New Multicomponent Approach for the Creation of Chiral Quaternary Centers in the Carbonyl Allylation Reactions
Genia Sklute; Ilan Marek; Journal of the American Chemical Society 128 (2006) 4642–4649; doi:10.1021/ja060498q

data_4110550
_publ_section_title
;
 New Multicomponent Approach for the Creation of Chiral Quaternary Centers
 in the Carbonyl Allylation Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4642
_journal_page_last               4649
_journal_paper_doi               10.1021/ja060498q
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C25 H34 O2 S'
_chemical_formula_sum            'C25 H34 O2 S'
_chemical_formula_weight         398.58
_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                 95.8100(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2320(4)
_cell_length_b                   9.0030(3)
_cell_length_c                   19.6340(7)
_cell_measurement_reflns_used    11402
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     2326.94(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius (1997), KappaCCD Collect Program'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics
;
Molecular Structure Corporation (1999). 
ORTEP. TEXRAY Structure Analysis Package. 
MSC, 3200 Research Forest Drive, The 
Woodlands,TX 77381, USA.
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland 
"maXus": a computer program for the solution and refinement of crystal 
structures from diffraction data University of Glasgow, Scotland, UK, 
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd.,
Yokohama, Japan (1998)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7708
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.9519
_exptl_absorpt_correction_T_min  0.9220
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         7708
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.2373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                3579
_reflns_number_total             7708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja060498qsi20060122_054844.cif
_cod_data_source_block           sotol
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4110550