Synthesis, Characterization, and Anticancer Activity of a Series of Ketone-N4-Substituted Thiosemicarbazones and Their Ruthenium(II) Arene Complexes
Wei Su; Quanquan Qian; Peiyuan Li; Xiaolin Lei; Qi Xiao; Shan Huang; Chusheng Huang; Jianguo Cui; Inorganic Chemistry 52 (2013) 12440–12449; doi:10.1021/ic401362s

data_4336539
_publ_contact_author_address
; 
College of Chemistry and Life Science, 
Guangxi Teachers Education University, 
Nanning, China
;
_publ_contact_author_email       suwmail@163.com
_publ_contact_author_name        'Wei Su'
_publ_section_title
;
 Synthesis, Characterization, and Anticancer Activity of a Series of
 Ketone-N4-Substituted Thiosemicarbazones and Their Ruthenium(II) Arene
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12440
_journal_page_last               12449
_journal_paper_doi               10.1021/ic401362s
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C9 H11 N3 S), O2'
_chemical_formula_sum            'C18 H22 N6 O2 S2'
_chemical_formula_weight         418.54
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-03
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  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
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_cell_angle_alpha                90.00
_cell_angle_beta                 97.044(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2988(14)
_cell_length_b                   5.8431(4)
_cell_length_c                   25.917(2)
_cell_measurement_reflns_used    2814
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4727
_cell_measurement_theta_min      2.8834
_cell_volume                     2299.3(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9784
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -74.00  -40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889 -178.0000  150.0000 34

  2 omega    8.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608   38.0000  120.0000 75

  3 omega  -51.00   58.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608    0.0000   90.0000 109

  4 omega  -52.00    0.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608  -38.0000  -30.0000 52
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0021081000
_diffrn_orient_matrix_UB_12      -0.0146526000
_diffrn_orient_matrix_UB_13      0.0269842000
_diffrn_orient_matrix_UB_21      0.0369879000
_diffrn_orient_matrix_UB_22      0.0725844000
_diffrn_orient_matrix_UB_23      0.0056844000
_diffrn_orient_matrix_UB_31      -0.0283114000
_diffrn_orient_matrix_UB_32      0.0964632000
_diffrn_orient_matrix_UB_33      -0.0001102000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10231
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.17
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4695
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1292P)^2^+0.9297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2367
_reflns_number_gt                3359
_reflns_number_total             4695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401362s_si_001_1.cif
_cod_data_source_block           941661
_cod_database_code               4336539
_reflns_odcompleteness_completeness 99.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32