# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1495658'
_audit_update_record             
;
2016-09-05 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT430_1                   
;
PROBLEM: Short Inter D...A Contact O1W .. O14W .. 1.78 Ang.
RESPONSE: In the crystal structure, there are a number of short connections
 between  OW(H2O) and O(POM) or OW(H2O) atoms in the range 2.16-2.41 Ang,
 which indicate extensive H bonding interactions among them. 
 Some shorter connections between OW(H2O) or OW(H2O) atoms result from
 the disordered water molecules. 
;

_vrf_PLAT201_1                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 2 Report 
RESPONSE: Due to the large structure and the existence of a large 
 amount of weight atoms, the intensity data are not very good, 
 leading to the ADP max/min ratio of some O atoms and water molecules, 
 and it is very difficult to refine this large structure. Therefore,
 in the final refinement, all the W, B, lanthanoid, Na and K atoms 
 were refined anisotropically and some O atoms and water molecules
 were refined isotropically.
;

_vrf_PLAT220_1                   
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range   8.2 Ratio 
RESPONSE: In polyoxometalate (POM) compounds, the Ueq of oxygen atoms in
 the POM skeleton is small due to multiple covalent bonds, whereas
 the Ueq values of these discrete water oxygen atoms are biggish 
 without the constraint of covalent bonds. 
;

_vrf_PLAT306_1                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check  
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

_vrf_PLAT342_1                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.  
RESPONSE: The alert derives from shading of reciprocal space
 by the pressure cell and it is unavoidable in high pressure
 crystal structure determinations.
;

# end Validation Reply Form

_audit_creation_date             2016-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C16 H40 B4 Ce4 K8 N8 Na8 O200 W44), 9(O)'
_chemical_formula_sum            'C8 H70 B2 Ce2 K4 N4 Na4 O109 W22'
_chemical_formula_weight         6561.60
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        P2(1)/c
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.783(2)
_cell_length_b                   21.459(4)
_cell_length_c                   21.350(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.787(3)
_cell_angle_gamma                90.00
_cell_volume                     5395.9(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4271
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.796
_cell_measurement_theta_min      2.215
_exptl_absorpt_coefficient_mu    24.457
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0786 after correction.
The Ratio of minimum to maximum transmission is 0.5352.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    4.039
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_special_details           
;
Thanks to the large structure of 1 and the existence of a 
large amount of weight atoms, the intensity data are not 
very good, leading to the ADP max/min ratio of some atoms,
and it is very difficult to refine this large structure,
therefore, some unit-occupancy atoms have been refined 
isotropically and restrainedly refined. The ISOR 
instruction is used for O6, O23, O28, O33, O38, O42, C2,
 O41, O1, O39, O1W, O21, O17, O4, O9, O43, C3, O36, O25,
 O13, O10W, O15, O8, O7, O14, B1, O10, O24, O28 and O34. 
O6W-O9W, O11W-O14W and O3 are refined isostropicallly. 
674 parameters and 180 restraints are used in the 
refinement. In addition, the specific reason why that
 the Ueq value of the B1 atom is extremely small 
is well understood and may be related to the fact 
that the atomic weight of the B1 atom is very small
 in contrast to other atoms in the structure. 
This phenomenon is already encountered in other
 borotungstates (H. An, Z. Han and T. Xu, 
Inorg. Chem., 2010, 49, 11403; J. Niu, J. Zhao,
 J. Wang, P. Ma, J. Mol. Struct., 2004, 699, 85).
;
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         26214
_reflns_number_gt                6502
_reflns_number_total             9217
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         4.140
_refine_diff_density_min         -3.155
_refine_diff_density_rms         0.513
_refine_ls_extinction_coef       0.000054(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         9217
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0579
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0614P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1417
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O33)
\\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(O41) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O1W)
\\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(O36) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O13) \\sim Ueq,
Uanis(O10W) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O34) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O8W(0.5) O11W(0.5) O12W(0.5) O13W(0.5) O14W(0.5)
 Fixed Uiso: O12W(0.08772) O13W(0.08186) O14W(0.08676)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
4.b Me refined with riding coordinates:
 N1(H1C,H1D,H1E), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ce1 Ce 0.39251(9) 0.52064(5) 0.42479(5) 0.0129(3) Uani 1 d . . . .
B1 B 0.2230(16) 0.6528(9) 0.2703(9) 0.004(4) Uani 1 d . . . U
W1 W 0.10195(7) 0.50511(4) 0.31833(4) 0.0144(2) Uani 1 d . . . .
W2 W -0.03207(7) 0.72813(4) 0.30521(4) 0.0186(2) Uani 1 d . . . .
W3 W 0.46240(7) 0.56853(4) 0.24044(4) 0.0167(2) Uani 1 d . . . .
W4 W 0.22120(7) 0.53145(4) 0.16206(4) 0.0170(2) Uani 1 d . . . .
W5 W 0.46912(7) 0.69293(4) 0.35228(4) 0.0176(2) Uani 1 d . . . .
W6 W 0.34867(7) 0.66507(4) 0.13007(4) 0.0186(2) Uani 1 d . . . .
W7 W 0.23413(7) 0.77302(4) 0.38270(4) 0.0182(2) Uani 1 d . . . .
W8 W 0.10312(7) 0.62132(4) 0.42345(4) 0.0152(2) Uani 1 d . . . .
W9 W 0.35427(7) 0.79219(4) 0.24512(4) 0.0191(2) Uani 1 d . . . .
W10 W -0.03842(7) 0.61178(4) 0.20064(4) 0.0177(2) Uani 1 d . . . .
W11 W 0.08467(7) 0.74761(4) 0.16571(4) 0.0186(2) Uani 1 d . . . .
Na1 Na 0.0964(11) 0.8950(7) 0.2798(7) 0.078(4) Uani 1 d . . . .
Na2 Na 0.0751(7) 0.6235(5) 0.0292(4) 0.031(2) Uani 1 d . . . .
K1 K 0.1524(4) 0.3749(3) 0.4281(2) 0.0342(13) Uani 1 d . . . .
K2 K 0.3660(5) 0.4094(3) 0.2715(3) 0.0362(13) Uani 1 d . . . .
O1W O 0.2632(15) 0.9578(8) 0.3371(9) 0.047(5) Uani 1 d . . . U
O2W O 0.3384(17) 0.3430(8) 0.1611(11) 0.061(6) Uani 1 d . . . .
O3W O 0.2065(15) 0.8959(9) 0.0847(9) 0.054(5) Uani 1 d . . . .
O4W O -0.3283(16) 0.7086(9) 0.1923(10) 0.062(6) Uani 1 d . . . .
O5W O 0.2306(19) 0.9577(9) 0.2000(10) 0.064(6) Uani 1 d . . . .
O6W O 0.257(2) 0.2836(12) 0.5036(12) 0.093(8) Uiso 1 d . . . .
O7W O -0.033(3) 0.7289(14) -0.0174(15) 0.120(10) Uiso 1 d . . . .
O8W O 0.364(5) 0.569(3) -0.022(3) 0.12(2) Uiso 0.50 d . . . .
O9W O 0.550(3) 0.6504(16) -0.0464(17) 0.144(13) Uiso 1 d . . . .
O10W O 0.2237(15) 0.3251(9) 0.3192(9) 0.053(5) Uani 1 d . . . U
O11W O 0.656(4) 0.591(2) 0.084(2) 0.067(12) Uiso 0.50 d . . . .
O12W O -0.333(4) 0.642(3) 0.081(2) 0.088 Uiso 0.50 d . . . .
O13W O -0.021(4) 0.619(2) -0.098(2) 0.082 Uiso 0.50 d . . . .
O14W O -0.251(4) 0.505(2) 0.095(2) 0.087 Uiso 0.50 d . . . .
O1 O -0.1441(12) 0.7668(7) 0.3361(7) 0.024(3) Uani 1 d . . . U
O2 O 0.2153(13) 0.8275(7) 0.4390(7) 0.033(4) Uani 1 d . . . .
O3 O 0.6036(14) 0.6999(8) 0.3866(7) 0.036(4) Uiso 1 d . . . .
O4 O 0.1925(13) 0.4694(7) 0.1154(7) 0.031(4) Uani 1 d . . . U
O5 O 0.2885(12) 0.7070(6) 0.2990(6) 0.022(3) Uani 1 d . . . .
O6 O 0.1956(10) 0.6090(6) 0.3224(6) 0.015(3) Uani 1 d . . . U
O7 O 0.3730(11) 0.5116(6) 0.1861(6) 0.018(3) Uani 1 d . . . U
O8 O 0.3894(13) 0.7351(7) 0.1810(7) 0.026(4) Uani 1 d . . . U
O9 O 0.4716(11) 0.6204(6) 0.1602(6) 0.018(3) Uani 1 d . . . U
O10 O -0.0199(11) 0.7755(6) 0.2295(6) 0.017(3) Uani 1 d . . . U
O11 O 0.2879(12) 0.8275(7) 0.3200(7) 0.024(3) Uani 1 d . . . .
O12 O -0.1152(12) 0.6683(7) 0.2544(7) 0.026(4) Uani 1 d . . . .
O13 O 0.0916(11) 0.7760(6) 0.3381(6) 0.017(3) Uani 1 d . . . U
O14 O 0.1076(10) 0.6759(6) 0.2457(6) 0.011(3) Uani 1 d . . . U
O15 O 0.4068(12) 0.8594(7) 0.2158(7) 0.023(3) Uani 1 d . . . U
O16 O 0.3872(12) 0.7532(7) 0.4032(6) 0.024(3) Uani 1 d . . . .
O17 O 0.4845(13) 0.7648(7) 0.2923(7) 0.029(4) Uani 1 d . . . U
O18 O 0.4139(12) 0.5353(7) 0.3085(6) 0.027(4) Uani 1 d . . . .
O19 O 0.0227(11) 0.4378(6) 0.3181(6) 0.018(3) Uani 1 d . . . .
O20 O 0.2761(11) 0.5875(7) 0.1024(7) 0.023(3) Uani 1 d . . . .
O21 O 0.4106(12) 0.6309(6) 0.3916(6) 0.022(3) Uani 1 d . . . U
O22 O 0.2033(12) 0.7924(7) 0.2065(7) 0.026(4) Uani 1 d . . . .
O23 O 0.0383(12) 0.5496(7) 0.3870(6) 0.023(3) Uani 1 d . . . U
O24 O -0.0056(11) 0.5592(6) 0.2666(6) 0.015(3) Uani 1 d . . . U
O25 O 0.1785(11) 0.4979(6) 0.2387(6) 0.015(3) Uani 1 d . . . U
O26 O -0.0010(11) 0.6691(7) 0.3641(7) 0.022(3) Uani 1 d . . . .
O27 O 0.0453(12) 0.8007(7) 0.1073(7) 0.023(3) Uani 1 d . . . .
O28 O -0.0203(11) 0.6835(6) 0.1447(6) 0.019(3) Uani 1 d . . . U
O29 O -0.1559(13) 0.5777(7) 0.1649(7) 0.029(4) Uani 1 d . . . .
O30 O 0.2204(12) 0.4826(6) 0.3637(6) 0.018(3) Uani 1 d . . . .
O31 O 0.2008(12) 0.7009(6) 0.1248(6) 0.019(3) Uani 1 d . . . .
O32 O 0.0219(11) 0.6293(7) 0.4881(6) 0.022(3) Uani 1 d . . . .
O33 O 0.5091(12) 0.6445(7) 0.2818(6) 0.023(3) Uani 1 d . . . U
O34 O 0.1837(11) 0.6998(6) 0.4224(6) 0.018(3) Uani 1 d . . . U
O35 O 0.2859(12) 0.6191(6) 0.2208(7) 0.021(3) Uani 1 d . . . .
O36 O 0.0784(11) 0.5728(6) 0.1557(6) 0.016(3) Uani 1 d . . . U
O37 O 0.3952(13) 0.6888(7) 0.0597(7) 0.030(4) Uani 1 d . . . .
O38 O 0.2238(11) 0.5817(6) 0.4549(6) 0.018(3) Uani 1 d . . . U
O39 O 0.5921(12) 0.5351(7) 0.2331(7) 0.027(4) Uani 1 d . . . U
O40 O 0.4039(12) 0.4584(7) 0.5933(7) 0.026(4) Uani 1 d . . . .
O41 O 0.2971(12) 0.4561(7) 0.5045(6) 0.022(3) Uani 1 d . . . U
O42 O 0.4637(12) 0.5695(7) 0.5239(6) 0.023(3) Uani 1 d . . . U
O43 O 0.5730(12) 0.5908(7) 0.6066(7) 0.025(3) Uani 1 d . . . U
N1 N 0.2437(18) 0.4145(10) 0.6646(9) 0.042(6) Uani 1 d . . . .
H1C H 0.1847 0.3992 0.6846 0.063 Uiso 1 calc . . R .
H1D H 0.2610 0.4521 0.6799 0.063 Uiso 1 calc . . R .
H1E H 0.3031 0.3893 0.6701 0.063 Uiso 1 calc . . R .
N2 N 0.3603(18) 0.6837(11) 0.5245(9) 0.045(6) Uani 1 d . . . .
H2A H 0.3429 0.7240 0.5252 0.068 Uiso 1 calc . . R .
H2B H 0.3045 0.6618 0.5410 0.068 Uiso 1 calc . . R .
H2C H 0.3693 0.6717 0.4850 0.068 Uiso 1 calc . . R .
C1 C 0.215(2) 0.4196(14) 0.5983(11) 0.043(7) Uani 1 d . . . .
H1A H 0.1490 0.4462 0.5923 0.052 Uiso 1 calc . . R .
H1B H 0.1965 0.3788 0.5815 0.052 Uiso 1 calc . . R .
C2 C 0.3150(17) 0.4471(10) 0.5637(9) 0.018(5) Uani 1 d . . . U
C3 C 0.5032(18) 0.6064(10) 0.5634(10) 0.022(5) Uani 1 d . . . U
C4 C 0.4671(19) 0.6730(12) 0.5614(12) 0.036(6) Uani 1 d . . . .
H4A H 0.4572 0.6875 0.6039 0.044 Uiso 1 calc . . R .
H4B H 0.5270 0.6976 0.5435 0.044 Uiso 1 calc . . R .


