#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:13:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180382 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/51/7205110.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_7205110
loop_
_publ_author_name
'He, Haiyan'
'Dou, Jianmin'
'Li, Dacheng'
'Ma, Huiqing'
'Sun, Daofeng'
_publ_section_title
;
 Synthesis, crystal structures and properties of four topological
 structures based on 2,3,5,6-tetramethyl-1,4-benzenedicarboxylate acid
 and bipyridine ligands
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1509
_journal_paper_doi               10.1039/c0ce00047g
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C22 H28 Co N2 O8'
_chemical_formula_weight         507.39
_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                 113.459(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.578(4)
_cell_length_b                   11.488(4)
_cell_length_c                   9.342(3)
_cell_measurement_reflns_used    1212
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.6
_cell_volume                     1139.9(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT+ (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2007)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3338
_diffrn_reflns_theta_full        27.4
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.9385
_exptl_absorpt_correction_T_min  0.8822
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0001(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0322
_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)+(0.0317P)²+1.0090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                1214
_reflns_number_total             1331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CE00047G.TXT
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7205110
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 0.5000 0.5000 0.5000 0.02072(17) Uani 1 4 d S . .
O1 O 0.30892(16) 0.5000 0.3351(2) 0.0287(4) Uani 1 2 d S . .
N1 N 0.5000 0.31112(18) 0.5000 0.0266(5) Uani 1 2 d S . .
C1 C 0.2694(2) 0.5000 0.1886(3) 0.0337(6) Uani 1 2 d S . .
H1 H 0.722(4) 0.5000 0.108(6) 0.081(16) Uiso 1 2 d S . .
O2 O 0.3382(2) 0.5000 0.1135(3) 0.0714(9) Uani 1 2 d S . .
C2 C 0.1276(2) 0.5000 0.0927(3) 0.0300(6) Uani 1 2 d S . .
H2 H 0.800(8) 0.5000 0.228(11) 0.22(5) Uiso 1 2 d S . .
O3 O 0.5669(2) 0.5000 0.3194(2) 0.0346(5) Uani 1 2 d S . .
C3 C 0.06479(17) 0.39358(17) 0.0469(2) 0.0306(4) Uani 1 1 d . . .
H3A H 0.498(3) 0.5000 0.233(4) 0.046(9) Uiso 1 2 d S . .
H3B H 0.627(3) 0.5000 0.298(4) 0.040(9) Uiso 1 2 d S . .
O4 O 0.7484(3) 0.5000 0.2005(4) 0.0606(8) Uani 1 2 d S . .
C4 C 0.1346(2) 0.2786(2) 0.0964(3) 0.0455(5) Uani 1 1 d . . .
H4A H 0.1383 0.2396 0.0050 0.068 Uiso 1 1 calc R . .
H4B H 0.0902 0.2287 0.1431 0.068 Uiso 1 1 calc R . .
H4C H 0.2203 0.2933 0.1731 0.068 Uiso 1 1 calc R . .
C5 C 0.57894(19) 0.24929(17) 0.4570(3) 0.0361(5) Uani 1 1 d . . .
H5 H 0.6365 0.2906 0.4265 0.043 Uiso 1 1 calc R . .
C6 C 0.5819(2) 0.12910(17) 0.4543(3) 0.0372(5) Uani 1 1 d . . .
H6 H 0.6395 0.0902 0.4213 0.045 Uiso 1 1 calc R . .
C7 C 0.5000 0.0650(2) 0.5000 0.0255(5) Uani 1 2 d S . .
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'
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'
H H 0.0000 0.0000 '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
O3 Co1 O3 180.0 . 5_666 ?
O3 Co1 O1 91.58(8) . . ?
O3 Co1 O1 88.42(8) 5_666 . ?
O3 Co1 O1 88.42(8) . 5_666 ?
O3 Co1 O1 91.58(8) 5_666 5_666 ?
O1 Co1 O1 180.0 . 5_666 ?
O3 Co1 N1 90.0 . . ?
O3 Co1 N1 90.0 5_666 . ?
O1 Co1 N1 90.0 . . ?
O1 Co1 N1 90.0 5_666 . ?
O3 Co1 N1 90.0 . 5_666 ?
O3 Co1 N1 90.0 5_666 5_666 ?
