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_1571462
_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         'Br, C23 H19 N2'
_chemical_formula_sum            'C23 H19 Br N2'
_chemical_formula_weight         403.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-30
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-07-10 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.4840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   23.0173(3)
_cell_length_b                   10.11520(10)
_cell_length_c                   26.4430(3)
_cell_measurement_reflns_used    21664
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      79.4250
_cell_measurement_theta_min      4.6940
_cell_volume                     5646.64(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.980
_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     -7.00  20.00   0.50    1.68    --    0.00  77.00  30.00   54
  2  \w    -29.00  89.00   0.50    1.68    --    0.00  77.00-180.00  236
  3  \w    -16.00  10.00   0.50    1.68    --    0.00  77.00 -30.00   52
  4  \w    -39.00 -13.00   0.50    1.68    --    0.00 -37.00 -30.00   52
  5  \w     22.00  81.00   0.50    1.68    --    0.00  77.00  30.00  118
  6  \w     18.00  83.00   0.50    6.68    --  107.20 -30.00 -60.00  130
  7  \w     48.00 127.00   0.50    6.68    --  107.20 -30.00-180.00  158
  8  \w     33.00 135.00   0.50    6.68    --  107.20 -15.00 150.00  204
  9  \w     42.00 110.00   0.50    6.68    --  107.20 -61.00-150.00  136
 10  \w     84.00 114.00   0.50    6.68    --  107.20 -82.00 -90.00   60
 11  \w     21.00 140.00   0.50    6.68    --  107.20 -82.00 -30.00  238
 12  \w     18.00 127.00   0.50    6.68    --  107.20 -30.00  90.00  218
 13  \w     34.00 111.00   0.50    6.68    --  107.20 -61.00 -30.00  154
;
_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      -0.0677205000
_diffrn_orient_matrix_UB_12      -0.0251781000
_diffrn_orient_matrix_UB_13      -0.0429530000
_diffrn_orient_matrix_UB_21      0.0236699000
_diffrn_orient_matrix_UB_22      0.0127544000
_diffrn_orient_matrix_UB_23      -0.0466755000
_diffrn_orient_matrix_UB_31      0.0134335000
_diffrn_orient_matrix_UB_32      -0.1496614000
_diffrn_orient_matrix_UB_33      0.0032342000
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35513
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.756
_diffrn_reflns_theta_min         4.188
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.023
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+4.2607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11186
_reflns_number_total             12044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sd00345k2.cif
_cod_data_source_block           exp_844_bk-s1_autored
_cod_database_code               1571462
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C23 H19 Br N2'
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.695
_reflns_odcompleteness_completeness 99.92
_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
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C217(H21A,H21B), C317(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C206(H206), C203(H203), C12(H12), C16(H16), C10(H10),
 C202(H202), C302(H302), C8(H8), C7(H7), C219(H219), C6(H6), C9(H9), C223(H223),
  C303(H303), C208(H208), C216(H216), C23(H23), C306(H306), C13(H13),
 C222(H222), C221(H221), C15(H15), C220(H220), C207(H207), C212(H212),
 C210(H210), C307(H307), C215(H215), C323(H323), C316(H316), C214(H214),
 C313(H313), C209(H209), C312(H312), C14(H14), C22(H22), C308(H308), C213(H213),
  C19(H19), C314(H314), C315(H315), C310(H310), C309(H309), C319(H319),
 C322(H322), C20(H20), C21(H21), C320(H320), C321(H321)
;
_shelx_res_checksum              3660
_shelx_hkl_checksum              14910
_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 2.750
_oxdiff_exptl_absorpt_empirical_full_min 0.672