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_4107599
_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_formula_moiety         'C57 H79 Si3, C14 H28 Li N2 O4, C7 H8'
_chemical_formula_sum            'C78 H115 Li N2 O4 Si3'
_chemical_formula_weight         1235.93
_chemical_name_common            SSIP-Diphenylcyclotrisilanide
_chemical_name_systematic
; 
 [Lithum(Cryptand-2.1.1)][3,3-Diphenyl-1,2,2-(2',4',6'-
 triisopropylphenyl)cyclotrisilan-1-ide] 
;
_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                84.8470(10)
_cell_angle_beta                 86.0650(10)
_cell_angle_gamma                85.1380(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0569(4)
_cell_length_b                   16.6258(4)
_cell_length_c                   17.0696(5)
_cell_measurement_reflns_used    9225
_cell_measurement_temperature    97(2)
_cell_volume                     3670.28(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  POV-RAY
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      97(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            232386
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.920515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         14989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0295P)^2^+2.5304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                13028
_reflns_number_total             14989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja711169w-file007.cif
_cod_data_source_block           sad
_cod_database_code               4107599