# Supplementary Information (SI) for RSC Mechanochemistry.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2024NCS0186
_database_code_depnum_ccdc_archive 'CCDC 2432426'
loop_
_audit_author_name
_audit_author_address
'Daniel N. Rainer'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2025-03-19 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_audit_creation_date             2025-03-19
_audit_creation_method           
;
Olex2 1.5-ac7-014
(compiled 2025.02.27 svn.r6f4c0eaf for Rigaku Oxford Diffraction, GUI svn.r7171)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Al Na0.901 O4 Si, 0.099(Na)'
_chemical_formula_sum            'Al Na O4 Si'
_chemical_formula_weight         142.05
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Si Al O C H Na'
_chemical_oxdiff_usercomment     
;
'Agar lacey carbon grid, ground between glass slides & grid tapped, cryo
transfer (no plunging) @ 175 K, coll @ 175 K'
;
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   9.0311(7)
_cell_length_b                   9.0311(7)
_cell_length_c                   9.0311(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     736.58(17)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    2387
_cell_measurement_temperature    175(5)
_cell_measurement_theta_max      1.0140
_cell_measurement_theta_min      0.1120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.44.98a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'white (bulk)'
_exptl_crystal_colour_primary    'white (bulk)'
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             146
_exptl_crystal_preparation       
;
'sample ground between glass slides, grid dabbed in solid'
;
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2499
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8931
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.894
_diffrn_reflns_theta_min         0.113
_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      175(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector.description     'Hybrid Pixel Array Detector'
_diffrn_detector.make            'Rigaku HyPix-ED'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku HyPix-ED'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement.rotation_mode rotation
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.25  62.00   0.25    0.50    --    0.00   0.00   0.00  337
  2  ω    -22.25  62.00   0.25    0.50    --    0.00   0.00   0.00  337
  3  ω    -19.75  58.00   0.25    0.50    --    0.00   0.00   0.00  311
  4  ω    -24.75  58.00   0.25    0.50    --    0.00   0.00   0.00  331
  5  ω    -62.00  62.00   0.25    0.50    --    0.00   0.00   0.00  496
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_measurement_specimen_support 
;
'lacey carbon copper grid, 200 mesh; Gatan Elsa cryo-transfer holder 698'
;
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027786000
_diffrn_orient_matrix_UB_12      -0.0000002000
_diffrn_orient_matrix_UB_13      -0.0000059000
_diffrn_orient_matrix_UB_21      -0.0000001000
_diffrn_orient_matrix_UB_22      0.0027802000
_diffrn_orient_matrix_UB_23      -0.0000040000
_diffrn_orient_matrix_UB_31      0.0000000000
_diffrn_orient_matrix_UB_32      0.0000005000
_diffrn_orient_matrix_UB_33      0.0027788000
_diffrn_oxdiff_digest_creation   
;
CAP 1.171.44.98a, AC 1.5-ac7-014
;
_diffrn_oxdiff_digest_hkl        
;
432676d7317de38003d57bb30080b95017383b
;
_diffrn_oxdiff_digest_hkl_ed     
;
53ddfcf6f4c044a6618f888382907ce8c36524
;
_diffrn_oxdiff_digest_od_ed      
;

;
_diffrn_radiation.wavelength     0.0251
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'electron gun'
_diffrn_source.description       'electron gun'
_diffrn_source.ed_diffracting_area_selection SAED
_diffrn_source.make              LaB6
_diffrn_source.voltage           200
_diffrn_source_details           LaB6
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_diffrn_source_voltage           200
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.658
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                161
_reflns_number_total             257
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.44.98a (Rigaku OD, 2025)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.118a 64-bit (release 27-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.44.98a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine.diffraction_theory       kinematical
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       10288(48)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         257
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1784
_refine_ls_R_factor_gt           0.1554
_refine_ls_restrained_S_all      1.024
_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/[σ²(Fo²)+(0.3357P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3633
_refine_ls_wR_factor_ref         0.4033
_refine_special_details          
;
An extinction correction parameter (EXTI) was refined to account roughly for
dynamical effects in the kinematical refinement of 3D ED data.
A global rigid bond restraint (RIGU) as well as a similarity restraint (SIMU)
on the split oxygen (O1, O1a) were applied to achieve more sensible AADPs.
The occupancies of the split oxygen atoms (O1, O1a) were intially refined
freely, and later on fixed to 2/3 and 1/3, representative of the freely refined
values.
Besides the atom sites building up the zeolite framework (Si1, Al1, O1, O1a),
there are 2 distinct maxima in the difference map, which were assigned as sodium
atoms, whose combined occupancy was effectively constrained to 1/4, to charge
balance the present aluminium. However, the presence of protons or additional
sodium sites cannot be excluded.
;
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
O1 \\sim O1A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 1*[Sof(Na1)]+1*[Sof(Na2)]=0.25 with esd of 0.0001
 Fixed Sof: O1(0.6667) O1A(0.3333)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.000000 0.500000 0.250000 0.041(3) Uani 1 4 d S T P . .
Al1 Al 0.000000 0.750000 0.500000 0.025(3) Uani 1 4 d S T P . .
O1 O -0.0237(18) 0.6583(18) 0.3443(17) 0.044(4) Uani 0.6667 1 d . U P A 1
O1A O 0.067(6) 0.634(4) 0.366(4) 0.046(5) Uani 0.3333 1 d . U P A 2
Na1 Na 0.313(4) 0.687(4) 0.313(4) 0.114(15) Uani 0.675(11) 3 d S T P B 1
Na2 Na 0.500000 0.500000 0.500000 0.053(19) Uani 0.30(4) 12 d S T P C 2

