# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_jcr255_auto
_database_code_depnum_ccdc_archive 'CCDC 2293848'
loop_
_audit_author_name
_audit_author_address
'Jan-Christian Raabe'
;University Hamburg
Germany
;
_audit_update_record             
;
2023-09-08 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
JanChristian.Raabe@uni-hamburg.de
maximilian.poller@uni-hamburg.de
jakob.albert@uni-hamburg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Na6 O48 Sb W6, 4(O)'
_chemical_formula_sum            'Na6 H1 Sb1 W6 O24'
_chemical_formula_weight         2194.79
_chemical_melting_point          ?
_chemical_oxdiff_formula         Na7SbW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 06.01.2023, Mo, 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5698(5)
_cell_length_b                   10.9770(4)
_cell_length_c                   11.3410(5)
_cell_angle_alpha                69.081(4)
_cell_angle_beta                 85.409(4)
_cell_angle_gamma                69.784(4)
_cell_volume                     1151.98(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    51314
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      32.5430
_cell_measurement_theta_min      2.6990
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.164
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             977
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72269
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.776
_diffrn_reflns_theta_min         2.303
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  62.00   1.00   12.50    --  -17.86  19.00-120.00   89
  2  ω    -42.00  15.00   1.00   12.50    --  -17.86 -77.00 -30.00   57
  3  ω    -94.00 -43.00   1.00   12.50    --  -17.86 154.00 173.50   51
  4  ω     -9.00  92.00   1.00   12.50    --   18.80  57.00-150.00  101
  5  ω    -42.00  51.00   1.00   12.50    --   18.80 -77.00  60.00   93
  6  ω     -9.00  92.00   1.00   12.50    --   18.80  57.00 -30.00  101
  7  ω    -53.00  47.00   1.00   12.50    --   18.80 -57.00 -60.00  100
  8  ω     -6.00  93.00   1.00   12.50    --   18.80  38.00 120.00   99
  9  ω     -6.00  93.00   1.00   12.50    --   18.80  38.00   0.00   99
 10  ω     -5.00  67.00   1.00   12.50    --   18.80-112.00-161.52   72
 11  ω    -93.00 -42.00   1.00   12.50    --  -17.86 153.00 -29.97   51
 12  ω    -42.00  15.00   1.00   12.50    --  -17.86 -77.00  90.00   57
 13  ω    -50.00  21.00   1.00   12.50    --  -17.86  77.00 120.00   71
 14  ω    -75.00 -28.00   1.00   12.50    --  -17.86 126.00  32.77   47
 15  ω    -75.00 -28.00   1.00   12.50    --  -17.86 126.00  80.20   47
 16  ω    -94.00 -43.00   1.00   12.50    --  -17.86 154.00-118.92   51
 17  ω     39.00 108.00   1.00   12.50    --   18.80 178.00 -60.00   69
 18  ω    -69.00 107.00   1.00   12.50    --   18.80   0.00-180.00  176
 19  ω    -69.00 107.00   1.00   12.50    --   18.80   0.00-120.00  176
 20  ω    -69.00 107.00   1.00   12.50    --   18.80   0.00 -90.00  176
 21  ω    -69.00 107.00   1.00   12.50    --   18.80   0.00-150.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0292666000
_diffrn_orient_matrix_UB_12      0.0308368000
_diffrn_orient_matrix_UB_13      -0.0561870000
_diffrn_orient_matrix_UB_21      0.0508210000
_diffrn_orient_matrix_UB_22      -0.0651084000
_diffrn_orient_matrix_UB_23      0.0082308000
_diffrn_orient_matrix_UB_31      -0.0410751000
_diffrn_orient_matrix_UB_32      -0.0149247000
_diffrn_orient_matrix_UB_33      -0.0356282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7973
_reflns_number_total             8114
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         6.729
_refine_diff_density_min         -1.888
_refine_diff_density_rms         0.258
_refine_ls_extinction_coef       0.00212(8)
_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   1.136
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         8114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0254
_refine_ls_restrained_S_all      1.136
_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)+(0.0290P)²+9.2027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0689
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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
W1 W -0.30845(2) 0.16317(2) 0.05538(2) 0.00582(4) Uani 1 1 d . . . . .
W2 W -0.10418(2) -0.08527(2) 0.28697(2) 0.00575(4) Uani 1 1 d . . . . .
W3 W 0.20331(2) -0.24869(2) 0.22945(2) 0.00584(4) Uani 1 1 d . . . . .
Sb1 Sb 0.000000 0.000000 0.000000 0.00335(6) Uani 1 2 d S . P . .
O1 O 0.0022(3) 0.1696(3) -0.1417(3) 0.0059(4) Uani 1 1 d . . . . .
O2 O -0.1851(3) 0.0556(3) -0.0708(3) 0.0065(5) Uani 1 1 d . . . . .
O3 O -0.0946(3) 0.0945(3) 0.1188(3) 0.0061(5) Uani 1 1 d . . . . .
O4 O -0.2663(3) -0.0216(3) 0.1828(3) 0.0084(5) Uani 1 1 d . . . . .
O5 O -0.3708(3) 0.2630(3) 0.1519(3) 0.0115(5) Uani 1 1 d . . . . .
O6 O -0.2677(3) 0.3049(3) -0.0850(3) 0.0082(5) Uani 1 1 d . . . . .
O7 O -0.4522(3) 0.1590(3) -0.0069(3) 0.0117(5) Uani 1 1 d . . . . .
O8 O 0.0879(3) -0.1287(3) 0.3162(3) 0.0085(5) Uani 1 1 d . . . . .
O9 O -0.1193(3) -0.2430(3) 0.3842(3) 0.0121(5) Uani 1 1 d . . . . .
O10 O -0.1562(3) 0.0195(3) 0.3794(3) 0.0121(5) Uani 1 1 d . . . . .
O11 O 0.3517(3) -0.2540(3) 0.2903(3) 0.0136(6) Uani 1 1 d . . . . .
O12 O 0.1840(3) -0.4070(3) 0.3236(3) 0.0111(5) Uani 1 1 d . . . . .
Na1 Na 0.4260(2) -0.5851(2) 0.64963(19) 0.0201(4) Uani 1 1 d . . . . .
Na2 Na 0.1148(2) -0.43124(19) 0.73987(18) 0.0141(3) Uani 1 1 d . . . . .
Na3 Na -0.2166(2) -0.2530(2) 0.78422(19) 0.0198(4) Uani 1 1 d . . . . .
OW1 O 0.5244(7) -0.4063(5) 0.5651(4) 0.0492(15) Uani 1 1 d . . . . .
OW2 O 0.4140(4) -0.8118(4) 0.7691(4) 0.0236(8) Uani 1 1 d . . . . .
OW3 O 0.3451(4) -0.5042(3) 0.8247(3) 0.0160(6) Uani 1 1 d . . . . .
OW4 O 0.2018(4) -0.5358(3) 0.5882(3) 0.0147(6) Uani 1 1 d . . . . .
OW5 O 0.1854(6) -0.2595(4) 0.5840(4) 0.0342(11) Uani 1 1 d . . . . .
OW6 O 0.1021(4) -0.6420(3) 0.8834(3) 0.0173(6) Uani 1 1 d . . . . .
OW7 O -0.1087(3) -0.3701(3) 0.6518(3) 0.0128(5) Uani 1 1 d . . . . .
OW8 O 0.0103(4) -0.3083(4) 0.8740(3) 0.0194(7) Uani 1 1 d . . . . .
OW9 O -0.1916(4) -0.0503(4) 0.6368(3) 0.0167(6) Uani 1 1 d . . . . .
OW10 O -0.3360(3) -0.4115(4) 0.8952(4) 0.0186(6) Uani 1 1 d . . . . .
OW11 O -0.3045(5) -0.1275(6) 0.9156(6) 0.0513(17) Uani 1 1 d . . . . .
OW12 O -0.4148(4) 0.0727(4) 0.6611(4) 0.0271(8) Uani 1 1 d . . . . .
OW13 O -0.4593(7) -0.1319(7) 0.6614(6) 0.0567(15) Uani 1 1 d . . . . .
OW14 O -0.5553(11) -0.1421(11) 0.5680(9) 0.102(3) Uani 1 1 d . . . . .


_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
W1 O2 2.233(3) . ?
W1 O3 2.211(3) . ?
W1 O4 1.946(3) . ?
W1 O5 1.753(3) . ?
W1 O6 1.930(3) . ?
W1 O7 1.747(3) . ?
W2 O1 2.201(3) 2 ?
W2 O3 2.227(3) . ?
W2 O4 1.931(3) . ?
W2 O8 1.946(3) . ?
W2 O9 1.744(3) . ?
W2 O10 1.748(3) . ?
W3 O1 2.211(3) 2 ?
W3 O2 2.194(3) 2 ?
W3 O6 1.944(3) 2 ?
W3 O8 1.953(3) . ?
W3 O11 1.738(3) . ?
W3 O12 1.756(3) . ?
Sb1 O1 1.984(3) . ?
Sb1 O1 1.984(3) 2 ?
Sb1 O2 1.980(3) 2 ?
Sb1 O2 1.980(3) . ?
Sb1 O3 1.989(3) . ?
Sb1 O3 1.989(3) 2 ?
O11 Na1 2.374(4) 2_646 ?
Na1 OW1 2.478(5) 2_646 ?
Na1 OW1 2.401(5) . ?
Na1 OW2 2.415(4) . ?
Na1 OW3 2.434(4) . ?
Na1 OW4 2.346(4) . ?
Na2 OW3 2.444(4) . ?
Na2 OW4 2.356(4) . ?
Na2 OW5 2.370(5) . ?
Na2 OW6 2.347(4) . ?
Na2 OW7 2.415(4) . ?
Na2 OW8 2.350(4) . ?
Na3 OW7 2.302(4) . ?
Na3 OW8 2.470(5) . ?
Na3 OW9 2.344(4) . ?
Na3 OW10 2.430(4) . ?
Na3 OW11 2.311(4) . ?
Na3 OW13 2.679(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
O3 W1 O2 72.98(10) . . ?
O4 W1 O2 85.53(11) . . ?
O4 W1 O3 73.08(11) . . ?
O5 W1 O2 165.34(12) . . ?
O5 W1 O3 95.24(13) . . ?
O5 W1 O4 99.58(13) . . ?
O5 W1 O6 96.91(13) . . ?
O6 W1 O2 73.97(11) . . ?
O6 W1 O3 85.66(11) . . ?
O6 W1 O4 154.10(12) . . ?
O7 W1 O2 88.47(12) . . ?
O7 W1 O3 158.08(12) . . ?
O7 W1 O4 94.37(13) . . ?
O7 W1 O5 104.70(15) . . ?
O7 W1 O6 100.62(13) . . ?
O1 W2 O3 73.18(10) 2 . ?
O4 W2 O1 85.09(11) . 2 ?
O4 W2 O3 72.99(11) . . ?
O4 W2 O8 154.32(12) . . ?
O8 W2 O1 73.91(11) . 2 ?
O8 W2 O3 86.68(11) . . ?
O9 W2 O1 93.12(13) . 2 ?
O9 W2 O3 163.14(12) . . ?
O9 W2 O4 96.54(13) . . ?
O9 W2 O8 99.14(14) . . ?
O9 W2 O10 104.04(14) . . ?
O10 W2 O1 161.05(12) . 2 ?
O10 W2 O3 91.08(12) . . ?
O10 W2 O4 100.62(14) . . ?
O10 W2 O8 95.16(14) . . ?
O2 W3 O1 73.02(10) 2 2 ?
O6 W3 O1 87.01(11) 2 2 ?
O6 W3 O2 74.60(11) 2 2 ?
O6 W3 O8 155.62(12) 2 . ?
O8 W3 O1 73.55(11) . 2 ?
O8 W3 O2 85.54(11) . 2 ?
O11 W3 O1 161.32(13) . 2 ?
O11 W3 O2 92.89(13) . 2 ?
O11 W3 O6 101.28(14) . 2 ?
O11 W3 O8 93.58(14) . . ?
O11 W3 O12 104.16(14) . . ?
O12 W3 O1 91.55(12) . 2 ?
O12 W3 O2 161.72(12) . 2 ?
O12 W3 O6 95.29(13) . 2 ?
O12 W3 O8 99.71(13) . . ?
O1 Sb1 O1 180.0 . 2 ?
O1 Sb1 O3 83.28(11) . 2 ?
O1 Sb1 O3 83.28(11) 2 . ?
O1 Sb1 O3 96.72(11) 2 2 ?
O1 Sb1 O3 96.72(11) . . ?
O2 Sb1 O1 82.78(11) . . ?
O2 Sb1 O1 97.22(11) 2 . ?
O2 Sb1 O1 97.21(11) . 2 ?
O2 Sb1 O1 82.78(11) 2 2 ?
O2 Sb1 O2 180.0 . 2 ?
O2 Sb1 O3 83.50(12) 2 2 ?
O2 Sb1 O3 96.50(12) . 2 ?
O2 Sb1 O3 83.50(12) . . ?
O2 Sb1 O3 96.50(12) 2 . ?
O3 Sb1 O3 180.0 2 . ?
W2 O1 W3 95.53(10) 2 2 ?
Sb1 O1 W2 102.29(12) . 2 ?
Sb1 O1 W3 101.72(12) . 2 ?
W3 O2 W1 94.28(11) 2 . ?
Sb1 O2 W1 101.53(12) . . ?
Sb1 O2 W3 102.45(12) . 2 ?
W1 O3 W2 95.06(10) . . ?
Sb1 O3 W1 101.98(12) . . ?
Sb1 O3 W2 101.25(11) . . ?
W2 O4 W1 115.26(14) . . ?
W1 O6 W3 113.79(14) . 2 ?
W2 O8 W3 113.86(14) . . ?
W3 O11 Na1 137.05(18) . 2_646 ?
O11 Na1 OW1 87.6(2) 2_646 . ?
O11 Na1 OW1 85.83(19) 2_646 2_646 ?
O11 Na1 OW2 71.00(14) 2_646 . ?
O11 Na1 OW3 107.02(14) 2_646 . ?
OW1 Na1 OW1 79.35(18) . 2_646 ?
OW1 Na1 OW2 158.0(2) . . ?
OW1 Na1 OW3 89.92(16) . . ?
OW2 Na1 OW1 103.32(17) . 2_646 ?
OW2 Na1 OW3 91.59(15) . . ?
OW3 Na1 OW1 163.00(18) . 2_646 ?
OW4 Na1 O11 149.58(15) . 2_646 ?
OW4 Na1 OW1 118.6(2) . . ?
OW4 Na1 OW1 84.42(19) . 2_646 ?
OW4 Na1 OW2 83.36(13) . . ?
OW4 Na1 OW3 89.33(14) . . ?
OW4 Na2 OW3 88.86(13) . . ?
OW4 Na2 OW5 77.58(14) . . ?
OW4 Na2 OW7 88.22(13) . . ?
OW5 Na2 OW3 81.54(15) . . ?
OW5 Na2 OW7 99.24(16) . . ?
OW6 Na2 OW3 87.71(13) . . ?
OW6 Na2 OW4 90.61(13) . . ?
OW6 Na2 OW5 164.11(18) . . ?
OW6 Na2 OW7 90.86(13) . . ?
OW6 Na2 OW8 93.21(14) . . ?
OW7 Na2 OW3 176.74(14) . . ?
OW8 Na2 OW3 96.24(14) . . ?
OW8 Na2 OW4 173.75(15) . . ?
OW8 Na2 OW5 99.54(15) . . ?
OW8 Na2 OW7 86.77(14) . . ?
OW7 Na3 OW8 86.53(13) . . ?
OW7 Na3 OW9 88.93(13) . . ?
OW7 Na3 OW10 96.10(13) . . ?
OW7 Na3 OW11 173.67(17) . . ?
OW7 Na3 OW13 97.18(18) . . ?
OW8 Na3 OW13 166.26(18) . . ?
OW9 Na3 OW8 87.63(14) . . ?
OW9 Na3 OW10 156.02(17) . . ?
OW9 Na3 OW13 79.25(18) . . ?
OW10 Na3 OW8 116.02(15) . . ?
OW10 Na3 OW13 76.86(18) . . ?
OW11 Na3 OW8 88.24(18) . . ?
OW11 Na3 OW9 87.29(18) . . ?
OW11 Na3 OW10 89.40(16) . . ?
OW11 Na3 OW13 87.1(2) . . ?
Na1 OW1 Na1 100.65(18) . 2_646 ?
Na1 OW3 Na2 88.44(12) . . ?
Na1 OW4 Na2 92.69(13) . . ?
Na3 OW7 Na2 94.64(13) . . ?
Na2 OW8 Na3 92.04(13) . . ?

