#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:35:21 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180344 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/13/7201304.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_7201304
loop_
_publ_author_name
'Fabelo, Oscar'
'Pasán, Jorge'
'Cañadillas-Delgado, Laura'
'Delgado, Fernando S.'
'Yuste, Consuelo'
'Lloret, Francesc'
'Julve, Miguel'
'Ruiz-Pérez, Catalina'
_publ_section_title
;
 Novel cobalt(II) coordination polymers based on
 1,2,4,5-benzenetetracarboxylic acid and extended bis-monodentate
 ligands
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2169
_journal_paper_doi               10.1039/b907895a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C15 H11 Co N2 O5'
_chemical_formula_weight         358.19
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.699(11)
_cell_angle_beta                 103.187(9)
_cell_angle_gamma                101.465(9)
_cell_formula_units_Z            2
_cell_length_a                   8.0891(12)
_cell_length_b                   9.4027(9)
_cell_length_c                   10.1213(11)
_cell_measurement_temperature    293(2)
_cell_volume                     642.21(16)
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6296
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         6.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0540
_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)+(0.0166P)²+0.4801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                2133
_reflns_number_total             2857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907895a.txt
_cod_data_source_block           Compound-1
_cod_original_cell_volume        642.21(13)
_cod_database_code               7201304
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.13295(6) 0.15190(6) 0.46433(5) 0.01587(14) Uani 1 1 d . . .
C1 C -0.1171(4) 0.4870(4) 0.8655(3) 0.0145(7) Uani 1 1 d . . .
C2 C -0.0318(4) 0.3695(4) 0.8521(3) 0.0153(7) Uani 1 1 d . . .
C3 C 0.0816(4) 0.3851(4) 0.9866(3) 0.0166(7) Uani 1 1 d . . .
C4 C -0.2544(4) 0.4791(4) 0.7313(4) 0.0178(7) Uani 1 1 d . . .
C5 C -0.0413(4) 0.2309(4) 0.7019(3) 0.0180(7) Uani 1 1 d . . .
C6 C -0.1029(5) 0.0476(5) 0.1382(4) 0.0269(8) Uani 1 1 d . . .
C7 C -0.2227(5) 0.0417(5) 0.0143(4) 0.0290(9) Uani 1 1 d . . .
C8 C -0.3057(4) 0.1610(4) 0.0381(4) 0.0186(7) Uani 1 1 d . . .
C9 C -0.2635(5) 0.2783(5) 0.1915(4) 0.0303(9) Uani 1 1 d . . .
C10 C -0.1439(5) 0.2743(5) 0.3101(4) 0.0303(9) Uani 1 1 d . . .
C11 C -0.6246(5) 0.2739(4) -0.2044(4) 0.0267(8) Uani 1 1 d . . .
C12 C -0.5076(5) 0.2829(4) -0.0765(4) 0.0266(8) Uani 1 1 d . . .
C13 C -0.4330(4) 0.1585(4) -0.0953(4) 0.0191(8) Uani 1 1 d . . .
C14 C -0.4848(5) 0.0305(4) -0.2455(4) 0.0240(8) Uani 1 1 d . . .
C15 C -0.6058(4) 0.0287(5) -0.3661(4) 0.0235(8) Uani 1 1 d . . .
N1 N -0.0609(3) 0.1610(4) 0.2859(3) 0.0191(6) Uani 1 1 d . . .
N2 N -0.6779(4) 0.1486(3) -0.3480(3) 0.0194(6) Uani 1 1 d . . .
O1 O -0.2879(3) 0.6106(3) 0.7543(3) 0.0339(6) Uani 1 1 d . . .
O2 O -0.3281(3) 0.3434(3) 0.6100(2) 0.0264(6) Uani 1 1 d . . .
O3 O 0.0201(3) 0.2708(3) 0.6139(2) 0.0229(5) Uani 1 1 d . . .
O4 O -0.0946(3) 0.0861(3) 0.6812(2) 0.0230(5) Uani 1 1 d . . .
O1W O 0.3356(4) 0.2966(3) 0.4549(3) 0.0330(7) Uani 1 1 d . . .
H1WA H 0.328(5) 0.330(5) 0.399(4) 0.033(12) Uiso 1 1 d . . .
H1WB H 0.445(6) 0.319(5) 0.506(4) 0.035(12) Uiso 1 1 d . . .
H3 H 0.1371 0.3054 0.9772 0.020 Uiso 1 1 calc R . .
