# ic980672e.cif _audit_creation_date 98-00-08 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? Synthesized in the laboratory _chemical_name_systematic ? _chemical_name_common ? chemical_formula_analytical ? C54 H68 N8 O5 Ni _chemical_formula_moiety ? "Ni C38 N6 O4 H26 2-, C16 N2 H40 2+" O H2 _chemical_formula_structural ? (Ni(C19 N3 O2 H13)(C19 N3 O2 H13)) ((N C8 H20)(N C8 H20))(O H2)) _chemical_formula_sum ? C54 H68 N8 O5 Ni _chemical_formula_weight ? 966.69 _chemical_melting_point ? decompose above 300 degree celcius _computing_data_collection ? #ActaC _computing_cell_refinement ? #ActaC _computing_data_reduction xtal_DIFDAT_SORTRF_ADDREF_ABSORB #ActaC _computing_structure_solution xtal_SIMPEL #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 10.175(2) #ActaC _cell_length_b 20.834(3) #ActaC _cell_length_c 23.765(4) #ActaC _cell_angle_alpha 90.00(1) #ActaC _cell_angle_beta 90.00(2) #ActaC _cell_angle_gamma 90.00(2) #ActaC _cell_volume 5038(1) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 25 #ActaC _cell_measurement_theta_min 16 #ActaC _cell_measurement_theta_max 28 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting orthorhombic #ActaC _symmetry_space_group_name_H-M Pccn #ActaC _symmetry_space_group_name_Hall -P_2ab_2ac #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2-x,1/2-y,+z 1/2+x,-y,1/2-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2+y,-z 1/2-x,+y,1/2+z +x,1/2-y,1/2+z _exptl_crystal_description Block shaped #ActaC _exptl_crystal_preparation Ethyl acetate diffusion to acetonitrile solution _exptl_crystal_colour Yellowish brown _exptl_crystal_size_max 0.3 mm #ActaC _exptl_crystal_size_mid 0.2 mm #ActaC _exptl_crystal_size_min 0.1 mm #ActaC _exptl_crystal_density_diffrn 1.276 #ActaC _exptl_crystal_density_meas 1.281 #ActaC _exptl_crystal_density_method flotation #ActaC _exptl_crystal_F_000 2063.58 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 0.44 #ActaC _exptl_absorpt_correction_type analytical #ActaC _exptl_absorpt_correction_T_min 0.8221 #ActaC _exptl_absorpt_correction_T_max 0.8229 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo K- alpha #ActaC _diffrn_radiation_source sealed xray_tube #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector proportional counter #ActaC _diffrn_measurement_device CAD4mach #ActaC _diffrn_measurement_method theta-2theta #ActaC _diffrn_standards_number three #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time every hour #ActaC _diffrn_standards_decay_% 0.69% #ActaC loop_ _diffrn_standard_refln_index_h 2 -4 -6 #ActaC _diffrn_standard_refln_index_k -2 1 -6 #ActaC _diffrn_standard_refln_index_l 1 -3 -6 #ActaC ? ? ? loop_ _diffrn_attenuator_code 13.364 _diffrn_attenuator_scale ? ? _diffrn_reflns_number 4954 #ActaC _diffrn_reflns_av_R_equivalents 0.069 #ActaC _diffrn_reflns_av_sigmaI/netI .108 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 12 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 24 #ActaC _diffrn_reflns_limit_l_min 0 #ActaC _diffrn_reflns_limit_l_max 28 #ActaC _diffrn_reflns_theta_min 1.71 #ActaC _diffrn_reflns_theta_max 24.97 #ActaC _diffrn_reflns_reduction_process No_monochr_Lp_applied #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC c ? 0 216 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 h ? 0 272 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 n ? 0 32 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 o ? 0 20 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ni ? 0 4 .285 1.113 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ni .25000 .25000 .43172(7) .0328(9) Uani ? ? N1 .3573(8) .2989(4) .4954(3) .037(6) Uani ? ? N2 .4211(7) .2035(3) .4349(4) .035(5) Uani ? ? N3 .2278(9) .1794(4) .3673(3) .037(6) Uani ? ? O1 .5462(7) .2932(3) .5493(3) .067(6) Uani ? ? O2 .3489(6) .0987(3) .3214(3) .050(5) Uani ? ? C1 .2965(9) .3469(5) .5283(4) .035(7) Uani ? ? C2 .268(2) .3413(5) .5837(5) .063(9) Uani ? ? C3 .198(1) .3868(7) .6139(5) .08(1) Uani ? ? C4 .159(2) .4394(8) .5872(7) .10(1) Uani ? ? C5 .173(1) .4461(6) .5314(6) .09(1) Uani ? ? C6 .249(2) .4010(5) .5028(4) .067(8) Uani ? ? C7 .471(1) .2750(5) .5105(5) .042(8) Uani ? ? C8 .508(1) .2188(5) .4735(5) .037(7) Uani ? ? C9 .628(1) .1866(5) .4787(5) .049(8) Uani ? ? C10 .649(1) .1366(5) .4416(5) .055(8) Uani ? ? C11 .559(1) .1212(5) .4009(5) .058(9) Uani ? ? C12 .444(1) .1554(4) .3990(4) .033(7) Uani ? ? C13 .333(1) .1422(5) .3573(4) .038(8) Uani ? ? C14 .122(1) .1777(4) .3302(5) .040(8) Uani ? ? C15 -.004(1) .1792(5) .3529(5) .057(9) Uani ? ? C16 -.113(1) .1850(6) .3191(6) .070(9) Uani ? ? C17 -.100(1) .1894(6) .2621(6) .07(1) Uani ? ? C18 .022(2) .1875(6) .2391(5) .07(1) Uani ? ? C19 .133(1) .1803(5) .2718(5) .051(8) Uani ? ? O3 .75000 .25000 .6185(4) .089(8) Uani ? ? N4 .615(1) .4482(5) .6682(4) .056(7) Uani ? ? C20 .696(1) .4664(7) .7177(6) .10(1) Uani ? ? C21 .572(1) .5109(6) .6417(7) .11(1) Uani ? ? C22 .499(1) .4071(6) .6835(7) .11(1) Uani ? ? C23 .699(2) .4117(7) .6290(7) .11(1) Uani ? ? C24 .638(2) .4979(8) .7654(6) .18(2) Uani ? ? C25 .499(2) .5052(8) .5852(9) .21(2) Uani ? ? C26 .525(1) .3474(6) .7100(6) .11(1) Uani ? ? C27 .805(2) .4402(8) .6017(7) .15(2) Uani ? ? H2 .30163 .30318 .60487 .03800 Uani ? ? H3 .18402 .38514 .65727 .03800 Uani ? ? H4 .09289 .46724 .60903 .03800 Uani ? ? H5 .14209 .49056 .51711 .03800 Uani ? ? H6 .26096 .40970 .46187 .03800 Uani ? ? H9 .69291 .19509 .50835 .03800 Uani ? ? H10 .73428 .11162 .44089 .03800 Uani ? ? H11 .57853 .08689 .37262 .03800 Uani ? ? H15 -.02324 .17559 .39187 .03800 Uani ? ? H16 -.20225 .18716 .33049 .03800 Uani ? ? H17 -.17527 .19069 .23495 .03800 Uani ? ? H18 .02995 .18903 .19707 .03800 Uani ? ? H19 .21968 .17624 .25292 .03800 Uani ? ? H201 .77423 .49402 .71011 .03800 Uani ? ? H202 .74172 .42899 .73709 .03800 Uani ? ? H211 .64651 .53930 .64134 .03800 Uani ? ? H212 .51431 .53122 .67164 .03800 Uani ? ? H221 .45399 .39815 .64799 .03800 Uani ? ? H222 .43990 .43281 .70466 .03800 Uani ? ? H231 .64339 .39411 .59854 .03800 Uani ? ? H232 .73490 .37309 .64830 .03800 Uani ? ? H241 .55568 .47106 .77559 .03800 Uani ? ? H242 .58888 .53748 .74804 .03800 Uani ? ? H243 .67866 .50996 .79587 .03800 Uani ? ? H251 .42973 .47575 .59408 .03800 Uani ? ? H252 .56475 .48400 .56314 .03800 Uani ? ? H253 .47617 .54401 .57490 .03800 Uani ? ? H261 .56812 .35681 .74701 .03800 Uani ? ? H262 .58250 .32141 .68914 .03800 Uani ? ? H263 .44861 .32124 .72070 .03800 Uani ? ? H271 .86647 .45793 .63149 .03800 Uani ? ? H272 .77496 .47895 .58173 .03800 Uani ? ? H1w .73159 .21692 .62500 .03800 Uani ? ? H273 .86187 .41800 .57636 .03800 Uani ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ni .0298(9) .0321(9) .0365(9) .003(2) .00000 .00000 N1 .033(6) .038(5) .039(6) .014(5) -.002(5) -.009(5) N2 .030(5) .028(5) .046(5) .005(4) -.004(6) .006(5) N3 .031(7) .039(5) .041(5) .000(5) -.004(6) -.002(4) O1 .048(5) .083(6) .071(6) .005(5) -.024(5) -.030(5) O2 .054(5) .040(4) .057(5) .003(4) -.001(5) -.014(4) C1 .033(8) .031(7) .040(7) -.009(6) -.015(6) .002(6) C2 .08(1) .055(7) .057(9) -.006(9) -.002(9) -.009(6) C3 .07(1) .10(1) .07(1) -.014(9) .024(9) -.04(1) C4 .09(1) .11(1) .11(1) .06(1) -.01(1) -.04(1) C5 .13(1) .050(9) .08(1) .023(9) -.03(1) -.008(9) C6 .10(1) .052(7) .049(7) .01(1) .01(1) -.017(7) C7 .048(9) .032(7) .046(8) -.003(6) -.003(7) .001(6) C8 .027(7) .041(7) .043(7) .004(6) .004(6) .002(6) C9 .027(7) .060(8) .059(8) .002(7) -.012(7) -.006(7) C10 .036(7) .058(8) .073(9) .027(6) -.021(8) -.015(8) C11 .054(9) .058(8) .063(9) .022(7) .008(8) -.011(7) C12 .033(7) .028(6) .037(7) .009(6) .007(6) .005(6) C13 .049(9) .026(7) .039(8) -.005(6) -.010(7) .005(6) C14 .047(8) .021(6) .05(1) -.001(6) -.004(7) .001(6) C15 .055(9) .051(8) .064(9) -.012(8) -.002(9) -.003(7) C16 .040(8) .09(1) .08(1) -.009(7) -.01(1) .00(1) C17 .06(1) .059(9) .09(1) .010(8) -.038(9) -.004(8) C18 .09(1) .07(1) .051(9) .01(1) -.01(1) -.003(8) C19 .048(9) .060(9) .047(8) .004(8) -.006(7) .004(7) O3 .128(9) .056(6) .082(8) .02(1) .00000 .00000 N4 .050(7) .076(7) .044(7) -.000(6) .005(6) -.019(6) C20 .10(2) .10(1) .10(1) -.03(1) -.01(1) -.00(1) C21 .08(1) .055(9) .19(2) .017(9) -.04(1) .02(1) C22 .048(9) .10(1) .18(2) -.006(9) .00(1) .03(1) C23 .13(2) .08(1) .13(1) -.01(1) .05(1) -.01(1) C24 .31(3) .16(2) .07(1) -.12(2) .06(1) -.04(1) C25 .14(2) .16(2) .35(3) -.05(1) -.12(2) .15(2) C26 .11(1) .07(1) .15(2) .02(1) .05(1) .04(1) C27 .15(2) .15(2) .15(2) .06(1) .07(1) .03(1) H2 .03800 .03800 .03800 .00000 .00000 .00000 H3 .03800 .03800 .03800 .00000 .00000 .00000 H4 .03800 .03800 .03800 .00000 .00000 .00000 H5 .03800 .03800 .03800 .00000 .00000 .00000 H6 .03800 .03800 .03800 .00000 .00000 .00000 H9 .03800 .03800 .03800 .00000 .00000 .00000 H10 .03800 .03800 .03800 .00000 .00000 .00000 H11 .03800 .03800 .03800 .00000 .00000 .00000 H15 .03800 .03800 .03800 .00000 .00000 .00000 H16 .03800 .03800 .03800 .00000 .00000 .00000 H17 .03800 .03800 .03800 .00000 .00000 .00000 H18 .03800 .03800 .03800 .00000 .00000 .00000 H19 .03800 .03800 .03800 .00000 .00000 .00000 H201 .03800 .03800 .03800 .00000 .00000 .00000 H202 .03800 .03800 .03800 .00000 .00000 .00000 H211 .03800 .03800 .03800 .00000 .00000 .00000 H212 .03800 .03800 .03800 .00000 .00000 .00000 H221 .03800 .03800 .03800 .00000 .00000 .00000 H222 .03800 .03800 .03800 .00000 .00000 .00000 H231 .03800 .03800 .03800 .00000 .00000 .00000 H232 .03800 .03800 .03800 .00000 .00000 .00000 H241 .03800 .03800 .03800 .00000 .00000 .00000 H242 .03800 .03800 .03800 .00000 .00000 .00000 H243 .03800 .03800 .03800 .00000 .00000 .00000 H251 .03800 .03800 .03800 .00000 .00000 .00000 H252 .03800 .03800 .03800 .00000 .00000 .00000 H253 .03800 .03800 .03800 .00000 .00000 .00000 H261 .03800 .03800 .03800 .00000 .00000 .00000 H262 .03800 .03800 .03800 .00000 .00000 .00000 H263 .03800 .03800 .03800 .00000 .00000 .00000 H271 .03800 .03800 .03800 .00000 .00000 .00000 H272 .03800 .03800 .03800 .00000 .00000 .00000 H1w .03800 .03800 .03800 .00000 .00000 .00000 H273 .03800 .03800 .03800 .00000 .00000 .00000 _atom_sites_solution_primary Ni, N _atom_sites_solution_secondary rest non-hydrogen atoms _atom_sites_solution_hydrogens positions calculated _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment no #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression no _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 1509 #ActaC _refine_ls_number_parameters 308 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .212 #ActaC _refine_ls_R_factor_obs .069 #ActaC _refine_ls_wR_factor_all .058 #ActaC _refine_ls_wR_factor_obs .044 #ActaC _refine_ls_goodness_of_fit_all 1.407 #ActaC _refine_ls_goodness_of_fit_obs 1.99 #ActaC _refine_ls_shift/esd_max . #ActaC _refine_ls_shift/esd_mean 0 #ActaC _refine_diff_density_min -2.598 #ActaC _refine_diff_density_max .961 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ni N1 2.127(8) 5_666 6_556 ? Ni N2 1.994(7) 5_666 6_556 ? Ni N3 2.135(8) 5_666 6_556 ? Ni N1 2.127(8) 5_666 5_666 ? Ni N2 1.994(7) 5_666 5_666 ? Ni N3 2.135(8) 5_666 5_666 ? N4 C20 1.49(2) . . ? N4 C21 1.52(2) . . ? N4 C22 1.51(2) . . ? N4 C23 1.47(2) . . ? C20 C24 1.44(2) . . ? C20 H201 1.00(1) . . ? C20 H202 1.02(1) . . ? C21 C25 1.54(3) . . ? C21 H211 .96(1) . . ? C21 H212 1.02(1) . . ? C22 C26 1.42(2) . . ? C22 H221 .98(2) . . ? C22 H222 .95(1) . . ? C23 C27 1.39(2) . . ? C23 H231 .99(2) . . ? C23 H232 1.00(1) . . ? C24 H241 1.04(2) . . ? C24 H242 1.05(2) . . ? C24 H243 .87(2) . . ? C25 H251 .96(2) . . ? C25 H252 .96(2) . . ? C25 H253 .88(2) . . ? C26 H261 1.00(1) . . ? C26 H262 .94(1) . . ? C26 H263 .98(1) . . ? C27 H271 1.01(2) . . ? C27 H272 .98(2) . . ? C27 H273 .96(2) . . ? Ni N2 1.994(7) 5_666 6_556 ? Ni N2 1.994(7) 5_666 5_666 ? N1 C1 1.41(1) 6_556 6_556 ? N1 C7 1.31(1) 6_556 6_556 ? N2 C8 1.32(1) 6_556 6_556 ? N2 C12 1.34(1) 6_556 6_556 ? N3 C13 1.35(1) 6_556 6_556 ? N3 C14 1.39(1) 6_556 6_556 ? O1 C7 1.26(1) 6_556 6_556 ? O2 C13 1.25(1) 6_556 6_556 ? C1 C2 1.35(2) 6_556 6_556 ? C1 C6 1.37(2) 6_556 6_556 ? C2 C3 1.39(2) 6_556 6_556 ? C2 H2 1.00(1) 6_556 6_556 ? C3 C4 1.33(2) 6_556 6_556 ? C3 H3 1.04(1) 6_556 6_556 ? C4 C5 1.34(2) 6_556 6_556 ? C4 H4 1.03(2) 6_556 6_556 ? C5 C6 1.39(2) 6_556 6_556 ? C5 H5 1.04(1) 6_556 6_556 ? C6 H6 1.00(1) 6_556 6_556 ? C7 C8 1.51(1) 6_556 6_556 ? C8 C9 1.39(1) 6_556 6_556 ? C9 C10 1.38(2) 6_556 6_556 ? C9 H9 .98(1) 6_556 6_556 ? C10 C11 1.37(2) 6_556 6_556 ? C10 H10 1.01(1) 6_556 6_556 ? C11 C12 1.38(2) 6_556 6_556 ? C11 H11 1.00(1) 6_556 6_556 ? C12 C13 1.52(1) 6_556 6_556 ? C14 C15 1.39(2) 6_556 6_556 ? C14 C19 1.39(2) 6_556 6_556 ? C15 C16 1.37(2) 6_556 6_556 ? C15 H15 .95(1) 6_556 6_556 ? C16 C17 1.36(2) 6_556 6_556 ? C16 H16 .95(1) 6_556 6_556 ? C17 C18 1.36(2) 6_556 6_556 ? C17 H17 1.00(1) 6_556 6_556 ? C18 C19 1.38(2) 6_556 6_556 ? C18 H18 1.00(1) 6_556 6_556 ? C19 H19 .99(1) 6_556 6_556 ? O3 H1w .731(2) . 