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_7713670
_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 H22 Br2 Cl4 Cu N9 O2'
_chemical_formula_sum            'C38 H22 Br2 Cl4 Cu N9 O2'
_chemical_formula_weight         1001.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 97.788(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.4053(15)
_cell_length_b                   14.7639(8)
_cell_length_c                   22.8746(16)
_cell_measurement_reflns_used    3409
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4730
_cell_measurement_theta_min      2.5100
_cell_volume                     7831.5(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  88.00   1.00   12.00    --   30.00  54.00-180.00   26
  2  \w    -69.00 113.00   1.00   12.00    --   30.00  54.00   0.00  182
;
_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      -0.0117219000
_diffrn_orient_matrix_UB_12      0.0270350000
_diffrn_orient_matrix_UB_13      0.0210875000
_diffrn_orient_matrix_UB_21      0.0248534000
_diffrn_orient_matrix_UB_22      0.0280101000
_diffrn_orient_matrix_UB_23      0.0027491000
_diffrn_orient_matrix_UB_31      -0.0134520000
_diffrn_orient_matrix_UB_32      0.0281160000
_diffrn_orient_matrix_UB_33      -0.0229763000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12775
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.34
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85497
_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            green
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3968
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6890
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+9.1867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                4393
_reflns_number_total             6890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt01750h2.cif
_cod_data_source_block           220423e
_cod_database_code               7713670
_reflns_odcompleteness_completeness 99.93
_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
2. Uiso/Uaniso restraints and constraints
Uanis(Br2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(Br1) = Uanis(Br1')
Uanis(Br2) = Uanis(Br2')
3. Others
 Sof(Br1')=Sof(Br2')=1-FVAR(1)
 Sof(Br1)=Sof(Br2)=FVAR(1)
4.a 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),
 C16(H16), C22(H22), C24(H24), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34)
4.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C)
4.c 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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.834