# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_jcr88
_database_code_depnum_ccdc_archive 'CCDC 2205006'
loop_
_audit_author_name
_audit_author_address
'J.-C. Raabe'
;Hamburg University
Germany
;
_audit_update_record             
;
2022-09-02 deposited with the CCDC.	2023-07-17 downloaded from the CCDC.
;
_audit_creation_date             2022-09-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Jan-Christian.Raabe@chemie.uni-hamburg.de
Maximilian.Poller@chemie.uni-hamburg.de
Tobias.Esser@chemie.uni-hamburg.de
Jakob.Albert@chemie.uni-hamburg.de
_chemical_name_common            ?
_chemical_name_systematic        H9PMo9O34
_chemical_formula_moiety         '2(Mo9 O34 P1), 12(O)'
_chemical_formula_sum            'P1 Mo9 O34'
_chemical_formula_weight         3068.86
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'O204 P6 K54 Mo54 C1 H1 '
_chemical_oxdiff_usercomment     'Raabe/Albert, 4.11.2021, Mo, 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'

_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      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'

_cell_length_a                   14.11802(9)
_cell_length_b                   14.11802(9)
_cell_length_c                   10.65823(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1839.77(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    89401
_cell_measurement_temperature    99.95(13)
_cell_measurement_theta_max      32.6830
_cell_measurement_theta_min      3.3380
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.770
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1426
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            118316
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.887
_diffrn_reflns_theta_min         3.462
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2063
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  15.00   1.00    7.50    --  -18.04 -77.00 -60.00   57
  2  ω     -9.00  92.00   1.00    7.50    --   18.98  57.00 -90.00  101
  3  ω     -1.00  70.00   1.00    7.50    --   18.98-117.00 105.00   71
  4  ω      8.00  78.00   1.00    7.50    --   18.98-129.00 -98.72   70
  5  ω    -22.00  99.00   1.00    7.50    --   18.98  19.00 120.00  121
  6  ω    -61.00  26.00   1.00    7.50    --   18.98 -19.00 -90.00   87
  7  ω    -61.00  26.00   1.00    7.50    --   18.98 -19.00 -30.00   87
  8  ω    -61.00  26.00   1.00    7.50    --   18.98 -19.00 120.00   87
  9  ω      7.00  76.00   1.00    7.50    --   18.98-126.00   5.16   69
 10  ω     -9.00  92.00   1.00    7.50    --   18.98  57.00-180.00  101
 11  ω    -89.00 -38.00   1.00    7.50    --  -18.04 148.00  92.64   51
 12  ω    -94.00 -43.00   1.00    7.50    --  -18.04 154.00-159.00   51
 13  ω    -42.00  15.00   1.00    7.50    --  -18.04 -77.00  30.00   57
 14  ω    -42.00  15.00   1.00    7.50    --  -18.04 -77.00-120.00   57
 15  ω      7.00  76.00   1.00    7.50    --   18.98-127.00 174.56   69
 16  ω    -69.00 107.00   1.00    7.50    --   18.98   0.00-180.00  176
 17  ω      2.00  73.00   1.00    7.50    --   18.98-121.00  57.09   71
 18  ω    -54.00  47.00   1.00    7.50    --   18.98 -57.00  90.00  101
 19  ω    -69.00 107.00   1.00    7.50    --   18.98   0.00-120.00  176
 20  ω    -69.00  82.00   1.00    7.50    --   18.98   0.00 -90.00  151
 21  ω    -69.00 107.00   1.00    7.50    --   18.98   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      -0.0494082000
_diffrn_orient_matrix_UB_12      -0.0001405000
_diffrn_orient_matrix_UB_13      0.0127481000
_diffrn_orient_matrix_UB_21      0.0292490000
_diffrn_orient_matrix_UB_22      0.0579480000
_diffrn_orient_matrix_UB_23      0.0029196000
_diffrn_orient_matrix_UB_31      -0.0083258000
_diffrn_orient_matrix_UB_32      0.0025915000
_diffrn_orient_matrix_UB_33      -0.0652227000
_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         0.890
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                4469
_reflns_number_total             4488
_reflns_odcompleteness_completeness 99.85
_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 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.220
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 
;
 Flack x determined using 2090 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(16)
_refine_ls_extinction_coef       0.00117(14)
_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   1.111
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         4488
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0181
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0252P)²+3.9554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0498
_refine_special_details          SQUEEZE
_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
Mo1 Mo 0.39850(2) 0.11758(2) 0.16726(3) 0.00890(6) Uani 1 1 d . . . . .
Mo2 Mo 0.59849(2) 0.06087(2) 0.22443(3) 0.00838(6) Uani 1 1 d . . . . .
Mo3 Mo 0.75701(2) 0.49337(2) 0.49082(3) 0.00657(6) Uani 1 1 d . . . . .
P1 P 0.666667 0.333333 0.21305(14) 0.0069(2) Uani 1 3 d S T P . .
O1 O 0.5869(2) 0.2170(2) 0.1678(3) 0.0099(4) Uani 1 1 d . . . . .
O2 O 0.666667 0.333333 0.3595(4) 0.0082(7) Uani 1 3 d S T P . .
O3 O 0.8262(2) 0.5941(2) 0.5978(3) 0.0116(5) Uani 1 1 d . . . . .
O4 O 0.6217(2) 0.4129(2) 0.5612(2) 0.0085(4) Uani 1 1 d . . . . .
O5 O 0.4488(2) 0.0176(2) 0.2162(3) 0.0118(4) Uani 1 1 d . . . . .
O6 O 0.7403(2) 0.1494(2) 0.1670(3) 0.0121(4) Uani 1 1 d . . . . .
O7 O 0.2636(2) 0.0380(2) 0.2048(3) 0.0139(5) Uani 1 1 d . . . . .
O8 O 0.5744(3) 0.0353(3) 0.0199(3) 0.0162(6) Uani 1 1 d . . . . .
O9 O 0.6267(2) 0.1118(2) 0.3824(3) 0.0106(4) Uani 1 1 d . . . . .
O10 O 0.3991(3) 0.1056(3) 0.0079(3) 0.0191(6) Uani 1 1 d . . . . .
O11 O 0.5895(2) -0.0624(2) 0.2404(3) 0.0145(5) Uani 1 1 d . . . . .
O12 O 0.4388(2) 0.1684(2) 0.3674(3) 0.0099(4) Uani 1 1 d . . . . .
O1W O 0.1679(2) -0.1646(3) 0.3161(3) 0.0175(6) Uani 1 1 d . . . . .
O2W O 0.2264(4) -0.0198(4) 0.4760(5) 0.0448(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
Mo1 O1 2.304(3) . ?
Mo1 O5 1.941(3) . ?
Mo1 O6 1.936(3) 5_665 ?
Mo1 O7 1.706(3) . ?
Mo1 O10 1.708(3) . ?
Mo1 O12 2.232(3) . ?
Mo2 O1 2.369(3) . ?
Mo2 O5 1.886(3) . ?
Mo2 O6 1.856(3) . ?
Mo2 O8 2.208(3) . ?
Mo2 O9 1.796(3) . ?
Mo2 O11 1.690(3) . ?
Mo3 O2 2.410(3) . ?
Mo3 O3 1.699(3) . ?
Mo3 O4 1.826(3) . ?
Mo3 O4 2.054(3) 5_665 ?
Mo3 O9 2.072(3) 3_655 ?
Mo3 O12 1.779(3) 5_665 ?
P1 O1 1.533(2) 3_655 ?
P1 O1 1.533(2) . ?
P1 O1 1.533(2) 5_665 ?
P1 O2 1.561(5) . ?

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 Mo1 O1 73.28(10) . . ?
O5 Mo1 O12 81.35(11) . . ?
O6 Mo1 O1 84.33(10) 5_665 . ?
O6 Mo1 O5 152.50(11) 5_665 . ?
O6 Mo1 O12 78.07(11) 5_665 . ?
O7 Mo1 O1 165.72(13) . . ?
O7 Mo1 O5 98.72(13) . . ?
O7 Mo1 O6 99.51(12) . 5_665 ?
O7 Mo1 O10 103.12(15) . . ?
O7 Mo1 O12 90.52(12) . . ?
O10 Mo1 O1 90.08(13) . . ?
O10 Mo1 O5 99.99(15) . . ?
O10 Mo1 O6 95.72(15) . 5_665 ?
O10 Mo1 O12 165.85(13) . . ?
O12 Mo1 O1 76.74(10) . . ?
O5 Mo2 O1 72.64(10) . . ?
O5 Mo2 O8 81.11(12) . . ?
O6 Mo2 O1 80.95(10) . . ?
O6 Mo2 O5 149.31(13) . . ?
O6 Mo2 O8 79.07(13) . . ?
O8 Mo2 O1 79.87(11) . . ?
O9 Mo2 O1 88.35(11) . . ?
O9 Mo2 O5 99.29(12) . . ?
O9 Mo2 O6 95.24(12) . . ?
O9 Mo2 O8 167.56(12) . . ?
O11 Mo2 O1 168.51(13) . . ?
O11 Mo2 O5 100.18(13) . . ?
O11 Mo2 O6 103.10(13) . . ?
O11 Mo2 O8 90.27(14) . . ?
O11 Mo2 O9 101.84(14) . . ?
O3 Mo3 O2 170.94(12) . . ?
O3 Mo3 O4 103.29(13) . . ?
O3 Mo3 O4 98.77(12) . 5_665 ?
O3 Mo3 O9 98.84(12) . 3_655 ?
O3 Mo3 O12 103.56(13) . 5_665 ?
O4 Mo3 O2 72.20(10) 5_665 . ?
O4 Mo3 O2 75.92(10) . . ?
O4 Mo3 O4 86.86(15) . 5_665 ?
O4 Mo3 O9 76.88(11) 5_665 3_655 ?
O4 Mo3 O9 154.28(11) . 3_655 ?
O9 Mo3 O2 80.16(9) 3_655 . ?
O12 Mo3 O2 85.38(12) 5_665 . ?
O12 Mo3 O4 153.60(11) 5_665 5_665 ?
O12 Mo3 O4 101.34(12) 5_665 . ?
O12 Mo3 O9 85.87(11) 5_665 3_655 ?
O1 P1 O1 110.56(12) 3_655 5_665 ?
O1 P1 O1 110.56(12) . 5_665 ?
O1 P1 O1 110.56(12) 3_655 . ?
O1 P1 O2 108.36(12) 3_655 . ?
O1 P1 O2 108.36(12) . . ?
O1 P1 O2 108.36(12) 5_665 . ?
Mo1 O1 Mo2 91.69(9) . . ?
P1 O1 Mo1 131.28(15) . . ?
P1 O1 Mo2 124.11(15) . . ?
Mo3 O2 Mo3 89.66(13) . 3_655 ?
Mo3 O2 Mo3 89.66(13) 5_665 . ?
Mo3 O2 Mo3 89.66(13) 5_665 3_655 ?
P1 O2 Mo3 125.50(9) . 3_655 ?
P1 O2 Mo3 125.50(9) . 5_665 ?
P1 O2 Mo3 125.50(9) . . ?
Mo3 O4 Mo3 122.20(13) . 3_655 ?
Mo2 O5 Mo1 122.33(14) . . ?
Mo2 O6 Mo1 153.78(16) . 3_655 ?
Mo2 O9 Mo3 142.90(15) . 5_665 ?
Mo3 O12 Mo1 154.66(15) 3_655 . ?

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 Mo2 O5 Mo1 2.15(15) . . . . ?
O1 Mo2 O6 Mo1 58.1(4) . . . 3_655 ?
O1 Mo2 O9 Mo3 -60.4(2) . . . 5_665 ?
O1 P1 O1 Mo1 -45.4(4) 5_665 . . . ?
O1 P1 O1 Mo1 -168.13(10) 3_655 . . . ?
O1 P1 O1 Mo2 61.9(3) 3_655 . . . ?
O1 P1 O1 Mo2 -175.30(11) 5_665 . . . ?
O1 P1 O2 Mo3 67.87(10) 3_655 . . . ?
O1 P1 O2 Mo3 -52.13(10) 5_665 . . . ?
O1 P1 O2 Mo3 -172.13(10) . . . . ?
O1 P1 O2 Mo3 -172.13(10) 3_655 . . 3_655 ?
O1 P1 O2 Mo3 67.87(10) . . . 5_665 ?
O1 P1 O2 Mo3 -52.13(10) 3_655 . . 5_665 ?
O1 P1 O2 Mo3 -172.13(10) 5_665 . . 5_665 ?
O1 P1 O2 Mo3 67.87(10) 5_665 . . 3_655 ?
O1 P1 O2 Mo3 -52.13(10) . . . 3_655 ?
O2 Mo3 O4 Mo3 1.13(14) . . . 3_655 ?
O2 P1 O1 Mo1 73.3(2) . . . . ?
O2 P1 O1 Mo2 -56.68(17) . . . . ?
O3 Mo3 O4 Mo3 -169.58(15) . . . 3_655 ?
O4 Mo3 O4 Mo3 -71.30(17) 5_665 . . 3_655 ?
O5 Mo2 O6 Mo1 88.8(5) . . . 3_655 ?
O5 Mo2 O9 Mo3 -132.5(2) . . . 5_665 ?
O6 Mo2 O5 Mo1 -29.7(3) . . . . ?
O6 Mo2 O9 Mo3 20.4(3) . . . 5_665 ?
O8 Mo2 O5 Mo1 -79.93(18) . . . . ?
O8 Mo2 O6 Mo1 139.5(4) . . . 3_655 ?
O8 Mo2 O9 Mo3 -41.7(7) . . . 5_665 ?
O9 Mo2 O5 Mo1 87.47(18) . . . . ?
O9 Mo2 O6 Mo1 -29.4(4) . . . 3_655 ?
O9 Mo3 O4 Mo3 -20.9(4) 3_655 . . 3_655 ?
O11 Mo2 O5 Mo1 -168.60(18) . . . . ?
O11 Mo2 O6 Mo1 -132.8(4) . . . 3_655 ?
O11 Mo2 O9 Mo3 125.0(3) . . . 5_665 ?
O12 Mo3 O4 Mo3 83.37(17) 5_665 . . 3_655 ?

_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 0.000 0.000 -0.400 285.8 62.4 '7 H2O'
2 0.333 0.667 0.356 70.3 37.5 '3.5 H2O'
3 0.667 0.333 0.856 70.3 36.9 '3.5 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'Dual Thickness MiTeGen'
_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 1.141
_oxdiff_exptl_absorpt_empirical_full_min 0.896

# start Validation Reply Form
_vrf_PLAT975_jcr88               
;
PROBLEM: Check Calcd Resid. Dens. 1.08Ang From O1W . 2.23 eA-3
RESPONSE: Residual density is disordered and minimally occupied water.
;
_vrf_PLAT306_jcr88               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: The isolated oxygen atom belongs to a crystal water
molecule. However, the protons cannot be meaningfully simulated due to strong
disorder.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_jcr101_0m_v1_sq
_database_code_depnum_ccdc_archive 'CCDC 2205007'
loop_
_audit_author_name
_audit_author_address
'J.-C. Raabe'
;Hamburg University
Germany
;
_audit_update_record             
;
2022-09-02 deposited with the CCDC.	2023-07-17 downloaded from the CCDC.
;
_audit_creation_date             2022-08-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Jan-Christian.Raabe@chemie.uni-hamburg.de
Maximilian.Poller@chemie.uni-hamburg.de
Jakob.Albert@chemie.uni-hamburg.de
_chemical_name_common            ?
_chemical_name_systematic        Na4H2PV3Mo9O40
_chemical_formula_moiety         'Mo9 Na4 O40 P V3, 2(O)'
_chemical_formula_sum            'Mo9 Na4 O42 P V3'
_chemical_formula_weight         1811.21
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+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'

_cell_length_a                   12.486(3)
_cell_length_b                   12.486(3)
_cell_length_c                   17.510(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2729.9(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9009
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.84
_shelx_estimated_absorpt_T_max   0.871
_shelx_estimated_absorpt_T_min   0.800
_exptl_absorpt_coefficient_mu    2.626
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5877
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1684
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.0180
0.00 -1.00 0.00 0.0290
1.00 0.00 -1.00 0.0210
-1.00 0.00 1.00 0.0260
0.00 1.00 -1.00 0.0080
0.00 -1.00 1.00 0.0300
0.00 0.00 -1.00 0.0190
0.00 0.00 1.00 0.0470
0.00 -1.00 -1.00 0.0190
0.00 1.00 1.00 0.0290
0.50 -0.50 1.00 0.0390
-0.50 0.50 -1.00 0.0140