_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
Ce1 Ce1 4.124(2) 3_666 ?
Ce1 K2 4.054(6) . ?
Ce1 O18 2.523(14) . ?
Ce1 O21 2.481(13) . ?
Ce1 O30 2.513(13) . ?
Ce1 O38 2.483(13) . ?
Ce1 O40 2.482(14) 3_666 ?
Ce1 O41 2.488(13) . ?
Ce1 O42 2.774(14) 3_666 ?
Ce1 O42 2.484(14) . ?
Ce1 O43 2.520(14) 3_666 ?
Ce1 C3 3.00(2) 3_666 ?
B1 O5 1.51(2) . ?
B1 O6 1.50(2) . ?
B1 O14 1.53(2) . ?
B1 O35 1.50(2) . ?
W1 K1 3.682(6) . ?
W1 K2 3.885(6) . ?
W1 O6 2.488(13) . ?
W1 O19 1.721(14) . ?
W1 O23 1.921(14) . ?
W1 O24 2.021(13) . ?
W1 O25 1.956(13) . ?
W1 O30 1.743(13) . ?
W2 O1 1.708(14) . ?
W2 O10 1.919(13) . ?
W2 O12 1.928(15) . ?
W2 O13 1.900(14) . ?
W2 O14 2.390(12) . ?
W2 O26 1.814(14) . ?
W3 K2 3.665(6) . ?
W3 O7 1.968(13) . ?
W3 O9 2.049(13) . ?
W3 O18 1.732(14) . ?
W3 O33 1.926(15) . ?
W3 O35 2.372(13) . ?
W3 O39 1.700(14) . ?
W4 K2 3.870(6) . ?
W4 O4 1.691(15) . ?
W4 O7 1.894(14) . ?
W4 O20 1.881(14) . ?
W4 O25 1.870(13) . ?
W4 O35 2.374(14) . ?
W4 O36 1.904(14) . ?
W5 O3 1.731(16) . ?
W5 O5 2.401(13) . ?
W5 O16 1.963(14) . ?
W5 O17 2.016(14) . ?
W5 O21 1.729(13) . ?
W5 O33 1.900(14) . ?
W6 O8 1.908(15) . ?
W6 O9 1.837(13) . ?
W6 O20 1.955(14) . ?
W6 O31 1.904(14) . ?
W6 O35 2.316(14) . ?
W6 O37 1.693(15) . ?
W7 O2 1.695(14) . ?
W7 O5 2.383(15) . ?
W7 O11 1.901(15) . ?
W7 O13 1.905(13) . ?
W7 O16 1.891(15) . ?
W7 O34 1.890(13) . ?
W8 O6 2.462(13) . ?
W8 O23 1.877(14) . ?
W8 O26 2.016(14) . ?
W8 O32 1.712(13) . ?
W8 O34 1.934(13) . ?
W8 O38 1.771(13) . ?
W9 O5 2.308(13) . ?
W9 O8 1.892(15) . ?
W9 O11 1.955(15) . ?
W9 O15 1.696(13) . ?
W9 O17 1.903(14) . ?
W9 O22 1.938(14) . ?
W10 O12 1.917(15) . ?
W10 O14 2.381(12) . ?
W10 O24 1.837(13) . ?
W10 O28 1.963(14) . ?
W10 O29 1.723(15) . ?
W10 O36 1.896(13) . ?
W11 O10 1.958(14) . ?
W11 O14 2.308(12) . ?
W11 O22 1.887(14) . ?
W11 O27 1.740(13) . ?
W11 O28 1.895(14) . ?
W11 O31 1.927(14) . ?
Na1 O1W 2.65(2) . ?
Na1 O5W 2.72(3) . ?
Na1 O13W 3.00(5) 4_576 ?
Na1 O11 2.795(18) . ?
Na1 O13 2.843(19) . ?
Na1 O19 2.645(18) 2 ?
Na1 O22 3.00(2) . ?
Na2 O7W 2.76(3) . ?
Na2 O13W 2.91(5) . ?
Na2 O2 2.782(17) 4_575 ?
Na2 O20 2.902(16) . ?
Na2 O31 2.989(16) . ?
Na2 O36 2.912(15) . ?
K1 K2 4.311(7) . ?
K1 O6W 2.80(3) . ?
K1 O10W 2.72(2) . ?
K1 O19 3.072(14) . ?
K1 O27 2.903(14) 2_545 ?
K1 O30 2.817(14) . ?
K1 O32 2.768(14) 3_566 ?
K1 O41 2.905(16) . ?
K1 O43 3.422(16) 3_666 ?
K2 O2W 2.77(2) . ?
K2 O10W 2.689(19) . ?
K2 O7 2.853(14) . ?
K2 O15 2.889(15) 2_645 ?
K2 O18 2.865(17) . ?
K2 O25 2.980(14) . ?
K2 O30 3.081(15) . ?
K2 O43 2.678(15) 3_666 ?
O1W O14W 1.78(5) 2 ?
O11W O12W 1.10(6) 1_655 ?
O12W O11W 1.10(5) 1_455 ?
O13W Na1 3.00(5) 4_575 ?
O14W O1W 1.78(5) 2_545 ?
O2 Na2 2.782(17) 4_576 ?
O15 K2 2.889(15) 2_655 ?
O19 Na1 2.645(18) 2_545 ?
O27 K1 2.903(14) 2 ?
O32 K1 2.768(14) 3_566 ?
O40 Ce1 2.482(14) 3_666 ?
O40 C2 1.23(2) . ?
O41 C2 1.29(2) . ?
O42 Ce1 2.774(14) 3_666 ?
O42 C3 1.24(2) . ?
O43 Ce1 2.520(14) 3_666 ?
O43 K1 3.422(16) 3_666 ?
O43 K2 2.678(15) 3_666 ?
O43 C3 1.26(2) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N1 C1 1.45(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.48(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.53(3) . ?
C3 Ce1 3.00(2) 3_666 ?
C3 C4 1.49(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
K2 Ce1 Ce1 122.15(9) . 3_666 ?
O18 Ce1 Ce1 135.7(3) . 3_666 ?
O18 Ce1 K2 44.5(4) . . ?
O18 Ce1 O42 113.4(5) . 3_666 ?
O18 Ce1 C3 98.2(5) . 3_666 ?
O21 Ce1 Ce1 111.8(3) . 3_666 ?
O21 Ce1 K2 109.6(3) . . ?
O21 Ce1 O18 65.7(5) . . ?
O21 Ce1 O30 103.7(4) . . ?
O21 Ce1 O38 69.3(5) . . ?
O21 Ce1 O40 72.0(5) . 3_666 ?
O21 Ce1 O41 140.4(5) . . ?
O21 Ce1 O42 79.1(5) . . ?
O21 Ce1 O42 136.1(5) . 3_666 ?
O21 Ce1 O43 144.4(5) . 3_666 ?
O21 Ce1 C3 148.5(5) . 3_666 ?
O30 Ce1 Ce1 143.2(3) . 3_666 ?
O30 Ce1 K2 49.4(3) . . ?
O30 Ce1 O18 68.5(4) . . ?
O30 Ce1 O42 116.8(4) . 3_666 ?
O30 Ce1 O43 71.8(4) . 3_666 ?
O30 Ce1 C3 94.0(5) . 3_666 ?
O38 Ce1 Ce1 112.9(3) . 3_666 ?
O38 Ce1 K2 118.5(3) . . ?
O38 Ce1 O18 107.1(5) . . ?
O38 Ce1 O30 70.5(5) . . ?
O38 Ce1 O41 74.6(5) . . ?
O38 Ce1 O42 138.6(4) . 3_666 ?
O38 Ce1 O42 78.9(4) . . ?
O38 Ce1 O43 135.0(5) . 3_666 ?
O38 Ce1 C3 142.0(5) . 3_666 ?
O40 Ce1 Ce1 65.6(3) 3_666 3_666 ?
O40 Ce1 K2 91.8(3) 3_666 . ?
O40 Ce1 O18 72.4(5) 3_666 . ?
O40 Ce1 O30 138.3(5) 3_666 . ?
O40 Ce1 O38 136.9(5) 3_666 . ?
O40 Ce1 O41 131.8(5) 3_666 . ?
O40 Ce1 O42 66.8(5) 3_666 3_666 ?
O40 Ce1 O42 75.7(5) 3_666 . ?
O40 Ce1 O43 88.1(5) 3_666 3_666 ?
O40 Ce1 C3 77.4(5) 3_666 3_666 ?
O41 Ce1 Ce1 68.1(3) . 3_666 ?
O41 Ce1 K2 101.5(4) . . ?
O41 Ce1 O18 143.5(5) . . ?
O41 Ce1 O30 78.4(4) . . ?
O41 Ce1 O42 68.0(4) . 3_666 ?
O41 Ce1 O43 74.6(5) . 3_666 ?
O41 Ce1 C3 68.2(5) . 3_666 ?
O42 Ce1 Ce1 40.9(3) . 3_666 ?
O42 Ce1 Ce1 35.9(3) 3_666 3_666 ?
O42 Ce1 K2 86.5(3) 3_666 . ?
O42 Ce1 K2 162.1(3) . . ?
O42 Ce1 O18 138.1(5) . . ?
O42 Ce1 O30 145.6(4) . . ?
O42 Ce1 O41 78.5(5) . . ?
O42 Ce1 O42 76.8(5) . 3_666 ?
O42 Ce1 O43 125.0(5) . 3_666 ?
O42 Ce1 C3 100.7(5) . 3_666 ?
O42 Ce1 C3 24.4(5) 3_666 3_666 ?
O43 Ce1 Ce1 84.4(3) 3_666 3_666 ?
O43 Ce1 K2 40.2(3) 3_666 . ?
O43 Ce1 O18 80.5(5) 3_666 . ?
O43 Ce1 O42 48.8(4) 3_666 3_666 ?
O43 Ce1 C3 24.5(5) 3_666 3_666 ?
C3 Ce1 Ce1 59.9(4) 3_666 3_666 ?
C3 Ce1 K2 63.5(4) 3_666 . ?
O5 B1 O14 109.2(14) . . ?
O6 B1 O5 107.5(13) . . ?
O6 B1 O14 104.4(14) . . ?
O35 B1 O5 113.6(15) . . ?
O35 B1 O6 110.0(14) . . ?
O35 B1 O14 111.7(13) . . ?
K1 W1 K2 69.41(11) . . ?
O6 W1 K1 126.5(3) . . ?
O6 W1 K2 97.1(3) . . ?
O19 W1 K1 56.0(4) . . ?
O19 W1 K2 89.7(4) . . ?
O19 W1 O6 173.2(5) . . ?
O19 W1 O23 101.2(6) . . ?
O19 W1 O24 98.6(6) . . ?
O19 W1 O25 101.3(6) . . ?
O19 W1 O30 101.2(6) . . ?
O23 W1 K1 87.1(4) . . ?
O23 W1 K2 142.5(4) . . ?
O23 W1 O6 73.3(5) . . ?
O23 W1 O24 83.0(6) . . ?
O23 W1 O25 154.7(6) . . ?
O24 W1 K1 150.4(4) . . ?
O24 W1 K2 131.0(4) . . ?
O24 W1 O6 77.0(5) . . ?
O25 W1 K1 115.1(4) . . ?
O25 W1 K2 48.7(4) . . ?
O25 W1 O6 83.4(5) . . ?
O25 W1 O24 82.5(5) . . ?
O30 W1 K1 47.6(4) . . ?
O30 W1 K2 50.4(5) . . ?
O30 W1 O6 83.3(5) . . ?
O30 W1 O23 92.2(6) . . ?
O30 W1 O24 160.2(6) . . ?
O30 W1 O25 94.5(6) . . ?
O1 W2 O10 98.5(6) . . ?
O1 W2 O12 98.9(7) . . ?
O1 W2 O13 100.8(6) . . ?
O1 W2 O14 170.4(6) . . ?
O1 W2 O26 102.3(6) . . ?
O10 W2 O12 85.9(6) . . ?
O10 W2 O14 74.3(5) . . ?
O12 W2 O14 74.6(5) . . ?
O13 W2 O10 87.1(6) . . ?
O13 W2 O12 159.8(6) . . ?
O13 W2 O14 85.3(5) . . ?
O26 W2 O10 159.2(6) . . ?
O26 W2 O12 90.7(6) . . ?
O26 W2 O13 89.2(6) . . ?
O26 W2 O14 85.0(5) . . ?
O7 W3 K2 50.6(4) . . ?
O7 W3 O9 83.5(5) . . ?
O7 W3 O35 74.3(5) . . ?
O9 W3 K2 133.0(4) . . ?
O9 W3 O35 70.9(5) . . ?
O18 W3 K2 49.6(5) . . ?
O18 W3 O7 93.1(6) . . ?
O18 W3 O9 162.4(6) . . ?
O18 W3 O33 93.5(6) . . ?
O18 W3 O35 91.5(6) . . ?
O33 W3 K2 142.3(4) . . ?
O33 W3 O7 159.4(6) . . ?
O33 W3 O9 84.4(5) . . ?
O33 W3 O35 86.0(5) . . ?
O35 W3 K2 100.6(3) . . ?
O39 W3 K2 84.7(5) . . ?
O39 W3 O7 98.6(7) . . ?
O39 W3 O9 94.7(6) . . ?
O39 W3 O18 103.0(7) . . ?
O39 W3 O33 98.9(7) . . ?
O39 W3 O35 164.3(6) . . ?
O4 W4 K2 84.3(5) . . ?
O4 W4 O7 98.8(7) . . ?
O4 W4 O20 99.8(7) . . ?
O4 W4 O25 99.1(7) . . ?
O4 W4 O35 172.1(6) . . ?
O4 W4 O36 99.5(7) . . ?
O7 W4 K2 44.7(4) . . ?
O7 W4 O35 75.5(5) . . ?
O7 W4 O36 161.7(6) . . ?
O20 W4 K2 133.4(4) . . ?
O20 W4 O7 89.2(6) . . ?
O20 W4 O35 74.9(6) . . ?
O20 W4 O36 88.6(6) . . ?
O25 W4 K2 48.5(4) . . ?
O25 W4 O7 87.3(6) . . ?
O25 W4 O20 161.0(6) . . ?
O25 W4 O35 86.2(5) . . ?
O25 W4 O36 88.9(5) . . ?
O35 W4 K2 95.1(3) . . ?
O36 W4 K2 136.9(4) . . ?
O36 W4 O35 86.4(5) . . ?
O3 W5 O5 167.4(6) . . ?
O3 W5 O16 99.7(7) . . ?
O3 W5 O17 95.9(7) . . ?
O3 W5 O33 97.8(7) . . ?
O16 W5 O5 74.7(5) . . ?
O16 W5 O17 84.5(6) . . ?
O17 W5 O5 72.5(5) . . ?
O21 W5 O3 103.5(7) . . ?
O21 W5 O5 88.0(6) . . ?
O21 W5 O16 91.6(6) . . ?
O21 W5 O17 160.5(6) . . ?
O21 W5 O33 94.3(6) . . ?
O33 W5 O5 86.1(6) . . ?
O33 W5 O16 159.7(6) . . ?
O33 W5 O17 83.5(6) . . ?
O8 W6 O20 160.6(6) . . ?
O8 W6 O35 86.5(6) . . ?
O9 W6 O8 91.7(6) . . ?
O9 W6 O20 89.7(6) . . ?
O9 W6 O31 160.3(6) . . ?
O9 W6 O35 75.7(5) . . ?
O20 W6 O35 75.1(5) . . ?
O31 W6 O8 85.9(6) . . ?
O31 W6 O20 86.3(6) . . ?
O31 W6 O35 84.6(5) . . ?
O37 W6 O8 100.7(7) . . ?
O37 W6 O9 101.2(6) . . ?
O37 W6 O20 98.0(7) . . ?
O37 W6 O31 98.5(6) . . ?
O37 W6 O35 172.3(6) . . ?
O2 W7 O5 170.1(6) . . ?
O2 W7 O11 97.4(7) . . ?
O2 W7 O13 101.4(7) . . ?
O2 W7 O16 97.8(7) . . ?
O2 W7 O34 101.8(7) . . ?
O11 W7 O5 74.6(5) . . ?
O11 W7 O13 86.3(6) . . ?
O13 W7 O5 84.2(5) . . ?
O16 W7 O5 76.3(5) . . ?
O16 W7 O11 88.0(6) . . ?
O16 W7 O13 160.5(6) . . ?
O34 W7 O5 86.4(5) . . ?
O34 W7 O11 160.7(6) . . ?
O34 W7 O13 88.1(6) . . ?
O34 W7 O16 91.1(6) . . ?
O23 W8 O6 74.6(5) . . ?
O23 W8 O26 85.7(6) . . ?
O23 W8 O34 154.6(6) . . ?
O26 W8 O6 77.4(5) . . ?
