# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_1_a
_database_code_depnum_ccdc_archive 'CCDC 1862500'
loop_
_audit_author_name
_audit_author_address
'Pavel Abramov'
;Nikolaev Institute of Inorganic Chemistry SB RAS
Russia
;
_audit_update_record             
;
2018-08-17 deposited with the CCDC.	2019-05-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_1_a                 
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info
RESPONSE: Composition of the complex was found from analytical data
;
# Added during the CSD deposition process: Friday 17 August 2018 07:53 AM
# end Validation Reply Form

# Li4.2(NH4)31H[(P8W48O184)(NbO(H2O))3.6(C2O4)3]*64H2O
_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H0 Nb3.68 O238 P8 W48'
_chemical_formula_weight         13222.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 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.
;

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'
'-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                   25.6122(5)
_cell_length_b                   25.6122(5)
_cell_length_c                   22.0939(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14493.3(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    5811
_cell_measurement_theta_min      3.6610
_cell_measurement_theta_max      29.3080

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.030
_exptl_crystal_F_000             11454
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    19.235
_shelx_estimated_absorpt_T_min   0.206
_shelx_estimated_absorpt_T_max   0.446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.52873
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_reflns_number            19190
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.375
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.349
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6795
_reflns_number_gt                4745
_reflns_threshold_expression     >2σ(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0458P)²+505.5680P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6795
_refine_ls_number_parameters     386
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O1 O 0.1932(5) 0.6047(5) 0.500000 0.033(3) Uani 1 2 d S T P . .
O2 O 0.2024(6) 0.5078(5) 0.500000 0.043(4) Uani 1 2 d S T P . .
O3 O 0.2676(4) 0.5619(4) 0.4442(4) 0.036(2) Uani 1 1 d . . . . .
O4 O 0.1153(6) 0.4637(5) 0.500000 0.047(4) Uani 1 2 d S T P . .
O5 O 0.2320(4) 0.5571(4) 0.2736(4) 0.047(3) Uani 1 1 d . . . . .
O6 O 0.3041(5) 0.5115(5) 0.3460(4) 0.069(4) Uani 1 1 d . . . . .
O7 O 0.2013(4) 0.5049(4) 0.3735(4) 0.044(3) Uani 1 1 d . . . . .
O8 O 0.1032(5) 0.4557(4) 0.3743(4) 0.056(3) Uani 1 1 d . . . . .
O9 O 0.1881(5) 0.4165(4) 0.4330(4) 0.057(3) Uani 1 1 d . . . . .
O10 O 0.1492(6) 0.3372(6) 0.500000 0.046(4) Uani 1 2 d S T P . .
O27 O 0.1328(5) 0.2321(6) 0.3129(5) 0.074(4) Uani 1 1 d . . . . .
O11 O 0.2458(6) 0.3439(5) 0.500000 0.039(4) Uani 1 2 d S T P . .
O12 O 0.1347(4) 0.3384(4) 0.3751(4) 0.050(3) Uani 1 1 d . . . . .
O13 O 0.2445(4) 0.3462(4) 0.3739(4) 0.043(3) Uani 1 1 d . . . . .
O14 O 0.3367(6) 0.3920(4) 0.3461(5) 0.072(4) Uani 1 1 d . . . . .
O15 O 0.2965(4) 0.3168(4) 0.2732(4) 0.047(3) Uani 1 1 d . . . . .
O16 O 0.3809(4) 0.2945(4) 0.3427(4) 0.048(3) Uani 1 1 d . . . . .
O17 O 0.3301(4) 0.3306(3) 0.4439(4) 0.036(2) Uani 1 1 d . . . . .
O18 O 0.2884(4) 0.2539(3) 0.3731(4) 0.032(2) Uani 1 1 d . . . . .
O19 O 0.2881(5) 0.2559(5) 0.500000 0.026(3) Uani 1 2 d S T P . .
O20 O 0.2223(5) 0.1846(5) 0.500000 0.031(3) Uani 1 2 d S T P . .
