En Route to Osmium Analogues of KP1019: Synthesis, Structure, Spectroscopic Properties and Antiproliferative Activity of trans-[OsIVCl4(Hazole)2]
Gabriel E. Büchel; Iryna N. Stepanenko; Michaela Hejl; Michael A. Jakupec; Bernhard K. Keppler; Vladimir B. Arion; Inorganic Chemistry 50 (2011) 7690–7697; doi:10.1021/ic200728b

data_4325894
_publ_section_title
;
 En Route to Osmium Analogues of KP1019: Synthesis, Structure,
 Spectroscopic Properties and Antiproliferative Activity of
 trans-[OsIVCl4(Hazole)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7690
_journal_page_last               7697
_journal_paper_doi               10.1021/ic200728b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'C42 H42 N28 O14, C6 H8 C14 N4 Os, 4(H2 O), 7.25O'
_chemical_formula_sum            'C48 H72.5 Cl4 N32 O25.25 Os'
_chemical_formula_weight         1833.88
_chemical_name_systematic
; 
trans-tetrachlorido-bis(1H-pyrazole)osmium(IV)-cucurbit[7]uril
hydrate 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            4
_cell_length_a                   31.5673(9)
_cell_length_b                   16.9392(6)
_cell_length_c                   14.3896(5)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.42
_cell_measurement_theta_min      2.68
_cell_volume                     7694.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1029
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            123966
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  0.9282
_exptl_absorpt_correction_T_min  0.7037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       plate
_exptl_crystal_F_000             3722
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         13832
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0636P)^2^+24.5976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                10892
_reflns_number_total             13832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200728b_si_002_3.cif
_cod_data_source_block           gabu299
_cod_original_formula_sum        'C48 H72.50 Cl4 N32 O25.25 Os'
_cod_database_code               4325894