Novel Bis-C,N-Cyclometalated Iridium(III) Thiosemicarbazide Antitumor Complexes: Interactions with Human Serum Albumin and DNA, and Inhibition of Cathepsin B
José Ruiz; Consuelo Vicente; Concepción de Haro; Delia Bautista; Inorganic Chemistry 52 (2013) 974–982; doi:10.1021/ic302219v

data_4333612
_publ_section_title
;
 Novel Bis-C,N-Cyclometalated Iridium(III) Thiosemicarbazide Antitumor
 Complexes: Interactions with Human Serum Albumin and DNA, and Inhibition
 of Cathepsin B
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              974
_journal_page_last               982
_journal_paper_doi               10.1021/ic302219v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C24 H23 Cl Ir N5 S'
_chemical_formula_weight         641.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.836(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5488(12)
_cell_length_b                   9.3007(7)
_cell_length_c                   20.6588(17)
_cell_measurement_reflns_used    6500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.62
_cell_volume                     2987.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19904
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    4.646
_exptl_absorpt_correction_T_max  0.8009
_exptl_absorpt_correction_T_min  0.5675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;

The structure contains a poorly-resolved region of residual
elelctron density; this could not be adequately modelled and 
so was "removed" using the program SQUEEZE, which is part 
of the PLATON system. The void volume per cell was 888.6 \%A^3^, 
with a void electron count per cell of 187. 
This additional solvent was NOT taken account of when
 calculating derived parameters such as the formula weight, 
because the nature of the solvent was uncertain.

;
_refine_diff_density_max         1.680
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    'NH with DFIX, rigid methyl others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         6549
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                4786
_reflns_number_total             6549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302219v_si_001.cif
_cod_data_source_block           cvi55s_squeezed
_cod_database_code               4333612