#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:52:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180360 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/29/7202927.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_7202927
loop_
_publ_author_name
'Fabelo, Oscar'
'Pasán, Jorge'
'Lloret, Francesc'
'Julve, Miguel'
'Ruiz-Pérez, Catalina'
_publ_section_title
;
 Structural versatility in cobalt(ii) complexes with
 1,2,4,5-benzenetetracarboxylic acid (H4bta) and
 4,4′-bipyridine-N,N′-dioxide (dpo)
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              815
_journal_paper_doi               10.1039/b706035c
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C20 H32 Co N2 O20'
_chemical_formula_weight         679.41
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                114.311(10)
_cell_angle_beta                 102.450(11)
_cell_angle_gamma                95.860(14)
_cell_formula_units_Z            2
_cell_length_a                   7.4425(11)
_cell_length_b                   14.654(2)
_cell_length_c                   14.796(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1402.6(4)
_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    CRYSTALMAKER
_computing_publication_material  'PARST97 (Nardelli, 1997)'
_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 0.834
_diffrn_measured_fraction_theta_max 0.934
_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    0.0451
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16419
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         4.52
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         16419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0315P)²+3.2072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                12532
_reflns_number_total             16419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B706035C.txt
_cod_data_source_block           compound1
_cod_database_code               7202927
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 0.5000 0.02973(18) Uani 1 2 d S . .
Co2 Co 0.5000 1.0000 0.0000 0.02908(18) Uani 1 2 d S . .
C1 C 0.7033(6) 0.3303(3) -0.1560(4) 0.0473(11) Uani 1 1 d . . .
C2 C 0.6978(5) 0.3298(3) -0.0004(4) 0.0452(10) Uani 1 1 d . . .
C3 C 0.7322(5) 0.4351(3) -0.1113(3) 0.0400(10) Uani 1 1 d . . .
C4 C 0.7280(5) 0.4347(3) 0.0464(3) 0.0416(10) Uani 1 1 d . . .
C5 C 0.7470(4) 0.4907(2) -0.0075(3) 0.0284(7) Uani 1 1 d . . .
C6 C 0.7843(4) 0.6040(2) 0.0417(3) 0.0273(8) Uani 1 1 d . . .
C7 C 0.8194(5) 0.6599(3) -0.0101(3) 0.0402(10) Uani 1 1 d . . .
C8 C 0.7871(5) 0.6595(3) 0.1444(3) 0.0397(9) Uani 1 1 d . . .
C9 C 0.8567(5) 0.7654(3) 0.0379(3) 0.0408(9) Uani 1 1 d . . .
C10 C 0.8241(5) 0.7646(3) 0.1904(3) 0.0405(9) Uani 1 1 d . . .
C11 C 0.4528(4) 0.3975(2) 0.4491(3) 0.0255(8) Uani 1 1 d . . .
C12 C 0.5010(4) 0.4499(2) 0.3953(3) 0.0220(7) Uani 1 1 d . . .
C13 C 0.4488(4) 0.4420(2) 0.5510(3) 0.0231(7) Uani 1 1 d . . .
C14 C 0.4957(4) 0.3796(3) 0.2839(3) 0.0334(8) Uani 1 1 d . . .
C15 C 0.3933(4) 0.3664(3) 0.5917(3) 0.0333(8) Uani 1 1 d . . .
C16 C 0.0210(4) 0.5878(2) 0.5848(3) 0.0260(8) Uani 1 1 d . . .
C17 C 0.0310(4) 0.5035(2) 0.4096(3) 0.0220(7) Uani 1 1 d . . .
C18 C 0.0531(4) 0.5950(2) 0.4996(3) 0.0222(7) Uani 1 1 d . . .
C19 C 0.0587(4) 0.4896(3) 0.3065(3) 0.0317(8) Uani 1 1 d . . .
C20 C 0.1090(4) 0.7048(3) 0.5158(3) 0.0352(9) Uani 1 1 d . . .
N1 N 0.8583(3) 0.8154(2) 0.1366(2) 0.0342(7) Uani 1 1 d . . .
N2 N 0.6896(4) 0.2788(2) -0.1002(3) 0.0394(8) Uani 1 1 d . . .
