#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2008587.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_2008587
loop_
_publ_author_name
'Karanovi\'c, L.'
'Poleti, D.'
'Bogdanovi\'c, G. A.'
'Spasojevi\'c-de Bir\'e, A.'
_publ_section_title
;
 Disodium hexaaquacobalt(II) bis[dihydrogen
 1,2,4,5-benzenetetracarboxylate(2 --)] tetrahydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              911
_journal_page_last               913
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          'Na2 [Co (H2 O)6] (C10 H4 O8)2 , 4H2 O'
_chemical_formula_moiety         '2C10 H4 O8, Co H12  O6 2- , 4H2 O, 2Na+'
_chemical_formula_structural     'Na2 (Co (H2 O)6) (C10 H4 O8)2 .(H2 O)4'
_chemical_formula_sum            'C20 H28 Co Na2 O26'
_chemical_formula_weight         789.33
_chemical_name_systematic
;
Disodium hexaaquacobalt(II) dihydrogen 1,2,4,5-benzenetetracarboxylate(2-)
tetrahydrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 103.33(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.320(4)
_cell_length_b                   20.150(5)
_cell_length_c                   10.448(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    299(3)
_cell_measurement_theta_max      16.62
_cell_measurement_theta_min      13.18
_cell_volume                     1499.5(10)
_diffrn_ambient_temperature      299(3)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \o/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1901
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'De Tita (1985)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             810.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.945
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_restrained_S_obs      0.987
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0744P)^2^+1.4558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.1207
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                1549
_reflns_number_total             1807
_reflns_observed_criterion       I>2\s(I)
_[local]_cod_data_source_file    na1397.cif
_[local]_cod_data_source_block   a3
_[local]_cod_cif_authors_sg_H-M  'C 2/m'
_cod_database_code               2008587
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-x, y, -z'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co 0.0357(3) 0.0208(3) 0.0247(3) 0.000 0.0037(2) 0.000
Na 0.0601(9) 0.0225(6) 0.0372(7) 0.000 0.0048(6) 0.000
O1 0.0564(15) 0.0215(11) 0.0349(12) 0.000 -0.0109(10) 0.000
O2 0.0365(12) 0.0253(11) 0.0407(13) 0.000 0.0079(10) 0.000
O3 0.0511(14) 0.0233(10) 0.0389(13) 0.000 0.0170(11) 0.000
O4 0.0582(11) 0.0232(8) 0.0380(8) 0.0031(7) 0.0053(7) 0.0055(6)
O5 0.0791(14) 0.0309(9) 0.0398(10) 0.0022(8) -0.0191(9) 0.0044(7)
O6 0.0780(14) 0.0226(9) 0.0465(10) -0.0046(8) -0.0089(9) -0.0043(7)
O7 0.0780(14) 0.0316(9) 0.0402(10) -0.0030(8) -0.0211(9) -0.0036(7)
O8 0.079(2) 0.0356(14) 0.059(2) 0.000 0.034(2) 0.000
O9 0.0453(13) 0.0257(10) 0.0336(11) 0.000 -0.0036(9) 0.000
C1 0.0343(14) 0.0182(12) 0.0307(14) 0.000 0.0071(11) 0.000
C2 0.0311(9) 0.0235(9) 0.0251(9) 0.0016(7) 0.0032(7) 0.0014(7)
C3 0.0322(9) 0.0222(9) 0.0267(9) -0.0015(7) 0.0030(7) -0.0006(7)
C4 0.0353(14) 0.0186(12) 0.0285(14) 0.000 0.0045(11) 0.000
C5 0.0380(10) 0.0266(10) 0.0301(10) 0.0021(8) 0.0035(8) 0.0037(8)
C6 0.0412(11) 0.0249(10) 0.0325(11) -0.0022(8) 0.0003(8) -0.0035(8)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Co 0.0000 0.0000 0.0000 0.0276(2) Uani d S 1 Co
Na -0.3168(2) 0.0000 -0.32640(13) 0.0410(3) Uani d S 1 Na
O1 0.0000 0.10198(11) 0.0000 0.0410(6) Uani d S 1 O
