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_7154965
_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 H24 Br4 N2'
_chemical_formula_sum            'C36 H24 Br4 N2'
_chemical_formula_weight         804.21
_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/cc1kj7dq
_audit_creation_date             2016-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-07 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                87.2838(12)
_cell_angle_beta                 81.2554(13)
_cell_angle_gamma                82.7604(12)
_cell_formula_units_Z            6
_cell_length_a                   15.3203(2)
_cell_length_b                   15.5925(2)
_cell_length_c                   19.8315(3)
_cell_measurement_reflns_used    43392
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8620
_cell_measurement_theta_min      3.4130
_cell_volume                     4643.06(11)
_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    'olex2.solve (Bourhis et al., 2015)'
_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 0.986
_diffrn_measurement_details
;
  1 omega  -75.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   77.0000 -120.0000 113

  2 omega  -49.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   37.0000 -120.0000 84

  3 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -77.0000  120.0000 113

  4 omega -117.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -37.0000  -90.0000 102

  5 omega  -49.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   37.0000   60.0000 84

  6 omega   23.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8987 -125.0000   60.0000 75

  7 omega   33.00  121.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628 -125.0000  150.0000 88

  8 omega   80.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   45.0000   60.0000 98

  9 omega   29.00  141.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -77.0000  -60.0000 112

 10 omega   77.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000   90.0000 101

 11 omega   94.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628  125.0000  -90.0000 84

 12 omega   33.00  121.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628 -125.0000 -120.0000 88

 13 omega   33.00  121.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628 -125.0000  -60.0000 88

 14 omega   24.00  109.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -94.0000  -30.0000 85

 15 omega   33.00   98.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -45.0000  -60.0000 65

 16 omega   77.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000    0.0000 101

 17 omega   30.00   91.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -30.0000   90.0000 61

 18 omega   77.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   30.0000  150.0000 101

 19 omega   33.00  138.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -61.0000  120.0000 105

 20 omega  -49.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   37.0000  150.0000 84

 21 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -77.0000 -180.0000 113

 22 omega -115.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -57.0000 -150.0000 104

 23 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -77.0000  -90.0000 113

 24 omega -115.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -57.0000    0.0000 104

 25 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -77.0000    0.0000 113

 26 omega   77.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   30.0000 -120.0000 101

 27 omega   74.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   77.0000  120.0000 104

 28 omega   74.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   77.0000 -150.0000 104

 29 omega   77.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000  -30.0000 101

 30 omega   74.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   77.0000 -120.0000 104

 31 omega   80.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   45.0000 -180.0000 98

 32 omega   74.00  156.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   77.0000    0.0000 82

 33 omega   80.00  178.00   1.0000    1.7500
omega____ theta____ kappa____ phi______ frames
    -      107.6628   45.0000  -60.0000 98
;
_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      0.0336133000
_diffrn_orient_matrix_UB_12      0.0893809000
_diffrn_orient_matrix_UB_13      -0.0034473000
_diffrn_orient_matrix_UB_21      0.0968153000
_diffrn_orient_matrix_UB_22      -0.0437204000
_diffrn_orient_matrix_UB_23      -0.0111440000
_diffrn_orient_matrix_UB_31      -0.0000904000
_diffrn_orient_matrix_UB_32      0.0052041000
_diffrn_orient_matrix_UB_33      -0.0777586000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88456
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.05
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.564
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.201
_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    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.4519
_exptl_crystal_size_mid          0.2202
_exptl_crystal_size_min          0.0592
_refine_diff_density_max         2.420
_refine_diff_density_min         -1.520
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         18598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0540P)^2^+7.7024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                16449
_reflns_number_total             18598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ob00140h2.cif
_cod_data_source_block           raj25b
_cod_depositor_comments
'Adding full bibliography for 7154963--7154965.cif.'
_cod_original_cell_volume        4643.06(12)
_cod_database_code               7154965
_chemical_oxdiff_formula         'C36 H24 Br4 N2'
_reflns_odcompleteness_completeness 99.99
_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:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), 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),
 C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B), C8B(H8B), C9B(H9B), C11B(H11B),
 C12B(H12B), C14B(H14B), C15B(H15B), C17B(H17B), C18B(H18B), C20B(H20B),
 C21B(H21B), C23B(H23B), C24B(H24B), C26B(H26B), C27B(H27B), C29B(H29B),
 C30B(H30B), C32B(H32B), C33B(H33B), C35B(H35B), C36B(H36B), C2A(H2A), C3A(H3A),
  C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A), C11A(H11A), C12A(H12A), C14A(H14A),
 C15A(H15A), C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A), C23A(H23A),
 C24A(H24A), C26A(H26A), C27A(H27A), C29A(H29A), C30A(H30A), C32A(H32A),
 C33A(H33A), C35A(H35A), C36A(H36A)
;
_olex2_date_sample_data_collection 2015-01-26
_olex2_date_sample_submission    2015-01-26
_olex2_submission_special_instructions 'No special instructions were received'