#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/89/2238936.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_2238936
loop_
_publ_author_name
'Camara, Magatte'
'Tine, Modou'
'Daiguebonne, Carole'
'Guillou, Olivier'
'Roisnel, Thierry'
_publ_section_title
;
 Poly[[octaaqua-μ₄-(benzene-1,2,4,5-tetracarboxylato)-dicobalt(II)]
 octahydrate]
;
_journal_coeditor_code           VN2077
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m680
_journal_page_last               m681
_journal_paper_doi               10.1107/S1600536813031577
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Co2 (C10 H2 O8) (H2 O)8], 8H2 O'
_chemical_formula_moiety         'C10 H34 Co2 O24'
_chemical_formula_sum            'C10 H34 Co2 O24'
_chemical_formula_weight         656.22
_chemical_name_systematic
;
Poly[[octaaqua-μ₄-(benzene-1,2,4,5-tetracarboxylato)-dicobalt(II)]
octahydrate]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                96.4450(10)
_cell_angle_beta                 91.2320(10)
_cell_angle_gamma                91.3280(10)
_cell_formula_units_Z            1
_cell_length_a                   5.43710(10)
_cell_length_b                   9.8496(3)
_cell_length_c                   10.2564(3)
_cell_measurement_temperature    298(2)
_cell_volume                     545.49(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'CCD rotation images, thin slices scans'
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8487
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         1.999
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'very light pink'
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_description       prism
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.808
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0911P)²+2.3818P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                2092
_reflns_number_total             2456
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            vn2077.cif
_cod_data_source_block           I
_cod_original_cell_volume        545.48(3)
_cod_database_code               2238936
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.908
_shelxl_version_number           2.013
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_occupancy
H H1 0.0869 0.1434 0.3071 0.050 Uiso d 1
H H13 0.0780 -0.2852 -0.0807 0.050 Uiso d 1
H H4 0.2169 -0.2460 0.0208 0.050 Uiso d 1
H H5 0.4549 0.1226 0.5668 0.050 Uiso d 1
H H6 -0.4194 -0.4465 0.1454 0.050 Uiso d 1
H H7 0.2609 0.1784 0.6194 0.050 Uiso d 1
H H9 -0.1925 -0.3972 0.2127 0.050 Uiso d 1
H H10 0.1381 0.0269 0.2641 0.050 Uiso d 1
Co Co1 0.0000 0.0000 0.5000 0.0165(2) Uani d 1
Co Co2 0.0000 -0.5000 0.0000 0.0180(2) Uani d 1
O O22 -0.0419(5) -0.3362(3) 0.3694(3) 0.0246(6) Uani d 1
O O12 0.2439(5) -0.5016(3) 0.1641(3) 0.0212(6) Uani d 1
O O23 0.2189(5) -0.1729(3) 0.4617(3) 0.0224(6) Uani d 1
O O11 0.0733(6) -0.6758(3) 0.2541(3) 0.0352(8) Uani d 1
O O1 0.3013(5) 0.1098(3) 0.5906(3) 0.0308(7) Uani d 1
O O2 -0.2644(6) -0.4222(4) 0.1330(3) 0.0399(8) Uani d 1
