Structural insight into piezo-solvatochromism of Reichardt's dye.
Sobczak, Szymon; Katrusiak, Andrzej; IUCrJ 11 (2024) –; doi:10.1107/S2052252524004603

data_1571773
_publ_section_title
;
 Structural insight into piezo-solvatochromism of Reichardt's dye.
;
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524004603
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C29 H21 N O, 4(C H4 O)'
_chemical_formula_sum            'C33 H37 N O5'
_chemical_formula_weight         527.63
_chemical_name_common
;
ET(1)*4CH3OH
;
_chemical_name_systematic
;
4-(2,4,6-triphenylpyridinium-1-yl)-phenolate tetramethanol solvate
;
_chemical_properties_physical    Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-20 deposited with the CCDC. 2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.819(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4704(11)
_cell_length_b                   19.80(3)
_cell_length_c                   13.3135(15)
_cell_measurement_reflns_used    3200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0630
_cell_measurement_theta_min      2.2000
_cell_volume                     2746(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_pressure         570000
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.399
_diffrn_measured_fraction_theta_max 0.226
_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    -19.00   3.50   0.75   35.00    --  -28.48 -57.00  30.00   30
  2  \w    -27.00  36.00   0.75   35.00    --  -28.48 -13.00   3.00   84
  3  \w    -57.00 -21.00   0.75   35.00    --  -28.48  77.00 -30.00   48
  4  \w    -44.00 -11.00   0.75   35.00    --  -28.48  19.00   0.00   44
  5  \w    -19.00   3.50   0.75   35.00    --  -28.48 -57.00-150.00   30
  6  \w    -55.00   8.00   0.75   35.00    --  -28.48  67.00 157.00   84
  7  \w    -19.00  17.00   0.75   35.00    --  -28.48 -39.00  12.00   48
  8  \w    -19.00  17.00   0.75   35.00    --  -28.48 -39.00-167.00   48
  9  \w    -44.00  19.00   0.75   35.00    --  -28.48  19.00-180.00   84
 10  \w    -89.00 -26.00   0.75   35.00    --  -28.48 135.00 -57.00   84
 11  \w     -8.00  19.00   0.75   35.00    --  -28.48 -38.00-180.00   36
 12  \w    -10.00   9.50   0.75   35.00    --   29.42  77.00 -60.00   26
 13  \w     -3.00  18.00   0.75   35.00    --   29.42  57.00 150.00   28
 14  \w     -3.00  18.00   0.75   35.00    --   29.42  57.00 -30.00   28
 15  \w    -44.00  19.00   0.75   35.00    --  -28.48  39.00 167.00   84
 16  \w    -19.00  44.00   0.75   35.00    --  -28.48 -19.00-180.00   84
 17  \w    -24.00  39.00   0.75   35.00    --  -28.48 -26.00   8.00   84
 18  \w    -89.00 -26.00   0.75   35.00    --  -28.48 135.00 123.00   84
 19  \w     20.00  56.00   0.75   35.00    --   29.42 -77.00-150.00   48
 20  \w     -3.00  30.00   0.75   35.00    --   29.42  57.00 -60.00   44
 21  \w      0.75  60.00   0.75   35.00    --   29.42 -81.00-151.00   79
 22  \w    -38.00 -11.00   0.75   35.00    --   29.42  19.00   0.00   36
 23  \w     -9.25  44.00   0.75   35.00    --   29.42 -39.00  12.00   71
 24  \w    -18.00   7.50   0.75   35.00    --   29.42  38.00   0.00   34
 25  \w    -26.00   0.25   0.75   35.00    --   29.42   0.00   0.00   35
 26  \w    -17.00  19.00   0.75   35.00    --   29.42  39.00 167.00   48
 27  \w    -17.00  19.00   0.75   35.00    --   29.42  39.00 -12.00   48
 28  \w     30.50  87.50   0.75   35.00    --   29.42-135.00  57.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1418
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.399
_diffrn_reflns_Laue_measured_fraction_max 0.226
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22964
_diffrn_reflns_point_group_measured_fraction_full 0.399
_diffrn_reflns_point_group_measured_fraction_max 0.226
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         4.601
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.999
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_preparation       'crystallized in DAC,solvatochromic'
_exptl_crystal_recrystallization_method 'crystallized at high pressure'
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.039
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         1643
_refine_ls_number_restraints     618
_refine_ls_restrained_S_all      1.467
_refine_ls_R_factor_all          0.1681
_refine_ls_R_factor_gt           0.0857
_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^)+(0.1734P)^2^+1.5201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2285
_refine_ls_wR_factor_ref         0.2956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                801
_reflns_number_total             1643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5066.cif
_cod_data_source_block           et1_meoh_0_57gpa
_cod_database_code               1571773
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.968
_exptl_absorpt_special_details
;
Data were collected at room temperature (295(2) K) and pressure of 0.57(2) GPa
(570000 kPa).
;
_exptl_oxdiff_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.396     0.455
         range of gasket transmission (min-max)           0.917     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 1:  0.000 mm, mu =  0.0000 mm-1

