#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:55:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179084 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/46/4304650.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_4304650
loop_
_publ_author_name
'Oscar Fabelo'
'Jorge Pasán'
'Francesc Lloret'
'Miguel Julve'
'Catalina Ruiz-Pérez'
_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_name        'Professor Catalina Ruiz-Pérez'
_publ_section_title
;
1,2,4,5-Benzenetetracarboxylate- and 2,2'-Bipyrimidine-Containing
Cobalt(II) Coordination Polymers: Preparation, Crystal Structure, and
Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3568
_journal_page_last               3576
_journal_paper_doi               10.1021/ic702187k
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C18 H12 Co2 N4 O10'
_chemical_formula_weight         562.18
_chemical_name_systematic
;
 ?
;
_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'
_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                 103.104(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.265(5)
_cell_length_b                   13.915(5)
_cell_length_c                   13.202(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1836.6(13)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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    0.0320
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2177
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         5.02
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.881
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0387
_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)+(0.0250P)²+3.1463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                1724
_reflns_number_total             2177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702187k-file004.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        1836.7(13)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4304650
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.16517(4) 0.20427(3) 0.29323(3) 0.01536(12) Uani 1 1 d . . .
C1 C 0.3718(5) 0.0000 0.5319(4) 0.0218(11) Uani 1 2 d S . .
C2 C 0.3295(3) 0.0846(2) 0.4812(3) 0.0200(7) Uani 1 1 d . . .
C3 C 0.2008(4) 0.0000 0.3479(3) 0.0153(9) Uani 1 2 d S . .
C4 C 0.0944(4) 0.0000 0.2508(4) 0.0151(9) Uani 1 2 d S . .
C5 C -0.0522(3) 0.0850(2) 0.1274(3) 0.0220(7) Uani 1 1 d . . .
C6 C -0.1061(5) 0.0000 0.0832(4) 0.0239(11) Uani 1 2 d S . .
C10 C 0.4139(3) 0.31947(19) 0.3960(2) 0.0126(6) Uani 1 1 d . . .
C11 C 0.4565(3) 0.4131(2) 0.4510(2) 0.0118(6) Uani 1 1 d . . .
C12 C 0.4116(4) 0.5000 0.4040(4) 0.0118(8) Uani 1 2 d S . .
C13 C 0.0862(3) 0.3208(2) 0.1032(3) 0.0182(7) Uani 1 1 d . . .
C14 C 0.0345(3) 0.4138(2) 0.0523(2) 0.0145(6) Uani 1 1 d . . .
C15 C 0.0665(4) 0.5000 0.1039(4) 0.0165(9) Uani 1 2 d S . .
N1 N 0.0486(3) 0.08494(18) 0.2126(2) 0.0165(6) Uani 1 1 d . . .
N2 N 0.2428(2) 0.08511(18) 0.3886(2) 0.0148(5) Uani 1 1 d . . .
O1 O 0.2909(2) 0.30195(16) 0.37841(18) 0.0215(5) Uani 1 1 d . . .
O2 O 0.0736(2) 0.30796(16) 0.19627(17) 0.0209(5) Uani 1 1 d . . .
O3 O 0.5016(2) 0.26673(13) 0.37326(17) 0.0184(4) Uani 1 1 d . . .
O4W O 0.2983(3) 0.16033(18) 0.1991(2) 0.0268(6) Uani 1 1 d . . .
O5 O 0.1411(3) 0.26530(18) 0.0540(2) 0.0458(7) Uani 1 1 d . . .
H6 H -0.182(5) 0.0000 0.017(4) 0.033(15) Uiso 1 2 d S . .
H2 H 0.359(3) 0.140(2) 0.511(2) 0.002(7) Uiso 1 1 d . . .
H15 H 0.111(5) 0.5000 0.175(4) 0.021(13) Uiso 1 2 d S . .
H12 H 0.356(5) 0.5000 0.344(4) 0.028(15) Uiso 1 2 d S . .
H5 H -0.085(3) 0.141(3) 0.103(3) 0.022(10) Uiso 1 1 d . . .
H1 H 0.437(5) 0.0000 0.607(4) 0.021(13) Uiso 1 2 d S . .
