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_7216448
_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 H40 O32 S8 8-) 2.5(C12 N2 H14 2+) (C2 O1 H6) (C1 O1 H4) 5,6(O1 H2) 3(o1 H3 +)'
_chemical_formula_sum            'C89 H105.2 N5 O42.6 S8'
_chemical_formula_weight         2182.90
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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            16
_cell_length_a                   26.6699(5)
_cell_length_b                   37.3628(9)
_cell_length_c                   54.356(1)
_cell_measurement_reflns_used    7379
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.85
_cell_measurement_theta_min      2.75
_cell_volume                     54163.7(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.109
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            58546
_diffrn_reflns_theta_full        20.87
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             17804.8
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.612
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         7063
_refine_ls_number_restraints     707
_refine_ls_restrained_S_all      1.558
_refine_ls_R_factor_all          0.1805
_refine_ls_R_factor_gt           0.1429
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3737
_refine_ls_wR_factor_ref         0.3943
_reflns_number_gt                5082
_reflns_number_total             7101
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3ce42303d2.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        54164(2)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'C89 H105.20 N5 O42.60 S8'
_cod_database_code               7216448