Continuum of Outer- and Inner-Sphere Mechanisms for Organic Electron Transfer. Steric Modulation of the Precursor Complex in Paramagnetic (Ion-Radical) Self-Exchanges
Sergiy V. Rosokha; Jay K. Kochi; Journal of the American Chemical Society 129 (2007) 3683–3697; doi:10.1021/ja069149m

data_4109229
_publ_section_title
;
 Continuum of Outer- and Inner-Sphere Mechanisms for Organic Electron
 Transfer. Steric Modulation of the Precursor Complex in Paramagnetic
 (Ion-Radical) Self-Exchanges
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3683
_journal_page_last               3697
_journal_paper_doi               10.1021/ja069149m
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C13 H36 B11, C10 H14 O2'
_chemical_formula_sum            'C23 H50 B11 O2'
_chemical_formula_weight         477.54
_chemical_name_systematic
; 
 ? 
;
_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                74.14(3)
_cell_angle_beta                 66.70(3)
_cell_angle_gamma                87.18(3)
_cell_formula_units_Z            1
_cell_length_a                   9.142(8)
_cell_length_b                   9.238(5)
_cell_length_c                   10.094(7)
_cell_measurement_reflns_used    1439
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.17
_cell_measurement_theta_min      2.29
_cell_volume                     751.5(10)
_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. 6.14 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL v. 6.14 (Sheldrick, 2001)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11133
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_description       plate
_exptl_crystal_F_000             259
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4353
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0634P)^2^+0.3085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                2356
_reflns_number_total             4353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja069149msi20061220_055547.cif
_cod_data_source_block           ros69
_cod_original_cell_volume        751.5(9)
_cod_database_code               4109229