# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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. 
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data_jtm475a_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1040276'
_audit_update_record             
;
2015-03-12 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H25 N3 Nd2 O54 Si W12, 3(H2 O)'
_chemical_formula_sum            'C18 H31 N3 Nd2 O57 Si W12'
_chemical_formula_weight         3724.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   12.6060(19)
_cell_length_b                   12.9593(19)
_cell_length_c                   18.631(3)
_cell_angle_alpha                82.317(2)
_cell_angle_beta                 88.815(2)
_cell_angle_gamma                71.173(2)
_cell_volume                     2854.2(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      2.2077
_cell_measurement_theta_max      26.9234
_cell_measurement_temperature    150.(2)


_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    4.333
_exptl_crystal_F_000             3276
_exptl_transmission_factor_min   0.391
_exptl_transmission_factor_max   0.745
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    26.000
_shelx_estimated_absorpt_T_min   0.191
_shelx_estimated_absorpt_T_max   0.624
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_T_max  0.62

_exptl_special_details           
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5° in ω, colllected at φ = 0.00,
90.00 and 180.00° and 2 sets of 800 frames, each of
width 0.45° in φ, collected at ω = --30.00 and 210.00°.
The scan time was 40 sec/frame.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean 8.3660

_diffrn_reflns_number            44800
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.675
_diffrn_reflns_theta_max         26.940
_diffrn_reflns_theta_full        26.940
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             12254
_reflns_number_gt                8616
_reflns_threshold_expression     'I > 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       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2012)'
_computing_publication_material  'SHELXTL (Bruker, 2014)'

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms attached to carbon
were placed in calculated positions (C---H = 0.95 Å) and were included
as riding contributions with isotropic displacement parameters 1.2 times
those of the attached atoms. Location of H-atoms attached to oxygen atoms 
of  water proved impossible so those were placed in idealized positions 
so as to generate a reasonable hydrogen bonding network without occasioning 
unreasonably short H...H contacts and were included as riding contributions. 
In order to have charge balance it is assumed that the anion is 
[H₂W₁₂SiO₄₀]²⁻ with these two H-atoms placed arbitrarily on two 
bridging oxygens subject to the restraints noted above. N1 is disordered over
the two sites ortho to the substituents in the ring built on C2
while N3 is disordered over the ortho and meta positions
of the ring built on C14. Because the light atoms represent a small
percentage of the total scattering material, significant ISOR restraints
were required to permit their reasonable refinement. Residual density in
the close vicinity of the metal atoms could not be successfully interpreted
as disorder and is therefore attributed to inadequacies in the absorption
correction due to the very large absorption coefficient and difficulties in
accurately determining the thickness of the very thin, plate-like crystal.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0776P)²+136.1817P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12254
_refine_ls_number_parameters     832
_refine_ls_number_restraints     504
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.1747
_refine_ls_wR_factor_gt          0.1483
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.014
_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
Nd1 Nd 0.34548(9) 0.35566(9) 0.66788(6) 0.0106(2) Uani 1 1 d . . . . .
Nd2 Nd 0.42377(9) 0.35700(9) 0.89106(6) 0.0111(2) Uani 1 1 d . . . . .
O1 O 0.2504(13) 0.2241(12) 0.7310(8) 0.017(3) Uani 1 1 d . U . . .
O2 O 0.3529(12) 0.2780(11) 0.8030(8) 0.011(3) Uani 1 1 d . U . . .
O3 O 0.2957(12) 0.2697(12) 0.9470(8) 0.016(3) Uani 1 1 d . U . . .
O4 O 0.4591(14) 0.3339(14) 0.5550(9) 0.026(4) Uani 1 1 d . U . . .
H4A H 0.4699 0.3918 0.5353 0.031 Uiso 1 1 d R U . . .
H4B H 0.4367 0.3032 0.5243 0.031 Uiso 1 1 d R U . . .
O5 O 0.2403(14) 0.2810(14) 0.5896(9) 0.026(4) Uani 1 1 d . U . . .
H5A H 0.2433 0.2149 0.5993 0.031 Uiso 1 1 d R U . . .
H5B H 0.2388 0.2996 0.5446 0.031 Uiso 1 1 d R U . . .
O6 O 0.2317(14) 0.4997(14) 0.5727(9) 0.026(4) Uani 1 1 d . U . . .
H6A H 0.1992 0.5627 0.5840 0.031 Uiso 1 1 d R U . . .
H6B H 0.1903 0.4819 0.5453 0.031 Uiso 1 1 d R U . . .
O7 O 0.3529(12) 0.5421(12) 0.6743(8) 0.016(3) Uani 1 1 d . U . . .
O8 O 0.3703(12) 0.5039(12) 0.7938(8) 0.015(3) Uani 1 1 d . U . . .
O9 O 0.5324(12) 0.3425(12) 0.7022(8) 0.017(3) Uani 1 1 d . U . . .
O10 O 0.5874(12) 0.3209(12) 0.8180(8) 0.014(3) Uani 1 1 d . U . . .
O11 O 0.5512(13) 0.4723(12) 0.9144(8) 0.018(3) Uani 1 1 d . U . . .
H11A H 0.5694 0.4983 0.8741 0.022 Uiso 1 1 d R U . . .
H11B H 0.6119 0.4288 0.9334 0.022 Uiso 1 1 d R U . . .
O12 O 0.2614(12) 0.5073(12) 0.9256(8) 0.016(3) Uani 1 1 d . U . . .
H12A H 0.2224 0.4938 0.9604 0.019 Uiso 1 1 d R U . . .
H12B H 0.2209 0.5533 0.8929 0.019 Uiso 1 1 d R U . . .
O13 O 0.4603(14) 0.3512(13) 1.0190(9) 0.022(4) Uani 1 1 d . U . . .
H13A H 0.4242 0.4013 1.0430 0.026 Uiso 1 1 d R U . . .
H13B H 0.4895 0.2921 1.0465 0.026 Uiso 1 1 d R U . . .
O14 O 0.5392(14) 0.1640(13) 0.9368(9) 0.024(4) Uani 1 1 d . U . . .
N1 N 0.1774(18) 0.1767(17) 0.9834(11) 0.020(4) Uani 0.5 1 d . U P A 1
N1A N 0.1522(18) 0.1339(18) 0.8437(12) 0.022(5) Uani 0.5 1 d . U P B 2
N2 N 0.3094(15) 0.8696(15) 0.6797(10) 0.016(4) Uani 1 1 d . U . . .
C1 C 0.2801(19) 0.2292(19) 0.7925(13) 0.019(5) Uani 1 1 d . U . . .
