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_4110330
_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            'C39 H80 N2 O6 S Si8'
_chemical_formula_weight         929.83
_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                109.700(7)
_cell_angle_beta                 98.805(7)
_cell_angle_gamma                91.992(7)
_cell_formula_units_Z            4
_cell_length_a                   9.803(4)
_cell_length_b                   22.251(9)
_cell_length_c                   27.639(11)
_cell_measurement_temperature    100(2)
_cell_volume                     5585(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0868
_diffrn_reflns_av_sigmaI/netI    0.1496
_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       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            53909
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption corrections were made based on correspondance of
equivalent intensities usingprogram SADABS (G. Sheldrick, Bruker 
Analytical X-ray Systems, Madison, WI)
;
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         19676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          1.082
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                11387
_reflns_number_total             19676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054725ksi20051025_023813.cif
_cod_data_source_block           boxer13s
_cod_database_code               4110330