_exptl_crystal_preparation       'Synthesized from Na2MoO4, Na2HPO4 and NaVO3'
_exptl_crystal_recrystallization_method 
'precipitation with KCl from aqueous solution'
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.054
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            140274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.574
_diffrn_reflns_theta_min         2.003
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4113
_reflns_number_total             4184
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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         2.892
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.52(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         4184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0303
_refine_ls_restrained_S_all      1.089
_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)+(0.0297P)²+15.1239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0784
_refine_special_details          
'Refined as a 2-component inversion twin.,Twin,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.48(6)
 0.52(6)
2. Shared sites
{Mo1, V1}
{Mo3, V3}
{Mo2, V2}
3. Uiso/Uaniso restraints and constraints
Uanis(Mo1) = Uanis(V1)
Uanis(Mo2) = Uanis(V2)
Uanis(Mo3) = Uanis(V3)
4. Others
 Fixed Sof: Mo1(0.75) Mo2(0.75) Mo3(0.75) V1(0.25) V2(0.25) V3(0.25)
;
_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
Mo1 Mo 0.96328(4) 0.19739(4) 0.14182(3) 0.01610(12) Uani 0.75 1 d . . P A 1
Mo2 Mo 1.19290(4) 0.04804(4) 0.14227(3) 0.01189(11) Uani 0.75 1 d . . P A 1
Mo3 Mo 1.15131(4) 0.23857(3) 0.00426(3) 0.01258(10) Uani 0.75 1 d . . P A 1
V1 V 0.96328(4) 0.19739(4) 0.14182(3) 0.01610(12) Uani 0.25 1 d . . P A 2
V2 V 1.19290(4) 0.04804(4) 0.14227(3) 0.01189(11) Uani 0.25 1 d . . P A 2
V3 V 1.15131(4) 0.23857(3) 0.00426(3) 0.01258(10) Uani 0.25 1 d . . P A 2
P1 P 1.000000 0.000000 0.000000 0.0059(3) Uani 1 4 d S T P A .
Na1 Na 1.43021(18) 0.1053(2) -0.00387(16) 0.0240(5) Uani 1 1 d . . . . .
O1 O 1.0546(3) 0.0848(3) 0.0503(2) 0.0110(6) Uani 1 1 d . . . . .
O2 O 1.0885(3) 0.1414(3) 0.1922(2) 0.0154(7) Uani 1 1 d . . . . .
O3 O 1.0532(3) 0.2896(3) 0.0856(2) 0.0168(7) Uani 1 1 d . . . . .
O4 O 1.2347(4) 0.1784(3) 0.0853(2) 0.0184(8) Uani 1 1 d . . . . .
O5 O 0.8908(4) 0.0684(3) 0.1692(2) 0.0173(8) Uani 1 1 d . . . . .
O6 O 1.2106(3) 0.1444(3) -0.0654(2) 0.0181(8) Uani 1 1 d . . . . .
O7 O 1.0340(3) 0.2529(3) -0.0628(2) 0.0164(7) Uani 1 1 d . . . . .
O8 O 0.9227(4) 0.2827(4) 0.2080(3) 0.0216(9) Uani 1 1 d . . . . .
O9 O 1.2874(3) 0.0504(4) 0.2095(2) 0.0183(8) Uani 1 1 d . . . . .
O10 O 1.2190(3) 0.3529(3) -0.0082(3) 0.0185(8) Uani 1 1 d . . . . .
O1W O 1.000000 0.000000 0.3112(3) 0.0235(12) Uani 1 2 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
Mo1 O1 2.418(4) . ?
Mo1 O2 1.927(4) . ?
Mo1 O3 1.886(4) . ?
Mo1 O5 1.909(4) . ?
Mo1 O6 1.905(4) 4_645 ?
Mo1 O8 1.654(4) . ?
Mo2 O1 2.406(4) . ?
Mo2 O2 1.954(4) . ?
Mo2 O4 1.979(4) . ?
Mo2 O5 1.851(4) 2_755 ?
Mo2 O7 1.883(4) 3_665 ?
Mo2 O9 1.667(4) . ?
Mo3 O1 2.407(4) . ?
Mo3 O3 1.983(4) . ?
Mo3 O4 1.913(4) . ?
Mo3 O6 1.848(4) . ?
Mo3 O7 1.886(4) . ?
Mo3 O10 1.673(4) . ?
V1 O1 2.418(4) . ?
V1 O2 1.927(4) . ?
V1 O3 1.886(4) . ?
V1 O5 1.909(4) . ?
V1 O6 1.905(4) 4_645 ?
V1 O8 1.654(4) . ?
V2 O1 2.406(4) . ?
V2 O2 1.954(4) . ?
V2 O4 1.979(4) . ?
V2 O5 1.851(4) 2_755 ?
V2 O7 1.883(4) 3_665 ?
V2 O9 1.667(4) . ?
V3 O1 2.407(4) . ?
V3 O3 1.983(4) . ?
V3 O4 1.913(4) . ?
V3 O6 1.848(4) . ?
V3 O7 1.886(4) . ?
V3 O10 1.673(4) . ?
P1 O1 1.537(4) 2_755 ?
P1 O1 1.537(4) . ?
P1 O1 1.537(4) 4_645 ?
P1 O1 1.537(4) 3_665 ?
Na1 Na1 3.154(6) 2_855 ?
Na1 O3 3.008(5) 3_665 ?
Na1 O6 2.986(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O1 73.12(15) . . ?
O3 Mo1 O1 74.20(15) . . ?
O3 Mo1 O2 88.69(17) . . ?
O3 Mo1 O5 158.22(18) . . ?
O3 Mo1 O6 90.05(18) . 4_645 ?
O5 Mo1 O1 84.24(16) . . ?
O5 Mo1 O2 87.94(18) . . ?
O6 Mo1 O1 85.26(16) 4_645 . ?
O6 Mo1 O2 157.84(18) 4_645 . ?
O6 Mo1 O5 85.08(18) 4_645 . ?
O8 Mo1 O1 169.6(2) . . ?
O8 Mo1 O2 99.3(2) . . ?
O8 Mo1 O3 98.9(2) . . ?
O8 Mo1 O5 102.8(2) . . ?
O8 Mo1 O6 102.7(2) . 4_645 ?
O2 Mo2 O1 72.96(14) . . ?
O2 Mo2 O4 84.88(17) . . ?
O4 Mo2 O1 72.20(16) . . ?
O5 Mo2 O1 85.14(16) 2_755 . ?
O5 Mo2 O2 88.77(18) 2_755 . ?
O5 Mo2 O4 157.34(19) 2_755 . ?
O5 Mo2 O7 89.16(18) 2_755 3_665 ?
O7 Mo2 O1 83.97(16) 3_665 . ?
O7 Mo2 O2 156.94(18) 3_665 . ?
O7 Mo2 O4 88.27(18) 3_665 . ?
O9 Mo2 O1 167.82(18) . . ?
O9 Mo2 O2 98.4(2) . . ?
O9 Mo2 O4 98.9(2) . . ?
O9 Mo2 O5 103.5(2) . 2_755 ?
O9 Mo2 O7 104.4(2) . 3_665 ?
O3 Mo3 O1 72.91(15) . . ?
O4 Mo3 O1 73.24(15) . . ?
O4 Mo3 O3 85.97(18) . . ?
O6 Mo3 O1 85.10(16) . . ?
O6 Mo3 O3 157.71(18) . . ?
O6 Mo3 O4 91.23(18) . . ?
O6 Mo3 O7 87.75(18) . . ?
O7 Mo3 O1 83.95(16) . . ?
O7 Mo3 O3 86.39(17) . . ?
O7 Mo3 O4 157.17(18) . . ?
O10 Mo3 O1 167.86(18) . . ?
O10 Mo3 O3 97.57(19) . . ?
O10 Mo3 O4 99.0(2) . . ?
O10 Mo3 O6 104.7(2) . . ?
O10 Mo3 O7 103.3(2) . . ?
O2 V1 O1 73.12(15) . . ?
O3 V1 O1 74.20(15) . . ?
O3 V1 O2 88.69(17) . . ?
O3 V1 O5 158.22(18) . . ?
O3 V1 O6 90.05(18) . 4_645 ?
O5 V1 O1 84.24(16) . . ?
O5 V1 O2 87.94(18) . . ?
O6 V1 O1 85.26(16) 4_645 . ?
O6 V1 O2 157.84(18) 4_645 . ?
O6 V1 O5 85.08(18) 4_645 . ?
O8 V1 O1 169.6(2) . . ?
O8 V1 O2 99.3(2) . . ?
O8 V1 O3 98.9(2) . . ?
O8 V1 O5 102.8(2) . . ?
O8 V1 O6 102.7(2) . 4_645 ?
O2 V2 O1 72.96(14) . . ?
O2 V2 O4 84.88(17) . . ?
O4 V2 O1 72.20(16) . . ?
O5 V2 O1 85.14(16) 2_755 . ?
O5 V2 O2 88.77(18) 2_755 . ?
O5 V2 O4 157.34(19) 2_755 . ?
O5 V2 O7 89.16(18) 2_755 3_665 ?
O7 V2 O1 83.97(16) 3_665 . ?
O7 V2 O2 156.94(18) 3_665 . ?
O7 V2 O4 88.27(18) 3_665 . ?
O9 V2 O1 167.82(18) . . ?
O9 V2 O2 98.4(2) . . ?
O9 V2 O4 98.9(2) . . ?
O9 V2 O5 103.5(2) . 2_755 ?
O9 V2 O7 104.4(2) . 3_665 ?
O3 V3 O1 72.91(15) . . ?
O4 V3 O1 73.24(15) . . ?
O4 V3 O3 85.97(18) . . ?
O6 V3 O1 85.10(16) . . ?
O6 V3 O3 157.71(18) . . ?
O6 V3 O4 91.23(18) . . ?
O6 V3 O7 87.75(18) . . ?
O7 V3 O1 83.95(16) . . ?
O7 V3 O3 86.39(17) . . ?
O7 V3 O4 157.17(18) . . ?
O10 V3 O1 167.86(18) . . ?
O10 V3 O3 97.57(19) . . ?
O10 V3 O4 99.0(2) . . ?
O10 V3 O6 104.7(2) . . ?
O10 V3 O7 103.3(2) . . ?
O1 P1 O1 109.15(14) 2_755 3_665 ?
O1 P1 O1 110.1(3) 2_755 . ?
O1 P1 O1 109.15(14) 4_645 . ?
O1 P1 O1 109.15(14) 4_645 2_755 ?
O1 P1 O1 110.1(3) 4_645 3_665 ?
O1 P1 O1 109.15(14) 3_665 . ?
O3 Na1 Na1 76.94(11) 3_665 2_855 ?
O6 Na1 Na1 130.08(13) . 2_855 ?
O6 Na1 O3 53.15(12) . 3_665 ?
Mo2 O1 Mo1 90.32(12) . . ?
Mo2 O1 Mo3 90.93(12) . . ?
Mo3 O1 Mo1 89.71(12) . . ?
V2 O1 V1 90.32(12) . . ?
V2 O1 V3 90.93(12) . . ?
V3 O1 V1 89.71(12) . . ?
P1 O1 Mo1 124.84(19) . . ?
P1 O1 Mo2 124.8(2) . . ?
P1 O1 Mo3 125.5(2) . . ?
P1 O1 V1 124.84(19) . . ?
P1 O1 V2 124.8(2) . . ?
P1 O1 V3 125.5(2) . . ?
Mo1 O2 Mo2 123.6(2) . . ?
V1 O2 V2 123.6(2) . . ?
Mo1 O3 Mo3 123.1(2) . . ?
Mo1 O3 Na1 102.28(17) . 4_645 ?
Mo3 O3 Na1 104.61(17) . 4_645 ?
V1 O3 V3 123.1(2) . . ?
Mo3 O4 Mo2 123.6(2) . . ?
V3 O4 V2 123.6(2) . . ?
Mo2 O5 Mo1 150.1(2) 2_755 . ?
Mo1 O6 Na1 102.55(17) 3_665 . ?
Mo3 O6 Mo1 151.4(2) . 3_665 ?
Mo3 O6 Na1 103.53(17) . . ?
V3 O6 Na1 103.53(17) . . ?
Mo2 O7 Mo3 147.6(2) 4_645 . ?

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 Mo1 O3 Mo3 -2.1(2) . . . . ?
O1 Mo1 O3 Na1 114.65(16) . . . 4_645 ?
O1 Mo3 O6 Mo1 51.6(5) . . . 3_665 ?
O1 Mo3 O6 Na1 -103.70(16) . . . . ?
O1 Mo3 O7 Mo2 -61.5(4) . . . 4_645 ?
O1 V1 O3 V3 -2.1(2) . . . . ?
O1 V1 O3 Na1 114.65(16) . . . 4_645 ?
O1 V3 O6 Na1 -103.70(16) . . . . ?
O1 P1 O1 Mo1 -60.05(18) 2_755 . . . ?
O1 P1 O1 Mo1 -179.9(3) 3_665 . . . ?
O1 P1 O1 Mo1 59.75(10) 4_645 . . . ?
O1 P1 O1 Mo2 59.38(18) 2_755 . . . ?
O1 P1 O1 Mo2 179.2(3) 4_645 . . . ?
O1 P1 O1 Mo2 -60.43(10) 3_665 . . . ?
O1 P1 O1 Mo3 60.9(3) 3_665 . . . ?
O1 P1 O1 Mo3 -59.5(3) 4_645 . . . ?
O1 P1 O1 Mo3 -179.3(3) 2_755 . . . ?
O1 P1 O1 V1 59.75(10) 4_645 . . . ?
O1 P1 O1 V1 -60.05(18) 2_755 . . . ?
O1 P1 O1 V1 -179.9(3) 3_665 . . . ?
O1 P1 O1 V2 179.2(3) 4_645 . . . ?
O1 P1 O1 V2 -60.43(10) 3_665 . . . ?
O1 P1 O1 V2 59.38(18) 2_755 . . . ?
O1 P1 O1 V3 -59.5(3) 4_645 . . . ?
O1 P1 O1 V3 60.9(3) 3_665 . . . ?
O1 P1 O1 V3 -179.3(3) 2_755 . . . ?
O2 Mo1 O3 Mo3 70.7(3) . . . . ?
O2 Mo1 O3 Na1 -172.53(17) . . . 4_645 ?
O2 V1 O3 V3 70.7(3) . . . . ?
O2 V1 O3 Na1 -172.53(17) . . . 4_645 ?
O3 Mo3 O6 Mo1 42.3(8) . . . 3_665 ?
O3 Mo3 O6 Na1 -113.0(4) . . . . ?
O3 Mo3 O7 Mo2 -134.7(5) . . . 4_645 ?
O3 V3 O6 Na1 -113.0(4) . . . . ?
O4 Mo3 O6 Mo1 124.6(5) . . . 3_665 ?
O4 Mo3 O6 Na1 -30.6(2) . . . . ?
O4 Mo3 O7 Mo2 -64.0(7) . . . 4_645 ?
O4 V3 O6 Na1 -30.6(2) . . . . ?
O5 Mo1 O3 Mo3 -10.4(6) . . . . ?
O5 Mo1 O3 Na1 106.4(5) . . . 4_645 ?
O5 V1 O3 V3 -10.4(6) . . . . ?
O5 V1 O3 Na1 106.4(5) . . . 4_645 ?
O6 Mo1 O3 Mo3 -87.2(3) 4_645 . . . ?
O6 Mo1 O3 Na1 29.60(18) 4_645 . . 4_645 ?
O6 Mo3 O7 Mo2 23.8(5) . . . 4_645 ?
O6 V1 O3 V3 -87.2(3) 4_645 . . . ?
O6 V1 O3 Na1 29.60(18) 4_645 . . 4_645 ?
O7 Mo3 O6 Mo1 -32.5(5) . . . 3_665 ?
O7 Mo3 O6 Na1 172.18(19) . . . . ?
O7 V3 O6 Na1 172.18(19) . . . . ?
O8 Mo1 O3 Mo3 169.9(3) . . . . ?
O8 Mo1 O3 Na1 -73.3(2) . . . 4_645 ?
O8 V1 O3 V3 169.9(3) . . . . ?
O8 V1 O3 Na1 -73.3(2) . . . 4_645 ?
O10 Mo3 O6 Mo1 -135.7(5) . . . 3_665 ?
O10 Mo3 O6 Na1 69.0(2) . . . . ?
O10 Mo3 O7 Mo2 128.4(5) . . . 4_645 ?
O10 V3 O6 Na1 69.0(2) . . . . ?

_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 -0.906 -0.497 -0.934 957.8 460.4 '48 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'Dual Thicknes MiTeGen'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.48(6)
2 0.52(6)

