#------------------------------------------------------------------------------ #$Date: 2026-06-25 02:27:21 +0100 (Thu, 25 Jun 2026) $ #$Revision: 306645 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064453.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_7064453 loop_ _publ_author_name 'Duan, Ran' 'Mori, Shigeki' 'Saeki, Akinori' 'Iwasaki, Takanori' 'Shimizu, Soji' _publ_section_title ; Supramolecular Polymerization of Antiaromatic 5,15-Dioxaporphyrin ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ01964A _journal_year 2026 _chemical_formula_moiety '2(C15 H9 N2 Ni0.5 O2), C4 H8 O' _chemical_formula_sum 'C34 H26 N4 Ni O5' _chemical_formula_weight 629.30 _chemical_name_systematic '4-hydroxyphenyl-substituted 5,15-dioxaporphyrin nickel complex' _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc2r8f0h _audit_creation_date 2025-12-24 _audit_creation_method ; Olex2 1.5 (compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314) ; _audit_update_record ; 2026-03-24 deposited with the CCDC. 2026-06-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 13.0699(4) _cell_length_b 37.9564(15) _cell_length_c 11.1243(4) _cell_measurement_reflns_used 11909 _cell_measurement_temperature 99.95(10) _cell_measurement_theta_max 30.9950 _cell_measurement_theta_min 2.1390 _cell_volume 5518.6(3) _computing_cell_refinement 'CrysAlisPro 1.171.44.128a (Rigaku OD, 2025)' _computing_data_collection 'CrysAlisPro system (CCD 44.128a 64-bit (release 04-11-2025))' _computing_data_reduction 'CrysAlisPro 1.171.44.128a (Rigaku OD, 2025)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.95(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.974 _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 -24.00 6.00 0.25 0.59 -- 5.60 77.00 -30.00 120 2 \w -82.00 8.00 0.25 0.59 -- -5.21 -17.00 11.00 360 3 \w -44.00 6.00 0.25 0.59 -- -5.21 -77.00 90.00 200 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0013209000 _diffrn_orient_matrix_UB_12 -0.0148313000 _diffrn_orient_matrix_UB_13 0.0329545000 _diffrn_orient_matrix_UB_21 -0.0147260000 _diffrn_orient_matrix_UB_22 -0.0111160000 _diffrn_orient_matrix_UB_23 -0.0418189000 _diffrn_orient_matrix_UB_31 0.0620204000 _diffrn_orient_matrix_UB_32 -0.0023302000 _diffrn_orient_matrix_UB_33 -0.0105831000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_unetI/netI 0.0442 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.974 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 30265 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.999 _diffrn_reflns_theta_min 1.908 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.38329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.44.128a (Rigaku Oxford Diffraction, 2025) 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 1.515 _exptl_crystal_description plate _exptl_crystal_F_000 2608 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.549 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 346 _refine_ls_number_reflns 6594 _refine_ls_number_restraints 138 _refine_ls_restrained_S_all 1.163 _refine_ls_R_factor_all 0.1350 _refine_ls_R_factor_gt 0.0789 _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^)+43.7224P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1757 _refine_ls_wR_factor_ref 0.1861 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3496 _reflns_number_total 6594 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj01964a3.cif _cod_data_source_block 20251223shimizu1_autored _cod_database_code 7064453 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula C30H18N4Ni1O4 _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. ; _cell_oxdiff_angle_alpha 90.042(2) _cell_oxdiff_angle_beta 90.052(2) _cell_oxdiff_angle_gamma 89.9900(19) _cell_oxdiff_length_a 11.1248(2) _cell_oxdiff_length_b 37.9657(9) _cell_oxdiff_length_c 13.0662(3) _cell_oxdiff_measurement_reflns_used 11907 _cell_oxdiff_volume 5518.6(2) _diffrn_oxdiff_digest_hkl ; 43434e8c22826af10ecbcb792923f84dda5fcb ; _diffrn_oxdiff_digest_od_ed ; ; _diffrn_oxdiff_measurement_exp_name 20251223Shimizu1.par _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H) groups 2. Restrained distances C43-C44 1.54 with sigma of 0.02 C10-C11 1.39 with sigma of 0.02 C16-C17 1.39 with sigma of 0.02 C11-C12 1.39 with sigma of 0.02 C31-C32 1.39 with sigma of 0.02 C12-C13 1.39 with sigma of 0.02 C13-C14 1.39 with sigma of 0.02 C17-C18 1.39 with sigma of 0.02 C44-C45 1.54 with sigma of 0.02 C14-C15 1.39 with sigma of 0.02 C18-C19 1.39 with sigma of 0.02 C15-C10 1.39 with sigma of 0.02 C10-C12 2.41 with sigma of 0.04 C19-C20 1.39 with sigma of 0.02 C32-C33 1.39 with sigma of 0.02 C11-C13 2.41 with sigma of 0.04 C45-C46 1.54 with sigma of 0.02 C12-C14 2.41 with sigma of 0.04 C20-C21 1.39 with sigma of 0.02 C13-C15 2.41 with sigma of 0.04 C14-C10 2.41 with sigma of 0.04 C33-C34 1.39 with sigma of 0.02 C21-C16 1.39 with sigma of 0.02 C15-C11 2.41 with sigma of 0.04 C13-O3 1.35 with sigma of 0.02 C16-C18 2.41 with sigma of 0.04 O9-C43 1.43 with sigma of 0.02 C12-O3 2.38 with sigma of 0.04 C14-O3 2.38 with sigma of 0.04 C34-C35 1.39 with sigma of 0.02 C17-C19 2.41 with sigma of 0.04 O9-C46 1.43 with sigma of 0.02 C18-C20 2.41 with sigma of 0.04 C35-C36 1.39 with sigma of 0.02 C19-C21 2.41 with sigma of 0.04 C20-C16 2.41 with sigma of 0.04 C36-C37 1.39 with sigma of 0.02 O9-C44 2.4 with sigma of 0.04 C21-C17 2.41 with sigma of 0.04 C19-O4 1.35 with sigma of 0.02 O9-C45 2.4 with sigma of 0.04 C31-C33 2.41 with sigma of 0.04 C18-O4 2.38 with sigma of 0.04 C20-O4 2.38 with sigma of 0.04 C43-C45 2.49 with sigma of 0.04 C32-C34 2.41 with sigma of 0.04 C44-C46 2.49 with sigma of 0.04 C33-C35 2.41 with sigma of 0.04 C34-C36 2.41 with sigma of 0.04 C43-C46 2.31 with sigma of 0.04 C35-C31 2.41 with sigma of 0.04 C36-C32 2.41 with sigma of 0.04 C47-C48 1.54 with sigma of 0.02 C48-C49 1.54 with sigma of 0.02 C34-O7 1.35 with sigma of 0.02 C49-C50 1.54 with sigma of 0.02 C33-O7 2.38 with