#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/45/2204576.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_2204576
loop_
_publ_author_name
'Xie, Cheng-Zhi'
'Zhang, Bao-Feng'
'Wang, Xiao-Qing'
'Shen, Guang-Qiu'
'Shen, De-Zhong'
_publ_section_title
;catena-poly[[[tetraaquacobalt(II)]-μ-4,4'-bipyridine-κ²N:N']
 phthalate dihydrate]
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1703
_journal_page_last               m1705
_journal_paper_doi               10.1107/S1600536804025930
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Co (C10 H8 N2) (H2 O)4] (C8 H4 O4), 2H2 O'
_chemical_formula_moiety         'C18 H24 Co N2 O10'
_chemical_formula_structural     '[Co (C10 H8 N2) (H2 O)4] (C8 H4 O4), 2H2 O'
_chemical_formula_sum            'C18 H24 Co N2 O10'
_chemical_formula_weight         487.32
_chemical_name_systematic
;
catena-poly[[[tetraaquacobalt(II)]-μ-4,4-bipyridine-κ²N:N'] phthalate
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                 125.287(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.511(3)
_cell_length_b                   11.496(3)
_cell_length_c                   11.528(4)
_cell_measurement_reflns_used    925
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.80
_cell_volume                     1028.9(6)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD 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  0.036
_diffrn_reflns_av_sigmaI/netI    0.042
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5821
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2111
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.052
_refine_ls_R_factor_gt           0.036
_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)+(0.0379P)²+0.3271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.078
_refine_ls_wR_factor_ref         0.084
_reflns_number_gt                1665
_reflns_number_total             2111
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wk6022.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1028.9(5)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2204576
_cod_database_fobs_code          2204576
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_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_type_symbol
Co1 0.5000 0.01953(4) 0.2500 0.02130(14) Uani d S 1 Co
N1 0.5000 0.2085(2) 0.2500 0.0250(6) Uani d S 1 N
N2 0.5000 0.8285(2) 0.2500 0.0248(6) Uani d S 1 N
C1 0.5956(3) 0.2703(2) 0.2216(3) 0.0359(6) Uani d . 1 C
H1 0.6631 0.2300 0.2007 0.043 Uiso calc R 1 H
C2 0.6003(3) 0.3895(2) 0.2214(3) 0.0357(6) Uani d . 1 C
H2 0.6709 0.4274 0.2021 0.043 Uiso calc R 1 H
C3 0.5000 0.4538(3) 0.2500 0.0239(7) Uani d S 1 C
C4 0.5000 0.5825(3) 0.2500 0.0238(7) Uani d S 1 C
C5 0.5586(3) 0.6475(2) 0.1838(3) 0.0299(6) Uani d . 1 C
H5 0.5996 0.6097 0.1375 0.036 Uiso calc R 1 H
C6 0.5564(3) 0.7664(2) 0.1864(3) 0.0306(6) Uani d . 1 C
H6 0.5967 0.8066 0.1411 0.037 Uiso calc R 1 H
O1 0.1812(3) 0.12805(17) 0.3772(2) 0.0464(5) Uani d . 1 O
O2 0.0753(3) 0.17483(19) 0.4985(2) 0.0534(6) Uani d . 1 O
C7 0.1002(3) 0.1938(2) 0.4056(3) 0.0298(6) Uani d . 1 C
C8 0.0389(3) 0.3059(2) 0.3227(2) 0.0265(5) Uani d . 1 C
C9 0.0755(3) 0.4109(2) 0.3942(3) 0.0410(7) Uani d . 1 C
H9 0.1260 0.4113 0.4914 0.049 Uiso calc R 1 H
C10 0.0374(4) 0.5152(2) 0.3215(4) 0.0544(8) Uani d . 1 C
H10 0.0627 0.5853 0.3701 0.065 Uiso calc R 1 H
O3 0.6092(2) 0.02703(15) 0.46407(17) 0.0325(4) Uani d D 1 O
H3A 0.524(3) 0.021(3) 0.469(4) 0.049 Uiso d PD 0.67 H
H3B 0.657(3) 0.0934(12) 0.493(3) 0.049 Uiso d PD 0.67 H
H3C 0.683(3) -0.0262(18) 0.512(3) 0.049 Uiso d PD 0.67 H
O4 0.2463(2) 0.00320(15) 0.19401(19) 0.0377(4) Uani d . 1 O
H4A 0.1831 0.0464 0.2059 0.057 Uiso d R 1 H
H4B 0.1875 -0.0500 0.1335 0.057 Uiso d R 1 H
O5 0.8740(3) 0.19927(18) 0.6005(2) 0.0602(6) Uani d D 1 O
H5A 0.917(5) 0.209(4) 0.554(3) 0.090 Uiso d PD 0.67 H
H5B 0.954(4) 0.189(4) 0.6880(11) 0.090 Uiso d PD 0.67 H
H5C 0.807(5) 0.141(2) 0.568(4) 0.090 Uiso d PD 0.67 H
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
_geom_angle_publ_flag
O3 Co1 O3 2_655 . 175.18(10) yes
O3 Co1 O4 2_655 . 86.62(7) yes
O3 Co1 O4 . . 93.81(7) yes
O3 Co1 O4 2_655 2_655 93.81(7) ?
