sim N4-C16 with sigma of 0.01 N4-C17A \\sim N4-C17 \\sim N4-C21 \\sim N4-C21A with sigma of 0.01 C18A-C17A \\sim C18-C17 \\sim C21-C20 \\sim C21A-C20A with sigma of 0.01 C19A-C18A \\sim C19-C18 \\sim C20-C19 \\sim C20A-C19A with sigma of 0.01 N3-C13A \\sim N3-C13 with sigma of 0.01 C9-C10 \\sim C9-C10A with sigma of 0.01 3. Uiso/Uaniso restraints and constraints O1 \\sim O2 \\sim O3 \\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 C35 \\sim C36 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim O1A \\sim O2A \\sim O3A \\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A \\sim C21A \\sim C22A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Uanis(C22A) = Uanis(C22) 4. Rigid body (RIGU) restrains O1, O2, O3, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C10, C11, C12, C13, C14, C16, C17, C18, C19, C20, C21, C22, O1A, O2A, O3A, C23A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, C35A, C36A, C10A, C11A, C12A, C13A, C14A, C16A, C17A, C18A, C19A, C20A, C21A, C22A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Same fragment restrains {C10, C11, C12, C13, C14} sigma for 1-2: 0.01, 1-3: 0.04 as in {C10A, C11A, C12A, C13A, C14A} {O1, O2, O3, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36} sigma for 1-2: 0.01, 1-3: 0.04 as in {O1A, O2A, O3A, C23A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, C35A, C36A} 6. Others Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(C26A)=Sof(H26A)= Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)= Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)= Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C10A)=Sof(H10A)=Sof(C11A)= Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(H14D)=Sof(H14E)= Sof(H14F)=Sof(C22A)=1-FVAR(1) Sof(O1)=Sof(O2)=Sof(O3)=Sof(C23)=Sof(C24)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)= Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(C31)=Sof(C32)= Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)= Sof(H36)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)= Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C22)=FVAR(1) 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(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(2) 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(C20)=Sof(H20A)= Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(2) 7.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C15(H15C,H15D), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,H18D), C19A(H19C,H19D), C20A(H20C, H20D), C21A(H21C,H21D) 7.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C10(H10), C11(H11), C12(H12), C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C10A(H10A), C11A(H11A), C12A(H12A) 7.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F) ; _shelx_res_file ; TITL kskr38_a.res in P2(1)/n kskr38.res created by SHELXL-2019/1 at 13:41:54 on 02-Aug-2024 REM Old TITL KSKR38 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.165, Rweak 0.018, Alpha 0.042 REM 2.672 for 156 systematic absences, Orientation as input REM Formula found by SHELXT: C36 N3 O8 Cl Ni CELL 1.54184 9.6511 29.7064 12.0379 90 105.978 90 ZERR 4 0.0001 0.0003 0.0001 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl N Ni O UNIT 144 156 4 16 4 28 EADP C22A C22 SADI 0.01 C16A C15 C16 C15 SADI 0.01 N4 C16A N4 C16 SADI 0.01 N4 C17A N4 C17 N4 C21 N4 C21A SADI 0.01 C18A C17A C18 C17 C21 C20 C21A C20A SADI 0.01 C19A C18A C19 C18 C20 C19 C20A C19A SADI 0.01 N3 C13A N3 C13 SADI 0.01 C9 C10 C9 C10A RIGU 0.01 0.01 O1 > C22A SIMU 0.01 0.02 2 O1 > C22A L.S. 8 0 0 PLAN 10 SIZE 0.139 0.413 0.54 TEMP -172.5(10) CONF BOND list 4 MORE -1 BOND $H wpdb -1 fmap 2 53 acta REM REM REM WGHT 0.037600 2.942300 FVAR 0.30930 0.68999 0.79069 NI1 5 0.654252 0.648336 0.643769 11.00000 0.01936 0.02492 = 0.03656 0.00110 0.00785 -0.00225 N1 4 0.692681 0.590067 0.544153 11.00000 0.02165 0.02596 = 0.04396 -0.00349 0.00510 -0.00170 N2 4 0.747703 0.677142 0.526099 11.00000 0.03205 0.02570 = 0.02447 -0.00097 0.00618 -0.00153 N3 4 0.866563 0.648096 0.752902 11.00000 0.02803 0.02912 = 0.02733 -0.00075 0.00339 0.00375 N4 4 0.618308 0.717214 0.688543 11.00000 0.02652 0.02715 = 0.03438 0.00165 0.01296 0.00052 C1 1 0.711858 0.531657 0.686899 11.00000 0.05050 0.03053 = 0.06241 0.00549 0.01832 -0.00010 AFIX 137 H1A 2 0.804915 0.543451 0.732655 11.00000 -1.50000 H1B 2 0.712725 0.498715 0.691410 11.00000 -1.50000 H1C 2 0.634864 0.543494 0.717370 11.00000 -1.50000 AFIX 0 C2 1 0.686247 0.545742 0.564762 11.00000 0.02479 0.02845 = 0.05594 0.00149 0.01233 0.00018 C3 1 0.655665 0.514762 0.473616 11.00000 0.03133 0.02570 = 0.07305 -0.00843 0.01737 -0.00162 AFIX 43 H3 2 0.649980 0.483553 0.489017 11.00000 -1.20000 AFIX 0 C4 1 0.633742 0.529542 0.361272 11.00000 0.03375 0.03882 = 0.05866 -0.01631 0.00926 -0.00277 AFIX 43 H4 2 0.610104 0.508796 0.298828 11.00000 -1.20000 AFIX 0 C5 1 0.646542 0.574428 0.341247 11.00000 0.03677 0.03823 = 0.04348 -0.01180 0.00043 0.00085 AFIX 43 H5 2 0.634975 0.585305 0.265019 11.00000 -1.20000 AFIX 0 C6 1 0.676899 0.603928 0.434869 11.00000 0.02813 0.03357 = 0.03353 -0.00518 -0.00051 0.00037 C7 1 0.689747 0.653573 0.414990 11.00000 0.05409 0.03339 = 0.02529 -0.00276 0.00073 0.00208 AFIX 23 H7A 2 0.754456 0.658508 0.365023 11.00000 -1.20000 H7B 2 0.593783 0.665972 0.374931 11.00000 -1.20000 AFIX 0 C8 1 0.905224 0.670044 0.568486 11.00000 0.03019 0.03505 = 0.03640 -0.00398 0.01605 -0.00486 AFIX 23 H8A 2 0.954922 0.696065 0.545206 11.00000 -1.20000 H8B 2 0.931097 0.642889 0.530894 11.00000 -1.20000 AFIX 0 C9 1 0.958634 0.664446 0.697032 11.00000 0.02228 0.02458 = 0.03941 -0.00627 0.00555 0.00073 C15 1 0.710444 0.725712 0.517997 11.00000 0.04797 0.02470 = 0.03324 0.00282 0.01415 0.00075 PART 1 AFIX 23 H15A 2 0.612229 0.729887 0.465877 31.00000 -1.20000 H15B 2 0.778817 0.742360 0.485144 31.00000 -1.20000 AFIX 23 PART 2 H15C 2 0.685169 0.735200 0.436027 -31.00000 -1.20000 H15D 2 0.795327 0.743403 0.560755 -31.00000 -1.20000 AFIX 0 PART 1 O1 6 0.518608 0.619424 0.721236 21.00000 0.02572 0.03441 = 0.02454 0.00158 0.00594 -0.00577 O2 6 0.458520 0.646360 0.503273 21.00000 0.02300 0.03034 = 0.02848 0.00124 0.00511 -0.00407 O3 6 0.160414 0.572469 0.600310 21.00000 0.02296 0.03313 = 0.03246 -0.00388 0.00917 -0.00654 C23 1 0.367734 