#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/63/2236353.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_2236353
loop_
_publ_author_name
'Ge, Xin'
'Song, Shu-Yan'
_publ_section_title
;
 Poly[[diaqua(μ-4,4'-bipyridine
 N,N'-dioxide-κ²O:O')(μ-terephthalato-κ²O¹:O⁴)cobalt(II)]
 4,4'-bipyridine N,N'-dioxide monosolvate]
;
_journal_coeditor_code           HY2589
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1307
_journal_paper_doi               10.1107/S1600536812040056
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Co (C8 H4 O4) (C10 H8 N2 O2) (H2 O)2] , C10 H8 N2 O2'
_chemical_formula_moiety         'C18 H16 Co N2 O8, C10 H8 N2 O2'
_chemical_formula_sum            'C28 H24 Co N4 O10'
_chemical_formula_weight         635.44
_chemical_name_systematic
;
Poly[[diaqua(μ-4,4'-bipyridine
N,N'-dioxide-κ²O:O')(μ-terephthalato-
κ²O¹:O⁴)cobalt(II)] 4,4'-bipyridine
N,N'-dioxide monosolvate]
;
_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                81.312(2)
_cell_angle_beta                 82.200(2)
_cell_angle_gamma                79.301(2)
_cell_formula_units_Z            1
_cell_length_a                   7.3883(10)
_cell_length_b                   9.1788(13)
_cell_length_c                   9.8054(13)
_cell_measurement_reflns_used    2899
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.28
_cell_volume                     641.92(15)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3574
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.8661
_exptl_absorpt_correction_T_min  0.8252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             327
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.328
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2516
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0308
_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)+(0.0389P)²+0.3924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                2340
_reflns_number_total             2516
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2589.cif
_cod_data_source_block           I
_cod_database_code               2236353
_cod_database_fobs_code          2236353
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
_atom_site_symmetry_multiplicity
Co Co1 0.5000 0.5000 0.5000 0.01630(11) Uani d S 1 2
C C1 0.3852(3) 0.7380(2) 0.2083(2) 0.0221(4) Uani d . 1 1
H H1 0.3528 0.6439 0.2142 0.027 Uiso calc R 1 1
C C2 0.4275(3) 0.8156(2) 0.08038(19) 0.0209(4) Uani d . 1 1
H H2 0.4249 0.7727 0.0007 0.025 Uiso calc R 1 1
C C3 0.4745(2) 0.9580(2) 0.06822(18) 0.0186(4) Uani d . 1 1
C C4 0.4684(3) 1.0181(2) 0.1918(2) 0.0233(4) Uani d . 1 1
H H4 0.4925 1.1145 0.1887 0.028 Uiso calc R 1 1