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 W3 O11 Na1 -166.3(3) 2 . . 2_646 ?
O2 W3 O11 Na1 -126.1(2) 2 . . 2_646 ?
O6 W3 O11 Na1 -51.3(3) 2 . . 2_646 ?
O8 W3 O11 Na1 148.2(2) . . . 2_646 ?
O12 W3 O11 Na1 47.2(3) . . . 2_646 ?

_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 1.598
_oxdiff_exptl_absorpt_empirical_full_min 0.802

# start Validation Reply Form
_vrf_PLAT971_jcr255_auto         
;
PROBLEM: Check Calcd Resid. Dens. 1.03Ang From Ow12 6.63 eA-3
RESPONSE: The "Residuel Density" results from disordered hydration
water molecules.
;
_vrf_PLAT975_jcr255_auto         
;
PROBLEM: Check Calcd Resid. Dens. 1.03Ang From Ow12 . 6.63 eA-3
RESPONSE: The "Residuel Density" results from disordered hydration
water molecules.
;
_vrf_PLAT306_jcr255_auto         
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow1 Check
RESPONSE: The oxygen atoms belong to hydration water molecules, of
which the hydrogen atoms were not modeled.
;
_vrf_PLAT976_jcr255_auto         
;
PROBLEM: Check Calcd Resid. Dens. 0.59Ang From Ow14 . -1.84 eA-3
RESPONSE: The "Residuel Density" results from disordered hydration
water molecules.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# 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_jcr253-2_auto
_database_code_depnum_ccdc_archive 'CCDC 2293849'
loop_
_audit_author_name
_audit_author_address
'Jan-Christian Raabe'
;University Hamburg
Germany
;
_audit_update_record             
;
2023-09-08 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_audit_creation_date             2023-04-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Na6 O76 P4 W14, 2.5(O)'
_chemical_formula_sum            'Na6 H6 P4 W14 O58'
_chemical_formula_weight         4091.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         Na7PW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 15.02.2023, Mo, 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8321(2)
_cell_length_b                   12.6641(3)
_cell_length_c                   15.4456(3)
_cell_angle_alpha                99.1067(16)
_cell_angle_beta                 91.2955(16)
_cell_angle_gamma                104.3378(18)
_cell_volume                     2022.72(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    56046
_cell_measurement_temperature    99.92(18)
_cell_measurement_theta_max      29.3570
_cell_measurement_theta_min      2.8500
_shelx_estimated_absorpt_T_max   0.123
_shelx_estimated_absorpt_T_min   0.060
_exptl_absorpt_coefficient_mu    20.037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            88070
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.455
_diffrn_reflns_theta_min         2.288
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.92(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00 -43.00   1.00   20.00    --   -9.92 154.00  82.20   43
  2  ω    -15.00  31.00   1.00   20.00    --   -9.92 -99.00   0.00   46
  3  ω    -86.00 -43.00   1.00   20.00    --   -9.92 154.00 163.41   43
  4  ω    -85.00 -42.00   1.00   20.00    --   -9.92 153.00 -28.92   43
  5  ω    -69.00  27.00   1.00   20.00    --   10.55 -19.00-180.00   96
  6  ω    -69.00  27.00   1.00   20.00    --   10.55 -19.00   0.00   96
  7  ω      2.00  63.00   1.00   20.00    --   10.55-120.00 -25.80   61
  8  ω    -14.00  85.00   1.00   20.00    --   10.55  38.00-180.00   99
  9  ω    -27.00  91.00   1.00   20.00    --   10.55  19.00   0.00  118
 10  ω    -84.00 -41.00   1.00   20.00    --   -9.92 152.00-104.93   43
 11  ω    -15.00  31.00   1.00   20.00    --   -9.92 -99.00 150.00   46
 12  ω    -85.00 -42.00   1.00   20.00    --   -9.92 153.00  17.67   43
 13  ω    -69.00 -30.00   1.00   20.00    --   -9.92 129.00 -46.76   39
 14  ω    -42.00  23.00   1.00   20.00    --   -9.92 -77.00-120.00   65
 15  ω    -43.00  21.00   1.00   20.00    --   -9.92  77.00 -90.00   64
 16  ω    -15.00  31.00   1.00   20.00    --   -9.92 -99.00 -60.00   46
 17  ω    -81.00 -38.00   1.00   20.00    --   -9.92 148.00  -8.82   43
 18  ω    -69.00 -30.00   1.00   20.00    --   -9.92 129.00-118.80   39
 19  ω    -43.00  21.00   1.00   20.00    --   -9.92  77.00   0.00   64
 20  ω    -42.00  23.00   1.00   20.00    --   -9.92 -77.00-150.00   65
 21  ω    -43.00  21.00   1.00   20.00    --   -9.92  77.00 -60.00   64
 22  ω    -78.00  30.00   1.00   20.00    --   10.55   0.00-150.00  108
 23  ω    -78.00  99.00   1.00   20.00    --   10.55   0.00-180.00  177
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0379700000
_diffrn_orient_matrix_UB_12      -0.0370519000
_diffrn_orient_matrix_UB_13      -0.0138964000
_diffrn_orient_matrix_UB_21      -0.0340321000
_diffrn_orient_matrix_UB_22      -0.0146716000
_diffrn_orient_matrix_UB_23      -0.0417207000
_diffrn_orient_matrix_UB_31      0.0445774000
_diffrn_orient_matrix_UB_32      0.0430380000
_diffrn_orient_matrix_UB_33      -0.0154399000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10049
_reflns_number_total             10454
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.567
_refine_diff_density_min         -4.396
_refine_diff_density_rms         0.305
_refine_ls_extinction_coef       0.00039(3)
_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   1.076
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         10454
_refine_ls_number_restraints     641
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0283
_refine_ls_restrained_S_all      1.049
_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/[σ²(Fo²)+(0.0313P)²+19.9366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0719
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Restrained distances
 Na3-O9X \\sim Na3-O9W
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(P1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O17) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O9X) = Uanis(O9W)
3. 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
4. Others
 Sof(O9X)=1-FVAR(1)
 Sof(O9W)=FVAR(1)
 Fixed Sof: O28(0.25)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     heavy
_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
W1 W 0.37237(2) 1.08332(2) 0.73505(2) 0.00588(5) Uani 1 1 d . . . . .
W2 W 0.10971(2) 0.84046(2) 0.63875(2) 0.01493(6) Uani 1 1 d . . . . .
W3 W -0.00999(2) 0.65882(2) 0.77093(2) 0.01364(6) Uani 1 1 d . . . . .
W4 W 0.12640(2) 0.72348(2) 1.00190(2) 0.00944(6) Uani 1 1 d . . . . .
W5 W 0.43961(2) 0.70264(2) 0.91176(2) 0.00398(5) Uani 1 1 d . . . . .
W6 W 0.31779(2) 0.66471(2) 0.70007(2) 0.00517(5) Uani 1 1 d . . . . .
W7 W 0.56767(2) 0.88616(2) 0.77745(2) 0.00352(5) Uani 1 1 d . . . . .
P1 P 0.25235(13) 0.87822(11) 0.84988(9) 0.0052(2) Uani 1 1 d . U . . .
P2 P 0.59047(13) 1.13275(11) 0.90237(9) 0.0046(2) Uani 1 1 d . . . . .
Na1 Na 0.1363(2) 1.2634(2) 0.71297(16) 0.0169(5) Uani 1 1 d . . . . .
Na2 Na 0.6662(2) 0.5849(2) 1.05591(17) 0.0157(5) Uani 1 1 d . . . . .
Na3 Na 0.7020(2) 0.92698(18) 0.99505(14) 0.0082(4) Uani 1 1 d D . . . .
O1 O 0.3074(4) 0.9995(3) 0.8454(2) 0.0070(7) Uani 1 1 d . U . . .
O1W O 0.3366(6) 1.3547(5) 0.6680(4) 0.0406(16) Uani 1 1 d . . . . .
O2 O 0.1328(4) 0.8291(4) 0.7850(3) 0.0117(8) Uani 1 1 d . . . . .
O2W O 0.0407(7) 1.3779(6) 0.6362(3) 0.0442(17) Uani 1 1 d . . . . .
O3 O 0.2186(3) 0.8678(3) 0.9433(3) 0.0076(7) Uani 1 1 d . . . . .
O3W O 0.0637(5) 1.1216(4) 0.5857(3) 0.0262(11) Uani 1 1 d . . . . .
O4 O 0.3529(3) 0.8115(3) 0.8220(2) 0.0064(7) Uani 1 1 d . U . . .
O4W O -0.0401(6) 1.1491(8) 0.7720(4) 0.073(3) Uani 1 1 d . . . . .
O5 O 0.2484(4) 0.9674(3) 0.6669(3) 0.0110(8) Uani 1 1 d . . . . .
O5W O 0.5169(5) 0.6110(4) 1.1636(4) 0.0226(10) Uani 1 1 d . . . . .
O6 O 0.0138(4) 0.6964(4) 0.6550(3) 0.0172(9) Uani 1 1 d . . . . .
O6W O 0.8450(4) 0.5808(4) 1.1533(3) 0.0139(8) Uani 1 1 d . . . . .
O7 O 0.0447(4) 0.6646(4) 0.8914(3) 0.0177(9) Uani 1 1 d . . . . .
O7W O 0.7481(5) 0.5204(5) 0.9262(3) 0.0289(12) Uani 1 1 d . . . . .
O8 O 0.2791(4) 0.6701(3) 0.9466(3) 0.0116(8) Uani 1 1 d . . . . .
O8W O 0.7640(4) 0.7800(3) 1.0545(3) 0.0114(8) Uani 1 1 d . . . . .
O9 O 0.5832(3) 0.8033(3) 0.8693(2) 0.0043(7) Uani 1 1 d . . . . .
O9W O 0.8809(8) 0.9234(8) 0.9078(6) 0.0117(12) Uani 0.478(9) 1 d D . P A 1
O10 O 0.4041(3) 0.6177(3) 0.8001(2) 0.0054(7) Uani 1 1 d . . . . .
O11 O 0.5000(4) 0.7578(3) 0.6986(2) 0.0062(7) Uani 1 1 d . . . . .
O12 O 0.4892(4) 0.9724(3) 0.7250(2) 0.0071(7) Uani 1 1 d . U . . .
O13 O 0.2625(4) 0.7569(3) 0.6390(3) 0.0097(7) Uani 1 1 d . . . . .
O14 O 0.1665(4) 0.6120(3) 0.7460(3) 0.0100(8) Uani 1 1 d . . . . .
O15 O 0.5877(3) 1.0096(3) 0.8869(2) 0.0057(7) Uani 1 1 d . . . . .
O16 O 0.5169(4) 1.1635(3) 0.8276(2) 0.0064(7) Uani 1 1 d . U . . .
O17 O 0.7291(4) 1.2023(3) 0.9039(2) 0.0076(7) Uani 1 1 d . U . . .
O18 O 0.5290(3) 1.1610(3) 0.9889(2) 0.0062(7) Uani 1 1 d . . . . .
O19 O 0.4487(4) 1.1429(4) 0.6506(3) 0.0143(8) Uani 1 1 d . . . . .
O20 O 0.2779(4) 1.1733(3) 0.7720(3) 0.0083(7) Uani 1 1 d . . . . .
O21 O 0.1049(5) 0.8202(4) 0.5247(3) 0.0250(11) Uani 1 1 d . . . . .
O22 O -0.0116(5) 0.9066(4) 0.6614(4) 0.0243(11) Uani 1 1 d . . . . .
O23 O -0.0934(4) 0.5221(4) 0.7435(3) 0.0207(10) Uani 1 1 d . . . . .
O24 O -0.1325(5) 0.7259(5) 0.7941(4) 0.0378(15) Uani 1 1 d . . . . .
O25 O 0.0785(4) 0.6102(4) 1.0546(3) 0.0170(9) Uani 1 1 d . . . . .
O26 O 0.0270(4) 0.8073(4) 1.0460(3) 0.0135(8) Uani 1 1 d . . . . .
O27 O 0.5094(4) 0.6187(3) 0.9621(3) 0.0102(8) Uani 1 1 d . . . . .
O29 O 0.3321(4) 0.5569(3) 0.6192(2) 0.0084(7) Uani 1 1 d . . . . .
O35 O 0.9270(4) 0.9350(4) 0.7944(3) 0.0181(9) Uani 1 1 d . . . . .
O36 O 0.7204(4) 0.9219(3) 0.7453(3) 0.0093(7) Uani 1 1 d . . . . .
O9X O 0.9201(7) 0.9676(7) 0.9466(5) 0.0117(12) Uani 0.522(9) 1 d D . P A 2
O28 O -0.1150(15) 1.0240(13) 0.6647(11) 0.012(3) Uiso 0.25 1 d . . P . .


