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_7057432
_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 H34 Cl N4 P Pd S, 0.25(H2 O)'
_chemical_formula_sum            'C34 H34.5 Cl N4 O0.25 P Pd S'
_chemical_formula_weight         708.03
_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
_audit_block_doi                 10.5517/ccdc.csd.cc1ppj96
_audit_creation_date             2014-06-06
_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                 94.015(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5377(5)
_cell_length_b                   9.5497(5)
_cell_length_c                   35.8336(14)
_cell_measurement_reflns_used    5116
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      60.753
_cell_measurement_theta_min      2.472
_cell_volume                     3255.8(3)
_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 0.786
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.786
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            22035
_diffrn_reflns_point_group_measured_fraction_full 0.786
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         60.814
_diffrn_reflns_theta_min         2.472
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.651
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0914 before and 0.0619 after correction.
The Ratio of minimum to maximum transmission is 0.8034.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             1450
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+1.0980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3666
_reflns_number_total             4642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03743k2.cif
_cod_data_source_block           inkpd
_cod_depositor_comments
'Adding full bibliography for 7057427--7057432.cif.'
_cod_original_formula_sum        'C34 H34.50 Cl N4 O0.25 P Pd S'
_cod_database_code               7057432
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.777
_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 O(H,H) groups
2. Others
 Fixed Sof: O1W(0.25) H1WA(0.25) H1WB(0.25)
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Ternary CH refined with riding coordinates:
 C11(H11)
3.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C12(H12A,H12B), C15(H15A,H15B), C13(H13A,H13B), C14(H14A,H14B)
3.d Aromatic/amide H refined with riding coordinates:
 N4(H4), N2(H2), C22(H22), C20(H20), C24(H24), C33(H33), C9(H9), C19(H19),
 C27(H27), C21(H21), C32(H32), C1(H1), C25(H25), C18(H18), C28(H28), C34(H34),
 C31(H31), C30(H30), C3(H3), C26(H26), C7(H7), C8(H8), C6(H6)
;
_shelx_res_checksum              32819