Synthesis of large macrocyclic azacalix[n]pyridines (n = 6 - 9) and their complexation with fullerenes C(60) and C(70).
Zhang, En-Xuan; Wang, De-Xian; Zheng, Qi-Yu; Wang, Mei-Xiang; Organic letters 10 (2008) 2565–2568; doi:10.1021/ol800840m

data_1504710
_publ_section_title
;
 Synthesis of large macrocyclic azacalix[n]pyridines (n = 6 - 9) and their
 complexation with fullerenes C(60) and C(70).
;
_journal_issue                   12
_journal_name_full               'Organic letters'
_journal_page_first              2565
_journal_page_last               2568
_journal_paper_doi               10.1021/ol800840m
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C28 H28 N9.33'
_chemical_formula_sum            'C28 H28 N9.33'
_chemical_formula_weight         495.26
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   27.601(6)
_cell_length_b                   15.053(3)
_cell_length_c                   9.1793(18)
_cell_measurement_temperature    293(2)
_cell_volume                     3813.8(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7012
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.9694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3759
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2093
_refine_ls_wR_factor_ref         0.2369
_reflns_number_gt                2261
_reflns_number_total             3759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol800840m-file003.cif
_cod_data_source_block           2117
_cod_original_cell_volume        3813.9(13)
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               1504710