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_4107404
_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         'C8 Br2 N2 O2'
_chemical_formula_sum            'C8 Br2 N2 O2'
_chemical_formula_weight         315.92
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.395(8)
_cell_length_b                   6.057(2)
_cell_length_c                   18.058(9)
_cell_measurement_reflns_used    634
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.09
_cell_measurement_theta_min      2.25
_cell_volume                     1793.2(14)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT & SADABS (Bruker, 2003)'
_computing_molecular_graphics    'XP (Bruker, 1999)'
_computing_publication_material  'SHELXL, XCIF (Bruker, 1999)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.981
_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  0.1178
_diffrn_reflns_av_sigmaI/netI    0.1082
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11731
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.28
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    9.010
_exptl_absorpt_correction_T_max  0.3451
_exptl_absorpt_correction_T_min  0.2659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.340
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                1362
_reflns_number_total             2635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076591b-file003.cif
_cod_data_source_block           alm14
_cod_original_cell_volume        1793.2(13)
_cod_database_code               4107404