Selective Synthesis of Fullerenol Derivatives with Terminal Alkyne and Crown Ether Addends
Huan Huang; Gang Zhang; Sisi Liang; Nana Xin; Liangbing Gan; Journal of Organic Chemistry 77 (2012) 2456–2462; doi:10.1021/jo300118h

data_4027054
_publ_section_title
;
 Selective Synthesis of Fullerenol Derivatives with Terminal Alkyne and
 Crown Ether Addends
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2456
_journal_page_last               2462
_journal_paper_doi               10.1021/jo300118h
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         '4(C71 H30 O10), 2(C7 H8), C S2'
_chemical_formula_sum            'C299 H136 O40 S2'
_chemical_formula_weight         4432.20
_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                88.480(5)
_cell_angle_beta                 73.520(4)
_cell_angle_gamma                82.880(5)
_cell_formula_units_Z            1
_cell_length_a                   14.809(2)
_cell_length_b                   17.264(3)
_cell_length_c                   19.650(4)
_cell_measurement_reflns_used    879
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.17
_cell_volume                     4780.0(14)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49375
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.9558
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       plate
_exptl_crystal_F_000             2282
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1557
_refine_ls_number_reflns         16833
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.1298
_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^)+(0.1818P)^2^+17.3007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3344
_refine_ls_wR_factor_ref         0.3468
_reflns_number_gt                15013
_reflns_number_total             16833
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo300118h_si_002.cif
_cod_data_source_block           sa424
_cod_database_code               4027054