#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/98/2219823.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_2219823
loop_
_publ_author_name
'Yang, Ming-Hua'
_publ_section_title
;
 catena-Poly[[[bis[aquanickel(II)]bis(μ-pyridine-2,6-dicarboxylato
 N-oxide)]-μ-1,2-di-4-pyridylethane] tetrahydrate]
;
_journal_coeditor_code           CV2458
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1358
_journal_paper_doi               10.1107/S1600536808031619
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac
'[Ni2 (C7 H3 N O5)2 (C12 H12 N2) (H2 O)2], 4H2 O'
_chemical_formula_moiety         'C26 H22 N4 Ni2 O12, 4(H2 O)'
_chemical_formula_sum            'C26 H30 N4 Ni2 O16'
_chemical_formula_weight         771.96
_chemical_name_systematic
;
catena-Poly[[[bis[aquanickel(II)]bis(μ-pyridine-2,6-dicarboxylato
N-oxide)]-μ-1,2-di-4-pyridylethane] tetrahydrate]
;
_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                113.727(2)
_cell_angle_beta                 104.282(2)
_cell_angle_gamma                100.255(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2803(16)
_cell_length_b                   10.3542(15)
_cell_length_c                   11.1326(16)
_cell_measurement_reflns_used    2850
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.14
_cell_volume                     804.4(2)
_computing_cell_refinement       'APEX2 (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'APEX2 (Bruker, 2004)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia,
1997) and
PLATON (Spek, 2003)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and 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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4146
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.14
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  0.8250
_exptl_absorpt_correction_T_min  0.7452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0281
_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)+(0.0269P)²+0.19P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                2180
_reflns_number_total             2850
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2458.cif
_cod_data_source_block           I
_cod_database_code               2219823
_cod_database_fobs_code          2219823
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
Ni Ni1 0.19610(4) 0.10188(3) 0.85792(3) 0.03124(11) Uani d . 1
O O1 0.0912(2) 0.1451(2) 0.70832(19) 0.0473(5) Uani d . 1
O O2 -0.1257(2) 0.1548(2) 0.5550(2) 0.0600(6) Uani d . 1
O O3 -0.03449(19) 0.0177(2) 0.85274(17) 0.0433(4) Uani d . 1
N N1 0.4335(2) 0.2138(2) 0.8837(2) 0.0376(5) Uani d . 1
N N2 -0.1753(2) -0.0555(2) 0.7358(2) 0.0354(5) Uani d . 1
C C1 -0.0673(3) 0.1028(3) 0.6318(3) 0.0401(6) Uani d . 1
C C2 -0.2011(3) -0.0227(3) 0.6272(3) 0.0368(6) Uani d . 1
C C3 -0.3544(3) -0.1043(3) 0.5128(3) 0.0489(7) Uani d . 1
H H3 -0.3736 -0.0847 0.4369 0.059 Uiso calc R 1
C C4 -0.4795(4) -0.2144(3) 0.5092(3) 0.0570(8) Uani d . 1
H H4 -0.5824 -0.2686 0.4315 0.068 Uiso calc R 1
C C5 -0.4508(3) -0.2433(3) 0.6215(3) 0.0492(7) Uani d . 1
H H5 -0.5343 -0.3172 0.6205 0.059 Uiso calc R 1
C C6 -0.2980(3) -0.1624(3) 0.7350(3) 0.0366(6) Uani d . 1
C C8 0.5711(3) 0.1727(3) 0.9306(3) 0.0490(7) Uani d . 1
H H8 0.5514 0.0953 0.9529 0.059 Uiso calc R 1
C C9 0.7394(3) 0.2397(3) 0.9470(3) 0.0507(7) Uani d . 1
H H9 0.8307 0.2077 0.9798 0.061 Uiso calc R 1
C C10 0.7726(3) 0.3553(3) 0.9144(3) 0.0436(6) Uani d . 1
C C11 0.9551(3) 0.4316(3) 0.9304(3) 0.0518(7) Uani d . 1
H H11A 1.0234 0.3635 0.9215 0.062 Uiso calc R 1
H H11B 0.9488 0.4587 0.8559 0.062 Uiso calc R 1