_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
W1 O1 2.187(4) . ?
W1 O5 1.880(4) . ?
W1 O12 2.102(4) . ?
W1 O16 2.044(4) . ?
W1 O19 1.734(4) . ?
W1 O20 1.752(4) . ?
W2 O2 2.298(4) . ?
W2 O5 1.893(4) . ?
W2 O6 1.920(5) . ?
W2 O13 2.174(4) . ?
W2 O21 1.738(5) . ?
W2 O22 1.739(5) . ?
W3 O2 2.297(4) . ?
W3 O6 1.931(5) . ?
W3 O7 1.924(5) . ?
W3 O14 2.162(4) . ?
W3 O23 1.723(4) . ?
W3 O24 1.759(5) . ?
W4 O3 2.195(4) . ?
W4 O7 1.859(4) . ?
W4 O8 2.088(4) . ?
W4 O17 2.046(4) 2_677 ?
W4 O25 1.735(4) . ?
W4 O26 1.766(4) . ?
W5 O4 2.426(4) . ?
W5 O8 1.800(4) . ?
W5 O9 1.950(3) . ?
W5 O10 1.859(4) . ?
W5 O18 2.073(4) 2_677 ?
W5 O27 1.715(4) . ?
W6 O4 2.379(4) . ?
W6 O10 2.030(4) . ?
W6 O11 2.035(4) . ?
W6 O13 1.811(4) . ?
W6 O14 1.815(4) . ?
W6 O29 1.738(4) . ?
W7 O4 2.443(4) . ?
W7 O9 1.921(4) . ?
W7 O11 1.846(4) . ?
W7 O12 1.812(4) . ?
W7 O15 2.080(4) . ?
W7 O36 1.710(4) . ?
P1 O1 1.517(4) . ?
P1 O2 1.553(4) . ?
P1 O3 1.515(4) . ?
P1 O4 1.565(4) . ?
P2 O15 1.533(4) . ?
P2 O16 1.541(4) . ?
P2 O17 1.539(4) . ?
P2 O18 1.538(4) . ?
Na1 Na2 4.057(3) 2_677 ?
Na1 O1W 2.368(6) . ?
Na1 O2W 2.411(6) . ?
Na1 O3W 2.412(6) . ?
Na1 O4W 2.389(7) . ?
Na1 O6W 2.587(5) 2_677 ?
Na1 O20 2.372(5) . ?
Na2 O5W 2.388(6) . ?
Na2 O6W 2.441(5) . ?
Na2 O7W 2.322(6) . ?
Na2 O8W 2.439(5) . ?
Na2 O27 2.769(5) 2_667 ?
Na2 O27 2.368(5) . ?
Na3 O1 2.506(4) 2_677 ?
Na3 O3 2.544(4) 2_677 ?
Na3 O8W 2.428(5) . ?
Na3 O9 2.409(4) . ?
Na3 O9W 2.391(8) . ?
Na3 O15 2.552(4) . ?
Na3 O18 2.509(4) 2_677 ?
Na3 O9X 2.451(8) . ?

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
O5 W1 O1 85.05(16) . . ?
O5 W1 O12 86.01(16) . . ?
O5 W1 O16 159.85(16) . . ?
O12 W1 O1 80.93(14) . . ?
O16 W1 O1 80.02(14) . . ?
O16 W1 O12 78.37(15) . . ?
O19 W1 O1 169.87(17) . . ?
O19 W1 O5 98.7(2) . . ?
O19 W1 O12 89.88(17) . . ?
O19 W1 O16 94.00(18) . . ?
O19 W1 O20 102.28(19) . . ?
O20 W1 O1 86.24(16) . . ?
O20 W1 O5 100.08(18) . . ?
O20 W1 O12 165.30(16) . . ?
O20 W1 O16 92.41(17) . . ?
O5 W2 O2 84.22(16) . . ?
O5 W2 O6 152.63(17) . . ?
O5 W2 O13 81.94(16) . . ?
O6 W2 O2 72.12(17) . . ?
O6 W2 O13 80.07(16) . . ?
O13 W2 O2 78.53(14) . . ?
O21 W2 O2 166.20(19) . . ?
O21 W2 O5 100.8(2) . . ?
O21 W2 O6 99.5(2) . . ?
O21 W2 O13 89.36(19) . . ?
O21 W2 O22 102.2(2) . . ?
O22 W2 O2 89.8(2) . . ?
O22 W2 O5 97.1(2) . . ?
O22 W2 O6 96.3(2) . . ?
O22 W2 O13 168.3(2) . . ?
O6 W3 O2 71.98(16) . . ?
O6 W3 O14 81.00(16) . . ?
O7 W3 O2 84.41(17) . . ?
O7 W3 O6 153.45(18) . . ?
O7 W3 O14 82.72(17) . . ?
O14 W3 O2 78.89(15) . . ?
O23 W3 O2 166.88(18) . . ?
O23 W3 O6 99.9(2) . . ?
O23 W3 O7 100.8(2) . . ?
O23 W3 O14 89.77(19) . . ?
O23 W3 O24 102.4(3) . . ?
O24 W3 O2 88.8(2) . . ?
O24 W3 O6 95.3(3) . . ?
O24 W3 O7 96.2(2) . . ?
O24 W3 O14 167.7(2) . . ?
O7 W4 O3 85.91(17) . . ?
O7 W4 O8 83.82(18) . . ?
O7 W4 O17 159.37(16) . 2_677 ?
O8 W4 O3 79.81(15) . . ?
O17 W4 O3 80.54(15) 2_677 . ?
O17 W4 O8 78.55(16) 2_677 . ?
O25 W4 O3 170.63(19) . . ?
O25 W4 O7 100.1(2) . . ?
O25 W4 O8 93.62(19) . . ?
O25 W4 O17 91.66(19) . 2_677 ?
O25 W4 O26 101.5(2) . . ?
O26 W4 O3 84.20(17) . . ?
O26 W4 O7 101.0(2) . . ?
O26 W4 O8 162.93(18) . . ?
O26 W4 O17 93.04(17) . 2_677 ?
O8 W5 O4 82.58(16) . . ?
O8 W5 O9 151.04(17) . . ?
O8 W5 O10 96.92(18) . . ?
O8 W5 O18 85.22(17) . 2_677 ?
O9 W5 O4 72.43(14) . . ?
O9 W5 O18 78.98(15) . 2_677 ?
O10 W5 O4 74.05(14) . . ?
O10 W5 O9 90.20(15) . . ?
O10 W5 O18 159.92(15) . 2_677 ?
O18 W5 O4 86.50(14) 2_677 . ?
O27 W5 O4 172.07(16) . . ?
O27 W5 O8 102.63(19) . . ?
O27 W5 O9 103.87(17) . . ?
O27 W5 O10 99.20(18) . . ?
O27 W5 O18 99.80(17) . 2_677 ?
O10 W6 O4 72.44(14) . . ?
O10 W6 O11 79.28(15) . . ?
O11 W6 O4 72.55(14) . . ?
O13 W6 O4 86.10(16) . . ?
O13 W6 O10 157.87(17) . . ?
O13 W6 O11 89.37(17) . . ?
O13 W6 O14 96.06(18) . . ?
O14 W6 O4 85.45(15) . . ?
O14 W6 O10 87.74(16) . . ?
O14 W6 O11 156.95(16) . . ?
O29 W6 O4 165.09(16) . . ?
O29 W6 O10 96.45(16) . . ?
O29 W6 O11 95.99(17) . . ?
O29 W6 O13 103.64(18) . . ?
O29 W6 O14 104.40(18) . . ?
O9 W7 O4 72.49(14) . . ?
O9 W7 O15 79.85(15) . . ?
O11 W7 O4 74.05(14) . . ?
O11 W7 O9 91.23(16) . . ?
O11 W7 O15 160.42(15) . . ?
O12 W7 O4 82.90(15) . . ?
O12 W7 O9 151.38(16) . . ?
O12 W7 O11 95.92(17) . . ?
O12 W7 O15 84.42(16) . . ?
O15 W7 O4 86.61(13) . . ?
O36 W7 O4 172.78(16) . . ?
O36 W7 O9 102.77(17) . . ?
O36 W7 O11 100.95(18) . . ?
O36 W7 O12 103.00(18) . . ?
O36 W7 O15 98.02(17) . . ?
O1 P1 O2 110.5(2) . . ?
O1 P1 O4 109.8(2) . . ?
O2 P1 O4 107.3(2) . . ?
O3 P1 O1 108.6(2) . . ?
O3 P1 O2 110.8(2) . . ?
O3 P1 O4 109.8(2) . . ?
O15 P2 O16 112.1(2) . . ?
O15 P2 O17 109.6(2) . . ?
O15 P2 O18 109.1(2) . . ?
O17 P2 O16 106.0(2) . . ?
O18 P2 O16 108.4(2) . . ?
O18 P2 O17 111.7(2) . . ?
O1W Na1 Na2 77.04(19) . 2_677 ?
O1W Na1 O2W 88.1(2) . . ?
O1W Na1 O3W 99.9(2) . . ?
O1W Na1 O4W 167.8(3) . . ?
O1W Na1 O6W 90.9(2) . 2_677 ?
O1W Na1 O20 77.27(18) . . ?
O2W Na1 Na2 115.81(18) . 2_677 ?
O2W Na1 O3W 86.0(2) . . ?
O2W Na1 O6W 84.65(18) . 2_677 ?
O3W Na1 Na2 157.62(16) . 2_677 ?
O3W Na1 O6W 165.5(2) . 2_677 ?
O4W Na1 Na2 97.64(16) . 2_677 ?
O4W Na1 O2W 104.1(3) . . ?
O4W Na1 O3W 80.8(2) . . ?
O4W Na1 O6W 90.7(2) . 2_677 ?
O6W Na1 Na2 35.01(10) 2_677 2_677 ?
O20 Na1 Na2 62.64(11) . 2_677 ?
O20 Na1 O2W 165.3(2) . . ?
O20 Na1 O3W 95.00(19) . . ?
O20 Na1 O4W 90.6(3) . . ?
O20 Na1 O6W 96.89(16) . 2_677 ?
O5W Na2 W5 82.69(13) . 2_667 ?
O5W Na2 O6W 98.99(18) . . ?
O5W Na2 O8W 97.11(17) . . ?
O5W Na2 O27 75.65(16) . 2_667 ?
O6W Na2 W5 81.36(12) . 2_667 ?
O6W Na2 O27 107.83(16) . 2_667 ?
O7W Na2 W5 87.47(15) . 2_667 ?
O7W Na2 O5W 160.4(2) . . ?
O7W Na2 O6W 96.19(19) . . ?
O7W Na2 O8W 95.43(18) . . ?
O7W Na2 O27 87.99(18) . 2_667 ?
O7W Na2 O27 84.70(19) . . ?
O8W Na2 W5 170.24(13) . 2_667 ?
O8W Na2 O6W 89.05(16) . . ?
O8W Na2 O27 162.35(17) . 2_667 ?
O27 Na2 W5 107.70(12) . 2_667 ?
O27 Na2 W5 26.68(9) 2_667 2_667 ?
O27 Na2 O5W 82.25(18) . . ?
O27 Na2 O6W 170.93(18) . . ?
O27 Na2 O8W 81.88(15) . . ?
O27 Na2 O27 81.21(15) . 2_667 ?
O1 Na3 P1 29.17(9) 2_677 2_677 ?
O1 Na3 O3 58.36(13) 2_677 2_677 ?
O1 Na3 O15 115.97(15) 2_677 . ?
O1 Na3 O18 81.64(14) 2_677 2_677 ?
O3 Na3 P1 29.20(9) 2_677 2_677 ?
O3 Na3 O15 79.12(14) 2_677 . ?
O8W Na3 P1 105.01(13) . 2_677 ?
O8W Na3 O1 82.29(14) . 2_677 ?
O8W Na3 O3 125.09(16) . 2_677 ?
O8W Na3 O15 155.77(16) . . ?
O8W Na3 O18 90.61(15) . 2_677 ?
O8W Na3 O9X 84.1(2) . . ?
O9 Na3 P1 154.75(13) . 2_677 ?
O9 Na3 O1 144.10(15) . 2_677 ?
O9 Na3 O3 140.99(16) . 2_677 ?
O9 Na3 O8W 93.47(15) . . ?
O9 Na3 O15 62.34(13) . . ?
O9 Na3 O18 62.70(13) . 2_677 ?
O9 Na3 O9X 102.3(2) . . ?
O9W Na3 P1 114.9(2) . 2_677 ?
O9W Na3 O1 130.6(3) . 2_677 ?
O9W Na3 O3 94.0(3) . 2_677 ?
O9W Na3 O8W 83.7(2) . . ?
O9W Na3 O9 83.7(3) . . ?
O9W Na3 O15 94.4(2) . . ?
O9W Na3 O18 145.6(3) . 2_677 ?
O15 Na3 P1 97.75(11) . 2_677 ?
O18 Na3 P1 99.43(11) 2_677 2_677 ?
O18 Na3 O3 116.51(15) 2_677 2_677 ?
O18 Na3 O15 77.37(13) 2_677 . ?
O9X Na3 O15 101.6(2) . . ?
W1 O1 Na3 131.41(18) . 2_677 ?
P1 O1 W1 131.4(2) . . ?
P1 O1 Na3 97.21(19) . 2_677 ?
W3 O2 W2 93.86(14) . . ?
P1 O2 W2 128.8(2) . . ?
P1 O2 W3 128.6(2) . . ?
W4 O3 Na3 133.01(18) . 2_677 ?
P1 O3 W4 131.2(2) . . ?
P1 O3 Na3 95.77(19) . 2_677 ?
W5 O4 W7 89.19(12) . . ?
W6 O4 W5 90.55(13) . . ?
W6 O4 W7 90.13(12) . . ?
P1 O4 W5 125.9(2) . . ?
P1 O4 W6 123.5(2) . . ?
P1 O4 W7 126.5(2) . . ?
W1 O5 W2 159.6(2) . . ?
W2 O6 W3 121.3(2) . . ?
Na2 O6W Na1 107.54(18) . 2_677 ?
W4 O7 W3 158.6(3) . . ?
W5 O8 W4 149.3(2) . . ?
Na3 O8W Na2 135.4(2) . . ?
W5 O9 Na3 107.80(16) . . ?
W7 O9 W5 124.05(19) . . ?
W7 O9 Na3 109.17(16) . . ?
W5 O10 W6 122.74(19) . . ?
W7 O11 W6 123.11(19) . . ?
W7 O12 W1 148.7(2) . . ?
W6 O13 W2 139.4(2) . . ?
W6 O14 W3 138.8(2) . . ?
W7 O15 Na3 99.18(15) . . ?
P2 O15 W7 135.5(2) . . ?
P2 O15 Na3 121.6(2) . . ?
P2 O16 W1 136.6(2) . . ?
P2 O17 W4 136.0(2) . 2_677 ?
W5 O18 Na3 100.45(15) 2_677 2_677 ?
P2 O18 W5 135.1(2) . 2_677 ?
P2 O18 Na3 120.2(2) . 2_677 ?
W1 O20 Na1 138.9(2) . . ?
W5 O27 Na2 106.86(19) . 2_667 ?
W5 O27 Na2 153.5(2) . . ?
Na2 O27 Na2 98.79(15) . 2_667 ?

