Mechanistic Studies of the Hydroamination of Norbornene with Electrophilic Platinum Complexes: The Role of Proton Transfer
Jennifer L. McBee; Alexis T. Bell; T. Don Tilley; Journal of the American Chemical Society 130 (2008) 16562–16571; doi:10.1021/ja8030104

data_4108784
_publ_section_title
;
 Mechanistic Studies of the Hydroamination of Norbornene with
 Electrophilic Platinum Complexes: The Role of Proton Transfer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16562
_journal_page_last               16571
_journal_paper_doi               10.1021/ja8030104
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C56 H76 N6 O4 Pt2 S2, C2 F6 O6 S2, C H2 Cl2'
_chemical_formula_sum            'C59 H78 Cl2 F6 N6 O10 Pt2 S4'
_chemical_formula_weight         1734.6
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.69(3)
_cell_angle_beta                 106.84(3)
_cell_angle_gamma                96.14(2)
_cell_formula_units_Z            2
_cell_length_a                   11.779(3)
_cell_length_b                   16.296(4)
_cell_length_c                   20.316(8)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    141(2)
_cell_measurement_theta_max      24.67
_cell_measurement_theta_min      2.24
_cell_volume                     3614(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       \w/2\q-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  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20696
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.127
_exptl_absorpt_correction_T_max  0.8862
_exptl_absorpt_correction_T_min  0.8202
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       block
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.414
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         12158
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+12.1939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                10287
_reflns_number_total             12158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8030104_si_003.cif
_cod_data_source_block           bubpyso0
_cod_original_cell_volume        3613.7(19)
_cod_database_code               4108784