Fluorescence emission enhancement of a T-shaped benzimidazole with a mechanically-interlocked 'suit'.
Xu, Houyang; Lin, Meng-Di; Yuan, Jun; Zhou, Baiyang; Mu, Yingxiao; Huo, Yanping; Zhu, Kelong; Chemical communications (Cambridge, England) 57 (2021) 3239–3242; doi:10.1039/d0cc07471c

data_7127974
_publ_section_title
;
 Fluorescence emission enhancement of a T-shaped benzimidazole with a
 mechanically-interlocked 'suit'.
;
_journal_issue                   26
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3239
_journal_page_last               3242
_journal_paper_doi               10.1039/d0cc07471c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C34 H34 N2 O, C2 H6 O'
_chemical_formula_sum            'C36 H40 N2 O2'
_chemical_formula_weight         532.70
_chemical_melting_point          180
_chemical_name_common            XHY-1
_chemical_name_systematic        XHY-1
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-12 deposited with the CCDC.	2021-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                63.465(3)
_cell_angle_beta                 72.555(2)
_cell_angle_gamma                65.144(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6578(3)
_cell_length_b                   12.4438(3)
_cell_length_c                   13.0555(4)
_cell_measurement_reflns_used    10289
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      75.8020
_cell_measurement_theta_min      4.1810
_cell_volume                     1522.76(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.945
_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  -9.00   1.00    1.00    --  -41.14 -77.00 -30.00   65
  2  \w    -97.00 -71.00   1.00    1.00    --  -41.14 -77.00 150.00   26
  3  \w    -59.00  -9.00   1.00    1.00    --  -41.14 -77.00 150.00   50
  4  \w    -78.00 -28.00   1.00    1.00    --  -41.14 -37.00-150.00   50
  5  \w   -106.00 -65.00   1.00    1.00    --  -41.14 -57.00  90.00   41
  6  \w    -62.00  29.00   1.00    1.00    --  -41.14  37.00-150.00   91
  7  \w    -59.00 -13.00   1.00    1.00    --  -41.14 -57.00  90.00   46
  8  \w    -85.00  -7.00   1.00    1.00    --  -41.14 125.00-150.00   78
  9  \w    -47.00  32.00   1.00    1.00    --  -41.14  57.00   0.00   79
 10  \w   -112.00  -9.00   1.00    1.00    --  -41.14 -77.00  60.00  103
 11  \w   -115.00 -11.00   1.00    1.00    --  -41.14 -77.00-120.00  104
 12  \w     18.00  44.00   1.00    1.00    --   41.14  37.00 -60.00   26
 13  \w      2.00  81.00   1.00    1.00    --   41.14 -99.00  90.00   79
 14  \w     81.00 116.00   1.00    1.00    --   41.14  37.00 -60.00   35
 15  \w     83.00 108.00   1.00    3.00    --  111.37  61.00   0.00   25
 16  \w     82.00 143.00   1.00    3.00    --  111.37  61.00-150.00   61
 17  \w     83.00 108.00   1.00    3.00    --  111.37  61.00-120.00   25
 18  \w    125.00 157.00   1.00    3.00    --  111.37  61.00  90.00   32
 19  \w     79.00 174.00   1.00    3.00    --  111.37  77.00  30.00   95
 20  \w     83.00 110.00   1.00    3.00    --  111.37  61.00  90.00   27
 21  \w     83.00 153.00   1.00    3.00    --  111.37  61.00-180.00   70
 22  \w     38.00 117.00   1.00    3.00    --  111.37-125.00  90.00   79
 23  \w    135.00 162.00   1.00    3.00    --  111.37  61.00 -60.00   27
 24  \w     82.00 131.00   1.00    3.00    --  111.37  61.00 -60.00   49
 25  \w     82.00 145.00   1.00    3.00    --  111.37  61.00 -90.00   63
 26  \w     79.00 177.00   1.00    3.00    --  111.37  77.00 120.00   98
 27  \w     86.00 112.00   1.00    3.00    --  111.37  45.00-120.00   26
 28  \w     82.00 146.00   1.00    3.00    --  111.37  61.00 120.00   64
 29  \w     83.00 110.00   1.00    3.00    --  111.37  61.00  60.00   27
 30  \w     43.00 114.00   1.00    3.00    --  111.37-125.00-150.00   71
 31  \w     33.00 102.00   1.00    3.00    --  111.37 -94.00 -30.00   69
 32  \w     79.00 177.00   1.00    3.00    --  111.37  77.00 -30.00   98
 33  \w     79.00 178.00   1.00    3.00    --  111.37  77.00-150.00   99
 34  \w     79.00 105.00   1.00    3.00    --  111.37  77.00 -60.00   26
 35  \w     79.00 105.00   1.00    3.00    --  111.37  77.00  90.00   26
 36  \w     79.00 105.00   1.00    3.00    --  111.37  77.00-180.00   26
 37  \w     79.00 106.00   1.00    3.00    --  111.37  77.00 -90.00   27
 38  \w    132.00 175.00   1.00    3.00    --  111.37  77.00 -90.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1334275000
_diffrn_orient_matrix_UB_12      0.1028446000
_diffrn_orient_matrix_UB_13      -0.0061243000
_diffrn_orient_matrix_UB_21      -0.0261721000
_diffrn_orient_matrix_UB_22      -0.0394286000
_diffrn_orient_matrix_UB_23      -0.0848031000
_diffrn_orient_matrix_UB_31      -0.0559893000
_diffrn_orient_matrix_UB_32      -0.0971940000
_diffrn_orient_matrix_UB_33      0.1024922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18924
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.719
_diffrn_reflns_theta_min         3.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0613P)^2^+0.3707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5308
_reflns_number_total             6000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07471c2.cif
_cod_data_source_block           a20100701a0121
_cod_depositor_comments
'Adding full bibliography for 7127974--7127975.cif.'
_cod_database_code               7127974
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C34H34N2O
_chemical_oxdiff_usercomment     XHY-TAXLE-NEU
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.809
_reflns_odcompleteness_completeness 97.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C010(H01J,H01K)
2.b Aromatic/amide H refined with riding coordinates:
 N003(H003), C00E(H00E), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00T(H00T), C00U(H00U), C00W(H00W)
2.c Idealised Me refined as rotating group:
 C00X(H00A,H00B,H00C), C00Y(H00D,H00F,H00M), C00Z(H00S,H00V,H00X), C011(H01A,
 H01B,H01C), C012(H01D,H01E,H01F), C013(H01G,H01H,H01I), C014(H01L,H01M,H01N)
2.d Idealised tetrahedral OH refined as rotating group:
 O001(H001)
;
_olex2_submission_original_sample_id XHY-1
_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 1.352
_oxdiff_exptl_absorpt_empirical_full_min 0.633