O21 O 0.2138(4) 0.1728(4) 0.3743(4) 0.033(2) Uani 1 1 d . . . . .
O22 O 0.3069(4) 0.1634(3) 0.4323(4) 0.031(2) Uani 1 1 d . . . . .
O23 O 0.3922(4) 0.1912(4) 0.3723(4) 0.036(2) Uani 1 1 d . . . . .
O24 O 0.3667(5) 0.0994(5) 0.500000 0.034(3) Uani 1 2 d S T P . .
O25 O 0.4497(4) 0.1230(4) 0.4289(4) 0.039(2) Uani 1 1 d . . . . .
O26 O 0.3615(4) 0.0865(4) 0.3745(4) 0.041(2) Uani 1 1 d . . . . .
O1W O 0.3532(15) 0.4592(14) 0.4440(16) 0.079(10) Uiso 0.4 1 d . . P . .
O2W O 0.3434(15) 0.4587(15) 0.2491(19) 0.099(12) Uiso 0.4 1 d . . P . .
O3W O 0.3111(18) 0.4497(15) 0.4389(18) 0.053(10) Uiso 0.3 1 d . . P . .
O4W O 0.2047(14) 0.4237(14) 0.2813(16) 0.052(9) Uiso 0.3 1 d . . P . .
O5W O 0.1050(14) 0.3835(13) 0.2568(16) 0.046(9) Uiso 0.3 1 d . . P . .
O6W O 0.3689(11) 0.5736(11) 0.500000 0.065(8) Uiso 0.6 2 d S . P . .
O7W O 0.039(3) 0.370(3) 0.500000 0.05(2) Uiso 0.2 2 d S . P . .
O8W O 0.107(2) 0.212(2) 0.500000 0.071(17) Uiso 0.3 2 d S . P . .
O9W O 0.4576(17) 0.0198(17) 0.500000 0.065(12) Uiso 0.4 2 d S . P . .
O10W O 0.2351(19) 0.0722(18) 0.500000 0.074(13) Uiso 0.4 2 d S . P . .
O11W O 0.2486(17) 0.0725(16) 0.324(2) 0.067(12) Uiso 0.3 1 d . . P . .
O12W O 0.1986(4) 0.2673(4) 0.4294(4) 0.034(2) Uani 1 1 d . . . . .
O13W O 0.1895(5) 0.3081(4) 0.2376(4) 0.056(3) Uani 1 1 d . . . . .
O14W O 0.1446(14) 0.4020(14) 0.2584(16) 0.050(9) Uiso 0.3 1 d . . P . .
O15W O 0.2862(15) 0.4411(14) 0.4583(17) 0.048(10) Uiso 0.3 1 d . . P . .
O16W O 0.0846(19) 0.1331(19) 0.286(2) 0.065(13) Uiso 0.25 1 d . . P . .
O17W O 0.038(2) 0.448(2) 0.205(2) 0.071(14) Uiso 0.25 1 d . . P . .
O18W O 0.027(2) 0.368(2) 0.367(3) 0.078(16) Uiso 0.25 1 d . . P . .
O19W O 0.214(2) 0.082(2) 0.300(3) 0.054(15) Uiso 0.2 1 d . . P . .
O20W O 0.277(4) 0.044(4) 0.500000 0.07(3) Uiso 0.2 2 d S . P . .
O21W O 0.039(3) 0.366(3) 0.464(3) 0.052(19) Uiso 0.15 1 d . . P . .
P1 P 0.2342(2) 0.5598(2) 0.500000 0.0339(13) Uani 1 2 d S T P . .
P2 P 0.3001(2) 0.3155(2) 0.500000 0.0350(13) Uani 1 2 d S T P . .
Nb1 Nb 0.3532(2) 0.4617(2) 0.3644(3) 0.0482(15) Uiso 0.25 1 d . . P . .
Nb2 Nb 0.3499(4) 0.4597(4) 0.3095(5) 0.045(2) Uiso 0.15 1 d . . P . .