 thickness of diamond anvil 2: 19.500 mm, mu =  0.0202 mm-1
       thickness of platten 2:  0.000 mm, mu =  0.0000 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 300.0 microns, radius = 300.0 microns
    Gasket absorption coeff =        21.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.00

    Non-absorbing pressure medium
;
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10'(0.08) H9'(0.068) H5'(0.065) H6'(0.067) H13'(0.076)
 H16(0.069) H16'(0.079) H15'(0.062) H2MA(0.211) H2MB(0.211) H2MC(0.211)
 H11'(0.08) H1M(0.2) H6(0.079) H5(0.059) H15(0.069) H4M(0.281) H3M(0.221)
 H13(0.091) H9(0.082) H7(0.073) H2(0.067) H2'(0.054) H11(0.128) H1MA(0.137)
 H1MB(0.137) H1MC(0.137) H12(0.121) H3MA(0.182) H3MB(0.182) H3MC(0.182)
 H2M(0.187) H4MA(0.179) H4MB(0.179) H4MC(0.179) H10(0.092) H12'(0.083)
 Fixed X: H10'(0.775817) H9'(0.842013) H5'(1.29675) H6'(1.500672)
 H13'(0.864053) H16(0.43263) H16'(0.63607) H15'(0.817636) H2MA(0.799685)
 H2MB(0.844372) H2MC(0.937281) H11'(0.745938) H1M(1.087951) H6(1.384803)
 H5(1.181075) H15(0.614993) H4M(1.049596) H3M(1.24222) H13(0.977611)
 H9(0.659031) H7(1.541652) H2(1.050244) H2'(1.07642) H11(0.666672)
 H1MA(0.994756) H1MB(0.938433) H1MC(0.88872) H12(0.87533) H3MA(1.149625)
 H3MB(1.047434) H3MC(1.186425) H2M(0.812095) H4MA(0.938911) H4MB(0.894372)
 H4MC(0.838565) H10(0.558718) H12'(0.790725)
 Fixed Y: H10'(0.460934) H9'(0.381787) H5'(0.236392) H6'(0.193766)
 H13'(0.244911) H16(0.283962) H16'(0.382821) H15'(0.324081) H2MA(0.043865)
 H2MB(0.022636) H2MC(0.063383) H11'(0.434944) H1M(-0.035586) H6(0.014648)
 H5(0.059656) H15(0.229351) H4M(0.440925) H3M(0.379692) H13(0.169366)
 H9(0.144866) H7(0.084121) H2(0.126501) H2'(0.240417) H11(0.083799) H1MA(-
 0.045028) H1MB(0.027691) H1MC(-0.03226) H12(0.12196) H3MA(0.291062)
 H3MB(0.321407) H3MC(0.305453) H2M(0.114136) H4MA(0.460859) H4MB(0.526195)
 H4MC(0.45564) H10(0.097604) H12'(0.325677)
 Fixed Z: H10'(0.485869) H9'(0.378796) H5'(0.478346) H6'(0.520601)
 H13'(0.601393) H16(0.309687) H16'(0.119353) H15'(0.178833) H2MA(0.381193)
 H2MB(0.492672) H2MC(0.430019) H11'(0.65242) H1M(0.25174) H6(0.399652)
 H5(0.356942) H15(0.375733) H4M(0.27835) H3M(0.191722) H13(0.084494)
 H9(0.222287) H7(0.477291) H2(0.255758) H2'(0.503079) H11(-0.062259)
 H1MA(0.10994) H1MB(0.120477) H1MC(0.18286) H12(-0.062712) H3MA(0.181992)
 H3MB(0.247571) H3MC(0.297078) H2M(0.537071) H4MA(0.162671) H4MB(0.215757)
 H4MC(0.242083) H10(0.076868) H12'(0.702688)
;
_shelx_res_checksum              20731
_shelx_hkl_checksum              72096
_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
;