Selective gas sorption in a [2+3] 'propeller' cage crystal
Shan Jiang; John Bacsa; Xiaofeng Wu; James T. A. Jones; Robert Dawson; Abbie Trewin; Dave J. Adams; Andrew I. Cooper; Chem.Commun. 47 (2011) 8919–; doi:10.1039/c1cc12460a

data_7106720
_publ_section_title
;
 Selective gas sorption in a [2+3] 'propeller' cage crystal
;
_journal_name_full               Chem.Commun.
_journal_page_first              8919
_journal_paper_doi               10.1039/c1cc12460a
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C138 H132 N12, 6(C H4 O)'
_chemical_formula_sum            'C144 H156 N12 O6'
_chemical_formula_weight         2150.81
_chemical_name_common            2+3cage
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            2
_cell_length_a                   26.055(4)
_cell_length_b                   15.571(2)
_cell_length_c                   14.686(2)
_cell_measurement_reflns_used    2718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.5
_cell_volume                     5958.1(14)
_computing_cell_refinement       'SAINT v6.45a (Bruker, 2005)'
_computing_data_collection       'SMART v.5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT v6.45a (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker D8 diffractometer with APEX detector'
_diffrn_measurement_method       '\w scans with a narrow frame width'
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19523
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.9963
_exptl_absorpt_correction_T_min  0.9643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008-1 (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The MeOH solvent molecules can be identified as electron density
within these voids, but these guests were only partially resolved
and too disordered to be modelled effectively. The data was
therefore treated by using PLATON/SQUEEZE[19] which calculates
six MeOH molecules per cage molecule.
;
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         10077
_refine_ls_number_restraints     439
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                6755
_reflns_number_total             10077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12460a.txt
_cod_data_source_block           sj17
_cod_original_cell_volume        5958.3(14)
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               7106720