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_4109228
_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         'C28 H40 K O10, 3(C8 Cl2 N2 O2), 4(C H2 Cl2)'
_chemical_formula_sum            'C56 H48 Cl14 K N6 O16'
_chemical_formula_weight         1596.40
_chemical_name_common            '[(benzo-15-crown-5)2 K] (DDQ)3, (CH2Cl2)x'
_chemical_name_systematic
; 
 Bis(benzo-15-crown-5) potassium dichlorodicyanobenzoquinonide,
 dichloromethane solvate
;
_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                99.396(2)
_cell_angle_beta                 110.047(3)
_cell_angle_gamma                102.147(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1118(15)
_cell_length_b                   16.378(2)
_cell_length_c                   18.010(2)
_cell_measurement_reflns_used    275
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.06
_cell_measurement_theta_min      1.56
_cell_volume                     3433.2(7)
_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 0.986
_diffrn_measured_fraction_theta_max 0.934
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52482
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.97
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Semi-empirical (SADABS procedure)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       plate
_exptl_crystal_F_000             1622
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         20384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1107P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                11163
_reflns_number_total             20384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja069149msi20061220_055531.cif
_cod_data_source_block           ros19
_cod_original_cell_volume        3433.3(7)
_cod_database_code               4109228