O1 O 0.8941(3) 0.91799(16) 0.1823(2) 0.0389(6) Uani 1 1 d . . .
O2 O 0.6700(4) 0.17823(18) -0.1433(2) 0.0588(8) Uani 1 1 d . . .
O3 O 0.5532(4) 0.4182(2) 0.2290(2) 0.0544(8) Uani 1 1 d . . .
O4 O 0.4402(3) 0.28763(18) 0.2499(2) 0.0532(7) Uani 1 1 d . . .
O5 O 0.3691(4) 0.27383(18) 0.5344(2) 0.0592(8) Uani 1 1 d . . .
O6 O 0.3679(4) 0.3990(2) 0.6801(2) 0.0557(7) Uani 1 1 d . . .
O7 O 0.1149(4) 0.7209(2) 0.4396(3) 0.0632(9) Uani 1 1 d . . .
O8 O 0.1501(4) 0.77436(18) 0.6041(2) 0.0546(7) Uani 1 1 d . . .
O9 O 0.0776(4) 0.5672(2) 0.2873(2) 0.0625(9) Uani 1 1 d . . .
O10 O 0.0609(3) 0.40617(19) 0.2419(2) 0.0504(7) Uani 1 1 d . . .
O1W O 0.9436(4) 0.0436(2) 0.3830(3) 0.0555(9) Uani 1 1 d . . .
O2W O 0.7582(4) -0.1183(2) 0.4214(2) 0.0426(7) Uani 1 1 d . . .
O3W O 1.1429(4) -0.1041(2) 0.4206(2) 0.0470(8) Uani 1 1 d . . .
O4W O 0.5908(4) 1.15679(16) 0.1073(2) 0.0494(7) Uani 1 1 d . . .
O5W O 0.2231(3) 0.99981(18) 0.0099(2) 0.0417(6) Uani 1 1 d . . .
O6W O 0.5601(4) 0.9616(2) 0.1199(2) 0.0491(8) Uani 1 1 d . . .
O10W O 0.4767(5) 0.1294(2) 0.3754(3) 0.0508(8) Uani 1 1 d . . .
O11W O 0.5646(4) 0.0661(3) 0.6481(3) 0.0433(7) Uani 1 1 d . . .
O12W O 0.9805(4) 0.1946(3) 0.1534(3) 0.0562(9) Uani 1 1 d . . .
O13W O 0.1802(5) 0.0625(2) 0.1980(3) 0.0497(8) Uani 1 1 d . . .
H1 H 0.701(5) 0.294(3) -0.220(3) 0.060(13) Uiso 1 1 d . . .
H1A H 0.415(4) 0.325(2) 0.412(3) 0.043(9) Uiso 1 1 d . . .
H1B H 0.033(4) 0.640(2) 0.638(3) 0.027(9) Uiso 1 1 d . . .
H2 H 0.687(4) 0.287(2) 0.034(3) 0.049(10) Uiso 1 1 d . . .
H2A H 0.583(5) 0.488(3) 0.259(4) 0.080(15) Uiso 1 1 d . . .
H2B H 0.096(7) 0.646(5) 0.357(5) 0.15(2) Uiso 1 1 d . . .
H3 H 0.745(4) 0.463(2) -0.151(3) 0.055(11) Uiso 1 1 d . . .
H4 H 0.733(5) 0.464(3) 0.115(3) 0.075(14) Uiso 1 1 d . . .
H7 H 0.829(4) 0.631(2) -0.071(3) 0.041(11) Uiso 1 1 d . . .
H8 H 0.758(4) 0.627(2) 0.181(3) 0.041(9) Uiso 1 1 d . . .
H9 H 0.891(4) 0.811(2) 0.009(3) 0.062(11) Uiso 1 1 d . . .
H10 H 0.827(4) 0.804(2) 0.262(3) 0.043(10) Uiso 1 1 d . . .
H11 H 0.918(4) 0.091(3) 0.384(3) 0.046(13) Uiso 1 1 d . . .
H12 H 0.917(7) 0.000(4) 0.315(5) 0.12(2) Uiso 1 1 d . . .
H21 H 0.654(5) -0.098(3) 0.404(3) 0.069(15) Uiso 1 1 d . . .