Nb3 Nb 0.2480(8) 0.4325(8) 0.3680(9) 0.030(5) Uiso 0.06 1 d . . P . .
W1 W 0.37596(3) 0.13608(2) 0.42449(3) 0.03895(17) Uani 1 1 d . . . . .
W2 W 0.24956(3) 0.21026(2) 0.42431(2) 0.03484(16) Uani 1 1 d . . . . .
W3 W 0.31353(3) 0.32398(3) 0.34765(2) 0.04289(19) Uani 1 1 d . . . . .
W4 W 0.18601(3) 0.34069(3) 0.42468(2) 0.0502(2) Uani 1 1 d . . . . .
W5 W 0.14887(3) 0.47935(3) 0.42474(3) 0.0512(2) Uani 1 1 d . . . . .
W6 W 0.24891(3) 0.56048(3) 0.34805(2) 0.0477(2) 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
O1 P1 1.559(13) . ?
O1 W1 2.273(9) 4_565 ?
O1 W1 2.273(9) 11_566 ?
O2 P1 1.560(16) . ?
O2 W5 2.276(11) . ?
O2 W5 2.276(11) 10_556 ?
O3 P1 1.502(9) . ?
O3 W6 2.177(8) . ?
O4 W5 1.914(8) 10_556 ?
O4 W5 1.914(8) . ?
O5 W6 1.702(9) . ?
O6 Nb1 1.837(12) . ?
O6 W6 1.891(11) . ?
O6 Nb2 1.946(14) . ?
O6 Nb3 2.53(3) . ?
O7 W5 1.875(10) . ?
O7 W6 1.957(11) . ?
O7 Nb3 2.21(2) . ?
O8 W5 1.726(11) . ?
O9 W5 1.906(11) . ?
O9 W4 1.952(11) . ?
O9 Nb3 2.14(2) . ?
O10 W4 1.915(8) . ?
O10 W4 1.915(8) 10_556 ?
O11 P2 1.568(16) . ?
O11 W4 2.264(10) . ?
O11 W4 2.264(10) 10_556 ?
O12 W4 1.713(10) . ?
O13 W4 1.878(10) . ?
O13 W3 1.945(11) . ?
O13 Nb3 2.22(2) . ?
O14 W3 1.841(11) . ?
O14 Nb1 1.877(13) . ?
O14 Nb2 1.942(14) . ?
O14 Nb3 2.55(3) . ?
O15 W3 1.713(9) . ?
O16 W3 1.887(11) . ?
O16 W6 1.906(11) 3_655 ?
O17 P2 1.508(9) . ?
O17 W3 2.175(8) . ?
O18 W2 1.876(8) . ?
O18 W3 1.988(9) . ?
O19 P2 1.559(12) . ?
O19 W2 2.266(8) 10_556 ?
O19 W2 2.266(8) . ?
O20 W2 1.928(6) 10_556 ?
O20 W2 1.928(6) . ?
O21 W2 1.727(8) . ?
O22 W2 1.904(9) . ?
O22 W1 1.910(9) . ?
O23 W1 1.869(9) . ?
O23 W6 1.986(9) 3_655 ?
O24 W1 1.930(6) 10_556 ?
O24 W1 1.930(6) . ?
O25 W1 1.921(10) . ?
O25 W5 1.936(10) 3_655 ?
O26 W1 1.722(9) . ?
O1W O3W 1.11(5) . ?
O1W Nb1 1.76(4) . ?
O1W O15W 1.80(5) . ?
O2W Nb2 1.35(4) . ?
O2W Nb1 2.56(4) . ?
O3W O15W 0.80(4) . ?
O3W Nb1 1.99(5) . ?
O3W Nb3 2.29(5) . ?
O4W O14W 1.71(5) . ?
O4W Nb3 2.22(4) . ?
O5W O14W 1.12(4) . ?
O7W O21W 0.82(7) . ?
O7W O21W 0.82(7) 10_556 ?
O10W O20W 1.29(10) . ?
O11W O19W 1.06(6) . ?
