Reactions of [o-(Fluorodimethylsilyl)phenyl]lithium with GeCl2and SnCl2: Preparation of Polyfunctionalized Four-Membered and Five-Membered Cyclic Linkages of Heavier Group 14 Elements
Kawachi, Atsushi; Machida, Koji; Yamamoto, Yohsuke; Organometallics 28 (2009) 6347–; doi:10.1021/om900694u

data_4070264
_publ_section_title
;
 Reactions of [o-(Fluorodimethylsilyl)phenyl]lithium with GeCl2and SnCl2:
 Preparation of Polyfunctionalized Four-Membered and Five-Membered Cyclic
 Linkages of Heavier Group 14 Elements
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6347
_journal_paper_doi               10.1021/om900694u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C43 H50 F5 Li Si5 Sn2'
_chemical_formula_sum            'C43 H50 F5 Li Si5 Sn2'
_chemical_formula_weight         1046.60
_chemical_melting_point          469
_chemical_name_common            Benzosiladistannacyclopentene
_chemical_name_systematic
;4,5-Benzo-2,2,3,3-tetrakis[(2-fluorodimethylsilyl)phenyl]-1,1-
dimethyl-1-sila-2,3-distannacyclopent-4-ene 
 ? 
;
_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                 90.8900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8690(2)
_cell_length_b                   16.6950(3)
_cell_length_c                   26.2210(3)
_cell_measurement_reflns_used    11577
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.45
_cell_volume                     5195.14(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  DIP2030
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1050
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11577
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.654
_refine_diff_density_min         -2.232
_refine_diff_density_rms         0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         11577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.586
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+2.1824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                10809
_reflns_number_total             11577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900694u_si_002.cif
_cod_data_source_block           Benzodistannacyclopent-4-ene
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4070264