Synthesis of open-cage ketolactam derivatives of fullerene c60 encapsulating a hydrogen molecule.
Hashikawa, Yoshifumi; Murata, Michihisa; Wakamiya, Atsushi; Murata, Yasujiro; Organic letters 16 (2014) 2970–2973; doi:10.1021/ol501113y

data_1516114
_publ_section_title
;
 Synthesis of open-cage ketolactam derivatives of fullerene c60
 encapsulating a hydrogen molecule.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2970
_journal_page_last               2973
_journal_paper_doi               10.1021/ol501113y
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C72 H23 N O8'
_chemical_formula_weight         1029.91
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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-2013
_cell_angle_alpha                85.270(5)
_cell_angle_beta                 77.477(5)
_cell_angle_gamma                78.869(5)
_cell_formula_units_Z            2
_cell_length_a                   10.128(5)
_cell_length_b                   10.497(5)
_cell_length_c                   20.664(5)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.88
_cell_volume                     2102.4(15)
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70926
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15546
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.186
_diffrn_reflns_theta_max         25.002
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         6906
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1883
_refine_ls_R_factor_gt           0.1784
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+52.3720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4210
_refine_ls_wR_factor_ref         0.4281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6103
_reflns_number_total             6906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol501113y_si_002.cif
_cod_data_source_block           ketolac1
_cod_depositor_comments          'Adding full bibliography for 1516114.cif.'
_cod_database_code               1516114
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2013-3
_shelx_res_checksum              8525
_shelx_hkl_checksum              14468