O3 Co1 O4 . 2_655 86.62(7) ?
O4 Co1 O4 . 2_655 169.82(9) yes
O3 Co1 N1 2_655 . 87.59(5) ?
O3 Co1 N1 . . 87.59(5) yes
O4 Co1 N1 . . 95.09(5) yes
O4 Co1 N1 2_655 . 95.09(5) ?
O3 Co1 N2 2_655 1_545 92.41(5) ?
O3 Co1 N2 . 1_545 92.41(5) yes
O4 Co1 N2 . 1_545 84.91(5) yes
O4 Co1 N2 2_655 1_545 84.91(5) ?
N1 Co1 N2 . 1_545 180.0 yes
C1 N1 C1 2_655 . 115.7(3) ?
C1 N1 Co1 2_655 . 122.14(14) ?
C1 N1 Co1 . . 122.14(14) ?
C6 N2 C6 . 2_655 115.5(3) ?
C6 N2 Co1 . 1_565 122.27(14) ?
C6 N2 Co1 2_655 1_565 122.27(14) ?
N1 C1 C2 . . 124.0(2) ?
N1 C1 H1 . . 118.0 ?
C2 C1 H1 . . 118.0 ?
C1 C2 C3 . . 120.3(2) ?
C1 C2 H2 . . 119.9 ?
C3 C2 H2 . . 119.9 ?
C2 C3 C2 2_655 . 115.7(3) ?
C2 C3 C4 2_655 . 122.17(15) ?
C2 C3 C4 . . 122.17(15) ?
C5 C4 C5 2_655 . 115.2(3) ?
C5 C4 C3 2_655 . 122.38(15) ?
C5 C4 C3 . . 122.38(15) ?
C6 C5 C4 . . 120.4(2) ?
C6 C5 H5 . . 119.8 ?
C4 C5 H5 . . 119.8 ?
N2 C6 C5 . . 124.2(2) ?
N2 C6 H6 . . 117.9 ?
C5 C6 H6 . . 117.9 ?
O2 C7 O1 . . 125.0(2) ?
O2 C7 C8 . . 120.0(2) ?
O1 C7 C8 . . 115.0(2) ?
C8 C8 C9 2 . 119.56(16) ?
C8 C8 C7 2 . 120.48(14) ?
C9 C8 C7 . . 119.7(2) ?
C10 C9 C8 . . 120.3(3) ?
C10 C9 H9 . . 119.8 ?
C8 C9 H9 . . 119.8 ?
C10 C10 C9 2 . 120.09(17) ?
C10 C10 H10 2 . 120.0 ?
C9 C10 H10 . . 120.0 ?
Co1 O3 H3A . . 104(2) ?
Co1 O3 H3B . . 107(2) ?
H3A O3 H3B . . 111.3(12) ?
Co1 O3 H3C . . 114(2) ?
H3A O3 H3C . . 110.4(12) ?
H3B O3 H3C . . 110.0(12) ?
Co1 O4 H4A . . 133.4 ?
Co1 O4 H4B . . 114.1 ?
H4A O4 H4B . . 111.2 ?
H5A O5 H5B . . 110.0(12) ?
H5A O5 H5C . . 110.0(12) ?
