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_7063898
_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 H20 Cl Cu N5 O7, 2(C H4 O), H2 O'
_chemical_formula_sum            'C35 H30 Cl Cu N5 O10'
_chemical_formula_weight         779.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-12-14
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.11.29 svn.rc9064207 for OlexSys, GUI svn.r7097)
;
_audit_update_record
;
2024-12-14 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            8
_cell_length_a                   18.1151(2)
_cell_length_b                   16.9077(2)
_cell_length_c                   21.8085(3)
_cell_measurement_reflns_used    31924
_cell_measurement_temperature    99.97(15)
_cell_measurement_theta_max      71.9430
_cell_measurement_theta_min      4.0520
_cell_volume                     6679.61(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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -62.00  27.00   0.50    2.49    --  -40.58  58.00 120.00  178
  2  \w    -70.00  29.00   0.50    2.49    --  -40.58  84.00-125.00  198
  3  \w    -69.00  29.00   0.50    2.49    --  -40.58  82.00 -16.00  196
  4  \w   -111.00 -13.00   0.50    2.49    --  -82.50  82.00 -16.00  196
  5  \w   -152.00 -78.00   0.50    2.49    --  -82.50 -84.00 114.00  148
  6  \w   -150.00 -61.00   0.50    2.49    --  -82.50 -58.00 -20.00  178
  7  \w    100.00 174.00   0.50    2.49    --  104.00  84.00-125.00  148
  8  \w     34.00 133.00   0.50    2.49    --  104.00 -84.00 114.00  198
  9  \w     37.00  67.00   0.50    2.49    --  104.00 -58.00 -20.00   60
 10  \w     83.00 171.00   0.50    2.49    --  104.00  58.00 120.00  176
 11  \w    100.00 173.00   0.50    2.49    --  104.00  82.00 -16.00  146
 12  \w    -26.00  62.00   0.50    2.49    --   40.58 -58.00 -20.00  176
 13  \w    -35.00  24.00   0.50    2.49    --   40.58 -11.00-150.00  118
 14  \w     18.00  78.00   0.50    2.49    --   40.58-104.00 -60.00  120
 15  \w     19.00 108.00   0.50    2.49    --   40.58  58.00 120.00  178
 16  \w    -22.00  70.00   0.50    2.49    --   40.58 -84.00 114.00  184
 17  \w    -22.00  69.00   0.50    2.49    --   40.58 -82.00-138.00  182
 18  \w    -47.00 -15.00   0.50    2.49    --  -82.50  42.00-180.00   64
 19  \w    -47.00 -15.00   0.50    2.49    --  -82.50  42.00 120.00   64
 20  \w    -47.00 -15.00   0.50    2.49    --  -82.50  42.00   0.00   64
 21  \w    -47.00 -15.00   0.50    2.49    --  -82.50  42.00-150.00   64
 22  \w     36.00  68.00   0.50    2.49    --  104.00 -59.00 120.00   64
 23  \w     36.00  68.00   0.50    2.49    --  104.00 -59.00-180.00   64
 24  \w     36.00  83.00   0.50    2.49    --  104.00 -68.00 120.00   94
 25  \w     38.00 118.00   0.50    2.49    --  104.00-133.00   0.00  160
 26  \w     36.00  68.00   0.50    2.49    --  104.00 -59.00 -30.00   64
 27  \w     36.00  83.00   0.50    2.49    --  104.00 -68.00 -60.00   94
 28  \w     36.00  68.00   0.50    2.49    --  104.00 -59.00-120.00   64
 29  \w     36.00  68.00   0.50    2.49    --  104.00 -59.00 -90.00   64
 30  \w     35.00 105.00   0.50    2.49    --  104.00 -77.00  30.00  140
 31  \w     36.00  83.00   0.50    2.49    --  104.00 -68.00-180.00   94
 32  \w    104.00 177.00   0.50    2.49    --  104.00  93.00  30.00  146
 33  \w     36.00  68.00   0.50    2.49    --  104.00 -59.00 150.00   64
 34  \w     36.00  68.00   0.50    2.49    --  104.00 -59.00   0.00   64
 35  \w     36.00  83.00   0.50    2.49    --  104.00 -68.00  30.00   94
 36  \w     79.00 177.00   0.50    2.49    --  104.00  17.00-120.00  196
;
_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      0.0165823000
_diffrn_orient_matrix_UB_12      -0.0401529000
_diffrn_orient_matrix_UB_13      -0.0619109000
_diffrn_orient_matrix_UB_21      -0.0719723000
_diffrn_orient_matrix_UB_22      -0.0480734000
_diffrn_orient_matrix_UB_23      0.0055172000
_diffrn_orient_matrix_UB_31      -0.0422162000
_diffrn_orient_matrix_UB_32      0.0661093000
_diffrn_orient_matrix_UB_33      -0.0335921000
_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  0.0338
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.948
_diffrn_reflns_theta_min         4.054
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91280
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       needle
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0693P)^2^+7.8064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5507
_reflns_number_total             6535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01491c2.cif
_cod_data_source_block           lh2-c-4_auto
_cod_depositor_comments
'Adding full bibliography for 7063897--7063900.cif.'
_cod_original_cell_volume        6679.63(15)
_cod_database_code               7063898
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Cu'
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.637
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C23(H23), C15(H15), C4(H4), C25(H25), C9(H9), C5(H5), C26(H26),
 C16(H16), C18(H18), C10(H10), C2(H2), C17(H17), C12(H12), C29(H29), C30(H30),
 C33(H33), C32(H32)
2.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C34(H34A,H34B,H34C)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O1(H1), O9(H9A)
;
_shelx_res_checksum              9955
_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 1.165
_oxdiff_exptl_absorpt_empirical_full_min 0.883