Tri-substituted hexahomotrioxacalix[3]arene derivatives bearing imidazole units: synthesis and extraction properties for cations and chromate anions.
Ni, Xin-Long; Jin, Cheng-Cheng; Jiang, Xue-Kai; Takimoto, Masashi; Rahman, Shofiur; Zeng, Xi; Hughes, David L.; Redshaw, Carl; Yamato, Takehiko; Organic & biomolecular chemistry 11 (2013) 5435–5442; doi:10.1039/c3ob40601f

data_7153008
_publ_section_title
;
 Tri-substituted hexahomotrioxacalix[3]arene derivatives bearing imidazole
 units: synthesis and extraction properties for cations and chromate
 anions.
;
_journal_issue                   33
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5435
_journal_page_last               5442
_journal_paper_doi               10.1039/c3ob40601f
_journal_volume                  11
_journal_year                    2013
_chemical_formula_moiety         'C51 H66 N6 O6, H2 O'
_chemical_formula_structural
{CH2C6H2OCH2(cyclo-C3N2H2Me)-2,-tBu-5,CH2O-3-}3.H2O
_chemical_formula_sum            'C51 H68 N6 O7'
_chemical_formula_weight         877.11
_chemical_name_common            'Compound partial-cone-2'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 100.908(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.7295(17)
_cell_length_b                   12.6213(4)
_cell_length_c                   37.718(3)
_cell_measurement_temperature    140(2)
_cell_volume                     9690.0(12)
_computing_cell_refinement
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta 
;
_computing_data_collection
;
 CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p5 beta 
;
_computing_data_reduction
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta 
;
_computing_molecular_graphics    'ORTEP (Johnson, 1976 and Farrugia, 2012)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 2008) and WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(1)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0883
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            76163
_diffrn_reflns_theta_full        22.55
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         4.18
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.05
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         12630
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                7989
_reflns_number_total             12630
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c3ob40601f.txt
_cod_data_source_block           cr3b
_cod_original_cell_volume        9690.0(11)
_cod_original_sg_symbol_H-M      'P 2(1)/a'
_cod_database_code               7153008