Determination of Na+ Cation Locations in Nanozeolite ECR-1 Using a 3D ED Method
Örs, Taylan; Deroche, Irena; Chatelard, Corentin; Dodin, Mathias; Martinez-Franco, Raquel; Tuel, Alain; Paillaud, Jean-Louis; Symmetry 16 (2024) 477–; doi:10.3390/sym16040477

data_1571563
_publ_section_title
;
 Determination of Na+ Cation Locations in Nanozeolite ECR-1 Using a 3D ED
 Method
;
_journal_issue                   4
_journal_name_full               Symmetry
_journal_page_first              477
_journal_paper_doi               10.3390/sym16040477
_journal_volume                  16
_journal_year                    2024
_chemical_formula_sum            'Na8.154744 O124.8117 Si60'
_chemical_formula_weight         3869.5
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n :2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      59
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   7.4865
_cell_length_b                   17.8463
_cell_length_c                   25.6545
_cell_measurement_reflns_used    677
_cell_measurement_temperature    103
_cell_measurement_theta_max      1.01
_cell_measurement_theta_min      0.05
_cell_volume                     3427.603
_diffrn_ambient_temperature      103
_diffrn_measured_fraction_theta_full 0.93
_diffrn_measured_fraction_theta_max 0.82
_diffrn_measurement_device       TEM_CM200_DIGISTAR_Precession
_diffrn_measurement_device_type  Electron_microscope_with_beam_precession
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.1837
_diffrn_reflns_av_unetI/netI     1.0918
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            152274
_diffrn_reflns_theta_full        0.88
_diffrn_reflns_theta_max         1.01
_diffrn_reflns_theta_min         0.05
_exptl_absorpt_coefficient_mu    0
_exptl_crystal_density_diffrn    1.8746
_exptl_crystal_description       plate
_exptl_crystal_F_000             635.553
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    2.7302
_refine_ls_goodness_of_fit_ref   0.7976
_refine_ls_number_constraints    32
_refine_ls_number_parameters     275
_refine_ls_number_reflns         17481
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.5174
_refine_ls_R_factor_gt           0.0966
_refine_ls_shift/su_max          5.9233
_refine_ls_shift/su_mean         0.6636
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.02P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.2245
_reflns_number_gt                1040
_reflns_number_total             17481
_reflns_threshold_expression     I>3\s(I)
_publcif_datablock.id            {d42f901b-72a3-4363-ad01-e0162464385e}
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_cod_data_source_file            ECR-1_tomo14_dyn_final_SI_revised.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P -2xa;-2yb;-2zab'
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               1571563
_jana_m40_file
;
   43    0    0    1    0
 1.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 0.000000 0.000000 0.000000                                 000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
Si1       1  1     1.000000 0.547629 0.448793 0.361717
 0.033418 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
Si2       1  1     1.000000 0.451967 0.554464 0.452496
 0.021786 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
Si3       1  1     0.500000 0.750000 0.426979 0.101845
 0.046186 0.000000 0.000000 0.000000 0.000000 0.000000      0011100000
Si4       1  1     1.000000 0.452849 0.442184 0.248038
 0.024109 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
Si5       1  1     0.500000 0.250000 0.336641 0.395500
 0.024713 0.000000 0.000000 0.000000 0.000000 0.000000      0011100000
Si6       1  1     1.000000 0.454991 0.522799 0.145020
 0.030123 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
Si7       1  1     0.500000 0.250000 0.334445 0.518648
 0.039115 0.000000 0.000000 0.000000 0.000000 0.000000      0011100000
Si8       1  1     1.000000 0.542944 0.666549 0.086786
 0.033688 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
Si9       1  1     0.500000 0.750000 0.339769 0.210243
 0.042861 0.000000 0.000000 0.000000 0.000000 0.000000      0011100000