C2 C 0.2217(17) 0.1900(16) 0.8566(11) 0.011(4) Uani 1 1 d . U . . .
C3 C 0.1522(18) 0.1339(18) 0.8437(12) 0.022(5) Uani 0.5 1 d . U P B 1
H3 H 0.1411 0.1219 0.7964 0.027 Uiso 0.5 1 d R U P B 1
C3A C 0.1774(18) 0.1767(17) 0.9834(11) 0.020(4) Uani 0.5 1 d . U P A 2
H3A H 0.1850 0.1908 1.0314 0.024 Uiso 0.5 1 calc R U P A 2
C4 C 0.0930(19) 0.0940(19) 0.9028(12) 0.020(5) Uani 1 1 d . U . . .
H4 H 0.0464 0.0516 0.8947 0.023 Uiso 1 1 d R U . B .
C5 C 0.107(2) 0.118(2) 0.9693(15) 0.030(6) Uani 1 1 d . U . . .
H5 H 0.0672 0.0938 1.0082 0.036 Uiso 1 1 d R U . A .
C6 C 0.2371(18) 0.2156(18) 0.9278(12) 0.015(4) Uani 1 1 d . U . . .
C7 C 0.3555(18) 0.5706(17) 0.7338(12) 0.014(4) Uani 1 1 d . U . . .
C8 C 0.3403(17) 0.6904(17) 0.7403(11) 0.012(4) Uani 1 1 d . U . . .
C9 C 0.3401(19) 0.7290(19) 0.8067(13) 0.019(5) Uani 1 1 d . U . . .
H9 H 0.3464 0.6817 0.8511 0.023 Uiso 1 1 calc R U . . .
C10 C 0.330(2) 0.840(2) 0.8058(13) 0.022(5) Uani 1 1 d . U . . .
H10 H 0.3344 0.8676 0.8500 0.027 Uiso 1 1 calc R U . . .
C11 C 0.315(2) 0.908(2) 0.7421(13) 0.023(5) Uani 1 1 d . U . . .
H11 H 0.3089 0.9830 0.7420 0.028 Uiso 1 1 calc R U . . .
C12 C 0.3233(18) 0.7636(18) 0.6777(12) 0.018(5) Uani 1 1 d . U . . .
H12 H 0.3215 0.7383 0.6323 0.021 Uiso 1 1 calc R U . . .
C13 C 0.6029(17) 0.3285(16) 0.7524(11) 0.010(4) Uani 1 1 d . U . . .
C14 C 0.7202(17) 0.3183(17) 0.7278(11) 0.013(4) Uani 1 1 d . U . . .
N3 N 0.8033(17) 0.3289(17) 0.7718(11) 0.016(4) Uani 0.25 1 d . U P C 1
C15 C 0.8033(17) 0.3289(17) 0.7718(11) 0.016(4) Uani 0.75 1 d . U P C 2
H15 H 0.7857 0.3396 0.8206 0.020 Uiso 0.75 1 calc R U P C 2
N3A N 0.9053(18) 0.3251(17) 0.7500(12) 0.017(4) Uani 0.25 1 d . U P C 1
C16 C 0.9053(18) 0.3251(17) 0.7500(12) 0.017(4) Uani 0.75 1 d . U P C 2
H16 H 0.9574 0.3375 0.7811 0.020 Uiso 0.75 1 calc R U P C 2
C17 C 0.9343(19) 0.3011(18) 0.6758(12) 0.018(5) Uani 1 1 d . U . . .
H17 H 1.0069 0.2943 0.6577 0.022 Uiso 1 1 calc R U . C 1
N3B N 0.8555(18) 0.2892(17) 0.6352(12) 0.017(4) Uani 0.25 1 d . U P C 1
C18 C 0.8555(18) 0.2892(17) 0.6352(12) 0.017(4) Uani 0.75 1 d . U P C 2
H18 H 0.8740 0.2741 0.5871 0.021 Uiso 0.75 1 calc R U P C 2
N3C N 0.7509(18) 0.2970(17) 0.6567(11) 0.017(4) Uani 0.25 1 d . U P C 1
C19 C 0.7509(18) 0.2970(17) 0.6567(11) 0.017(4) Uani 0.75 1 d . U P C 2
H19 H 0.6983 0.2882 0.6242 0.020 Uiso 0.75 1 calc R U P C 2
W1 W 0.58656(7) 0.05034(7) 0.70169(5) 0.01243(19) Uani 1 1 d . . . . .
W2 W 0.62145(7) -0.13397(7) 0.84975(5) 0.01370(19) Uani 1 1 d . . . . .
W3 W 0.78845(7) 0.02422(7) 0.82428(5) 0.01426(19) Uani 1 1 d . . . . .
W4 W 0.79510(8) 0.00555(8) 0.55889(5) 0.0206(2) Uani 1 1 d . . . . .
W5 W 0.61389(8) -0.16997(7) 0.58945(5) 0.0164(2) Uani 1 1 d . . . . .
W6 W 0.65572(8) -0.35504(7) 0.73783(5) 0.0165(2) Uani 1 1 d . . . . .
W7 W 0.87421(7) -0.38331(7) 0.87433(5) 0.01485(19) Uani 1 1 d . . . . .
W8 W 1.03772(7) -0.22298(7) 0.84493(5) 0.01358(19) Uani 1 1 d . . . . .
W9 W 0.99691(8) -0.01902(7) 0.67999(5) 0.0164(2) Uani 1 1 d . . . . .
W10 W 1.02180(8) -0.21679(7) 0.57764(5) 0.0160(2) Uani 1 1 d . . . . .
W11 W 0.84363(8) -0.39379(7) 0.60680(5) 0.0169(2) Uani 1 1 d . . . . .
W12 W 1.06075(7) -0.42236(7) 0.74168(5) 0.01168(18) Uani 1 1 d . . . . .
Si1 Si 0.8244(4) -0.1867(4) 0.7156(3) 0.002 Uiso 1 1 d . U . . .
O15 O 0.4714(12) 0.1635(12) 0.6725(8) 0.014(3) Uani 1 1 d . U . . .
O16 O 0.5290(12) -0.1409(12) 0.9182(8) 0.015(3) Uani 1 1 d . U . . .
O17 O 0.8031(12) 0.1166(11) 0.8774(8) 0.012(3) Uani 1 1 d . U . . .
O18 O 0.7463(13) 0.1017(12) 0.4853(8) 0.018(3) Uani 1 1 d . U . . .
O19 O 0.5116(12) -0.1325(12) 0.5233(8) 0.016(3) Uani 1 1 d . U . . .
O20 O 0.5782(12) -0.4351(12) 0.7710(8) 0.015(3) Uani 1 1 d . U . . .
