#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/18/4321858.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_4321858
loop_
_publ_author_name
'Apurba Kumar Patra'
'Rabindranath Mukherjee'
_publ_contact_author
;
     Prof. R. N. Mukherjee
     Indian Institute of Technology Kanpur
     Department of Chemistry
     208 016
     Kanpur
     India
;
_publ_contact_author_email       rnm@iitk.ernet.in
_publ_section_title
;
 Bivalent, Trivalent, and Tetravalent Nickel Complexes with a Common
 Tridentate Deprotonated Pyridine Bis-Amide Ligand. Molecular Structures
 of Nickel(II) and Nickel(IV) and Redox Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1388
_journal_page_last               1393
_journal_paper_doi               10.1021/ic980672e
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'Synthesized in the laboratory'
_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 Ni O4.75'
_chemical_formula_weight         702.19
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             98-00-08
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 99.68(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   14.874(7)
_cell_length_b                   13.300(4)
_cell_length_c                   16.604(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      9.66
_cell_volume                     3238(2)
_computing_data_reduction        xtal_DIFDAT_SORTRF_ADDREF
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal_SIMPEL
_diffrn_ambient_temperature      293
_diffrn_attenuator_code          13.364
_diffrn_measurement_device       CAD4mach
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_detector       'proportional counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed xray_tube'
_diffrn_radiation_type           'Mo K-alpha'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .124
_diffrn_reflns_av_sigmaI/netI    .128
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6220
_diffrn_reflns_reduction_process No_monochr_Lp_applied
_diffrn_reflns_theta_max         25.
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        1.17
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.65
_exptl_absorpt_correction_T_max  0.8323
_exptl_absorpt_correction_T_min  0.8317
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    flotation
_exptl_crystal_description       'block shaped'
_exptl_crystal_F_000             1453.68
_exptl_crystal_preparation
'Ether diffusion to a chloroform solution of the compound'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.143
_refine_diff_density_min         -2.031
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_expression no
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.984
_refine_ls_goodness_of_fit_obs   1.305
_refine_ls_hydrogen_treatment    no
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     451
_refine_ls_number_reflns         2366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .164
_refine_ls_R_factor_obs          .061
_refine_ls_shift/esd_mean        0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .159
_refine_ls_wR_factor_obs         .064
_reflns_d_resolution_high        .841
_reflns_d_resolution_low         16.368
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_observed          2368
_reflns_number_total             5697
_reflns_observed_criterion       refl_observed_if_Inet_>_.000_sigma(Inet)
_cod_data_source_file            ic980672e_2.cif
_cod_data_source_block           C38H27.5N6O4.75Ni
_cod_original_sg_symbol_Hall     -P_2yab
_cod_original_formula_sum        'C38 H27.5 N6 O4.75 Ni'
_cod_database_code               4321858
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,1/2+y,-z
-x,-y,-z
1/2+x,1/2-y,+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
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_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 2 -3
-4 0 4
1 -2 -3
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
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) . . . . ?
loop_
_reflns_scale_group_code
_reflns_scale_meas_F
? 5.1997
