Reactions of C70(2-) with Organic Halides Revisited: Unusual Magnetic Equivalence for the Diastereotopic Methylene Protons in 2,5-(PhCH2)2C70
Shu-Hui Li; Zong-Jun Li; Wei-Wei Yang; Xiang Gao; Journal of Organic Chemistry 78 (2013) 7208–7215; doi:10.1021/jo4011848

data_4028446
_publ_section_title
;
 Reactions of C70(2-) with Organic Halides Revisited: Unusual Magnetic
 Equivalence for the Diastereotopic Methylene Protons in 2,5-(PhCH2)2C70
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7208
_journal_page_last               7215
_journal_paper_doi               10.1021/jo4011848
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C84.5 H12 Br2 S'
_chemical_formula_weight         1218.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.8240(10)
_cell_angle_beta                 104.7000(10)
_cell_angle_gamma                101.0710(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7742(8)
_cell_length_b                   11.1529(9)
_cell_length_c                   20.3030(16)
_cell_measurement_reflns_used    4574
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.53
_cell_volume                     2262.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12538
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  0.8326
_exptl_absorpt_correction_T_min  0.5023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.070
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         8843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0956P)^2^+2.5102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                5779
_reflns_number_total             8843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo4011848_si_005.cif
_cod_data_source_block           3br
_cod_original_formula_sum        'C84.50 H12 Br2 S'
_cod_database_code               4028446