Structural Evolution of Ag-LEV Zeolite upon Heating: An In Situ Single-Crystal X-ray Diffraction (SC-XRD) and X-ray Absorption Spectroscopy (XAS) Study.
Cametti, Georgia; Scheinost, Andreas C.; Churakov, Sergey V.; ACS omega 5 (2020) 31774–31783; doi:10.1021/acsomega.0c04455

data_4518281
_publ_section_title
;
 Structural Evolution of Ag-LEV Zeolite upon Heating: An In Situ
 Single-Crystal X-ray Diffraction (SC-XRD) and X-ray Absorption
 Spectroscopy (XAS) Study.
;
_journal_issue                   49
_journal_name_full               'ACS omega'
_journal_page_first              31774
_journal_page_last               31783
_journal_paper_doi               10.1021/acsomega.0c04455
_journal_volume                  5
_journal_year                    2020
_chemical_formula_sum            'Ag9.54 O108.74 Si54'
_chemical_formula_weight         4285.78
_chemical_name_common            Ag-levyne
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   12.9559(18)
_cell_length_b                   12.9559(18)
_cell_length_c                   23.611(5)
_cell_measurement_reflns_used    2367
_cell_measurement_temperature    498(2)
_cell_measurement_theta_max      22.34
_cell_measurement_theta_min      2.5
_cell_volume                     3432.3(10)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      498(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7233
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.010
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4739
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            gray
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2074
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 322 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.34(9)
_refine_ls_extinction_coef       0.0004(3)
_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   0.908
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1713
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0645
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1203P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1967
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.820
_reflns_Friedel_fraction_max     0.770
_reflns_number_gt                874
_reflns_number_total             1713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c04455_si_006.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4518279--4518286.cif.'
_cod_original_cell_volume        3432.3(12)
_cod_database_code               4518281
_shelxl_version_number           2014-1
_shelx_res_checksum              59224
_shelx_hkl_checksum              9564