Chemical biology suggests pleiotropic effects for a novel hexanuclear copper(II) complex inducing apoptosis in hepatocellular carcinoma cells
Zhang, Junshuai; Hu, Jiyong; Peng, Kun; Song, Wei; Zhi, Shuangcheng; Yang, Endian; Zhao, Jin'an; Hou, Hongwei; Chemical Communications  (2019) –; doi:10.1039/C9CC05995D

data_7124145
_publ_section_title
;
 Chemical biology suggests pleiotropic effects for a novel hexanuclear
 copper(II) complex inducing apoptosis in hepatocellular carcinoma cells
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05995D
_journal_year                    2019
_chemical_formula_moiety         'C45 H33 Cu3 N15 O18'
_chemical_formula_sum            'C45 H33 Cu3 N15 O18'
_chemical_formula_weight         1262.48
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-12-16 deposited with the CCDC.    2019-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.521(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1943(4)
_cell_length_b                   24.9979(10)
_cell_length_c                   19.9314(7)
_cell_measurement_reflns_used    5175
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.2010
_cell_measurement_theta_min      4.0210
_cell_volume                     6056.8(4)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5281
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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    -93.00  -2.00   1.00    3.50    --  -40.54 125.00 -30.00   91
  2  \w    -76.00  -2.00   1.00    3.50    --  -40.54 125.00 -90.00   74
  3  \w   -110.00 -23.00   1.00    3.50    --  -40.54 -37.00  30.00   87
  4  \w      3.00  81.00   1.00    3.50    --   40.54 -99.00 -90.00   78
  5  \w     92.00 162.00   1.00   14.00    --  106.40  45.00 120.00   70
  6  \w     94.00 178.00   1.00   14.00    --  106.40 125.00  30.00   84
  7  \w    126.00 153.00   1.00   14.00    --  106.40 125.00   0.00   27
  8  \w     96.00 178.00   1.00   14.00    --  106.40  61.00-150.00   82
  9  \w     77.00 173.00   1.00   14.00    --  106.40  61.00 150.00   96
 10  \w     30.00 133.00   1.00   14.00    --  106.40 -77.00  90.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0393185000
_diffrn_orient_matrix_UB_12      0.0500897000
_diffrn_orient_matrix_UB_13      0.0364135000
_diffrn_orient_matrix_UB_21      0.0067532000
_diffrn_orient_matrix_UB_22      -0.0310925000
_diffrn_orient_matrix_UB_23      0.0668315000
_diffrn_orient_matrix_UB_31      0.1202867000
_diffrn_orient_matrix_UB_32      0.0180655000
_diffrn_orient_matrix_UB_33      0.0145821000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_number            10705
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         4.044
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44029
_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_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             2556
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.067
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         10705
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1613
_refine_ls_R_factor_gt           0.0997
_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^)+(0.1550P)^2^+13.1008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2623
_refine_ls_wR_factor_ref         0.3155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5657
_reflns_number_total             10705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05995d2.cif
_cod_data_source_block           1
_cod_database_code               7124145
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.704
_reflns_odcompleteness_completeness 99.28
_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
2. Restrained distances
 O10-N13
 1.284 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C32(H32A,H32B), C19(H19A,H19B)
3.b Aromatic/amide H refined with riding coordinates:
 C73(H73), C15(H15), C17(H17), C10(H10), C43(H43), C33(H33), C20(H20), C8(H8),
 C4(H4), C30(H30), C21(H21), C22(H22), C11(H11), C2(H2), C1(H1), C27(H27),
 C23(H23), C36(H36), C9(H9), C3(H3), C35(H35), C28(H28), C42(H42), C40(H40),
 C29(H29), C41(H41), C34(H34)
;
_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 2.088
_oxdiff_exptl_absorpt_empirical_full_min 0.556