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_7047130
_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 Pd S2, H2 O'
_chemical_formula_sum            'C39 H32 N2 O7 P2 Pd S2'
_chemical_formula_weight         873.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-09
_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                 117.04(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.662(5)
_cell_length_b                   17.152(2)
_cell_length_c                   23.382(4)
_cell_measurement_reflns_used    2354
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.0460
_cell_measurement_theta_min      3.4100
_cell_volume                     7738(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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     -8.00  91.00   1.00   57.79    --   19.91  68.00  67.00   99
  2  \w    -35.00  64.00   1.00   57.79    --   19.91 -19.00 120.00   99
;
_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      0.0148373000
_diffrn_orient_matrix_UB_12      0.0263502000
_diffrn_orient_matrix_UB_13      0.0263874000
_diffrn_orient_matrix_UB_21      0.0326459000
_diffrn_orient_matrix_UB_22      -0.0041757000
_diffrn_orient_matrix_UB_23      0.0001415000
_diffrn_orient_matrix_UB_31      -0.0079474000
_diffrn_orient_matrix_UB_32      0.0319927000
_diffrn_orient_matrix_UB_33      -0.0217005000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.1798
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23748
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.869
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.840
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       prism
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.069
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         13573
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1764
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0427P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6708
_reflns_number_total             13573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02389a2.cif
_cod_data_source_block           Compound_I
_cod_database_code               7047130
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C39 H32 N2 O7 P2 Pd S2'
_reflns_odcompleteness_completeness 99.10
_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 O(H,H) groups
2. Restrained distances
 C2-C3
 1.39 with sigma of 0.01
 C4-C5
 1.39 with sigma of 0.01
 C5-C6
 1.39 with sigma of 0.01
 C17-C18
 1.39 with sigma of 0.01
 C18-C19
 1.39 with sigma of 0.01
 C19-C14
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O2W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) = Uanis(C7)
Uanis(C8) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C10) = Uanis(C9)
Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19)
Uanis(C53) = Uanis(C58) = Uanis(C57) = Uanis(C56) = Uanis(C55) = Uanis(C54)
4. Rigid body (RIGU) restrains
 C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C68, C69
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C75, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C40(H40A,H40B)
5.c 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), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54),
 C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63),
  C64(H64), C67(H67), C68(H68), C69(H69), C70(H70), C74(H74), C75(H75),
 C76(H76), C77(H77)
;
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.070
_oxdiff_exptl_absorpt_empirical_full_min 0.892