sigma of 0.04 C35-O7 2.38 with sigma of 0.04 O10-C48 2.4 with sigma of 0.04 O10-C49 2.4 with sigma of 0.04 C47-C49 2.49 with sigma of 0.04 C48-C50 2.49 with sigma of 0.04 C47-C50 2.31 with sigma of 0.04 C37-C38 1.39 with sigma of 0.02 C38-C39 1.39 with sigma of 0.02 C39-C40 1.39 with sigma of 0.02 C40-C41 1.39 with sigma of 0.02 C41-C42 1.39 with sigma of 0.02 C42-C37 1.39 with sigma of 0.02 C37-C39 2.41 with sigma of 0.04 C38-C40 2.41 with sigma of 0.04 C39-C41 2.41 with sigma of 0.04 C40-C42 2.41 with sigma of 0.04 C41-C37 2.41 with sigma of 0.04 C42-C38 2.41 with sigma of 0.04 C40-O8 1.35 with sigma of 0.02 C39-O8 2.38 with sigma of 0.04 C41-O8 2.38 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(O3) Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(O4) Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(O7) Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42) = Uanis(O8) Uanis(O6) = Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) 4. Rigid body (RIGU) restrains O9, C43, C44, C45, C46 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O10, C47, C48, C49, C50 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(O10)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)= Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=1-FVAR(1) Sof(O9)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)= Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=FVAR(1) Sof(O4)=Sof(H4)=Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)= Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=1-FVAR(2) Sof(O3)=Sof(H3A)=Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)= Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=FVAR(2) Sof(O7)=Sof(H7A)=Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)= Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=1-FVAR(3) Sof(O8)=Sof(H8A)=Sof(C37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=Sof(C40)= Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=FVAR(3) 6.a Secondary CH2 refined with riding coordinates: C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A, H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B) 6.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C7(H7), C8(H8), C17(H17), C18(H18), C20(H20), C21(H21), C11(H11), C12(H12), C14(H14), C15(H15), C23(H23), C24(H24), C28(H28), C29(H29), C32(H32), C33(H33), C35(H35), C36(H36), C38(H38), C39(H39), C41(H41), C42(H42) 6.c Fitted hexagon refined as free rotating group: C16(C17,C18,C19,C20,C21), C10(C11,C12,C13,C14,C15), C31(C32,C33,C34,C35,C36) 6.d Tetrahedral OH refined with riding coordinates: O4(H4), O3(H3A), O7(H7A), O8(H8A) ; _shelx_res_file ; 20251223shimizu1_autored.res created by SHELXL-2014/7 TITL 20251223shimizu1_autored_a.res in Pnma REM Old TITL 20251223Shimizu1_autored in Pbcn REM SHELXT solution in Pnma REM R1 0.219, Rweak 0.003, Alpha 0.058, Orientation a =c, b =-b, c =a REM Formula found by SHELXT: C32 N4 Ni O5 CELL 0.71073 13.0699 37.9564 11.1243 90 90 90 ZERR 8 0.0004 0.0015 0.0004 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H N Ni O UNIT 272 208 32 8 40 DFIX 1.54 C43 C44 DFIX 1.39 C10 C11 DFIX 1.39 C16 C17 DFIX 1.39 C11 C12 DFIX 1.39 C31 C32 DFIX 1.39 C12 C13 DFIX 1.39 C13 C14 DFIX 1.39 C17 C18 DFIX 1.54 C44 C45 DFIX 1.39 C14 C15 DFIX 1.39 C18 C19 DFIX 1.39 C15 C10 DFIX 2.41 0.04 C10 C12 DFIX 1.39 C19 C20 DFIX 1.39 C32 C33 DFIX 2.41 0.04 C11 C13 DFIX 1.54 C45 C46 DFIX 2.41 0.04 C12 C14 DFIX 1.39 C20 C21 DFIX 2.41 0.04 C13 C15 DFIX 2.41 0.04 C14 C10 DFIX 1.39 C33 C34 DFIX 1.39 C21 C16 DFIX 2.41 0.04 C15 C11 DFIX 1.35 C13 O3 DFIX 2.41 0.04 C16 C18 DFIX 1.43 O9 C43 DFIX 2.38 0.04 C12 O3 DFIX 2.38 0.04 C14 O3 DFIX 1.39 C34 C35 EADP C10 C11 C12 C13 C14 C15 O3 DFIX 2.41 0.04 C17 C19 DFIX 1.43 O9 C46 DFIX 2.41 0.04 C18 C20 DFIX 1.39 C35 C36 DFIX 2.41 0.04 C19 C21 DFIX 2.41 0.04 C20 C16 DFIX 1.39 C36 C37 DFIX 2.4 0.04 O9 C44 DFIX 2.41 0.04 C21 C17 DFIX 1.35 C19 O4 DFIX 2.4 0.04 O9 C45 DFIX 2.41 0.04 C31 C33 DFIX 2.38 0.04 C18 O4 DFIX 2.38 0.04 C20 O4 DFIX 2.49 0.04 C43 C45 EADP C16 C17 C18 C19 C20 C21 O4 DFIX 2.41 0.04 C32 C34 DFIX 2.49 0.04 C44 C46 DFIX 2.41 0.04 C33 C35 DFIX 2.41 0.04 C34 C36 DFIX 2.31 0.04 C43 C46 DFIX 2.41 0.04 C35 C31 DFIX 2.41 0.04 C36 C32 DFIX 1.54 C47 C48 DFIX 1.54 C48 C49 DFIX 1.35 C34 O7 DFIX 1.54 C49 C50 DFIX 2.38 0.04 C33 O7 DFIX 2.38 0.04 C35 O7 DFIX 2.4 0.04 O10 C48 EADP C31 C32 C33 C34 C35 C36 O7 DFIX 2.4 0.04 O10 C49 DFIX 2.49 0.04 C47 C49 DFIX 2.49 0.04 C48 C50 DFIX 2.31 0.04 C47 C50 DFIX 1.39 C37 C38 DFIX 1.39 C38 C39 DFIX 1.39 C39 C40 DFIX 1.39 C40 C41 DFIX 1.39 C41 C42 DFIX 1.39 C42 C37 DFIX 2.41 0.04 C37 C39 DFIX 2.41 0.04 C38 C40 DFIX 2.41 0.04 C39 C41 DFIX 2.41 0.04 C40 C42 DFIX 2.41 0.04 C41 C37 DFIX 2.41 0.04 C42 C38 DFIX 1.35 C40 O8 DFIX 2.38 0.04 C39 O8 DFIX 2.38 0.04 C41 O8 EADP C37 C38 C39 C40 C41 C42 O8 RIGU O9 C43 C44 C45 C46 RIGU O10 C47 C48 C49 C50 EADP O6 C22 > C30 L.S. 20 0 0 PLAN 50 TEMP -173.2(1) CONF BOND $H list 4 MORE -1 fmap 2 53 acta OMIT 0 56 OMIT 1 2 3 OMIT 3 1 2 OMIT 3 2 2 OMIT 3 3 2 OMIT 3 4 2 OMIT 4 1 1 OMIT 5 2 4 OMIT 5 3 4 REM REM REM WGHT 0.000000 43.722401 FVAR 0.15901 0.54036 0.57008 0.55945 NI1 4 0.106443 0.250000 0.586412 10.50000 0.01756 0.01295 = 0.01647 0.00000 -0.00033 0.00000 O1 5 -0.107543 0.250000 0.425929 10.50000 0.03852 0.01588 = 0.05359 0.00000 -0.02786 0.00000 O2 5 0.345942 0.250000 0.694300 10.50000 0.01509 0.00893 = 0.04213 0.00000 -0.00304 0.00000 N1 3 0.013552 0.285378 0.530916 11.00000 0.01988 0.01959 = 0.01682 0.00248 -0.00403 -0.00162 N2 3 0.201531 0.285810 0.642578 11.00000 0.02181 0.01224 = 0.02237 -0.00467 -0.00001 0.00025 C1 1 -0.069515 0.280654 0.467800 11.00000 0.01766 0.02265 = 0.02083 0.00095 -0.00547 0.00201 C2 1 -0.126245 0.313046 0.442991 11.00000 0.02902 0.02678 = 0.03829 0.01082 -0.01291 0.00602 AFIX 43 H2 2 -0.188391 0.315905 0.399788 11.00000 -1.20000 AFIX 0 C3 1 -0.069536 0.337307 0.495612 11.00000 0.03211 0.02162 = 0.02859 0.00565 -0.00290 0.00855 AFIX 43 H3 2 -0.085492 