Structural characterization of inclusion complexes of para-sulphonato-calix[8]arene with 1,2-bis(4-pyridyl)-ethane and 1,3-bis(4-pyridyl)-propane. New ‘double cone’ and ‘up‒flat‒down’ conformations of para-sulphonato-calix[8]arene
Lesniewska, B.; Perret, F.; Suwinska, K.; Coleman, A. W.; CrystEngComm 16 (2014) 4399–; doi:10.1039/c3ce42303d

data_7216449
_publ_section_title
;
 Structural characterization of inclusion complexes of
 para-sulphonato-calix[8]arene with 1,2-bis(4-pyridyl)-ethane and
 1,3-bis(4-pyridyl)-propane. New &#x2018;double cone&#x2019; and
 &#x2018;up--flat--down&#x2019; conformations of
 para-sulphonato-calix[8]arene
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              4399
_journal_paper_doi               10.1039/c3ce42303d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'(C56 H38 O32 S8 10-) 5(C13 N2 H16 2+) 29(H2 O1)'
_chemical_formula_sum            'C121 H176 N10 O61 S8'
_chemical_formula_weight         3002.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.790(2)
_cell_angle_beta                 90.699(1)
_cell_angle_gamma                107.796(4)
_cell_formula_units_Z            2
_cell_length_a                   14.6443(4)
_cell_length_b                   19.4468(6)
_cell_length_c                   26.594(1)
_cell_measurement_reflns_used    19695
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.82
_cell_measurement_theta_min      2.75
_cell_volume                     7089.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaApexII
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.178
_diffrn_reflns_av_sigmaI/netI    0.0809
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            67445
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.915
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2464
_refine_ls_number_reflns         18369
_refine_ls_number_restraints     2218
_refine_ls_restrained_S_all      1.919
_refine_ls_R_factor_all          0.1756
_refine_ls_R_factor_gt           0.1094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1649P)^2^+42.6200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2716
_refine_ls_wR_factor_ref         0.3107
_reflns_number_gt                16723
_reflns_number_total             18431
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3ce42303d2.cif
_cod_data_source_block           sc8_nab_52
_cod_database_code               7216449