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 W1 O5 W2 8.0(7) . . . . ?
O1 W1 O20 Na1 -139.0(3) . . . . ?
O1 P1 O2 W2 49.7(3) . . . . ?
O1 P1 O2 W3 -171.5(2) . . . . ?
O1 P1 O3 W4 176.3(3) . . . . ?
O1 P1 O3 Na3 -1.9(2) . . . 2_677 ?
O1 P1 O4 W5 121.0(2) . . . . ?
O1 P1 O4 W6 -119.5(2) . . . . ?
O1 P1 O4 W7 0.0(3) . . . . ?
O2 W2 O5 W1 -9.9(7) . . . . ?
O2 P1 O1 W1 -55.9(3) . . . . ?
O2 P1 O1 Na3 123.6(2) . . . 2_677 ?
O2 P1 O3 W4 54.8(4) . . . . ?
O2 P1 O3 Na3 -123.4(2) . . . 2_677 ?
O2 P1 O4 W5 -118.9(3) . . . . ?
O2 P1 O4 W6 0.6(3) . . . . ?
O2 P1 O4 W7 120.2(3) . . . . ?
O3 W4 O7 W3 -8.5(7) . . . . ?
O3 P1 O1 W1 -177.6(3) . . . . ?
O3 P1 O1 Na3 1.9(2) . . . 2_677 ?
O3 P1 O2 W2 170.1(3) . . . . ?
O3 P1 O2 W3 -51.1(3) . . . . ?
O3 P1 O4 W5 1.6(3) . . . . ?
O3 P1 O4 W6 121.1(2) . . . . ?
O3 P1 O4 W7 -119.4(3) . . . . ?
O4 W5 O8 W4 -57.2(5) . . . . ?
O4 W5 O10 W6 -4.35(18) . . . . ?
O4 W6 O13 W2 -63.8(3) . . . . ?
O4 W6 O14 W3 65.4(3) . . . . ?
O4 W7 O11 W6 3.58(19) . . . . ?
O4 W7 O12 W1 53.0(4) . . . . ?
O4 P1 O1 W1 62.3(3) . . . . ?
O4 P1 O1 Na3 -118.22(19) . . . 2_677 ?
O4 P1 O2 W2 -70.0(3) . . . . ?
O4 P1 O2 W3 68.8(3) . . . . ?
O4 P1 O3 W4 -63.5(3) . . . . ?
O4 P1 O3 Na3 118.27(19) . . . 2_677 ?
O5 W1 O20 Na1 -54.7(3) . . . . ?
O6 W2 O5 W1 -39.9(9) . . . . ?
O8 W4 O7 W3 -88.6(7) . . . . ?
O8 W5 O10 W6 75.9(2) . . . . ?
O8 W5 O27 Na2 42.2(2) . . . 2_667 ?
O8 W5 O27 Na2 -122.8(5) . . . . ?
O9 W5 O8 W4 -26.9(7) . . . . ?
O9 W5 O10 W6 -76.0(2) . . . . ?
O9 W5 O27 Na2 45.4(5) . . . . ?
O9 W5 O27 Na2 -149.54(16) . . . 2_667 ?
O9 W7 O11 W6 75.0(2) . . . . ?
O9 W7 O12 W1 22.5(6) . . . . ?
O10 W5 O8 W4 -130.0(5) . . . . ?
O10 W5 O27 Na2 137.9(5) . . . . ?
O10 W5 O27 Na2 -57.04(19) . . . 2_667 ?
O10 W6 O13 W2 -77.8(6) . . . . ?
O10 W6 O14 W3 138.0(3) . . . . ?
O11 W6 O13 W2 -136.4(3) . . . . ?
O11 W6 O14 W3 82.6(5) . . . . ?
O11 W7 O12 W1 126.1(4) . . . . ?
O12 W1 O5 W2 89.3(7) . . . . ?
O12 W1 O20 Na1 -168.2(5) . . . . ?
O12 W7 O11 W6 -77.3(2) . . . . ?
O13 W2 O5 W1 -89.1(7) . . . . ?
O13 W6 O14 W3 -20.2(3) . . . . ?
O14 W6 O13 W2 21.1(3) . . . . ?
O15 W7 O11 W6 12.7(6) . . . . ?
O15 W7 O12 W1 -34.2(4) . . . . ?
O15 P2 O16 W1 24.4(4) . . . . ?
O15 P2 O17 W4 -92.5(4) . . . 2_677 ?
O15 P2 O18 W5 145.3(3) . . . 2_677 ?
O15 P2 O18 Na3 -63.2(3) . . . 2_677 ?
O16 W1 O5 W2 50.3(10) . . . . ?
O16 W1 O20 Na1 141.2(3) . . . . ?
O16 P2 O15 W7 26.0(4) . . . . ?
O16 P2 O15 Na3 179.0(2) . . . . ?
O16 P2 O17 W4 146.4(3) . . . 2_677 ?
O16 P2 O18 W5 -92.4(3) . . . 2_677 ?
O16 P2 O18 Na3 59.1(3) . . . 2_677 ?
O17 W4 O7 W3 -57.3(11) 2_677 . . . ?
O17 P2 O15 W7 -91.4(3) . . . . ?
O17 P2 O15 Na3 61.6(3) . . . . ?
O17 P2 O16 W1 143.9(3) . . . . ?
O17 P2 O18 W5 24.0(4) . . . 2_677 ?
O17 P2 O18 Na3 175.5(2) . . . 2_677 ?
O18 W5 O8 W4 29.9(5) 2_677 . . . ?
O18 W5 O10 W6 -19.2(6) 2_677 . . . ?
O18 W5 O27 Na2 -35.5(5) 2_677 . . . ?
O18 W5 O27 Na2 129.50(16) 2_677 . . 2_667 ?
O18 P2 O15 W7 146.1(3) . . . . ?
O18 P2 O15 Na3 -60.9(3) . . . . ?
O18 P2 O16 W1 -96.0(3) . . . . ?
O18 P2 O17 W4 28.5(4) . . . 2_677 ?
O19 W1 O5 W2 178.5(7) . . . . ?
O19 W1 O20 Na1 46.6(3) . . . . ?
O20 W1 O5 W2 -77.2(7) . . . . ?
O21 W2 O5 W1 -176.9(7) . . . . ?
O22 W2 O5 W1 79.1(7) . . . . ?
O25 W4 O7 W3 178.8(7) . . . . ?
O26 W4 O7 W3 74.8(7) . . . . ?
O27 W5 O8 W4 128.9(5) . . . . ?
O27 W5 O10 W6 179.9(2) . . . . ?
O29 W6 O13 W2 127.6(3) . . . . ?
O29 W6 O14 W3 -126.0(3) . . . . ?
O36 W7 O11 W6 178.2(2) . . . . ?
O36 W7 O12 W1 -131.2(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.509 -0.510 0.500 493.8 215.4 '21.6 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 3.400
_oxdiff_exptl_absorpt_empirical_full_min 0.560

