#------------------------------------------------------------------------------
#$Date: 2025-08-19 21:17:10 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301807 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/13/2241358.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_2241358
loop_
_publ_author_name
'Pérez-Aguirre, Rubén'
'Pérez-Yáñez, Sonia'
'Beobide, Garikoitz'
'Castillo, Oscar'
'Gutiérrez-Zorrilla, Juan Manuel'
'Luque, Antonio'
_publ_section_title
;
 The crystal structure of a new polymorph of hexaaquanickel(II)
 bis(6-oxo-1,6-dihydropyridine-3-carboxylate)
;
_journal_coeditor_code           WM5241
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m238
_journal_page_last               m239
_journal_paper_doi               10.1107/S2056989015022422
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni (H2 O)6] (C6 H4 N O3)2'
_chemical_formula_moiety         'H12 Ni O6 2+, 2(C6 H4 N O3 -)'
_chemical_formula_sum            'C12 H20 N2 Ni O12'
_chemical_formula_weight         443.01
_chemical_name_systematic
;
Hexaaquanickel(II) bis(6-oxo-1,6-dihydropyridine-3-carboxylate)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                102.461(8)
_cell_angle_beta                 96.754(7)
_cell_angle_gamma                114.823(8)
_cell_formula_units_Z            1
_cell_length_a                   6.2620(5)
_cell_length_b                   7.1053(7)
_cell_length_c                   10.7101(10)
_cell_measurement_reflns_used    2781
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.239
_cell_measurement_theta_min      2.003
_cell_volume                     410.49(8)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare et al.,  1993)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'thin-slice ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2781
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.239
_diffrn_reflns_theta_min         2.003
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlisRED; Oxford Diffraction, 2003)
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             230
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.387
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0191P)²+0.3293P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                1654
_reflns_number_total             1801
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5241sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        410.49(7)
_cod_database_code               2241358
_cod_database_fobs_code          2241358
loop_
_space_group_symop_operation_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_occupancy
Ni Ni1 0.5000 0.0000 0.5000 0.01281(12) Uani d 1
O O1W 0.7185(3) 0.1609(3) 0.68193(15) 0.0168(3) Uani d 1
O O71 0.5271(3) -0.1565(3) 1.13681(15) 0.0202(4) Uani d 1
O O2W 0.3038(3) -0.2654(3) 0.56622(15) 0.0154(3) Uani d 1
O O3W 0.2933(3) 0.1461(3) 0.55076(17) 0.0231(4) Uani d 1
O O2 0.8636(3) -0.3362(3) 0.62046(14) 0.0176(3) Uani d 1
O O72 0.8231(3) -0.2245(3) 1.21937(15) 0.0202(4) Uani d 1
N N1 0.6616(3) -0.2558(3) 0.76999(18) 0.0162(4) Uani d 1
C C2 0.8355(4) -0.3128(4) 0.7379(2) 0.0141(4) Uani d 1
C C4 0.9331(4) -0.3021(3) 0.9661(2) 0.0140(4) Uani d 1
H H4 1.0278 -0.3170 1.0333 0.017 Uiso calc 1
