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_7056492
_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         'C22 H21 N3 O2 P Pd S, 0.5(C6)'
_chemical_formula_sum            'C25 H21 N3 O2 P Pd S'
_chemical_formula_weight         564.88
_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
_atom_sites_solution_primary     iterative
_audit_creation_date
;
'Thu Feb 05 17:20:11 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                93.946(2)
_cell_angle_beta                 98.609(2)
_cell_angle_gamma                107.392(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5318(3)
_cell_length_b                   11.2368(4)
_cell_length_c                   11.4307(3)
_cell_measurement_reflns_used    9359
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7240
_cell_measurement_theta_min      3.8330
_cell_volume                     1267.08(7)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
;
  1 omega  -22.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4725   77.0000   90.0000 127

  2 omega  -22.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4725   77.0000  -30.0000 127

  3 omega  -22.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4725   77.0000 -150.0000 127

  4 omega   35.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4725  178.0000  -30.0000 77

  5 omega  -20.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4725  -99.0000    0.0000 82

  6 omega   35.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4725  178.0000 -120.0000 77

  7 omega -112.00  -57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7069 -178.0000 -180.0000 55

  8 omega -112.00  -57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7069 -178.0000   90.0000 55

  9 omega -112.00  -57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7069 -178.0000  -60.0000 55

 10 omega  -71.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4725  -19.0000 -150.0000 146

 11 omega  -20.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       16.4725  -99.0000   90.0000 82
;
_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      0.0350451000
_diffrn_orient_matrix_UB_12      -0.0366682000
_diffrn_orient_matrix_UB_13      0.0309585000
_diffrn_orient_matrix_UB_21      0.0618024000
_diffrn_orient_matrix_UB_22      0.0386344000
_diffrn_orient_matrix_UB_23      -0.0129982000
_diffrn_orient_matrix_UB_31      0.0098835000
_diffrn_orient_matrix_UB_32      0.0400324000
_diffrn_orient_matrix_UB_33      0.0535657000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28373
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.269
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90053
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         6263
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0477P)^2^+0.7671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5128
_reflns_number_total             6263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01556a2.cif
_cod_data_source_block           apl14de
_cod_database_code               7056492
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.79
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C9B
 1.4 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C9B) = Uanis(C9A)
4. Others
 Fixed Sof: C9A(0.75) H9AA(0.75) H9AB(0.75) H9AC(0.75) C1C(0.5) C1D(0.5)
 C0AA(0.5) C1AA(0.5) C1(0.5) C2(0.5) C9B(0.25) H9BA(0.25) H9BB(0.25) H9BC(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21)
5.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
5.d Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC)
;
_olex2_submission_special_instructions 'No special instructions were received'