0.361715 0.498049 11.00000 -1.20000 AFIX 0 C4 1 0.018146 0.321924 0.547774 11.00000 0.02186 0.01540 = 0.01648 0.00233 0.00325 0.00418 C5 1 0.100265 0.339211 0.603717 11.00000 0.02269 0.01290 = 0.01552 0.00098 0.00416 -0.00305 C6 1 0.186011 0.323186 0.646285 11.00000 0.02038 0.01440 = 0.01474 -0.00208 0.00087 -0.00251 C7 1 0.276998 0.338282 0.696531 11.00000 0.02726 0.02128 = 0.01199 -0.00247 0.00280 -0.01251 AFIX 43 H7 2 0.287744 0.362536 0.713420 11.00000 -1.20000 AFIX 0 C8 1 0.344272 0.312217 0.715533 11.00000 0.01878 0.02625 = 0.02221 0.00026 -0.00126 -0.00664 AFIX 43 H8 2 0.412116 0.314174 0.745446 11.00000 -1.20000 AFIX 0 C9 1 0.292798 0.281588 0.681743 11.00000 0.01773 0.02165 = 0.01702 0.00326 -0.00019 0.00347 PART -2 O4 5 0.051998 0.487620 0.633581 -31.00000 0.01426 0.01390 = 0.01605 -0.00333 0.00156 -0.00513 AFIX 83 H4 2 0.040668 0.495146 0.563831 -31.00000 -1.50000 AFIX 66 C16 1 0.091459 0.379124 0.615646 -31.00000 0.01426 0.01390 = 0.01605 -0.00333 0.00156 -0.00513 C17 1 0.088555 0.399005 0.510767 -31.00000 0.01426 0.01390 = 0.01605 -0.00333 0.00156 -0.00513 AFIX 43 H17 2 0.091487 0.387654 0.434734 -31.00000 -1.20000 AFIX 65 C18 1 0.081360 0.435494 0.517137 -31.00000 0.01426 0.01390 = 0.01605 -0.00333 0.00156 -0.00513 AFIX 43 H18 2 0.079375 0.449082 0.445457 -31.00000 -1.20000 AFIX 65 C19 1 0.077070 0.452103 0.628386 -31.00000 0.01426 0.01390 = 0.01605 -0.00333 0.00156 -0.00513 C20 1 0.079975 0.432222 0.733265 -31.00000 0.01426 0.01390 = 0.01605 -0.00333 0.00156 -0.00513 AFIX 43 H20 2 0.077043 0.443573 0.809298 -31.00000 -1.20000 AFIX 65 C21 1 0.087169 0.395732 0.726897 -31.00000 0.01426 0.01390 = 0.01605 -0.00333 0.00156 -0.00513 AFIX 43 H21 2 0.089154 0.382145 0.798577 -31.00000 -1.20000 AFIX 0 PART -1 O3 5 0.075687 0.488365 0.635492 31.00000 0.03592 0.01481 = 0.04460 -0.00913 -0.00004 -0.00023 AFIX 83 H3A 2 0.071698 0.496561 0.565508 31.00000 -1.50000 AFIX 66 C10 1 0.090028 0.379072 0.614550 31.00000 0.03592 0.01481 = 0.04460 -0.00913 -0.00004 -0.00023 C11 1 0.145752 0.400540 0.537343 31.00000 0.03592 0.01481 = 0.04460 -0.00913 -0.00004 -0.00023 AFIX 43 H11 2 0.189774 0.390321 0.479016 31.00000 -1.20000 AFIX 65 C12 1 0.137063 0.436961 0.545475 31.00000 0.03592 0.01481 = 0.04460 -0.00913 -0.00004 -0.00023 AFIX 43 H12 2 0.175148 0.451633 0.492707 31.00000 -1.20000 AFIX 65 C13 1 0.072652 0.451913 0.630815 31.00000 0.03592 0.01481 = 0.04460 -0.00913 -0.00004 -0.00023 C14 1 0.016928 0.430445 0.708023 31.00000 0.03592 0.01481 = 0.04460 -0.00913 -0.00004 -0.00023 AFIX 43 H14 2 -0.027094 0.440665 0.766349 31.00000 -1.20000 AFIX 65 C15 1 0.025615 0.394025 0.699892 31.00000 0.03592 0.01481 = 0.04460 -0.00913 -0.00004 -0.00023 AFIX 43 H15 2 -0.012469 0.379353 0.752661 31.00000 -1.20000 AFIX 0 PART 0 NI2 4 0.393337 0.250000 0.413172 10.50000 0.01549 0.01387 = 0.01711 0.00000 -0.00211 0.00000 O5 5 0.160714 0.250000 0.299015 10.50000 0.01665 0.03117 = 0.02550 0.00000 -0.00696 0.00000 O6 5 0.612265 0.250000 0.569894 10.50000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 N3 3 0.302193 0.284825 0.359025 11.00000 0.01534 0.01925 = 0.01427 -0.00462 -0.00187 0.00055 N4 3 0.487007 0.285221 0.468402 11.00000 0.01543 0.01513 = 0.02092 0.00070 0.00314 -0.00117 C22 1 0.204324 0.280411 0.313270 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 C23 1 0.155548 0.312511 0.282934 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 AFIX 43 H23 2 0.088854 0.315673 0.250738 11.00000 -1.20000 AFIX 0 C24 1 0.226767 0.338264 0.310676 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 AFIX 43 H24 2 0.217932 0.362958 0.301422 11.00000 -1.20000 AFIX 0 C25 1 0.314582 0.321230 0.355048 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 C26 1 0.404067 0.339221 0.395137 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 C27 1 0.482549 0.322168 0.449772 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 C28 1 0.568009 0.338592 0.504983 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 AFIX 43 H28 2 0.583229 0.363063 0.506206 11.00000 -1.20000 AFIX 0 C29 1 0.625870 0.311250 0.557735 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 AFIX 43 H29 2 0.687428 0.313664 0.602392 11.00000 -1.20000 AFIX 0 C30 1 0.576352 0.281077 0.532087 11.00000 0.02233 0.01838 = 0.02133 0.00000 -0.00096 0.00000 PART -1 O7 5 0.436401 0.486810 0.377717 -41.00000 0.02107 0.01441 = 0.01543 -0.00610 0.00880 0.00128 AFIX 83 H7A 2 0.451821 0.493280 0.307815 -41.00000 -1.50000 AFIX 66 C31 1 0.404075 0.378078 0.384391 -41.00000 0.02107 0.01441 = 0.01543 -0.00610 0.00880 0.00128 C32 1 0.473483 0.393672 0.306084 -41.00000 0.02107 0.01441 = 0.01543 -0.00610 0.00880 0.00128 AFIX 43 H32 2 0.513623 0.379431 0.254048 -41.00000 -1.20000 AFIX 65 C33 1 0.484159 0.430102 0.303911 -41.00000 0.02107 0.01441 = 0.01543 -0.00610 0.00880 0.00128 AFIX 43 H33 2 0.531596 0.440759 0.250391 -41.00000 -1.20000 AFIX 65 C34 1 0.425427 0.450939 0.380046 -41.00000 0.02107 0.01441 = 0.01543 -0.00610 0.00880 0.00128 C35 1 0.356019 0.435346 0.458354 -41.00000 0.02107 0.01441 = 0.01543 -0.00610 0.00880 0.00128 AFIX 43 H35 2 0.315879 0.449587 0.510389 -41.00000 -1.20000 AFIX 65 C36 1 0.345342 0.398916 0.460528 -41.00000 0.02107 0.01441 = 0.01543 -0.00610 0.00880 0.00128 AFIX 43 H36 2 0.297904 0.388259 0.514048 -41.00000 -1.20000 AFIX 0 PART -2 O8 5 0.434779 0.486917 0.349171 41.00000 0.03157 0.01906 = 0.02551 -0.00415 0.00118 -0.00679 AFIX 83 H8A 2 0.437987 0.492365 0.276081 41.00000 -1.50000 AFIX 0 C37 1 0.408848 0.377921 0.385932 41.00000 0.03157 0.01906 = 0.02551 -0.00415 0.00118 -0.00679 C38 1 0.412165 0.393419 0.271955 41.00000 0.03157 0.01906 = 0.02551 -0.00415 0.00118 -0.00679 AFIX 43 H38 2 0.410378 0.378763 0.202762 41.00000 -1.20000 AFIX 0 C39 1 0.418041 0.429929 0.257299 41.00000 0.03157 0.01906 = 0.02551 -0.00415 0.00118 -0.00679 AFIX 43 H39 2 0.416858 0.440146 0.179353 41.00000 -1.20000 AFIX 0 C40 1 0.425711 0.451147 0.359934 41.00000 0.03157 0.01906 = 0.02551 -0.00415 