Synthesis, characterization and biological studies of pyrazole-linked Schiff bases and their copper(ii) complexes as potential therapeutics
Kumari, Pratima; Kumar, Aman; Kataria, Ramesh; Kaushik, Navin Kumar; Ahmed, Mukhtar; Ansari, Azaj; Ekta,; Brahma, Mettle; Maruthi, Mulaka; Babu, Yangala Sudheer; Singh, Bijender; Kumar, Vinod; RSC Advances 15 (2025) 42299–42314; doi:10.1039/D5RA06008G

data_7251228
_publ_section_title
;
 Synthesis, characterization and biological studies of pyrazole-linked
 Schiff bases and their copper(ii) complexes as potential therapeutics
;
_journal_issue                   50
_journal_name_full               'RSC Advances'
_journal_page_first              42299
_journal_page_last               42314
_journal_paper_doi               10.1039/D5RA06008G
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         '2(C27 H24 Br Cu N5 O5), 5(H2 O)'
_chemical_formula_sum            'C54 H58 Br2 Cu2 N10 O15'
_chemical_formula_weight         1374.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-25
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2025-06-26 deposited with the CCDC.	2025-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                102.979(3)
_cell_angle_beta                 109.334(4)
_cell_angle_gamma                107.627(4)
_cell_formula_units_Z            2
_cell_length_a                   14.0326(6)
_cell_length_b                   15.3151(6)
_cell_length_c                   15.7791(6)
_cell_measurement_reflns_used    14925
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3210
_cell_measurement_theta_min      3.3800
_cell_volume                     2843.7(3)
_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-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.945
_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     -2.00  55.00   0.50   13.86    --   -9.32  67.00  73.00  114
  2  \w    -41.00  -6.00   0.50   13.86    --   -9.32 -67.00 -60.00   70
  3  \w    -53.00  15.00   0.50   13.86    --    9.60 -67.00 -60.00  136
  4  \w     -7.00  24.00   0.50   13.86    --    9.60  67.00  73.00   62
  5  \w    -33.00  36.00   0.50   13.86    --   -9.32  77.00 -30.00  138
  6  \w    -14.00  18.00   0.50   13.86    --   -9.32 -97.00-168.55   64
  7  \w    -41.00 -15.00   0.50   13.86    --   -9.32 -77.00-150.00   52
  8  \w    -72.00   9.00   0.50   13.86    --   -9.32 -57.00-150.00  162
  9  \w    -24.00  42.00   0.50   13.86    --   -9.32  77.00 120.00  132
 10  \w     28.00  56.00   0.50   13.86    --    9.60-125.00-150.00   56
 11  \w    -54.00  22.00   0.50   13.86    --    9.60 -38.00   0.00  152
 12  \w      9.00  56.00   0.50   13.86    --    9.60-125.00-180.00   94
 13  \w    -34.00  -9.00   0.50   13.86    --    9.60 129.00 -27.14   50
 14  \w    -32.00  -6.00   0.50   13.86    --    9.60 123.00 -59.36   52
 15  \w      7.00  56.00   0.50   13.86    --    9.60-125.00  90.00   98
 16  \w    -32.00   8.00   0.50   13.86    --    9.60 -57.00 150.00   80
 17  \w    -46.00  -4.00   0.50   13.86    --    9.60 -38.00 -30.00   84
 18  \w      7.00  56.00   0.50   13.86    --    9.60-125.00 150.00   98
 19  \w    -46.00  12.00   0.50   13.86    --    9.60 -38.00-150.00  116
 20  \w      1.00  26.00   0.50   13.86    --    9.60  38.00   0.00   50
 21  \w    -10.00  23.00   0.50   13.86    --    9.60 -38.00 150.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0058276000
_diffrn_orient_matrix_UB_12      0.0275439000
_diffrn_orient_matrix_UB_13      0.0391252000
_diffrn_orient_matrix_UB_21      0.0420240000
_diffrn_orient_matrix_UB_22      0.0431473000
_diffrn_orient_matrix_UB_23      0.0046804000
_diffrn_orient_matrix_UB_31      -0.0406203000
_diffrn_orient_matrix_UB_32      0.0097752000
_diffrn_orient_matrix_UB_33      -0.0325164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.1493
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50678
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.149
_diffrn_reflns_theta_min         3.247
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63656
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.008
_exptl_crystal_size_mid          0.006
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         11920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1905
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0884P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.2034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5161
_reflns_number_total             11920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra06008g2.cif
_cod_data_source_block           Complex-4c
_cod_original_cell_volume        2843.7(2)
_cod_database_code               7251228
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O Cu Br'
_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,H) groups
2. Rigid bond restraints
 O8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Free rotating group:
 O6(H6A,H6B), O8(H8D,H8E), O7(H7A,H7B), O10(H10A,H10B), O9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C24A(H24A), C24(H24), C17A(H17A), C16A(H16A), C13A(H13A), C17(H17),
 C14A(H14A), C2A(H2A), C16(H16), C14(H14), C2(H2), C25(H25), C13(H13),
 C19A(H19A), C25A(H25A), C23(H23), C19(H19), C23A(H23A), C22A(H22A), C20(H20),
 C22(H22), C21(H21), C20A(H20A), C21A(H21A)
3.c Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C8A(H8AA,H8AB,H8AC), C8(H8A,H8B,H8C), C4(H4A,H4B,H4C),
 C27A(H27A,H27B,H27C), C26A(H26A,H26B,H26C), C27(H27D,H27E,H27F), C26(H26D,H26E,
 H26F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49080
_shelx_fab_checksum              13646
_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 1.477
_oxdiff_exptl_absorpt_empirical_full_min 0.676