O12W W4 1.910(9) . ?
O12W W2 1.962(9) . ?
O15W Nb3 2.23(4) . ?
O21W O21W 1.61(15) 10_556 ?
Nb1 Nb2 1.215(11) . ?
Nb1 Nb3 2.80(2) . ?
Nb2 Nb3 3.00(2) . ?
Nb3 W5 3.08(2) . ?
Nb3 W4 3.10(2) . ?

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
P1 O1 W1 126.5(4) . 4_565 ?
P1 O1 W1 126.5(4) . 11_566 ?
W1 O1 W1 94.4(5) 4_565 11_566 ?
P1 O2 W5 126.0(4) . . ?
P1 O2 W5 126.0(4) . 10_556 ?
W5 O2 W5 93.9(6) . 10_556 ?
P1 O3 W6 132.5(6) . . ?
W5 O4 W5 120.6(9) 10_556 . ?
Nb1 O6 W6 165.4(6) . . ?
Nb1 O6 Nb2 37.3(4) . . ?
W6 O6 Nb2 155.9(7) . . ?
Nb1 O6 Nb3 77.9(7) . . ?
W6 O6 Nb3 95.8(7) . . ?
Nb2 O6 Nb3 82.9(7) . . ?
W5 O7 W6 150.9(5) . . ?
W5 O7 Nb3 97.3(7) . . ?
W6 O7 Nb3 104.9(7) . . ?
W5 O9 W4 144.7(7) . . ?
W5 O9 Nb3 98.8(7) . . ?
W4 O9 Nb3 98.4(7) . . ?
W4 O10 W4 120.7(8) . 10_556 ?
P2 O11 W4 125.7(4) . . ?
P2 O11 W4 125.7(4) . 10_556 ?
W4 O11 W4 94.6(6) . 10_556 ?
W4 O13 W3 151.8(5) . . ?
W4 O13 Nb3 98.2(7) . . ?
W3 O13 Nb3 103.8(7) . . ?
W3 O14 Nb1 165.4(7) . . ?
W3 O14 Nb2 155.3(7) . . ?
Nb1 O14 Nb2 37.1(4) . . ?
W3 O14 Nb3 95.4(7) . . ?
Nb1 O14 Nb3 76.8(7) . . ?
Nb2 O14 Nb3 82.6(7) . . ?
W3 O16 W6 164.2(6) . 3_655 ?
P2 O17 W3 133.2(6) . . ?
W2 O18 W3 151.6(5) . . ?
P2 O19 W2 126.2(4) . 10_556 ?
P2 O19 W2 126.2(4) . . ?
W2 O19 W2 95.1(4) 10_556 . ?
W2 O20 W2 120.3(6) 10_556 . ?
W2 O22 W1 159.5(5) . . ?
W1 O23 W6 149.8(5) . 3_655 ?
W1 O24 W1 119.7(7) 10_556 . ?
W1 O25 W5 149.4(6) . 3_655 ?
O3W O1W Nb1 85(3) . . ?
O3W O1W O15W 16(3) . . ?
Nb1 O1W O15W 101(2) . . ?
Nb2 O2W Nb1 1.6(10) . . ?
O15W O3W O1W 141(6) . . ?
O15W O3W Nb1 157(5) . . ?
O1W O3W Nb1 62(3) . . ?
O15W O3W Nb3 76(4) . . ?
O1W O3W Nb3 143(4) . . ?
Nb1 O3W Nb3 81.2(15) . . ?
O14W O4W Nb3 137(2) . . ?
O21W O7W O21W 163(10) . 10_556 ?
W4 O12W W2 147.3(5) . . ?
O5W O14W O4W 164(4) . . ?
O3W O15W O1W 23(4) . . ?
O3W O15W Nb3 84(4) . . ?
O1W O15W Nb3 107(2) . . ?
O7W O21W O21W 9(9) . 10_556 ?
O3 P1 O3 110.5(8) 10_556 . ?
O3 P1 O1 111.0(5) 10_556 . ?