0.621772 0.530845 21.00000 0.02181 0.02551 = 0.02921 0.00050 0.00716 0.00127 C24 1 0.240888 0.605005 0.446371 21.00000 0.02417 0.02533 = 0.03352 -0.00030 0.00538 -0.00076 C25 1 0.140439 0.580993 0.486570 21.00000 0.02494 0.02801 = 0.03352 -0.00127 0.00569 -0.00012 C26 1 0.015058 0.563710 0.411684 21.00000 0.02583 0.03387 = 0.04263 -0.00154 0.00575 -0.00725 AFIX 43 H26 2 -0.053143 0.547763 0.440406 21.00000 -1.20000 AFIX 0 C27 1 -0.007381 0.570397 0.294519 21.00000 0.03468 0.04410 = 0.04598 -0.00361 -0.00621 -0.00775 AFIX 43 H27 2 -0.093316 0.559542 0.242037 21.00000 -1.20000 AFIX 0 C28 1 0.095459 0.593105 0.251737 21.00000 0.04303 0.04459 = 0.03243 0.00192 -0.00264 -0.00847 AFIX 43 H28 2 0.079932 0.596457 0.170746 21.00000 -1.20000 AFIX 0 C29 1 0.217480 0.610342 0.326162 21.00000 0.03540 0.03495 = 0.03364 0.00415 0.00491 -0.00442 AFIX 43 H29 2 0.286173 0.625841 0.297030 21.00000 -1.20000 AFIX 0 C30 1 0.286774 0.584175 0.682028 21.00000 0.02437 0.02666 = 0.03189 -0.00368 0.00738 -0.00272 C31 1 0.285738 0.568096 0.795758 21.00000 0.03565 0.02619 = 0.03553 -0.00395 0.01686 -0.00427 C32 1 0.399054 0.578427 0.894287 21.00000 0.03922 0.03718 = 0.03499 0.00103 0.01667 -0.00841 AFIX 43 H32 2 0.478176 0.596130 0.887244 21.00000 -1.20000 AFIX 0 C33 1 0.394580 0.562621 1.001721 21.00000 0.06086 0.04590 = 0.03439 -0.00133 0.01370 -0.01665 AFIX 43 H33 2 0.470483 0.570126 1.068094 21.00000 -1.20000 AFIX 0 C34 1 0.281820 0.536152 1.014140 21.00000 0.07580 0.05102 = 0.03817 0.00321 0.02755 -0.01895 AFIX 43 H34 2 0.281250 0.524979 1.087957 21.00000 -1.20000 AFIX 0 C35 1 0.170818 0.526260 0.918366 21.00000 0.06167 0.05022 = 0.04752 -0.00275 0.02622 -0.02304 AFIX 43 H35 2 0.092428 0.508437 0.926425 21.00000 -1.20000 AFIX 0 C36 1 0.171466 0.541719 0.811351 21.00000 0.04657 0.04428 = 0.04330 -0.00610 0.01830 -0.01502 AFIX 43 H36 2 0.093250 0.534496 0.746384 21.00000 -1.20000 AFIX 0 C10 1 1.100135 0.673233 0.762488 21.00000 0.02562 0.03044 = 0.03555 -0.00358 0.00711 -0.00167 AFIX 43 H10 2 1.166755 0.685716 0.725786 21.00000 -1.20000 AFIX 0 C11 1 1.144516 0.664083 0.879332 21.00000 0.02598 0.03157 = 0.03417 -0.00341 -0.00023 0.00020 AFIX 43 H11 2 1.240665 0.670199 0.923098 21.00000 -1.20000 AFIX 0 C12 1 1.047413 0.646028 0.930997 21.00000 0.03316 0.03297 = 0.02733 -0.00067 -0.00073 -0.00026 AFIX 43 H12 2 1.076982 0.639153 1.011148 21.00000 -1.20000 AFIX 0 C13 1 0.905799 0.637615 0.867503 21.00000 0.02947 0.02845 = 0.02945 -0.00053 0.00275 -0.00049 C14 1 0.799416 0.618212 0.923937 21.00000 0.04071 0.04669 = 0.02379 0.00575 0.00354 -0.00807 AFIX 137 H14A 2 0.825556 0.586966 0.946321 21.00000 -1.50000 H14B 2 0.702869 0.619066 0.869681 21.00000 -1.50000 H14C 2 0.800038 0.635877 0.992828 21.00000 -1.50000 AFIX 0 C16 1 0.716904 0.744063 0.635634 31.00000 0.03043 0.02362 = 0.03593 0.00025 0.01422 -0.00357 AFIX 23 H16A 2 0.687029 0.776057 0.629055 31.00000 -1.20000 H16B 2 0.817010 0.742340 0.685872 31.00000 -1.20000 AFIX 0 C17 1 0.662704 0.724472 0.816880 31.00000 0.04326 0.03550 = 0.03496 0.00123 0.01631 0.00501 AFIX 23 H17A 2 0.766613 0.717504 0.847134 31.00000 -1.20000 H17B 2 0.609114 0.703110 0.852785 31.00000 -1.20000 AFIX 0 C18 1 0.636150 0.772231 0.853138 31.00000 0.05433 0.04118 = 0.03687 -0.00282 0.01778 0.00666 AFIX 23 H18A 2 0.659924 0.773795 0.938465 31.00000 -1.20000 H18B 2 0.700382 0.793365 0.827408 31.00000 -1.20000 AFIX 0 C19 1 0.480003 0.786438 0.801512 31.00000 0.04837 0.04064 = 0.05214 0.00284 0.02833 0.01258 AFIX 23 H19A 2 0.416901 0.768905 0.837846 31.00000 -1.20000 H19B 2 0.469188 0.818711 0.817871 31.00000 -1.20000 AFIX 0 C20 1 0.434221 0.778746 0.672252 31.00000 0.03356 0.03460 = 0.05559 0.00373 0.01784 0.00871 AFIX 23 H20A 2 0.485187 0.800336 0.634697 31.00000 -1.20000 H20B 2 0.329466 0.784410 0.642135 31.00000 -1.20000 AFIX 0 C21 1 0.467215 0.730970 0.641706 31.00000 0.02579 0.03323 = 0.05410 0.00103 0.01157 0.00195 AFIX 23 H21A 2 0.405540 0.709909 0.670550 31.00000 -1.20000 H21B 2 0.440859 0.728129 0.556507 31.00000 -1.20000 AFIX 0 C22 1 0.393582 0.608022 0.650868 21.00000 0.02082 0.02434 = 0.02541 -0.00058 0.00741 -0.00188 SAME 0.01 0.04 O1 > C36 PART 2 O1A 6 0.451952 0.639893 0.556702 -21.00000 0.01824 0.02941 = 0.03048 -0.00148 0.00763 -0.00243 O2A 6 0.568598 0.620101 0.777387 -21.00000 0.02317 0.03255 = 0.02883 0.00227 0.00461 -0.00286 O3A 6 0.165124 0.575421 0.624154 -21.00000 0.02661 0.03069 = 0.04182 -0.00791 0.01160 -0.00500 C23A 1 0.440514 0.608048 0.733165 -21.00000 0.02123 0.02566 = 0.03009 -0.00159 0.00882 -0.00152 C24A 1 0.357224 0.584431 0.797481 -21.00000 0.03153 0.02706 = 0.03877 -0.00447 0.01375 -0.00279 C25A 1 0.219749 0.569376 0.738229 -21.00000 0.03060 0.02893 = 0.04596 -0.00621 0.01770 -0.00513 C26A 1 0.134572 0.546413 0.794920 -21.00000 0.04280 0.03292 = 0.04770 -0.00144 0.02374 -0.01194 AFIX 43 H26A 2 0.042300 0.535509 0.753437 -21.00000 -1.20000 AFIX 0 C27A 1 0.185514 0.539579 0.912482 -21.00000 0.05615 0.04033 = 0.05361 -0.00049 0.02876 -0.01639 AFIX 43 H27A 2 0.125528 0.524974 0.952077 -21.00000 -1.20000 AFIX 0 C28A 1 0.324791 0.553773 0.975506 -21.00000 0.05531 0.04376 = 0.04603 0.00173 0.02035 -0.01595 AFIX 43 H28A 2 0.361183 0.547514 1.055667 -21.00000 -1.20000 AFIX 0 C29A 1 0.405306 0.576844 0.916945 -21.00000 0.04397 0.03592 = 0.03670 0.00027 0.01334 -0.01054 AFIX 43 H29A 2 0.496978 0.588117 0.958664 -21.00000 -1.20000 AFIX 0 C30A 1 0.243748 0.596614 0.558904 -21.00000 0.01877 0.02501 = 0.03742 -0.00439 0.00641 -0.00196 C31A 1 0.174053 0.592343 0.436997 -21.00000 0.02023 0.02513 = 0.04029 -0.00449 0.00355 -0.00449 C32A 1 0.242761 0.605416 0.353345 -21.00000 0.02432 0.03263 = 0.03579 -0.00414 -0.00386 -0.00791 AFIX 43 H32A 2 0.332554 0.620683 0.377499 -21.00000 -1.20000 AFIX 0 C33A 1 0.183909 0.596782 0.236771 -21.00000 0.03400 0.03840 = 0.03630 -0.00016 -0.00338 -0.00979 AFIX 43 H33A 2 0.234509 0.605458 0.182758 -21.00000 -1.20000 AFIX 0 C34A 1 0.051757 0.575577 0.198785 -21.00000 0.03559 0.03930 = 0.04124 -0.00112 -0.00685 -0.00613 AFIX 43 H34A 2 0.011976 0.569081 0.119077 -21.00000 -1.20000 AFIX 0 C35A 1 -0.021109 0.564050 0.277491 -21.00000 0.02889 0.03355 = 0.04424 -0.00392 -0.00096 -0.00791 AFIX 43 H35A 2 -0.113729 0.550611 0.251394 -21.00000 -1.20000 AFIX 0 C36A 1 0.037413 0.571586 