Double diastereoselection in anti aldol reactions mediated by dicyclohexylchloroborane between an l-erythrulose derivative and chiral aldehydes.
Díaz-Oltra, Santiago; Ruiz, Purificación; Falomir, Eva; Murga, Juan; Carda, Miguel; Marco, J. Alberto; Organic & biomolecular chemistry 10 (2012) 6937–6944; doi:10.1039/c2ob25803j

data_7152556
_publ_section_title
;
 Double diastereoselection in anti aldol reactions mediated by
 dicyclohexylchloroborane between an l-erythrulose derivative and chiral
 aldehydes.
;
_journal_issue                   34
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6937
_journal_page_last               6944
_journal_paper_doi               10.1039/c2ob25803j
_journal_volume                  10
_journal_year                    2012
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C40 H61 N O6 Si2'
_chemical_formula_sum            'C40 H61 N O6 Si2'
_chemical_formula_weight         708.08
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4889(15)
_cell_length_b                   12.379(3)
_cell_length_c                   45.450(9)
_cell_measurement_reflns_used    4244
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      2.43
_cell_volume                     4213.4(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.2246
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            31100
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         0.90
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fiber
_exptl_crystal_F_000             1536
_exptl_crystal_recrystallization_method 'MeOH, CH2Cl2'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.743
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         22377
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.2755
_refine_ls_R_factor_gt           0.1152
_refine_ls_shift/su_max          0.269
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1834P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2810
_refine_ls_wR_factor_ref         0.3674
_reflns_number_gt                8381
_reflns_number_total             22377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob25803j.txt
_cod_data_source_block           p21z2
_cod_original_cell_volume        4213.4(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7152556