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_7716371
_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         'C47 H43 O6 P2 Pd, F6 P, 0.6[CHCl3]'
_chemical_formula_sum            'C47 H43 F6 O6 P3 Pd'
_chemical_formula_weight         1017.12
_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
_audit_creation_date             2023-04-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.924(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0940(2)
_cell_length_b                   22.4280(3)
_cell_length_c                   16.0300(3)
_cell_measurement_reflns_used    51698
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.6260
_cell_measurement_theta_min      2.2740
_cell_volume                     4666.90(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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    -79.00   5.00   0.50   15.00    --   -5.51 -19.00-180.00  168
  2  \w    -23.00  27.00   0.50   15.00    --   -5.51 -99.00  60.00  100
  3  \w    -23.00  27.00   0.50   15.00    --   -5.51 -99.00 -90.00  100
  4  \w    -19.00  67.00   0.50   15.00    --   -5.51  57.00  30.00  172
  5  \w    -23.00  27.00   0.50   15.00    --   -5.51 -99.00-120.00  100
  6  \w    -16.00  67.00   0.50   15.00    --   -5.51  38.00 150.00  166
  7  \w    -16.00  67.00   0.50   15.00    --   -5.51  38.00-180.00  166
  8  \w    -27.00  67.00   0.50   15.00    --   -5.51  77.00 -30.00  188
  9  \w    -16.00  69.00   0.50   15.00    --   -5.51  19.00 -90.00  170
;
_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      0.0379325000
_diffrn_orient_matrix_UB_12      -0.0214402000
_diffrn_orient_matrix_UB_13      0.0237017000
_diffrn_orient_matrix_UB_21      -0.0349227000
_diffrn_orient_matrix_UB_22      -0.0232450000
_diffrn_orient_matrix_UB_23      -0.0219415000
_diffrn_orient_matrix_UB_31      0.0180828000
_diffrn_orient_matrix_UB_32      0.0000577000
_diffrn_orient_matrix_UB_33      -0.0355688000
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0211
_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       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            94656
_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         25.750
_diffrn_reflns_theta_min         1.871
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+4.8220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7970
_reflns_number_total             8938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01045k2.cif
_cod_data_source_block           A2
_cod_depositor_comments
'Adding full bibliography for 7716368--7716371.cif.'
_cod_database_code               7716371
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pd1 P3 O4 C33 H44 F6'
_chemical_oxdiff_usercomment     'Alzir - Jocely - curcumina'
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.906
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C100(H10A,H10B), C200(H20A,H20B)
2.b 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),
 C212(H212), C213(H213), C214(H214), C215(H215), C216(H216), C222(H222),
 C223(H223), C224(H224), C225(H225), C226(H226)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C21(H21A,H21B,H21C)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26432
_shelx_hkl_checksum              61056
_shelx_fab_checksum              52564
_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 1.522
_oxdiff_exptl_absorpt_empirical_full_min 0.550