C C5 0.4271(3) 0.9365(2) 0.3176(2) 0.0242(4) Uani d . 1 1
H H5 0.4246 0.9781 0.3988 0.029 Uiso calc R 1 1
C C6 0.8804(3) 0.7935(2) 0.2615(2) 0.0270(4) Uani d . 1 1
H H6 0.8534 0.6980 0.2909 0.032 Uiso calc R 1 1
C C7 0.9285(3) 0.8359(2) 0.1234(2) 0.0264(4) Uani d . 1 1
H H7 0.9313 0.7689 0.0606 0.032 Uiso calc R 1 1
C C8 0.9735(3) 0.9770(2) 0.0743(2) 0.0217(4) Uani d . 1 1
C C9 0.9655(3) 1.0700(2) 0.1762(2) 0.0317(5) Uani d . 1 1
H H9 0.9958 1.1649 0.1496 0.038 Uiso calc R 1 1
C C10 0.9150(3) 1.0265(2) 0.3131(2) 0.0344(5) Uani d . 1 1
H H10 0.9102 1.0920 0.3777 0.041 Uiso calc R 1 1
C C11 0.6942(2) 0.44694(19) 0.21107(18) 0.0164(4) Uani d . 1 1
C C12 0.8539(2) 0.47312(19) 0.10187(18) 0.0162(3) Uani d . 1 1
C C13 1.0328(2) 0.46045(19) 0.13839(18) 0.0175(4) Uani d . 1 1
H H13 1.0549 0.4345 0.2308 0.021 Uiso calc R 1 1
C C14 1.1778(2) 0.4865(2) 0.03689(18) 0.0179(4) Uani d . 1 1
H H14 1.2970 0.4770 0.0617 0.021 Uiso calc R 1 1
N N1 0.3901(2) 0.79675(17) 0.32562(16) 0.0206(3) Uani d . 1 1
N N2 0.8716(2) 0.88841(18) 0.35576(18) 0.0254(4) Uani d . 1 1
O O1 0.3567(2) 0.71908(15) 0.44822(14) 0.0266(3) Uani d . 1 1
O O2 0.8186(2) 0.84874(17) 0.48725(15) 0.0350(4) Uani d . 1 1
O O3 0.57776(18) 0.37620(15) 0.18300(14) 0.0232(3) Uani d . 1 1
O O4 0.68909(17) 0.50355(14) 0.32145(12) 0.0194(3) Uani d . 1 1
O O5 0.67652(19) 0.59404(15) 0.59885(14) 0.0225(3) Uani d D 1 1
H H5A 0.719(3) 0.6689(19) 0.555(2) 0.034 Uiso d D 1 1
H H5B 0.605(3) 0.626(3) 0.6676(17) 0.034 Uiso d 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'
Co Co 0.3494 0.9721 '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
O4 Co1 O4 2_666 . 180.0
O4 Co1 O5 2_666 . 90.46(5)
O4 Co1 O5 . . 89.54(5)
O4 Co1 O5 2_666 2_666 89.54(5)
O4 Co1 O5 . 2_666 90.46(5)
O5 Co1 O5 . 2_666 180.00(6)
O4 Co1 O1 2_666 2_666 95.05(5)
O4 Co1 O1 . 2_666 84.95(5)
O5 Co1 O1 . 2_666 92.31(6)
O5 Co1 O1 2_666 2_666 87.69(6)
O4 Co1 O1 2_666 . 84.95(5)
O4 Co1 O1 . . 95.05(5)
O5 Co1 O1 . . 87.69(6)
O5 Co1 O1 2_666 . 92.31(6)
O1 Co1 O1 2_666 . 180.0
N1 C1 C2 . . 120.77(17)
N1 C1 H1 . . 119.6
C2 C1 H1 . . 119.6
C1 C2 C3 . . 120.92(17)
C1 C2 H2 . . 119.5
C3 C2 H2 . . 119.5
C2 C3 C4 . . 116.56(17)
C2 C3 C3 . 2_675 121.9(2)
C4 C3 C3 . 2_675 121.5(2)
C5 C4 C3 . . 120.68(18)
C5 C4 H4 . . 119.7
C3 C4 H4 . . 119.7
N1 C5 C4 . . 121.11(17)
N1 C5 H5 . . 119.4
C4 C5 H5 . . 119.4
N2 C6 C7 . . 120.93(18)
N2 C6 H6 . . 119.5
C7 C6 H6 . . 119.5
C6 C7 C8 . . 121.82(19)
C6 C7 H7 . . 119.1
C8 C7 H7 . . 119.1
C7 C8 C9 . . 115.04(18)
C7 C8 C8 . 2_775 122.1(2)
C9 C8 C8 . 2_775 122.9(2)
C10 C9 C8 . . 122.32(19)
C10 C9 H9 . . 118.8
C8 C9 H9 . . 118.8
N2 C10 C9 . . 120.4(2)
N2 C10 H10 . . 119.8
