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_4333512
_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 Ca, C36 H44 N4 Ni, 2(C7 H8)'
_chemical_formula_sum            'C144 H60 Ca N4 Ni'
_chemical_formula_weight         1944.75
_chemical_name_common            Ca@C94.NiOEP.2toluene
_chemical_name_systematic
; 
 ? 
;
_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                 96.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.740(5)
_cell_length_b                   15.106(3)
_cell_length_c                   21.320(4)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      32.6
_cell_measurement_theta_min      2.7
_cell_volume                     8232(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'Apex2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL v. 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      91(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 SMART 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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            56378
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.108
_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     859
_refine_ls_number_reflns         12968
_refine_ls_number_restraints     2006
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0824
_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^)+(0.1415P)^2^+27.2454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2523
_reflns_number_gt                10427
_reflns_number_total             12968
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic900322dsup1.cif
_cod_data_source_block           mn1872
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4333512