Self-reversible mechanofluorochromism of AIE-active C6-unsubstituted tetrahydropyrimidine derivatives
Liu, Yanshan; Liao, Yunhui; Ye, Ziwei; Chen, Lina; He, Yun; Huang, Yifan; Lai, Yingyu; Chen, Junguo; Zhu, Qiuhua; RSC Advances 11 (2021) 15–22; doi:10.1039/D0RA09209F

data_7241933
_publ_section_title
;
 Self-reversible mechanofluorochromism of AIE-active C6-unsubstituted
 tetrahydropyrimidine derivatives
;
_journal_issue                   1
_journal_name_full               'RSC Advances'
_journal_page_first              15
_journal_page_last               22
_journal_paper_doi               10.1039/D0RA09209F
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C29 H21 F9 N2 O4'
_chemical_formula_sum            'C29 H21 F9 N2 O4'
_chemical_formula_weight         632.48
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-30 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.852(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2291(17)
_cell_length_b                   11.4539(14)
_cell_length_c                   17.931(2)
_cell_measurement_reflns_used    4929
_cell_measurement_temperature    187.49
_cell_measurement_theta_max      26.903
_cell_measurement_theta_min      2.318
_cell_volume                     2811.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      187.49
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16551
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         2.781
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1142 before and 0.0387 after correction. The Ratio of minimum to maximum transmission is 0.9215. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0067(6)
_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   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6350
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0480P)^2^+0.5065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4133
_reflns_number_total             6350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09209f2.cif
_cod_data_source_block           191230lyh_0m
_cod_database_code               7241933
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 F1, F1A, F2, F2A, F3, F3A, F4, F4A, F5, F5A, F6, F6A, F7, F7A, F8, F8A, F9,
 F9A, C1, C16, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C5(H5)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C17(H17), C18(H18), C19(H19), C21(H21), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C29(H29)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              15004
_olex2_submission_special_instructions 'No special instructions were received'