Isolable Silylene Anion Radical: Structural Characteristics in the Solid State and in Solution
Shigeyoshi Inoue; Masaaki Ichinohe; Akira Sekiguchi; Journal of the American Chemical Society 129 (2007) 6096–6097; doi:10.1021/ja0711314

data_4109421
_publ_section_title
;
 Isolable Silylene Anion Radical: Structural Characteristics in the Solid
 State and in Solution
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6096
_journal_page_last               6097
_journal_paper_doi               10.1021/ja0711314
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C34 H74 Li O8 Si3'
_chemical_formula_weight         702.14
_chemical_name_systematic
; 
 [Bis(1,4,7,10-tetraoxacyclododecane)lithium(I)] 
 1,1,3,3-tetra-tert-butyl-1,3-dimethyltrisilane-2-yl-2-ylide
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.236(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.1250(5)
_cell_length_b                   13.9720(4)
_cell_length_c                   34.8770(9)
_cell_measurement_reflns_used    43656
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.20
_cell_volume                     8343.1(4)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      120.0(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            43656
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       Cube
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.00103(12)
_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   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         10009
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.689
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+3.7381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                7762
_reflns_number_total             10009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0711314si20070216_043113.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4109421