Reversal of Enantioselectivity in the Hydroformylation of Styrene with [2S,4S-BDPP]Pt(SnCl3)Cl at High Temperature Arises from a Change in the Enantioselective-Determining Step
Charles P. Casey; Susie C. Martins; Maureen A. Fagan; Journal of the American Chemical Society 126 (2004) 5585–5592; doi:10.1021/ja0318479

data_4112524
_publ_contact_author
; 
   Prof. Charles P. Casey 
   Department of Chemistry 
   University of Wisconsin 
   1101 University Ave. 
   Madison, WI  53706-1396  USA 
;
_publ_contact_author_email       casey@chem.wisc.edu
_publ_contact_author_fax         1(608)2620381
_publ_contact_author_phone       1(608)2620584
_publ_section_title
;
 Reversal of Enantioselectivity in the Hydroformylation of Styrene with
 [2S,4S-BDPP]Pt(SnCl3)Cl at High Temperature Arises from a Change in the
 Enantioselective-Determining Step
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5585
_journal_page_last               5592
_journal_paper_doi               10.1021/ja0318479
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C29 H30 Cl4 P2 Pt Sn'
_chemical_formula_sum            'C29 H30 Cl4 P2 Pt Sn'
_chemical_formula_weight         896.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   9.4421(12)
_cell_length_b                   18.289(2)
_cell_length_c                   55.173(7)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     9528(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device       'Bruker SMART/Platform'
_diffrn_measurement_method       '\w scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1228
_diffrn_reflns_av_sigmaI/netI    0.2491
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            42876
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.58
_diffrn_reflns_theta_min         4.70
_diffrn_standards_decay_%        -0.10
_diffrn_standards_number         377
_exptl_absorpt_coefficient_mu    5.642
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       needle
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.868
_refine_diff_density_min         -2.666
_refine_diff_density_rms         0.234
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         18166
_refine_ls_number_restraints     3753
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.2092
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.2040
_reflns_number_gt                8021
_reflns_number_total             18166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0318479rom20031224_121051.cif
_cod_data_source_block           n98048
_cod_database_code               4112524