O32 W8 O6 172.3(5) . . ?
O32 W8 O23 100.7(6) . . ?
O32 W8 O26 96.4(6) . . ?
O32 W8 O34 102.1(6) . . ?
O32 W8 O38 101.8(6) . . ?
O34 W8 O6 81.5(5) . . ?
O34 W8 O26 80.8(5) . . ?
O38 W8 O6 84.8(5) . . ?
O38 W8 O23 94.3(6) . . ?
O38 W8 O26 161.5(6) . . ?
O38 W8 O34 91.9(6) . . ?
O8 W9 O5 86.1(6) . . ?
O8 W9 O11 160.9(6) . . ?
O8 W9 O17 89.5(6) . . ?
O8 W9 O22 85.0(6) . . ?
O11 W9 O5 75.5(6) . . ?
O15 W9 O5 171.7(6) . . ?
O15 W9 O8 101.1(7) . . ?
O15 W9 O11 97.6(7) . . ?
O15 W9 O17 99.2(7) . . ?
O15 W9 O22 100.5(6) . . ?
O17 W9 O5 76.6(6) . . ?
O17 W9 O11 91.3(6) . . ?
O17 W9 O22 160.2(6) . . ?
O22 W9 O5 84.0(5) . . ?
O22 W9 O11 87.8(6) . . ?
O12 W10 O14 75.0(5) . . ?
O12 W10 O28 86.0(6) . . ?
O24 W10 O12 91.2(6) . . ?
O24 W10 O14 85.0(5) . . ?
O24 W10 O28 157.5(6) . . ?
O24 W10 O36 88.8(6) . . ?
O28 W10 O14 72.7(5) . . ?
O29 W10 O12 98.4(7) . . ?
O29 W10 O14 169.8(6) . . ?
O29 W10 O24 103.0(6) . . ?
O29 W10 O28 99.5(6) . . ?
O29 W10 O36 100.1(7) . . ?
O36 W10 O12 161.0(6) . . ?
O36 W10 O14 86.1(5) . . ?
O36 W10 O28 86.8(6) . . ?
O10 W11 O14 75.6(5) . . ?
O22 W11 O10 89.8(6) . . ?
O22 W11 O14 86.0(5) . . ?
O22 W11 O28 161.4(6) . . ?
O22 W11 O31 87.0(6) . . ?
O27 W11 O10 98.0(6) . . ?
O27 W11 O14 171.2(6) . . ?
O27 W11 O22 100.0(6) . . ?
O27 W11 O28 98.5(6) . . ?
O27 W11 O31 101.1(6) . . ?
O28 W11 O10 88.0(6) . . ?
O28 W11 O14 75.6(5) . . ?
O28 W11 O31 89.0(6) . . ?
O31 W11 O10 160.9(5) . . ?
O31 W11 O14 85.4(5) . . ?
O1W Na1 O5W 66.4(7) . . ?
O1W Na1 O13W 90.3(11) . 4_576 ?
O1W Na1 O11 62.7(6) . . ?
O1W Na1 O13 106.2(6) . . ?
O1W Na1 O22 107.2(7) . . ?
O5W Na1 O13W 152.4(12) . 4_576 ?
O5W Na1 O11 88.2(7) . . ?
O5W Na1 O13 137.7(7) . . ?
O5W Na1 O22 76.9(6) . . ?
O11 Na1 O13W 94.1(10) . 4_576 ?
O11 Na1 O13 55.0(5) . . ?
O11 Na1 O22 55.4(5) . . ?
O13 Na1 O13W 61.0(10) . 4_576 ?
O13 Na1 O22 65.4(5) . . ?
O19 Na1 O1W 123.8(7) 2 . ?
O19 Na1 O5W 68.7(6) 2 . ?
O19 Na1 O13W 118.2(11) 2 4_576 ?
O19 Na1 O11 145.7(7) 2 . ?
O19 Na1 O13 129.8(7) 2 . ?
O19 Na1 O22 93.6(6) 2 . ?
O22 Na1 O13W 126.4(11) . 4_576 ?
O7W Na2 O13W 62.1(12) . . ?
O7W Na2 O2 73.6(8) . 4_575 ?
O7W Na2 O20 140.4(8) . . ?
O7W Na2 O31 90.2(8) . . ?
O7W Na2 O36 129.2(8) . . ?
O13W Na2 O31 145.8(10) . . ?
O2 Na2 O13W 65.8(11) 4_575 . ?
O2 Na2 O20 88.9(5) 4_575 . ?
O2 Na2 O31 88.3(5) 4_575 . ?
O2 Na2 O36 142.4(5) 4_575 . ?
O20 Na2 O13W 141.3(11) . . ?
O20 Na2 O31 53.2(4) . . ?
O20 Na2 O36 54.1(4) . . ?
O36 Na2 O13W 147.7(11) . . ?
O36 Na2 O31 65.3(4) . . ?
Ce1 K1 K2 56.74(10) . . ?
W1 K1 Ce1 61.46(8) . . ?
W1 K1 K2 57.51(10) . . ?
O6W K1 Ce1 104.1(6) . . ?
O6W K1 W1 163.1(6) . . ?
O6W K1 K2 108.0(6) . . ?
O6W K1 O19 161.3(6) . . ?
O6W K1 O27 95.8(6) . 2_545 ?
O6W K1 O30 136.7(7) . . ?
O6W K1 O41 81.7(6) . . ?
O6W K1 O43 82.6(6) . 3_666 ?
O10W K1 Ce1 93.0(4) . . ?
O10W K1 W1 78.6(4) . . ?
O10W K1 K2 36.9(4) . . ?
O10W K1 O6W 94.3(7) . . ?
O10W K1 O19 71.2(5) . . ?
O10W K1 O27 80.1(5) . 2_545 ?
O10W K1 O30 78.7(5) . . ?
O10W K1 O32 142.8(5) . 3_566 ?
O10W K1 O41 121.7(5) . . ?
O10W K1 O43 65.1(5) . 3_666 ?
O19 K1 Ce1 88.8(3) . . ?
O19 K1 W1 27.7(3) . . ?
O19 K1 K2 67.7(3) . . ?
O19 K1 O43 101.0(4) . 3_666 ?
O27 K1 Ce1 159.3(3) 2_545 . ?
O27 K1 W1 98.0(3) 2_545 . ?
O27 K1 K2 112.1(3) 2_545 . ?
O27 K1 O19 70.5(4) 2_545 . ?
O27 K1 O41 158.2(4) 2_545 . ?
O27 K1 O43 144.9(4) 2_545 3_666 ?
O30 K1 Ce1 35.2(3) . . ?
O30 K1 W1 27.2(3) . . ?
O30 K1 K2 45.5(3) . . ?
O30 K1 O19 53.8(4) . . ?
O30 K1 O27 124.2(4) . 2_545 ?
O30 K1 O41 67.1(4) . . ?
O30 K1 O43 55.4(4) . 3_666 ?
O32 K1 Ce1 123.1(3) 3_566 . ?
O32 K1 W1 109.2(3) 3_566 . ?
O32 K1 K2 166.0(4) 3_566 . ?
O32 K1 O6W 85.8(7) 3_566 . ?
O32 K1 O19 98.5(4) 3_566 . ?
O32 K1 O27 62.9(4) 3_566 2_545 ?
O32 K1 O30 124.8(5) 3_566 . ?
O32 K1 O41 95.2(4) 3_566 . ?
O32 K1 O43 150.8(4) 3_566 3_666 ?
O41 K1 Ce1 35.1(3) . . ?
O41 K1 W1 89.0(3) . . ?
O41 K1 K2 89.2(3) . . ?
O41 K1 O19 115.8(4) . . ?
O41 K1 O43 56.6(4) . 3_666 ?
O43 K1 Ce1 36.7(2) 3_666 . ?
O43 K1 W1 80.5(3) 3_666 . ?
O43 K1 K2 38.4(2) 3_666 . ?
W1 K2 Ce1 61.53(9) . . ?
W3 K2 Ce1 65.25(9) . . ?
W3 K2 W1 79.02(11) . . ?
W3 K2 W4 52.69(8) . . ?
W4 K2 Ce1 96.35(12) . . ?
W4 K2 W1 57.06(8) . . ?
O2W K2 Ce1 174.6(5) . . ?
O2W K2 W1 114.7(5) . . ?
O2W K2 W3 110.8(5) . . ?
O2W K2 W4 78.2(5) . . ?
O2W K2 O7 81.7(5) . . ?
O2W K2 O15 88.4(5) . 2_645 ?
O2W K2 O18 137.6(6) . . ?
O2W K2 O25 93.5(5) . . ?
O2W K2 O30 138.9(5) . . ?
O10W K2 Ce1 97.1(4) . . ?
O10W K2 W1 75.2(4) . . ?
O10W K2 W3 153.6(5) . . ?
O10W K2 W4 114.5(4) . . ?
O10W K2 O2W 85.3(6) . . ?
O10W K2 O7 142.1(5) . . ?
O10W K2 O15 107.5(5) . 2_645 ?
O10W K2 O18 130.5(5) . . ?
O10W K2 O25 92.9(5) . . ?
O10W K2 O30 74.6(5) . . ?
O7 K2 Ce1 93.5(3) . . ?
O7 K2 W1 78.3(3) . . ?
O7 K2 W3 32.2(3) . . ?
O7 K2 W4 27.8(3) . . ?
O7 K2 O15 107.5(4) . 2_645 ?
O7 K2 O18 56.1(4) . . ?
O7 K2 O25 52.9(4) . . ?
O7 K2 O30 92.6(4) . . ?
O15 K2 Ce1 95.5(3) 2_645 . ?
O15 K2 W1 156.9(3) 2_645 . ?
O15 K2 W3 94.1(3) 2_645 . ?
O15 K2 W4 134.3(3) 2_645 . ?
O15 K2 O25 159.5(4) 2_645 . ?
O15 K2 O30 131.5(4) 2_645 . ?
O18 K2 Ce1 38.1(3) . . ?
O18 K2 W1 65.4(3) . . ?
O18 K2 W3 27.4(3) . . ?
O18 K2 W4 66.9(3) . . ?
O18 K2 O15 98.7(4) . 2_645 ?
O18 K2 O25 66.6(4) . . ?
O18 K2 O30 56.8(4) . . ?
O25 K2 Ce1 81.5(3) . . ?
O25 K2 W1 29.5(3) . . ?
O25 K2 W3 66.1(3) . . ?
O25 K2 W4 28.0(3) . . ?
O25 K2 O30 53.3(4) . . ?
O30 K2 Ce1 38.3(3) . . ?
O30 K2 W1 25.8(2) . . ?
O30 K2 W3 79.8(3) . . ?
O30 K2 W4 78.3(3) . . ?
O43 K2 Ce1 37.4(3) 3_666 . ?
O43 K2 W1 86.8(3) 3_666 . ?
O43 K2 W3 95.9(4) 3_666 . ?
O43 K2 W4 133.5(3) 3_666 . ?
O43 K2 O2W 148.0(6) 3_666 . ?
O43 K2 O10W 77.4(5) 3_666 . ?
O43 K2 O7 127.6(5) 3_666 . ?
O43 K2 O15 71.9(4) 3_666 2_645 ?
O43 K2 O18 71.9(4) 3_666 . ?
O43 K2 O25 113.8(4) 3_666 . ?
O43 K2 O30 61.2(4) 3_666 . ?
O14W O1W Na1 126.1(19) 2 . ?
K2 O10W K1 105.8(7) . . ?
Na2 O13W Na1 129.5(18) . 4_575 ?
W7 O2 Na2 147.6(8) . 4_576 ?
B1 O5 W5 121.9(10) . . ?
B1 O5 W7 127.9(11) . . ?
B1 O5 W9 125.5(10) . . ?
W7 O5 W5 88.5(5) . . ?
W9 O5 W5 91.7(5) . . ?
W9 O5 W7 90.3(5) . . ?
B1 O6 W1 130.0(10) . . ?
B1 O6 W8 133.9(11) . . ?
W8 O6 W1 85.3(4) . . ?
W3 O7 K2 97.3(5) . . ?
W4 O7 W3 120.2(7) . . ?
W4 O7 K2 107.5(5) . . ?
W9 O8 W6 149.9(9) . . ?
W6 O9 W3 121.0(7) . . ?
W2 O10 W11 119.3(7) . . ?
W7 O11 W9 119.2(7) . . ?
W7 O11 Na1 104.6(6) . . ?
W9 O11 Na1 106.8(6) . . ?
W10 O12 W2 121.2(8) . . ?
W2 O13 W7 145.1(8) . . ?
W2 O13 Na1 110.4(6) . . ?
W7 O13 Na1 102.7(6) . . ?
B1 O14 W2 126.2(10) . . ?
B1 O14 W10 125.2(10) . . ?
B1 O14 W11 123.6(10) . . ?
W10 O14 W2 89.1(4) . . ?
W11 O14 W2 90.8(4) . . ?
W11 O14 W10 91.2(4) . . ?
W9 O15 K2 129.0(7) . 2_655 ?
W7 O16 W5 120.1(7) . . ?
W9 O17 W5 119.0(8) . . ?
Ce1 O18 K2 97.4(5) . . ?
W3 O18 Ce1 157.4(8) . . ?
W3 O18 K2 102.9(6) . . ?
W1 O19 Na1 124.6(7) . 2_545 ?
W1 O19 K1 96.3(5) . . ?
Na1 O19 K1 133.7(6) 2_545 . ?
W4 O20 W6 119.8(8) . . ?
W4 O20 Na2 104.1(5) . . ?
W6 O20 Na2 106.1(6) . . ?
W5 O21 Ce1 155.8(8) . . ?
W9 O22 Na1 100.1(6) . . ?
W11 O22 W9 148.4(9) . . ?
W11 O22 Na1 107.3(7) . . ?
W8 O23 W1 124.1(8) . . ?
W10 O24 W1 152.3(8) . . ?
W1 O25 K2 101.8(5) . . ?
W4 O25 W1 150.9(8) . . ?
W4 O25 K2 103.5(5) . . ?
W2 O26 W8 153.7(7) . . ?
W11 O27 K1 137.7(7) . 2 ?
W11 O28 W10 120.5(7) . . ?
Ce1 O30 K1 104.5(4) . . ?
Ce1 O30 K2 92.3(4) . . ?
W1 O30 Ce1 144.8(7) . . ?
W1 O30 K1 105.3(6) . . ?
W1 O30 K2 103.8(5) . . ?
K1 O30 K2 93.8(4) . . ?
W6 O31 W11 147.6(7) . . ?
W6 O31 Na2 104.4(6) . . ?
W11 O31 Na2 104.7(6) . . ?
W8 O32 K1 164.3(7) . 3_566 ?
W5 O33 W3 138.8(8) . . ?
W7 O34 W8 152.9(7) . . ?
B1 O35 W3 123.2(10) . . ?
B1 O35 W4 126.8(11) . . ?
B1 O35 W6 124.3(10) . . ?
W3 O35 W4 89.8(5) . . ?
W6 O35 W3 92.4(5) . . ?
W6 O35 W4 90.0(5) . . ?
W4 O36 Na2 103.1(5) . . ?
W10 O36 W4 145.4(7) . . ?
W10 O36 Na2 108.4(6) . . ?
W8 O38 Ce1 142.6(7) . . ?
C2 O40 Ce1 140.2(13) . 3_666 ?
Ce1 O41 K1 102.7(5) . . ?
C2 O41 Ce1 133.7(13) . . ?
C2 O41 K1 122.3(12) . . ?
Ce1 O42 Ce1 103.2(5) . 3_666 ?
C3 O42 Ce1 88.0(12) . 3_666 ?
C3 O42 Ce1 163.9(14) . . ?
Ce1 O43 K1 89.1(4) 3_666 3_666 ?
Ce1 O43 K2 102.5(5) 3_666 3_666 ?
K2 O43 K1 89.1(4) 3_666 3_666 ?
C3 O43 Ce1 99.5(13) . 3_666 ?
C3 O43 K1 112.6(13) . 3_666 ?
C3 O43 K2 149.3(13) . 3_666 ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
N1 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
N1 C1 C2 110.0(19) . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
O40 C2 O41 125.6(18) . . ?
O40 C2 C1 119.1(18) . . ?
O41 C2 C1 115.3(18) . . ?
O42 C3 Ce1 67.6(12) . 3_666 ?
O42 C3 O43 123(2) . . ?
O42 C3 C4 119.5(19) . . ?
O43 C3 Ce1 56.0(11) . 3_666 ?
O43 C3 C4 117(2) . . ?
C4 C3 Ce1 171.8(15) . 3_666 ?
N2 C4 C3 114(2) . . ?
N2 C4 H4A 108.8 . . ?
N2 C4 H4B 108.8 . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?

