Synthesis and Characterization of New Trifunctional Tetraorganylsilanes of the Formula Types MeSi(CH2X)3, MeSi(CH2X)2CH2X′, and MeSi(CH2X)(CH2X′)CH2X′′
Troegel, Dennis; Möller, Frank; Burschka, Christian; Tacke, Reinhold; Organometallics 28 (2009) 5765–; doi:10.1021/om9005577

data_4070007
_publ_section_title
;
 Synthesis and Characterization of New Trifunctional Tetraorganylsilanes
 of the Formula Types MeSi(CH2X)3, MeSi(CH2X)2CH2X&#x2032;, and
 MeSi(CH2X)(CH2X&#x2032;)CH2X&#x2032;&#x2032;
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5765
_journal_paper_doi               10.1021/om9005577
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C25 H30 O9 S3 Si'
_chemical_formula_sum            'C25 H30 O9 S3 Si'
_chemical_formula_weight         598.76
_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                88.88(3)
_cell_angle_beta                 87.78(3)
_cell_angle_gamma                76.12(3)
_cell_formula_units_Z            4
_cell_length_a                   12.673(3)
_cell_length_b                   15.215(3)
_cell_length_c                   15.689(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.
_cell_measurement_theta_min      6.35
_cell_volume                     2934.4(11)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    Ortep/Povray
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  image_plate_Stoe-IPDS
_diffrn_measurement_method       omega_scan
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42507
_diffrn_reflns_theta_full        29.10
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         14389
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0525P)^2^+0.5925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                10337
_reflns_number_total             14389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9005577_si_001.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        2934.7(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070007