Asymmetric Synthesis of All Eight Seven-Carbon Dipropionate Stereotetrads
Ahmad El-Awa; Xavier Mollat du Jourdin; Philip L. Fuchs; Journal of the American Chemical Society 129 (2007) 9086–9093; doi:10.1021/ja071217x

data_4109693
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     560 Oval Dr.
     W. Lafayette
     IN 47907-2084
     USA
;
_publ_contact_author_email       pfuchs@purdue.edu
_publ_contact_author_name        'Philip F. Fuchs'
_publ_contact_author_phone       '1(765) 4945242'
_publ_section_title
;
 Asymmetric Synthesis of All Eight Seven-Carbon Dipropionate Stereotetrads
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9086
_journal_page_last               9093
_journal_paper_doi               10.1021/ja071217x
_journal_volume                  129
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H34 O4 S1 Si1'
_chemical_formula_sum            'C21 H34 O4 S Si'
_chemical_formula_weight         410.65
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             19-02-07
_audit_creation_method           'SHELXL and local programs'
_audit_update_record             ' ?'
_cell_angle_alpha                87.798(5)
_cell_angle_beta                 86.717(6)
_cell_angle_gamma                64.962(5)
_cell_formula_units_Z            2
_cell_length_a                   6.6816(5)
_cell_length_b                   7.5785(7)
_cell_length_c                   25.490(2)
_cell_measurement_reflns_used    12219
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1167.37(17)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 1997)
;
_computing_publication_material  'SHELX97(Sheldrick, 1997) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution
;
 direct methods (SIR2004, Burla et al., 2005)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.7839
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.084
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12219
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_correction_T_min  0.9048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       needle
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.46
_refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         6374
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.072
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.1514P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.190
_refine_ls_wR_factor_ref         0.203
_reflns_Friedel_coverage         0.8748
_reflns_number_gt                5253
_reflns_number_total             6374
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ja071217xsi20070220_105400.cif
_cod_data_source_block           115654
_cod_original_sg_symbol_Hall     ' P 1'
_cod_original_formula_sum        'C21 H34 O4 S1 Si1'
_cod_database_code               4109693