#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:35:21 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180344 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/13/7201306.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_7201306
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            'C30 H24 Co N8 O10'
_chemical_formula_weight         715.50
_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                96.211(7)
_cell_angle_beta                 114.225(12)
_cell_angle_gamma                105.727(12)
_cell_formula_units_Z            1
_cell_length_a                   8.9901(14)
_cell_length_b                   9.5945(9)
_cell_length_c                   10.2763(12)
_cell_measurement_temperature    293(2)
_cell_volume                     753.4(2)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13601
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         6.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange-pink
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             367
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0433
_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)+(0.0378P)²+0.6423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                2883
_reflns_number_total             3409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907895a.txt
_cod_data_source_block           Compound-3
_cod_original_cell_volume        753.37(16)
_cod_database_code               7201306
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 0.0000 0.0000 0.0000 0.02000(13) Uani 1 2 d S . .
C1 C 0.4781(3) 0.3548(2) -0.0621(2) 0.0238(5) Uani 1 1 d . . .
C2 C 0.3394(3) 0.3848(2) -0.0523(2) 0.0231(4) Uani 1 1 d . . .
C3 C 0.3629(3) 0.5303(2) 0.0085(3) 0.0254(5) Uani 1 1 d . . .
C4 C 0.4675(3) 0.2037(2) -0.1295(3) 0.0279(5) Uani 1 1 d . . .
C5 C 0.1694(3) 0.2644(2) -0.0897(2) 0.0239(4) Uani 1 1 d . . .
C6 C 0.0517(4) 0.1327(3) 0.3067(3) 0.0340(6) Uani 1 1 d . . .
C7 C 0.0613(4) 0.2286(3) 0.4226(3) 0.0349(6) Uani 1 1 d . . .
C8 C 0.0339(3) 0.3609(3) 0.4003(3) 0.0292(5) Uani 1 1 d . . .
C9 C 0.0076(3) 0.3962(3) 0.2683(3) 0.0312(5) Uani 1 1 d . . .
C10 C 0.0056(3) 0.2951(3) 0.1610(3) 0.0305(5) Uani 1 1 d . . .
C11 C 0.6645(4) 0.1433(3) 0.4970(3) 0.0487(7) Uani 1 1 d . . .
C12 C 0.6255(5) 0.2561(4) 0.5545(3) 0.0532(8) Uani 1 1 d . . .
C13 C 0.5603(4) 0.3442(3) 0.4670(3) 0.0411(6) Uani 1 1 d . . .
C14 C 0.5366(4) 0.3172(3) 0.3240(3) 0.0481(7) Uani 1 1 d . . .
C15 C 0.5773(4) 0.2007(3) 0.2749(3) 0.0443(7) Uani 1 1 d . . .
H2 H 0.334(5) 0.023(5) -0.292(5) 0.089(13) Uiso 1 1 d . . .
H3 H 0.2700 0.5513 0.0135 0.030 Uiso 1 1 calc R . .
H6 H 0.0648 0.0415 0.3195 0.041 Uiso 1 1 calc R . .
H7 H 0.0855 0.2049 0.5128 0.042 Uiso 1 1 calc R . .
H9 H -0.0085 0.4856 0.2518 0.037 Uiso 1 1 calc R . .
H10 H -0.0098 0.3195 0.0723 0.037 Uiso 1 1 calc R . .
H11 H 0.7095 0.0840 0.5571 0.058 Uiso 1 1 calc R . .
H12 H 0.6432 0.2723 0.6514 0.064 Uiso 1 1 calc R . .
H14 H 0.4942 0.3763 0.2624 0.058 Uiso 1 1 calc R . .
H15 H 0.5595 0.1811 0.1780 0.053 Uiso 1 1 calc R . .
H1WA H 0.262(5) -0.076(4) 0.131(4) 0.057(11) Uiso 1 1 d . . .
H1WB H 0.141(5) -0.133(4) 0.171(4) 0.061(11) Uiso 1 1 d . . .
N1 N 0.0247(3) 0.1639(2) 0.1779(2) 0.0278(4) Uani 1 1 d . . .
N2 N 0.0366(3) 0.4546(2) 0.5198(2) 0.0350(5) Uani 1 1 d . . .
N3 N 0.6407(3) 0.1153(2) 0.3592(2) 0.0354(5) Uani 1 1 d . . .
N4 N 0.5235(4) 0.4600(3) 0.5388(3) 0.0505(6) Uani 1 1 d . . .
O1 O 0.5884(3) 0.1602(2) -0.0734(2) 0.0497(5) Uani 1 1 d . . .
