Ruthenium(II)-bisdemethoxycurcumin conjugate complexes as potent antitumour agents through simultaneous inhibition of 20S proteasome and HMG-CoA reductase.
Pagliaricci, Sara; Pagliaricci, Noemi; Tombesi, Alessia; Pettinari, Claudio; Cuccioloni, Massimiliano; Juricic, Helena; Galindo, Agustín; Fadaei-Tirani, Farzaneh; Pettinari, Riccardo; Marchetti, Fabio; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11324–11336; doi:10.1039/d5dt01240f

data_7718992
_publ_section_title
;
 Ruthenium(II)-bisdemethoxycurcumin conjugate complexes as potent
 antitumour agents through simultaneous inhibition of 20S proteasome and
 HMG-CoA reductase.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11324
_journal_page_last               11336
_journal_paper_doi               10.1039/d5dt01240f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C39 H33 Cl O8 Ru, 1[CHCl3]'
_chemical_formula_sum            'C40 H34 Cl4 O8 Ru'
_chemical_formula_weight         885.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-17 deposited with the CCDC.	2025-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.4732(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.9810(4)
_cell_length_b                   11.5684(2)
_cell_length_c                   33.7222(5)
_cell_measurement_reflns_used    20949
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      69.5830
_cell_measurement_theta_min      2.6180
_cell_volume                     7759.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.135a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.131a 64-bit (release 19-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.135a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.950
_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     22.00  52.00   0.50    0.05    --   52.35 -95.00-120.00   60
  2  \w     35.00  61.00   0.50    0.05    --   52.35-125.00 -60.00   52
  3  \w     17.00  52.00   0.50    0.05    --   52.35 -95.00-150.00   70
  4  \w     21.00  47.00   0.50    0.05    --   52.35 -95.00   0.00   52
  5  \w     20.00  61.00   0.50    0.05    --   52.35 -95.00 -60.00   82
  6  \w     15.00  56.00   0.50    0.05    --   52.35 -95.00 150.00   82
  7  \w    -74.00 -47.00   0.50    0.05    --  -54.63 -15.00  60.00   54
  8  \w    -46.00 -16.00   0.50    0.05    --  -54.63 125.00 150.00   60
  9  \w    -79.00 -49.00   0.50    0.05    --  -54.63 125.00 150.00   60
 10  \w    -83.00 -23.00   0.50    0.05    --  -54.63 -15.00 120.00  120
 11  \w    -53.00 -27.00   0.50    0.05    --  -54.63   0.00-180.00   52
 12  \w    -59.00 -20.00   0.50    0.05    --  -54.63   0.00  60.00   78
 13  \w    -98.00 -23.00   0.50    0.05    --  -54.63 -15.00-120.00  150
 14  \w     46.00  72.00   0.50    0.05    --   67.75 -95.00 -90.00   52
 15  \w     34.00  69.00   0.50    0.05    --   67.75 -95.00  30.00   70
 16  \w     46.00  72.00   0.50    0.05    --   67.75 -95.00  90.00   52
 17  \w     46.00  72.00   0.50    0.05    --   67.75 -95.00-150.00   52
 18  \w     33.00  71.00   0.50    0.05    --   67.75 -95.00-180.00   76
 19  \w     46.00 112.00   0.50    0.05    --   67.75  15.00 -30.00  132
 20  \w     46.00  71.00   0.50    0.05    --   67.75 -95.00-120.00   50
 21  \w     30.00  73.00   0.50    0.05    --   67.75 -95.00 120.00   86
 22  \w    -68.00 -37.00   0.50    0.05    --  -69.23   0.00-120.00   62
 23  \w    -72.00 -41.00   0.50    0.05    --  -69.23   0.00 -60.00   62
 24  \w    -72.00 -43.00   0.50    0.05    --  -69.23   0.00 150.00   58
 25  \w    -98.00 -55.00   0.50    0.05    --  -69.23 -15.00 -30.00   86
 26  \w    -61.00 -36.00   0.50    0.05    --  -69.23   0.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0401664000
_diffrn_orient_matrix_UB_12      -0.1138203000
_diffrn_orient_matrix_UB_13      -0.0012271000
_diffrn_orient_matrix_UB_21      0.0201749000
_diffrn_orient_matrix_UB_22      -0.0245268000
_diffrn_orient_matrix_UB_23      -0.0421484000
_diffrn_orient_matrix_UB_31      0.0630779000
_diffrn_orient_matrix_UB_32      -0.0646513000
_diffrn_orient_matrix_UB_33      0.0181172000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            57017
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.066
_diffrn_reflns_theta_min         2.221
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.239
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.135a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       prism
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.577
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         13987
_refine_ls_number_restraints     924
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0998P)^2^+45.2487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2206
_refine_ls_wR_factor_ref         0.2332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10345
_reflns_number_total             13987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01240f3.cif
_cod_data_source_block           rul5a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718990--7718993.cif.
;
_cod_database_code               7718992
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C39 H33 Cl4 O8 Ru'
_chemical_oxdiff_usercomment     'crystallised from DCM, Hexane'
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.316
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
O12 \\sim C51: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C36(H36), C73(H73), C75(H75)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24),
  C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35),
 C41(H41), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50), C53(H53),
  C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C62(H62),
 C63(H63), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71), C74(H74)
4.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25655
_shelx_hkl_checksum              61838
_shelx_fab_checksum              99759
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.177
_oxdiff_exptl_absorpt_empirical_full_min 0.865