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_4135480
_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_moiety         'C24 H52 N2 P3 Ru, C2 F6 N O4 S2'
_chemical_formula_sum            'C26 H52 F6 N3 O4 P3 Ru S2'
_chemical_formula_weight         842.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.345(3)
_cell_angle_gamma                90
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_cell_length_b                   14.3288(4)
_cell_length_c                   20.7537(6)
_cell_measurement_reflns_used    26300
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5620
_cell_measurement_theta_min      3.2780
_cell_volume                     3612.08(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.44a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.44a (Rigaku OD, 2019)'
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      100(2)
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_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  0.0659
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49254
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.369
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.843
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_exptl_crystal_colour            red
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_exptl_crystal_size_min          0.090
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_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         7366
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0365P)^2^+3.3656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6458
_reflns_number_total             7366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11043_si_004.cif
_cod_data_source_block           Ma004_Hartwig
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4135480
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.835
_shelx_estimated_absorpt_t_max   0.936
_shelx_res_checksum              73919
_shelx_hkl_checksum              53433