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_7711518
_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_absolute_configuration rm
_chemical_formula_moiety         'C17 H19 Cu N4 O3, Cl O4, 0.5(O)'
_chemical_formula_sum            'C17 H19 Cl Cu N4 O7.5'
_chemical_formula_weight         498.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-31 deposited with the CCDC.	2022-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3660(2)
_cell_length_b                   15.6213(3)
_cell_length_c                   21.2384(4)
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.2320
_cell_measurement_theta_min      4.0620
_cell_volume                     4102.69(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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   -101.00  -6.00   1.00    1.00    --  -40.09 -77.00 -30.00   95
  2  \w    -64.00  -2.00   1.00    1.00    --  -40.09 125.00  90.00   62
  3  \w     58.00  94.00   1.00    1.00    --   40.09-125.00-150.00   36
  4  \w     74.00 142.00   1.00    3.00    --  107.60  77.00 -60.00   68
  5  \w     81.00 134.00   1.00    3.00    --  107.60  45.00 120.00   53
  6  \w     94.00 135.00   1.00    3.00    --  107.60 125.00 120.00   41
  7  \w     36.00  91.00   1.00    3.00    --  107.60 -30.00-120.00   55
  8  \w     65.00 106.00   1.00    3.00    --  107.60 -94.00-180.00   41
  9  \w     88.00 117.00   1.00    3.00    --  107.60-125.00 -30.00   29
 10  \w    115.00 177.00   1.00    3.00    --  107.60  87.00 -20.00   62
 11  \w     23.00 110.00   1.00    3.00    --  107.60 -94.00  90.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0220295000
_diffrn_orient_matrix_UB_12      -0.0205690000
_diffrn_orient_matrix_UB_13      0.0697777000
_diffrn_orient_matrix_UB_21      0.1096726000
_diffrn_orient_matrix_UB_22      -0.0465139000
_diffrn_orient_matrix_UB_23      0.0044611000
_diffrn_orient_matrix_UB_31      0.0549392000
_diffrn_orient_matrix_UB_32      0.0844436000
_diffrn_orient_matrix_UB_33      0.0193262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15289
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.563
_diffrn_reflns_theta_min         3.512
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.567
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 3271 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.021(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+6.7112P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1623
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                7746
_reflns_number_total             8049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02985e2.cif
_cod_data_source_block           a20102204a0826
_cod_depositor_comments
;

2024-09-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H38 Cl2 Cu2 N8 O15'
_cod_original_formula_weight         996.70
_cod_original_formula_moiety         '2(C17 H19 Cu N4 O3), 2(Cl O4), O'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        4102.69(12)
_cod_database_code               7711518
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         CHONZn
_chemical_oxdiff_usercomment     Ipy-Phe
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O3(H3A,H3B)
2.b Ternary CH refined with riding coordinates:
 C27(H27), C10(H10)
2.c Secondary CH2 refined with riding coordinates:
 N8(H8A,H8B), N4(H4A,H4B), C28(H28A,H28B), C11(H11A,H11B)
2.d Aromatic/amide H refined with riding coordinates:
 C25(H25), C24(H24), N3(H3), C8(H8), C1(H1), C21(H21), C2(H2), C30(H30),
 C3(H3C), C19(H19), N7(H7), C20(H20), C4(H4), C18(H18), C34(H34), C31(H31),
 C32(H32), C33(H33), C7(H7A), C13(H13), C17(H17), C15(H15), C14(H14), C16(H16)
;
_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 1.090
_oxdiff_exptl_absorpt_empirical_full_min 0.902