Structure and Chemistry of 1-Silafluorenyl Dianion, Its Derivatives, and an Organosilicon Diradical Dianion
Yuxia Liu; Thomas C. Stringfellow; David Ballweg; Ilia A. Guzei; Robert West; Journal of the American Chemical Society 124 (2002) 49–57; doi:10.1021/ja011821m

data_4114566
_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
;
 Structure and Chemistry of 1-Silafluorenyl Dianion, Its Derivatives, and
 an Organosilicon Diradical Dianion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              49
_journal_page_last               57
_journal_paper_doi               10.1021/ja011821m
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         '2K+ 2(C12 H8 Si)2- 4(C4 H8 O)'
_chemical_formula_sum            'C40 H48 K2 O4 Si2'
_chemical_formula_weight         727.16
_chemical_name_systematic
; 
 ? 
;
_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                 112.597(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4065(13)
_cell_length_b                   23.313(2)
_cell_length_c                   12.3328(11)
_cell_measurement_reflns_used    6376
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.32
_cell_volume                     3824.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  '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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17441
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0.08
_diffrn_standards_number         312
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8585
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1557
_reflns_number_gt                4833
_reflns_number_total             8585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011821m_5.cif
_cod_data_source_block           n99054a
_cod_database_code               4114566