Preparation and Structural Characterization of the Ih and the D5h Isomers of the Endohedral Fullerenes Tm3N@C80: Icosahedral C80 Cage Encapsulation of a Trimetallic Nitride Magnetic Cluster with Three Uncoupled Tm3+ Ions
Tianming Zuo; Marilyn M. Olmstead; Christine M. Beavers; Alan L. Balch; Guangbin Wang; Gordon T. Yee; Chunying Shu; Liaosa Xu; Bevan Elliott; Luis Echegoyen; James C. Duchamp; Harry C. Dorn; Inorganic Chemistry 47 (2008) 5234–5244; doi:10.1021/ic800227x

data_4305038
_publ_section_title
;
Preparation and Structural Characterization of the Ih and the D5h Isomers of
the Endohedral Fullerenes Tm3N@C80: Icosahedral C80 Cage Encapsulation of a
Trimetallic Nitride Magnetic Cluster with Three Uncoupled Tm3+ Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5234
_journal_page_last               5244
_journal_paper_doi               10.1021/ic800227x
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C80 N Tm3, C36 H44 N4 Ni, C6 H6, 2(C3 H3)'
_chemical_formula_sum            'C128 H56 N5 Ni Tm3'
_chemical_formula_weight         2229.28
_chemical_name_systematic
;
(\m~3~-Nitrido)-\h^12^,\h^12^, \h^9^-C80-Fullerene)-trithulim
(2,3,7,8,12,13,17,18-octaethylporphyrinato)nickel(II) benzene disolvate
;
_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                 95.483(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2777(5)
_cell_length_b                   15.0945(3)
_cell_length_c                   19.6748(4)
_cell_measurement_reflns_used    7018
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.5
_cell_volume                     7472.7(3)
_computing_cell_refinement       'SAINT 7.16 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker 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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42936
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.847
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.124
_refine_diff_density_min         -1.514
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8913
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0789P)^2^+80.5466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                7470
_reflns_number_total             8913
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic800227x-file002_2.cif
_cod_data_source_block           cb22
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4305038