Isolation and Structural Characterization of Two Very Large, and Largely Empty, Endohedral Fullerenes: Tm@C3v-C94and Ca@C3v-C94
Che, Yuliang; Yang, Hua; Wang, Zhimin; Jin, Hongxiao; Liu, Ziyang; Lu, Chunxin; Zuo, Tianming; Dorn, Harry C.; Beavers, Christine M.; Olmstead, Marilyn M.; Balch, Alan L.; Inorganic Chemistry 48 (2009) 6004–6010; doi:10.1021/ic900322d

data_4333511
_publ_section_title
;
 Isolation and Structural Characterization of Two Very Large, and Largely
 Empty, Endohedral Fullerenes: Tm@C3v-C94and Ca@C3v-C94
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6004
_journal_page_last               6010
_journal_paper_doi               10.1021/ic900322d
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C94 Tm, 2(C36 H44 N4 Ni), 2.5(C6 H6)'
_chemical_formula_sum            'C181 H103 N8 Ni2 Tm'
_chemical_formula_weight         2676.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.672(4)
_cell_length_b                   25.672(4)
_cell_length_c                   69.62(2)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.8
_cell_volume                     45883(17)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       '\w  and  \f'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            125844
_diffrn_reflns_theta_full        22.79
_diffrn_reflns_theta_max         22.79
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  0.9716
_exptl_absorpt_correction_T_min  0.8452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2007/4 (Shedrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             21896
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.459
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1246
_refine_ls_number_reflns         11978
_refine_ls_number_restraints     1959
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0934
_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^)+(0.1338P)^2^+756.2352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2360
_refine_ls_wR_factor_ref         0.2539
_reflns_number_gt                10015
_reflns_number_total             11978
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic900322dsup1.cif
_cod_data_source_block           cb67x
_cod_original_cell_volume        45884(17)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4333511