Synthesis, structural studies, interaction with DNA/HSA and antitumor evaluation of new Cu(ii) complexes containing 2-(1H-imidazol-2-yl)pyridine and amino acids
Cai, Dai-Hong; Chen, Bai-Hua; Liu, Qi-Yan; Le, Xue-Yi; He, Liang; Dalton Transactions  (2022) –; doi:10.1039/D2DT02985E

data_7711517
_publ_section_title
;
 Synthesis, structural studies, interaction with DNA/HSA and antitumor
 evaluation of new Cu(ii) complexes containing
 2-(1H-imidazol-2-yl)pyridine and amino acids
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02985E
_journal_year                    2022
_chemical_formula_moiety         'C16 H14 Cu N6, 2(Cl O4)'
_chemical_formula_sum            'C16 H14 Cl2 Cu N6 O8'
_chemical_formula_weight         552.77
_chemical_name_systematic        '[Cu(ipy)2(ClO4)2]'
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-02 deposited with the CCDC.	2022-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                68.331(7)
_cell_angle_beta                 78.340(5)
_cell_angle_gamma                86.540(6)
_cell_formula_units_Z            2
_cell_length_a                   8.4596(5)
_cell_length_b                   9.9394(8)
_cell_length_c                   13.2717(9)
_cell_measurement_reflns_used    1739
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      64.5840
_cell_measurement_theta_min      4.7880
_cell_volume                     1015.54(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0855
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.920
_diffrn_measured_fraction_theta_max 0.979
_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    -44.00  28.00   1.00   15.20    --  -51.25  77.00  90.00   72
  2  \w     35.00  70.00   1.00    4.42    --    0.00 178.00  30.00   35
  3  \w     42.00  84.00   1.00    4.42    --    0.00 178.00 -60.00   42
  4  \w     84.00 109.00   1.00   15.20    --   51.25 125.00-150.00   25
  5  \w     79.00 127.00   1.00   15.20    --   51.25 125.00-180.00   48
  6  \w     37.00  79.00   1.00    4.42    --    0.00 178.00-180.00   42
  7  \w    -29.00 110.00   1.00   15.20    --   51.25 -30.00 120.00  139
  8  \w     61.00  87.00   1.00    5.00    --  102.50-104.00 150.00   26
  9  \w     99.00 151.00   1.00    5.00    --  102.50 -37.00 120.00   52
 10  \w    112.00 176.00   1.00    5.00    --  102.50  12.00 120.00   64
 11  \w    118.00 153.00   1.00    5.00    --  102.50  50.00 150.00   35
 12  \w     83.00 110.00   1.00   15.20    --   51.25  92.00 165.00   27
 13  \w     71.00 114.00   1.00    5.00    --  102.50  50.00 150.00   43
 14  \w     80.00 107.00   1.00    5.00    --  102.50  92.00 165.00   27
 15  \w     24.00 109.00   1.00    5.00    --  102.50  12.00 120.00   85
 16  \w    119.00 172.00   1.00    5.00    --  102.50  50.00   0.00   53
 17  \w    101.00 134.00   1.00    5.00    --  102.50 -63.00-180.00   33
 18  \w     90.00 117.00   1.00    5.00    --  102.50 -91.00 -90.00   27
 19  \w     49.00  75.00   1.00   15.20    --   51.25 -94.00 -60.00   26
 20  \w     21.00  87.00   1.00    5.00    --  102.50-104.00 -30.00   66
 21  \w     95.00 122.00   1.00    5.00    --  102.50 -92.00  53.00   27
 22  \w     31.00  57.00   1.00    5.00    --  102.50-104.00 -60.00   26
 23  \w     27.00 135.00   1.00    5.00    --  102.50 -50.00 -30.00  108
 24  \w     68.00  94.00   1.00    5.00    --  102.50  50.00   0.00   26
 25  \w     27.00  69.00   1.00    5.00    --  102.50 -37.00 120.00   42
 26  \w     22.00 134.00   1.00    5.00    --  102.50 -93.00 167.52  112
 27  \w     21.00 138.00   1.00    5.00    --  102.50 -93.00  -4.16  117
 28  \w     36.00  95.00   1.00    5.00    --  102.50 -63.00-180.00   59
 29  \w     18.00  43.00   1.00    4.42    --    0.00 -99.00-120.00   25
 30  \w    -23.00  17.00   1.00    4.42    --    0.00 -99.00-120.00   40
 31  \w    -26.00   7.00   1.00   15.20    --   51.25 -94.00 -60.00   33
 32  \w      2.00  92.00   1.00   15.20    --   51.25-125.00  60.00   90
 33  \w     15.00  81.00   1.00   15.20    --   51.25 -94.00 150.00   66
 34  \w    -30.00  -4.00   1.00   15.20    --   51.25 -94.00 150.00   26
 35  \w    -79.00  22.00   1.00   15.20    --  -51.25  61.00 -30.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0955744000
_diffrn_orient_matrix_UB_12      0.1121953000
_diffrn_orient_matrix_UB_13      0.0418739000
_diffrn_orient_matrix_UB_21      -0.0607257000
_diffrn_orient_matrix_UB_22      0.0670944000
_diffrn_orient_matrix_UB_23      -0.1097319000
_diffrn_orient_matrix_UB_31      -0.1475189000
_diffrn_orient_matrix_UB_32      -0.1036044000
_diffrn_orient_matrix_UB_33      0.0491533000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.920
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5709
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         64.770
_diffrn_reflns_theta_min         3.653
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0779P)^2^+0.6893P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2740
_reflns_number_total             3373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02985e2.cif
_cod_data_source_block           exp_22406
_cod_original_cell_volume        1015.54(14)
_cod_database_code               7711517
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60
_olex2_refinement_description
;
1. Rigid bond restraints
 Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
Cl1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O0AA) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1AA) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O2(0.33333) O1AA(0.33333) O0AA(0.33333)
;
_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 1.924
_oxdiff_exptl_absorpt_empirical_full_min 0.720