Synthesis, DNA/protein binding, molecular docking, DNA cleavage and in vitro anticancer activity of nickel(ii) bis(thiosemicarbazone) complexes
Haribabu, Jebiti; Jeyalakshmi, Kumaramangalam; Arun, Yuvaraj; Bhuvanesh, Nattamai S. P.; Perumal, Paramasivan Thirumalai; Karvembu, Ramasamy; RSC Adv. 5 (2015) 46031–; doi:10.1039/C5RA04498G

data_7220545
_publ_section_title
;
 Synthesis, DNA/protein binding, molecular docking, DNA cleavage and in
 vitro anticancer activity of nickel(ii) bis(thiosemicarbazone) complexes
;
_journal_issue                   57
_journal_name_full               'RSC Adv.'
_journal_page_first              46031
_journal_paper_doi               10.1039/C5RA04498G
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C20 H18 N8 Ni O2 S2, 3(C3 H7 N1 O1)'
_chemical_formula_sum            'C29 H39 N11 Ni O5 S2'
_chemical_formula_weight         744.54
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-01-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2015-03-07 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.181(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2985(14)
_cell_length_b                   11.9741(14)
_cell_length_c                   15.3857(13)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      38.50
_cell_measurement_theta_min      3.01
_cell_volume                     3414.5(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(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_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  0.0687
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            94121
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.714
_diffrn_reflns_theta_min         2.025
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.6356
_exptl_absorpt_correction_T_min  0.5450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1134 before and 0.0967 after correction.
The Ratio of minimum to maximum transmission is 0.8575.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         9435
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+2.4776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8419
_reflns_number_total             9435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra04498g2.cif
_cod_data_source_block           niip
_cod_database_code               7220545
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.680
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N22-C24 \\sim N22-C23
 with sigma of 0.02
 N17-C20 \\sim N17A-C20A \\sim N17-C19 \\sim N17A-C19A
 with sigma of 0.02
 N17-C18 \\sim N17A-C18A
 with sigma of 0.02
 O16-C18 \\sim O16A-C18A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C21)
Uanis(O16) = Uanis(O16A)
Uanis(N17) = Uanis(N17A)
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
4. Same fragment restrains
{O16, N17, C18, C19, C20}
as
{O16A, N17A, C18A, C19A, C20A}
5. Others
 Sof(O16A)=Sof(N17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(O16)=Sof(N17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Fixed Sof: O20(0.5) C21(0.5) H21(0.5) N22(0.5) C23(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C18(H18), C18A(H18A), C21(H21)
6.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C19A(H19D,H19E,
 H19F), C20A(H20D,H20E,H20F), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              64519
_shelx_hkl_checksum              1077