0.00118 -0.00679 C41 1 0.423640 0.436517 0.473589 41.00000 0.03157 0.01906 = 0.02551 -0.00415 0.00118 -0.00679 AFIX 43 H41 2 0.426071 0.451162 0.542784 41.00000 -1.20000 AFIX 0 C42 1 0.417947 0.400048 0.485570 41.00000 0.03157 0.01906 = 0.02551 -0.00415 0.00118 -0.00679 AFIX 43 H42 2 0.420320 0.389959 0.563672 41.00000 -1.20000 AFIX 0 PART -1 O9 5 0.195062 0.521238 0.494848 21.00000 0.04607 0.04659 = 0.05272 -0.00300 0.00530 -0.01183 C43 1 0.191716 0.530181 0.369956 21.00000 0.04429 0.03953 = 0.05176 -0.01122 0.01262 0.01509 AFIX 23 H43A 2 0.122157 0.526792 0.336679 21.00000 -1.20000 H43B 2 0.240798 0.515815 0.323140 21.00000 -1.20000 AFIX 0 C44 1 0.221871 0.568937 0.368906 21.00000 0.08151 0.04291 = 0.06947 -0.00736 0.02572 0.00832 AFIX 23 H44A 2 0.161111 0.584267 0.378288 21.00000 -1.20000 H44B 2 0.257487 0.575178 0.293305 21.00000 -1.20000 AFIX 0 C45 1 0.294805 0.572380 0.478792 21.00000 0.07731 0.05229 = 0.06279 -0.01530 0.03377 -0.01495 AFIX 23 H45A 2 0.366422 0.575574 0.451933 21.00000 -1.20000 H45B 2 0.275106 0.592749 0.529330 21.00000 -1.20000 AFIX 0 C46 1 0.283113 0.537804 0.549076 21.00000 0.04163 0.06085 = 0.06418 -0.00751 0.00859 -0.01683 AFIX 23 H46A 2 0.344763 0.522870 0.540306 21.00000 -1.20000 H46B 2 0.271217 0.542445 0.635528 21.00000 -1.20000 AFIX 0 PART -2 O10 5 0.305467 0.520894 0.506395 -21.00000 0.04761 0.01979 = 0.05467 -0.01738 -0.00744 0.01787 C47 1 0.219399 0.539490 0.452317 -21.00000 0.02795 0.02465 = 0.05462 0.00331 0.00826 0.00545 AFIX 23 H47A 2 0.156011 0.525378 0.459723 -21.00000 -1.20000 H47B 2 0.232577 0.543993 0.366037 -21.00000 -1.20000 AFIX 0 C48 1 0.208804 0.574180 0.520610 -21.00000 0.05908 0.02910 = 0.10219 -0.01697 0.00330 0.02009 AFIX 23 H48A 2 0.137048 0.578067 0.545842 -21.00000 -1.20000 H48B 2 0.231011 0.594264 0.470180 -21.00000 -1.20000 AFIX 0 C49 1 0.278899 0.569985 0.630318 -21.00000 0.05023 0.03081 = 0.08095 -0.02666 0.01755 0.01191 AFIX 23 H49A 2 0.243341 0.576979 0.705186 -21.00000 -1.20000 H49B 2 0.341892 0.584237 0.621498 -21.00000 -1.20000 AFIX 0 C50 1 0.303424 0.530347 0.630161 -21.00000 0.03397 0.03050 = 0.05734 -0.02224 -0.00075 0.01116 AFIX 23 H50A 2 0.370483 0.525767 0.668480 -21.00000 -1.20000 H50B 2 0.250017 0.516928 0.673594 -21.00000 -1.20000 AFIX 0 HKLF 4 REM 20251223shimizu1_autored_a.res in Pnma REM R1 = 0.0789 for 3496 Fo > 4sig(Fo) and 0.1350 for all 6594 data REM 346 parameters refined using 138 restraints END WGHT 0.0000 43.7215 REM Highest difference peak 0.549, deepest hole -0.456, 1-sigma level 0.098 Q1 1 0.5078 0.2500 0.7167 10.50000 0.05 0.43 Q2 1 -0.0543 0.2500 0.4368 10.50000 0.05 0.42 Q3 1 0.4167 0.4968 0.2841 11.00000 0.05 0.41 Q4 1 0.2384 0.5817 0.4089 11.00000 0.05 0.40 Q5 1 0.3416 0.2787 0.3988 11.00000 0.05 0.40 Q6 1 0.4843 0.3030 0.4515 11.00000 0.05 0.35 Q7 1 0.0765 0.4051 0.5206 11.00000 0.05 0.35 Q8 1 0.6182 0.2500 0.5322 10.50000 0.05 0.35 Q9 1 0.0171 0.2993 0.5538 11.00000 0.05 0.34 Q10 1 -0.0199 0.2783 0.4870 11.00000 0.05 0.34 Q11 1 0.6136 0.3036 0.5229 11.00000 0.05 0.33 Q12 1 0.3592 0.4390 0.1766 11.00000 0.05 0.33 Q13 1 0.5411 0.3453 0.5498 11.00000 0.05 0.32 Q14 1 0.2843 0.3778 0.7086 11.00000 0.05 0.32 Q15 1 0.3252 0.3043 0.7021 11.00000 0.05 0.32 Q16 1 0.1021 0.5819 0.5938 11.00000 0.05 0.32 Q17 1 0.5269 0.2781 0.5208 11.00000 0.05 0.32 Q18 1 0.2251 0.4015 0.5215 11.00000 0.05 0.31 Q19 1 0.0698 0.4389 0.6827 11.00000 0.05 0.31 Q20 1 0.0812 0.3772 0.6561 11.00000 0.05 0.31 Q21 1 0.1016 0.2992 0.4259 11.00000 0.05 0.30 Q22 1 0.1971 0.5809 0.2205 11.00000 0.05 0.30 Q23 1 0.1423 0.5815 0.3359 11.00000 0.05 0.30 Q24 1 0.1732 0.3025 0.2978 11.00000 0.05 0.30 Q25 1 0.4392 0.4193 0.4807 11.00000 0.05 0.29 Q26 1 0.2549 0.5832 0.5832 11.00000 0.05 0.29 Q27 1 0.4212 0.4370 0.3149 11.00000 0.05 0.29 Q28 1 0.1136 0.4232 0.5384 11.00000 0.05 0.29 Q29 1 0.1943 0.5553 0.3583 11.00000 0.05 0.28 Q30 1 0.3212 0.2766 0.2981 11.00000 0.05 0.28 Q31 1 0.7648 0.2500 0.6248 10.50000 0.05 0.28 Q32 1 0.3616 0.3814 0.8001 11.00000 0.05 0.28 Q33 1 0.3769 0.3202 0.5293 11.00000 0.05 0.28 Q34 1 0.3380 0.2500 0.8156 10.50000 0.05 0.27 Q35 1 0.0738 0.2809 0.5868 11.00000 0.05 0.27 Q36 1 -0.1926 0.2980 0.3633 11.00000 0.05 0.27 Q37 1 0.1694 0.2500 0.1566 10.50000 0.05 0.27 Q38 1 0.2164 0.2782 0.7105 11.00000 0.05 0.27 Q39 1 0.6876 0.3028 0.6360 11.00000 0.05 0.26 Q40 1 0.0391 0.2805 0.4511 11.00000 0.05 0.26 Q41 1 0.2158 0.5632 0.6084 11.00000 0.05 0.26 Q42 1 0.3174 0.5638 0.7048 11.00000 0.05 0.26 Q43 1 0.2561 0.2500 0.7895 10.50000 0.05 0.26 Q44 1 0.0719 0.2230 0.3765 11.00000 0.05 0.26 Q45 1 0.3884 0.3824 0.6245 11.00000 0.05 0.26 Q46 1 -0.1060 0.3002 0.4737 11.00000 0.05 0.26 Q47 1 0.3041 0.3217 0.7326 11.00000 0.05 0.26 Q48 1 0.2127 0.3813 0.3202 11.00000 0.05 0.26 Q49 1 0.4398 0.5793 0.4962 11.00000 0.05 0.26 Q50 1 0.3788 0.3239 0.6974 11.00000 0.05 0.25 ; _shelx_res_checksum 55596 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.593 _oxdiff_exptl_absorpt_empirical_full_min 0.485 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, 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 0.10644(8) 0.2500 0.58641(9) 0.0157(2) Uani 1 2 d S T P . . O1 O -0.1075(5) 0.2500 0.4259(7) 0.0360(16) Uani 1 2 d S T P . . O2 O 0.3459(4) 0.2500 0.6943(6) 0.0220(13) Uani 1 2 d S T P . . N1 N 0.0136(4) 0.28538(13) 0.5309(4) 0.0188(10) Uani 1 1 d . . . . . N2 N 0.2015(4) 0.28581(12) 0.6426(5) 0.0188(11) Uani 1 1 d . . . . . C1 C -0.0695(4) 0.28065(16) 0.4678(5) 0.0204(11) Uani 1 1 d . . . . . C2 C -0.1262(5) 0.31305(17) 0.4430(7) 0.0314(14) Uani 1 1 d . . . . . H2 H -0.1884 0.3159 0.3998 0.038 Uiso 1 1 calc R U . . . C3 C -0.0695(5) 0.33731(18) 0.4956(6) 0.0274(13) Uani 1 1 d . . . . . H3 H -0.0855 0.3617 0.4980 0.033 Uiso 1 1 calc R U . . . C4 C 0.0181(4) 0.32192(15) 0.5478(5) 0.0179(11) Uani 1 1 d . . . . . C5 C 0.1003(4) 0.33921(14) 0.6037(5) 0.0170(10) Uani 1 1 d . . . . . C6 C 0.1860(4) 0.32319(14) 0.6463(5) 0.0165(10) Uani 1 1 d . . . . . C7 C 0.2770(5) 