O1 Co1 N1 90.0 . 5_666 ?
O1 Co1 N1 90.0 5_666 5_666 ?
N1 Co1 N1 180.0 . 5_666 ?
C1 O1 Co1 127.51(17) . . ?
C5 N1 C5 115.9(2) . 2_656 ?
C5 N1 Co1 122.03(11) . . ?
C5 N1 Co1 122.03(11) 2_656 . ?
O2 C1 O1 124.9(2) . . ?
O2 C1 C2 116.5(2) . . ?
O1 C1 C2 118.6(2) . . ?
C3 C2 C3 121.7(2) 6_565 . ?
C3 C2 C1 119.10(12) 6_565 . ?
C3 C2 C1 119.10(12) . . ?
Co1 O3 H3A 104(2) . . ?
Co1 O3 H3B 147(2) . . ?
H3A O3 H3B 109(3) . . ?
C2 C3 C3 119.13(12) . 2 ?
C2 C3 C4 121.13(17) . . ?
C3 C3 C4 119.74(11) 2 . ?
H1 O4 H2 113(10) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 124.07(19) . . ?
N1 C5 H5 118.0 . . ?
C6 C5 H5 118.0 . . ?
C5 C6 C7 119.84(19) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C6 116.2(2) 2_656 . ?
C6 C7 C7 121.88(12) 2_656 5_656 ?
C6 C7 C7 121.88(12) . 5_656 ?
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 O3 2.118(2) . ?
Co1 O3 2.118(2) 5_666 ?
Co1 O1 2.1341(17) . ?
Co1 O1 2.1341(17) 5_666 ?
Co1 N1 2.170(2) . ?
Co1 N1 2.170(2) 5_666 ?
O1 C1 1.258(3) . ?
N1 C5 1.339(2) . ?
N1 C5 1.339(2) 2_656 ?
C1 O2 1.254(3) . ?
C1 C2 1.525(3) . ?
C2 C3 1.400(2) 6_565 ?
C2 C3 1.400(2) . ?
O3 H3A 0.88(4) . ?
O3 H3B 0.81(3) . ?
C3 C3 1.404(4) 2 ?
C3 C4 1.522(3) . ?
O4 H1 0.80(5) . ?
O4 H2 0.55(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.382(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(2) . ?
C6 H6 0.9500 . ?
C7 C6 1.395(2) 2_656 ?
C7 C7 1.492(5) 5_656 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Co1 O1 C1 180.0 5_666 . . . ?
O1 Co1 O1 C1 16.2(16) 5_666 . . . ?
N1 Co1 O1 C1 90.0 5_666 . . . ?
O3 Co1 N1 C5 28.01(13) . . . . ?
O3 Co1 N1 C5 -151.99(13) 5_666 . . . ?
O1 Co1 N1 C5 119.59(12) . . . . ?
O1 Co1 N1 C5 -60.41(12) 5_666 . . . ?
N1 Co1 N1 C5 180(100) 5_666 . . . ?
O3 Co1 N1 C5 -151.99(13) . . . 2_656 ?
O3 Co1 N1 C5 28.01(13) 5_666 . . 2_656 ?
O1 Co1 N1 C5 -60.41(12) . . . 2_656 ?
O1 Co1 N1 C5 119.59(12) 5_666 . . 2_656 ?
N1 Co1 N1 C5 0(23) 5_666 . . 2_656 ?
O2 C1 C2 C3 -88.5(2) . . . 6_565 ?
O1 C1 C2 C3 91.5(2) . . . 6_565 ?
O2 C1 C2 C3 88.5(2) . . . . ?
O1 C1 C2 C3 -91.5(2) . . . . ?
C3 C2 C3 C3 -0.3(4) 6_565 . . 2 ?
C1 C2 C3 C3 -177.4(2) . . . 2 ?
C3 C2 C3 C4 179.43(17) 6_565 . . . ?
C1 C2 C3 C4 2.4(3) . . . . ?
C5 N1 C5 C6 0.39(17) 2_656 . . . ?
Co1 N1 C5 C6 -179.61(17) . . . . ?
N1 C5 C6 C7 -0.8(3) . . . . ?
C5 C6 C7 C6 0.36(15) . . . 2_656 ?
C5 C6 C7 C7 -179.64(15) . . . 5_656 ?