O3 P1 O1 110.9(5) . . ?
O3 P1 O2 109.1(5) 10_556 . ?
O3 P1 O2 109.1(5) . . ?
O1 P1 O2 106.2(8) . . ?
O17 P2 O17 110.5(8) . 10_556 ?
O17 P2 O19 110.5(5) . . ?
O17 P2 O19 110.5(5) 10_556 . ?
O17 P2 O11 109.5(5) . . ?
O17 P2 O11 109.5(5) 10_556 . ?
O19 P2 O11 106.2(8) . . ?
Nb2 Nb1 O1W 174.1(14) . . ?
Nb2 Nb1 O6 76.2(6) . . ?
O1W Nb1 O6 104.2(12) . . ?
Nb2 Nb1 O14 74.4(6) . . ?
O1W Nb1 O14 100.4(12) . . ?
O6 Nb1 O14 117.4(7) . . ?
Nb2 Nb1 O3W 141.3(14) . . ?
O1W Nb1 O3W 33.7(14) . . ?
O6 Nb1 O3W 85.4(12) . . ?
O14 Nb1 O3W 84.8(12) . . ?
Nb2 Nb1 O2W 1.8(11) . . ?
O1W Nb1 O2W 173.3(16) . . ?
O6 Nb1 O2W 74.6(10) . . ?
O14 Nb1 O2W 74.7(10) . . ?
O3W Nb1 O2W 139.9(15) . . ?
Nb2 Nb1 Nb3 87.2(7) . . ?
O1W Nb1 Nb3 87.8(13) . . ?
O6 Nb1 Nb3 62.2(7) . . ?
O14 Nb1 Nb3 62.4(7) . . ?
O3W Nb1 Nb3 54.1(13) . . ?
O2W Nb1 Nb3 85.8(10) . . ?
Nb1 Nb2 O2W 177(2) . . ?
Nb1 Nb2 O14 68.6(6) . . ?
O2W Nb2 O14 112.0(19) . . ?
Nb1 Nb2 O6 66.5(6) . . ?
O2W Nb2 O6 110.4(18) . . ?
O14 Nb2 O6 109.4(7) . . ?
Nb1 Nb2 Nb3 68.9(7) . . ?
O2W Nb2 Nb3 108.4(18) . . ?
O14 Nb2 Nb3 57.4(6) . . ?
O6 Nb2 Nb3 57.0(6) . . ?
O9 Nb3 O7 74.7(8) . . ?
O9 Nb3 O13 75.0(8) . . ?
O7 Nb3 O13 144.3(11) . . ?
O9 Nb3 O4W 101.7(13) . . ?
O7 Nb3 O4W 82.2(12) . . ?
O13 Nb3 O4W 86.0(12) . . ?
O9 Nb3 O15W 74.5(13) . . ?
O7 Nb3 O15W 96.0(12) . . ?
O13 Nb3 O15W 93.6(12) . . ?
O4W Nb3 O15W 176.1(18) . . ?
O9 Nb3 O3W 94.7(14) . . ?
O7 Nb3 O3W 100.5(13) . . ?
O13 Nb3 O3W 100.3(13) . . ?
O4W Nb3 O3W 163.5(18) . . ?
O15W Nb3 O3W 20.3(11) . . ?
O9 Nb3 O6 133.5(10) . . ?
O7 Nb3 O6 69.3(7) . . ?
O13 Nb3 O6 146.3(10) . . ?
O4W Nb3 O6 101.5(12) . . ?
O15W Nb3 O6 81.0(12) . . ?
O3W Nb3 O6 65.0(12) . . ?
O9 Nb3 O14 133.6(10) . . ?
O7 Nb3 O14 146.7(10) . . ?
O13 Nb3 O14 68.9(7) . . ?
O4W Nb3 O14 103.9(12) . . ?
O15W Nb3 O14 79.5(12) . . ?
O3W Nb3 O14 65.1(12) . . ?
O6 Nb3 O14 77.4(7) . . ?
O9 Nb3 Nb1 139.4(10) . . ?