# start Validation Reply Form
_vrf_PLAT094_jcr101_0m_v1_sq     
;
PROBLEM: Ratio of Maximum / Minimum Residual Density .... 4.46 Report
RESPONSE: The excess residual density comes from misordered water molecules. 
A SQUEEZE has already been performed for this purpose.
;
_vrf_PLAT306_jcr101_0m_v1_sq     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: The isolated oxygen atom belongs to a crystal water
molecule. However, the protons cannot be meaningfully simulated due to strong
disorder.
;
_vrf_PLAT971_jcr101_0m_v1_sq     
;
PROBLEM: Check Calcd Resid. Dens. 2.58Ang From Na1 3.27 eA-3
RESPONSE: Residual density is minimally occupied water.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_mp-katsyn-005_v1
_database_code_depnum_ccdc_archive 'CCDC 2216947'
loop_
_audit_author_name
_audit_author_address
'J.-C. Raabe'
;Hamburg University
Germany
;
_audit_update_record             
;
2022-11-02 deposited with the CCDC.	2023-07-17 downloaded from the CCDC.
;
_audit_creation_date             2022-11-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Jan-Christian.Raabe@chemie.uni-hamburg.de
Tobias.Esser@chemie.uni-hamburg.de
Jakob.Albert@chemie.uni-hamburg.de
Maximilian.Poller@chemie.uni-hamburg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'K6.913 Na1.087 Nb6 O33'
_chemical_formula_sum            'K6.91 Na1.09 Nb6 O33'
_chemical_formula_weight         1380.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'K28 Nb24 O136 '
_chemical_oxdiff_usercomment     'Poller/Albert, 23.03.2021, Mo, 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Nb Nb -2.0727 0.6215 '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'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.63957(11)
_cell_length_b                   10.69819(9)
_cell_length_c                   24.26416(18)
_cell_angle_alpha                90
_cell_angle_beta                 92.1646(7)
_cell_angle_gamma                90
_cell_volume                     3278.67(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    109552
_cell_measurement_temperature    99.96(13)
_cell_measurement_theta_max      32.7670
_cell_measurement_theta_min      3.1530
_shelx_estimated_absorpt_T_max   0.659
_shelx_estimated_absorpt_T_min   0.463
_exptl_absorpt_coefficient_mu    3.030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
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    2.797
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2613
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'Slow evaporation of water'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            204566
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.916
_diffrn_reflns_theta_min         2.974
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.96(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2063
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  15.00   1.00   30.00    --  -18.04 -77.00-180.00   57
  2  ω    -95.00 -44.00   1.00   30.00    --  -18.04 156.00 152.16   51
  3  ω    -42.00  15.00   1.00   30.00    --  -18.04 -77.00   0.00   57
  4  ω     21.00  95.00   1.00   30.00    --   18.98-154.00-156.74   74
  5  ω    -61.00  26.00   1.00   30.00    --   18.98 -19.00-150.00   87
  6  ω    -22.00  99.00   1.00   30.00    --   18.98  19.00-150.00  121
  7  ω     -6.00  93.00   1.00   30.00    --   18.98  38.00   0.00   99
  8  ω    -61.00  26.00   1.00   30.00    --   18.98 -19.00  30.00   87
  9  ω    -61.00  26.00   1.00   30.00    --   18.98 -19.00-180.00   87
 10  ω      2.00  73.00   1.00   30.00    --   18.98-121.00  18.07   71
 11  ω    -77.00 -30.00   1.00   30.00    --  -18.04 129.00   5.10   47
 12  ω    -90.00  10.00   1.00   30.00    --  -18.04 -57.00-150.00  100
 13  ω    -42.00  15.00   1.00   30.00    --  -18.04 -77.00  90.00   57
 14  ω    -90.00  10.00   1.00   30.00    --  -18.04 -57.00  30.00  100
 15  ω     14.00  86.00   1.00   30.00    --   18.98-142.00  92.53   72
 16  ω    -69.00 107.00   1.00   30.00    --   18.98   0.00-180.00  176
 17  ω      2.00  73.00   1.00   30.00    --   18.98-121.00 -39.93   71
 18  ω    -69.00 107.00   1.00   30.00    --   18.98   0.00-150.00  176
 19  ω    -69.00 107.00   1.00   30.00    --   18.98   0.00 -90.00  176
 20  ω    -69.00 -15.00   1.00   30.00    --   18.98   0.00 -60.00   54
 21  ω    -69.00 107.00   1.00   30.00    --   18.98   0.00-120.00  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      -0.0269363000
_diffrn_orient_matrix_UB_12      0.0307396000
_diffrn_orient_matrix_UB_13      0.0212594000
_diffrn_orient_matrix_UB_21      0.0261260000
_diffrn_orient_matrix_UB_22      -0.0388504000
_diffrn_orient_matrix_UB_23      0.0199065000
_diffrn_orient_matrix_UB_31      0.0417825000
_diffrn_orient_matrix_UB_32      0.0440615000
_diffrn_orient_matrix_UB_33      0.0027318000
_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                11564
_reflns_number_total             11834
_reflns_odcompleteness_completeness 99.87
_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 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.487
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         11834
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0258
_refine_ls_restrained_S_all      1.252
_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)+(0.0217P)²+9.0695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0673
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{K1, Na1}
2. Uiso/Uaniso restraints and constraints
Uanis(K1) = Uanis(Na1)
3. Others
 Sof(Na1)=1-FVAR(1)
 Sof(K1)=FVAR(1)
;
_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
Nb1 Nb 0.20484(2) 0.24218(2) 0.28948(2) 0.00388(4) Uani 1 1 d . . . . .
Nb2 Nb 0.38241(2) 0.09798(2) 0.37156(2) 0.00401(4) Uani 1 1 d . . . . .
Nb3 Nb 0.29393(2) 0.25602(2) 0.47960(2) 0.00397(4) Uani 1 1 d . . . . .
Nb4 Nb 0.11725(2) 0.40217(2) 0.39522(2) 0.00411(4) Uani 1 1 d . . . . .
Nb5 Nb 0.37371(2) 0.41147(2) 0.36800(2) 0.00391(4) Uani 1 1 d . . . . .
Nb6 Nb 0.12467(2) 0.08990(2) 0.39887(2) 0.00417(4) Uani 1 1 d . . . . .
K1 K 0.05674(4) -0.08820(4) 0.26194(2) 0.00923(18) Uani 0.913(8) 1 d . . P A 1
K3 K 0.32825(4) 0.49822(4) 0.60067(2) 0.00900(8) Uani 1 1 d . . . . .
K4 K 0.19397(4) 0.59363(4) 0.26593(2) 0.00984(8) Uani 1 1 d . . . . .
K5 K 0.49548(4) 0.24908(4) 0.24536(2) 0.00936(8) Uani 1 1 d . . . . .
K6 K 0.69163(3) -0.01219(4) 0.39674(2) 0.00892(8) Uani 1 1 d . . . . .
K7 K 0.44094(4) -0.24255(4) 0.40986(2) 0.01105(8) Uani 1 1 d . . . . .
K8 K -0.00268(4) 0.25084(4) 0.52414(2) 0.00923(8) Uani 1 1 d . . . . .
Na1 Na 0.05674(4) -0.08820(4) 0.26194(2) 0.00923(18) Uani 0.087(8) 1 d . . P A
2
Na2 Na 0.26716(7) 0.75236(8) 0.52171(4) 0.00762(16) Uani 1 1 d . . . . .
O1 O 0.25045(11) 0.25061(13) 0.38317(6) 0.0051(3) Uani 1 1 d . . . . .
O1W O 0.03411(14) -0.30033(18) 0.32044(8) 0.0167(3) Uani 1 1 d . . . . .
O2 O 0.32485(12) 0.12154(14) 0.29451(6) 0.0064(2) Uani 1 1 d . . . . .
O2W O 0.15561(13) 0.00873(16) 0.16380(7) 0.0134(3) Uani 1 1 d . . . . .
O3 O 0.39485(12) 0.12873(14) 0.45259(6) 0.0060(2) Uani 1 1 d . . . . .
O3W O 0.21485(14) 0.74110(15) 0.42863(7) 0.0115(3) Uani 1 1 d . . . . .
O4 O 0.17655(12) 0.37875(14) 0.47189(6) 0.0063(2) Uani 1 1 d . . . . .
O4W O 0.40607(13) 0.60966(15) 0.50472(7) 0.0095(3) Uani 1 1 d . . . . .
O5 O 0.10709(12) 0.37261(14) 0.31412(6) 0.0062(2) Uani 1 1 d . . . . .
O5W O 0.15069(13) 0.58289(15) 0.53397(7) 0.0094(3) Uani 1 1 d . . . . .
O6 O 0.31781(12) 0.37627(14) 0.29182(6) 0.0060(2) Uani 1 1 d . . . . .
O6W O 0.39730(13) 0.90297(15) 0.50643(7) 0.0099(3) Uani 1 1 d . . . . .
O7 O 0.46181(12) 0.25663(13) 0.36065(6) 0.0060(3) Uani 1 1 d . . . . .
O7W O 0.14548(12) 0.91712(15) 0.53485(7) 0.0091(3) Uani 1 1 d . . . . .
O8 O 0.38915(12) 0.38656(14) 0.45008(6) 0.0061(2) Uani 1 1 d . . . . .
O8W O 0.33046(13) 0.75567(14) 0.61421(7) 0.0094(3) Uani 1 1 d . . . . .
O9 O 0.24307(11) 0.50829(14) 0.38031(6) 0.0058(2) Uani 1 1 d . . . . .
O9W O 0.27192(15) 0.82324(16) 0.29787(8) 0.0156(3) Uani 1 1 d . . . . .
O10 O 0.11241(12) 0.11460(14) 0.31766(6) 0.0066(2) Uani 1 1 d . . . . .
O10W O 0.14218(14) 0.75298(16) 0.17701(8) 0.0138(3) Uani 1 1 d . . . . .
O11 O 0.25579(11) -0.00875(14) 0.38488(6) 0.0061(2) Uani 1 1 d . . . . .
O11W O 0.13172(13) 0.46052(16) 0.16963(7) 0.0119(3) Uani 1 1 d . . . . .
O12 O 0.18273(12) 0.12438(14) 0.47476(6) 0.0061(2) Uani 1 1 d . . . . .
O12W O 0.38604(13) 0.54809(15) 0.21888(7) 0.0104(3) Uani 1 1 d . . . . .
O13 O 0.03875(12) 0.24501(13) 0.40505(7) 0.0066(3) Uani 1 1 d . . . . .
O14 O 0.17169(12) 0.23332(15) 0.21567(6) 0.0078(3) Uani 1 1 d . . . . .
O15 O 0.48195(12) -0.01805(14) 0.36266(6) 0.0077(3) Uani 1 1 d . . . . .
O16 O 0.33019(13) 0.25999(14) 0.55170(7) 0.0085(3) Uani 1 1 d . . . . .
O17 O 0.01704(12) 0.51998(15) 0.40485(6) 0.0076(3) Uani 1 1 d . . . . .
O18 O 0.46801(12) 0.53249(14) 0.35670(6) 0.0078(3) Uani 1 1 d . . . . .
O19 O 0.02734(12) -0.02773(15) 0.41039(6) 0.0083(3) Uani 1 1 d . . . . .
O13W O 0.35511(13) 0.24797(15) 0.65987(7) 0.0107(3) Uani 1 1 d . . . . .
O14W O 0.38745(13) -0.04242(16) 0.21885(7) 0.0116(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
Nb1 O1 2.3258(15) . ?
Nb1 O2 1.9918(15) . ?
Nb1 O5 1.9716(15) . ?
Nb1 O6 2.0234(15) . ?
Nb1 O10 1.9380(15) . ?
Nb1 O14 1.8263(16) . ?
Nb2 O1 2.3585(14) . ?
Nb2 O2 1.9962(15) . ?
Nb2 O3 1.9938(15) . ?
Nb2 O7 1.9946(15) . ?
Nb2 O11 2.0021(15) . ?
Nb2 O15 1.7864(15) . ?
Nb3 O1 2.3839(15) . ?
Nb3 O3 1.9936(15) . ?
Nb3 O4 1.9847(15) . ?
Nb3 O8 1.9943(15) . ?
Nb3 O12 1.9900(15) . ?
Nb3 O16 1.7923(16) . ?
Nb4 O1 2.3635(14) . ?
Nb4 O4 1.9951(15) . ?
Nb4 O5 1.9923(15) . ?
Nb4 O9 1.9980(15) . ?
Nb4 O13 1.9714(15) . ?
Nb4 O17 1.8083(15) . ?
Nb5 O1 2.3596(14) . ?
Nb5 O6 1.9896(15) . ?
Nb5 O7 2.0077(15) . ?
Nb5 O8 2.0115(15) . ?
Nb5 O9 1.9814(15) . ?
Nb5 O18 1.7878(15) . ?
Nb6 O1 2.3821(14) . ?
Nb6 O10 1.9884(15) . ?
Nb6 O11 2.0046(15) . ?
Nb6 O12 1.9908(15) . ?
Nb6 O13 1.9919(15) . ?
Nb6 O19 1.7892(15) . ?
K1 O1W 2.6976(19) . ?
K1 O2W 2.9211(19) . ?
K1 O5 2.7534(15) 2_545 ?
K1 O9W 2.979(2) 1_545 ?
K1 O10 2.6378(16) . ?
K1 O10W 2.9099(19) 1_545 ?
K3 O2W 2.7141(18) 4_566 ?
K3 O4W 2.8251(17) . ?
K3 O5W 2.8639(17) . ?
K3 O8W 2.7738(16) . ?
K3 O16 2.8124(16) . ?
K3 O18 2.7584(16) 3_666 ?
K4 O1W 2.7057(19) 1_565 ?
K4 O6 2.8597(16) . ?
K4 O9W 2.7474(18) . ?
K4 O10W 2.8076(18) . ?
K4 O11W 2.8228(18) . ?
K4 O12W 2.7648(17) . ?
K5 O2 2.8513(16) . ?
K5 O6 2.8908(16) . ?
K5 O7 2.8465(16) . ?
K5 O12W 2.7424(17) 2_645 ?
K5 O13W 2.6784(17) 4_565 ?
K5 O14W 2.7968(18) 2_655 ?
K6 O6W 2.8894(17) 3_666 ?
K6 O7W 2.7876(17) 3_666 ?
K6 O8W 2.7703(16) 3_666 ?
K6 O11W 2.8169(18) 2_645 ?
K6 O15 2.7470(16) . ?
K6 O13W 2.9217(17) 3_656 ?
K7 O3W 2.9159(19) 1_545 ?
K7 O4W 2.8407(17) 1_545 ?
K7 O6W 2.8839(18) 1_545 ?
K7 O15 2.7191(16) . ?
K7 O16 3.0116(17) 3_656 ?
K7 O18 2.7579(16) 1_545 ?
K8 O3W 2.9572(19) 3_566 ?
K8 O4 2.9713(16) . ?
K8 O5W 2.9073(17) 3_566 ?
K8 O7W 2.8879(17) 3_566 ?
K8 O13 2.9567(17) . ?
K8 O19 2.8905(16) 3_556 ?
Na1 O1W 2.6976(19) . ?
Na1 O2W 2.9211(19) . ?
Na1 O5 2.7534(15) 2_545 ?
Na1 O9W 2.979(2) 1_545 ?
Na1 O10 2.6378(16) . ?
Na1 O10W 2.9099(19) 1_545 ?
Na1 O11W 3.0003(18) 2_545 ?
Na2 O3W 2.332(2) . ?
Na2 O4W 2.3745(18) . ?
Na2 O5W 2.3613(18) . ?
Na2 O6W 2.3421(18) . ?
Na2 O7W 2.3687(18) . ?
Na2 O8W 2.3544(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Nb1 O1 78.76(6) . . ?
O2 Nb1 O6 85.57(6) . . ?
O5 Nb1 O1 79.11(6) . . ?
O5 Nb1 O2 157.59(6) . . ?
O5 Nb1 O6 86.52(6) . . ?
O6 Nb1 O1 78.25(5) . . ?
O10 Nb1 O1 79.22(6) . . ?
O10 Nb1 O2 89.42(6) . . ?
O10 Nb1 O5 89.91(7) . . ?
O10 Nb1 O6 157.46(6) . . ?
O14 Nb1 O1 178.68(6) . . ?
O14 Nb1 O2 99.93(7) . . ?
O14 Nb1 O5 102.18(7) . . ?
O14 Nb1 O6 101.53(7) . . ?
O14 Nb1 O10 100.98(7) . . ?
O2 Nb2 O1 77.88(6) . . ?
O2 Nb2 O11 87.59(6) . . ?
O3 Nb2 O1 78.34(6) . . ?
O3 Nb2 O2 156.21(6) . . ?
O3 Nb2 O7 88.23(6) . . ?
O3 Nb2 O11 88.20(6) . . ?
O7 Nb2 O1 77.78(6) . . ?
O7 Nb2 O2 86.31(6) . . ?
O7 Nb2 O11 156.35(6) . . ?
O11 Nb2 O1 78.60(5) . . ?
O15 Nb2 O1 179.77(7) . . ?
O15 Nb2 O2 102.00(7) . . ?
O15 Nb2 O3 101.78(7) . . ?
O15 Nb2 O7 102.42(7) . . ?
O15 Nb2 O11 101.20(7) . . ?
O3 Nb3 O1 77.73(5) . . ?
O3 Nb3 O8 87.59(6) . . ?
O4 Nb3 O1 77.28(5) . . ?
O4 Nb3 O3 154.99(6) . . ?
O4 Nb3 O8 87.82(6) . . ?
O4 Nb3 O12 86.50(6) . . ?
O8 Nb3 O1 77.55(5) . . ?
O12 Nb3 O1 77.81(5) . . ?
O12 Nb3 O3 87.50(6) . . ?
O12 Nb3 O8 155.35(6) . . ?
O16 Nb3 O1 178.51(6) . . ?
O16 Nb3 O3 101.18(7) . . ?
O16 Nb3 O4 103.83(7) . . ?
O16 Nb3 O8 101.45(7) . . ?
O16 Nb3 O12 103.20(7) . . ?
O4 Nb4 O1 77.58(6) . . ?
O4 Nb4 O9 88.08(6) . . ?
O5 Nb4 O1 77.79(6) . . ?
O5 Nb4 O4 155.37(6) . . ?
O5 Nb4 O9 86.19(6) . . ?
O9 Nb4 O1 77.99(5) . . ?
O13 Nb4 O1 78.11(6) . . ?
O13 Nb4 O4 87.32(6) . . ?
O13 Nb4 O5 88.29(6) . . ?
O13 Nb4 O9 156.09(6) . . ?
O17 Nb4 O1 179.03(6) . . ?
O17 Nb4 O4 101.97(7) . . ?
O17 Nb4 O5 102.64(7) . . ?
O17 Nb4 O9 101.16(7) . . ?
O17 Nb4 O13 102.74(7) . . ?
O6 Nb5 O1 78.08(6) . . ?
O6 Nb5 O7 86.56(6) . . ?
O6 Nb5 O8 155.85(6) . . ?
O7 Nb5 O1 77.51(6) . . ?
O7 Nb5 O8 86.86(6) . . ?
O8 Nb5 O1 77.81(6) . . ?
O9 Nb5 O1 78.39(6) . . ?
O9 Nb5 O6 88.30(6) . . ?
O9 Nb5 O7 155.90(6) . . ?
O9 Nb5 O8 88.29(6) . . ?
O18 Nb5 O1 179.51(7) . . ?
O18 Nb5 O6 102.12(7) . . ?
O18 Nb5 O7 102.04(7) . . ?
O18 Nb5 O8 101.97(7) . . ?
O18 Nb5 O9 102.05(7) . . ?
O10 Nb6 O1 76.88(6) . . ?
O10 Nb6 O11 86.34(6) . . ?
O10 Nb6 O12 154.72(6) . . ?
O10 Nb6 O13 86.65(6) . . ?
O11 Nb6 O1 77.99(5) . . ?
O12 Nb6 O1 77.84(6) . . ?
O12 Nb6 O11 88.62(6) . . ?
O12 Nb6 O13 87.65(6) . . ?
O13 Nb6 O1 77.28(6) . . ?
O13 Nb6 O11 155.22(6) . . ?
O19 Nb6 O1 178.43(6) . . ?
O19 Nb6 O10 102.70(7) . . ?
O19 Nb6 O11 103.53(7) . . ?
O19 Nb6 O12 102.56(7) . . ?
O19 Nb6 O13 101.19(7) . . ?
O1W K1 O2W 141.69(6) . . ?
O1W K1 O5 97.62(5) . 2_545 ?
O1W K1 O9W 72.08(5) . 1_545 ?
O1W K1 O10W 86.04(6) . 1_545 ?
O2W K1 O9W 86.42(5) . 1_545 ?
O5 K1 O2W 80.89(5) 2_545 . ?
O5 K1 O9W 143.41(5) 2_545 1_545 ?
O5 K1 O10W 74.11(5) 2_545 1_545 ?
O10 K1 O1W 116.99(6) . . ?
O10 K1 O2W 90.68(5) . . ?
O10 K1 O5 130.40(5) . 2_545 ?
O10 K1 O9W 83.61(5) . 1_545 ?
O10 K1 O10W 138.09(5) . 1_545 ?
O10W K1 O2W 56.52(5) 1_545 . ?
O10W K1 O9W 70.27(5) 1_545 1_545 ?
O2W K3 O4W 142.10(5) 4_566 . ?
O2W K3 O5W 72.42(5) 4_566 . ?
O2W K3 O8W 88.00(5) 4_566 . ?
O2W K3 O16 103.51(5) 4_566 . ?
O2W K3 O18 122.97(5) 4_566 3_666 ?
O4W K3 O5W 71.98(5) . . ?
O8W K3 O4W 71.12(5) . . ?
O8W K3 O5W 75.94(5) . . ?
O8W K3 O16 161.74(5) . . ?
O16 K3 O4W 91.46(5) . . ?
O16 K3 O5W 93.85(5) . . ?
O18 K3 O4W 90.58(5) 3_666 . ?
O18 K3 O5W 161.84(5) 3_666 . ?
O18 K3 O8W 93.94(5) 3_666 . ?
O18 K3 O16 91.58(5) 3_666 . ?
O1W K4 O6 130.26(5) 1_565 . ?
O1W K4 O9W 75.74(6) 1_565 . ?
O1W K4 O10W 87.96(5) 1_565 . ?
O1W K4 O11W 115.23(6) 1_565 . ?
O1W K4 O12W 163.60(6) 1_565 . ?
O9W K4 O6 118.52(5) . . ?
O9W K4 O10W 75.20(6) . . ?
O9W K4 O11W 140.39(5) . . ?
O9W K4 O12W 87.87(5) . . ?
O10W K4 O6 140.57(5) . . ?
O10W K4 O11W 67.70(5) . . ?
O11W K4 O6 84.54(5) . . ?
O12W K4 O6 57.69(5) . . ?
O12W K4 O10W 88.42(5) . . ?
O12W K4 O11W 77.93(5) . . ?
O2 K5 O6 56.71(5) . . ?
O7 K5 O2 57.25(4) . . ?
O7 K5 O6 57.06(4) . . ?
O12W K5 O2 84.55(5) 2_645 . ?
O12W K5 O6 131.96(5) 2_645 . ?
O12W K5 O7 79.13(5) 2_645 . ?
O12W K5 O14W 104.53(5) 2_645 2_655 ?
O13W K5 O2 80.81(5) 4_565 . ?
O13W K5 O6 78.16(5) 4_565 . ?
O13W K5 O7 129.91(5) 4_565 . ?
O13W K5 O12W 126.31(5) 4_565 2_645 ?
O13W K5 O14W 123.94(5) 4_565 2_655 ?
O14W K5 O2 130.65(5) 2_655 . ?
O14W K5 O6 85.02(5) 2_655 . ?
O14W K5 O7 76.65(5) 2_655 . ?
O6W K6 O13W 130.80(5) 3_666 3_656 ?
O7W K6 O6W 70.70(5) 3_666 3_666 ?
O7W K6 O11W 78.15(5) 3_666 2_645 ?
O7W K6 O13W 136.60(5) 3_666 3_656 ?
O8W K6 O6W 68.68(5) 3_666 3_666 ?
O8W K6 O7W 76.42(5) 3_666 3_666 ?
O8W K6 O11W 97.30(5) 3_666 2_645 ?
O8W K6 O13W 142.40(5) 3_666 3_656 ?
O11W K6 O6W 147.98(5) 2_645 3_666 ?
O11W K6 O13W 78.02(5) 2_645 3_656 ?
O15 K6 O6W 81.57(5) . 3_666 ?
O15 K6 O7W 150.47(5) . 3_666 ?
O15 K6 O8W 84.33(5) . 3_666 ?
O15 K6 O11W 127.02(5) . 2_645 ?
O15 K6 O13W 70.31(5) . 3_656 ?
O3W K7 O16 152.06(5) 1_545 3_656 ?
O4W K7 O3W 69.94(5) 1_545 1_545 ?
O4W K7 O6W 66.53(5) 1_545 1_545 ?
O4W K7 O16 83.75(5) 1_545 3_656 ?
O6W K7 O3W 71.75(5) 1_545 1_545 ?
O6W K7 O16 89.58(5) 1_545 3_656 ?
O15 K7 O3W 108.80(5) . 1_545 ?
O15 K7 O4W 150.55(5) . 1_545 ?
O15 K7 O6W 84.88(5) . 1_545 ?
O15 K7 O16 89.37(5) . 3_656 ?
O15 K7 O18 123.01(5) . 1_545 ?
O18 K7 O3W 99.23(5) 1_545 1_545 ?
O18 K7 O4W 85.36(5) 1_545 1_545 ?
O18 K7 O6W 151.89(5) 1_545 1_545 ?
O18 K7 O16 87.49(5) 1_545 3_656 ?
O3W K8 O4 150.35(5) 3_566 . ?
O5W K8 O3W 66.03(5) 3_566 3_566 ?
O5W K8 O4 89.91(4) 3_566 . ?
O5W K8 O13 70.94(4) 3_566 . ?
O7W K8 O3W 69.59(5) 3_566 3_566 ?
O7W K8 O4 123.19(5) 3_566 . ?
O7W K8 O5W 76.21(5) 3_566 3_566 ?
O7W K8 O13 68.47(4) 3_566 . ?
O7W K8 O19 71.35(5) 3_566 3_556 ?
O13 K8 O3W 125.17(5) . 3_566 ?
O13 K8 O4 55.02(4) . . ?
O19 K8 O3W 72.11(5) 3_556 3_566 ?
O19 K8 O4 135.61(5) 3_556 . ?
O19 K8 O5W 133.70(5) 3_556 3_566 ?
O19 K8 O13 123.13(5) 3_556 . ?
K4 Na1 K4 147.655(16) 2_545 1_545 ?
O1W Na1 K4 115.13(4) . 2_545 ?
O1W Na1 K4 45.10(4) . 1_545 ?
O1W Na1 O2W 141.69(6) . . ?
O1W Na1 O5 97.62(5) . 2_545 ?
O1W Na1 O9W 72.08(5) . 1_545 ?
O1W Na1 O10W 86.04(6) . 1_545 ?
O1W Na1 O11W 75.69(5) . 2_545 ?
O2W Na1 K4 97.42(4) . 1_545 ?
O2W Na1 K4 93.06(4) . 2_545 ?
O2W Na1 O9W 86.42(5) . 1_545 ?
O2W Na1 O11W 139.69(5) . 2_545 ?
O5 Na1 K4 102.16(3) 2_545 1_545 ?
O5 Na1 K4 49.49(3) 2_545 2_545 ?
O5 Na1 O2W 80.89(5) 2_545 . ?
O5 Na1 O9W 143.41(5) 2_545 1_545 ?
O5 Na1 O10W 74.11(5) 2_545 1_545 ?
O5 Na1 O11W 78.74(5) 2_545 2_545 ?
O9W Na1 K4 166.31(4) 1_545 2_545 ?
O9W Na1 K4 45.62(3) 1_545 1_545 ?
O9W Na1 O11W 128.93(5) 1_545 2_545 ?
O10 Na1 K4 127.43(4) . 1_545 ?
O10 Na1 K4 82.72(4) . 2_545 ?
O10 Na1 O1W 116.99(6) . . ?
O10 Na1 O2W 90.68(5) . . ?
O10 Na1 O5 130.40(5) . 2_545 ?
O10 Na1 O9W 83.61(5) . 1_545 ?
O10 Na1 O10W 138.09(5) . 1_545 ?
O10 Na1 O11W 77.02(5) . 2_545 ?
O10W Na1 K4 120.52(4) 1_545 2_545 ?
O10W Na1 K4 46.95(4) 1_545 1_545 ?
O10W Na1 O2W 56.52(5) 1_545 . ?
O10W Na1 O9W 70.27(5) 1_545 1_545 ?
O10W Na1 O11W 144.78(5) 1_545 2_545 ?
O11W Na1 K4 47.77(3) 2_545 2_545 ?
O11W Na1 K4 120.67(4) 2_545 1_545 ?
K3 Na2 K6 107.22(3) . 3_666 ?
K3 Na2 K7 107.99(3) . 1_565 ?
K3 Na2 K8 111.54(3) . 3_566 ?
K6 Na2 K7 110.01(3) 3_666 1_565 ?
K6 Na2 K8 108.32(3) 3_666 3_566 ?
K8 Na2 K7 111.68(3) 3_566 1_565 ?
O3W Na2 K3 123.69(5) . . ?
O3W Na2 K6 129.04(5) . 3_666 ?
O3W Na2 K7 54.72(5) . 1_565 ?
O3W Na2 K8 57.09(5) . 3_566 ?
O3W Na2 O4W 89.03(7) . . ?
O3W Na2 O5W 85.81(6) . . ?
O3W Na2 O6W 93.29(7) . . ?
O3W Na2 O7W 90.40(6) . . ?
O3W Na2 O8W 176.03(7) . . ?
O4W Na2 K3 55.23(4) . . ?
O4W Na2 K6 121.50(5) . 3_666 ?
O4W Na2 K7 52.78(4) . 1_565 ?
O4W Na2 K8 130.19(5) . 3_566 ?
O5W Na2 K3 56.23(4) . . ?
O5W Na2 K6 129.02(5) . 3_666 ?
O5W Na2 K7 120.92(5) . 1_565 ?
O5W Na2 K8 55.76(4) . 3_566 ?
O5W Na2 O4W 89.82(6) . . ?
O5W Na2 O7W 98.24(7) . . ?
O6W Na2 K3 119.58(5) . . ?
O6W Na2 K6 56.17(5) . 3_666 ?
O6W Na2 K7 53.91(5) . 1_565 ?
O6W Na2 K8 128.87(5) . 3_566 ?
O6W Na2 O4W 83.48(7) . . ?
O6W Na2 O5W 173.25(7) . . ?
O6W Na2 O7W 88.45(6) . . ?
O6W Na2 O8W 85.71(6) . . ?
O7W Na2 K3 130.87(5) . . ?
O7W Na2 K6 53.58(4) . 3_666 ?
O7W Na2 K7 120.95(5) . 1_565 ?
O7W Na2 K8 55.26(4) . 3_566 ?
O7W Na2 O4W 171.86(7) . . ?
O8W Na2 K3 54.04(4) . . ?
O8W Na2 K6 53.20(4) . 3_666 ?
O8W Na2 K7 122.00(5) . 1_565 ?
O8W Na2 K8 126.31(5) . 3_566 ?
O8W Na2 O4W 87.03(6) . . ?
O8W Na2 O5W 94.73(6) . . ?
O8W Na2 O7W 93.41(6) . . ?
Nb1 O1 Nb2 90.39(5) . . ?
Nb1 O1 Nb3 178.68(7) . . ?
Nb1 O1 Nb4 89.78(5) . . ?
Nb1 O1 Nb5 90.95(5) . . ?
Nb1 O1 Nb6 89.20(5) . . ?
Nb2 O1 Nb3 89.78(5) . . ?
Nb2 O1 Nb4 179.47(8) . . ?
Nb2 O1 Nb5 90.70(5) . . ?
Nb2 O1 Nb6 89.92(5) . . ?
Nb4 O1 Nb3 90.04(5) . . ?
Nb4 O1 Nb6 89.57(5) . . ?
Nb5 O1 Nb3 90.36(5) . . ?
Nb5 O1 Nb4 89.80(5) . . ?
Nb5 O1 Nb6 179.35(7) . . ?
Nb6 O1 Nb3 89.49(5) . . ?
K1 O1W K4 89.98(6) . 1_545 ?
Nb1 O2 Nb2 112.89(7) . . ?
Nb1 O2 K5 104.51(6) . . ?
Nb2 O2 K5 101.39(6) . . ?
K3 O2W K1 145.92(7) 4_565 . ?
K3 O2W Na1 145.92(7) 4_565 . ?
Nb3 O3 Nb2 114.16(7) . . ?
K7 O3W K8 165.30(7) 1_565 3_566 ?
Na2 O3W K7 84.52(6) . 1_565 ?
Na2 O3W K8 81.45(6) . 3_566 ?
Nb3 O4 Nb4 115.09(7) . . ?
Nb3 O4 K8 103.55(6) . . ?
Nb4 O4 K8 100.95(6) . . ?
K3 O4W K7 166.44(6) . 1_565 ?
Na2 O4W K3 81.11(5) . . ?
Na2 O4W K7 85.48(5) . 1_565 ?
Nb1 O5 Nb4 113.21(7) . . ?
Nb1 O5 K1 111.62(6) . 2 ?
Nb1 O5 K4 101.85(6) . . ?
Nb4 O5 K1 131.05(7) . 2 ?
Nb4 O5 K4 105.06(6) . . ?
K1 O5 K4 83.76(4) 2 . ?
K3 O5W K8 160.69(6) . 3_566 ?
Na2 O5W K3 80.51(5) . . ?
Na2 O5W K8 82.07(5) . 3_566 ?
Nb1 O6 K4 100.98(6) . . ?
Nb1 O6 K5 102.30(6) . . ?
Nb5 O6 Nb1 112.70(7) . . ?
Nb5 O6 K4 102.85(6) . . ?
Nb5 O6 K5 101.39(6) . . ?
K4 O6 K5 136.38(6) . . ?
K7 O6W K6 166.23(6) 1_565 3_666 ?
Na2 O6W K6 81.51(5) . 3_666 ?
Na2 O6W K7 85.08(5) . 1_565 ?
Nb2 O7 Nb5 114.00(7) . . ?
Nb2 O7 K5 101.59(6) . . ?
Nb5 O7 K5 102.40(6) . . ?
K6 O7W K8 162.92(6) 3_666 3_566 ?
Na2 O7W K6 83.28(5) . 3_666 ?
Na2 O7W K8 82.36(5) . 3_566 ?
Nb3 O8 Nb5 114.27(7) . . ?
K6 O8W K3 166.35(7) 3_666 . ?
Na2 O8W K3 82.56(5) . . ?
Na2 O8W K6 83.92(5) . 3_666 ?
Nb4 O9 K4 101.80(6) . . ?
Nb5 O9 Nb4 113.82(7) . . ?
Nb5 O9 K4 99.55(6) . . ?
K1 O9W K5 143.94(7) 1_565 2_655 ?
K4 O9W K1 83.57(5) . 1_565 ?
K4 O9W K5 90.56(5) . 2_655 ?
Nb1 O10 Nb6 114.70(7) . . ?
Nb1 O10 K1 123.44(7) . . ?
Nb1 O10 Na1 123.44(7) . . ?
Nb6 O10 K1 114.07(7) . . ?
Nb6 O10 Na1 114.07(7) . . ?
K4 O10W K1 83.82(5) . 1_565 ?
Nb2 O11 Nb6 113.46(7) . . ?
K4 O11W K1 80.32(5) . 2 ?
K6 O11W K1 175.85(7) 2_655 2 ?
K6 O11W K4 102.64(5) 2_655 . ?
Nb3 O12 Nb6 114.87(7) . . ?
Nb3 O12 K8 102.61(6) . . ?
Nb6 O12 K8 100.78(6) . . ?
K4 O12W K6 99.34(5) . 2_655 ?
K5 O12W K4 102.05(6) 2_655 . ?
K5 O12W K6 128.21(6) 2_655 2_655 ?
Nb4 O13 Nb6 115.03(8) . . ?
Nb4 O13 K8 102.05(6) . . ?
Nb6 O13 K8 102.02(6) . . ?
Nb2 O15 K6 128.59(8) . . ?
Nb2 O15 K7 114.61(7) . . ?
K7 O15 K6 95.19(5) . . ?
Nb3 O16 K3 115.33(7) . . ?
Nb3 O16 K6 111.61(7) . 3_656 ?
Nb3 O16 K7 120.54(7) . 3_656 ?
K3 O16 K6 129.28(6) . 3_656 ?
K3 O16 K7 87.07(4) . 3_656 ?
K6 O16 K7 85.24(4) 3_656 3_656 ?
Nb4 O17 K8 134.45(7) . 3_566 ?
Nb5 O18 K3 118.33(7) . 3_666 ?
Nb5 O18 K7 117.71(7) . 1_565 ?
K7 O18 K3 93.39(5) 1_565 3_666 ?
Nb6 O19 K8 139.08(8) . 3_556 ?
K3 O13W K7 80.87(4) . 3_656 ?
K5 O13W K3 114.39(6) 4_566 . ?
K5 O13W K6 119.38(6) 4_566 3_656 ?
K5 O13W K7 83.34(5) 4_566 3_656 ?
K6 O13W K3 121.28(6) 3_656 . ?
K6 O13W K7 83.47(4) 3_656 3_656 ?
K5 O14W K3 122.49(6) 2_645 4_565 ?

