#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/70/2217014.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_2217014
loop_
_publ_author_name
'Licai Zhu'
'Hebing Zhu'
'Feng Sun'
_publ_section_title
Poly[[diaquanickel(II)]-μ₂-4,4'-bipyridine-κ²N:N'-μ-p-phenylenedioxydiacetato-κ²O:O']
_journal_coeditor_code           DN2287
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m57
_journal_page_last               m57
_journal_paper_doi               10.1107/S1600536807062794
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C10 H8 O6) (C10 H8 N2) (H2 O)2]'
_chemical_formula_moiety         'C20 H20 N2 Ni O8'
_chemical_formula_sum            'C20 H20 N2 Ni O8'
_chemical_formula_weight         475.09
_chemical_name_systematic
;
Poly[[diaquanickel(II)]-μ₂-4,4'-bipyridine-κ²N:N'-
μ-p-phenylenedioxydiacetato-κ²O:O']
;
_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           SHELXL97
_cell_angle_alpha                106.1570(10)
_cell_angle_beta                 96.8180(10)
_cell_angle_gamma                97.3410(10)
_cell_formula_units_Z            1
_cell_length_a                   5.75410(10)
_cell_length_b                   8.17040(10)
_cell_length_c                   10.6437(2)
_cell_measurement_reflns_used    1800
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.36
_cell_volume                     470.399(14)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
;
ORTEPIII within PLATON (Spek, 2003) and CAMERON (Watkin et al.,
1993)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6907
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.8201
_exptl_absorpt_correction_T_min  0.7653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             246
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0335
_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)+(0.0346P)²+0.4701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                1769
_reflns_number_total             1952
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2287.cif
_cod_data_source_block           I
_cod_original_cell_volume        470.400(10)
_cod_database_code               2217014
_cod_database_fobs_code          2217014
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
C C1 0.1666(4) 0.7074(3) 0.7930(2) 0.0318(6) Uani d . 1
H H1 0.2876 0.7217 0.8633 0.038 Uiso calc R 1
C C2 0.1734(4) 0.5879(3) 0.6736(2) 0.0314(6) Uani d . 1
H H2 0.2965 0.5240 0.6655 0.038 Uiso calc R 1
C C3 -0.0019(4) 0.5624(3) 0.5655(2) 0.0201(5) Uani d . 1
C C4 -0.1819(4) 0.6612(3) 0.5876(2) 0.0262(5) Uani d . 1
H H4 -0.3058 0.6487 0.5192 0.031 Uiso calc R 1
C C5 -0.1772(4) 0.7772(3) 0.7101(2) 0.0264(5) Uani d . 1
H H5 -0.3005 0.8405 0.7218 0.032 Uiso calc R 1
C C6 0.1281(4) 0.7277(3) 1.1257(2) 0.0253(5) Uani d . 1
C C7 0.3161(5) 0.6440(3) 1.1868(3) 0.0327(6) Uani d . 1
H H7A 0.2457 0.5854 1.2444 0.039 Uiso calc R 1
H H7B 0.3633 0.5572 1.1163 0.039 Uiso calc R 1
C C8 0.5001(4) 0.8782(3) 1.3782(2) 0.0273(5) Uani d . 1
C C9 0.6973(4) 1.0042(3) 1.4391(3) 0.0315(6) Uani d . 1
H H9 0.8307 1.0079 1.3978 0.038 Uiso calc R 1
C C10 0.6996(4) 1.1242(3) 1.5598(3) 0.0315(6) Uani d . 1
H H10 0.8344 1.2067 1.5997 0.038 Uiso calc R 1
N N1 -0.0044(3) 0.8038(2) 0.81332(18) 0.0227(4) Uani d . 1
Ni Ni1 0.0000 1.0000 1.0000 0.02315(14) Uani d S 1
O O1 0.2019(3) 0.8651(2) 1.09891(15) 0.0251(4) Uani d . 1
O O2 -0.0799(3) 0.6527(2) 1.1047(2) 0.0427(5) Uani d . 1
O O3 0.5228(3) 0.7621(2) 1.26119(17) 0.0332(4) Uani d . 1
O O1W 0.3239(3) 1.1425(2) 0.98244(16) 0.0289(4) Uani d . 1
H H1W 0.2733 1.2183 0.9556 0.043 Uiso d R 1
H H2W 0.4307 1.1122 0.9424 0.043 Uiso d R 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
_geom_angle_publ_flag
N1 C1 C2 . . 123.6(2) ?
