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_4082461
_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         'C152 H20 N4 O4 Os3,2(C1S2)'
_chemical_formula_sum            'C154 H20 N4 O4 Os3 S4'
_chemical_formula_weight         2688.58
_chemical_name_systematic
;
 ?
;
_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                 114.453(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.076(3)
_cell_length_b                   14.7591(19)
_cell_length_c                   25.284(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     9198(2)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1766
_diffrn_reflns_av_sigmaI/netI    0.2044
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            63749
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    4.302
_exptl_absorpt_correction_T_max  0.8818
_exptl_absorpt_correction_T_min  0.3490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2003 '
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5184
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.03
_platon_squeeze_details
; 
?
;
_refine_diff_density_max         1.139
_refine_diff_density_min         -1.843
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1402
_refine_ls_number_reflns         16050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                8562
_reflns_number_total             16050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4011164_si_002.cif
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4082461