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 0.046(4) 0.046(4) 0.031(5) 0.000 0.000 0.000
Al1 0.027(3) 0.022(5) 0.027(3) 0.000 0.000 0.000
O1 0.068(10) 0.037(7) 0.027(7) -0.002(4) 0.005(8) -0.004(9)
O1A 0.074(17) 0.030(13) 0.033(13) 0.004(7) -0.003(10) 0.007(10)
Na1 0.114(15) 0.114(15) 0.114(15) -0.03(2) 0.03(2) -0.03(2)
Na2 0.053(19) 0.053(19) 0.053(19) 0.000 0.000 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O1 1.678(17) . ?
Si1 O1 1.678(17) 16 ?
Si1 O1 1.678(17) 15_455 ?
Si1 O1 1.678(17) 2_565 ?
Si1 O1A 1.71(4) . ?
Si1 O1A 1.71(4) 16 ?
Si1 O1A 1.71(4) 2_565 ?
Si1 O1A 1.71(4) 15_455 ?
Al1 O1 1.646(17) . ?
Al1 O1 1.646(17) 24_565 ?
Al1 O1 1.646(17) 22_465 ?
Al1 O1 1.646(17) 3_556 ?
Al1 O1A 1.71(4) 24_565 ?
Al1 O1A 1.71(4) 3_556 ?
Al1 O1A 1.71(4) . ?
Al1 O1A 1.71(4) 22_465 ?
O1 Na1 2.48(3) 16 ?

