#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:50:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179734 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/30/7003052.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_7003052
loop_
_publ_author_name
'Singh, Akhilesh Kumar'
'Mukherjee, Rabindranath'
_publ_section_title
;
 Cobalt(ii) and cobalt(iii) complexes of thioether-containing
 hexadentate pyrazine amide ligands: C--S bond cleavage and
 cyclometallation reaction
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              260
_journal_page_last               270
_journal_paper_doi               10.1039/b709901k
_journal_year                    2008
_chemical_formula_moiety         'C31 H26 Co N6 O2 S2'
_chemical_formula_sum            'C31 H26 Co N6 O2 S2'
_chemical_formula_weight         637.63
_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                90.0
_cell_angle_beta                 104.864(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   21.722(5)
_cell_length_b                   12.058(5)
_cell_length_c                   10.524(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2664.2(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'Bruker SAINT PLUS'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97(Altomare, et. al. 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8566
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.9202
_exptl_absorpt_correction_T_min  0.7856
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Dark-brown
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3266
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0565
_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)+(0.0532P)²+16.8213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                2579
_reflns_number_total             3266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b709901k.txt
_cod_data_source_block           3octb
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7003052
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
Co1 Co 0.0000 0.23267(6) 0.2500 0.01396(19) Uani 1 2 d S . .
S1 S -0.07083(5) 0.10127(8) 0.30040(9) 0.0225(2) Uani 1 1 d . . .
O1 O -0.06197(12) 0.2998(2) -0.1391(2) 0.0204(6) Uani 1 1 d . . .
N1 N 0.04806(14) 0.3470(3) 0.1693(3) 0.0176(6) Uani 1 1 d . . .
N2 N 0.10814(15) 0.4713(3) 0.0124(3) 0.0216(7) Uani 1 1 d . . .
N3 N -0.05710(14) 0.2366(3) 0.0744(3) 0.0160(6) Uani 1 1 d . . .
C1 C 0.09987(17) 0.4062(3) 0.2227(4) 0.0188(7) Uani 1 1 d . . .
H1 H 0.1170 0.4052 0.3153 0.023 Uiso 1 1 calc R . .
C2 C 0.12945(18) 0.4700(3) 0.1439(4) 0.0209(8) Uani 1 1 d . . .
H2 H 0.1656 0.5135 0.1847 0.025 Uiso 1 1 calc R . .
C3 C 0.05628(18) 0.4110(3) -0.0397(3) 0.0180(7) Uani 1 1 d . . .
H3 H 0.0403 0.4090 -0.1326 0.022 Uiso 1 1 calc R . .
C4 C 0.02472(16) 0.3508(3) 0.0377(3) 0.0155(7) Uani 1 1 d . . .
C5 C -0.03667(17) 0.2913(3) -0.0182(3) 0.0161(7) Uani 1 1 d . . .
C6 C -0.11662(17) 0.1830(3) 0.0491(3) 0.0160(7) Uani 1 1 d . . .
C7 C -0.16584(17) 0.1953(3) -0.0673(4) 0.0211(8) Uani 1 1 d . . .
H7 H -0.1597 0.2425 -0.1353 0.025 Uiso 1 1 calc R . .
C8 C -0.22278(19) 0.1393(4) -0.0832(4) 0.0260(9) Uani 1 1 d . . .
H8 H -0.2553 0.1492 -0.1622 0.031 Uiso 1 1 calc R . .
C9 C -0.23387(19) 0.0688(4) 0.0134(4) 0.0282(9) Uani 1 1 d . . .
H9 H -0.2729 0.0293 -0.0002 0.034 Uiso 1 1 calc R . .
C10 C -0.18686(19) 0.0575(3) 0.1298(4) 0.0250(8) Uani 1 1 d . . .
H10 H -0.1939 0.0106 0.1973 0.030 Uiso 1 1 calc R . .
C11 C -0.12939(18) 0.1144(3) 0.1486(4) 0.0201(8) Uani 1 1 d . . .
C12 C -0.0482(2) -0.0444(4) 0.2981(5) 0.0339(11) Uani 1 1 d D . .
H12B H -0.083(3) -0.085(5) 0.299(6) 0.06(2) Uiso 1 1 d . . .
H12A H -0.031(5) -0.060(9) 0.383(3) 0.15(4) Uiso 1 1 d D . .
C13 C -0.0195(4) -0.0747(6) 0.1954(8) 0.0240(16) Uani 0.50 1 d PD . .
H13A H -0.044(4) -0.050(7) 0.118(4) 0.02(2) Uiso 0.50 1 d PD . .
H13B H -0.025(4) -0.1479(18) 0.180(9) 0.04(3) Uiso 0.50 1 d PD . .
