#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:43:10 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301803 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/37/2203796.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_2203796
loop_
_publ_author_name
'Zhen-Feng Chen'
'Jian Zhou'
'Dong-Qing Li'
'Ming-Xiong Tan'
'Hong Liang'
'Yong Zhang'
_publ_section_title
;Bis{3-[(E)-2-(aminocarbonyl)hydrazonomethyl]pyridine-κN}tetraaquanickel(II)
 diacetate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m861
_journal_page_last               m862
_journal_paper_doi               10.1107/S1600536804012425
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (C14 H16 N8 O2)2 (H2 O)4] (C2 H3 O2)2'
_chemical_formula_moiety         'C14 H24 N8 Ni O6 2+, 2C2 H3 O2 1-'
_chemical_formula_sum            'C18 H30 N8 Ni O10'
_chemical_formula_weight         577.21
_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           SHELXL-97
_cell_angle_alpha                65.822(15)
_cell_angle_beta                 69.678(16)
_cell_angle_gamma                82.14(2)
_cell_formula_units_Z            1
_cell_length_a                   7.8498(19)
_cell_length_b                   8.836(2)
_cell_length_c                   10.2711(17)
_cell_measurement_reflns_used    2857
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     609.5(2)
_computing_cell_refinement       'CrystalClear (Rigaku, 1999)'
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2000)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6785
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.9184
_exptl_absorpt_correction_T_min  0.6427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0376
_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)+(0.0234P)²+0.4761P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                2567
_reflns_number_total             2731
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng6031.cif
_cod_data_source_block           I
_cod_original_cell_volume        609.4(2)
_cod_database_code               2203796
_cod_database_fobs_code          2203796
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Ni1 0.5000 0.5000 0.5000 0.01550(11) Uani d S 1 Ni
O1 1.37861(19) 1.20067(17) -0.02653(16) 0.0248(3) Uani d . 1 O
O2 0.25190(19) 0.47181(19) 0.48349(18) 0.0231(3) Uani d . 1 O
O3 0.6289(2) 0.51561(19) 0.28078(16) 0.0204(3) Uani d . 1 O
O4 0.9793(2) 0.4510(2) 0.18607(19) 0.0316(4) Uani d . 1 O
O5 1.05363(19) 0.60590(18) 0.28327(16) 0.0255(3) Uani d . 1 O
N1 0.4678(2) 0.7599(2) 0.41767(18) 0.0190(3) Uani d . 1 N
N2 0.9296(2) 1.0631(2) 0.17038(19) 0.0222(4) Uani d . 1 N
N3 1.0764(2) 1.1672(2) 0.0907(2) 0.0256(4) Uani d . 1 N
N4 1.2605(3) 0.9399(2) 0.0947(2) 0.0251(4) Uani d . 1 N
C1 0.3062(3) 0.8327(3) 0.4540(2) 0.0236(4) Uani d . 1 C
H1 0.2004 0.7649 0.5110 0.028 Uiso calc R 1 H
C2 0.2882(3) 1.0023(3) 0.4116(2) 0.0268(4) Uani d . 1 C
H2A 0.1718 1.0500 0.4378 0.032 Uiso calc R 1 H
C3 0.4415(3) 1.1019(3) 0.3306(2) 0.0250(4) Uani d . 1 C
H3A 0.4320 1.2185 0.3026 0.030 Uiso calc R 1 H
C4 0.6094(3) 1.0296(2) 0.2904(2) 0.0200(4) Uani d . 1 C
C5 0.6148(3) 0.8577(2) 0.3352(2) 0.0198(4) Uani d . 1 C
H5 0.7287 0.8075 0.3057 0.024 Uiso calc R 1 H
C6 0.7752(3) 1.1301(2) 0.2085(2) 0.0219(4) Uani d . 1 C
H6 0.7683 1.2464 0.1832 0.026 Uiso calc R 1 H
C7 1.2461(3) 1.1033(2) 0.0500(2) 0.0205(4) Uani d . 1 C
C8 1.0929(3) 0.5264(2) 0.1986(2) 0.0195(4) Uani d . 1 C
C9 1.2899(3) 0.5237(3) 0.1074(3) 0.0283(5) Uani d . 1 C
H9A 1.3049 0.4496 0.0547 0.042 Uiso calc R 1 H
H9B 1.3637 0.4837 0.1747 0.042 Uiso calc R 1 H
H9C 1.3293 0.6361 0.0335 0.042 Uiso calc R 1 H
H2B 0.217(4) 0.524(4) 0.408(3) 0.048(8) Uiso d . 1 H
H2C 0.155(4) 0.447(4) 0.563(4) 0.056(9) Uiso d . 1 H
H3B 1.068(3) 1.262(3) 0.078(3) 0.024(6) Uiso d . 1 H
H3C 0.743(4) 0.500(4) 0.261(3) 0.045(8) Uiso d . 1 H
H3D 0.618(4) 0.599(4) 0.214(4) 0.060(10) Uiso d . 1 H
H4A 1.168(4) 0.876(3) 0.152(3) 0.035(7) Uiso d . 1 H
H4B 1.371(4) 0.896(3) 0.073(3) 0.035(7) Uiso d . 1 H
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'
Ni Ni 0.3393 1.1124 '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'
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
_geom_angle_publ_flag
O2 Ni1 O2 . 2_666 180.0 ?
O2 Ni1 O3 . . 90.14(6) yes
O2 Ni1 O3 2_666 . 89.86(6) ?
O2 Ni1 O3 . 2_666 89.86(6) yes
O2 Ni1 O3 2_666 2_666 90.14(6) ?
O3 Ni1 O3 . 2_666 180.0 ?
