A pyrazinium-based fluorescent chemosensor for the selective detection of 2,4,6-trinitrophenol in an aqueous medium
Pragya,; Saini, Vaishali; Rangan, Krishnan; Khungar, Bharti; New Journal of Chemistry 46 (2022) 16907–16913; doi:10.1039/D2NJ02999E

data_7061712
_publ_section_title
;
 A pyrazinium-based fluorescent chemosensor for the selective detection of
 2,4,6-trinitrophenol in an aqueous medium
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16907
_journal_page_last               16913
_journal_paper_doi               10.1039/D2NJ02999E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'Br, C19 H15 N2 S2, 0.5(C H4 O)'
_chemical_formula_sum            'C19.5 H17 Br N2 O0.5 S2'
_chemical_formula_weight         431.38
_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             2021-02-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-09-20 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6130(2)
_cell_length_b                   18.6032(2)
_cell_length_c                   15.0166(2)
_cell_measurement_reflns_used    11702
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      79.3720
_cell_measurement_theta_min      3.8260
_cell_volume                     3802.84(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_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      93(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.965
_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    -20.00  29.00   0.50    3.10    --    0.00  57.00  60.00   98
  2  \w    -72.00  15.00   0.50    3.10    --    0.00 -37.00-120.00  174
  3  \w     19.00  44.00   0.50    3.10    --    0.00  37.00  90.00   50
  4  \w     43.00  68.00   0.50    3.10    --    0.00  57.00  60.00   50
  5  \w     98.00 196.00   0.50   12.30    --  107.20  30.00 -90.00  196
  6  \w    118.00 157.00   0.50   12.30    --  107.20  61.00  30.00   78
  7  \w    125.00 188.00   0.50   12.30    --  107.20  30.00-150.00  126
  8  \w    108.00 196.00   0.50   12.30    --  107.20  30.00   0.00  176
  9  \w     19.00 127.00   0.50   12.30    --  107.20 -82.00  30.00  216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0885002000
_diffrn_orient_matrix_UB_12      -0.0396273000
_diffrn_orient_matrix_UB_13      0.0404546000
_diffrn_orient_matrix_UB_21      0.0688603000
_diffrn_orient_matrix_UB_22      -0.0596467000
_diffrn_orient_matrix_UB_23      0.0342201000
_diffrn_orient_matrix_UB_31      0.0147344000
_diffrn_orient_matrix_UB_32      0.0416247000
_diffrn_orient_matrix_UB_33      0.0879011000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15315
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.937
_diffrn_reflns_theta_min         3.783
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.481
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+9.6035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6974
_reflns_number_total             7340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02999e2.cif
_cod_data_source_block           exp_798_bk_4
_cod_depositor_comments
'Adding full bibliography for 7061712--7061713.cif.'
_cod_original_formula_sum        'C19.50 H17 Br N2 O0.50 S2'
_cod_database_code               7061712
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H13 Br N2 S2'
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.632
_reflns_odcompleteness_completeness 92.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C113(H11A,H11B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C3(H3), C102(H102), C15(H15), C6(H6), C16(H16), C103(H103),
 C106(H106), C110(H110), C00X(H00X), C11(H11), C19(H19), C116(H116), C115(H115),
  C17(H17), C7(H7), C111(H111), C12(H12), C8(H8), C108(H108), C117(H117),
 C118(H118), C107(H107), C112(H112), C18(H18)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              55933
_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 1.626
_oxdiff_exptl_absorpt_empirical_full_min 0.713