Room-Temperature Synthesis of Trisubstituted Allenylsilanes via Regioselective C-H Functionalization
Rong Zeng; Shangze Wu; Chunling Fu; Shengming Ma; Journal of the American Chemical Society 135 (2013) 18284–18287; doi:10.1021/ja409861s

data_4121293
_publ_section_title
;
 Room-Temperature Synthesis of Trisubstituted Allenylsilanes via
 Regioselective C-H Functionalization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18284
_journal_page_last               18287
_journal_paper_doi               10.1021/ja409861s
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C24 H31 N O Si'
_chemical_formula_sum            'C24 H31 N O Si'
_chemical_formula_weight         377.59
_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_method           SHELXL-97
_cell_angle_alpha                103.609(17)
_cell_angle_beta                 94.386(16)
_cell_angle_gamma                108.491(17)
_cell_formula_units_Z            2
_cell_length_a                   9.1348(16)
_cell_length_b                   10.404(2)
_cell_length_c                   13.375(3)
_cell_measurement_reflns_used    1173
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5069
_cell_measurement_theta_min      2.9948
_cell_volume                     1155.8(4)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7410
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.9580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     528
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1562
_refine_ls_R_factor_gt           0.0934
_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^)+(0.1597P)^2^+0.3764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2574
_refine_ls_wR_factor_ref         0.3161
_reflns_number_gt                2214
_reflns_number_total             4212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409861s_si_001.cif
_cod_data_source_block           130625_wsz_2_29
_cod_database_code               4121293