Charge-Localized p-Phenylenedihydrazine Radical Cations: ESR and Optical Studies of Intramolecular Electron Transfer Rates
Stephen F. Nelsen; Rustem F. Ismagilov; Douglas R. Powell; Journal of the American Chemical Society 119 (1997) 10213–10222; doi:10.1021/ja9720321

data_4117043
_publ_contact_author
; 
    Prof. Stephen F. Nelsen 
    Department of Chemistry 
    University of Wisconsin 
    Madison, WI  53706-1396  USA 
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_publ_contact_author_email       nelsen@chem.wisc.edu
_publ_contact_author_fax         1(608)2620381
_publ_contact_author_phone       1(608)2623426
_publ_section_title
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 Charge-Localized p-Phenylenedihydrazine Radical Cations: ESR and Optical
 Studies of Intramolecular Electron Transfer Rates
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10213
_journal_page_last               10222
_journal_paper_doi               10.1021/ja9720321
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C54 H70 B N4'
_chemical_formula_weight         785.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.102(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7130(3)
_cell_length_b                   9.6069(2)
_cell_length_c                   23.0974(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.0
_cell_volume                     4524.85(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi scan frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16640
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        -0.54
_diffrn_standards_number         286
_exptl_absorpt_coefficient_mu    0.066
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       'opaque prism'
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.178
_refine_ls_goodness_of_fit_obs   1.208
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         7722
_refine_ls_number_restraints     422
_refine_ls_restrained_S_all      1.162
_refine_ls_restrained_S_obs      1.183
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_obs          0.0643
_refine_ls_shift/esd_max         -0.021
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+4.9004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1524
_refine_ls_wR_factor_obs         0.1372
_reflns_number_observed          6158
_reflns_number_total             7726
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9720321_4.cif
_cod_data_source_block           compound_4+BPh4-
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+4.9004P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+4.9004P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4117043