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_7154963
_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, Cl6 Sb, C H2 Cl2'
_chemical_formula_sum            'C37 H26 Br4 Cl8 N2 Sb'
_chemical_formula_weight         1223.59
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-25
_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                90.00
_cell_angle_beta                 91.4952(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.37545(18)
_cell_length_b                   14.15367(14)
_cell_length_c                   19.4760(2)
_cell_measurement_reflns_used    18498
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8380
_cell_measurement_theta_min      3.5670
_cell_volume                     4236.91(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -49.00   35.00   1.0000    1.0450
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   37.0000  150.0000 84

  2 omega  -75.00   38.00   1.0000    1.0450
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   77.0000  -60.0000 113

  3 omega  -49.00   35.00   1.0000    1.0450
omega____ theta____ kappa____ phi______ frames
    -      -40.8987   37.0000 -150.0000 84

  4 omega   23.00   98.00   1.0000    1.0450
omega____ theta____ kappa____ phi______ frames
    -       40.8987 -125.0000 -180.0000 75

  5 omega   30.00   91.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -30.0000 -150.0000 61

  6 omega   30.00   91.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -30.0000   60.0000 61

  7 omega   94.00  178.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628  125.0000    0.0000 84

  8 omega   33.00  121.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628 -125.0000  150.0000 88

  9 omega   24.00  109.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -94.0000  -60.0000 85

 10 omega   77.00  178.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628   30.0000 -120.0000 101

 11 omega   30.00   91.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -30.0000  120.0000 61

 12 omega   94.00  178.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628  125.0000  -90.0000 84

 13 omega   33.00   98.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628  -45.0000  -60.0000 65

 14 omega -115.00  -11.00   1.0000    1.0450
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -57.0000  -60.0000 104

 15 omega -115.00  -11.00   1.0000    1.0450
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -57.0000 -180.0000 104

 16 omega -115.00  -11.00   1.0000    1.0450
omega____ theta____ kappa____ phi______ frames
    -      -40.8987  -57.0000   60.0000 104

 17 omega   77.00  121.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628   61.0000 -180.0000 44

 18 omega   46.00  178.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628   15.0000   30.0000 132

 19 omega   46.00  178.00   1.0000    4.1850
omega____ theta____ kappa____ phi______ frames
    -      107.6628   15.0000  150.0000 132
;
_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      -0.0010563000
_diffrn_orient_matrix_UB_12      0.1082999000
_diffrn_orient_matrix_UB_13      0.0079741000
_diffrn_orient_matrix_UB_21      -0.0899565000
_diffrn_orient_matrix_UB_22      -0.0058643000
_diffrn_orient_matrix_UB_23      0.0327968000
_diffrn_orient_matrix_UB_31      0.0440588000
_diffrn_orient_matrix_UB_32      -0.0095238000
_diffrn_orient_matrix_UB_33      0.0715910000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41012
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.10
_diffrn_reflns_theta_min         3.62
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.474
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.144
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2356
_exptl_crystal_size_max          0.2391
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.0323
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0293P)^2^+6.6529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                7643
_reflns_number_total             8456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ob00140h2.cif
_cod_data_source_block           raj25f
_cod_depositor_comments
'Adding full bibliography for 7154963--7154965.cif.'
_cod_original_cell_volume        4236.90(8)
_cod_database_code               7154963
_audit_block_doi                 10.5517/cc1kj519
_chemical_oxdiff_formula         'Sb Cl6 C36 N2 H24 Br4 C H2 Cl2'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
2.b 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)
;
_olex2_date_sample_data_collection 2015-02-24
_olex2_date_sample_submission    2015-02-24
_olex2_submission_special_instructions 'No special instructions were received'