#------------------------------------------------------------------------------
#$Date: 2018-09-26 06:29:44 +0300 (Wed, 26 Sep 2018) $
#$Revision: 211175 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/22/8102285.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_8102285
loop_
_publ_author_name
'Chun-Sheng Zhou'
'Guo-Chun Zhang'
_publ_contact_author
;
  C. S. Zhou   
;
_publ_section_title
;
 Crystal structure of poly-aqua[(pyridine-2,6-dicarboxylic acid
 N-oxide) (4,4'-bipyridine)nickel(II) dihydrate,
 (Ni(C7H3NO5)(C10N2H8)0.5(H2O)) · 2H2O
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              175
_journal_volume                  223
_journal_year                    2008
_chemical_formula_moiety         'C12 H13 N2 Ni O8'
_chemical_formula_sum            'C12 H13 N2 Ni O8'
_chemical_formula_weight         371.95
_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                109.295(2)
_cell_angle_beta                 107.267(2)
_cell_angle_gamma                104.026(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5793(10)
_cell_length_b                   10.4791(13)
_cell_length_c                   11.0258(14)
_cell_measurement_reflns_used    2550
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.15
_cell_volume                     730.80(16)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3739
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.8592
_exptl_absorpt_correction_T_min  0.6271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0097(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2550
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0502P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                2250
_reflns_number_total             2550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2267.cff
_cod_data_source_block
;
;
_cod_database_code               8102285
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.35767(4) 0.12744(3) 0.25001(3) 0.02624(12) Uani 1 1 d . . .
N1 N 0.0701(2) 0.25882(18) 0.20545(18) 0.0286(4) Uani 1 1 d . . .
N2 N 0.5996(3) 0.09354(19) 0.34366(18) 0.0315(4) Uani 1 1 d . . .
O1 O 0.3842(2) 0.25930(18) 0.43273(16) 0.0420(4) Uani 1 1 d . . .
O2 O 0.3081(3) 0.4154(2) 0.57803(17) 0.0537(5) Uani 1 1 d . . .
O3 O 0.0960(2) 0.13254(16) 0.16824(15) 0.0358(4) Uani 1 1 d . . .
O4 O -0.2846(2) 0.03788(16) -0.06935(15) 0.0357(4) Uani 1 1 d . . .
O5 O -0.0767(3) 0.16668(19) -0.13056(17) 0.0483(4) Uani 1 1 d . . .
O6 O 0.5235(3) 0.2967(2) 0.2041(2) 0.0577(5) Uani 1 1 d D . .
O7 O 0.4732(4) 0.6361(3) 0.1894(3) 0.0919(8) Uani 1 1 d D . .
O8 O 0.6833(4) 0.6549(3) 0.0209(3) 0.0823(7) Uani 1 1 d D . .
C1 C 0.2931(3) 0.3435(2) 0.4592(2) 0.0355(5) Uani 1 1 d . . .
C2 C 0.1574(3) 0.3641(2) 0.3408(2) 0.0312(5) Uani 1 1 d . . .
C3 C 0.1189(4) 0.4906(2) 0.3686(2) 0.0410(6) Uani 1 1 d . . .
H3 H 0.1757 0.5632 0.4606 0.049 Uiso 1 1 calc R . .
C4 C -0.0032(4) 0.5104(3) 0.2613(3) 0.0471(6) Uani 1 1 d . . .
H4 H -0.0260 0.5968 0.2803 0.057 Uiso 1 1 calc R . .
C5 C -0.0904(4) 0.4015(2) 0.1264(2) 0.0411(6) Uani 1 1 d . . .
H5 H -0.1735 0.4136 0.0535 0.049 Uiso 1 1 calc R . .
C6 C -0.0551(3) 0.2742(2) 0.0988(2) 0.0309(5) Uani 1 1 d . . .
C7 C -0.1447(3) 0.1487(2) -0.0462(2) 0.0321(5) Uani 1 1 d . . .
C8 C 0.6617(3) 0.1147(2) 0.4785(2) 0.0356(5) Uani 1 1 d . . .
H8 H 0.5972 0.1550 0.5315 0.043 Uiso 1 1 calc R . .
C9 C 0.8159(3) 0.0796(2) 0.5420(2) 0.0363(5) Uani 1 1 d . . .