C C3 0.9726(4) -0.3378(4) 0.8423(2) 0.0148(4) Uani d 1
H H3 1.0917 -0.3793 0.8264 0.018 Uiso calc 1
C C5 0.7512(4) -0.2432(3) 0.9937(2) 0.0130(4) Uani d 1
C C7 0.6965(4) -0.2048(3) 1.1271(2) 0.0144(4) Uani d 1
C C6 0.6196(4) -0.2203(4) 0.8921(2) 0.0154(4) Uani d 1
H H6 0.4995 -0.1797 0.9070 0.018 Uiso calc 1
H H1 0.574(4) -0.240(4) 0.708(3) 0.018 Uiso d 1
H H31W 0.266(5) 0.177(4) 0.615(3) 0.023 Uiso d 1
H H21W 0.262(5) -0.387(5) 0.505(3) 0.023 Uiso d 1
H H22W 0.189(5) -0.270(4) 0.588(3) 0.023 Uiso d 1
H H11W 0.650(5) 0.171(4) 0.736(3) 0.023 Uiso d 1
H H12W 0.844(5) 0.170(4) 0.712(3) 0.023 Uiso d 1
H H32W 0.236(5) 0.196(5) 0.503(3) 0.038(9) Uiso d 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
O1W Ni1 O1W . 2_656 180.0
O1W Ni1 O2W . . 89.95(6)
O1W Ni1 O2W . 2_656 90.05(6)
O1W Ni1 O3W . . 88.06(7)
O1W Ni1 O3W . 2_656 91.94(7)
O2W Ni1 O3W . . 92.99(7)
O2W Ni1 O3W . 2_656 87.01(7)
O1W Ni1 O3W 2_656 2_656 88.06(7)
O1W Ni1 O3W 2_656 . 91.94(7)
O3W Ni1 O3W 2_656 . 180.0
O1W Ni1 O2W 2_656 2_656 89.95(6)
O3W Ni1 O2W 2_656 2_656 92.99(7)
O1W Ni1 O2W 2_656 . 90.05(6)
O3W Ni1 O2W 2_656 . 87.01(7)
O2W Ni1 O2W 2_656 . 180.0
Ni1 O1W H11W . . 114(2)
Ni1 O1W H12W . . 130(2)
H11W O1W H12W . . 110(3)
Ni1 O2W H21W . . 110.1(17)
Ni1 O2W H22W . . 116(2)
H21W O2W H22W . . 108(3)
Ni1 O3W H31W . . 129(2)
Ni1 O3W H32W . . 124(2)
H31W O3W H32W . . 106(3)
C6 N1 C2 . . 124.28(18)
C6 N1 H1 . . 118.1(16)
C2 N1 H1 . . 117.6(16)
O2 C2 N1 . . 118.94(19)
O2 C2 C3 . . 125.81(19)
N1 C2 C3 . . 115.24(18)
C3 C4 C5 . . 121.08(19)
C3 C4 H4 . . 119.5
C5 C4 H4 . . 119.5
C4 C3 C2 . . 121.22(19)
C4 C3 H3 . . 119.4
C2 C3 H3 . . 119.4
C6 C5 C4 . . 117.18(19)
C6 C5 C7 . . 119.20(18)
C4 C5 C7 . . 123.62(18)
O71 C7 O72 . . 125.51(19)
O71 C7 C5 . . 116.72(18)
O72 C7 C5 . . 117.77(18)
N1 C6 C5 . . 120.98(19)
N1 C6 H6 . . 119.5
C5 C6 H6 . . 119.5
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 O1W . 2.0184(16) y
Ni1 O1W 2_656 2.0184(16) ?
Ni1 O3W 2_656 2.0242(16) ?
Ni1 O3W . 2.0242(16) y
Ni1 O2W 2_656 2.0990(16) ?
Ni1 O2W . 2.0990(16) y
O1W H11W . 0.77(3) ?
O1W H12W . 0.78(3) ?
O71 C7 . 1.253(2) ?
O2W H21W . 0.88(3) ?
O2W H22W . 0.77(3) ?
O3W H31W . 0.74(3) ?
O3W H32W . 0.81(3) ?
O2 C2 . 1.275(2) ?
O72 C7 . 1.262(3) ?
N1 C6 . 1.356(3) ?
N1 C2 . 1.366(3) ?
N1 H1 . 0.87(2) ?
C2 C3 . 1.417(3) ?
C4 C3 . 1.367(3) ?
C4 C5 . 1.409(3) ?
C4 H4 . 0.9300 ?
C3 H3 . 0.9300 ?
C5 C6 . 1.366(3) ?
C5 C7 . 1.503(3) ?
C6 H6 . 0.9300 ?
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
N1 H1 O2W . 0.87(2) 2.06(3) 2.906(2) 167(2)
O1W H11W O71 2_657 0.77(3) 1.85(3) 2.612(2) 173(3)
O1W H12W O72 2_757 0.78(3) 1.97(3) 2.748(2) 173(3)
O2W H21W O2 2_646 0.88(3) 1.90(3) 2.772(2) 173(2)
O2W H22W O2 1_455 0.77(3) 1.98(3) 2.743(2) 169(3)
O3W H31W O72 2_657 0.74(3) 1.92(3) 2.660(2) 174(3)
O3W H32W O2 2_656 0.81(3) 2.01(3) 2.813(2) 172(3)
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
C6 N1 C2 O2 -178.1(2)
C6 N1 C2 C3 1.1(3)
C5 C4 C3 C2 1.2(3)
O2 C2 C3 C4 177.9(2)
N1 C2 C3 C4 -1.2(3)
C3 C4 C5 C6 -1.0(3)
C3 C4 C5 C7 179.1(2)
C6 C5 C7 O71 1.2(3)
C4 C5 C7 O71 -178.9(2)
C6 C5 C7 O72 -179.1(2)
C4 C5 C7 O72 0.8(3)
C2 N1 C6 C5 -1.0(3)
C4 C5 C6 N1 0.8(3)
C7 C5 C6 N1 -179.3(2)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168326404
