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_4109232
_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, C12 H9 N S, H2 O'
_chemical_formula_sum            'C25 H47 B11 N O S'
_chemical_formula_weight         528.61
_chemical_name_common            'PhTZ Car * H2O'
_chemical_name_systematic
; 
 Phenothiazolium dodecamethylcarboranate hydrate
;
_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                 100.382(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1694(12)
_cell_length_b                   19.703(3)
_cell_length_c                   17.610(3)
_cell_measurement_reflns_used    196
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.84
_cell_measurement_theta_min      2.35
_cell_volume                     3129.4(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.962
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47809
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.98
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         9582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1442P)^2^+0.6950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1974
_reflns_number_gt                7112
_reflns_number_total             9582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja069149msi20061220_055636.cif
_cod_data_source_block           ros31
_cod_database_code               4109232