2_655 ? O3 H1w .731(2) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC N1 Ni N2 76.0(3) 6_556 5_666 6_556 ? N1 Ni N3 153.5(3) 6_556 5_666 6_556 ? N1 Ni N1 89.2(3) 6_556 5_666 5_666 ? N1 Ni N2 100.8(3) 6_556 5_666 5_666 ? N1 Ni N3 97.2(3) 6_556 5_666 5_666 ? N2 Ni N1 100.8(3) 6_556 5_666 5_666 ? N2 Ni N2 175.6(4) 6_556 5_666 5_666 ? N2 Ni N3 77.6(3) 6_556 5_666 6_556 ? N2 Ni N3 105.7(3) 6_556 5_666 5_666 ? N3 Ni N1 97.2(3) 6_556 5_666 5_666 ? N3 Ni N2 105.7(3) 6_556 5_666 5_666 ? N3 Ni N3 88.4(3) 6_556 5_666 5_666 ? N1 Ni N2 76.0(3) 5_666 5_666 5_666 ? N1 Ni N3 153.5(3) 5_666 5_666 5_666 ? N2 Ni N3 77.6(3) 5_666 5_666 5_666 ? Ni N1 C1 120.6(6) . . . ? Ni N1 C7 117.7(7) . . . ? Ni N3 C13 116.0(7) . . . ? Ni N3 C14 123.5(7) . . . ? C20 N4 C21 106(1) . . . ? C20 N4 C22 113(1) . . . ? C20 N4 C23 108(1) . . . ? C21 N4 C22 111.3(9) . . . ? C21 N4 C23 110(1) . . . ? C22 N4 C23 108(1) . . . ? N4 C20 C24 121(1) . . . ? N4 C20 H201 117(1) . . . ? N4 C20 H202 115(1) . . . ? C24 C20 H201 102(1) . . . ? C24 C20 H202 100(1) . . . ? H201 C20 H202 99(1) . . . ? N4 C21 C25 116(1) . . . ? N4 C21 H211 108(1) . . . ? N4 C21 H212 104(1) . . . ? C25 C21 H211 115(1) . . . ? C25 C21 H212 111(1) . . . ? H211 C21 H212 102(1) . . . ? N4 C22 C26 117(1) . . . ? N4 C22 H221 106(1) . . . ? N4 C22 H222 108(1) . . . ? C26 C22 H221 108(1) . . . ? C26 C22 H222 112(1) . . . ? H221 C22 H222 106(1) . . . ? N4 C23 C27 121(1) . . . ? N4 C23 H231 109(1) . . . ? N4 C23 H232 110(1) . . . ? C27 C23 H231 105(1) . . . ? C27 C23 H232 106(1) . . . ? H231 C23 H232 104(1) . . . ? C20 C24 H241 106(1) . . . ? C20 C24 H242 104(1) . . . ? C20 C24 H243 127(2) . . . ? H241 C24 H242 97(2) . . . ? H241 C24 H243 110(1) . . . ? H242 C24 H243 109(2) . . . ? C21 C25 H251 102(2) . . . ? C21 C25 H252 100(2) . . . ? C21 C25 H253 107(2) . . . ? H251 C25 H252 110(2) . . . ? H251 C25 H253 117(2) . . . ? H252 C25 H253 117(2) . . . ? C22 C26 H261 107(1) . . . ? C22 C26 H262 113(1) . . . ? C22 C26 H263 117(1) . . . ? H261 C26 H262 107(1) . . . ? H261 C26 H263 103(1) . . . ? H262 C26 H263 108(1) . . . ? C23 C27 H271 108(1) . . . ? C23 C27 H272 110(2) . . . ? C23 C27 H273 124(2) . . . ? H271 C27 H272 103(2) . . . ? H271 C27 H273 104(2) . . . ? H272 C27 H273 106(2) . . . ? N2 Ni N2 175.6(4) 6_556 5_666 5_666 ? C1 N1 C7 120.3(8) 6_556 6_556 6_556 ? Ni N2 C8 119.8(7) 5_666 6_556 6_556 ? Ni N2 C12 119.3(7) 5_666 6_556 6_556 ? C8 N2 C12 120.9(8) 6_556 6_556 6_556 ? C13 N3 C14 119.5(8) 6_556 6_556 6_556 ? N1 C1 C2 124.8(9) 6_556 6_556 6_556 ? N1 C1 C6 119.5(9) 6_556 6_556 6_556 ? C2 C1 C6 115(1) 6_556 6_556 6_556 ? C1 C2 C3 124(1) 6_556 6_556 6_556 ? C1 C2 H2 119(1) 6_556 6_556 6_556 ? C3 C2 H2 117(1) 6_556 6_556 6_556 ? C2 C3 C4 118(1) 6_556 6_556 6_556 ? C2 C3 H3 124(1) 6_556 6_556 6_556 ? C4 C3 H3 117(1) 6_556 6_556 6_556 ? C3 C4 C5 122(1) 6_556 6_556 6_556 ? C3 C4 H4 115(1) 6_556 6_556 6_556 ? C5 C4 H4 121(1) 6_556 6_556 6_556 ? C4 C5 C6 118(1) 6_556 6_556 6_556 ? C4 C5 H5 113(1) 6_556 6_556 6_556 ? C6 C5 H5 128(1) 6_556 6_556 6_556 ? C1 C6 C5 122(1) 6_556 6_556 6_556 ? C1 C6 H6 123(1) 6_556 6_556 6_556 ? C5 C6 H6 115(1) 6_556 6_556 6_556 ? N1 C7 O1 129(1) 6_556 6_556 6_556 ? N1 C7 C8 111.0(9) 6_556 6_556 6_556 ? O1 C7 C8 120(1) 6_556 6_556 6_556 ? N2 C8 C7 115.1(9) 6_556 6_556 6_556 ? N2 C8 C9 122.1(9) 6_556 6_556 6_556 ? C7 C8 C9 123(1) 6_556 6_556 6_556 ? C8 C9 C10 116(1) 6_556 6_556 6_556 ? C8 C9 H9 124(1) 6_556 6_556 6_556 ? C10 C9 H9 119(1) 6_556 6_556 6_556 ? C9 C10 C11 121(1) 6_556 6_556 6_556 ? C9 C10 H10 122(1) 6_556 6_556 6_556 ? C11 C10 H10 116(1) 6_556 6_556 6_556 ? C10 C11 C12 118(1) 6_556 6_556 6_556 ? C10 C11 H11 121(1) 6_556 6_556 6_556 ? C12 C11 H11 121(1) 6_556 6_556 6_556 ? N2 C12 C11 121.0(9) 6_556 6_556 6_556 ? N2 C12 C13 115.2(9) 6_556 6_556 6_556 ? C11 C12 C13 123.8(9) 6_556 6_556 6_556 ? N3 C13 O2 129(1) 6_556 6_556 6_556 ? N3 C13 C12 111.6(8) 6_556 6_556 6_556 ? O2 C13 C12 119(1) 6_556 6_556 6_556 ? N3 C14 C15 118(1) 6_556 6_556 6_556 ? N3 C14 C19 124(1) 6_556 6_556 6_556 ? C15 C14 C19 117(1) 6_556 6_556 6_556 ? C14 C15 C16 121(1) 6_556 6_556 6_556 ? C14 C15 H15 124(1) 6_556 6_556 6_556 ? C16 C15 H15 114(1) 6_556 6_556 6_556 ? C15 C16 C17 120(1) 6_556 6_556 6_556 ? C15 C16 H16 128(1) 6_556 6_556 6_556 ? C17 C16 H16 112(1) 6_556 6_556 6_556 ? C16 C17 C18 119(1) 6_556 6_556 6_556 ? C16 C17 H17 125(1) 6_556 6_556 6_556 ? C18 C17 H17 116(1) 6_556 6_556 6_556 ? C17 C18 C19 122(1) 6_556 6_556 6_556 ? C17 C18 H18 118(1) 6_556 6_556 6_556 ? C19 C18 H18 120(1) 6_556 6_556 6_556 ? C14 C19 C18 120(1) 6_556 6_556 6_556 ? C14 C19 H19 121(1) 6_556 6_556 6_556 ? C18 C19 H19 119(1) 6_556 6_556 6_556 ? H1w O3 H1w 156(1) 2_655 . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC C21 N4 C20 C24 67(2) . . . . ? C21 N4 C20 H201 -57(1) . . . . ? C21 N4 C20 H202 -173(1) . . . . ? C22 N4 C20 C24 -55(2) . . . . ? C22 N4 C20 H201 -179(1) . . . . ? C22 N4 C20 H202 65(1) . . . . ? C23 N4 C20 C24 -175(1) . . . . ? C23 N4 C20 H201 61(2) . . . . ? C23 N4 C20 H202 -55(1) . . . . ? C20 N4 C21 C25 173(1) . . . . ? C20 N4 C21 H211 43(2) . . . . ? C20 N4 C21 H212 -65(1) . . . . ? C22 N4 C21 C25 -64(2) . . . . ? C22 N4 C21 H211 166(1) . . . . ? C22 N4 C21 H212 59(1) . . . . ? C23 N4 C21 C25 57(2) . . . . ? C23 N4 C21 H211 -74(2) . . . . ? C23 N4 C21 H212 179(1) . . . . ? C20 N4 C22 C26 -60(2) . . . . ? C20 N4 C22 H221 -180(1) . . . . ? C20 N4 C22 H222 68(2) . . . . ? C21 N4 C22 C26 -179(1) . . . . ? C21 N4 C22 H221 62(1) . . . . ? C21 N4 C22 H222 -51(2) . . . . ? C23 N4 C22 C26 60(2) . . . . ? C23 N4 C22 H221 -60(1) . . . . ? C23 N4 C22 H222 -172(1) . . . . ? C20 N4 C23 C27 -66(2) . . . . ? C20 N4 C23 H231 172(1) . . . . ? C20 N4 C23 H232 58(2) . . . . ? C21 N4 C23 C27 50(2) . . . . ? C21 N4 C23 H231 -73(1) . . . . ? C21 N4 C23 H232 173(1) . . . . ? C22 N4 C23 C27 172(1) . . . . ? C22 N4 C23 H231 49(2) . . . . ? C22 N4 C23 H232 -65(2) . . . . ? N4 C20 C24 H241 49(2) . . . . ? N4 C20 C24 H242 -53(2) . . . . ? N4 C20 C24 H243 180(2) . . . . ? H201 C20 C24 H241 -180(1) . . . . ? H201 C20 C24 H242 78(2) . . . . ? H201 C20 C24 H243 -49(2) . . . . ? H202 C20 C24 H241 -78(2) . . . . ? H202 C20 C24 H242 -180(1) . . . . ? H202 C20 C24 H243 53(2) . . . . ? N4 C21 C25 H251 53(2) . . . . ? N4 C21 C25 H252 -60(2) . . . . ? N4 C21 C25 H253 177(1) . . . . ? H211 C21 C25 H251 -180(1) . . . . ? H211 C21 C25 H252 67(2) . . . . ? H211 C21 C25 H253 -56(2) . . . . ? H212 C21 C25 H251 -64(2) . . . . ? H212 C21 C25 H252 -178(1) . . . . ? H212 C21 C25 H253 60(2) . . . . ? N4 C22 C26 H261 63(2) . . . . ? N4 C22 C26 H262 -55(2) . . . . ? N4 C22 C26 H263 179(1) . . . . ? H221 C22 C26 H261 -178(1) . . . . ? H221 C22 C26 H262 64(2) . . . . ? H221 C22 C26 H263 -63(2) . . . . ? H222 C22 C26 H261 -62(2) . . . . ? H222 C22 C26 H262 179(1) . . . . ? H222 C22 C26 H263 53(2) . . . . ? N4 