Synthesis, X-ray crystal structure, DNA/protein binding and DNA cleavage studies of novel copper(ii) complexes of N-substituted isatin thiosemicarbazone ligands
Muralisankar, Mathiyan; Bhuvanesh, Nattamai S. P.; Sreekanth, Anandaram; New J. Chem. 40 (2016) 2661–; doi:10.1039/C5NJ02806J

data_7055277
_publ_section_title
;
 Synthesis, X-ray crystal structure, DNA/protein binding and DNA cleavage
 studies of novel copper(ii) complexes of N-substituted isatin
 thiosemicarbazone ligands
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2661
_journal_paper_doi               10.1039/C5NJ02806J
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C16 H17 Cl Cu N4 O S'
_chemical_formula_sum            'C16 H17 Cl Cu N4 O S'
_chemical_formula_weight         412.38
_chemical_melting_point          519
_chemical_name_systematic
'N'-(1-allyl-2-oxoindolin-3-ylidene)pyrrolidine-1-carbothiohydrazide) copper(II) complex'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-11-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_audit_update_record
;
2015-08-16 deposited with the CCDC.
2016-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                105.822(4)
_cell_angle_beta                 98.341(4)
_cell_angle_gamma                108.844(4)
_cell_formula_units_Z            2
_cell_length_a                   8.984(3)
_cell_length_b                   9.757(4)
_cell_length_c                   10.524(4)
_cell_measurement_reflns_used    5043
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.530
_cell_measurement_theta_min      2.346
_cell_volume                     812.0(5)
_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  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9526
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         2.081
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.6804.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: METHANOL / ACETONITRILE'
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0458P)^2^+0.2724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3261
_reflns_number_total             3682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj02806j1.cif
_cod_data_source_block           mc1acu
_cod_depositor_comments
'Adding full bibliography for 7055272--7055277.cif.'
_cod_database_code               7055277
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.487
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C15(H15A,H15B), C9(H9A,H9B), C14(H14A,H14B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C8(H8), C6(H6), C7(H7)
2.c X=CH2 refined with riding coordinates:
 C11(H11A,H11B)
;
_shelx_res_checksum              87789
_olex2_submission_special_instructions 'No special instructions were received'