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
N1 H1C O12 0.89 2.13 2.93(2) 150.0 3_566
N1 H1C O24 0.89 2.54 3.26(2) 137.4 3_566
N1 H1D O5W 0.89 2.02 2.85(3) 154.9 4_576
N1 H1D O39 0.89 2.51 3.07(3) 120.9 3_666
N1 H1E O3 0.89 2.53 3.25(3) 138.4 3_666
N1 H1E O33 0.89 2.52 3.34(3) 155.0 3_666
N2 H2A O37 0.89 2.10 2.86(3) 144.0 4_576
N2 H2B O3W 0.89 1.95 2.83(3) 168.6 4_576
N2 H2C O16 0.89 2.49 3.01(3) 118.4 .
N2 H2C O21 0.89 2.24 3.13(2) 171.4 .
N2 H2C O38 0.89 2.65 3.07(3) 110.2 .

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1495659'
_audit_update_record             
;
2016-09-05 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT430_5                   
;
PROBLEM: Short Inter D...A Contact O1W    ..  O13W    ..   2.35 Ang.
RESPONSE: In the crystal structure, there are a number of short connections
 between  OW(H2O) and O(POM) or OW(H2O) atoms in the range 2.35-2.84 Ang,
 which indicate extensive H bonding interactions among them.  
;

_vrf_PLAT201_5                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 1 Report 
RESPONSE: Due to the large structure and the existence of a large 
 amount of weight atoms, the intensity data are not very good, 
 leading to the ADP max/min ratio of some water molecules, 
 and it is very difficult to refine this large structure. Therefore,
 in the final refinement, all the W, B, lanthanoid, Na and K atoms 
 were refined anisotropically and some water molecules
 were refined isotropically.
;

_vrf_PLAT220_5                   
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range   8.3 Ratio 
RESPONSE: In polyoxometalate (POM) compounds, the Ueq of oxygen atoms in
 the POM skeleton is small due to multiple covalent bonds, whereas
 the Ueq values of these discrete water oxygen atoms are biggish 
 without the constraint of covalent bonds. 
;

_vrf_PLAT306_5                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check  
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

