#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/74/2217408.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_2217408
loop_
_publ_author_name
'Zhang, Xiao'
'Yi, ZhiHui'
'Xia, Wujiong'
'Yang, Chao'
'Li, Bing'
_publ_section_title
;
 Poly[[diaqua-μ₂-4,4'-bipyridyl-μ₂-o-phthalato-nickel(II)]
 dihydrate]
;
_journal_coeditor_code           BG2157
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m345
_journal_page_last               m346
_journal_paper_doi               10.1107/S1600536807064562
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C8 H4 O4) (C10 H8 N2) (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C18 H16 N2 Ni O6, 2(H2 O)'
_chemical_formula_sum            'C18 H20 N2 Ni O8'
_chemical_formula_weight         451.07
_chemical_name_systematic
;
Poly[[diaqua-μ₂-4,4'-bipyridyl-μ₂-o-phthalato-nickel(II)] dihydrate]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 123.63(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6160(15)
_cell_length_b                   11.372(2)
_cell_length_c                   12.954(4)
_cell_measurement_reflns_used    8171
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.21
_cell_volume                     934.2(4)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        RAPID-AUTO
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10
_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
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8992
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2142
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0548P)²+0.4267P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                1968
_reflns_number_total             2142
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bg2157.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2217408
_cod_database_fobs_code          2217408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -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
Ni Ni1 0.0000 0.72030(2) 0.2500 0.01769(12) Uani d S 1
O O1 0.3358(2) 0.70882(11) 0.37051(13) 0.0245(3) Uani d . 1
O O2 0.6416(2) 0.65853(13) 0.39977(15) 0.0373(4) Uani d . 1
N N1 0.0000 -0.09196(17) 0.2500 0.0177(4) Uani d S 1
N N2 0.0000 0.53103(17) 0.2500 0.0207(4) Uani d S 1
C C1 -0.0330(3) -0.03021(15) 0.15229(16) 0.0223(4) Uani d . 1
H H1 -0.0574 -0.0713 0.0834 0.027 Uiso calc R 1
C C2 -0.0327(3) 0.09169(15) 0.14895(16) 0.0228(4) Uani d . 1
H H2 -0.0542 0.1307 0.0797 0.027 Uiso calc R 1
C C3 0.0000 0.1551(2) 0.2500 0.0191(5) Uani d S 1
C C4 0.0000 0.28534(19) 0.2500 0.0197(5) Uani d S 1
C C5 0.1289(3) 0.34832(15) 0.22487(18) 0.0244(4) Uani d . 1
H H5 0.2156 0.3093 0.2064 0.029 Uiso calc R 1
C C6 0.1261(3) 0.47013(15) 0.22773(19) 0.0244(4) Uani d . 1
H H6 0.2161 0.5115 0.2135 0.029 Uiso calc R 1
C C7 0.4933(2) 0.84072(14) 0.30166(14) 0.0160(3) Uani d . 1
C C8 0.4914(3) 0.94753(17) 0.35359(18) 0.0259(4) Uani d . 1
H H8 0.4854 0.9479 0.4234 0.031 Uiso calc R 1
C C9 0.4982(3) 1.05329(17) 0.3028(2) 0.0340(5) Uani d . 1
H H9 0.5003 1.1240 0.3396 0.041 Uiso calc R 1
C C10 0.4895(3) 0.72697(14) 0.36067(16) 0.0190(3) Uani d . 1
O O1W 0.0029(2) 0.71811(10) 0.08697(12) 0.0216(3) Uani d D 1
O O2W 0.3483(3) 0.58768(15) 0.56342(15) 0.0392(4) Uani d D 1
H H2WA 0.385(5) 0.608(2) 0.516(2) 0.059 Uiso d D 1
H H1WA -0.091(3) 0.673(2) 0.034(2) 0.048(8) Uiso d D 1
H H1WB 0.113(2) 0.705(2) 0.090(2) 0.032(6) Uiso d D 1
H H2WB 0.362(5) 0.5147(9) 0.571(3) 0.060(10) Uiso d 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'