C23 C27 H271 58(2) . . . . ? N4 C23 C27 H272 -54(2) . . . . ? N4 C23 C27 H273 179(1) . . . . ? H231 C23 C27 H271 -178(1) . . . . ? H231 C23 C27 H272 70(2) . . . . ? H231 C23 C27 H273 -57(2) . . . . ? H232 C23 C27 H271 -68(2) . . . . ? H232 C23 C27 H272 180(1) . . . . ? H232 C23 C27 H273 53(2) . . . . ? N2 Ni N2 C8 38(4) 5_666 5_666 6_556 6_556 ? N2 Ni N2 C12 -139(4) 5_666 5_666 6_556 6_556 ? C7 N1 C1 C2 56(2) 6_556 6_556 6_556 6_556 ? C7 N1 C1 C6 -132(1) 6_556 6_556 6_556 6_556 ? C1 N1 C7 O1 8(2) 6_556 6_556 6_556 6_556 ? C1 N1 C7 C8 -172.7(9) 6_556 6_556 6_556 6_556 ? Ni N2 C8 C7 4(1) 5_666 6_556 6_556 6_556 ? Ni N2 C8 C9 -178.0(8) 5_666 6_556 6_556 6_556 ? C12 N2 C8 C7 -178.9(9) 6_556 6_556 6_556 6_556 ? C12 N2 C8 C9 0(2) 6_556 6_556 6_556 6_556 ? Ni N2 C12 C11 178.3(8) 5_666 6_556 6_556 6_556 ? Ni N2 C12 C13 -1(1) 5_666 6_556 6_556 6_556 ? C8 N2 C12 C11 0(1) 6_556 6_556 6_556 6_556 ? C8 N2 C12 C13 -178.9(9) 6_556 6_556 6_556 6_556 ? C14 N3 C13 O2 9(2) 6_556 6_556 6_556 6_556 ? C14 N3 C13 C12 -174.5(8) 6_556 6_556 6_556 6_556 ? C13 N3 C14 C15 -140(1) 6_556 6_556 6_556 6_556 ? C13 N3 C14 C19 46(1) 6_556 6_556 6_556 6_556 ? N1 C1 C2 C3 174(1) 6_556 6_556 6_556 6_556 ? N1 C1 C2 H2 -8(2) 6_556 6_556 6_556 6_556 ? C6 C1 C2 C3 1(2) 6_556 6_556 6_556 6_556 ? C6 C1 C2 H2 179(1) 6_556 6_556 6_556 6_556 ? N1 C1 C6 C5 -171(1) 6_556 6_556 6_556 6_556 ? N1 C1 C6 H6 5(2) 6_556 6_556 6_556 6_556 ? C2 C1 C6 C5 2(2) 6_556 6_556 6_556 6_556 ? C2 C1 C6 H6 178(1) 6_556 6_556 6_556 6_556 ? C1 C2 C3 C4 1(2) 6_556 6_556 6_556 6_556 ? C1 C2 C3 H3 173(1) 6_556 6_556 6_556 6_556 ? H2 C2 C3 C4 -176(1) 6_556 6_556 6_556 6_556 ? H2 C2 C3 H3 -4(2) 6_556 6_556 6_556 6_556 ? C2 C3 C4 C5 -7(2) 6_556 6_556 6_556 6_556 ? C2 C3 C4 H4 -169(1) 6_556 6_556 6_556 6_556 ? H3 C3 C4 C5 -179(1) 6_556 6_556 6_556 6_556 ? H3 C3 C4 H4 19(2) 6_556 6_556 6_556 6_556 ? C3 C4 C5 C6 10(2) 6_556 6_556 6_556 6_556 ? C3 C4 C5 H5 177(1) 6_556 6_556 6_556 6_556 ? H4 C4 C5 C6 171(1) 6_556 6_556 6_556 6_556 ? H4 C4 C5 H5 -22(2) 6_556 6_556 6_556 6_556 ? C4 C5 C6 C1 -7(2) 6_556 6_556 6_556 6_556 ? C4 C5 C6 H6 177(1) 6_556 6_556 6_556 6_556 ? H5 C5 C6 C1 -172(1) 6_556 6_556 6_556 6_556 ? H5 C5 C6 H6 11(2) 6_556 6_556 6_556 6_556 ? N1 C7 C8 N2 2(1) 6_556 6_556 6_556 6_556 ? N1 C7 C8 C9 -177(1) 6_556 6_556 6_556 6_556 ? O1 C7 C8 N2 -179.2(9) 6_556 6_556 6_556 6_556 ? O1 C7 C8 C9 3(2) 6_556 6_556 6_556 6_556 ? N2 C8 C9 C10 1(2) 6_556 6_556 6_556 6_556 ? N2 C8 C9 H9 177(1) 6_556 6_556 6_556 6_556 ? C7 C8 C9 C10 179(1) 6_556 6_556 6_556 6_556 ? C7 C8 C9 H9 -5(2) 6_556 6_556 6_556 6_556 ? C8 C9 C10 C11 -2(2) 6_556 6_556 6_556 6_556 ? C8 C9 C10 H10 -177(1) 6_556 6_556 6_556 6_556 ? H9 C9 C10 C11 -178(1) 6_556 6_556 6_556 6_556 ? H9 C9 C10 H10 7(2) 6_556 6_556 6_556 6_556 ? C9 C10 C11 C12 2(2) 6_556 6_556 6_556 6_556 ? C9 C10 C11 H11 -176(1) 6_556 6_556 6_556 6_556 ? H10 C10 C11 C12 178(1) 6_556 6_556 6_556 6_556 ? H10 C10 C11 H11 0(2) 6_556 6_556 6_556 6_556 ? C10 C11 C12 N2 -2(2) 6_556 6_556 6_556 6_556 ? C10 C11 C12 C13 178(1) 6_556 6_556 6_556 6_556 ? H11 C11 C12 N2 176(1) 6_556 6_556 6_556 6_556 ? H11 C11 C12 C13 -4(2) 6_556 6_556 6_556 6_556 ? N2 C12 C13 N3 4(1) 6_556 6_556 6_556 6_556 ? N2 C12 C13 O2 -178.4(9) 6_556 6_556 6_556 6_556 ? C11 C12 C13 N3 -175(1) 6_556 6_556 6_556 6_556 ? C11 C12 C13 O2 2(2) 6_556 6_556 6_556 6_556 ? N3 C14 C15 C16 -173(1) 6_556 6_556 6_556 6_556 ? N3 C14 C15 H15 9(2) 6_556 6_556 6_556 6_556 ? C19 C14 C15 C16 2(2) 6_556 6_556 6_556 6_556 ? C19 C14 C15 H15 -177(1) 6_556 6_556 6_556 6_556 ? N3 C14 C19 C18 171(1) 6_556 6_556 6_556 6_556 ? N3 C14 C19 H19 -10(2) 6_556 6_556 6_556 6_556 ? C15 C14 C19 C18 -3(1) 6_556 6_556 6_556 6_556 ? C15 C14 C19 H19 175(1) 6_556 6_556 6_556 6_556 ? C14 C15 C16 C17 0(2) 6_556 6_556 6_556 6_556 ? C14 C15 C16 H16 179(1) 6_556 6_556 6_556 6_556 ? H15 C15 C16 C17 179(1) 6_556 6_556 6_556 6_556 ? H15 C15 C16 H16 -2(2) 6_556 6_556 6_556 6_556 ? C15 C16 C17 C18 0(2) 6_556 6_556 6_556 6_556 ? C15 C16 C17 H17 -176(1) 6_556 6_556 6_556 6_556 ? H16 C16 C17 C18 -180(1) 6_556 6_556 6_556 6_556 ? H16 C16 C17 H17 5(2) 6_556 6_556 6_556 6_556 ? C16 C17 C18 C19 0(2) 6_556 6_556 6_556 6_556 ? C16 C17 C18 H18 -178(1) 6_556 6_556 6_556 6_556 ? H17 C17 C18 C19 175(1) 6_556 6_556 6_556 6_556 ? H17 C17 C18 H18 -2(2) 6_556 6_556 6_556 6_556 ? C17 C18 C19 C14 3(2) 6_556 6_556 6_556 6_556 ? C17 C18 C19 H19 -176(1) 6_556 6_556 6_556 6_556 ? H18 C18 C19 C14 180(1) 6_556 6_556 6_556 6_556 ? H18 C18 C19 H19 0(2) 6_556 6_556 6_556 6_556 ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _reflns_number_total 4422 #ActaC _reflns_number_observed 1512 #ActaC _reflns_observed_criterion refl_observed_if_Inet_>_.000_sigma(Inet) _reflns_d_resolution_high .842 _reflns_d_resolution_low 11.883 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 6.8492 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_observed_status _refln_scale_group_code ? ? ? ? ? ? ? ? _publ_requested_journal Inorganic Chemistry #ActaC _publ_requested_coeditor_name Prof. Kenneth R. Poeppelmeier (Email: kpacs@chem.nwu.edu) _publ_contact_author #ActaC ; ? name Prof. R. N. Mukherjee ? institute Indian Institute of Technology Kanpur ? department Department of Chemistry ? address 208 016 ? city Kanpur ? country India ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone ? #ActaC _publ_contact_author_fax ? #ActaC _publ_contact_author_email rnm@iitk.ernet.in #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title Bivalent, Trivalent, and Tetravalent Nickel Complexes with a Common Tridentate Deprotonated Pyridine Bis-Amide Ligand. Molecular Structures of Nickel(II) and Ni(IV) and Redox Activity. _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _audit_creation_date 98-00-08 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record _chemical_compound_source Synthesized in the laboratory #ActaC _chemical_name_systematic _chemical_name_common _chemical_formula_analytical C38 H27.5 N6 O4.75 Ni _chemical_formula_moiety "Ni 4+, C38 N6 O4 H26 4-" O0.75 H1.5 _chemical_formula_structural (Ni(C19 N3 O2 H13)(C19 N3 O2 H13)) (O0.75 H1.5) _chemical_formula_sum C38 H27.5 N6 O4.75 Ni _chemical_formula_weight 702.19 _chemical_melting_point decomposes above 300 degree celcius _computing_data_collection ? #ActaC _computing_cell_refinement ? #ActaC _computing_data_reduction xtal_DIFDAT_SORTRF_ADDREF #ActaC _computing_structure_solution xtal_SIMPEL #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 14.874(7) #ActaC _cell_length_b 13.300(4) #ActaC _cell_length_c 16.604(5) #ActaC _cell_angle_alpha 90.00(3) #ActaC _cell_angle_beta 99.68(3) #ActaC _cell_angle_gamma 90.00(3) #ActaC _cell_volume 3238(2) #ActaC _cell_formula_units_Z 4 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used 25 #ActaC _cell_measurement_theta_min 9.66 #ActaC _cell_measurement_theta_max 23.48 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting monoclinic #ActaC _symmetry_space_group_name_H-M P21/a #ActaC _symmetry_space_group_name_Hall -P_2yab #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,+z _exptl_crystal_description block shaped #ActaC _exptl_crystal_preparation Ether diffusion to a chloroform solution of the compound _exptl_crystal_colour violet #ActaC _exptl_crystal_size_max 0.2 mm #ActaC _exptl_crystal_size_mid 0.2 mm #ActaC _exptl_crystal_size_min 0.1 mm #ActaC _exptl_crystal_density_diffrn 1.442 #ActaC _exptl_crystal_density_meas _exptl_crystal_density_method flotation #ActaC _exptl_crystal_F_000 1453.68 #ActaC _exptl_absorpt_process_details _exptl_absorpt_coefficient_mu 0.65 #ActaC _exptl_absorpt_correction_type analytical #ActaC _exptl_absorpt_correction_T_min 0.8317 #ActaC _exptl_absorpt_correction_T_max 0.8323 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type Mo K-alpha #ActaC _diffrn_radiation_source sealed xray_tube #ActaC _diffrn_radiation_monochromator graphite #ActaC _diffrn_radiation_detector proportional counter #ActaC _diffrn_measurement_device CAD4mach #ActaC _diffrn_measurement_method theta-2theta #ActaC _diffrn_standards_number three #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time every hour #ActaC _diffrn_standards_decay_% 1.17% #ActaC loop_ _diffrn_standard_refln_index_h 1 2 -3 #ActaC _diffrn_standard_refln_index_k -4 0 4 #ActaC _diffrn_standard_refln_index_l 1 -2 -3 #ActaC ? ? ? loop_ _diffrn_attenuator_code 13.364 _diffrn_attenuator_scale ? ? _diffrn_reflns_number 6220 #ActaC _diffrn_reflns_av_R_equivalents .124 #ActaC _diffrn_reflns_av_sigmaI/netI .128 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 17 #ActaC _diffrn_reflns_limit_k_min 0 #ActaC _diffrn_reflns_limit_k_max 15 #ActaC _diffrn_reflns_limit_l_min -19 #ActaC _diffrn_reflns_limit_l_max 19 #ActaC _diffrn_reflns_theta_min 1.24 #ActaC _diffrn_reflns_theta_max 25. #ActaC _diffrn_reflns_reduction_process No_monochr_Lp_applied #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC c ? 0 152 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 h ? 0 110 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 n ? 0 24 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 o ? 0 19 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Ni ? 0 4 .285 1.113 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Ni .24346(8) .51094(8) .73541(7) .0323(6) Uani ? ? N1 .3677(5) .5455(5) .7832(4) .037(4) Uani ? ? N2 .3022(5) .4080(5) .6900(4) .033(4) Uani ? ? N3 .1350(5) .4452(6) .6757(4) .039(4) Uani ? ? N4 .2277(5) .4409(6) .8352(5) .041(5) Uani ? ? N5 .1847(5) .6129(5) .7806(5) .039(5) Uani ? ? N6 .2431(5) .6082(6) .6481(4) .042(5) Uani ? ? O1 .5152(4) .4917(6) .7872(4) .065(4) Uani ? ? O2 .0916(5) .3107(5) .5936(4) .059(4) Uani ? ? O3 .1609(5) .4642(5) .9499(4) .073(5) Uani ? ? O4 .1962(5) .7691(5) .6140(4) .059(4) Uani ? ? C1 .3868(6) .6145(7) .8482(5) .035(5) Uani ? ? C2 .3775(7) .7180(8) .8354(6) .051(6) Uani ? ? C3 .3860(8) .7826(7) .9003(8) .065(7) Uani ? ? C4 .4068(8) .7480(9) .9787(8) .068(8) Uani ? ? C5 .4201(8) .6462(9) .9930(6) .064(7) Uani ? ? C6 .4091(7) .5818(7) .9275(6) .052(6) Uani ? ? C7 .4335(6) .4857(7) .7620(5) .038(5) Uani ? ? C8 .3926(6) .4067(7) .7037(5) .036(5) Uani ? ? C9 .4365(6) .3328(7) .6688(6) .046(6) Uani ? ? C10 .3863(8) .2642(7) .6181(6) .053(7) Uani ? ? C11 .2912(7) .2677(7) .6037(6) .049(6) Uani ? ? C12 .2495(7) .3424(7) .6414(5) .036(6) Uani ? ? C13 .1495(6) .3629(7) .6345(6) .039(6) Uani ? ? C14 .0478(6) .4914(8) .6703(5) .039(5) Uani ? ? C15 -.0040(7) .4755(8) .7307(6) .058(7) Uani ? ? C16 -.0881(8) .522(1) .7238(8) .077(8) Uani ? ? C17 -.1186(8) .583(1) .661(1) .09(1) Uani ? ? C18 -.0680(9) .5987(9) .5996(8) .075(8) Uani ? ? C19 .0146(7) .5507(8) .6043(6) .052(6) Uani ? ? C20 .2443(8) .3357(7) .8466(6) .042(6) Uani ? ? C21 .1763(7) .2651(8) .8261(6) .052(7) Uani ? ? C22 .1953(9) .1656(9) .8352(8) .069(8) Uani ? ? C23 .279(1) .1333(8) .8637(8) .075(9) Uani ? ? C24 .3480(8) .2009(9) .8822(7) .065(8) Uani ? ? C25 .3319(8) .3026(8) .8750(6) .057(7) Uani ? ? C26 .1837(6) .4937(8) .8860(6) .049(6) Uani ? ? C27 .1637(6) .5984(7) .8543(6) .044(6) Uani ? ? C28 .1242(7) .6764(9) .8915(6) .057(7) Uani ? ? C29 .1091(7) .7680(8) .8506(7) .056(7) Uani ? ? C30 .1297(7) .7788(7) .7725(7) .052(6) Uani ? ? C31 .1689(6) .6989(7) .7396(6) .038(5) Uani ? ? C32 .2034(7) .6980(8) .6601(6) .045(6) Uani ? ? C33 .2985(7) .5958(7) .5856(6) .039(6) Uani ? ? C34 .2681(7) .5352(7) .5188(6) .052(6) Uani ? ? C35 .3243(8) .5194(8) .4607(6) .063(7) Uani ? ? C36 .4055(9) .566(1) .4689(8) .072(8) Uani ? ? C37 .4352(7) .6254(9) .5333(8) .062(7) Uani ? ? C38 .3829(7) .6396(7) .5938(6) .051(6) Uani ? ? O1w .019(1) .514(1) 1.0487(9) .18(1) Uani ? ? H1w .05883 .48267 1.01471 .03500 Uani ? ? H2w .06171 .57289 1.01471 .03500 Uani ? ? H2 .36407 .74410 .77910 .03800 Uani ? ? H3 .37854 .85510 .89086 .03800 Uani ? ? H4 .41298 .79529 1.02482 .03800 Uani ? ? H5 .43624 .62029 1.04973 .03800 Uani ? ? H6 .41805 .50918 .93595 .03800 Uani ? ? H9 .50322 .33006 .67827 .03800 Uani ? ? H10 .41761 .21201 .59243 .03800 Uani ? ? H11 .25385 .21778 .56764 .03800 Uani ? ? H15 .01962 .43335 .77904 .03800 Uani ? ? H16 -.12799 .50875 .76408 .03800 Uani ? ? H17 -.17788 .61753 .65780 .03800 Uani ? ? H18 -.09032 .64485 .55394 .03800 Uani ? ? H19 .05177 .55872 .56099 .03800 Uani ? ? H21 .11352 .28882 .80689 .03800 Uani ? ? H22 .14545 .11593 .81652 .03800 Uani ? ? H23 .29339 .06233 .87408 .03800 Uani ? ? H24 .41184 .17686 .90157 .03800 Uani ? ? H25 .38182 .35281 .89069 .03800 Uani ? ? H28 .10561 .66705 .94501 .03800 Uani ? ? H29 .08615 .82575 .87833 .03800 Uani ? ? H30 .11526 .84206 .74074 .03800 Uani ? ? H34 .20802 .50345 .51370 .03800 Uani ? ? H35 .30293 .47488 .41330 .03800 Uani ? ? H36 .44240 .55898 .42597 .03800 Uani ? ? H37 .49557 .65784 .53869 .03800 Uani ? ? H38 .40446 .68225 .64195 .03800 Uani ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Ni .0294(6) .0306(7) .0388(6) .0011(8) .0115(5) -.0010(7) N1 .032(5) .033(4) .046(5) -.001(4) .010(4) .002(4) N2 .037(5) .029(5) .037(5) .008(4) .014(4) .006(4) N3 .024(4) .041(5) .053(5) -.006(4) .009(4) -.003(4) N4 .044(5) .031(5) .056(5) .003(4) .029(4) .004(4) N5 .035(5) .032(5) .052(5) .003(4) .016(4) -.003(4) N6 .050(6) .036(5) .042(5) -.004(4) .016(4) .001(4) O1 .036(4) .063(5) .095(5) .002(5) .009(4) -.023(5) O2 .043(5) .059(5) .077(5) -.012(4) .011(4) -.025(4) O3 .099(6) .068(5) .061(5) .017(5) .047(5) .015(4) O4 .067(5) .041(4) .075(5) .007(4) .027(4) .019(4) C1 .024(5) .044(6) .036(6) -.005(5) .005(4) -.009(5) C2 .045(7) .045(7) .061(7) -.001(6) .008(6) .002(6) C3 .071(9) .029(6) .092(9) .000(6) .006(8) -.021(7) C4 .066(8) .066(9) .070(9) .007(7) .001(7) -.033(7) C5 .072(9) .072(9) .048(7) .001(7) .011(6) -.011(7) C6 .061(7) .040(6) .055(7) -.004(6) .013(6) -.010(6) C7 .039(6) .028(5) .047(5) -.002(6) .005(5) -.001(5) C8 .035(6) .034(6) .044(6) .011(5) .018(5) .004(5) C9 .041(6) .040(6) .060(7) -.002(6) .019(6) -.004(6) C10 .055(8) .044(7) .068(7) .017(6) .034(6) .003(6) C11 .064(8) .032(6) .053(6) -.000(6) .017(6) -.009(5) C12 .040(7) .038(6) .034(6) -.003(5) .013(5) -.003(5) C13 .027(6) .040(6) .054(7) -.001(5) .020(5) .000(5) C14 .028(5) .045(6) .044(5) -.004(6) .003(4) .007(6) C15 .044(7) .066(8) .069(7) .006(6) .019(6) .008(6) C16 .040(7) .09(1) .104(9) .009(8) .028(7) .005(9) C17 .040(8) .09(1) .13(1) .028(8) -.006(8) -.03(1) C18 .08(1) .053(8) .084(9) .019(8) -.022(8) .000(7) C19 .046(7) .058(7) .050(7) -.010(6) .003(5) -.013(6) C20 .059(8) .029(6) .042(6) .002(6) .022(6) .007(5) C21 .045(7) .052(7) .063(7) -.002(6) .017(6) .002(6) C22 .08(1) .036(7) .09(1) -.012(7) .027(8) .003(6) C23 .11(1) .035(7) .08(1) .014(8) .034(9) .013(7) C24 .062(9) .047(7) .085(9) .014(7) .007(7) .010(7) C25 .062(8) .043(7) .069(8) .003(6) .016(7) .013(6) C26 .051(6) .039(6) .059(6) .003(6) .018(5) .004(6) C27 .041(6) .042(6) .053(7) .003(5) .022(6) -.007(5) C28 .056(7) .066(8) .056(7) .006(7) .029(6) -.010(7) C29 .054(7) .048(7) .070(8) .016(6) .025(6) -.008(6) C30 .040(6) .040(6) .078(8) .011(5) .014(6) -.001(6) C31 .026(6) .033(6) .058(6) .000(5) .014(5) -.008(5) C32 .041(7) .034(6) .061(7) -.004(5) .013(6) .000(6) C33 .049(7) .034(6) .036(6) .002(5) .011(5) .009(5) C34 .050(7) .053(7) .055(7) -.014(6) .017(5) .002(6) C35 .095(9) .056(7) .043(6) .007(7) .028(6) -.008(6) C36 .072(9) .072(9) .086(9) .004(8) .054(8) .010(8) C37 .044(7) .062(8) .088(9) -.004(6) .034(7) .012(7) C38 .056(7) .041(6) .062(7) -.017(6) .024(6) -.006(6) O1w .18(2) .21(2) .17(1) -.01(1) .10(1) -.03(2) H1w .03500 .03500 .03500 .00000 .00588 .00000 H2w .03500 .03500 .03500 .00000 .00588 .00000 H2 .03800 .03800 .03800 .00000 .00639 .00000 H3 .03800 .03800 .03800 .00000 .00639 .00000 H4 .03800 .03800 .03800 .00000 .00639 .00000 H5 .03800 .03800 .03800 .00000 .00639 .00000 H6 .03800 .03800 .03800 .00000 .00639 .00000 H9 .03800 .03800 .03800 .00000 .00639 .00000 H10 .03800 .03800 .03800 .00000 .00639 .00000 H11 .03800 .03800 .03800 .00000 .00639 .00000 H15 .03800 .03800 .03800 .00000 .00639 .00000 H16 .03800 .03800 .03800 .00000 .00639 .00000 H17 .03800 .03800 .03800 .00000 .00639 .00000 H18 .03800 .03800 .03800 .00000 .00639 .00000 H19 .03800 .03800 .03800 .00000 .00639 .00000 H21 .03800 .03800 .03800 .00000 .00639 .00000 H22 .03800 .03800 .03800 .00000 .00639 .00000 H23 .03800 .03800 .03800 .00000 .00639 .00000 H24 .03800 .03800 .03800 .00000 .00639 .00000 H25 .03800 .03800 .03800 .00000 .00639 .00000 H28 .03800 .03800 .03800 .00000 .00639 .00000 H29 .03800 .03800 .03800 .00000 .00639 .00000 H30 .03800 .03800 .03800 .00000 .00639 .00000 H34 .03800 .03800 .03800 .00000 .00639 .00000 H35 .03800 .03800 .03800 .00000 .00639 .00000 H36 .03800 .03800 .03800 .00000 .00639 .00000 H37 .03800 .03800 .03800 .00000 .00639 .00000 H38 .03800 .03800 .03800 .00000 .00639 .00000 _atom_sites_solution_primary Ni,N _atom_sites_solution_secondary rest of the non-hydrogen atoms _atom_sites_solution_hydrogens positions calculated _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type full #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment no #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression no _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 2366 #ActaC _refine_ls_number_parameters 451 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .164 #ActaC _refine_ls_R_factor_obs .061 #ActaC _refine_ls_wR_factor_all .159 #ActaC _refine_ls_wR_factor_obs .064 #ActaC _refine_ls_goodness_of_fit_all 1.984 #ActaC _refine_ls_goodness_of_fit_obs 1.305 #ActaC _refine_ls_shift/esd_max . #ActaC _refine_ls_shift/esd_mean 0 #ActaC _refine_diff_density_min -2.031 #ActaC _refine_diff_density_max 1.143 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Ni N1 1.940(7) . . ? Ni N2 1.852(8) . . ? Ni N3 1.953(7) . . ? Ni N4 1.949(8) . . ? Ni N5 1.840(8) . . ? Ni N6 1.942(8) . . ? N1 C1 1.41(1) . . ? N1 C7 1.35(1) . . ? N2 C8 1.33(1) . . ? N2 C12 1.35(1) . . ? N3 C13 1.33(1) . . ? N3 C14 1.42(1) . . ? N4 C20 1.43(1) . . ? N4 C26 1.35(1) . . ? N5 C27 1.33(1) . . ? N5 C31 1.33(1) . . ? N6 C32 1.36(1) . . ? N6 C33 1.44(1) . . ? O1 C7 1.22(1) . . ? O2 C13 1.22(1) . . ? O3 C26 1.23(1) . . ? O4 C32 1.21(1) . . ? C1 C2 1.40(1) . . ? C1 C6 1.37(1) . . ? C2 C3 1.37(2) . . ? C2 H2 .99(1) . . ? C3 C4 1.37(2) . . ? C3 H3 .98(1) . . ? C4 C5 1.38(2) . . ? C4 H4 .98(1) . . ? C5 C6 1.37(2) . . ? C5 H5 .99(1) . . ? C6 H6 .98(1) . . ? C7 C8 1.49(1) . . ? C8 C9 1.36(1) . . ? C9 C10 1.37(1) . . ? C9 H9 .980(9) . . ? C10 C11 1.40(2) . . ? C10 H10 .97(1) . . ? C11 C12 1.38(1) . . ? C11 H11 .998(9) . . ? C12 C13 1.50(1) . . ? C14 C15 1.38(1) . . ? C14 C19 1.37(1) . . ? C15 C16 1.38(2) . . ? C15 H15 .99(1) . . ? C16 C17 1.34(2) . . ? C16 H16 .98(1) . . ? C17 C18 1.38(2) . . ? C17 H17 .99(1) . . ? C18 C19 1.37(2) . . ? C18 H18 .99(1) . . ? C19 H19 .98(1) . . ? C20 C21 1.38(1) . . ? C20 C25 1.38(2) . . ? C21 C22 1.36(2) . . ? C21 H21 .99(1) . . ? C22 C23 1.33(2) . . ? C22 H22 1.00(1) . . ? C23 C24 1.36(2) . . ? C23 H23 .98(1) . . ? C24 C25 1.38(2) . . ? C24 H24 1.00(1) . . ? C25 H25 1.00(1) . . ? C26 C27 1.50(1) . . ? C27 C28 1.39(2) . . ? C28 C29 1.39(2) . . ? C28 H28 .98(1) . . ? C29 C30 1.39(2) . . ? C29 H29 .99(1) . . ? C30 C31 1.37(1) . . ? C30 H30 1.00(1) . . ? C31 C32 1.50(1) . . ? C33 C34 1.38(1) . . ? C33 C38 1.37(1) . . ? C34 C35 1.40(2) . . ? C34 H34 .98(1) . . ? C35 C36 1.35(2) . . ? C35 H35 .99(1) . . ? C36 C37 1.34(2) . . ? C36 H36 .97(1) . . ? C37 C38 1.38(2) . . ? C37 H37 .99(1) . . ? C38 H38 .99(1) . . ? O1w H1w .98(2) . . ? O1w H2w 1.21(2) . . ? O1w O1w 1.67(2) . 