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
O1 Si1 O1 104.9(5) . 16 ?
O1 Si1 O1 119.0(10) 16 15_455 ?
O1 Si1 O1 104.9(5) . 15_455 ?
O1 Si1 O1 104.9(5) 16 2_565 ?
O1 Si1 O1 119.0(10) . 2_565 ?
O1 Si1 O1 104.9(5) 15_455 2_565 ?
O1 Si1 O1A 85.5(13) . 16 ?
O1 Si1 O1A 85.5(13) 16 2_565 ?
O1 Si1 O1A 104.2(9) 16 15_455 ?
O1 Si1 O1A 29.7(14) 16 16 ?
O1 Si1 O1A 85.5(13) 2_565 15_455 ?
O1 Si1 O1A 134.6(15) 15_455 2_565 ?
O1 Si1 O1A 29.7(14) 15_455 15_455 ?
O1 Si1 O1A 29.7(14) 2_565 2_565 ?
O1 Si1 O1A 104.2(9) 15_455 16 ?
O1 Si1 O1A 104.2(9) . 2_565 ?
O1 Si1 O1A 134.6(15) 2_565 16 ?
O1 Si1 O1A 134.6(15) . 15_455 ?
O1A Si1 O1A 112.2(10) . 15_455 ?
O1A Si1 O1A 104(2) 16 15_455 ?
O1A Si1 O1A 112.2(10) 2_565 15_455 ?
O1 Al1 O1 104.7(5) 22_465 . ?
O1 Al1 O1 119.6(10) 24_565 22_465 ?
O1 Al1 O1 104.7(5) 3_556 22_465 ?
O1 Al1 O1 119.6(11) 3_556 . ?
O1 Al1 O1 104.7(5) 24_565 . ?
O1 Al1 O1 104.7(5) 24_565 3_556 ?
O1 Al1 O1A 29.9(14) 24_565 24_565 ?
O1 Al1 O1A 29.9(14) 3_556 3_556 ?
O1 Al1 O1A 85.2(13) . 22_465 ?
O1 Al1 O1A 134.5(15) 24_565 3_556 ?
O1 Al1 O1A 134.5(15) 3_556 22_465 ?
O1 Al1 O1A 29.9(14) 22_465 22_465 ?
O1 Al1 O1A 134.5(15) . 24_565 ?
O1 Al1 O1A 85.2(13) 3_556 24_565 ?
O1 Al1 O1A 104.4(9) 24_565 22_465 ?
O1 Al1 O1A 85.2(13) 22_465 3_556 ?
O1 Al1 O1A 104.4(9) 22_465 24_565 ?
O1 Al1 O1A 104.4(10) . 3_556 ?
O1A Al1 O1A 112.1(10) 24_565 3_556 ?
O1A Al1 O1A 112.1(10) 24_565 . ?
O1A Al1 O1A 112.1(10) 22_465 3_556 ?
O1A Al1 O1A 112.1(10) 22_465 . ?
O1A Al1 O1A 104(2) 3_556 . ?
Si1 O1 Na1 105.4(8) . 16 ?
Al1 O1 Si1 147.8(10) . . ?
Al1 O1 Na1 106.5(8) . 16 ?
Al1 O1A Si1 138(3) . . ?
O1 Na1 O1 110.6(15) 24_565 17_554 ?
O1 Na1 O1 110.6(15) 15_455 24_565 ?
O1 Na1 O1 110.6(15) 15_455 17_554 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Si1 O1 Al1 -94.5(14) 15_455 . . . ?
O1 Si1 O1 Al1 22.4(15) 2_565 . . . ?
O1 Si1 O1 Al1 139.3(16) 16 . . . ?
O1 Si1 O1 Na1 95(2) 15_455 . . 16 ?
O1 Si1 O1 Na1 -31.6(19) 16 . . 16 ?
O1 Si1 O1 Na1 -148.5(19) 2_565 . . 16 ?
O1 Al1 O1 Si1 -139.1(16) 22_465 . . . ?
O1 Al1 O1 Si1 94.4(14) 24_565 . . . ?
O1 Al1 O1 Si1 -22.3(15) 3_556 . . . ?
O1 Al1 O1 Na1 31.8(19) 22_465 . . 16 ?
O1 Al1 O1 Na1 148.6(19) 3_556 . . 16 ?
O1 Al1 O1 Na1 -95(2) 24_565 . . 16 ?
O1A Si1 O1A Al1 -62(2) 2_565 . . . ?
O1A Si1 O1A Al1 177(3) 15_455 . . . ?
O1A Si1 O1A Al1 59.8(15) 16 . . . ?
O1A Al1 O1A Si1 -59.8(15) 22_465 . . . ?
O1A Al1 O1A Si1 -177(3) 24_565 . . . ?
O1A Al1 O1A Si1 62(2) 3_556 . . . ?

_shelx_res_file                  
;
TITL m_769_772_773_774_776_cf_c.res in P-43n
    m_769_772_773_774_776_cf.res
    created by SHELXL-2019/3 at 11:46:05 on 18-Mar-2025
REM Old TITL m_769_772_773_774_776_cf in P-43n
REM SHELXT solution in P-43n: R1 0.248, Rweak 0.092, Alpha 0.030
REM <I/s> 0.368 for 38 systematic absences, Orientation as input
REM Flack x = -1.170 ( 0.744 ) from 64 Parsons' quotients
REM Formula found by SHELXT: O17 Si6
CELL 0.0251 9.0311 9.0311 9.0311 90 90 90
ZERR 6 0.0007 0.0007 0.0007 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Z,+X,+Y
SYMM +Z,-X,-Y
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,+Z,+X
SYMM -Y,+Z,-X
SYMM +Y,-Z,-X
SYMM -Y,-Z,+X
SYMM 0.5+Y,0.5+X,0.5+Z
SYMM 0.5-Y,0.5-X,0.5+Z
SYMM 0.5+Y,0.5-X,0.5-Z
SYMM 0.5-Y,0.5+X,0.5-Z
SYMM 0.5+X,0.5+Z,0.5+Y
SYMM 0.5-X,0.5+Z,0.5-Y
SYMM 0.5-X,0.5-Z,0.5+Y
SYMM 0.5+X,0.5-Z,0.5-Y
SYMM 0.5+Z,0.5+Y,0.5+X
SYMM 0.5+Z,0.5-Y,0.5-X
SYMM 0.5-Z,0.5+Y,0.5-X
SYMM 0.5-Z,0.5-Y,0.5+X
SFAC  Al 1.913 80.5 0.359 0.454 0.974 3.78 2.638 23.357 0 0 0 0 1.26 26.982
SFAC  Na 1.972 118.259 0.331 0.493 0.985 4.081 1.483 31.374 0 0 0 0 1.55 22.99
SFAC  O 0.392 25.675 0.144 0.306 0.511 2.272 0.937 8.27 0 0 0 0 0.63 15.999
SFAC  Si 1.762 64.441 0.362 0.428 0.974 3.553 2.725 19.406 0 0 0 0 1.16 28.086
UNIT 6 6 24 6

