Reprecipitation-driven access to solvates and solvent-free crystals: achieving two-solvent-mediated vapochromic luminescence
Ogawa, Kota; Sumida, Ayaka; Kubota, Rikuto; Tachikawa, Takashi; Ito, Suguru; CrystEngComm 27 (2025) 7484–7490; doi:10.1039/D5CE00946D

data_7251101
_publ_section_title
;
 Reprecipitation-driven access to solvates and solvent-free crystals:
 achieving two-solvent-mediated vapochromic luminescence
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              7484
_journal_page_last               7490
_journal_paper_doi               10.1039/D5CE00946D
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C31 H18 N4 S2'
_chemical_formula_sum            'C31 H18 N4 S2'
_chemical_formula_weight         510.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-31 deposited with the CCDC.	2025-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.3450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.71580(10)
_cell_length_b                   5.86670(10)
_cell_length_c                   17.8200(2)
_cell_measurement_reflns_used    5977
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.79
_cell_measurement_theta_min      5.17
_cell_volume                     1175.32(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7372
_diffrn_reflns_point_group_measured_fraction_full 0.797
_diffrn_reflns_point_group_measured_fraction_max 0.766
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.213
_diffrn_reflns_theta_min         5.173
_exptl_absorpt_coefficient_mu    2.285
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.66a (Rigaku Oxford Diffraction, 2019)

Empirical absorption correction using spherical harmonics,

 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.021(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         3615
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0516P)^2^+0.2596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.424
_reflns_Friedel_fraction_full    0.548
_reflns_Friedel_fraction_max     0.508
_reflns_number_gt                3535
_reflns_number_total             3615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00946d8.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7251100--7251101.cif.'
_cod_database_code               7251101
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.262
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S2-C21 \\sim S2A-C21
 with sigma of 0.02
 S2-C24 \\sim S2A-C24A
 with sigma of 0.02
 C22-H22 \\sim C22A-H22A
 with sigma of 0.02
 C22-C21 \\sim C22A-C21
 with sigma of 0.02
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 C23-H23 \\sim C23A-H23A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C24-H24 \\sim C24A-H24A
 with sigma of 0.02
 S2-C22 \\sim S2A-C22A
 with sigma of 0.04
 S2-C18 \\sim S2A-C18
 with sigma of 0.04
 S2-C23 \\sim S2A-C23A
 with sigma of 0.04
 C22-C18 \\sim C22A-C18
 with sigma of 0.04
 C22-C24 \\sim C22A-C24A
 with sigma of 0.04
 C21-C23 \\sim C21-C23A
 with sigma of 0.04
 C21-C24 \\sim C21-C24A
 with sigma of 0.04
 S2-C22 \\sim C22A-S2A
 with sigma of 0.04
 C21-S2 \\sim C21-C22 \\sim C21-C18 \\sim C21-C22A \\sim C21-S2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24A) = Uanis(C23A)
4. Rigid body (RIGU) restrains
 S2, H22, C23, H23, C24, H24, C21, C22, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22A, H22A, C23A, H23A, C24A, H24A, S2A, C21, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(S2A)=1-FVAR(1)
 Sof(S2)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C20(H20), C12(H12), C13(H13), C26(H26), C29(H29), C27(H27),
 C19(H19), C30(H30), C4(H4), C28(H28), C11(H11), C5(H5), C10(H10), C7(H7),
 C23(H23), C6(H6), C24(H24), C22A(H22A), C23A(H23A), C24A(H24A)
;
_shelx_res_checksum              20801
_olex2_submission_special_instructions 'No special instructions were received'