# end Validation Reply Form


_audit_creation_date             2016-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C16 H40 B4 Eu4 K8 N8 Na8 O198 W44), 10(O)'
_chemical_formula_sum            'C8 H70 B2 Eu2 K4 N4 Na4 O109 W22'
_chemical_formula_weight         6585.28
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        P2(1)/c
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.7069(7)
_cell_length_b                   21.6010(13)
_cell_length_c                   21.3932(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.3710(10)
_cell_angle_gamma                90.00
_cell_volume                     5405.3(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8905
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.170
_cell_measurement_theta_min      2.166
_exptl_absorpt_coefficient_mu    24.733
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1368 before and 0.0571 after correction. 
The Ratio of minimum to maximum transmission is 0.4070. 
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.046
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5804
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
Thanks to the large structure of 5 and the existence of a 
large amount of weight atoms, the intensity data are not 
very good, leading to the ADP max/min ratio of some atoms,
and it is very difficult to refine this large structure,
therefore, some unit-occupancy atoms have been refined 
isotropically and restrainedly refined. The ISOR 
instruction is used for O23, O31, O33 and B1. 
O6W-O9W and O11W-O14W are refined isostropicallly. 
681 parameters and 24 restraints are used in the 
refinement. In addition, the specific reason why
 that the Ueq value of the B1 atom is extremely 
small is well understood and may be related to 
the fact that the atomic weight of the B1 atom 
is very small in contrast to other atoms in the 
structure. This phenomenon is already encountered 
in other borotungstates (H. An, Z. Han and T. Xu, 
Inorg. Chem., 2010, 49, 11403; J. Niu, J. Zhao, 
J. Wang, P. Ma, J. Mol. Struct., 2004, 699, 85). 
This explanation is added to the cif file.  
;
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27009
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         27009
_reflns_number_gt                7737
_reflns_number_total             9396
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         2.145
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.323
_refine_ls_extinction_coef       0.000060(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         9396
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0352
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0399P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0849
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O31) \\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(B1) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: O8W(0.5) O11W(0.5) O12W(0.5) O13W(0.5) O14W(0.5)
 Fixed Uiso: O13W(0.08314)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
4.b Me refined with riding coordinates:
 N1(H1C,H1D,H1E), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Eu1 Eu 0.39214(5) 0.52348(3) 0.42508(3) 0.01055(13) Uani 1 d . . . .
B1 B 0.2181(9) 0.6561(5) 0.2735(5) 0.004(2) Uani 1 d . . . U
W1 W 0.10228(4) 0.50754(2) 0.31988(2) 0.01288(12) Uani 1 d . . . .
W2 W -0.03492(4) 0.72873(2) 0.30882(2) 0.01705(12) Uani 1 d . . . .
W3 W 0.46210(4) 0.57151(2) 0.24437(2) 0.01422(12) Uani 1 d . . . .
W4 W 0.21933(4) 0.53527(2) 0.16422(2) 0.01546(12) Uani 1 d . . . .
W5 W 0.46965(4) 0.69343(2) 0.35674(2) 0.01481(12) Uani 1 d . . . .
W6 W 0.34763(4) 0.66865(2) 0.13452(2) 0.01628(12) Uani 1 d . . . .
W7 W 0.23335(4) 0.77287(2) 0.38727(2) 0.01600(12) Uani 1 d . . . .
W8 W 0.10350(4) 0.62140(2) 0.42567(2) 0.01308(12) Uani 1 d . . . .
W9 W 0.35344(4) 0.79340(2) 0.25065(2) 0.01686(12) Uani 1 d . . . .
W10 W -0.04187(4) 0.61416(2) 0.20331(2) 0.01638(12) Uani 1 d . . . .
W11 W 0.08167(4) 0.74958(2) 0.16992(2) 0.01696(12) Uani 1 d . . . .
Na1 Na 0.0978(7) 0.8970(4) 0.2803(4) 0.073(2) Uani 1 d . . . .
Na2 Na 0.0690(4) 0.6265(2) 0.0327(2) 0.0308(13) Uani 1 d . . . .
K1 K 0.1522(3) 0.37830(14) 0.42572(14) 0.0305(7) Uani 1 d . . . .
K2 K 0.3671(3) 0.41346(14) 0.27142(14) 0.0318(7) Uani 1 d . . . .
O1W O 0.2662(9) 0.9604(4) 0.3328(6) 0.048(3) Uani 1 d . . . .
O2W O 0.3427(10) 0.3475(5) 0.1623(6) 0.063(4) Uani 1 d . . . .
O3W O 0.2064(9) 0.8941(5) 0.0872(5) 0.053(3) Uani 1 d . . . .
O4W O -0.3307(11) 0.7137(6) 0.1950(6) 0.067(4) Uani 1 d . . . .
O5W O 0.2326(11) 0.9604(5) 0.2007(6) 0.063(4) Uani 1 d . . . .
O6W O 0.2618(15) 0.2883(7) 0.4962(8) 0.099(5) Uiso 1 d . . . .
O7W O -0.0385(15) 0.7319(7) -0.0092(8) 0.100(5) Uiso 1 d . . . .
O8W O 0.359(2) 0.5726(12) -0.0150(13) 0.071(7) Uiso 0.50 d . . . .
O9W O 0.544(2) 0.6489(10) -0.0428(11) 0.145(8) Uiso 1 d . . . .
O10W O 0.2258(8) 0.3277(5) 0.3185(5) 0.042(3) Uani 1 d . . . .
O11W O 0.660(2) 0.6389(12) 0.0873(13) 0.074(8) Uiso 0.50 d . . . .
O12W O -0.240(3) 0.6913(15) 0.0753(16) 0.100(10) Uiso 0.50 d . . . .
O13W O -0.245(3) 0.5196(13) 0.0760(14) 0.083 Uiso 0.50 d . . . .
O14W O -0.159(3) 0.5773(14) 0.0129(15) 0.093(10) Uiso 0.50 d . . . .
O1 O -0.1490(7) 0.7674(4) 0.3388(4) 0.025(2) Uani 1 d . . . .
O2 O 0.2139(8) 0.8269(4) 0.4453(4) 0.027(2) Uani 1 d . . . .
O3 O 0.6027(7) 0.7005(4) 0.3930(4) 0.029(2) Uani 1 d . . . .
O4 O 0.1936(8) 0.4747(4) 0.1152(4) 0.029(2) Uani 1 d . . . .
O5 O 0.2869(7) 0.7080(3) 0.3030(4) 0.0141(17) Uani 1 d . . . .
O6 O 0.1951(6) 0.6091(3) 0.3258(3) 0.0117(16) Uani 1 d . . . .
O7 O 0.3730(6) 0.5171(4) 0.1888(4) 0.0169(18) Uani 1 d . . . .
O8 O 0.3902(7) 0.7375(3) 0.1852(4) 0.0193(19) Uani 1 d . . . .
O9 O 0.4726(7) 0.6236(4) 0.1641(4) 0.0206(19) Uani 1 d . . . .
O10 O -0.0201(7) 0.7770(4) 0.2327(4) 0.023(2) Uani 1 d . . . .
O11 O 0.2871(7) 0.8274(3) 0.3239(4) 0.021(2) Uani 1 d . . . .
O12 O -0.1212(6) 0.6699(4) 0.2576(4) 0.0209(19) Uani 1 d . . . .
O13 O 0.0879(7) 0.7761(4) 0.3437(4) 0.0172(18) Uani 1 d . . . .
O14 O 0.1053(6) 0.6782(3) 0.2486(4) 0.0160(18) Uani 1 d . . . .
O15 O 0.4070(7) 0.8610(4) 0.2221(4) 0.026(2) Uani 1 d . . . .
O16 O 0.3875(7) 0.7527(4) 0.4076(4) 0.0190(19) Uani 1 d . . . .
O17 O 0.4786(7) 0.7669(4) 0.2993(4) 0.0217(19) Uani 1 d . . . .
O18 O 0.4095(7) 0.5382(4) 0.3140(4) 0.022(2) Uani 1 d . . . .
O19 O 0.0248(7) 0.4405(4) 0.3199(4) 0.0197(19) Uani 1 d . . . .
O20 O 0.2746(7) 0.5926(4) 0.1049(4) 0.0184(18) Uani 1 d . . . .
O21 O 0.4096(7) 0.6303(4) 0.3954(4) 0.0208(19) Uani 1 d . . . .
O22 O 0.2006(7) 0.7936(3) 0.2123(4) 0.0181(18) Uani 1 d . . . .
O23 O 0.0356(7) 0.5494(4) 0.3870(4) 0.0188(18) Uani 1 d . . . U
O24 O -0.0085(7) 0.5604(4) 0.2679(4) 0.0171(18) Uani 1 d . . . .
O25 O 0.1739(7) 0.5020(4) 0.2421(3) 0.0165(18) Uani 1 d . . . .
O26 O -0.0046(7) 0.6683(4) 0.3674(4) 0.0208(19) Uani 1 d . . . .
O27 O 0.0393(7) 0.8029(4) 0.1124(4) 0.024(2) Uani 1 d . . . .
O28 O -0.0257(7) 0.6860(4) 0.1486(4) 0.0203(19) Uani 1 d . . . .
O29 O -0.1593(7) 0.5809(4) 0.1665(4) 0.025(2) Uani 1 d . . . .
O30 O 0.2264(7) 0.4857(4) 0.3660(4) 0.0179(18) Uani 1 d . . . .
O31 O 0.1963(7) 0.7048(3) 0.1290(4) 0.0166(18) Uani 1 d . . . U
O32 O 0.0229(7) 0.6273(4) 0.4909(4) 0.0188(18) Uani 1 d . . . .
O33 O 0.5091(7) 0.6454(3) 0.2863(4) 0.0183(18) Uani 1 d . . . U
O34 O 0.1841(6) 0.7001(3) 0.4249(4) 0.0165(18) Uani 1 d . . . .
O35 O 0.2834(7) 0.6228(4) 0.2247(3) 0.0158(17) Uani 1 d . . . .
O36 O 0.0778(7) 0.5766(4) 0.1579(4) 0.0190(19) Uani 1 d . . . .
O37 O 0.3963(8) 0.6932(4) 0.0631(4) 0.026(2) Uani 1 d . . . .
O38 O 0.2262(7) 0.5814(3) 0.4554(4) 0.0171(18) Uani 1 d . . . .
O39 O 0.5914(7) 0.5367(4) 0.2373(4) 0.028(2) Uani 1 d . . . .
O40 O 0.4084(7) 0.4580(4) 0.5907(4) 0.0198(19) Uani 1 d . . . .
O41 O 0.3004(7) 0.4588(4) 0.5022(4) 0.0194(19) Uani 1 d . . . .
O42 O 0.4616(7) 0.5669(4) 0.5215(4) 0.0190(19) Uani 1 d . . . .
O43 O 0.5663(7) 0.5821(4) 0.6077(4) 0.024(2) Uani 1 d . . . .
N1 N 0.2438(10) 0.4149(6) 0.6575(5) 0.040(3) Uani 1 d . . . .
H1C H 0.1826 0.3995 0.6753 0.060 Uiso 1 calc . . R .
H1D H 0.2613 0.4515 0.6744 0.060 Uiso 1 calc . . R .
H1E H 0.3025 0.3891 0.6636 0.060 Uiso 1 calc . . R .
N2 N 0.3671(11) 0.6824(5) 0.5272(5) 0.034(3) Uani 1 d . . . .
H2A H 0.3530 0.7228 0.5295 0.051 Uiso 1 calc . . R .
H2B H 0.3077 0.6614 0.5408 0.051 Uiso 1 calc . . R .
H2C H 0.3786 0.6721 0.4876 0.051 Uiso 1 calc . . R .
C1 C 0.2195(11) 0.4223(6) 0.5913(6) 0.028(3) Uani 1 d . . . .
H1A H 0.1543 0.4496 0.5850 0.033 Uiso 1 calc . . R .
H1B H 0.1990 0.3824 0.5733 0.033 Uiso 1 calc . . R .
C2 C 0.3185(11) 0.4482(6) 0.5575(6) 0.021(3) Uani 1 d . . . .
C3 C 0.4999(10) 0.6015(5) 0.5642(5) 0.014(3) Uani 1 d . . . .
C4 C 0.4678(12) 0.6677(6) 0.5655(7) 0.035(4) Uani 1 d . . . .
H4A H 0.4547 0.6795 0.6083 0.041 Uiso 1 calc . . R .
H4B H 0.5313 0.6921 0.5514 0.041 Uiso 1 calc . . R .