# start Validation Reply Form
_vrf_PLAT972_jcr253-2_auto       
;
PROBLEM: Check Calcd Resid. Dens. 0.79Ang From W2 -4.52 eA-3
RESPONSE: The "Residuel Density" results from the heavy atoms W(VI) 
and the related difficulties to perform an absorption correction.
;
_vrf_PLAT220_jcr253-2_auto       
;
PROBLEM: NonSolvent Resd 1 O Ueq(max)/Ueq(min) Range 8.9 Ratio
RESPONSE: Results from the heavy atoms W(VI) and the related 
difficulties to perform an absorption correction.
;
_vrf_PLAT306_jcr253-2_auto       
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: The oxygen atoms belong to hydration water molecules, of which 
the hydrogen atoms were not modeled.
;
_vrf_PLAT975_jcr253-2_auto       
;
PROBLEM: Check Calcd Resid. Dens. 0.45Ang From O4W . 1.69 eA-3
RESPONSE: Results from disordered hydration water molecules.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# 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_jcr256_auto
_database_code_depnum_ccdc_archive 'CCDC 2293850'
loop_
_audit_author_name
_audit_author_address
'Jan-Christian Raabe'
;University Hamburg
Germany
;
_audit_update_record             
;
2023-09-08 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_audit_creation_date             2023-03-24
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Paradodecatungstate B'
_chemical_formula_moiety         'Na8 O64 W12, 1.5(O4)'
_chemical_formula_sum            'Na8 W12 O40'
_chemical_formula_weight         3510.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         Na7NW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 10.02.2023, Mo, 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7511(4)
_cell_length_b                   12.1744(4)
_cell_length_c                   12.4107(4)
_cell_angle_alpha                82.286(3)
_cell_angle_beta                 66.379(3)
_cell_angle_gamma                64.875(3)
_cell_volume                     1471.45(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    55286
_cell_measurement_temperature    99.97(15)
_cell_measurement_theta_max      32.6870
_cell_measurement_theta_min      3.1860
_shelx_estimated_absorpt_T_max   0.164
_shelx_estimated_absorpt_T_min   0.064
_exptl_absorpt_coefficient_mu    23.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.961
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            93161
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.768
_diffrn_reflns_theta_min         2.289
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00 -24.00   1.00   15.00    --  -18.02 121.00  28.58   48
  2  ω    -42.00  15.00   1.00   15.00    --  -18.02 -77.00  30.00   57
  3  ω    -42.00  15.00   1.00   15.00    --  -18.02 -77.00-180.00   57
  4  ω    -94.00 -43.00   1.00   15.00    --  -18.02 154.00 178.42   51
  5  ω     -6.00  93.00   1.00   15.00    --   18.80  38.00  60.00   99
  6  ω    -22.00  99.00   1.00   15.00    --   18.80  19.00-150.00  121
  7  ω     -6.00  93.00   1.00   15.00    --   18.80  38.00 -30.00   99
  8  ω     39.00 108.00   1.00   15.00    --   18.80 178.00-120.00   69
  9  ω    -61.00  27.00   1.00   15.00    --   18.80 -19.00-150.00   88
 10  ω     39.00 108.00   1.00   15.00    --   18.80 178.00  60.00   69
 11  ω    -61.00  27.00   1.00   15.00    --   18.80 -19.00  30.00   88
 12  ω    -94.00 -43.00   1.00   15.00    --  -18.02 154.00 107.67   51
 13  ω    -42.00  15.00   1.00   15.00    --  -18.02 -77.00 120.00   57
 14  ω    -33.00  17.00   1.00   15.00    --  -18.02 -84.00 -93.00   50
 15  ω    -77.00 -30.00   1.00   15.00    --  -18.02 129.00  68.90   47
 16  ω    -87.00 -37.00   1.00   15.00    --  -18.02 145.00 -38.79   50
 17  ω   -107.00 -61.00   1.00   15.00    --  -18.02-178.00  60.00   46
 18  ω    -42.00  15.00   1.00   15.00    --  -18.02 -77.00   0.00   57
 19  ω   -107.00 -61.00   1.00   15.00    --  -18.02-178.00-180.00   46
 20  ω    -77.00 -30.00   1.00   15.00    --  -18.02 129.00 -82.14   47
 21  ω    -69.00 107.00   1.00   15.00    --   18.80   0.00-180.00  176
 22  ω    -69.00 107.00   1.00   15.00    --   18.80   0.00-150.00  176
 23  ω    -69.00 107.00   1.00   15.00    --   18.80   0.00-120.00  176
 24  ω    -69.00  32.00   1.00   15.00    --   18.80   0.00 -90.00  101
 25  ω      8.00  77.00   1.00   15.00    --   18.80-128.00-141.87   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0004483000
_diffrn_orient_matrix_UB_12      0.0412657000
_diffrn_orient_matrix_UB_13      -0.0461542000
_diffrn_orient_matrix_UB_21      -0.0706451000
_diffrn_orient_matrix_UB_22      0.0345389000
_diffrn_orient_matrix_UB_23      0.0302491000
_diffrn_orient_matrix_UB_31      0.0147696000
_diffrn_orient_matrix_UB_32      0.0353975000
_diffrn_orient_matrix_UB_33      0.0292085000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9939
_reflns_number_total             10357
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         5.596
_refine_diff_density_min         -11.466
_refine_diff_density_rms         0.465
_refine_ls_extinction_coef       0.00042(3)
_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   1.078
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         10357
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0474
_refine_ls_restrained_S_all      1.129
_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)+(0.0001P)²+93.5284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0947
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O13) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O14) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O7W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O20) \\sim Ueq, Uanis(W6) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(O18) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(W3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     heavy
_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
W1 W 0.44607(3) 0.07243(3) 0.22865(2) 0.00482(6) Uani 1 1 d . . . . .
W2 W 0.40846(5) 0.25528(3) 0.00732(3) 0.01702(8) Uani 1 1 d . . . . .
W3 W 0.70566(5) 0.13244(5) 0.03869(3) 0.02238(10) Uani 1 1 d . U . . .
W4 W 0.80349(3) -0.18837(4) 0.10967(3) 0.02023(9) Uani 1 1 d . . . . .
W5 W 0.55229(4) -0.25043(3) 0.30520(3) 0.01215(7) Uani 1 1 d . . . . .
W6 W 0.26215(4) -0.12302(3) 0.26974(3) 0.01218(7) Uani 1 1 d . U . . .
Na1 Na 0.9134(5) 0.2135(4) 0.1740(4) 0.0242(9) Uani 1 1 d . . . . .
Na2 Na 0.8594(5) 0.0392(4) 0.4327(4) 0.0202(8) Uani 1 1 d . . . . .
Na3 Na 0.7622(4) -0.1869(4) 0.4301(3) 0.0133(7) Uani 1 1 d . . . . .
Na4 Na 0.3788(5) -0.4681(4) 0.3366(4) 0.0217(9) Uani 1 1 d . . . . .
O1 O 0.3640(7) 0.2332(6) 0.1752(5) 0.0137(12) Uani 1 1 d . . . . .
O1W O 0.7682(13) 0.4192(11) 0.1651(11) 0.054(3) Uani 1 1 d . U . . .
O2 O 0.5998(7) 0.1291(6) 0.1983(6) 0.0152(12) Uani 1 1 d . U . . .
O2W O 1.0709(9) 0.2197(9) 0.2473(11) 0.041(2) Uani 1 1 d . . . . .
O3 O 0.5516(6) 0.0725(5) 0.0317(5) 0.0079(10) Uani 1 1 d . . . . .
O3W O 0.7716(7) 0.2404(7) 0.3794(7) 0.0200(14) Uani 1 1 d . . . . .
O4 O 0.5692(8) 0.2764(7) 0.0190(7) 0.0222(14) Uani 1 1 d . U . . .
O4W O 0.9432(7) 0.0072(7) 0.2205(6) 0.0210(14) Uani 1 1 d . . . . .
O5 O 0.8023(7) -0.0411(7) 0.0403(6) 0.0209(14) Uani 1 1 d . U . . .
O5W O 0.9496(9) -0.1813(8) 0.4730(7) 0.0252(16) Uani 1 1 d . . . . .
O6 O 0.7291(7) -0.3078(6) 0.1852(6) 0.0182(13) Uani 1 1 d . . . . .
O6W O 0.6686(7) 0.0275(6) 0.4086(6) 0.0151(12) Uani 1 1 d . . . . .
O7 O 0.3656(7) -0.1425(6) 0.3651(5) 0.0128(12) Uani 1 1 d . . . . .
O7W O 0.8703(13) -0.4097(11) 0.4329(11) 0.052(3) Uani 1 1 d . U . . .
O8 O 0.5858(6) -0.0846(6) 0.2187(5) 0.0088(10) Uani 1 1 d . . . . .
O8W O 0.2938(10) -0.4701(7) 0.5407(7) 0.0275(18) Uani 1 1 d . . . . .
O9 O 0.3365(6) 0.0195(5) 0.2040(5) 0.0081(10) Uani 1 1 d . . . . .
O9W O 0.5172(7) -0.6801(7) 0.3525(7) 0.0199(14) Uani 1 1 d . . . . .
O10 O 0.2990(7) 0.1917(8) 0.0027(6) 0.0247(17) Uani 1 1 d . . . . .
O10W O 0.2213(9) -0.5514(6) 0.3212(6) 0.0213(15) Uani 1 1 d . . . . .
O11 O 0.3124(14) 0.4110(10) 0.0164(9) 0.051(3) Uani 1 1 d . U . . .
O11W O 0.4550(8) -0.4896(6) 0.1346(6) 0.0174(13) Uani 1 1 d . . . . .
O12 O 0.5211(8) 0.2249(6) -0.1551(5) 0.0148(12) Uani 1 1 d . . . . .
O13 O 0.8130(11) 0.1895(10) 0.0464(9) 0.041(2) Uani 1 1 d . U . . .
O13W O 0.8383(8) 0.4035(7) -0.0188(6) 0.0198(14) Uani 1 1 d . . . . .
O14 O 0.9551(10) -0.2861(9) 0.0057(8) 0.0348(19) Uani 1 1 d . U . . .
O15 O 0.8549(6) -0.1815(7) 0.2229(5) 0.0165(13) Uani 1 1 d . . . . .
O16 O 0.5407(10) -0.3909(7) 0.3318(7) 0.0261(18) Uani 1 1 d . . . . .
O17 O 0.5862(7) -0.2283(6) 0.4237(6) 0.0137(12) Uani 1 1 d . . . . .
O18 O 0.2358(8) -0.2566(7) 0.3106(7) 0.0207(14) Uani 1 1 d . U . . .
O19 O 0.1093(7) -0.0149(8) 0.3656(6) 0.0226(16) Uani 1 1 d . . . . .
O20 O 0.2256(7) -0.1000(7) 0.1318(6) 0.0158(12) Uani 1 1 d . U . . .
O22 O 0.3730(6) 0.1106(6) 0.3774(5) 0.0102(10) Uani 1 1 d . . . . .
O12W O 0.3084(8) 0.5963(7) 0.0095(6) 0.0200(14) Uani 1 1 d . . . . .
O14W O 0.1223(7) -0.3401(6) 0.1987(6) 0.0142(12) Uani 1 1 d . . . . .


_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
W1 O1 1.940(6) . ?
W1 O2 2.080(7) . ?
W1 O3 2.255(6) . ?
W1 O8 1.897(6) . ?
W1 O9 1.800(6) . ?
W1 O22 1.727(6) . ?
W2 O1 1.945(6) . ?
W2 O3 2.218(6) . ?
W2 O4 2.073(8) . ?
W2 O10 1.781(9) . ?
W2 O11 1.737(11) . ?
W2 O12 1.897(6) . ?
W3 O2 1.876(7) . ?
W3 O3 2.255(5) . ?
W3 O4 1.875(8) . ?
W3 O5 1.930(8) . ?
W3 O13 1.715(10) . ?
W3 O20 1.967(7) 2_655 ?
W4 Na1 3.687(5) 2_755 ?
W4 O5 1.879(7) . ?
W4 O6 1.953(8) . ?
W4 O8 2.216(6) . ?
W4 O10 2.191(7) 2_655 ?
W4 O14 1.739(10) . ?
W4 O15 1.761(6) . ?
W5 O6 1.895(8) . ?
W5 O7 1.897(7) . ?
W5 O8 2.267(6) . ?
W5 O12 2.284(6) 2_655 ?
W5 O16 1.750(7) . ?
W5 O17 1.750(6) . ?
W6 Na2 3.503(4) 2_656 ?
W6 O7 1.941(6) . ?
W6 O9 2.185(6) . ?
W6 O12 2.222(7) 2_655 ?
W6 O18 1.755(7) . ?
W6 O19 1.753(8) . ?
W6 O20 1.884(7) . ?
Na1 O1W 2.375(13) . ?
Na1 O2W 2.397(10) . ?
Na1 O3W 2.396(9) . ?
Na1 O4W 2.407(9) . ?
Na1 O13 2.429(11) . ?
Na1 O14 2.452(11) 2_755 ?
Na2 O3W 2.338(9) . ?
Na2 O4W 2.434(8) . ?
Na2 O5W 2.496(10) . ?
Na2 O6W 2.440(8) . ?
Na2 O19 2.509(8) 1_655 ?
Na2 O19 2.635(8) 2_656 ?
Na3 O5W 2.493(9) . ?
Na3 O6W 2.389(8) . ?
Na3 O7W 2.462(13) . ?
Na3 O15 2.361(7) . ?
Na3 O17 2.359(8) . ?
Na3 O22 2.323(7) 2_656 ?
Na4 O8W 2.322(9) . ?
Na4 O9W 2.429(9) . ?
Na4 O10W 2.534(9) . ?
Na4 O11W 2.309(8) . ?
Na4 O16 2.433(9) . ?
Na4 O18 2.469(9) . ?
O13W O12W 1.680(11) 2_665 ?

