#------------------------------------------------------------------------------
#$Date: 2025-01-11 00:54:38 +0200 (Sat, 11 Jan 2025) $
#$Revision: 297274 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/41/7134160.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7134160
loop_
_publ_author_name
'Guo, Jian'
'Nie, Chenyang'
'Li, Shitai'
'Yan, Nana'
'Guo, Peng'
'Liu, Zhongmin'
_publ_section_title
;
 Revealing CO2 Adsorption Blocking Mechanism in Flexible Low-Silica
 Small-pore Zeolites via Three-Dimensional Electron Diffraction
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D4CC06791F
_journal_year                    2025
_chemical_formula_moiety         'Al5.80 O32 Si10.20, 2.872(K2)'
_chemical_formula_sum            'Al5.8 K5.74 O32 Si10.2'
_chemical_formula_weight         1179.59
_chemical_melting_point          293
_chemical_name_systematic        DH-K-GIS
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-11-13 deposited with the CCDC.	2025-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   9.7240(14)
_cell_length_b                   9.7240(14)
_cell_length_c                   9.4320(19)
_cell_measurement_reflns_used    1953
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.1
_cell_measurement_theta_min      59.9
_cell_volume                     891.9(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'JEOL 2100 Plus'
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.1497
_diffrn_reflns_av_unetI/netI     0.1189
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1953
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.897
_diffrn_reflns_theta_min         0.106
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_description       block
_exptl_crystal_F_000             211
_refine_diff_density_max         0.151
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       1364(71)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         452
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.1745
_refine_ls_R_factor_gt           0.1222
_refine_ls_shift/su_max          0.147
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3285
_refine_ls_wR_factor_ref         0.3714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                260
_reflns_number_total             452
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc06791f2.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '293K' was changed to '293'
-- the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'Al5.80 K5.74 O32 Si10.20'
_cod_database_code               7134160
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_res_file
;

REM SHELXT solution in I4(1)/a
REM R1 0.208,  Rweak 0.082,  Alpha 0.076,  Orientation as input
REM Formula found by SHELXT:  O3 Si

CELL  0.0251   9.7240   9.7240   9.4320   90.000   90.000   90.000
ZERR   16.000   0.0014   0.0014   0.0019    0.000    0.000    0.000
LATT  2
SYMM 1/2-X, -Y, 1/2+Z
SYMM 3/4-Y, 1/4+X, 1/4+Z
SYMM 3/4+Y, 3/4-X, 3/4+Z

SFAC O      0.45480  23.78030   0.91730   7.62200   0.47190   2.14400 =
            0.13840   0.29590   0.00000   0.000   0.000   0.000   0.730  15.999
SFAC SI     2.12930  57.77480   2.53330  16.47560   0.83490   2.87960 =
            0.32160   0.38600   0.00000   0.000   0.000   0.000   1.110  28.086
SFAC K      3.95070 137.07480   2.54520  22.40170   1.97950   4.53190 =
            0.48170   0.43400   0.00000   0.000   0.000   0.000   1.330  39.098
SFAC AL     2.27560  72.32200   2.42800  19.77290   0.85780   3.07990 =
            0.31660   0.40760   0.00000   0.000   0.000   0.000   1.180  26.982
UNIT 32 10 6 6
L.S. 30
BOND $H
LIST 6
FMAP 2
SUMP 5.8 0.1 16 2
EXYZ SI1 Al1
EADP SI1 Al1
PLAN 20
ACTA
WGHT    0.200000
EXTI 1363.724976
FVAR       2.83123   0.35918
SI1   2    0.627882    0.572325    0.660985    10.63750    0.02605    0.02618 =
         0.03357   -0.00525   -0.00699   -0.00126
AL1   4    0.627882    0.572325    0.660985    10.36250    0.02605    0.02618 =
         0.03357   -0.00525   -0.00699   -0.00126
O1    1    0.686266    0.437484    0.574492    11.00000    0.05336    0.02977 =
         0.03510    0.00079    0.00474    0.00538
O2    1    0.680467    0.709886    0.576154    11.00000    0.05453    0.02865 =
         0.06039    0.01130   -0.00073    0.00692

