Controlling Secondary Alkyl Radicals: Ligand Effects in Chromium-Catalyzed C‒P Bond Formation
Zhou, Wen; MacLeod, K. Cory; Patrick, Brian O.; Smith, Kevin M.; Organometallics 31 (2012) 7324–; doi:10.1021/om300846u

data_4079570
_publ_section_title
;
 Controlling Secondary Alkyl Radicals: Ligand Effects in
 Chromium-Catalyzed C--P Bond Formation
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              7324
_journal_paper_doi               10.1021/om300846u
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C36 H43 Cr N2 O3 S'
_chemical_formula_weight         635.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                83.332(5)
_cell_angle_beta                 78.022(5)
_cell_angle_gamma                63.468(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9124(13)
_cell_length_b                   11.3990(12)
_cell_length_c                   14.8482(18)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.33
_cell_volume                     1615.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27862
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6304
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+1.3120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                4984
_reflns_number_total             6304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300846u_si_002.cif
_cod_data_source_block           4_CpCr(Dpp/Tol-Nacnac)(OTs)
_cod_database_code               4079570