Osmium(III) Analogues of KP1019: Electrochemical and Chemical Synthesis, Spectroscopic Characterization, X-ray Crystallography, Hydrolytic Stability, and Antiproliferative Activity.
Kuhn, Paul-Steffen; Büchel, Gabriel E; Jovanović, Katarina K; Filipović, Lana; Radulović, Siniša; Rapta, Peter; Arion, Vladimir B.; Inorganic chemistry 53 (2014) 11130–11139; doi:10.1021/ic501710k

data_4341247
_publ_section_title
;
 Osmium(III) Analogues of KP1019: Electrochemical and Chemical Synthesis,
 Spectroscopic Characterization, X-ray Crystallography, Hydrolytic
 Stability, and Antiproliferative Activity.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11130
_journal_page_last               11139
_journal_paper_doi               10.1021/ic501710k
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C6 H8 Cl4 N4 Os, C3 H5 N2'
_chemical_formula_sum            'C9 H13 Cl4 N6 Os'
_chemical_formula_weight         537.25
_chemical_name_systematic
; 
Pyrazolium trans-tetrachlorido-bis(1H-pyrazole)osmate(III) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.6356(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4126(4)
_cell_length_b                   12.9016(6)
_cell_length_c                   16.1850(8)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.53
_cell_volume                     1542.78(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19761
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    8.956
_exptl_absorpt_correction_T_max  0.3889
_exptl_absorpt_correction_T_min  0.1775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0144
_refine_ls_R_factor_gt           0.0132
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+1.8670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0302
_refine_ls_wR_factor_ref         0.0306
_reflns_number_gt                2718
_reflns_number_total             2824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501710k_si_002.cif
_cod_data_source_block           PAKU435
_cod_depositor_comments
'Adding full bibliography for 4341247--4341249.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4341247