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_1504275
_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_moiety         'C59.27 H41.16 Cl3.61 N8 O9.57'
_chemical_formula_sum            'C59.27 H41.16 Cl3.61 N8 O9.57'
_chemical_formula_weight         1146.43
_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                 102.147(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.262(4)
_cell_length_b                   27.241(4)
_cell_length_c                   16.704(3)
_cell_measurement_reflns_used    15008
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.5
_cell_volume                     10793(3)
_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      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50494
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9685
_exptl_absorpt_correction_T_min  0.9483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4725
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         12815
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1258P)^2^+7.9454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2205
_reflns_number_gt                10185
_reflns_number_total             12815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol902246c_si_004.cif
_cod_data_source_block           shelxl
_cod_database_code               1504275