The Shape of the Sc2(μ2-S) Unit Trapped in C82: Crystallographic, Computational, and Electrochemical Studies of the Isomers, Sc2(μ2-S)@Cs(6)-C82 and Sc2(μ2-S)@C3v(8)-C82
Brandon Q. Mercado; Ning Chen; Antonio Rodríguez-Fortea; Mary A. Mackey; Steven Stevenson; Luis Echegoyen; Josep M. Poblet; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 133 (2011) 6752–6760; doi:10.1021/ja200289w

data_4106069
_publ_section_title
;
 The Shape of the Sc2(\m2-S) Unit Trapped in C82: Crystallographic,
 Computational, and Electrochemical Studies of the Isomers,
 Sc2(\m2-S)@Cs(6)-C82 and Sc2(\m2-S)@C3v(8)-C82
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6752
_journal_page_last               6760
_journal_paper_doi               10.1021/ja200289w
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C82 Sc2 S, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C130 H56 N4 Ni S Sc2'
_chemical_formula_weight         1854.48
_chemical_name_common            Sc2S@C3v(8)-C84.Ni(OEP).2(benzene)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.042(9)
_cell_angle_beta                 84.611(9)
_cell_angle_gamma                61.109(8)
_cell_formula_units_Z            2
_cell_length_a                   14.697(2)
_cell_length_b                   14.756(2)
_cell_length_c                   20.104(3)
_cell_measurement_reflns_used    22456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.66
_cell_measurement_theta_min      2.22
_cell_volume                     3791.9(10)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (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 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Advanced Light Source beamline 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57354
_diffrn_reflns_theta_full        36.87
_diffrn_reflns_theta_max         33.66
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.65
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.017
_refine_diff_density_min         -1.851
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1286
_refine_ls_number_reflns         28404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1915
_refine_ls_R_factor_gt           0.1126
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2936
_refine_ls_wR_factor_ref         0.3450
_reflns_number_gt                15544
_reflns_number_total             22456
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja200289w_si_002.cif
_cod_data_source_block           bqm56
_cod_original_cell_volume        3791.9(9)
_cod_database_code               4106069