#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/17/2231732.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2231732
loop_
_publ_author_name
'Chen, Xiao-Hua'
'Xie, Chun-Ling'
'Yang, Ming-Xing'
'Chen, Li-Juan'
_publ_section_title
;
 Bis[μ-N'-(2-methyl-1-oxidopropanylidene)-2-oxidobenzohydrazidato]tetrapyridinetrinickel(II)
;
_journal_coeditor_code           XU5275
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1308
_journal_page_last               m1309
_journal_paper_doi               10.1107/S1600536811034362
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni3 (C11 H11 N2 O3) (C5 H5 N)4]'
_chemical_formula_moiety         'C42 H42 N8 Ni3 O6'
_chemical_formula_sum            'C42 H42 N8 Ni3 O6'
_chemical_formula_weight         930.97
_chemical_name_systematic
;
Bis[μ-N'-(2-methyl-1-oxidopropanylidene)-2-
oxidobenzohydrazidato]tetrapyridinetrinickel(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                109.324(15)
_cell_angle_beta                 96.474(13)
_cell_angle_gamma                93.516(13)
_cell_formula_units_Z            2
_cell_length_a                   9.866(3)
_cell_length_b                   12.325(5)
_cell_length_c                   18.240(7)
_cell_measurement_reflns_used    5875
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.11
_cell_volume                     2068.1(13)
_computing_cell_refinement
'TEXRAY (Molecular Structure Corporation, 1999)'
_computing_data_collection
'TEXRAY (Molecular Structure Corporation, 1999)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1999)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20490
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.409
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'TEXRAY (Molecular Structure Corporation, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0318P)²+0.8559P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                5875
_reflns_number_total             9360
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu5275.cif
_cod_data_source_block           I
_cod_original_cell_volume        2068.2(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2231732
_cod_database_fobs_code          2231732
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Ni Ni1 0.93957(4) 0.66089(3) 0.05241(2) 0.03894(12) Uani d . 1 1
Ni Ni2 1.0000 1.0000 0.0000 0.03734(15) Uani d S 1 2
Ni Ni3 -0.06516(5) 0.32923(4) 0.44143(3) 0.05115(14) Uani d . 1 1
Ni Ni4 0.0000 0.0000 0.5000 0.04078(16) Uani d S 1 2
O O1 0.7678(2) 0.5919(2) 0.01168(15) 0.0569(7) Uani d . 1 1
O O2 0.8335(2) 0.88568(18) -0.05727(13) 0.0420(5) Uani d . 1 1