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
O2 Nb2 O15 K6 127.24(9) . . . . ?
O2 Nb2 O15 K7 -113.23(7) . . . . ?
O3 Nb2 O15 K6 -52.37(10) . . . . ?
O3 Nb2 O15 K7 67.16(8) . . . . ?
O3 Nb3 O16 K3 141.18(7) . . . . ?
O3 Nb3 O16 K6 -58.63(8) . . . 3_656 ?
O3 Nb3 O16 K7 38.85(9) . . . 3_656 ?
O4 Nb3 O16 K3 -39.18(9) . . . . ?
O4 Nb3 O16 K6 121.01(7) . . . 3_656 ?
O4 Nb3 O16 K7 -141.51(7) . . . 3_656 ?
O4 Nb4 O17 K8 38.23(11) . . . 3_566 ?
O5 Nb4 O17 K8 -140.73(9) . . . 3_566 ?
O6 Nb5 O18 K3 -127.17(7) . . . 3_666 ?
O6 Nb5 O18 K7 121.79(7) . . . 1_565 ?
O7 Nb2 O15 K6 38.42(10) . . . . ?
O7 Nb2 O15 K7 157.94(7) . . . . ?
O7 Nb5 O18 K3 -38.14(9) . . . 3_666 ?
O7 Nb5 O18 K7 -149.18(7) . . . 1_565 ?
O8 Nb3 O16 K3 51.39(8) . . . . ?
O8 Nb3 O16 K6 -148.42(6) . . . 3_656 ?
O8 Nb3 O16 K7 -50.94(8) . . . 3_656 ?
O8 Nb5 O18 K3 51.17(8) . . . 3_666 ?
O8 Nb5 O18 K7 -59.87(8) . . . 1_565 ?
O9 Nb4 O17 K8 -52.17(11) . . . 3_566 ?
O9 Nb5 O18 K3 141.98(7) . . . 3_666 ?
O9 Nb5 O18 K7 30.94(9) . . . 1_565 ?
O10 Nb6 O19 K8 139.00(11) . . . 3_556 ?
O11 Nb2 O15 K6 -142.86(9) . . . . ?
O11 Nb2 O15 K7 -23.33(8) . . . . ?
O11 Nb6 O19 K8 49.76(13) . . . 3_556 ?
O12 Nb3 O16 K3 -128.78(7) . . . . ?
O12 Nb3 O16 K6 31.41(8) . . . 3_656 ?
O12 Nb3 O16 K7 128.89(7) . . . 3_656 ?
O12 Nb6 O19 K8 -41.86(13) . . . 3_556 ?
O13 Nb4 O17 K8 128.16(10) . . . 3_566 ?
O13 Nb6 O19 K8 -131.94(11) . . . 3_556 ?

