An insight into ion-transport by calixarenes; the structure of the dipotassium complex of p-tert-butylcalix[8]arene crystallised from a protogenic, coordinating solvent [ethanol/diethylcarbonate (10:1)]
Clague, Nicholas P.; Crane, Jonathan D.; Sinn, Ekkehard; Young, Nigel A.; Clegg, William; Clegg, William; Coles, Simon J.; Teat, Simon J.; Moreton, David J.; Chemical Communications  (1999) 379–; doi:10.1039/a809401b

data_7110429
_publ_section_title
;
 An insight into ion-transport by calixarenes; the structure of the
 dipotassium complex of p-tert-butylcalix[8]arene crystallised from a
 protogenic, coordinating solvent [ethanol/diethylcarbonate (10:1)]
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              379
_journal_paper_doi               10.1039/a809401b
_journal_year                    1999
_chemical_formula_sum            'C104 H148.66 K2 O16.66'
_chemical_formula_weight         1743.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.827(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.1867(3)
_cell_length_b                   12.1515(2)
_cell_length_c                   26.4092(4)
_cell_measurement_reflns_used    16470
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      1.79
_cell_volume                     4997.57(15)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68790
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            25725
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10828
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.909
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1865P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2475
_refine_ls_wR_factor_ref         0.2642
_reflns_number_gt                7613
_reflns_number_total             10828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            809401bsup1.cif
_cod_data_source_block           hull4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110429