O O3 1.1140(2) 0.73331(19) 0.09258(14) 0.0468(6) Uani d . 1 1
O O4 0.0721(3) 0.3594(2) 0.39034(17) 0.0677(8) Uani d . 1 1
O O5 0.1519(2) 0.0692(2) 0.45856(14) 0.0476(6) Uani d . 1 1
O O6 -0.1979(2) 0.3001(2) 0.49806(15) 0.0572(7) Uani d . 1 1
N N1 0.9243(3) 0.7769(2) 0.01130(15) 0.0374(6) Uani d . 1 1
N N2 1.0431(2) 0.8583(2) 0.03276(15) 0.0378(6) Uani d . 1 1
N N3 0.9702(3) 0.5467(2) 0.10306(16) 0.0427(7) Uani d . 1 1
N N4 0.8942(3) 1.0555(2) 0.10051(16) 0.0419(7) Uani d . 1 1
N N5 0.0080(3) 0.2072(2) 0.46030(16) 0.0447(7) Uani d . 1 1
N N6 -0.0704(3) 0.1552(2) 0.50322(16) 0.0435(7) Uani d . 1 1
N N7 -0.1622(4) 0.4484(3) 0.41838(19) 0.0596(8) Uani d . 1 1
N N8 -0.1065(3) -0.0751(2) 0.38106(17) 0.0484(7) Uani d . 1 1
C C1 0.6842(3) 0.6149(3) -0.0418(2) 0.0451(8) Uani d . 1 1
C C2 0.7023(3) 0.7135(3) -0.06517(19) 0.0395(8) Uani d . 1 1
C C3 0.6044(3) 0.7264(3) -0.1220(2) 0.0526(9) Uani d . 1 1
H H3A 0.6150 0.7918 -0.1365 0.063 Uiso calc R 1 1
C C4 0.4933(4) 0.6470(4) -0.1574(2) 0.0647(11) Uani d . 1 1
H H4A 0.4300 0.6579 -0.1955 0.078 Uiso calc R 1 1
C C5 0.4767(4) 0.5501(4) -0.1356(2) 0.0650(11) Uani d . 1 1
H H5A 0.4021 0.4948 -0.1597 0.078 Uiso calc R 1 1
C C6 0.5686(4) 0.5351(3) -0.0793(2) 0.0590(11) Uani d . 1 1
H H6A 0.5546 0.4699 -0.0651 0.071 Uiso calc R 1 1
C C7 0.8246(3) 0.7977(3) -0.03513(19) 0.0376(7) Uani d . 1 1
C C8 1.1369(3) 0.8261(3) 0.07424(19) 0.0389(8) Uani d . 1 1
C C9 1.2773(3) 0.8907(3) 0.1018(2) 0.0502(9) Uani d . 1 1
H H9A 1.2785 0.9612 0.0882 0.060 Uiso calc R 1 1
C C10 1.3833(4) 0.8170(4) 0.0608(3) 0.0841(14) Uani d . 1 1
H H10A 1.3609 0.7974 0.0050 0.126 Uiso calc R 1 1
H H10B 1.3833 0.7475 0.0737 0.126 Uiso calc R 1 1
H H10C 1.4726 0.8596 0.0778 0.126 Uiso calc R 1 1
C C11 1.3106(5) 0.9247(4) 0.1904(3) 0.0884(15) Uani d . 1 1
H H11A 1.2415 0.9695 0.2149 0.133 Uiso calc R 1 1
H H11B 1.3984 0.9698 0.2078 0.133 Uiso calc R 1 1
H H11C 1.3130 0.8563 0.2044 0.133 Uiso calc R 1 1
C C12 0.8723(4) 0.4652(3) 0.0996(2) 0.0598(11) Uani d . 1 1
H H12A 0.7873 0.4614 0.0706 0.072 Uiso calc R 1 1
C C13 0.8922(5) 0.3859(4) 0.1375(3) 0.0742(13) Uani d . 1 1
H H13A 0.8215 0.3300 0.1337 0.089 Uiso calc R 1 1
C C14 1.0156(5) 0.3904(3) 0.1804(2) 0.0666(12) Uani d . 1 1
H H14A 1.0297 0.3396 0.2078 0.080 Uiso calc R 1 1
C C15 1.1185(4) 0.4712(3) 0.1824(2) 0.0595(10) Uani d . 1 1
H H15A 1.2053 0.4744 0.2095 0.071 Uiso calc R 1 1
C C16 1.0912(4) 0.5474(3) 0.1436(2) 0.0556(10) Uani d . 1 1
H H16A 1.1614 0.6028 0.1458 0.067 Uiso calc R 1 1
C C17 0.7578(4) 1.0526(3) 0.0959(2) 0.0589(10) Uani d . 1 1
H H17A 0.7054 1.0243 0.0465 0.071 Uiso calc R 1 1
