A Distorted Tetrahedral Metal Oxide Cluster inside an Icosahedral Carbon Cage. Synthesis, Isolation, and Structural Characterization of Sc4(μ3-O)2@Ih-C80
Steven Stevenson; Mary A. Mackey; Melissa A. Stuart; J. Paige Phillips; Michael L. Easterling; Christopher J. Chancellor; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 130 (2008) 11844–11845; doi:10.1021/ja803679u

data_4108307
_publ_section_title
;
 A Distorted Tetrahedral Metal Oxide Cluster inside an Icosahedral Carbon
 Cage. Synthesis, Isolation, and Structural Characterization of
 Sc4(\m3-O)2@Ih-C80
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11844
_journal_page_last               11845
_journal_paper_doi               10.1021/ja803679u
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C80 Sc4 O2, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C128 H56 N4 Ni O2 Sc4'
_chemical_formula_weight         1920.32
_chemical_name_common            'Sc4O2@C80.NiOEP.2benzene '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 95.174(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2074(12)
_cell_length_b                   15.1047(7)
_cell_length_c                   19.7780(9)
_cell_measurement_reflns_used    9048
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      62.853
_cell_measurement_theta_min      5.567
_cell_volume                     7499.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'Apex2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;SHELXTL 5.1, XP (Sheldrick, 1994), ORTEP-3 for Windows(Farrugia, 1997),
POV-Ray-3.6 for Windows(Persistence of Vision Pty. Ltd., 2004)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART ApexII'
_diffrn_measurement_method       \w
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60793
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       block
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.457
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         12357
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.1203
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1877P)^2^+73.2401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3233
_refine_ls_wR_factor_ref         0.3435
_reflns_number_gt                9950
_reflns_number_total             12357
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja803679u_si_001.cif
_cod_data_source_block           cjc133
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4108307