Synthesis of homoazafullerene [C59N(CH2)]R and azahomoazafullerene [C59N(NH)]R
Xu, Dan; Li, Yanbang; Lou, Ning; Gan, Liangbing; Organic Chemistry Frontiers 4 (2017) 750–; doi:10.1039/C7QO00098G

data_1553737
_publ_section_title
;
 Synthesis of homoazafullerene [C59N(CH2)]R and azahomoazafullerene
 [C59N(NH)]R
;
_journal_issue                   5
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              750
_journal_paper_doi               10.1039/C7QO00098G
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C76 H39 N O9'
_chemical_formula_weight         1110.08
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-12-14 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.489(4)
_cell_length_b                   10.179(2)
_cell_length_c                   22.215(4)
_cell_measurement_reflns_used    300
_cell_measurement_temperature    100
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     4859.2(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  synchrotron
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27095
_diffrn_reflns_theta_full        31.26
_diffrn_reflns_theta_max         31.26
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.100
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2.6(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         14273
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+2.1081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                11323
_reflns_number_total             14273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qo00098g2.cif
_cod_data_source_block           test31
_cod_original_cell_volume        4859.2(17)
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               1553737