Mechanistic Study of β-Hydrogen Elimination from Organoplatinum(II) Enolate Complexes
Erik J. Alexanian; John F. Hartwig; Journal of the American Chemical Society 130 (2008) 15627–15635; doi:10.1021/ja8056908

data_4108679
_publ_section_title
;
 Mechanistic Study of \b-Hydrogen Elimination from Organoplatinum(II)
 Enolate Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15627
_journal_page_last               15635
_journal_paper_doi               10.1021/ja8056908
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C46 H42 O P2 Pt'
_chemical_formula_sum            'C46 H42 O P2 Pt'
_chemical_formula_weight         867.83
_chemical_name_systematic
; 
? 
;
_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
_audit_update_record
; 
2006-12-11    text and data added, mr 
;
_cell_angle_alpha                80.922(2)
_cell_angle_beta                 86.846(2)
_cell_angle_gamma                69.2990(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6235(3)
_cell_length_b                   12.6966(4)
_cell_length_c                   12.7120(3)
_cell_measurement_reflns_used    7609
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      48.655
_cell_measurement_theta_min      4.738
_cell_volume                     1882.01(9)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'APEX2 V1.0-27 (Bruker, 2004)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  g60oas
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23057
_diffrn_reflns_theta_full        25.70
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  0.7483
_exptl_absorpt_correction_T_min  0.5284
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
_exptl_crystal_id                g60oas
_exptl_crystal_preparation
; 
The data crystal was mounted using epoxy to a 0.3 mm cryo-loop 
(Hampton Research) with the (-3 -1 2) scattering planes roughly normal 
to the spindle axis. 
;
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.673
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+8.5806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                6110
_reflns_number_total             7124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8056908_si_002.cif
_cod_data_source_block           compound1
_cod_database_code               4108679