Arene Osmium Complexes with Ethacrynic Acid-Modified Ligands: Synthesis, Characterization, and Evaluation of Intracellular GlutathioneS-Transferase Inhibition and Antiproliferative Activity
Agonigi, Gabriele; Riedel, Tina; Gay, M. Pilar; Biancalana, Lorenzo; Oñate, Enrique; Dyson, Paul J.; Pampaloni, Guido; Păunescu, Emilia; Esteruelas, Miguel A.; Marchetti, Fabio; Organometallics 35 (2016) 1046–; doi:10.1021/acs.organomet.6b00197

data_4086442
_publ_section_title
;
 Arene Osmium Complexes with Ethacrynic Acid-Modified Ligands: Synthesis,
 Characterization, and Evaluation of Intracellular
 GlutathioneS-Transferase Inhibition and Antiproliferative Activity
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1046
_journal_paper_doi               10.1021/acs.organomet.6b00197
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C28 H32 Cl2 O6 Os'
_chemical_formula_weight         725.64
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.6723(19)
_cell_length_b                   11.5289(11)
_cell_length_c                   24.095(2)
_cell_measurement_reflns_used    9113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     5464.7(9)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57473
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    4.903
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 7.56a (2008).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.501
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         7332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+1.8673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                5223
_reflns_number_total             7332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00197_si_001.cif
_cod_data_source_block           enriquen66
_cod_depositor_comments
'Adding full bibliography for 4086441--4086442.cif.'
_cod_original_cell_volume        5464.8(9)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4086442