O2 -0.2917(3) 0.0000 -0.0833(2) 0.0343(5) Uani d S 1 O
O3 -0.0282(4) 0.0000 0.1972(2) 0.0367(5) Uani d S 1 O
O4 0.3107(2) 0.39593(8) 0.3010(2) 0.0407(4) Uani d . 1 O
O5 0.2016(3) 0.31233(9) 0.1738(2) 0.0553(5) Uani d . 1 O
O6 0.3064(3) 0.11200(8) 0.3033(2) 0.0528(5) Uani d . 1 O
O7 0.1999(3) 0.19404(9) 0.1733(2) 0.0556(6) Uani d . 1 O
O8 0.6680(5) 0.0000 0.4359(3) 0.0549(7) Uani d S 1 O
O9 0.5000 0.09615(11) 0.0000 0.0369(5) Uani d S 1 O
C1 0.5000 0.32083(13) 0.5000 0.0278(6) Uani d S 1 C
H6 0.5000 0.36698(13) 0.5000 0.033 Uiso calc SR 1 H
C2 0.3974(3) 0.28895(9) 0.3886(2) 0.0271(4) Uani d . 1 C
C3 0.3975(3) 0.21888(9) 0.3887(2) 0.0277(4) Uani d . 1 C
C4 0.5000 0.18714(14) 0.5000 0.0279(6) Uani d S 1 C
H4 0.5000 0.14098(14) 0.5000 0.033 Uiso calc SR 1 H
C5 0.2968(3) 0.33584(11) 0.2808(2) 0.0323(4) Uani d . 1 C
C6 0.2962(3) 0.17102(10) 0.2827(2) 0.0342(5) Uani d . 1 C
H1 0.058(5) 0.1283(16) 0.051(4) 0.073(11) Uiso d . 1 H
H2 -0.346(4) -0.0290(13) -0.067(3) 0.042(8) Uiso d . 1 H
H3 -0.086(5) -0.0290(15) 0.215(3) 0.057(10) Uiso d . 1 H
H5 0.197(7) 0.253(2) 0.181(5) 0.101(15) Uiso d . 1 H
H7 0.436(5) 0.1241(16) -0.056(4) 0.070(10) Uiso d . 1 H
H8 0.727(6) -0.0318(19) 0.417(5) 0.105(16) Uiso d . 1 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'
Co Co 0.3494 0.9721 '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'
N N 0.0061 0.0033 '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
O1 Co O1 . 5 180.0
O1 Co O2 . 5 90.0
O1 Co O2 5 5 90.0
O1 Co O2 . . 90.0
O1 Co O2 5 . 90.0
O2 Co O2 5 . 180.0
O1 Co O3 . 5 90.0
O1 Co O3 5 5 90.0
O2 Co O3 5 5 94.87(11)
O2 Co O3 . 5 85.13(11)
O1 Co O3 . . 90.0
O1 Co O3 5 . 90.0
O2 Co O3 5 . 85.13(11)
O2 Co O3 . . 94.87(11)
O3 Co O3 5 . 180.0
O6 Na O6 6 5 168.09(11)
O6 Na O8 6 1_454 95.73(6)
O6 Na O8 5 1_454 95.73(6)
O6 Na O2 6 . 84.23(6)
O6 Na O2 5 . 84.23(6)
O8 Na O2 1_454 . 178.41(11)
O6 Na O8 6 5 93.04(6)
O6 Na O8 5 5 93.04(6)
O8 Na O8 1_454 5 75.04(12)
O2 Na O8 . 5 106.54(11)
O6 Na O3 6 5 86.53(6)
O6 Na O3 5 5 86.53(6)
O8 Na O3 1_454 5 109.87(12)
O2 Na O3 . 5 68.55(9)
O8 Na O3 5 5 175.09(10)
O6 Na Na 6 5_454 95.50(6)
O6 Na Na 5 5_454 95.50(6)
O8 Na Na 1_454 5_454 38.41(9)
O2 Na Na . 5_454 143.18(9)
O8 Na Na 5 5_454 36.63(7)
O3 Na Na 5 5_454 148.28(9)
Co O2 Na . . 104.43(11)
Co O3 Na . 5 101.89(11)
C6 O6 Na . 5 175.9(2)
Na O8 Na 1_656 5 104.96(12)
C2 C1 C2 . 6_656 124.9(3)
C1 C2 C3 . . 117.5(2)
C1 C2 C5 . . 114.1(2)
C3 C2 C5 . . 128.3(2)
C4 C3 C2 . . 117.5(2)
C4 C3 C6 . . 113.3(2)
C2 C3 C6 . . 129.2(2)
C3 C4 C3 6_656 . 125.1(3)
O4 C5 O5 . . 121.9(2)
O4 C5 C2 . . 118.4(2)
O5 C5 C2 . . 119.7(2)
O6 C6 O7 . . 120.9(2)
O6 C6 C3 . . 119.5(2)
O7 C6 C3 . . 119.6(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co O1 . 2.055(2)
Co O1 5 2.055(2)
Co O2 5 2.112(3)
Co O2 . 2.112(3)
Co O3 5 2.117(2)
Co O3 . 2.117(2)
Na O6 6 2.269(2)
Na O6 5 2.269(2)
Na O8 1_454 2.460(3)
Na O2 . 2.503(3)
Na O8 5 2.561(4)
Na O3 5 2.575(3)
Na Na 5_454 3.983(3)
O3 Na 5 2.575(3)
O4 C5 . 1.229(3)
O5 C5 . 1.264(3)
O6 C6 . 1.208(3)
O6 Na 5 2.269(2)
O7 C6 . 1.283(3)
O8 Na 1_656 2.460(3)
O8 Na 5 2.561(4)
C1 C2 . 1.388(2)
C1 C2 6_656 1.388(2)
C2 C3 . 1.412(3)
C2 C5 . 1.524(3)
C3 C4 . 1.386(2)
C3 C6 . 1.526(3)
C4 C3 6_656 1.386(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
_geom_hbond_publ_flag
O5 H5 O7 1_555 1.20(4) 1.19(4) 2.384(3) 171(4) yes
O1 H1 O7 1_555 0.80(3) 1.96(3) 2.764(2) 178(4) yes
O2 H2 O9 5_555 0.75(3) 1.99(3) 2.729(3) 170(2) yes
O3 H3 O4 3_445 0.77(3) 2.00(3) 2.748(3) 166(3) yes
O8 H8 O4 3_545 0.82(4) 2.08(5) 2.856(3) 158(4) yes
O9 H7 O5 7_555 0.87(3) 1.90(3) 2.764(2) 178(2) yes