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_7718993
_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         'C41 H45 Cl O6 Ru'
_chemical_formula_sum            'C41 H45 Cl O6 Ru'
_chemical_formula_weight         770.29
_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                 103.6285(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0501(3)
_cell_length_b                   17.3102(3)
_cell_length_c                   11.13310(13)
_cell_measurement_reflns_used    11264
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      73.7560
_cell_measurement_theta_min      2.3840
_cell_volume                     3567.89(10)
_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      139.99(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 1.000
_diffrn_measured_fraction_theta_max 0.972
_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     69.00 103.00   0.50    0.50    --   77.93-125.00 -60.00   68
  2  \w     35.00  94.00   0.50    0.50    --   69.57-125.00-120.00  118
  3  \w     41.00  93.00   0.50    0.50    --   69.57-125.00-180.00  104
  4  \w     80.00 105.00   0.50    0.50    --   77.93-125.00-180.00   50
  5  \w     41.00  72.00   0.50    0.50    --   77.93-125.00-180.00   62
  6  \w     79.00 104.00   0.50    0.50    --   77.93-125.00-150.00   50
  7  \w     69.00 105.00   0.50    0.50    --   77.93-125.00 -90.00   72
  8  \w     40.00  70.00   0.50    0.50    --   77.93 -95.00-150.00   60
  9  \w     37.00  75.00   0.50    0.50    --   66.04 -95.00-180.00   76
 10  \w     41.00  71.00   0.50    0.50    --   77.93 -95.00 -60.00   60
 11  \w     34.00  78.00   0.50    0.50    --   69.57 -95.00  60.00   88
 12  \w     34.00  64.00   0.50    0.50    --   69.57-108.00 137.00   60
 13  \w     30.00  55.00   0.50    0.50    --   66.04-108.00 137.00   50
 14  \w     40.00  72.00   0.50    0.50    --   77.93-108.00 137.00   64
 15  \w     33.00  74.00   0.50    0.50    --   69.57 -95.00  30.00   82
 16  \w     59.00  84.00   0.50    0.50    --   77.93 -95.00 -30.00   50
 17  \w     42.00  87.00   0.50    0.50    --   77.93   0.00 -60.00   90
 18  \w     54.00  79.00   0.50    0.50    --   77.93  15.00 150.00   50
 19  \w     83.00 108.00   0.50    0.50    --   77.93  15.00 150.00   50
 20  \w     56.00 115.00   0.50    0.50    --   77.93  15.00 -60.00  118
 21  \w     48.00 123.00   0.50    0.50    --   77.93  15.00-150.00  150
 22  \w    -80.00 -27.00   0.50    0.50    --  -66.76 108.00-126.00  106
 23  \w    -77.00 -33.00   0.50    0.50    --  -66.76 125.00 -90.00   88
 24  \w    -61.00 -33.00   0.50    0.50    --  -69.34 108.00-126.00   56
 25  \w    -68.00 -35.00   0.50    0.50    --  -69.34   0.00-120.00   66
 26  \w    -72.00 -38.00   0.50    0.50    --  -69.34   0.00-180.00   68
 27  \w    -72.00 -47.00   0.50    0.50    --  -66.76   0.00   0.00   50
 28  \w    -71.00 -33.00   0.50    0.50    --  -69.34   0.00  30.00   76
 29  \w    -70.00 -32.00   0.50    0.50    --  -69.34   0.00  90.00   76
 30  \w   -109.00 -45.00   0.50    0.50    --  -66.76 -15.00 150.00  128
;
_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      -0.0005858000
_diffrn_orient_matrix_UB_12      0.0862641000
_diffrn_orient_matrix_UB_13      0.0338399000
_diffrn_orient_matrix_UB_21      0.0780761000
_diffrn_orient_matrix_UB_22      0.0081639000
_diffrn_orient_matrix_UB_23      -0.0147627000
_diffrn_orient_matrix_UB_31      -0.0289480000
_diffrn_orient_matrix_UB_32      0.0203791000
_diffrn_orient_matrix_UB_33      -0.1374244000
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34477
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.678
_diffrn_reflns_theta_min         2.387
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.628
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.466
_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 light orange'
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7107
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0433P)^2^+4.1880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5796
_reflns_number_total             7107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01240f3.cif
_cod_data_source_block           rul1b
_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_original_cell_volume        3567.91(10)
_cod_database_code               7718993
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C41 H45 Cl O6 Ru'
_chemical_oxdiff_usercomment
'crystallised from DCM, 2 drops of Hexane, MeOH'
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.319
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C27 \\sim C31 \\sim C30 \\sim C29 \\sim C28: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
3.a Ternary CH refined with riding coordinates:
 C13(H13), C27(H27), C38(H38)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C18(H18),
 C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C33(H33), C34(H34), C36(H36),
  C37(H37)
3.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              46032
_shelx_hkl_checksum              30136
_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 1.279
_oxdiff_exptl_absorpt_empirical_full_min 0.741