0.393264 -21.00000 0.02325 0.03096 = 0.04375 -0.00301 0.00844 -0.00781 AFIX 43 H36A 2 -0.015024 0.562652 0.445790 -21.00000 -1.20000 AFIX 0 SAME 0.01 0.04 C10 > C14 C10A 1 1.103742 0.677016 0.730311 -21.00000 0.01649 0.02329 = 0.03901 -0.00540 -0.00002 -0.00210 AFIX 43 H10A 2 1.152422 0.689145 0.678410 -21.00000 -1.20000 AFIX 0 C11A 1 1.168918 0.670043 0.845841 -21.00000 0.02444 0.02754 = 0.03646 -0.00336 0.00183 -0.00104 AFIX 43 H11A 2 1.268576 0.676276 0.877389 -21.00000 -1.20000 AFIX 0 C12A 1 1.089066 0.654123 0.914381 -21.00000 0.02727 0.03024 = 0.02984 -0.00039 0.00069 -0.00151 AFIX 43 H12A 2 1.132966 0.649375 0.994396 -21.00000 -1.20000 AFIX 0 C13A 1 0.942674 0.644713 0.867630 -21.00000 0.03003 0.03075 = 0.03238 0.00156 0.00661 0.00032 C14A 1 0.854356 0.627504 0.943399 -21.00000 0.03550 0.05166 = 0.03687 0.00534 -0.00274 -0.00786 AFIX 137 H14D 2 0.770790 0.647174 0.936049 -21.00000 -1.50000 H14E 2 0.913238 0.627206 1.023975 -21.00000 -1.50000 H14F 2 0.821310 0.596884 0.919700 -21.00000 -1.50000 AFIX 0 C16A 1 0.587509 0.735265 0.566229 -31.00000 0.03647 0.02366 = 0.04602 -0.00042 0.00292 -0.00052 AFIX 23 H16C 2 0.499034 0.721021 0.517079 -31.00000 -1.20000 H16D 2 0.571095 0.768158 0.566424 -31.00000 -1.20000 AFIX 0 C17A 1 0.727431 0.738735 0.779556 -31.00000 0.04004 0.02944 = 0.03730 -0.00234 0.01102 -0.00241 AFIX 23 H17C 2 0.820140 0.738574 0.759305 -31.00000 -1.20000 H17D 2 0.740710 0.721503 0.852132 -31.00000 -1.20000 AFIX 0 C18A 1 0.686567 0.786930 0.798464 -31.00000 0.04180 0.03061 = 0.04231 -0.00072 0.01514 0.00171 AFIX 23 H18C 2 0.763848 0.800826 0.860681 -31.00000 -1.20000 H18D 2 0.676739 0.804524 0.726862 -31.00000 -1.20000 AFIX 0 C19A 1 0.545707 0.788368 0.831269 -31.00000 0.04080 0.03559 = 0.04778 0.00048 0.02146 0.00552 AFIX 23 H19C 2 0.556302 0.771811 0.904511 -31.00000 -1.20000 H19D 2 0.520476 0.819973 0.843083 -31.00000 -1.20000 AFIX 0 C20A 1 0.426914 0.767171 0.736132 -31.00000 0.03325 0.03873 = 0.05875 0.00176 0.01724 0.00755 AFIX 23 H20C 2 0.408957 0.785636 0.665120 -31.00000 -1.20000 H20D 2 0.336716 0.765930 0.760055 -31.00000 -1.20000 AFIX 0 C21A 1 0.471767 0.719437 0.711729 -31.00000 0.02909 0.03333 = 0.05467 -0.00435 0.01887 0.00435 AFIX 23 H21C 2 0.472991 0.700027 0.778845 -31.00000 -1.20000 H21D 2 0.398546 0.707181 0.643957 -31.00000 -1.20000 AFIX 0 C22A 1 0.376262 0.616418 0.608408 -21.00000 0.02082 0.02434 = 0.02541 -0.00058 0.00741 -0.00188 PART 0 CL1 3 1.024444 0.817155 0.618475 11.00000 0.02526 0.03146 = 0.03050 -0.00101 0.00156 0.00160 O4 6 1.140432 0.848906 0.634125 11.00000 0.03598 0.04053 = 0.04116 0.00420 0.00666 -0.00804 O5 6 0.981853 0.802465 0.500733 11.00000 0.04513 0.06795 = 0.03842 -0.01894 0.00468 0.00112 O6 6 1.070505 0.779054 0.692772 11.00000 0.04123 0.03567 = 0.06283 0.01486 -0.00290 -0.00287 O7 6 0.904409 0.838183 0.646355 11.00000 0.04081 0.04396 = 0.05248 -0.00325 0.02076 0.00454 HKLF 4 REM kskr38_a.res in P2(1)/n REM wR2 = 0.1023, GooF = S = 1.108, Restrained GooF = 1.037 for all data REM R1 = 0.0413 for 6555 Fo > 4sig(Fo) and 0.0422 for all 6767 data REM 702 parameters refined using 1325 restraints END WGHT 0.0376 2.9417 REM Highest difference peak 0.608, deepest hole -0.443, 1-sigma level 0.049 Q1 1 0.6650 0.6454 0.7125 11.00000 0.05 0.61 Q2 1 1.0295 0.8363 0.6775 11.00000 0.05 0.43 Q3 1 0.6836 0.5862 0.6018 11.00000 0.05 0.27 Q4 1 0.6048 0.5619 0.3802 11.00000 0.05 0.26 Q5 1 0.7182 0.6753 0.5822 11.00000 0.05 0.24 Q6 1 0.7712 0.5394 0.7458 11.00000 0.05 0.24 Q7 1 0.6175 0.6826 0.6748 11.00000 0.05 0.23 Q8 1 0.6363 0.6432 0.4465 11.00000 0.05 0.23 Q9 1 0.7154 0.5426 0.6324 11.00000 0.05 0.22 Q10 1 0.4354 0.7219 0.7079 11.00000 0.05 0.22 ; _shelx_res_checksum 5951 _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder' _olex2_submission_original_sample_id KSB_240727_SDc_KSKR38 _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 1.316 _oxdiff_exptl_absorpt_empirical_full_min 0.793 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 0.65425(3) 0.64834(2) 0.64377(3) 0.02692(10) Uani 1 1 d . . . . . N1 N 0.69268(17) 0.59007(6) 0.54415(16) 0.0313(4) Uani 1 1 d . . . . . N2 N 0.74770(17) 0.67714(5) 0.52610(13) 0.0277(3) Uani 1 1 d . . . . . N3 N 0.86656(17) 0.64810(5) 0.75290(14) 0.0290(3) Uani 1 1 d D . . . . N4 N 0.61831(17) 0.71721(5) 0.68854(14) 0.0284(3) Uani 1 1 d D . . . . C1 C 0.7119(3) 0.53166(8) 0.6869(2) 0.0473(6) Uani 1 1 d . . . . . H1A H 0.804915 0.543451 0.732655 0.071 Uiso 1 1 calc R U . . . H1B H 0.712725 0.498715 0.691410 0.071 Uiso 1 1 calc R U . . . H1C H 0.634864 0.543494 0.717370 0.071 Uiso 1 1 calc R U . . . C2 C 0.6862(2) 0.54574(7) 0.5648(2) 0.0362(5) Uani 1 1 d . . . . . C3 C 0.6557(2) 0.51476(7) 0.4736(2) 0.0428(5) Uani 1 1 d . . . . . H3 H 0.649980 0.483553 0.489017 0.051 Uiso 1 1 calc R U . . . C4 C 0.6337(2) 0.52954(8) 0.3613(2) 0.0444(5) Uani 1 1 d . . . . . H4 H 0.610104 0.508796 0.298828 0.053 Uiso 1 1 calc R U . . . C5 C 0.6465(2) 0.57443(8) 0.3412(2) 0.0416(5) Uani 1 1 d . . . . . H5 H 0.634975 0.585305 0.265019 0.050 Uiso 1 1 calc R U . . . C6 C 0.6769(2) 0.60393(7) 0.43487(18) 0.0335(4) Uani 1 1 d . . . . . C7 C 0.6897(3) 0.65357(7) 0.41499(18) 0.0396(5) Uani 1 1 d . . . . . H7A H 0.754456 0.658508 0.365023 0.048 Uiso 1 1 calc R U . . . H7B H 0.593783 0.665972 0.374931 0.048 Uiso 1 1 calc R U . . . C8 C 0.9052(2) 0.67004(7) 0.56849(18) 0.0325(4) Uani 1 1 d . . . . . H8A H 0.954922 0.696065 0.545206 0.039 Uiso 1 1 calc R U . . . H8B H 0.931097 0.642889 0.530894 0.039 Uiso 1 1 calc R U . . . C9 C 0.9586(2) 0.66445(6) 0.69703(18) 0.0293(4) Uani 1 1 d D . . . . C15 C 0.7104(2) 0.72571(7) 0.51800(18) 0.0347(4) Uani 1 1 d D . . . . H15A H 0.612229 0.729887 0.465877 0.042 Uiso 0.791(3) 1 calc R U P A 1 H15B H 0.778817 0.742360 0.485144 0.042 Uiso 0.791(3) 1 calc R U P A 1 H15C H 0.685169 0.735200 0.436027 0.042 Uiso 0.209(3) 1 calc R U P A 2 H15D H 0.795327 0.743403 0.560755 0.042 Uiso 0.209(3) 1 calc R U P A 2 O1 O 0.5186(3) 0.61942(8) 0.7212(2) 0.0284(5) Uani 0.690(2) 1 d D U P B 1 O2 O 0.4585(2) 0.64636(8) 0.5033(2) 0.0277(5) Uani 0.690(2) 1 d D U P B 1 O3 O 0.1604(7) 0.5725(3) 0.6003(4) 0.0292(10) Uani 0.690(2) 1 d D U P B 1 C23 C 0.3677(3) 0.62177(9) 0.5308(2) 0.0255(6) Uani 0.690(2) 1 d D U P B 1 C24 C 0.2409(3) 