O21 O 0.8598(12) -0.4673(12) 0.9491(8) 0.017(3) Uani 1 1 d . U . . .
O22 O 1.1338(12) -0.2105(11) 0.9041(8) 0.014(3) Uani 1 1 d . U . . .
O23 O 1.0801(13) 0.0603(12) 0.6863(8) 0.018(3) Uani 1 1 d . U . . .
O24 O 1.1211(13) -0.2677(12) 0.5178(8) 0.018(3) Uani 1 1 d . U . . .
O25 O 0.8829(13) -0.4948(12) 0.5529(8) 0.017(3) Uani 1 1 d . U . . .
O26 O 1.1724(12) -0.5353(12) 0.7306(8) 0.016(3) Uani 1 1 d . U . . .
O27 O 0.6606(12) 0.1102(12) 0.7656(8) 0.014(3) Uani 1 1 d . U . . .
O28 O 0.6902(12) 0.0643(12) 0.6296(8) 0.013(3) Uani 1 1 d . U . . .
O29 O 0.5613(12) -0.0565(11) 0.6497(7) 0.011(3) Uani 1 1 d . U . . .
H29 H 0.4899 -0.0340 0.6422 0.013 Uiso 1 1 d R U . . .
O30 O 0.5251(11) -0.0120(11) 0.7851(7) 0.008(3) Uani 1 1 d . U . . .
O31 O 0.6854(12) -0.0320(11) 0.8846(8) 0.012(3) Uani 1 1 d . U . . .
O32 O 0.7542(12) -0.2517(11) 0.8849(8) 0.012(3) Uani 1 1 d . U . . .
O33 O 0.5983(11) -0.2333(11) 0.7899(7) 0.009(3) Uani 1 1 d . U . . .
O34 O 0.8810(12) 0.0394(12) 0.7454(8) 0.013(3) Uani 1 1 d . U . . .
O35 O 0.9052(12) -0.1040(12) 0.8612(8) 0.016(3) Uani 1 1 d . U . . .
O36 O 0.9007(12) 0.0618(11) 0.6018(8) 0.012(3) Uani 1 1 d . U . . .
H36 H 0.9294 0.0956 0.5695 0.015 Uiso 1 1 d R U . . .
O37 O 0.9216(12) -0.0961(12) 0.5192(8) 0.016(3) Uani 1 1 d . U . . .
O38 O 0.7115(11) -0.0894(11) 0.5499(7) 0.010(3) Uani 1 1 d . U . . .
O39 O 0.7142(11) -0.2970(11) 0.5526(7) 0.009(3) Uani 1 1 d . U . . .
O40 O 0.5642(11) -0.2672(11) 0.6573(7) 0.010(3) Uani 1 1 d . U . . .
O41 O 0.7399(12) -0.4427(12) 0.6705(8) 0.013(3) Uani 1 1 d . U . . .
O42 O 0.7745(11) -0.4051(11) 0.8058(7) 0.011(3) Uani 1 1 d . U . . .
O43 O 0.9959(12) -0.4784(12) 0.8279(8) 0.014(3) Uani 1 1 d . U . . .
O44 O 0.9740(12) -0.3178(12) 0.9087(8) 0.014(3) Uani 1 1 d . U . . .
O45 O 1.1290(11) -0.3538(11) 0.8064(7) 0.011(3) Uani 1 1 d . U . . .
O46 O 1.0564(12) -0.1344(12) 0.7620(8) 0.014(3) Uani 1 1 d . U . . .
O47 O 1.0825(12) -0.1191(12) 0.6180(8) 0.016(3) Uani 1 1 d . U . . .
O48 O 0.9260(11) -0.3019(11) 0.5692(7) 0.008(3) Uani 1 1 d . U . . .
O49 O 1.0795(12) -0.3231(12) 0.6647(8) 0.013(3) Uani 1 1 d . U . . .
O50 O 0.9494(12) -0.4449(11) 0.6844(8) 0.011(3) Uani 1 1 d . U . . .
O51 O 0.7355(11) -0.0948(10) 0.7585(7) 0.006(3) Uani 1 1 d . U . . .
O52 O 0.9172(10) -0.2732(10) 0.7744(7) 0.004(3) Uani 1 1 d . U . . .
O53 O 0.7587(11) -0.2535(10) 0.6761(7) 0.007(3) Uani 1 1 d . U . . .
O54 O 0.8866(11) -0.1261(10) 0.6558(7) 0.007(3) Uani 1 1 d . U . . .
O55 O 0.7379(15) 0.3055(15) 0.9567(10) 0.033(4) Uani 1 1 d . U . . .
H55A H 0.7456 0.2465 0.9400 0.040 Uiso 1 1 d R U . . .
H55B H 0.7711 0.2855 0.9974 0.040 Uiso 1 1 d R U . . .
O56 O 0.3232(17) 0.0543(17) 0.6009(12) 0.044(5) Uani 1 1 d . U . . .
H56A H 0.3053 -0.0008 0.6184 0.053 Uiso 1 1 d R U . . .
H56B H 0.3277 0.0578 0.5556 0.053 Uiso 1 1 d R U . . .
O57 O 0.4282(17) 0.4702(16) 0.4295(11) 0.041(5) Uani 1 1 d . U . . .
H57A H 0.3696 0.4607 0.4152 0.049 Uiso 1 1 d R U . . .
H57B H 0.4595 0.4962 0.3947 0.049 Uiso 1 1 d R U . . .


_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
Nd1 O9 2.401(15) . ?
Nd1 O7 2.467(15) . ?
Nd1 O5 2.470(17) . ?
Nd1 O15 2.475(14) . ?
Nd1 O6 2.486(17) . ?
Nd1 O4 2.515(17) . ?
Nd1 O1 2.540(15) . ?
Nd1 O26 2.543(15) 1_465 ?
Nd1 O2 2.575(14) . ?
Nd2 O2 2.375(14) . ?
Nd2 O8 2.379(14) . ?
Nd2 O10 2.400(14) . ?
Nd2 O3 2.401(14) . ?
Nd2 O13 2.424(16) . ?
Nd2 O12 2.471(15) . ?
Nd2 O14 2.497(16) . ?
Nd2 O11 2.599(15) . ?
O1 C1 1.23(3) . ?
O2 C1 1.30(3) . ?
O3 C6 1.26(3) . ?
O4 H4A 0.8401 . ?
O4 H4B 0.8400 . ?
O5 H5A 0.8400 . ?
O5 H5B 0.8400 . ?
O6 H6A 0.8404 . ?
O6 H6B 0.8403 . ?
O7 C7 1.22(3) . ?
