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_4331640
_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 H45 N8 O -1), 2(Zn, +2), 3(Cl O4, -1)'
_chemical_formula_sum            'C12 H22.5 Cl1.5 N4 O6.5 Zn'
_chemical_formula_weight         445.38
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   15.252(2)
_cell_length_b                   15.419(3)
_cell_length_c                   14.605(3)
_cell_measurement_temperature    298
_cell_volume                     3434.7(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      298
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.802
_diffrn_measured_fraction_theta_max 0.802
_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  0.0748
_diffrn_reflns_av_sigmaI/netI    0.1438
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17138
_diffrn_reflns_theta_full        32.54
_diffrn_reflns_theta_max         32.54
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'SADABS, Sheldrick (1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.2095
_refine_ls_R_factor_gt           0.0896
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                2438
_reflns_number_total             5001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051304vsup1.cif
_cod_data_source_block           8
_cod_original_sg_symbol_Hall     '-P 2n 2ab '
_cod_original_formula_sum        'C12 H22.50 Cl1.50 N4 O6.50 Zn'
_cod_database_code               4331640