Mechanical deformation and multiple thermal restoration of organic crystals: reversible multi-stage shape-changing effect with luminescence-color changes
Feng, Chi; Seki, Tomohiro; Sakamoto, Shunichi; Sasaki, Toshiyuki; Takamizawa, Satoshi; Ito, Hajime; Chemical Science 13 (2022) 9544–9551; doi:10.1039/D2SC03414J

data_1567385
_publ_section_title
;
 Mechanical deformation and multiple thermal restoration of organic
 crystals: reversible multi-stage shape-changing effect with
 luminescence-color changes
;
_journal_issue                   33
_journal_name_full               'Chemical Science'
_journal_page_first              9544
_journal_page_last               9551
_journal_paper_doi               10.1039/D2SC03414J
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C11 H8 Au Br F4 N2'
_chemical_formula_sum            'C11 H8 Au Br F4 N2'
_chemical_formula_weight         521.07
_chemical_name_systematic
'1-bromo-2,3,5,6-tetrafluorobenzenyl(1,3-dimethylimidazolin-2-ylidene)gold complex'
_chemical_properties_physical    Heat-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-01 deposited with the CCDC.	2022-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.584(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0976(5)
_cell_length_b                   15.4992(5)
_cell_length_c                   12.9484(4)
_cell_measurement_reflns_used    13007
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2030
_cell_measurement_theta_min      3.0650
_cell_volume                     2711.56(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.920
_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    -72.00 -26.00   0.50    3.04    --   -2.10  14.00-120.00   92
  2  \w     37.00  63.00   0.50    3.04    --   -2.10  14.00-120.00   52
  3  \w    -80.00 -54.00   0.50    3.04    --    2.20  29.00 120.00   52
  4  \w     39.00  91.00   0.50    3.04    --    2.20  29.00 120.00  104
  5  \w    -39.00 -13.00   0.50    3.04    --    2.20  29.00 120.00   52
  6  \w    -86.00  92.00   0.50    3.04    --    2.20  57.00  30.00  356
  7  \w    -76.00 -51.00   0.50    3.04    --    2.20  57.00   0.00   50
  8  \w    -55.00 -29.00   0.50    3.04    --    2.20  57.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0155280000
_diffrn_orient_matrix_UB_12      -0.0133020000
_diffrn_orient_matrix_UB_13      -0.0547014000
_diffrn_orient_matrix_UB_21      0.0048155000
_diffrn_orient_matrix_UB_22      -0.0437999000
_diffrn_orient_matrix_UB_23      0.0165516000
_diffrn_orient_matrix_UB_31      -0.0499039000
_diffrn_orient_matrix_UB_32      -0.0000857000
_diffrn_orient_matrix_UB_33      0.0014123000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12298
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.503
_diffrn_reflns_theta_min         2.298
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    13.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.553
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         12298
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0836
_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^)+(0.0840P)^2^+60.5152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8091
_reflns_number_total             12298
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9168\% 
 around [-0.30 -0.00 0.95] (reciprocal) or [0.00 -0.00 1.00] (direct)
;
_cod_data_source_file            d2sc03414j6.cif
_cod_data_source_block           hyo-227-rt_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1567382--1567387.cif.'
_cod_original_cell_volume        2711.55(16)
_cod_database_code               1567385
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H N F Au Br'
_shelx_estimated_absorpt_t_max   0.444
_shelx_estimated_absorpt_t_min   0.072
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8232(12)
 0.1768(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C00X \\sim F00H \\sim F00D \\sim C00S \\sim C00N \\sim C00E \\sim C00F \\sim
C012 \\sim F006 \\sim F009: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.08
C00V \\sim N00J \\sim C00M \\sim C00U \\sim N00A \\sim C00R \\sim C011: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 F006, C00F, C00E, C00N, F009, C00S, F00D, F00H, C00X, C012
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.004
 C00V, N00J, C00M, C00U
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.004
 C00L, F005, C00P, C010, C13, F00B, C00Q, F00C, C14, F007, Br03
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.004
 F00H, C00X, F00D, C00S, C00N, C00E, C00F, C012, F006, F009
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00U(H00U), C00Z(H00Z), C011(H011)
5.b Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C00V(H00D,H00E,H00F), C00W(H00G,H00H,H00I), C00Y(H00J,
 H00K,H00L)
;
_shelx_res_checksum              25330
_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 2.679
_oxdiff_exptl_absorpt_empirical_full_min 0.501
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2