Electron Transfer between Two Silyl-Substituted Phenylene Rings: EPR/ENDOR Spectra, DFT Calculations, and Crystal Structure of the One-Electron Reduction Compound of a Di(m-silylphenylenedisiloxane)
Cosmina Dutan; Sylvie Choua; Théo Berclaz; Michel Geoffroy; Nicolas Mézailles; Audrey Moores; Louis Ricard; Pascal Le Floch; Journal of the American Chemical Society 125 (2003) 4487–4494; doi:10.1021/ja0209060

data_4113649
_publ_contact_author             'Louis Ricard'
_publ_contact_author_address
;
                    Labo DCPH,
                    Ecole Polytechnique
                    Route de Saclay
                    91128 Palaiseau
                    France
;
_publ_contact_author_email       louis.ricard@polytechnique.fr
_publ_contact_author_fax         01-69-33-39-90
_publ_contact_author_phone       01-69-33-45-72
_publ_section_title
;
 Electron Transfer between Two Silyl-Substituted Phenylene Rings:
 EPR/ENDOR Spectra, DFT Calculations, and Crystal Structure of the
 One-Electron Reduction Compound of a Di(m-silylphenylenedisiloxane)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4487
_journal_page_last               4494
_journal_paper_doi               10.1021/ja0209060
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C40 H72 K O10 Si4'
_chemical_formula_weight         864.44
_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                72.950(5)
_cell_angle_beta                 87.140(5)
_cell_angle_gamma                81.820(5)
_cell_formula_units_Z            1
_cell_length_a                   10.268(5)
_cell_length_b                   10.604(5)
_cell_length_c                   11.829(5)
_cell_measurement_reflns_used    251
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      3.0
_cell_volume                     1218.8(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6308
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.9699
_exptl_absorpt_correction_T_min  0.9411
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       'plate '
_exptl_crystal_F_000             467
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0548P)^2^+0.5546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                3193
_reflns_number_total             3980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0209060_2.cif
_cod_data_source_block           cyclosim;compound6
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4113649