Synthesis, structures and mechanistic pathways of anticancer activity of palladium(ii) complexes with indole-3-carbaldehyde thiosemicarbazones
Haribabu, Jebiti; Tamizh, Manoharan Muthu; Balachandran, Chandrasekar; Arun, Yuvaraj; Bhuvanesh, Nattamai S. P.; Endo, Akira; Karvembu, Ramasamy; New Journal of Chemistry 42 (2018) 10818–; doi:10.1039/C7NJ03743K

data_7057431
_publ_section_title
;
 Synthesis, structures and mechanistic pathways of anticancer activity of
 palladium(ii) complexes with indole-3-carbaldehyde thiosemicarbazones
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10818
_journal_paper_doi               10.1039/C7NJ03743K
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C34 H28 Cl N4 P Pd S'
_chemical_formula_sum            'C34 H28 Cl N4 P Pd S'
_chemical_formula_weight         697.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1ppjb7
_audit_creation_date             2014-06-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2017-08-19 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.909(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0748(19)
_cell_length_b                   11.326(2)
_cell_length_c                   15.049(3)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      27.343
_cell_measurement_theta_min      2.256
_cell_volume                     1704.7(6)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18810
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.344
_diffrn_reflns_theta_min         1.798
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0797 before and 0.0381 after correction.
The Ratio of minimum to maximum transmission is 0.7876.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 3670 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7602
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0151
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.1473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0398
_reflns_Friedel_coverage         0.977
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                7505
_reflns_number_total             7602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03743k2.cif
_cod_data_source_block           inppd_sq
_cod_depositor_comments
'Adding full bibliography for 7057427--7057432.cif.'
_cod_database_code               7057431
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C1(H1), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34)
;
_shelx_res_checksum              21346
_shelx_fab_checksum              3400