Intermolecular Methyl Group Exchange and Reversible P‒Me Bond Cleavage at Cobalt(III) Dimethyl Halide Species
Xu, Hongwei; Williard, Paul G.; Bernskoetter, Wesley H.; Organometallics 32 (2013) 798–; doi:10.1021/om3009537

data_4079836
_publ_section_title
;
 Intermolecular Methyl Group Exchange and Reversible P--Me Bond Cleavage
 at Cobalt(III) Dimethyl Halide Species
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              798
_journal_paper_doi               10.1021/om3009537
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C12 H33 Co F3 O3 P3 S'
_chemical_formula_weight         466.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.909(12)
_cell_length_b                   14.831(12)
_cell_length_c                   21.003(18)
_cell_measurement_temperature    183(2)
_cell_volume                     4333(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1421
_diffrn_reflns_av_sigmaI/netI    0.0773
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41161
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.142
_exptl_absorpt_correction_T_max  0.8038
_exptl_absorpt_correction_T_min  0.7634
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.0062(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   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0659P)^2^+1.2009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                3411
_reflns_number_total             4558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3009537_si_001.cif
_cod_data_source_block           wb12aug11_0m
_cod_database_code               4079836