SIMU 0.02 0.04 2 O1 O1A
RIGU
SUMP 0.25 0.0001 1 2 1 3

L.S. 10
PLAN  10
TEMP -98(5)
CONF
MORE -1
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc ".\\2024NCS0186">
REM </olex2.extras>

WGHT    0.335700
EXTI10288.428711
FVAR       4.98813   0.22516   0.02484
SI1   4    0.000000    0.500000    0.250000    10.25000    0.04595    0.04595 =
         0.03052    0.00000    0.00000    0.00000
AL1   1    0.000000    0.750000    0.500000    10.25000    0.02732    0.02152 =
         0.02732    0.00000    0.00000    0.00000
PART 1
O1    3   -0.023736    0.658270    0.344298    10.66667    0.06813    0.03660 =
         0.02742   -0.00195    0.00516   -0.00370
PART 2
O1A   3    0.066566    0.633810    0.366285    10.33333    0.07387    0.03042 =
         0.03330    0.00375   -0.00318    0.00698
PART 1
NA1   2    0.313288    0.686712    0.313288    21.00000    0.11414    0.11414 =
         0.11414   -0.02722    0.02722   -0.02722
PART 2
NA2   2    0.500000    0.500000    0.500000    31.00000    0.05319    0.05319 =
         0.05319    0.00000    0.00000    0.00000
HKLF 4




