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_7716368
_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
'C55 H47 Fe O6 P2 Pd, 2.89(C H Cl3), F6 P, 0.7[CHCl3]'
_chemical_formula_sum            'C58.59 H50.59 Cl10.77 F6 Fe O6 P3 Pd'
_chemical_formula_weight         1601.61
_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
_audit_creation_date             2024-05-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-20 deposited with the CCDC.	2024-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.1174(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9737(3)
_cell_length_b                   15.9310(3)
_cell_length_c                   23.2031(5)
_cell_measurement_reflns_used    34045
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      31.7050
_cell_measurement_theta_min      1.9730
_cell_volume                     6617.5(2)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -78.00   6.00   0.50    5.00    --   -5.36 -37.00 152.00  168
  2  \w    -20.00  24.00   0.50    5.00    --   -5.36 -99.00-180.00   88
  3  \w      4.00  67.00   0.50    5.00    --   -5.36  37.00 -51.00  126
  4  \w    -23.00  27.00   0.50    5.00    --   -5.36 -99.00-150.00  100
  5  \w    -20.00  37.00   0.50    5.00    --    5.98 -99.00 150.00  114
  6  \w    -31.00 -27.00   0.50    5.00    --    5.98 -38.00 -90.00    8
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57856
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.177
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60614
_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    1.608
_exptl_crystal_description       block
_exptl_crystal_F_000             3217
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.175
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         12520
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0247P)^2^+24.3357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9882
_reflns_number_total             12520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01045k2.cif
_cod_data_source_block           A5
_cod_depositor_comments
'Adding full bibliography for 7716368--7716371.cif.'
_cod_database_code               7716368
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.728
_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. Restrained distances
 C4S-Cl11 = C4S-Cl10 = C4S-Cl12
 1.78 with sigma of 0.02
 C3S-Cl9S = C3S-Cl8S = C3S-Cl7S
 1.78 with sigma of 0.02
 Cl11-Cl10 \\sim Cl10-Cl12 \\sim Cl12-Cl11
 with sigma of 0.04
 C4S-Cl11 \\sim C4S-Cl10 \\sim C4S-Cl12
 with sigma of 0.02
 C3S-Cl9S \\sim C3S-Cl8S \\sim C3S-Cl7S
 with sigma of 0.02
 Cl9S-Cl8S \\sim Cl8S-Cl7S \\sim Cl7S-Cl9S
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl10 \\sim Cl11 \\sim Cl12 \\sim C4S: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Cl7S \\sim Cl8S \\sim Cl9S \\sim C3S: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 Cl10, Cl11, Cl12, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl7S, Cl8S, Cl9S, C3S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl7S(0.31) Cl8S(0.31) Cl9S(0.31) Cl10(0.58) Cl11(0.58) Cl12(0.58)
 C3S(0.31) H3S(0.31) C4S(0.58) H4S(0.58)
6.a Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4A), C5(H5), C7(H7), 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), 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)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C21(H21A,H21B,H21C)
6.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6(H6)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 168 electrons were 
found in a volume of 504\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.7[CHCl3] per Asymmetric Unit 
which account for 162 electrons 
per unit cell.
;
_shelx_res_checksum              81414
_shelx_hkl_checksum              23258
_shelx_fab_checksum              79008
_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
;