#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:13:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179472 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/69/4336979.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_4336979
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 Cl5 Co N6'
_chemical_formula_weight         598.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   14.090(5)
_cell_length_b                   14.745(5)
_cell_length_c                   23.495(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      1.7
_cell_volume                     4881(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51895
_diffrn_reflns_theta_full        27.78
_diffrn_reflns_theta_max         27.78
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_F_000             2400.0
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0370P)²+1.5195P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                4243
_reflns_number_total             5776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4018079_si_002_4.cif
_cod_data_source_block           4
_cod_database_code               4336979
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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 0.501035(18) 0.237829(18) 0.619475(11) 0.02891(8) Uani 1 1 d .
Cl1 Cl 0.37287(4) 0.14342(4) 0.62815(2) 0.04062(13) Uani 1 1 d .
Cl4 Cl 0.68827(5) 0.34403(4) 0.52560(3) 0.06392(19) Uani 1 1 d .
Cl2 Cl 0.30364(4) 0.35257(5) 0.71342(3) 0.06109(19) Uani 1 1 d .
Cl5 Cl 0.59787(5) -0.00620(4) 0.56299(3) 0.06065(19) Uani 1 1 d .
Cl3 Cl 0.66405(4) 0.43948(5) 0.65966(3) 0.05911(18) Uani 1 1 d .
N6 N 0.61425(11) 0.18685(11) 0.59594(7) 0.0318(4) Uani 1 1 d .
N3 N 0.47261(12) 0.35700(11) 0.63748(7) 0.0331(4) Uani 1 1 d .
N2 N 0.44920(13) 0.41558(12) 0.59766(8) 0.0398(4) Uani 1 1 d .
N1 N 0.45839(12) 0.28027(11) 0.54717(7) 0.0323(4) Uani 1 1 d .
N5 N 0.68013(12) 0.16418(12) 0.63307(7) 0.0378(4) Uani 1 1 d .
N4 N 0.55298(12) 0.20312(11) 0.69126(7) 0.0331(4) Uani 1 1 d .
C3 C 0.39386(19) 0.36503(19) 0.44952(11) 0.0573(7) Uani 1 1 d .
H3 H 0.3733 0.3932 0.4163 0.069 Uiso 1 1 calc R
C10 C 0.58468(18) 0.47268(16) 0.76191(10) 0.0496(6) Uani 1 1 d .
H10 H 0.6431 0.4969 0.7723 0.059 Uiso 1 1 calc R
C11 C 0.57159(15) 0.43728(14) 0.70805(10) 0.0396(5) Uani 1 1 d .
C6 C 0.48509(14) 0.39955(14) 0.69198(9) 0.0350(4) Uani 1 1 d .
C2 C 0.41093(17) 0.27234(18) 0.45029(10) 0.0509(6) Uani 1 1 d .
H2 H 0.4009 0.2376 0.4178 0.061 Uiso 1 1 calc R
C9 C 0.51040(18) 0.47188(17) 0.80024(11) 0.0537(6) Uani 1 1 d .
H9 H 0.5189 0.4960 0.8364 0.064 Uiso 1 1 calc R
C19 C 0.65947(18) 0.05773(19) 0.46282(11) 0.0581(7) Uani 1 1 d .
H19 H 0.6539 -0.0016 0.4498 0.070 Uiso 1 1 calc R
C18 C 0.63710(15) 0.07921(15) 0.51811(10) 0.0419(5) Uani 1 1 d .
C5 C 0.43854(14) 0.37036(14) 0.54691(9) 0.0353(5) Uani 1 1 d .
C15 C 0.69556(17) 0.14726(17) 0.73509(10) 0.0507(6) Uani 1 1 d .
H15 H 0.7586 0.1294 0.7316 0.061 Uiso 1 1 calc R
C17 C 0.64375(14) 0.16726(14) 0.53861(9) 0.0342(4) Uani 1 1 d .
C22 C 0.67561(15) 0.23422(16) 0.50152(10) 0.0444(5) Uani 1 1 d .
C1 C 0.44267(15) 0.23244(15) 0.49932(9) 0.0396(5) Uani 1 1 d .
H1 H 0.4537 0.1703 0.4996 0.047 Uiso 1 1 calc R
C12 C 0.51135(17) 0.20183(16) 0.74276(9) 0.0446(5) Uani 1 1 d .
H12 H 0.4481 0.2191 0.7458 0.053 Uiso 1 1 calc R
C7 C 0.41218(15) 0.40021(15) 0.73137(10) 0.0425(5) Uani 1 1 d .
C16 C 0.64375(15) 0.17223(14) 0.68709(9) 0.0365(5) Uani 1 1 d .
C20 C 0.6903(2) 0.1253(2) 0.42710(11) 0.0682(8) Uani 1 1 d .
H20 H 0.7054 0.1114 0.3896 0.082 Uiso 1 1 calc R
C4 C 0.40740(17) 0.41445(17) 0.49783(10) 0.0491(6) Uani 1 1 d .
