Expansion of Orifices of Open C60 Derivatives and Formation of an Open C59S Derivative by Reaction with Sulfur.
Futagoishi, Tsukasa; Murata, Michihisa; Wakamiya, Atsushi; Sasamori, Takahiro; Murata, Yasujiro; Organic letters 15 (2013) 2750–2753; doi:10.1021/ol401083c

data_1512094
_publ_section_title
;
 Expansion of Orifices of Open C60 Derivatives and Formation of an Open
 C59S Derivative by Reaction with Sulfur.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2750
_journal_page_last               2753
_journal_paper_doi               10.1021/ol401083c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C112 H61.04 N4.96 Ni0.5 O4.52 S2'
_chemical_formula_weight         1641.93
_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                 102.629(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.122(2)
_cell_length_b                   14.8245(19)
_cell_length_c                   31.170(4)
_cell_measurement_temperature    100(2)
_cell_volume                     7720.3(17)
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker SMART APAX'
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0784
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            30733
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.9390
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         13137
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0846P)^2^+1.2712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                8920
_reflns_number_total             13137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol401083c_si_002.cif
_cod_data_source_block           18SS
_cod_original_cell_volume        7720.4(18)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C112 H61.04 N4.96 Ni0.50 O4.52 S2'
_cod_database_code               1512094