K1    3    0.834007    0.295923    0.768472    21.00000    0.18615    0.06809 =
         0.08433    0.01858   -0.02520    0.02844
HKLF 4




REM
REM wR2 = 0.3714, GooF = S = 1.183, Restrained GooF = 1.182 for all data
REM R1 = 0.1222 for 260 Fo > 4sig(Fo) and 0.1745 for all 452 data
REM 39 parameters refined using 1 restraints

END

WGHT      0.1714      0.2282

REM Highest difference peak  0.151,  deepest hole -0.174,  1-sigma level  0.047
Q1    1   0.9155  0.2473  0.7313  11.00000  0.05    0.15
Q2    1   0.6714  0.6222  0.5877  11.00000  0.05    0.12
Q3    1   0.6313  0.6454  0.6843  11.00000  0.05    0.12
Q4    1   0.6148  0.4474  0.7229  11.00000  0.05    0.12
Q5    1   0.6954  0.5531  0.6021  11.00000  0.05    0.11
Q6    1   0.5985  0.6396  0.7041  11.00000  0.05    0.11
Q7    1   0.7409  0.6355  0.7085  11.00000  0.05    0.10
Q8    1   0.8730  0.2499  0.8180  11.00000  0.05    0.09
Q9    1   0.5547  0.6398  0.5820  11.00000  0.05    0.09
Q10   1   0.7500  0.2500  0.7500  10.50000  0.05    0.09
Q11   1   0.7430  0.5299  0.6690  11.00000  0.05    0.09
Q12   1   0.8899  0.3628  0.8513  11.00000  0.05    0.08
Q13   1   0.9517  0.3027  0.8086  11.00000  0.05    0.07
Q14   1   0.5842  0.5333  0.5765  11.00000  0.05    0.06
Q15   1   0.6281  0.3292  0.5624  11.00000  0.05    0.06
Q16   1   0.9302  0.4102  0.7339  11.00000  0.05    0.05
Q17   1   0.5266  0.3498  0.6326  11.00000  0.05    0.04
Q18   1   1.0000  0.2500  0.8673  10.50000  0.05    0.03
Q19   1   0.8354  0.4656  0.5064  11.00000  0.05    0.03
Q20   1   0.8325  0.2590  0.9214  11.00000  0.05    0.03
;
_shelx_res_checksum              15642
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.6279(4) 0.5723(4) 0.6610(4) 0.0286(15) Uani 0.6375 1 d . . P . .
Al1 Al 0.6279(4) 0.5723(4) 0.6610(4) 0.0286(15) Uani 0.3625 1 d . . P . .
O1 O 0.6863(7) 0.4375(7) 0.5745(7) 0.039(2) Uani 1 1 d . . . . .
O2 O 0.6805(8) 0.7099(7) 0.5762(8) 0.048(2) Uani 1 1 d . . . . .
K1 K 0.834(2) 0.2959(17) 0.7685(17) 0.113(8) Uani 0.359(6) 1 d . . P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.026(3) 0.026(3) 0.034(2) -0.0053(18) -0.0070(18) -0.0013(17)
Al1 0.026(3) 0.026(3) 0.034(2) -0.0053(18) -0.0070(18) -0.0013(17)
O1 0.053(5) 0.030(4) 0.035(4) 0.001(3) 0.005(3) 0.005(3)
O2 0.055(5) 0.029(4) 0.060(5) 0.011(3) -0.001(4) 0.007(3)
K1 0.19(2) 0.068(11) 0.084(12) 0.019(8) -0.025(11) 0.028(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Si1 O2 111.1(6) . 15_566 ?
O2 Si1 O1 107.5(4) . . ?
O2 Si1 O1 111.6(4) 15_566 . ?
O2 Si1 O1 112.8(4) . 8_454 ?
O2 Si1 O1 106.3(4) 15_566 8_454 ?
O1 Si1 O1 107.6(4) . 8_454 ?
Si1 O1 Si1 136.6(5) . 7_544 ?
Si1 O2 Si1 140.5(5) . 12_767 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 O2 1.640(8) . ?
Si1 O2 1.638(8) 15_566 ?
Si1 O1 1.645(8) . ?
Si1 O1 1.650(8) 8_454 ?
K1 K1 1.89(4) 13_656 ?
