Synthesis of Silylene-Bridged Endohedral Metallofullerene Lu3N@Ih-C80
Kumiko Sato; Masahiro Kako; Mitsuaki Suzuki; Naomi Mizorogi; Takahiro Tsuchiya; Marilyn M. Olmstead; Alan L. Balch; Takeshi Akasaka; Shigeru Nagase; Journal of the American Chemical Society 134 (2012) 16033–16039; doi:10.1021/ja3073929

data_4118695
_publ_section_title
;
 Synthesis of Silylene-Bridged Endohedral Metallofullerene Lu3N@Ih-C80
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16033
_journal_page_last               16039
_journal_paper_doi               10.1021/ja3073929
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'Lu3 N C100 H26 Si, C S2'
_chemical_formula_sum            'C101 H26 Lu3 N S2 Si'
_chemical_formula_weight         1870.35
_chemical_name_common            Lu3N@C80-SiDep2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                   10.9576(10)
_cell_length_b                   17.2860(15)
_cell_length_c                   28.760(2)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.31
_cell_volume                     5447.5(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            34063
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    5.564
_exptl_absorpt_correction_T_max  0.8081
_exptl_absorpt_correction_T_min  0.4342
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_description       plate
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.615
_refine_diff_density_min         -3.505
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6916
_refine_ls_number_restraints     776
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1043
_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^)+(0.0000P)^2^+372.4500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2339
_refine_ls_wR_factor_ref         0.2416
_reflns_number_gt                5646
_reflns_number_total             6916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3073929_si_002.cif
_cod_data_source_block           s1x
_cod_database_code               4118695