The Spectral Elucidation versus the X-ray Structure of the Critical Precursor Complex in Bimolecular Electron Transfers: Application of Experimental/Theoretical Solvent Probes to Ion-Radical (Redox) Dyads
Sergiy V. Rosokha; Marshall D. Newton; Almaz S. Jalilov; Jay K. Kochi; Journal of the American Chemical Society 130 (2008) 1944–1952; doi:10.1021/ja076591b

data_4107405
_publ_section_title
;
 The Spectral Elucidation versus the X-ray Structure of the Critical
 Precursor Complex in Bimolecular Electron Transfers: Application of
 Experimental/Theoretical Solvent Probes to Ion-Radical (Redox) Dyads
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1944
_journal_page_last               1952
_journal_paper_doi               10.1021/ja076591b
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C16 H32 Na O8, C8 Br2 N2 O2'
_chemical_formula_sum            'C24 H32 Br2 N2 Na O10'
_chemical_formula_weight         691.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 106.861(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.429(2)
_cell_length_b                   16.066(3)
_cell_length_c                   16.214(3)
_cell_measurement_reflns_used    623
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.75
_cell_volume                     2849.2(9)
_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 0.992
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_method       'omega-scan, full sphere'
_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    0.0464
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13828
_diffrn_reflns_theta_full        29.80
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    2.917
_exptl_absorpt_correction_T_max  0.6688
_exptl_absorpt_correction_T_min  0.5931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0853P)^2^+1.9178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1730
_reflns_number_gt                2459
_reflns_number_total             4190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076591b-file004.cif
_cod_data_source_block           alm06
_cod_original_cell_volume        2849.3(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4107405