Copper(ii) thiosemicarbazone complexes induce marked ROS accumulation and promote nrf2-mediated antioxidant response in highly resistant breast cancer cells.
Sîrbu, Angela; Palamarciuc, Oleg; Babak, Maria V.; Lim, Jia Min; Ohui, Kateryna; Enyedy, Eva A.; Shova, Sergiu; Darvasiová, Denisa; Rapta, Peter; Ang, Wee Han; Arion, Vladimir B.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3833–3847; doi:10.1039/c7dt00283a

data_7042281
_publ_section_title
;
 Copper(ii) thiosemicarbazone complexes induce marked ROS accumulation and
 promote nrf2-mediated antioxidant response in highly resistant breast
 cancer cells.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3833
_journal_page_last               3847
_journal_paper_doi               10.1039/c7dt00283a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C12 H19 Cu N3 O6 S4'
_chemical_formula_sum            'C12 H19 Cu N3 O6 S4'
_chemical_formula_weight         493.08
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-16
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_cell_angle_alpha                75.444(7)
_cell_angle_beta                 77.550(6)
_cell_angle_gamma                76.945(5)
_cell_formula_units_Z            2
_cell_length_a                   6.3750(3)
_cell_length_b                   12.3166(9)
_cell_length_c                   13.7976(12)
_cell_measurement_reflns_used    2830
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6180
_cell_measurement_theta_min      2.0870
_cell_volume                     1006.89(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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -51.00  37.00   1.00   10.00    --   17.94 -38.00 -30.00   88
  2  \w    -15.00  16.00   1.00   10.00    --  -15.76 -99.00 150.00   31
  3  \w     -1.00  87.00   1.00   10.00    --   17.94  38.00 150.00   88
  4  \w     -7.00  19.00   1.00   10.00    --   17.94  19.00 150.00   26
  5  \w    -81.00  10.00   1.00   10.00    --  -15.76 -77.00 -90.00   91
  6  \w     43.00  71.00   1.00   10.00    --   17.94 178.00 -90.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0432348000
_diffrn_orient_matrix_UB_12      -0.0518420000
_diffrn_orient_matrix_UB_13      0.0312688000
_diffrn_orient_matrix_UB_21      -0.0076002000
_diffrn_orient_matrix_UB_22      0.0291595000
_diffrn_orient_matrix_UB_23      0.0392442000
_diffrn_orient_matrix_UB_31      -0.1072327000
_diffrn_orient_matrix_UB_32      -0.0110918000
_diffrn_orient_matrix_UB_33      0.0196322000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6669
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.55
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84852
_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            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3554
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+3.6690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                3037
_reflns_number_total             3554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00283a2.cif
_cod_data_source_block           shi_3089
_cod_depositor_comments
'Adding full bibliography for 7042280--7042281.cif.'
_cod_original_cell_volume        1006.90(12)
_cod_database_code               7042281
_chemical_oxdiff_formula         'C30 H30 N4 O4 S2 Cu1'
_chemical_oxdiff_usercomment     S.A._20
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S3X-S3Y
 0.6 with sigma of 0.01
 S3X-O5 \\sim S3-O5 \\sim S3Y-O5
 with sigma of 0.01
 C11X-C10X \\sim C10Y-C11Y \\sim C11-C10
 with sigma of 0.01
 S3-C11 \\sim S3Y-C11Y \\sim S3X-C11X \\sim S3-C10 \\sim S3Y-C10Y \\sim S3X-C10X
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(S3) = Uiso(S3X) = Uiso(S3Y)
Uiso(C11) = Uiso(C11Y) = Uiso(C11X) = Uiso(C10) = Uiso(C10Y) = Uiso(C10X)
4. Others
 Fixed Sof: S3(0.4) S3X(0.4) S3Y(0.2) C10(0.4) H10A(0.4) H10B(0.4) H10C(0.4)
 C10X(0.4) H10D(0.4) H10E(0.4) H10F(0.4) C10Y(0.2) H10G(0.2) H10H(0.2)
 H10I(0.2) C11(0.4) H11A(0.4) H11B(0.4) H11C(0.4) C11X(0.4) H11D(0.4) H11E(0.4)
 H11F(0.4) C11Y(0.2) H11G(0.2) H11H(0.2) H11I(0.2)
5.a Riding coordinates:
 C10(H10A,H10B,H10C), C10X(H10D,H10E,H10F), C10Y(H10G,H10H,H10I), C11(H11A,
 H11B,H11C), C11X(H11D,H11E,H11F), C11Y(H11G,H11H,H11I), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C3(H3), C5(H5), C7(H7)
5.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
;
_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 1.102
_oxdiff_exptl_absorpt_empirical_full_min 0.881