Rapid, One-Pot Synthesis of β-Siloxy-α-haloaldehydes
Jakub Saadi; Matsujiro Akakura; Hisashi Yamamoto; Journal of the American Chemical Society 133 (2011) 14248–14251; doi:10.1021/ja2066169

data_4106763
_publ_section_title
;
 Rapid, One-Pot Synthesis of \b-Siloxy-\a-haloaldehydes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14248
_journal_page_last               14251
_journal_paper_doi               10.1021/ja2066169
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C36 H70 Br F N2 O8 Si8'
_chemical_formula_weight         982.57
_chemical_name_systematic
; 
 (1SR,2SR,3SR,4RS)-4-bromo-2,4-dideoxy-5-O-(2,3-dinitrobenzoyl)
-2-fluoro-1-C-phenyl-1,3-bis-O-[tris(trimethylsilyl)silyl]pentitol  
;
_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                97.960(7)
_cell_angle_beta                 98.905(8)
_cell_angle_gamma                101.953(7)
_cell_formula_units_Z            2
_cell_length_a                   10.133(4)
_cell_length_b                   14.885(6)
_cell_length_c                   18.339(8)
_cell_measurement_temperature    100(2)
_cell_volume                     2631.5(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0664
_diffrn_reflns_av_sigmaI/netI    0.1202
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25564
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.7936
_exptl_absorpt_correction_T_min  0.6428
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.282
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1789
_reflns_number_gt                5080
_reflns_number_total             9360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2066169_si_001.cif
_cod_data_source_block           saad04s
_cod_original_cell_volume        2631(2)
_cod_database_code               4106763