Synthesis of Silicon-Functionalized (Silylmethyl)silanes and α,ω-Dichlorocarbosilanes Using the TMOP (2,4,6-Trimethoxyphenyl) Protecting Group: (TMOP)Me2SiCH2Cl and (TMOP)2MeSiCH2Cl as Reagents To Introduce the ClMe2SiCH2, MeOMe2SiCH2, or Cl2MeSiCH2 Group by Nucleophilic Substitution at Silicon
Laskowski, Nadine; Reis, Eva-Maria; Kötzner, Lisa; Baus, Johannes A.; Burschka, Christian; Tacke, Reinhold; Organometallics 32 (2013) 3269–; doi:10.1021/om400190q

data_4089445
_publ_section_title
;
 Synthesis of Silicon-Functionalized (Silylmethyl)silanes and
 \a,\w-Dichlorocarbosilanes Using the TMOP (2,4,6-Trimethoxyphenyl)
 Protecting Group: (TMOP)Me2SiCH2Cl and (TMOP)2MeSiCH2Cl as Reagents To
 Introduce the ClMe2SiCH2, MeOMe2SiCH2, or Cl2MeSiCH2 Group by
 Nucleophilic Substitution at Silicon
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3269
_journal_paper_doi               10.1021/om400190q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C13 H22 Cl2 O3 Si2'
_chemical_formula_sum            'C13 H22 Cl2 O3 Si2'
_chemical_formula_weight         353.39
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                106.910(6)
_cell_angle_beta                 100.409(6)
_cell_angle_gamma                97.462(6)
_cell_formula_units_Z            2
_cell_length_a                   8.136(3)
_cell_length_b                   8.797(3)
_cell_length_c                   13.306(5)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.13
_cell_measurement_theta_min      2.59
_cell_volume                     879.2(6)
_computing_cell_refinement       Bruker-SAINT
_computing_data_collection       Bruker-SAINT
_computing_data_reduction        Bruker-SAINT
_computing_molecular_graphics    Ortep/Povray
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Bruker-Nonius_Kappa_Apex2_CCD
_diffrn_measurement_method       omega_and_phi_scans
_diffrn_radiation_monochromator  MONTEL_multi_layer_optics
_diffrn_radiation_source         rotating_anode
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38749
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  .7460
_exptl_absorpt_correction_T_min  .6641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .05
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.354
_refine_diff_density_rms
'0.049 -1 0 0 21.50 0.40 -1 0 0 21.54 0.41 -1 0 0 21.33 0.46 -1 0 0 21.31 0.41 -1 0 0 21.59 0.45 -1 0 0 21. 0.00'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         5169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.3084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                4642
_reflns_number_total             5169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400190q_si_001.cif
_cod_data_source_block           las10d
_cod_original_cell_volume        879.1(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089445