Structurally different mono, bi and trinuclear Pd(II) complexes and their DNA/Protein interaction, DNA cleavage, anti-oxidant, anti-microbial and cytotoxicity studies
Arumugam, Shanmugapriya; Jain, Ruchi; Devaraj, Sabarinathan; Giriraj, Kalaiarasi; Dallemer, Frederic; Prabhakaran, Rathinasabapathi; New J. Chem. 41 (2017) 10324–10338; doi:10.1039/C7NJ01556A

data_7056491
_publ_section_title
;
 Structurally different mono, bi and trinuclear Pd(II) complexes and their
 DNA/Protein interaction, DNA cleavage, anti-oxidant, anti-microbial and
 cytotoxicity studies
;
_journal_issue                   18
_journal_name_full               'New J. Chem.'
_journal_page_first              10324
_journal_page_last               10338
_journal_paper_doi               10.1039/C7NJ01556A
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C33 H39 N9 O6 Pd3 S3, C4 H8 O2'
_chemical_formula_sum            'C37 H47 N9 O8 Pd3 S3'
_chemical_formula_weight         1161.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date
;
'Fri Feb 06 02:47:03 2015'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_audit_update_record
;
2017-03-17 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                116.500(2)
_cell_angle_beta                 92.908(2)
_cell_angle_gamma                114.528(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2741(3)
_cell_length_b                   14.1583(3)
_cell_length_c                   15.4049(4)
_cell_measurement_reflns_used    16847
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7150
_cell_measurement_theta_min      3.6730
_cell_volume                     2256.01(12)
_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, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_details
;
  1 omega  -20.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7039  -99.0000    0.0000 73

  2 omega  -20.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7039  -99.0000   90.0000 73

  3 omega  -20.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7039  -99.0000 -180.0000 73

  4 omega  -36.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9382   38.0000  120.0000 98

  5 omega  -20.00   29.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9382  -99.0000 -150.0000 49

  6 omega -100.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9382    0.0000 -120.0000 176

  7 omega  -13.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7039   38.0000 -180.0000 99

  8 omega  -16.00   85.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7039   57.0000  -90.0000 101

  9 omega  -20.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7039  -99.0000 -120.0000 59

 10 omega  -20.00   29.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9382  -99.0000  150.0000 49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0135493000
_diffrn_orient_matrix_UB_12      0.0474939000
_diffrn_orient_matrix_UB_13      0.0223244000
_diffrn_orient_matrix_UB_21      -0.0207527000
_diffrn_orient_matrix_UB_22      -0.0108858000
_diffrn_orient_matrix_UB_23      -0.0487020000
_diffrn_orient_matrix_UB_31      -0.0561415000
_diffrn_orient_matrix_UB_32      -0.0418155000
_diffrn_orient_matrix_UB_33      -0.0044150000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50595
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.718
_diffrn_reflns_theta_min         3.364
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83394
_exptl_absorpt_correction_type   multi-scan
_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)
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    1.709
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.252
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         11417
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0405P)^2^+1.9382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8548
_reflns_number_total             11417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01556a2.cif
_cod_data_source_block           apl20de
_cod_original_cell_volume        2256.02(10)
_cod_database_code               7056491
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.75
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C22B = O4-C22C
 1.39 with sigma of 0.0005
3. Uiso/Uaniso restraints and constraints
Uanis(C22A) = Uanis(C22B) = Uanis(C22C)
4. Others
 Fixed Sof: C22A(0.33333) H22A(0.33333) H22B(0.33333) H22C(0.33333)
 C22B(0.33333) H22D(0.33333) H22E(0.33333) H22F(0.33333) C22C(0.33333)
 H22G(0.33333) H22H(0.33333) H22I(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C20(H20A,H20B), C31(H31A,H31B), C36(H36A,H36B)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N9(H9), C1(H1), C3(H3A), C4(H4), C5(H5), C12(H12), C14(H14),
 C15(H15), C16(H16), C23(H23), C25(H25), C26(H26), C27(H27)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C),
 C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F), C22C(H22G,H22H,H22I)
;
_olex2_submission_special_instructions 'No special instructions were received'