The lewis base-catalyzed silylation of alcohols-a mechanistic analysis.
Patschinski, Pascal; Zhang, Cong; Zipse, Hendrik; The Journal of organic chemistry 79 (2014) 8348–8357; doi:10.1021/jo5016568

data_4029848
_publ_section_title
;
 The lewis base-catalyzed silylation of alcohols-a mechanistic analysis.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              8348
_journal_page_last               8357
_journal_paper_doi               10.1021/jo5016568
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C6 H16 O Si, 0.5(H2 O)'
_chemical_formula_sum            'C6 H17 O1.5 Si'
_chemical_formula_weight         141.284
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_block_code                C6H16OSi_H2O_rv046_zipse
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             07-Feb-13
_cell_angle_alpha                90.00
_cell_angle_beta                 90.560(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.7122(4)
_cell_length_b                   22.1072(11)
_cell_length_c                   11.0668(6)
_cell_measurement_reflns_used    113
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.1854
_cell_measurement_theta_min      3.6727
_cell_volume                     1886.75(17)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_refinement
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'fixed-chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8Venture'
_diffrn_measurement_method       'mix of phi and omega scans'
_diffrn_radiation_collimation    0.8_mm
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35561
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         2.60
_diffrn_source_current           50
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    .99477(9)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+1.1005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                3492
_reflns_number_total             3851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo5016568_si_001.cif
_cod_data_source_block           rv046
_cod_depositor_comments          'Adding full bibliography for 4029848.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C6 H17 O1.50 Si'
_cod_database_code               4029848