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 W1 O2 81.7(3) . . ?
O1 W1 O3 70.9(2) . . ?
O2 W1 O3 73.4(2) . . ?
O8 W1 O1 155.4(3) . . ?
O8 W1 O2 83.4(3) . . ?
O8 W1 O3 86.1(2) . . ?
O9 W1 O1 93.0(3) . . ?
O9 W1 O2 161.5(3) . . ?
O9 W1 O3 88.1(2) . . ?
O9 W1 O8 95.0(3) . . ?
O22 W1 O1 97.4(3) . . ?
O22 W1 O2 93.3(3) . . ?
O22 W1 O3 163.1(3) . . ?
O22 W1 O8 102.9(3) . . ?
O22 W1 O9 105.0(3) . . ?
O1 W2 O3 71.7(2) . . ?
O1 W2 O4 81.6(3) . . ?
O4 W2 O3 73.0(3) . . ?
O10 W2 O1 93.2(3) . . ?
O10 W2 O3 90.0(3) . . ?
O10 W2 O4 163.1(3) . . ?
O10 W2 O12 95.3(3) . . ?
O11 W2 O1 97.1(4) . . ?
O11 W2 O3 162.7(4) . . ?
O11 W2 O4 92.7(5) . . ?
O11 W2 O10 103.9(5) . . ?
O11 W2 O12 102.8(4) . . ?
O12 W2 O1 155.8(3) . . ?
O12 W2 O3 85.7(3) . . ?
O12 W2 O4 83.7(3) . . ?
O2 W3 O3 77.2(2) . . ?
O2 W3 O5 87.8(3) . . ?
O2 W3 O20 156.4(3) . 2_655 ?
O4 W3 O2 92.3(3) . . ?
O4 W3 O3 75.9(3) . . ?
O4 W3 O5 155.6(3) . . ?
O4 W3 O20 87.0(3) . 2_655 ?
O5 W3 O3 80.4(3) . . ?
O5 W3 O20 83.4(3) . 2_655 ?
O13 W3 O2 101.8(4) . . ?
O13 W3 O3 175.5(4) . . ?
O13 W3 O4 99.8(4) . . ?
O13 W3 O5 104.0(4) . . ?
O13 W3 O20 101.5(4) . 2_655 ?
O20 W3 O3 79.8(2) 2_655 . ?
O5 W4 Na1 64.1(2) . 2_755 ?
O5 W4 O6 156.6(3) . . ?
O5 W4 O8 86.8(3) . . ?
O5 W4 O10 85.5(3) . 2_655 ?
O6 W4 Na1 129.4(2) . 2_755 ?
O6 W4 O8 73.4(3) . . ?
O6 W4 O10 78.3(3) . 2_655 ?
O8 W4 Na1 146.11(17) . 2_755 ?
O10 W4 Na1 83.4(2) 2_655 2_755 ?
O10 W4 O8 77.2(2) 2_655 . ?
O14 W4 Na1 34.2(4) . 2_755 ?
O14 W4 O5 98.2(4) . . ?
O14 W4 O6 98.0(4) . . ?
O14 W4 O8 164.0(3) . . ?
O14 W4 O10 88.0(3) . 2_655 ?
O14 W4 O15 101.8(4) . . ?
O15 W4 Na1 107.9(2) . 2_755 ?
O15 W4 O5 98.7(3) . . ?
O15 W4 O6 94.4(3) . . ?
O15 W4 O8 92.4(3) . . ?
O15 W4 O10 168.7(3) . 2_655 ?
O6 W5 O7 152.1(3) . . ?
O6 W5 O8 73.2(3) . . ?
O6 W5 O12 85.1(3) . 2_655 ?
O7 W5 O8 84.6(2) . . ?
O7 W5 O12 73.5(3) . 2_655 ?
O8 W5 O12 77.4(2) . 2_655 ?
O16 W5 O6 96.6(4) . . ?
O16 W5 O7 100.9(4) . . ?
O16 W5 O8 164.2(3) . . ?
O16 W5 O12 89.9(3) . 2_655 ?
O17 W5 O6 101.1(3) . . ?
O17 W5 O7 95.9(3) . . ?
O17 W5 O8 91.1(3) . . ?
O17 W5 O12 164.9(3) . 2_655 ?
O17 W5 O16 103.0(3) . . ?
O7 W6 Na2 51.5(2) . 2_656 ?
O7 W6 O9 79.0(2) . . ?
O7 W6 O12 74.2(3) . 2_655 ?
O9 W6 Na2 94.91(17) . 2_656 ?
O9 W6 O12 76.6(2) . 2_655 ?
O12 W6 Na2 125.59(18) 2_655 2_656 ?
O18 W6 Na2 89.8(3) . 2_656 ?
O18 W6 O7 96.3(3) . . ?
O18 W6 O9 168.9(3) . . ?
O18 W6 O12 92.5(3) . 2_655 ?
O18 W6 O20 97.2(3) . . ?
O19 W6 Na2 46.8(2) . 2_656 ?
O19 W6 O7 95.6(3) . . ?
O19 W6 O9 89.3(3) . . ?
O19 W6 O12 163.9(3) . 2_655 ?
O19 W6 O18 101.2(4) . . ?
O19 W6 O20 100.1(3) . . ?
O20 W6 Na2 146.9(2) . 2_656 ?
O20 W6 O7 156.9(3) . . ?
O20 W6 O9 84.3(3) . . ?
O20 W6 O12 86.5(3) . 2_655 ?
O1W Na1 O2W 105.9(5) . . ?
O1W Na1 O3W 84.4(4) . . ?
O1W Na1 O4W 149.8(4) . . ?
O1W Na1 O13 79.8(5) . . ?
O1W Na1 O14 74.9(4) . 2_755 ?
O2W Na1 O4W 97.2(3) . . ?
O2W Na1 O13 163.1(4) . . ?
O2W Na1 O14 83.8(4) . 2_755 ?
O3W Na1 O2W 81.9(4) . . ?
O3W Na1 O4W 79.7(3) . . ?
O3W Na1 O13 114.8(4) . . ?
O3W Na1 O14 150.5(4) . 2_755 ?
O4W Na1 O13 83.7(3) . . ?
O4W Na1 O14 127.8(4) . 2_755 ?
O13 Na1 O14 82.4(4) . 2_755 ?
O3W Na2 O4W 80.3(3) . . ?
O3W Na2 O5W 174.3(3) . . ?
O3W Na2 O6W 84.7(3) . . ?
O3W Na2 O19 114.2(3) . 2_656 ?
O3W Na2 O19 103.8(3) . 1_655 ?
O4W Na2 O5W 95.0(3) . . ?
O4W Na2 O6W 77.8(3) . . ?
O4W Na2 O19 153.3(3) . 2_656 ?
O4W Na2 O19 76.5(3) . 1_655 ?
O5W Na2 O19 77.9(3) . 1_655 ?
O5W Na2 O19 71.4(3) . 2_656 ?
O6W Na2 O5W 91.2(3) . . ?
O6W Na2 O19 150.9(3) . 1_655 ?
O6W Na2 O19 124.1(3) . 2_656 ?
O19 Na2 O19 78.2(3) 1_655 2_656 ?
O6W Na3 O5W 92.5(3) . . ?
O6W Na3 O7W 174.8(4) . . ?
O7W Na3 O5W 87.7(4) . . ?
O15 Na3 O5W 99.1(3) . . ?
O15 Na3 O6W 80.3(3) . . ?
O15 Na3 O7W 94.5(4) . . ?
O17 Na3 O5W 166.1(3) . . ?
O17 Na3 O6W 98.5(3) . . ?
O17 Na3 O7W 82.0(4) . . ?
O17 Na3 O15 91.1(3) . . ?
O22 Na3 O5W 84.9(3) 2_656 . ?
O22 Na3 O6W 76.9(2) 2_656 . ?
O22 Na3 O7W 108.3(4) 2_656 . ?
O22 Na3 O15 157.0(3) 2_656 . ?
O22 Na3 O17 89.5(3) 2_656 . ?
O8W Na4 O9W 82.8(3) . . ?
O8W Na4 O10W 93.0(3) . . ?
O8W Na4 O16 92.2(3) . . ?
O8W Na4 O18 99.8(3) . . ?
O9W Na4 O10W 83.8(3) . . ?
O9W Na4 O16 96.1(3) . . ?
O9W Na4 O18 176.5(3) . . ?
O11W Na4 O8W 171.6(3) . . ?
O11W Na4 O9W 92.3(3) . . ?
O11W Na4 O10W 79.7(3) . . ?
O11W Na4 O16 95.0(3) . . ?
O11W Na4 O18 84.9(3) . . ?
O16 Na4 O10W 174.7(3) . . ?
O16 Na4 O18 86.3(3) . . ?
O18 Na4 O10W 93.6(3) . . ?
W1 O1 W2 118.9(3) . . ?
W3 O2 W1 114.4(3) . . ?
W1 O3 W3 95.1(2) . . ?
W2 O3 W1 96.8(2) . . ?
W2 O3 W3 96.2(2) . . ?
Na2 O3W Na1 98.7(3) . . ?
W3 O4 W2 114.9(4) . . ?
Na1 O4W Na2 95.8(3) . . ?
W4 O5 W3 148.4(4) . . ?
Na3 O5W Na2 86.1(3) . . ?
W5 O6 W4 117.6(3) . . ?
Na3 O6W Na2 89.7(3) . . ?
W5 O7 W6 117.4(3) . . ?
W5 O7 Na2 144.4(3) . 2_656 ?
W6 O7 Na2 94.9(3) . 2_656 ?
W1 O8 W4 139.1(3) . . ?
W1 O8 W5 125.2(3) . . ?
W4 O8 W5 94.5(2) . . ?
W1 O9 W6 136.8(3) . . ?
W2 O10 W4 139.5(5) . 2_655 ?
W2 O12 W5 125.7(4) . 2_655 ?
W2 O12 W6 139.3(4) . 2_655 ?
W6 O12 W5 93.4(2) 2_655 2_655 ?
W3 O13 Na1 143.4(6) . . ?
W4 O14 Na1 122.3(5) . 2_755 ?
W4 O15 Na3 134.6(4) . . ?
W5 O16 Na4 135.0(5) . . ?
W5 O17 Na3 131.4(4) . . ?
W6 O18 Na4 135.0(4) . . ?
W6 O19 Na2 137.5(4) . 1_455 ?
W6 O19 Na2 104.1(4) . 2_656 ?
Na2 O19 Na2 101.8(3) 1_455 2_656 ?
W6 O20 W3 148.3(4) . 2_655 ?
W1 O22 Na3 168.9(4) . 2_656 ?

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
Na1 W4 O5 W3 169.2(9) 2_755 . . . ?
Na1 W4 O15 Na3 -171.8(4) 2_755 . . . ?
Na2 W6 O18 Na4 -94.7(5) 2_656 . . . ?
Na2 W6 O19 Na2 -126.0(7) 2_656 . . 1_455 ?
Na2 W6 O20 W3 170.6(4) 2_656 . . 2_655 ?
O1 W1 O8 W4 10.5(9) . . . . ?
O1 W1 O8 W5 -152.8(5) . . . . ?
O1 W1 O9 W6 -156.7(5) . . . . ?
O1 W1 O22 Na3 38.0(19) . . . 2_656 ?
O1 W2 O10 W4 161.0(6) . . . 2_655 ?
O1 W2 O12 W5 151.3(5) . . . 2_655 ?
O1 W2 O12 W6 -9.7(10) . . . 2_655 ?
O2 W1 O8 W4 -42.5(5) . . . . ?
O2 W1 O8 W5 154.2(4) . . . . ?
O2 W1 O9 W6 130.5(7) . . . . ?
O2 W1 O22 Na3 120.0(19) . . . 2_656 ?
O2 W3 O4 W2 -76.7(4) . . . . ?
O2 W3 O13 Na1 23.0(11) . . . . ?
O3 W1 O8 W4 31.2(4) . . . . ?
O3 W1 O8 W5 -132.1(3) . . . . ?
O3 W1 O9 W6 132.6(5) . . . . ?
O3 W1 O22 Na3 83(2) . . . 2_656 ?
O3 W2 O10 W4 -127.4(6) . . . 2_655 ?
O3 W2 O12 W5 130.8(4) . . . 2_655 ?
O3 W2 O12 W6 -30.3(5) . . . 2_655 ?
O3 W3 O2 W1 1.5(3) . . . . ?
O3 W3 O4 W2 -0.5(3) . . . . ?
O4 W2 O10 W4 -127.4(10) . . . 2_655 ?
O4 W2 O12 W5 -155.9(4) . . . 2_655 ?
O4 W2 O12 W6 43.1(5) . . . 2_655 ?
O4 W3 O2 W1 76.4(4) . . . . ?
O4 W3 O13 Na1 117.5(10) . . . . ?
O5 W3 O2 W1 -79.1(4) . . . . ?
O5 W3 O4 W2 13.1(10) . . . . ?
O5 W3 O13 Na1 -67.7(10) . . . . ?
O5 W4 O14 Na1 -3.9(6) . . . 2_755 ?
O5 W4 O15 Na3 122.7(5) . . . . ?
O6 W4 O5 W3 38.4(14) . . . . ?
O6 W4 O14 Na1 159.1(5) . . . 2_755 ?
O6 W4 O15 Na3 -37.8(6) . . . . ?
O6 W5 O7 W6 52.1(7) . . . . ?
O6 W5 O7 Na2 -155.1(5) . . . 2_656 ?
O6 W5 O16 Na4 -126.1(6) . . . . ?
O6 W5 O17 Na3 26.3(5) . . . . ?
O7 W5 O6 W4 48.8(8) . . . . ?
O7 W5 O16 Na4 32.1(6) . . . . ?
O7 W5 O17 Na3 -131.5(5) . . . . ?
O7 W6 O18 Na4 -43.5(6) . . . . ?
O7 W6 O19 Na2 -18.5(3) . . . 2_656 ?
O7 W6 O19 Na2 -144.5(6) . . . 1_455 ?
O7 W6 O20 W3 36.7(13) . . . 2_655 ?
O8 W1 O9 W6 46.6(5) . . . . ?
O8 W1 O22 Na3 -156.0(19) . . . 2_656 ?
O8 W4 O5 W3 7.0(8) . . . . ?
O8 W4 O14 Na1 103.1(13) . . . 2_755 ?
O8 W4 O15 Na3 35.7(5) . . . . ?
O8 W5 O6 W4 10.0(3) . . . . ?
O8 W5 O7 W6 89.1(3) . . . . ?
O8 W5 O7 Na2 -118.0(5) . . . 2_656 ?
O8 W5 O16 Na4 -77.2(16) . . . . ?
O8 W5 O17 Na3 -46.9(5) . . . . ?
O9 W1 O8 W4 119.0(5) . . . . ?
O9 W1 O8 W5 -44.3(4) . . . . ?
O9 W1 O22 Na3 -57(2) . . . 2_656 ?
O9 W6 O18 Na4 20.4(19) . . . . ?
O9 W6 O19 Na2 136.7(6) . . . 1_455 ?
O9 W6 O19 Na2 -97.4(3) . . . 2_656 ?
O9 W6 O20 W3 80.3(7) . . . 2_655 ?
O10 W2 O12 W5 41.1(4) . . . 2_655 ?
O10 W2 O12 W6 -120.0(5) . . . 2_655 ?
O10 W4 O5 W3 84.4(8) 2_655 . . . ?
O10 W4 O14 Na1 81.2(5) 2_655 . . 2_755 ?
O10 W4 O15 Na3 12(2) 2_655 . . . ?
O11 W2 O10 W4 62.9(7) . . . 2_655 ?
O11 W2 O12 W5 -64.5(6) . . . 2_655 ?
O11 W2 O12 W6 134.4(6) . . . 2_655 ?
O12 W2 O10 W4 -41.7(6) . . . 2_655 ?
O12 W5 O6 W4 88.3(4) 2_655 . . . ?
O12 W5 O7 W6 10.7(3) 2_655 . . . ?
O12 W5 O7 Na2 163.6(6) 2_655 . . 2_656 ?
O12 W5 O16 Na4 -41.1(6) 2_655 . . . ?
O12 W5 O17 Na3 -86.7(12) 2_655 . . . ?
O12 W6 O18 Na4 30.9(5) 2_655 . . . ?
O12 W6 O19 Na2 -68.2(11) 2_655 . . 2_656 ?
O12 W6 O19 Na2 165.8(7) 2_655 . . 1_455 ?
O12 W6 O20 W3 3.5(7) 2_655 . . 2_655 ?
O13 W3 O2 W1 177.0(5) . . . . ?
O13 W3 O4 W2 -179.1(5) . . . . ?
O14 W4 O5 W3 171.7(9) . . . . ?
O14 W4 O15 Na3 -137.0(6) . . . . ?
O15 W4 O5 W3 -85.0(9) . . . . ?
O15 W4 O14 Na1 -104.6(5) . . . 2_755 ?
O16 W5 O6 W4 177.6(4) . . . . ?
O16 W5 O7 W6 -75.9(4) . . . . ?
O16 W5 O7 Na2 77.0(5) . . . 2_656 ?
O16 W5 O17 Na3 125.8(5) . . . . ?
O17 W5 O6 W4 -77.8(4) . . . . ?
O17 W5 O7 W6 179.6(3) . . . . ?
O17 W5 O7 Na2 -27.5(5) . . . 2_656 ?
O17 W5 O16 Na4 130.9(6) . . . . ?
O18 W6 O19 Na2 -46.9(6) . . . 1_455 ?
O18 W6 O19 Na2 79.0(4) . . . 2_656 ?
O18 W6 O20 W3 -88.6(8) . . . 2_655 ?
O19 W6 O18 Na4 -140.4(5) . . . . ?
O19 W6 O20 W3 168.6(7) . . . 2_655 ?
O20 W3 O2 W1 -11.3(10) 2_655 . . . ?
O20 W3 O4 W2 79.7(4) 2_655 . . . ?
O20 W3 O13 Na1 -153.7(9) 2_655 . . . ?
O20 W6 O18 Na4 117.7(5) . . . . ?
O20 W6 O19 Na2 178.5(3) . . . 2_656 ?
O20 W6 O19 Na2 52.6(6) . . . 1_455 ?
O22 W1 O8 W4 -134.4(5) . . . . ?
O22 W1 O8 W5 62.3(4) . . . . ?
O22 W1 O9 W6 -58.2(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.001 0.476 0.180 21.5 10.3 '1 H2O'
2 -0.001 0.524 0.820 21.5 10.4 '1 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 4.266
_oxdiff_exptl_absorpt_empirical_full_min 0.625