H22 H 0.738(5) -0.158(3) 0.438(3) 0.068(15) Uiso 1 1 d . . .
H31 H 1.153(5) -0.151(3) 0.432(3) 0.070(15) Uiso 1 1 d . . .
H32 H 1.245(4) -0.085(2) 0.406(3) 0.037(10) Uiso 1 1 d . . .
H41 H 0.6991 1.1649 0.1247 0.11(2) Uiso 1 1 d . . .
H42 H 0.4982 1.1914 0.1378 0.128(19) Uiso 1 1 d . . .
H51 H 0.1766 1.0549 0.0788 0.24(3) Uiso 1 1 d . . .
H52 H 0.1515 0.9350 -0.0361 0.079(14) Uiso 1 1 d . . .
H61 H 0.502(5) 0.914(3) 0.116(3) 0.063(15) Uiso 1 1 d . . .
H62 H 0.692(7) 0.952(3) 0.141(4) 0.121(19) Uiso 1 1 d . . .
H101 H 0.566(5) 0.152(3) 0.369(4) 0.072(17) Uiso 1 1 d . . .
H102 H 0.441(5) 0.163(3) 0.416(3) 0.045(15) Uiso 1 1 d . . .
H111 H 0.598(6) 0.094(4) 0.708(4) 0.08(2) Uiso 1 1 d . . .
H112 H 0.540(6) 0.005(4) 0.633(4) 0.094(19) Uiso 1 1 d . . .
H121 H 1.045(6) 0.167(3) 0.181(4) 0.08(2) Uiso 1 1 d . . .
H122 H 1.009(6) 0.250(4) 0.177(4) 0.10(2) Uiso 1 1 d . . .
H131 H 0.272(6) 0.080(3) 0.251(4) 0.081(19) Uiso 1 1 d . . .
H132 H 0.116(6) 0.016(4) 0.198(4) 0.11(2) 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'
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'
Co Co 0.3494 0.9721 '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
O3W Co1 O3W 180.00(18) 2_756 . ?
O3W Co1 O1W 89.90(12) 2_756 . ?
O3W Co1 O1W 90.10(12) . . ?
O3W Co1 O1W 90.10(12) 2_756 2_756 ?
O3W Co1 O1W 89.90(12) . 2_756 ?
O1W Co1 O1W 180.000(1) . 2_756 ?
O3W Co1 O2W 93.27(11) 2_756 . ?
O3W Co1 O2W 86.73(11) . . ?
O1W Co1 O2W 90.01(13) . . ?
O1W Co1 O2W 89.99(13) 2_756 . ?
O3W Co1 O2W 86.73(11) 2_756 2_756 ?
O3W Co1 O2W 93.27(11) . 2_756 ?
O1W Co1 O2W 89.99(13) . 2_756 ?
O1W Co1 O2W 90.01(13) 2_756 2_756 ?
O2W Co1 O2W 180.0 . 2_756 ?
O6W Co2 O6W 180.00(14) . 2_675 ?
O6W Co2 O5W 89.57(11) . . ?
O6W Co2 O5W 90.43(11) 2_675 . ?
O6W Co2 O5W 90.43(11) . 2_675 ?
O6W Co2 O5W 89.57(11) 2_675 2_675 ?
O5W Co2 O5W 180.00(16) . 2_675 ?
O6W Co2 O4W 89.51(11) . . ?
O6W Co2 O4W 90.49(11) 2_675 . ?
O5W Co2 O4W 91.74(10) . . ?
O5W Co2 O4W 88.26(10) 2_675 . ?
O6W Co2 O4W 90.49(11) . 2_675 ?
O6W Co2 O4W 89.51(11) 2_675 2_675 ?
O5W Co2 O4W 88.26(10) . 2_675 ?
O5W Co2 O4W 91.74(10) 2_675 2_675 ?
O4W Co2 O4W 180.00(8) . 2_675 ?
N2 C1 C3 120.8(4) . . ?
N2 C2 C4 120.5(4) . . ?
C1 C3 C5 121.1(4) . . ?
C2 C4 C5 121.6(4) . . ?
C4 C5 C3 116.1(3) . . ?