C C1 0.3561(6) -0.5310(4) 0.3841(3) 0.0159(7) Uani d 1
O O3 0.0735(7) 0.0657(3) 0.3177(3) 0.0381(8) Uani d 1
C C3 0.5172(7) -0.6259(4) 0.4275(3) 0.0170(7) Uani d 1
H H3 0.5283 -0.7109 0.3786 0.020 Uiso calc 1
C C2 0.3387(6) -0.4025(3) 0.4587(3) 0.0150(7) Uani d 1
C C22 0.1578(6) -0.2968(4) 0.4251(3) 0.0158(7) Uani d 1
C C11 0.2111(7) -0.5719(4) 0.2586(3) 0.0180(7) Uani d 1
O O4 0.1143(9) -0.3016(4) -0.0152(4) 0.0596(13) Uani d 1
O O14 0.2936(16) -0.0732(8) 0.1144(8) 0.121(3) Uani d 1
O O16 0.5551(16) -0.1850(8) 0.0171(9) 0.121(3) Uani d 1
O O15 -0.4581(14) 0.0456(9) 0.1989(8) 0.116(2) Uani d 1
O O17 0.8066(16) -0.0714(9) 0.1011(8) 0.124(3) Uani 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'
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'
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 Co1 O1 . 2_556 180.0
O1 Co1 O3 . . 92.62(14)
O1 Co1 O3 2_556 . 87.38(14)
O1 Co1 O3 . 2_556 87.38(14)
O1 Co1 O3 2_556 2_556 92.62(14)
O3 Co1 O3 . 2_556 180.0
O1 Co1 O23 . . 90.10(11)
O1 Co1 O23 2_556 . 89.90(11)
O3 Co1 O23 . . 92.24(12)
O3 Co1 O23 2_556 . 87.76(12)
O1 Co1 O23 . 2_556 89.90(11)
O1 Co1 O23 2_556 2_556 90.10(11)
O3 Co1 O23 . 2_556 87.76(12)
O3 Co1 O23 2_556 2_556 92.24(12)
O23 Co1 O23 . 2_556 180.0
O4 Co2 O4 . 2_545 180.0
O4 Co2 O2 . 2_545 91.81(19)
O4 Co2 O2 2_545 2_545 88.19(19)
O4 Co2 O2 . . 88.19(19)
O4 Co2 O2 2_545 . 91.81(19)
O2 Co2 O2 2_545 . 180.0
O4 Co2 O12 . 2_545 91.09(12)
O4 Co2 O12 2_545 2_545 88.91(12)
O2 Co2 O12 2_545 2_545 87.12(11)
O2 Co2 O12 . 2_545 92.88(11)
O4 Co2 O12 . . 88.91(12)
O4 Co2 O12 2_545 . 91.09(12)
O2 Co2 O12 2_545 . 92.88(11)
O2 Co2 O12 . . 87.12(11)
O12 Co2 O12 2_545 . 180.0
C11 O12 Co2 . . 124.9(2)
C22 O23 Co1 . . 130.4(2)
C3 C1 C2 . . 118.8(3)
C3 C1 C11 . . 117.7(3)
C2 C1 C11 . . 123.5(3)
C2 C3 C1 2_646 . 122.2(3)
C3 C2 C1 2_646 . 119.0(3)
C3 C2 C22 2_646 . 118.1(3)
C1 C2 C22 . . 122.8(3)
O22 C22 O23 . . 124.9(3)
O22 C22 C2 . . 118.8(3)
O23 C22 C2 . . 116.2(3)
O11 C11 O12 . . 124.9(3)
O11 C11 C1 . . 117.4(3)
O12 C11 C1 . . 117.7(3)
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 O1 . 2.084(3) yes
Co1 O1 2_556 2.084(3) ?
Co1 O3 . 2.089(3) yes
Co1 O3 2_556 2.089(3) ?
Co1 O23 . 2.106(2) yes
Co1 O23 2_556 2.106(2) ?
Co2 O2 . 2.101(3) yes
Co2 O4 . 2.060(3) yes
Co2 O4 2_545 2.061(3) ?
Co2 O2 2_545 2.101(3) ?
Co2 O12 2_545 2.122(2) ?
Co2 O12 . 2.122(2) yes
O22 C22 . 1.249(4) ?
O12 C11 . 1.266(5) ?
O23 C22 . 1.270(4) ?
O11 C11 . 1.250(5) ?
C1 C3 . 1.398(5) ?
C1 C2 . 1.410(5) ?
C1 C11 . 1.505(5) ?
C3 C2 2_646 1.390(5) ?
C2 C3 2_646 1.390(5) ?
C2 C22 . 1.511(5) ?
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
O3 H1 O11 1_565 0.79 1.92 2.698(4) 169
O4 H4 O14 . 0.82 1.89 2.636(9) 150
O4 H4 O16 . 0.82 1.92 2.632(10) 143
O1 H5 O23 2_656 0.89 1.87 2.746(4) 171
O2 H6 O12 1_455 0.89 1.92 2.803(4) 177
O1 H7 O22 2_556 0.75 1.97 2.664(4) 154
O2 H9 O22 . 0.90 1.82 2.725(4) 176
O3 H10 O14 . 0.73 1.95 2.682(9) 176
O3 H10 O15 1_655 0.73 2.32 2.848(9) 130
O4 H13 O11 2_545 0.73 1.94 2.618(5) 154
