Steric Modulations in the Reversible Dimerizations of Phenalenyl Radicals via Unusually Weak Carbon-Centered π- and σ-Bonds
V. Zaitsev; S. V. Rosokha; M. Head-Gordon; J. K. Kochi; Journal of Organic Chemistry 71 (2006) 520–526; doi:10.1021/jo051612a

data_4021381
_publ_section_title
;
 Steric Modulations in the Reversible Dimerizations of Phenalenyl
 Radicals via Unusually Weak Carbon-Centered \p- and \s-Bonds
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              520
_journal_page_last               526
_journal_paper_doi               10.1021/jo051612a
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C21 H25, C24 B F20'
_chemical_formula_sum            'C45 H25 B F20'
_chemical_formula_weight         956.46
_chemical_name_common            'DBPhen B(C6F5)4'
_chemical_name_systematic
;
  1,5-Di-tert-butyl-phenalenyl tetrakis(pentafluorophenyl)borate
;
_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                 92.162(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6171(10)
_cell_length_b                   15.4337(12)
_cell_length_c                   17.8177(14)
_cell_measurement_reflns_used    247
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.14
_cell_measurement_theta_min      2.88
_cell_volume                     4016.7(5)
_computing_cell_refinement       'SAINT V6.28 (BrukerAXS, 1997-2001)'
_computing_data_collection       'SMART V5.630 (BrukerAXS, 1997-2001)'
_computing_data_reduction        'SAINT & SADABS V2.06 (Sheldrick, 2000)'
_computing_molecular_graphics    'XP V5.06 (BrukerAXS, 1997-99)'
_computing_publication_material  'SHELXL-93, XCIF V5.05 (BrukerAXS, 1997-99)'
_computing_structure_refinement  'SHELXTL v. 6.12 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL v. 6.12 (Sheldrick, 2001)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method
;
\w-scan, frame range 0.3 deg, hemisphere
;
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33786
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Semi-empirical (SADABS procedure)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.156
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         11893
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                4779
_reflns_number_total             11893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo051612asi20050803_090015.cif
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4021381