0.60500(10) 0.4464(3) 0.0282(6) Uani 0.690(2) 1 d D U P B 1 C25 C 0.1404(3) 0.58099(10) 0.4866(3) 0.0293(6) Uani 0.690(2) 1 d D U P B 1 C26 C 0.0151(6) 0.5637(2) 0.4117(5) 0.0348(10) Uani 0.690(2) 1 d D U P B 1 H26 H -0.053143 0.547763 0.440406 0.042 Uiso 0.690(2) 1 calc R U P B 1 C27 C -0.0074(9) 0.5704(3) 0.2945(6) 0.0450(14) Uani 0.690(2) 1 d D U P B 1 H27 H -0.093316 0.559542 0.242037 0.054 Uiso 0.690(2) 1 calc R U P B 1 C28 C 0.0955(4) 0.59310(13) 0.2517(3) 0.0426(8) Uani 0.690(2) 1 d D U P B 1 H28 H 0.079932 0.596457 0.170746 0.051 Uiso 0.690(2) 1 calc R U P B 1 C29 C 0.2175(6) 0.6103(2) 0.3262(4) 0.0356(11) Uani 0.690(2) 1 d D U P B 1 H29 H 0.286173 0.625841 0.297030 0.043 Uiso 0.690(2) 1 calc R U P B 1 C30 C 0.2868(3) 0.58417(9) 0.6820(2) 0.0277(6) Uani 0.690(2) 1 d D U P B 1 C31 C 0.2857(4) 0.56810(11) 0.7958(3) 0.0311(6) Uani 0.690(2) 1 d D U P B 1 C32 C 0.3991(9) 0.5784(4) 0.8943(5) 0.0358(10) Uani 0.690(2) 1 d D U P B 1 H32 H 0.478176 0.596130 0.887244 0.043 Uiso 0.690(2) 1 calc R U P B 1 C33 C 0.3946(5) 0.56262(14) 1.0017(3) 0.0469(9) Uani 0.690(2) 1 d D U P B 1 H33 H 0.470483 0.570126 1.068094 0.056 Uiso 0.690(2) 1 calc R U P B 1 C34 C 0.2818(5) 0.53615(14) 1.0141(3) 0.0526(9) Uani 0.690(2) 1 d D U P B 1 H34 H 0.281250 0.524979 1.087957 0.063 Uiso 0.690(2) 1 calc R U P B 1 C35 C 0.1708(7) 0.52626(19) 0.9184(5) 0.0509(12) Uani 0.690(2) 1 d D U P B 1 H35 H 0.092428 0.508437 0.926425 0.061 Uiso 0.690(2) 1 calc R U P B 1 C36 C 0.1715(6) 0.5417(3) 0.8114(5) 0.0435(13) Uani 0.690(2) 1 d D U P B 1 H36 H 0.093250 0.534496 0.746384 0.052 Uiso 0.690(2) 1 calc R U P B 1 C10 C 1.1001(5) 0.6732(3) 0.7625(4) 0.0308(12) Uani 0.690(2) 1 d D U P B 1 H10 H 1.166755 0.685716 0.725786 0.037 Uiso 0.690(2) 1 calc R U P B 1 C11 C 1.1445(5) 0.66408(17) 0.8793(4) 0.0323(11) Uani 0.690(2) 1 d D U P B 1 H11 H 1.240665 0.670199 0.923098 0.039 Uiso 0.690(2) 1 calc R U P B 1 C12 C 1.0474(5) 0.64603(16) 0.9310(4) 0.0330(10) Uani 0.690(2) 1 d D U P B 1 H12 H 1.076982 0.639153 1.011148 0.040 Uiso 0.690(2) 1 calc R U P B 1 C13 C 0.9058(5) 0.6376(2) 0.8675(3) 0.0302(10) Uani 0.690(2) 1 d D U P B 1 C14 C 0.7994(5) 0.61821(16) 0.9239(3) 0.0381(9) Uani 0.690(2) 1 d D U P B 1 H14A H 0.825556 0.586966 0.946321 0.057 Uiso 0.690(2) 1 calc R U P B 1 H14B H 0.702869 0.619066 0.869681 0.057 Uiso 0.690(2) 1 calc R U P B 1 H14C H 0.800038 0.635877 0.992828 0.057 Uiso 0.690(2) 1 calc R U P B 1 C16 C 0.7169(3) 0.74406(8) 0.6356(2) 0.0290(5) Uani 0.791(3) 1 d D U P A 1 H16A H 0.687029 0.776057 0.629055 0.035 Uiso 0.791(3) 1 calc R U P A 1 H16B H 0.817010 0.742340 0.685872 0.035 Uiso 0.791(3) 1 calc R U P A 1 C17 C 0.6627(3) 0.72447(9) 0.8169(2) 0.0368(6) Uani 0.791(3) 1 d D U P A 1 H17A H 0.766613 0.717504 0.847134 0.044 Uiso 0.791(3) 1 calc R U P A 1 H17B H 0.609114 0.703110 0.852785 0.044 Uiso 0.791(3) 1 calc R U P A 1 C18 C 0.6361(4) 0.77223(10) 0.8531(3) 0.0431(7) Uani 0.791(3) 1 d D U P A 1 H18A H 0.659924 0.773795 0.938465 0.052 Uiso 0.791(3) 1 calc R U P A 1 H18B H 0.700382 0.793365 0.827408 0.052 Uiso 0.791(3) 1 calc R U P A 1 C19 C 0.4800(4) 0.78644(13) 0.8015(3) 0.0442(8) Uani 0.791(3) 1 d D U P A 1 H19A H 0.416901 0.768905 0.837846 0.053 Uiso 0.791(3) 1 calc R U P A 1 H19B H 0.469188 0.818711 0.817871 0.053 Uiso 0.791(3) 1 calc R U P A 1 C20 C 0.4342(3) 0.77875(10) 0.6723(3) 0.0401(7) Uani 0.791(3) 1 d D U P A 1 H20A H 0.485187 0.800336 0.634697 0.048 Uiso 0.791(3) 1 calc R U P A 1 H20B H 0.329466 0.784410 0.642135 0.048 Uiso 0.791(3) 1 calc R U P A 1 C21 C 0.4672(3) 0.73097(9) 0.6417(3) 0.0376(6) Uani 0.791(3) 1 d D U P A 1 H21A H 0.405540 0.709909 0.670550 0.045 Uiso 0.791(3) 1 calc R U P A 1 H21B H 0.440859 0.728129 0.556507 0.045 Uiso 0.791(3) 1 calc R U P A 1 C22 C 0.3936(3) 0.60802(11) 0.6509(3) 0.0233(6) Uani 0.690(2) 1 d . U P B 1 O1A O 0.4520(5) 0.63989(18) 0.5567(5) 0.0259(10) Uani 0.310(2) 1 d D U P B 2 O2A O 0.5686(5) 0.62010(17) 0.7774(5) 0.0287(10) Uani 0.310(2) 1 d D U P B 2 O3A O 0.1651(16) 0.5754(7) 0.6242(10) 0.033(2) Uani 0.310(2) 1 d D U P B 2 C23A C 0.4405(7) 0.6080(2) 0.7332(5) 0.0253(11) Uani 0.310(2) 1 d D U P B 2 C24A C 0.3572(7) 0.5844(2) 0.7975(6) 0.0316(12) Uani 0.310(2) 1 d D U P B 2 C25A C 0.2197(7) 0.5694(2) 0.7382(6) 0.0337(13) Uani 0.310(2) 1 d D U P B 2 C26A C 0.1346(13) 0.5464(6) 0.7949(11) 0.039(2) Uani 0.310(2) 1 d D U P B 2 H26A H 0.042300 0.535509 0.753437 0.047 Uiso 0.310(2) 1 calc R U P B 2 C27A C 0.1855(14) 0.5396(4) 0.9125(11) 0.047(2) Uani 0.310(2) 1 d D U P B 2 H27A H 0.125528 0.524974 0.952077 0.057 Uiso 0.310(2) 1 calc R U P B 2 C28A C 0.3248(10) 0.5538(3) 0.9755(8) 0.0471(16) Uani 0.310(2) 1 d D U P B 2 H28A H 0.361183 0.547514 1.055667 0.057 Uiso 0.310(2) 1 calc R U P B 2 C29A C 0.405(2) 0.5768(9) 0.9169(10) 0.038(2) Uani 0.310(2) 1 d D U P B 2 H29A H 0.496978 0.588117 0.958664 0.046 Uiso 0.310(2) 1 calc R U P B 2 C30A C 0.2437(6) 0.5966(2) 0.5589(5) 0.0273(11) Uani 0.310(2) 1 d D U P B 2 C31A C 0.1741(8) 0.5923(2) 0.4370(6) 0.0295(13) Uani 0.310(2) 1 d D U P B 2 C32A C 0.2428(13) 0.6054(5) 0.3533(8) 0.033(2) Uani 0.310(2) 1 d D U P B 2 H32A H 0.332554 0.620683 0.377499 0.040 Uiso 0.310(2) 1 calc R U P B 2 C33A C 0.1839(8) 0.5968(2) 0.2368(6) 0.0388(15) Uani 0.310(2) 1 d D U P B 2 H33A H 0.234509 0.605458 0.182758 0.047 Uiso 0.310(2) 1 calc R U P B 2 C34A C 0.0518(7) 0.5756(3) 0.1988(7) 0.0422(16) Uani 0.310(2) 1 d D U P B 2 H34A H 0.011976 0.569081 0.119077 0.051 Uiso 0.310(2) 1 calc R U P B 2 C35A C -0.0211(19) 0.5640(8) 0.2775(11) 0.038(2) Uani 0.310(2) 1 d D U P B 2 H35A H -0.113729 0.550611 0.251394 0.045 Uiso 0.310(2) 1 calc R U P B 2 C36A C 0.0374(12) 0.5716(5) 0.3933(10) 0.033(2) Uani 0.310(2) 1 d D U P B 2 H36A H -0.015024 0.562652 0.445790 0.039 Uiso 0.310(2) 1 calc R U P B 2 C10A C 1.1037(9) 0.6770(6) 0.7303(10) 0.028(2) Uani 0.310(2) 1 d D U P B 2 H10A H 1.152422 0.689145 0.678410 0.033 Uiso 0.310(2) 1 calc R U P B 2 C11A C 1.1689(12) 0.6700(4) 0.8458(9) 0.031(2) Uani 0.310(2) 1 d D U P B 2 H11A H 1.268576 0.676276 0.877389 0.037 Uiso 0.310(2) 1 calc R U P B 2 C12A C 1.0891(10) 0.6541(3) 0.9144(9) 0.031(2) Uani 0.310(2) 1 d D U P B 2 H12A H 1.132966 0.649375 0.994396 0.037 Uiso 0.310(2) 1 calc R U P B 2 C13A C 0.9427(11) 0.6447(5) 0.8676(7) 0.031(2) Uani 0.310(2) 1 d D U P B 2 C14A