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_4324914
_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            'C104.5 H10.63 F48 N Sc3'
_chemical_formula_weight         2326.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   nodef
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.718(3)
_cell_length_b                   15.0190(10)
_cell_length_c                   38.040(4)
_cell_measurement_reflns_used    25000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     17528(3)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.744
_diffrn_measured_fraction_theta_max 0.604
_diffrn_measurement_device_type  MAR225
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  Cu(113)
_diffrn_radiation_source         'BL14.2, PSF, BESSY, Berlin, Germany'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.90500
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            111806
_diffrn_reflns_theta_full        32.60
_diffrn_reflns_theta_max         35.67
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       plate
_exptl_crystal_F_000             9117
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.00247(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2734
_refine_ls_number_reflns         23729
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.2050
_refine_ls_R_factor_gt           0.1791
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+600.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3935
_refine_ls_wR_factor_ref         0.4029
_reflns_number_gt                18167
_reflns_number_total             23729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200174u_si_002_5.cif
_cod_data_source_block           16-IIxyl
_cod_original_formula_sum        'C104.50 H10.63 F48 N Sc3'
_cod_database_code               4324914