Synthesis, Isolation, and Addition Patterns of Trifluoromethylated D5h and Ih Isomers of Sc3N@C80: Sc3N@D5h-C80(CF3)18 and Sc3N@Ih-C80(CF3)14
Shangfeng Yang; Chuanbao Chen; Mingzhi Jiao; Nadezhda B. Tamm; Maria A. Lanskikh; Erhard Kemnitz; Sergey I. Troyanov; Inorganic Chemistry 50 (2011) 3766–3771; doi:10.1021/ic200174u

data_4324915
_publ_contact_author
;
    Prof. S. I. Troyanov
    Chemistry Department
    Moscow State University
    Leninskie Gory
    119991 Moscow
    Russia
;
_publ_contact_author_email       stroyano@thermo.chem.msu.ru
_publ_contact_author_fax         '+007 095 9391240'
_publ_contact_author_phone       '+007 095 9395396'
_publ_section_title
;
 Synthesis, Isolation, and Addition Patterns of Trifluoromethylated D5h
 and Ih Isomers of Sc3N@C80: Sc3N@D5h-C80(CF3)18 and Sc3N@Ih-C80(CF3)14
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3766
_journal_page_last               3771
_journal_paper_doi               10.1021/ic200174u
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C103.23 H5.97 F54 N Sc3'
_chemical_formula_weight         2420.70
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.530(10)
_cell_angle_beta                 72.120(10)
_cell_angle_gamma                76.200(10)
_cell_formula_units_Z            2
_cell_length_a                   13.5620(10)
_cell_length_b                   14.6340(10)
_cell_length_c                   21.6720(10)
_cell_measurement_temperature    100(2)
_cell_volume                     3974.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.590
_diffrn_measured_fraction_theta_max 0.456
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.90500
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_sigmaI/netI    0.1320
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23499
_diffrn_reflns_theta_full        32.60
_diffrn_reflns_theta_max         36.47
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_correction_T_min  0.9828
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_F_000             2363
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         8595
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.2906
_refine_ls_R_factor_gt           0.2116
_refine_ls_shift/su_max          0.994
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4736
_refine_ls_wR_factor_ref         0.4944
_reflns_number_gt                4731
_reflns_number_total             8595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200174u_si_002_6.cif
_cod_data_source_block           18D5h-I
_cod_original_cell_volume        3974.9(4)
_cod_database_code               4324915