#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/08/2230865.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2230865
loop_
_publ_author_name
'Xu, Wei'
_publ_section_title
;
 catena-Poly[bis[(1,10-phenanthroline)cobalt(II)]-μ₄-3,6-dicarboxycyclohexane-1,2,4,5-tetracarboxylato]
;
_journal_coeditor_code           SJ5153
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m832
_journal_page_last               m833
_journal_paper_doi               10.1107/S1600536811019970
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co2 (C12 H8 O12) (C12 H8 N2)2]'
_chemical_formula_moiety         'C36 H24 Co2 N4 O12'
_chemical_formula_sum            'C36 H24 Co2 N4 O12'
_chemical_formula_weight         822.46
_chemical_name_systematic
;
catena-Poly[bis[(1,10-phenanthroline)cobalt(II)]-μ₄-3,6-
dicarboxycyclohexane-1,2,4,5-tetracarboxylato]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 93.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.180(4)
_cell_length_b                   8.9520(18)
_cell_length_c                   16.426(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.0
_cell_volume                     3256.0(11)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       θ/2θ
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4566
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.331
_refine_ls_extinction_coef       0.00077(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0308
_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)+(0.0413P)²+2.2781P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                3312
_reflns_number_total             3753
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj5153.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2230865
_cod_database_fobs_code          2230865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.098444(9) 0.64743(2) 0.140367(13) 0.02138(9) Uani d . 1 1 . .
O O1 0.07208(6) 0.79951(15) 0.23735(7) 0.0330(3) Uani d . 1 1 . .
O O2 0.04781(7) 0.83776(14) 0.10892(7) 0.0327(3) Uani d . 1 1 . .
O O3 0.08305(7) 1.16900(18) 0.04746(9) 0.0433(4) Uani d . 1 1 . .
O O4 -0.01738(6) 1.14637(17) 0.04776(8) 0.0363(3) Uani d . 1 1 . .
H H4A -0.0159(12) 1.148(3) -0.0004(19) 0.054 Uiso d . 1 1 . .
O O5 0.09100(5) 1.45307(15) 0.21296(8) 0.0314(3) Uani d . 1 1 . .
O O6 0.01745(5) 1.51543(15) 0.12579(8) 0.0329(3) Uani d . 1 1 . .
N N1 0.13438(6) 0.55177(17) 0.03690(9) 0.0277(3) Uani d . 1 1 . .
N N2 0.18993(7) 0.70526(19) 0.16045(9) 0.0322(3) Uani d . 1 1 . .
C C1 0.10617(9) 0.4793(2) -0.02411(11) 0.0378(4) Uani d . 1 1 . .
H H1A 0.0642 0.4771 -0.0272 0.045 Uiso calc R 1 1 . .
C C2 0.13708(13) 0.4053(3) -0.08457(14) 0.0544(6) Uani d . 1 1 . .
H H2A 0.1159 0.3563 -0.1272 0.065 Uiso calc R 1 1 . .
C C3 0.19861(13) 0.4065(3) -0.07970(15) 0.0591(7) Uani d . 1 1 . .
H H3A 0.2196 0.3561 -0.1186 0.071 Uiso calc R 1 1 . .
C C4 0.23052(10) 0.4833(3) -0.01624(14) 0.0472(5) Uani d . 1 1 . .
C C5 0.29531(12) 0.4955(4) -0.00706(19) 0.0673(8) Uani d . 1 1 . .
H H5A 0.3186 0.4468 -0.0441 0.081 Uiso calc R 1 1 . .
C C6 0.32300(10) 0.5748(4) 0.05321(19) 0.0686(9) Uani d . 1 1 . .
H H6A 0.3649 0.5806 0.0569 0.082 Uiso calc R 1 1 . .
C C7 0.28897(9) 0.6512(3) 0.11216(16) 0.0517(6) Uani d . 1 1 . .
C C8 0.31442(11) 0.7393(4) 0.17623(18) 0.0660(8) Uani d . 1 1 . .
H H8A 0.3561 0.7516 0.1821 0.079 Uiso calc R 1 1 . .
C C9 0.27855(12) 0.8067(4) 0.22961(17) 0.0658(8) Uani d . 1 1 . .
H H9A 0.2954 0.8650 0.2719 0.079 Uiso calc R 1 1 . .
C C10 0.21599(11) 0.7875(3) 0.22011(14) 0.0487(5) Uani d . 1 1 . .
H H10A 0.1917 0.8338 0.2568 0.058 Uiso calc R 1 1 . .
