Sc2(μ2-O) Trapped in a Fullerene Cage: The Isolation and Structural Characterization of Sc2(μ2-O)@Cs(6)-C82 and the Relevance of the Thermal and Entropic Effects in Fullerene Isomer Selection
Brandon Q. Mercado; Melissa A. Stuart; Mary A. Mackey; Jane E. Pickens; Bridget S. Confait; Steven Stevenson; Michael L. Easterling; Ramón Valencia; Antonio Rodríguez-Fortea; Josep M. Poblet; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 132 (2010) 12098–12105; doi:10.1021/ja104902e

data_4102963
_publ_section_title
;
 Sc2(\m2-O) Trapped in a Fullerene Cage: The Isolation and Structural
 Characterization of Sc2(\m2-O)@Cs(6)-C82 and the Relevance of the Thermal
 and Entropic Effects in Fullerene Isomer Selection
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12098
_journal_page_last               12105
_journal_paper_doi               10.1021/ja104902e
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'C82 O1 Sc2, C36 H44 N4 Ni, 1.4(C7 H8).0.6(C6 H6)'
_chemical_formula_sum            'C131.4 H58.8 N4 Ni O Sc2'
_chemical_formula_weight         1858.06
_chemical_name_common
Sc2O@Cs(6)-C82.Ni[OEP].1.4(toluene).0.6(benzene)
_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                 96.447(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.3421(6)
_cell_length_b                   14.7875(4)
_cell_length_c                   20.3492(5)
_cell_measurement_reflns_used    20400
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.79
_cell_measurement_theta_min      2.20
_cell_volume                     7577.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            144527
_diffrn_reflns_theta_full        41.79
_diffrn_reflns_theta_max         41.79
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.9341
_exptl_absorpt_correction_T_min  0.8701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3813
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1202
_refine_ls_number_reflns         20400
_refine_ls_number_restraints     2807
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1067P)^2^+13.3004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2147
_reflns_number_gt                17273
_reflns_number_total             20400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104902e_si_001.cif
_cod_data_source_block           mn2003
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4102963