C 0.8544(11) 0.6275(4) 0.9434(9) 0.044(2) Uani 0.310(2) 1 d D U P B 2 H14D H 0.770790 0.647174 0.936049 0.066 Uiso 0.310(2) 1 calc R U P B 2 H14E H 0.913238 0.627206 1.023975 0.066 Uiso 0.310(2) 1 calc R U P B 2 H14F H 0.821310 0.596884 0.919700 0.066 Uiso 0.310(2) 1 calc R U P B 2 C16A C 0.5875(9) 0.7353(3) 0.5662(7) 0.037(2) Uani 0.209(3) 1 d D U P A 2 H16C H 0.499034 0.721021 0.517079 0.044 Uiso 0.209(3) 1 calc R U P A 2 H16D H 0.571095 0.768158 0.566424 0.044 Uiso 0.209(3) 1 calc R U P A 2 C17A C 0.7274(10) 0.7387(3) 0.7796(8) 0.0355(19) Uani 0.209(3) 1 d D U P A 2 H17C H 0.820140 0.738574 0.759305 0.043 Uiso 0.209(3) 1 calc R U P A 2 H17D H 0.740710 0.721503 0.852132 0.043 Uiso 0.209(3) 1 calc R U P A 2 C18A C 0.6866(11) 0.7869(3) 0.7985(10) 0.0375(19) Uani 0.209(3) 1 d D U P A 2 H18C H 0.763848 0.800826 0.860681 0.045 Uiso 0.209(3) 1 calc R U P A 2 H18D H 0.676739 0.804524 0.726862 0.045 Uiso 0.209(3) 1 calc R U P A 2 C19A C 0.5457(11) 0.7884(5) 0.8313(11) 0.040(2) Uani 0.209(3) 1 d D U P A 2 H19C H 0.556302 0.771811 0.904511 0.047 Uiso 0.209(3) 1 calc R U P A 2 H19D H 0.520476 0.819973 0.843083 0.047 Uiso 0.209(3) 1 calc R U P A 2 C20A C 0.4269(11) 0.7672(3) 0.7361(13) 0.0427(19) Uani 0.209(3) 1 d D U P A 2 H20C H 0.408957 0.785636 0.665120 0.051 Uiso 0.209(3) 1 calc R U P A 2 H20D H 0.336716 0.765930 0.760055 0.051 Uiso 0.209(3) 1 calc R U P A 2 C21A C 0.4718(9) 0.7194(3) 0.7117(12) 0.0376(19) Uani 0.209(3) 1 d D U P A 2 H21C H 0.472991 0.700027 0.778845 0.045 Uiso 0.209(3) 1 calc R U P A 2 H21D H 0.398546 0.707181 0.643957 0.045 Uiso 0.209(3) 1 calc R U P A 2 C22A C 0.3763(9) 0.6164(3) 0.6084(8) 0.0233(6) Uani 0.310(2) 1 d . U P B 2 Cl1 Cl 1.02444(5) 0.81716(2) 0.61847(4) 0.03028(11) Uani 1 1 d . . . . . O4 O 1.14043(16) 0.84891(5) 0.63413(13) 0.0400(4) Uani 1 1 d . . . . . O5 O 0.98185(19) 0.80246(7) 0.50073(15) 0.0519(4) Uani 1 1 d . . . . . O6 O 1.07050(18) 0.77905(5) 0.69277(16) 0.0500(4) Uani 1 1 d . . . . . O7 O 0.90441(17) 0.83818(6) 0.64635(15) 0.0442(4) 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 0.01936(16) 0.02492(17) 0.03656(19) 0.00110(13) 0.00785(13) -0.00225(12) N1 0.0217(7) 0.0260(8) 0.0440(10) -0.0035(7) 0.0051(7) -0.0017(6) N2 0.0320(8) 0.0257(8) 0.0245(8) -0.0010(6) 0.0062(6) -0.0015(6) N3 0.0280(8) 0.0291(8) 0.0273(8) -0.0008(6) 0.0034(6) 0.0037(6) N4 0.0265(8) 0.0271(8) 0.0344(9) 0.0016(7) 0.0130(7) 0.0005(6) C1 0.0505(14) 0.0305(11) 0.0624(16) 0.0055(10) 0.0183(12) -0.0001(10) C2 0.0248(9) 0.0284(10) 0.0559(13) 0.0015(9) 0.0123(9) 0.0002(8) C3 0.0313(11) 0.0257(10) 0.0730(17) -0.0084(10) 0.0174(11) -0.0016(8) C4 0.0338(11) 0.0388(12) 0.0587(15) -0.0163(11) 0.0093(10) -0.0028(9) C5 0.0368(11) 0.0382(12) 0.0435(12) -0.0118(10) 0.0004(9) 0.0009(9) C6 0.0281(9) 0.0336(10) 0.0335(10) -0.0052(8) -0.0005(8) 0.0004(8) C7 0.0541(13) 0.0334(11) 0.0253(10) -0.0028(8) 0.0007(9) 0.0021(9) C8 0.0302(10) 0.0350(10) 0.0364(11) -0.0040(8) 0.0160(8) -0.0049(8) C9 0.0223(9) 0.0246(9) 0.0394(11) -0.0063(8) 0.0056(8) 0.0007(7) C15 0.0480(12) 0.0247(9) 0.0332(10) 0.0028(8) 0.0141(9) 0.0007(9) O1 0.0257(13) 0.0344(11) 0.0245(12) 0.0016(10) 0.0059(10) -0.0058(10) O2 0.0230(10) 0.0303(11) 0.0285(13) 0.0012(10) 0.0051(10) -0.0041(8) O3 0.0230(14) 0.0331(19) 0.0325(18) -0.0039(17) 0.0092(13) -0.0065(11) C23 0.0218(13) 0.0255(13) 0.0292(15) 0.0005(11) 0.0072(10) 0.0013(11) C24 0.0242(14) 0.0253(14) 0.0335(16) -0.0003(11) 0.0054(12) -0.0008(11) C25 0.0249(13) 0.0280(14) 0.0335(15) -0.0013(12) 0.0057(11) -0.0001(11) C26 0.0258(19) 0.034(2) 0.043(2) -0.0015(16) 0.0058(15) -0.0072(14) C27 0.035(2) 0.044(3) 0.046(2) -0.004(2) -0.006(2) -0.0077(18) C28 0.0430(19) 0.0446(18) 0.0324(16) 0.0019(14) -0.0026(15) -0.0085(16) C29 0.035(2) 0.035(2) 0.034(2) 0.0042(18) 0.0049(18) -0.0044(18) C30 0.0244(12) 0.0267(12) 0.0319(13) -0.0037(10) 0.0074(10) -0.0027(10) C31 0.0357(17) 0.0262(14) 0.0355(16) -0.0039(13) 0.0169(14) -0.0043(13) C32 0.039(2) 0.037(2) 0.035(2) 0.001(2) 0.0167(19) -0.0084(17) C33 0.061(2) 0.046(2) 0.0344(18) -0.0013(15) 0.0137(17) -0.0166(18) C34 0.076(2) 0.051(2) 0.0382(17) 0.0032(15) 0.0276(17) -0.0190(18) C35 0.062(2) 0.050(3) 0.048(2) -0.003(2) 0.0262(17) -0.023(2) C36 0.047(3) 0.044(3) 0.043(2) -0.0061(18) 0.0183(19) -0.015(2) C10 0.0256(17) 0.030(2) 0.036(3) -0.004(2) 0.0071(16) -0.0017(13) C11 0.026(2) 0.032(2) 0.034(3) -0.0034(19) -0.0002(17) 0.0002(17) C12 0.033(2) 0.033(2) 0.0273(17) -0.0007(13) -0.0007(15) -0.0003(16) C13 0.029(2) 0.028(2) 0.0295(17) -0.0005(13) 0.0027(14) -0.0005(17) C14 0.041(2) 0.047(2) 0.0238(18) 0.0058(15) 0.0035(17) -0.0081(19) C16 0.0304(12) 0.0236(11) 0.0359(13) 0.0003(9) 0.0142(10) -0.0036(9) C17 0.0433(15) 0.0355(14) 0.0350(13) 0.0012(11) 0.0163(12) 0.0050(12) C18 0.0543(18) 0.0412(15) 0.0369(14) -0.0028(12) 0.0178(13) 0.0067(14) C19 0.048(2) 0.0406(16) 0.052(2) 0.0028(15) 0.0283(17) 0.0126(17) C20 0.0336(14) 0.0346(14) 0.0556(18) 0.0037(13) 0.0178(13) 0.0087(11) C21 0.0258(12) 0.0332(14) 0.0541(17) 0.0010(13) 0.0116(12) 0.0020(10) C22 0.0208(11) 0.0243(13) 0.0254(18) -0.0006(12) 0.0074(14) -0.0019(10) O1A 0.018(2) 0.029(2) 0.030(3) -0.001(2) 0.008(2) -0.0024(18) O2A 0.023(2) 0.033(2) 0.029(3) 0.002(2) 0.005(2) -0.0029(18) O3A 0.027(3) 0.031(3) 0.042(4) -0.008(4) 0.012(3) -0.005(2) C23A 0.021(2) 0.026(2) 0.030(3) -0.002(2) 0.009(2) -0.002(2) C24A 0.032(3) 0.027(3) 0.039(3) -0.004(2) 0.014(2) -0.003(2) C25A 0.031(3) 0.029(3) 0.046(3) -0.006(2) 0.018(2) -0.005(2) C26A 0.043(4) 0.033(4) 0.048(4) -0.001(3) 0.024(3) -0.012(4) C27A 0.056(4) 0.040(4) 0.054(4) 0.000(4) 0.029(3) -0.016(4) C28A 0.055(3) 0.044(3) 0.046(3) 0.002(3) 0.020(3) -0.016(3) C29A 0.044(4) 0.036(4) 0.037(4) 0.000(4) 0.013(3) -0.011(3) C30A 0.019(2) 0.025(2) 0.037(2) -0.004(2) 0.0064(19) -0.0020(18) C31A 0.020(3) 0.025(3) 0.040(3) -0.004(2) 0.004(3) -0.004(2) C32A 0.024(3) 0.033(4) 0.036(4) -0.004(3) -0.004(3) -0.008(3) C33A 0.034(3) 0.038(3) 0.036(3) 0.000(3) -0.003(3) -0.010(3) C34A 0.036(3) 0.039(3) 0.041(3) -0.001(3) -0.007(3) -0.006(3) C35A 0.029(4) 0.034(4) 0.044(4) -0.004(3) -0.001(3) -0.008(3) C36A 0.023(3) 0.031(4) 0.044(4) -0.003(3) 0.008(3) -0.008(3) C10A 0.016(3) 0.023(4) 0.039(5) -0.005(4) 0.000(3) -0.002(2) C11A 0.024(3) 0.028(3) 0.036(4) -0.003(3) 0.002(3) -0.001(3) C12A 0.027(4) 