Oxidative evolution of <i>Z</i>/<i>E</i>-diaminotetraphenylethylene.
Li, Xin; Zhuang, Yongbing; Ran, Qichao; Liu, Xiangyang; Physical chemistry chemical physics : PCCP 24 (2022) 1960–1964; doi:10.1039/d1cp05303e

data_7244166
_publ_section_title
;
 Oxidative evolution of <i>Z</i>/<i>E</i>-diaminotetraphenylethylene.
;
_journal_issue                   4
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              1960
_journal_page_last               1964
_journal_paper_doi               10.1039/d1cp05303e
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C26 H22 N2'
_chemical_formula_sum            'C26 H22 N2'
_chemical_formula_weight         362.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-18
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                76.016(8)
_cell_angle_beta                 84.388(8)
_cell_angle_gamma                76.867(9)
_cell_formula_units_Z            2
_cell_length_a                   9.1427(9)
_cell_length_b                   10.2655(10)
_cell_length_c                   11.2401(11)
_cell_measurement_reflns_used    1033
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.3080
_cell_measurement_theta_min      3.4010
_cell_volume                     995.87(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   16.00   85.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5086   57.0000   30.0000 69

  2 omega    3.00   68.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5086   57.0000  -30.0000 65

  3 omega    1.00   87.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5086   38.0000 -150.0000 86

  4 omega  -19.00   21.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.3211  -99.0000 -150.0000 40

  5 omega    3.00   87.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -       17.5086   38.0000  120.0000 84

  6 omega  -66.00  -39.00   1.0000  160.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.3211 -178.0000  150.0000 27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0650577000
_diffrn_orient_matrix_UB_12      0.0281618000
_diffrn_orient_matrix_UB_13      -0.0057691000
_diffrn_orient_matrix_UB_21      -0.0457845000
_diffrn_orient_matrix_UB_22      0.0644745000
_diffrn_orient_matrix_UB_23      0.0047933000
_diffrn_orient_matrix_UB_31      0.0055550000
_diffrn_orient_matrix_UB_32      -0.0188692000
_diffrn_orient_matrix_UB_33      0.0646653000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7741
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.890
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1664
_reflns_number_total             4053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp05303e2.cif
_cod_data_source_block           Z-2NH2-TPE
_cod_depositor_comments
'Adding full bibliography for 7244164--7244166.cif.'
_cod_original_cell_volume        995.86(18)
_cod_database_code               7244166
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         c12h12n2o3br1
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.976
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Rotating group:
 N1(H1A,H1B), N2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26)
;
_shelx_res_checksum              2403
_shelx_hkl_checksum              19430
_olex2_submission_special_instructions 'No special instructions were received'