Confinement of dimeric sulfuric acid in a self-assembled molecular capsule: [(H2SO4)2⊂(calix[5]arenesulfonic acid)2]
Hardie, Michaele J.; Makha, Mohamed; Raston, Colin L.; Chemical Communications  (1999) 2409–; doi:10.1039/a907469d

data_7110717
_publ_section_title
;
 Confinement of dimeric sulfuric acid in a self-assembled molecular
 capsule: [(H2SO4)2&#x2282;(calix[5]arenesulfonic acid)2]
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2409
_journal_paper_doi               10.1039/a907469d
_journal_year                    1999
_chemical_formula_sum            'C35 H49 O37.5 S9'
_chemical_formula_weight         1358.28
_chemical_name_common            (calix[5]arene-p-sulfonicacid)(H2SO4)4(H2O)1.5
_chemical_name_systematic
;
 calix[5]arene-penta-(p-sulfonic acid) tetra-(sulfuric acid) hydrate
;
_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                105.459(1)
_cell_angle_beta                 90.871(1)
_cell_angle_gamma                105.767(1)
_cell_formula_units_Z            2
_cell_length_a                   11.7770(3)
_cell_length_b                   15.9118(4)
_cell_length_c                   16.0580(4)
_cell_measurement_temperature    123(1)
_cell_volume                     2778.69(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  CCD
_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  0.073
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57663
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.869
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.384
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         12660
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.384
_refine_ls_R_factor_all          0.1995
_refine_ls_R_factor_gt           0.1267
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_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          0.3569
_refine_ls_wR_factor_ref         0.4012
_reflns_number_gt                7156
_reflns_number_total             12660
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            907469dsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2778.68(12)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C35 H49 O37.50 S9'
_cod_database_code               7110717