Novel ion-pair receptors based on hexahomotrioxacalix[3]arene derivatives.
Ni, Xin-Long; Rahman, Shofuir; Zeng, Xi; Hughes, David L.; Redshaw, Carl; Yamato, Takehiko; Organic & biomolecular chemistry 9 (2011) 6535–6541; doi:10.1039/c1ob05564j

data_7151982
_publ_section_title
;
 Novel ion-pair receptors based on hexahomotrioxacalix[3]arene
 derivatives.
;
_journal_issue                   19
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6535
_journal_page_last               6541
_journal_paper_doi               10.1039/c1ob05564j
_journal_volume                  9
_journal_year                    2011
_chemical_formula_moiety         'C63 H66 F9 N3 O9'
_chemical_formula_structural
'calixarene (C6H2OCH2CONHC6H4CF3-2,-tBu-5,-CH2OCH2-3-)3'
_chemical_formula_sum            'C63 H66 F9 N3 O9'
_chemical_formula_weight         1180.19
_chemical_name_common            Cone-5d
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and CrysAlis RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 116.247(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3465(11)
_cell_length_b                   23.3116(18)
_cell_length_c                   17.2917(13)
_cell_measurement_temperature    293(1)
_cell_volume                     5909.9(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta
;
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(1)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42557
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'large, beautiful, colourless'
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.73
_exptl_crystal_size_min          0.51
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         16356
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+1.8626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                11023
_reflns_number_total             16356
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c1ob05564j.txt
_cod_data_source_block           carlr6
_cod_original_cell_volume        5909.8(8)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7151982