Intramolecular Electron Transfer between Doubly Six σ-Bond-Linked Trialkyldiazenium Cation and Diazenyl Radical Units
Stephen F. Nelsen; Dwight A. Trieber; J. Jens Wolff; Douglas R. Powell; Shervalen Rogers-Crowley; Journal of the American Chemical Society 119 (1997) 6873–6882; doi:10.1021/ja9634177

data_4116993
_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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 Intramolecular Electron Transfer between Doubly Six \s-Bond-Linked
 Trialkyldiazenium Cation and Diazenyl Radical Units
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6873
_journal_page_last               6882
_journal_paper_doi               10.1021/ja9634177
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C73 H81 B2 N5'
_chemical_formula_weight         1050.05
_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
_cell_angle_alpha                79.020(2)
_cell_angle_beta                 76.686(2)
_cell_angle_gamma                76.421(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2781(2)
_cell_length_b                   12.2227(2)
_cell_length_c                   22.9815(2)
_cell_measurement_reflns_used    6450
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      3.0
_cell_volume                     2965.33(8)
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29259
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0.79
_diffrn_standards_number         204
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0011(5)
_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   1.065
_refine_ls_goodness_of_fit_obs   1.160
_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_parameters     750
_refine_ls_number_reflns         12715
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.155
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_obs          0.0648
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+2.1492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1670
_refine_ls_wR_factor_obs         0.1457
_reflns_number_observed          8436
_reflns_number_total             12717
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9634177_1.cif
_cod_data_source_block           compound_SB6sigma2+
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+2.1492P] 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^)+(0.0605P)^2^+2.1492P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2965.34(8)
_cod_database_code               4116993