#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:35:21 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180344 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/13/7201307.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_7201307
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            'C17 H25 Co N2 O10'
_chemical_formula_weight         476.32
_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                60.996(8)
_cell_angle_beta                 66.612(8)
_cell_angle_gamma                66.832(8)
_cell_formula_units_Z            2
_cell_length_a                   9.3705(10)
_cell_length_b                   11.4792(13)
_cell_length_c                   11.6886(9)
_cell_measurement_temperature    293(2)
_cell_volume                     977.13(19)
_computing_cell_refinement       'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19033
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.45
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.9120
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.023(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0723
_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)+(0.1377P)²+1.1229P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2283
_reflns_number_gt                3187
_reflns_number_total             4468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907895a.txt
_cod_data_source_block           Compound-4
_cod_original_cell_volume        977.13(17)
_cod_database_code               7201307
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 1.0000 0.0000 1.0000 0.0314(3) Uani 1 2 d S . .
Co2 Co 0.5000 0.5000 0.5000 0.0274(3) Uani 1 2 d S . .
C1 C 0.5998(5) 0.3778(4) 0.9856(4) 0.0248(8) Uani 1 1 d . . .
C2 C 0.5287(5) 0.4829(4) 0.8818(4) 0.0242(8) Uani 1 1 d . . .
C3 C 0.4292(5) 0.6036(4) 0.8980(4) 0.0264(9) Uani 1 1 d . . .
C4 C 0.6932(5) 0.2389(4) 0.9778(4) 0.0270(9) Uani 1 1 d . . .
C5 C 0.5786(5) 0.4729(4) 0.7453(4) 0.0264(9) Uani 1 1 d . . .
C6 C 1.2441(6) 0.0612(5) 0.7263(5) 0.0410(11) Uani 1 1 d . . .
C7 C 1.3075(6) 0.1110(5) 0.5875(5) 0.0395(11) Uani 1 1 d . . .
C8 C 1.2092(6) 0.1853(5) 0.5008(5) 0.0370(11) Uani 1 1 d . . .
C9 C 1.0457(6) 0.2144(5) 0.5616(5) 0.0403(11) Uani 1 1 d . . .
C10 C 0.9895(6) 0.1638(5) 0.7005(5) 0.0379(11) Uani 1 1 d . . .
C11 C 1.2716(7) 0.2250(5) 0.3519(5) 0.0453(12) Uani 1 1 d . . .
C12 C 1.2139(7) 0.1589(5) 0.2971(5) 0.0465(13) Uani 1 1 d . . .
C13 C 1.2792(6) 0.0053(5) 0.3440(5) 0.0387(11) Uani 1 1 d . . .
C14 C 1.2289(6) -0.0841(5) 0.4768(5) 0.0392(11) Uani 1 1 d . . .
C15 C 1.2955(6) -0.2233(5) 0.5151(5) 0.0364(10) Uani 1 1 d . . .
C16 C 1.4546(6) -0.1961(5) 0.3011(5) 0.0365(10) Uani 1 1 d . . .
C17 C 1.3951(6) -0.0554(5) 0.2551(5) 0.0384(11) Uani 1 1 d . . .
O1 O 0.8315(4) 0.1900(3) 0.9975(3) 0.0356(8) Uani 1 1 d . . .
O2 O 0.6252(4) 0.1809(3) 0.9556(4) 0.0407(8) Uani 1 1 d . . .
O3 O 0.4697(4) 0.4952(3) 0.6950(3) 0.0337(7) Uani 1 1 d . . .
O4 O 0.7259(4) 0.4469(4) 0.6916(3) 0.0386(8) Uani 1 1 d . . .
O1W O 1.1702(4) 0.0650(4) 1.0165(4) 0.0466(9) Uani 1 1 d . . .
O2W O 0.7369(4) 0.5155(4) 0.4382(3) 0.0435(9) Uani 1 1 d . . .
O3W O 0.9944(5) 0.4071(5) 0.7704(4) 0.0641(12) Uani 1 1 d . . .
O4W O 0.9483(10) 0.2108(9) 1.1685(9) 0.140(3) Uani 1 1 d . . .
O5W O 1.2795(15) 0.2872(14) 0.9540(11) 0.203(5) Uani 1 1 d . . .
O6W O 0.9070(16) 0.4659(9) 1.1346(11) 0.198(5) Uani 1 1 d . . .
N1 N 1.0861(4) 0.0857(4) 0.7834(4) 0.0348(9) Uani 1 1 d . . .
N2 N 1.4063(5) -0.2813(4) 0.4297(4) 0.0341(9) Uani 1 1 d . . .
H3 H 0.3811 0.6732 0.8295 0.032 Uiso 1 1 calc R . .
H6 H 1.3141 0.0086 0.7820 0.049 Uiso 1 1 calc R . .
H7 H 1.4183 0.0938 0.5524 0.047 Uiso 1 1 calc R . .
H9 H 0.9734 0.2685 0.5080 0.048 Uiso 1 1 calc R . .
H10 H 0.8793 0.1851 0.7382 0.045 Uiso 1 1 calc R . .
H11A H 1.3881 0.1985 0.3294 0.054 Uiso 1 1 calc R . .
H11B H 1.2381 0.3243 0.3074 0.054 Uiso 1 1 calc R . .
H12A H 1.0975 0.1798 0.3254 0.056 Uiso 1 1 calc R . .
H12B H 1.2456 0.1995 0.1990 0.056 Uiso 1 1 calc R . .
H14 H 1.1500 -0.0495 0.5396 0.047 Uiso 1 1 calc R . .
H15 H 1.2618 -0.2803 0.6050 0.044 Uiso 1 1 calc R . .
