Pd(II)/diphosphine/curcumin complexes as potential anticancer agents.
Dutra, Jocely L.; Honorato, João; Graminha, Angélica; Moraes, Carlos André F; de Oliveira, Kleber T.; Cominetti, Marcia R.; Castellano, Eduardo E.; Batista, Alzir A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18902–18916; doi:10.1039/d4dt01045k

data_7716369
_publ_section_title
;
 Pd(II)/diphosphine/curcumin complexes as potential anticancer agents.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18902
_journal_page_last               18916
_journal_paper_doi               10.1039/d4dt01045k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C57 H49 O6 P2 Pd, F6 P'
_chemical_formula_sum            'C57 H49 F6 O6 P3 Pd'
_chemical_formula_weight         1143.27
_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
_audit_creation_date             2024-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.609(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0442(3)
_cell_length_b                   9.5822(2)
_cell_length_c                   37.0985(7)
_cell_measurement_reflns_used    32961
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      31.8200
_cell_measurement_theta_min      2.1940
_cell_volume                     4976.36(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -66.00  24.00   0.50   65.00    --    5.98 -68.00 -29.00  180
  2  \w    -12.00  78.00   0.50   65.00    --    5.98  68.00 103.00  180
  3  \w    -23.00  27.00   0.50   65.00    --   -5.51 -99.00   0.00  100
  4  \w    -23.00  17.00   0.50   65.00    --   -5.51 -99.00  30.00   80
  5  \w    -17.00  18.00   0.50   65.00    --   -5.51 -99.00-180.00   70
  6  \w    -19.00  49.00   0.50   65.00    --   -5.51  57.00 150.00  136
  7  \w    -18.00   7.00   0.50   65.00    --   -5.51 -99.00 -60.00   50
  8  \w     -5.00  78.00   0.50   65.00    --    5.98  38.00  90.00  166
  9  \w      0.00  37.00   0.50   65.00    --    5.98 -99.00 -60.00   74
 10  \w    -51.00 -38.50   0.50   65.00    --    5.98 -19.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0370785000
_diffrn_orient_matrix_UB_12      0.0289751000
_diffrn_orient_matrix_UB_13      -0.0117964000
_diffrn_orient_matrix_UB_21      -0.0062028000
_diffrn_orient_matrix_UB_22      -0.0651685000
_diffrn_orient_matrix_UB_23      -0.0089424000
_diffrn_orient_matrix_UB_31      -0.0339841000
_diffrn_orient_matrix_UB_32      -0.0197740000
_diffrn_orient_matrix_UB_33      0.0121989000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            76902
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.748
_diffrn_reflns_theta_min         1.753
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       plate
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         9514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0246P)^2^+7.2605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8619
_reflns_number_total             9514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01045k2.cif
_cod_data_source_block           A1
_cod_depositor_comments
'Adding full bibliography for 7716368--7716371.cif.'
_cod_database_code               7716369
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43 H34 O5 P3 Pd1 F6'
_chemical_oxdiff_usercomment     'JD25 Jocely'
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5A), C7(H7A), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C19(H19), C20(H20), C112(H112), C113(H113), C114(H114), C115(H115),
 C116(H116), C122(H122), C123(H123), C124(H124), C125(H125), C126(H126),
 C132(H132), C133(H133), C134(H134), C135(H135), C136(H136), C212(H212),
 C213(H213), C214(H214), C215(H215), C216(H216), C222(H222), C223(H223),
 C224(H224), C225(H225), C226(H226), C232(H232), C233(H233), C234(H234),
 C235(H235), C236(H236)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C21(H21A,H21B,H21C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O7(H7)
;
_shelx_res_checksum              21551
_shelx_hkl_checksum              81570
_olex2_date_sample_data_collection 2022-06-07
_olex2_date_sample_submission    2022-06-01
_olex2_submission_original_sample_id jh1
_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 1.573
_oxdiff_exptl_absorpt_empirical_full_min 0.641