O2 O 0.3261(2) 0.12853(19) -0.2502(2) 0.0390(4) Uani 1 1 d . . .
O3 O 0.1831(2) 0.15663(17) -0.03236(18) 0.0275(4) Uani 1 1 d . . .
O4 O 0.0319(2) 0.2853(2) -0.1647(2) 0.0394(4) Uani 1 1 d . . .
O1W O 0.1999(2) -0.05470(19) 0.1591(2) 0.0291(4) Uani 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
C1 C2 C5 123.26(19) . . ?
C2 C1 C4 123.91(19) . . ?
C2 C3 C1 121.6(2) . 2_665 ?
C3 C1 C2 119.54(19) 2_665 . ?
C3 C1 C4 116.55(19) 2_665 . ?
C3 C2 C1 118.9(2) . . ?
C3 C2 C5 117.51(19) . . ?
C5 O3 Co1 129.37(14) . . ?
C6 C7 C8 117.9(2) . . ?
C6 N1 C10 117.6(2) . . ?
C6 N1 Co1 120.13(15) . . ?
C7 C8 N2 116.7(2) . . ?
C8 C9 C10 118.1(2) . . ?
C9 C8 C7 119.6(2) . . ?
C9 C8 N2 123.8(2) . . ?
C10 N1 Co1 122.24(16) . . ?
C12 C13 C14 118.9(2) . . ?
C12 C13 N4 114.4(3) . . ?
C13 C12 C11 118.9(3) . . ?
C14 C13 N4 126.7(3) . . ?
C15 C14 C13 118.3(3) . . ?
C15 N3 C11 118.1(2) . . ?
N1 C10 C9 123.4(2) . . ?
N1 C6 C7 123.4(2) . . ?
N1 Co1 N1 180.00(10) . 2 ?
N2 N2 C8 112.7(3) 2_566 . ?
N3 C11 C12 122.8(3) . . ?
N3 C15 C14 123.0(3) . . ?
N4 N4 C13 112.1(3) 2_666 . ?
O1 C4 C1 120.0(2) . . ?
O1 C4 O2 124.1(2) . . ?
O2 C4 C1 115.8(2) . . ?
O3 C5 C2 115.27(19) . . ?
O3 Co1 N1 88.52(7) . 2 ?
O3 Co1 N1 88.52(7) 2 . ?
O3 Co1 N1 91.48(7) . . ?
O3 Co1 N1 91.48(7) 2 2 ?
O3 Co1 O1W 89.80(7) . 2 ?
O3 Co1 O1W 89.80(7) 2 . ?
O3 Co1 O1W 90.20(7) . . ?
O3 Co1 O1W 90.20(7) 2 2 ?
O3 Co1 O3 180.00(8) . 2 ?
O4 C5 C2 118.00(19) . . ?
O4 C5 O3 126.6(2) . . ?
O1W Co1 N1 88.06(7) . . ?
O1W Co1 N1 88.06(7) 2 2 ?
O1W Co1 N1 91.94(7) . 2 ?
O1W Co1 N1 91.94(7) 2 . ?
O1W Co1 O1W 180.00(15) 2 . ?
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 2.1725(18) . ?
Co1 N1 2.1725(18) 2 ?
Co1 O1W 2.1128(17) . ?
Co1 O1W 2.1128(17) 2 ?
Co1 O3 2.0727(15) . ?
Co1 O3 2.0727(15) 2 ?
C1 C3 1.389(3) 2_665 ?
C1 C4 1.498(3) . ?
C2 C1 1.393(3) . ?
C2 C5 1.512(3) . ?
C3 C1 1.389(3) 2_665 ?
C3 C2 1.388(3) . ?
C4 O1 1.213(3) . ?
C4 O2 1.300(3) . ?
C5 O3 1.254(3) . ?
C5 O4 1.244(3) . ?
C6 C7 1.382(3) . ?
C6 N1 1.328(3) . ?
C7 C8 1.382(3) . ?
C8 N2 1.429(3) . ?
C9 C8 1.375(3) . ?
C10 C9 1.378(3) . ?
C10 N1 1.335(3) . ?
C11 C12 1.371(4) . ?
C11 N3 1.327(4) . ?
C12 C13 1.366(4) . ?
C13 N4 1.453(3) . ?
C14 C13 1.380(4) . ?
C15 C14 1.374(4) . ?
C15 N3 1.323(4) . ?
N2 N2 1.234(4) 2_566 ?
N4 N4 1.198(5) 2_666 ?
