Encapsulation of Et3N±-H···OH2 in a hydrogen-bonded resorcarene capsule
Shivanyuk, Alexander; Rissanen, Kari; Kolehmainen, Erkki; Chemical Communications  (2000) 1107–; doi:10.1039/b002144j

data_7110932
_publ_section_title
;
 Encapsulation of Et3N+--H&#x00B7;&#x00B7;&#x00B7;OH2 in a hydrogen-bonded
 resorcarene capsule
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1107
_journal_paper_doi               10.1039/b002144j
_journal_year                    2000
_chemical_formula_moiety         'C78 H80 Br N O31.63'
_chemical_formula_sum            'C78 H80 Br N O31.63'
_chemical_formula_weight         1617.34
_chemical_name_common            resorcarene
_chemical_name_systematic
;
 4,6,10,12,16,18,22,24-Octahydroxy-2,8,14,20-(tetraethyl)calix[4]arene
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.2620(5)
_cell_length_b                   20.2620(5)
_cell_length_c                   43.1040(7)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      3.00
_cell_volume                     17696.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Kappa CCD'
_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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            58029
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             6744
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         7537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+28.1045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1800
_reflns_number_gt                5042
_reflns_number_total             7537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002144jsup1.cif
_cod_data_source_block           als5a
_cod_original_sg_symbol_H-M      I41/a
_cod_database_code               7110932