One-Electron Reduction of Kinetically Stabilized Dipnictenes: Synthesis of Dipnictene Anion Radicals
Takahiro Sasamori; Eiko Mieda; Noriyoshi Nagahora; Kazunobu Sato; Daisuke Shiomi; Takeji Takui; Yoshinobu Hosoi; Yukio Furukawa; Nozomi Takagi; Shigeru Nagase; Norihiro Tokitoh; Journal of the American Chemical Society 128 (2006) 12582–12588; doi:10.1021/ja064062m

data_4110914
_publ_section_title
;
 One-Electron Reduction of Kinetically Stabilized Dipnictenes: Synthesis
 of Dipnictene Anion Radicals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12582
_journal_page_last               12588
_journal_paper_doi               10.1021/ja064062m
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C60 H134 Sb2 Si14, C12 H30 Li O6'
_chemical_formula_sum            'C72 H164 Li O6 Sb2 Si14'
_chemical_formula_weight         1769.73
_chemical_name_common            '2b anion'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 116.5601(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.8773(2)
_cell_length_b                   25.2561(3)
_cell_length_c                   14.9110(2)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.72
_cell_volume                     5011.42(11)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51264
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.9291
_exptl_absorpt_correction_T_min  0.8070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       brown
_exptl_crystal_F_000             1890
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9298
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0483P)^2^+14.2148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                8007
_reflns_number_total             9298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064062msi20060609_052254.cif
_cod_data_source_block           2banion
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4110914