#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:30:47 +0100 (lun 21 de mar de 2016) $
#$Revision: 178654 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/65/4076598.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_4076598
loop_
_publ_author_name
'Al Thagfi, Jameel'
'Lavoie, Gino G.'
_publ_section_title
;
 Synthesis, Characterization, and Ethylene Polymerization Studies of
 Chromium, Iron, and Cobalt Complexes Containing
 1,3-Bis(imino)-N-Heterocyclic Carbene Ligands
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2463
_journal_paper_doi               10.1021/om3001058
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C23 H26 Cl2 Co N4, 2(C H2 Cl2)'
_chemical_formula_sum            'C25 H30 Cl6 Co N4'
_chemical_formula_weight         658.16
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.6970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0052(3)
_cell_length_b                   14.7348(3)
_cell_length_c                   23.3276(7)
_cell_measurement_reflns_used    14566
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     3084.94(15)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'CAMERON (Watkin, Prout & Pearce, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_solution    'SUPERFLIP (Palatinus L., Chapuis G., 2007)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20424
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0818P)²+4.0260P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1736
_reflns_number_gt                4602
_reflns_number_total             7033
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om3001058_si_002.cif
_cod_data_source_block           k10110
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4076598
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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 0.97755(6) 0.12026(3) 0.250668(19) 0.02606(15) Uani 1 1 d .
Cl2 Cl 0.73295(11) 0.12274(6) 0.25949(4) 0.0353(2) Uani 1 1 d .
Cl1 Cl 1.09752(11) 0.24936(6) 0.27201(4) 0.0390(2) Uani 1 1 d .
Cl3S Cl 0.47596(15) 0.31093(10) 0.13047(6) 0.0681(4) Uani 1 1 d .
Cl4S Cl 0.65908(17) 0.97306(10) 0.10006(7) 0.0737(4) Uani 1 1 d .
Cl5S Cl 0.53467(15) 0.83423(9) 0.17011(6) 0.0641(4) Uani 1 1 d .
Cl2S Cl 0.36488(19) 0.12695(11) 0.14334(8) 0.0848(5) Uani 1 1 d .
N4 N 0.9494(4) 0.12411(19) 0.03199(12) 0.0302(7) Uani 1 1 d .
N3 N 1.0945(3) 0.00871(19) 0.28500(12) 0.0251(6) Uani 1 1 d .
N1 N 1.0903(3) -0.02559(19) 0.18958(11) 0.0251(6) Uani 1 1 d .
N2 N 1.0049(3) 0.05687(19) 0.11909(12) 0.0268(6) Uani 1 1 d .
C12 C 0.7116(7) 0.2761(3) -0.06327(18) 0.0553(13) Uani 1 1 d .
H12 H 0.6117 0.2872 -0.0743 0.066 Uiso 1 1 calc R
C18 C 1.3265(5) 0.0183(3) 0.42433(18) 0.0443(10) Uani 1 1 d .
H18 H 1.4196 0.0385 0.4392 0.053 Uiso 1 1 calc R
C11 C 0.8191(8) 0.3262(3) -0.08778(18) 0.0628(16) Uani 1 1 d .
H11 H 0.7914 0.3702 -0.1152 0.075 Uiso 1 1 calc R
C8 C 0.9019(5) 0.1961(2) -0.00620(15) 0.0342(9) Uani 1 1 d .
C17 C 1.2851(4) 0.0277(3) 0.36582(16) 0.0341(9) Uani 1 1 d .
C13 C 0.7490(5) 0.2091(3) -0.02221(16) 0.0405(10) Uani 1 1 d .
C3 C 1.0610(5) -0.0220(2) 0.09577(16) 0.0322(8) Uani 1 1 d .
H3 H 1.0613 -0.0359 0.0569 0.039 Uiso 1 1 calc R
C9 C 1.0117(6) 0.2461(3) -0.03071(17) 0.0432(11) Uani 1 1 d .