C C18 0.6920(4) 1.0892(4) 0.1602(3) 0.0709(12) Uani d . 1 1
H H18A 0.5969 1.0864 0.1544 0.085 Uiso calc R 1 1
C C19 0.7665(5) 1.1297(4) 0.2327(3) 0.0807(14) Uani d . 1 1
H H19A 0.7234 1.1555 0.2772 0.097 Uiso calc R 1 1
C C20 0.9062(5) 1.1318(4) 0.2392(2) 0.0721(12) Uani d . 1 1
H H20A 0.9599 1.1582 0.2882 0.087 Uiso calc R 1 1
C C21 0.9648(4) 1.0943(3) 0.1721(2) 0.0550(10) Uani d . 1 1
H H21A 1.0599 1.0961 0.1769 0.066 Uiso calc R 1 1
C C22 0.1843(4) 0.3066(4) 0.3802(2) 0.0629(11) Uani d . 1 1
C C23 0.2116(3) 0.2087(3) 0.4006(2) 0.0486(9) Uani d . 1 1
C C24 0.3333(4) 0.1602(4) 0.3849(2) 0.0651(11) Uani d . 1 1
H H24A 0.3507 0.0952 0.3982 0.078 Uiso calc R 1 1
C C25 0.4290(5) 0.2053(5) 0.3502(3) 0.0870(15) Uani d . 1 1
H H25A 0.5096 0.1714 0.3400 0.104 Uiso calc R 1 1
C C26 0.4023(5) 0.3012(5) 0.3312(3) 0.0936(18) Uani d . 1 1
H H26A 0.4667 0.3332 0.3086 0.112 Uiso calc R 1 1
C C27 0.2836(5) 0.3508(4) 0.3446(3) 0.0805(15) Uani d . 1 1
H H27A 0.2678 0.4149 0.3300 0.097 Uiso calc R 1 1
C C28 0.1207(3) 0.1579(3) 0.4412(2) 0.0446(8) Uani d . 1 1
C C29 -0.1747(4) 0.2131(3) 0.5209(2) 0.0469(8) Uani d . 1 1
C C30 -0.2695(4) 0.1822(3) 0.5716(2) 0.0574(10) Uani d . 1 1
H H30A -0.2430 0.1121 0.5810 0.069 Uiso calc R 1 1
C C31 -0.2554(5) 0.2809(4) 0.6499(3) 0.0929(16) Uani d . 1 1
H H31A -0.1615 0.2951 0.6742 0.139 Uiso calc R 1 1
H H31B -0.3124 0.2602 0.6836 0.139 Uiso calc R 1 1
H H31C -0.2834 0.3494 0.6413 0.139 Uiso calc R 1 1
C C32 -0.4159(4) 0.1598(4) 0.5316(3) 0.0933(17) Uani d . 1 1
H H32A -0.4219 0.1016 0.4807 0.140 Uiso calc R 1 1
H H32B -0.4452 0.2299 0.5261 0.140 Uiso calc R 1 1
H H32C -0.4738 0.1335 0.5626 0.140 Uiso calc R 1 1
C C33 -0.1188(6) 0.5050(4) 0.3733(3) 0.1002(18) Uani d . 1 1
H H33A -0.0362 0.4888 0.3541 0.120 Uiso calc R 1 1
C C34 -0.1897(7) 0.5859(5) 0.3537(4) 0.119(2) Uani d . 1 1
H H34A -0.1563 0.6220 0.3210 0.143 Uiso calc R 1 1
C C35 -0.3087(7) 0.6130(4) 0.3823(3) 0.1012(18) Uani d . 1 1
H H35A -0.3583 0.6678 0.3700 0.121 Uiso calc R 1 1
C C36 -0.3529(6) 0.5582(4) 0.4291(3) 0.0996(17) Uani d . 1 1
H H36A -0.4343 0.5745 0.4497 0.120 Uiso calc R 1 1
C C37 -0.2764(5) 0.4775(4) 0.4463(3) 0.0839(14) Uani d . 1 1
H H37A -0.3077 0.4416 0.4796 0.101 Uiso calc R 1 1
C C38 -0.2429(4) -0.0946(4) 0.3670(3) 0.0684(12) Uani d . 1 1
H H38A -0.2918 -0.0726 0.4094 0.082 Uiso calc R 1 1
C C39 -0.3142(5) -0.1448(5) 0.2939(3) 0.0911(16) Uani d . 1 1
H H39A -0.4095 -0.1555 0.2867 0.109 Uiso calc R 1 1
C C40 -0.2437(6) -0.1797(4) 0.2305(3) 0.0912(16) Uani d . 1 1
H H40A -0.2897 -0.2164 0.1800 0.109 Uiso calc R 1 1
C C41 -0.1053(6) -0.1588(4) 0.2441(3) 0.0875(15) Uani d . 1 1
