Conformation perturbation of p-sulfonatocalix[5]arene via complexation of 1,4-diazabicyclo[2.2.2]octane.
Dalgarno, Scott J; Hardie, Michaele J; Raston, Colin L; Chemical communications (Cambridge, England)  (2004) 2802–2803; doi:10.1039/b410242h

data_7102740
_publ_section_title
;
 Conformation perturbation of p-sulfonatocalix[5]arene via complexation
 of 1,4-diazabicyclo[2.2.2]octane.
;
_journal_issue                   24
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2802
_journal_page_last               2803
_journal_paper_doi               10.1039/b410242h
_journal_year                    2004
_chemical_formula_sum            'C50 H74.5 N5 O29.25 S5'
_chemical_formula_weight         1373.95
_chemical_name_common
'[{(DABCO+2H+)} (p-sulfonatocalix[5]arene+H+)][DABCO+2H+].H2O9.25'
_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                85.7950(10)
_cell_angle_beta                 79.5540(10)
_cell_angle_gamma                74.4390(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7511(2)
_cell_length_b                   15.9188(3)
_cell_length_c                   16.7800(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3225.72(11)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
XSeed (Barbour, 2001)
;
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
Detector set at 30mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;
_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  0.0941
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            68394
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.955
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.0025(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.751
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         14404
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.756
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2649
_refine_ls_wR_factor_ref         0.2862
_reflns_number_gt                9211
_reflns_number_total             14404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b410242h.txt
_cod_data_source_block           dabcocalix5
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C50 H74.50 N5 O29.25 S5'
_cod_database_code               7102740