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_7057430
_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         'C30 H28 Cl N4 P Pd S, C3 H7 N O'
_chemical_formula_sum            'C33 H35 Cl N5 O P Pd S'
_chemical_formula_weight         722.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1ppjc8
_audit_creation_date             2015-04-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_audit_update_record
;
2017-08-19 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.159(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   32.724(9)
_cell_length_b                   8.830(2)
_cell_length_c                   35.834(10)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.393
_cell_measurement_theta_min      2.275
_cell_volume                     9839(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            111386
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         0.655
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.7362
_exptl_absorpt_correction_T_min  0.5761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1407 before and 0.0743 after correction.
The Ratio of minimum to maximum transmission is 0.7825.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.163
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         22425
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+32.0530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18130
_reflns_number_total             22425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03743k2.cif
_cod_data_source_block           jhpd5
_cod_depositor_comments
'Adding full bibliography for 7057427--7057432.cif.'
_cod_original_cell_volume        9838(5)
_cod_database_code               7057430
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.692
_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. Uiso/Uaniso restraints and constraints
Uanis(O11S) = Uanis(C12S) = Uanis(N13S) = Uanis(C14S) = Uanis(C15S) =
Uanis(O11T) = Uanis(C12T) = Uanis(N13T) = Uanis(C14T) = Uanis(C15T)
3. Same fragment restrains
{O6S, C7S, N8S, C9S, C10S} sigma for 1-2: 0.005, 1-3: 0.04
as
{O11S, C12S, N13S, C14S, C15S}
{O6S, C7S, N8S, C9S, C10S} sigma for 1-2: 0.005, 1-3: 0.04
as
{O11T, C12T, N13T, C14T, C15T}
4. Others
 Sof(O11T)=Sof(C12T)=Sof(H12T)=Sof(N13T)=Sof(C14T)=Sof(H14F)=Sof(H14G)=
 Sof(H14H)=Sof(C15T)=Sof(H15F)=Sof(H15G)=Sof(H15H)=1-FVAR(1)
 Sof(O11S)=Sof(C12S)=Sof(H12S)=Sof(N13S)=Sof(C14S)=Sof(H14A)=Sof(H14B)=
 Sof(H14D)=Sof(C15S)=Sof(H15A)=Sof(H15B)=Sof(H15D)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C11C(H11C,H11D), C11E(H11E,H11F)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C1(H1), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), N2C(H2C),
 N4C(H4C), C1C(H1C), C5C(H5C), C6C(H6C), C7C(H7C), C8C(H8C), C9C(H9C),
 C14C(H14C), C15C(H15C), C16C(H16C), C17C(H17C), C18C(H18C), C20C(H20C),
 C21C(H21C), C22C(H22C), C23C(H23C), C24C(H24C), C26C(H26C), C27C(H27C),
 C28C(H28C), C29C(H29C), C30C(H30C), N2E(H2E), N4E(H4E), C1E(H1E), C5E(H5E),
 C6E(H6E), C7E(H7E), C8E(H8E), C9E(H9E), C14E(H14E), C15E(H15E), C16E(H16E),
 C17E(H17E), C18E(H18E), C20E(H20E), C21E(H21E), C22E(H22E), C23E(H23E),
 C24E(H24E), C26E(H26E), C27E(H27E), C28E(H28E), C29E(H29E), C30E(H30E),
 C2S(H2S), C7S(H7S), C12S(H12S), C12T(H12T)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C12C(H12D,H12E,H12F), C12E(H12G,H12H,H12I), C4S(H4SA,
 H4SB,H4SC), C5S(H5SA,H5SB,H5SC), C9S(H9SA,H9SB,H9SC), C10S(H10A,H10B,H10C),
 C14S(H14A,H14B,H14D), C15S(H15A,H15B,H15D), C14T(H14F,H14G,H14H), C15T(H15F,
 H15G,H15H)
;
_shelx_res_checksum              17879
_olex2_submission_special_instructions 'No special instructions were received'