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_4066931
_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         'C22 H64 Si9'
_chemical_formula_sum            'C22 H64 Si9'
_chemical_formula_weight         581.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.836(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.138(2)
_cell_length_b                   13.614(2)
_cell_length_c                   18.046(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      6.2
_cell_volume                     3955.9(9)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  Stoe-IPDS_image_plate
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58711
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.976
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .5
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         10362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0596P)^2^+0.2742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                8108
_reflns_number_total             10362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100721t_si_002.cif
_cod_data_source_block           ber02g_Compound_6
_cod_original_cell_volume        3955.9(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4066931