Spontaneous and selective CO2 sorption under ambient conditions in seemingly nonporous molecular crystal of azacalix[5]arene pentamethyl ether.
Tsue, Hirohito; Ono, Kohei; Tokita, Satoshi; Ishibashi, Koichi; Matsui, Kazuhiro; Takahashi, Hiroki; Miyata, Kazuyuki; Takahashi, Daisuke; Tamura, Rui; Organic letters 13 (2011) 490–493; doi:10.1021/ol102829h

data_1501918
_publ_section_title
;
 Spontaneous and selective CO2 sorption under ambient conditions in
 seemingly nonporous molecular crystal of azacalix[5]arene pentamethyl
 ether.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              490
_journal_page_last               493
_journal_paper_doi               10.1021/ol102829h
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C44 H60 N4 O4'
_chemical_formula_weight         708.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.3320(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7494(7)
_cell_length_b                   16.1119(8)
_cell_length_c                   21.2918(11)
_cell_measurement_reflns_used    18959
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4288.4(4)
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41556
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0048(10)
_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   1.085
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+1.2355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.2083
_reflns_number_gt                5392
_reflns_number_total             9812
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol102829h_si_002.cif
_cod_data_source_block           cmpd_2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1501918