Synthesis and Functionalization of Heteroatom-Bridged Bicyclocalixaromatics, Large Molecular Triangular Prisms with Electron-Rich and -Deficient Aromatic Interiors
Muhammad Moazzam Naseer; De-Xian Wang; Liang Zhao; Zhi-Tang Huang; Mei-Xiang Wang; Journal of Organic Chemistry 76 (2011) 1804–1813; doi:10.1021/jo102483x

data_4026135
_publ_section_title
;
 Synthesis and Functionalization of Heteroatom-Bridged
 Bicyclocalixaromatics, Large Molecular Triangular Prisms with
 Electron-Rich and -Deficient Aromatic Interiors
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1804
_journal_page_last               1813
_journal_paper_doi               10.1021/jo102483x
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C69 H60 N12 O6'
_chemical_formula_weight         1153.29
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 117.468(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.845(5)
_cell_length_b                   13.192(3)
_cell_length_c                   19.392(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4277.4(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10189
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.9924
_exptl_absorpt_correction_T_min  0.9877
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.895
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
;
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         10189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1064P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                7256
_reflns_number_total             10189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo102483x_si_002.cif
_cod_data_source_block           mx17c
_cod_original_cell_volume        4277.6(18)
_cod_database_code               4026135