# start Validation Reply Form
_vrf_DIFMN02_jcr256_auto         
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: This effect might be caused by the difficulty to account
correctly the absorption effect of the heavy atom W. The applied 
absorption correction scheme had only a very minor influence on 
the residual electron/hole density values. Application of the new
algorithm "NoSpherA2" was also not successful, because the self-
consistent field calculation did not converge for unknown reasons.
Furthermore, an attempt to model a disorder of the WO6 octahedra 
was undertaken. This reduced drastically the electron density 
difference values with a maximum and minimum value of only 3.8 and 
-3.4, respectively. However, some other problems occured, for 
instance, atoms with non-positive definite (NPD) values of the 
displacement parameters and unrealistic W-O bond lengths. 
Therefore, we believe that the structure altogether is better 
represented by the non-disordered model.
;
_vrf_PLAT213_jcr256_auto         
;
PROBLEM: Atom W3 has ADP max/min Ratio ..... 15.8 prolat
RESPONSE: This effect might be caused by the difficulty to account
correctly the absorption effect of the heavy atom W. The applied 
absorption correction scheme had only a very minor influence on 
the residual electron/hole density values. Application of the new
algorithm "NoSpherA2" was also not successful, because the self-
consistent field calculation did not converge for unknown reasons.
Furthermore, an attempt to model a disorder of the WO6 octahedra 
was undertaken. This reduced drastically the electron density 
difference values with a maximum and minimum value of only 3.8 and 
-3.4, respectively. However, some other problems occured, for 
instance, atoms with non-positive definite (NPD) values of the 
displacement parameters and unrealistic W-O bond lengths. 
Therefore, we believe that the structure altogether is better 
represented by the non-disordered model.
;
_vrf_PLAT971_jcr256_auto         
;
PROBLEM: Check Calcd Resid. Dens. 1.02Ang From O7W 5.75 eA-3
RESPONSE: Residual density results from disordered hydration 
water molecules.
;
_vrf_PLAT972_jcr256_auto         
;
PROBLEM: Check Calcd Resid. Dens. 0.85Ang From W4 -11.06 eA-3
RESPONSE: This effect might be caused by the difficulty to account
correctly the absorption effect of the heavy atom W. The applied 
absorption correction scheme had only a very minor influence on 
the residual electron/hole density values. Application of the new
algorithm "NoSpherA2" was also not successful, because the self-
consistent field calculation did not converge for unknown reasons.
Furthermore, an attempt to model a disorder of the WO6 octahedra 
was undertaken. This reduced drastically the electron density 
difference values with a maximum and minimum value of only 3.8 and 
-3.4, respectively. However, some other problems occured, for 
instance, atoms with non-positive definite (NPD) values of the 
displacement parameters and unrealistic W-O bond lengths. 
Therefore, we believe that the structure altogether is better 
represented by the non-disordered model.
;
_vrf_PLAT974_jcr256_auto         
;
PROBLEM: Check Calcd Negative Resid. Density on W3 -3.44 eA-3
RESPONSE: This effect might be caused by the difficulty to account
correctly the absorption effect of the heavy atom W. The applied 
absorption correction scheme had only a very minor influence on 
the residual electron/hole density values. Application of the new
algorithm "NoSpherA2" was also not successful, because the self-
consistent field calculation did not converge for unknown reasons.
Furthermore, an attempt to model a disorder of the WO6 octahedra 
was undertaken. This reduced drastically the electron density 
difference values with a maximum and minimum value of only 3.8 and 
-3.4, respectively. However, some other problems occured, for 
instance, atoms with non-positive definite (NPD) values of the 
displacement parameters and unrealistic W-O bond lengths. 
Therefore, we believe that the structure altogether is better 
represented by the non-disordered model.
;
_vrf_PLAT975_jcr256_auto         
;
PROBLEM: Check Calcd Resid. Dens. 1.02Ang From O7W . 5.75 eA-3
RESPONSE: Residual density results from disordered hydration 
water molecules.
;
_vrf_PLAT976_jcr256_auto         
;
PROBLEM: Check Calcd Resid. Dens. 0.41Ang From O13 . -2.44 eA-3
RESPONSE: Residual density results from disordered hydration 
water molecules.
;
_vrf_PLAT098_jcr256_auto         
;
PROBLEM: Large Reported Min. (Negative) Residual Density -11.47 eA-3
RESPONSE: This effect might be caused by the difficulty to account
correctly the absorption effect of the heavy atom W. The applied 
absorption correction scheme had only a very minor influence on 
the residual electron/hole density values. Application of the new
algorithm "NoSpherA2" was also not successful, because the self-
consistent field calculation did not converge for unknown reasons.
Furthermore, an attempt to model a disorder of the WO6 octahedra 
was undertaken. This reduced drastically the electron density 
difference values with a maximum and minimum value of only 3.8 and 
-3.4, respectively. However, some other problems occured, for 
instance, atoms with non-positive definite (NPD) values of the 
displacement parameters and unrealistic W-O bond lengths. 
Therefore, we believe that the structure altogether is better 
represented by the non-disordered model.
;
_vrf_PLAT220_jcr256_auto         
;
PROBLEM: NonSolvent Resd 1 O Ueq(max)/Ueq(min) Range 6.7 Ratio
RESPONSE: This effect might be caused by the difficulty to account
correctly the absorption effect of the heavy atom W. The applied 
absorption correction scheme had only a very minor influence on 
the residual electron/hole density values. Application of the new
algorithm "NoSpherA2" was also not successful, because the self-
consistent field calculation did not converge for unknown reasons.
Furthermore, an attempt to model a disorder of the WO6 octahedra 
was undertaken. This reduced drastically the electron density 
difference values with a maximum and minimum value of only 3.8 and 
-3.4, respectively. However, some other problems occured, for 
instance, atoms with non-positive definite (NPD) values of the 
displacement parameters and unrealistic W-O bond lengths. 
Therefore, we believe that the structure altogether is better 
represented by the non-disordered model.
;
_vrf_PLAT306_jcr256_auto         
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: The oxygen atoms belong to hydration water molecules, of which 
the hydrogen atoms were not modeled.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# 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_jcr268_auto_v1
_database_code_depnum_ccdc_archive 'CCDC 2293851'
loop_
_audit_author_name
_audit_author_address
'Jan-Christian Raabe'
;University Hamburg
Germany
;
_audit_update_record             
;
2023-09-08 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_audit_creation_date             2023-09-08
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
JanChristian.Raabe@uni-hamburg.de
maximilian.poller@uni-hamburg.de
jakob.albert@uni-hamburg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'As K1.35 Na3.15 O39.647 W9, 7.858(O), 10.8[H2O]'
_chemical_formula_sum            'Na3.1 H5.9 As1 W9 O34'
_chemical_formula_weight         2809.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         Na7AsW6O24
_chemical_oxdiff_usercomment     'Raabe/Albert, 08.05.2023, Mo, 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 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, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+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, 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'
'-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, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+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, -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                   30.08540(9)
_cell_length_b                   30.08540(9)
_cell_length_c                   30.08540(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     27231.2(2)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    228300
_cell_measurement_temperature    99.95(13)
_cell_measurement_theta_max      29.4260
_cell_measurement_theta_min      2.5150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49516
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.741
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             19957
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            476401
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.594
_diffrn_reflns_theta_min         2.345
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4127
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  31.00   1.00   60.00    --   -9.92 -99.00  90.00   46
  2  ω    -14.00  85.00   1.00   60.00    --   10.55  38.00  60.00   99
  3  ω    -42.00  43.00   1.00   60.00    --   10.55 -77.00-120.00   85
  4  ω    -42.00  43.00   1.00   60.00    --   10.55 -77.00 120.00   85
  5  ω    -78.00  99.00   1.00   60.00    --   10.55   0.00 -90.00  177
  6  ω    -14.00  85.00   1.00   60.00    --   10.55  38.00 -60.00   99
  7  ω      6.00  67.00   1.00   60.00    --   10.55-125.00 -52.00   61
  8  ω     19.00  84.00   1.00   60.00    --   10.55-151.00  72.37   65
  9  ω    -69.00 -30.00   1.00   60.00    --   -9.92 129.00  55.17   39
 10  ω    -15.00  31.00   1.00   60.00    --   -9.92 -99.00  30.00   46
 11  ω    -69.00 -30.00   1.00   60.00    --   -9.92 129.00  -0.05   39
 12  ω    -87.00 -44.00   1.00   60.00    --   -9.92 156.00-107.40   43
 13  ω    -79.00 -37.00   1.00   60.00    --   -9.92 145.00  73.51   42
 14  ω    -69.00 -30.00   1.00   60.00    --   -9.92 129.00 141.56   39
 15  ω    -59.00 -17.00   1.00   60.00    --   -9.92 113.00-176.28   42
 16  ω    -84.00 -41.00   1.00   60.00    --   -9.92 152.00 -11.01   43
 17  ω    -15.00  31.00   1.00   60.00    --   -9.92 -99.00 120.00   46
 18  ω    -78.00 -31.00   1.00   60.00    --   10.55   0.00-180.00   47
 19  ω     -1.00  62.00   1.00   60.00    --   10.55-117.00 -11.69   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0178142501
_diffrn_orient_matrix_UB_12      0.0065108499
_diffrn_orient_matrix_UB_13      -0.0140068501
_diffrn_orient_matrix_UB_21      0.0122626488
_diffrn_orient_matrix_UB_22      -0.0070589512
_diffrn_orient_matrix_UB_23      -0.0188636512
_diffrn_orient_matrix_UB_31      -0.0093963484
_diffrn_orient_matrix_UB_32      -0.0215427484
_diffrn_orient_matrix_UB_33      0.0019551516
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2932
_reflns_number_total             3572
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.277
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.287
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         3572
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0422
_refine_ls_restrained_S_all      1.119
_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)+(0.0214P)²+2635.2891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1070
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Shared sites
{Na1, K1}
2. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Na1) = Uanis(K1)
3. Others
 Fixed Sof: K1(0.225) Na1(0.025)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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
W1 W 0.09850(2) 0.17926(2) 0.09850(2) 0.01484(11) Uani 1 2 d S T P . .
W2 W 0.10242(2) 0.27079(2) 0.18213(2) 0.01603(10) Uani 1 1 d . . . . .
As1 As 0.18281(4) 0.18281(4) 0.18281(4) 0.0115(4) Uani 1 6 d S T P . .
K1 K 0.000000 0.24651(13) 0.24651(13) 0.0309(10) Uani 0.9 4 d S T P . 2
Na1 Na 0.000000 0.24651(13) 0.24651(13) 0.0309(10) Uani 0.1 4 d S T P . 1
Na2 Na 0.19311(13) 0.37658(18) 0.19311(13) 0.0229(11) Uani 1 2 d S T P . .
O1 O 0.1503(3) 0.1503(3) 0.1503(3) 0.022(3) Uani 1 6 d S T P . .
O1W O 0.000000 0.1829(4) 0.1829(4) 0.033(2) Uani 1 4 d S TU P . .
O2 O 0.1713(2) 0.1713(2) 0.2364(3) 0.0182(17) Uani 1 2 d S T P . .
O2W O 0.1304(7) 0.3859(8) 0.1304(7) 0.050(10) Uani 0.49(4) 2 d S T . . .
O3 O 0.0826(2) 0.2169(2) 0.1434(2) 0.0173(12) Uani 1 1 d . . . . .
O3W O 0.22316(19) 0.3107(3) 0.22316(19) 0.007(3) Uiso 0.89(4) 2 d S . . . .
O4 O 0.0686(3) 0.1314(2) 0.1314(2) 0.0194(17) Uani 1 2 d S T P . .
O4W O 0.1013(3) 0.4232(4) 0.1013(3) 0.021(4) Uani 0.63(3) 2 d S T . . .
O5 O 0.1322(2) 0.3102(2) 0.2133(2) 0.0204(13) Uani 1 1 d . . . . .
O5W O 0.2136(6) 0.2864(6) 0.250000 0.046(9) Uiso 0.49(4) 2 d S . . . .
O6 O 0.1258(2) 0.2916(3) 0.1258(2) 0.0203(18) Uani 1 2 d S T P . .
O7 O 0.0957(3) 0.2299(2) 0.2299(2) 0.0224(19) Uani 1 2 d S T P . .
O8 O 0.0582(2) 0.1895(3) 0.0582(2) 0.0189(17) Uani 1 2 d S T P . .
O9 O 0.0502(2) 0.2947(2) 0.1804(2) 0.0229(13) Uani 1 1 d . . . . .
O6W O 0.0603(2) 0.3006(4) 0.0603(2) 0.032(2) Uani 1 2 d S T P . .
O7W O 0.000000 0.0881(5) 0.0881(5) 0.068(7) Uani 1 4 d S T P . .