C C12 0.6307(3) 0.3995(3) 0.8690(3) 0.0479(7) Uani d . 1
H H12 0.6474 0.4782 0.8482 0.058 Uiso calc R 1
C C13 0.46548(10) 0.32671(9) 0.85477(8) 0.0442(7) Uani d . 1
H H13 0.3722 0.3577 0.8236 0.053 Uiso calc R 1
O O1W 0.22201(10) -0.11885(9) 0.72089(8) 0.0584(5) Uani d . 1
H H1W 0.1610 -0.1939 0.7212 0.088 Uiso d R 1
H H2W 0.2045 -0.1367 0.6357 0.088 Uiso d R 1
O O2W 0.15515(10) 0.41900(9) 0.61420(8) 0.0944(8) Uani d . 1
H H3W 0.0828 0.3364 0.5887 0.142 Uiso d R 1
H H4W 0.1122 0.489 0.6354 0.142 Uiso d R 1
O O3W 0.03080(10) 0.37588(9) 0.33371(8) 0.0875(7) Uani d . 1
H H6W 0.0820 0.3592 0.2741 0.131 Uiso d R 1
H H5W 0.1116 0.4510 0.4044 0.131 Uiso d R 1
C C7 -0.25478(10) -0.18425(9) 0.86469(8) 0.0374(6) Uani d . 1
O O4 -0.28538(10) -0.09359(9) 0.96606(8) 0.0401(4) Uani d . 1
O O5 -0.19822(10) -0.28825(9) 0.85957(8) 0.0540(5) Uani 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'
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
O3 Ni1 O1 . . 89.83(7)
O3 Ni1 O4 . 2_557 86.14(5)
O1 Ni1 O4 . 2_557 167.38(6)
O3 Ni1 N1 . . 172.23(8)
O1 Ni1 N1 . . 90.76(7)
O4 Ni1 N1 2_557 . 91.65(6)
O3 Ni1 O1W . . 94.95(6)
O1 Ni1 O1W . . 97.00(6)
O4 Ni1 O1W 2_557 . 95.30(6)
N1 Ni1 O1W . . 92.67(6)
C1 O1 Ni1 . . 129.11(16)
N2 O3 Ni1 . . 123.58(13)
C13 N1 C8 . . 117.39(17)
C13 N1 Ni1 . . 123.82(12)
C8 N1 Ni1 . . 118.78(15)
O3 N2 C6 . . 114.80(18)
O3 N2 C2 . . 123.49(19)
C6 N2 C2 . . 121.6(2)
O2 C1 O1 . . 124.3(2)
O2 C1 C2 . . 115.3(2)
O1 C1 C2 . . 120.5(2)
N2 C2 C3 . . 118.2(2)
N2 C2 C1 . . 121.5(2)
C3 C2 C1 . . 120.3(2)
C4 C3 C2 . . 121.1(2)
C4 C3 H3 . . 119.5
C2 C3 H3 . . 119.5
C5 C4 C3 . . 119.4(3)
C5 C4 H4 . . 120.3
C3 C4 H4 . . 120.3
C6 C5 C4 . . 119.5(2)
C6 C5 H5 . . 120.3
C4 C5 H5 . . 120.3
N2 C6 C5 . . 120.3(2)
N2 C6 C7 . . 116.2(2)
C5 C6 C7 . . 123.6(3)
N1 C8 C9 . . 123.1(2)
N1 C8 H8 . . 118.5
C9 C8 H8 . . 118.5
C8 C9 C10 . . 119.7(2)
C8 C9 H9 . . 120.2
C10 C9 H9 . . 120.2
C9 C10 C12 . . 117.0(2)
C9 C10 C11 . . 121.5(2)
C12 C10 C11 . . 121.5(2)
C11 C11 C10 2_767 . 111.5(3)
C11 C11 H11A 2_767 . 109.3
C10 C11 H11A . . 109.3
C11 C11 H11B 2_767 . 109.3
C10 C11 H11B . . 109.3
H11A C11 H11B . . 108.0
C13 C12 C10 . . 120.0(2)
C13 C12 H12 . . 120.0
C10 C12 H12 . . 120.0
N1 C13 C12 . . 122.78(15)
N1 C13 H13 . . 118.6
C12 C13 H13 . . 118.6
Ni1 O1W H1W . . 115.3
Ni1 O1W H2W . . 114.2
H1W O1W H2W . . 108.3
H3W O2W H4W . . 113.1
H6W O3W H5W . . 99.6
O5 C7 O4 . . 127.30(10)
O5 C7 C6 . . 117.9(2)
O4 C7 C6 . . 114.9(2)
C7 O4 Ni1 . 2_557 114.70(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 O3 . 1.9290(16)
Ni1 O1 . 1.9373(16)
Ni1 O4 2_557 1.9588(10)
Ni1 N1 . 1.9828(18)
Ni1 O1W . 2.2643(11)
O1 C1 . 1.258(3)
O2 C1 . 1.230(3)
O3 N2 . 1.331(2)
N1 C13 . 1.3332(19)
N1 C8 . 1.345(3)
N2 C6 . 1.358(3)
N2 C2 . 1.361(3)
C1 C2 . 1.525(3)
C2 C3 . 1.379(3)
C3 C4 . 1.377(4)
C3 H3 . 0.9300
C4 C5 . 1.375(3)
C4 H4 . 0.9300
C5 C6 . 1.371(3)
C5 H5 . 0.9300
C6 C7 . 1.517(3)
C8 C9 . 1.373(3)
C8 H8 . 0.9300
C9 C10 . 1.386(3)
C9 H9 . 0.9300
C10 C12 . 1.390(3)
C10 C11 . 1.506(3)
C11 C11 2_767 1.501(5)
C11 H11A . 0.9700
C11 H11B . 0.9700
C12 C13 . 1.376(3)
C12 H12 . 0.9300
C13 H13 . 0.9300
O1W H1W . 0.85
O1W H2W . 0.86
O2W H3W . 0.84
O2W H4W . 0.84
O3W H6W . 0.85
O3W H5W . 0.86
C7 O5 . 1.2351(14)
C7 O4 . 1.2618(12)
O4 Ni1 2_557 1.9588(10)
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
O1W H1W O3W 2_556 0.85 1.99 2.8144(15) 162.0
O1W H2W O2 2_556 0.86 1.98 2.824(2) 167.5
O3W H6W O5 2_556 0.85 1.94 2.7791(13) 169.6
O3W H5W O2W . 0.86 2.44 2.8527(13) 110.4
O2W H3W O2 . 0.84 2.15 2.976(2) 167.4
O2W H4W O3W 2_566 0.84 1.97 2.7985(14) 169.0