O8 C7 1.30(2) . ?
O9 C13 1.26(2) . ?
O10 C13 1.23(2) . ?
O11 H11A 0.8400 . ?
O11 H11B 0.8414 . ?
O12 H12A 0.8400 . ?
O12 H12B 0.8401 . ?
O13 H13A 0.8400 . ?
O13 H13B 0.8400 . ?
N1 C5 1.39(3) . ?
N1 C6 1.40(3) . ?
N1A C2 1.35(3) . ?
N1A C4 1.45(3) . ?
N2 C12 1.33(3) . ?
N2 C11 1.34(3) . ?
C1 C2 1.51(3) . ?
C2 C3 1.35(3) . ?
C2 C6 1.44(3) . ?
C3 C4 1.45(3) . ?
C3 H3 0.9369 . ?
C3A C5 1.39(3) . ?
C3A C6 1.40(3) . ?
C3A H3A 0.9500 . ?
C4 C5 1.35(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9501 . ?
C7 C8 1.52(3) . ?
C8 C12 1.37(3) . ?
C8 C9 1.40(3) . ?
C9 C10 1.40(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.36(3) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.51(3) . ?
C14 C15 1.40(3) . ?
C14 N3 1.40(3) . ?
C14 C19 1.41(3) . ?
C14 N3C 1.41(3) . ?
N3 N3A 1.33(3) . ?
C15 C16 1.33(3) . ?
C15 H15 0.9500 . ?
N3A C17 1.47(3) . ?
C16 C17 1.47(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.32(3) . ?
C17 N3B 1.32(3) . ?
C17 H17 0.9500 . ?
N3B N3C 1.35(3) . ?
C18 C19 1.35(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
W1 O15 1.732(15) . ?
W1 O28 1.886(14) . ?
W1 O29 1.901(14) . ?
W1 O27 1.911(14) . ?
W1 O30 1.920(13) . ?
W1 O51 2.336(13) . ?
W2 O16 1.723(14) . ?
W2 O33 1.903(14) . ?
W2 O32 1.920(14) . ?
W2 O30 1.933(13) . ?
W2 O31 1.938(14) . ?
W2 O51 2.314(13) . ?
W3 O17 1.707(14) . ?
W3 O35 1.886(15) . ?
W3 O34 1.887(14) . ?
W3 O27 1.904(15) . ?
W3 O31 1.953(14) . ?
W3 O51 2.351(13) . ?
W4 O18 1.701(15) . ?
W4 O38 1.885(13) . ?
W4 O28 1.901(14) . ?
W4 O37 1.919(15) . ?
W4 O36 1.942(14) . ?
W4 O54 2.344(13) . ?
W5 O19 1.709(15) . ?
W5 O40 1.905(13) . ?
W5 O29 1.909(14) . ?
W5 O39 1.924(14) . ?
W5 O38 1.932(13) . ?
W5 O53 2.343(13) . ?
W6 O20 1.694(14) . ?
W6 O42 1.870(14) . ?
W6 O41 1.881(14) . ?
W6 O33 1.897(14) . ?
W6 O40 1.909(14) . ?
W6 O53 2.319(12) . ?
W7 O21 1.693(15) . ?
W7 O44 1.892(14) . ?
W7 O43 1.905(15) . ?
W7 O32 1.911(14) . ?
W7 O42 1.918(14) . ?
W7 O52 2.354(12) . ?
W8 O22 1.714(14) . ?
W8 O46 1.856(14) . ?
W8 O35 1.924(15) . ?
W8 O45 1.935(14) . ?
W8 O44 1.944(14) . ?
W8 O52 2.326(12) . ?
W9 O23 1.704(15) . ?
W9 O36 1.880(14) . ?
W9 O47 1.905(15) . ?
W9 O34 1.911(14) . ?
W9 O46 1.961(15) . ?
W9 O54 2.346(13) . ?
W10 O24 1.688(15) . ?
W10 O37 1.886(15) . ?
W10 O48 1.901(13) . ?
W10 O47 1.912(15) . ?
W10 O49 1.966(14) . ?
W10 O54 2.339(13) . ?
W11 O25 1.697(16) . ?
W11 O48 1.879(13) . ?
W11 O50 1.887(14) . ?
W11 O39 1.914(13) . ?
W11 O41 1.947(14) . ?
W11 O53 2.331(13) . ?
W12 O26 1.705(15) . ?
W12 O49 1.858(14) . ?
W12 O50 1.898(14) . ?
W12 O43 1.947(14) . ?
W12 O45 1.951(14) . ?
W12 O52 2.323(13) . ?
Si1 O54 1.613(13) . ?
Si1 O53 1.623(14) . ?
Si1 O51 1.634(14) . ?
Si1 O52 1.644(13) . ?
O26 Nd1 2.543(15) 1_645 ?
O29 H29 0.8600 . ?
O36 H36 0.8404 . ?
O55 H55A 0.8404 . ?
O55 H55B 0.8405 . ?
O56 H56A 0.8408 . ?
O56 H56B 0.8404 . ?
O57 H57A 0.8403 . ?
O57 H57B 0.8403 . ?

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
O9 Nd1 O7 71.0(5) . . ?
O9 Nd1 O5 142.3(5) . . ?
O7 Nd1 O5 133.5(5) . . ?
O9 Nd1 O15 69.8(5) . . ?
O7 Nd1 O15 140.4(5) . . ?
O5 Nd1 O15 79.0(5) . . ?
O9 Nd1 O6 122.9(5) . . ?
O7 Nd1 O6 65.4(5) . . ?
O5 Nd1 O6 68.1(5) . . ?
O15 Nd1 O6 135.9(5) . . ?
O9 Nd1 O4 73.4(5) . . ?
O7 Nd1 O4 93.5(5) . . ?
O5 Nd1 O4 76.5(5) . . ?
O15 Nd1 O4 70.0(5) . . ?
O6 Nd1 O4 74.3(6) . . ?
O9 Nd1 O1 121.1(5) . . ?
O7 Nd1 O1 139.0(5) . . ?
O5 Nd1 O1 63.4(5) . . ?
O15 Nd1 O1 69.9(5) . . ?
O6 Nd1 O1 116.1(5) . . ?
O4 Nd1 O1 127.3(5) . . ?
O9 Nd1 O26 122.9(5) . 1_465 ?
O7 Nd1 O26 70.6(5) . 1_465 ?
O5 Nd1 O26 94.5(5) . 1_465 ?
O15 Nd1 O26 138.9(5) . 1_465 ?
O6 Nd1 O26 74.1(5) . 1_465 ?
O4 Nd1 O26 148.3(5) . 1_465 ?
