A Disilapentalene and a Stable Diradical from the Reaction of a Dilithiosilole with a Dichlorocyclopropene
Irina S. Toulokhonova; Thomas C. Stringfellow; Sergei A. Ivanov; Artem Masunov; Robert West; Journal of the American Chemical Society 125 (2003) 5767–5773; doi:10.1021/ja020763h

data_4113721
_publ_contact_author
; 
   Prof. Robert West
   Department of Chemistry 
   University of Wisconsin 
   1101 University Ave. 
   Madison, WI  53706-1396  USA 
;
_publ_contact_author_email       west@chem.wisc.edu
_publ_contact_author_fax         1(608)2620381
_publ_contact_author_phone       1(608)2621873
_publ_section_title
;
 A Disilapentalene and a Stable Diradical from the Reaction of a
 Dilithiosilole with a Dichlorocyclopropene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5767
_journal_page_last               5773
_journal_paper_doi               10.1021/ja020763h
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         '(C43 H60 Si2) 2(C6 H6)'
_chemical_formula_sum            'C98 H72 Si2'
_chemical_formula_weight         1305.74
_chemical_melting_point          633(1)
_chemical_name_common            1,4-disila-1,4-dihydropentalene
_chemical_name_systematic
; 
 1,4-disila-1,4-dihydropentalene  
;
_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                 92.539(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4525(6)
_cell_length_b                   25.5330(16)
_cell_length_c                   13.6438(8)
_cell_measurement_reflns_used    4556
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.18
_cell_volume                     3637.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_method       '\w 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  0.1081
_diffrn_reflns_av_sigmaI/netI    0.1477
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19579
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0.13
_diffrn_standards_number         140
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.055
_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     506
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                3011
_reflns_number_total             6406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020763h.cif
_cod_data_source_block           1,4-disila-1,4-dihydropentalene
_cod_database_code               4113721