H9 H 0.8526 0.0955 0.6357 0.044 Uiso 1 1 calc R . .
C10 C 0.9171(3) 0.0206(2) 0.4672(2) 0.0292(5) Uani 1 1 d . . .
C11 C 0.8572(3) 0.0039(3) 0.3287(2) 0.0377(5) Uani 1 1 d . . .
H11 H 0.9235 -0.0316 0.2749 0.045 Uiso 1 1 calc R . .
C12 C 0.7002(3) 0.0400(3) 0.2717(2) 0.0376(5) Uani 1 1 d . . .
H12 H 0.6618 0.0267 0.1787 0.045 Uiso 1 1 calc R . .
H6A H 0.583(5) 0.3823(17) 0.271(2) 0.080 Uiso 1 1 d D . .
H6B H 0.465(4) 0.297(4) 0.1244(19) 0.080 Uiso 1 1 d D . .
H7A H 0.545(4) 0.646(4) 0.2697(18) 0.080 Uiso 1 1 d D . .
H7B H 0.421(5) 0.5456(14) 0.137(3) 0.080 Uiso 1 1 d D . .
H8A H 0.802(2) 0.715(3) 0.063(3) 0.080 Uiso 1 1 d D . .
H8B H 0.627(5) 0.674(4) 0.077(3) 0.080 Uiso 1 1 d D . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ni1 O1 87.93(6) . . ?
O3 Ni1 O4 87.39(6) . 2 ?
O1 Ni1 O4 166.97(7) . 2 ?
O3 Ni1 N2 168.96(7) . . ?
O1 Ni1 N2 90.47(7) . . ?
O4 Ni1 N2 91.80(7) 2 . ?
O3 Ni1 O6 97.09(7) . . ?
O1 Ni1 O6 96.61(8) . . ?
O4 Ni1 O6 96.03(7) 2 . ?
N2 Ni1 O6 93.94(8) . . ?
O3 N1 C2 123.00(17) . . ?
O3 N1 C6 115.16(16) . . ?
C2 N1 C6 121.82(17) . . ?
C12 N2 C8 116.89(18) . . ?
C12 N2 Ni1 121.27(14) . . ?
C8 N2 Ni1 121.72(15) . . ?
C1 O1 Ni1 128.63(15) . . ?
N1 O3 Ni1 120.31(12) . . ?
C7 O4 Ni1 111.97(14) . 2 ?
Ni1 O6 H6A 116(2) . . ?
Ni1 O6 H6B 117(2) . . ?
H6A O6 H6B 112(3) . . ?
H7A O7 H7B 106(3) . . ?
H8A O8 H8B 108(3) . . ?
O2 C1 O1 124.3(2) . . ?
O2 C1 C2 115.62(19) . . ?
O1 C1 C2 120.07(19) . . ?
N1 C2 C3 118.5(2) . . ?
N1 C2 C1 121.11(18) . . ?
C3 C2 C1 120.40(19) . . ?
C2 C3 C4 120.7(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.3(2) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.1(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
N1 C6 C5 119.6(2) . . ?
N1 C6 C7 116.71(17) . . ?
C5 C6 C7 123.70(19) . . ?
O5 C7 O4 126.8(2) . . ?
O5 C7 C6 116.7(2) . . ?
O4 C7 C6 116.50(19) . . ?
N2 C8 C9 123.1(2) . . ?
N2 C8 H8 118.4 . . ?
C9 C8 H8 118.4 . . ?
C8 C9 C10 120.3(2) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 116.47(19) . . ?
C9 C10 C10 121.4(2) . 2_756 ?
C11 C10 C10 122.1(2) . 2_756 ?
C12 C11 C10 120.0(2) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
N2 C12 C11 123.2(2) . . ?
N2 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O3 1.9419(14) . ?
Ni1 O1 1.9478(15) . ?
Ni1 O4 1.9686(15) 2 ?
Ni1 N2 1.9969(17) . ?
Ni1 O6 2.2081(18) . ?
N1 O3 1.332(2) . ?
N1 C2 1.361(3) . ?
N1 C6 1.359(3) . ?
N2 C12 1.341(3) . ?
N2 C8 1.341(3) . ?
O1 C1 1.259(3) . ?
