Controlling stereochemistry in polyketide synthesis: 1,3- vs. 1,2-asymmetric induction in methyl ketone aldol additions to β-super siloxy aldehydes
Brady, Patrick B.; Albert, Brian J.; Akakura, Matsujiro; Yamamoto, Hisashi; Chemical Science 4 (2013) 3223–; doi:10.1039/c3sc51183a

data_1514752
_publ_section_title
;
 Controlling stereochemistry in polyketide synthesis: 1,3- vs.
 1,2-asymmetric induction in methyl ketone aldol additions to \b-super
 siloxy aldehydes
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              3223
_journal_paper_doi               10.1039/c3sc51183a
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C47 H97 N O6 S Si9'
_chemical_formula_weight         1057.13
_space_group_IT_number           2
_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                110.618(7)
_cell_angle_beta                 111.892(6)
_cell_angle_gamma                93.200(6)
_cell_formula_units_Z            2
_cell_length_a                   13.583(4)
_cell_length_b                   15.995(5)
_cell_length_c                   16.961(5)
_cell_measurement_temperature    100(2)
_cell_volume                     3125.1(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.0970
_diffrn_reflns_av_sigmaI/netI    0.2319
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37882
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.9689
_exptl_absorpt_correction_T_min  0.9015
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.726
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         15162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.726
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                6006
_reflns_number_total             15162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc51183a.txt
_cod_data_source_block           brady11s
_cod_original_cell_volume        3125.1(17)
_cod_database_code               1514752