_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
Eu1 Eu1 4.1245(11) 3_666 ?
Eu1 K2 4.057(3) . ?
Eu1 O18 2.414(8) . ?
Eu1 O21 2.404(8) . ?
Eu1 O30 2.414(8) . ?
Eu1 O38 2.421(8) . ?
Eu1 O40 2.407(8) 3_666 ?
Eu1 O41 2.443(8) . ?
Eu1 O42 2.379(8) . ?
Eu1 O42 2.809(8) 3_666 ?
Eu1 O43 2.440(8) 3_666 ?
Eu1 C3 2.987(11) 3_666 ?
B1 O5 1.504(13) . ?
B1 O6 1.542(13) . ?
B1 O14 1.483(13) . ?
B1 O35 1.504(14) . ?
W1 K1 3.627(3) . ?
W1 K2 3.884(3) . ?
W1 O6 2.449(7) . ?
W1 O19 1.709(8) . ?
W1 O23 1.894(8) . ?
W1 O24 2.027(8) . ?
W1 O25 1.898(8) . ?
W1 O30 1.786(8) . ?
W2 O1 1.722(8) . ?
W2 O10 1.947(8) . ?
W2 O12 1.934(8) . ?
W2 O13 1.892(8) . ?
W2 O14 2.392(8) . ?
W2 O26 1.834(8) . ?
W3 K2 3.644(3) . ?
W3 O7 1.944(7) . ?
W3 O9 2.061(8) . ?
W3 O18 1.787(8) . ?
W3 O33 1.901(8) . ?
W3 O35 2.389(8) . ?
W3 O39 1.702(8) . ?
W4 K2 3.854(3) . ?
W4 O4 1.696(9) . ?
W4 O7 1.894(7) . ?
W4 O20 1.905(8) . ?
W4 O25 1.910(8) . ?
W4 O35 2.394(8) . ?
W4 O36 1.882(8) . ?
W5 O3 1.718(8) . ?
W5 O5 2.406(7) . ?
W5 O16 1.959(8) . ?
W5 O17 2.014(8) . ?
W5 O21 1.756(8) . ?
W5 O33 1.901(8) . ?
W6 O8 1.895(8) . ?
W6 O9 1.846(8) . ?
W6 O20 1.946(8) . ?
W6 O31 1.936(8) . ?
W6 O35 2.321(8) . ?
W6 O37 1.736(9) . ?
W7 O2 1.725(8) . ?
W7 O5 2.387(8) . ?
W7 O11 1.921(8) . ?
W7 O13 1.908(7) . ?
W7 O16 1.889(8) . ?
W7 O34 1.868(8) . ?
W8 O6 2.444(8) . ?
W8 O23 1.918(8) . ?
W8 O26 2.013(8) . ?
W8 O32 1.722(8) . ?
W8 O34 1.945(8) . ?
W8 O38 1.772(7) . ?
W9 O5 2.311(7) . ?
W9 O8 1.911(8) . ?
W9 O11 1.924(8) . ?
W9 O15 1.712(8) . ?
W9 O17 1.852(8) . ?
W9 O22 1.937(8) . ?
W10 O12 1.938(9) . ?
W10 O14 2.384(7) . ?
W10 O24 1.833(8) . ?
W10 O28 1.957(8) . ?
W10 O29 1.713(8) . ?
W10 O36 1.918(8) . ?
W11 O10 1.926(9) . ?
W11 O14 2.291(7) . ?
W11 O22 1.887(8) . ?
W11 O27 1.743(8) . ?
W11 O28 1.905(8) . ?
W11 O31 1.896(8) . ?
Na1 O1W 2.616(13) . ?
Na1 O5W 2.737(16) . ?
Na1 O11 2.806(11) . ?
Na1 O13 2.947(11) . ?
Na1 O19 2.699(10) 2 ?
Na1 O22 2.948(12) . ?
Na2 O7W 2.735(17) . ?
Na2 O14W 2.88(3) . ?
Na2 O2 2.767(10) 4_575 ?
Na2 O20 2.899(9) . ?
Na2 O31 3.012(9) . ?
Na2 O36 2.884(9) . ?
K1 K2 4.301(5) . ?
K1 O6W 2.746(16) . ?
K1 O10W 2.714(11) . ?
K1 O19 2.979(8) . ?
K1 O27 2.862(9) 2_545 ?
K1 O30 2.804(8) . ?
K1 O32 2.774(9) 3_566 ?
K1 O41 2.911(9) . ?
K2 O2W 2.740(13) . ?
K2 O10W 2.706(11) . ?
K2 O7 2.854(8) . ?
K2 O15 2.874(9) 2_645 ?
K2 O18 2.881(9) . ?
K2 O25 3.009(9) . ?
K2 O30 3.085(9) . ?
K2 O43 2.671(8) 3_666 ?
O11W O12W 1.65(4) 1_655 ?
O12W O11W 1.65(4) 1_455 ?
O2 Na2 2.767(10) 4_576 ?
O15 K2 2.874(9) 2_655 ?
O19 Na1 2.699(10) 2_545 ?
O27 K1 2.862(9) 2 ?
O32 K1 2.774(9) 3_566 ?
O40 Eu1 2.407(8) 3_666 ?
O40 C2 1.263(14) . ?
O41 C2 1.216(14) . ?
O42 Eu1 2.809(8) 3_666 ?
O42 C3 1.250(13) . ?
O43 Eu1 2.440(8) 3_666 ?
O43 K2 2.671(8) 3_666 ?
O43 C3 1.259(13) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N1 C1 1.442(17) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.442(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.500(17) . ?
C3 Eu1 2.987(11) 3_666 ?
C3 C4 1.478(17) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
K2 Eu1 Eu1 120.46(5) . 3_666 ?
O18 Eu1 Eu1 136.3(2) . 3_666 ?
O18 Eu1 K2 44.4(2) . . ?
O18 Eu1 O38 107.3(3) . . ?
O18 Eu1 O41 142.8(3) . . ?
O18 Eu1 O42 114.6(3) . 3_666 ?
O18 Eu1 O43 79.3(3) . 3_666 ?
O18 Eu1 C3 98.1(3) . 3_666 ?
O21 Eu1 Eu1 112.69(19) . 3_666 ?
O21 Eu1 K2 110.6(2) . . ?
O21 Eu1 O18 66.5(3) . . ?
O21 Eu1 O30 105.1(3) . . ?
O21 Eu1 O38 69.7(3) . . ?
O21 Eu1 O40 73.2(3) . 3_666 ?
O21 Eu1 O41 140.5(3) . . ?
O21 Eu1 O42 135.9(3) . 3_666 ?
O21 Eu1 O43 143.2(3) . 3_666 ?
O21 Eu1 C3 148.0(3) . 3_666 ?
O30 Eu1 Eu1 140.99(19) . 3_666 ?
O30 Eu1 K2 49.3(2) . . ?
O30 Eu1 O18 68.1(3) . . ?
O30 Eu1 O38 71.2(3) . . ?
O30 Eu1 O41 78.1(3) . . ?
O30 Eu1 O42 116.2(2) . 3_666 ?
O30 Eu1 O43 72.5(3) . 3_666 ?
O30 Eu1 C3 93.6(3) . 3_666 ?
O38 Eu1 Eu1 113.03(18) . 3_666 ?
O38 Eu1 K2 119.19(19) . . ?
O38 Eu1 O41 74.6(3) . . ?
O38 Eu1 O42 137.1(2) . 3_666 ?
O38 Eu1 O43 137.0(3) . 3_666 ?
O38 Eu1 C3 142.0(3) . 3_666 ?
O40 Eu1 Eu1 65.40(19) 3_666 3_666 ?
O40 Eu1 K2 91.2(2) 3_666 . ?
O40 Eu1 O18 73.6(3) 3_666 . ?
O40 Eu1 O30 138.2(3) 3_666 . ?
O40 Eu1 O38 138.2(3) 3_666 . ?
O40 Eu1 O41 130.2(3) 3_666 . ?
O40 Eu1 O42 66.0(3) 3_666 3_666 ?
O40 Eu1 O43 84.8(3) 3_666 3_666 ?
O40 Eu1 C3 75.6(3) 3_666 3_666 ?
O41 Eu1 Eu1 66.87(19) . 3_666 ?
O41 Eu1 K2 101.1(2) . . ?
O41 Eu1 O42 66.8(3) . 3_666 ?
O41 Eu1 C3 68.2(3) . 3_666 ?
O42 Eu1 Eu1 33.85(16) 3_666 3_666 ?
O42 Eu1 Eu1 41.12(19) . 3_666 ?
O42 Eu1 K2 86.83(16) 3_666 . ?
O42 Eu1 K2 160.8(2) . . ?
O42 Eu1 O18 139.6(3) . . ?
O42 Eu1 O21 79.7(3) . . ?
O42 Eu1 O30 145.7(3) . . ?
O42 Eu1 O38 79.2(3) . . ?
O42 Eu1 O40 76.0(3) . 3_666 ?
O42 Eu1 O41 77.5(3) . . ?
O42 Eu1 O42 75.0(3) . 3_666 ?
O42 Eu1 O43 123.6(3) . 3_666 ?
O42 Eu1 C3 99.3(3) . 3_666 ?
O42 Eu1 C3 24.7(3) 3_666 3_666 ?
O43 Eu1 Eu1 82.57(18) 3_666 3_666 ?
O43 Eu1 K2 39.50(19) 3_666 . ?
O43 Eu1 O41 76.0(3) 3_666 . ?
O43 Eu1 O42 48.8(2) 3_666 3_666 ?
O43 Eu1 C3 24.3(3) 3_666 3_666 ?
C3 Eu1 Eu1 58.3(2) 3_666 3_666 ?
C3 Eu1 K2 63.1(2) 3_666 . ?
O5 B1 O6 107.0(8) . . ?
O14 B1 O5 111.4(8) . . ?
O14 B1 O6 107.1(8) . . ?
O14 B1 O35 112.0(8) . . ?
O35 B1 O5 111.6(8) . . ?
O35 B1 O6 107.4(8) . . ?
K1 W1 K2 69.77(7) . . ?
O6 W1 K1 126.70(17) . . ?
O6 W1 K2 97.19(18) . . ?
O19 W1 K1 54.5(3) . . ?
O19 W1 K2 89.2(3) . . ?
O19 W1 O6 173.4(3) . . ?
O19 W1 O23 99.7(4) . . ?
O19 W1 O24 98.6(3) . . ?
O19 W1 O25 101.6(4) . . ?
O19 W1 O30 101.3(4) . . ?
O23 W1 K1 87.4(2) . . ?
O23 W1 K2 144.2(2) . . ?
O23 W1 O6 74.3(3) . . ?
O23 W1 O24 82.7(3) . . ?
O23 W1 O25 155.0(3) . . ?
O24 W1 K1 149.3(2) . . ?
O24 W1 K2 130.4(2) . . ?
O24 W1 O6 78.2(3) . . ?
O25 W1 K1 115.7(2) . . ?
O25 W1 K2 49.2(2) . . ?
O25 W1 O6 83.7(3) . . ?
O25 W1 O24 81.4(3) . . ?
O30 W1 K1 49.1(3) . . ?
O30 W1 K2 50.8(3) . . ?
O30 W1 O6 81.9(3) . . ?
O30 W1 O23 93.4(3) . . ?
O30 W1 O24 160.1(3) . . ?
O30 W1 O25 95.1(4) . . ?
O1 W2 O10 98.5(4) . . ?
O1 W2 O12 97.7(4) . . ?
O1 W2 O13 100.3(4) . . ?
O1 W2 O14 169.2(3) . . ?
O1 W2 O26 102.9(4) . . ?
O10 W2 O14 73.0(3) . . ?
O12 W2 O10 86.6(3) . . ?
O12 W2 O14 75.5(3) . . ?
O13 W2 O10 87.0(3) . . ?
O13 W2 O12 161.6(3) . . ?
O13 W2 O14 86.1(3) . . ?
O26 W2 O10 158.6(4) . . ?
O26 W2 O12 90.1(3) . . ?
O26 W2 O13 89.6(3) . . ?
O26 W2 O14 85.7(3) . . ?
O7 W3 K2 51.0(2) . . ?
O7 W3 O9 82.6(3) . . ?
O7 W3 O35 74.3(3) . . ?
O9 W3 K2 132.3(2) . . ?
O9 W3 O35 71.4(3) . . ?
O18 W3 K2 51.1(3) . . ?
O18 W3 O7 94.1(3) . . ?
O18 W3 O9 161.6(4) . . ?
O18 W3 O33 92.7(4) . . ?
O18 W3 O35 90.3(3) . . ?
O33 W3 K2 142.7(2) . . ?
O33 W3 O7 159.0(3) . . ?
O33 W3 O9 84.7(3) . . ?
O33 W3 O35 85.9(3) . . ?
O35 W3 K2 101.1(2) . . ?
O39 W3 K2 83.0(3) . . ?
O39 W3 O7 97.8(4) . . ?
O39 W3 O9 94.8(4) . . ?
O39 W3 O18 103.6(4) . . ?
O39 W3 O33 99.9(4) . . ?
O39 W3 O35 164.6(4) . . ?
O4 W4 K2 84.6(3) . . ?
O4 W4 O7 98.9(4) . . ?
O4 W4 O20 98.4(4) . . ?
O4 W4 O25 101.6(4) . . ?
O4 W4 O35 170.8(4) . . ?
O4 W4 O36 100.8(4) . . ?
O7 W4 K2 45.2(2) . . ?
O7 W4 O20 88.6(3) . . ?
O7 W4 O25 88.5(3) . . ?
O7 W4 O35 75.0(3) . . ?
O20 W4 K2 133.1(2) . . ?
O20 W4 O25 160.0(3) . . ?
O20 W4 O35 74.9(3) . . ?
O25 W4 K2 50.1(2) . . ?
O25 W4 O35 85.3(3) . . ?
O35 W4 K2 95.43(18) . . ?
O36 W4 K2 137.6(3) . . ?
O36 W4 O7 160.3(3) . . ?
O36 W4 O20 88.1(3) . . ?
O36 W4 O25 88.0(3) . . ?
O36 W4 O35 85.4(3) . . ?
O3 W5 O5 167.3(3) . . ?
O3 W5 O16 98.5(4) . . ?
O3 W5 O17 97.9(4) . . ?
O3 W5 O21 103.3(4) . . ?
O3 W5 O33 99.3(4) . . ?
O16 W5 O5 74.5(3) . . ?
O16 W5 O17 82.1(3) . . ?
O17 W5 O5 70.9(3) . . ?
O21 W5 O5 87.7(3) . . ?
O21 W5 O16 91.8(4) . . ?
O21 W5 O17 158.7(3) . . ?
O21 W5 O33 93.7(4) . . ?
O33 W5 O5 86.2(3) . . ?
O33 W5 O16 159.7(3) . . ?
O33 W5 O17 85.8(3) . . ?
O8 W6 O20 161.9(4) . . ?
O8 W6 O31 86.3(3) . . ?
O8 W6 O35 86.9(3) . . ?
O9 W6 O8 91.8(4) . . ?
O9 W6 O20 89.9(3) . . ?
O9 W6 O31 160.7(3) . . ?
O9 W6 O35 76.7(3) . . ?
O20 W6 O35 76.0(3) . . ?
O31 W6 O20 86.1(3) . . ?
O31 W6 O35 84.0(3) . . ?
O37 W6 O8 100.1(4) . . ?
O37 W6 O9 100.3(4) . . ?
O37 W6 O20 97.3(4) . . ?
O37 W6 O31 99.0(4) . . ?
O37 W6 O35 172.5(3) . . ?
O2 W7 O5 170.6(4) . . ?
O2 W7 O11 98.6(4) . . ?
O2 W7 O13 100.6(4) . . ?
O2 W7 O16 98.2(4) . . ?
O2 W7 O34 101.9(4) . . ?
O11 W7 O5 74.0(3) . . ?
O13 W7 O5 84.8(3) . . ?
O13 W7 O11 86.9(4) . . ?
O16 W7 O5 76.1(3) . . ?
O16 W7 O11 88.0(4) . . ?
