Detection of TNP and Sulfite Ion in Aqueous Medium by Pyrazinium-based Chemosensor
Pragya, Pragya; Rangan, Krishnan; Khungar, Bharti; Sensors & Diagnostics  (2024) –; doi:10.1039/D3SD00345K

data_1571463
_publ_section_title
;
 Detection of TNP and Sulfite Ion in Aqueous Medium by Pyrazinium-based
 Chemosensor
;
_journal_name_full               'Sensors &amp; Diagnostics'
_journal_paper_doi               10.1039/D3SD00345K
_journal_year                    2024
_chemical_formula_moiety         'C6 H2 N3 O7, C23 H19 N2'
_chemical_formula_sum            'C29 H21 N5 O7'
_chemical_formula_weight         551.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-07-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3755(2)
_cell_length_b                   19.6061(2)
_cell_length_c                   15.0107(2)
_cell_measurement_reflns_used    9445
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      79.4350
_cell_measurement_theta_min      4.9570
_cell_volume                     4975.02(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      93(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_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     -4.00  27.00   0.50    5.00    --    0.00  37.00 -90.00   62
  2  \w    -33.00  19.00   0.50    5.00    --    0.00 -37.00  30.00  104
  3  \w    -22.00  42.00   0.50    5.00    --    0.00  57.00-120.00  128
  4  \w     33.00  73.00   0.50    5.00    --    0.00  37.00 -60.00   80
  5  \w     42.00  70.00   0.50    5.00    --    0.00  37.00 -90.00   56
  6  \w     63.00 118.00   0.50   20.00    --  107.20 -61.00  60.00  110
  7  \w     47.00 125.00   0.50   20.00    --  107.20 -30.00  90.00  156
  8  \w     19.00 135.00   0.50   20.00    --  107.20 -15.00 120.00  232
  9  \w    117.00 194.00   0.50   20.00    --  107.20  30.00  90.00  154
 10  \w     65.00 128.00   0.50   20.00    --  107.20 -77.00  90.00  126
 11  \w     92.00 140.00   0.50   20.00    --  107.20 -82.00 120.00   96
 12  \w     18.00  51.00   0.50   20.00    --  107.20 -77.00  90.00   66
 13  \w     21.00 126.00   0.50   20.00    --  107.20 -30.00 -60.00  210
 14  \w     30.00  60.00   0.50   20.00    --  107.20 -82.00 120.00   60
 15  \w     70.00 111.00   0.50   20.00    --  107.20 -61.00-180.00   82
;
_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      -0.0209584000
_diffrn_orient_matrix_UB_12      -0.0762910000
_diffrn_orient_matrix_UB_13      -0.0117952000
_diffrn_orient_matrix_UB_21      -0.0178788000
_diffrn_orient_matrix_UB_22      0.0083609000
_diffrn_orient_matrix_UB_23      -0.1048322000
_diffrn_orient_matrix_UB_31      0.0868786000
_diffrn_orient_matrix_UB_32      -0.0167531000
_diffrn_orient_matrix_UB_33      0.0011381000
_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  0.0248
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15324
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.939
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00015(3)
_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   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0522P)^2^+8.8677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4806
_reflns_number_total             5281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sd00345k2.cif
_cod_data_source_block           exp_967-bk-8836_autored
_cod_database_code               1571463
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C29 H21 N5 O7'
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.884
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C26(H26), C28(H28)
;
_shelx_res_checksum              90033
_shelx_hkl_checksum              4293
_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 2.699
_oxdiff_exptl_absorpt_empirical_full_min 0.663