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_7047127
_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         'C40 H32 N2 O6 P2 Pt S2'
_chemical_formula_sum            'C40 H32 N2 O6 P2 Pt S2'
_chemical_formula_weight         957.82
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-10
_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            4
_cell_length_a                   15.7420(8)
_cell_length_b                   15.7420(8)
_cell_length_c                   19.1532(9)
_cell_measurement_reflns_used    1477
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.4580
_cell_measurement_theta_min      3.3330
_cell_volume                     4746.4(4)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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     -4.00  87.00   1.00   29.48    --   17.28  37.00 -60.00   91
;
_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      0.0002743000
_diffrn_orient_matrix_UB_12      -0.0446902000
_diffrn_orient_matrix_UB_13      -0.0039153000
_diffrn_orient_matrix_UB_21      0.0449801000
_diffrn_orient_matrix_UB_22      0.0004643000
_diffrn_orient_matrix_UB_23      -0.0027986000
_diffrn_orient_matrix_UB_31      0.0033856000
_diffrn_orient_matrix_UB_32      -0.0047880000
_diffrn_orient_matrix_UB_33      0.0367686000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7421
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.017
_diffrn_reflns_theta_max         25.017
_diffrn_reflns_theta_min         3.083
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.152
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.686
_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    1.340
_exptl_crystal_description       prism
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 790 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         4085
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+0.9343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.950
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                2404
_reflns_number_total             4085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02389a2.cif
_cod_data_source_block           Compound_VI
_cod_original_cell_volume        4746.4(5)
_cod_database_code               7047127
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H28 N2 O6 P2 Pt S2'
_reflns_odcompleteness_completeness 98.62
_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
2. Restrained distances
 C15-C16
 1.39 with sigma of 0.01
 C16-C17
 1.39 with sigma of 0.01
 C18-C17
 1.39 with sigma of 0.01
 C18-C19
 1.39 with sigma of 0.01
 C8-C13 \\sim C13-C12 \\sim C12-C11 \\sim C11-C10 \\sim C9-C10 \\sim C9-C8
 with sigma of 0.02
 C16-C15 \\sim C17-C16 \\sim C18-C17 \\sim C19-C18 \\sim C20-C19 \\sim C20-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C13)
Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) =
Uanis(C20)
Uanis(C2) = Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(C3)
4. Rigid body (RIGU) restrains
 C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, N1
 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:
 C13(H13), C10(H10), C9(H9), C3(H3), C5(H5), C4(H4), C11(H11), C6(H6),
 C19(H19), C18(H18), C16(H16), C17(H17), C7(H7), C12(H12)
;
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.915