Scope and Mechanism of the Pt-Catalyzed Enantioselective Diboration of Monosubstituted Alkenes
John R. Coombs; Fredrik Haeffner; Laura T. Kliman; James P. Morken; Journal of the American Chemical Society 135 (2013) 11222–11231; doi:10.1021/ja4041016

data_4120200
_publ_section_title
;
 Scope and Mechanism of the Pt-Catalyzed Enantioselective Diboration of
 Monosubstituted Alkenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11222
_journal_page_last               11231
_journal_paper_doi               10.1021/ja4041016
_journal_volume                  135
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C90 H98 Cl2 O8 P2 Pt'
_chemical_formula_sum            'C90 H98 Cl2 O8 P2 Pt'
_chemical_formula_weight         1635.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 113.170(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.342(5)
_cell_length_b                   20.400(6)
_cell_length_c                   23.191(7)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.22
_cell_volume                     7978(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0926
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            114289
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_correction_T_min  0.8310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. (2008). SADABS v2008/1. Bruker AXS Inc. Madison, WI USA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.383
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(3)
_refine_ls_extinction_coef       na
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1810
_refine_ls_number_reflns         38325
_refine_ls_number_restraints     1651
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                33128
_reflns_number_total             38325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4041016_si_002.cif
_cod_data_source_block           C90H98Cl2O8P2Pt
_cod_original_cell_volume        7977(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4120200