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_4107403
_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, 2(C8 Br2 N2 O2)'
_chemical_formula_sum            'C32 H32 Br4 N4 Na O12'
_chemical_formula_weight         1007.25
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.035(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.655(3)
_cell_length_b                   10.451(3)
_cell_length_c                   13.937(3)
_cell_measurement_reflns_used    2237
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.18
_cell_measurement_theta_min      2.44
_cell_volume                     1836.2(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.965
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.1283
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17712
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    4.463
_exptl_absorpt_correction_T_max  0.6638
_exptl_absorpt_correction_T_min  0.3478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_description       plate
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.476
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         10331
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                6384
_reflns_number_total             10331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076591b-file002.cif
_cod_data_source_block           alm07
_cod_original_cell_volume        1836.1(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4107403