[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_4105601
_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 (6,6 isomer) carbon disulfide disolvate'
_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                   14.7764(4)
_cell_length_b                   15.6777(5)
_cell_length_c                   19.5438(6)
_cell_measurement_reflns_used    179095
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.85
_cell_measurement_theta_min      1.88
_cell_volume                     4527.5(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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           syncrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            216696
_diffrn_reflns_theta_full        50.80
_diffrn_reflns_theta_max         50.80
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.8913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_description       plate
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.488
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         37767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+1.3317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                36408
_reflns_number_total             37767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1097176_si_002.cif
_cod_data_source_block           bqm63
_cod_depositor_comments
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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 
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_cod_database_code               4105601