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_4028443
_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            'C85 H14 S2'
_chemical_formula_weight         1099.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.635(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.190(3)
_cell_length_b                   13.797(2)
_cell_length_c                   19.557(2)
_cell_measurement_reflns_used    1615
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      18.55
_cell_measurement_theta_min      2.42
_cell_volume                     4455.3(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAIAT'
_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      188(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1095
_diffrn_reflns_av_sigmaI/netI    0.1268
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25446
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.9747
_exptl_absorpt_correction_T_min  0.9503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         7864
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.2668
_refine_ls_R_factor_gt           0.1412
_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^)+(0.0352P)^2^+24.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2409
_refine_ls_wR_factor_ref         0.2877
_reflns_number_gt                3297
_reflns_number_total             7864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo4011848_si_002.cif
_cod_data_source_block           w160
_cod_original_cell_volume        4455.3(11)
_cod_database_code               4028443