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_4336545
_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         'C20 H27 Cl N3 Ru S, Cl, C H Cl3'
_chemical_formula_sum            'C21 H0.5 Cl5 N3 Ru S'
_chemical_formula_weight         605.12
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-04
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  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
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_cell_angle_alpha                106.537(4)
_cell_angle_beta                 102.353(4)
_cell_angle_gamma                107.465(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9135(5)
_cell_length_b                   11.8264(5)
_cell_length_c                   12.9485(5)
_cell_measurement_reflns_used    4429
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6400
_cell_measurement_theta_min      2.9134
_cell_volume                     1311.72(12)
_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)
;
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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)
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_computing_molecular_graphics
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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 16.1623
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -13.00   25.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -      -19.3361  -99.0000  150.0000 38

  2 omega   -1.00   92.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       22.9299   57.0000   30.0000 93

  3 omega  -49.00   50.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       22.9299  -44.0000  111.0000 99

  4 omega   -8.00   54.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       22.9299  -99.0000   90.0000 62

  5 omega  -48.00   46.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       22.9299  -57.0000 -120.0000 94

  6 omega   -1.00   85.00   1.0000    2.8200
omega____ theta____ kappa____ phi______ frames
    -       22.9299   57.0000  -90.0000 86
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0332768000
_diffrn_orient_matrix_UB_12      0.0291371000
_diffrn_orient_matrix_UB_13      -0.0331029000
_diffrn_orient_matrix_UB_21      0.0704260000
_diffrn_orient_matrix_UB_22      0.0318737000
_diffrn_orient_matrix_UB_23      -0.0042836000
_diffrn_orient_matrix_UB_31      -0.0153020000
_diffrn_orient_matrix_UB_32      -0.0522749000
_diffrn_orient_matrix_UB_33      -0.0504285000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10993
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97594
_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    1.532
_exptl_crystal_F_000             585
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+0.4655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                4332
_reflns_number_total             5379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401362s_si_001_7.cif
_cod_data_source_block           941658
_cod_original_cell_volume        1311.71(10)
_cod_original_formula_sum        'C21 H0.50 Cl5 N3 Ru S'
_cod_database_code               4336545
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32