Terpyridine copper(II) complexes as potential anticancer agents by inhibiting cell proliferation, blocking the cell cycle and inducing apoptosis in BEL-7402 cells.
Gu, Yun-Qiong; Zhong, Yu-Jun; Hu, Mei-Qi; Li, Huan-Qing; Yang, Kun; Dong, Qi; Liang, Hong; Chen, Zhen-Feng; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1968–1978; doi:10.1039/d1dt02988f

data_7709102
_publ_section_title
;
 Terpyridine copper(II) complexes as potential anticancer agents by
 inhibiting cell proliferation, blocking the cell cycle and inducing
 apoptosis in BEL-7402 cells.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1968
_journal_page_last               1978
_journal_paper_doi               10.1039/d1dt02988f
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C21 H14 Br Cl Cu N3 O, Cl O4'
_chemical_formula_sum            'C21 H14 Br Cl2 Cu N3 O5'
_chemical_formula_weight         602.70
_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
_audit_creation_date             2021-11-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-14 deposited with the CCDC.	2021-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.083(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7892(4)
_cell_length_b                   7.3307(3)
_cell_length_c                   25.4885(10)
_cell_measurement_reflns_used    3588
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5670
_cell_measurement_theta_min      3.6440
_cell_volume                     2386.18(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_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     -8.00  90.00   1.00    6.00    --   17.61  38.00   0.00   98
  2  \w     -8.00  90.00   1.00    6.00    --   17.61  38.00  90.00   98
  3  \w    -20.00  60.00   1.00    6.00    --   17.61 -99.00  90.00   80
  4  \w    -96.00 -34.00   1.00    6.00    --  -19.88 178.00-150.00   62
  5  \w    -96.00 -35.00   1.00    6.00    --  -19.88-178.00 -60.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0057921000
_diffrn_orient_matrix_UB_12      -0.0044861000
_diffrn_orient_matrix_UB_13      -0.0274990000
_diffrn_orient_matrix_UB_21      0.0549819000
_diffrn_orient_matrix_UB_22      -0.0087588000
_diffrn_orient_matrix_UB_23      0.0044848000
_diffrn_orient_matrix_UB_31      -0.0052711000
_diffrn_orient_matrix_UB_32      -0.0962344000
_diffrn_orient_matrix_UB_33      0.0008853000
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            17830
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.324
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic bluish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4869
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0437P)^2^+3.1624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3368
_reflns_number_total             4869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02988f2.cif
_cod_data_source_block           20190422-czf-zyj-b4cuclo4aaa
_cod_depositor_comments
'Adding full bibliography for 7709100--7709103.cif.'
_cod_original_cell_volume        2386.17(15)
_cod_database_code               7709102
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.388
_reflns_odcompleteness_completeness 99.64
_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 O(H) groups
2. Restrained distances
 O2A-O4A
 2.5 with sigma of 0.02
 O5A-O4A
 2.5 with sigma of 0.02
 O5A-O3A
 2.5 with sigma of 0.02
 O5A-O2A
 2.5 with sigma of 0.02
 O3A-O5A
 2.5 with sigma of 0.02
 O4A-O5A
 2.5 with sigma of 0.02
 O3A-O2A
 2.5 with sigma of 0.02
 O2-O4 \\sim O5-O3
 with sigma of 0.002
 O4A-O5A \\sim O3A-O2A
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim O2 \\sim O4 \\sim O5 \\sim O3 \\sim O4A \\sim O5A \\sim O3A \\sim
O2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O3A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O2, O4, O5, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O4A, O5A, O3A, O2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O4A)=Sof(O5A)=Sof(O3A)=Sof(O2A)=1-FVAR(1)
 Sof(O2)=Sof(O4)=Sof(O5)=Sof(O3)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C21(H21), C5(H5), C4(H4), C3(H3), C11(H11), C14(H14), C15(H15),
 C18(H18), C13(H13), C16(H16), C12(H12), C17(H17)
6.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              4295
_shelx_hkl_checksum              4298
_shelx_fab_checksum              96975
_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 1.754
_oxdiff_exptl_absorpt_empirical_full_min 0.695