#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/64/2216422.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_2216422
loop_
_publ_author_name
'Liang-Gui, Wang'
_publ_section_title
;
 Bis(2-pyridinecarboxylato
 N-oxide-κ²O,O')nickel(II)
;
_journal_coeditor_code           DN2274
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3168
_journal_page_last               m3168
_journal_paper_doi               10.1107/S1600536807059958
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (C6 H4 N O3)2]'
_chemical_formula_moiety         'C12 H8 N2 Ni O6'
_chemical_formula_sum            'C12 H8 N2 Ni O6'
_chemical_formula_weight         334.91
_chemical_name_common
;
Bis(2-pyridinecarboxylic acid N-oxide)nickel(II)
;
_chemical_name_systematic
;
Bis(N-oxido-2-pyridinecarboxylato-κ²O,O')nickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   3.3900(7)
_cell_length_b                   12.590(3)
_cell_length_c                   12.170(2)
_cell_measurement_reflns_used    915
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.33
_cell_volume                     518.04(19)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997)
and Mercury (Version 1.4; Macrae et al.,  2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3157
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         2.33
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.910
_exptl_absorpt_correction_T_max  0.7249
_exptl_absorpt_correction_T_min  0.6073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0295P)²+0.1009P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                839
_reflns_number_total             915
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2274.cif
_cod_data_source_block           I
_cod_original_cell_volume        518.04(18)
_cod_original_sg_symbol_H-M      'P  21/c'
_cod_database_code               2216422
_cod_database_fobs_code          2216422
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Ni Ni1 0.5000 0.5000 0.5000 0.02274(13) Uani d S 1
O O2 0.8684(4) 0.39064(10) 0.52462(10) 0.0332(3) Uani d . 1
O O3 0.4295(4) 0.46542(10) 0.34855(10) 0.0321(3) Uani d . 1
O O6 0.5595(4) 0.38865(11) 0.19304(10) 0.0363(3) Uani d . 1
N N2 0.8894(4) 0.30378(11) 0.46114(12) 0.0234(3) Uani d . 1
C C1 0.8087(5) 0.20531(14) 0.29725(15) 0.0303(4) Uani d . 1
H H1 0.7196 0.2011 0.2233 0.036 Uiso calc R 1
C C2 0.9798(6) 0.11894(15) 0.34717(18) 0.0354(5) Uani d . 1
H H2 1.0072 0.0558 0.3089 0.042 Uiso calc R 1
C C3 1.1109(5) 0.12780(14) 0.45565(17) 0.0334(4) Uani d . 1
H H3 1.2339 0.0703 0.4918 0.040 Uiso calc R 1
C C4 1.0625(5) 0.22033(15) 0.51132(14) 0.0276(4) Uani d . 1
H H4 1.1517 0.2252 0.5853 0.033 Uiso calc R 1
C C5 0.7630(5) 0.29947(13) 0.35319(14) 0.0239(4) Uani d . 1
C C6 0.5738(5) 0.39276(13) 0.29371(14) 0.0253(4) Uani d . 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni1 0.0274(2) 0.02038(19) 0.01969(18) 0.00616(11) -0.00324(13) -0.00257(11)
O2 0.0392(8) 0.0295(7) 0.0294(7) 0.0109(6) -0.0084(5) -0.0096(5)
O3 0.0357(7) 0.0339(7) 0.0258(6) 0.0108(6) -0.0044(5) -0.0034(6)
O6 0.0428(8) 0.0429(8) 0.0226(7) 0.0039(6) -0.0008(6) -0.0025(6)
N2 0.0215(7) 0.0223(8) 0.0267(7) -0.0003(6) 0.0029(6) -0.0027(6)
C1 0.0239(9) 0.0338(10) 0.0335(9) -0.0038(7) 0.0033(7) -0.0066(8)
C2 0.0279(10) 0.0267(10) 0.0523(12) -0.0003(7) 0.0074(9) -0.0095(9)
C3 0.0250(10) 0.0256(10) 0.0499(12) 0.0011(7) 0.0050(9) 0.0036(8)
C4 0.0231(9) 0.0286(10) 0.0310(9) 0.0024(7) 0.0012(7) 0.0051(7)
C5 0.0198(9) 0.0263(9) 0.0258(8) -0.0045(7) 0.0027(7) -0.0014(7)
C6 0.0231(9) 0.0265(9) 0.0259(9) -0.0042(7) -0.0009(7) -0.0030(7)
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
O2 Ni1 O2 . 3_666 180.0000(10)
O2 Ni1 O3 . . 91.27(6)
O2 Ni1 O3 3_666 . 88.73(6)
O2 Ni1 O3 . 3_666 88.73(6)
O2 Ni1 O3 3_666 3_666 91.27(6)
O3 Ni1 O3 . 3_666 180.0000(10)
N2 O2 Ni1 . . 124.77(10)
C6 O3 Ni1 . . 131.34(12)
C4 N2 O2 . . 114.77(14)
C4 N2 C5 . . 120.80(15)
O2 N2 C5 . . 124.38(14)
C2 C1 C5 . . 121.83(18)
C2 C1 H1 . . 119.1
C5 C1 H1 . . 119.1
C1 C2 C3 . . 117.77(18)
C1 C2 H2 . . 121.1
C3 C2 H2 . . 121.1
C4 C3 C2 . . 120.49(17)
C4 C3 H3 . . 119.8
C2 C3 H3 . . 119.8
N2 C4 C3 . . 120.78(16)
N2 C4 H4 . . 119.6
C3 C4 H4 . . 119.6
N2 C5 C1 . . 118.30(16)
N2 C5 C6 . . 122.10(14)
C1 C5 C6 . . 119.59(16)
O6 C6 O3 . . 125.15(17)
O6 C6 C5 . . 115.76(15)
O3 C6 C5 . . 119.01(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 O2 . 1.8684(13)
Ni1 O2 3_666 1.8684(13)
Ni1 O3 . 1.8920(13)
Ni1 O3 3_666 1.8920(13)
O2 N2 . 1.3437(18)
O3 C6 . 1.253(2)
O6 C6 . 1.224(2)
N2 C4 . 1.330(2)
N2 C5 . 1.353(2)
C1 C2 . 1.355(3)
C1 C5 . 1.381(2)
C1 H1 . 0.9300
C2 C3 . 1.367(3)
C2 H2 . 0.9300
C3 C4 . 1.364(3)
C3 H3 . 0.9300
C4 H4 . 0.9300
C5 C6 . 1.499(2)