H H41A -0.0543 -0.1800 0.2026 0.105 Uiso calc R 1 1
C C42 -0.0414(4) -0.1066(4) 0.3187(2) 0.0658(11) Uani d . 1 1
H H42A 0.0537 -0.0920 0.3267 0.079 Uiso calc R 1 1
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'
O O 0.0106 0.0060 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Ni1 N1 . . 94.86(11)
O1 Ni1 O3 . . 178.73(10)
N1 Ni1 O3 . . 83.88(10)
O1 Ni1 N3 . . 90.25(11)
N1 Ni1 N3 . . 174.59(12)
O3 Ni1 N3 . . 91.01(10)
O2 Ni2 O2 . 2_775 180.0000(10)
O2 Ni2 N2 . 2_775 101.40(9)
O2 Ni2 N2 2_775 2_775 78.60(9)
O2 Ni2 N2 . . 78.60(9)
O2 Ni2 N2 2_775 . 101.40(9)
N2 Ni2 N2 2_775 . 180.00(13)
O2 Ni2 N4 . . 88.41(10)
O2 Ni2 N4 2_775 . 91.59(10)
N2 Ni2 N4 2_775 . 93.00(10)
N2 Ni2 N4 . . 87.00(10)
O2 Ni2 N4 . 2_775 91.59(10)
O2 Ni2 N4 2_775 2_775 88.41(10)
N2 Ni2 N4 2_775 2_775 87.00(10)
N2 Ni2 N4 . 2_775 93.00(10)
N4 Ni2 N4 . 2_775 180.0000(10)
O4 Ni3 N5 . . 94.82(12)
O4 Ni3 O6 . . 176.94(12)
N5 Ni3 O6 . . 83.73(11)
O4 Ni3 N7 . . 89.84(14)
N5 Ni3 N7 . . 173.64(13)
O6 Ni3 N7 . . 91.82(13)
O5 Ni4 O5 . 2_556 180.0
O5 Ni4 N6 . . 78.90(10)
O5 Ni4 N6 2_556 . 101.10(10)
O5 Ni4 N6 . 2_556 101.10(10)
O5 Ni4 N6 2_556 2_556 78.90(10)
N6 Ni4 N6 . 2_556 180.0
O5 Ni4 N8 . . 89.05(10)
O5 Ni4 N8 2_556 . 90.95(10)
N6 Ni4 N8 . . 88.16(11)
N6 Ni4 N8 2_556 . 91.84(11)
O5 Ni4 N8 . 2_556 90.95(10)
O5 Ni4 N8 2_556 2_556 89.05(10)
N6 Ni4 N8 . 2_556 91.84(11)
N6 Ni4 N8 2_556 2_556 88.16(11)
N8 Ni4 N8 . 2_556 180.0
C1 O1 Ni1 . . 126.08(19)
C7 O2 Ni2 . . 112.94(19)
C8 O3 Ni1 . . 112.0(2)
C22 O4 Ni3 . . 126.6(2)
C28 O5 Ni4 . . 113.2(2)
C29 O6 Ni3 . . 111.7(2)
C7 N1 N2 . . 114.7(2)
C7 N1 Ni1 . . 131.7(2)
N2 N1 Ni1 . . 113.58(18)
C8 N2 N1 . . 109.5(2)
C8 N2 Ni2 . . 140.3(2)
N1 N2 Ni2 . . 109.56(18)
C16 N3 C12 . . 116.8(3)
C16 N3 Ni1 . . 120.9(2)
C12 N3 Ni1 . . 122.3(2)
C21 N4 C17 . . 116.5(3)
C21 N4 Ni2 . . 119.9(2)
C17 N4 Ni2 . . 123.6(3)
C28 N5 N6 . . 114.2(3)
C28 N5 Ni3 . . 131.7(2)
N6 N5 Ni3 . . 114.1(2)
C29 N6 N5 . . 108.5(3)
C29 N6 Ni4 . . 140.6(2)
N5 N6 Ni4 . . 109.83(19)
C37 N7 C33 . . 115.9(4)
C37 N7 Ni3 . . 121.4(3)
C33 N7 Ni3 . . 122.7(3)
C42 N8 C38 . . 116.2(4)
C42 N8 Ni4 . . 122.8(3)
C38 N8 Ni4 . . 121.0(3)
O1 C1 C6 . . 117.4(3)
O1 C1 C2 . . 125.3(3)
C6 C1 C2 . . 117.3(3)
C3 C2 C1 . . 118.6(3)
C3 C2 C7 . . 119.0(3)
C1 C2 C7 . . 122.3(3)
C4 C3 C2 . . 122.6(3)
C4 C3 H3A . . 118.7
C2 C3 H3A . . 118.7
C3 C4 C5 . . 118.8(4)
C3 C4 H4A . . 120.6
C5 C4 H4A . . 120.6
C6 C5 C4 . . 120.4(3)
C6 C5 H5A . . 119.8
C4 C5 H5A . . 119.8
C5 C6 C1 . . 122.2(3)
C5 C6 H6A . . 118.9
C1 C6 H6A . . 118.9
O2 C7 N1 . . 122.2(3)
O2 C7 C2 . . 119.3(3)
N1 C7 C2 . . 118.5(3)
N2 C8 O3 . . 121.0(3)
N2 C8 C9 . . 122.1(3)
