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_7716370
_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         'C49 H47 O6 P2 Pd, F6 P, 2.4[H2O], 0.7[H2O]'
_chemical_formula_sum            'C49 H53.2 F6 O9.1 P3 Pd'
_chemical_formula_weight         1101.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                112.064(7)
_cell_angle_beta                 96.129(6)
_cell_angle_gamma                101.480(6)
_cell_formula_units_Z            2
_cell_length_a                   9.0366(6)
_cell_length_b                   16.4302(12)
_cell_length_c                   19.0475(13)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.6060
_cell_measurement_theta_min      2.7880
_cell_volume                     2516.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -69.00 118.00   1.00   90.00    --   27.63  54.00 -90.00  187
  2  \w    -69.00 118.00   1.00   90.00    --   27.63  54.00  30.00  187
  3  \w    -69.00 118.00   1.00   90.00    --   27.63  54.00 150.00  187
  4  \w    -69.00 118.00   1.00   90.00    --   27.63  54.00  90.00  187
  5  \w    -69.00 118.00   1.00   90.00    --   27.63  54.00-150.00  187
  6  \w    -69.00 -11.00   1.00   90.00    --   27.63  54.00-180.00   58
  7  \w    -69.00  92.00   1.00   90.00    --   27.63  54.00   0.00  161
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0593713000
_diffrn_orient_matrix_UB_12      -0.0227205000
_diffrn_orient_matrix_UB_13      -0.0335181000
_diffrn_orient_matrix_UB_21      0.0305961000
_diffrn_orient_matrix_UB_22      -0.0384989000
_diffrn_orient_matrix_UB_23      -0.0109593000
_diffrn_orient_matrix_UB_31      -0.0470925000
_diffrn_orient_matrix_UB_32      -0.0180845000
_diffrn_orient_matrix_UB_33      0.0209155000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47070
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.515
_diffrn_reflns_theta_min         2.530
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.100a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.453
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1130
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.011
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0799
_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^)+(0.1629P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2239
_refine_ls_wR_factor_ref         0.2576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6349
_reflns_number_total             9360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01045k2.cif
_cod_data_source_block           A4
_cod_depositor_comments
'Adding full bibliography for 7716368--7716371.cif.'
_cod_original_formula_sum        'C49 H53.20 F6 O9.10 P3 Pd'
_cod_database_code               7716370
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu1 O4 P3 C44 H55'
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.901
_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. Restrained distances
 P3-F3 = P3-F4 = P3-F1 = P3-F2 = P3-F6 = P3-F5
 1.65 with sigma of 0.02
 F3-F1 \\sim F4-F2 \\sim F5-F6
 with sigma of 0.05
 P3-F3 \\sim P3-F4 \\sim P3-F1 \\sim P3-F2 \\sim P3-F6 \\sim P3-F5
 with sigma of 0.02
 F3-F4 \\sim F3-F2 \\sim F3-F6 \\sim F3-F5 \\sim F1-F4 \\sim F1-F2 \\sim F1-F6
\\sim F1-F5
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
P3 \\sim F3 \\sim F4 \\sim F1 \\sim F2 \\sim F6 \\sim F5: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 P3, F3, F4, F1, F2, F6, F5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C012(H01A,H01B), C013(H01C,H01D), C015(H01E,H01F), C01C(H01G,H01H)
5.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C3B(H3BA), C4B(H4B), C3A(H3AA), C10B(H10B), C6A(H6A), C4A(H4A),
 C6B(H6B), C211(H211), C9B(H9B), C125(H125), C10A(H10A), C111(H111), C221(H221),
  C115(H115), C212(H212), C225(H225), C224(H224), C121(H121), C9A(H9A),
 C113(H113), C114(H114), C215(H215), C112(H112), C223(H223), C222(H222),
 C214(H214), C213(H213), C124(H124), C122(H122), C123(H123)
5.c Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F)
5.d Idealised tetrahedral OH refined as rotating group:
 O3B(H3B), O3A(H3A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53359
_shelx_hkl_checksum              5922
_shelx_fab_checksum              42816
_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 1.523
_oxdiff_exptl_absorpt_empirical_full_min 0.723