0.030(4) 0.030(4) 0.000(3) 0.001(3) -0.002(3) C13A 0.030(4) 0.031(4) 0.032(3) 0.002(3) 0.007(3) 0.000(3) C14A 0.036(5) 0.052(5) 0.037(5) 0.005(4) -0.003(4) -0.008(4) C16A 0.036(4) 0.024(4) 0.046(5) 0.000(4) 0.003(4) -0.001(3) C17A 0.040(4) 0.029(4) 0.037(4) -0.002(3) 0.011(3) -0.002(3) C18A 0.042(4) 0.031(4) 0.042(4) -0.001(3) 0.015(3) 0.002(3) C19A 0.041(4) 0.036(4) 0.048(4) 0.000(3) 0.021(4) 0.006(4) C20A 0.033(4) 0.039(4) 0.059(4) 0.002(4) 0.017(4) 0.008(3) C21A 0.029(4) 0.033(4) 0.055(4) -0.004(4) 0.019(3) 0.004(3) C22A 0.0208(11) 0.0243(13) 0.0254(18) -0.0006(12) 0.0074(14) -0.0019(10) Cl1 0.0253(2) 0.0315(2) 0.0305(2) -0.00101(17) 0.00156(17) 0.00160(17) O4 0.0360(8) 0.0405(9) 0.0412(8) 0.0042(7) 0.0067(7) -0.0080(6) O5 0.0451(9) 0.0679(12) 0.0384(9) -0.0189(8) 0.0047(7) 0.0011(8) O6 0.0412(9) 0.0357(8) 0.0628(11) 0.0149(8) -0.0029(8) -0.0029(7) O7 0.0408(9) 0.0440(9) 0.0525(10) -0.0032(7) 0.0208(7) 0.0045(7) 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 0.0723 0 1 0 0.0670 -1 0 0 0.2373 1 0 0 0.1757 0 0 1 0.2357 0 0 -1 0.2054 -2 -1 2 0.3028 2 1 -2 0.2530 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 77.31(6) . . ? N2 Ni1 N3 84.01(7) . . ? N2 Ni1 N4 84.80(6) . . ? N2 Ni1 O2 85.82(8) . . ? N2 Ni1 O2A 175.85(16) . . ? N3 Ni1 N1 93.23(6) . . ? N3 Ni1 N4 92.46(6) . . ? N3 Ni1 O2 167.89(8) . . ? N3 Ni1 O2A 92.29(15) . . ? N4 Ni1 N1 160.54(7) . . ? N4 Ni1 O2A 93.49(14) . . ? O1 Ni1 N1 98.45(8) . . ? O1 Ni1 N2 164.83(9) . . ? O1 Ni1 N3 110.92(9) . . ? O1 Ni1 N4 96.86(8) . . ? O1 Ni1 O2 79.04(10) . . ? O2 Ni1 N1 78.10(8) . . ? O2 Ni1 N4 93.15(8) . . ? O1A Ni1 N1 84.27(16) . . ? O1A Ni1 N2 104.19(18) . . ? O1A Ni1 N3 170.61(18) . . ? O1A Ni1 N4 92.85(16) . . ? O1A Ni1 O2A 79.6(2) . . ? O2A Ni1 N1 104.86(14) . . ? C2 N1 Ni1 130.41(15) . . ? C2 N1 C6 118.76(19) . . ? C6 N1 Ni1 107.58(13) . . ? C7 N2 Ni1 107.28(13) . . ? C7 N2 C8 109.99(16) . . ? C7 N2 C15 112.15(16) . . ? C8 N2 Ni1 107.82(12) . . ? C8 N2 C15 111.64(16) . . ? C15 N2 Ni1 107.74(12) . . ? C9 N3 Ni1 110.49(13) . . ? C9 N3 C13 123.5(2) . . ? C9 N3 C13A 106.5(5) . . ? C13 N3 Ni1 125.7(2) . . ? C13A N3 Ni1 141.6(5) . . ? C16 N4 Ni1 103.36(12) . . ? C17 N4 Ni1 111.82(13) . . ? C17 N4 C16 108.89(18) . . ? C21 N4 Ni1 112.14(14) . . ? C21 N4 C16 111.42(19) . . ? C21 N4 C17 109.1(2) . . ? C16A N4 Ni1 95.4(4) . . ? C17A N4 Ni1 118.3(4) . . ? C17A N4 C16A 119.2(6) . . ? C17A N4 C21A 111.3(6) . . ? C21A N4 Ni1 107.9(4) . . ? C21A N4 C16A 102.7(6) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C2 C1 117.1(2) . . ? N1 C2 C3 120.6(2) . . ? C3 C2 C1 122.2(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 C2 120.0(2) . . ? C4 C3 H3 120.0 . . ? C3 C4 H4 120.5 . . ? C5 C4 C3 119.1(2) . . ? C5 C4 H4 120.5 . . ? C4 C5 H5 120.7 . . ? C4 C5 C6 118.7(2) . . ? C6 C5 H5 120.7 . . ? N1 C6 C5 122.7(2) . . ? N1 C6 C7 117.58(18) . . ? C5 C6 C7 119.7(2) . . ? N2 C7 C6 110.36(17) . . ? N2 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C6 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N2 C8 H8A 108.8 . . ? N2 C8 H8B 108.8 . . ? N2 C8 C9 113.60(15) . . ? H8A C8 H8B 107.7 . . ? C9 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? N3 C9 C8 118.01(16) . . ? N3 C9 C10 117.5(3) . . ? N3 C9 C10A 134.6(5) . . ? C10 C9 C8 124.4(3) . . ? C10A C9 C8 107.4(5) . . ? N2 C15 H15A 109.6 . . ? N2 C15 H15B 109.6 . . ? N2 C15 H15C 109.3 . . ? N2 C15 H15D 109.3 . . ? N2 C15 C16 110.15(17) . . ? N2 C15 C16A 111.4(4) . . ? H15A C15 H15B 108.1 . . ? H15C C15 H15D 108.0 . . ? C16 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C16A C15 H15C 109.3 . . ? C16A C15 H15D 109.3 . . ? C22 O1 Ni1 114.4(2) . . ? C23 O2 Ni1 109.4(2) . . ? C25 O3 C30 121.6(4) . . ? O2 C23 C24 122.1(3) . . ? O2 C23 C22 119.0(3) . . ? C24 C23 C22 118.8(3) . . ? C25 C24 C23 117.8(3) . . ? C25 C24 C29 118.9(4) . . ? C29 C24 C23 123.2(4) . . ? O3 C25 C24 121.9(3) . . ? O3 C25 C26 116.3(4) . . ? C26 C25 C24 121.8(3) . . ? C25 C26 H26 120.9 . . ? C27 C26 C25 118.2(5) . . ? C27 C26 H26 120.9 . . ? C26 C27 H27 119.5 . . ? C26 C27 C28 120.9(5) . . ? C28 C27 H27 119.5 . . ? C27 C28 H28 119.8 . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C24 C29 H29 120.1 . . ? C28 C29 C24 119.7(5) . . ? C28 C29 H29 120.1 . . ? O3 C30 C31 110.7(3) . . ? O3 C30 C22 120.8(3) . . ? C22 C30 C31 128.5(3) . . ? C32 C31 C30 121.1(4) . . ? C36 C31 C30 121.2(4) . . ? C36 C31 C32 117.7(4) . . ? C31 C32 H32 120.2 . . ? C33 C32 C31 119.7(6) . . ? C33 C32 H32 120.2 . . ? C32 C33 H33 119.3 . . ? C34 C33 C32 121.3(5) . . ? C34 C33 H33 119.3 . . ? C33 C34 H34 120.5 . . ? C35 C34 C33 119.1(4) . . ? C35 C34 H34 120.5 . . ? C34 C35 H35 119.5 . . ? C36 C35 C34 120.9(5) . . ? C36 C35 H35 119.5 . . ? C31 C36 H36 119.4 . . ? C35 C36 C31 121.3(5) . . ? C35 C36 H36 119.4 . . ? C9 C10 H10 119.4 . . ? C11 C10 C9 121.2(4) . . ? C11 C10 H10 119.4 . . ? C10 C11 H11 120.6 . . ? C12 C11 C10 118.8(4) . . ? C12 C11 H11 120.6 . . ? C11 C12 H12 119.6 . . ? C11 C12 C13 120.8(4) . . ? C13 C12 H12 119.6 . . ? N3 C13 C12 118.2(4) . . ? N3 C13 C14 121.0(3) . . ? C12 C13 C14 120.9(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C16 H16A 109.7 . . ? N4 C16 H16B 109.7 . . ? C15 C16 N4 109.78(18) . . ? C15 C16 H16A 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? N4 C17 H17A 108.8 . . ? N4 C17 H17B 108.8 . . ? N4 C17 C18 113.9(2) . . ? H17A C17 H17B 107.7 . . ? C18 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? 