O1 Nd1 O26 70.9(5) . 1_465 ?
O9 Nd1 O2 78.7(5) . . ?
O7 Nd1 O2 101.6(5) . . ?
O5 Nd1 O2 114.3(5) . . ?
O15 Nd1 O2 76.2(5) . . ?
O6 Nd1 O2 143.8(5) . . ?
O4 Nd1 O2 141.8(5) . . ?
O1 Nd1 O2 51.1(5) . . ?
O26 Nd1 O2 69.7(5) 1_465 . ?
O2 Nd2 O8 77.9(5) . . ?
O2 Nd2 O10 84.3(5) . . ?
O8 Nd2 O10 77.2(5) . . ?
O2 Nd2 O3 70.6(5) . . ?
O8 Nd2 O3 123.0(5) . . ?
O10 Nd2 O3 141.3(5) . . ?
O2 Nd2 O13 145.5(5) . . ?
O8 Nd2 O13 132.5(5) . . ?
O10 Nd2 O13 114.7(5) . . ?
O3 Nd2 O13 77.5(5) . . ?
O2 Nd2 O12 105.4(5) . . ?
O8 Nd2 O12 70.1(5) . . ?
O10 Nd2 O12 142.7(5) . . ?
O3 Nd2 O12 74.2(5) . . ?
O13 Nd2 O12 77.4(5) . . ?
O2 Nd2 O14 85.4(5) . . ?
O8 Nd2 O14 149.0(5) . . ?
O10 Nd2 O14 75.3(5) . . ?
O3 Nd2 O14 73.9(5) . . ?
O13 Nd2 O14 73.1(5) . . ?
O12 Nd2 O14 140.3(5) . . ?
O2 Nd2 O11 145.6(5) . . ?
O8 Nd2 O11 77.7(5) . . ?
O10 Nd2 O11 66.9(5) . . ?
O3 Nd2 O11 143.7(5) . . ?
O13 Nd2 O11 67.6(5) . . ?
O12 Nd2 O11 88.5(5) . . ?
O14 Nd2 O11 103.9(5) . . ?
C1 O1 Nd1 95.2(13) . . ?
C1 O2 Nd2 143.2(14) . . ?
C1 O2 Nd1 91.7(12) . . ?
Nd2 O2 Nd1 120.4(5) . . ?
C6 O3 Nd2 136.9(14) . . ?
Nd1 O4 H4A 114.6 . . ?
Nd1 O4 H4B 114.6 . . ?
H4A O4 H4B 110.7 . . ?
Nd1 O5 H5A 119.0 . . ?
Nd1 O5 H5B 118.9 . . ?
H5A O5 H5B 110.7 . . ?
Nd1 O6 H6A 118.0 . . ?
Nd1 O6 H6B 117.9 . . ?
H6A O6 H6B 110.7 . . ?
C7 O7 Nd1 118.4(13) . . ?
C7 O8 Nd2 168.8(14) . . ?
C13 O9 Nd1 147.8(14) . . ?
C13 O10 Nd2 134.2(13) . . ?
Nd2 O11 H11A 108.0 . . ?
Nd2 O11 H11B 108.0 . . ?
H11A O11 H11B 104.4 . . ?
Nd2 O12 H12A 119.1 . . ?
Nd2 O12 H12B 119.2 . . ?
H12A O12 H12B 110.7 . . ?
Nd2 O13 H13A 122.6 . . ?
Nd2 O13 H13B 122.6 . . ?
H13A O13 H13B 110.7 . . ?
C5 N1 C6 121(2) . . ?
C2 N1A C4 120(2) . . ?
C12 N2 C11 121(2) . . ?
O1 C1 O2 121(2) . . ?
O1 C1 C2 119.3(19) . . ?
O2 C1 C2 119.1(19) . . ?
C3 C2 C6 122.1(19) . . ?
N1A C2 C6 122.1(19) . . ?
C3 C2 C1 117.1(19) . . ?
N1A C2 C1 117.1(19) . . ?
C6 C2 C1 120.8(18) . . ?
C2 C3 C4 120(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 119.9 . . ?
C5 C3A C6 121(2) . . ?
C5 C3A H3A 119.5 . . ?
C6 C3A H3A 119.5 . . ?
C5 C4 N1A 118(2) . . ?
C5 C4 C3 118(2) . . ?
C5 C4 H4 121.4 . . ?
N1A C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 N1 123(2) . . ?
C4 C5 C3A 123(2) . . ?
C4 C5 H5 118.5 . . ?
N1 C5 H5 118.7 . . ?
C3A C5 H5 118.7 . . ?
O3 C6 C3A 115.1(19) . . ?
O3 C6 N1 115.1(19) . . ?
O3 C6 C2 128.8(19) . . ?
C3A C6 C2 116.1(19) . . ?
N1 C6 C2 116.1(19) . . ?
O7 C7 O8 123(2) . . ?
O7 C7 C8 119.9(19) . . ?
O8 C7 C8 116.6(19) . . ?
C12 C8 C9 119(2) . . ?
C12 C8 C7 118.1(19) . . ?
C9 C8 C7 122.9(19) . . ?
C8 C9 C10 118(2) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 H9 121.1 . . ?
C11 C10 C9 120(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
N2 C11 C10 120(2) . . ?
N2 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
N2 C12 C8 121(2) . . ?
N2 C12 H12 119.5 . . ?
C8 C12 H12 119.5 . . ?
O10 C13 O9 127.8(19) . . ?
O10 C13 C14 117.3(18) . . ?
O9 C13 C14 114.9(18) . . ?
C15 C14 C19 116.3(19) . . ?
N3 C14 N3C 116.3(19) . . ?
C15 C14 C13 123.7(19) . . ?
N3 C14 C13 123.7(19) . . ?
C19 C14 C13 120.0(18) . . ?
N3C C14 C13 120.0(18) . . ?
N3A N3 C14 124(2) . . ?
C16 C15 C14 124(2) . . ?
C16 C15 H15 117.8 . . ?
C14 C15 H15 117.8 . . ?
N3 N3A C17 117(2) . . ?
C15 C16 C17 117(2) . . ?
C15 C16 H16 121.3 . . ?
C17 C16 H16 121.3 . . ?
N3B C17 N3A 117(2) . . ?
C18 C17 C16 117(2) . . ?
N3B C17 H17 121.3 . . ?
N3A C17 H17 121.3 . . ?
C17 N3B N3C 125(2) . . ?
C17 C18 C19 125(2) . . ?
C17 C18 H18 117.5 . . ?
C19 C18 H18 117.5 . . ?
N3B N3C C14 119(2) . . ?