O16 W7 O13 161.0(3) . . ?
O34 W7 O5 85.8(3) . . ?
O34 W7 O11 159.4(3) . . ?
O34 W7 O13 87.5(3) . . ?
O34 W7 O16 90.9(3) . . ?
O23 W8 O6 74.0(3) . . ?
O23 W8 O26 84.4(3) . . ?
O23 W8 O34 153.8(3) . . ?
O26 W8 O6 78.5(3) . . ?
O32 W8 O6 172.6(3) . . ?
O32 W8 O23 100.2(4) . . ?
O32 W8 O26 96.5(4) . . ?
O32 W8 O34 103.0(4) . . ?
O32 W8 O38 102.0(4) . . ?
O34 W8 O6 81.8(3) . . ?
O34 W8 O26 81.2(3) . . ?
O38 W8 O6 83.2(3) . . ?
O38 W8 O23 94.3(3) . . ?
O38 W8 O26 161.3(4) . . ?
O38 W8 O34 92.5(3) . . ?
O8 W9 O5 86.6(3) . . ?
O8 W9 O11 161.6(3) . . ?
O8 W9 O22 85.6(3) . . ?
O11 W9 O5 75.8(3) . . ?
O11 W9 O22 87.0(4) . . ?
O15 W9 O5 171.9(4) . . ?
O15 W9 O8 100.4(4) . . ?
O15 W9 O11 97.5(4) . . ?
O15 W9 O17 99.8(4) . . ?
O15 W9 O22 101.1(4) . . ?
O17 W9 O5 75.9(3) . . ?
O17 W9 O8 91.1(4) . . ?
O17 W9 O11 89.8(4) . . ?
O17 W9 O22 159.1(3) . . ?
O22 W9 O5 83.3(3) . . ?
O12 W10 O14 75.6(3) . . ?
O12 W10 O28 85.8(3) . . ?
O24 W10 O12 92.0(3) . . ?
O24 W10 O14 86.2(3) . . ?
O24 W10 O28 158.3(3) . . ?
O24 W10 O36 88.7(3) . . ?
O28 W10 O14 72.4(3) . . ?
O29 W10 O12 98.1(4) . . ?
O29 W10 O14 169.3(3) . . ?
O29 W10 O24 102.9(4) . . ?
O29 W10 O28 98.8(4) . . ?
O29 W10 O36 100.3(4) . . ?
O36 W10 O12 161.0(3) . . ?
O36 W10 O14 85.4(3) . . ?
O36 W10 O28 86.7(3) . . ?
O10 W11 O14 75.8(3) . . ?
O22 W11 O10 88.6(4) . . ?
O22 W11 O14 85.5(3) . . ?
O22 W11 O28 160.9(3) . . ?
O22 W11 O31 87.5(3) . . ?
O27 W11 O10 97.1(4) . . ?
O27 W11 O14 170.4(4) . . ?
O27 W11 O22 100.9(4) . . ?
O27 W11 O28 98.2(4) . . ?
O27 W11 O31 101.4(4) . . ?
O28 W11 O10 88.2(4) . . ?
O28 W11 O14 75.5(3) . . ?
O31 W11 O10 161.6(3) . . ?
O31 W11 O14 86.0(3) . . ?
O31 W11 O28 89.7(3) . . ?
O1W Na1 O5W 64.0(4) . . ?
O1W Na1 O11 64.3(3) . . ?
O1W Na1 O13 108.0(3) . . ?
O1W Na1 O19 121.7(4) . 2 ?
O1W Na1 O22 107.0(4) . . ?
O5W Na1 O11 90.4(4) . . ?
O5W Na1 O13 139.9(4) . . ?
O5W Na1 O22 79.3(4) . . ?
O11 Na1 O13 54.4(3) . . ?
O11 Na1 O22 55.0(3) . . ?
O13 Na1 O22 65.2(3) . . ?
O19 Na1 O5W 68.5(4) 2 . ?
O19 Na1 O11 146.9(4) 2 . ?
O19 Na1 O13 130.1(4) 2 . ?
O19 Na1 O22 95.0(3) 2 . ?
O7W Na2 O14W 81.3(7) . . ?
O7W Na2 O2 76.2(4) . 4_575 ?
O7W Na2 O20 138.2(4) . . ?
O7W Na2 O31 88.0(4) . . ?
O7W Na2 O36 127.9(4) . . ?
O14W Na2 O20 136.6(7) . . ?
O14W Na2 O31 137.4(7) . . ?
O2 Na2 O14W 128.5(7) 4_575 . ?
O2 Na2 O20 86.2(3) 4_575 . ?
O2 Na2 O31 87.6(3) 4_575 . ?
O2 Na2 O36 139.9(3) 4_575 . ?
O20 Na2 O31 53.2(2) . . ?
O36 Na2 O14W 89.8(7) . . ?
O36 Na2 O20 54.2(2) . . ?
O36 Na2 O31 65.0(2) . . ?
Eu1 K1 K2 56.93(6) . . ?
W1 K1 Eu1 60.98(4) . . ?
W1 K1 K2 57.93(6) . . ?
O6W K1 Eu1 103.4(4) . . ?
O6W K1 W1 161.3(4) . . ?
O6W K1 K2 105.8(4) . . ?
O6W K1 O19 160.8(4) . . ?
O6W K1 O27 95.5(4) . 2_545 ?
O6W K1 O30 133.6(4) . . ?
O6W K1 O32 87.5(4) . 3_566 ?
O6W K1 O41 82.0(4) . . ?
O10W K1 Eu1 93.6(2) . . ?
O10W K1 W1 80.3(2) . . ?
O10W K1 K2 37.4(2) . . ?
O10W K1 O6W 91.2(4) . . ?
O10W K1 O19 72.9(3) . . ?
O10W K1 O27 78.6(3) . 2_545 ?
O10W K1 O30 80.4(3) . . ?
O10W K1 O32 142.6(3) . 3_566 ?
O10W K1 O41 120.8(3) . . ?
O19 K1 Eu1 88.55(17) . . ?
O19 K1 W1 27.84(15) . . ?
O19 K1 K2 68.13(18) . . ?
O27 K1 Eu1 159.7(2) 2_545 . ?
O27 K1 W1 98.99(19) 2_545 . ?
O27 K1 K2 111.0(2) 2_545 . ?
O27 K1 O19 71.3(2) 2_545 . ?
O27 K1 O41 160.3(3) 2_545 . ?
O30 K1 Eu1 33.17(16) . . ?
O30 K1 W1 28.78(16) . . ?
O30 K1 K2 45.71(18) . . ?
O30 K1 O19 55.6(2) . . ?
O30 K1 O27 126.5(3) . 2_545 ?
O30 K1 O41 64.7(2) . . ?
O32 K1 Eu1 123.03(19) 3_566 . ?
O32 K1 W1 109.30(19) 3_566 . ?
O32 K1 K2 166.50(19) 3_566 . ?
O32 K1 O19 98.5(2) 3_566 . ?
O32 K1 O27 64.4(3) 3_566 2_545 ?
O32 K1 O30 125.5(3) 3_566 . ?
O32 K1 O41 96.0(2) 3_566 . ?
O41 K1 Eu1 34.37(16) . . ?
O41 K1 W1 88.14(17) . . ?
O41 K1 K2 88.37(18) . . ?
O41 K1 O19 115.2(2) . . ?
W1 K2 Eu1 60.58(5) . . ?
W3 K2 Eu1 64.38(5) . . ?
W3 K2 W1 78.71(6) . . ?
W3 K2 W4 53.00(4) . . ?
W4 K2 Eu1 95.61(7) . . ?
W4 K2 W1 57.16(4) . . ?
O2W K2 Eu1 175.2(3) . . ?
O2W K2 W1 116.3(3) . . ?
O2W K2 W3 112.0(3) . . ?
O2W K2 W4 79.6(3) . . ?
O2W K2 O7 83.4(3) . . ?
O2W K2 O15 84.2(3) . 2_645 ?
O2W K2 O18 140.1(3) . . ?
O2W K2 O25 95.9(3) . . ?
O2W K2 O30 141.4(3) . . ?
O10W K2 Eu1 97.1(2) . . ?
O10W K2 W1 75.6(2) . . ?
O10W K2 W3 153.6(2) . . ?
O10W K2 W4 115.0(2) . . ?
O10W K2 O2W 85.2(3) . . ?
O10W K2 O7 142.9(3) . . ?
O10W K2 O15 106.7(3) . 2_645 ?
O10W K2 O18 128.5(3) . . ?
O10W K2 O25 92.7(3) . . ?
O10W K2 O30 75.6(3) . . ?
O7 K2 Eu1 92.26(17) . . ?
O7 K2 W1 78.14(17) . . ?
O7 K2 W3 31.98(15) . . ?
O7 K2 W4 28.08(15) . . ?
O7 K2 O15 107.1(3) . 2_645 ?
O7 K2 O18 56.9(2) . . ?
O7 K2 O25 53.8(2) . . ?
O7 K2 O30 92.1(2) . . ?
O15 K2 Eu1 99.00(18) 2_645 . ?
O15 K2 W1 159.4(2) 2_645 . ?
O15 K2 W3 95.20(19) 2_645 . ?
O15 K2 W4 133.4(2) 2_645 . ?
O15 K2 O18 102.0(3) 2_645 . ?
O15 K2 O25 160.5(3) 2_645 . ?
O15 K2 O30 133.1(2) 2_645 . ?
O18 K2 Eu1 35.91(16) . . ?
O18 K2 W1 63.58(18) . . ?
O18 K2 W3 28.88(17) . . ?
O18 K2 W4 67.47(16) . . ?
O18 K2 O25 65.8(2) . . ?
O18 K2 O30 53.8(2) . . ?
O25 K2 Eu1 79.90(16) . . ?
O25 K2 W1 28.51(15) . . ?
O25 K2 W3 66.60(16) . . ?
O25 K2 W4 29.14(15) . . ?
O25 K2 O30 53.0(2) . . ?
O30 K2 Eu1 36.39(14) . . ?
O30 K2 W1 26.67(14) . . ?
O30 K2 W3 78.75(16) . . ?
O30 K2 W4 78.81(16) . . ?
O43 K2 Eu1 35.53(18) 3_666 . ?
O43 K2 W1 85.8(2) 3_666 . ?
O43 K2 W3 92.4(2) 3_666 . ?
O43 K2 W4 131.1(2) 3_666 . ?
O43 K2 O2W 149.3(3) 3_666 . ?
O43 K2 O10W 79.8(3) 3_666 . ?
O43 K2 O7 123.9(3) 3_666 . ?
O43 K2 O15 74.7(3) 3_666 2_645 ?
O43 K2 O18 67.7(2) 3_666 . ?
O43 K2 O25 111.4(3) 3_666 . ?
O43 K2 O30 59.3(2) 3_666 . ?
K2 O10W K1 105.0(3) . . ?
W7 O2 Na2 146.7(5) . 4_576 ?
B1 O5 W5 123.6(6) . . ?
B1 O5 W7 126.9(6) . . ?
B1 O5 W9 125.3(6) . . ?
W7 O5 W5 88.4(2) . . ?
W9 O5 W5 91.4(3) . . ?
W9 O5 W7 90.1(2) . . ?
B1 O6 W1 130.0(6) . . ?
B1 O6 W8 131.2(6) . . ?
W8 O6 W1 86.2(2) . . ?
W3 O7 K2 97.0(3) . . ?
W4 O7 W3 121.6(4) . . ?
W4 O7 K2 106.7(3) . . ?
W6 O8 W9 148.6(5) . . ?
W6 O9 W3 120.0(4) . . ?
W11 O10 W2 119.8(4) . . ?
W7 O11 W9 119.7(4) . . ?
W7 O11 Na1 106.6(4) . . ?
W9 O11 Na1 105.8(4) . . ?
W2 O12 W10 119.7(4) . . ?
W2 O13 W7 145.2(4) . . ?
W2 O13 Na1 109.9(3) . . ?
W7 O13 Na1 101.9(3) . . ?
B1 O14 W2 125.0(6) . . ?
B1 O14 W10 125.2(6) . . ?
B1 O14 W11 124.1(6) . . ?
W10 O14 W2 89.0(3) . . ?
W11 O14 W2 91.4(3) . . ?
W11 O14 W10 91.6(3) . . ?
W9 O15 K2 132.0(4) . 2_655 ?
W7 O16 W5 120.6(4) . . ?
W9 O17 W5 121.8(4) . . ?
Eu1 O18 K2 99.7(3) . . ?
W3 O18 Eu1 156.9(4) . . ?
W3 O18 K2 100.0(4) . . ?
W1 O19 Na1 124.1(4) . 2_545 ?
W1 O19 K1 97.7(3) . . ?
Na1 O19 K1 132.8(3) 2_545 . ?
W4 O20 W6 119.2(4) . . ?
W4 O20 Na2 102.8(3) . . ?
W6 O20 Na2 107.7(3) . . ?
W5 O21 Eu1 155.4(5) . . ?
W9 O22 Na1 100.5(3) . . ?
W11 O22 W9 148.4(4) . . ?
W11 O22 Na1 108.1(4) . . ?
W1 O23 W8 122.5(4) . . ?
W10 O24 W1 151.9(5) . . ?
W1 O25 W4 152.9(5) . . ?
W1 O25 K2 102.3(3) . . ?
W4 O25 K2 100.8(3) . . ?
W2 O26 W8 151.7(5) . . ?
W11 O27 K1 140.7(5) . 2 ?
W11 O28 W10 120.5(4) . . ?
Eu1 O30 K1 107.4(3) . . ?
Eu1 O30 K2 94.3(3) . . ?
W1 O30 Eu1 144.9(4) . . ?
W1 O30 K1 102.1(3) . . ?
W1 O30 K2 102.5(3) . . ?
K1 O30 K2 93.7(2) . . ?
W6 O31 Na2 103.9(3) . . ?
W11 O31 W6 147.2(4) . . ?
W11 O31 Na2 105.2(3) . . ?
W8 O32 K1 164.2(4) . 3_566 ?
W5 O33 W3 139.2(5) . . ?
W7 O34 W8 153.9(4) . . ?
B1 O35 W3 124.5(6) . . ?
B1 O35 W4 126.6(6) . . ?
B1 O35 W6 124.4(6) . . ?
W3 O35 W4 89.0(3) . . ?
W6 O35 W3 91.9(3) . . ?
W6 O35 W4 89.6(3) . . ?
W4 O36 W10 145.5(4) . . ?
W4 O36 Na2 104.0(4) . . ?
W10 O36 Na2 108.3(3) . . ?
W8 O38 Eu1 143.5(4) . . ?
C2 O40 Eu1 137.6(8) . 3_666 ?
Eu1 O41 K1 103.4(3) . . ?
C2 O41 Eu1 134.5(8) . . ?
C2 O41 K1 120.7(8) . . ?
Eu1 O42 Eu1 105.0(3) . 3_666 ?
C3 O42 Eu1 85.7(6) . 3_666 ?
C3 O42 Eu1 165.9(8) . . ?
Eu1 O43 K2 105.0(3) 3_666 3_666 ?
C3 O43 Eu1 103.0(7) . 3_666 ?
C3 O43 K2 148.1(8) . 3_666 ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
N1 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
N1 C1 C2 113.0(10) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
O40 C2 C1 115.7(11) . . ?
O41 C2 O40 128.7(12) . . ?
O41 C2 C1 115.6(11) . . ?
O42 C3 Eu1 69.7(6) . 3_666 ?
O42 C3 O43 122.1(10) . . ?
O42 C3 C4 120.5(10) . . ?
O43 C3 Eu1 52.8(5) . 3_666 ?
O43 C3 C4 117.3(10) . . ?
C4 C3 Eu1 168.5(8) . 3_666 ?
N2 C4 C3 113.9(10) . . ?
N2 C4 H4A 108.8 . . ?
N2 C4 H4B 108.8 . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?

