#------------------------------------------------------------------------------
#$Date: 2019-11-28 18:59:14 +0100 (jue 28 de nov de 2019) $
#$Revision: 244460 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/89/7238910.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_7238910
loop_
_publ_author_name
'Panja, Anangamohan'
_publ_section_title
;
 A series of tetrabromocatecholate chelated cobalt(iii) complexes with
 various N-donor ancillary ligands: syntheses, crystal structures,
 co-crystallization, thermally induced valence tautomerism and
 electrochemical studies
;
_journal_issue                   15
_journal_name_full               'RSC Advances'
_journal_page_first              4954
_journal_paper_doi               10.1039/c3ra22897e
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C18 H16 Br4 Cl Co N4 O6'
_chemical_formula_weight         798.37
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_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                 104.774(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.546(2)
_cell_length_b                   31.167(11)
_cell_length_c                   11.809(3)
_cell_measurement_reflns_used    8545
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.0
_cell_volume                     2329.6(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5192
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    7.757
_exptl_absorpt_correction_T_max  0.6532
_exptl_absorpt_correction_T_min  0.3060
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_colour            greenish-red
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.743
_refine_diff_density_min         -2.207
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0548
_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)+(0.1130P)²+0.7815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                2231
_reflns_number_total             2640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra22897e.txt
_cod_data_source_block           Complex4
_cod_original_cell_volume        2330(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7238910
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_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
Br2 Br 0.33850(9) -0.084366(17) 0.83782(5) 0.0331(2) Uani 1 1 d . . .
Br1 Br 0.17985(9) 0.008474(19) 0.92174(5) 0.0319(2) Uani 1 1 d . . .
Co1 Co 0.5000 0.12772(3) 0.7500 0.0236(3) Uani 1 2 d S . .
Cl1 Cl 1.0000 0.26055(6) 0.7500 0.0334(4) Uani 1 2 d S . .
O1 O 0.3722(6) 0.08414(10) 0.8182(3) 0.0231(7) Uani 1 1 d . . .
C8 C 0.7245(8) 0.16472(18) 0.9602(5) 0.0294(11) Uani 1 1 d . . .
N2 N 0.3706(7) 0.16908(15) 0.8351(4) 0.0309(10) Uani 1 1 d . . .
H2A H 0.2952 0.1889 0.7831 0.037 Uiso 1 1 calc R . .
H2B H 0.2775 0.1550 0.8687 0.037 Uiso 1 1 calc R . .
C6 C 1.0694(9) 0.14759(19) 1.0822(5) 0.0362(13) Uani 1 1 d . . .
H6 H 1.1836 0.1529 1.1486 0.043 Uiso 1 1 calc R . .
N1 N 0.7386(7) 0.13260(14) 0.8875(4) 0.0260(9) Uani 1 1 d . . .
C4 C 0.9108(8) 0.10798(18) 0.9085(5) 0.0326(11) Uani 1 1 d . . .
H4 H 0.9189 0.0854 0.8557 0.039 Uiso 1 1 calc R . .
O3 O 0.9549(16) 0.2300(3) 0.8265(8) 0.050(2) Uani 0.50 1 d P A 2
C5 C 1.0801(9) 0.1148(2) 1.0069(5) 0.0358(12) Uani 1 1 d . . .
H5 H 1.2011 0.0967 1.0212 0.043 Uiso 1 1 calc R . .
C7 C 0.8878(9) 0.17318(18) 1.0598(5) 0.0331(12) Uani 1 1 d . . .
H7 H 0.8758 0.1959 1.1114 0.040 Uiso 1 1 calc R . .
C1 C 0.4301(7) 0.04596(16) 0.7869(4) 0.0195(9) Uani 1 1 d . . .
C9 C 0.5286(9) 0.1917(2) 0.9271(6) 0.0406(14) Uani 1 1 d . . .
H9A H 0.4724 0.1964 0.9963 0.049 Uiso 1 1 calc R . .
H9B H 0.5615 0.2199 0.8978 0.049 Uiso 1 1 calc R . .
C2 C 0.3644(7) 0.00670(16) 0.8218(4) 0.0216(10) Uani 1 1 d . . .
C3 C 0.4330(7) -0.03219(16) 0.7862(4) 0.0241(10) Uani 1 1 d . . .
O4 O 1.154(2) 0.2547(4) 0.8692(9) 0.078(4) Uani 0.50 1 d P A 3
O2 O 0.795(2) 0.2545(4) 0.7673(15) 0.086(4) Uani 0.50 1 d P A 1
O5 O 1.022(2) 0.3033(3) 0.7147(8) 0.057(3) Uani 0.50 1 d P . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Br Br -0.2901 2.4595 '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'
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
O1 Co1 O1 87.5(2) . 2_656
O1 Co1 N1 93.64(17) . 2_656
O1 Co1 N1 92.81(16) 2_656 2_656
O1 Co1 N1 92.81(16) . .