0.33828(16) 0.6965(5) 0.0202(11) Uani 1 1 d . . . . . H7 H 0.2877 0.3625 0.7134 0.024 Uiso 1 1 calc R U . . . C8 C 0.3443(5) 0.31222(16) 0.7155(5) 0.0224(12) Uani 1 1 d . . . . . H8 H 0.4121 0.3142 0.7454 0.027 Uiso 1 1 calc R U . . . C9 C 0.2928(4) 0.28159(15) 0.6817(5) 0.0188(11) Uani 1 1 d . . . . . O4 O 0.0520(7) 0.4876(3) 0.6336(13) 0.0147(16) Uani 0.430(10) 1 d D . P A -2 H4 H 0.0407 0.4951 0.5638 0.022 Uiso 0.430(10) 1 calc R U P A -2 C16 C 0.0915(7) 0.37912(14) 0.6156(7) 0.0147(16) Uani 0.430(10) 1 d DG . P A -2 C17 C 0.0886(8) 0.3990(2) 0.5108(5) 0.0147(16) Uani 0.430(10) 1 d DG . P A -2 H17 H 0.0915 0.3877 0.4347 0.018 Uiso 0.430(10) 1 calc R U P A -2 C18 C 0.0814(8) 0.43549(19) 0.5171(5) 0.0147(16) Uani 0.430(10) 1 d DG . P A -2 H18 H 0.0794 0.4491 0.4455 0.018 Uiso 0.430(10) 1 calc R U P A -2 C19 C 0.0771(7) 0.45210(14) 0.6284(7) 0.0147(16) Uani 0.430(10) 1 d DG . P A -2 C20 C 0.0800(7) 0.43222(19) 0.7333(5) 0.0147(16) Uani 0.430(10) 1 d DG . P A -2 H20 H 0.0770 0.4436 0.8093 0.018 Uiso 0.430(10) 1 calc R U P A -2 C21 C 0.0872(7) 0.39573(18) 0.7269(6) 0.0147(16) Uani 0.430(10) 1 d DG . P A -2 H21 H 0.0892 0.3821 0.7986 0.018 Uiso 0.430(10) 1 calc R U P A -2 O3 O 0.0757(7) 0.4884(2) 0.6355(13) 0.0318(15) Uani 0.570(10) 1 d D . P A -1 H3A H 0.0717 0.4966 0.5655 0.048 Uiso 0.570(10) 1 calc R U P A -1 C10 C 0.0900(7) 0.37907(13) 0.6146(8) 0.0318(15) Uani 0.570(10) 1 d DG . P A -1 C11 C 0.1458(6) 0.40054(18) 0.5373(8) 0.0318(15) Uani 0.570(10) 1 d DG . P A -1 H11 H 0.1898 0.3903 0.4790 0.038 Uiso 0.570(10) 1 calc R U P A -1 C12 C 0.1371(7) 0.43696(17) 0.5455(8) 0.0318(15) Uani 0.570(10) 1 d DG . P A -1 H12 H 0.1751 0.4516 0.4927 0.038 Uiso 0.570(10) 1 calc R U P A -1 C13 C 0.0727(7) 0.45191(13) 0.6308(8) 0.0318(15) Uani 0.570(10) 1 d DG . P A -1 C14 C 0.0169(7) 0.43045(18) 0.7080(7) 0.0318(15) Uani 0.570(10) 1 d DG . P A -1 H14 H -0.0271 0.4407 0.7663 0.038 Uiso 0.570(10) 1 calc R U P A -1 C15 C 0.0256(7) 0.39403(17) 0.6999(8) 0.0318(15) Uani 0.570(10) 1 d DG . P A -1 H15 H -0.0125 0.3794 0.7527 0.038 Uiso 0.570(10) 1 calc R U P A -1 Ni2 Ni 0.39334(8) 0.2500 0.41317(9) 0.0155(2) Uani 1 2 d S T P . . O5 O 0.1607(4) 0.2500 0.2990(5) 0.0244(14) Uani 1 2 d S T P . . O6 O 0.6123(4) 0.2500 0.5699(5) 0.0207(4) Uani 1 2 d S T P . . N3 N 0.3022(3) 0.28482(12) 0.3590(4) 0.0163(10) Uani 1 1 d . . . . . N4 N 0.4870(4) 0.28522(13) 0.4684(4) 0.0172(10) Uani 1 1 d . . . . . C22 C 0.2043(5) 0.28041(16) 0.3133(5) 0.0207(4) Uani 1 1 d . . . . . C23 C 0.1555(5) 0.31251(15) 0.2829(5) 0.0207(4) Uani 1 1 d . . . . . H23 H 0.0889 0.3157 0.2507 0.025 Uiso 1 1 calc R U . . . C24 C 0.2268(5) 0.33826(16) 0.3107(5) 0.0207(4) Uani 1 1 d . . . . . H24 H 0.2179 0.3630 0.3014 0.025 Uiso 1 1 calc R U . . . C25 C 0.3146(5) 0.32123(15) 0.3550(5) 0.0207(4) Uani 1 1 d . . . . . C26 C 0.4041(5) 0.33922(16) 0.3951(5) 0.0207(4) Uani 1 1 d . . . . . C27 C 0.4825(5) 0.32217(16) 0.4498(6) 0.0207(4) Uani 1 1 d . . . . . C28 C 0.5680(5) 0.33859(16) 0.5050(5) 0.0207(4) Uani 1 1 d . . . . . H28 H 0.5832 0.3631 0.5062 0.025 Uiso 1 1 calc R U . . . C29 C 0.6259(5) 0.31125(15) 0.5577(5) 0.0207(4) Uani 1 1 d . . . . . H29 H 0.6874 0.3137 0.6024 0.025 Uiso 1 1 calc R U . . . C30 C 0.5764(5) 0.28108(15) 0.5321(5) 0.0207(4) Uani 1 1 d . . . . . O7 O 0.4364(12) 0.4868(3) 0.3777(9) 0.0170(16) Uani 0.441(9) 1 d D . P B -1 H7A H 0.4518 0.4933 0.3078 0.025 Uiso 0.441(9) 1 calc R U P B -1 C31 C 0.4041(8) 0.37808(15) 0.3844(9) 0.0170(16) Uani 0.441(9) 1 d DG . P B -1 C32 C 0.4735(7) 0.39367(19) 0.3061(8) 0.0170(16) Uani 0.441(9) 1 d DG . P B -1 H32 H 0.5136 0.3794 0.2540 0.020 Uiso 0.441(9) 1 calc R U P B -1 C33 C 0.4842(7) 0.4301(2) 0.3039(7) 0.0170(16) Uani 0.441(9) 1 d DG . P B -1 H33 H 0.5316 0.4408 0.2504 0.020 Uiso 0.441(9) 1 calc R U P B -1 C34 C 0.4254(8) 0.45094(15) 0.3800(8) 0.0170(16) Uani 0.441(9) 1 d DG . P B -1 C35 C 0.3560(7) 0.43535(18) 0.4584(7) 0.0170(16) Uani 0.441(9) 1 d DG . P B -1 H35 H 0.3159 0.4496 0.5104 0.020 Uiso 0.441(9) 1 calc R U P B -1 C36 C 0.3453(7) 0.39892(19) 0.4605(8) 0.0170(16) Uani 0.441(9) 1 d DG . P B -1 H36 H 0.2979 0.3883 0.5140 0.020 Uiso 0.441(9) 1 calc R U P B -1 O8 O 0.4348(10) 0.4869(2) 0.3492(8) 0.0254(14) Uani 0.559(9) 1 d D . P B -2 H8A H 0.4380 0.4924 0.2761 0.038 Uiso 0.559(9) 1 calc R U P B -2 C37 C 0.4088(10) 0.3779(3) 0.3859(10) 0.0254(14) Uani 0.559(9) 1 d D . P B -2 C38 C 0.4122(9) 0.3934(2) 0.2720(9) 0.0254(14) Uani 0.559(9) 1 d D . P B -2 H38 H 0.4104 0.3788 0.2028 0.030 Uiso 0.559(9) 1 calc R U P B -2 C39 C 0.4180(9) 0.4299(2) 0.2573(9) 0.0254(14) Uani 0.559(9) 1 d D . P B -2 H39 H 0.4169 0.4401 0.1794 0.030 Uiso 0.559(9) 1 calc R U P B -2 C40 C 0.4257(11) 0.4511(3) 0.3599(9) 0.0254(14) Uani 0.559(9) 1 d D . P B -2 C41 C 0.4236(9) 0.4365(2) 0.4736(9) 0.0254(14) Uani 0.559(9) 1 d D . P B -2 H41 H 0.4261 0.4512 0.5428 0.030 Uiso 0.559(9) 1 calc R U P B -2 C42 C 0.4179(9) 0.4000(2) 0.4856(9) 0.0254(14) Uani 0.559(9) 1 d D . P B -2 H42 H 0.4203 0.3900 0.5637 0.030 Uiso 0.559(9) 1 calc R U P B -2 O9 O 0.1951(8) 0.5212(3) 0.4948(9) 0.048(3) Uani 0.540(10) 1 d D U P C -1 C43 C 0.1917(12) 0.5302(3) 0.3700(12) 0.045(3) Uani 0.540(10) 1 d D U P C -1 H43A H 0.1222 0.5268 0.3367 0.054 Uiso 0.540(10) 1 calc R U P C -1 H43B H 0.2408 0.5158 0.3231 0.054 Uiso 0.540(10) 1 calc R U P C -1 C44 C 0.2219(14) 0.5689(4) 0.3689(14) 0.065(4) Uani 0.540(10) 1 d D U P C -1 H44A H 0.1611 0.5843 0.3783 0.078 Uiso 0.540(10) 1 calc R U P C -1 H44B H 0.2575 0.5752 0.2933 0.078 Uiso 0.540(10) 1 calc R U P C -1 C45 C 0.2948(14) 0.5724(4) 0.4788(14) 0.064(5) Uani 0.540(10) 1 d D U P C -1 H45A H 0.3664 0.5756 0.4519 0.077 Uiso 0.540(10) 1 calc R U P C -1 H45B H 0.2751 0.5927 0.5293 0.077 Uiso 0.540(10) 1 calc R U P C -1 C46 C 0.2831(13) 0.5378(5) 0.5491(16) 0.056(4) Uani 0.540(10) 1 d D U P C -1 H46A H 0.3448 0.5229 0.5403 0.067 Uiso 0.540(10) 1 calc R U P C -1 H46B H 0.2712 0.5424 0.6355 0.067 Uiso 0.540(10) 1 calc R U P C -1 O10 O 0.3055(9) 