O7 Nb3 Nb1 107.4(8) . . ?
O13 Nb3 Nb1 107.8(8) . . ?
O4W Nb3 Nb1 118.8(12) . . ?
O15W Nb3 Nb1 64.9(12) . . ?
O3W Nb3 Nb1 44.7(12) . . ?
O6 Nb3 Nb1 39.9(4) . . ?
O14 Nb3 Nb1 40.8(4) . . ?
O9 Nb3 Nb2 163.3(10) . . ?
O7 Nb3 Nb2 107.5(8) . . ?
O13 Nb3 Nb2 107.0(8) . . ?
O4W Nb3 Nb2 95.0(12) . . ?
O15W Nb3 Nb2 88.8(13) . . ?
O3W Nb3 Nb2 68.6(13) . . ?
O6 Nb3 Nb2 40.1(4) . . ?
O14 Nb3 Nb2 40.0(4) . . ?
Nb1 Nb3 Nb2 23.9(3) . . ?
O9 Nb3 W5 37.8(4) . . ?
O7 Nb3 W5 37.2(4) . . ?
O13 Nb3 W5 109.4(8) . . ?
O4W Nb3 W5 88.8(11) . . ?
O15W Nb3 W5 87.7(12) . . ?
O3W Nb3 W5 103.2(13) . . ?
O6 Nb3 W5 103.6(7) . . ?
O14 Nb3 W5 166.8(9) . . ?
Nb1 Nb3 W5 134.6(8) . . ?
Nb2 Nb3 W5 143.6(8) . . ?
O9 Nb3 W4 38.5(5) . . ?
O7 Nb3 W4 109.7(8) . . ?
O13 Nb3 W4 36.8(4) . . ?
O4W Nb3 W4 90.9(11) . . ?
O15W Nb3 W4 86.4(12) . . ?
O3W Nb3 W4 103.3(13) . . ?
O6 Nb3 W4 167.1(9) . . ?
O14 Nb3 W4 103.0(7) . . ?
Nb1 Nb3 W4 135.0(8) . . ?
Nb2 Nb3 W4 142.8(8) . . ?
W5 Nb3 W4 73.1(5) . . ?
O26 W1 O23 102.1(4) . . ?
O26 W1 O22 97.5(4) . . ?
O23 W1 O22 89.1(4) . . ?
O26 W1 O25 96.6(4) . . ?
O23 W1 O25 86.8(4) . . ?
O22 W1 O25 165.9(4) . . ?
O26 W1 O24 99.7(5) . . ?
O23 W1 O24 158.2(4) . . ?
O22 W1 O24 89.2(5) . . ?
O25 W1 O24 89.6(5) . . ?
O26 W1 O1 172.4(4) . 3_655 ?
O23 W1 O1 85.3(3) . 3_655 ?
O22 W1 O1 84.2(4) . 3_655 ?
O25 W1 O1 82.0(4) . 3_655 ?
O24 W1 O1 72.9(4) . 3_655 ?
O21 W2 O18 103.1(4) . . ?
O21 W2 O22 96.8(4) . . ?
O18 W2 O22 91.3(4) . . ?
O21 W2 O20 100.0(4) . . ?
O18 W2 O20 156.7(4) . . ?
O22 W2 O20 89.1(5) . . ?
O21 W2 O12W 95.6(4) . . ?
O18 W2 O12W 86.8(4) . . ?
O22 W2 O12W 167.5(4) . . ?
O20 W2 O12W 87.9(5) . . ?
O21 W2 O19 171.9(4) . . ?
O18 W2 O19 84.7(3) . . ?
O22 W2 O19 85.4(4) . . ?
O20 W2 O19 72.2(4) . . ?
O12W W2 O19 82.2(4) . . ?
O15 W3 O14 99.5(5) . . ?
O15 W3 O16 97.8(4) . . ?
O14 W3 O16 94.7(6) . . ?
O15 W3 O13 94.9(5) . . ?
O14 W3 O13 91.3(5) . . ?