C14 C 0.8071(2) 0.2208(4) 0.4712(4) 0.0285(9) Uani 1 1 d . . .
H14 H 0.8459 0.2009 0.4512 0.034 Uiso 1 1 calc R . .
C15 C 0.8076(2) 0.2684(4) 0.5919(4) 0.0309(10) Uani 1 1 d . . .
H15 H 0.8469 0.2811 0.6550 0.037 Uiso 1 1 calc R . .
C16 C 0.7510(2) 0.2973(4) 0.6200(4) 0.0285(9) Uani 1 1 d . . .
H16 H 0.7517 0.3299 0.7025 0.034 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Co1 N3 177.21(19) . 2 ?
N3 Co1 N1 96.29(12) . 2 ?
N3 Co1 N1 81.81(12) 2 2 ?
N3 Co1 N1 81.81(12) . . ?
N3 Co1 N1 96.29(12) 2 . ?
N1 Co1 N1 95.03(18) 2 . ?
N3 Co1 S1 86.35(9) . . ?
N3 Co1 S1 95.53(9) 2 . ?
N1 Co1 S1 85.84(9) 2 . ?
N1 Co1 S1 168.16(9) . . ?
N3 Co1 S1 95.53(9) . 2 ?
N3 Co1 S1 86.35(9) 2 2 ?
N1 Co1 S1 168.16(9) 2 2 ?
N1 Co1 S1 85.84(9) . 2 ?
S1 Co1 S1 95.73(6) . 2 ?
C11 S1 C12 101.9(2) . . ?
C11 S1 Co1 95.49(13) . . ?
C12 S1 Co1 116.72(16) . . ?
C1 N1 C4 118.1(3) . . ?
C1 N1 Co1 130.9(3) . . ?
C4 N1 Co1 110.6(2) . . ?
C3 N2 C2 116.6(3) . . ?
C5 N3 C6 123.1(3) . . ?
C5 N3 Co1 116.9(2) . . ?
C6 N3 Co1 120.0(2) . . ?
N1 C1 C2 120.8(3) . . ?
N2 C2 C1 121.8(4) . . ?
N2 C3 C4 122.2(3) . . ?
N1 C4 C3 120.4(3) . . ?
N1 C4 C5 116.8(3) . . ?
C3 C4 C5 122.8(3) . . ?
O1 C5 N3 129.5(3) . . ?
O1 C5 C4 118.3(3) . . ?
N3 C5 C4 112.2(3) . . ?
N3 C6 C7 124.8(3) . . ?
N3 C6 C11 118.2(3) . . ?
C7 C6 C11 117.0(3) . . ?
C8 C7 C6 120.6(4) . . ?
C7 C8 C9 121.8(4) . . ?
C10 C9 C8 118.6(4) . . ?
C9 C10 C11 120.5(4) . . ?
C10 C11 C6 121.4(4) . . ?
C10 C11 S1 119.5(3) . . ?
C6 C11 S1 119.1(3) . . ?
C13 C12 C13 50.1(6) . 2 ?
C13 C12 S1 115.3(4) . . ?
C13 C12 S1 119.8(4) 2 . ?
C13 C13 C12 68.0(7) 2 . ?
C13 C13 C12 61.9(7) 2 2 ?
C12 C13 C12 121.1(6) . 2 ?
C15 C14 C16 119.1(4) . 7_656 ?
C16 C15 C14 120.0(4) . . ?
C15 C16 C14 120.9(4) . 7_656 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N3 1.944(3) . ?
Co1 N3 1.944(3) 2 ?
Co1 N1 2.041(3) 2 ?
Co1 N1 2.041(3) . ?
Co1 S1 2.3617(12) . ?
Co1 S1 2.3617(12) 2 ?
S1 C11 1.776(4) . ?
S1 C12 1.826(5) . ?
O1 C5 1.254(4) . ?
N1 C1 1.329(5) . ?
N1 C4 1.348(4) . ?
N2 C3 1.335(5) . ?
N2 C2 1.342(5) . ?
N3 C5 1.343(4) . ?
N3 C6 1.408(4) . ?
C1 C2 1.402(5) . ?
C3 C4 1.395(5) . ?
C4 C5 1.495(5) . ?
C6 C7 1.412(5) . ?
C6 C11 1.417(5) . ?
C7 C8 1.381(5) . ?
C8 C9 1.393(6) . ?
C9 C10 1.386(6) . ?
C10 C11 1.393(5) . ?
C12 C13 1.427(9) . ?
C12 C13 1.501(10) 2 ?
C13 C13 1.242(16) 2 ?
C13 C12 1.501(10) 2 ?
C14 C15 1.392(6) . ?
C14 C16 1.393(6) 7_656 ?
C15 C16 1.380(6) . ?
C16 C14 1.393(6) 7_656 ?