0.5209(3) 0.5064(11) 0.041(3) Uani 0.460(10) 1 d D U P C -2 C47 C 0.2194(13) 0.5395(4) 0.4523(15) 0.036(3) Uani 0.460(10) 1 d D U P C -2 H47A H 0.1560 0.5254 0.4597 0.043 Uiso 0.460(10) 1 calc R U P C -2 H47B H 0.2326 0.5440 0.3660 0.043 Uiso 0.460(10) 1 calc R U P C -2 C48 C 0.2088(16) 0.5742(4) 0.5206(19) 0.063(6) Uani 0.460(10) 1 d D U P C -2 H48A H 0.1370 0.5781 0.5458 0.076 Uiso 0.460(10) 1 calc R U P C -2 H48B H 0.2310 0.5943 0.4702 0.076 Uiso 0.460(10) 1 calc R U P C -2 C49 C 0.2789(14) 0.5700(4) 0.6303(16) 0.054(5) Uani 0.460(10) 1 d D U P C -2 H49A H 0.2433 0.5770 0.7052 0.065 Uiso 0.460(10) 1 calc R U P C -2 H49B H 0.3419 0.5842 0.6215 0.065 Uiso 0.460(10) 1 calc R U P C -2 C50 C 0.3034(13) 0.5303(4) 0.6302(15) 0.041(4) Uani 0.460(10) 1 d D U P C -2 H50A H 0.3705 0.5258 0.6685 0.049 Uiso 0.460(10) 1 calc R U P C -2 H50B H 0.2500 0.5169 0.6736 0.049 Uiso 0.460(10) 1 calc R U P C -2 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 0.0176(5) 0.0130(5) 0.0165(5) 0.000 -0.0003(4) 0.000 O1 0.039(4) 0.016(3) 0.054(4) 0.000 -0.028(3) 0.000 O2 0.015(3) 0.009(3) 0.042(4) 0.000 -0.003(3) 0.000 N1 0.020(3) 0.020(3) 0.017(2) 0.002(2) -0.004(2) -0.002(2) N2 0.022(3) 0.012(2) 0.022(3) -0.0047(19) 0.000(2) 0.000(2) C1 0.018(3) 0.023(3) 0.021(3) 0.001(2) -0.005(2) 0.002(2) C2 0.029(3) 0.027(3) 0.038(4) 0.011(3) -0.013(3) 0.006(3) C3 0.032(3) 0.022(3) 0.029(3) 0.006(2) -0.003(3) 0.009(3) C4 0.022(3) 0.015(2) 0.016(2) 0.0023(19) 0.003(2) 0.004(2) C5 0.023(3) 0.013(2) 0.016(2) 0.0010(18) 0.004(2) -0.003(2) C6 0.020(2) 0.014(2) 0.015(2) -0.0021(18) 0.001(2) -0.003(2) C7 0.027(3) 0.021(3) 0.012(2) -0.0025(19) 0.003(2) -0.013(2) C8 0.019(3) 0.026(3) 0.022(3) 0.000(2) -0.001(2) -0.007(2) C9 0.018(2) 0.022(3) 0.017(3) 0.003(2) 0.000(2) 0.003(2) O4 0.014(3) 0.014(3) 0.016(3) -0.0033(18) 0.002(2) -0.0051(19) C16 0.014(3) 0.014(3) 0.016(3) -0.0033(18) 0.002(2) -0.0051(19) C17 0.014(3) 0.014(3) 0.016(3) -0.0033(18) 0.002(2) -0.0051(19) C18 0.014(3) 0.014(3) 0.016(3) -0.0033(18) 0.002(2) -0.0051(19) C19 0.014(3) 0.014(3) 0.016(3) -0.0033(18) 0.002(2) -0.0051(19) C20 0.014(3) 0.014(3) 0.016(3) -0.0033(18) 0.002(2) -0.0051(19) C21 0.014(3) 0.014(3) 0.016(3) -0.0033(18) 0.002(2) -0.0051(19) O3 0.036(3) 0.015(2) 0.045(3) -0.0091(18) 0.000(2) -0.0002(19) C10 0.036(3) 0.015(2) 0.045(3) -0.0091(18) 0.000(2) -0.0002(19) C11 0.036(3) 0.015(2) 0.045(3) -0.0091(18) 0.000(2) -0.0002(19) C12 0.036(3) 0.015(2) 0.045(3) -0.0091(18) 0.000(2) -0.0002(19) C13 0.036(3) 0.015(2) 0.045(3) -0.0091(18) 0.000(2) -0.0002(19) C14 0.036(3) 0.015(2) 0.045(3) -0.0091(18) 0.000(2) -0.0002(19) C15 0.036(3) 0.015(2) 0.045(3) -0.0091(18) 0.000(2) -0.0002(19) Ni2 0.0155(5) 0.0139(5) 0.0171(5) 0.000 -0.0021(4) 0.000 O5 0.017(3) 0.031(4) 0.026(3) 0.000 -0.007(3) 0.000 O6 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 N3 0.015(2) 0.019(3) 0.014(2) -0.0046(18) -0.0019(19) 0.001(2) N4 0.015(2) 0.015(2) 0.021(3) 0.0007(19) 0.003(2) -0.001(2) C22 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 C23 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 C24 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 C25 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 C26 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 C27 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 C28 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 C29 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 C30 0.0223(10) 0.0184(10) 0.0213(10) 0.000 -0.0010(8) 0.000 O7 0.021(3) 0.014(3) 0.015(2) -0.0061(18) 0.009(2) 0.001(2) C31 0.021(3) 0.014(3) 0.015(2) -0.0061(18) 0.009(2) 0.001(2) C32 0.021(3) 0.014(3) 0.015(2) -0.0061(18) 0.009(2) 0.001(2) C33 0.021(3) 0.014(3) 0.015(2) -0.0061(18) 0.009(2) 0.001(2) C34 0.021(3) 0.014(3) 0.015(2) -0.0061(18) 0.009(2) 0.001(2) C35 0.021(3) 0.014(3) 0.015(2) -0.0061(18) 0.009(2) 0.001(2) C36 0.021(3) 0.014(3) 0.015(2) -0.0061(18) 0.009(2) 0.001(2) O8 0.032(3) 0.019(2) 0.026(2) -0.0041(17) 0.001(2) -0.0068(18) C37 0.032(3) 0.019(2) 0.026(2) -0.0041(17) 0.001(2) -0.0068(18) C38 0.032(3) 0.019(2) 0.026(2) -0.0041(17) 0.001(2) -0.0068(18) C39 0.032(3) 0.019(2) 0.026(2) -0.0041(17) 0.001(2) -0.0068(18) C40 0.032(3) 0.019(2) 0.026(2) -0.0041(17) 0.001(2) -0.0068(18) C41 0.032(3) 0.019(2) 0.026(2) -0.0041(17) 0.001(2) -0.0068(18) C42 0.032(3) 0.019(2) 0.026(2) -0.0041(17) 0.001(2) -0.0068(18) O9 0.046(6) 0.047(6) 0.053(6) -0.003(4) 0.005(4) -0.012(5) C43 0.044(7) 0.040(6) 0.052(6) -0.011(5) 0.013(5) 0.015(5) C44 0.082(10) 0.043(7) 0.069(8) -0.007(5) 0.026(7) 0.008(6) C45 0.077(10) 0.052(7) 0.063(8) -0.015(6) 0.034(6) -0.015(7) C46 0.042(7) 0.061(8) 0.064(8) -0.008(6) 0.009(6) -0.017(7) O10 0.048(7) 0.020(5) 0.055(6) -0.017(4) -0.007(5) 0.018(5) C47 0.028(6) 0.025(6) 0.055(7) 0.003(5) 0.008(6) 0.005(5) C48 0.059(10) 0.029(7) 0.102(11) -0.017(7) 0.003(8) 0.020(7) C49 0.050(9) 0.031(7) 0.081(9) -0.027(6) 0.018(7) 0.012(6) C50 0.034(8) 0.030(7) 0.057(7) -0.022(5) -0.001(6) 0.011(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 89.2(3) 7_565 . ? N1 Ni1 N2 91.1(2) . . ? N1 Ni1 N2 179.7(2) 7_565 . ? N1 Ni1 N2 91.1(2) 7_565 7_565 ? N1 Ni1 N2 179.7(2) . 7_565 ? N2 Ni1 N2 88.7(3) . 7_565 ? C1 O1 C1 119.3(7) . 7_565 ? C9 O2 C9 118.8(6) 7_565 . ? C1 N1 Ni1 127.2(4) . . ? C1 N1 C4 104.1(5) . . ? C4 N1 Ni1 128.7(4) . . ? C6 N2 Ni1 127.6(4) . . ? C9 N2 Ni1 128.1(4) . . ? C9 N2 C6 104.2(5) . . ? O1 C1 C2 118.3(5) . . ? N1 C1 O1 127.7(6) . . ? N1 C1 C2 114.1(5) . . ? C1 C2 H2 128.7 . . ? C3 C2 C1 102.6(6) . . ? C3 C2 H2 128.7 . . ? C2 C3 H3 124.8 . . ? C2 C3 C4 110.5(6) . . ? C4 C3 H3 124.8 . . ? N1 C4 C3 108.7(5) . . ? N1 C4 C5 123.7(5) . . ? C5 C4 C3 127.6(6) . . ? C4 C5 C16 116.4(6) . . ? C4 C5 C10 115.6(6) . . ? C6 C5 C4 125.1(5) . . ? C6 C5 C16 118.4(6) . . ? C6 C5 C10 119.3(6) . . ? C5 C6 N2 123.3(5) . . ? C5 C6 C7 129.8(5) . . ? C7 C6 N2 106.8(5) . . ? C6 C7 H7 126.0 . . ? C8 C7 C6 108.1(5) . . ? C8 C7 H7 126.0 . . ? C7 C8 H8 127.6 . . ? C7 C8 C9 104.9(5) . . ? C9 C8 H8 127.6 . . ? O2 C9 C8 116.7(5) . . ? N2 C9 O2 127.4(6) . . ? N2 C9 C8 115.9(5) . . ? C19 O4 H4 109.5 . . ? C17 C16 C5 117.9(5) . . ? C17 C16 C21 120.0 . . ? C21 C16 C5 122.1(5) . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? O4 C19 C18 119.1(8) . . ? O4 C19 C20 119.9(8) . . ? C20 C19 C18 120.0 . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 120.0 . . ? C21 C20 H20 120.0 . . ? C16 C21 H21 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 H21 120.0 . . ? C13 O3 H3A 109.5 . . ? C11 C10 C5 119.2(5) . . ? C11 C10 C15 120.0 . . ? C15 C10 C5 120.8(5) . . ? C10 C11 H11 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 H12 120.0 . . ? C11 C12 C13 120.0 . . ? C13 C12 H12 120.0 . . ? O3 C13 C12 114.6(7) . . ? O3 C13 C14 125.3(7) . . ? C14 C13 C12 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C10 C15 H15 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15 120.0 . . ? N3 Ni2 N3 89.4(3) . 7_565 ? N3 Ni2 N4 179.6(2) 7_565 . ? N3 Ni2 N4 91.0(2) 7_565 7_565 ? N3 Ni2 N4 179.6(2) . 7_565 ? N3 Ni2 N4 91.0(2) . . ? N4 Ni2 N4 88.6(3) 7_565 . ? C22 O5 C22 125.7(7) 7_565 . ? C30 O6 C30 123.8(7) 7_565 . ? C22 N3 Ni2 128.1(4) . . ? C22 N3 C25 102.4(5) . . ? C25 N3 Ni2 129.4(4) . . ? C27 N4 Ni2 128.1(4) . . ? C30 N4 Ni2 129.0(4) . . ? C30 N4 C27 102.9(5) . . ? O5 C22 N3 123.9(6) . . ? O5 C22 C23 122.6(6) . . ? N3 C22 C23 113.5(5) . . ? C22 C23 H23 127.7 . . ? C24 C23 C22 104.6(5) . . ? C24 C23 H23 127.7 . . ? C23 C24 H24 126.2 . . ? C23 C24 C25 107.6(5) . . ? C25 C24 H24 126.2 . . ? N3 C25 C24 111.9(5) . . ? N3 C25 C26 124.1(5) . . ? C24 C25 C26 124.0(5) . . ? C25 C26 C31 116.9(7) . . ? C25 C26 C37 119.4(7) . . ? C27 C26 C25 122.1(6) . . ? C27 C26 C31 120.8(7) . . ? C27 C26 C37 118.3(7) . . ? N4 C27 C28 109.8(5) . . ? C26 C27 N4 124.6(6) . . ? C26 C27 C28 125.4(6) . . ? C27 C28 H28 126.9 . . ? C29 C28 C27 106.2(5) . . ? C29 C28 H28 126.9 . . ? C28 C29 H29 126.9 . . ? C30 C29 C28 106.2(6) . . ? C30 C29 H29 126.9 . . ? O6 C30 N4 124.1(5) . . ? O6 C30 C29 121.0(6) . . ? C29 C30 N4 114.9(5) . . ? C34 O7 H7A 109.5 . . ? C32 C31 C26 118.4(5) . . ? C32 C31 C36 120.0 . . ? C36 C31 C26 121.2(5) . . ? C31 C32 H32 120.0 . . ? C31 C32 C33 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? O7 C34 C33 119.8(7) . . ? O7 C34 C35 120.2(7) . . ? C33 C34 C35 120.0 . . ? C34 C35 H35 120.0 . . ? C34 C35 C36 120.0 . . ? C36 C35 H35 120.0 . . ? C31 C36 H36 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C40 O8 H8A 109.5 . . ? C38 C37 C26 118.9(8) . . ? C42 C37 C26 123.2(9) . . ? C42 C37 C38 117.7(9) . . ? C37 C38 H38 119.2 . . ? C39 C38 C37 121.6(9) . . ? C39 C38 H38 119.2 . . ? C38 C39 H39 120.7 . . ? C38 C39 C40 118.6(9) . . ? C40 C39 H39 120.7 . . ? O8 C40 C39 120.4(8) . . ? O8 C40 C41 118.7(8) . . ? C41 C40 C39 120.9(8) . . ? C40 C41 H41 120.4 . . ? C40 C41 C42 119.2(9) . . ? C42 C41 H41 120.4 . . ? C37 C42 H42 119.1 . . ? C41 C42 C37 121.8(9) . . ? C41 C42 H42 119.1 . . ? C43 O9 C46 109.1(11) . . ? O9 C43 H43A 111.1 . . ? O9 C43 H43B 111.1 . . ? O9 C43 C44 103.2(10) . . ? H43A C43 H43B 109.1 . . ? C44 C43 H43A 111.1 . . ? C44 C43 H43B 111.1 . . ? C43 C44 H44A 111.1 . . ? C43 C44 H44B 111.1 . . ? C43 C44 C45 103.5(11) . . ? H44A C44 H44B 109.0 . . ? C45 C44 H44A 111.1 . . ? C45 C44 H44B 111.1 . . ? C44 C45 H45A 110.6 . . ? C44 C45 H45B 110.6 . . ? H45A C45 H45B 108.8 . . ? C46 C45 C44 105.5(11) . . ? C46 C45 H45A 110.6 . . ? C46 C45 H45B 110.6 . . ? O9 C46 C45 103.8(12) . . ? O9 C46 H46A 111.0 . . ? O9 C46 H46B 111.0 . . ? C45 C46 H46A 111.0 . . ? C45 C46 H46B 111.0 . . ? H46A C46 H46B 109.0 . . ? C50 O10 C47 105.2(10) . . ? O10 C47 H47A 110.5 . . ? O10 C47 H47B 110.4 . . ? O10 C47 C48 106.4(12) . . ? H47A C47 H47B 108.6 . . ? C48 C47 H47A 110.5 . . ? C48 C47 H47B 110.4 . . ? C47 C48 H48A 110.8 . . ? C47 C48 H48B 110.8 . . ? C47 C48 C49 104.6(11) . . ? H48A C48 H48B 108.9 . . ? C49 C48 H48A 110.8 . . ? C49 C48 H48B 110.8 . . ? C48 C49 H49A 111.2 . . ? C48 C49 H49B 111.2 . . ? C48 C49 C50 103.0(11) . . ? H49A C49 H49B 109.1 . . ? C50 C49 H49A 111.2 . . ? C50 C49 H49B 111.2 . . ? O10 C50 C49 104.6(12) . . ? O10 C50 H50A 110.8 . . ? O10 C50 H50B 110.8 . . ? C49 C50 H50A 110.8 . . ? C49 C50 H50B 110.8 . . ? H50A C50 H50B 108.9 . . ? 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 1.913(5) 7_565 ? Ni1 N1 1.913(5) . ? Ni1 N2 1.945(5) . ? Ni1 N2 1.945(5) 7_565 ? O1 C1 1.348(7) . ? O1 C1 1.348(7) 7_565 ? O2 C9 1.393(6) . ? O2 C9 1.393(6) 7_565 ? N1 C1 1.305(7) . ? N1 C4 1.401(7) . ? N2 C6 1.434(7) . ? N2 C9 1.280(8) . ? C1 C2 1.462(8) . ? C2 H2 0.9500 . ? C2 C3 1.319(10) . ? C3 H3 0.9500 . ? C3 C4 1.411(8) . ? C4 C5 1.403(8) . ? C5 C6 1.360(8) . ? C5 C16 1.525(8) . ? C5 C10 1.524(7) . ? C6 C7 1.433(8) . ? C7 H7 0.9500 . ? C7 C8 1.340(9) . ? C8 H8 0.9500 . ? C8 C9 1.395(8) . ? O4 H4 0.8400 . ? O4 C19 1.389(11) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 H17 0.9500 . ? C17 C18 1.3900 . ? C18 H18 0.9500 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 H20 0.9500 . ? C20 C21 1.3900 . ? C21 H21 0.9500 . ? O3 H3A 0.8400 . ? O3 C13 1.385(10) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 H11 0.9500 . ? C11 C12 1.3900 . ? C12 H12 0.9500 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 H14 0.9500 . ? C14 C15 1.3900 . ? C15 H15 0.9500 . ? Ni2 N3 1.879(5) . ? Ni2 N3 1.879(5) 7_565 ? Ni2 N4 1.914(5) 7_565 ? Ni2 N4 1.914(5) . ? O5 C22 1.297(6) 7_565 ? O5 C22 1.297(6) . ? O6 C30 1.337(6) 7_565 ? O6 C30 1.337(6) . ? N3 C22 1.387(8) . ? N3 C25 1.392(7) . ? N4 C27 1.419(7) . ? N4 C30 1.375(8) . ? C22 C23 1.416(8) . ? C23 H23 0.9500 . ? C23 C24 1.385(8) . ? C24 H24 0.9500 . ? C24 C25 1.407(8) . ? C25 C26 1.426(8) . ? C26 C27 1.357(8) . ? C26 C31 1.480(8) . ? C26 C37 1.474(11) . ? C27 C28 1.419(8) . ? C28 H28 0.9500 . ? C28 C29 1.412(8) . ? C29 H29 0.9500 . ? C29 C30 1.346(8) . ? O7 H7A 0.8400 . ? O7 C34 1.369(10) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 H32 0.9500 . ? C32 C33 1.3900 . ? C33 