X-ray Crystallographic and EPR Spectroscopic Characterization of a Pyrrolidine Adduct of Y3N@C80
A. L. Balch; Claudia M. Cardona; Christopher J. Chancellor; Luis Echegoyen; Bevan Elliott; Marylin Olmstead; Jose Rivera; Chemical Communications  (2006) –; doi:10.1039/b604011j

data_7101237
_publ_section_title
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X-ray Crystallographic and EPR Spectroscopic
Characterization of a Pyrrolidine Adduct of Y3N@C80
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_journal_issue                   25
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b604011j
_journal_year                    2006
_chemical_formula_moiety         'Y3N@C80(CH2N(CH2CH3)CH2) . 2.5 CS2'
_chemical_formula_sum            'C86.5 H9 N2 S5 Y3'
_chemical_formula_weight         1502.99
_chemical_name_common
'Y3N@N-ethyl-3,4-fullero[80]pyrrolidine (5,6 isomer)'
_chemical_name_systematic
;
?
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.949(2)
_cell_length_b                   14.949(2)
_cell_length_c                   41.966(8)
_cell_measurement_reflns_used    7050
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.1
_cell_volume                     9378(3)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics
'XP, SHELXTL 5.1(Sheldrick, 1994), ORTEP-3 for Windows(Farrugia, 1997)'
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  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  0.1043
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            98411
_diffrn_reflns_theta_full        29.75
_diffrn_reflns_theta_max         29.75
_diffrn_reflns_theta_min         1.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.975
_exptl_absorpt_correction_T_max  0.7766
_exptl_absorpt_correction_T_min  0.3919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             5912
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.810
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         13176
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.810
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.163
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+79.5222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                10805
_reflns_number_total             13176
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b604011j.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C86.50 H9 N2 S5 Y3'
_cod_database_code               7101237