O16 W3 O13 164.9(4) . . ?
O15 W3 O18 95.3(4) . . ?
O14 W3 O18 164.7(4) . . ?
O16 W3 O18 87.2(4) . . ?
O13 W3 O18 83.5(4) . . ?
O15 W3 O17 176.0(5) . . ?
O14 W3 O17 83.2(4) . . ?
O16 W3 O17 84.8(4) . . ?
O13 W3 O17 82.1(4) . . ?
O18 W3 O17 81.8(3) . . ?
O15 W3 Nb3 95.3(5) . . ?
O14 W3 Nb3 50.6(6) . . ?
O16 W3 Nb3 144.6(5) . . ?
O13 W3 Nb3 41.0(5) . . ?
O18 W3 Nb3 124.1(5) . . ?
O17 W3 Nb3 84.3(4) . . ?
O12 W4 O13 103.5(5) . . ?
O12 W4 O12W 97.5(4) . . ?
O13 W4 O12W 88.4(4) . . ?
O12 W4 O10 100.2(6) . . ?
O13 W4 O10 156.4(5) . . ?
O12W W4 O10 89.4(5) . . ?
O12 W4 O9 96.6(5) . . ?
O13 W4 O9 87.6(5) . . ?
O12W W4 O9 165.8(4) . . ?
O10 W4 O9 88.8(5) . . ?
O12 W4 O11 172.4(5) . . ?
O13 W4 O11 84.1(4) . . ?
O12W W4 O11 83.2(4) . . ?
O10 W4 O11 72.3(5) . . ?
O9 W4 O11 82.9(5) . . ?
O12 W4 Nb3 99.2(5) . . ?
O13 W4 Nb3 45.0(5) . . ?
O12W W4 Nb3 133.0(5) . . ?
O10 W4 Nb3 129.7(6) . . ?
O9 W4 Nb3 43.0(5) . . ?
O11 W4 Nb3 85.6(5) . . ?
O8 W5 O7 102.6(5) . . ?
O8 W5 O9 97.1(5) . . ?
O7 W5 O9 88.5(5) . . ?
O8 W5 O4 100.6(6) . . ?
O7 W5 O4 156.8(5) . . ?
O9 W5 O4 88.7(5) . . ?
O8 W5 O25 97.4(5) . 4_565 ?
O7 W5 O25 86.9(4) . 4_565 ?
O9 W5 O25 165.5(5) . 4_565 ?
O4 W5 O25 90.1(5) . 4_565 ?
O8 W5 O2 173.3(5) . . ?
O7 W5 O2 84.1(4) . . ?
O9 W5 O2 83.2(5) . . ?
O4 W5 O2 72.7(5) . . ?
O25 W5 O2 82.6(4) 4_565 . ?
O8 W5 Nb3 99.1(5) . . ?
O7 W5 Nb3 45.5(5) . . ?
O9 W5 Nb3 43.4(5) . . ?
O4 W5 Nb3 130.0(6) . . ?
O25 W5 Nb3 131.9(5) 4_565 . ?
O2 W5 Nb3 85.7(5) . . ?
O5 W6 O6 97.6(5) . . ?
O5 W6 O16 97.8(5) . 4_565 ?
O6 W6 O16 93.6(6) . 4_565 ?
O5 W6 O7 94.7(5) . . ?
O6 W6 O7 89.5(5) . . ?
O16 W6 O7 166.6(4) 4_565 . ?
O5 W6 O23 95.9(4) . 4_565 ?
O6 W6 O23 165.5(4) . 4_565 ?
O16 W6 O23 89.5(4) 4_565 4_565 ?
O7 W6 O23 84.4(4) . 4_565 ?
O5 W6 O3 177.1(5) . . ?
O6 W6 O3 82.5(4) . . ?
O16 W6 O3 85.0(4) 4_565 . ?
O7 W6 O3 82.4(4) . . ?
O23 W6 O3 83.7(3) 4_565 . ?

_refine_diff_density_max         1.463
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.245

_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2

