Quinones as Electron Acceptors. X-Ray Structures, Spectral (EPR, UV-vis) Characteristics and Electron-Transfer Reactivities of Their Reduced Anion Radicals as Separated vs Contact Ion Pairs
Jian-Ming Lü; Sergiy V. Rosokha; Ivan S. Neretin; Jay K. Kochi; Journal of the American Chemical Society 128 (2006) 16708–16719; doi:10.1021/ja066471o

data_4111283
_publ_section_title
;
 Quinones as Electron Acceptors. X-Ray Structures, Spectral (EPR, UV-vis)
 Characteristics and Electron-Transfer Reactivities of Their Reduced Anion
 Radicals as Separated vs Contact Ion Pairs
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16708
_journal_page_last               16719
_journal_paper_doi               10.1021/ja066471o
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C18 H36 K N2 O6, C6 H4 O2'
_chemical_formula_sum            'C24 H40 K N2 O8'
_chemical_formula_weight         523.68
_chemical_name_common            '[Crypt K]+ BQ-'
_chemical_name_systematic
; 
 2,2,2-Cryptand potassium benzoquinonide
;
_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                91.18(14)
_cell_angle_beta                 99.91(17)
_cell_angle_gamma                92.50(18)
_cell_formula_units_Z            2
_cell_length_a                   9.178(18)
_cell_length_b                   11.08(3)
_cell_length_c                   13.54(3)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.42
_cell_measurement_theta_min      3.93
_cell_volume                     1355(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 0.982
_diffrn_measured_fraction_theta_max 0.976
_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  0.0770
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20203
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       needle
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         7756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                4818
_reflns_number_total             7756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066471osi20060907_103851.cif
_cod_data_source_block           lu4
_cod_database_code               4111283