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_7222368
_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            'C89.1 H128.9 F3.9 K0.1 N O16.3'
_chemical_formula_weight         1552.83
_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/cc13wm6t
_audit_creation_date             2015-09-03T13:37:17-00:00
_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                   22.509(1)
_cell_length_b                   22.972(2)
_cell_length_c                   35.249(2)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.387
_cell_measurement_theta_min      6.57
_cell_measurement_wavelength     0.8
_cell_volume                     18226(2)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_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     0.8
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            62295
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.387
_diffrn_reflns_theta_max         26.387
_diffrn_reflns_theta_min         6.57
_exptl_absorpt_coefficient_mu    0.07
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       spear-shaped
_exptl_crystal_F_000             6635
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The SQUEEZE procedure removed 10 TFE disordered solvent molecules
from the cell (namely 1.3 molecules in the asymmetric unit).

(replace by semicolon in column 1 when used as .sqf)
TITL shelx     P b c n      R = 0.21
CELL   22.5090   22.9720   35.2490     90.00     90.00     90.00
SPGR Pbcn
C101 0.797 0.017 0.867 !       2.93 eA-3
C102 0.680 0.045 0.508 !       2.59 eA-3
C103 0.750 0.535 0.882 !       2.40 eA-3
C104 0.767 0.512 0.397 !       2.07 eA-3
C105 0.202 0.478 0.139 !       2.06 eA-3
C106 0.459 0.006 0.024 !       2.06 eA-3
C107 0.408 0.031 0.000 !       1.89 eA-3
C108 0.585 0.996 0.031 !       1.87 eA-3
C109 0.858 0.471 0.982 !       1.71 eA-3
C110 0.299 0.585 0.586 !       1.70 eA-3
C111 0.248 0.916 0.102 !       1.58 eA-3
C112 0.744 0.909 0.360 !       1.56 eA-3
C113 0.431 0.922 0.490 !       1.53 eA-3
Q114 0.279 0.749 0.920 !       1.46 eA-3
C115 0.722 0.957 0.410 !       1.22 eA-3
Q116 0.711 0.906 0.432 !       0.81 eA-3
Q117 0.812 0.788 0.493 !       0.75 eA-3
Q118 0.088 0.761 0.774 !       0.74 eA-3
Q119 0.180 0.906 0.467 !       0.74 eA-3
Q120 0.743 0.307 0.967 !       0.63 eA-3
Q121 0.874 0.940 0.976 !       0.62 eA-3
Q122 0.704 0.670 0.448 !       0.61 eA-3
Q123 0.875 0.016 0.466 !       0.59 eA-3
Q124 0.482 0.499 0.115 !       0.58 eA-3
Q125 0.093 0.156 0.570 !       0.57 eA-3
Q126 0.056 0.522 0.405 !       0.56 eA-3
Q127 0.275 0.110 0.344 !       0.55 eA-3
Q128 0.938 0.778 0.320 !       0.55 eA-3
Q129 0.915 0.186 0.813 !       0.54 eA-3
Q130 0.134 0.081 0.936 !       0.53 eA-3
Q131 0.664 0.971 0.477 !       0.53 eA-3
Q132 0.264 0.625 0.855 !       0.53 eA-3
Q133 0.858 0.863 0.038 !       0.52 eA-3
Q134 0.593 0.798 0.382 !       0.52 eA-3
Q135 0.429 0.349 0.213 !       0.51 eA-3
Q136 0.166 0.258 0.518 !       0.51 eA-3
Q137 0.755 0.613 0.663 !       0.50 eA-3
Q138 0.053 0.338 0.110 !       0.50 eA-3
Q139 0.851 0.031 0.980 !       0.50 eA-3
(replace by semicolon in column 1 when used as .sqf)
;
_refine_diff_density_max         0.021
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0129(15)
_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   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         12628
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1579
_refine_ls_R_factor_gt           0.1251
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1940P)^2^+26.6113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3275
_refine_ls_wR_factor_ref         0.3592
_reflns_Friedel_coverage         0
_reflns_number_gt                8637
_reflns_number_total             12628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01558h2.cif
_cod_data_source_block           TBU4_C11
_cod_depositor_comments
'Adding full bibliography for 7222366--7222368.cif.'
_cod_original_formula_sum        'C89.1 H128.9 F3.9 K0.10 N O16.3'
_cod_database_code               7222368
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              2269
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              21184