Formation of a Silylated 1-Silaallene via an Intermediate 1-Chloro-1-silaallene
Spirk, Stefan; Belaj, Ferdinand; Albering, Jörg H.; Pietschnig, Rudolf; Organometallics 29 (2010) 2981–; doi:10.1021/om100299w

data_4066119
_publ_section_title
;
 Formation of a Silylated 1-Silaallene via an Intermediate
 1-Chloro-1-silaallene
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2981
_journal_paper_doi               10.1021/om100299w
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         '2(C37 H52 Si2), C6 H6'
_chemical_formula_sum            'C80 H110 Si4'
_chemical_formula_weight         1184.04
_chemical_name_systematic
; 1-(2,6-dimesitylphenyl)-1,3-di(tert-butyl)-3-trimethylsilyl-1-sila-allene
benzene solvate (2:1)
;
_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           'manual edited SHELXL-97 .cif file'
_cell_angle_alpha                102.985(3)
_cell_angle_beta                 104.076(3)
_cell_angle_gamma                90.135(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8900(9)
_cell_length_b                   13.6503(9)
_cell_length_c                   23.2007(16)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.14
_cell_measurement_theta_min      2.41
_cell_volume                     3552.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62663
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         16042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0423P)^2^+5.6023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                14089
_reflns_number_total             16042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100299w_si_003.cif
_cod_data_source_block           SiCC
_cod_database_code               4066119