H1W H 0.269(5) 0.190(4) 0.146(4) 0.065(18) Uiso 1 1 d . . .
H2W H 0.379(5) 0.169(3) 0.211(3) 0.047(13) Uiso 1 1 d . . .
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'
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'
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
_geom_angle_publ_flag
O2 Co1 O1 91.09(9) . . ?
O2 Co1 N2 173.56(9) . . ?
O1 Co1 N2 95.07(10) . . ?
O2 Co1 O4W 95.93(10) . . ?
O1 Co1 O4W 95.96(10) . . ?
N2 Co1 O4W 85.30(11) . . ?
O2 Co1 N1 96.30(10) . . ?
O1 Co1 N1 172.35(9) . . ?
N2 Co1 N1 77.61(9) . . ?
O4W Co1 N1 81.38(10) . . ?
O2 Co1 O3 82.96(9) . 8_455 ?
O1 Co1 O3 93.98(9) . 8_455 ?
N2 Co1 O3 94.74(9) . 8_455 ?
O4W Co1 O3 170.02(9) . 8_455 ?
N1 Co1 O3 88.88(9) . 8_455 ?
C2 C1 C2 117.8(4) 6 . ?
N2 C2 C1 121.4(3) . . ?
N2 C3 N2 125.7(4) . 6 ?
N2 C3 C4 117.1(2) . . ?
N2 C3 C4 117.1(2) 6 . ?
N1 C4 N1 125.6(4) 6 . ?
N1 C4 C3 117.1(2) 6 . ?
N1 C4 C3 117.1(2) . . ?
N1 C5 C6 120.9(3) . . ?
C5 C6 C5 118.2(5) . 6 ?
O3 C10 O1 126.2(3) . . ?
O3 C10 C11 118.5(3) . . ?
O1 C10 C11 115.3(2) . . ?
C12 C11 C11 119.5(2) . 2_656 ?
C12 C11 C10 120.4(3) . . ?
C11 C11 C10 120.09(15) 2_656 . ?
C11 C12 C11 121.0(4) 6_565 . ?
O5 C13 O2 125.6(3) . . ?
O5 C13 C14 117.7(3) . . ?
O2 C13 C14 116.7(3) . . ?
C15 C14 C14 119.7(2) . 2 ?
C15 C14 C13 120.6(3) . . ?
C14 C14 C13 119.34(17) 2 . ?
C14 C15 C14 120.5(4) . 6_565 ?
C4 N1 C5 117.2(3) . . ?
C4 N1 Co1 112.6(2) . . ?
C5 N1 Co1 130.0(2) . . ?
C3 N2 C2 116.8(3) . . ?
C3 N2 Co1 114.3(2) . . ?
C2 N2 Co1 128.9(2) . . ?
C10 O1 Co1 136.0(2) . . ?
C13 O2 Co1 125.2(2) . . ?
C10 O3 Co1 132.30(18) . 8 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.015(2) . ?
Co1 O1 2.030(2) . ?
Co1 N2 2.125(3) . ?
Co1 O4W 2.135(2) . ?
Co1 N1 2.178(3) . ?
Co1 O3 2.215(2) 8_455 ?
C1 C2 1.375(4) 6 ?
C1 C2 1.375(4) . ?
C2 N2 1.339(4) . ?
C3 N2 1.331(3) . ?
C3 N2 1.331(3) 6 ?
C3 C4 1.483(6) . ?
C4 N1 1.329(3) 6 ?
C4 N1 1.329(3) . ?
C5 N1 1.344(4) . ?
C5 C6 1.377(4) . ?
C6 C5 1.377(4) 6 ?
C10 O3 1.249(3) . ?
C10 O1 1.255(4) . ?
C10 C11 1.508(4) . ?
C11 C12 1.389(4) . ?
C11 C11 1.394(6) 2_656 ?
C12 C11 1.389(4) 6_565 ?
C13 O5 1.226(4) . ?
C13 O2 1.277(4) . ?
C13 C14 1.498(4) . ?
C14 C15 1.382(4) . ?
C14 C14 1.403(6) 2 ?
C15 C14 1.382(4) 6_565 ?
O3 Co1 2.215(2) 8 ?
