Tris(trimethylsilyl)silyl-Governed Aldehyde Cross-Aldol Cascade Reaction
Matthew B. Boxer; Hisashi Yamamoto; Journal of the American Chemical Society 128 (2006) 48–49; doi:10.1021/ja054725k

data_4110328
_publ_section_title
;
 Tris(trimethylsilyl)silyl-Governed Aldehyde Cross-Aldol Cascade Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              48
_journal_page_last               49
_journal_paper_doi               10.1021/ja054725k
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C72 H160 N4 O10 S2 Si16'
_chemical_formula_weight         1755.60
_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                66.357(4)
_cell_angle_beta                 89.047(5)
_cell_angle_gamma                88.998(5)
_cell_formula_units_Z            2
_cell_length_a                   10.080(3)
_cell_length_b                   22.194(6)
_cell_length_c                   26.478(7)
_cell_measurement_temperature    100(2)
_cell_volume                     5425(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0948
_diffrn_reflns_av_sigmaI/netI    0.1497
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            52211
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_correction_T_min  0.9111
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         19048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.1058
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2316
_refine_ls_wR_factor_ref         0.2612
_reflns_number_gt                11634
_reflns_number_total             19048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054725ksi20050714_091222.cif
_cod_data_source_block           boxer10s
_cod_original_cell_volume        5425(2)
_cod_database_code               4110328