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_4085707
_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         'C34 H43 Co P4'
_chemical_formula_sum            'C34 H43 Co P4'
_chemical_formula_weight         634.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.64(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.430(4)
_cell_length_b                   15.676(3)
_cell_length_c                   17.132(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.117
_cell_measurement_theta_min      5.214
_cell_volume                     3328.8(13)
_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      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15931
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 397
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0445P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                5039
_reflns_number_total             7661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500816t_si_002.cif
_cod_data_source_block           k949
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4085707--4085709.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4085707