Si10      1  1     0.500000 0.750000 0.339587-0.005990
 0.044220 0.000000 0.000000 0.000000 0.000000 0.000000      0011100000
O1        2  1     1.000000 0.486539 0.513657 0.397947
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
O2        2  1     1.000000 0.566742 0.366378 0.240485
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O3        2  1     1.000000 0.066812 0.373131 0.538454
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O4        2  1     0.500000 0.750000 0.385262 0.047120
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0011000000
O5        2  1     0.500000 0.250000 0.573835 0.458722
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0011000000
O6        2  1     0.500000 0.750000 0.428546 0.369371
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0011000000
O7        2  1     0.500000 0.250000 0.419537 0.247824
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0011000000
O8        2  1     0.250000 0.250000 0.250000 0.536343
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0001000000
O9        2  1     0.250000 0.750000 0.250000 0.221750
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0001000000
O10       2  1     1.000000 0.425432 0.639406 0.035021
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O11       2  1     1.000000 0.502321 0.501321 0.202485
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O12       2  1     0.250000 0.750000 0.250000 0.011894
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0001000000
O13       2  1     0.250000 0.250000 0.250000 0.375777
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0001000000
O14       2  1     1.000000 0.509547 0.482160 0.301265
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O15       2  1     1.000000 0.563110 0.470110 0.105117
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O16       2  1     1.000000 0.437271 0.372684 0.369199
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O17       2  1     0.500000 0.502096 0.750000 0.105431
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0101000000
O18       2  1     0.500000 0.250000 0.350802 0.454887
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0011000000
O19       2  1     1.000000 0.506305 0.606733 0.133390
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O20       2  1     0.500000 0.750000 0.363015 0.147514
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0011000000
O21       2  1     0.500000 0.250000 0.506895 0.130111
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0011000000
O22       2  1     0.500000 0.750000 0.664514 0.069453
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0011000000
O23       2  1     0.500000 0.500000 0.500000 0.500000
 0.070191 0.000000 0.000000 0.000000 0.000000 0.000000      0000000000
Na1       3  1     0.253383 0.250000 0.415297 0.020900
 0.120000 0.000000 0.000000 0.000000 0.000000 0.000000      1011000000
Na2       3  1     0.394729 0.492457 0.250000 0.300118
 0.120000 0.000000 0.000000 0.000000 0.000000 0.000000      1101000000
Na3       3  1     0.105840 0.750000 0.552937 0.262719
 0.120000 0.000000 0.000000 0.000000 0.000000 0.000000      1011000000
Na4       3  1     0.104537 0.750000 0.560950 0.343022
 0.120000 0.000000 0.000000 0.000000 0.000000 0.000000      1011000000
Na5       3  1     0.041056 0.930024 0.250000 0.427103
 0.120000 0.000000 0.000000 0.000000 0.000000 0.000000      1101000000
Na6       3  1     0.119798 0.250000 0.547382 0.278713
 0.120000 0.000000 0.000000 0.000000 0.000000 0.000000      1011000000
Ow1       2  1     0.177661 0.250000 0.250000 0.243947
 0.130000 0.000000 0.000000 0.000000 0.000000 0.000000      1001000000
Ow2       2  1     0.175215 0.750000 0.250000 0.347666
 0.130000 0.000000 0.000000 0.000000 0.000000 0.000000      1001000000
Ow3       2  1     0.159423 0.313313 0.306508 0.079202
 0.130000 0.000000 0.000000 0.000000 0.000000 0.000000      1111000000
Ow4       2  1     0.089169 0.750000 0.250000 0.453694
 0.130000 0.000000 0.000000 0.000000 0.000000 0.000000      1001000000
--------------------------   s.u. block   --------------------------------------
