Palladium(II) and platinum(II) saccharinate complexes with bis(diphenylphosphino)methane/ethane: synthesis, S-phase arrest and ROS-mediated apoptosis in human colon cancer cells
Icsel, Ceyda; Yilmaz, Veysel T.; Aygün, Muhittin; Cevatemre, Buse; Alper, Pinar; Ulukaya, Engin; Dalton Transactions  (2018) –; doi:10.1039/C8DT02389A

data_7047129
_publ_section_title
;
 Palladium(II) and platinum(II) saccharinate complexes with
 bis(diphenylphosphino)methane/ethane: synthesis, S-phase arrest and
 ROS-mediated apoptosis in human colon cancer cells
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT02389A
_journal_year                    2018
_chemical_formula_moiety         'C39 H30 N2 O6 P2 Pt S2, C2 H6 O S'
_chemical_formula_sum            'C41 H36 N2 O7 P2 Pt S3'
_chemical_formula_weight         1021.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-06-06 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   37.9658(17)
_cell_length_b                   37.9658(17)
_cell_length_c                   12.1250(9)
_cell_measurement_reflns_used    917
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.7190
_cell_measurement_theta_min      3.4420
_cell_volume                     17477.0(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -52.00  52.00   1.00  149.54    --   19.91 -77.00-150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0135123000
_diffrn_orient_matrix_UB_12      0.0128891000
_diffrn_orient_matrix_UB_13      -0.0024738000
_diffrn_orient_matrix_UB_21      0.0126350000
_diffrn_orient_matrix_UB_22      0.0134091000
_diffrn_orient_matrix_UB_23      0.0095584000
_diffrn_orient_matrix_UB_31      0.0026735000
_diffrn_orient_matrix_UB_32      0.0016981000
_diffrn_orient_matrix_UB_33      -0.0576504000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1172
_diffrn_reflns_av_unetI/netI     0.2482
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14104
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.012
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         3.166
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.477
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       prism
_exptl_crystal_F_000             8128
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.778
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7687
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.2173
_refine_ls_R_factor_gt           0.0859
_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^)+(0.0736P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.2193
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3088
_reflns_number_total             7687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02389a2.cif
_cod_data_source_block           Compound_II
_cod_original_cell_volume        17477(2)
_cod_database_code               7047129
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C39 H30 N2 O6 P2 Pt S2 '
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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
2. Restrained distances
 C16-C17
 1.39 with sigma of 0.01
 C14-C19
 1.39 with sigma of 0.01
 C15-C14
 1.39 with sigma of 0.01
 C9-C10
 1.39 with sigma of 0.02
 C23-C24
 1.39 with sigma of 0.02
 C23-C22
 1.39 with sigma of 0.02
 C7-C2
 1.39 with sigma of 0.02
 C4-C5
 1.39 with sigma of 0.02
 C5-C6
 1.39 with sigma of 0.02
 C11-C12
 1.39 with sigma of 0.02
 C10-C11
 1.39 with sigma of 0.02
 C34-C39
 1.39 with sigma of 0.02
 C36-C37
 1.39 with sigma of 0.02
 C35-C34
 1.39 with sigma of 0.02
 O4-C26 \\sim O1-C33
 with sigma of 0.02
 C8-C13 \\sim C13-C12 \\sim C12-C11 \\sim C11-C10 \\sim C9-C10 \\sim C9-C8
 with sigma of 0.02
 C2-C3 \\sim C4-C5 \\sim C6-C7
 with sigma of 0.02
 C20-C21 \\sim C22-C23 \\sim C24-C25
 with sigma of 0.02
 C34-C35 \\sim C36-C37 \\sim C38-C39
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C10) = Uanis(C9)
Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) =
Uanis(C39)
Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19)
Uanis(C2) = Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3)
Uanis(O1) = Uanis(O2) = Uanis(O3)
Uanis(C20) = Uanis(C25) = Uanis(C24) = Uanis(C23) = Uanis(C22) = Uanis(C21)
Uanis(N1) = Uanis(N2)
4. Rigid body (RIGU) restrains
 N1, S1, C39, O3, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 S1, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 S1, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 S1, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 S2, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 P2, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 P1, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 O1, C33
 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:
 C1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31),
 C35(H35), C36(H36), C37(H37), C38(H38)
5.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_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 1.042
_oxdiff_exptl_absorpt_empirical_full_min 0.941