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 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C20 C19 C18 110.7(3) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? C19 C20 H20A 109.3 . . ? C19 C20 H20B 109.3 . . ? C19 C20 C21 111.6(3) . . ? H20A C20 H20B 108.0 . . ? C21 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? N4 C21 C20 114.7(2) . . ? N4 C21 H21A 108.6 . . ? N4 C21 H21B 108.6 . . ? C20 C21 H21A 108.6 . . ? C20 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? O1 C22 C23 116.3(3) . . ? O1 C22 C30 125.3(3) . . ? C30 C22 C23 118.4(3) . . ? C22A O1A Ni1 115.1(5) . . ? C23A O2A Ni1 109.1(5) . . ? C25A O3A C30A 121.3(9) . . ? O2A C23A C24A 122.7(6) . . ? O2A C23A C22A 118.1(6) . . ? C24A C23A C22A 119.1(6) . . ? C25A C24A C23A 118.3(6) . . ? C25A C24A C29A 118.2(9) . . ? C29A C24A C23A 123.5(8) . . ? O3A C25A C24A 122.1(7) . . ? O3A C25A C26A 116.8(8) . . ? C26A C25A C24A 121.1(8) . . ? C25A C26A H26A 120.5 . . ? C27A C26A C25A 119.1(11) . . ? C27A C26A H26A 120.5 . . ? C26A C27A H27A 119.2 . . ? C26A C27A C28A 121.6(11) . . ? C28A C27A H27A 119.2 . . ? C27A C28A H28A 121.2 . . ? C29A C28A C27A 117.6(11) . . ? C29A C28A H28A 121.2 . . ? C24A C29A H29A 118.9 . . ? C28A C29A C24A 122.3(13) . . ? C28A C29A H29A 118.9 . . ? O3A C30A C31A 111.2(7) . . ? O3A C30A C22A 122.3(8) . . ? C22A C30A C31A 126.3(7) . . ? C32A C31A C30A 121.7(7) . . ? C32A C31A C36A 115.3(8) . . ? C36A C31A C30A 122.8(8) . . ? C31A C32A H32A 118.9 . . ? C33A C32A C31A 122.2(10) . . ? C33A C32A H32A 118.9 . . ? C32A C33A H33A 119.9 . . ? C34A C33A C32A 120.2(9) . . ? C34A C33A H33A 119.9 . . ? C33A C34A H34A 120.4 . . ? C35A C34A C33A 119.2(9) . . ? C35A C34A H34A 120.4 . . ? C34A C35A H35A 119.5 . . ? C34A C35A C36A 121.1(12) . . ? C36A C35A H35A 119.5 . . ? C31A C36A H36A 119.0 . . ? C35A C36A C31A 121.9(10) . . ? C35A C36A H36A 119.0 . . ? C9 C10A H10A 123.4 . . ? C11A C10A C9 113.1(9) . . ? C11A C10A H10A 123.4 . . ? C10A C11A H11A 120.4 . . ? C12A C11A C10A 119.2(9) . . ? C12A C11A H11A 120.4 . . ? C11A C12A H12A 119.9 . . ? C11A C12A C13A 120.3(9) . . ? C13A C12A H12A 119.9 . . ? N3 C13A C12A 126.2(8) . . ? N3 C13A C14A 113.5(8) . . ? C12A C13A C14A 120.3(7) . . ? C13A C14A H14D 109.5 . . ? C13A C14A H14E 109.5 . . ? C13A C14A H14F 109.5 . . ? H14D C14A H14E 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? N4 C16A H16C 109.6 . . ? N4 C16A H16D 109.6 . . ? C15 C16A N4 110.3(5) . . ? C15 C16A H16C 109.6 . . ? C15 C16A H16D 109.6 . . ? H16C C16A H16D 108.1 . . ? N4 C17A H17C 109.3 . . ? N4 C17A H17D 109.3 . . ? N4 C17A C18A 111.5(7) . . ? H17C C17A H17D 108.0 . . ? C18A C17A H17C 109.3 . . ? C18A C17A H17D 109.3 . . ? C17A C18A H18C 109.5 . . ? C17A C18A H18D 109.5 . . ? H18C C18A H18D 108.1 . . ? C19A C18A C17A 110.7(9) . . ? C19A C18A H18C 109.5 . . ? C19A C18A H18D 109.5 . . ? C18A C19A H19C 109.7 . . ? C18A C19A H19D 109.7 . . ? H19C C19A H19D 108.2 . . ? C20A C19A C18A 109.7(10) . . ? C20A C19A H19C 109.7 . . ? C20A C19A H19D 109.7 . . ? C19A C20A H20C 109.8 . . ? C19A C20A H20D 109.8 . . ? C19A C20A C21A 109.5(9) . . ? H20C C20A H20D 108.2 . . ? C21A C20A H20C 109.8 . . ? C21A C20A H20D 109.8 . . ? N4 C21A C20A 113.7(7) . . ? N4 C21A H21C 108.8 . . ? N4 C21A H21D 108.8 . . ? C20A C21A H21C 108.8 . . ? C20A C21A H21D 108.8 . . ? H21C C21A H21D 107.7 . . ? O1A C22A C23A 116.5(7) . . ? O1A C22A C30A 127.0(8) . . ? C30A C22A C23A 116.4(7) . . ? O5 Cl1 O4 109.35(11) . . ? O5 Cl1 O6 109.39(12) . . ? O5 Cl1 O7 109.52(10) . . ? O6 Cl1 O4 109.86(9) . . ? O7 Cl1 O4 109.50(10) . . ? O7 Cl1 O6 109.21(11) . . ? 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 2.1947(17) . ? Ni1 N2 2.0629(16) . ? Ni1 N3 2.1077(16) . ? Ni1 N4 2.1680(17) . ? Ni1 O1 1.998(2) . ? Ni1 O2 2.162(2) . ? Ni1 O1A 1.961(5) . ? Ni1 O2A 2.169(5) . ? N1 C2 1.345(3) . ? N1 C6 1.347(3) . ? N2 C7 1.477(3) . ? N2 C8 1.480(3) . ? N2 C15 1.484(2) . ? N3 C9 1.344(3) . ? N3 C13 1.362(4) . ? N3 C13A 1.378(7) . ? N4 C16 1.510(3) . ? N4 C17 1.501(3) . ? N4 C21 1.469(3) . ? N4 C16A 1.518(8) . ? N4 C17A 1.443(7) . ? N4 C21A 1.517(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.482(3) . ? C2 C3 1.400(3) . ? C3 H3 0.9500 . ? C3 C4 1.382(4) . ? C4 H4 0.9500 . ? C4 C5 1.367(3) . ? C5 H5 0.9500 . ? C5 C6 1.394(3) . ? C6 C7 1.505(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.500(3) . ? C9 C10 1.401(4) . ? C9 C10A 1.397(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 H15C 0.9900 . ? C15 H15D 0.9900 . ? C15 C16 1.503(3) . ? C15 C16A 1.485(8) . ? O1 C22 1.314(4) . ? O2 C23 1.254(4) . ? O3 C25 1.353(6) . ? O3 C30 1.384(5) . ? C23 C24 1.448(4) . ? C23 C22 1.455(4) . ? C24 C25 1.393(4) . ? C24 C29 1.411(6) . ? C25 C26 1.393(6) . ? C26 H26 0.9500 . ? C26 C27 1.381(8) . ? C27 H27 0.9500 . ? C27 C28 1.410(8) . ? C28 H28 0.9500 . ? C28 C29 1.368(7) . ? C29 H29 0.9500 . ? C30 C31 1.453(4) . ? C30 C22 1.385(4) . ? C31 C32 1.408(7) . ? C31 C36 1.407(7) . ? C32 H32 0.9500 . ? C32 C33 1.388(6) . ? C33 H33 0.9500 . ? C33 C34 1.384(5) . ? C34 H34 0.9500 . ? C34 C35 1.372(7) . ? C35 H35 0.9500 . ? C35 C36 1.369(8) . ? C36 H36 0.9500 . ? C10 H10 0.9500 . ? C10 C11 1.380(6) . ? C11 H11 0.9500 . ? C11 C12 1.369(6) . ? C12 H12 0.9500 . ? C12 C13 1.393(5) . ? C13 C14 1.494(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.527(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.523(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.513(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.522(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? O1A C22A 1.288(11) . ? O2A C23A 1.256(7) . ? O3A C25A 1.341(11) . ? O3A C30A 1.385(9) . ? C23A C24A 1.442(8) . ? C23A C22A 1.480(10) . ? C24A C25A 1.396(7) . ? C24A C29A 1.402(10) . ? C25A C26A 1.384(10) . ? C26A H26A 0.9500 . ? C26A C27A 1.379(12) . ? C27A H27A 0.9500 . ? C27A C28A 1.414(11) . ? C28A H28A 0.9500 . ? C28A C29A 1.368(12) . ? C29A H29A 0.9500 . ? C30A C31A 1.442(7) . ? C30A C22A 1.385(10) . ? C31A C32A 1.404(11) . ? C31A C36A 1.419(10) . ? C32A H32A 0.9500 . ? C32A C33A 1.385(9) . ? C33A H33A 0.9500 . ? C33A C34A 1.383(8) . ? C34A H34A 0.9500 . ? C34A C35A 1.370(12) . ? C35A H35A 0.9500 . ? C35A C36A 1.370(12) . ? C36A H36A 0.9500 . ? C10A H10A 0.9500 . ? C10A C11A 1.375(9) . ? C11A H11A 0.9500 . ? C11A C12A 1.360(9) . ? C12A H12A 0.9500 . ? C12A C13A 1.398(9) . ? C13A C14A 1.499(9) . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C16A H16C 0.9900 . ? C16A H16D 0.9900 . ? C17A H17C 0.9900 . ? C17A H17D 0.9900 . ? C17A C18A 1.519(8) . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C18A C19A 1.517(8) . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? C19A C20A 1.516(8) . ? C20A H20C 0.9900 . ? C20A H20D 0.9900 . ? C20A C21A 1.534(8) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? Cl1 O4 1.4360(15) . ? Cl1 O5 1.4309(17) . ? Cl1 O6 1.4352(16) . ? Cl1 O7 1.4349(16) . ? 