O1 Co1 N1 93.64(17) 2_656 .
N1 Co1 N1 171.1(3) 2_656 .
O1 Co1 N2 173.99(18) . 2_656
O1 Co1 N2 87.59(18) 2_656 2_656
N1 Co1 N2 83.14(18) 2_656 2_656
N1 Co1 N2 90.96(18) . 2_656
O1 Co1 N2 87.59(18) . .
O1 Co1 N2 173.99(18) 2_656 .
N1 Co1 N2 90.96(18) 2_656 .
N1 Co1 N2 83.14(18) . .
N2 Co1 N2 97.5(3) 2_656 .
O3 Cl1 O3 93.8(9) . 2_756
O3 Cl1 O5 113.5(6) . 2_756
O3 Cl1 O5 152.7(6) 2_756 2_756
O3 Cl1 O5 152.7(6) . .
O3 Cl1 O5 113.5(6) 2_756 .
O5 Cl1 O5 39.2(9) 2_756 .
O3 Cl1 O2 56.8(8) . .
O3 Cl1 O2 111.4(6) 2_756 .
O5 Cl1 O2 85.0(7) 2_756 .
O5 Cl1 O2 109.8(8) . .
O3 Cl1 O2 111.4(6) . 2_756
O3 Cl1 O2 56.8(8) 2_756 2_756
O5 Cl1 O2 109.8(8) 2_756 2_756
O5 Cl1 O2 85.0(7) . 2_756
O2 Cl1 O2 164.6(10) . 2_756
O3 Cl1 O4 61.1(7) . .
O3 Cl1 O4 108.5(6) 2_756 .
O5 Cl1 O4 86.2(6) 2_756 .
O5 Cl1 O4 107.1(7) . .
O2 Cl1 O4 106.1(9) . .
O2 Cl1 O4 71.9(8) 2_756 .
O3 Cl1 O4 108.5(6) . 2_756
O3 Cl1 O4 61.1(7) 2_756 2_756
O5 Cl1 O4 107.1(7) 2_756 2_756
O5 Cl1 O4 86.2(6) . 2_756
O2 Cl1 O4 71.9(9) . 2_756
O2 Cl1 O4 106.1(9) 2_756 2_756
O4 Cl1 O4 166.1(10) . 2_756
C1 O1 Co1 109.8(3) . .
N1 C8 C7 121.2(5) . .
N1 C8 C9 116.5(5) . .
C7 C8 C9 122.3(5) . .
C9 N2 Co1 112.3(3) . .
C5 C6 C7 119.0(5) . .
C4 N1 C8 120.3(5) . .
C4 N1 Co1 124.7(4) . .
C8 N1 Co1 114.9(4) . .
N1 C4 C5 121.3(5) . .
C6 C5 C4 119.4(6) . .
C8 C7 C6 118.8(5) . .
O1 C1 C2 124.9(4) . .
O1 C1 C1 116.5(3) . 2_656
C2 C1 C1 118.6(3) . 2_656
N2 C9 C8 108.6(5) . .
C1 C2 C3 121.8(4) . .
C1 C2 Br1 116.9(3) . .
C3 C2 Br1 121.3(4) . .
C3 C3 C2 119.6(3) 2_656 .
C3 C3 Br2 120.89(16) 2_656 .
C2 C3 Br2 119.5(4) . .
O5 O5 Cl1 70.4(4) 2_756 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br2 C3 1.895(5) .
Br1 C2 1.893(5) .
Co1 O1 1.880(4) .
Co1 O1 1.880(4) 2_656
Co1 N1 1.951(4) 2_656
Co1 N1 1.951(4) .
Co1 N2 1.955(5) 2_656
Co1 N2 1.955(5) .
Cl1 O3 1.395(8) .
Cl1 O3 1.395(8) 2_756
Cl1 O5 1.413(9) 2_756
Cl1 O5 1.413(9) .
Cl1 O2 1.420(11) .
Cl1 O2 1.420(11) 2_756
Cl1 O4 1.518(10) .
Cl1 O4 1.518(10) 2_756
O1 C1 1.329(6) .
C8 N1 1.338(7) .
C8 C7 1.398(8) .
C8 C9 1.498(8) .
N2 C9 1.473(7) .
C6 C5 1.368(9) .
C6 C7 1.399(9) .
N1 C4 1.334(7) .
C4 C5 1.403(8) .
C1 C2 1.394(7) .
C1 C1 1.416(9) 2_656
C2 C3 1.394(7) .
C3 C3 1.372(10) 2_656
O5 O5 0.95(2) 2_756