O3 C8 C9 . . 116.8(3)
C8 C9 C11 . . 110.1(3)
C8 C9 C10 . . 110.0(3)
C11 C9 C10 . . 111.0(3)
C8 C9 H9A . . 108.6
C11 C9 H9A . . 108.6
C10 C9 H9A . . 108.6
C9 C10 H10A . . 109.5
C9 C10 H10B . . 109.5
H10A C10 H10B . . 109.5
C9 C10 H10C . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
C9 C11 H11A . . 109.5
C9 C11 H11B . . 109.5
H11A C11 H11B . . 109.5
C9 C11 H11C . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
N3 C12 C13 . . 122.6(4)
N3 C12 H12A . . 118.7
C13 C12 H12A . . 118.7
C14 C13 C12 . . 119.5(4)
C14 C13 H13A . . 120.2
C12 C13 H13A . . 120.2
C13 C14 C15 . . 118.7(3)
C13 C14 H14A . . 120.7
C15 C14 H14A . . 120.7
C14 C15 C16 . . 118.6(4)
C14 C15 H15A . . 120.7
C16 C15 H15A . . 120.7
N3 C16 C15 . . 123.8(3)
N3 C16 H16A . . 118.1
C15 C16 H16A . . 118.1
N4 C17 C18 . . 123.0(4)
N4 C17 H17A . . 118.5
C18 C17 H17A . . 118.5
C19 C18 C17 . . 119.4(4)
C19 C18 H18A . . 120.3
C17 C18 H18A . . 120.3
C18 C19 C20 . . 118.8(4)
C18 C19 H19A . . 120.6
C20 C19 H19A . . 120.6
C21 C20 C19 . . 118.4(4)
C21 C20 H20A . . 120.8
C19 C20 H20A . . 120.8
N4 C21 C20 . . 123.9(4)
N4 C21 H21A . . 118.1
C20 C21 H21A . . 118.1
O4 C22 C23 . . 125.2(3)
O4 C22 C27 . . 117.2(4)
C23 C22 C27 . . 117.6(4)
C24 C23 C22 . . 119.1(3)
C24 C23 C28 . . 117.7(3)
C22 C23 C28 . . 123.1(4)
C25 C24 C23 . . 122.1(4)
C25 C24 H24A . . 119.0
C23 C24 H24A . . 119.0
C26 C25 C24 . . 118.4(5)
C26 C25 H25A . . 120.8
C24 C25 H25A . . 120.8
C27 C26 C25 . . 121.5(4)
C27 C26 H26A . . 119.2
C25 C26 H26A . . 119.2
C26 C27 C22 . . 121.2(4)
C26 C27 H27A . . 119.4
C22 C27 H27A . . 119.4
O5 C28 N5 . . 121.8(3)
O5 C28 C23 . . 120.0(3)
N5 C28 C23 . . 118.2(3)
O6 C29 N6 . . 121.9(3)
O6 C29 C30 . . 118.3(3)
N6 C29 C30 . . 119.7(3)
C29 C30 C32 . . 110.6(3)
C29 C30 C31 . . 109.0(3)
C32 C30 C31 . . 110.4(4)
C29 C30 H30A . . 108.9
C32 C30 H30A . . 108.9
C31 C30 H30A . . 108.9
C30 C31 H31A . . 109.5
C30 C31 H31B . . 109.5
H31A C31 H31B . . 109.5
C30 C31 H31C . . 109.5
H31A C31 H31C . . 109.5
H31B C31 H31C . . 109.5
C30 C32 H32A . . 109.5
C30 C32 H32B . . 109.5
H32A C32 H32B . . 109.5
C30 C32 H32C . . 109.5
H32A C32 H32C . . 109.5
H32B C32 H32C . . 109.5
N7 C33 C34 . . 123.3(5)
N7 C33 H33A . . 118.3
C34 C33 H33A . . 118.3
C35 C34 C33 . . 119.5(5)
C35 C34 H34A . . 120.3
C33 C34 H34A . . 120.3
C36 C35 C34 . . 118.0(5)
C36 C35 H35A . . 121.0
C34 C35 H35A . . 121.0
C35 C36 C37 . . 119.4(5)
C35 C36 H36A . . 120.3
C37 C36 H36A . . 120.3
N7 C37 C36 . . 123.8(5)
N7 C37 H37A . . 118.1
C36 C37 H37A . . 118.1
N8 C38 C39 . . 123.3(4)
N8 C38 H38A . . 118.4
C39 C38 H38A . . 118.4
C38 C39 C40 . . 119.3(5)
C38 C39 H39A . . 120.4
C40 C39 H39A . . 120.4
