Copper-Catalyzed P-H Insertions of α-Imino Carbenes for the Preparation of 3-Phosphinoylindoles.
Wang, Lisheng; Wu, Yi; Liu, Yang; Yang, Hua; Liu, Xu; Wang, Jianyi; Li, Xiaoxun; Jiang, Jun; Organic letters 19 (2017) 782–785; doi:10.1021/acs.orglett.6b03752

data_1545467
_publ_section_title
;
 Copper-Catalyzed P-H Insertions of \a-Imino Carbenes for the Preparation
 of 3-Phosphinoylindoles.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              782
_journal_page_last               785
_journal_paper_doi               10.1021/acs.orglett.6b03752
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration s
_chemical_formula_sum            'C40 H54 Br N2 O4 P S'
_chemical_formula_weight         769.79
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 97.966(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7121(11)
_cell_length_b                   9.9230(11)
_cell_length_c                   19.323(2)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.195
_cell_measurement_theta_min      2.958
_cell_volume                     2034.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_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  0.1143
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26793
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.6835
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.483
_exptl_crystal_size_min          0.361
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7135
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+0.0814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                6057
_reflns_number_total             7135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b03752_si_003.cif
_cod_data_source_block           111
_cod_original_sg_symbol_H-M      P21
_cod_database_code               1545467