C1 C 1.0223(4) 0.0558(2) 0.17713(14) 0.0264(7) Uani 1 1 d .
C6 C 0.9442(4) 0.1321(2) 0.08525(15) 0.0270(8) Uani 1 1 d .
C4 C 1.1364(4) -0.0472(2) 0.24793(14) 0.0250(7) Uani 1 1 d .
C1S C 0.4179(6) 0.2278(3) 0.1785(2) 0.0562(12) Uani 1 1 d .
H1S1 H 0.4987 0.2154 0.2075 0.067 Uiso 1 1 calc R
H1S2 H 0.3346 0.2512 0.1978 0.067 Uiso 1 1 calc R
C5 C 1.2305(4) -0.1286(2) 0.25819(16) 0.0325(8) Uani 1 1 d .
H5A H 1.2418 -0.1586 0.2223 0.049 Uiso 1 1 calc R
H5B H 1.1843 -0.1691 0.2836 0.049 Uiso 1 1 calc R
H5C H 1.3267 -0.1109 0.2753 0.049 Uiso 1 1 calc R
C7 C 0.8898(5) 0.2098(2) 0.11900(15) 0.0357(9) Uani 1 1 d .
H7A H 0.9003 0.1952 0.1592 0.053 Uiso 1 1 calc R
H7B H 0.7868 0.2211 0.1073 0.053 Uiso 1 1 calc R
H7C H 0.9474 0.2630 0.1122 0.053 Uiso 1 1 calc R
C22 C 1.3894(5) 0.0706(3) 0.32643(18) 0.0438(10) Uani 1 1 d .
H22A H 1.3430 0.0716 0.2879 0.066 Uiso 1 1 calc R
H22B H 1.4799 0.0360 0.3274 0.066 Uiso 1 1 calc R
H22C H 1.4117 0.1315 0.3389 0.066 Uiso 1 1 calc R
C21 C 1.0442(5) -0.0425(2) 0.38143(15) 0.0328(9) Uani 1 1 d .
C2 C 1.1143(4) -0.0737(3) 0.13973(15) 0.0329(8) Uani 1 1 d .
H2 H 1.1585 -0.1305 0.1375 0.040 Uiso 1 1 calc R
C16 C 1.1441(4) -0.0034(2) 0.34547(14) 0.0280(8) Uani 1 1 d .
C20 C 1.0915(5) -0.0507(3) 0.43961(16) 0.0417(10) Uani 1 1 d .
H20 H 1.0284 -0.0767 0.4646 0.050 Uiso 1 1 calc R
C15 C 0.6321(6) 0.1518(3) 0.0023(2) 0.0551(12) Uani 1 1 d .
H15A H 0.6788 0.1102 0.0299 0.083 Uiso 1 1 calc R
H15B H 0.5785 0.1184 -0.0280 0.083 Uiso 1 1 calc R
H15C H 0.5643 0.1901 0.0209 0.083 Uiso 1 1 calc R
C2S C 0.6729(6) 0.9188(4) 0.1668(2) 0.0660(15) Uani 1 1 d .
H2S1 H 0.6622 0.9632 0.1968 0.079 Uiso 1 1 calc R
H2S2 H 0.7707 0.8913 0.1734 0.079 Uiso 1 1 calc R
C19 C 1.2302(6) -0.0208(3) 0.46050(17) 0.0480(11) Uani 1 1 d .
H19 H 1.2597 -0.0270 0.4994 0.058 Uiso 1 1 calc R
C23 C 0.8933(5) -0.0743(3) 0.35784(18) 0.0409(10) Uani 1 1 d .
H23A H 0.8823 -0.0644 0.3170 0.061 Uiso 1 1 calc R
H23B H 0.8179 -0.0409 0.3757 0.061 Uiso 1 1 calc R
H23C H 0.8829 -0.1378 0.3657 0.061 Uiso 1 1 calc R
C10 C 0.9660(7) 0.3113(3) -0.07188(18) 0.0552(14) Uani 1 1 d .