N1 C1 H1 . . 118.2 ?
C2 C1 H1 . . 118.2 ?
C1 C2 C3 . . 120.4(2) ?
C1 C2 H2 . . 119.8 ?
C3 C2 H2 . . 119.8 ?
C2 C3 C4 . . 115.8(2) ?
C2 C3 C3 . 2_566 122.1(2) ?
C4 C3 C3 . 2_566 122.1(2) ?
C5 C4 C3 . . 120.3(2) ?
C5 C4 H4 . . 119.8 ?
C3 C4 H4 . . 119.8 ?
N1 C5 C4 . . 123.5(2) ?
N1 C5 H5 . . 118.3 ?
C4 C5 H5 . . 118.3 ?
O2 C6 O1 . . 126.6(2) ?
O2 C6 C7 . . 116.8(2) ?
O1 C6 C7 . . 116.6(2) ?
O3 C7 C6 . . 114.3(2) ?
O3 C7 H7A . . 108.7 ?
C6 C7 H7A . . 108.7 ?
O3 C7 H7B . . 108.7 ?
C6 C7 H7B . . 108.7 ?
H7A C7 H7B . . 107.6 ?
O3 C8 C9 . . 115.9(2) ?
O3 C8 C10 . 2_678 125.3(2) ?
C9 C8 C10 . 2_678 118.8(2) ?
C10 C9 C8 . . 121.3(2) ?
C10 C9 H9 . . 119.3 ?
C8 C9 H9 . . 119.3 ?
C9 C10 C8 . 2_678 119.9(2) ?
C9 C10 H10 . . 120.0 ?
C8 C10 H10 2_678 . 120.0 ?
C1 N1 C5 . . 116.27(19) ?
C1 N1 Ni1 . . 122.60(15) ?
C5 N1 Ni1 . . 121.09(15) ?
O1 Ni1 O1 . 2_577 180.0000(10) ?
O1 Ni1 O1W . 2_577 92.17(6) ?
O1 Ni1 O1W 2_577 2_577 87.83(6) ?
O1 Ni1 O1W . . 87.83(6) y
O1 Ni1 O1W 2_577 . 92.17(6) ?
O1W Ni1 O1W 2_577 . 180.0 ?
O1 Ni1 N1 . 2_577 90.23(7) ?
O1 Ni1 N1 2_577 2_577 89.77(7) ?
O1W Ni1 N1 2_577 2_577 91.96(7) ?
O1W Ni1 N1 . 2_577 88.04(7) ?
O1 Ni1 N1 . . 89.77(7) y
O1 Ni1 N1 2_577 . 90.23(7) ?
O1W Ni1 N1 2_577 . 88.04(7) ?
O1W Ni1 N1 . . 91.96(7) y
N1 Ni1 N1 2_577 . 180.0000(10) ?
C6 O1 Ni1 . . 126.73(15) ?
C8 O3 C7 . . 117.78(19) ?
Ni1 O1W H1W . . 100.2 ?
Ni1 O1W H2W . . 131.1 ?
H1W O1W H2W . . 108.2 ?
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
C1 N1 . 1.338(3) ?
C1 C2 . 1.379(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.386(3) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.395(3) ?
C3 C3 2_566 1.486(4) ?
C4 C5 . 1.377(3) ?
C4 H4 . 0.9300 ?
C5 N1 . 1.340(3) ?
C5 H5 . 0.9300 ?
C6 O2 . 1.237(3) ?
C6 O1 . 1.268(3) ?
C6 C7 . 1.526(3) ?
C7 O3 . 1.425(3) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C8 O3 . 1.372(3) ?
C8 C9 . 1.387(3) ?
C8 C10 2_678 1.392(3) ?
C9 C10 . 1.380(4) ?
C9 H9 . 0.9300 ?
C10 C8 2_678 1.392(3) ?
C10 H10 . 0.9300 ?
N1 Ni1 . 2.1735(18) y
Ni1 O1 . 2.0869(15) y
Ni1 O1 2_577 2.0869(15) n
Ni1 O1W 2_577 2.1245(16) n
Ni1 O1W . 2.1245(16) y
Ni1 N1 2_577 2.1735(18) n
O1W H1W . 0.8206 ?
O1W H2W . 0.8144 ?
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 O2 2_577 0.82 1.81 2.605(2) 163.2
O1W H2W O1 2_677 0.81 2.21 2.962(2) 154.7
