Ruthenium-Catalyzed Hydroamination of Unactivated Terminal Alkenes with Stoichiometric Amounts of Alkene and an Ammonia Surrogate by Sequential Oxidation and Reduction.
Ma, Senjie; Hill, Christopher K.; Olen, Casey L.; Hartwig, John F.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11043

data_4135477
_publ_section_title
;
 Ruthenium-Catalyzed Hydroamination of Unactivated Terminal Alkenes with
 Stoichiometric Amounts of Alkene and an Ammonia Surrogate by Sequential
 Oxidation and Reduction.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11043
_journal_year                    2020
_chemical_formula_sum            'C26 H54 F6 N3.8 O4 P3 Ru S2'
_chemical_formula_weight         856.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                79.6870(10)
_cell_angle_beta                 82.7900(10)
_cell_angle_gamma                78.3830(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2586(2)
_cell_length_b                   11.4779(2)
_cell_length_c                   16.7535(2)
_cell_measurement_reflns_used    36515
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.1050
_cell_measurement_theta_min      2.9350
_cell_volume                     1892.84(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60357
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.500
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             887
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         11552
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9849
_reflns_number_total             11552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11043_si_005.cif
_cod_data_source_block           Ma006_Hartwig
_cod_original_formula_sum        'C26 H54 F6 N3.80 O4 P3 Ru S2'
_cod_database_code               4135477
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.808
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              27494
_shelx_hkl_checksum              35218