_olex2_exptl_crystal_mounting_method 'Dual Thickness MiTeGen'
_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 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.876

# start Validation Reply Form
_vrf_PLAT196_mp-katsyn-005_v1    
;
PROBLEM: No TEMP record and _measurement_temperature .NE. 293 Degree
RESPONSE: The measurement temperature was 100 K.
;
_vrf_PLAT306_mp-katsyn-005_v1    
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: The isolated oxygen atom belongs to a crystal water
molecule.
;
_vrf_PLAT971_mp-katsyn-005_v1    
;
PROBLEM: Check Calcd Resid. Dens. 0.78Ang From K1 2.72 eA-3
RESPONSE: The residual density results from crystal water molecules.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_jcr85_sq_sq
_database_code_depnum_ccdc_archive 'CCDC 2216946'
loop_
_audit_author_name
_audit_author_address
'J.-C. Raabe'
;Hamburg University
Germany
;
_audit_update_record             
;
2022-11-02 deposited with the CCDC.	2023-07-17 downloaded from the CCDC.
;
_audit_creation_date             2022-11-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Jan-Christian.Raabe@chemie.uni-hamburg.de
Maximilian.Poller@chemie.uni-hamburg.de
Tobias.Esser@chemie.uni-hamburg.de
Jakob.Albert@chemie.uni-hamburg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'K2 Mo18 Na2 O69 P2, 4(O)'
_chemical_formula_sum            'K2 Mo18 Na2 O73 P2'
_chemical_formula_weight         3081.04
_chemical_melting_point          ?
_chemical_oxdiff_formula         'O102 P3 K27 Mo27 C1 '
_chemical_oxdiff_usercomment     'Raabe/Albert, 03.11.2021, Mo, 100K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'
P P 0.1023 0.0942 '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                   12.71140(10)
_cell_length_b                   14.7642(2)
_cell_length_c                   19.7054(2)
_cell_angle_alpha                102.4650(10)
_cell_angle_beta                 99.1190(10)
_cell_angle_gamma                114.6200(10)
_cell_volume                     3151.58(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    93343
_cell_measurement_temperature    99.95(16)
_cell_measurement_theta_max      29.3350
_cell_measurement_theta_min      3.1770
_shelx_estimated_absorpt_T_max   0.660
_shelx_estimated_absorpt_T_min   0.550
_exptl_absorpt_coefficient_mu    3.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.247
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            139665
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.566
_diffrn_reflns_theta_min         2.827
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2063
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_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   17.50    --   -9.87 -99.00  60.00   46
  2  ω    -67.00 -28.00   1.00   17.50    --   -9.87 126.00-166.50   39
  3  ω      7.00  68.00   1.00   17.50    --   10.57-127.00  20.14   61
  4  ω    -14.00  85.00   1.00   17.50    --   10.57  38.00   0.00   99
  5  ω    -14.00  85.00   1.00   17.50    --   10.57  38.00 -90.00   99
  6  ω    -78.00  99.00   1.00   17.50    --   10.57   0.00-150.00  177
  7  ω      6.00  67.00   1.00   17.50    --   10.57-125.00 101.92   61
  8  ω    -14.00  85.00   1.00   17.50    --   10.57  38.00  60.00   99
  9  ω      3.00  65.00   1.00   17.50    --   10.57-122.00-136.71   62
 10  ω    -42.00  23.00   1.00   17.50    --   -9.87 -77.00 120.00   65
 11  ω    -67.00 -28.00   1.00   17.50    --   -9.87 126.00 164.63   39
 12  ω    -86.00 -43.00   1.00   17.50    --   -9.87 154.00-130.56   43
 13  ω     22.00  87.00   1.00   17.50    --   10.57-155.00 179.30   65
 14  ω      5.00  66.00   1.00   17.50    --   10.57-124.00 -32.54   61
 15  ω    -64.00  35.00   1.00   17.50    --   10.57 -38.00 -90.00   99
 16  ω      3.00  65.00   1.00   17.50    --   10.57-122.00 174.10   62
 17  ω    -86.00 -43.00   1.00   17.50    --   -9.87 154.00 -49.63   43
 18  ω    -42.00  23.00   1.00   17.50    --   -9.87 -77.00-120.00   65
 19  ω    -26.00  91.00   1.00   17.50    --   10.57  19.00   0.00  117
 20  ω    -78.00 -24.00   1.00   17.50    --   10.57   0.00-180.00   54
 21  ω    -42.00  43.00   1.00   17.50    --   10.57 -77.00 -30.00   85
;
_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      0.0312529000
_diffrn_orient_matrix_UB_12      -0.0301330000
_diffrn_orient_matrix_UB_13      -0.0034309000
_diffrn_orient_matrix_UB_21      -0.0342904000
_diffrn_orient_matrix_UB_22      -0.0265563000
_diffrn_orient_matrix_UB_23      -0.0367492000
_diffrn_orient_matrix_UB_31      0.0439898000
_diffrn_orient_matrix_UB_32      0.0385357000
_diffrn_orient_matrix_UB_33      -0.0105907000
_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                15885
_reflns_number_total             16647
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         15.064
_refine_diff_density_min         -1.805
_refine_diff_density_rms         0.257
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         16647
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.030
_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)+(0.0424P)²+60.0753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1007
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
;
_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
Mo1 Mo 0.52529(4) 0.58443(3) 0.20053(2) 0.00671(8) Uani 1 1 d . . . . .
Mo2 Mo 0.62269(4) 0.62732(3) 0.37827(2) 0.00703(8) Uani 1 1 d . . . . .
Mo3 Mo 0.89440(4) 0.60198(3) 0.44207(2) 0.00783(8) Uani 1 1 d . . . . .
Mo4 Mo 0.96204(4) 0.44750(3) 0.32878(2) 0.00645(8) Uani 1 1 d . . . . .
Mo5 Mo 0.84295(4) 0.39256(4) 0.13308(2) 0.00843(8) Uani 1 1 d . . . . .
Mo6 Mo 0.59737(4) 0.41442(4) 0.07212(2) 0.00843(8) Uani 1 1 d . . . . .
Mo7 Mo 0.92155(4) 0.79411(3) 0.34514(2) 0.00791(8) Uani 1 1 d . . . . .
Mo8 Mo 1.04407(4) 0.66912(3) 0.24478(2) 0.00882(9) Uani 1 1 d . . . . .
Mo9 Mo 0.81767(4) 0.70521(3) 0.16151(2) 0.00837(8) Uani 1 1 d . . . . .
Mo10 Mo 0.29128(4) 0.32193(3) 0.20870(2) 0.00644(8) Uani 1 1 d . . . . .
Mo11 Mo 0.39294(4) 0.36591(3) 0.38601(2) 0.00741(8) Uani 1 1 d . . . . .
Mo12 Mo 0.66356(4) 0.34357(3) 0.45414(2) 0.00731(8) Uani 1 1 d . . . . .
Mo13 Mo 0.72713(4) 0.18632(3) 0.33706(2) 0.00708(8) Uani 1 1 d . . . . .
Mo14 Mo 0.61462(4) 0.12921(3) 0.14152(2) 0.00858(8) Uani 1 1 d . . . . .
Mo15 Mo 0.36978(4) 0.15280(3) 0.08392(2) 0.00887(9) Uani 1 1 d . . . . .
Mo16 Mo 0.19714(4) 0.03824(3) 0.20526(3) 0.00913(9) Uani 1 1 d . . . . .
Mo17 Mo 0.35089(4) 0.10270(3) 0.37977(2) 0.00855(8) Uani 1 1 d . . . . .
Mo18 Mo 0.41812(4) -0.02780(3) 0.24393(3) 0.00873(9) Uani 1 1 d . . . . .
K1 K 0.92946(10) 0.76695(9) 0.65681(6) 0.0131(2) Uani 1 1 d . . . . .
K2 K 0.14577(14) 0.00378(11) -0.13518(8) 0.0243(3) Uani 1 1 d . . . . .
P1 P 0.75118(11) 0.52272(10) 0.25829(7) 0.0056(2) Uani 1 1 d . . . . .
P2 P 0.49938(11) 0.23839(10) 0.26824(7) 0.0057(2) Uani 1 1 d . . . . .
Na1 Na 1.2146(3) 0.8010(3) 0.44434(15) 0.0326(7) Uani 1 1 d . . . . .
Na2 Na 1.3675(3) 1.1103(3) 0.6041(3) 0.0495(10) Uani 1 1 d . . . . .
O1 O 0.6432(3) 0.5362(3) 0.27370(19) 0.0069(6) Uani 1 1 d . . . . .
O1W O 1.4182(7) 0.9742(8) 0.5396(4) 0.067(3) Uani 1 1 d . . . . .
O2 O 0.8128(3) 0.4979(3) 0.3196(2) 0.0073(6) Uani 1 1 d . . . . .
O2W O 1.3807(7) 0.7828(5) 0.3641(3) 0.0476(18) Uani 1 1 d . . . . .
O3 O 0.7139(3) 0.4397(3) 0.1847(2) 0.0075(7) Uani 1 1 d . . . . .
O3W O 1.3157(9) 1.1094(7) 0.7289(18) 0.33(2) Uani 1 1 d . . . A 2
O4 O 0.8460(3) 0.6302(3) 0.2541(2) 0.0075(7) Uani 1 1 d . . . . .
O4W O 1.0603(5) 0.9730(3) 0.7196(3) 0.0236(10) Uani 1 1 d . . . . .
O5 O 0.5385(3) 0.6499(3) 0.2972(2) 0.0093(7) Uani 1 1 d . . . . .
O5W O 0.8967(4) 0.8513(4) 0.5457(3) 0.0217(9) Uani 1 1 d . . . . .
O6 O 0.7432(3) 0.6037(3) 0.4241(2) 0.0091(7) Uani 1 1 d . . . . .
O6W O -0.0053(5) -0.0849(5) -0.0511(4) 0.0438(16) Uani 1 1 d . . . . .
O7 O 0.9990(3) 0.5478(3) 0.4213(2) 0.0090(7) Uani 1 1 d . . . . .
O7W O 0.0564(4) -0.2044(3) -0.2051(2) 0.0145(8) Uani 1 1 d . . . . .
O8 O 0.8961(3) 0.3871(3) 0.2266(2) 0.0088(7) Uani 1 1 d . . . . .
O9 O 0.7317(3) 0.3896(3) 0.0559(2) 0.0087(7) Uani 1 1 d . . . . .
O10 O 0.5203(3) 0.4756(3) 0.1259(2) 0.0088(7) Uani 1 1 d . . . . .
O11 O 0.6643(3) 0.6794(3) 0.1925(2) 0.0099(7) Uani 1 1 d . . . . .
O12 O 0.7762(3) 0.7462(3) 0.3599(2) 0.0103(7) Uani 1 1 d . . . . .
O13 O 0.9567(3) 0.7139(3) 0.4084(2) 0.0107(7) Uani 1 1 d . . . . .
O14 O 1.0443(3) 0.5857(3) 0.2988(2) 0.0100(7) Uani 1 1 d . . . . .
O15 O 0.9471(3) 0.5318(3) 0.1606(2) 0.0089(7) Uani 1 1 d . . . . .
O16 O 0.7293(3) 0.5736(3) 0.1008(2) 0.0104(7) Uani 1 1 d . . . . .
O17 O 0.8859(3) 0.8186(3) 0.2586(2) 0.0100(7) Uani 1 1 d . . . . .
O18 O 1.0660(3) 0.7843(3) 0.3161(2) 0.0103(7) Uani 1 1 d . . . . .
O19 O 0.9687(3) 0.7171(3) 0.1700(2) 0.0105(7) Uani 1 1 d . . . . .
O20 O 0.3888(3) 0.4534(3) 0.2154(2) 0.0090(7) Uani 1 1 d . . . . .
O21 O 0.4958(3) 0.5120(3) 0.3756(2) 0.0098(7) Uani 1 1 d . . . . .
O22 O 0.7859(3) 0.4572(3) 0.4511(2) 0.0091(7) Uani 1 1 d . . . . .
O23 O 0.8640(3) 0.3357(3) 0.3473(2) 0.0087(7) Uani 1 1 d . . . . .
O24 O 0.7068(3) 0.2437(3) 0.1211(2) 0.0094(7) Uani 1 1 d . . . . .
O25 O 0.5038(3) 0.2836(3) 0.0691(2) 0.0093(7) Uani 1 1 d . . . . .
O26 O 0.4475(3) 0.3154(3) 0.2810(2) 0.0075(7) Uani 1 1 d . . . . .
O27 O 0.6159(3) 0.2762(3) 0.3275(2) 0.0076(7) Uani 1 1 d . . . . .
O28 O 0.5186(3) 0.2186(3) 0.1927(2) 0.0078(7) Uani 1 1 d . . . . .
O29 O 0.4044(3) 0.1310(3) 0.2723(2) 0.0078(7) Uani 1 1 d . . . . .
O30 O 0.2763(3) 0.3538(3) 0.3054(2) 0.0086(7) Uani 1 1 d . . . . .
O31 O 0.5450(3) 0.3859(3) 0.4334(2) 0.0091(7) Uani 1 1 d . . . . .
O32 O 0.7344(3) 0.2509(3) 0.4325(2) 0.0084(7) Uani 1 1 d . . . . .
O33 O 0.7110(3) 0.1754(3) 0.2376(2) 0.0088(7) Uani 1 1 d . . . . .
O34 O 0.4717(3) 0.0919(3) 0.0675(2) 0.0096(7) Uani 1 1 d . . . . .
O35 O 0.3332(3) 0.2585(3) 0.1320(2) 0.0088(7) Uani 1 1 d . . . . .
O36 O 0.2060(3) 0.1636(3) 0.2118(2) 0.0093(7) Uani 1 1 d . . . . .
O37 O 0.3226(3) 0.2277(3) 0.3797(2) 0.0099(7) Uani 1 1 d . . . . .
O38 O 0.5027(3) 0.1958(3) 0.4280(2) 0.0092(7) Uani 1 1 d . . . . .
O39 O 0.5869(3) 0.0696(3) 0.3160(2) 0.0094(7) Uani 1 1 d . . . . .
O40 O 0.4928(3) 0.0186(3) 0.1785(2) 0.0100(7) Uani 1 1 d . . . . .
O41 O 0.2741(3) 0.0601(3) 0.1215(2) 0.0105(7) Uani 1 1 d . . . . .
O42 O 0.1949(3) 0.0337(3) 0.2968(2) 0.0105(7) Uani 1 1 d . . . . .
O43 O 0.3752(3) -0.0099(3) 0.3379(2) 0.0099(7) Uani 1 1 d . . . . .
O44 O 0.2635(3) -0.0666(3) 0.1965(2) 0.0104(7) Uani 1 1 d . . . . .
O45 O 0.4257(4) 0.6167(3) 0.1586(2) 0.0119(7) Uani 1 1 d . . . . .
O46 O 0.6241(4) 0.7216(3) 0.4452(2) 0.0120(7) Uani 1 1 d . . . . .
O47 O 0.9528(4) 0.6606(3) 0.5320(2) 0.0113(7) Uani 1 1 d . . . . .
O48 O 1.0911(3) 0.4366(3) 0.3393(2) 0.0102(7) Uani 1 1 d . . . . .
O49 O 0.9181(4) 0.3414(3) 0.0873(2) 0.0114(7) Uani 1 1 d . . . . .
O50 O 0.5424(4) 0.4126(3) -0.0124(2) 0.0133(8) Uani 1 1 d . . . . .
O51 O 0.9997(4) 0.9183(3) 0.4038(2) 0.0135(8) Uani 1 1 d . . . . .
O52 O 1.1791(4) 0.7076(3) 0.2269(2) 0.0139(8) Uani 1 1 d . . . . .
O53 O 0.8097(4) 0.7801(3) 0.1091(2) 0.0130(7) Uani 1 1 d . . . . .
O54 O 0.1551(3) 0.3054(3) 0.1644(2) 0.0119(7) Uani 1 1 d . . . . .
O55 O 0.3438(4) 0.4142(3) 0.4519(2) 0.0128(7) Uani 1 1 d . . . . .
O56 O 0.6861(4) 0.3607(3) 0.5438(2) 0.0126(7) Uani 1 1 d . . . . .
O57 O 0.8293(3) 0.1428(3) 0.3548(2) 0.0118(7) Uani 1 1 d . . . . .
O58 O 0.6565(4) 0.0416(3) 0.1000(2) 0.0116(7) Uani 1 1 d . . . . .
O59 O 0.2827(4) 0.1151(3) -0.0011(2) 0.0121(7) Uani 1 1 d . . . . .
O60 O 0.0537(4) -0.0473(3) 0.1542(2) 0.0146(8) Uani 1 1 d . . . . .
O61 O 0.2866(4) 0.0641(3) 0.4444(2) 0.0130(7) Uani 1 1 d . . . . .
O62 O 0.4200(3) -0.1439(3) 0.2357(2) 0.0124(7) Uani 1 1 d . . . . .
O8W O 0.1776(4) 0.5064(3) 0.1445(3) 0.0157(8) Uani 1 1 d . . . . .
O9W O 0.0236(6) 0.5995(5) 0.0409(3) 0.0381(14) Uani 1 1 d . . . . .
O10W O 0.2703(9) 0.8477(6) 0.0384(4) 0.068(2) Uani 1 1 d . . . . .
O11W O 0.2511(5) 0.3846(4) 0.0410(3) 0.0303(11) 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
Mo1 O1 2.341(4) . ?
Mo1 O5 1.887(4) . ?
Mo1 O10 1.901(4) . ?
Mo1 O11 1.797(4) . ?
Mo1 O20 2.110(4) . ?
Mo1 O45 1.689(4) . ?
Mo2 O1 2.322(4) . ?
Mo2 O5 1.948(4) . ?
Mo2 O6 1.851(4) . ?
Mo2 O12 2.160(4) . ?
Mo2 O21 1.775(4) . ?
Mo2 O46 1.690(4) . ?
Mo3 O2 2.353(4) . ?
Mo3 O6 1.911(4) . ?
Mo3 O7 1.868(4) . ?
Mo3 O13 1.830(4) . ?
Mo3 O22 2.071(4) . ?
Mo3 O47 1.681(4) . ?
Mo4 K1 3.9888(13) 2_766 ?
Mo4 O2 2.304(4) . ?
Mo4 O7 1.930(4) . ?
Mo4 O8 1.903(4) . ?
Mo4 O14 2.132(4) . ?
Mo4 O23 1.761(4) . ?
Mo4 O48 1.699(4) . ?
Mo5 O3 2.321(4) . ?
Mo5 O8 1.890(4) . ?
Mo5 O9 1.885(4) . ?
Mo5 O15 1.816(4) . ?
Mo5 O24 2.088(4) . ?
Mo5 O49 1.696(4) . ?
Mo6 O3 2.323(4) . ?
Mo6 O9 1.948(4) . ?
Mo6 O10 1.884(4) . ?
Mo6 O16 2.120(4) . ?
Mo6 O25 1.778(4) . ?
Mo6 O50 1.691(4) . ?
Mo7 O4 2.375(4) . ?
Mo7 O12 1.780(4) . ?
Mo7 O13 2.014(4) . ?
Mo7 O17 1.845(4) . ?
Mo7 O18 2.059(4) . ?
Mo7 O51 1.700(4) . ?
Mo8 O4 2.385(4) . ?
Mo8 O14 1.794(4) . ?
Mo8 O15 2.050(4) . ?
Mo8 O18 1.842(4) . ?
Mo8 O19 2.039(4) . ?
Mo8 O52 1.691(4) . ?
Mo9 O4 2.383(4) . ?
Mo9 O11 2.045(4) . ?
Mo9 O16 1.795(4) . ?
Mo9 O17 2.023(4) . ?
Mo9 O19 1.830(4) . ?
Mo9 O53 1.688(4) . ?
Mo10 O20 1.775(4) . ?
Mo10 O26 2.303(4) . ?
Mo10 O30 1.921(4) . ?
Mo10 O35 1.872(4) . ?
Mo10 O36 2.148(4) . ?
Mo10 O54 1.702(4) . ?
Mo11 K1 3.5842(12) 2_666 ?
Mo11 O21 2.081(4) . ?
Mo11 O26 2.353(4) . ?
Mo11 O30 1.914(4) . ?
Mo11 O31 1.878(4) . ?
Mo11 O37 1.821(4) . ?
Mo11 O55 1.678(4) . ?
Mo12 O22 1.771(4) . ?
Mo12 O27 2.351(4) . ?
Mo12 O31 1.879(4) . ?
Mo12 O32 1.939(4) . ?
Mo12 O38 2.161(4) . ?
Mo12 O56 1.689(4) . ?
Mo13 K1 4.1028(13) 2_766 ?
Mo13 O23 2.105(4) . ?
Mo13 O27 2.320(4) . ?
Mo13 O32 1.885(4) . ?
Mo13 O33 1.903(4) . ?
Mo13 O39 1.794(4) . ?
Mo13 O57 1.694(4) . ?
Mo14 O24 1.784(4) . ?
Mo14 O28 2.325(4) . ?
Mo14 O33 1.887(4) . ?
Mo14 O34 1.926(4) . ?
Mo14 O40 2.088(4) . ?
Mo14 O58 1.697(4) . ?
Mo15 O25 2.092(4) . ?
Mo15 O28 2.324(4) . ?
Mo15 O34 1.889(4) . ?
Mo15 O35 1.912(4) . ?
Mo15 O41 1.800(4) . ?
Mo15 O59 1.684(4) . ?
Mo16 K2 4.0939(15) 2 ?
Mo16 O29 2.382(4) . ?
Mo16 O36 1.781(4) . ?
Mo16 O41 2.064(4) . ?
Mo16 O42 1.823(4) . ?
Mo16 O44 2.039(4) . ?
Mo16 O60 1.698(4) . ?
Mo17 O29 2.392(4) . ?
Mo17 O37 2.022(4) . ?
Mo17 O38 1.778(4) . ?
Mo17 O42 2.053(4) . ?
Mo17 O43 1.859(4) . ?
Mo17 O61 1.695(4) . ?
Mo18 O29 2.376(4) . ?
Mo18 O39 2.066(4) . ?
Mo18 O40 1.805(4) . ?
Mo18 O43 2.007(4) . ?
Mo18 O44 1.820(4) . ?
Mo18 O62 1.697(4) . ?
K1 O4W 2.656(5) . ?
K1 O5W 2.800(5) . ?
K1 O7W 2.779(4) 1_666 ?
K1 O30 2.807(4) 2_666 ?
K1 O37 3.209(4) 2_666 ?
K1 O47 2.749(4) . ?
K1 O48 2.925(4) 2_766 ?
K1 O55 3.352(4) 2_666 ?
K1 O57 2.861(4) 2_766 ?
K2 O4W 2.761(5) 1_444 ?
K2 O6W 2.827(7) . ?
K2 O7W 2.721(4) . ?
K2 O53 2.909(4) 2_665 ?
K2 O58 2.881(4) 2_655 ?
K2 O59 2.645(4) . ?
K2 O60 2.854(4) 2 ?
P1 O1 1.532(4) . ?
P1 O2 1.530(4) . ?
P1 O3 1.536(4) . ?
P1 O4 1.572(4) . ?
P2 O26 1.532(4) . ?
P2 O27 1.533(4) . ?
P2 O28 1.532(4) . ?
P2 O29 1.571(4) . ?
Na1 O1W 2.763(10) . ?
Na1 O2W 2.894(8) . ?
Na1 O13 2.874(5) . ?
Na1 O18 2.801(5) . ?
Na1 O32 2.759(4) 2_766 ?
Na2 O1W 2.512(11) . ?
Na2 O2W 2.804(9) 2_876 ?
Na2 O3W 2.65(3) . ?
Na2 O46 2.822(6) 2_776 ?
Na2 O61 2.980(6) 1_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
O5 Mo1 O1 73.48(14) . . ?