3_567 ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC N1 Ni N2 81.9(3) . . . ? N1 Ni N3 164.3(3) . . . ? N1 Ni N4 90.4(3) . . . ? N1 Ni N5 98.2(3) . . . ? N1 Ni N6 91.7(3) . . . ? N2 Ni N3 82.4(3) . . . ? N2 Ni N4 97.2(3) . . . ? N2 Ni N5 179.8(4) . . . ? N2 Ni N6 97.5(3) . . . ? N3 Ni N4 90.6(3) . . . ? N3 Ni N5 97.4(3) . . . ? N3 Ni N6 91.2(3) . . . ? N4 Ni N5 82.7(3) . . . ? N4 Ni N6 165.3(3) . . . ? N5 Ni N6 82.6(3) . . . ? Ni N1 C1 121.5(6) . . . ? Ni N1 C7 115.8(6) . . . ? C1 N1 C7 121.4(7) . . . ? Ni N2 C8 118.3(6) . . . ? Ni N2 C12 117.1(6) . . . ? C8 N2 C12 124.5(8) . . . ? Ni N3 C13 116.0(6) . . . ? Ni N3 C14 120.3(6) . . . ? C13 N3 C14 123.3(7) . . . ? Ni N4 C20 122.6(6) . . . ? Ni N4 C26 115.0(6) . . . ? C20 N4 C26 121.3(8) . . . ? Ni N5 C27 118.0(6) . . . ? Ni N5 C31 118.7(7) . . . ? C27 N5 C31 123.2(8) . . . ? Ni N6 C32 115.0(7) . . . ? Ni N6 C33 122.2(6) . . . ? C32 N6 C33 121.3(8) . . . ? N1 C1 C2 121.6(8) . . . ? N1 C1 C6 120.8(8) . . . ? C2 C1 C6 117.4(9) . . . ? C1 C2 C3 120.4(9) . . . ? C1 C2 H2 119(1) . . . ? C3 C2 H2 120(1) . . . ? C2 C3 C4 121(1) . . . ? C2 C3 H3 120(1) . . . ? C4 C3 H3 119(1) . . . ? C3 C4 C5 120(1) . . . ? C3 C4 H4 120(1) . . . ? C5 C4 H4 120(1) . . . ? C4 C5 C6 119(1) . . . ? C4 C5 H5 120(1) . . . ? C6 C5 H5 121(1) . . . ? C1 C6 C5 122.6(9) . . . ? C1 C6 H6 117(1) . . . ? C5 C6 H6 120(1) . . . ? N1 C7 O1 126.6(9) . . . ? N1 C7 C8 110.5(8) . . . ? O1 C7 C8 122.9(9) . . . ? N2 C8 C7 113.2(8) . . . ? N2 C8 C9 118.7(8) . . . ? C7 C8 C9 127.9(9) . . . ? C8 C9 C10 119.4(9) . . . ? C8 C9 H9 120.2(9) . . . ? C10 C9 H9 120(1) . . . ? C9 C10 C11 121(1) . . . ? C9 C10 H10 119(1) . . . ? C11 C10 H10 120(1) . . . ? C10 C11 C12 117.8(9) . . . ? C10 C11 H11 122(1) . . . ? C12 C11 H11 120(1) . . . ? N2 C12 C11 118.6(9) . . . ? N2 C12 C13 113.5(8) . . . ? C11 C12 C13 127.8(9) . . . ? N3 C13 O2 126.5(9) . . . ? N3 C13 C12 110.8(8) . . . ? O2 C13 C12 122.6(9) . . . ? N3 C14 C15 120.2(8) . . . ? N3 C14 C19 120.0(9) . . . ? C15 C14 C19 119.9(9) . . . ? C14 C15 C16 119(1) . . . ? C14 C15 H15 120.5(9) . . . ? C16 C15 H15 121(1) . . . ? C15 C16 C17 121(1) . . . ? C15 C16 H16 120(1) . . . ? C17 C16 H16 118(1) . . . ? C16 C17 C18 121(1) . . . ? C16 C17 H17 120(2) . . . ? C18 C17 H17 119(1) . . . ? C17 C18 C19 119(1) . . . ? C17 C18 H18 120(1) . . . ? C19 C18 H18 121(1) . . . ? C14 C19 C18 121(1) . . . ? C14 C19 H19 118(1) . . . ? C18 C19 H19 121(1) . . . ? N4 C20 C21 122.0(9) . . . ? N4 C20 C25 119.3(9) . . . ? C21 C20 C25 118.6(9) . . . ? C20 C21 C22 120(1) . . . ? C20 C21 H21 118(1) . . . ? C22 C21 H21 121(1) . . . ? C21 C22 C23 121(1) . . . ? C21 C22 H22 119(1) . . . ? C23 C22 H22 120(1) . . . ? C22 C23 C24 120(1) . . . ? C22 C23 H23 123(1) . . . ? C24 C23 H23 118(1) . . . ? C23 C24 C25 121(1) . . . ? C23 C24 H24 120(1) . . . ? C25 C24 H24 119(1) . . . ? C20 C25 C24 119(1) . . . ? C20 C25 H25 120(1) . . . ? C24 C25 H25 122(1) . . . ? N4 C26 O3 127.3(9) . . . ? N4 C26 C27 110.6(8) . . . ? O3 C26 C27 122.1(9) . . . ? N5 C27 C26 113.3(8) . . . ? N5 C27 C28 119.0(9) . . . ? C26 C27 C28 127.7(9) . . . ? C27 C28 C29 119(1) . . . ? C27 C28 H28 121(1) . . . ? C29 C28 H28 120(1) . . . ? C28 C29 C30 120(1) . . . ? C28 C29 H29 120(1) . . . ? C30 C29 H29 120(1) . . . ? C29 C30 C31 117.8(9) . . . ? C29 C30 H30 121(1) . . . ? C31 C30 H30 121(1) . . . ? N5 C31 C30 120.9(9) . . . ? N5 C31 C32 112.8(8) . . . ? C30 C31 C32 126.2(9) . . . ? N6 C32 O4 126(1) . . . ? N6 C32 C31 111.0(8) . . . ? O4 C32 C31 123.0(9) . . . ? N6 C33 C34 119.7(9) . . . ? N6 C33 C38 120.3(8) . . . ? C34 C33 C38 120(1) . . . ? C33 C34 C35 119.3(9) . . . ? C33 C34 H34 119(1) . . . ? C35 C34 H34 121(1) . . . ? C34 C35 C36 119(1) . . . ? C34 C35 H35 119(1) . . . ? C36 C35 H35 121(1) . . . ? C35 C36 C37 122(1) . . . ? C35 C36 H36 119(1) . . . ? C37 C36 H36 119(1) . . . ? C36 C37 C38 121(1) . . . ? C36 C37 H37 120(1) . . . ? C38 C37 H37 119(1) . . . ? C33 C38 C37 119.1(9) . . . ? C33 C38 H38 120(1) . . . ? C37 C38 H38 121(1) . . . ? H1w O1w H2w 66(1) . . . ? H1w O1w O1w 59(1) . . 3_567 ? H2w O1w O1w 79(1) . . 3_567 ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC N2 Ni N1 C1 -166.2(7) . . . . ? N2 Ni N1 C7 1.3(6) . . . . ? N3 Ni N1 C1 -163(1) . . . . ? N3 Ni N1 C7 5(2) . . . . ? N4 Ni N1 C1 -68.9(7) . . . . ? N4 Ni N1 C7 98.5(7) . . . . ? N5 Ni N1 C1 13.7(7) . . . . ? N5 Ni N1 C7 -178.8(7) . . . . ? N6 Ni N1 C1 96.5(7) . . . . ? N6 Ni N1 C7 -96.0(7) . . . . ? N1 Ni N2 C8 -4.0(7) . . . . ? N1 Ni N2 C12 179.5(7) . . . . ? N3 Ni N2 C8 177.0(7) . . . . ? N3 Ni N2 C12 .4(7) . . . . ? N4 Ni N2 C8 -93.4(7) . . . . ? N4 Ni N2 C12 90.1(7) . . . . ? N5 Ni N2 C8 -147(90) . . . . ? N5 Ni N2 C12 36(91) . . . . ? N6 Ni N2 C8 86.7(7) . . . . ? N6 Ni N2 C12 -89.8(7) . . . . ? N1 Ni N3 C13 -2(2) . . . . ? N1 Ni N3 C14 -175(1) . . . . ? N2 Ni N3 C13 1.3(7) . . . . ? N2 Ni N3 C14 -171.8(7) . . . . ? N4 Ni N3 C13 -95.9(7) . . . . ? N4 Ni N3 C14 91.0(7) . . . . ? N5 Ni N3 C13 -178.6(7) . . . . ? N5 Ni N3 C14 8.4(7) . . . . ? N6 Ni N3 C13 98.7(7) . . . . ? N6 Ni N3 C14 -74.4(7) . . . . ? N1 Ni N4 C20 -92.8(7) . . . . ? N1 Ni N4 C26 99.3(6) . . . . ? N2 Ni N4 C20 -10.9(7) . . . . ? N2 Ni N4 C26 -178.8(6) . . . . ? N3 Ni N4 C20 71.5(7) . . . . ? N3 Ni N4 C26 -96.3(6) . . . . ? N5 Ni N4 C20 168.9(7) . . . . ? N5 Ni N4 C26 1.1(6) . . . . ? N6 Ni N4 C20 169(1) . . . . ? N6 Ni N4 C26 0(2) . . . . ? N1 Ni N5 C27 -86.4(7) . . . . ? N1 Ni N5 C31 90.7(6) . . . . ? N2 Ni N5 C27 57(91) . . . . ? N2 Ni N5 C31 -126(90) . . . . ? N3 Ni N5 C27 92.6(7) . . . . ? N3 Ni N5 C31 -90.2(6) . . . . ? N4 Ni N5 C27 2.9(6) . . . . ? N4 Ni N5 C31 -179.9(7) . . . . ? N6 Ni N5 C27 -177.1(7) . . . . ? N6 Ni N5 C31 .0(6) . . . . ? N1 Ni N6 C32 -98.0(7) . . . . ? N1 Ni N6 C33 68.2(7) . . . . ? N2 Ni N6 C32 179.9(6) . . . . ? N2 Ni N6 C33 -13.9(7) . . . . ? N3 Ni N6 C32 97.4(7) . . . . ? N3 Ni N6 C33 -96.4(7) . . . . ? N4 Ni N6 C32 0(2) . . . . ? N4 Ni N6 C33 167(1) . . . . ? N5 Ni N6 C32 .1(6) . . . . ? N5 Ni N6 C33 166.2(7) . . . . ? Ni N1 C1 C2 -77(1) . . . . ? Ni N1 C1 C6 98.6(9) . . . . ? C7 N1 C1 C2 116(1) . . . . ? C7 N1 C1 C6 -68(1) . . . . ? Ni N1 C7 O1 -177.1(8) . . . . ? Ni N1 C7 C8 1(1) . . . . ? C1 N1 C7 O1 -10(1) . . . . ? C1 N1 C7 C8 168.7(8) . . . . ? Ni N2 C8 C7 6(1) . . . . ? Ni N2 C8 C9 -178.4(7) . . . . ? C12 N2 C8 C7 -178.1(8) . . . . ? C12 N2 C8 C9 -2(1) . . . . ? Ni N2 C12 C11 177.1(7) . . . . ? Ni N2 C12 C13 -2(1) . . . . ? C8 N2 C12 C11 0(1) . . . . ? C8 N2 C12 C13 -178.1(8) . . . . ? Ni N3 C13 O2 179.9(8) . . . . ? Ni N3 C13 C12 -2(1) . . . . ? C14 N3 C13 O2 -7(2) . . . . ? C14 N3 C13 C12 170.4(8) . . . . ? Ni N3 C14 C15 -87(1) . . . . ? Ni N3 C14 C19 93.9(9) . . . . ? C13 N3 C14 C15 100(1) . . . . ? C13 N3 C14 C19 -79(1) . . . . ? Ni N4 C20 C21 -91(1) . . . . ? Ni N4 C20 C25 85(1) . . . . ? C26 N4 C20 C21 76(1) . . . . ? C26 N4 C20 C25 -108(1) . . . . ? Ni N4 C26 O3 175.5(8) . . . . ? Ni N4 C26 C27 -4.2(9) . . . . ? C20 N4 C26 O3 8(1) . . . . ? C20 N4 C26 C27 -172.2(8) . . . . ? Ni N5 C27 C26 -6(1) . . . . ? Ni N5 C27 C28 176.3(7) . . . . ? C31 N5 C27 C26 177.0(8) . . . . ? C31 N5 C27 C28 0(1) . . . . ? Ni N5 C31 C30 -176.7(7) . . . . ? Ni N5 C31 C32 -.1(9) . . . . ? C27 N5 C31 C30 0(1) . . . . ? C27 N5 C31 C32 176.9(8) . . . . ? Ni N6 C32 O4 179.6(8) . . . . ? Ni N6 C32 C31 -.1(9) . . . . ? C33 N6 C32 O4 13(1) . . . . ? C33 N6 C32 C31 -166.4(7) . . . . ? Ni N6 C33 C34 83(1) . . . . ? Ni N6 C33 C38 -94.1(9) . . . . ? C32 N6 C33 C34 -112(1) . . . . ? C32 N6 C33 C38 71(1) . . . . ? N1 C1 C2 C3 172.3(9) . . . . ? N1 C1 C2 H2 -7(1) . . . . ? C6 C1 C2 C3 -3(1) . . . . ? C6 C1 C2 H2 177.5(9) . . . . ? N1 C1 C6 C5 -174.0(9) . . . . ? N1 C1 C6 H6 7(1) . . . . ? C2 C1 C6 C5 2(2) . . . . ? C2 C1 C6 H6 -177.4(9) . . . . ? C1 C2 C3 C4 2(2) . . . . ? C1 C2 C3 H3 -179(1) . . . . ? H2 C2 C3 C4 -178(1) . . . . ? H2 C2 C3 H3 0(2) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C2 C3 C4 H4 180(1) . . . . ? H3 C3 C4 C5 -178(1) . . . . ? H3 C3 C4 H4 1(2) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C3 C4 C5 H5 179(1) . . . . ? H4 C4 C5 C6 179(1) . . . . ? H4 C4 C5 H5 0(2) . . . . ? C4 C5 C6 C1 1(2) . . . . ? C4 C5 C6 H6 180(1) . . . . ? H5 C5 C6 C1 180(1) . . . . ? H5 C5 C6 H6 -1(2) . . . . ? N1 C7 C8 N2 -4(1) . . . . ? N1 C7 C8 C9 -179.8(9) . . . . ? O1 C7 C8 N2 174.2(9) . . . . ? O1 C7 C8 C9 -1(2) . . . . ? N2 C8 C9 C10 3(1) . . . . ? N2 C8 C9 H9 -179.7(9) . . . . ? C7 C8 C9 C10 177.8(9) . . . . ? C7 C8 C9 H9 -4(2) . . . . ? C8 C9 C10 C11 -2(2) . . . . ? C8 C9 C10 H10 179(1) . . . . ? H9 C9 C10 C11 -180(1) . . . . ? H9 C9 C10 H10 1(2) . . . . ? C9 C10 C11 C12 0(2) . . . . ? C9 C10 C11 H11 -179(1) . . . . ? H10 C10 C11 C12 180(1) . . . . ? H10 C10 C11 H11 0(2) . . . . ? C10 C11 C12 N2 0(1) . . . . ? C10 C11 C12 C13 179(1) . . . . ? H11 C11 C12 N2 179.7(9) . . . . ? H11 C11 C12 C13 -2(2) . . . . ? N2 C12 C13 N3 3(1) . . . . ? N2 C12 C13 O2 -179.5(9) . . . . ? C11 C12 C13 N3 -176.1(9) . . . . ? C11 C12 C13 O2 2(2) . . . . ? N3 C14 C15 C16 180(1) . . . . ? N3 C14 C15 H15 2(2) . . . . ? C19 C14 C15 C16 -1(2) . . . . ? C19 C14 C15 H15 -179(1) . . . . ? N3 C14 C19 C18 -177.7(9) . . . . ? N3 C14 C19 H19 1(1) . . . . ? C15 C14 C19 C18 3(2) . . . . ? C15 C14 C19 H19 -177.6(9) . . . . ? C14 C15 C16 C17 -2(2) . . . . ? C14 C15 C16 H16 176(1) . . . . ? H15 C15 C16 C17 176(1) . . . . ? H15 C15 C16 H16 -6(2) . . . . ? C15 C16 C17 C18 2(2) . . . . ? C15 C16 C17 H17 -178(1) . . . . ? H16 C16 C17 C18 -176(1) . . . . ? H16 C16 C17 H17 4(2) . . . . ? C16 C17 C18 C19 0(2) . . . . ? C16 C17 C18 H18 -179(1) . . . . ? H17 C17 C18 C19 180(1) . . . . ? H17 C17 C18 H18 1(2) . . . . ? C17 C18 C19 C14 -2(2) . . . . ? C17 C18 C19 H19 178(1) . . . . ? H18 C18 C19 C14 176(1) . . . . ? H18 C18 C19 H19 -3(2) . . . . ? N4 C20 C21 C22 178(1) . . . . ? N4 C20 C21 H21 -5(2) . . . . ? C25 C20 C21 C22 1(2) . . . . ? C25 C20 C21 H21 179(1) . . . . ? N4 C20 C25 C24 -177(1) . . . . ? N4 C20 C25 H25 4(2) . . . . ? C21 C20 C25 C24 0(2) . . . . ? C21 C20 C25 H25 -179(1) . . . . ? C20 C21 C22 C23 0(2) . . . . ? C20 C21 C22 H22 -176(1) . . . . ? H21 C21 C22 C23 -178(1) . . . . ? H21 C21 C22 H22 6(2) . . . . ? C21 C22 C23 C24 -2(2) . . . . ? C21 C22 C23 H23 176(1) . . . . ? H22 C22 C23 C24 174(1) . . . . ? H22 C22 C23 H23 -8(2) . . . . ? C22 C23 C24 C25 3(2) . . . . ? C22 C23 C24 H24 -178(1) . . . . ? H23 C23 C24 C25 -175(1) . . . . ? H23 C23 C24 H24 5(2) . . . . ? C23 C24 C25 C20 -2(2) . . . . ? C23 C24 C25 H25 177(1) . . . . ? H24 C24 C25 C20 179(1) . . . . ? H24 C24 C25 H25 -2(2) . . . . ? N4 C26 C27 N5 6(1) . . . . ? N4 C26 C27 C28 -176.0(9) . . . . ? O3 C26 C27 N5 -173.3(8) . . . . ? O3 C26 C27 C28 4(1) . . . . ? N5 C27 C28 C29 0(1) . . . . ? N5 C27 C28 H28 177.4(9) . . . . ? C26 C27 C28 C29 -178.2(9) . . . . ? C26 C27 C28 H28 0(2) . . . . ? C27 C28 C29 C30 3(1) . . . . ? C27 C28 C29 H29 -174.7(9) . . . . ? H28 C28 C29 C30 -175.5(9) . . . . ? H28 C28 C29 H29 7(2) . . . . ? C28 C29 C30 C31 -3(1) . . . . ? C28 C29 C30 H30 175.6(9) . . . . ? H29 C29 C30 C31 174.3(9) . . . . ? H29 C29 C30 H30 -7(2) . . . . ? C29 C30 C31 N5 2(1) . . . . ? C29 C30 C31 C32 -174.4(9) . . . . ? H30 C30 C31 N5 -177.2(8) . . . . ? H30 C30 C31 C32 7(1) . . . . ? N5 C31 C32 N6 0(1) . . . . ? N5 C31 C32 O4 -179.6(8) . . . . ? C30 C31 C32 N6 176.5(8) . . . . ? C30 C31 C32 O4 -3(1) . . . . ? N6 C33 C34 C35 -176.6(9) . . . . ? N6 C33 C34 H34 3(1) . . . . ? C38 C33 C34 C35 0(1) . . . . ? C38 C33 C34 H34 179.3(9) . . . . ? N6 C33 C38 C37 179.1(9) . . . . ? N6 C33 C38 H38 -3(1) . . . . ? C34 C33 C38 C37 2(1) . . . . ? C34 C33 C38 H38 -179.3(9) . . . . ? C33 C34 C35 C36 -2(2) . . . . ? C33 C34 C35 H35 179.0(9) . . . . ? H34 C34 C35 C36 178(1) . . . . ? H34 C34 C35 H35 0(2) . . . . ? C34 C35 C36 C37 2(2) . . . . ? C34 C35 C36 H36 -175(1) . . . . ? H35 C35 C36 C37 -179(1) . . . . ? H35 C35 C36 H36 3(2) . . . . ? C35 C36 C37 C38 0(2) . . . . ? C35 C36 C37 H37 179(1) . . . . ? H36 C36 C37 C38 178(1) . . . . ? H36 C36 C37 H37 -4(2) . . . . ? C36 C37 C38 C33 -3(2) . . . . ? C36 C37 C38 H38 179(1) . . . . ? H37 C37 C38 C33 179(1) . . . . ? H37 C37 C38 H38 0(2) . . . . ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _reflns_number_total 5697 #ActaC _reflns_number_observed 2368 #ActaC _reflns_observed_criterion refl_observed_if_Inet_>_.000_sigma(Inet) _reflns_d_resolution_high .841 _reflns_d_resolution_low 16.368 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 5.1997 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_observed_status _refln_scale_group_code _publ_requested_journal Inorganic Chemistry #ActaC _publ_requested_coeditor_name Prof. Kenneth R. Poeppelmeier (Email: kpacs@chem.nwu.edu) _publ_contact_author #ActaC ; ? name Prof. R. N. Mukherjee ? institute Indian Institute of Technology Kanpur ? department Department of Chemistry ? address 208 016 ? city Kanpur ? country India ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone ? #ActaC _publ_contact_author_fax ? #ActaC _publ_contact_author_email rnm@iitk.ernet.in #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title Bivalent, Trivalent, and Tetravalent Nickel Complexes with a Common Tridentate Deprotonated Pyridine Bis-Amide Ligand. Molecular Structures of Nickel(II) and Ni(IV) and Redox Activity. _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? ? ? ? ? ? ? ? ?