Heterocyclic compounds bearing s-triazine and cyclotriphosphazene scaffolds: facile synthesis, hydrogen-bonded organic framework construction and fluorescent amine sensing
Lv, Mei-Xin; Jiang, Shan; Wang, Chen; Dong, Qi; Bai, Feng-Ying; Xing, Yong-Heng; CrystEngComm  (2022) –; doi:10.1039/D2CE00717G

data_7245174
_publ_section_title
;
 Heterocyclic compounds bearing s-triazine and cyclotriphosphazene
 scaffolds: facile synthesis, hydrogen-bonded organic framework
 construction and fluorescent amine sensing
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00717G
_journal_year                    2022
_chemical_formula_moiety         'C24 H15 N3 O6'
_chemical_formula_sum            'C24 H15 N3 O6'
_chemical_formula_weight         441.39
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.5753(7)
_cell_length_b                   14.5753(7)
_cell_length_c                   20.6709(19)
_cell_measurement_reflns_used    1940
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      0.7
_cell_measurement_theta_min      0.6
_cell_volume                     3803.0(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.273
_diffrn_reflns_theta_min         1.890
_diffrn_source_current           25.0
_diffrn_source_power             1.125
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0542 before and 0.0358 after correction.
The Ratio of minimum to maximum transmission is 0.8971.
The \l/2 correction factor is 0.00150.
;
_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    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2109
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0523
_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^)+(0.1101P)^2^+0.5524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.2090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1218
_reflns_number_total             2109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00717g2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        3803.0(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7245174
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C8-O2 \\sim C8-O2A
 with sigma of 0.02
3. Others
 Sof(H8B)=Sof(O2A)=1-FVAR(1)
 Sof(H8A)=Sof(O2)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8A), C8(H8B)
;
_shelx_res_checksum              73087
_shelx_hkl_checksum              46018
_shelx_fab_checksum              11918
_platon_squeeze_special_details
;
A solvent mask was calculated and 84 electrons were 
found in a volume of 875\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.049[C3H6O], 0.097[C3H6O] per Unit Cell 
which account for 84 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'