# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_jcr22-jcr13_auto_jcr_v1
_database_code_depnum_ccdc_archive 'CCDC 2441126'
loop_
_audit_author_name
_audit_author_address
'Jan-Christian Raabe'
;University Hamburg
Germany
;
_audit_update_record             
;
2025-05-06 deposited with the CCDC.	2025-05-26 downloaded from the CCDC.
;
_audit_creation_date             2025-04-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
?
?
?
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Al0.5 O20 P0.5 W5.5), 4[C16H36N+]'
_chemical_formula_sum            'C64 H144 Al N4 O40 P W11'
_chemical_formula_weight         3690.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         C87H187O40N5PAlW11
_chemical_oxdiff_usercomment     'Poller/Albert, 01.07.2024, Mo, 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        Im-3m
_space_group_name_Hall           '-I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+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, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+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'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+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, 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'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+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, y+1/2, z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'x+1/2, -y+1/2, z+1/2'
'z+1/2, -y+1/2, -x+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'
'-z+1/2, x+1/2, y+1/2'
'y+1/2, -z+1/2, x+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, -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'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   17.4284(2)
_cell_length_b                   17.4284(2)
_cell_length_c                   17.4284(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5293.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    22139
_cell_measurement_temperature    99.95(13)
_cell_measurement_theta_max      27.3480
_cell_measurement_theta_min      2.8310
_shelx_estimated_absorpt_T_max   0.447
_shelx_estimated_absorpt_T_min   0.221
_exptl_absorpt_coefficient_mu    11.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39767
_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    2.315
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3436
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65214
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.962
_diffrn_reflns_theta_min         2.337
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  32.00   1.00   90.00    --   -8.55 -99.00  90.00   47
  2  ω    -19.00  82.00   1.00   90.00    --    9.33  57.00  90.00  101
  3  ω    -19.00  82.00   1.00   90.00    --    9.33  57.00 -30.00  101
  4  ω    -64.00  37.00   1.00   90.00    --    9.33 -57.00 -60.00  101
  5  ω    -42.00  42.00   1.00   90.00    --    9.33 -76.00 161.91   84
  6  ω     22.00  86.00   1.00   90.00    --    9.33-155.00 109.64   64
  7  ω    -15.00  84.00   1.00   90.00    --    9.33  38.00 -90.00   99
  8  ω     20.00  85.00   1.00   90.00    --    9.33-153.00 -36.94   65
  9  ω    -65.00 -27.00   1.00   90.00    --   -8.55 125.00 142.60   38
 10  ω    -84.00 -42.00   1.00   90.00    --   -8.55 153.00 -82.00   42
 11  ω    -84.00 -42.00   1.00   90.00    --   -8.55 153.00  15.58   42
 12  ω    -41.00  21.00   1.00   90.00    --   -8.55  77.00  90.00   62
 13  ω      7.00  67.00   1.00   90.00    --    9.33-127.00 178.60   60
;
_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      -0.0339847000
_diffrn_orient_matrix_UB_12      0.0160559000
_diffrn_orient_matrix_UB_13      -0.0155815000
_diffrn_orient_matrix_UB_21      -0.0214510000
_diffrn_orient_matrix_UB_22      -0.0313458000
_diffrn_orient_matrix_UB_23      0.0146998000
_diffrn_orient_matrix_UB_31      -0.0062034000
_diffrn_orient_matrix_UB_32      0.0205865000
_diffrn_orient_matrix_UB_33      0.0345203000
_diffrn_oxdiff_digest_hkl        
;
01006f844450679c9e9affaecf1e2559f67cf5
;
_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                537
_reflns_number_total             724
_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         8.206
_refine_diff_density_min         -2.474
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         724
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0571
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+203.4304P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1046
_refine_special_details          
'SQUEEZE,Disorder of the PO4 tetrahedron, constraints were used to force that the P atom has a positive displacement parameter'
_olex2_refinement_description    
;
1. Shared sites
{W1, Al1}
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(W1) = Uanis(Al1)
3. Others
 Fixed Sof: W1(0.229167) Al1(0.020833) O1(0.083333)
 Fixed Uiso: P1(0.015)
;
_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 0.000000 0.14299(3) 0.14299(3) 0.0747(4) Uani 0.9167 4 d S T P A 1
P1 P 0.000000 0.000000 0.000000 0.015 Uiso 1 48 d S U P A .
Al1 Al 0.000000 0.14299(3) 0.14299(3) 0.0747(4) Uani 0.0833 4 d S T P A 2
O1 O 0.0505(7) 0.0505(7) 0.0505(7) 0.0342(19) Uani 0.5 6 d S TU P . .
O2 O 0.0737(4) 0.1770(6) 0.0737(4) 0.104(4) Uani 1 2 d S T P . .
O3 O 0.000000 0.2101(6) 0.2101(6) 0.133(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 2.443(12) 2 ?
W1 O1 2.443(12) . ?
W1 O2 1.860(3) 62 ?
W1 O2 1.860(3) . ?
W1 O2 1.860(3) 11 ?
W1 O2 1.860(3) 54 ?
W1 O3 1.655(14) . ?
P1 O1 1.53(2) 3 ?
P1 O1 1.53(2) 52 ?
P1 O1 1.53(2) 50 ?
P1 O1 1.53(2) 2 ?
P1 O1 1.53(2) . ?
P1 O1 1.53(2) 49 ?
P1 O1 1.53(2) 4 ?
P1 O1 1.53(2) 51 ?
Al1 O2 1.860(3) 62 ?
Al1 O2 1.860(3) 54 ?
Al1 O2 1.860(3) . ?
Al1 O2 1.860(3) 11 ?
Al1 O3 1.655(14) . ?
O1 O1 1.76(2) 2 ?
O1 O1 1.76(2) 4 ?
O1 O1 1.76(2) 51 ?