REM  m_769_772_773_774_776_cf_c.res in P-43n
REM wR2 = 0.4033, GooF = S = 1.059, Restrained GooF = 1.024 for all data
REM R1 = 0.1554 for 161 Fo > 4sig(Fo) and 0.1784 for all 257 data
REM 30 parameters refined using 22 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.254,  deepest hole -0.159,  1-sigma level  0.072
Q1    1   0.5842  0.4159  0.5309  11.00000  0.05    0.25
Q2    1   0.5033  0.4158  0.5780  11.00000  0.05    0.24
Q3    1   0.2815  0.7185  0.2815  10.33333  0.05    0.17
Q4    1   0.2173  0.7827  0.2173  10.33333  0.05    0.16
Q5    1   0.4373  0.5159  0.2740  11.00000  0.05    0.13
Q6    1   0.2780  0.7156  0.4256  11.00000  0.05    0.05
Q7    1  -0.1695  0.6557  0.3509  11.00000  0.05    0.04
Q8    1  -0.1482  0.6473  0.3233  11.00000  0.05    0.04
Q9    1   0.4074  0.7024  0.2522  11.00000  0.05    0.01
Q10   1   0.1754  0.6135  0.3455  11.00000  0.05    0.01
;
_shelx_res_checksum              83948
_exptl.crystals_number           5
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.815
_oxdiff_exptl_absorpt_empirical_full_min 0.550
_vrf_PLAT020_2024NCS0186         
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.250 Report
RESPONSE: This dataset has been derived from merging 5 individual data
collections of 3DED data. The merging, together with dynamical effects often
result in higher Rint values, however, this is considered acceptable for this
structure. No in depth analysis is performed on this structure.
;
_vrf_PLAT082_2024NCS0186         
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE: This structure has been refined employing the kinematical
approximation on data obtained from a 3DED experiment, where dynamical effects
occur. This can lead to higher R1 values, but in-depth analysis of the crystal
structure is not performed.
;
_vrf_PLAT084_2024NCS0186         
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.40 Report
RESPONSE: This structure has been refined employing the kinematical
approximation on data obtained from a 3DED experiment, where dynamical effects
occur. This can lead to higher wR2 values, but in-depth analysis of the crystal
structure is not performed.
;
_vrf_PLAT089_2024NCS0186         
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       5.17 Note  
RESPONSE: Thermal restraints and a restraint on the occupancy of the
extra-framework sodium ions were applied. Together with the high symmetry and
small unit cell paramaters, these led to a slightly lower data/parameter ratio.
However, this is still considered acceptable for the level of analysis required
for this study.
;
_vrf_RINTA01_2024NCS0186         
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: This dataset has been derived from merging 5 individual data
collections of 3DED data. The merging, together with dynamical effects often
result in higher Rint values, however, this is considered acceptable for this
structure. No in depth analysis is performed on this structure.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2024NCS0187
_database_code_depnum_ccdc_archive 'CCDC 2432427'
loop_
_audit_author_name
_audit_author_address
'Daniel N. Rainer'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2025-03-19 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_audit_creation_date             2025-03-19
_audit_creation_method           
;
Olex2 1.5-ac7-014
(compiled 2025.02.27 svn.r6f4c0eaf for Rigaku Oxford Diffraction, GUI svn.r7171)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Al Na0.901 O4 Si, 0.099(Na)'
_chemical_formula_sum            'Al Na O4 Si'
_chemical_formula_weight         142.05
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Si Al O C H Na'
_chemical_oxdiff_usercomment     
;
'Agar holey carbon grid, grid into vial + shake, cryo transfer (no plunging) @
175 K, coll @ 175 K'
;
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   9.0718(9)
_cell_length_b                   9.0718(9)
_cell_length_c                   9.0718(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     746.6(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    269
_cell_measurement_temperature    175(5)
_cell_measurement_theta_max      0.8500
_cell_measurement_theta_min      0.1090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.44.47a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'white (bulk)'
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             146
_exptl_crystal_preparation       
;
grid placed in sample vial, vial manually shaken
;
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.5615
_diffrn_reflns_av_unetI/netI     0.1203
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10280
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.900
_diffrn_reflns_theta_min         0.112
_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      175(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector.description     'Hybrid Pixel Array Detector'
_diffrn_detector.make            'Rigaku HyPix-ED'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku HyPix-ED'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement.rotation_mode rotation
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00  60.00   0.25    0.25    --    0.00   0.00   0.00  480
  2  ω    -60.00  60.00   0.25    0.50    --    0.00   0.00   0.00  480
  3  ω    -64.00  62.00   0.25    0.50    --    0.00   0.00   0.00  504
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_measurement_specimen_support 
;
holey carbon copper grid, 200 mesh; Gatan Elsa cryo-transfer holder 698
;
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0023743000
_diffrn_orient_matrix_UB_12      0.0012709000
_diffrn_orient_matrix_UB_13      -0.0006628000
_diffrn_orient_matrix_UB_21      0.0014213000
_diffrn_orient_matrix_UB_22      -0.0019277000
_diffrn_orient_matrix_UB_23      0.0013907000
_diffrn_orient_matrix_UB_31      0.0001876000
_diffrn_orient_matrix_UB_32      -0.0015293000
_diffrn_orient_matrix_UB_33      -0.0022954000
_diffrn_oxdiff_ac3_digest_hkl    41dbf3c7ae15aa4ba49cae3e78af31cd411f87
_diffrn_oxdiff_digest_creation   
;
CAP 1.171.44.47a, AC 1.5-ac6-020
;
_diffrn_oxdiff_digest_dyn_ed     
;
6148fcd2cf77428327587db2623698d14b5758
;
_diffrn_oxdiff_digest_hkl_ed     
;
53c81d996c30de6628244f3c0a3abbf0648a93
;
_diffrn_radiation.wavelength     0.0251
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'electron gun'
_diffrn_source.description       'electron gun'
_diffrn_source.ed_diffracting_area_selection SAED
_diffrn_source.make              LaB6
_diffrn_source.voltage           200
_diffrn_source_details           LaB6
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_diffrn_source_voltage           200
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                184
_reflns_number_total             261
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.44.47a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.118a 64-bit (release 27-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.44.47a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine.diffraction_theory       kinematical
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       9748(124)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         261
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.2034
_refine_ls_R_factor_gt           0.1831
_refine_ls_restrained_S_all      0.972
_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/[σ²(Fo²)+(0.3249P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4271
_refine_ls_wR_factor_ref         0.4606
_refine_special_details          
;
An extinction correction parameter (EXTI) was refined to account roughly for
dynamical effects in the kinematical refinement of 3D ED data.
A global rigid bond restraint (RIGU) was applied to achieve more sensible
AADPs.
Besides the atom sites building up the zeolite framework (Si1, Al1, O1), there
are 3 distinct maxima in the difference map, which were assigned as sodium
atoms, whose combined occupancy was effectively constrained to 1/4, to charge
balance the present aluminium. However, the presence of protons or additional
sodium sites cannot be excluded. Additionally, thermal restraints (ISOR on Na1,
SIMU on Na1, Na2) were employed to ensure sensible AADPs of these atoms.
;
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Na2 \\sim Na1: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(Na1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 1*[Sof(Na1)]+1*[Sof(Na2)]+1*[Sof(Na3)]=0.25 with esd of 0.0001
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.500000 1.000000 0.250000 0.011(3) Uani 1 4 d S T P . .
Al1 Al 0.750000 1.000000 0.500000 0.012(3) Uani 1 4 d S T P . .
O1 O 0.6432(12) 0.9608(12) 0.3490(12) 0.019(3) Uani 1 1 d . . . . .
Na1 Na 0.779(3) 0.779(3) 0.221(3) 0.012(5) Uani 0.339(13) 3 d S TU P . 1
Na2 Na 0.691(3) 0.691(3) 0.309(3) 0.014(5) Uani 0.337(13) 3 d S TU P . 2
Na3 Na 0.500000 0.500000 0.500000 0.07(6) Uani 0.30(5) 12 d S T P A 3

