α,ω-Alkanediyldiammonium dications sealed within calix[5]arene capsules with a hydrophobic bayonet-mount fastening
Brancatelli, Giovanna; Gattuso, Giuseppe; Geremia, Silvano; Manganaro, Nadia; Notti, Anna; Pappalardo, Sebastiano; Parisi, Melchiorre F.; Pisagatti, Ilenia; CrystEngComm 17 (2015) 7915–; doi:10.1039/C5CE01558H

data_7222366
_publ_section_title
;
 \a,\w-Alkanediyldiammonium dications sealed within calix[5]arene capsules
 with a hydrophobic bayonet-mount fastening
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              7915
_journal_paper_doi               10.1039/C5CE01558H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C94.8 H137.2 N O23.8'
_chemical_formula_weight         1852.03
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2c'
_symmetry_space_group_name_H-M   'P c a n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-25T14:20:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.92(1)
_cell_length_b                   23.62(1)
_cell_length_c                   36.17(2)
_cell_measurement_reflns_used    7517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.198
_cell_measurement_theta_min      1.426
_cell_volume                     19581(16)
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_molecular_graphics    Pymol
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution
'SIR2011, updated version of SIR2008 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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     0.9
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_laue_measured_fraction_full 0.969
_diffrn_reflns_laue_measured_fraction_max 0.969
_diffrn_reflns_number            7517
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        24.198
_diffrn_reflns_theta_max         24.198
_diffrn_reflns_theta_min         1.426
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       spearlike
_exptl_crystal_F_000             7889
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The crystal structure of the capsular complex showed
two disordered orientations for one tert-butyl group at the upper rim, that
were refined at 0.8/0.2 of partial occupancy.
The cell contained severely disordered solvent molecules with partial 
occupancy, that were not modelled but taken into account using the 
SQUEEZE/PLATON procedure. The residual electron density of 1753 electrons/cell
found in the inner space of the crystal structure (corresponding to about 
23% of the cell volume) was attributed to 35 trifluoroethanol (TFE) solvent 
molecules. Thus the 8.8  TFE molecules reported in the formula unit have 
been removed. A refinement using reflections modified by the SQUEEZE procedure 
gave good results and the R-factor was reduced from 26.2 to 17.7%. 

;
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0000173(12)
_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   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         7517
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1537
_refine_ls_R_factor_gt           0.1118
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+94.9700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2162
_reflns_Friedel_coverage         0
_reflns_number_gt                4194
_reflns_number_total             7517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01558h2.cif
_cod_data_source_block           TBU4_C10
_cod_depositor_comments
;
The following automatic conversions were performed:
'__computing_data_collection' tag replaced with
'_computing_data_collection' tag.

Automatic conversion script
Id: cif_correct_tags 3376 2015-05-07 07:48:27Z andrius 

 Adding full bibliography for 7222366--7222368.cif.
;
_cod_database_code               7222366
_audit_block_doi                 10.5517/cc13t9qy
_shelx_estimated_absorpt_t_min   0.99
_shelx_estimated_absorpt_t_max   0.999
_refinement_special_details
;The crystal structure of the capsular complex showed
 two disordered orientations for one tert-butyl group at the upper rim, that
 were refined at 0.8/0.2 of partial occupancy.
The cell contained severely disordered solvent molecules with partial 
occupancy, that were not modelled but taken into account using the 
SQUEEZE/PLATON  procedure. The residual electron density of 1753 electrons/cell
 found in the inner space of the crystal structure (corresponding to about 
23% of the cell volume) was attributed to 35 trifluoroethanol (TFE) solvent 
molecules. A refinement using reflections modified by the SQUEEZE procedure 
gave good results and the R-factor was reduced from 26.2 to 17.7%.
;
_shelx_res_checksum              74291