C18 C19 C14 119(2) . . ?
C18 C19 H19 120.3 . . ?
C14 C19 H19 120.3 . . ?
O15 W1 O28 100.9(6) . . ?
O15 W1 O29 100.5(6) . . ?
O28 W1 O29 86.2(6) . . ?
O15 W1 O27 101.4(6) . . ?
O28 W1 O27 89.4(6) . . ?
O29 W1 O27 158.1(6) . . ?
O15 W1 O30 99.8(6) . . ?
O28 W1 O30 159.2(6) . . ?
O29 W1 O30 88.2(6) . . ?
O27 W1 O30 88.3(6) . . ?
O15 W1 O51 171.3(6) . . ?
O28 W1 O51 85.5(5) . . ?
O29 W1 O51 85.6(5) . . ?
O27 W1 O51 72.6(5) . . ?
O30 W1 O51 74.1(5) . . ?
O16 W2 O33 101.6(6) . . ?
O16 W2 O32 102.1(6) . . ?
O33 W2 O32 85.8(6) . . ?
O16 W2 O30 99.4(6) . . ?
O33 W2 O30 89.6(6) . . ?
O32 W2 O30 158.6(6) . . ?
O16 W2 O31 99.1(6) . . ?
O33 W2 O31 159.3(6) . . ?
O32 W2 O31 88.6(6) . . ?
O30 W2 O31 88.4(6) . . ?
O16 W2 O51 170.9(6) . . ?
O33 W2 O51 85.2(5) . . ?
O32 W2 O51 84.4(5) . . ?
O30 W2 O51 74.4(5) . . ?
O31 W2 O51 74.4(5) . . ?
O17 W3 O35 101.5(7) . . ?
O17 W3 O34 103.2(6) . . ?
O35 W3 O34 87.4(6) . . ?
O17 W3 O27 101.8(6) . . ?
O35 W3 O27 156.5(6) . . ?
O34 W3 O27 89.4(6) . . ?
O17 W3 O31 98.4(6) . . ?
O35 W3 O31 88.1(6) . . ?
O34 W3 O31 158.5(6) . . ?
O27 W3 O31 86.4(6) . . ?
O17 W3 O51 169.8(6) . . ?
O35 W3 O51 84.2(6) . . ?
O34 W3 O51 85.4(5) . . ?
O27 W3 O51 72.4(5) . . ?
O31 W3 O51 73.3(5) . . ?
O18 W4 O38 100.8(7) . . ?
O18 W4 O28 101.2(7) . . ?
O38 W4 O28 86.1(6) . . ?
O18 W4 O37 101.0(7) . . ?
O38 W4 O37 89.4(6) . . ?
O28 W4 O37 157.8(6) . . ?
O18 W4 O36 101.6(7) . . ?
O38 W4 O36 157.5(6) . . ?
O28 W4 O36 88.6(6) . . ?
O37 W4 O36 87.3(6) . . ?
O18 W4 O54 172.2(6) . . ?
O38 W4 O54 84.8(5) . . ?
O28 W4 O54 84.4(5) . . ?
O37 W4 O54 73.5(5) . . ?
O36 W4 O54 72.9(5) . . ?
O19 W5 O40 101.8(6) . . ?
O19 W5 O29 102.6(7) . . ?
O40 W5 O29 90.3(6) . . ?
O19 W5 O39 98.5(7) . . ?
O40 W5 O39 88.2(6) . . ?
O29 W5 O39 158.6(6) . . ?
O19 W5 O38 101.2(6) . . ?
O40 W5 O38 157.0(6) . . ?
O29 W5 O38 85.3(6) . . ?
O39 W5 O38 87.8(6) . . ?
O19 W5 O53 169.7(6) . . ?
O40 W5 O53 72.9(5) . . ?
O29 W5 O53 86.4(5) . . ?
O39 W5 O53 72.8(5) . . ?
O38 W5 O53 84.2(5) . . ?
O20 W6 O42 99.8(6) . . ?
O20 W6 O41 99.2(6) . . ?
O42 W6 O41 92.1(6) . . ?
O20 W6 O33 101.1(6) . . ?
O42 W6 O33 86.3(6) . . ?
O41 W6 O33 159.6(6) . . ?
O20 W6 O40 101.3(6) . . ?
O42 W6 O40 158.8(6) . . ?
O41 W6 O40 86.6(6) . . ?
O33 W6 O40 87.6(6) . . ?
O20 W6 O53 171.6(6) . . ?
O42 W6 O53 85.8(5) . . ?
O41 W6 O53 74.1(5) . . ?
O33 W6 O53 85.5(5) . . ?
O40 W6 O53 73.5(5) . . ?
O21 W7 O44 101.7(7) . . ?
O21 W7 O43 101.9(7) . . ?
O44 W7 O43 89.3(6) . . ?
O21 W7 O32 101.3(7) . . ?
O44 W7 O32 88.4(6) . . ?
O43 W7 O32 156.7(6) . . ?
O21 W7 O42 102.1(6) . . ?
O44 W7 O42 156.0(6) . . ?
O43 W7 O42 88.3(6) . . ?
O32 W7 O42 84.5(6) . . ?
O21 W7 O52 173.1(6) . . ?
O44 W7 O52 73.1(5) . . ?
O43 W7 O52 73.8(5) . . ?
O32 W7 O52 83.3(5) . . ?
O42 W7 O52 83.3(5) . . ?
O22 W8 O46 102.2(7) . . ?
O22 W8 O35 102.6(7) . . ?
O46 W8 O35 87.0(6) . . ?
O22 W8 O45 99.2(6) . . ?
O46 W8 O45 91.1(6) . . ?
O35 W8 O45 158.0(6) . . ?
O22 W8 O44 99.1(6) . . ?
O46 W8 O44 158.7(6) . . ?
O35 W8 O44 86.6(6) . . ?
O45 W8 O44 87.3(6) . . ?
O22 W8 O52 169.5(6) . . ?
O46 W8 O52 86.2(5) . . ?
O35 W8 O52 84.0(5) . . ?
O45 W8 O52 74.0(5) . . ?
O44 W8 O52 72.9(5) . . ?
O23 W9 O36 101.4(7) . . ?
O23 W9 O47 101.0(7) . . ?
O36 W9 O47 90.4(6) . . ?
O23 W9 O34 101.3(7) . . ?
O36 W9 O34 89.4(6) . . ?
O47 W9 O34 157.3(6) . . ?
O23 W9 O46 100.5(7) . . ?
O36 W9 O46 158.0(6) . . ?
O47 W9 O46 88.0(6) . . ?
O34 W9 O46 83.8(6) . . ?