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Si1                0.000000 0.000607 0.000500 0.000167
 0.001729 0.000000 0.000000 0.000000 0.000000 0.000000
Si2                0.000000 0.000569 0.000404 0.000154
 0.001401 0.000000 0.000000 0.000000 0.000000 0.000000
Si3                0.000000 0.000000 0.000711 0.000251
 0.002728 0.000000 0.000000 0.000000 0.000000 0.000000
Si4                0.000000 0.000609 0.000476 0.000163
 0.001516 0.000000 0.000000 0.000000 0.000000 0.000000
Si5                0.000000 0.000000 0.000717 0.000229
 0.002516 0.000000 0.000000 0.000000 0.000000 0.000000
Si6                0.000000 0.000650 0.000503 0.000172
 0.001697 0.000000 0.000000 0.000000 0.000000 0.000000
Si7                0.000000 0.000000 0.000694 0.000239
 0.002990 0.000000 0.000000 0.000000 0.000000 0.000000
Si8                0.000000 0.000597 0.000556 0.000155
 0.001775 0.000000 0.000000 0.000000 0.000000 0.000000
Si9                0.000000 0.000000 0.000715 0.000280
 0.002930 0.000000 0.000000 0.000000 0.000000 0.000000
Si10               0.000000 0.000000 0.000491 0.000235
 0.003078 0.000000 0.000000 0.000000 0.000000 0.000000
O1                 0.000000 0.001140 0.000828 0.000293
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O2                 0.000000 0.001371 0.000616 0.000348
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O3                 0.000000 0.001106 0.000612 0.000355
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O4                 0.000000 0.000000 0.000968 0.000430
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O5                 0.000000 0.000000 0.001450 0.000475
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O6                 0.000000 0.000000 0.001369 0.000475
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O7                 0.000000 0.000000 0.001639 0.000500
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O8                 0.000000 0.000000 0.000000 0.000838
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O9                 0.000000 0.000000 0.000000 0.000866
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O10                0.000000 0.001206 0.000979 0.000309
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O11                0.000000 0.001115 0.000717 0.000345
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O12                0.000000 0.000000 0.000000 0.000784
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O13                0.000000 0.000000 0.000000 0.000817
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O14                0.000000 0.001132 0.001026 0.000398
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O15                0.000000 0.001264 0.001038 0.000335
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O16                0.000000 0.001404 0.000654 0.000358
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O17                0.000000 0.001816 0.000000 0.000569
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O18                0.000000 0.000000 0.001403 0.000493
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O19                0.000000 0.001386 0.001255 0.000372
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O20                0.000000 0.000000 0.001406 0.000515
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O21                0.000000 0.000000 0.001532 0.000429
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O22                0.000000 0.000000 0.001477 0.000466
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
O23                0.000000 0.000000 0.000000 0.000000
 0.000864 0.000000 0.000000 0.000000 0.000000 0.000000
Na1                0.006528 0.000000 0.002526 0.000946
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Na2                0.007514 0.002110 0.000000 0.000670
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Na3                0.007108 0.000000 0.006008 0.002183
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Na4                0.007563 0.000000 0.002760 0.002548
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Na5                0.009515 0.024421 0.000000 0.004217
