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_7718991
_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         'C31 H36 O6'
_chemical_formula_sum            'C31 H36 O6'
_chemical_formula_weight         504.60
_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
_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                 101.2029(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.62759(17)
_cell_length_b                   5.94440(6)
_cell_length_c                   25.1312(2)
_cell_measurement_reflns_used    17384
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.7910
_cell_measurement_theta_min      2.4400
_cell_volume                     2729.75(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.967
_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     76.00 104.00   0.50    0.05    --   76.80 160.00-170.00   56
  2  \w     60.00  85.00   0.50    0.05    --   69.57 160.00-170.00   50
  3  \w     52.00  77.00   0.50    0.05    --   69.57-160.00 158.00   50
  4  \w     74.00  99.00   0.50    0.05    --   64.18-160.00 158.00   50
  5  \w     81.00 106.00   0.50    0.05    --   76.80-160.00 158.00   50
  6  \w     40.00  68.00   0.50    0.05    --   76.80-125.00  90.00   56
  7  \w     74.00 104.00   0.50    0.05    --   76.80-125.00  90.00   60
  8  \w     79.00 104.00   0.50    0.05    --   76.80-125.00  60.00   50
  9  \w     48.00  73.00   0.50    0.05    --   76.80-125.00  60.00   50
 10  \w     47.00  72.00   0.50    0.05    --   76.80-125.00   0.00   50
 11  \w     75.00 104.00   0.50    0.05    --   76.80-125.00   0.00   58
 12  \w     48.00  76.00   0.50    0.05    --   76.80-118.00 -48.00   56
 13  \w     31.00  91.00   0.50    0.05    --   69.57-118.00 -48.00  120
 14  \w     39.00  83.00   0.50    0.05    --   76.80 -95.00-150.00   88
 15  \w     46.00  75.00   0.50    0.05    --   64.18-118.00 -48.00   58
 16  \w     34.00  77.00   0.50    0.05    --   69.57 -95.00-120.00   86
 17  \w     26.00  64.00   0.50    0.05    --   64.18 -95.00-150.00   76
 18  \w     58.00  83.00   0.50    0.05    --   76.80 -95.00   0.00   50
 19  \w     39.00  64.00   0.50    0.05    --   76.80 -95.00 120.00   50
 20  \w     27.00  71.00   0.50    0.05    --   64.18 -95.00 150.00   88
 21  \w     46.00  85.00   0.50    0.05    --   76.80 -95.00 150.00   78
 22  \w     33.00  58.00   0.50    0.05    --   69.57   0.00-150.00   50
 23  \w     48.00  79.00   0.50    0.05    --   76.80  15.00 -90.00   62
 24  \w     58.00  94.00   0.50    0.05    --   76.80  15.00 -60.00   72
 25  \w     95.00 120.00   0.50    0.05    --   76.80  15.00 -90.00   50
 26  \w     82.00 107.00   0.50    0.05    --   69.57   0.00-150.00   50
 27  \w    -78.00 -52.00   0.50    0.05    --  -64.90 160.00-170.00   52
 28  \w   -112.00 -86.00   0.50    0.05    --  -74.82 140.00-106.34   52
 29  \w    -95.00 -36.00   0.50    0.05    --  -69.34 125.00 -30.00  118
 30  \w    -91.00 -28.00   0.50    0.05    --  -69.34 118.00  37.00  126
 31  \w    -71.00 -34.00   0.50    0.05    --  -69.34   0.00 -60.00   74
 32  \w    -72.00 -36.00   0.50    0.05    --  -69.34   0.00  30.00   72
 33  \w    -66.00 -27.00   0.50    0.05    --  -64.90   0.00  60.00   78
 34  \w    -72.00 -46.00   0.50    0.05    --  -69.34   0.00  90.00   52
 35  \w    -66.00 -27.00   0.50    0.05    --  -64.90   0.00 120.00   78
 36  \w    -85.00 -50.00   0.50    0.05    --  -64.90-160.00 158.00   70
 37  \w   -101.00 -76.00   0.50    0.05    --  -69.34-160.00 158.00   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      -0.0109903000
_diffrn_orient_matrix_UB_12      -0.2553874000
_diffrn_orient_matrix_UB_13      0.0052658000
_diffrn_orient_matrix_UB_21      0.0069669000
_diffrn_orient_matrix_UB_22      0.0262486000
_diffrn_orient_matrix_UB_23      0.0618079000
_diffrn_orient_matrix_UB_31      -0.0832300000
_diffrn_orient_matrix_UB_32      0.0359851000
_diffrn_orient_matrix_UB_33      -0.0078051000
_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  0.0174
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27385
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.064
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.524
_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 yellow'
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.00120(15)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5380
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0490P)^2^+0.8077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4800
_reflns_number_total             5380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01240f3.cif
_cod_data_source_block           hl4b
_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        2729.75(5)
_cod_database_code               7718991
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C31 H36 O6'
_chemical_oxdiff_usercomment     'crystallised from DCM, EtOH'
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.833
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-C12A \\sim O3-C12B
 with sigma of 0.02
 C13-C12A \\sim C12B-C13
 with sigma of 0.02
 O4A-C12A \\sim O4B-C12B
 with sigma of 0.02
 O6A-C26 \\sim O6B-C26
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4A \\sim O4B \\sim C12A \\sim C12B: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
O6A \\sim O6B \\sim C26: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
4. Others
 Sof(H2)=1-FVAR(1)
 Sof(H1)=FVAR(1)
 Sof(O4B)=Sof(C12B)=Sof(H13C)=Sof(H13D)=1-FVAR(2)
 Sof(O4A)=Sof(C12A)=Sof(H13A)=Sof(H13B)=FVAR(2)
 Sof(O6B)=1-FVAR(3)
 Sof(O6A)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C13(H13C,H13D), C27(H27A,H27B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C18(H18),
 C19(H19), C21(H21), C22(H22), C24(H24), C25(H25)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_shelx_res_checksum              25000
_shelx_hkl_checksum              17257
_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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.922