#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/65/2236574.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_2236574
loop_
_publ_author_name
'Li, Jie'
'Lei, Ke-Wei'
'Xia, Dong-Guo'
_publ_section_title
;
 Poly[[hexaaqua(μ₃-2,2'-bipyridine-4,4',6,6'-tetracarboxylato-κ⁶O⁴:N,O⁶,O^6'^,N':O^4'^)dinickel(II)]
 dihydrate]
;
_journal_coeditor_code           RK2355
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1421
_journal_paper_doi               10.1107/S1600536812043942
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni2 (C14 H4 N2 O8) (H2 O)6], 2H2 O'
_chemical_formula_moiety         'C14 H16 N2 Ni2 O14, 2(H2 O)'
_chemical_formula_sum            'C14 H20 N2 Ni2 O16'
_chemical_formula_weight         589.70
_chemical_name_systematic
;
Poly[[hexaaqua(μ₃-2,2'-bipyridine-4,4',6,6'-tetracarboxylato-
κ⁶O⁴:N,O⁶,O^6'^,N':O^4'^)
dinickel(II)] dihydrate]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.1840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3588(8)
_cell_length_b                   11.8463(13)
_cell_length_c                   11.9942(13)
_cell_measurement_reflns_used    8794
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.7
_cell_volume                     1032.19(19)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scans'
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8794
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.422
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0230
_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)+(0.0255P)²+0.5729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                2248
_reflns_number_total             2365
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rk2355.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2236574
_cod_database_fobs_code          2236574
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
_atom_site_symmetry_multiplicity
Ni Ni1 0.2500 0.36726(2) 0.7500 0.01154(8) Uani d S 1 2
Ni Ni2 0.0000 1.0000 1.0000 0.01064(8) Uani d S 1 2
O O1 -0.10038(16) 0.87338(9) 0.89420(9) 0.0161(2) Uani d . 1 1
O O3 0.10695(15) 1.06255(9) 0.86383(9) 0.0145(2) Uani d . 1 1
H H3A 0.0846 1.1302 0.8571 0.022 Uiso calc R 1 1
O O2 -0.33996(15) 0.76758(9) 0.92552(9) 0.0162(2) Uani d . 1 1
O O4 0.23852(15) 0.90408(10) 1.03816(9) 0.0162(2) Uani d . 1 1
H H4A 0.3218 0.9436 1.0709 0.024 Uiso calc R 1 1
O O8 0.04444(15) 0.28697(9) 0.82901(9) 0.0152(2) Uani d . 1 1
C C1 0.1670(2) 0.60269(12) 0.77858(12) 0.0118(3) Uani d . 1 1
N N1 0.10800(18) 0.49784(10) 0.79747(10) 0.0110(2) Uani d . 1 1
C C6 -0.1837(2) 0.78123(12) 0.89848(11) 0.0112(3) Uani d . 1 1
C C4 -0.1418(2) 0.56825(12) 0.88022(11) 0.0112(3) Uani d . 1 1
H H4C -0.2463 0.5552 0.9130 0.013 Uiso calc R 1 1
C C2 0.0741(2) 0.69601(13) 0.81220(12) 0.0123(3) Uani d . 1 1
H H2A 0.1153 0.7688 0.8011 0.015 Uiso calc R 1 1
C C5 -0.0391(2) 0.47890(12) 0.84663(12) 0.0112(3) Uani d . 1 1
C C3 -0.0820(2) 0.67854(12) 0.86283(11) 0.0108(3) Uani d . 1 1
O O7 -0.21194(15) 0.32298(9) 0.90173(9) 0.0157(2) Uani d . 1 1
O O5 0.07941(17) 0.35897(11) 0.59723(10) 0.0201(2) Uani d . 1 1
H H5A 0.1245 0.3169 0.5548 0.030 Uiso calc R 1 1
C C7 -0.0751(2) 0.35285(12) 0.86043(12) 0.0120(3) Uani d . 1 1