C41 C40 C39 . . 117.9(5)
C41 C40 H40A . . 121.1
C39 C40 H40A . . 121.1
C40 C41 C42 . . 119.4(5)
C40 C41 H41A . . 120.3
C42 C41 H41A . . 120.3
N8 C42 C41 . . 123.9(4)
N8 C42 H42A . . 118.0
C41 C42 H42A . . 118.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O1 . 1.808(2) yes
Ni1 N1 . 1.828(2) yes
Ni1 O3 . 1.841(2) yes
Ni1 N3 . 1.943(3) yes
Ni2 O2 . 2.032(2) yes
Ni2 O2 2_775 2.032(2) no
Ni2 N2 2_775 2.076(2) no
Ni2 N2 . 2.076(2) yes
Ni2 N4 . 2.146(3) yes
Ni2 N4 2_775 2.146(3) no
Ni3 O4 . 1.815(3) yes
Ni3 N5 . 1.823(3) yes
Ni3 O6 . 1.845(2) yes
Ni3 N7 . 1.934(3) yes
Ni4 O5 . 2.018(2) yes
Ni4 O5 2_556 2.018(2) no
Ni4 N6 . 2.060(3) yes
Ni4 N6 2_556 2.060(3) no
Ni4 N8 . 2.169(3) yes
Ni4 N8 2_556 2.169(3) no
O1 C1 . 1.321(4) no
O2 C7 . 1.278(3) no
O3 C8 . 1.308(3) no
O4 C22 . 1.318(5) no
O5 C28 . 1.279(4) no
O6 C29 . 1.296(4) no
N1 C7 . 1.318(4) no
N1 N2 . 1.423(3) no
N2 C8 . 1.293(4) no
N3 C16 . 1.329(4) no
N3 C12 . 1.331(4) no
N4 C21 . 1.327(4) no
N4 C17 . 1.336(4) no
N5 C28 . 1.325(4) no
N5 N6 . 1.425(3) no
N6 C29 . 1.298(4) no
N7 C37 . 1.310(5) no
N7 C33 . 1.329(5) no
N8 C42 . 1.326(5) no
N8 C38 . 1.333(5) no
C1 C6 . 1.407(5) no
C1 C2 . 1.421(4) no
C2 C3 . 1.392(4) no
C2 C7 . 1.467(4) no
C3 C4 . 1.366(5) no
C3 H3A . 0.9300 no
C4 C5 . 1.386(5) no
C4 H4A . 0.9300 no
C5 C6 . 1.359(5) no
C5 H5A . 0.9300 no
C6 H6A . 0.9300 no
C8 C9 . 1.499(4) no
C9 C11 . 1.520(5) no
C9 C10 . 1.524(5) no
C9 H9A . 0.9800 no
C10 H10A . 0.9600 no
C10 H10B . 0.9600 no
C10 H10C . 0.9600 no
C11 H11A . 0.9600 no
C11 H11B . 0.9600 no
C11 H11C . 0.9600 no
C12 C13 . 1.382(5) no
C12 H12A . 0.9300 no
C13 C14 . 1.358(6) no
C13 H13A . 0.9300 no
C14 C15 . 1.366(5) no
C14 H14A . 0.9300 no
C15 C16 . 1.373(5) no
C15 H15A . 0.9300 no
C16 H16A . 0.9300 no
C17 C18 . 1.363(5) no
C17 H17A . 0.9300 no
C18 C19 . 1.356(6) no
C18 H18A . 0.9300 no
C19 C20 . 1.367(6) no
C19 H19A . 0.9300 no
C20 C21 . 1.366(5) no
C20 H20A . 0.9300 no
C21 H21A . 0.9300 no
C22 C23 . 1.409(5) no
C22 C27 . 1.410(5) no
C23 C24 . 1.391(5) no
C23 C28 . 1.461(4) no
C24 C25 . 1.380(5) no
C24 H24A . 0.9300 no
C25 C26 . 1.369(7) no
C25 H25A . 0.9300 no
C26 C27 . 1.364(7) no
C26 H26A . 0.9300 no
C27 H27A . 0.9300 no
C29 C30 . 1.503(5) no
C30 C32 . 1.509(5) no
C30 C31 . 1.525(6) no
C30 H30A . 0.9800 no
C31 H31A . 0.9600 no
C31 H31B . 0.9600 no
C31 H31C . 0.9600 no
C32 H32A . 0.9600 no
C32 H32B . 0.9600 no
C32 H32C . 0.9600 no
C33 C34 . 1.370(6) no
C33 H33A . 0.9300 no
C34 C35 . 1.354(7) no
C34 H34A . 0.9300 no
C35 C36 . 1.342(6) no
C35 H35A . 0.9300 no
C36 C37 . 1.379(6) no
C36 H36A . 0.9300 no
C37 H37A . 0.9300 no
C38 C39 . 1.359(6) no
