#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:09:31 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179469 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/66/4336655.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4336655
loop_
_publ_author_name
'Oscar Fabelo'
'Laura Cañadillas-Delgado'
'Jorge Pasán'
'Pau Díaz-Gallifa'
'Catalina Ruiz-Pérez'
'Francesc Lloret'
'Miguel Julve'
'Inés Puente Orench'
'Javier Campo'
'Juan Rodríguez-Carvajal'
_publ_contact_author_address
;Laboratorio de Rayos X y Materiales Moleculares
 Dpto. Física Fundamental II. Facultad de Física
 Universidad de La Laguna
 E-38204. La Laguna. Tenerife
 Spain
;
_publ_contact_author_email       caruiz@ull.es
_publ_contact_author_fax         +34922318320
_publ_contact_author_name        'Professor Catalina Ruiz-Pérez'
_publ_contact_author_phone       +34922318300
_publ_section_title
;
 Neutron Diffraction Studies of the Molecular Compound [Co2(bta)]n (H4bta
 =1,2,4,5-Benzenetetracarboxylic Acid): In the Quest of Canted
 Ferromagnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12818
_journal_page_last               12827
_journal_paper_doi               10.1021/ic402186p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C10 H2 Co2 O8'
_chemical_formula_weight         367.98
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 115.763(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1453(5)
_cell_length_b                   17.4650(9)
_cell_length_c                   4.5525(5)
_cell_measurement_temperature    100(2)
_cell_volume                     440.04(7)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            928
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         3.86
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.816
_exptl_absorpt_correction_type   twinabs
_exptl_absorpt_process_details
'Sheldrick, G.M. TWINABS University of Gottingen 2002.'
_exptl_crystal_colour            'Dark Violet'
_exptl_crystal_density_diffrn    2.777
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0338
_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)+(0.0390P)²+3.5280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0909
_reflns_number_gt                873
_reflns_number_total             928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402186p_si_002.cif
_cod_data_source_block           twin_hklf5
_cod_original_cell_volume        440.04(6)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4336655
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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.0000 0.21032(3) 0.5000 0.0099(2) Uani 1 2 d S
O1 O 0.2402(4) 0.30017(11) 0.7113(5) 0.0100(5) Uani 1 1 d .
O2 O 0.2057(4) 0.13417(13) 0.8433(5) 0.0130(5) Uani 1 1 d .
C1 C 0.2132(5) 0.35980(18) 0.8543(8) 0.0089(7) Uani 1 1 d .
C2 C 0.0910(5) 0.42998(16) 0.6603(7) 0.0094(6) Uani 1 1 d .
C3 C 0.1755(8) 0.5000 0.8138(11) 0.0115(10) Uani 1 2 d S
H3 H 0.2937 0.5000 1.0284 0.014 Uiso 1 2 calc SR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0098(3) 0.0074(3) 0.0094(3) 0.000 0.0014(2) 0.000
O1 0.0109(10) 0.0072(10) 0.0111(11) -0.0005(8) 0.0040(9) -0.0006(8)
O2 0.0159(12) 0.0119(11) 0.0077(13) 0.0017(9) 0.0019(10) 0.0040(9)
C1 0.0061(13) 0.0083(14) 0.0112(18) -0.0012(12) 0.0026(13) -0.0008(11)
C2 0.0106(15) 0.0070(14) 0.0090(15) 0.0009(12) 0.0029(13) 0.0000(11)
C3 0.010(2) 0.011(2) 0.009(2) 0.000 -0.0008(17) 0.000
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Co1 O2 97.78(13) 2_556 .
O2 Co1 O1 158.78(9) 2_556 .
O2 Co1 O1 93.39(8) . .
O2 Co1 O1 93.39(8) 2_556 2_556
O2 Co1 O1 158.78(9) . 2_556
O1 Co1 O1 82.15(12) . 2_556
O2 Co1 O1 87.40(9) 2_556 8_455
O2 Co1 O1 86.32(8) . 8_455
O1 Co1 O1 111.36(8) . 8_455
O1 Co1 O1 76.19(9) 2_556 8_455
O2 Co1 O1 86.32(8) 2_556 7_556
O2 Co1 O1 87.40(9) . 7_556
O1 Co1 O1 76.19(9) . 7_556
O1 Co1 O1 111.36(8) 2_556 7_556
O1 Co1 O1 170.45(10) 8_455 7_556
C1 O1 Co1 128.8(2) . .
C1 O1 Co1 124.81(19) . 7_556
Co1 O1 Co1 103.81(9) . 7_556
O2 C1 O1 123.6(3) 7_557 .
O2 C1 C2 115.9(3) 7_557 .
O1 C1 C2 120.5(3) . .
C3 C2 C2 118.5(2) . 2_556
C3 C2 C1 116.0(3) . .
C2 C2 C1 125.42(16) 2_556 .
C2 C3 C2 122.9(4) . 6_565
C1 O2 Co1 127.8(2) 7_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.023(2) 2_556
Co1 O2 2.023(2) .
Co1 O1 2.082(2) .
Co1 O1 2.082(2) 2_556
Co1 O1 2.201(2) 8_455
Co1 O1 2.201(2) 7_556
O1 C1 1.277(4) .
O1 Co1 2.201(2) 7_556
O2 C1 1.248(4) 7_557
C1 O2 1.248(4) 7_557
C1 C2 1.506(4) .
C2 C3 1.392(3) .
C2 C2 1.401(6) 2_556
C3 C2 1.392(3) 6_565
