New Class of Pyridine Catalyst Having a Conformation Switch System: Asymmetric Acylation of Various sec-Alcohols
Shinji Yamada; Tomoko Misono; Yuko Iwai; Ayako Masumizu; Yukiko Akiyama; Journal of Organic Chemistry 71 (2006) 6872–6880; doi:10.1021/jo060989t

data_4021935
_publ_section_title
;
 New Class of Pyridine Catalyst Having a Conformation Switch
 System: Asymmetric Acylation of Various sec-Alcohols
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6872
_journal_page_last               6880
_journal_paper_doi               10.1021/jo060989t
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C12 H16 Br N3 O S2'
_chemical_formula_weight         362.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.982(9)
_cell_angle_beta                 100.171(10)
_cell_angle_gamma                70.470(9)
_cell_formula_units_Z            2
_cell_length_a                   9.6935(11)
_cell_length_b                   11.6333(14)
_cell_length_c                   8.0350(11)
_cell_measurement_temperature    298(2)
_cell_volume                     805.17(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3952
_diffrn_reflns_theta_full        67.99
_diffrn_reflns_theta_max         67.99
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    5.875
_exptl_absorpt_correction_T_max  0.2717
_exptl_absorpt_correction_T_min  0.2022
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0.016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2759
_refine_ls_wR_factor_ref         0.2808
_reflns_number_gt                2747
_reflns_number_total             2874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo060989tsi20060512_024434.cif
_cod_database_code               4021935