Tris(<i>tert</i>-butylisonitrile)hexacarbonyl-μ~3~-ethylidyne-<i>triangulo</i>-tricobalt(I)(3 <i>Co{—</i>Co})
Brown, Jolene M.; Nicholson, Brian K.; Acta Crystallographica Section E 63 (2007) m2542–m2542; doi:10.1107/S1600536807044261

data_2215668
_publ_section_title
;Tris(<i>tert</i>-butylisonitrile)hexacarbonyl-\m~3~-ethylidyne-<i>triangulo</i>-tricobalt(I)(3
 <i>Co{---</i>Co})
;
_journal_coeditor_code           SJ2355
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2542
_journal_page_last               m2542
_journal_paper_doi               10.1107/S1600536807044261
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Co3 (C2 H3) (C5 H9 N)3 (C O)6]'
_chemical_formula_moiety         'C23 H30 Co3 N3 O6'
_chemical_formula_sum            'C23 H30 Co3 N3 O6'
_chemical_formula_weight         621.29
_chemical_name_systematic
;
tris(<i>tert</i>-butylisonitrile)hexacarbonyl-\m~3~-ethylidyne-
triangulo-tricobalt(I)(3 Co---Co)
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.9804(6)
_cell_length_b                   16.9804(6)
_cell_length_c                   17.4605(11)
_cell_measurement_reflns_used    5750
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.4
_cell_volume                     4360.0(4)
_computing_cell_refinement       'SAINT (Bruker 2001)'
_computing_data_collection       'SMART (Bruker 2001)'
_computing_data_reduction        'SAINT (Bruker 2001)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Version 1.70.01; Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       multi-scan
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10767
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal rod'
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.159
_refine_ls_abs_structure_details 'Flack (1983), with 989 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1991
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0247
_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/[\s^2^(Fo^2^)+(0.0388P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                1757
_reflns_number_total             1991
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2355.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3c'
_cod_database_code               2215668
_cod_database_fobs_code          2215668