H33 0.9500 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 H35 0.9500 . ? C35 C36 1.3900 . ? C36 H36 0.9500 . ? O8 H8A 0.8400 . ? O8 C40 1.368(11) . ? C37 C38 1.398(12) . ? C37 C42 1.396(12) . ? C38 H38 0.9500 . ? C38 C39 1.397(11) . ? C39 H39 0.9500 . ? C39 C40 1.401(11) . ? C40 C41 1.381(12) . ? C41 H41 0.9500 . ? C41 C42 1.393(11) . ? C42 H42 0.9500 . ? O9 C43 1.431(13) . ? O9 C46 1.444(14) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.523(14) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.556(16) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.535(15) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? O10 C47 1.458(18) . ? O10 C50 1.423(19) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C48 1.526(15) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C48 C49 1.534(16) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C49 C50 1.538(14) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? 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 O1 -1.2(10) . . . . ? Ni1 N1 C1 C2 178.0(4) . . . . ? Ni1 N1 C4 C3 -177.2(4) . . . . ? Ni1 N1 C4 C5 5.1(8) . . . . ? Ni1 N2 C6 C5 -3.3(8) . . . . ? Ni1 N2 C6 C7 179.1(4) . . . . ? Ni1 N2 C9 O2 -0.5(9) . . . . ? Ni1 N2 C9 C8 179.6(4) . . . . ? O1 C1 C2 C3 179.8(7) . . . . ? N1 C1 C2 C3 0.5(8) . . . . ? N1 C4 C5 C6 1.4(9) . . . . ? N1 C4 C5 C16 -179.3(5) . . . . ? N1 C4 C5 C10 -179.3(6) . . . . ? N2 C6 C7 C8 3.1(6) . . . . ? C1 O1 C1 N1 12.9(14) 7_565 . . . ? C1 O1 C1 C2 -166.3(5) 7_565 . . . ? C1 N1 C4 C3 2.8(7) . . . . ? C1 N1 C4 C5 -174.9(6) . . . . ? C1 C2 C3 C4 1.3(8) . . . . ? C2 C3 C4 N1 -2.7(8) . . . . ? C2 C3 C4 C5 174.9(6) . . . . ? C3 C4 C5 C6 -175.9(6) . . . . ? C3 C4 C5 C16 3.5(9) . . . . ? C3 C4 C5 C10 3.4(9) . . . . ? C4 N1 C1 O1 178.8(7) . . . . ? C4 N1 C1 C2 -2.1(7) . . . . ? C4 C5 C6 N2 -2.2(9) . . . . ? C4 C5 C6 C7 174.9(6) . . . . ? C4 C5 C16 C17 -63.9(7) . . . . ? C4 C5 C16 C21 116.6(7) . . . . ? C4 C5 C10 C11 -104.0(7) . . . . ? C4 C5 C10 C15 75.7(8) . . . . ? C5 C6 C7 C8 -174.4(6) . . . . ? C5 C16 C17 C18 -179.5(7) . . . . ? C5 C16 C21 C20 179.5(8) . . . . ? C5 C10 C11 C12 179.7(8) . . . . ? C5 C10 C15 C14 -179.7(8) . . . . ? C6 N2 C9 O2 -178.9(6) . . . . ? C6 N2 C9 C8 1.1(7) . . . . ? C6 C5 C16 C17 115.5(6) . . . . ? C6 C5 C16 C21 -64.0(8) . . . . ? C6 C5 C10 C11 75.4(8) . . . . ? C6 C5 C10 C15 -104.9(7) . . . . ? C6 C7 C8 C9 -2.4(6) . . . . ? C7 C8 C9 O2 -179.2(5) . . . . ? C7 C8 C9 N2 0.8(7) . . . . ? C9 O2 C9 N2 -10.9(11) 7_565 . . . ? C9 O2 C9 C8 169.1(4) 7_565 . . . ? C9 N2 C6 C5 175.2(5) . . . . ? C9 N2 C6 C7 -2.5(6) . . . . ? O4 C19 C20 C21 168.7(9) . . . . ? C16 C5 C6 N2 178.4(5) . . . . ? C16 C5 C6 C7 -4.4(9) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C16 C21 C20 0.0 . . . . ? C17 C18 C19 O4 -168.8(9) . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C16 0.0 . . . . ? C21 C16 C17 C18 0.0 . . . . ? O3 C13 C14 C15 -175.4(10) . . . . ? C10 C5 C6 N2 178.6(6) . . . . ? C10 C5 C6 C7 -4.3(9) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? C11 C12 C13 O3 175.9(9) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C15 C10 C11 C12 0.0 . . . . ? Ni2 N3 C22 O5 -1.3(9) . . . . ? Ni2 N3 C22 C23 178.8(4) . . . . ? Ni2 N3 C25 C24 -178.5(4) . . . . ? Ni2 N3 C25 C26 -0.7(9) . . . . ? Ni2 N4 C27 C26 5.2(9) . . . . ? Ni2 N4 C27 C28 -179.3(4) . . . . ? Ni2 N4 C30 O6 -1.8(9) . . . . ? Ni2 N4 C30 C29 179.9(4) . . . . ? O5 C22 C23 C24 -179.7(6) . . . . ? N3 Ni2 N3 C22 6.5(6) 7_565 . . . ? N3 Ni2 N3 C25 -174.0(4) 7_565 . . . ? N3 C22 C23 C24 0.3(7) . . . . ? N3 C25 C26 C27 -5.2(10) . . . . ? N3 C25 C26 C31 -179.9(6) . . . . ? N3 C25 C26 C37 179.7(6) . . . . ? N4 Ni2 N3 C22 -173.7(5) . . . . ? N4 Ni2 N3 C25 5.9(5) . . . . ? N4 C27 C28 C29 0.3(7) . . . . ? C22 O5 C22 N3 -7.4(13) 7_565 . . . ? C22 O5 C22 C23 172.6(5) 7_565 . . . ? C22 N3 C25 C24 1.1(7) . . . . ? C22 N3 C25 C26 179.0(6) . . . . ? C22 C23 C24 C25 0.4(7) . . . . ? C23 C24 C25 N3 -1.0(7) . . . . ? C23 C24 C25 C26 -178.9(6) . . . . ? C24 C25 C26 C27 172.4(6) . . . . ? C24 C25 C26 C31 -2.3(9) . . . . ? C24 C25 C26 C37 -2.7(10) . . . . ? C25 N3 C22 O5 179.1(6) . . . . ? C25 N3 C22 C23 -0.8(7) . . . . ? C25 C26 C27 N4 2.8(10) . . . . ? C25 C26 C27 C28 -171.9(6) . . . . ? C25 C26 C31 C32 -114.7(7) . . . . ? C25 C26 C31 C36 72.9(9) . . . . ? C25 C26 C37 C38 -67.3(13) . . . . ? C25 C26 C37 C42 117.6(12) . . . . ? C26 C27 C28 C29 175.6(6) . . . . ? C26 C31 C32 C33 -172.4(10) . . . . ? C26 C31 C36 C35 172.2(10) . . . . ? C26 C37 C38 C39 -179.2(10) . . . . ? C26 C37 C42 C41 179.1(10) . . . . ? C27 N4 C30 O6 -179.9(6) . . . . ? C27 N4 C30 C29 1.8(7) . . . . ? C27 C26 C31 C32 70.5(9) . . . . ? C27 C26 C31 C36 -101.9(8) . . . . ? C27 C26 C37 C38 117.3(12) . . . . ? C27 C26 C37 C42 -57.7(14) . . . . ? C27 C28 C29 C30 0.8(7) . . . . ? C28 C29 C30 O6 180.0(6) . . . . ? C28 C29 C30 N4 -1.7(7) . . . . ? C30 O6 C30 N4 12.8(12) 7_565 . . . ? C30 O6 C30 C29 -169.0(5) 7_565 . . . ? C30 N4 C27 C26 -176.6(6) . . . . ? C30 N4 C27 C28 -1.2(6) . . . . ? O7 C34 C35 C36 -179.9(11) . . . . ? C31 C26 C27 N4 177.3(6) . . . . ? C31 C26 C27 C28 2.6(10) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? C32 C33 C34 O7 179.9(11) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C36 C31 C32 C33 0.0 . . . . ? O8 C40 C41 C42 -177.8(11) . . . . ? C37 C26 C27 N4 178.0(6) . . . . ? C37 C26 C27 C28 3.3(10) . . . . ? C37 C38 C39 C40 3.1(18) . . . . ? C38 C37 C42 C41 4.0(18) . . . . ? C38 C39 C40 O8 178.0(12) . . . . ? C38 C39 C40 C41 -2.4(19) . . . . ? C39 C40 C41 C42 2.6(19) . . . . ? C40 C41 C42 C37 -3.4(18) . . . . ? C42 C37 C38 C39 -3.9(18) . . . . ? O9 C43 C44 C45 30.5(16) . . . . ? C43 O9 C46 C45 32.7(18) . . . . ? C43 C44 C45 C46 -11.6(18) . . . . ? C44 C45 C46 O9 -11.4(19) . . . . ? C46 O9 C43 C44 -40.6(16) . . . . ? O10 C47 C48 C49 -11(2) . . . . ? C47 O10 C50 C49 -41.5(17) . . . . ? C47 C48 C49 C50 -13(2) . . . . ? C48 C49 C50 O10 33.2(19) . . . . ? C50 O10 C47 C48 33.2(19) . . . . ?