Superior thermoelasticity and shape-memory nanopores in a porous supramolecular organic framework
You-Gui Huang; Yoshihito Shiota; Ming-Yan Wu; Sheng-Qun Su; Zi-Shuo Yao; Soonchul Kang; Shinji Kanegawa; Guo-Ling Li; Shu-Qi Wu; Takashi Kamachi; Kazunari Yoshizawa; Katsuhiko Ariga; Mao-Chun Hong; Osamu Sato; Nature Communications 7 (2016) 11564–; doi:10.1038/ncomms11564

data_1548018
_publ_section_title
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 Superior thermoelasticity and shape-memory nanopores in a porous
 supramolecular organic framework
;
_journal_name_full               'Nature Communications'
_journal_page_first              11564
_journal_paper_doi               10.1038/ncomms11564
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C10 H8.50 N O2'
_chemical_formula_sum            'C10 H8.5 N O2'
_chemical_formula_weight         174.68
_chemical_name_common            'C10 H8.50 N O2'
_space_group_crystal_system      tetragonal
_space_group_IT_number           133
_space_group_name_Hall           '-P 4ac 2b'
_space_group_name_H-M_alt        'P 42/n b c'
_symmetry_space_group_name_Hall  '-P 4ac 2b'
_symmetry_space_group_name_H-M   'P 42/n b c :2'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.856(6)
_cell_length_b                   17.856(6)
_cell_length_c                   12.787(7)
_cell_measurement_reflns_used    11007
_cell_measurement_temperature    438(2)
_cell_measurement_theta_max      30.9997
_cell_measurement_theta_min      2.2812
_cell_volume                     4077(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      438(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Rigaku CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14093
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         6.045
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5205
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The following poor diffraction spots were omitted in the refinement.
OMIT      3   1   1
OMIT      8   8   0
OMIT       1   1   1
OMIT       2   4   0
OMIT       1   3   1
OMIT     2   2   2
OMIT      2   0   2
OMIT      2   4   3
OMIT       2   2   1
OMIT     4   0   0
OMIT    10   6   0
OMIT     0   8   0
OMIT     10   4   0
OMIT      2   2   0
OMIT     1  11   1
OMIT    0   0   4
OMIT     4   8   0
OMIT    8   4   0
OMIT    0   6   2
OMIT    4   8   1
OMIT    4  12   0
OMIT   8   2   2
OMIT     2   8   0
OMIT    5   5   1
OMIT    1   9   1
OMIT      7   7   3
OMIT    6   4   1
OMIT      0   2   2
OMIT     6   8   0
OMIT     1   3   6
OMIT   4  10   2
OMIT    4   6   2
OMIT    2   8   2
OMIT    1   9   2
OMIT    5   3   5
The following constraints were performed in the refinement.
DFIX 1.25 0.02 C8A O4B C8A O3B
DFIX 1.25 0.02 C8B O4A C8B O3A
DFIX 2.22 0.02 O3A O4A O3B O4B
DFIX 1.50 0.02 C1 C8B
Because the disorder, desolvation process,thermal cycling,and phase transition, the structure refine with poor R value.
;
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1831
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.2123
_refine_ls_R_factor_gt           0.1735
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+1.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4425
_refine_ls_wR_factor_ref         0.4742
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                998
_reflns_number_total             1831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ncomms11564-s13.cif
_cod_data_source_block           12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
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_cod_original_cell_volume        4077(4)
_cod_original_formula_sum        'C10 H8.50 N O2'
_cod_database_code               1548018
_shelx_res_checksum              63553
_shelx_hkl_checksum              15532