C38 H38A . 0.9300 no
C39 C40 . 1.376(7) no
C39 H39A . 0.9300 no
C40 C41 . 1.353(6) no
C40 H40A . 0.9300 no
C41 C42 . 1.357(6) no
C41 H41A . 0.9300 no
C42 H42A . 0.9300 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C9 H9A O2 2_775 0.98 2.43 3.332(5) 152
C30 H30A O5 2_556 0.98 2.38 3.272(5) 152
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_site_symmetry_1
_geom_torsion
N1 Ni1 O1 C1 . 11.6(3)
O3 Ni1 O1 C1 . 3(6)
N3 Ni1 O1 C1 . -170.2(3)
O2 Ni2 O2 C7 2_775 4E1(10)
N2 Ni2 O2 C7 2_775 -168.4(2)
N2 Ni2 O2 C7 . 11.6(2)
N4 Ni2 O2 C7 . -75.6(2)
N4 Ni2 O2 C7 2_775 104.4(2)
O1 Ni1 O3 C8 . 10(6)
N1 Ni1 O3 C8 . 1.2(2)
N3 Ni1 O3 C8 . -177.0(2)
N5 Ni3 O4 C22 . -3.7(3)
O6 Ni3 O4 C22 . 58(2)
N7 Ni3 O4 C22 . -179.4(3)
O5 Ni4 O5 C28 2_556 17E1(10)
N6 Ni4 O5 C28 . -12.1(2)
N6 Ni4 O5 C28 2_556 167.9(2)
N8 Ni4 O5 C28 . 76.2(2)
N8 Ni4 O5 C28 2_556 -103.8(2)
O4 Ni3 O6 C29 . -62(2)
N5 Ni3 O6 C29 . -0.4(2)
N7 Ni3 O6 C29 . 175.1(3)
O1 Ni1 N1 C7 . -3.2(3)
O3 Ni1 N1 C7 . 176.7(3)
N3 Ni1 N1 C7 . -163.9(11)
O1 Ni1 N1 N2 . 177.9(2)
O3 Ni1 N1 N2 . -2.3(2)
N3 Ni1 N1 N2 . 17.1(14)
C7 N1 N2 C8 . -176.2(3)
Ni1 N1 N2 C8 . 2.9(3)
C7 N1 N2 Ni2 . 11.2(3)
Ni1 N1 N2 Ni2 . -169.66(12)
O2 Ni2 N2 C8 . 179.1(4)
O2 Ni2 N2 C8 2_775 -0.9(4)
N2 Ni2 N2 C8 2_775 -6E1(10)
N4 Ni2 N2 C8 . -91.9(4)
N4 Ni2 N2 C8 2_775 88.1(4)
O2 Ni2 N2 N1 . -11.92(18)
O2 Ni2 N2 N1 2_775 168.08(18)
N2 Ni2 N2 N1 2_775 11E1(10)
N4 Ni2 N2 N1 . 77.06(19)
N4 Ni2 N2 N1 2_775 -102.94(19)
O1 Ni1 N3 C16 . 177.1(3)
N1 Ni1 N3 C16 . -22.1(14)
O3 Ni1 N3 C16 . -2.8(3)
O1 Ni1 N3 C12 . -3.5(3)
N1 Ni1 N3 C12 . 157.4(12)
O3 Ni1 N3 C12 . 176.7(3)
O2 Ni2 N4 C21 . 149.5(3)
O2 Ni2 N4 C21 2_775 -30.5(3)
N2 Ni2 N4 C21 2_775 -109.2(3)
N2 Ni2 N4 C21 . 70.8(3)
N4 Ni2 N4 C21 2_775 -10E1(10)
O2 Ni2 N4 C17 . -29.8(3)
O2 Ni2 N4 C17 2_775 150.2(3)
N2 Ni2 N4 C17 2_775 71.6(3)
N2 Ni2 N4 C17 . -108.4(3)
N4 Ni2 N4 C17 2_775 9E1(10)
O4 Ni3 N5 C28 . -1.3(3)
O6 Ni3 N5 C28 . -178.6(3)
N7 Ni3 N5 C28 . 135.8(11)
O4 Ni3 N5 N6 . 178.9(2)
O6 Ni3 N5 N6 . 1.6(2)
N7 Ni3 N5 N6 . -44.1(13)
C28 N5 N6 C29 . 177.7(3)
Ni3 N5 N6 C29 . -2.4(3)
C28 N5 N6 Ni4 . -11.8(3)
Ni3 N5 N6 Ni4 . 168.04(13)
O5 Ni4 N6 C29 . 178.2(4)
O5 Ni4 N6 C29 2_556 -1.8(4)
N6 Ni4 N6 C29 2_556 15.9(4)
N8 Ni4 N6 C29 . 88.8(4)
N8 Ni4 N6 C29 2_556 -91.2(4)
O5 Ni4 N6 N5 . 12.52(19)
O5 Ni4 N6 N5 2_556 -167.48(19)
N6 Ni4 N6 N5 2_556 -149.8(4)
N8 Ni4 N6 N5 . -76.9(2)
N8 Ni4 N6 N5 2_556 103.1(2)
O4 Ni3 N7 C37 . -175.2(4)
N5 Ni3 N7 C37 . 47.6(14)
O6 Ni3 N7 C37 . 2.2(4)
O4 Ni3 N7 C33 . 5.3(4)
N5 Ni3 N7 C33 . -131.9(12)
O6 Ni3 N7 C33 . -177.2(4)
O5 Ni4 N8 C42 . 30.4(3)
O5 Ni4 N8 C42 2_556 -149.6(3)
N6 Ni4 N8 C42 . 109.3(3)