O5 Mo1 O10 153.20(16) . . ?
O5 Mo1 O20 83.02(15) . . ?
O10 Mo1 O1 82.87(14) . . ?
O10 Mo1 O20 80.53(15) . . ?
O11 Mo1 O1 86.66(15) . . ?
O11 Mo1 O5 99.01(17) . . ?
O11 Mo1 O10 91.88(17) . . ?
O11 Mo1 O20 165.23(16) . . ?
O20 Mo1 O1 79.87(13) . . ?
O45 Mo1 O1 169.71(16) . . ?
O45 Mo1 O5 98.42(18) . . ?
O45 Mo1 O10 103.42(18) . . ?
O45 Mo1 O11 101.10(18) . . ?
O45 Mo1 O20 93.01(17) . . ?
O5 Mo2 O1 72.94(14) . . ?
O5 Mo2 O12 81.10(15) . . ?
O6 Mo2 O1 83.68(15) . . ?
O6 Mo2 O5 152.99(16) . . ?
O6 Mo2 O12 80.64(16) . . ?
O12 Mo2 O1 77.05(14) . . ?
O21 Mo2 O1 90.51(15) . . ?
O21 Mo2 O5 94.81(17) . . ?
O21 Mo2 O6 98.79(17) . . ?
O21 Mo2 O12 167.54(16) . . ?
O46 Mo2 O1 164.11(16) . . ?
O46 Mo2 O5 97.50(18) . . ?
O46 Mo2 O6 101.93(18) . . ?
O46 Mo2 O12 89.10(17) . . ?
O46 Mo2 O21 103.14(18) . . ?
O6 Mo3 O2 81.17(14) . . ?
O6 Mo3 O22 80.55(15) . . ?
O7 Mo3 O2 73.73(15) . . ?
O7 Mo3 O6 153.51(16) . . ?
O7 Mo3 O22 86.39(15) . . ?
O13 Mo3 O2 86.08(15) . . ?
O13 Mo3 O6 89.31(17) . . ?
O13 Mo3 O7 97.19(17) . . ?
O13 Mo3 O22 163.05(16) . . ?
O22 Mo3 O2 79.00(14) . . ?
O47 Mo3 O2 171.53(16) . . ?
O47 Mo3 O6 102.76(18) . . ?
O47 Mo3 O7 101.08(18) . . ?
O47 Mo3 O13 101.36(19) . . ?
O47 Mo3 O22 94.15(17) . . ?
O2 Mo4 K1 150.46(9) . 2_766 ?
O7 Mo4 K1 113.10(11) . 2_766 ?
O7 Mo4 O2 73.89(14) . . ?
O7 Mo4 O14 82.77(15) . . ?
O8 Mo4 K1 92.59(12) . 2_766 ?
O8 Mo4 O2 83.39(15) . . ?
O8 Mo4 O7 154.30(16) . . ?
O8 Mo4 O14 81.14(15) . . ?
O14 Mo4 K1 129.64(11) . 2_766 ?
O14 Mo4 O2 78.80(14) . . ?
O23 Mo4 K1 62.52(12) . 2_766 ?
O23 Mo4 O2 88.52(15) . . ?
O23 Mo4 O7 96.87(16) . . ?
O23 Mo4 O8 94.35(17) . . ?
O23 Mo4 O14 166.92(16) . . ?
O48 Mo4 K1 40.93(13) . 2_766 ?
O48 Mo4 O2 168.41(16) . . ?
O48 Mo4 O7 99.90(17) . . ?
O48 Mo4 O8 100.24(17) . . ?
O48 Mo4 O14 90.82(17) . . ?
O48 Mo4 O23 102.09(18) . . ?
O8 Mo5 O3 82.51(15) . . ?
O8 Mo5 O24 82.21(15) . . ?
O9 Mo5 O3 74.19(14) . . ?
O9 Mo5 O8 154.76(16) . . ?
O9 Mo5 O24 84.45(15) . . ?
O15 Mo5 O3 86.94(15) . . ?
O15 Mo5 O8 90.99(17) . . ?
O15 Mo5 O9 97.22(17) . . ?
O15 Mo5 O24 166.32(16) . . ?
O24 Mo5 O3 80.43(14) . . ?
O49 Mo5 O3 171.29(16) . . ?
O49 Mo5 O8 100.97(18) . . ?
O49 Mo5 O9 100.83(18) . . ?
O49 Mo5 O15 100.90(18) . . ?
O49 Mo5 O24 92.07(17) . . ?
O9 Mo6 O3 73.06(14) . . ?
O9 Mo6 O16 82.43(15) . . ?
O10 Mo6 O3 84.61(14) . . ?
O10 Mo6 O9 154.89(16) . . ?
O10 Mo6 O16 81.85(15) . . ?
O16 Mo6 O3 78.16(14) . . ?
O25 Mo6 O3 88.29(15) . . ?
O25 Mo6 O9 94.89(16) . . ?
O25 Mo6 O10 95.79(17) . . ?
O25 Mo6 O16 166.39(16) . . ?
O50 Mo6 O3 167.29(17) . . ?
O50 Mo6 O9 97.96(18) . . ?
O50 Mo6 O10 102.02(18) . . ?
O50 Mo6 O16 91.93(18) . . ?
O50 Mo6 O25 101.66(19) . . ?
O12 Mo7 O4 87.08(15) . . ?
O12 Mo7 O13 86.77(17) . . ?
O12 Mo7 O17 99.30(17) . . ?
O12 Mo7 O18 156.37(16) . . ?
O13 Mo7 O4 81.76(14) . . ?
O13 Mo7 O18 79.14(16) . . ?
O17 Mo7 O4 74.52(15) . . ?
O17 Mo7 O13 155.10(16) . . ?
O17 Mo7 O18 86.43(16) . . ?
O18 Mo7 O4 72.29(14) . . ?
O51 Mo7 O4 168.69(17) . . ?
O51 Mo7 O12 104.11(19) . . ?
O51 Mo7 O13 100.29(18) . . ?
O51 Mo7 O17 101.55(18) . . ?
O51 Mo7 O18 97.06(18) . . ?
O14 Mo8 O4 87.20(15) . . ?
O14 Mo8 O15 84.83(16) . . ?
O14 Mo8 O18 99.09(17) . . ?
O14 Mo8 O19 155.46(16) . . ?
O15 Mo8 O4 80.69(14) . . ?
O18 Mo8 O4 75.66(15) . . ?
O18 Mo8 O15 155.77(16) . . ?
O18 Mo8 O19 88.97(17) . . ?
O19 Mo8 O4 72.31(14) . . ?
O19 Mo8 O15 78.77(15) . . ?
O52 Mo8 O4 169.29(17) . . ?
O52 Mo8 O14 103.40(19) . . ?
O52 Mo8 O15 98.47(18) . . ?
O52 Mo8 O18 103.76(18) . . ?
O52 Mo8 O19 97.02(18) . . ?
O11 Mo9 O4 80.32(14) . . ?
O16 Mo9 O4 87.16(15) . . ?
O16 Mo9 O11 84.67(16) . . ?
O16 Mo9 O17 154.96(16) . . ?
O16 Mo9 O19 99.68(17) . . ?
O17 Mo9 O4 71.46(14) . . ?
O17 Mo9 O11 79.14(15) . . ?
O19 Mo9 O4 75.82(15) . . ?
O19 Mo9 O11 155.46(16) . . ?
O19 Mo9 O17 87.84(16) . . ?
O53 Mo9 O4 169.02(17) . . ?
O53 Mo9 O11 98.56(18) . . ?
O53 Mo9 O16 103.65(19) . . ?
O53 Mo9 O17 97.58(18) . . ?
O53 Mo9 O19 103.76(18) . . ?
O20 Mo10 O26 90.11(15) . . ?
O20 Mo10 O30 95.71(17) . . ?
O20 Mo10 O35 96.20(17) . . ?
O20 Mo10 O36 168.41(16) . . ?
O30 Mo10 O26 73.83(14) . . ?
O30 Mo10 O36 82.60(15) . . ?
O35 Mo10 O26 84.67(15) . . ?
O35 Mo10 O30 155.37(16) . . ?
O35 Mo10 O36 81.41(15) . . ?
O36 Mo10 O26 78.40(13) . . ?
O54 Mo10 O20 102.01(18) . . ?
O54 Mo10 O26 166.02(16) . . ?
O54 Mo10 O30 97.78(18) . . ?
O54 Mo10 O35 100.71(18) . . ?
O54 Mo10 O36 89.58(17) . . ?
O21 Mo11 K1 125.35(11) . 2_666 ?
O21 Mo11 O26 79.54(14) . . ?
O26 Mo11 K1 107.98(9) . 2_666 ?
O30 Mo11 K1 51.03(11) . 2_666 ?
O30 Mo11 O21 83.56(15) . . ?
O30 Mo11 O26 72.75(14) . . ?
O31 Mo11 K1 151.05(12) . 2_666 ?
O31 Mo11 O21 82.33(16) . . ?
O31 Mo11 O26 83.28(14) . . ?
O31 Mo11 O30 154.02(16) . . ?
O37 Mo11 K1 63.30(12) . 2_666 ?
O37 Mo11 O21 165.39(16) . . ?
O37 Mo11 O26 86.53(15) . . ?
O37 Mo11 O30 96.58(17) . . ?
O37 Mo11 O31 91.75(17) . . ?
O55 Mo11 K1 68.42(14) . 2_666 ?
O55 Mo11 O21 93.84(17) . . ?
O55 Mo11 O26 168.77(17) . . ?
O55 Mo11 O30 97.64(18) . . ?
O55 Mo11 O31 104.97(18) . . ?
O55 Mo11 O37 100.60(18) . . ?
O22 Mo12 O27 88.51(15) . . ?
O22 Mo12 O31 96.55(17) . . ?
O22 Mo12 O32 96.03(16) . . ?
O22 Mo12 O38 165.22(16) . . ?
O31 Mo12 O27 84.02(15) . . ?
O31 Mo12 O32 152.73(16) . . ?
O31 Mo12 O38 79.89(15) . . ?
O32 Mo12 O27 72.23(14) . . ?
O32 Mo12 O38 81.80(15) . . ?
O38 Mo12 O27 76.88(13) . . ?
O56 Mo12 O22 102.97(19) . . ?
O56 Mo12 O27 165.88(17) . . ?
O56 Mo12 O31 102.51(18) . . ?
O56 Mo12 O32 98.08(18) . . ?
O56 Mo12 O38 91.81(17) . . ?
O23 Mo13 K1 59.62(10) . 2_766 ?
O23 Mo13 O27 79.43(14) . . ?
O27 Mo13 K1 138.56(9) . 2_766 ?
O32 Mo13 K1 105.59(11) . 2_766 ?
O32 Mo13 O23 84.08(15) . . ?
O32 Mo13 O27 73.85(14) . . ?
O32 Mo13 O33 153.65(16) . . ?
O33 Mo13 K1 84.36(11) . 2_766 ?
O33 Mo13 O23 80.14(15) . . ?
O33 Mo13 O27 82.56(15) . . ?
O39 Mo13 K1 132.25(12) . 2_766 ?
O39 Mo13 O23 165.46(16) . . ?
O39 Mo13 O27 87.44(15) . . ?
O39 Mo13 O32 98.35(17) . . ?
O39 Mo13 O33 92.07(17) . . ?
O57 Mo13 K1 34.04(13) . 2_766 ?
O57 Mo13 O23 91.49(17) . . ?
O57 Mo13 O27 169.17(16) . . ?
O57 Mo13 O32 99.52(18) . . ?
O57 Mo13 O33 101.84(18) . . ?
O57 Mo13 O39 102.17(18) . . ?
O24 Mo14 O28 88.74(15) . . ?
O24 Mo14 O33 94.63(17) . . ?
O24 Mo14 O34 94.80(16) . . ?
O24 Mo14 O40 166.39(16) . . ?
O33 Mo14 O28 83.87(15) . . ?
O33 Mo14 O34 155.11(16) . . ?
O33 Mo14 O40 82.36(15) . . ?
O34 Mo14 O28 73.37(14) . . ?
O34 Mo14 O40 83.08(15) . . ?
O40 Mo14 O28 77.77(14) . . ?
O58 Mo14 O24 101.51(18) . . ?
O58 Mo14 O28 168.06(16) . . ?
O58 Mo14 O33 101.19(18) . . ?
O58 Mo14 O34 99.41(18) . . ?
O58 Mo14 O40 92.10(17) . . ?
O25 Mo15 O28 78.89(14) . . ?
O34 Mo15 O25 84.43(15) . . ?
O34 Mo15 O28 74.04(15) . . ?
O34 Mo15 O35 154.30(16) . . ?
O35 Mo15 O25 80.80(15) . . ?
O35 Mo15 O28 82.52(14) . . ?
O41 Mo15 O25 164.82(16) . . ?
O41 Mo15 O28 87.30(15) . . ?
O41 Mo15 O34 97.90(17) . . ?
O41 Mo15 O35 91.26(17) . . ?
O59 Mo15 O25 91.98(17) . . ?
O59 Mo15 O28 169.70(17) . . ?
O59 Mo15 O34 100.53(18) . . ?
O59 Mo15 O35 100.89(18) . . ?
O59 Mo15 O41 102.26(18) . . ?
O29 Mo16 K2 156.13(9) . 2 ?
O36 Mo16 K2 71.99(12) . 2 ?
O36 Mo16 O29 86.45(15) . . ?
O36 Mo16 O41 83.97(16) . . ?
O36 Mo16 O42 101.02(17) . . ?
O36 Mo16 O44 154.26(16) . . ?
O41 Mo16 K2 106.47(11) . 2 ?
O41 Mo16 O29 80.56(14) . . ?
O42 Mo16 K2 97.64(12) . 2 ?
O42 Mo16 O29 76.08(15) . . ?
O42 Mo16 O41 155.70(16) . . ?
O42 Mo16 O44 87.98(17) . . ?
O44 Mo16 K2 131.14(11) . 2 ?
O44 Mo16 O29 72.24(14) . . ?
O44 Mo16 O41 78.54(15) . . ?
O60 Mo16 K2 34.20(14) . 2 ?
O60 Mo16 O29 169.54(17) . . ?
O60 Mo16 O36 103.68(19) . . ?
O60 Mo16 O41 97.72(18) . . ?
O60 Mo16 O42 104.03(19) . . ?
O60 Mo16 O44 97.30(18) . . ?
O37 Mo17 O29 80.57(14) . . ?
O37 Mo17 O42 79.37(15) . . ?
O38 Mo17 O29 86.80(15) . . ?
O38 Mo17 O37 86.16(17) . . ?
O38 Mo17 O42 155.94(16) . . ?
O38 Mo17 O43 99.09(17) . . ?
O42 Mo17 O29 72.02(14) . . ?
O43 Mo17 O29 74.53(15) . . ?
O43 Mo17 O37 154.16(16) . . ?
O43 Mo17 O42 86.40(16) . . ?
O61 Mo17 O29 168.70(17) . . ?
O61 Mo17 O37 100.96(18) . . ?
O61 Mo17 O38 104.46(19) . . ?
O61 Mo17 O42 97.15(18) . . ?
O61 Mo17 O43 102.13(18) . . ?
O39 Mo18 O29 81.12(14) . . ?
O40 Mo18 O29 86.07(15) . . ?
O40 Mo18 O39 83.49(16) . . ?
O40 Mo18 O43 154.26(16) . . ?
O40 Mo18 O44 99.58(17) . . ?
O43 Mo18 O29 72.52(14) . . ?
O43 Mo18 O39 79.31(15) . . ?
O44 Mo18 O29 76.01(15) . . ?
O44 Mo18 O39 156.61(16) . . ?
O44 Mo18 O43 89.15(17) . . ?
O62 Mo18 O29 170.66(17) . . ?
O62 Mo18 O39 98.20(17) . . ?
O62 Mo18 O40 103.15(18) . . ?
O62 Mo18 O43 98.18(18) . . ?
O62 Mo18 O44 103.57(18) . . ?
Mo4 K1 Mo13 56.430(18) 2_766 2_766 ?
Mo11 K1 Mo4 106.44(3) 2_666 2_766 ?
Mo11 K1 Mo13 159.35(4) 2_666 2_766 ?
O4W K1 Mo4 125.99(12) . 2_766 ?
O4W K1 Mo11 122.89(12) . 2_666 ?
O4W K1 Mo13 77.56(11) . 2_766 ?
O4W K1 O5W 75.86(15) . . ?
O4W K1 O7W 73.76(14) . 1_666 ?
O4W K1 O30 122.44(14) . 2_666 ?
O4W K1 O37 94.73(13) . 2_666 ?
O4W K1 O47 123.10(14) . . ?
O4W K1 O48 143.97(14) . 2_766 ?
O4W K1 O55 141.22(14) . 2_666 ?
O4W K1 O57 64.14(14) . 2_766 ?
O5W K1 Mo4 132.05(10) . 2_766 ?
O5W K1 Mo11 85.89(11) . 2_666 ?
O5W K1 Mo13 97.76(11) . 2_766 ?
O5W K1 O30 117.40(14) . 2_666 ?
O5W K1 O37 65.29(12) . 2_666 ?
O5W K1 O48 134.25(13) . 2_766 ?
O5W K1 O55 77.02(13) . 2_666 ?
O5W K1 O57 80.91(13) . 2_766 ?
O7W K1 Mo4 64.87(9) 1_666 2_766 ?
O7W K1 Mo11 116.76(9) 1_666 2_666 ?
O7W K1 Mo13 68.92(9) 1_666 2_766 ?
O7W K1 O5W 148.80(14) 1_666 . ?
O7W K1 O30 85.38(12) 1_666 2_666 ?
O7W K1 O37 124.07(12) 1_666 2_666 ?
O7W K1 O48 72.59(12) 1_666 2_766 ?
O7W K1 O55 132.90(12) 1_666 2_666 ?
O7W K1 O57 79.67(12) 1_666 2_766 ?
O30 K1 Mo4 87.96(8) 2_666 2_766 ?
O30 K1 Mo11 32.02(8) 2_666 2_666 ?
O30 K1 Mo13 142.13(9) 2_666 2_766 ?
O30 K1 O37 54.75(10) 2_666 2_666 ?
O30 K1 O48 67.02(11) 2_666 2_766 ?
O30 K1 O55 51.23(11) 2_666 2_666 ?
O30 K1 O57 161.10(12) 2_666 2_766 ?
O37 K1 Mo4 136.88(8) 2_666 2_766 ?
O37 K1 Mo11 30.46(7) 2_666 2_666 ?
O37 K1 Mo13 162.83(8) 2_666 2_766 ?
O37 K1 O55 48.41(10) 2_666 2_666 ?
O47 K1 Mo4 63.36(9) . 2_766 ?
O47 K1 Mo11 98.09(9) . 2_666 ?
O47 K1 Mo13 64.87(9) . 2_766 ?
O47 K1 O5W 69.15(13) . . ?
O47 K1 O7W 123.58(13) . 1_666 ?
O47 K1 O30 113.27(12) . 2_666 ?
O47 K1 O37 108.71(11) . 2_666 ?
O47 K1 O48 68.26(12) . 2_766 ?
O47 K1 O55 70.36(11) . 2_666 ?
O47 K1 O57 67.10(12) . 2_766 ?
O48 K1 Mo4 22.36(7) 2_766 2_766 ?
O48 K1 Mo11 84.22(8) 2_766 2_666 ?
O48 K1 Mo13 78.68(8) 2_766 2_766 ?
O48 K1 O37 114.68(11) 2_766 2_666 ?
O48 K1 O55 73.72(11) 2_766 2_666 ?
O55 K1 Mo4 92.78(7) 2_666 2_766 ?
O55 K1 Mo11 27.73(7) 2_666 2_666 ?
O55 K1 Mo13 133.50(8) 2_666 2_766 ?
O57 K1 Mo4 75.29(8) 2_766 2_766 ?
O57 K1 Mo11 162.92(9) 2_766 2_666 ?
O57 K1 Mo13 19.36(8) 2_766 2_766 ?
O57 K1 O37 144.08(11) 2_766 2_666 ?
O57 K1 O48 97.25(11) 2_766 2_766 ?
O57 K1 O55 136.72(11) 2_766 2_666 ?
Mo16 K2 K1 64.20(3) 2 1_444 ?
O4W K2 Mo16 63.00(11) 1_444 2 ?
O4W K2 K1 35.97(10) 1_444 1_444 ?
O4W K2 O6W 122.96(17) 1_444 . ?
O4W K2 O53 87.26(13) 1_444 2_665 ?
O4W K2 O58 114.70(14) 1_444 2_655 ?
O4W K2 O60 71.56(14) 1_444 2 ?
O6W K2 Mo16 66.69(14) . 2 ?
O6W K2 K1 97.79(12) . 1_444 ?
O6W K2 O53 107.99(16) . 2_665 ?
O6W K2 O58 104.08(16) . 2_655 ?
O6W K2 O60 70.03(16) . 2 ?
O7W K2 Mo16 86.98(9) . 2 ?
O7W K2 K1 38.41(9) . 1_444 ?
O7W K2 O4W 73.08(13) . 1_444 ?
O7W K2 O6W 79.28(16) . . ?
O7W K2 O53 159.56(13) . 2_665 ?
O7W K2 O58 74.58(12) . 2_655 ?
O7W K2 O60 106.45(13) . 2 ?
O53 K2 Mo16 78.94(9) 2_665 2 ?
O53 K2 K1 121.19(9) 2_665 1_444 ?
O58 K2 Mo16 160.86(9) 2_655 2 ?
O58 K2 K1 102.24(9) 2_655 1_444 ?
O58 K2 O53 120.19(12) 2_655 2_665 ?
O59 K2 Mo16 122.21(10) . 2 ?
O59 K2 K1 167.78(10) . 1_444 ?
O59 K2 O4W 154.85(14) . 1_444 ?
O59 K2 O6W 77.23(15) . . ?
O59 K2 O7W 129.38(13) . . ?
O59 K2 O53 71.03(12) . 2_665 ?
O59 K2 O58 68.74(12) . 2_655 ?
O59 K2 O60 106.53(13) . 2 ?
O60 K2 Mo16 19.53(8) 2 2 ?
O60 K2 K1 81.73(9) 2 1_444 ?
O60 K2 O53 60.65(12) 2 2_665 ?
O60 K2 O58 173.45(13) 2 2_655 ?
O1 P1 O3 111.0(2) . . ?
O1 P1 O4 107.7(2) . . ?
O2 P1 O1 111.5(2) . . ?
O2 P1 O3 111.7(2) . . ?
O2 P1 O4 107.2(2) . . ?
O3 P1 O4 107.4(2) . . ?
O26 P2 O27 111.2(2) . . ?
O26 P2 O28 111.2(2) . . ?
O26 P2 O29 107.6(2) . . ?
O27 P2 O29 107.5(2) . . ?
O28 P2 O27 111.5(2) . . ?
O28 P2 O29 107.6(2) . . ?
O1W Na1 O2W 83.9(2) . . ?
O1W Na1 O13 139.6(2) . . ?
O1W Na1 O18 129.2(2) . . ?
O13 Na1 O2W 133.80(19) . . ?
O18 Na1 O2W 88.44(17) . . ?
O18 Na1 O13 54.40(12) . . ?
O32 Na1 O1W 73.30(17) 2_766 . ?
O32 Na1 O2W 106.64(18) 2_766 . ?
O32 Na1 O13 102.14(15) 2_766 . ?
O32 Na1 O18 155.04(18) 2_766 . ?
O1W Na2 O2W 76.5(3) . 2_876 ?
O1W Na2 O3W 120.6(3) . . ?
O1W Na2 O46 123.2(3) . 2_776 ?
O1W Na2 O61 69.8(2) . 1_665 ?
O2W Na2 O46 84.58(18) 2_876 2_776 ?
O2W Na2 O61 103.1(2) 2_876 1_665 ?
O3W Na2 O61 149.8(3) . 1_665 ?
O46 Na2 O61 63.29(14) 2_776 1_665 ?
Mo2 O1 Mo1 91.80(13) . . ?
P1 O1 Mo1 125.2(2) . . ?
P1 O1 Mo2 130.8(2) . . ?
Na2 O1W Na1 111.4(3) . . ?
Mo4 O2 Mo3 90.66(13) . . ?
P1 O2 Mo3 126.0(2) . . ?
P1 O2 Mo4 131.4(2) . . ?
Na2 O2W Na1 132.5(3) 2_876 . ?
Mo5 O3 Mo6 91.72(13) . . ?
P1 O3 Mo5 125.4(2) . . ?
P1 O3 Mo6 130.9(2) . . ?
Mo7 O4 Mo8 91.04(12) . . ?
Mo7 O4 Mo9 91.16(12) . . ?
Mo9 O4 Mo8 90.23(12) . . ?
P1 O4 Mo7 124.2(2) . . ?
P1 O4 Mo8 125.0(2) . . ?
P1 O4 Mo9 124.9(2) . . ?
K1 O4W K2 106.40(16) . 1_666 ?
Mo1 O5 Mo2 121.68(19) . . ?
Mo2 O6 Mo3 156.3(2) . . ?
Mo3 O7 Mo4 121.4(2) . . ?
K2 O7W K1 104.12(14) . 1_444 ?
Mo5 O8 Mo4 152.9(2) . . ?
Mo5 O9 Mo6 120.80(19) . . ?
Mo6 O10 Mo1 151.3(2) . . ?
Mo1 O11 Mo9 146.8(2) . . ?
Mo7 O12 Mo2 151.7(2) . . ?
Mo3 O13 Mo7 146.4(2) . . ?
Mo3 O13 Na1 109.50(18) . . ?
Mo7 O13 Na1 103.39(16) . . ?
Mo8 O14 Mo4 153.0(2) . . ?
Mo5 O15 Mo8 146.3(2) . . ?
Mo9 O16 Mo6 153.6(2) . . ?
Mo7 O17 Mo9 122.9(2) . . ?
Mo7 O18 Na1 104.62(16) . . ?
Mo8 O18 Mo7 120.98(19) . . ?
Mo8 O18 Na1 108.02(18) . . ?
Mo9 O19 Mo8 121.59(19) . . ?
Mo10 O20 Mo1 161.6(2) . . ?
Mo2 O21 Mo11 160.7(2) . . ?
Mo12 O22 Mo3 165.0(2) . . ?
Mo4 O23 Mo13 163.6(2) . . ?
Mo14 O24 Mo5 161.3(2) . . ?
Mo6 O25 Mo15 162.5(2) . . ?
Mo10 O26 Mo11 91.86(13) . . ?
P2 O26 Mo10 130.7(2) . . ?
P2 O26 Mo11 124.8(2) . . ?
Mo13 O27 Mo12 91.55(13) . . ?
P2 O27 Mo12 131.0(2) . . ?
P2 O27 Mo13 125.5(2) . . ?
Mo15 O28 Mo14 91.28(13) . . ?
P2 O28 Mo14 130.4(2) . . ?
P2 O28 Mo15 125.6(2) . . ?
Mo16 O29 Mo17 90.31(12) . . ?
Mo18 O29 Mo16 90.14(12) . . ?
Mo18 O29 Mo17 90.55(12) . . ?
P2 O29 Mo16 125.4(2) . . ?
P2 O29 Mo17 124.7(2) . . ?
P2 O29 Mo18 125.0(2) . . ?
Mo10 O30 K1 122.77(17) . 2_666 ?
Mo11 O30 Mo10 121.40(19) . . ?
Mo11 O30 K1 96.95(14) . 2_666 ?
Mo11 O31 Mo12 154.3(2) . . ?
Mo12 O32 Na1 107.38(17) . 2_766 ?
Mo13 O32 Mo12 122.18(19) . . ?
Mo13 O32 Na1 128.65(19) . 2_766 ?
Mo14 O33 Mo13 150.8(2) . . ?
Mo15 O34 Mo14 121.18(19) . . ?
Mo10 O35 Mo15 151.9(2) . . ?
Mo16 O36 Mo10 153.8(2) . . ?
Mo11 O37 Mo17 145.2(2) . . ?
Mo11 O37 K1 86.25(14) . 2_666 ?
Mo17 O37 K1 128.28(16) . 2_666 ?
Mo17 O38 Mo12 153.7(2) . . ?
Mo13 O39 Mo18 146.3(2) . . ?
Mo18 O40 Mo14 155.4(2) . . ?
Mo15 O41 Mo16 146.7(2) . . ?
Mo16 O42 Mo17 121.59(19) . . ?
Mo17 O43 Mo18 122.37(19) . . ?
Mo18 O44 Mo16 121.50(19) . . ?
Mo2 O46 Na2 110.4(2) . 2_776 ?
Mo3 O47 K1 146.5(2) . . ?
Mo4 O48 K1 116.71(18) . 2_766 ?
Mo9 O53 K2 135.5(2) . 2_665 ?
Mo11 O55 K1 83.85(15) . 2_666 ?
Mo13 O57 K1 126.60(19) . 2_766 ?
Mo14 O58 K2 135.4(2) . 2_655 ?
Mo15 O59 K2 163.4(2) . . ?
Mo16 O60 K2 126.3(2) . 2 ?
Mo17 O61 Na2 136.3(2) . 1_445 ?