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 O1 42.3(8) 2 . ?
O2 W1 O1 91.8(5) 54 . ?
O2 W1 O1 91.8(5) . 2 ?
O2 W1 O1 91.8(5) 62 . ?
O2 W1 O1 91.8(5) 11 2 ?
O2 W1 O1 62.1(4) 11 . ?
O2 W1 O1 62.1(4) 62 2 ?
O2 W1 O1 62.1(4) 54 2 ?
O2 W1 O1 62.1(4) . . ?
O2 W1 O2 86.3(6) 62 54 ?
O2 W1 O2 86.3(6) 11 . ?
O2 W1 O2 87.4(6) 54 . ?
O2 W1 O2 87.4(6) 62 11 ?
O2 W1 O2 153.0(7) 62 . ?
O2 W1 O2 153.0(7) 54 11 ?
O3 W1 O1 158.9(4) . 2 ?
O3 W1 O1 158.9(4) . . ?
O3 W1 O2 103.5(3) . 62 ?
O3 W1 O2 103.5(3) . . ?
O3 W1 O2 103.5(3) . 54 ?
O3 W1 O2 103.5(3) . 11 ?
O1 P1 O1 180(2) . 49 ?
O1 P1 O1 109.471(2) . 50 ?
O1 P1 O1 70.529(2) . 2 ?
O1 P1 O1 109.471(1) . 52 ?
O1 P1 O1 70.5 52 51 ?
O1 P1 O1 70.529(1) 49 52 ?
O1 P1 O1 109.471(2) 49 2 ?
O1 P1 O1 70.529(1) . 4 ?
O1 P1 O1 70.529(2) 49 50 ?
O1 P1 O1 70.5 52 2 ?
O1 P1 O1 180(2) 52 4 ?
O1 P1 O1 109.471(1) 49 51 ?
O1 P1 O1 70.5 50 4 ?
O1 P1 O1 109.5 52 3 ?
O1 P1 O1 70.529(1) 49 3 ?
O1 P1 O1 109.5 2 51 ?
O1 P1 O1 70.5 2 3 ?
O1 P1 O1 70.5 4 3 ?
O1 P1 O1 180(2) 2 50 ?
O1 P1 O1 109.5 4 51 ?
O1 P1 O1 109.471(1) 49 4 ?
O1 P1 O1 70.5 50 51 ?
O1 P1 O1 109.5 2 4 ?
O1 P1 O1 180(2) 3 51 ?
O1 P1 O1 109.5 52 50 ?
O1 P1 O1 109.5 50 3 ?
O1 P1 O1 109.471(1) . 3 ?
O1 P1 O1 70.529(1) . 51 ?
O2 Al1 O2 86.3(6) 62 54 ?
O2 Al1 O2 153.0(7) 54 11 ?
O2 Al1 O2 87.4(6) 62 11 ?
O2 Al1 O2 86.3(6) 11 . ?
O2 Al1 O2 87.4(6) 54 . ?
O2 Al1 O2 153.0(7) 62 . ?
O3 Al1 O2 103.5(3) . . ?
O3 Al1 O2 103.5(3) . 11 ?
O3 Al1 O2 103.5(3) . 62 ?
O3 Al1 O2 103.5(3) . 54 ?
W1 O1 W1 92.3(6) 8 . ?
W1 O1 W1 92.3(6) 8 4 ?
W1 O1 W1 92.3(6) 4 . ?
P1 O1 W1 123.6(4) . 8 ?
P1 O1 W1 123.6(4) . . ?
P1 O1 W1 123.6(4) . 4 ?
P1 O1 O1 54.736(1) . 2 ?
P1 O1 O1 54.736(1) . 4 ?
P1 O1 O1 54.736(1) . 51 ?
O1 O1 W1 131.27(14) 2 8 ?
O1 O1 W1 68.9(4) 4 4 ?
O1 O1 W1 131.27(14) 51 4 ?
O1 O1 W1 131.27(14) 51 . ?
O1 O1 W1 68.9(4) 51 8 ?
O1 O1 W1 131.27(14) 2 4 ?
O1 O1 W1 131.27(14) 4 8 ?
O1 O1 W1 131.27(14) 4 . ?
O1 O1 W1 68.9(4) 2 . ?
O1 O1 O1 90.001(1) 4 51 ?
O1 O1 O1 90.001(1) 51 2 ?
O1 O1 O1 90.001(1) 4 2 ?
W1 O2 W1 142.7(6) 8 . ?

