Synthesis, Structure, and Transformation of Novel Osmium Azine and Ylide Complexes
Te-Wei Chiu; Yen-Hsiang Liu; Kai-Ming Chi; Yuh-Sheng Wen; Kuang-Lieh Lu; Inorganic Chemistry 44 (2005) 6425–6430; doi:10.1021/ic050431o

data_4309491
_publ_section_title
;
Synthesis, Structure, and Transformation of Novel Osmium Azine and Ylide
Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6425
_journal_page_last               6430
_journal_paper_doi               10.1021/ic050431o
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C18 H10 O11 Os3'
_chemical_formula_weight         972.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.098(16)
_cell_angle_beta                 96.73(2)
_cell_angle_gamma                98.318(18)
_cell_formula_units_Z            4
_cell_length_a                   8.287(2)
_cell_length_b                   14.998(3)
_cell_length_c                   18.674(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.52
_cell_measurement_theta_min      7.662
_cell_volume                     2280.3(9)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8621
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.730
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_correction_T_min  0.3001
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.088
_refine_diff_density_min         -3.153
_refine_diff_density_rms         0.397
_refine_ls_extinction_coef       0.00205(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         8013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          1.355
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1233P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1694
_reflns_number_gt                5735
_reflns_number_total             8013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050431osi20050607_024010.cif
_cod_data_source_block           i1115
_cod_database_code               4309491