Catalytic asymmetric construction of tetrasubstituted carbon stereocenters by conjugate addition of dialkyl phosphine oxides to B,B-disubstituted a,B-unsaturated carbonyl compounds
Depeng Zhao; Lijuan Mao; Linqing Wang; Dongxu Yang; Rui Wang; Chem.Commun. 48 (2012) 889–; doi:10.1039/c1cc16079f

data_7107199
_publ_section_title
;
 Catalytic asymmetric construction of tetrasubstituted carbon
 stereocenters by conjugate addition of dialkyl phosphine oxides to
 B,B-disubstituted a,B-unsaturated carbonyl compounds
;
_journal_name_full               Chem.Commun.
_journal_page_first              889
_journal_paper_doi               10.1039/c1cc16079f
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration none
_chemical_formula_sum            'C20 H25 O2 P'
_chemical_formula_weight         328.37
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.410(5)
_cell_length_b                   13.410(5)
_cell_length_c                   8.943(5)
_cell_measurement_reflns_used    780
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.81
_cell_measurement_theta_min      2.87
_cell_volume                     1392.7(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.1118
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6187
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.9578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3064
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                1806
_reflns_number_total             3064
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc16079f.txt
_cod_data_source_block           p31
_cod_original_cell_volume        1392.8(10)
_cod_original_sg_symbol_H-M      P3(1)
_cod_database_code               7107199