Unusual Coupling Reaction of C60and Benzonitrile with Triosmium Carbonyls To Generate Fullerodiketimide Cluster Complexes
Lin, Yi-Sin; Yeh, Wen-Yann; Organometallics 33 (2014) 731–; doi:10.1021/om4011164

data_4082460
_publ_section_title
;
 Unusual Coupling Reaction of C60and Benzonitrile with Triosmium Carbonyls
 To Generate Fullerodiketimide Cluster Complexes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              731
_journal_paper_doi               10.1021/om4011164
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C146 H15 N3 O5 Os3, 3(C1 S2)'
_chemical_formula_sum            'C149 H15 N3 O5 Os3 S6'
_chemical_formula_weight         2689.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.957(5)
_cell_angle_beta                 113.190(4)
_cell_angle_gamma                111.212(4)
_cell_formula_units_Z            2
_cell_length_a                   17.2115(11)
_cell_length_b                   18.9698(14)
_cell_length_c                   19.1654(14)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4985.8(7)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius?Kappa CCD Axis'
_diffrn_measurement_method       CCD
_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  0.0995
_diffrn_reflns_av_sigmaI/netI    0.1865
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44037
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    4.009
_exptl_absorpt_correction_T_max  0.8561
_exptl_absorpt_correction_T_min  0.4108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2003 '
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
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_platon_squeeze_details
;
;
_refine_diff_density_max         8.354
_refine_diff_density_min         -3.750
_refine_diff_density_rms         0.401
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         17411
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1577
_refine_ls_R_factor_gt           0.1050
_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^)+(0.1758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2802
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4011164_si_002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        4985.8(6)
_cod_database_code               4082460