C9 C10 H10 . . 119.8
O3 C11 O4 . . 126.25(16)
O3 C11 C12 . . 117.81(15)
O4 C11 C12 . . 115.90(15)
C14 C12 C13 2_765 . 119.39(16)
C14 C12 C11 2_765 . 119.82(15)
C13 C12 C11 . . 120.77(15)
C14 C13 C12 . . 120.09(16)
C14 C13 H13 . . 120.0
C12 C13 H13 . . 120.0
C13 C14 C12 . 2_765 120.52(16)
C13 C14 H14 . . 119.7
C12 C14 H14 2_765 . 119.7
O1 N1 C5 . . 119.74(16)
O1 N1 C1 . . 120.43(16)
C5 N1 C1 . . 119.82(16)
O2 N2 C6 . . 120.49(16)
O2 N2 C10 . . 120.07(17)
C6 N2 C10 . . 119.44(18)
N1 O1 Co1 . . 121.82(11)
C11 O4 Co1 . . 130.60(11)
Co1 O5 H5A . . 117.3(17)
Co1 O5 H5B . . 102.4(17)
H5A O5 H5B . . 106(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O4 2_666 2.0865(12)
Co1 O4 . 2.0865(12)
Co1 O5 . 2.0975(13)
Co1 O5 2_666 2.0976(13)
Co1 O1 2_666 2.1141(13)
Co1 O1 . 2.1141(13)
C1 N1 . 1.350(2)
C1 C2 . 1.373(3)
C1 H1 . 0.9300
C2 C3 . 1.397(3)
C2 H2 . 0.9300
C3 C4 . 1.398(3)
C3 C3 2_675 1.479(4)
C4 C5 . 1.371(3)
C4 H4 . 0.9300
C5 N1 . 1.349(3)
C5 H5 . 0.9300
C6 N2 . 1.350(3)
C6 C7 . 1.368(3)
C6 H6 . 0.9300
C7 C8 . 1.395(3)
C7 H7 . 0.9300
C8 C9 . 1.398(3)
C8 C8 2_775 1.475(4)
C9 C10 . 1.364(3)
C9 H9 . 0.9300
C10 N2 . 1.356(3)
C10 H10 . 0.9300
C11 O3 . 1.250(2)
C11 O4 . 1.263(2)
C11 C12 . 1.510(2)
C12 C14 2_765 1.395(2)
C12 C13 . 1.396(2)
C13 C14 . 1.389(3)
C13 H13 . 0.9300
C14 C12 2_765 1.395(2)
C14 H14 . 0.9300
N1 O1 . 1.319(2)
N2 O2 . 1.312(2)
O5 H5A . 0.84(2)
O5 H5B . 0.85(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
O5 H5A O2 . 0.84(2) 1.92(2) 2.755(2) 170(2)
O5 H5B O3 2_666 0.85(2) 1.85(2) 2.660(2) 158(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
N1 C1 C2 C3 . . -0.8(3)
C1 C2 C3 C4 . . -2.5(3)
C1 C2 C3 C3 . 2_675 178.3(2)
C2 C3 C4 C5 . . 3.1(3)
C3 C3 C4 C5 2_675 . -177.7(2)
C3 C4 C5 N1 . . -0.5(3)
N2 C6 C7 C8 . . 1.1(3)
C6 C7 C8 C9 . . 0.0(3)
C6 C7 C8 C8 . 2_775 179.6(2)
C7 C8 C9 C10 . . -0.9(3)
C8 C8 C9 C10 2_775 . 179.5(2)
C8 C9 C10 N2 . . 0.6(4)
O3 C11 C12 C14 . 2_765 42.0(2)
O4 C11 C12 C14 . 2_765 -135.93(17)
O3 C11 C12 C13 . . -139.35(17)
O4 C11 C12 C13 . . 42.7(2)
C14 C12 C13 C14 2_765 . -0.6(3)
C11 C12 C13 C14 . . -179.28(16)
C12 C13 C14 C12 . 2_765 0.6(3)
C4 C5 N1 O1 . . 177.84(17)
C4 C5 N1 C1 . . -3.0(3)
C2 C1 N1 O1 . . -177.21(16)
C2 C1 N1 C5 . . 3.6(3)
C7 C6 N2 O2 . . 177.42(19)
C7 C6 N2 C10 . . -1.4(3)
C9 C10 N2 O2 . . -178.3(2)
C9 C10 N2 C6 . . 0.5(3)
C5 N1 O1 Co1 . . -128.29(15)
C1 N1 O1 Co1 . . 52.5(2)
O4 Co1 O1 N1 2_666 . -171.81(14)
O4 Co1 O1 N1 . . 8.19(14)
O5 Co1 O1 N1 . . 97.52(14)
O5 Co1 O1 N1 2_666 . -82.48(14)
O3 C11 O4 Co1 . . 2.1(3)
C12 C11 O4 Co1 . . 179.77(11)
O5 Co1 O4 C11 . . 170.87(15)
O5 Co1 O4 C11 2_666 . -9.13(15)
O1 Co1 O4 C11 2_666 . 78.51(15)
O1 Co1 O4 C11 . . -101.49(15)
