Structural and chemical investigation of a tridentate fluorescein hydrazone (LH3), a selective Cu2+ and Hg2+ chelator: detection of CN− and HSO4− by its Cu2+ complexes and effect on HeLa cell division
Bharti, Shachendra Kumar; Odera, Keiko; Tripathi, Kamini; Ward, Benzamin D.; Bhattacharya, S.; Takahashi, Ryoya; Mishra, Lallan; New Journal of Chemistry 49 (2025) 14219–14230; doi:10.1039/D5NJ01491C

data_7063897
_publ_section_title
;
 Structural and chemical investigation of a tridentate fluorescein
 hydrazone (LH3), a selective Cu2+ and Hg2+ chelator: detection of
 CN&#x2212; and HSO4&#x2212; by its Cu2+ complexes and effect on HeLa cell
 division
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14219
_journal_page_last               14230
_journal_paper_doi               10.1039/D5NJ01491C
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C33 H21 N5 O7'
_chemical_formula_sum            'C33 H21 N5 O7'
_chemical_formula_weight         599.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5246(5)
_cell_length_b                   11.8748(3)
_cell_length_c                   13.3999(4)
_cell_measurement_reflns_used    16424
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5130
_cell_measurement_theta_min      2.5660
_cell_volume                     2788.53(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     37.00  63.00   0.50   11.00    --   11.77  53.00  76.00   52
  2  \w    -57.00 -27.00   0.50   11.00    --   11.77 -79.00 164.00   60
  3  \w     -2.00  32.00   0.50   11.00    --   11.77 -79.00 164.00   68
  4  \w     -8.00  28.00   0.50   11.00    --   11.77  53.00  76.00   72
  5  \w    -26.00  18.00   0.50   11.00    --  -11.14 -99.00-180.00   88
  6  \w    -26.00  17.00   0.50   11.00    --  -11.14 -99.00 -60.00   86
  7  \w    -34.00  22.00   0.50   11.00    --  -11.14 -95.00  66.00  112
  8  \w    -33.00   0.00   0.50   11.00    --  -11.14 -53.00 -68.00   66
  9  \w    -19.00   6.00   0.50   11.00    --  -11.14 -99.00   0.00   50
 10  \w    -65.00 -40.00   0.50   11.00    --  -11.14 -53.00 -68.00   50
 11  \w     16.00  60.00   0.50   11.00    --   11.77-125.00  60.00   88
 12  \w    -42.00  -3.00   0.50   11.00    --   11.77 -19.00  60.00   78
 13  \w     11.00  55.00   0.50   11.00    --   11.77-125.00-180.00   88
 14  \w     25.00  51.00   0.50   11.00    --   11.77-125.00 120.00   52
 15  \w    -36.00  20.00   0.50   11.00    --   11.77 -38.00 120.00  112
 16  \w    -56.00   5.00   0.50   11.00    --   11.77 -19.00 150.00  122
 17  \w     11.00  69.00   0.50   11.00    --   11.77  57.00 -60.00  116
 18  \w     32.00  57.00   0.50   11.00    --   11.77-125.00   0.00   50
 19  \w    -54.00  -9.00   0.50   11.00    --   11.77 -19.00-180.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28927
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.570
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish red'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Flack x determined using 1510 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(5)
_refine_ls_extinction_coef       0.0035(10)
_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   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         4895
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0603P)^2^+0.2184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3872
_reflns_number_total             4895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01491c2.cif
_cod_data_source_block           c-23_auto
_cod_depositor_comments
'Adding full bibliography for 7063897--7063900.cif.'
_cod_original_cell_volume        2788.52(14)
_cod_database_code               7063897
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co N H C O '
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.976
_olex2_refinement_description
;
1. Rigid bond restraints
 N4, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33, N4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C33, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
2. Rigid body (RIGU) restrains
 C33, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.04
3. Others
 Fixed Sof: O1(0.25) H1(0.25) O2(0.75) H2A(0.75)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C24(H24), C26(H26), C4(H4), C5(H5), C29(H29), C30(H30), C12(H12),
 C18(H18), C17(H17), C37(H37), C9(H9), C38(H38), C20(H20), C19(H19), C10(H10),
 C35(H35), C34(H34)
4.b Idealised tetrahedral OH refined as rotating group:
 O42(H42), O45(H45), O1(H1), O2(H2A)
;
_shelx_res_checksum              71498
_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 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.870