Sc2S@Cs(10528)-C72: A Dimetallic Sulfide Endohedral Fullerene with a Non Isolated Pentagon Rule Cage
Ning Chen; Christine M. Beavers; Marc Mulet-Gas; Antonio Rodríguez-Fortea; Elias J. Munoz; Yu-Yang Li; Marilyn M. Olmstead; Alan L. Balch; Josep M. Poblet; Luis Echegoyen; Journal of the American Chemical Society 134 (2012) 7851–7860; doi:10.1021/ja300765z

data_4117910
_publ_contact_author_address
;Advanced Light Source
Lawrence Berkeley National Lab
One Cyclotron Rd
MS 7-222
Berkeley, CA 94720
;
_publ_contact_author_email       cmbeavers@lbl.gov
_publ_contact_author_name        'Christine M. Beavers'
_publ_contact_author_phone       (510)495-2448
_publ_section_title
;
 Sc2S@Cs(10528)-C72: A Dimetallic Sulfide Endohedral Fullerene with a Non
 Isolated Pentagon Rule Cage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7851
_journal_page_last               7860
_journal_paper_doi               10.1021/ja300765z
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'Sc2 S C72, C36 H44 N4 Ni, 1.5(C7 H8)'
_chemical_formula_sum            'C118.5 H56 N4 Ni S Sc2'
_chemical_formula_weight         1716.36
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.032(2)
_cell_angle_beta                 74.752(2)
_cell_angle_gamma                65.310(2)
_cell_formula_units_Z            2
_cell_length_a                   15.1733(4)
_cell_length_b                   15.9533(4)
_cell_length_c                   16.7953(4)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.0
_cell_measurement_theta_min      2.23
_cell_volume                     3523.49(17)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2010)'
_computing_data_collection       'Apex2 v2010.3 (Bruker, 2010)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_source         'Advanced Light Source Beamline 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            163650
_diffrn_reflns_theta_full        36.00
_diffrn_reflns_theta_max         40.31
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_correction_T_min  0.9469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS-2008/4 (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1762
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.801
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1837
_refine_ls_number_reflns         33273
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+1.1340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                25487
_reflns_number_total             33273
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja300765z_si_002.cif
_cod_data_source_block           twin5a
_cod_original_cell_volume        3523.50(15)
_cod_original_formula_sum        'C118.50 H56 N4 Ni S Sc2'
_cod_database_code               4117910