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Na6                0.007409 0.000000 0.002808 0.002037
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Ow1                0.008656 0.000000 0.000000 0.001268
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Ow2                0.008345 0.000000 0.000000 0.001255
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Ow3                0.012257 0.009280 0.004079 0.002050
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Ow4                0.010090 0.000000 0.000000 0.003012
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
--------------------------   Saved points   ------------------------------------
    0
--------------------------   Critical points   ---------------------------------
    0
--------------------------   Fourier maxima   ----------------------------------
    1    1    3
Max1      1  1     1.000000 0.749972 0.250000 0.302758      000  0  0  0
     0.18     0.14
Max2      1  1     1.000000 0.543690 0.737286 0.344942      000  0  0  0
     0.11     0.11
Max3      1  1     1.000000 0.825603 0.250000 0.096747      000  0  0  0
     0.15     0.11
Max4      1  1     1.000000 0.174191 0.555452 0.031507      000  0  0  0
     0.13     0.10
Max5      1  1     1.000000 0.575564 0.077126 0.050310      000  0  0  0
     0.12     0.10
Max6      1  1     1.000000 0.749971 0.250000 0.404503      000  0  0  0
     0.16     0.10
Max7      1  1     1.000000 0.249973 0.750000 0.160805      000  0  0  0
     0.14     0.10
Max8      1  1     1.000000 0.749960 0.033163 0.396756      000  0  0  0
     0.11     0.10
Max9      1  1     1.000000 0.749964 0.644836 0.438789      000  0  0  0
     0.13     0.09
Max10     1  1     1.000000 0.090226 0.595937 0.432562      000  0  0  0
     0.13     0.09
--------------------------   Fourier minima   ----------------------------------
    1    1    3
Min1      1  1     1.000000 0.011398 0.250000 0.044300      000  0  0  0
     0.12     0.12
Min2      1  1     1.000000 0.557513 0.250000 0.295943      000  0  0  0
     0.16     0.12
Min3      1  1     1.000000 0.036510 0.083195 0.459177      000  0  0  0
     0.14     0.12
Min4      1  1     1.000000 0.250015 0.059881 0.006011      000  0  0  0
     0.18     0.11
Min5      1  1     1.000000 0.250047 0.750000 0.253794      000  0  0  0
     0.11     0.10
--------------------------------------------------------------------------------
;
_jana_m50_file
;
Version Jana2020
title ECR-1
cell 7.4865 17.8463 25.6545 90 90 90
esdcell 0 0 0 0 0 0
spgroup Pmmn 59 3
sgshift 0.25 0.25 0
lattice P
symmetry x y z
symmetry -x+1/2 -y+1/2 z
symmetry -x y+1/2 -z
symmetry x+1/2 -y -z
symmetry -x -y -z
symmetry x+1/2 y+1/2 -z
symmetry x -y+1/2 z
symmetry -x+1/2 y z
unitsnumb 1
atlist Si60 O120 Na8.567
formtab -62
atom Si atradius 1.18 color 27059250
atom O atradius 0.74 color 254003000
atom Na atradius 1.91 color 249220060
roundmethod 1
end
*******************************************************************************
contour
end contour
dist
  expdmax 33
  selfirst Si1 Si2 Si3 Si4 Si5 Si6 Si7 Si8 Si9 Si10 Na1 Na2 Na3 Na4 Na5
  selfirst Na6
  selsecnd O1 O2 O3 O4 O5 O6 O7 O8 O9 O10 O11 O12 O13 O14 O15 O16 O17 O18
  selsecnd O19 O20 O21 O22 O23 Ow1 Ow2 Ow3 Ow4
end dist
fourier
  maptype 6 orient 123
end fourier
refine
  cycles 1 damp 0.5 uisolim 0.5
  restric O1 12 O2 O3 O4 O5 O6 O7 O8 O9 O10 O11 O12 O13 O14 O15 O16 O17 O18 O19
  & O20 O21 O22 O23
  !restric Na* 12
  !restric Ow* 12
  fixed u Na*
  fixed u Ow*
  distfix 1.62 0.0099999998 Si1 O6;
  distfix 1.62 0.0099999998 Si1 O16;
  distfix 1.62 0.0099999998 Si2 O1;
  distfix 1.62 0.0099999998 Si2 O3#s4t0,1,1;
  distfix 1.62 0.0099999998 Si3 O4;
  distfix 1.62 0.0099999998 Si4 O2;
  distfix 1.62 0.0099999998 Si4 O11;
  distfix 1.62 0.0099999998 Si7 O3;
  distfix 1.62 0.0099999998 Si10 O4;
  distfix 1.62 0.0099999998 Si10 O12;
  distfix 2.5 0.0500000007 Na1 O22#s4t-1,1,0;
  distfix 2.5 0.0500000007 Na1 Ow3;
  distfix 2.5 0.0199999996 Na2 Ow2;
  distfix 2.5 0.0500000007 Na3 O11;
  distfix 2.5 0.0500000007 Na4 O6;
  distfix 2.5 0.0199999996 Na5 Ow2;
  distfix 2.5 0.0500000007 Na6 O7;
end refine
;
_publcif_funding_html
;
;