How Delocalized IsN,N,N',N'-Tetraphenylphenylenediamine Radical Cation? An Experimental and Theoretical Study on the Electronic and Molecular Structure
Adriana V. Szeghalmi; Marco Erdmann; Volker Engel; Michael Schmitt; Stephan Amthor; Volker Kriegisch; Gilbert Nöll; Rainer Stahl; Christoph Lambert; Dirk Leusser; Dietmar Stalke; Manfred Zabel; Jürgen Popp; Journal of the American Chemical Society 126 (2004) 7834–7845; doi:10.1021/ja0395386

data_4112695
_publ_contact_author_address
;Prof. Dr. C. Lambert
Am Hubland
97074 W\"urzburg
Germany
;
_publ_contact_author_email       lambert@chemie.uni-wuerzburg.de
_publ_contact_author_fax         ++49(0)931-8884606
_publ_contact_author_name        'C. Lambert'
_publ_contact_author_phone       ++49(0)931-8885318
_publ_section_title
;
 How Delocalized IsN,N,N',N'-Tetraphenylphenylenediamine Radical Cation?
 An Experimental and Theoretical Study on the Electronic and Molecular
 Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7834
_journal_page_last               7845
_journal_paper_doi               10.1021/ja0395386
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source        'University of Regensburg'
_chemical_formula_moiety         'C30 H24 N2, 0.5(C4 H8 O), Cl6 Sb'
_chemical_formula_sum            'C32 H28 Cl6 N2 O0.5 Sb'
_chemical_formula_weight         783.02
_chemical_name_systematic
'[N,N,N',N'-Tetraphenylphenylendiamino+][SbCl6-)]-THF'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_cell_angle_alpha                90
_cell_angle_beta                 111.431(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.713(2)
_cell_length_b                   17.6662(10)
_cell_length_c                   18.0240(17)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      1.98
_cell_volume                     6732.1(11)
_computing_cell_refinement       'STOE (1998)'
_computing_data_collection       'STOE (1998)'
_computing_data_reduction        'STOE (1998)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE-IPDS diffractometer'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32276
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         1.93
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.32
_exptl_absorpt_correction_T_max  0.9221
_exptl_absorpt_correction_T_min  0.6041
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'numerical from crystal shape ( X-RED. STOE, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       'platelike rod'
_exptl_crystal_F_000             3128
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0608P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                3756
_reflns_number_total             6418
_reflns_threshold_expression     >4sigma(i)
_cod_data_source_file            ja0395386si20031118_044057.cif
_cod_data_source_block           00159
_cod_depositor_comments
;

2022-02-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C64 H56 Cl12 N4 O Sb2'
_cod_original_formula_weight         1566.05
_cod_original_formula_moiety         '2(C30 H24 N2), C4 H8 O, 2(Cl6 Sb)'
_cod_original_formula_units_Z            4
_cod_database_code               4112695