Acceleration of the thermal back-reaction and the finding of a non-photochromic isomer for a negative photochromic binaphthyl-bridged imidazole dimer.
Mutoh, Katsuya; Moriyama, Natsuho; Abe, Jiro; Chemical communications (Cambridge, England) 59 (2023) 2962–2965; doi:10.1039/d2cc06942c

data_7131304
_publ_section_title
;
 Acceleration of the thermal back-reaction and the finding of a
 non-photochromic isomer for a negative photochromic binaphthyl-bridged
 imidazole dimer.
;
_journal_issue                   20
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2962
_journal_page_last               2965
_journal_paper_doi               10.1039/d2cc06942c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C52 H36 N4'
_chemical_formula_sum            'C52 H36 N4'
_chemical_formula_weight         716.892
_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_Int_Tables_number      14
_audit_creation_date             2023-01-17
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.01.17 svn.r1b7d262c for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-01-20 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.105(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6158(3)
_cell_length_b                   25.7155(8)
_cell_length_c                   12.4043(4)
_cell_measurement_reflns_used    7640
_cell_measurement_temperature    104(7)
_cell_measurement_theta_max      29.6100
_cell_measurement_theta_min      2.0990
_cell_volume                     3695.73(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      104(7)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.9949
_diffrn_measured_fraction_theta_max 0.9934
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     61.00  87.00   0.50  257.17    --   20.00  54.00 150.00   52
  2  \w    -72.00 110.00   0.50  257.17    --   20.00  54.00 -90.00  364
  3  \w    -68.00 -36.00   0.50  257.17    --   20.00  54.00 -30.00   64
  4  \w     13.00  39.00   0.50  257.17    --   20.00  54.00 -30.00   52
  5  \w    -74.00  61.00   0.50  257.17    --   20.00  54.00-150.00  270
  6  \w    -67.00  28.00   0.50  257.17    --   20.00  54.00-120.00  190
  7  \w    -65.00 -38.00   0.50  257.17    --   20.00  54.00 -60.00   54
  8  \w    -68.00 -41.00   0.50  257.17    --   20.00  54.00   0.00   54
  9  \w      1.00  26.00   0.50  257.17    --   20.00  54.00   0.00   50
 10  \w    -59.00 -32.00   0.50  257.17    --   20.00  54.00 150.00   54
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.1071
_diffrn_reflns_Laue_measured_fraction_full 0.9949
_diffrn_reflns_Laue_measured_fraction_max 0.9934
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39620
_diffrn_reflns_point_group_measured_fraction_full 0.9949
_diffrn_reflns_point_group_measured_fraction_max 0.9934
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504.822
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.4759
_refine_diff_density_min         -0.4254
_refine_diff_density_rms         0.0982
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             8.9153
_refine_ls_extinction_coef       0.0013
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0332
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    63
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7227
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.0190
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.6253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -14
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -9
_reflns_number_gt                4668
_reflns_number_total             7227
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2cc06942c3.cif
_cod_data_source_block           220715_dmbnimd_mutoh
_cod_depositor_comments
'Adding full bibliography for 7131304--7131306.cif.'
_cod_database_code               7131304
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C3AA, C4AA, C2AA, C3, C0AA, C1AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C3AA, C4AA, C1AA, C0AA, C3, C2AA
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C53(H53), C54(H54), C52(H52), C50(H50), C27(H27), C26(H26),
 C31(H31), C25(H25), C51(H51), C7(H7), C24(H24), C30(H30), C18(H18), C22(H22),
 C21(H21), C20(H20), C33(H33), C34(H34), C19(H19), C1AA(H1AA), C3(H3),
 C3AA(H3AA), C4AA(H4AA), C2AA(H2AA)
3.b Idealised Me refined as rotating group:
 C55(H55a,H55b,H55c), C56(H56a,H56b,H56c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;