C4 C5 C6 122.6(3) . . ?
C3 C5 C6 121.2(3) . . ?
C7 C6 C8 116.5(3) . . ?
C7 C6 C5 122.4(3) . . ?
C8 C6 C5 121.1(3) . . ?
C6 C7 C9 121.3(4) . . ?
C10 C8 C6 121.0(3) . . ?
N1 C9 C7 120.0(4) . . ?
N1 C10 C8 120.1(4) . . ?
C13 C11 C12 125.7(3) . . ?
C11 C12 C13 117.4(3) . 2_666 ?
C11 C12 C14 113.6(3) . . ?
C13 C12 C14 129.0(3) 2_666 . ?
C11 C13 C12 117.0(3) . 2_666 ?
C11 C13 C15 114.9(3) . . ?
C12 C13 C15 128.1(3) 2_666 . ?
O4 C14 O3 121.2(3) . . ?
O4 C14 C12 119.2(3) . . ?
O3 C14 C12 119.7(3) . . ?
O5 C15 O6 122.0(3) . . ?
O5 C15 C13 118.1(3) . . ?
O6 C15 C13 119.9(3) . . ?
C18 C16 C17 125.3(3) . 2_566 ?
C16 C17 C18 116.5(3) 2_566 . ?
C16 C17 C19 114.5(3) 2_566 . ?
C18 C17 C19 129.0(3) . . ?
C16 C18 C17 118.2(3) . . ?
C16 C18 C20 113.9(3) . . ?
C17 C18 C20 127.9(3) . . ?
O10 C19 O9 119.7(3) . . ?
O10 C19 C17 120.7(3) . . ?
O9 C19 C17 119.6(3) . . ?
O8 C20 O7 122.4(3) . . ?
O8 C20 C18 118.3(3) . . ?
O7 C20 C18 119.3(3) . . ?
C9 N1 C10 121.0(3) . . ?
C9 N1 O1 119.4(3) . . ?
C10 N1 O1 119.6(3) . . ?
O2 N2 C2 120.1(3) . . ?
O2 N2 C1 120.1(3) . . ?
C2 N2 C1 119.8(3) . . ?
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 O3W 2.057(2) 2_756 ?
Co1 O3W 2.057(2) . ?
Co1 O1W 2.057(3) . ?
Co1 O1W 2.057(3) 2_756 ?
Co1 O2W 2.097(2) . ?
Co1 O2W 2.097(2) 2_756 ?
Co2 O6W 2.048(3) . ?
Co2 O6W 2.048(3) 2_675 ?
Co2 O5W 2.0972(19) . ?
Co2 O5W 2.0972(19) 2_675 ?
Co2 O4W 2.115(2) . ?
Co2 O4W 2.115(2) 2_675 ?
C1 N2 1.340(4) . ?
C1 C3 1.370(5) . ?
C2 N2 1.336(5) . ?
C2 C4 1.371(5) . ?
C3 C5 1.383(5) . ?
C4 C5 1.377(5) . ?
C5 C6 1.478(4) . ?
C6 C7 1.374(4) . ?
C6 C8 1.391(5) . ?
C7 C9 1.377(5) . ?
C8 C10 1.371(5) . ?
C9 N1 1.334(4) . ?
C10 N1 1.338(4) . ?
C11 C13 1.383(4) . ?
C11 C12 1.387(4) . ?
C12 C13 1.412(4) 2_666 ?
C12 C14 1.530(4) . ?
C13 C12 1.412(4) 2_666 ?
C13 C15 1.523(4) . ?
C14 O4 1.216(4) . ?
C14 O3 1.282(4) . ?
C15 O5 1.237(4) . ?
C15 O6 1.259(4) . ?
C16 C18 1.375(4) . ?
C16 C17 1.394(4) 2_566 ?
C17 C16 1.394(4) 2_566 ?
C17 C18 1.410(4) . ?
C17 C19 1.518(4) . ?
C18 C20 1.524(4) . ?
C19 O10 1.207(4) . ?
C19 O9 1.282(4) . ?
C20 O8 1.228(4) . ?
C20 O7 1.253(4) . ?
N1 O1 1.338(3) . ?
N2 O2 1.320(3) . ?
