Stereocontrolled (Me3Si)3SiH-Mediated Radical and Ionic Hydride Transfer in Synthesis of 2,3,5-Trisubstituted THF.
Grélaud, Simon; Desvergnes, Valérie; Landais, Yannick; Organic letters 18 (2016) 1542–1545; doi:10.1021/acs.orglett.6b00303

data_1542993
_publ_section_title
;
 Stereocontrolled (Me3Si)3SiH-Mediated Radical and Ionic Hydride Transfer
 in Synthesis of 2,3,5-Trisubstituted THF.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1542
_journal_page_last               1545
_journal_paper_doi               10.1021/acs.orglett.6b00303
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C28 H40 O4 Si'
_chemical_formula_weight         468.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.879(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.8904(2)
_cell_length_b                   32.7758(6)
_cell_length_c                   18.3035(13)
_cell_measurement_reflns_used    7803
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.08
_cell_measurement_theta_min      6.33
_cell_volume                     5902.2(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku RAXIS Rapid'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50623
_diffrn_reflns_theta_full        70.08
_diffrn_reflns_theta_max         70.08
_diffrn_reflns_theta_min         6.33
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.9306
_exptl_absorpt_correction_T_min  0.8041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.00094(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         10921
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.339
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.7241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                7803
_reflns_number_total             10921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b00303_si_001.cif
_cod_data_source_block           sg570
_cod_depositor_comments
;

2019-08-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        5902.2(4)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C56 H80 O8 Si2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     937.38
_cod_database_code               1542993