C C11 0.22540(8) 0.6391(2) 0.10648(12) 0.0339(4) Uani d . 1 1 . .
C C12 0.19595(8) 0.5557(2) 0.04106(11) 0.0318(4) Uani d . 1 1 . .
C C13 0.00497(7) 1.00717(17) 0.20407(9) 0.0213(3) Uani d . 1 1 . .
H H13A -0.0344 0.9985 0.1741 0.026 Uiso calc R 1 1 . .
C C14 0.03623(7) 1.15052(16) 0.17600(9) 0.0205(3) Uani d . 1 1 . .
H H14A 0.0778 1.1519 0.1998 0.025 Uiso calc R 1 1 . .
C C15 0.00349(7) 1.29201(17) 0.20377(9) 0.0194(3) Uani d . 1 1 . .
H H15A -0.0367 1.2958 0.1758 0.023 Uiso calc R 1 1 . .
C C16 0.04335(8) 0.87293(17) 0.18323(10) 0.0234(3) Uani d . 1 1 . .
C C17 0.03790(8) 1.15477(18) 0.08330(10) 0.0256(3) Uani d . 1 1 . .
C C18 0.03920(7) 1.42928(17) 0.17948(9) 0.0209(3) Uani d . 1 1 . .
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Co1 N1 . . 110.87(6) ?
O2 Co1 N2 . . 109.77(6) ?
N1 Co1 N2 . . 79.58(6) ?
O2 Co1 O5 . 1_545 138.57(6) ?
N1 Co1 O5 . 1_545 99.55(6) ?
N2 Co1 O5 . 1_545 102.70(6) ?
O2 Co1 O6 . 1_545 89.26(5) ?
N1 Co1 O6 . 1_545 92.27(6) ?
N2 Co1 O6 . 1_545 160.89(6) ?
O5 Co1 O6 1_545 1_545 61.34(5) ?
O2 Co1 O1 . . 60.84(5) ?
N1 Co1 O1 . . 165.26(6) ?
N2 Co1 O1 . . 91.64(6) ?
O5 Co1 O1 1_545 . 93.89(5) ?
O6 Co1 O1 1_545 . 99.50(6) ?
O2 Co1 C18 . 1_545 115.12(6) ?
N1 Co1 C18 . 1_545 96.96(6) ?
N2 Co1 C18 . 1_545 132.85(6) ?
O5 Co1 C18 1_545 1_545 30.88(5) ?
O6 Co1 C18 1_545 1_545 30.46(5) ?
O1 Co1 C18 . 1_545 97.68(5) ?
O2 Co1 C16 . . 30.74(5) ?
N1 Co1 C16 . . 140.98(6) ?
N2 Co1 C16 . . 104.00(6) ?
O5 Co1 C16 1_545 . 116.86(6) ?
O6 Co1 C16 1_545 . 93.24(6) ?
O1 Co1 C16 . . 30.20(5) ?
C18 Co1 C16 1_545 . 106.99(5) ?
C16 O1 Co1 . . 87.50(10) ?
C16 O2 Co1 . . 92.02(10) ?
C17 O4 H4A . . 110(2) ?
C18 O5 Co1 . 1_565 89.55(10) ?
C18 O6 Co1 . 1_565 88.55(10) ?
C1 N1 C12 . . 118.65(16) ?
C1 N1 Co1 . . 128.96(13) ?
C12 N1 Co1 . . 112.02(12) ?
C10 N2 C11 . . 118.66(18) ?
C10 N2 Co1 . . 128.76(15) ?
C11 N2 Co1 . . 112.44(12) ?
N1 C1 C2 . . 122.6(2) ?
N1 C1 H1A . . 118.7 ?
C2 C1 H1A . . 118.7 ?
C3 C2 C1 . . 118.9(2) ?
C3 C2 H2A . . 120.6 ?
C1 C2 H2A . . 120.6 ?
C2 C3 C4 . . 120.5(2) ?
C2 C3 H3A . . 119.8 ?
C4 C3 H3A . . 119.8 ?
C3 C4 C12 . . 116.8(2) ?
C3 C4 C5 . . 124.8(2) ?
C12 C4 C5 . . 118.3(2) ?
C6 C5 C4 . . 122.0(2) ?
C6 C5 H5A . . 119.0 ?
C4 C5 H5A . . 119.0 ?
C5 C6 C7 . . 121.0(2) ?
C5 C6 H6A . . 119.5 ?
C7 C6 H6A . . 119.5 ?
C8 C7 C11 . . 116.6(2) ?
C8 C7 C6 . . 124.6(2) ?
C11 C7 C6 . . 118.8(2) ?
