Triptycene-derived N(H)-bridged azacalixarenes: synthesis, structure, and encapsulation of small neutral molecules in the solid state.
Xue, Min; Chen, Chuan-Feng; Organic letters 11 (2009) 5294–5297; doi:10.1021/ol902246c

data_1504274
_publ_section_title
;
 Triptycene-derived N(H)-bridged azacalixarenes: synthesis, structure, and
 encapsulation of small neutral molecules in the solid state.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5294
_journal_page_last               5297
_journal_paper_doi               10.1021/ol902246c
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C10 H10 Cl2 N10 O'
_chemical_formula_weight         356.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 112.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   26.903(5)
_cell_length_b                   19.366(4)
_cell_length_c                   27.680(6)
_cell_measurement_reflns_used    15988
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      1.7
_cell_volume                     13319(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_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  0.1045
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37390
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.9887
_exptl_absorpt_correction_T_min  0.9687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6096
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.551
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.813
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         11719
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.816
_refine_ls_R_factor_all          0.2723
_refine_ls_R_factor_gt           0.2099
_refine_ls_shift/su_max          0.197
_refine_ls_shift/su_mean         0.195
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5191
_refine_ls_wR_factor_ref         0.5498
_reflns_number_gt                6348
_reflns_number_total             11719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol902246c_si_003.cif
_cod_data_source_block           r081015c1
_cod_original_cell_volume        13319(5)
_cod_original_formula_sum        'C10 H10 Cl2 N10 O1'
_cod_database_code               1504274