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_7047124
_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         'C52 H48 P4 Pd, 2(C7 H4 N O3 S)'
_chemical_formula_sum            'C66 H56 N2 O6 P4 Pd S2'
_chemical_formula_weight         1267.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-22
_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                90
_cell_angle_beta                 102.841(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0527(17)
_cell_length_b                   15.931(2)
_cell_length_c                   17.923(2)
_cell_measurement_reflns_used    1717
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.7640
_cell_measurement_theta_min      3.6450
_cell_volume                     3355.4(8)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -92.00   5.00   1.00   12.95    --  -24.36 -57.00  30.00   97
  2  \w    -25.00  25.00   1.00   12.95    --  -24.36 -99.00 -60.00   50
  3  \w   -111.00 -55.00   1.00   12.95    --  -24.36-178.00  90.00   56
;
_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      -0.0563312000
_diffrn_orient_matrix_UB_12      -0.0143545000
_diffrn_orient_matrix_UB_13      -0.0021448000
_diffrn_orient_matrix_UB_21      -0.0103670000
_diffrn_orient_matrix_UB_22      0.0351480000
_diffrn_orient_matrix_UB_23      0.0218117000
_diffrn_orient_matrix_UB_31      -0.0190107000
_diffrn_orient_matrix_UB_32      0.0232957000
_diffrn_orient_matrix_UB_33      -0.0341494000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9542
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.909
_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    1.255
_exptl_crystal_description       prism
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5885
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0686P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3584
_reflns_number_total             5885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02389a2.cif
_cod_data_source_block           Compound_VII
_cod_original_cell_volume        3355.3(8)
_cod_database_code               7047124
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C66 H56 N2 O6 P4 Pd S2'
_reflns_odcompleteness_completeness 99.08
_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
 C28-C29
 1.395 with sigma of 0.005
 C31-C30
 1.395 with sigma of 0.005
 C31-C32
 1.395 with sigma of 0.005
 C32-C33
 1.395 with sigma of 0.005
 C33-C28
 1.395 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C33) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) = Uanis(C1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32)
;
_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 1.111
_oxdiff_exptl_absorpt_empirical_full_min 0.943