C9 C8 C7 . . 120.5(2) ?
C9 C8 H8A . . 119.8 ?
C7 C8 H8A . . 119.8 ?
C8 C9 C10 . . 119.2(2) ?
C8 C9 H9A . . 120.4 ?
C10 C9 H9A . . 120.4 ?
N2 C10 C9 . . 122.4(2) ?
N2 C10 H10A . . 118.8 ?
C9 C10 H10A . . 118.8 ?
N2 C11 C7 . . 122.6(2) ?
N2 C11 C12 . . 117.47(15) ?
C7 C11 C12 . . 119.9(2) ?
N1 C12 C4 . . 122.56(19) ?
N1 C12 C11 . . 117.50(16) ?
C4 C12 C11 . . 119.94(18) ?
C16 C13 C13 . 2 109.53(11) ?
C16 C13 C14 . . 108.82(12) ?
C13 C13 C14 2 . 112.70(10) ?
C16 C13 H13A . . 108.6 ?
C13 C13 H13A 2 . 108.6 ?
C14 C13 H13A . . 108.6 ?
C17 C14 C13 . . 110.89(13) ?
C17 C14 C15 . . 108.29(12) ?
C13 C14 C15 . . 111.56(12) ?
C17 C14 H14A . . 108.7 ?
C13 C14 H14A . . 108.7 ?
C15 C14 H14A . . 108.7 ?
C18 C15 C15 . 2 109.99(10) ?
C18 C15 C14 . . 108.86(12) ?
C15 C15 C14 2 . 111.64(10) ?
C18 C15 H15A . . 108.8 ?
C15 C15 H15A 2 . 108.8 ?
C14 C15 H15A . . 108.8 ?
O1 C16 O2 . . 119.22(15) ?
O1 C16 C13 . . 121.57(14) ?
O2 C16 C13 . . 119.17(14) ?
O1 C16 Co1 . . 62.30(9) ?
O2 C16 Co1 . . 57.23(8) ?
C13 C16 Co1 . . 174.86(12) ?
O3 C17 O4 . . 124.52(17) ?
O3 C17 C14 . . 124.24(17) ?
O4 C17 C14 . . 111.20(14) ?
O6 C18 O5 . . 120.56(15) ?
O6 C18 C15 . . 119.79(14) ?
O5 C18 C15 . . 119.64(14) ?
O6 C18 Co1 . 1_565 60.99(9) ?
O5 C18 Co1 . 1_565 59.57(8) ?
C15 C18 Co1 . 1_565 178.92(11) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O1 . 2.2002(13) y
Co1 O2 . 2.0890(13) y
Co1 O5 1_545 2.1211(13) y
Co1 O6 1_545 2.1519(13) y
Co1 N1 . 2.1012(15) y
Co1 N2 . 2.1016(15) y
Co1 C18 1_545 2.4599(16) ?
Co1 C16 . 2.4827(16) ?
O1 C16 . 1.250(2) ?
O2 C16 . 1.270(2) ?
O3 C17 . 1.198(2) ?
O4 C17 . 1.329(2) ?
O4 H4A . 0.79(3) ?
O5 C18 . 1.263(2) ?
O5 Co1 1_565 2.1211(13) ?
O6 C18 . 1.247(2) ?
O6 Co1 1_565 2.1519(13) ?
N1 C1 . 1.321(2) ?
N1 C12 . 1.364(2) ?
N2 C10 . 1.330(3) ?
N2 C11 . 1.355(3) ?
C1 C2 . 1.405(3) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.363(4) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.405(4) ?
C3 H3A . 0.9300 ?
C4 C12 . 1.406(3) ?
C4 C5 . 1.440(3) ?
C5 C6 . 1.338(5) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.435(4) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.407(4) ?
C7 C11 . 1.412(3) ?
C8 C9 . 1.359(4) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.398(3) ?
C9 H9A . 0.9300 ?
C10 H10A . 0.9300 ?
C11 C12 . 1.435(3) ?
C13 C16 . 1.523(2) ?
C13 C13 2 1.538(3) ?
C13 C14 . 1.542(2) ?
C13 H13A . 0.9800 ?
C14 C17 . 1.526(2) ?
C14 C15 . 1.542(2) ?
C14 H14A . 0.9800 ?
C15 C18 . 1.528(2) ?
C15 C15 2 1.535(3) ?
C15 H15A . 0.9800 ?
C18 Co1 1_565 2.4599(16) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O4 H4A O2 . . 5_575 0.79(3) 1.89(3) 2.627(2) 156(2) y
