Reactivity differences of Sc3N at C2n (2n = 68 and 80). Synthesis of the first methanofullerene derivatives of Sc3N at D5h-C80
Maira R. Ceron; Marta Izquierdo; Nuria Alegret; Juan A. Valdez; Antonio Rodriguez-Fortea; Marilyn M. Olmstead; Alan L. Balch; Josep M. Poblet; Luis Echegoyen; Chem.Commun. 52 (2016) 64–; doi:10.1039/C5cc07416A

data_7118165
_publ_section_title
;
 Reactivity differences of Sc3N at C2n (2n = 68 and 80). Synthesis of the
 first methanofullerene derivatives of Sc3N at D5h-C80
;
_journal_name_full               Chem.Commun.
_journal_page_first              64
_journal_paper_doi               10.1039/C5cc07416A
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C92 H14 N O2 Sc3, C S2'
_chemical_formula_sum            'C93 H14 N O2 S2 Sc3'
_chemical_formula_weight         1376.05
_chemical_name_systematic        'PCBM-Sc3N@D5h-C80 CS2 solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-08-28 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9441(6)
_cell_length_b                   15.7417(6)
_cell_length_c                   14.9924(4)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.6
_cell_volume                     4706.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with ApexII detector'
_diffrn_measurement_method       '\w/\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            64302
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         27.820
_diffrn_reflns_theta_min         1.797
_diffrn_source                   'ALS Beamline 11.3.1'
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       plate
_exptl_crystal_F_000             2760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: carbon disulfide, chloroform, hexanes'
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.021
_refine_diff_density_max         3.500
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.314
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.22(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         8566
_refine_ls_number_restraints     715
_refine_ls_restrained_S_all      2.012
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.1649
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3903
_refine_ls_wR_factor_ref         0.4000
_reflns_Friedel_coverage         0.921
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                7646
_reflns_number_total             8566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc07416a2.cif
_cod_data_source_block           mn2142
_cod_database_code               7118165
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              59425