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
K1 Mo4 O23 Mo13 -92.7(8) 2_766 . . . ?
K1 Mo11 O31 Mo12 60.1(6) 2_666 . . . ?
K1 Mo11 O37 Mo17 172.9(4) 2_666 . . . ?
K1 Mo13 O32 Mo12 132.76(18) 2_766 . . . ?
K1 Mo13 O32 Na1 -64.5(2) 2_766 . . 2_766 ?
K1 Mo13 O39 Mo18 -111.6(4) 2_766 . . . ?
K2 Mo16 O36 Mo10 -147.8(5) 2 . . . ?
K2 Mo16 O42 Mo17 -156.35(19) 2 . . . ?
O1 Mo1 O5 Mo2 -2.99(19) . . . . ?
O1 Mo1 O11 Mo9 58.6(4) . . . . ?
O1 Mo2 O6 Mo3 49.7(5) . . . . ?
O1 Mo2 O21 Mo11 77.5(7) . . . . ?
O1 Mo2 O46 Na2 21.1(7) . . . 2_776 ?
O1 P1 O2 Mo3 -57.7(3) . . . . ?
O1 P1 O2 Mo4 171.1(2) . . . . ?
O1 P1 O3 Mo5 177.8(2) . . . . ?
O1 P1 O3 Mo6 46.3(3) . . . . ?
O1 P1 O4 Mo7 52.6(3) . . . . ?
O1 P1 O4 Mo8 172.7(2) . . . . ?
O1 P1 O4 Mo9 -67.6(3) . . . . ?
O2 Mo3 O7 Mo4 -5.26(19) . . . . ?
O2 Mo3 O13 Mo7 56.7(4) . . . . ?
O2 Mo3 O13 Na1 -111.29(17) . . . . ?
O2 Mo4 O23 Mo13 81.2(8) . . . . ?
O2 Mo4 O48 K1 170.6(7) . . . 2_766 ?
O2 P1 O1 Mo1 176.2(2) . . . . ?
O2 P1 O1 Mo2 45.0(3) . . . . ?
O2 P1 O3 Mo5 -57.1(3) . . . . ?
O2 P1 O3 Mo6 171.4(2) . . . . ?
O2 P1 O4 Mo7 -67.5(3) . . . . ?
O2 P1 O4 Mo8 52.6(3) . . . . ?
O2 P1 O4 Mo9 172.3(2) . . . . ?
O3 Mo5 O8 Mo4 -58.6(5) . . . . ?
O3 Mo5 O9 Mo6 -4.35(19) . . . . ?
O3 Mo5 O15 Mo8 57.0(4) . . . . ?
O3 Mo6 O10 Mo1 50.7(4) . . . . ?
O3 Mo6 O25 Mo15 83.9(7) . . . . ?
O3 P1 O1 Mo1 -58.5(3) . . . . ?
O3 P1 O1 Mo2 170.2(2) . . . . ?
O3 P1 O2 Mo3 177.5(2) . . . . ?
O3 P1 O2 Mo4 46.3(3) . . . . ?
O3 P1 O4 Mo7 172.3(2) . . . . ?
O3 P1 O4 Mo8 -67.6(3) . . . . ?
O3 P1 O4 Mo9 52.0(3) . . . . ?
O4 Mo7 O12 Mo2 49.3(5) . . . . ?
O4 Mo7 O17 Mo9 0.03(19) . . . . ?
O4 Mo8 O14 Mo4 41.7(5) . . . . ?
O4 Mo8 O18 Mo7 -1.41(19) . . . . ?
O4 Mo8 O18 Na1 118.92(18) . . . . ?
O4 Mo9 O16 Mo6 43.5(5) . . . . ?
O4 Mo9 O19 Mo8 -2.0(2) . . . . ?
O4 Mo9 O53 K2 -7.7(11) . . . 2_665 ?
O4 P1 O1 Mo1 58.8(3) . . . . ?
O4 P1 O1 Mo2 -72.4(3) . . . . ?
O4 P1 O2 Mo3 60.0(3) . . . . ?
O4 P1 O2 Mo4 -71.2(3) . . . . ?
O4 P1 O3 Mo5 60.3(3) . . . . ?
O4 P1 O3 Mo6 -71.3(3) . . . . ?
O5 Mo1 O11 Mo9 131.3(4) . . . . ?
O5 Mo2 O6 Mo3 19.9(8) . . . . ?
O5 Mo2 O21 Mo11 150.5(7) . . . . ?
O5 Mo2 O46 Na2 -30.7(2) . . . 2_776 ?
O6 Mo2 O21 Mo11 -6.1(7) . . . . ?
O6 Mo2 O46 Na2 130.42(19) . . . 2_776 ?
O6 Mo3 O7 Mo4 14.0(5) . . . . ?
O6 Mo3 O13 Mo7 -24.5(4) . . . . ?
O6 Mo3 O13 Na1 167.51(18) . . . . ?
O6 Mo3 O47 K1 -7.1(4) . . . . ?
O7 Mo3 O13 Mo7 129.8(4) . . . . ?
O7 Mo3 O13 Na1 -38.25(19) . . . . ?
O7 Mo3 O47 K1 -175.5(4) . . . . ?
O7 Mo4 O23 Mo13 154.8(8) . . . . ?
O7 Mo4 O48 K1 113.99(18) . . . 2_766 ?
O8 Mo4 O23 Mo13 -2.0(8) . . . . ?
O8 Mo4 O48 K1 -82.1(2) . . . 2_766 ?
O8 Mo5 O9 Mo6 19.0(5) . . . . ?
O8 Mo5 O15 Mo8 -25.4(4) . . . . ?
O9 Mo5 O8 Mo4 -81.2(6) . . . . ?
O9 Mo5 O15 Mo8 130.7(4) . . . . ?
O9 Mo6 O10 Mo1 23.7(7) . . . . ?
O9 Mo6 O25 Mo15 156.7(7) . . . . ?
O10 Mo1 O5 Mo2 26.1(5) . . . . ?
O10 Mo1 O11 Mo9 -24.1(4) . . . . ?
O10 Mo6 O25 Mo15 -0.5(8) . . . . ?
O11 Mo1 O5 Mo2 -86.8(2) . . . . ?
O11 Mo9 O16 Mo6 -37.0(5) . . . . ?
O11 Mo9 O19 Mo8 11.8(5) . . . . ?
O11 Mo9 O53 K2 75.5(3) . . . 2_665 ?
O12 Mo2 O6 Mo3 -28.1(5) . . . . ?
O12 Mo2 O21 Mo11 80.3(11) . . . . ?
O12 Mo2 O46 Na2 50.18(19) . . . 2_776 ?
O12 Mo7 O17 Mo9 -84.3(2) . . . . ?
O13 Mo3 O7 Mo4 -89.0(2) . . . . ?
O13 Mo3 O47 K1 84.8(4) . . . . ?
O13 Mo7 O12 Mo2 -32.6(5) . . . . ?
O13 Mo7 O17 Mo9 18.3(5) . . . . ?
O14 Mo4 O23 Mo13 67.2(12) . . . . ?
O14 Mo4 O48 K1 -163.20(18) . . . 2_766 ?
O14 Mo8 O18 Mo7 -86.1(2) . . . . ?
O14 Mo8 O18 Na1 34.2(2) . . . . ?
O15 Mo5 O8 Mo4 28.2(5) . . . . ?
O15 Mo5 O9 Mo6 -89.1(2) . . . . ?
O15 Mo8 O14 Mo4 -39.2(5) . . . . ?
O15 Mo8 O18 Mo7 11.5(5) . . . . ?
O15 Mo8 O18 Na1 131.9(3) . . . . ?
O16 Mo6 O10 Mo1 -28.1(4) . . . . ?
O16 Mo6 O25 Mo15 78.7(11) . . . . ?
O16 Mo9 O19 Mo8 -86.6(2) . . . . ?
O16 Mo9 O53 K2 162.1(3) . . . 2_665 ?
O17 Mo7 O12 Mo2 123.1(5) . . . . ?
O17 Mo9 O16 Mo6 12.7(8) . . . . ?
O17 Mo9 O19 Mo8 69.4(2) . . . . ?
O17 Mo9 O53 K2 -4.6(3) . . . 2_665 ?
O18 Mo7 O12 Mo2 20.5(8) . . . . ?
O18 Mo7 O17 Mo9 72.6(2) . . . . ?
O18 Mo8 O14 Mo4 116.7(5) . . . . ?
O19 Mo8 O14 Mo4 8.8(8) . . . . ?
O19 Mo8 O18 Mo7 70.6(2) . . . . ?
O19 Mo8 O18 Na1 -169.08(17) . . . . ?
O19 Mo9 O16 Mo6 118.6(5) . . . . ?
O19 Mo9 O53 K2 -94.2(3) . . . 2_665 ?
O20 Mo1 O5 Mo2 78.5(2) . . . . ?
O20 Mo1 O11 Mo9 34.4(9) . . . . ?
O20 Mo10 O35 Mo15 139.5(5) . . . . ?
O21 Mo2 O6 Mo3 139.3(5) . . . . ?
O21 Mo2 O46 Na2 -127.47(19) . . . 2_776 ?
O21 Mo11 O31 Mo12 -135.6(5) . . . . ?
O21 Mo11 O37 Mo17 43.3(9) . . . . ?
O21 Mo11 O37 K1 -129.6(6) . . . 2_666 ?
O21 Mo11 O55 K1 126.66(12) . . . 2_666 ?
O22 Mo3 O7 Mo4 74.3(2) . . . . ?
O22 Mo3 O13 Mo7 28.5(8) . . . . ?
O22 Mo3 O13 Na1 -139.5(5) . . . . ?
O22 Mo3 O47 K1 -88.3(4) . . . . ?
O22 Mo12 O31 Mo11 135.1(5) . . . . ?
O23 Mo4 O48 K1 14.7(2) . . . 2_766 ?
O23 Mo13 O32 Mo12 76.6(2) . . . . ?
O23 Mo13 O32 Na1 -120.6(2) . . . 2_766 ?
O23 Mo13 O39 Mo18 29.8(9) . . . . ?
O23 Mo13 O57 K1 -19.6(2) . . . 2_766 ?
O24 Mo5 O8 Mo4 -139.9(5) . . . . ?
O24 Mo5 O9 Mo6 77.3(2) . . . . ?
O24 Mo5 O15 Mo8 34.4(9) . . . . ?
O24 Mo14 O33 Mo13 142.6(4) . . . . ?
O24 Mo14 O58 K2 81.2(3) . . . 2_655 ?
O25 Mo6 O10 Mo1 138.4(4) . . . . ?
O25 Mo15 O34 Mo14 76.6(2) . . . . ?
O25 Mo15 O41 Mo16 31.5(9) . . . . ?
O25 Mo15 O59 K2 128.5(8) . . . . ?
O26 Mo10 O20 Mo1 74.2(7) . . . . ?
O26 Mo10 O35 Mo15 50.0(5) . . . . ?
O26 Mo11 O31 Mo12 -55.3(5) . . . . ?
O26 Mo11 O37 Mo17 60.8(4) . . . . ?
O26 Mo11 O37 K1 -112.12(11) . . . 2_666 ?
O26 Mo11 O55 K1 73.3(9) . . . 2_666 ?
O26 P2 O27 Mo12 45.7(3) . . . . ?
O26 P2 O27 Mo13 177.4(2) . . . . ?
O26 P2 O28 Mo14 171.4(2) . . . . ?
O26 P2 O28 Mo15 -58.5(3) . . . . ?
O26 P2 O29 Mo16 52.5(3) . . . . ?
O26 P2 O29 Mo17 -67.6(3) . . . . ?
O26 P2 O29 Mo18 172.6(2) . . . . ?
O27 Mo12 O22 Mo3 85.0(9) . . . . ?
O27 Mo12 O31 Mo11 47.3(5) . . . . ?
O27 Mo13 O32 Mo12 -4.09(19) . . . . ?
O27 Mo13 O32 Na1 158.7(3) . . . 2_766 ?
O27 Mo13 O39 Mo18 55.1(4) . . . . ?
O27 Mo13 O57 K1 -52.4(10) . . . 2_766 ?
O27 P2 O26 Mo10 171.3(2) . . . . ?
O27 P2 O26 Mo11 -58.2(3) . . . . ?
O27 P2 O28 Mo14 46.7(3) . . . . ?
O27 P2 O28 Mo15 176.8(2) . . . . ?
O27 P2 O29 Mo16 172.4(2) . . . . ?
O27 P2 O29 Mo17 52.3(3) . . . . ?
O27 P2 O29 Mo18 -67.5(3) . . . . ?
O28 Mo14 O24 Mo5 78.4(7) . . . . ?
O28 Mo14 O33 Mo13 54.4(4) . . . . ?
O28 Mo14 O58 K2 -130.1(7) . . . 2_655 ?
O28 Mo15 O34 Mo14 -3.40(19) . . . . ?
O28 Mo15 O41 Mo16 55.9(4) . . . . ?
O28 Mo15 O59 K2 101.0(11) . . . . ?
O28 P2 O26 Mo10 46.5(3) . . . . ?
O28 P2 O26 Mo11 177.0(2) . . . . ?
O28 P2 O27 Mo12 170.4(2) . . . . ?
O28 P2 O27 Mo13 -57.9(3) . . . . ?
O28 P2 O29 Mo16 -67.4(3) . . . . ?
O28 P2 O29 Mo17 172.5(2) . . . . ?
O28 P2 O29 Mo18 52.7(3) . . . . ?
O29 Mo16 O36 Mo10 42.6(5) . . . . ?
O29 Mo16 O42 Mo17 0.2(2) . . . . ?
O29 Mo16 O60 K2 172.2(8) . . . 2 ?
O29 Mo17 O38 Mo12 47.0(5) . . . . ?
O29 Mo17 O43 Mo18 -1.68(19) . . . . ?
O29 Mo17 O61 Na2 172.6(6) . . . 1_445 ?
O29 Mo18 O40 Mo14 44.7(5) . . . . ?
O29 Mo18 O44 Mo16 -2.9(2) . . . . ?
O29 P2 O26 Mo10 -71.1(3) . . . . ?
O29 P2 O26 Mo11 59.4(3) . . . . ?
O29 P2 O27 Mo12 -71.9(3) . . . . ?
O29 P2 O27 Mo13 59.8(3) . . . . ?
O29 P2 O28 Mo14 -70.9(3) . . . . ?
O29 P2 O28 Mo15 59.1(3) . . . . ?
O30 Mo10 O20 Mo1 148.0(7) . . . . ?
O30 Mo10 O35 Mo15 21.0(7) . . . . ?
O30 Mo11 O31 Mo12 -78.0(7) . . . . ?
O30 Mo11 O37 Mo17 133.0(4) . . . . ?
O30 Mo11 O37 K1 -39.94(13) . . . 2_666 ?
O30 Mo11 O55 K1 42.65(13) . . . 2_666 ?
O31 Mo11 O37 Mo17 -22.4(4) . . . . ?
O31 Mo11 O37 K1 164.72(13) . . . 2_666 ?
O31 Mo11 O55 K1 -150.26(12) . . . 2_666 ?
O31 Mo12 O22 Mo3 1.2(9) . . . . ?
O32 Mo12 O22 Mo3 156.9(9) . . . . ?
O32 Mo12 O31 Mo11 18.2(8) . . . . ?
O32 Mo13 O39 Mo18 128.4(4) . . . . ?
O32 Mo13 O57 K1 -103.8(2) . . . 2_766 ?
O33 Mo13 O32 Mo12 23.3(5) . . . . ?
O33 Mo13 O32 Na1 -174.0(3) . . . 2_766 ?
O33 Mo13 O39 Mo18 -27.3(4) . . . . ?
O33 Mo13 O57 K1 60.7(2) . . . 2_766 ?
O33 Mo14 O24 Mo5 -5.4(7) . . . . ?
O33 Mo14 O58 K2 -16.0(3) . . . 2_655 ?
O34 Mo14 O24 Mo5 151.6(7) . . . . ?
O34 Mo14 O33 Mo13 30.6(7) . . . . ?
O34 Mo14 O58 K2 178.1(3) . . . 2_655 ?
O34 Mo15 O41 Mo16 129.4(4) . . . . ?
O34 Mo15 O59 K2 43.8(8) . . . . ?
O35 Mo10 O20 Mo1 -10.4(7) . . . . ?
O35 Mo15 O34 Mo14 21.6(5) . . . . ?
O35 Mo15 O41 Mo16 -26.6(4) . . . . ?
O35 Mo15 O59 K2 -150.5(8) . . . . ?
O36 Mo10 O20 Mo1 67.0(12) . . . . ?
O36 Mo10 O35 Mo15 -29.0(4) . . . . ?
O36 Mo16 O42 Mo17 -83.3(2) . . . . ?
O36 Mo16 O60 K2 -22.4(3) . . . 2 ?
O37 Mo11 O31 Mo12 30.9(5) . . . . ?
O37 Mo11 O55 K1 -55.55(15) . . . 2_666 ?
O37 Mo17 O38 Mo12 -33.7(5) . . . . ?
O37 Mo17 O43 Mo18 14.3(5) . . . . ?
O37 Mo17 O61 Na2 -90.7(3) . . . 1_445 ?
O38 Mo12 O22 Mo3 76.2(11) . . . . ?
O38 Mo12 O31 Mo11 -30.4(5) . . . . ?
O38 Mo17 O43 Mo18 -85.8(2) . . . . ?
O38 Mo17 O61 Na2 -1.8(3) . . . 1_445 ?
O39 Mo13 O32 Mo12 -89.0(2) . . . . ?
O39 Mo13 O32 Na1 73.8(2) . . . 2_766 ?
O39 Mo13 O57 K1 155.4(2) . . . 2_766 ?
O39 Mo18 O40 Mo14 -36.8(5) . . . . ?
O39 Mo18 O44 Mo16 9.3(6) . . . . ?
O40 Mo14 O24 Mo5 71.2(11) . . . . ?
O40 Mo14 O33 Mo13 -24.1(4) . . . . ?
O40 Mo14 O58 K2 -98.6(3) . . . 2_655 ?
O40 Mo18 O44 Mo16 -86.4(2) . . . . ?
O41 Mo15 O34 Mo14 -88.3(2) . . . . ?
O41 Mo15 O59 K2 -56.8(8) . . . . ?
O41 Mo16 O36 Mo10 -38.3(5) . . . . ?
O41 Mo16 O42 Mo17 16.5(5) . . . . ?
O41 Mo16 O60 K2 -108.0(2) . . . 2 ?
O42 Mo16 O36 Mo10 117.6(5) . . . . ?
O42 Mo16 O60 K2 82.9(3) . . . 2 ?
O42 Mo17 O38 Mo12 19.1(8) . . . . ?
O42 Mo17 O43 Mo18 70.7(2) . . . . ?
O42 Mo17 O61 Na2 -171.2(3) . . . 1_445 ?
O43 Mo17 O38 Mo12 120.8(5) . . . . ?
O43 Mo17 O61 Na2 101.0(3) . . . 1_445 ?
O43 Mo18 O40 Mo14 11.5(8) . . . . ?
O43 Mo18 O44 Mo16 69.2(2) . . . . ?
O44 Mo16 O36 Mo10 8.9(8) . . . . ?
O44 Mo16 O42 Mo17 72.4(2) . . . . ?
O44 Mo16 O60 K2 172.6(2) . . . 2 ?
O44 Mo18 O40 Mo14 119.8(5) . . . . ?
O45 Mo1 O5 Mo2 170.5(2) . . . . ?
O45 Mo1 O11 Mo9 -128.2(4) . . . . ?
O46 Mo2 O6 Mo3 -115.2(6) . . . . ?
O46 Mo2 O21 Mo11 -110.7(7) . . . . ?
O47 Mo3 O7 Mo4 167.8(2) . . . . ?
O47 Mo3 O13 Mo7 -127.3(4) . . . . ?
O47 Mo3 O13 Na1 64.6(2) . . . . ?
O48 Mo4 O23 Mo13 -103.5(8) . . . . ?
O49 Mo5 O8 Mo4 129.5(5) . . . . ?
O49 Mo5 O9 Mo6 168.3(2) . . . . ?
O49 Mo5 O15 Mo8 -126.8(4) . . . . ?
O50 Mo6 O10 Mo1 -118.3(5) . . . . ?
O50 Mo6 O25 Mo15 -104.1(7) . . . . ?
O51 Mo7 O12 Mo2 -132.4(5) . . . . ?
O51 Mo7 O17 Mo9 169.1(2) . . . . ?
O52 Mo8 O14 Mo4 -136.7(5) . . . . ?
O52 Mo8 O18 Mo7 167.6(2) . . . . ?
O52 Mo8 O18 Na1 -72.1(2) . . . . ?
O53 Mo9 O16 Mo6 -134.5(5) . . . . ?
O53 Mo9 O19 Mo8 166.7(2) . . . . ?
O54 Mo10 O20 Mo1 -112.8(7) . . . . ?
O54 Mo10 O35 Mo15 -117.0(5) . . . . ?
O55 Mo11 O31 Mo12 132.4(5) . . . . ?
O55 Mo11 O37 Mo17 -127.9(4) . . . . ?
O55 Mo11 O37 K1 59.13(17) . . . 2_666 ?
O56 Mo12 O22 Mo3 -103.3(9) . . . . ?
O56 Mo12 O31 Mo11 -120.0(5) . . . . ?
O57 Mo13 O32 Mo12 167.1(2) . . . . ?
O57 Mo13 O32 Na1 -30.1(3) . . . 2_766 ?
O57 Mo13 O39 Mo18 -129.9(4) . . . . ?
O58 Mo14 O24 Mo5 -107.8(7) . . . . ?
O58 Mo14 O33 Mo13 -114.7(4) . . . . ?
O59 Mo15 O34 Mo14 167.6(2) . . . . ?
O59 Mo15 O41 Mo16 -128.0(4) . . . . ?
O60 Mo16 O36 Mo10 -134.8(5) . . . . ?
O60 Mo16 O42 Mo17 169.4(2) . . . . ?
O61 Mo17 O38 Mo12 -134.1(5) . . . . ?
O61 Mo17 O43 Mo18 167.2(2) . . . . ?
O62 Mo18 O40 Mo14 -133.7(5) . . . . ?
O62 Mo18 O44 Mo16 167.4(2) . . . . ?

