#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:13:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179472 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/69/4336978.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_4336978
loop_
_publ_author_name
'Pradip Ghosh'
'Subhas Samanta'
'Suman K Roy'
'Sucheta Joy'
'Tobias Krämer'
'John E. McGrady'
'Sreebrata Goswami'
_publ_section_title
;
 Redox Noninnocence in Coordinated 2-(Arylazo)pyridines: Steric Control of
 Ligand-Based Redox Processes in Cobalt Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14040
_journal_page_last               14049
_journal_paper_doi               10.1021/ic4018079
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C22 H14 Cl6 Co N6'
_chemical_formula_weight         634.02
_chemical_name_systematic
;
 ?
;
_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                90.000(5)
_cell_angle_beta                 105.227(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   13.346(5)
_cell_length_b                   13.800(5)
_cell_length_c                   14.367(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2553.1(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11960
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_F_000             1268.0
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0712P)²+0.3196P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                1843
_reflns_number_total             2343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4018079_si_002_3.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4336978
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
Co1 Co 0.0000 0.32213(4) 0.7500 0.0401(2) Uani 1 2 d S
Cl1 Cl -0.04777(6) 0.41551(6) 0.85985(6) 0.0550(3) Uani 1 1 d .
Cl3 Cl 0.07141(7) 0.18623(7) 0.37362(7) 0.0655(3) Uani 1 1 d .
Cl2 Cl 0.13184(7) 0.01013(7) 0.72127(6) 0.0627(3) Uani 1 1 d .
N1 N -0.12879(17) 0.24590(17) 0.67656(16) 0.0391(5) Uani 1 1 d .
C5 C -0.1183(2) 0.18108(19) 0.6104(2) 0.0385(6) Uani 1 1 d .
C1 C -0.2245(2) 0.2603(2) 0.6876(2) 0.0478(7) Uani 1 1 d .
H1 H -0.2335 0.3056 0.7326 0.057 Uiso 1 1 calc R
C4 C -0.2005(2) 0.1291(2) 0.5539(2) 0.0453(7) Uani 1 1 d .
H4 H -0.1901 0.0850 0.5084 0.054 Uiso 1 1 calc R
C3 C -0.2984(2) 0.1440(2) 0.5664(2) 0.0537(8) Uani 1 1 d .
H3 H -0.3555 0.1102 0.5296 0.064 Uiso 1 1 calc R
C2 C -0.3095(2) 0.2105(3) 0.6350(2) 0.0561(8) Uani 1 1 d .
H2 H -0.3744 0.2215 0.6454 0.067 Uiso 1 1 calc R
N2 N -0.01146(18) 0.16947(16) 0.61166(17) 0.0397(5) Uani 1 1 d .
N3 N 0.00388(18) 0.12155(19) 0.54360(18) 0.0477(6) Uani 1 1 d .
C8 C 0.2842(2) 0.0494(2) 0.6364(2) 0.0526(8) Uani 1 1 d .
H8 H 0.3283 0.0200 0.6899 0.063 Uiso 1 1 calc R
C6 C 0.1126(2) 0.1071(2) 0.5520(2) 0.0424(7) Uani 1 1 d .
C11 C 0.1531(2) 0.1347(2) 0.4764(2) 0.0465(7) Uani 1 1 d .
C7 C 0.1800(2) 0.0613(2) 0.6312(2) 0.0462(7) Uani 1 1 d .
C10 C 0.2570(3) 0.1238(2) 0.4808(3) 0.0540(8) Uani 1 1 d .
H10 H 0.2828 0.1446 0.4301 0.065 Uiso 1 1 calc R
C9 C 0.3220(2) 0.0817(2) 0.5612(3) 0.0560(8) Uani 1 1 d .
H9 H 0.3923 0.0749 0.5649 0.067 Uiso 1 1 calc R
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'
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'
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
N1 Co1 N1 118.41(13) . 2_556
N1 Co1 Cl1 106.58(7) . 2_556
N1 Co1 Cl1 107.45(7) 2_556 2_556
N1 Co1 Cl1 107.45(7) . .
N1 Co1 Cl1 106.58(7) 2_556 .
Cl1 Co1 Cl1 110.30(6) 2_556 .
C5 N1 C1 117.6(2) . .
C5 N1 Co1 118.49(19) . .
C1 N1 Co1 123.9(2) . .
N1 C5 C4 123.3(3) . .
N1 C5 N2 110.8(2) . .
C4 C5 N2 125.8(3) . .
N1 C1 C2 122.4(3) . .
C3 C4 C5 118.6(3) . .
C4 C3 C2 118.3(3) . .
C1 C2 C3 119.9(3) . .
N3 N2 C5 114.8(2) . .
N2 N3 C6 112.3(2) . .
C9 C8 C7 119.2(3) . .
C11 C6 C7 117.4(3) . .
C11 C6 N3 119.3(3) . .
C7 C6 N3 123.2(3) . .
C10 C11 C6 121.8(3) . .
C10 C11 Cl3 118.8(2) . .
C6 C11 Cl3 119.3(2) . .
C8 C7 C6 121.3(3) . .
C8 C7 Cl2 118.3(2) . .
C6 C7 Cl2 120.2(2) . .
C9 C10 C11 119.3(3) . .
C10 C9 C8 120.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N1 2.055(2) .
Co1 N1 2.055(2) 2_556
Co1 Cl1 2.2554(10) 2_556
Co1 Cl1 2.2554(10) .
Cl3 C11 1.740(3) .
Cl2 C7 1.739(3) .
N1 C5 1.339(4) .
N1 C1 1.343(3) .
C5 C4 1.382(4) .
C5 N2 1.430(4) .
C1 C2 1.371(4) .
C4 C3 1.381(4) .
C3 C2 1.383(5) .
N2 N3 1.241(3) .
N3 C6 1.438(3) .
C8 C9 1.381(5) .
C8 C7 1.383(4) .
C6 C11 1.387(4) .
C6 C7 1.402(4) .
C11 C10 1.379(4) .
C10 C9 1.378(5) .