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 0.012(4) 0.012(4) 0.007(5) 0.000 0.000 0.000
Al1 0.011(5) 0.012(4) 0.012(4) 0.000 0.000 0.000
O1 0.020(5) 0.016(5) 0.021(5) -0.006(4) -0.009(3) 0.007(3)
Na1 0.012(5) 0.012(5) 0.012(5) 0.001(5) 0.001(5) -0.001(5)
Na2 0.014(5) 0.014(5) 0.014(5) -0.002(5) -0.002(5) 0.002(5)
Na3 0.07(6) 0.07(6) 0.07(6) 0.000 0.000 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Al1 O1 1.715(8) . ?
Al1 O1 1.715(8) 19_664 ?
Al1 O1 1.715(7) 4_576 ?
Al1 O1 1.715(7) 18_656 ?
Al1 Na1 3.239(6) . ?
Al1 Na1 3.239(6) 4_576 ?
Al1 Na1 3.239(6) 16_655 ?
Al1 Na1 3.239(6) 14_665 ?
O1 Na2 2.51(2) . ?
O1 Na1 2.363(16) . ?
O1 Si1 1.619(7) . ?

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
O1 Al1 O1 108.6(5) . 19_664 ?
O1 Al1 O1 108.6(5) 19_664 4_576 ?
O1 Al1 O1 111.2(9) . 4_576 ?
O1 Al1 O1 111.2(9) 19_664 18_656 ?
O1 Al1 O1 108.6(5) . 18_656 ?
O1 Al1 O1 108.6(5) 4_576 18_656 ?
O1 Al1 Na1 106.7(9) 18_656 4_576 ?
O1 Al1 Na1 142.9(8) 19_664 14_665 ?
O1 Al1 Na1 67.7(4) 18_656 . ?
O1 Al1 Na1 106.7(9) 19_664 . ?
O1 Al1 Na1 106.7(9) 4_576 16_655 ?
O1 Al1 Na1 142.9(8) 4_576 . ?
O1 Al1 Na1 45.1(4) 19_664 16_655 ?
O1 Al1 Na1 45.1(4) 4_576 4_576 ?
O1 Al1 Na1 142.9(8) 18_656 16_655 ?
O1 Al1 Na1 45.1(4) 18_656 14_665 ?
O1 Al1 Na1 67.7(5) 4_576 14_665 ?
O1 Al1 Na1 106.7(9) . 14_665 ?
O1 Al1 Na1 142.9(8) . 4_576 ?
O1 Al1 Na1 67.7(5) . 16_655 ?
O1 Al1 Na1 67.7(5) 19_664 4_576 ?
O1 Al1 Na1 45.1(4) . . ?
Na1 Al1 Na1 170.8(9) . 4_576 ?
Na1 Al1 Na1 170.8(9) 16_655 14_665 ?
Na1 Al1 Na1 90.37(7) . 14_665 ?
Na1 Al1 Na1 90.37(7) 4_576 14_665 ?
Na1 Al1 Na1 90.37(7) 4_576 16_655 ?
Na1 Al1 Na1 90.37(7) . 16_655 ?
Al1 O1 Na2 102.7(4) . . ?
Al1 O1 Na1 104.0(5) . . ?
Si1 O1 Al1 148.3(8) . . ?
Si1 O1 Na2 105.8(5) . . ?
Si1 O1 Na1 107.4(5) . . ?
O1 Na2 O1 106.6(12) . 8_656 ?
O1 Na2 O1 106.6(12) 11_566 8_656 ?
O1 Na2 O1 106.6(12) . 11_566 ?
O1 Na1 O1 116.8(7) 8_656 . ?
O1 Na1 O1 116.8(7) 11_566 . ?
O1 Na1 O1 116.8(7) 8_656 11_566 ?
O1 Si1 O1 107.9(5) 15_465 2_675 ?
O1 Si1 O1 107.9(5) 15_465 . ?
O1 Si1 O1 112.6(10) . 2_675 ?
O1 Si1 O1 107.9(5) . 16_655 ?
O1 Si1 O1 112.6(10) 15_465 16_655 ?
O1 Si1 O1 107.9(5) 16_655 2_675 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Al1 O1 Si1 O1 -160.7(17) . . . 15_465 ?
