Encapsulation of biogenic polyamines by carboxylcalix[5]arenes: when solid-state design beats recognition in solution
Brancatelli, Giovanna; Gattuso, Giuseppe; Geremia, Silvano; Manganaro, Nadia; Notti, Anna; Pappalardo, Sebastiano; Parisi, Melchiorre F.; Pisagatti, Ilenia; CrystEngComm 18 (2016) 5012–; doi:10.1039/C6CE00468G

data_7224923
_publ_section_title
;
 Encapsulation of biogenic polyamines by carboxylcalix[5]arenes: when
 solid-state design beats recognition in solution
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              5012
_journal_paper_doi               10.1039/C6CE00468G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C86 H133 N2 O7'
_chemical_formula_weight         1306.94
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1kr07k
_audit_creation_date             2016-02-21T20:58:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-02-22 deposited with the CCDC.
2016-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.450(10)
_cell_length_b                   23.020(10)
_cell_length_c                   32.88(2)
_cell_measurement_reflns_used    16955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      6.253
_cell_measurement_theta_min      24.057
_cell_volume                     17749(15)
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_molecular_graphics    Pymol
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'SIR2011, updated version of SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_wavelength     0.6525
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_number            16955
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        23.048
_diffrn_reflns_theta_max         24.057
_diffrn_reflns_theta_min         6.253
_exptl_absorpt_coefficient_mu    0.051
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5752
_exptl_crystal_recrystallization_method
'slow evaporation af a CHCl3/Trifluoroethanol solvent mixture'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         16955
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.1128
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1656P)^2^+12.5733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3043
_refine_ls_wR_factor_ref         0.3384
_reflns_Friedel_coverage         0
_reflns_number_gt                13065
_reflns_number_total             16955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00468g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7224922--7224923.cif.'
_cod_database_code               7224923
_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              37760
_shelx_fab_checksum              20944