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 C2 C1 -26.3(3) . . . . ? Ni1 N1 C2 C3 153.35(16) . . . . ? Ni1 N1 C6 C5 -158.24(17) . . . . ? Ni1 N1 C6 C7 20.3(2) . . . . ? Ni1 N2 C7 C6 -39.6(2) . . . . ? Ni1 N2 C8 C9 -25.71(19) . . . . ? Ni1 N2 C15 C16 39.6(2) . . . . ? Ni1 N2 C15 C16A -17.0(4) . . . . ? Ni1 N3 C9 C8 -12.6(2) . . . . ? Ni1 N3 C9 C10 170.1(4) . . . . ? Ni1 N3 C9 C10A 170.3(11) . . . . ? Ni1 N3 C13 C12 -169.9(3) . . . . ? Ni1 N3 C13 C14 9.3(7) . . . . ? Ni1 N3 C13A C12A -167.4(7) . . . . ? Ni1 N3 C13A C14A 15.0(19) . . . . ? Ni1 N4 C16 C15 41.4(2) . . . . ? Ni1 N4 C17 C18 -178.6(2) . . . . ? Ni1 N4 C21 C20 178.8(2) . . . . ? Ni1 N4 C16A C15 -56.9(6) . . . . ? Ni1 N4 C17A C18A 179.0(6) . . . . ? Ni1 N4 C21A C20A -175.8(9) . . . . ? Ni1 O1 C22 C23 -5.6(4) . . . . ? Ni1 O1 C22 C30 174.2(3) . . . . ? Ni1 O2 C23 C24 -164.6(2) . . . . ? Ni1 O2 C23 C22 12.7(3) . . . . ? Ni1 O1A C22A C23A 13.4(9) . . . . ? Ni1 O1A C22A C30A -163.8(6) . . . . ? Ni1 O2A C23A C24A 174.6(5) . . . . ? Ni1 O2A C23A C22A -2.1(7) . . . . ? N1 C2 C3 C4 0.9(3) . . . . ? N1 C6 C7 N2 11.6(3) . . . . ? N2 C8 C9 N3 26.8(3) . . . . ? N2 C8 C9 C10 -156.1(5) . . . . ? N2 C8 C9 C10A -155.3(9) . . . . ? N2 C15 C16 N4 -56.4(2) . . . . ? N2 C15 C16A N4 53.9(7) . . . . ? N3 C9 C10 C11 2.0(9) . . . . ? N3 C9 C10A C11A 2(2) . . . . ? N4 C17 C18 C19 54.1(3) . . . . ? N4 C17A C18A C19A 59.8(12) . . . . ? C1 C2 C3 C4 -179.5(2) . . . . ? C2 N1 C6 C5 3.5(3) . . . . ? C2 N1 C6 C7 -177.92(19) . . . . ? C2 C3 C4 C5 1.9(3) . . . . ? C3 C4 C5 C6 -2.0(3) . . . . ? C4 C5 C6 N1 -0.7(3) . . . . ? C4 C5 C6 C7 -179.3(2) . . . . ? C5 C6 C7 N2 -169.73(19) . . . . ? C6 N1 C2 C1 176.83(19) . . . . ? C6 N1 C2 C3 -3.5(3) . . . . ? C7 N2 C8 C9 -142.39(17) . . . . ? C7 N2 C15 C16 157.44(19) . . . . ? C7 N2 C15 C16A 100.9(4) . . . . ? C8 N2 C7 C6 77.4(2) . . . . ? C8 N2 C15 C16 -78.6(2) . . . . ? C8 N2 C15 C16A -135.2(4) . . . . ? C8 C9 C10 C11 -175.0(5) . . . . ? C8 C9 C10A C11A -175.2(10) . . . . ? C9 N3 C13 C12 2.7(7) . . . . ? C9 N3 C13 C14 -178.1(4) . . . . ? C9 N3 C13A C12A -3.3(16) . . . . ? C9 N3 C13A C14A 179.1(9) . . . . ? C9 C10 C11 C12 0.1(10) . . . . ? C9 C10A C11A C12A -2.5(19) . . . . ? C15 N2 C7 C6 -157.69(18) . . . . ? C15 N2 C8 C9 92.4(2) . . . . ? O2 C23 C24 C25 -174.9(3) . . . . ? O2 C23 C24 C29 7.7(5) . . . . ? O2 C23 C22 O1 -5.7(4) . . . . ? O2 C23 C22 C30 174.5(3) . . . . ? O3 C25 C26 C27 -178.0(8) . . . . ? O3 C30 C31 C32 -175.9(8) . . . . ? O3 C30 C31 C36 4.0(7) . . . . ? O3 C30 C22 O1 -177.8(5) . . . . ? O3 C30 C22 C23 2.0(6) . . . . ? C23 C24 C25 O3 -1.4(7) . . . . ? C23 C24 C25 C26 179.8(4) . . . . ? C23 C24 C29 C28 179.3(4) . . . . ? C24 C23 C22 O1 171.7(3) . . . . ? C24 C23 C22 C30 -8.1(4) . . . . ? C24 C25 C26 C27 0.9(10) . . . . ? C25 O3 C30 C31 -175.3(6) . . . . ? C25 O3 C30 C22 4.7(11) . . . . ? C25 C24 C29 C28 1.9(7) . . . . ? C25 C26 C27 C28 1.6(14) . . . . ? C26 C27 C28 C29 -2.3(13) . . . . ? C27 C28 C29 C24 0.5(9) . . . . ? C29 C24 C25 O3 176.2(6) . . . . ? C29 C24 C25 C26 -2.6(6) . . . . ? C30 O3 C25 C24 -5.0(11) . . . . ? C30 O3 C25 C26 173.9(7) . . . . ? C30 C31 C32 C33 179.9(7) . . . . ? C30 C31 C36 C35 179.5(5) . . . . ? C31 C30 C22 O1 2.2(5) . . . . ? C31 C30 C22 C23 -178.1(3) . . . . ? C31 C32 C33 C34 1.1(13) . . . . ? C32 C31 C36 C35 -0.6(10) . . . . ? C32 C33 C34 C35 -1.5(9) . . . . ? C33 C34 C35 C36 0.8(9) . . . . ? C34 C35 C36 C31 0.2(10) . . . . ? C36 C31 C32 C33 -0.1(13) . . . . ? C10 C11 C12 C13 -0.9(8) . . . . ? C11 C12 C13 N3 -0.4(8) . . . . ? C11 C12 C13 C14 -179.6(5) . . . . ? C13 N3 C9 C8 173.8(4) . . . . ? C13 N3 C9 C10 -3.5(6) . . . . ? C16 N4 C17 C18 67.8(3) . . . . ? C16 N4 C21 C20 -65.9(3) . . . . ? C17 N4 C16 C15 160.40(19) . . . . ? C17 N4 C21 C20 54.4(3) . . . . ? C17 C18 C19 C20 -51.7(4) . . . . ? C18 C19 C20 C21 51.7(4) . . . . ? C19 C20 C21 N4 -55.0(4) . . . . ? C21 N4 C16 C15 -79.2(2) . . . . ? C21 N4 C17 C18 -54.0(3) . . . . ? C22 C23 C24 C25 7.8(4) . . . . ? C22 C23 C24 C29 -169.7(4) . . . . ? C22 C30 C31 C32 4.1(8) . . . . ? C22 C30 C31 C36 -175.9(5) . . . . ? O2A C23A C24A C25A -175.0(6) . . . . ? O2A C23A C24A C29A 6.8(18) . . . . ? O2A C23A C22A O1A -7.2(10) . . . . ? O2A C23A C22A C30A 170.3(6) . . . . ? O3A C25A C26A C27A -179.6(16) . . . . ? O3A C30A C31A C32A -170.8(14) . . . . ? O3A C30A C31A C36A 4.1(15) . . . . ? O3A C30A C22A O1A -174.0(13) . . . . ? O3A C30A C22A C23A 8.8(15) . . . . ? C23A C24A C25A O3A 1.4(15) . . . . ? C23A C24A C25A C26A 179.8(10) . . . . ? C23A C24A C29A C28A -179.1(16) . . . . ? C24A C23A C22A O1A 176.1(6) . . . . ? C24A C23A C22A C30A -6.4(10) . . . . ? C24A C25A C26A C27A 2(2) . . . . ? C25A O3A C30A C31A 170.0(15) . . . . ? C25A O3A C30A C22A -6(3) . . . . ? C25A C24A C29A C28A 3(3) . . . . ? C25A C26A C27A C28A -3(2) . . . . ? C26A C27A C28A C29A 3(2) . . . . ? C27A C28A C29A C24A -3(3) . . . . ? C29A C24A C25A O3A 179.7(19) . . . . ? C29A C24A C25A C26A -1.9(19) . . . . ? C30A O3A C25A C24A 1(3) . . . . ? C30A O3A C25A C26A -177.8(16) . . . . ? C30A C31A C32A C33A 172.5(10) . . . . ? C30A C31A C36A C35A -173.8(16) . . . . ? C31A C30A C22A O1A 10.3(13) . . . . ? C31A C30A C22A C23A -166.8(6) . . . . ? C31A C32A C33A C34A 1.5(18) . . . . ? C32A C31A C36A C35A 1(2) . . . . ? C32A C33A C34A C35A 1.2(18) . . . . ? C33A C34A C35A C36A -3(3) . . . . ? C34A C35A C36A C31A 1(3) . . . . ? C36A C31A C32A C33A -2.8(18) . . . . ? C10A C11A C12A C13A 0.4(19) . . . . ? C11A C12A C13A N3 3(2) . . . . ? C11A C12A C13A C14A -179.5(12) . . . . ? C13A N3 C9 C8 177.8(8) . . . . ? C13A N3 C9 C10A 0.7(13) . . . . ? C16A N4 C17A C18A 64.1(10) . . . . ? C16A N4 C21A C20A -75.8(11) . . . . ? C17A N4 C16A C15 69.8(8) . . . . ? C17A N4 C21A C20A 52.8(12) . . . . ? C17A C18A C19A C20A -59.2(14) . . . . ? C18A C19A C20A C21A 55.0(15) . . . . ? C19A C20A C21A N4 -52.4(14) . . . . ? C21A N4 C16A C15 -166.7(6) . . . . ? C21A N4 C17A C18A -55.1(10) . . . . ? C22A C23A C24A C25A 1.6(9) . . . . ? C22A C23A C24A C29A -176.6(16) . . . . ? C22A C30A C31A C32A 5.3(13) . . . . ? C22A C30A C31A C36A -179.8(10) . . . . ? 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 -0.0003 -0.9997 -0.0000 0.0016 0.0515 0.0052 0.0003 0.9997 0.0000 -0.0016 -0.0515 -0.0052 -1.0017 0.0016 0.0016 0.1007 -0.0165 0.1313 1.0017 -0.0016 -0.0016 -0.1007 0.0165 -0.1313 0.0009 -0.0015 1.0014 -0.1242 -0.0012 0.0486 0.0004 -0.0055 -1.0013 0.1241 0.0016 -0.0487 -2.0039 -1.0189 2.0026 -0.0449 0.0172 0.3653 1.9967 0.9864 -2.0023 0.0456 -0.0156 -0.3641