_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
W1 O1 2.370(9) . ?
W1 O3 1.827(6) 72 ?
W1 O3 1.827(6) . ?
W1 O4 1.965(4) . ?
W1 O4 1.965(4) 9 ?
W1 O8 1.742(9) . ?
W2 O2 2.340(6) 9 ?
W2 O3 2.082(6) . ?
W2 O5 1.756(6) . ?
W2 O6 1.939(4) . ?
W2 O7 1.9025(13) . ?
W2 O9 1.728(7) . ?
As1 O1 1.694(17) . ?
As1 O2 1.684(9) 5 ?
As1 O2 1.684(9) 9 ?
As1 O2 1.684(9) . ?
K1 O1W 2.707(17) . ?
K1 O7 2.966(9) . ?
K1 O9 2.888(7) 67 ?
K1 O9 2.888(7) . ?
K1 O9 2.888(7) 18 ?
K1 O9 2.888(7) 52 ?
Na1 O1W 2.707(17) . ?
Na1 O7 2.966(9) . ?
Na1 O9 2.888(7) 67 ?
Na1 O9 2.888(7) . ?
Na1 O9 2.888(7) 18 ?
Na1 O9 2.888(7) 52 ?
Na2 O2W 2.68(3) 72 ?
Na2 O2W 2.68(3) . ?
Na2 O3W 2.358(10) 72 ?
Na2 O3W 2.358(10) . ?
Na2 O5 2.779(8) 72 ?
Na2 O5 2.779(8) . ?
O2W O2W 0.00(4) 72 ?
O3W O3W 0.00(2) 72 ?
O3W O5W 1.127(10) 77 ?
O5W O5W 1.55(3) 81 ?
O5W O5W 1.55(3) 77 ?

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
O3 W1 O1 85.0(3) . . ?
O3 W1 O1 85.0(3) 72 . ?
O3 W1 O3 90.1(4) 72 . ?
O3 W1 O4 157.6(3) 72 . ?
O3 W1 O4 87.9(3) 72 9 ?
O3 W1 O4 157.6(3) . 9 ?
O3 W1 O4 87.9(3) . . ?
O4 W1 O1 72.6(3) 9 . ?
O4 W1 O1 72.6(3) . . ?
O4 W1 O4 85.6(5) 9 . ?
O8 W1 O1 168.6(5) . . ?
O8 W1 O3 102.9(3) . 72 ?
O8 W1 O3 102.9(3) . . ?
O8 W1 O4 99.2(3) . 9 ?
O8 W1 O4 99.2(3) . . ?
O3 W2 O2 80.3(3) . 9 ?
O5 W2 O2 85.4(3) . 9 ?
O5 W2 O3 165.7(3) . . ?
O5 W2 O6 93.6(3) . . ?
O5 W2 O7 94.9(4) . . ?
O6 W2 O2 72.5(3) . 9 ?
O6 W2 O3 82.4(3) . . ?
O7 W2 O2 85.0(3) . 9 ?
O7 W2 O3 83.7(3) . . ?
O7 W2 O6 155.2(4) . . ?
O9 W2 O2 170.1(3) . 9 ?
O9 W2 O3 92.7(3) . . ?
O9 W2 O5 101.5(3) . . ?
O9 W2 O6 99.8(3) . . ?
O9 W2 O7 101.3(4) . . ?
O2 As1 O1 108.4(3) 9 . ?
O2 As1 O1 108.4(3) 5 . ?
O2 As1 O1 108.4(3) . . ?
O2 As1 O2 110.5(3) 9 . ?
O2 As1 O2 110.5(3) 9 5 ?
O2 As1 O2 110.5(3) 5 . ?
O1W K1 O7 76.2(2) . . ?
O1W K1 O9 82.41(17) . 52 ?
O1W K1 O9 82.41(17) . . ?
O1W K1 O9 82.41(17) . 18 ?
O1W K1 O9 82.41(17) . 67 ?
O9 K1 O7 57.35(14) . . ?
O9 K1 O7 118.47(16) 52 . ?
O9 K1 O7 118.47(16) 18 . ?
O9 K1 O7 57.35(14) 67 . ?
O9 K1 O9 164.8(3) 52 67 ?
O9 K1 O9 63.1(3) 18 67 ?
O9 K1 O9 164.8(3) . 18 ?
O9 K1 O9 63.1(3) . 52 ?
O9 K1 O9 114.7(3) 18 52 ?
O9 K1 O9 114.7(3) . 67 ?
O1W Na1 O7 76.2(2) . . ?
O1W Na1 O9 82.41(17) . . ?
O1W Na1 O9 82.41(17) . 18 ?
O1W Na1 O9 82.41(17) . 67 ?
O1W Na1 O9 82.41(17) . 52 ?
O9 Na1 O7 118.47(16) 18 . ?
O9 Na1 O7 57.35(14) 67 . ?
O9 Na1 O7 57.35(14) . . ?
O9 Na1 O7 118.47(16) 52 . ?
O9 Na1 O9 114.7(3) 18 52 ?
O9 Na1 O9 114.7(3) . 67 ?
O9 Na1 O9 164.8(3) 52 67 ?
O9 Na1 O9 63.1(3) 18 67 ?
O9 Na1 O9 63.1(3) . 52 ?
O9 Na1 O9 164.8(3) . 18 ?
O2W Na2 O2W 0.0(13) . 72 ?
O2W Na2 O5 76.4(4) . 72 ?
O2W Na2 O5 76.4(4) 72 72 ?
O2W Na2 O5 76.4(4) 72 . ?
O2W Na2 O5 76.4(4) . . ?
O3W Na2 O2W 128.8(6) 72 72 ?
O3W Na2 O2W 128.8(6) . . ?
O3W Na2 O2W 128.8(6) . 72 ?
O3W Na2 O2W 128.8(6) 72 . ?
O3W Na2 O3W 0.0(3) 72 . ?
O3W Na2 O5 64.2(2) . . ?
O3W Na2 O5 64.2(2) 72 . ?
O3W Na2 O5 64.2(2) . 72 ?
O3W Na2 O5 64.2(2) 72 72 ?
O5 Na2 O5 76.8(3) . 72 ?
W1 O1 W1 92.9(5) 5 . ?
W1 O1 W1 92.9(5) 5 9 ?
W1 O1 W1 92.9(5) 9 . ?
As1 O1 W1 123.2(3) . . ?
As1 O1 W1 123.2(3) . 9 ?
As1 O1 W1 123.2(3) . 5 ?
W2 O2 W2 92.9(3) 67 5 ?
As1 O2 W2 125.2(3) . 5 ?
As1 O2 W2 125.2(3) . 67 ?
O2W O2W Na2 90(10) 72 . ?
W1 O3 W2 145.3(3) . . ?
O3W O3W Na2 90(3) 72 . ?
O3W O3W O5W 133.4(5) 72 77 ?
O5W O3W Na2 136.2(14) 77 . ?
W1 O4 W1 121.9(5) . 5 ?
W2 O5 Na2 134.8(3) . . ?
W2 O5 Na2 117.4(3) . 81 ?
Na2 O5 Na2 107.7(2) . 81 ?
O5W O5W O5W 120.000(5) 81 77 ?
W2 O6 W2 122.0(5) . 72 ?
W2 O7 W2 165.0(6) . 67 ?
W2 O7 K1 96.9(3) . . ?
W2 O7 K1 96.9(3) 67 . ?
W2 O7 Na1 96.9(3) 67 . ?
W2 O7 Na1 96.9(3) . . ?
W2 O9 K1 104.2(3) . . ?
W2 O9 Na1 104.2(3) . . ?

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 W1 O3 W2 69.5(6) . . . . ?
O1 As1 O2 W2 62.5(4) . . . 5 ?
O1 As1 O2 W2 -62.5(4) . . . 67 ?
O2 W2 O5 Na2 70.1(5) 9 . . . ?
O2 W2 O5 Na2 -105.9(3) 9 . . 81 ?
O2 As1 O1 W1 120.000(1) . . . . ?
O2 As1 O1 W1 -120.000(1) 9 . . 5 ?
O2 As1 O1 W1 0.000(0) 5 . . 9 ?
O2 As1 O1 W1 120.000(1) 9 . . 9 ?
O2 As1 O1 W1 0.000(0) . . . 5 ?
O2 As1 O1 W1 -120.000(1) . . . 9 ?
O2 As1 O1 W1 120.000(1) 5 . . 5 ?
O2 As1 O1 W1 -120.000(1) 5 . . . ?
O2 As1 O1 W1 0.000(1) 9 . . . ?
O2 As1 O2 W2 178.84(6) 5 . . 67 ?
O2 As1 O2 W2 -178.84(6) 9 . . 5 ?
O2 As1 O2 W2 56.2(8) 9 . . 67 ?
O2 As1 O2 W2 -56.2(8) 5 . . 5 ?
O3 W1 O3 W2 -15.5(8) 72 . . . ?
O3 W2 O5 Na2 71.0(13) . . . . ?
O3 W2 O5 Na2 -105.0(11) . . . 81 ?
O3 W2 O9 K1 80.1(3) . . . . ?
O3 W2 O9 Na1 80.1(3) . . . . ?
O4 W1 O3 W2 69.2(11) 9 . . . ?
O4 W1 O3 W2 142.2(6) . . . . ?
O5 W2 O9 K1 -101.4(3) . . . . ?
O5 W2 O9 Na1 -101.4(3) . . . . ?
O6 W2 O5 Na2 -2.0(5) . . . . ?
O6 W2 O5 Na2 -178.0(4) . . . 81 ?
O6 W2 O9 K1 162.8(3) . . . . ?
O6 W2 O9 Na1 162.8(3) . . . . ?
O7 W2 O5 Na2 -21.3(4) . . . 81 ?
O7 W2 O5 Na2 154.7(5) . . . . ?
O7 W2 O9 K1 -4.0(4) . . . . ?
O7 W2 O9 Na1 -4.0(4) . . . . ?
O8 W1 O3 W2 -118.8(6) . . . . ?
O9 W2 O5 Na2 -102.7(5) . . . . ?
O9 W2 O5 Na2 81.3(4) . . . 81 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.490 -0.858 -0.745 10463.4 1706.0 '172.8 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.577
_oxdiff_exptl_absorpt_empirical_full_min 0.668

# start Validation Reply Form
_vrf_PLAT214_jcr268_auto_v1      
;
PROBLEM: Atom O4W (Anion/Solvent) ADP max/min Ratio 14.8 prolat
RESPONSE: O4W is a disordered hydration water molecule.
;
_vrf_PLAT971_jcr268_auto_v1      
;
PROBLEM: Check Calcd Resid. Dens. 0.52Ang From O1W 3.68 eA-3
RESPONSE: Residual electron density originates from missing hydrate
water molecules. A solvent mask (aka SQUEEZE) did not lead to any significant
improvement.
;
_vrf_PLAT975_jcr268_auto_v1      
;
PROBLEM: Check Calcd Resid. Dens. 0.52Ang From O1W . 3.68 eA-3
RESPONSE: Residual electron density originates from missing hydrate
water molecules. A solvent mask (aka SQUEEZE) did not lead to any significant
improvement.
;
_vrf_PLAT196_jcr268_auto_v1      
;
PROBLEM: No TEMP record and _measurement_temperature .NE. 293 Degree
RESPONSE: The measurement temperature was 100 K.
;
_vrf_PLAT306_jcr268_auto_v1      
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: The oxygen atoms belong to hydrate water molecules.
Protons were not simulated.
;
_vrf_PLAT972_jcr268_auto_v1      
;
PROBLEM: Check Calcd Resid. Dens. 0.83Ang From K1 -2.55 eA-3
RESPONSE: Residual electron density originates from disordered
hydration water molecules. A solvent mask (aka SQUEEZE) did not lead to any
significant improvement.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_chemical_properties_physical    Hygroscopic
