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_4114564
_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_sum            'C42 H42 Si5'
_chemical_formula_weight         687.21
_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                94.279(2)
_cell_angle_beta                 94.337(2)
_cell_angle_gamma                99.094(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7130(10)
_cell_length_b                   13.4592(14)
_cell_length_c                   13.6979(13)
_cell_measurement_temperature    173(2)
_cell_volume                     1937.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7264
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9390
_exptl_absorpt_correction_T_min  0.9011
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0852P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                5359
_reflns_number_total             7264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja011821m_3.cif
_cod_data_source_block           west16
_cod_database_code               4114564