A search for blues brothers: X-ray crystallographic/spectroscopic characterization of the tetraarylbenzidine cation radical as a product of aging of solid magic blue.
Talipov, Marat R.; Hossain, Mohammad M.; Boddeda, Anitha; Thakur, Khushabu; Rathore, Rajendra; Organic & biomolecular chemistry 14 (2016) 2961–2968; doi:10.1039/c6ob00140h

data_7154964
_publ_section_title
;
 A search for blues brothers: X-ray crystallographic/spectroscopic
 characterization of the tetraarylbenzidine cation radical as a product of
 aging of solid magic blue.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2961
_journal_page_last               2968
_journal_paper_doi               10.1039/c6ob00140h
_journal_volume                  14
_journal_year                    2016
_chemical_formula_moiety         'C36 H22 Br6 N2'
_chemical_formula_sum            'C36 H22 Br6 N2'
_chemical_formula_weight         962.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_block_doi                 10.5517/cc1kj52b
_audit_creation_date             2015-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-01-07 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                107.983(2)
_cell_angle_beta                 106.750(2)
_cell_angle_gamma                96.924(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1188(2)
_cell_length_b                   13.8839(3)
_cell_length_c                   16.4081(5)
_cell_measurement_reflns_used    19279
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4720
_cell_measurement_theta_min      3.6740
_cell_volume                     2043.20(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -49.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362   37.0000   90.0000 84

  2 omega  -96.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362  125.0000 -180.0000 94

  3 omega -122.00    5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362  -19.0000  -90.0000 127

  4 omega   23.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8362 -125.0000  -30.0000 75

  5 omega   23.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8362 -125.0000 -150.0000 75

  6 omega   23.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8362 -125.0000  150.0000 75

  7 omega   23.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8362 -125.0000 -120.0000 75

  8 omega   74.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   77.0000  -30.0000 104

  9 omega   30.00   91.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -30.0000   30.0000 61

 10 omega   30.00   91.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -30.0000  150.0000 61

 11 omega   33.00  121.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628 -125.0000   30.0000 88

 12 omega   94.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  125.0000 -120.0000 84

 13 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   30.0000   60.0000 101

 14 omega   29.00  141.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -77.0000 -120.0000 112

 15 omega   24.00  109.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -94.0000 -180.0000 85

 16 omega   24.00  109.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -94.0000   90.0000 85

 17 omega   24.00  109.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -94.0000 -150.0000 85

 18 omega   33.00   98.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -45.0000  -60.0000 65

 19 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000  -60.0000 101

 20 omega   24.00  109.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -94.0000   60.0000 85

 21 omega -115.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362  -57.0000   30.0000 104

 22 omega  -49.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362   37.0000    0.0000 84

 23 omega -115.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362  -57.0000  120.0000 104

 24 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362  -77.0000  120.0000 113

 25 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362  -77.0000  -30.0000 113

 26 omega -115.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8362  -57.0000 -150.0000 104

 27 omega   46.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   15.0000 -150.0000 132

 28 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000 -180.0000 101

 29 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000  -90.0000 101

 30 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000   60.0000 101

 31 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000 -150.0000 101

 32 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000 -120.0000 101

 33 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000  120.0000 101

 34 omega   77.00  178.00   1.0000    1.2950
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000   90.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0426323000
_diffrn_orient_matrix_UB_12      -0.0353343000
_diffrn_orient_matrix_UB_13      -0.0855789000
_diffrn_orient_matrix_UB_21      -0.1573029000
_diffrn_orient_matrix_UB_22      -0.0458311000
_diffrn_orient_matrix_UB_23      -0.0599932000
_diffrn_orient_matrix_UB_31      -0.0114045000
_diffrn_orient_matrix_UB_32      0.1049809000
_diffrn_orient_matrix_UB_33      -0.0116074000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38897
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.70
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.282
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.3829
_exptl_crystal_size_mid          0.1448
_exptl_crystal_size_min          0.0709
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+1.2526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                7246
_reflns_number_total             8166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ob00140h2.cif
_cod_data_source_block           raj25j
_cod_depositor_comments
'Adding full bibliography for 7154963--7154965.cif.'
_cod_original_cell_volume        2043.19(9)
_cod_database_code               7154964
_chemical_oxdiff_formula         'C36 H22 Br6 N2'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15),
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27),
  C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36)
;
_olex2_date_sample_submission    2015-03-24
_olex2_submission_special_instructions 'No special instructions were received'