Cobalt-Promoted Tandem C(sp2)‒H Activation and C‒C Coupling of Vinyldiphenylphosphine: σ- vs π-Coordination Modes within Cyclometalation
Beck, Robert; Flörke, Ulrich; Klein, Hans-Friedrich; Organometallics 34 (2015) 1454–; doi:10.1021/om500816t

data_4085708
_publ_section_title
;
 Cobalt-Promoted Tandem C(sp2)--H Activation and C--C Coupling of
 Vinyldiphenylphosphine: \s- vs \p-Coordination Modes within
 Cyclometalation
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1454
_journal_paper_doi               10.1021/om500816t
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C24 H41 Co P4'
_chemical_formula_sum            'C24 H41 Co P4'
_chemical_formula_weight         512.38
_chemical_name_systematic
; 
 (diphenylphosphanyl)propyl-C,P)-tris-
 (trimethylphospane)cobalt 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.602(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.612(2)
_cell_length_b                   14.7922(15)
_cell_length_c                   18.010(3)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      15.02
_cell_measurement_theta_min      6.53
_cell_volume                     2769.4(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      566(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12846
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 397
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.8469
_exptl_absorpt_correction_T_min  0.7249
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0019(3)
_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   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0391P)^2^+0.0411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                3442
_reflns_number_total             6107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500816t_si_002.cif
_cod_data_source_block           k946
_cod_depositor_comments
'Adding full bibliography for 4085707--4085709.cif.'
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4085708