Isocyano Analogues of [Co(CO)4]n: A Tetraisocyanide of Cobalt Isolated in Three States of Charge
Grant W. Margulieux; Nils Weidemann; David C. Lacy; Curtis E. Moore; Arnold L. Rheingold; Joshua S. Figueroa; Journal of the American Chemical Society 132 (2010) 5033–5035; doi:10.1021/ja1012382

data_4102256
_publ_section_title
;
 Isocyano Analogues of [Co(CO)4]n: A Tetraisocyanide of Cobalt Isolated in
 Three States of Charge
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5033
_journal_page_last               5035
_journal_paper_doi               10.1021/ja1012382
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C109 H118 Co F3 N4 O5 S'
_chemical_formula_weight         1712.06
_chemical_name_common            '[(THF)Co(CNArMes2)4]OTf'
_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                 103.099(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.959(4)
_cell_length_b                   20.543(5)
_cell_length_c                   31.517(8)
_cell_measurement_reflns_used    9213
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.22
_cell_volume                     9433(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1108
_diffrn_reflns_av_sigmaI/netI    0.1706
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            55801
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.9778
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1134
_refine_ls_number_reflns         21772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1878
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1898
_reflns_number_gt                9793
_reflns_number_total             21772
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1012382_si_002_7.cif
_cod_data_source_block           jfig235
_cod_original_cell_volume        9434(4)
_cod_database_code               4102256