Al1 O1 Si1 O1 77.4(12) . . . 16_655 ?
Al1 O1 Si1 O1 -41.6(14) . . . 2_675 ?
O1 Al1 O1 Na2 7.7(12) 18_656 . . . ?
O1 Al1 O1 Na2 -111.7(12) 4_576 . . . ?
O1 Al1 O1 Na2 128.8(13) 19_664 . . . ?
O1 Al1 O1 Na1 -25.7(12) 18_656 . . . ?
O1 Al1 O1 Na1 -145.2(13) 4_576 . . . ?
O1 Al1 O1 Na1 95.3(14) 19_664 . . . ?
O1 Al1 O1 Si1 42.1(15) 4_576 . . . ?
O1 Al1 O1 Si1 161.5(17) 18_656 . . . ?
O1 Al1 O1 Si1 -77.4(12) 19_664 . . . ?
Na2 O1 Si1 O1 -7.3(12) . . . 15_465 ?
Na2 O1 Si1 O1 111.8(12) . . . 2_675 ?
Na2 O1 Si1 O1 -129.2(13) . . . 16_655 ?
Na1 Al1 O1 Na1 114.7(7) 16_655 . . . ?
Na1 Al1 O1 Na1 172.8(7) 4_576 . . . ?
Na1 Al1 O1 Na1 -73.1(12) 14_665 . . . ?
Na1 Al1 O1 Si1 -58.0(17) 16_655 . . . ?
Na1 Al1 O1 Si1 -173(2) . . . . ?
Na1 Al1 O1 Si1 114.1(15) 14_665 . . . ?
Na1 Al1 O1 Si1 0(2) 4_576 . . . ?
Na1 O1 Si1 O1 -95.2(15) . . . 16_655 ?
Na1 O1 Si1 O1 145.7(13) . . . 2_675 ?
Na1 O1 Si1 O1 26.7(12) . . . 15_465 ?

_shelx_res_file                  
;
TITL exp_757_759_761_cp_a.res in P-43n
    exp_757_759_761_cp.res
    created by SHELXL-2019/3 at 13:53:59 on 18-Mar-2025
REM Old TITL exp_757_759_761_cp_a.res in P-43n
REM SHELXT solution in P-43n: R1 0.165, Rweak 0.133, Alpha 0.037
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.159 ( 0.148 ) from 59 Parsons' quotients
REM Formula found by SHELXT: O8 Si17 I3
CELL 0.0251 9.0718 9.0718 9.0718 90 90 90
ZERR 6 0.0009 0.0009 0.0009 0 0 0
LATT -1
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SYMM +Z,+X,+Y
SYMM +Z,-X,-Y
SYMM -Z,-X,+Y
SYMM -Z,+X,-Y
SYMM +Y,+Z,+X
SYMM -Y,+Z,-X
SYMM +Y,-Z,-X
SYMM -Y,-Z,+X
SYMM 0.5+Y,0.5+X,0.5+Z
SYMM 0.5-Y,0.5-X,0.5+Z
SYMM 0.5+Y,0.5-X,0.5-Z
SYMM 0.5-Y,0.5+X,0.5-Z
SYMM 0.5+X,0.5+Z,0.5+Y
SYMM 0.5-X,0.5+Z,0.5-Y
SYMM 0.5-X,0.5-Z,0.5+Y
SYMM 0.5+X,0.5-Z,0.5-Y
SYMM 0.5+Z,0.5+Y,0.5+X
SYMM 0.5+Z,0.5-Y,0.5-X
SYMM 0.5-Z,0.5+Y,0.5-X
SYMM 0.5-Z,0.5-Y,0.5+X
SFAC  Al 1.913 80.5 0.359 0.454 0.974 3.78 2.638 23.357 0 0 0 0 1.26 26.982
SFAC  Na 1.972 118.259 0.331 0.493 0.985 4.081 1.483 31.374 0 0 0 0 1.55 22.99
SFAC  O 0.392 25.675 0.144 0.306 0.511 2.272 0.937 8.27 0 0 0 0 0.63 15.999
SFAC  Si 1.762 64.441 0.362 0.428 0.974 3.553 2.725 19.406 0 0 0 0 1.16 28.086
UNIT 6 6 24 6

