A Synthetic Cycle for the Ruthenium-Promoted Formation of 1H-Phosphindoles from Phosphaalkynes
Joseph G. Cordaro; Daniel Stein; Hansjörg Grützmacher; Journal of the American Chemical Society 128 (2006) 14962–14971; doi:10.1021/ja0651198

data_4111098
_publ_section_title
;
 A Synthetic Cycle for the Ruthenium-Promoted Formation of
 1H-Phosphindoles from Phosphaalkynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14962
_journal_page_last               14971
_journal_paper_doi               10.1021/ja0651198
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C72 H64 P5 Ru, C7 H8, C F3 O3 S'
_chemical_formula_sum            'C80 H72 F3 O3 P5 Ru S'
_chemical_formula_weight         1426.36
_chemical_name_systematic        ' ?'
_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   geom
_atom_sites_solution_primary     patt
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 101.116(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.285(7)
_cell_length_b                   17.059(7)
_cell_length_c                   23.956(10)
_cell_measurement_temperature    200(2)
_cell_volume                     6931(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 for Windows'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker AXS Apex with CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0682
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36429
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.9463
_exptl_absorpt_correction_T_min  0.8820
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       cube
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         13977
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                7876
_reflns_number_total             13977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0651198si20060908_052021.cif
_cod_data_source_block           RuPhosphaindole
_cod_original_cell_volume        6932(5)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4111098