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_4336546
_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         'C25 H29 Cl N3 Ru S, Cl, C H Cl3'
_chemical_formula_sum            'C26 H0.5 Cl5 N3 Ru S'
_chemical_formula_weight         665.17
_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             2013-05-03
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  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.441(3)
_cell_angle_beta                 104.198(3)
_cell_angle_gamma                94.091(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9199(4)
_cell_length_b                   11.3989(5)
_cell_length_c                   13.7623(5)
_cell_measurement_reflns_used    6727
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8000
_cell_measurement_theta_min      2.8271
_cell_volume                     1504.29(11)
_computing_cell_refinement
;
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 16.1623
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -99.00  -74.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3361 -178.0000  -30.0000 25

  2 omega  -14.00   14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3361  -99.0000  -30.0000 28

  3 omega   -8.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3361  -99.0000   90.0000 33

  4 omega  -34.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.9299   19.0000  150.0000 127

  5 omega    1.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.9299   57.0000  -30.0000 92

  6 omega  -46.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.9299  -57.0000 -180.0000 93

  7 omega   34.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.9299 -178.0000   90.0000 71

  8 omega   -8.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.9299   38.0000 -120.0000 104
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0579595000
_diffrn_orient_matrix_UB_12      -0.0144845000
_diffrn_orient_matrix_UB_13      0.0204088000
_diffrn_orient_matrix_UB_21      -0.0081839000
_diffrn_orient_matrix_UB_22      0.0607009000
_diffrn_orient_matrix_UB_23      0.0061896000
_diffrn_orient_matrix_UB_31      -0.0452196000
_diffrn_orient_matrix_UB_32      -0.0001307000
_diffrn_orient_matrix_UB_33      -0.0487175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15287
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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    1.469
_exptl_crystal_F_000             645
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.8698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                5202
_reflns_number_total             6160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401362s_si_001_8.cif
_cod_data_source_block           941659
_cod_original_cell_volume        1504.31(11)
_cod_original_formula_sum        'C26 H0.50 Cl5 N3 Ru S'
_cod_database_code               4336546
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32