O23 W9 O54 172.9(6) . . ?
O36 W9 O54 73.9(5) . . ?
O47 W9 O54 74.0(5) . . ?
O34 W9 O54 84.2(5) . . ?
O46 W9 O54 84.6(5) . . ?
O24 W10 O37 101.5(7) . . ?
O24 W10 O48 100.7(6) . . ?
O37 W10 O48 90.5(6) . . ?
O24 W10 O47 101.1(7) . . ?
O37 W10 O47 90.0(6) . . ?
O48 W10 O47 157.7(6) . . ?
O24 W10 O49 100.6(7) . . ?
O37 W10 O49 157.8(6) . . ?
O48 W10 O49 83.7(6) . . ?
O47 W10 O49 87.6(6) . . ?
O24 W10 O54 173.3(6) . . ?
O37 W10 O54 74.2(5) . . ?
O48 W10 O54 84.7(5) . . ?
O47 W10 O54 74.0(5) . . ?
O49 W10 O54 83.9(5) . . ?
O25 W11 O48 101.9(6) . . ?
O25 W11 O50 103.9(7) . . ?
O48 W11 O50 87.1(6) . . ?
O25 W11 O39 99.1(7) . . ?
O48 W11 O39 89.6(6) . . ?
O50 W11 O39 156.9(6) . . ?
O25 W11 O41 101.1(6) . . ?
O48 W11 O41 157.0(6) . . ?
O50 W11 O41 87.4(6) . . ?
O39 W11 O41 86.7(6) . . ?
O25 W11 O53 170.2(6) . . ?
O48 W11 O53 84.4(5) . . ?
O50 W11 O53 83.6(5) . . ?
O39 W11 O53 73.3(5) . . ?
O41 W11 O53 72.7(5) . . ?
O26 W12 O49 100.5(7) . . ?
O26 W12 O50 100.8(7) . . ?
O49 W12 O50 87.9(6) . . ?
O26 W12 O43 100.5(7) . . ?
O49 W12 O43 158.9(6) . . ?
O50 W12 O43 89.0(6) . . ?
O26 W12 O45 99.9(6) . . ?
O49 W12 O45 89.1(6) . . ?
O50 W12 O45 159.3(6) . . ?
O43 W12 O45 86.4(6) . . ?
O26 W12 O52 171.6(6) . . ?
O49 W12 O52 85.1(5) . . ?
O50 W12 O52 85.5(5) . . ?
O43 W12 O52 73.9(5) . . ?
O45 W12 O52 73.8(5) . . ?
O54 Si1 O53 109.6(7) . . ?
O54 Si1 O51 109.3(7) . . ?
O53 Si1 O51 109.9(7) . . ?
O54 Si1 O52 109.8(7) . . ?
O53 Si1 O52 109.4(7) . . ?
O51 Si1 O52 108.8(7) . . ?
W1 O15 Nd1 155.8(8) . . ?
W12 O26 Nd1 155.1(8) . 1_645 ?
W3 O27 W1 123.4(8) . . ?
W1 O28 W4 151.4(8) . . ?
W1 O29 W5 150.5(8) . . ?
W1 O29 H29 104.0 . . ?
W5 O29 H29 103.3 . . ?
W1 O30 W2 119.9(7) . . ?
W2 O31 W3 119.9(7) . . ?
W7 O32 W2 152.1(8) . . ?
W6 O33 W2 150.4(8) . . ?
W3 O34 W9 152.5(8) . . ?
W3 O35 W8 149.4(9) . . ?
W9 O36 W4 122.1(7) . . ?
W9 O36 H36 115.6 . . ?
W4 O36 H36 110.4 . . ?
W10 O37 W4 121.8(8) . . ?
W4 O38 W5 151.2(8) . . ?
W11 O39 W5 122.0(7) . . ?
W5 O40 W6 122.1(7) . . ?
W6 O41 W11 121.4(7) . . ?
W6 O42 W7 153.1(8) . . ?
W7 O43 W12 120.8(7) . . ?
W7 O44 W8 122.2(8) . . ?
W8 O45 W12 119.6(7) . . ?
W8 O46 W9 151.8(8) . . ?
W9 O47 W10 121.3(8) . . ?
W11 O48 W10 153.5(8) . . ?
W12 O49 W10 151.2(8) . . ?
W11 O50 W12 149.3(8) . . ?
Si1 O51 W2 124.6(7) . . ?
Si1 O51 W1 123.8(7) . . ?
W2 O51 W1 91.6(5) . . ?
Si1 O51 W3 123.3(7) . . ?
W2 O51 W3 92.4(5) . . ?
W1 O51 W3 91.6(4) . . ?
Si1 O52 W12 122.8(7) . . ?
Si1 O52 W8 124.1(7) . . ?
W12 O52 W8 92.5(4) . . ?
Si1 O52 W7 124.8(7) . . ?
W12 O52 W7 91.5(4) . . ?
W8 O52 W7 91.7(4) . . ?
Si1 O53 W6 123.5(7) . . ?
Si1 O53 W11 124.8(7) . . ?
W6 O53 W11 91.8(4) . . ?
Si1 O53 W5 123.9(7) . . ?
W6 O53 W5 91.5(4) . . ?
W11 O53 W5 91.8(5) . . ?
Si1 O54 W10 124.4(7) . . ?
Si1 O54 W4 124.5(7) . . ?
W10 O54 W4 90.5(5) . . ?
Si1 O54 W9 125.5(7) . . ?
W10 O54 W9 90.5(4) . . ?
W4 O54 W9 91.0(4) . . ?
H55A O55 H55B 104.5 . . ?
H56A O56 H56B 110.7 . . ?
H57A O57 H57B 110.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4A O57 0.84 2.09 2.69(3) 128 .
O4 H4B O19 0.84 2.38 3.07(2) 140 2_656
O4 H4B O39 0.84 2.43 3.18(2) 149 2_656
O5 H5A O56 0.84 1.99 2.76(3) 152 .
O5 H5B O39 0.84 1.89 2.69(2) 159 2_656
O6 H6A O24 0.84 2.29 2.93(2) 133 1_465
O6 H6A O49 0.84 2.41 3.16(2) 149 1_465
O6 H6B O25 0.84 2.03 2.79(2) 151 2_656
O11 H11A O20 0.84 2.01 2.84(2) 167 1_565
O11 H11B O55 0.84 1.86 2.68(2) 163 .
O12 H12A O21 0.84 2.01 2.85(2) 174 2_657
O12 H12B O45 0.84 2.01 2.85(2) 172 1_465
O13 H13A O11 0.84 2.02 2.71(2) 138 2_667
O13 H13B O16 0.84 2.07 2.78(2) 143 2_657
O29 H29 O56 0.86 2.14 2.98(2) 164 .