N6 Ni4 N8 C42 2_556 -70.7(3)
N8 Ni4 N8 C42 2_556 13E1(10)
O5 Ni4 N8 C38 . -151.1(3)
O5 Ni4 N8 C38 2_556 28.9(3)
N6 Ni4 N8 C38 . -72.2(3)
N6 Ni4 N8 C38 2_556 107.8(3)
N8 Ni4 N8 C38 2_556 -5E1(10)
Ni1 O1 C1 C6 . 165.5(3)
Ni1 O1 C1 C2 . -13.8(5)
O1 C1 C2 C3 . -179.4(3)
C6 C1 C2 C3 . 1.2(5)
O1 C1 C2 C7 . 4.5(5)
C6 C1 C2 C7 . -174.8(3)
C1 C2 C3 C4 . -1.5(6)
C7 C2 C3 C4 . 174.7(4)
C2 C3 C4 C5 . 0.5(6)
C3 C4 C5 C6 . 0.7(6)
C4 C5 C6 C1 . -0.9(7)
O1 C1 C6 C5 . -179.5(4)
C2 C1 C6 C5 . -0.1(6)
Ni2 O2 C7 N1 . -9.4(4)
Ni2 O2 C7 C2 . 173.7(2)
N2 N1 C7 O2 . -1.6(4)
Ni1 N1 C7 O2 . 179.5(2)
N2 N1 C7 C2 . 175.4(3)
Ni1 N1 C7 C2 . -3.6(5)
C3 C2 C7 O2 . 5.3(5)
C1 C2 C7 O2 . -178.7(3)
C3 C2 C7 N1 . -171.8(3)
C1 C2 C7 N1 . 4.3(5)
N1 N2 C8 O3 . -2.0(4)
Ni2 N2 C8 O3 . 167.0(2)
N1 N2 C8 C9 . 176.4(3)
Ni2 N2 C8 C9 . -14.6(6)
Ni1 O3 C8 N2 . 0.2(4)
Ni1 O3 C8 C9 . -178.3(2)
N2 C8 C9 C11 . 125.0(4)
O3 C8 C9 C11 . -56.6(4)
N2 C8 C9 C10 . -112.4(4)
O3 C8 C9 C10 . 66.0(4)
C16 N3 C12 C13 . 1.6(6)
Ni1 N3 C12 C13 . -178.0(3)
N3 C12 C13 C14 . 0.2(7)
C12 C13 C14 C15 . -2.3(7)
C13 C14 C15 C16 . 2.6(6)
C12 N3 C16 C15 . -1.2(6)
Ni1 N3 C16 C15 . 178.3(3)
C14 C15 C16 N3 . -0.8(6)
C21 N4 C17 C18 . 1.3(5)
Ni2 N4 C17 C18 . -179.4(3)
N4 C17 C18 C19 . -0.7(6)
C17 C18 C19 C20 . -0.5(7)
C18 C19 C20 C21 . 0.8(7)
C17 N4 C21 C20 . -1.0(5)
Ni2 N4 C21 C20 . 179.7(3)
C19 C20 C21 N4 . -0.1(6)
Ni3 O4 C22 C23 . 6.7(6)
Ni3 O4 C22 C27 . -174.5(3)
O4 C22 C23 C24 . 178.6(4)
C27 C22 C23 C24 . -0.2(6)
O4 C22 C23 C28 . -4.4(6)
C27 C22 C23 C28 . 176.9(4)
C22 C23 C24 C25 . 0.4(6)
C28 C23 C24 C25 . -176.8(4)
C23 C24 C25 C26 . 0.2(7)
C24 C25 C26 C27 . -1.1(8)
C25 C26 C27 C22 . 1.3(8)
O4 C22 C27 C26 . -179.5(4)
C23 C22 C27 C26 . -0.7(7)
Ni4 O5 C28 N5 . 9.5(4)
Ni4 O5 C28 C23 . -171.7(2)
N6 N5 C28 O5 . 1.9(5)
Ni3 N5 C28 O5 . -177.9(2)
N6 N5 C28 C23 . -177.0(3)
Ni3 N5 C28 C23 . 3.2(5)
C24 C23 C28 O5 . -2.5(5)
C22 C23 C28 O5 . -179.6(3)
C24 C23 C28 N5 . 176.5(3)
C22 C23 C28 N5 . -0.6(5)
Ni3 O6 C29 N6 . -1.1(4)
Ni3 O6 C29 C30 . 176.7(3)
N5 N6 C29 O6 . 2.3(5)
Ni4 N6 C29 O6 . -163.5(3)
N5 N6 C29 C30 . -175.5(3)
Ni4 N6 C29 C30 . 18.7(6)
O6 C29 C30 C32 . 56.5(5)
N6 C29 C30 C32 . -125.7(4)
O6 C29 C30 C31 . -65.0(5)
N6 C29 C30 C31 . 112.8(4)
C37 N7 C33 C34 . -2.5(8)
Ni3 N7 C33 C34 . 177.0(5)
N7 C33 C34 C35 . 1.5(10)
C33 C34 C35 C36 . -0.2(10)
C34 C35 C36 C37 . 0.1(9)
C33 N7 C37 C36 . 2.4(7)
Ni3 N7 C37 C36 . -177.1(4)
C35 C36 C37 N7 . -1.3(9)
C42 N8 C38 C39 . 0.8(6)
Ni4 N8 C38 C39 . -177.8(4)
N8 C38 C39 C40 . 1.1(7)
C38 C39 C40 C41 . -2.0(8)
C39 C40 C41 C42 . 1.0(8)
C38 N8 C42 C41 . -1.8(6)
Ni4 N8 C42 C41 . 176.7(3)
C40 C41 C42 N8 . 0.9(8)