O2 C1 1.231(3) . ?
O4 C7 1.259(3) . ?
O4 Ni1 1.9686(15) 2 ?
O5 C7 1.233(3) . ?
O6 H6A 0.848(10) . ?
O6 H6B 0.859(10) . ?
O7 H7A 0.845(10) . ?
O7 H7B 0.842(10) . ?
O8 H8A 0.839(10) . ?
O8 H8B 0.847(10) . ?
C1 C2 1.518(3) . ?
C2 C3 1.381(3) . ?
C3 C4 1.380(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.510(3) . ?
C8 C9 1.373(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.394(3) . ?
C10 C10 1.489(4) 2_756 ?
C11 C12 1.373(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
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
O3 Ni1 N2 C12 117.5(3) . . . . ?
O1 Ni1 N2 C12 -160.93(18) . . . . ?
O4 Ni1 N2 C12 31.90(18) 2 . . . ?
O6 Ni1 N2 C12 -64.27(18) . . . . ?
O3 Ni1 N2 C8 -58.4(4) . . . . ?
O1 Ni1 N2 C8 23.18(18) . . . . ?
O4 Ni1 N2 C8 -143.99(18) 2 . . . ?
O6 Ni1 N2 C8 119.84(18) . . . . ?
O3 Ni1 O1 C1 -21.5(2) . . . . ?
O4 Ni1 O1 C1 -90.5(3) 2 . . . ?
N2 Ni1 O1 C1 169.5(2) . . . . ?
O6 Ni1 O1 C1 75.4(2) . . . . ?
C2 N1 O3 Ni1 -41.0(2) . . . . ?
C6 N1 O3 Ni1 140.78(15) . . . . ?
O1 Ni1 O3 N1 44.55(15) . . . . ?
O4 Ni1 O3 N1 -147.61(15) 2 . . . ?
N2 Ni1 O3 N1 126.4(3) . . . . ?
O6 Ni1 O3 N1 -51.86(15) . . . . ?
Ni1 O1 C1 O2 174.22(18) . . . . ?
Ni1 O1 C1 C2 -7.1(3) . . . . ?
O3 N1 C2 C3 -179.19(19) . . . . ?
C6 N1 C2 C3 -1.0(3) . . . . ?
O3 N1 C2 C1 0.4(3) . . . . ?
C6 N1 C2 C1 178.56(19) . . . . ?
O2 C1 C2 N1 -155.7(2) . . . . ?
O1 C1 C2 N1 25.5(3) . . . . ?
O2 C1 C2 C3 23.9(3) . . . . ?
O1 C1 C2 C3 -154.9(2) . . . . ?
N1 C2 C3 C4 -0.9(4) . . . . ?
C1 C2 C3 C4 179.5(2) . . . . ?
C2 C3 C4 C5 1.6(4) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
O3 N1 C6 C5 -179.5(2) . . . . ?
C2 N1 C6 C5 2.2(3) . . . . ?
O3 N1 C6 C7 -0.8(3) . . . . ?
C2 N1 C6 C7 -179.12(18) . . . . ?
C4 C5 C6 N1 -1.5(4) . . . . ?
C4 C5 C6 C7 180.0(2) . . . . ?
Ni1 O4 C7 O5 11.0(3) 2 . . . ?
Ni1 O4 C7 C6 -170.93(13) 2 . . . ?
N1 C6 C7 O5 -105.6(2) . . . . ?
C5 C6 C7 O5 72.9(3) . . . . ?
N1 C6 C7 O4 76.1(2) . . . . ?
C5 C6 C7 O4 -105.3(3) . . . . ?
C12 N2 C8 C9 -2.3(3) . . . . ?
Ni1 N2 C8 C9 173.78(17) . . . . ?
N2 C8 C9 C10 0.6(4) . . . . ?
C8 C9 C10 C11 1.8(3) . . . . ?
C8 C9 C10 C10 -179.0(2) . . . 2_756 ?
C9 C10 C11 C12 -2.5(3) . . . . ?
C10 C10 C11 C12 178.4(2) 2_756 . . . ?
C8 N2 C12 C11 1.5(3) . . . . ?
Ni1 N2 C12 C11 -174.55(18) . . . . ?
C10 C11 C12 N2 0.9(4) . . . . ?
