Impact of Defects and Crystal Size on Negative Gas Adsorption in DUT-49 Analyzed by In Situ 129Xe NMR Spectroscopy
Krause, Simon; Reuter, Florian S.; Ehrling, Sebastian; Bon, Volodymyr; Senkovska, Irena; Kaskel, Stefan; Brunner, Eike; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c01059

data_4003543
_publ_section_title
;
 Impact of Defects and Crystal Size on Negative Gas Adsorption in DUT-49
 Analyzed by In Situ 129Xe NMR Spectroscopy
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01059
_journal_year                    2020
_chemical_formula_sum            'C32 H26 Cu2 N2 O10'
_chemical_formula_weight         725.63
_space_group_crystal_system      trigonal
_space_group_IT_number           164
_space_group_name_Hall           '-P 3 2"'
_space_group_name_H-M_alt        'P -3 m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.515(3)
_cell_length_b                   23.515(3)
_cell_length_c                   11.052(2)
_cell_measurement_reflns_used    573
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      3.85
_cell_volume                     5292.5(14)
_computing_cell_refinement       'XDSAPP 2.0 Sparta et al., 2016'
_computing_data_collection       'marCCD 1994-2002'
_computing_data_reduction        'XDSAPP 2.0 Sparta et al., 2016'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       '\D\f scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            41015
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        32.098
_diffrn_reflns_theta_max         35.098
_diffrn_reflns_theta_min         1.246
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    1.139
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.683
_exptl_crystal_description       block
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.287
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         4222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.1039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3214
_refine_ls_wR_factor_ref         0.3435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3530
_reflns_number_total             4222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm0c01059_si_002.cif
_cod_data_source_block           p3m1_sq
_cod_original_cell_volume        5292.5(18)
_cod_database_code               4003543
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.914
_shelx_res_checksum              21480
_shelx_hkl_checksum              1383
_shelx_fab_checksum              14554