KF and CsF Recognition and Extraction by a Calix[4]crown-5 Strapped Calix[4]pyrrole Multitopic Receptor
Sung Kuk Kim; Vincent M. Lynch; Neil J. Young; Benjamin P. Hay; Chang-Hee Lee; Jong Seung Kim; Bruce A. Moyer; Jonathan L. Sessler; Journal of the American Chemical Society 134 (2012) 20837–20843; doi:10.1021/ja310673p

data_4119057
_publ_section_title
;
 KF and CsF Recognition and Extraction by a Calix[4]crown-5 Strapped
 Calix[4]pyrrole Multitopic Receptor
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20837
_journal_page_last               20843
_journal_paper_doi               10.1021/ja310673p
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety
'C78 H82 N4 O9, Cs 1+, F 1-, 2 C H4 O, 2 C H Cl3'
_chemical_formula_sum            'C82 H92 Cl6 Cs F N4 O11'
_chemical_formula_weight         1674.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   20.6930(13)
_cell_length_b                   26.3422(16)
_cell_length_c                   28.8106(16)
_cell_measurement_reflns_used    98460
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.0
_cell_volume                     15704.6(16)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1549
_diffrn_reflns_av_sigmaI/netI    0.1335
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            94734
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001).  The Rigaku Corporation, Tokyo Japan.
;
_exptl_crystal_colour            needle
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       colorless
_exptl_crystal_F_000             6928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         13811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.1695
_refine_ls_R_factor_gt           0.0917
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+1.4865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1926
_reflns_number_gt                7175
_reflns_number_total             13811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja310673p_si_003.cif
_cod_data_source_block           shelxl
_cod_database_code               4119057