New egg-shaped fullerenes: non-isolated pentagon structures of Tm3N@C(s)(51 365)-C84 and Gd3N@C(s)(51 365)-C84.
Zuo, Tianming; Walker, Kenneth; Olmstead, Marilyn M.; Melin, Frederic; Holloway, Brian C.; Echegoyen, Luis; Dorn, Harry C.; Chaur, Manuel N.; Chancellor, Christopher J.; Beavers, Christine M.; Balch, Alan L.; Athans, Andreas J.; Chemical communications (Cambridge, England)  (2008) 1067–1069; doi:10.1039/b716037b

data_7113143
_publ_section_title
;
 New egg-shaped fullerenes: non-isolated pentagon structures of
 Tm3N@C(s)(51 365)-C84 and Gd3N@C(s)(51 365)-C84.
;
_journal_issue                   9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1067
_journal_page_last               1069
_journal_paper_doi               10.1039/b716037b
_journal_year                    2008
_chemical_formula_moiety         'C84 N Tm3, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C132 H56 N5 Ni Tm3'
_chemical_formula_weight         2277.32
_chemical_name_common
;
(mu !3$-Nitrido)-eta $6!, eta$4!,eta$5!-C84 Fullerene)-
trithulium (2,3,7,8,12,13,17,18-octaethylporphyrinato)nickel(ii)
benzene disolvate
;
_chemical_name_systematic
;
(\m ~3~-Nitrido)-\h ^6^, \h^4^,\h^5^-C84 Fullerene)-trithulium
(2,3,7,8,12,13,17,18-octaethylporphyrinato)nickel(II) benzene disolvate
;
_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
_cell_angle_alpha                85.178(2)
_cell_angle_beta                 89.457(2)
_cell_angle_gamma                62.276(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6305(7)
_cell_length_b                   15.0074(7)
_cell_length_c                   19.8162(9)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      2.7
_cell_volume                     3835.7(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_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            49412
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    3.750
_exptl_absorpt_correction_T_max  0.8063
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Bruker-AXS, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.891
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         17563
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1097P)^2^+20.8469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.1953
_reflns_number_gt                13851
_reflns_number_total             17563
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b716037b.txt
_cod_data_source_block           cb58a
_cod_database_code               7113143