Crystallographic analysis of CO2 sorption state in seemingly nonporous molecular crystal of azacalix[4]arene tetramethyl ether exhibiting highly selective CO2 uptake
Tsue, Hirohito; Takahashi, Hiroki; Ishibashi, Koichi; Inoue, Rikako; Shimizu, Shun; Takahashi, Daisuke; Tamura, Rui; CrystEngComm 14 (2012) 1021–; doi:10.1039/c1ce06126g

data_7207189
_publ_section_title
;
 Crystallographic analysis of CO2 sorption state in seemingly nonporous
 molecular crystal of azacalix[4]arene tetramethyl ether exhibiting highly
 selective CO2 uptake
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              1021
_journal_paper_doi               10.1039/c1ce06126g
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C44.4 H60 N4 O4.8'
_chemical_formula_weight         726.56
_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                 101.817(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.836(8)
_cell_length_b                   16.215(9)
_cell_length_c                   21.460(13)
_cell_measurement_reflns_used    7690
_cell_measurement_temperature    133
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4372(5)
_computing_cell_refinement
;
Rigaku CrystalClear-SM Expert 2.0 r4
;
_computing_data_collection
;
Rigaku CrystalClear-SM Expert 2.0 r4
;
_computing_data_reduction
;
Rigaku CrystalClear-SM Expert 2.0 r4
;
_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      133(2)
_diffrn_detector_area_resol_mean 28.6533
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
;
Rigaku CrystalClear-SM Expert 2.0 r4
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34429
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1571.2
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         9903
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.2393
_refine_ls_R_factor_gt           0.1433
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3704
_refine_ls_wR_factor_ref         0.4355
_reflns_number_gt                4346
_reflns_number_total             9903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce06126g.txt
_cod_data_source_block           cmpd_2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7207189