H16 H 1.5320 -0.2340 0.2401 0.044 Uiso 1 1 calc R . .
H17 H 1.4319 -0.0007 0.1649 0.046 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 0.0030 0.0020 '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 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 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 120.1(4) . . ?
C1 C3 C2 121.1(4) 2_667 . ?
C2 C1 C4 120.4(3) . . ?
C3 C1 C2 119.6(4) 2_667 . ?
C3 C1 C4 119.7(4) 2_667 . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 C5 120.0(3) . . ?
C4 O1 Co1 130.1(3) . . ?
C5 O3 Co2 127.0(3) . . ?
C6 N1 Co1 119.6(3) . . ?
C7 C8 C11 122.7(5) . . ?
C7 C8 C9 115.7(4) . . ?
C8 C11 C12 113.4(4) . . ?
C8 C7 C6 121.0(5) . . ?
C9 C8 C11 121.5(5) . . ?
C10 C9 C8 120.6(4) . . ?
C10 N1 C6 117.1(4) . . ?
C10 N1 Co1 123.4(3) . . ?
C13 C12 C11 113.6(4) . . ?
C14 C13 C12 122.5(5) . . ?
C14 C13 C17 116.3(5) . . ?
C15 C14 C13 120.1(5) . . ?
C15 N2 C16 116.9(4) . . ?
C15 N2 Co2 120.3(3) . 1_645 ?
C16 C17 C13 120.0(5) . . ?
C16 N2 Co2 122.8(3) . 1_645 ?
C17 C13 C12 121.2(5) . . ?
N1 C10 C9 122.9(4) . . ?
N1 C6 C7 122.5(4) . . ?
N1 Co1 N1 180.0 . 2_757 ?
N2 C15 C14 123.5(4) . . ?
N2 C16 C17 123.1(4) . . ?
N2 Co2 N2 180.000(1) 1_465 2_756 ?
N2 Co2 O3 89.11(13) 1_465 . ?
N2 Co2 O3 89.11(13) 2_756 2_666 ?
N2 Co2 O3 90.89(13) 1_465 2_666 ?
N2 Co2 O3 90.89(13) 2_756 . ?
O1 C4 C1 117.5(4) . . ?
O1 Co1 N1 88.93(13) . 2_757 ?
O1 Co1 N1 88.93(13) 2_757 . ?
O1 Co1 N1 91.07(13) . . ?
O1 Co1 N1 91.07(13) 2_757 2_757 ?
O1 Co1 O1 180.0(2) . 2_757 ?
O2 C4 C1 117.2(4) . . ?
O2 C4 O1 125.3(4) . . ?
O3 C5 C2 118.0(4) . . ?
O3 Co2 O3 180.00(18) . 2_666 ?
O4 C5 C2 116.2(4) . . ?
O4 C5 O3 125.8(4) . . ?
O1W Co1 N1 89.72(15) . . ?
O1W Co1 N1 89.72(15) 2_757 2_757 ?
O1W Co1 N1 90.28(15) . 2_757 ?
O1W Co1 N1 90.28(15) 2_757 . ?
O1W Co1 O1 89.20(13) . . ?
O1W Co1 O1 89.20(13) 2_757 2_757 ?
O1W Co1 O1 90.80(13) . 2_757 ?
O1W Co1 O1 90.80(13) 2_757 . ?
O1W Co1 O1W 180.00(17) 2_757 . ?
O2W Co2 N2 87.46(15) . 2_756 ?
O2W Co2 N2 87.46(15) 2_666 1_465 ?
O2W Co2 N2 92.54(15) . 1_465 ?
O2W Co2 N2 92.54(15) 2_666 2_756 ?
O2W Co2 O2W 180.0(2) . 2_666 ?
O2W Co2 O3 89.38(12) . 2_666 ?
O2W Co2 O3 89.38(12) 2_666 . ?
O2W Co2 O3 90.62(12) . . ?
O2W Co2 O3 90.62(12) 2_666 2_666 ?
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
O2W Co2 2.096(3) . ?
O1W Co1 2.112(4) . ?
Co2 O2W 2.096(3) 2_666 ?
Co2 N2 2.142(4) 1_465 ?
Co2 N2 2.142(4) 2_756 ?
Co2 O3 2.158(3) . ?
Co2 O3 2.158(3) 2_666 ?
Co1 O1W 2.112(4) 2_757 ?
Co1 O1 2.125(3) . ?
Co1 O1 2.125(3) 2_757 ?
Co1 N1 2.149(4) . ?
Co1 N1 2.149(4) 2_757 ?
O2 C4 1.245(5) . ?
O1 C4 1.260(5) . ?
O3 C5 1.256(5) . ?
O4 C5 1.249(5) . ?
N1 C10 1.333(6) . ?
N1 C6 1.336(6) . ?
C2 C3 1.387(6) . ?
C2 C1 1.401(5) . ?
C2 C5 1.523(5) . ?
C4 C1 1.515(6) . ?
N2 C15 1.340(6) . ?
N2 C16 1.343(6) . ?
N2 Co2 2.142(4) 1_645 ?
C3 C1 1.383(5) 2_667 ?
C1 C3 1.383(5) 2_667 ?
C14 C15 1.373(7) . ?
C14 C13 1.393(7) . ?
C13 C17 1.398(7) . ?
C13 C12 1.505(7) . ?
C17 C16 1.377(7) . ?
C9 C10 1.378(7) . ?
C9 C8 1.388(7) . ?
C6 C7 1.383(7) . ?
C7 C8 1.374(7) . ?
C8 C11 1.487(7) . ?
C12 C11 1.533(8) . ?
