Frustrated Organic Solids Display Unexpected Gas Sorption
Praveen K. Thallapally; Scott J. Dalgarno; Jerry L. Atwood; Journal of the American Chemical Society 128 (2006) 15060–15061; doi:10.1021/ja065499x

data_4111149
_publ_contact_author_address
;      
   Department of Chemistry 
   University of Missouri-Columbia
   Columbia 
   MO 65211
   USA
;
_publ_contact_author_email       atwoodj@missouri.edu
_publ_contact_author_fax         '+1 (573)882 2754'
_publ_contact_author_name        'Jerry L. Atwood'
_publ_contact_author_phone       '+1 (573)882 8371'
_publ_section_title
;
 Frustrated Organic Solids Display Unexpected Gas Sorption
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15060
_journal_page_last               15061
_journal_paper_doi               10.1021/ja065499x
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C27.50 H35 O2.50'
_chemical_formula_sum            'C27.5 H35 O2.5'
_chemical_formula_weight         405.55
_chemical_name_common            'Sublimed p-tBu-calix5arene'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            8
_cell_length_a                   12.780(3)
_cell_length_b                   25.035(6)
_cell_length_c                   15.340(4)
_cell_measurement_temperature    173(2)
_cell_volume                     4908(2)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_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  0.1290
_diffrn_reflns_av_sigmaI/netI    0.1354
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12069
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9905
_exptl_absorpt_correction_T_min  0.9865
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0030(5)
_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   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1874
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+1.1978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.2005
_reflns_number_gt                1793
_reflns_number_total             3610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065499xsi20060809_072947_2.cif
_cod_data_source_block           sublimedTBC5
_cod_original_formula_sum        'C27.50 H35 O2.50'
_cod_database_code               4111149