New dinuclear ruthenium arene complexes containing thiosemicarbazone ligands: synthesis, structure and cytotoxic studies.
Su, Wei; Tang, Zhaofeng; Li, Peiyuan; Wang, Gufeng; Xiao, Qi; Li, Yuchun; Huang, Shan; Gu, Yunqiong; Lai, Zefeng; Zhang, Yuexing; Dalton transactions (Cambridge, England : 2003) 45 (2016) 19329–19340; doi:10.1039/c6dt03306g

data_7041118
_publ_section_title
;
 New dinuclear ruthenium arene complexes containing thiosemicarbazone
 ligands: synthesis, structure and cytotoxic studies.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19329
_journal_page_last               19340
_journal_paper_doi               10.1039/c6dt03306g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C20 H27 Cl N3 O Ru S, Cl, 0.5(C H2 Cl2), 0.25(H2 O)'
_chemical_formula_sum            'C20.5 H28.5 Cl3 N3 O1.25 Ru S'
_chemical_formula_weight         575.69
_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             2012-11-14
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2016-10-10 deposited with the CCDC.
2016-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                113.651(8)
_cell_angle_beta                 90.091(5)
_cell_angle_gamma                99.696(7)
_cell_formula_units_Z            8
_cell_length_a                   13.1337(9)
_cell_length_b                   20.1079(19)
_cell_length_c                   20.8773(13)
_cell_measurement_reflns_used    8702
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5111
_cell_measurement_theta_min      2.9267
_cell_volume                     4963.6(7)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -18.00   25.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000  120.0000 86

  2 omega  -12.00   22.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2889  -99.0000  -30.0000 68

  3 omega  -49.00   -4.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608  -57.0000 -180.0000 90

  4 omega    5.00   91.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608   57.0000  -30.0000 172

  5 omega  -32.00   93.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608   19.0000  120.0000 250

  6 omega   43.00  101.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608  178.0000  -30.0000 116

  7 omega   73.00  100.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608  178.0000  150.0000 54

  8 omega    6.00   53.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608  -38.0000   60.0000 94

  9 omega  -10.00   95.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608   38.0000  120.0000 210

 10 omega  -54.00   88.00   0.5000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4608  -19.0000  -60.0000 284
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0533858000
_diffrn_orient_matrix_UB_12      0.0130775000
_diffrn_orient_matrix_UB_13      -0.0009106000
_diffrn_orient_matrix_UB_21      0.0066523000
_diffrn_orient_matrix_UB_22      0.0129369000
_diffrn_orient_matrix_UB_23      0.0370058000
_diffrn_orient_matrix_UB_31      0.0111775000
_diffrn_orient_matrix_UB_32      -0.0346012000
_diffrn_orient_matrix_UB_33      -0.0036624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1159
_diffrn_reflns_av_unetI/netI     0.1478
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            57057
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42873
_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_colour            red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2342
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.762
_refine_diff_density_min         -2.877
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1092
_refine_ls_number_reflns         17957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.2166
_refine_ls_R_factor_gt           0.1715
_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^)+(0.1360P)^2^+219.9565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4172
_refine_ls_wR_factor_ref         0.4411
_reflns_number_gt                11072
_reflns_number_total             17957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03306g2.cif
_cod_data_source_block           980124
_cod_depositor_comments
;
Adding full bibliography for 7041117--7041126.cif.

2017-10-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C82 H111 Cl12 N12 O5 Ru4 S4'
_cod_original_formula_weight         2302.75
_cod_original_formula_moiety
'C20 H26 Cl N3 O Ru S, 3(C20 H27 Cl N3 O Ru S), 4(Cl), 2(C H2 Cl2), O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4963.6(6)
_cod_database_code               7041118
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32