Syntheses of Trisila Analogues of Allyl Chlorides and Their Transformations to Chlorocyclotrisilanes, Cyclotrisilanides, and a Trisilaindane
Kai Abersfelder; David Scheschkewitz; Journal of the American Chemical Society 130 (2008) 4114–4121; doi:10.1021/ja711169w

data_4107597
_publ_contact_author_address
;
Dr. David Scheschkewitz
Institute for Inorganic Chemistry
Julius-Maximilians-University
Am Hubland
97074 W\"urzburg
GERMANY
;
_publ_contact_author_email       scheschkewitz@mail.uni-wuerzburg.de
_publ_contact_author_fax         +49-931-888-4623
_publ_contact_author_name        'Dr. David Scheschkewitz'
_publ_contact_author_phone       +49-931-888-4788
_publ_section_title
;
 Syntheses of Trisila Analogues of Allyl Chlorides and Their
 Transformations to Chlorocyclotrisilanes, Cyclotrisilanides, and a
 Trisilaindane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4114
_journal_page_last               4121
_journal_paper_doi               10.1021/ja711169w
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C57 H79 Cl Si3, C4 H8 O'
_chemical_formula_sum            'C61 H87 Cl O Si3'
_chemical_formula_weight         956.03
_chemical_name_common            Tip3Ph2-Chlorocyclotrisilan
_chemical_name_systematic
; 
 [S]-1-Chlor-1,2,2-tris(2',4',6'-triisopropylphenyl)-3,3-diphenylcyclotrisilan 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   10.8740(5)
_cell_length_b                   15.4908(8)
_cell_length_c                   34.2768(17)
_cell_measurement_reflns_used    7388
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.22
_cell_volume                     5773.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    POV-Ray
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            46564
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.7916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), 4523 Friedel pairs'
_refine_ls_abs_structure_Flack   0.09(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.307
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         10194
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.302
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+4.5577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                10029
_reflns_number_total             10194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711169w-file005.cif
_cod_data_source_block           final
_cod_database_code               4107597