O O6 0.02584(17) 0.96743(11) 0.64958(10) 0.0191(2) Uani d . 1 1
H H6A -0.015(3) 0.909(2) 0.6259(19) 0.031(6) Uiso d . 1 1
H H6B 0.114(4) 0.976(2) 0.621(2) 0.037(7) Uiso d . 1 1
H H5B -0.025(4) 0.352(2) 0.603(2) 0.043(7) Uiso d . 1 1
H H4B 0.240(4) 0.842(2) 1.059(2) 0.047(8) Uiso d . 1 1
H H3B 0.069(3) 1.031(2) 0.801(2) 0.035(6) Uiso d . 1 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
N1 Ni1 N1 2_556 . 78.65(7)
N1 Ni1 O5 2_556 . 93.20(5)
N1 Ni1 O5 . . 91.05(5)
N1 Ni1 O5 2_556 2_556 91.05(5)
N1 Ni1 O5 . 2_556 93.20(5)
O5 Ni1 O5 . 2_556 174.51(7)
N1 Ni1 O8 2_556 . 155.70(5)
N1 Ni1 O8 . . 77.21(5)
O5 Ni1 O8 . . 89.96(5)
O5 Ni1 O8 2_556 . 87.60(5)
N1 Ni1 O8 2_556 2_556 77.21(5)
N1 Ni1 O8 . 2_556 155.70(5)
O5 Ni1 O8 . 2_556 87.60(5)
O5 Ni1 O8 2_556 2_556 89.96(5)
O8 Ni1 O8 . 2_556 127.03(6)
O1 Ni2 O1 . 3_577 180.00(4)
O1 Ni2 O3 . 3_577 94.76(4)
O1 Ni2 O3 3_577 3_577 85.24(4)
O1 Ni2 O3 . . 85.24(4)
O1 Ni2 O3 3_577 . 94.76(4)
O3 Ni2 O3 3_577 . 180.0000(10)
O1 Ni2 O4 . 3_577 93.22(5)
O1 Ni2 O4 3_577 3_577 86.78(5)
O3 Ni2 O4 3_577 3_577 87.43(4)
O3 Ni2 O4 . 3_577 92.57(4)
O1 Ni2 O4 . . 86.78(5)
O1 Ni2 O4 3_577 . 93.22(5)
O3 Ni2 O4 3_577 . 92.57(4)
O3 Ni2 O4 . . 87.43(4)
O4 Ni2 O4 3_577 . 180.0
C6 O1 Ni2 . . 138.47(10)
Ni2 O3 H3A . . 109.5
Ni2 O3 H3B . . 115.5(17)
H3A O3 H3B . . 108.0
Ni2 O4 H4A . . 109.5
Ni2 O4 H4B . . 124(2)
H4A O4 H4B . . 114.4
C7 O8 Ni1 . . 115.42(9)
N1 C1 C2 . . 119.82(13)
N1 C1 C1 . 2_556 112.73(8)
C2 C1 C1 . 2_556 127.45(8)
C5 N1 C1 . . 122.43(12)
C5 N1 Ni1 . . 119.63(10)
C1 N1 Ni1 . . 117.94(10)
O2 C6 O1 . . 126.58(14)
O2 C6 C3 . . 118.75(13)
O1 C6 C3 . . 114.64(13)
C5 C4 C3 . . 117.70(13)
C5 C4 H4C . . 121.1
C3 C4 H4C . . 121.1
C1 C2 C3 . . 118.91(13)
C1 C2 H2A . . 120.5
C3 C2 H2A . . 120.5
N1 C5 C4 . . 121.05(13)
N1 C5 C7 . . 112.28(12)
C4 C5 C7 . . 126.67(13)
C2 C3 C4 . . 120.06(13)
C2 C3 C6 . . 118.55(13)
C4 C3 C6 . . 121.39(13)
Ni1 O5 H5A . . 109.5
Ni1 O5 H5B . . 113.3(19)
H5A O5 H5B . . 119.4
O7 C7 O8 . . 125.72(14)
O7 C7 C5 . . 119.10(13)
O8 C7 C5 . . 115.18(13)
H6A O6 H6B . . 105(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 N1 2_556 1.9996(12)
Ni1 N1 . 1.9996(12)
Ni1 O5 . 2.0516(12)
Ni1 O5 2_556 2.0516(12)
Ni1 O8 . 2.1327(11)
Ni1 O8 2_556 2.1327(11)
Ni2 O1 . 2.0265(11)
Ni2 O1 3_577 2.0265(11)
Ni2 O3 3_577 2.0607(10)
Ni2 O3 . 2.0607(10)
Ni2 O4 3_577 2.0796(11)
Ni2 O4 . 2.0796(11)
O1 C6 . 1.2570(18)
O3 H3A . 0.8200
O3 H3B . 0.85(2)
O2 C6 . 1.2541(18)
O4 H4A . 0.8200
O4 H4B . 0.78(3)
O8 C7 . 1.2769(18)
C1 N1 . 1.3468(18)
C1 C2 . 1.393(2)
C1 C1 2_556 1.493(3)
N1 C5 . 1.3317(19)
C6 C3 . 1.525(2)
C4 C5 . 1.397(2)
C4 C3 . 1.405(2)
C4 H4C . 0.9300
C2 C3 . 1.398(2)
C2 H2A . 0.9300
C5 C7 . 1.530(2)
O7 C7 . 1.2427(19)
O5 H5A . 0.8200
O5 H5B . 0.78(3)
O6 H6A . 0.79(3)
O6 H6B . 0.79(3)
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
O3 H3B O6 . 0.85(2) 1.95(2) 2.7821(16) 169(2)
O3 H3A O8 1_565 0.82 1.90 2.7189(16) 174.4
O4 H4A O6 4_676 0.82 1.95 2.7697(17) 177.8
O4 H4B O7 3_567 0.78(3) 2.03(3) 2.7997(16) 172(3)
O5 H5A O2 4_665 0.82 1.90 2.6891(16) 161.9
O5 H5B O7 2_456 0.78(3) 1.96(3) 2.7395(17) 172(3)
O6 H6A O2 2_456 0.79(3) 2.03(3) 2.8096(17) 170(2)