H4 H 0.3961 0.4766 0.4981 0.059 Uiso 1 1 calc R
C8 C 0.42404(18) 0.43575(17) 0.78537(10) 0.0506(6) Uani 1 1 d .
H8 H 0.3742 0.4352 0.8113 0.061 Uiso 1 1 calc R
C13 C 0.5588(2) 0.17597(19) 0.79098(10) 0.0582(7) Uani 1 1 d .
H13 H 0.5282 0.1764 0.8260 0.070 Uiso 1 1 calc R
C14 C 0.6531(2) 0.14916(19) 0.78712(11) 0.0605(7) Uani 1 1 d .
H14 H 0.6868 0.1328 0.8196 0.073 Uiso 1 1 calc R
C21 C 0.69912(18) 0.2131(2) 0.44583(11) 0.0599(7) Uani 1 1 d .
H21 H 0.7208 0.2580 0.4213 0.072 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'
N N 0.0061 0.0033 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N6 Co1 N3 129.88(7)
N6 Co1 N1 97.98(7)
N3 Co1 N1 79.86(7)
N6 Co1 N4 79.88(7)
N3 Co1 N4 97.79(7)
N1 Co1 N4 174.77(7)
N6 Co1 Cl1 117.40(6)
N3 Co1 Cl1 112.72(6)
N1 Co1 Cl1 91.74(5)
N4 Co1 Cl1 93.48(5)
N5 N6 C17 111.44(16)
N5 N6 Co1 120.90(13)
C17 N6 Co1 127.66(13)
N2 N3 C6 112.19(16)
N2 N3 Co1 121.00(14)
C6 N3 Co1 126.28(13)
N3 N2 C5 109.02(17)
C1 N1 C5 118.37(18)
C1 N1 Co1 128.61(14)
C5 N1 Co1 112.95(14)
N6 N5 C16 109.08(17)
C12 N4 C16 118.02(18)
C12 N4 Co1 129.18(15)
C16 N4 Co1 112.73(14)
C4 C3 C2 119.4(2)
C11 C10 C9 119.5(2)
C10 C11 C6 121.1(2)
C10 C11 Cl3 119.65(18)
C6 C11 Cl3 119.25(17)
C7 C6 C11 117.78(19)
C7 C6 N3 120.57(18)
C11 C6 N3 121.58(19)
C1 C2 C3 119.4(2)
C8 C9 C10 120.6(2)
C18 C19 C20 118.9(2)
C19 C18 C17 121.9(2)
C19 C18 Cl5 118.75(19)
C17 C18 Cl5 119.35(17)
N1 C5 N2 116.63(18)
N1 C5 C4 121.7(2)
N2 C5 C4 121.7(2)
C14 C15 C16 119.5(2)
C18 C17 C22 117.9(2)
C18 C17 N6 119.54(18)
C22 C17 N6 122.48(19)
C21 C22 C17 120.6(2)
C21 C22 Cl4 119.8(2)
C17 C22 Cl4 119.62(18)
N1 C1 C2 122.1(2)
N4 C12 C13 122.3(2)
C6 C7 C8 121.8(2)
C6 C7 Cl2 119.30(16)
C8 C7 Cl2 118.88(18)
N4 C16 N5 116.49(18)
N4 C16 C15 121.5(2)
N5 C16 C15 122.0(2)
C21 C20 C19 121.1(2)
C3 C4 C5 118.9(2)
C9 C8 C7 119.2(2)
C12 C13 C14 119.5(2)
C15 C14 C13 119.0(2)
C20 C21 C22 119.6(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 N6 1.8481(17)
Co1 N3 1.8512(17)
Co1 N1 1.9075(16)
Co1 N4 1.9084(17)
Co1 Cl1 2.2892(8)
Cl4 C22 1.724(3)
Cl2 C7 1.735(2)
Cl5 C18 1.733(2)
Cl3 C11 1.729(2)
N6 N5 1.317(2)
N6 C17 1.439(3)
N3 N2 1.315(2)
N3 C6 1.437(3)
N2 C5 1.374(3)
N1 C1 1.346(3)
N1 C5 1.357(3)
N5 C16 1.374(3)
N4 C12 1.345(3)
N4 C16 1.361(3)
C3 C4 1.362(4)
C3 C2 1.388(4)
C10 C11 1.381(3)
C10 C9 1.381(3)
C11 C6 1.392(3)
C6 C7 1.383(3)
C2 C1 1.369(3)
C9 C8 1.374(3)
C19 C18 1.374(3)
C19 C20 1.373(4)
C18 C17 1.388(3)
C5 C4 1.395(3)
C15 C14 1.361(4)
C15 C16 1.393(3)
C17 C22 1.391(3)
C22 C21 1.385(3)
C12 C13 1.370(3)
C7 C8 1.383(3)
C20 C21 1.372(4)
C13 C14 1.389(4)