O2 Ni1 N1 . . 90.34(6) yes
O2 Ni1 N1 . 2_666 89.66(6) yes
O2 Ni1 N1 2_666 2_666 90.34(6) ?
O3 Ni1 N1 . . 89.83(6) yes
O3 Ni1 N1 . 2_666 90.17(6) yes
O3 Ni1 N1 2_666 2_666 89.83(6) ?
O2 Ni1 N1 2_666 . 89.66(6) ?
O3 Ni1 N1 2_666 . 90.17(6) ?
N1 Ni1 N1 2_666 . 180.0 ?
Ni1 O2 H2B . . 126(2) ?
Ni1 O2 H2C . . 120(2) ?
H2B O2 H2C . . 107(3) ?
Ni1 O3 H3C . . 113.0(19) ?
Ni1 O3 H3D . . 118(2) ?
H3C O3 H3D . . 105(3) ?
C5 N1 C1 . . 117.85(17) ?
C5 N1 Ni1 . . 119.32(13) ?
C1 N1 Ni1 . . 122.64(13) ?
C6 N2 N3 . . 116.60(17) yes
N2 N3 C7 . . 119.62(17) yes
N2 N3 H3B . . 121.2(17) ?
C7 N3 H3B . . 118.5(17) ?
C7 N4 H4A . . 121.1(18) ?
C7 N4 H4B . . 118.6(17) ?
H4A N4 H4B . . 120(2) ?
N1 C1 C2 . . 122.47(19) ?
N1 C1 H1 . . 118.8 ?
C2 C1 H1 . . 118.8 ?
C1 C2 C3 . . 119.23(19) ?
C1 C2 H2A . . 120.4 ?
C3 C2 H2A . . 120.4 ?
C2 C3 C4 . . 119.28(19) ?
C2 C3 H3A . . 120.4 ?
C4 C3 H3A . . 120.4 ?
C3 C4 C5 . . 117.69(18) ?
C3 C4 C6 . . 120.93(18) ?
C5 C4 C6 . . 121.35(18) ?
N1 C5 C4 . . 123.43(18) ?
N1 C5 H5 . . 118.3 ?
C4 C5 H5 . . 118.3 ?
N2 C6 C4 . . 120.71(18) ?
N2 C6 H6 . . 119.6 ?
C4 C6 H6 . . 119.6 ?
O1 C7 N4 . . 123.52(19) ?
O1 C7 N3 . . 118.87(18) ?
N4 C7 N3 . . 117.61(18) ?
O4 C8 O5 . . 124.30(18) ?
O4 C8 C9 . . 118.62(18) ?
O5 C8 C9 . . 117.09(17) ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
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 O2 . 2.0689(15) yes
Ni1 O2 2_666 2.0689(15) ?
Ni1 O3 . 2.0770(15) yes
Ni1 O3 2_666 2.0770(15) ?
Ni1 N1 2_666 2.1098(17) ?
Ni1 N1 . 2.1098(17) yes
C7 O1 . 1.250(2) ?
O2 H2B . 0.84(3) ?
O2 H2C . 0.87(3) ?
O3 H3C . 0.85(3) ?
O3 H3D . 0.79(4) ?
C8 O4 . 1.252(2) ?
C8 O5 . 1.265(2) ?
C5 N1 . 1.338(2) ?
N1 C1 . 1.344(3) ?
C6 N2 . 1.279(3) ?
C7 N3 . 1.367(3) ?
C7 N4 . 1.326(3) ?
N2 N3 . 1.364(2) ?
N3 H3B . 0.79(2) ?
N4 H4A . 0.86(3) ?
N4 H4B . 0.89(3) ?
C1 C2 . 1.381(3) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.381(3) ?
C2 H2A . 0.9500 ?
C3 C4 . 1.387(3) ?
C3 H3A . 0.9500 ?
C4 C5 . 1.394(3) ?
C4 C6 . 1.461(3) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C8 C9 . 1.507(3) ?
C9 H9A . 0.9800 ?
C9 H9B . 0.9800 ?
C9 H9C . 0.9800 ?
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
O2 H2b O5 1_455 0.84(3) 1.98(3) 2.789(2) 160(3)
N3 H3b O4 1_565 0.79(2) 2.27(2) 2.966(2) 147(2)
O3 H3c O4 . 0.85(3) 1.81(3) 2.647(2) 166(3)
N4 H4a O5 . 0.86(3) 2.33(3) 3.089(3) 147(2)
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
O2 Ni1 N1 C5 . -148.10(14)
O2 Ni1 N1 C5 2_666 31.90(14)
O3 Ni1 N1 C5 . -57.96(14)
O3 Ni1 N1 C5 2_666 122.04(14)
O2 Ni1 N1 C1 . 37.12(16)
O2 Ni1 N1 C1 2_666 -142.88(16)
O3 Ni1 N1 C1 . 127.26(16)
O3 Ni1 N1 C1 2_666 -52.74(16)
C6 N2 N3 C7 . 178.21(19)
C5 N1 C1 C2 . -1.1(3)
Ni1 N1 C1 C2 . 173.78(16)
N1 C1 C2 C3 . -0.9(3)
C1 C2 C3 C4 . 1.6(3)
C2 C3 C4 C5 . -0.3(3)
C2 C3 C4 C6 . -178.24(19)
C1 N1 C5 C4 . 2.5(3)
Ni1 N1 C5 C4 . -172.54(15)
C3 C4 C5 N1 . -1.8(3)
C6 C4 C5 N1 . 176.11(18)
N3 N2 C6 C4 . 178.32(17)
C3 C4 C6 N2 . -179.32(19)
C5 C4 C6 N2 . 2.8(3)
N2 N3 C7 O1 . 178.03(17)
N2 N3 C7 N4 . -2.0(3)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168308747