H5B O5 H5C . . 109.9(12) ?
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
Co1 O3 2_655 2.0529(17) yes
Co1 O3 . 2.0529(17) yes
Co1 O4 . 2.1158(17) yes
Co1 O4 2_655 2.1158(17) yes
Co1 N1 . 2.173(3) yes
Co1 N2 1_545 2.197(3) yes
N1 C1 2_655 1.334(3) ?
N1 C1 . 1.334(3) ?
N2 C6 . 1.337(3) ?
N2 C6 2_655 1.337(3) ?
N2 Co1 1_565 2.197(3) ?
C1 C2 . 1.371(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.388(3) ?
C2 H2 . 0.9300 ?
C3 C2 2_655 1.388(3) ?
C3 C4 . 1.480(4) ?
C4 C5 2_655 1.394(3) ?
C4 C5 . 1.394(3) ?
C5 C6 . 1.368(3) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
O1 C7 . 1.250(3) yes
O2 C7 . 1.242(3) yes
C7 C8 . 1.507(3) ?
C8 C8 2 1.387(5) ?
C8 C9 . 1.388(3) ?
C9 C10 . 1.386(4) ?
C9 H9 . 0.9300 ?
C10 C10 2 1.368(7) ?
C10 H10 . 0.9300 ?
O3 H3A . 0.8499(11) ?
O3 H3B . 0.8499(11) ?
O3 H3C . 0.8502(11) ?
O4 H4A . 0.8499 ?
O4 H4B . 0.8499 ?
O5 H5A . 0.8501(11) ?
O5 H5B . 0.8501(11) ?
O5 H5C . 0.8501(11) ?
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
_geom_hbond_publ_flag
O5 H5C O3 . 0.8501(11) 2.019(9) 2.856(3) 168(4) yes
O5 H5B O5 2_756 0.8501(11) 2.007(10) 2.843(5) 167(4) yes
O5 H5A O2 1_655 0.8501(11) 1.98(2) 2.780(3) 156(4) yes
O4 H4B O2 4 0.85 1.92 2.771(3) 174 yes
O3 H3C O1 3_656 0.8502(11) 1.663(6) 2.507(2) 172(3) yes
O3 H3B O5 . 0.8499(11) 2.081(15) 2.856(3) 151(3) yes
O3 H3A O3 3_656 0.8499(11) 1.904(12) 2.716(3) 159(3) yes
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
O3 Co1 N1 C1 2_655 2_655 114.54(15)
O3 Co1 N1 C1 . 2_655 -65.46(15)
O4 Co1 N1 C1 . 2_655 28.15(15)
O4 Co1 N1 C1 2_655 2_655 -151.85(15)
O3 Co1 N1 C1 2_655 . -65.46(15)
O3 Co1 N1 C1 . . 114.54(15)
O4 Co1 N1 C1 . . -151.85(15)
O4 Co1 N1 C1 2_655 . 28.15(15)
N2 Co1 N1 C1 1_545 . 37.0(8)
C1 N1 C1 C2 2_655 . 0.5(2)
Co1 N1 C1 C2 . . -179.5(2)
N1 C1 C2 C3 . . -0.9(4)
C1 C2 C3 C2 . 2_655 0.43(19)
C1 C2 C3 C4 . . -179.57(19)
C2 C3 C4 C5 2_655 2_655 18.73(18)
C2 C3 C4 C5 . 2_655 -161.26(18)
C2 C3 C4 C5 2_655 . -161.27(18)
C2 C3 C4 C5 . . 18.73(18)
C5 C4 C5 C6 2_655 . 0.03(17)
C3 C4 C5 C6 . . -179.97(17)
C6 N2 C6 C5 2_655 . 0.03(18)
Co1 N2 C6 C5 1_565 . -179.97(18)
C4 C5 C6 N2 . . -0.1(4)
O2 C7 C8 C8 . 2 -137.9(3)
O1 C7 C8 C8 . 2 45.1(4)
O2 C7 C8 C9 . . 48.5(3)
O1 C7 C8 C9 . . -128.6(3)
C8 C8 C9 C10 2 . -1.0(4)
C7 C8 C9 C10 . . 172.7(2)
C8 C9 C10 C10 . 2 0.2(5)
