One-step conversion of methoxysilanes to aminosilanes: a convenient synthetic strategy to N,O-functionalised organosilanes
Bauer, Jonathan O.; Strohmann, Carsten; Chemical Communications 48 (2012) 7212–7214; doi:10.1039/c2cc32727a

data_7107975
_publ_section_title
;
 One-step conversion of methoxysilanes to aminosilanes: a convenient
 synthetic strategy to N,O-functionalised organosilanes
;
_journal_issue                   57
_journal_name_full               'Chemical Communications'
_journal_page_first              7212
_journal_page_last               7214
_journal_paper_doi               10.1039/c2cc32727a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C31 H28 O2 Si2'
_chemical_formula_sum            'C31 H28 O2 Si2'
_chemical_formula_weight         488.71
_chemical_name_systematic
;
1-Methoxy-1,1,3,3,3-pentaphenyldisiloxane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-04-02T17:47:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.523(3)
_cell_angle_beta                 92.493(3)
_cell_angle_gamma                103.426(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1738(3)
_cell_length_b                   10.1328(4)
_cell_length_c                   16.4692(6)
_cell_measurement_reflns_used    5131
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      2.26
_cell_volume                     1307.80(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)'
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_molecular_graphics
;
Ortep-3 (Farrugia, 1997) and Schakal 92
(Keller 1992)
;
_computing_publication_material  'wingx (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Xcalibur S Oxford Diffraction'
_diffrn_measurement_method       Omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22177
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd. Empirical absorption correction using
spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.068
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                3603
_reflns_number_total             5131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32727a.txt
_cod_data_source_block           1802
_cod_database_code               7107975