"Open Rather than Closed" Malonate Methano-Fullerene Derivatives. The Formation of Methanofulleroid Adducts of Y3N@C80
Olena Lukoyanova; Claudia M. Cardona; José Rivera; Leyda Z. Lugo-Morales; Christopher J. Chancellor; Marilyn M. Olmstead; Antonio Rodríguez-Fortea; Josep M. Poblet; Alan L. Balch; Luis Echegoyen; Journal of the American Chemical Society 129 (2007) 10423–10430; doi:10.1021/ja071733n

data_4109806
_publ_section_title
;
 "Open Rather than Closed" Malonate Methano-Fullerene Derivatives. The
 Formation of Methanofulleroid Adducts of Y3N@C80
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10423
_journal_page_last               10430
_journal_paper_doi               10.1021/ja071733n
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         '(C97 H14 N O4 Y3), 0.5(C6 H6), 0.5(C H Cl3)'
_chemical_formula_sum            'C100.5 H17.5 Cl1.5 N O4 Y3'
_chemical_formula_weight         1622.56
_chemical_name_common            Y3N@C80adduct.0.5benzene.0.5chloroform
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   11.2082(11)
_cell_length_b                   17.1248(16)
_cell_length_c                   27.882(3)
_cell_measurement_reflns_used    4591
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      19.0
_cell_measurement_theta_min      3.0
_cell_volume                     5351.6(9)
_computing_cell_refinement       'SAINT v. 7.23A'
_computing_data_collection       'Apex 2'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'XP, SHELXTL 5.1(Sheldrick, 1994), ORTEP-3 for Windows(Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1515
_diffrn_reflns_av_sigmaI/netI    0.1062
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57360
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.381
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_description       needle
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.462
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.336(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         9694
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.1508
_refine_ls_R_factor_gt           0.1013
_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^)+(0.1786P)^2^+7.5887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2620
_refine_ls_wR_factor_ref         0.3006
_reflns_number_gt                6611
_reflns_number_total             9694
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja071733nsi20070312_015358.cif
_cod_data_source_block           cjc120z
_cod_original_formula_sum        'C100.50 H17.50 Cl1.50 N O4 Y3'
_cod_database_code               4109806