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 O2 W1 -41.1(10) 2 . . 8 ?
O1 W1 O2 W1 -9.7(9) . . . 8 ?
O1 P1 O1 W1 120.000(0) 51 . . . ?
O1 P1 O1 W1 0.000(0) 2 . . . ?
O1 P1 O1 W1 -120.0 51 . . 4 ?
O1 P1 O1 W1 -60.0 52 . . 8 ?
O1 P1 O1 W1 -120.0 4 . . . ?
O1 P1 O1 W1 60.0 52 . . . ?
O1 P1 O1 W1 0.0 4 . . 4 ?
O1 P1 O1 W1 -120.0 2 . . 8 ?
O1 P1 O1 W1 0.000(0) 51 . . 8 ?
O1 P1 O1 W1 120.0 4 . . 8 ?
O1 P1 O1 W1 180.0 52 . . 4 ?
O1 P1 O1 W1 180.0 50 . . . ?
O1 P1 O1 W1 120.000(0) 2 . . 4 ?
O1 P1 O1 W1 -60.000(0) 3 . . . ?
O1 P1 O1 W1 -60.0 50 . . 4 ?
O1 P1 O1 W1 60.0 3 . . 4 ?
O1 P1 O1 W1 60.000(0) 50 . . 8 ?
O1 P1 O1 W1 180.000(0) 3 . . 8 ?
O1 P1 O1 O1 -60.000(0) 52 . . 51 ?
O1 P1 O1 O1 -120.0 51 . . 4 ?
O1 P1 O1 O1 180.000(0) 50 . . 2 ?
O1 P1 O1 O1 -60.0 3 . . 2 ?
O1 P1 O1 O1 60.000(0) 52 . . 2 ?
O1 P1 O1 O1 -60.000(0) 50 . . 4 ?
O1 P1 O1 O1 120.0 4 . . 51 ?
O1 P1 O1 O1 -120.000(0) 2 . . 51 ?
O1 P1 O1 O1 120.0 2 . . 4 ?
O1 P1 O1 O1 180.0 52 . . 4 ?
O1 P1 O1 O1 60.0 3 . . 4 ?
O1 P1 O1 O1 60.000(0) 50 . . 51 ?
O1 P1 O1 O1 120.0 51 . . 2 ?
O1 P1 O1 O1 -120.000(0) 4 . . 2 ?
O1 P1 O1 O1 180.000(0) 3 . . 51 ?
O2 W1 O2 W1 -103.1(9) 54 . . 8 ?
O2 W1 O2 W1 50.6(12) 11 . . 8 ?
O2 W1 O2 W1 -26.4(9) 62 . . 8 ?
O3 W1 O2 W1 153.6(9) . . . 8 ?

_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 0.598 -0.992 -0.744 4059.7 991.3 '8 C16H36N+'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_special_details  ?
_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.680

# start Validation Reply Form
_vrf_PLAT971_jcr22-jcr13_auto_jcr_v1 
;
PROBLEM: Check Calcd Resid. Dens. 0.00Ang From P1 13.77 eA-3
RESPONSE: The phosphorus atom is the center of a disorder (inversion
of the asymmetric unit (AU) at P1). The phosphorus is located in a 
tetrahedral environment of four oxygen atoms. The remaining electron 
density is a result that some PO4 tetrahedra in different unit cells 
are rotated by 90 degrees to each other.

We tried to refine this position with other elements (Al, W and O)
but P results in the best model.

Residual electron density around the phosphorus could also be a
result of the constraints we put in to force the phosphorus atom to
have a positive displacement parameter or of isotropic treatment of
this atom.
;
_vrf_PLAT973_jcr22-jcr13_auto_jcr_v1 
;
PROBLEM: Check Calcd Positive Resid. Density on W1 2.30 eA-3
RESPONSE: This effect might be caused by the difficulty to account
correctly the absorption effect of the heavy atom W.
;
_vrf_PLAT097_jcr22-jcr13_auto_jcr_v1 
;
PROBLEM: Large Reported Max. (Positive) Residual Density 8.21 eA-3
RESPONSE: This effect might be caused by the difficulty to account
correctly the absorption effect of the heavy atom W.
;
_vrf_PLAT196_jcr22-jcr13_auto_jcr_v1 
;
PROBLEM: No TEMP record and measurement temperature .NE. 293 Degree
RESPONSE: The measurement temperature was 100 K.
;
_vrf_PLAT201_jcr22-jcr13_auto_jcr_v1 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 1 Report
RESPONSE: The phosphorus atom is the center of a disorder (inversion
of the asymmetric unit (AU) at P1). Therefore, a non positive 
definite (NPD) was obtained. The displacement parameters were 
therefore set to a reasonable positive value using constraints. 
Splitting and inverting the AU failed.
;
_vrf_PLAT241_jcr22-jcr13_auto_jcr_v1 
;
PROBLEM: High 'MainMol' Ueq as Compared to Neighbors of O3 Check
RESPONSE: This indicates a disorder for the terminal oxygen atoms.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile'
