Synthesis, Structure, and Reactions of NH-Bridged Calix[m]arene[n]pyridines
Bo Yao; De-Xian Wang; Han-Yuan Gong; Zhi-Tang Huang; Mei-Xiang Wang; Journal of Organic Chemistry 74 (2009) 5361–5368; doi:10.1021/jo900826n

data_4024696
_publ_section_title
;
Synthesis, Structure, and Reactions of NH-Bridged Calix[m]arene[n]pyridines
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5361
_journal_page_last               5368
_journal_paper_doi               10.1021/jo900826n
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C22 H18 N6'
_chemical_formula_sum            'C22 H18 N6'
_chemical_formula_weight         366.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                98.76(3)
_cell_angle_beta                 101.25(3)
_cell_angle_gamma                97.86(3)
_cell_formula_units_Z            4
_cell_length_a                   8.3972(17)
_cell_length_b                   10.175(2)
_cell_length_c                   21.221(4)
_cell_measurement_reflns_used    6720
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.99
_cell_volume                     1731.5(6)
_computing_cell_refinement       'Rapid Auto(Rigaku 2001)'
_computing_data_collection       'Rapid Auto(Rigaku 2001)'
_computing_data_reduction        'Rapid Auto(Rigaku 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku raxis Rapid IP'
_diffrn_measurement_method       oscillation
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11252
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.9639
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+1.2864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                5015
_reflns_number_total             6071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo900826n_si_002.cif
_cod_data_source_block           sx2323
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4024696