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_7047123
_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         'C50 H44 P4 Pd, 2(C7 H4 N O3 S)'
_chemical_formula_sum            'C64 H52 N2 O6 P4 Pd S2'
_chemical_formula_weight         1239.47
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-06 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                76.066(5)
_cell_angle_beta                 66.277(4)
_cell_angle_gamma                85.214(4)
_cell_formula_units_Z            1
_cell_length_a                   11.1137(4)
_cell_length_b                   11.1173(8)
_cell_length_c                   13.1286(6)
_cell_measurement_reflns_used    4728
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9970
_cell_measurement_theta_min      3.2360
_cell_volume                     1441.17(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -48.00   26.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -       17.2817  -57.0000  -90.0000 74

  2 omega  -24.00   19.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -      -19.3130  -99.0000 -150.0000 43

  3 omega  -42.00  -13.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -       17.2817  -57.0000 -120.0000 29

  4 omega  -12.00   16.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -      -19.3130  -99.0000   60.0000 28

  5 omega  -89.00   11.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -      -19.3130  -77.0000   30.0000 100

  6 omega  -40.00   46.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -      -19.3130   77.0000  150.0000 86

  7 omega    4.00   29.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -      -19.3130   96.0000  -21.0000 25

  8 omega   49.00   84.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -       17.2817  178.0000  -90.0000 35

  9 omega  -60.00  -16.00   1.0000   25.4850
omega____ theta____ kappa____ phi______ frames
    -      -19.3130   96.0000  -21.0000 44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0113006000
_diffrn_orient_matrix_UB_12      -0.0590590000
_diffrn_orient_matrix_UB_13      -0.0135609000
_diffrn_orient_matrix_UB_21      -0.0007404000
_diffrn_orient_matrix_UB_22      -0.0269383000
_diffrn_orient_matrix_UB_23      0.0550278000
_diffrn_orient_matrix_UB_31      -0.0687952000
_diffrn_orient_matrix_UB_32      -0.0104198000
_diffrn_orient_matrix_UB_33      0.0214506000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12075
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.129
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.5199
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1742
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5872
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0610P)^2^+0.9796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4649
_reflns_number_total             5872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02389a2.cif
_cod_data_source_block           Compound_III
_cod_database_code               7047123
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C64 H54 N2 O6 P4 Pd S2 '
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.760
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C26-C27
 1.34 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O1, C26
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N1, C26
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C26, C27
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
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)
;
_olex2_submission_special_instructions 'No special instructions were received'