O36 H36 O24 0.84 2.49 3.18(2) 141 2_756
O55 H55A O17 0.84 2.10 2.91(2) 161 .
O55 H55B O22 0.84 2.15 2.98(2) 171 2_757
O56 H56A N2 0.84 1.89 2.69(3) 159 1_545
O56 H56B O38 0.84 1.99 2.81(3) 163 2_656
O57 H57A O41 0.84 2.22 2.99(2) 152 2_656
O57 H57B O7 0.84 2.60 3.31(2) 142 2_666
O57 H57B O9 0.84 2.60 3.36(2) 151 2_666

_refine_diff_density_max         5.148
_refine_diff_density_min         -4.820
_refine_diff_density_rms         0.670

_vrf_PLAT_971                    
;
PROBLEM: ALERT_2_A Check Calcd Residual Density  0.05A From Si1  4.99 eA-3
ALERT_2_A Check Calcd Residual Density  0.91A From      W8       4.91 eA-3
ALERT_2_A Check Calcd Residual Density  0.83A From      W2       4.86 eA-3
ALERT_2_A Check Calcd Residual Density  0.80A From     Nd1       4.80 eA-3
ALERT_2_A Check Calcd Residual Density  1.00A From     W10       4.78 eA-3
ALERT_2_A Check Calcd Residual Density  0.88A From      W7       4.49 eA-3
ALERT_2_A Check Calcd Residual Density  0.25A From      W2       4.45 eA-3
ALERT_2_A Check Calcd Residual Density  0.67A From     W12       4.38 eA-3
ALERT_2_A Check Calcd Residual Density  0.95A From     O34       4.34 eA-3
ALERT_2_A Check Calcd Residual Density  0.79A From     W11       4.17 eA-3
ALERT_2_A Check Calcd Residual Density  1.04A From     W12       4.12 eA-3
ALERT_2_A Check Calcd Residual Density  0.92A From      W5       4.08 eA-3
ALERT_2_A Check Calcd Residual Density  1.00A From      W1       4.01 eA-3
ALERT_2_A Check Calcd Residual Density  0.89A From      W3       4.00 eA-3
ALERT_2_A Check Calcd Residual Density  0.89A From      W7       3.96 eA-3
ALERT_2_A Check Calcd Residual Density  1.15A From      W9       3.89 eA-3
ALERT_2_A Check Calcd Residual Density  1.00A From      W4       3.82 eA-3
ALERT_2_A Check Calcd Residual Density  0.95A From      W1       3.82 eA-3
RESPONSE:  Residual density in the close vicinity of the metal atoms 
could not be successfully interpreted as disorder and is therefore 
attributed to inadequacies in the absorption correction due to the very 
large absorption coefficient and difficulties in accurately determining the 
thickness of the very thin, plate-like crystal.
;

_vrf_PLAT_972                    
;
PROBLEM: ALERT_2_A Check Calcd Residual Density  0.87A From  W11 -4.66 eA-3
ALERT_2_A Check Calcd Residual Density  0.74A From      W4      -4.65 eA-3
ALERT_2_A Check Calcd Residual Density  0.77A From      W4      -4.49 eA-3
ALERT_2_A Check Calcd Residual Density  0.63A From      W5      -4.42 eA-3
ALERT_2_A Check Calcd Residual Density  0.73A From      W4      -4.42 eA-3
ALERT_2_A Check Calcd Residual Density  0.88A From     O18      -4.30 eA-3
ALERT_2_A Check Calcd Residual Density  0.79A From     W11      -4.17 eA-3
ALERT_2_A Check Calcd Residual Density  0.76A From      W6      -4.12 eA-3
ALERT_2_A Check Calcd Residual Density  0.66A From      W2      -4.00 eA-3
ALERT_2_A Check Calcd Residual Density  0.88A From      W5      -3.96 eA-3
ALERT_2_A Check Calcd Residual Density  0.87A From      W7      -3.91 eA-3
ALERT_2_A Check Calcd Residual Density  0.85A From      W6      -3.88 eA-3
ALERT_2_A Check Calcd Residual Density  0.93A From     W10      -3.78 eA-3
ALERT_2_A Check Calcd Residual Density  0.79A From      W3      -3.76 eA-3
ALERT_2_A Check Calcd Residual Density  0.74A From     W11      -3.75 eA-3
ALERT_2_A Check Calcd Residual Density  0.87A From      W5      -3.71 eA-3
ALERT_2_A Check Calcd Residual Density  0.81A From      W9      -3.54 eA-3
ALERT_2_A Check Calcd Residual Density  0.70A From      W2      -3.51 eA-3
ALERT_2_A Check Calcd Residual Density  0.84A From      W7      -3.51 eA-3
ALERT_2_B Check Calcd Residual Density  0.67A From      W9      -3.50 eA-3
ALERT_2_B Check Calcd Residual Density  0.83A From     W10      -3.46 eA-3
ALERT_2_B Check Calcd Residual Density  1.02A From     W12      -3.44 eA-3
ALERT_2_B Check Calcd Residual Density  0.83A From     W10      -3.43 eA-3
ALERT_2_B Check Calcd Residual Density  0.76A From      W9      -3.37 eA-3
ALERT_2_B Check Calcd Residual Density  0.79A From     W10      -3.30 eA-3
RESPONSE:  Residual density in the close vicinity of the metal atoms 
could not be successfully interpreted as disorder and is therefore 
attributed to inadequacies in the absorption correction due to the very 
large absorption coefficient and difficulties in accurately determining the 
thickness of the very thin, plate-like crystal.
;

_vrf_PLAT_973                    
;
PROBLEM: ALERT_2_A Check Calcd Positive Residual Density on  W1  5.50 eA-3
ALERT_2_A Check Calcd Positive Residual Density on     W12       5.37 eA-3
ALERT_2_A Check Calcd Positive Residual Density on      W8       4.80 eA-3
ALERT_2_A Check Calcd Positive Residual Density on      W7       4.51 eA-3
ALERT_2_A Check Calcd Positive Residual Density on     Nd2       4.49 eA-3
ALERT_2_A Check Calcd Positive Residual Density on      W3       4.24 eA-3
ALERT_2_A Check Calcd Positive Residual Density on     Nd1       4.05 eA-3
RESPONSE:  Residual density in the close vicinity of the metal atoms 
could not be successfully interpreted as disorder and is therefore 
attributed to inadequacies in the absorption correction due to the very 
large absorption coefficient and difficulties in accurately determining the 
thickness of the very thin, plate-like crystal.
;


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
