Chiral Tetraaminophosphonium Carboxylate-Catalyzed Direct Mannich-Type Reaction
Daisuke Uraguchi; Yusuke Ueki; Takashi Ooi; Journal of the American Chemical Society 130 (2008) 14088–14089; doi:10.1021/ja806311e

data_4108562
_publ_section_title
;
 Chiral Tetraaminophosphonium Carboxylate-Catalyzed Direct Mannich-Type
 Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14088
_journal_page_last               14089
_journal_paper_doi               10.1021/ja806311e
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C40 H48 N2 O10 S'
_chemical_formula_weight         748.86
_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                 90.208(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.360(3)
_cell_length_b                   50.827(12)
_cell_length_c                   13.745(3)
_cell_measurement_reflns_used    7146
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     7936(3)
_computing_cell_refinement       'Bruker SMART'
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -65
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60804
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.9862
_exptl_absorpt_correction_T_min  0.8964
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       prism
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.275
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1963
_refine_ls_number_reflns         34870
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1013P)^2^+1.6652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1789
_reflns_number_gt                26803
_reflns_number_total             34870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806311e_si_002.cif
_cod_data_source_block           abs_config
_cod_database_code               4108562