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#$Date: 2024-11-01 04:55:46 +0200 (Fri, 01 Nov 2024) $
#$Revision: 295714 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023300.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_2023300
loop_
_publ_author_name
'Kumagai, Hitoshi'
'Kawata, Satoshi'
'Ogihara, Nobuhiro'
_publ_section_title
;
 Crystal structure of
 catena-poly[[diaquadiimidazolecobalt(II)]-μ2-2,3,5,6-tetrabromobenzene-1,4-dicarboxylato]
;
_journal_coeditor_code           JP2013
_journal_issue                   11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1217
_journal_page_last               1220
_journal_paper_doi               10.1107/S2056989024009915
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Co (C8 Br4 O4) (C3 H4 N2)2 (H2 O1)2]'
_chemical_formula_moiety         'C14 H12 Br4 Co N4 O6'
_chemical_formula_sum            'C14 H12 Br4 Co N4 O6'
_chemical_formula_weight         710.85
_chemical_name_systematic
catena-Poly[[diaquadiimidazolecobalt(II)]-μ₂-2,3,5,6-tetrabromobenzene-1,4-dicarboxylato]
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 121.853(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8050(7)
_cell_length_b                   12.2925(6)
_cell_length_c                   10.8938(5)
_cell_measurement_reflns_used    9142
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.31
_cell_volume                     2138.98(18)
_computing_cell_refinement
;
RAPID AUTO (Rigaku, 1995)
;
_computing_data_collection
;
RAPID AUTO (Rigaku, 1995)
;
_computing_data_reduction
;
RAPID AUTO (Rigaku, 1995)
;
_computing_molecular_graphics
;
CrystalStructure 4.3 (Rigaku, 2019)
;
_computing_publication_material
;
CrystalStructure 4.3 (Rigaku, 2019)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10419
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         3.315
_exptl_absorpt_coefficient_mu    8.313
_exptl_absorpt_correction_T_max  0.007
_exptl_absorpt_correction_T_min  0.004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Rigaku, 1995)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.207
_exptl_crystal_description       Block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.600
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.595
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0356P)²+0.8085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                2277
_reflns_number_total             2448
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jp2013.cif
_cod_data_source_block           I
_cod_original_cell_volume        2138.97(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2023300
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.082
_shelx_estimated_absorpt_t_max   0.082
loop_
_space_group_symop_operation_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br1 0.40878(2) 1.36557(2) 0.78290(2) 0.02796(9) Uani d 1 . .
Br Br2 0.30071(2) 1.49911(2) 0.46852(3) 0.03101(10) Uani d 1 . .
Co Co1 0.500000 1.000000 1.000000 0.01141(10) Uani d 1 . .
O O1 0.40770(8) 1.08127(12) 0.80246(14) 0.0157(3) Uani d 1 . .
O O2 0.31711(10) 1.14631(14) 0.85848(17) 0.0282(4) Uani d 1 . .
O O3 0.41853(11) 1.01046(14) 1.0767(2) 0.0236(4) Uani d 1 . .
N N1 0.44446(11) 0.85236(14) 0.90200(19) 0.0179(3) Uani d 1 . .
N N2 0.34569(13) 0.73172(17) 0.7762(2) 0.0275(4) Uani d 1 . .
C C1 0.34466(12) 1.13493(16) 0.7774(2) 0.0159(4) Uani d 1 . .
C C2 0.29633(12) 1.19335(16) 0.6314(2) 0.0153(4) Uani d 1 . .
C C3 0.31735(12) 1.29953(17) 0.6185(2) 0.0159(4) Uani d 1 . .
C C4 0.27151(13) 1.35524(16) 0.4882(2) 0.0167(4) Uani d 1 . .
C C5 0.47955(14) 0.76163(19) 0.8814(3) 0.0254(5) Uani d 1 . .
H H5 0.537318 0.752777 0.915853 0.030 Uiso calc 1 . .
C C6 0.41879(16) 0.6861(2) 0.8039(3) 0.0329(6) Uani d 1 . .
H H6 0.425979 0.616103 0.775114 0.039 Uiso calc 1 . .
C C7 0.36370(14) 0.8307(2) 0.8368(2) 0.0257(5) Uani d 1 . .
H H7 0.323364 0.879232 0.833300 0.031 Uiso calc 1 . .
H H1 0.2999(19) 0.706(2) 0.733(3) 0.036(8) Uiso d 1 . .
H H2 0.383(2) 1.050(3) 1.028(3) 0.032(8) Uiso d 1 . .
