Self-assembled octameric cage constructed by potassium salt of p-tert-butylcalix[6]arene p-bromophenylalanine derivative in solid state
Tetsuaki Tanaka; Yoichi Hiyama; Toshimasa Ishida; Naoyoshi Maezaki; Hirofumi Ohishi; Koji Tsukamoto; Chemical Communications  (2006) –; doi:10.1039/b605555a

data_7101359
_publ_section_title
;
Self-assembled octameric cage constructed by potassium
salt of p-tert-butylcalix[6]arene p-bromophenylalanine derivative in
solid state
;
_journal_issue                   34
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b605555a
_journal_year                    2006
_chemical_formula_sum            'C849 H1212 Br24 K12 N24 O219'
_chemical_formula_weight         17645.6
_chemical_name_common
;
5,11,17,23,29,35-Hexa-tert-butyl-37,39,41-
trimethoxycalix(6)arene-38,40,42-tris-oxyacetyl-N-p-bromo-L-
phenylalanine potassium salt
;
_chemical_name_systematic
;
5,11,17,23,29,35-Hexa-tert-butyl-37,39,41-
trimethoxycalix[6]arene-38,40,42-tris-oxyacetyl-
N-p-bromo-L-phenylalanine potassium salt
;
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'multiwavelength anomalous diffraction'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   43.053(43)
_cell_length_b                   43.053(43)
_cell_length_c                   44.166(44)
_cell_measurement_temperature    95(2)
_cell_volume                     70897(123)
_computing_cell_refinement       'HKL2000(Otwinowski, 1997)'
_computing_data_collection       'BSS(Beamline Scheduling Software)'
_computing_data_reduction        'HKL2000(Otwinowski, 1997)'
_computing_molecular_graphics    'Turbo Frodo'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD/E (Sheldrick, 2002)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  Si
_diffrn_radiation_source         'SPring-8 BL38B1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            60089
_diffrn_reflns_theta_full        17.56
_diffrn_reflns_theta_max         17.56
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.145
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             27108
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.036
_refine_diff_density_min         -0.029
_refine_diff_density_rms         0.003
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.078(16)
_refine_ls_extinction_coef       0.00014(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.343
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3205
_refine_ls_number_reflns         20981
_refine_ls_number_restraints     4522
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.1347
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3000
_refine_ls_wR_factor_ref         0.3053
_reflns_number_gt                18674
_reflns_number_total             20981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b605555a.txt
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7101359