Ni Ni 0.3393 1.1124 '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
O1W Ni1 O1W . 2 178.66(6)
O1W Ni1 N1 . 1_565 90.67(3)
O1W Ni1 N1 2 1_565 90.67(3)
O1W Ni1 O1 . . 93.34(6)
O1W Ni1 O1 2 . 86.58(6)
N1 Ni1 O1 1_565 . 93.50(4)
O1W Ni1 O1 . 2 86.58(6)
O1W Ni1 O1 2 2 93.34(6)
N1 Ni1 O1 1_565 2 93.50(4)
O1 Ni1 O1 . 2 173.00(7)
O1W Ni1 N2 . . 89.33(3)
O1W Ni1 N2 2 . 89.33(3)
N1 Ni1 N2 1_565 . 180.0
O1 Ni1 N2 . . 86.50(4)
O1 Ni1 N2 2 . 86.50(4)
C10 O1 Ni1 . . 135.82(12)
C1 N1 C1 . 2 117.0(2)
C1 N1 Ni1 . 1_545 121.51(10)
C1 N1 Ni1 2 1_545 121.51(10)
C6 N2 C6 . 2 117.7(2)
C6 N2 Ni1 . . 121.15(10)
C6 N2 Ni1 2 . 121.15(10)
N1 C1 C2 . . 123.31(16)
N1 C1 H1 . . 118.3
C2 C1 H1 . . 118.3
C1 C2 C3 . . 119.41(16)
C1 C2 H2 . . 120.3
C3 C2 H2 . . 120.3
C2 C3 C2 . 2 117.6(2)
C2 C3 C4 . . 121.22(11)
C2 C3 C4 2 . 121.22(11)
C5 C4 C5 . 2 118.0(2)
C5 C4 C3 . . 120.98(10)
C5 C4 C3 2 . 120.98(11)
C6 C5 C4 . . 119.00(17)
C6 C5 H5 . . 120.5
C4 C5 H5 . . 120.5
N2 C6 C5 . . 123.11(17)
N2 C6 H6 . . 118.4
C5 C6 H6 . . 118.4
C8 C7 C7 . 2_655 119.25(11)
C8 C7 C10 . . 119.60(16)
C7 C7 C10 2_655 . 121.10(9)
C9 C8 C7 . . 120.97(19)
C9 C8 H8 . . 119.5
C7 C8 H8 . . 119.5
C9 C9 C8 2_655 . 119.73(12)
C9 C9 H9 2_655 . 120.1
C8 C9 H9 . . 120.1
O2 C10 O1 . . 124.17(16)
O2 C10 C7 . . 117.79(15)
O1 C10 C7 . . 118.01(15)
Ni1 O1W H1WA . . 109.8(19)
Ni1 O1W H1WB . . 121.7(17)
H1WA O1W H1WB . . 108.2(19)
H2WA O2W H2WB . . 106(2)
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 . 2.1244(14) y
Ni1 O1W 2 2.1244(14) ?
Ni1 N1 1_565 2.135(2) y
Ni1 O1 . 2.1383(15) y
Ni1 O1 2 2.1383(15) ?
Ni1 N2 . 2.152(2) y
O1 C10 . 1.263(2) ?
O2 C10 . 1.247(2) ?
N1 C1 . 1.344(2) ?
N1 C1 2 1.344(2) ?
N1 Ni1 1_545 2.135(2) ?
N2 C6 . 1.339(2) ?
N2 C6 2 1.339(2) ?
C1 C2 . 1.387(2) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.391(2) ?
C2 H2 . 0.9300 ?
C3 C2 2 1.391(2) ?
C3 C4 . 1.481(3) ?
C4 C5 . 1.392(2) ?
C4 C5 2 1.392(2) ?
C5 C6 . 1.386(2) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.393(2) ?
C7 C7 2_655 1.397(3) ?
C7 C10 . 1.511(2) ?
C8 C9 . 1.385(3) ?
C8 H8 . 0.9300 ?
C9 C9 2_655 1.384(5) ?
C9 H9 . 0.9300 ?
O1W H1WA . 0.84(3) ?
O1W H1WB . 0.83(3) ?
O2W H2WA . 0.84(3) ?
O2W H2WB . 0.84(2) ?
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
O2W H2WA O1 . 0.84(3) 2.056(16) 2.809(2) 149(3)
O1W H1WA O2W 2 0.84(3) 1.906(11) 2.716(2) 163(2)
O1W H1WB O2 2_655 0.83(3) 1.874(10) 2.703(2) 174(2)
O2W H2WB O2 3_666 0.84(2) 2.009(11) 2.834(2) 169(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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O1W Ni1 O1 C10 . . 18.21(17)
O1W Ni1 O1 C10 2 . -163.14(17)
N1 Ni1 O1 C10 1_565 . -72.67(17)
N2 Ni1 O1 C10 . . 107.33(17)
O1W Ni1 N2 C6 . . 43.77(11)
O1W Ni1 N2 C6 2 . -136.23(11)
O1 Ni1 N2 C6 . . -49.62(11)
O1 Ni1 N2 C6 2 . 130.38(11)
O1W Ni1 N2 C6 . 2 -136.23(11)
O1W Ni1 N2 C6 2 2 43.77(11)
O1 Ni1 N2 C6 . 2 130.38(11)
O1 Ni1 N2 C6 2 2 -49.62(11)
Ni1 N1 C1 C2 1_545 . -179.49(13)
N1 C1 C2 C3 . . -1.0(3)
C1 C2 C3 C2 . 2 0.47(12)
C1 C2 C3 C4 . . -179.53(12)
C2 C3 C4 C5 . . -53.29(13)
C2 C3 C4 C5 2 . 126.71(13)
C2 C3 C4 C5 . 2 126.71(13)
C2 C3 C4 C5 2 2 -53.29(13)
C5 C4 C5 C6 2 . 0.97(13)
C3 C4 C5 C6 . . -179.03(13)
C6 N2 C6 C5 2 . 1.05(14)
Ni1 N2 C6 C5 . . -178.95(14)
C4 C5 C6 N2 . . -2.1(3)
C7 C7 C8 C9 2_655 . 1.3(3)
C10 C7 C8 C9 . . 178.96(17)
C7 C8 C9 C9 . 2_655 1.6(4)
Ni1 O1 C10 O2 . . -133.71(17)
Ni1 O1 C10 C7 . . 48.5(2)
C8 C7 C10 O2 . . -119.1(2)
C7 C7 C10 O2 2_655 . 58.5(3)
C8 C7 C10 O1 . . 58.9(2)
C7 C7 C10 O1 2_655 . -123.5(2)
