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_4106068
_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@Cs(6)-C82.Ni(OEP).2benzene
_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
_audit_update_record
;
2010-08-11 # Formatted by publCIF
;
_cell_angle_alpha                85.831(2)
_cell_angle_beta                 89.630(2)
_cell_angle_gamma                88.845(2)
_cell_formula_units_Z            4
_cell_length_a                   14.9420(5)
_cell_length_b                   19.9180(8)
_cell_length_c                   25.3474(9)
_cell_measurement_reflns_used    5306
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.6
_cell_measurement_theta_min      2.5
_cell_volume                     7522.2(5)
_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 0.981
_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_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            159528
_diffrn_reflns_theta_full        36.60
_diffrn_reflns_theta_max         36.60
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.078
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2523
_refine_ls_number_reflns         56317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1317P)^2^+5.2214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2027
_refine_ls_wR_factor_ref         0.2202
_reflns_number_gt                47544
_reflns_number_total             56317
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja200289w_si_001.cif
_cod_data_source_block           bqm54
_cod_database_code               4106068