[2 + 2] Cycloaddition Reaction to Sc3N@Ih-C80. The Formation of Very Stable [5,6]- and [6,6]-Adducts
Fang-Fang Li; Julio R. Pinzón; Brandon Q. Mercado; Marilyn M. Olmstead; Alan L. Balch; Luis Echegoyen; Journal of the American Chemical Society 133 (2011) 1563–1571; doi:10.1021/ja1097176

data_4105600
_publ_section_title
;
 [2 + 2] Cycloaddition Reaction to Sc3N@Ih-C80. The Formation of Very
 Stable [5,6]- and [6,6]-Adducts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1563
_journal_page_last               1571
_journal_paper_doi               10.1021/ja1097176
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C86 H4 N Sc3, 2(C S2)'
_chemical_formula_sum            'C88 H4 N S4 Sc3'
_chemical_formula_weight         1338.04
_chemical_name_common
"Sc3N@l,2-fullero[80(Ih)]benzyne (5,6 isomer) carbon disulfide disolvate' "
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   19.6998(6)
_cell_length_b                   14.7348(5)
_cell_length_c                   15.5859(5)
_cell_measurement_reflns_used    10896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.07
_cell_measurement_theta_min      3.06
_cell_volume                     4524.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            90812
_diffrn_reflns_theta_full        40.07
_diffrn_reflns_theta_max         40.07
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.9214
_exptl_absorpt_correction_T_min  0.8035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.565
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         10896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0662
_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^)+(0.1237P)^2^+4.1815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2011
_reflns_number_gt                9978
_reflns_number_total             10896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1097176_si_001.cif
_cod_data_source_block           bqm62
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4105600