_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 -0.004 0.220 0.971 13.1 12.3 ?
2 0.004 0.780 0.029 13.1 12.1 ?
3 0.417 0.769 0.092 31.2 26.6 ?
4 0.293 0.561 0.303 11.0 16.8 ?
5 0.583 0.231 0.908 31.2 26.7 ?
6 0.707 0.439 0.697 11.0 16.5 ?

_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.845

# start Validation Reply Form
_vrf_PLAT094_jcr85_sq_sq         
;
PROBLEM: Ratio of Maximum / Minimum Residual Density .... 8.35 Report
RESPONSE: The residual electron density is attributed to crystal water
molecules, all of which are highly disordered. A solvent mask/SQUEEZE was
applied but does not significantly improve the model.
;
_vrf_PLAT097_jcr85_sq_sq         
;
PROBLEM: Large Reported Max. (Positive) Residual Density 15.06 eA-3
RESPONSE: The residual electron density is attributed to crystal water
molecules, all of which are highly disordered. A solvent mask/SQUEEZE was
applied but does not significantly improve the model.
;
_vrf_PLAT214_jcr85_sq_sq         
;
PROBLEM: Atom O3W (Anion/Solvent) ADP max/min Ratio 8.3 prolat
RESPONSE: O3W is a hydrated water molecule that appears to be highly disordered.
;
_vrf_PLAT971_jcr85_sq_sq         
;
PROBLEM: Check Calcd Resid. Dens. 2.63Ang From Na2 14.18 eA-3
RESPONSE: The residual electron density is attributed to crystal water
molecules, all of which are highly disordered. A solvent mask/SQUEEZE was
applied but does not significantly improve the model.
;
_vrf_PLAT196_jcr85_sq_sq         
;
PROBLEM: No TEMP record and _measurement_temperature .NE. 293 Degree
RESPONSE: The measurement temperature was 100 K.
;
_vrf_PLAT260_jcr85_sq_sq         
;
PROBLEM: Large Average Ueq of Residue Including O3W 0.334 Check
RESPONSE: Atom O3W (Anion/Solvent) ADP max/min Ratio 8.3 prolat
RESPONSE: O3W is a hydrated water molecule that appears to be highly disordered.
;
_vrf_PLAT306_jcr85_sq_sq         
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: The isolated oxygen atom belongs to a crystal water
molecule.
;
_vrf_PLAT910_jcr85_sq_sq         
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 14 Note
RESPONSE: "Missing FCF Reflections below theta-min" is a known
problem of the instrument used. It has already been tried to adjust the beam
stop mask, which did not bring any success so far.
;
_vrf_PLAT975_jcr85_sq_sq         
;
PROBLEM: Check Calcd Resid. Dens. 0.98Ang From O9W . 1.69 eA-3
RESPONSE: The residual electron density is attributed to crystal water
molecules, all of which are highly disordered. A solvent mask/SQUEEZE was
applied but does not significantly improve the model.
;
# end Validation Reply Form
