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_4089444
_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         'C14 H25 Cl O3 Si2'
_chemical_formula_sum            'C14 H25 Cl O3 Si2'
_chemical_formula_weight         332.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                77.339(2)
_cell_angle_beta                 83.886(2)
_cell_angle_gamma                81.017(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2187(4)
_cell_length_b                   9.2752(4)
_cell_length_c                   12.1689(6)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.96
_cell_measurement_theta_min      2.52
_cell_volume                     891.46(7)
_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-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  Bruker_Kappa_Apex2_CCD
_diffrn_measurement_method       omega_scan
_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  0.0240
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33338
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.330
_diffrn_reflns_theta_min         1.720
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  .7462
_exptl_absorpt_correction_T_min  .6592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       diamond_shaped
_exptl_crystal_F_000             356
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .14
_exptl_transmission_factor_max   .7462
_exptl_transmission_factor_min   .6592
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         5369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.2628P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4957
_reflns_number_total             5369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400190q_si_001.cif
_cod_data_source_block           las011d
_cod_database_code               4089444
_shelxl_version_number           2012-9
_shelx_res_checksum
'86125 -1 0 0 298.34 7.21 -1 0 0 286.36 8.53 -1 0 0 288.60 7.64 -1 0 0 303.59 9.37 -1 0 0 302.81 8.00 -1 0  0.00'