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_7131305
_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_absolute_configuration unk
_chemical_formula_moiety         'C50 H32 N4'
_chemical_formula_sum            'C50 H32 N4'
_chemical_formula_weight         688.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-12-20
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_audit_update_record
;
2022-12-20 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5250(5)
_cell_length_b                   14.4544(9)
_cell_length_c                   26.1380(12)
_cell_measurement_reflns_used    4731
_cell_measurement_temperature    106(8)
_cell_measurement_theta_max      29.1590
_cell_measurement_theta_min      2.1640
_cell_volume                     3598.6(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_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     74.00 101.00   0.50    4.11    --   20.00  54.00   0.00   54
  2  \w    -60.00 -34.00   0.50    4.11    --   20.00  54.00 -90.00   52
  3  \w     -2.00 109.00   0.50    4.11    --   20.00  54.00 -90.00  222
  4  \w     15.00  61.00   0.50    4.11    --   20.00  54.00-180.00   92
  5  \w    -63.00 -38.00   0.50    4.11    --   20.00  54.00-150.00   50
  6  \w    -32.00  -7.00   0.50    4.11    --   20.00  54.00-150.00   50
  7  \w     68.00 110.00   0.50    4.11    --   20.00  54.00  90.00   84
  8  \w     -8.00  17.00   0.50    4.11    --   20.00  54.00   0.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0643341000
_diffrn_orient_matrix_UB_12      0.0176086000
_diffrn_orient_matrix_UB_13      -0.0095803000
_diffrn_orient_matrix_UB_21      -0.0239364000
_diffrn_orient_matrix_UB_22      0.0458032000
_diffrn_orient_matrix_UB_23      0.0044222000
_diffrn_orient_matrix_UB_31      0.0288472000
_diffrn_orient_matrix_UB_32      -0.0014142000
_diffrn_orient_matrix_UB_33      0.0249934000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            19914
_diffrn_reflns_point_group_measured_fraction_full 0.878
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.559
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72282
_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            'dull reddish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 2106 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.5123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.504
_reflns_Friedel_fraction_full    0.721
_reflns_Friedel_fraction_max     0.601
_reflns_number_gt                7186
_reflns_number_total             8837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06942c3.cif
_cod_data_source_block           moriyama_bnimd
_cod_depositor_comments
'Adding full bibliography for 7131304--7131306.cif.'
_cod_database_code               7131305
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.985
_diffrn_oxdiff_digest_frames
;
014dd102197204b48a85b7397dd82f2b72006543f41
;
_diffrn_oxdiff_digest_hkl
;
01ac8ca16e75b432146d53ab9e6d8a4d1282d3
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C48(H48), C44(H44), C42(H42), C21(H21), C27(H27), C13(H13), C20(H20),
 C18(H18), C22(H22), C53(H53), C52(H52), C46(H46), C54(H54), C19(H19), C7(H7),
 C26(H26), C41(H41), C12(H12), C29(H29), C24(H24), C10(H10), C47(H47), C50(H50),
  C25(H25), C45(H45), C9(H9), C30(H30), C38(H38), C39(H39), C51(H51), C8(H8),
 C40(H40)
;
_shelx_res_checksum              47604
_shelx_hkl_checksum              25206
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.715