Osmium(vi) nitrido complexes bearing azole heterocycles: a new class of antitumor agents
Ni, Wen-Xiu; Man, Wai-Lun; Yiu, Shek-Man; Ho, Man; Cheung, Myra Ting-Wai; Ko, Chi-Chiu; Che, Chi-Ming; Lam, Yun-Wah; Lau, Tai-Chu; Chemical Science 3 (2012) 1582–; doi:10.1039/c2sc01031c

data_1515230
_publ_section_title
;
 Osmium(vi) nitrido complexes bearing azole heterocycles: a new class of
 antitumor agents
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1582
_journal_paper_doi               10.1039/c2sc01031c
_journal_volume                  3
_journal_year                    2012
_chemical_formula_moiety         '0.5(C20 H32 Cl6 N10 Os2)'
_chemical_formula_sum            'C10 H16 Cl3 N5 Os'
_chemical_formula_weight         502.83
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-18
_audit_creation_method
;
Olex2 1.1
(compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.79
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.466
_cell_length_b                   14.595
_cell_length_c                   10.063
_cell_measurement_reflns_used    4491
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.3607
_cell_measurement_theta_min      4.4007
_cell_volume                     1535.314
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
1 omega -36.00 27.00 0.5000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6700 77.0000 150.0000 126

2 omega -62.00 32.00 0.5000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6700 37.0000 30.0000 188

3 omega -77.00 -30.00 0.5000 1.5000
omega____ theta____ kappa____ phi______ frames
- -40.6700 125.0000 150.0000 94

4 omega 22.00 101.00 0.5000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6700 77.0000 30.0000 158

5 omega 32.00 63.00 0.5000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6700 -77.0000 -90.0000 62

6 omega -30.00 59.00 0.5000 1.5000
omega____ theta____ kappa____ phi______ frames
- 40.6700 -37.0000 -150.0000 178

7 omega -129.00 -49.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- -64.0000 -45.0000 90.0000 160

8 omega -140.00 -86.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- -64.0000 179.0000 -60.0000 108

9 omega 80.00 144.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 77.0000 60.0000 128

10 omega 80.00 178.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 77.0000 30.0000 196

11 omega 37.00 168.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 0.0000 -150.0000 262

12 omega 60.00 148.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 -92.0000 -73.0000 176

13 omega 64.00 133.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 -45.0000 60.0000 138

14 omega 41.00 133.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 -45.0000 -120.0000 184

15 omega 139.00 175.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 77.0000 -120.0000 72

16 omega 69.00 118.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 -45.0000 120.0000 98

17 omega 72.00 111.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 -92.0000 -32.0000 78

18 omega 45.00 70.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 -78.0000 -3.0000 50

19 omega 48.00 114.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 -92.0000 84.0000 132

20 omega 60.00 130.00 0.5000 8.0000
omega____ theta____ kappa____ phi______ frames
- 109.6546 -90.0000 168.0000 140
;
_diffrn_measurement_device_type
;
Goniometer Xcalibur, detector: Sapphire3,
removed Mo collimator (Gemini ultra Cu)
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1307319321
_diffrn_orient_matrix_UB_12      -0.0469146234
_diffrn_orient_matrix_UB_13      0.0247215321
_diffrn_orient_matrix_UB_21      -0.0638992105
_diffrn_orient_matrix_UB_22      -0.0765577164
_diffrn_orient_matrix_UB_23      0.0779662004
_diffrn_orient_matrix_UB_31      -0.0220222759
_diffrn_orient_matrix_UB_32      -0.0552223990
_diffrn_orient_matrix_UB_33      -0.1296329648
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3882
_diffrn_reflns_theta_full        66.98
_diffrn_reflns_theta_max         66.98
_diffrn_reflns_theta_min         5.20
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    20.450
_exptl_absorpt_correction_T_max  0.389
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.2799
_exptl_crystal_size_mid          0.1717
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.353
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0271P)^2^+4.4444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                1372
_reflns_number_total             1372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc01031c.txt
_cod_data_source_block           4
_cod_original_cell_volume        1535.3
_cod_database_code               1515230
_chemical_oxdiff_formula         'Os1 Cl3 N5 C10'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49