Synthesis and Characterization of a Novel Cobalt Carbonyl N-Heterocyclic Carbene Salt. Crystal Structure of [Co(CO)3(IMes)2]+[Co(CO)4]-
Hendrik van Rensburg; Robert P. Tooze; Douglas F. Foster; Stefanus Otto; Inorganic Chemistry 46 (2007) 1963–1965; doi:10.1021/ic062368o

data_4307859
_publ_contact_author
;
      Stefanus Otto
      Sasol Technology Research & Development      
      P.O. Box 1
      Sasolburg
      1947
      South Africa
;
_publ_contact_author_email       Fanie.otto@sasol.com
_publ_contact_author_fax         Intl-27-11-5223218
_publ_contact_author_phone       Intl-27-16-9604456
_publ_section_title
;
Synthesis and Characterization of a Novel Cobalt Carbonyl N-Heterocyclic
Carbene Salt. Crystal Structure of [Co(CO)3(IMes)2]+[Co(CO)4]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1963
_journal_page_last               1965
_journal_paper_doi               10.1021/ic062368o
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C50.50 H51 Co2 N4 O7'
_chemical_formula_sum            'C50.5 H51 Co2 N4 O7'
_chemical_formula_weight         943.81
_chemical_name_systematic
; 
Di[1,3-bis(2,4,6-trimethylphenyl)imidazol-2-ylidene]tricarbonylcobalt(1+) 
Tetracarbonylcobaltate(1-) cyclohexane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.352(3)
_cell_angle_beta                 98.820(3)
_cell_angle_gamma                90.829(4)
_cell_formula_units_Z            2
_cell_length_a                   11.554(2)
_cell_length_b                   11.940(2)
_cell_length_c                   18.039(3)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      12
_cell_volume                     2328.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker 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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14967
_diffrn_reflns_theta_full        25.48
_diffrn_reflns_theta_max         25.48
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0014(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8362
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+2.3054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1624
_reflns_number_gt                5563
_reflns_number_total             8362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062368osi20061214_110823.cif
_cod_data_source_block           sasol33
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Multi scan' changed
to 'multi-scan' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measurted' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2328.9(8)
_cod_original_formula_sum        'C50.50 H51 Co2 N4 O7'
_cod_database_code               4307859