Synthesis of a Large Amino-Phenolic Cage. Synthesis, Crystal Structures, and Acid−Base and Coordination Behavior toward Cations and Anions
Ambrosi, Gianluca; Dapporto, Paolo; Formica, Mauro; Fusi, Vieri; Giorgi, Luca; Guerri, Annalisa; Micheloni, Mauro; Paoli, Paola; Pontellini, Roberto; Rossi, Patrizia; Inorganic Chemistry 45 (2006) 304–314; doi:10.1021/ic051304v

data_4331639
_publ_section_title
;
 Synthesis of a Large Amino-Phenolic Cage. Synthesis, Crystal Structures,
 and Acid&#x2212;Base and Coordination Behavior toward Cations and Anions
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              304
_journal_page_last               314
_journal_paper_doi               10.1021/ic051304v
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '(C24 H52 N8 O, 6+), 6(Cl, 1-), 11(H2 O)'
_chemical_formula_sum            'C24 H74 Cl6 N8 O12'
_chemical_formula_weight         879.61
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 117.650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.483(3)
_cell_length_b                   13.674(2)
_cell_length_c                   19.648(2)
_cell_measurement_temperature    200
_cell_volume                     4398.7(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.pre23_10 beta (release 21.06.2004 CrysAlis171 .NET)
(compiled Jun 21 2004,12:00:08)
;
_computing_molecular_graphics    'ORTEP-3 (Farruggia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir97 (Altomare, 1997)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.631
_diffrn_measured_fraction_theta_max 0.631
_diffrn_measurement_device_type  'Xcalibur Oxford Diffraction'
_diffrn_measurement_method       'intensity from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_sigmaI/netI    0.1795
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16691
_diffrn_reflns_theta_full        30.43
_diffrn_reflns_theta_max         30.43
_diffrn_reflns_theta_min         4.02
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'SADABS, Sheldrick (1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.2419
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.2548
_reflns_number_gt                3038
_reflns_number_total             8410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051304vsup1.cif
_cod_data_source_block           7
_cod_original_sg_symbol_Hall     '-P 2yab '
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4331639