Poly(perfluoroalkylation) of Metallic Nitride Fullerenes Reveals Addition-Pattern Guidelines: Synthesis and Characterization of a Family of Sc3N@C80(CF3)n (n = 2-16) and Their Radical Anions
Natalia B. Shustova; Dmitry V. Peryshkov; Igor V. Kuvychko; Yu-Sheng Chen; Mary A. Mackey; Curtis E. Coumbe; David T. Heaps; Bridget S. Confait; Thomas Heine; J. Paige Phillips; Steven Stevenson; Lothar Dunsch; Alexey A. Popov; Steven H. Strauss; Olga V. Boltalina; Journal of the American Chemical Society 133 (2011) 2672–2690; doi:10.1021/ja109462j

data_4105677
_publ_contact_author_address
; Department of Chemistry
  Colorado State University
  Fort Collins, Colorado 80523
  USA
;
_publ_contact_author_email       ovbolt@lamar.colostate.edu'
_publ_contact_author_fax         970-491-1801
_publ_contact_author_name        'Olga V. Boltalina'
_publ_contact_author_phone       970-491-5088
_publ_section_title
;
 Poly(perfluoroalkylation) of Metallic Nitride Fullerenes Reveals
 Addition-Pattern Guidelines: Synthesis and Characterization of a Family
 of Sc3N@C80(CF3)n (n = 2-16) and Their Radical Anions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2672
_journal_page_last               2690
_journal_paper_doi               10.1021/ja109462j
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C90 F30 N Sc3, 1.5(C8 H10)'
_chemical_formula_sum            'C102 H15 F30 N Sc3'
_chemical_formula_weight         1959.03
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2010-09-20 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.696(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2149(15)
_cell_length_b                   20.0393(15)
_cell_length_c                   24.432(3)
_cell_measurement_reflns_used    9396
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      15.52
_cell_measurement_theta_min      2.20
_cell_volume                     6438.1(12)
_computing_cell_refinement       'APEX II v.2.2 (Bruker, 2007)'
_computing_data_collection       'APEX II v.2.2 (Bruker, 2007)'
_computing_data_reduction        'APEX II v.2.2 (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXTL, v. 6.14, Bruker AXS'
_computing_structure_solution    'SHELXTL, v. 6.14, Bruker AXS'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'diamond 1 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1212
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            135825
_diffrn_reflns_theta_full        14.84
_diffrn_reflns_theta_max         14.84
_diffrn_reflns_theta_min         0.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.9989
_exptl_absorpt_correction_T_min  0.9894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, v. 2.10, Bruker AXS, Madison, WI'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             3868
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1316
_refine_ls_number_reflns         12625
_refine_ls_number_restraints     996
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+25.0693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                8634
_reflns_number_total             12625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109462j_si_001.cif
_cod_data_source_block           c
_cod_original_cell_volume        6438.1(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4105677