Low-Coordinate Cobalt Fluoride Complexes: Synthesis, Reactions, and Production from C‒F Activation Reactions
Dugan, Thomas R.; Goldberg, Jonathan M.; Brennessel, William W.; Holland, Patrick L.; Organometallics 31 (2012) 1349–; doi:10.1021/om200991k

data_4089378
_publ_section_title
;
 Low-Coordinate Cobalt Fluoride Complexes: Synthesis, Reactions, and
 Production from C--F Activation Reactions
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1349
_journal_paper_doi               10.1021/om200991k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C70 H108 Co2 N4, C6 D6'
_chemical_formula_sum            'C76 H108 Co2 D6 N4'
_chemical_formula_weight         1207.61
_chemical_name_common            '[L(tBu)Co(H)]2'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                98.582(2)
_cell_angle_beta                 94.212(2)
_cell_angle_gamma                117.175(1)
_cell_formula_units_Z            2
_cell_length_a                   12.2671(6)
_cell_length_b                   13.3398(7)
_cell_length_c                   23.7920(17)
_cell_measurement_reflns_used    3781
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      38.15
_cell_measurement_theta_min      2.78
_cell_volume                     3380.1(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            92575
_diffrn_reflns_theta_full        33.73
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9005
_exptl_absorpt_correction_T_min  0.8646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         26825
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0624P)^2^+1.3158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                16603
_reflns_number_total             26825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200991k_si_002.cif
_cod_data_source_block           '[L(tBu)Co(H)]2'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089378