Platinum-Catalyzed Direct Amination of Allylic Alcohols under Mild Conditions: Ligand and Microwave Effects, Substrate Scope, and Mechanistic Study
Takashi Ohshima; Yoshiki Miyamoto; Junji Ipposhi; Yasuhito Nakahara; Masaru Utsunomiya; Kazushi Mashima; Journal of the American Chemical Society 131 (2009) 14317–14328; doi:10.1021/ja9046075

data_4105102
_publ_section_title
;
 Platinum-Catalyzed Direct Amination of Allylic Alcohols under Mild
 Conditions: Ligand and Microwave Effects, Substrate Scope, and
 Mechanistic Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14317
_journal_page_last               14328
_journal_paper_doi               10.1021/ja9046075
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C44 H39 Cl2 F3 O4 P2 Pt S '
_chemical_formula_sum            'C44 H39 Cl2 F3 O4 P2 Pt S'
_chemical_formula_weight         1048.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.618(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.188(3)
_cell_length_b                   18.326(5)
_cell_length_c                   25.212(7)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4197(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29455
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    3.638
_exptl_absorpt_correction_T_max  0.336
_exptl_absorpt_correction_T_min  0.172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             2080.00
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         3.11
_refine_diff_density_min         -2.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9521
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0528P)^2^+33.9084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                7217
_reflns_number_total             9521
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja9046075_si_003.cif
_cod_data_source_block           '__piallyl'
_cod_original_cell_volume        4198(2)
_cod_original_formula_sum        'C44 H39 Cl2 F3 O4 P2 Pt S '
_cod_database_code               4105102