Water-Coordinated Neutral Silane Complex: A Frozen Intermediate of Hydrolysis of Alkoxysilanes
Junji Kobayashi; Keiko Kawaguchi; Takayuki Kawashima; Journal of the American Chemical Society 126 (2004) 16318–16319; doi:10.1021/ja047249r

data_4113315
_publ_section_title
;
 Water-Coordinated Neutral Silane Complex: A Frozen Intermediate of
 Hydrolysis of Alkoxysilanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16318
_journal_page_last               16319
_journal_paper_doi               10.1021/ja047249r
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C38 H55 O5 Si'
_chemical_formula_weight         619.91
_chemical_melting_point          536(4)
_chemical_name_common            1-aquo-5-carbasilatrane
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(11)
_cell_angle_beta                 90.3493(11)
_cell_angle_gamma                90.0000(11)
_cell_formula_units_Z            4
_cell_length_a                   10.451(3)
_cell_length_b                   20.497(6)
_cell_length_c                   16.753(5)
_cell_measurement_temperature    130(2)
_cell_volume                     3588.7(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.551
_diffrn_measured_fraction_theta_max 0.551
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15473
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_correction_T_min  0.9493
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         4530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.193
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+4.7326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                3910
_reflns_number_total             4530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047249rsi20040511_115548.cif
_cod_data_source_block           silax
_cod_original_sg_symbol_H-M      ' P 1 21/n 1'
_cod_database_code               4113315