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_4070263
_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         'C24 H30 F2 Ge Si3'
_chemical_formula_sum            'C24 H30 F2 Ge Si3'
_chemical_formula_weight         513.34
_chemical_melting_point          401
_chemical_name_common            Benzosilagermacyclobutene
_chemical_name_systematic
;3,4-Benzo-2,2-bis[(2-fluorodimethylsilyl)phenyl]-1,1-
dimethyl-1-sila-2-germacyclobut-3-ene
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.4270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.1530(9)
_cell_length_b                   9.2050(2)
_cell_length_c                   9.8930(3)
_cell_measurement_reflns_used    6021
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.40
_cell_volume                     2654.75(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.1786
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10342
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.335
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.116(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.1054
_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^)+(0.1252P)^2^+27.1290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3062
_refine_ls_wR_factor_ref         0.3095
_reflns_number_gt                5350
_reflns_number_total             5982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900694u_si_001.cif
_cod_data_source_block           Benzosilagermacyclobutene-2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4070263