RIGU 0.001 0.001
ISOR 0.01 0.02 Na1
SIMU 0.01 0.02 2 Na2 Na1
SUMP 0.25 0.0001 1 2 1 3 1 4

L.S. 10
PLAN  5
TEMP -98(5)
CONF
CONN 3 Na1
CONN 6 Na2
list 4
MORE -1
fmap 2
acta
OMIT 0 5 5
REM <olex2.extras>
REM <HklSrc ".\\2024NCS0187">
REM </olex2.extras>

WGHT    0.324900    0.500000
EXTI 9748.045898
FVAR       0.53508   0.11292   0.11224   0.02485
SI1   4    0.500000    1.000000    0.250000    10.25000    0.01219    0.01219 =
         0.00736    0.00000    0.00000    0.00000
AL1   1    0.750000    1.000000    0.500000    10.25000    0.01109    0.01217 =
         0.01217    0.00000    0.00000    0.00000
O1    3    0.643185    0.960842    0.349010    11.00000    0.02003    0.01575 =
         0.02106   -0.00567   -0.00892    0.00659
PART 1
NA1   2    0.778712    0.778712    0.221288    21.00000    0.01211    0.01211 =
         0.01211    0.00140    0.00140   -0.00140
PART 0
PART 2
NA2   2    0.691322    0.691322    0.308678    31.00000    0.01374    0.01374 =
         0.01374   -0.00161   -0.00161    0.00161
PART0
PART 3
NA3   2    0.500000    0.500000    0.500000    41.00000    0.06622    0.06622 =
         0.06622    0.00000    0.00000    0.00000
HKLF 4




REM  exp_757_759_761_cp_a.res in P-43n
REM wR2 = 0.4606, GooF = S = 1.045, Restrained GooF = 0.972 for all data
REM R1 = 0.1831 for 184 Fo > 4sig(Fo) and 0.2034 for all 261 data
REM 25 parameters refined using 40 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.719,  deepest hole -0.217,  1-sigma level  0.117
Q1    1   0.5761  0.5761  0.5761  10.33333  0.05    0.52
Q2    1   0.5000  0.6747  0.5000  10.50000  0.05    0.40
Q3    1   0.7572  0.7572  0.2428  10.33333  0.05    0.28
Q4    1   0.7346  0.7346  0.2654  10.33333  0.05    0.27
Q5    1   0.6663  0.9106  0.3843  11.00000  0.05    0.13
;
_shelx_res_checksum              74852
_exptl.crystals_number           3
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.922
_oxdiff_exptl_absorpt_empirical_full_min 0.265
_vrf_PLAT020_2024NCS0187         
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.562 Report
RESPONSE: This dataset has been derived from merging 5 individual data
collections of 3DED data. The merging, together with dynamical effects often
result in higher Rint values, however, this is considered acceptable for this
structure. No in depth analysis is performed on this structure.
;
_vrf_PLAT082_2024NCS0187         
;
PROBLEM: High R1 Value ..................................       0.18 Report
RESPONSE: This structure has been refined employing the kinematical
approximation on data obtained from a 3DED experiment, where dynamical effects
occur. This can lead to higher R1 values. Additionally, the data
quality of both the individual collections and the merged dataset is
relatively poor. However, in-depth analysis of the crystal structure is not
performed and the quality of the structure adequate for this particular study.
structure is not performed.
;
_vrf_PLAT084_2024NCS0187         
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.46 Report
RESPONSE: This structure has been refined employing the kinematical
approximation on data obtained from a 3DED experiment, where dynamical
effects occur. This can lead to higher wR2 values. Additionally, the data
quality of both the individual collections and the merged dataset is
relatively poor. However, in-depth analysis of the crystal structure is not
performed and the quality of the structure adequate for this particular study.
;
_vrf_RINTA01_2024NCS0187         
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: This dataset has been derived from merging 5 individual data
collections of 3DED data. The merging, together with dynamical effects often
result in higher Rint values, however, this is considered acceptable for this
structure. No in depth analysis is performed on this structure.
;