H6 H -0.0471 -0.0328 0.1178 0.032 Uiso 1 1 calc R . .
H7 H -0.2482 -0.0425 -0.0858 0.035 Uiso 1 1 calc R . .
H9 H -0.3165 0.3607 0.2147 0.036 Uiso 1 1 calc R . .
H10 H -0.1199 0.3542 0.4117 0.036 Uiso 1 1 calc R . .
H11 H -0.6692 0.3612 -0.1893 0.032 Uiso 1 1 calc R . .
H12 H -0.4790 0.3719 0.0217 0.032 Uiso 1 1 calc R . .
H14 H -0.4370 -0.0553 -0.2649 0.029 Uiso 1 1 calc R . .
H15 H -0.6392 -0.0602 -0.4653 0.028 Uiso 1 1 calc R . .
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
C1 C2 C5 125.5(3) . . ?
C2 C1 C4 124.3(3) . . ?
C2 C3 C1 123.7(3) . 2_567 ?
C3 C1 C2 117.8(3) 2_567 . ?
C3 C1 C4 117.7(3) 2_567 . ?
C3 C2 C1 118.4(3) . . ?
C3 C2 C5 115.9(3) . . ?
C5 O3 Co1 129.5(2) . . ?
C5 O4 Co1 143.4(2) . 2_556 ?
C6 C7 C8 120.0(3) . . ?
C6 N1 C10 116.0(3) . . ?
C6 N1 Co1 119.0(2) . . ?
C7 C8 C13 120.7(3) . . ?
C7 C8 C9 115.8(3) . . ?
C9 C8 C13 123.5(3) . . ?
C10 C9 C8 120.8(3) . . ?
C10 N1 Co1 125.1(2) . . ?
C11 C12 C13 119.5(3) . . ?
C11 N2 C15 116.2(3) . . ?
C11 N2 Co1 119.5(2) . 1_454 ?
C12 C13 C8 122.1(3) . . ?
C14 C13 C12 116.1(3) . . ?
C14 C13 C8 121.8(3) . . ?
C15 C14 C13 120.7(3) . . ?
C15 N2 Co1 124.3(2) . 1_454 ?
N1 C10 C9 123.0(3) . . ?
N1 C6 C7 124.3(3) . . ?
N1 Co1 N2 177.21(11) . 1_656 ?
N2 C11 C12 124.3(3) . . ?
N2 C15 C14 123.2(3) . . ?
O1 C4 C1 116.5(3) . . ?
O2 C4 C1 117.8(3) . . ?
O2 C4 O1 125.7(3) . . ?
O3 C5 C2 117.3(3) . . ?
O3 Co1 N1 88.50(9) . . ?
O3 Co1 N2 88.72(9) . 1_656 ?
O3 Co1 O4 135.85(10) . 2_556 ?
O4 C5 C2 117.2(3) . . ?
O4 C5 O3 125.2(3) . . ?
O4 Co1 N1 90.35(10) 2_556 . ?
O4 Co1 N2 91.58(10) 2_556 1_656 ?
O1W Co1 N1 92.93(11) . . ?
O1W Co1 N2 88.32(12) . 1_656 ?
O1W Co1 O3 114.74(11) . . ?
O1W Co1 O4 109.40(11) . 2_556 ?
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 N1 2.149(3) . ?
Co1 N2 2.166(3) 1_656 ?
Co1 O1W 1.959(3) . ?
Co1 O3 1.999(2) . ?
Co1 O4 2.009(2) 2_556 ?
C1 C3 1.390(4) 2_567 ?
C1 C4 1.510(4) . ?
C2 C1 1.391(4) . ?
C2 C5 1.505(4) . ?
C3 C1 1.390(4) 2_567 ?
C3 C2 1.388(4) . ?
C4 O1 1.257(4) . ?
C4 O2 1.243(4) . ?
C6 C7 1.372(4) . ?
C7 C8 1.383(4) . ?
C9 C8 1.386(4) . ?
C10 C9 1.378(4) . ?
C11 C12 1.377(4) . ?
C12 C13 1.384(5) . ?
C13 C8 1.488(4) . ?
C14 C13 1.384(4) . ?
C15 C14 1.371(4) . ?
N1 C10 1.337(4) . ?
N1 C6 1.334(4) . ?
N2 C11 1.330(4) . ?
N2 C15 1.335(4) . ?
N2 Co1 2.166(3) 1_454 ?
O3 C5 1.261(4) . ?
O4 C5 1.253(4) . ?
O4 Co1 2.009(2) 2_556 ?
