Hydrazylpyridine salicylaldehyde-copper(II)-1,10-phenanthroline complexes as potential anticancer agents: synthesis, characterization and anticancer evaluation
Chen, Yating; Ke, zhilin; Yuan, Lingyu; Liang, Meixiang; Zhang, Shuhua; Dalton Transactions  (2023) –; doi:10.1039/D3DT01750H

data_7713669
_publ_section_title
;
 Hydrazylpyridine salicylaldehyde-copper(II)-1,10-phenanthroline complexes
 as potential anticancer agents: synthesis, characterization and
 anticancer evaluation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01750H
_journal_year                    2023
_chemical_formula_moiety         'C38 H28 Cl2 Cu N8 O2, 0.5(H2 O)'
_chemical_formula_sum            'C38 H28 Cl2 Cu N8 O2.5'
_chemical_formula_weight         771.12
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-18 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.498(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6984(7)
_cell_length_b                   11.6109(5)
_cell_length_c                   20.2139(11)
_cell_measurement_reflns_used    3667
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7020
_cell_measurement_theta_min      2.5850
_cell_volume                     3684.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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      4.00  37.00   1.00    6.00    --   30.00  54.00-150.00   33
  2  \w     43.00  98.00   1.00    6.00    --   30.00  54.00-150.00   55
  3  \w    -74.00  37.00   1.00    6.00    --   30.00  54.00 120.00  111
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0349912000
_diffrn_orient_matrix_UB_12      -0.0023067000
_diffrn_orient_matrix_UB_13      -0.0224197000
_diffrn_orient_matrix_UB_21      -0.0286022000
_diffrn_orient_matrix_UB_22      0.0054881000
_diffrn_orient_matrix_UB_23      0.0267869000
_diffrn_orient_matrix_UB_31      0.0013061000
_diffrn_orient_matrix_UB_32      0.0607823000
_diffrn_orient_matrix_UB_33      -0.0032136000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11361
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1197P)^2^+4.4325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1958
_reflns_number_gt                4617
_reflns_number_total             6160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt01750h2.cif
_cod_data_source_block           220627c
_cod_original_formula_sum        'C38 H28 Cl2 Cu N8 O2.50'
_cod_database_code               7713669
_reflns_odcompleteness_completeness 92.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq, Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O1W) = Uanis(O1W')
3. Others
 Sof(O1W')=Sof(H1WC)=Sof(H1WD)=0.5*(1-FVAR(2))
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=0.5*FVAR(2)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O1W'(H1WC,H1WD)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C18(H18), C20(H20), C24(H24), C25(H25), C28(H28), C30(H30), C31(H31),
  C32(H32), C35(H35), C36(H36), C37(H37)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C)
4.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.844