H H3 0.418(2) 0.987(2) 1.139(4) 0.040(9) Uiso d 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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Co1 N1 5_677 . 180.00(11) yes
N1 Co1 O3 5_677 5_677 89.06(7) yes
N1 Co1 O3 . 5_677 90.94(7) yes
N1 Co1 O3 5_677 . 90.94(7) yes
N1 Co1 O3 . . 89.06(7) yes
O3 Co1 O3 5_677 . 180.00(4) yes
N1 Co1 O1 5_677 5_677 88.31(6) yes
N1 Co1 O1 . 5_677 91.69(6) yes
O3 Co1 O1 5_677 5_677 89.81(6) yes
O3 Co1 O1 . 5_677 90.19(6) yes
N1 Co1 O1 5_677 . 91.69(6) yes
N1 Co1 O1 . . 88.31(6) yes
O3 Co1 O1 5_677 . 90.19(6) yes
O3 Co1 O1 . . 89.81(6) yes
O1 Co1 O1 5_677 . 180.0 yes
C1 O1 Co1 . . 128.92(12) ?
Co1 O3 H2 . . 109(2) ?
Co1 O3 H3 . . 135(3) ?
H2 O3 H3 . . 117(3) ?
C7 N1 C5 . . 105.28(19) ?
C7 N1 Co1 . . 125.05(15) ?
C5 N1 Co1 . . 129.53(14) ?
C7 N2 C6 . . 107.5(2) ?
C7 N2 H1 . . 124(2) ?
C6 N2 H1 . . 128(2) ?
O2 C1 O1 . . 127.11(18) ?
O2 C1 C2 . . 116.28(17) ?
O1 C1 C2 . . 116.61(16) ?
C4 C2 C3 7_576 . 118.53(18) ?
C4 C2 C1 7_576 . 121.38(18) ?
C3 C2 C1 . . 120.00(17) ?
C4 C3 C2 . . 120.56(18) ?
C4 C3 Br1 . . 121.29(15) ?
C2 C3 Br1 . . 118.15(14) ?
C2 C4 C3 7_576 . 120.90(18) ?
C2 C4 Br2 7_576 . 118.19(15) ?
C3 C4 Br2 . . 120.90(15) ?
C6 C5 N1 . . 109.6(2) ?
C6 C5 H5 . . 125.2 ?
N1 C5 H5 . . 125.2 ?
N2 C6 C5 . . 106.0(2) ?
N2 C6 H6 . . 127.0 ?
C5 C6 H6 . . 127.0 ?
N1 C7 N2 . . 111.6(2) ?
N1 C7 H7 . . 124.2 ?
N2 C7 H7 . . 124.2 ?
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
Br1 C3 . 1.890(2) ?
Br2 C4 . 1.897(2) ?
Co1 N1 5_677 2.0850(18) yes
Co1 N1 . 2.0850(18) yes
Co1 O3 5_677 2.1006(16) yes
Co1 O3 . 2.1007(16) yes
Co1 O1 5_677 2.1678(13) yes
Co1 O1 . 2.1678(13) yes
O1 C1 . 1.254(2) ?
O2 C1 . 1.246(2) ?
O3 H2 . 0.76(3) ?
O3 H3 . 0.75(4) ?
N1 C7 . 1.320(3) ?
N1 C5 . 1.373(3) ?
N2 C7 . 1.340(3) ?
N2 C6 . 1.363(3) ?
N2 H1 . 0.80(3) ?
C1 C2 . 1.531(3) ?
C2 C4 7_576 1.388(3) ?
C2 C3 . 1.392(3) ?
C3 C4 . 1.392(3) ?
C5 C6 . 1.364(3) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 H7 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_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
C6 H6 Br1 1_545 0.95 3.10 3.946(3) 148.8 no
N2 H1 O2 4_546 0.80(3) 2.01(3) 2.808(2) 174(3) yes
O3 H2 O2 . 0.76(3) 1.99(3) 2.700(2) 155(3) yes
O3 H3 O1 6_576 0.75(4) 2.06(4) 2.809(2) 176(4) yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Co1 O1 C1 O2 . . . . -6.2(3) ?
Co1 O1 C1 C2 . . . . 173.49(12) ?
O2 C1 C2 C4 . . . 7_576 -87.3(2) ?
O1 C1 C2 C4 . . . 7_576 93.0(2) ?
O2 C1 C2 C3 . . . . 89.4(2) ?
O1 C1 C2 C3 . . . . -90.4(2) ?
C4 C2 C3 C4 7_576 . . . -0.3(3) ?
C1 C2 C3 C4 . . . . -177.08(16) ?
C4 C2 C3 Br1 7_576 . . . 179.07(14) ?
C1 C2 C3 Br1 . . . . 2.3(2) ?
C2 C3 C4 C2 . . . 7_576 0.4(3) ?
Br1 C3 C4 C2 . . . 7_576 -179.05(15) ?
C2 C3 C4 Br2 . . . . -178.98(14) ?
Br1 C3 C4 Br2 . . . . 1.6(2) ?
C7 N1 C5 C6 . . . . -0.2(3) ?
Co1 N1 C5 C6 . . . . -176.08(16) ?
C7 N2 C6 C5 . . . . -0.4(3) ?
N1 C5 C6 N2 . . . . 0.4(3) ?
C5 N1 C7 N2 . . . . 0.0(3) ?
Co1 N1 C7 N2 . . . . 176.07(15) ?
C6 N2 C7 N1 . . . . 0.3(3) ?
