Synthesis of Fullerene Oxides Containing Both 6,6-Closed Epoxide and 5,6-Open Ether Moieties through Thermolysis of Fullerene Peroxides
Jiayao Yao; Dazhi Yang; Zuo Xiao; Liangbing Gan; Zheming Wang; Journal of Organic Chemistry 74 (2009) 3528–3531; doi:10.1021/jo9000977

data_4024488
_publ_section_title
;
Synthesis of Fullerene Oxides Containing Both 6,6-Closed Epoxide and
5,6-Open Ether Moieties through Thermolysis of Fullerene Peroxides
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3528
_journal_page_last               3531
_journal_paper_doi               10.1021/jo9000977
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C77 H36 O10 S2'
_chemical_formula_weight         1185.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.2792(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.9125(3)
_cell_length_b                   14.3843(2)
_cell_length_c                   20.3313(4)
_cell_measurement_reflns_used    36063
_cell_measurement_temperature    200
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_volume                     5251.89(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.1119
_diffrn_reflns_av_sigmaI/netI    0.1054
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77101
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  1.022
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constraint
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         10321
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1715
_reflns_number_gt                5072
_reflns_number_total             10321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo9000977_si_002.cif
_cod_data_source_block           07feb27a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               4024488