Synthesis and Characterization of {[Tris(trimethylsilyl)silyl]methyl}silanes of the Formula Type Me4−nSi[CH2Si(SiMe3)3]n(n= 1−3) and Derivatives
Berkefeld, André; Troegel, Dennis; Burschka, Christian; Tacke, Reinhold; Organometallics 29 (2010) 4548–; doi:10.1021/om100721t

data_4066932
_publ_section_title
;
 Synthesis and Characterization of
 {[Tris(trimethylsilyl)silyl]methyl}silanes of the Formula Type
 Me4&#x2212;nSi[CH2Si(SiMe3)3]n(n= 1&#x2212;3) and Derivatives
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4548
_journal_paper_doi               10.1021/om100721t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C31 H90 Si13, 0.45786( C4 H10 O)'
_chemical_formula_sum            'C32.83 H94.58 O0.45 Si13'
_chemical_formula_weight         862.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.156(4)
_cell_length_b                   14.3086(17)
_cell_length_c                   34.201(5)
_cell_measurement_reflns_used    4997
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.6
_cell_volume                     11821(3)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            150836
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.8437
_exptl_absorpt_correction_T_min  0.7437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .5
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         28371
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0548
_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^)+(0.0724P)^2^+0.6252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1126
_reflns_number_gt                23806
_reflns_number_total             28371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100721t_si_002.cif
_cod_data_source_block           ber01c_Compound_7
_cod_depositor_comments
;

2025-11-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C65.66 H189.16 O0.91 Si26'
_cod_original_formula_weight         1724.26
_cod_original_formula_moiety
'C31 H90 Si13, C31 H90 Si13,  0.91572( C4 H10 O)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               4066932