H10 H 1.0376 0.3453 -0.0888 0.066 Uiso 1 1 calc R
C14 C 1.1720(6) 0.2303(4) -0.0140(2) 0.0631(14) Uani 1 1 d .
H14A H 1.2308 0.2706 -0.0353 0.095 Uiso 1 1 calc R
H14B H 1.1968 0.1686 -0.0223 0.095 Uiso 1 1 calc R
H14C H 1.1922 0.2415 0.0264 0.095 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
C1 Co1 N3 79.99(12)
C1 Co1 Cl1 117.57(10)
N3 Co1 Cl1 111.64(9)
C1 Co1 Cl2 110.61(11)
N3 Co1 Cl2 116.81(8)
Cl1 Co1 Cl2 115.52(4)
C6 N4 C8 121.0(3)
C4 N3 C16 119.6(3)
C4 N3 Co1 114.8(2)
C16 N3 Co1 125.2(2)
C1 N1 C2 111.5(3)
C1 N1 C4 119.3(3)
C2 N1 C4 129.1(3)
C1 N2 C3 111.4(3)
C1 N2 C6 124.4(3)
C3 N2 C6 124.1(3)
C11 C12 C13 121.6(5)
C19 C18 C17 120.5(4)
C10 C11 C12 120.0(4)
C9 C8 C13 122.0(4)
C9 C8 N4 117.6(4)
C13 C8 N4 120.2(4)
C18 C17 C16 117.7(4)
C18 C17 C22 120.6(4)
C16 C17 C22 121.7(3)
C12 C13 C8 116.9(4)
C12 C13 C15 121.5(4)
C8 C13 C15 121.5(4)
C2 C3 N2 107.1(3)
C8 C9 C10 117.9(5)
C8 C9 C14 121.2(4)
C10 C9 C14 121.0(5)
N2 C1 N1 103.7(3)
N2 C1 Co1 145.8(3)
N1 C1 Co1 110.3(2)
N4 C6 N2 115.3(3)
N4 C6 C7 129.4(3)
N2 C6 C7 115.2(3)
N3 C4 N1 115.2(3)
N3 C4 C5 127.8(3)
N1 C4 C5 117.0(3)
Cl2S C1S Cl3S 112.1(3)
C20 C21 C16 117.3(4)
C20 C21 C23 121.7(4)
C16 C21 C23 121.0(3)
C3 C2 N1 106.3(3)
C17 C16 C21 122.8(3)
C17 C16 N3 119.2(3)
C21 C16 N3 118.0(3)
C19 C20 C21 120.9(4)
Cl4S C2S Cl5S 111.3(3)
C20 C19 C18 120.9(4)
C11 C10 C9 121.5(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 C1 2.030(3)
Co1 N3 2.077(3)
Co1 Cl1 2.2239(10)
Co1 Cl2 2.2293(11)
Cl3S C1S 1.768(5)
Cl4S C2S 1.745(5)
Cl5S C2S 1.768(5)
Cl2S C1S 1.745(5)
N4 C6 1.253(4)
N4 C8 1.428(5)
N3 C4 1.273(4)
N3 C16 1.455(4)
N1 C1 1.367(4)
N1 C2 1.394(4)
N1 C4 1.426(4)
N2 C1 1.350(4)
N2 C3 1.395(4)
N2 C6 1.443(4)
C12 C11 1.378(8)
C12 C13 1.397(6)
C18 C19 1.384(6)
C18 C17 1.392(5)
C11 C10 1.362(8)
C8 C9 1.393(6)
C8 C13 1.410(6)
C17 C16 1.396(5)
C17 C22 1.506(6)
C13 C15 1.499(6)
C3 C2 1.335(5)
C9 C10 1.397(6)
C9 C14 1.482(7)
C6 C7 1.495(5)
C4 C5 1.477(5)
C21 C20 1.394(5)
C21 C16 1.403(5)
C21 C23 1.499(6)
C20 C19 1.376(6)
