Selective Formation of Functionalized Disiloxanes from Terphenylfluorosilanes
Pietschnig, Rudolf; Merz, Klaus; Organometallics 23 (2004) 1373–; doi:10.1021/om034193l

data_4076246
_publ_section_title
;
 Selective Formation of Functionalized Disiloxanes from
 Terphenylfluorosilanes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1373
_journal_paper_doi               10.1021/om034193l
_journal_volume                  23
_journal_year                    2004
_chemical_formula_moiety         'C52 H62 O Si2'
_chemical_formula_sum            'C52 H62 O Si2'
_chemical_formula_weight         759.20
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.065(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.251(2)
_cell_length_b                   13.0494(9)
_cell_length_c                   14.9190(10)
_cell_measurement_reflns_used    4727
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.67
_cell_volume                     4423.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device       'Bruker SMART/P4'
_diffrn_measurement_method       '\f scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10715
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0.06
_diffrn_standards_number         214
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                3275
_reflns_number_total             5088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om034193lsi20030925_081417.cif
_cod_data_source_block           RPMedisiloxan
_cod_original_cell_volume        4423.0(5)
_cod_database_code               4076246