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_7063900
_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 H22 Cu N5 O8, Cl O4, 2(H2 O)'
_chemical_formula_sum            'C33 H26 Cl Cu N5 O14'
_chemical_formula_weight         815.58
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.465(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8093(2)
_cell_length_b                   18.7650(4)
_cell_length_c                   23.2256(6)
_cell_measurement_reflns_used    11433
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.7410
_cell_measurement_theta_min      3.0080
_cell_volume                     3402.40(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.911
_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    -85.00  -9.00   0.50    1.61    --  -40.83 121.00  37.00  152
  2  \w   -108.00 -59.00   0.50    1.61    --  -40.83-145.00  60.00   98
  3  \w   -118.00   5.00   0.50    1.61    --  -40.83  -9.00  58.00  246
  4  \w    -87.00 -12.00   0.50    1.61    --  -40.83 126.00 -55.00  150
  5  \w    -25.00  36.00   0.50    1.61    --  -40.83   9.00-127.00  122
  6  \w    -18.00 118.00   0.50    1.61    --   40.83   9.00-127.00  272
  7  \w     31.00  87.00   0.50    1.61    --   40.83-121.00 -44.00  112
  8  \w    -36.00  25.00   0.50    1.61    --   40.83  -9.00  58.00  122
  9  \w     34.00  91.00   0.50    1.61    --   40.83-126.00-131.00  114
 10  \w   -106.00 -26.00   0.50    2.00    --  -82.50 153.00-162.00  160
 11  \w   -159.00 -37.00   0.50    2.00    --  -82.50  -9.00  58.00  244
 12  \w   -148.00 -72.00   0.50    2.00    --  -82.50-126.00-131.00  152
 13  \w     81.00 170.00   0.50    2.00    --  104.00 145.00 112.00  178
 14  \w     45.00 178.00   0.50    2.00    --  104.00   9.00-127.00  266
 15  \w     97.00 168.00   0.50    2.00    --  104.00 121.00  37.00  142
 16  \w     39.00 113.00   0.50    2.00    --  104.00-126.00-131.00  148
 17  \w     40.00 110.00   0.50    2.00    --  104.00-121.00 -44.00  140
 18  \w   -107.00 -24.00   0.50    1.61    --  -40.83 -43.00-150.00  166
 19  \w    -48.00  26.00   0.50    1.61    --  -40.83  43.00 -90.00  148
 20  \w    -27.00  37.00   0.50    1.61    --   40.83 -32.00-180.00  128
 21  \w   -151.00 -59.00   0.50    2.00    --  -82.50-145.00  60.00  184
 22  \w    -47.00 -15.00   0.50    2.00    --  -82.50  42.00   0.00   64
 23  \w     35.00 105.00   0.50    2.00    --  104.00 -77.00   0.00  140
 24  \w     36.00  68.00   0.50    2.00    --  104.00 -59.00 -60.00   64
 25  \w     36.00  68.00   0.50    2.00    --  104.00 -59.00-180.00   64
 26  \w    102.00 170.00   0.50    2.00    --  104.00 111.00  60.00  136
 27  \w     89.00 174.00   0.50    2.00    --  104.00  25.00 -30.00  170
 28  \w     62.00 146.00   0.50    2.00    --  104.00 178.00  60.00  168
 29  \w     38.00  67.00   0.50    2.00    --  104.00 -68.00-180.00   58
 30  \w     37.00  64.00   0.50    2.00    --  104.00 -59.00 150.00   54
 31  \w     96.00 142.00   0.50    2.00    --  104.00  77.00-150.00   92
 32  \w    148.00 173.00   0.50    2.00    --  104.00  77.00-150.00   50
 33  \w     36.00  80.00   0.50    2.00    --  104.00 -68.00 -60.00   88
 34  \w     74.00 106.00   0.50    2.00    --  104.00 -93.00   0.00   64
 35  \w     38.00  71.00   0.50    2.00    --  104.00 -68.00 -90.00   66
 36  \w     42.00  67.00   0.50    2.00    --  104.00 -59.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0189714000
_diffrn_orient_matrix_UB_12      -0.0815495000
_diffrn_orient_matrix_UB_13      0.0040751000
_diffrn_orient_matrix_UB_21      0.0158800000
_diffrn_orient_matrix_UB_22      0.0046285000
_diffrn_orient_matrix_UB_23      0.0661518000
_diffrn_orient_matrix_UB_31      -0.1957500000
_diffrn_orient_matrix_UB_32      0.0083436000
_diffrn_orient_matrix_UB_33      0.0032460000
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26759
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.115
_diffrn_reflns_theta_min         3.028
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       needle
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1190P)^2^+0.9387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3889
_reflns_number_total             6103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01491c2.cif
_cod_data_source_block           lh2-c-3_autored
_cod_depositor_comments
'Adding full bibliography for 7063897--7063900.cif.'
_cod_database_code               7063900
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C N H O Cu Cl'
_olex2_refinement_description
;
1. Restrained distances
 Cu1-H3A \\sim Cu1-H3B
 with sigma of 0.02
2.a Free rotating group:
 O3(H3A,H3B), O14(H14A,H14B), O13(H13A,H13B)
;
_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 1.595
_oxdiff_exptl_absorpt_empirical_full_min 0.568