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
N1 H1C O12 0.89 2.22 2.988(14) 145.0 3_566
N1 H1C O24 0.89 2.57 3.284(15) 138.3 3_566
N1 H1D O5W 0.89 2.02 2.853(18) 156.1 4_576
N1 H1D O39 0.89 2.52 3.087(14) 122.3 3_666
N1 H1E O3 0.89 2.56 3.281(16) 138.6 3_666
N1 H1E O33 0.89 2.52 3.350(15) 154.5 3_666
N2 H2A O37 0.89 2.01 2.811(14) 149.4 4_576
N2 H2B O3W 0.89 1.98 2.849(18) 164.8 4_576
N2 H2C O16 0.89 2.45 2.993(15) 120.0 .
N2 H2C O21 0.89 2.21 3.096(14) 170.3 .

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1495660'
_audit_update_record             
;
2016-09-05 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT430_6                   
;
PROBLEM: Short Inter D...A Contact O11W   ..  O12W    ..       1.81 Ang. 
RESPONSE: In the crystal structure, there are a number of short connections
 between  OW(H2O) and O(POM) or OW(H2O) atoms in the range 2.56-2.84 Ang,
 which indicate extensive H bonding interactions among them. 
 Some shorter connections between OW(H2O) or OW(H2O) atoms result from
 the disordered water molecules. 
;

_vrf_PLAT306_6                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check  
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

# end Validation Reply Form

_audit_creation_date             2016-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C16 H40 B4 K8 N8 Na8 O198 Tm4 W44), 10(O)'
_chemical_formula_sum            'C8 H70 B2 K4 N4 Na4 O109 Tm2 W22'
_chemical_formula_weight         6619.22
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        P2(1)/c
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.6408(10)
_cell_length_b                   21.7217(18)
_cell_length_c                   21.4679(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.451(2)
_cell_angle_gamma                90.00
_cell_volume                     5423.4(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4067
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.829
_cell_measurement_theta_min      2.233
_exptl_absorpt_coefficient_mu    25.130
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1385 before and 0.0564 after correction. 
The Ratio of minimum to maximum transmission is 0.4916. 
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5828
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_special_details           
;
Thanks to the large structure of 6 and the existence of a 
large amount of weight atoms, the intensity data are not 
very good, leading to the ADP max/min ratio of some atoms,
and it is very difficult to refine this large structure,
therefore, some unit-occupancy atoms have been refined 
isotropically and restrainedly refined. The ISOR 
instruction is used for C3, O22, O9, O19 and B1. 
O6W-O9W and O11W-O14W are refined isostropicallly. The 
DFIX instruction is used for N2 and C4. 682 parameters
and 31 restraints are used in the refinement. 
;
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27540
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         27685
_reflns_number_gt                6841
_reflns_number_total             9511
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         2.227
_refine_diff_density_min         -1.606
_refine_diff_density_rms         0.357
_refine_ls_extinction_coef       0.000035(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         9511
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0327P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0932
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Restrained distances
 N2-C4
 1.48 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O19) \\sim Ueq, Uanis(B1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Fixed Sof: O6W(0.5) O9W(0.5) O11W(0.5) O13W(0.5) O14W(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
5.b Me refined with riding coordinates:
 N1(H1C,H1D,H1E), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Tm1 Tm 0.39208(6) 0.52537(3) 0.42519(3) 0.02126(18) Uani 1 d . . . .
B1 B 0.2169(15) 0.6580(8) 0.2752(8) 0.016(4) Uani 1 d . . . U
W1 W 0.10277(5) 0.51025(3) 0.32099(3) 0.02030(16) Uani 1 d . . . .
W2 W -0.03551(6) 0.72977(3) 0.31158(3) 0.02580(18) Uani 1 d . . . .
W3 W 0.46381(5) 0.57391(3) 0.24688(3) 0.02102(17) Uani 1 d . . . .
W4 W 0.21993(6) 0.53858(3) 0.16603(3) 0.02325(17) Uani 1 d . . . .
W5 W 0.47140(5) 0.69411(3) 0.35971(3) 0.02133(17) Uani 1 d . . . .
W6 W 0.34898(6) 0.67138(3) 0.13799(3) 0.02390(17) Uani 1 d . . . .
W7 W 0.23421(6) 0.77334(3) 0.39034(3) 0.02362(17) Uani 1 d . . . .
W8 W 0.10441(5) 0.62228(3) 0.42731(3) 0.02021(17) Uani 1 d . . . .
W9 W 0.35504(6) 0.79469(3) 0.25440(3) 0.02442(18) Uani 1 d . . . .
W10 W -0.04263(6) 0.61681(3) 0.20551(3) 0.02541(18) Uani 1 d . . . .
W11 W 0.08156(6) 0.75165(3) 0.17326(3) 0.02537(18) Uani 1 d . . . .
Na1 Na 0.0874(12) 0.8978(6) 0.2840(7) 0.127(5) Uani 1 d . . . .
Na2 Na 0.0684(6) 0.6287(3) 0.0365(3) 0.0399(19) Uani 1 d . . . .
K1 K 0.1507(3) 0.3809(2) 0.42464(19) 0.0389(10) Uani 1 d . . . .
K2 K 0.3664(4) 0.41663(19) 0.2728(2) 0.0397(11) Uani 1 d . . . .
O1W O 0.2654(12) 0.9608(6) 0.3256(8) 0.065(5) Uani 1 d . . . .
O2W O 0.3404(13) 0.3503(7) 0.1659(8) 0.075(5) Uani 1 d . . . .
O3W O 0.2061(13) 0.8950(8) 0.0922(7) 0.077(5) Uani 1 d . . . .
O4W O -0.3317(11) 0.7157(6) 0.2025(7) 0.057(4) Uani 1 d . . . .
O5W O 0.2355(15) 0.9642(8) 0.1972(9) 0.096(6) Uani 1 d . . . .
O6W O 0.259(2) 0.2876(12) 0.4919(13) 0.055(8) Uiso 0.50 d . . . .
O7W O -0.0365(19) 0.7306(10) -0.0056(10) 0.126(8) Uiso 1 d . . . .
O8W O 0.384(2) 0.5808(11) -0.0083(11) 0.142(9) Uiso 1 d . . . .
O9W O 0.548(3) 0.6541(14) -0.0334(15) 0.075(10) Uiso 0.50 d . . . .
O10W O 0.2286(11) 0.3297(6) 0.3171(6) 0.054(4) Uani 1 d . . . .
O11W O 0.636(3) 0.5677(14) 0.0987(15) 0.072(10) Uiso 0.50 d . . . .
O12W O -0.337(2) 0.6494(11) 0.0921(11) 0.143(9) Uiso 1 d . . . .
O13W O -0.025(3) 0.6130(15) -0.0923(16) 0.078(10) Uiso 0.50 d . . . .
O14W O 0.830(3) 0.5784(14) 0.0187(15) 0.073(9) Uiso 0.50 d . . . .
O1 O -0.1499(10) 0.7677(6) 0.3420(6) 0.046(4) Uani 1 d . . . .
O2 O 0.2137(10) 0.8258(5) 0.4491(5) 0.037(3) Uani 1 d . . . .
O3 O 0.6044(10) 0.7006(6) 0.3962(6) 0.040(3) Uani 1 d . . . .
O4 O 0.1941(9) 0.4790(6) 0.1158(5) 0.035(3) Uani 1 d . . . .
O5 O 0.2884(9) 0.7095(5) 0.3065(5) 0.024(3) Uani 1 d . . . .
O6 O 0.1969(8) 0.6110(4) 0.3276(4) 0.016(2) Uani 1 d . . . .
O7 O 0.3758(9) 0.5201(5) 0.1912(5) 0.028(3) Uani 1 d . . . .
O8 O 0.3908(10) 0.7395(5) 0.1902(5) 0.029(3) Uani 1 d . . . .
O9 O 0.4723(8) 0.6268(5) 0.1675(5) 0.023(3) Uani 1 d . . . U
O10 O -0.0205(9) 0.7777(5) 0.2374(5) 0.033(3) Uani 1 d . . . .
O11 O 0.2906(9) 0.8285(5) 0.3287(5) 0.029(3) Uani 1 d . . . .
O12 O -0.1224(9) 0.6714(5) 0.2592(5) 0.028(3) Uani 1 d . . . .
O13 O 0.0885(9) 0.7761(5) 0.3464(5) 0.030(3) Uani 1 d . . . .
O14 O 0.1048(8) 0.6806(5) 0.2504(5) 0.021(3) Uani 1 d . . . .
O15 O 0.4092(10) 0.8615(5) 0.2265(6) 0.037(3) Uani 1 d . . . .
O16 O 0.3885(9) 0.7522(5) 0.4102(5) 0.025(3) Uani 1 d . . . .
O17 O 0.4833(10) 0.7678(5) 0.3031(5) 0.031(3) Uani 1 d . . . .
O18 O 0.4137(9) 0.5409(5) 0.3147(5) 0.029(3) Uani 1 d . . . .
O19 O 0.0256(9) 0.4419(5) 0.3202(5) 0.023(3) Uani 1 d . . . U
O20 O 0.2761(9) 0.5959(5) 0.1075(5) 0.026(3) Uani 1 d . . . .
O21 O 0.4101(8) 0.6303(5) 0.3987(5) 0.026(3) Uani 1 d . . . .
O22 O 0.2024(9) 0.7944(4) 0.2161(5) 0.022(3) Uani 1 d . . . U
O23 O 0.0348(9) 0.5525(5) 0.3890(5) 0.025(3) Uani 1 d . . . .
O24 O -0.0100(9) 0.5633(5) 0.2695(5) 0.028(3) Uani 1 d . . . .
O25 O 0.1741(9) 0.5046(5) 0.2432(5) 0.031(3) Uani 1 d . . . .
O26 O -0.0050(9) 0.6691(5) 0.3701(5) 0.030(3) Uani 1 d . . . .
O27 O 0.0394(11) 0.8044(5) 0.1164(6) 0.040(3) Uani 1 d . . . .
O28 O -0.0249(9) 0.6874(5) 0.1508(5) 0.026(3) Uani 1 d . . . .
O29 O -0.1617(10) 0.5839(6) 0.1686(6) 0.039(3) Uani 1 d . . . .
O30 O 0.2282(8) 0.4892(5) 0.3675(5) 0.020(3) Uani 1 d . . . .
O31 O 0.1976(9) 0.7055(5) 0.1327(5) 0.029(3) Uani 1 d . . . .
O32 O 0.0274(9) 0.6275(5) 0.4928(5) 0.029(3) Uani 1 d . . . .
O33 O 0.5109(8) 0.6482(5) 0.2888(5) 0.022(3) Uani 1 d . . . .
O34 O 0.1830(9) 0.7005(5) 0.4284(5) 0.024(3) Uani 1 d . . . .
O35 O 0.2852(9) 0.6254(5) 0.2272(5) 0.023(3) Uani 1 d . . . .
O36 O 0.0774(9) 0.5801(5) 0.1599(5) 0.027(3) Uani 1 d . . . .
O37 O 0.3969(10) 0.6975(5) 0.0674(5) 0.033(3) Uani 1 d . . . .
O38 O 0.2271(8) 0.5824(5) 0.4557(5) 0.022(3) Uani 1 d . . . .
O39 O 0.5945(9) 0.5389(6) 0.2393(6) 0.040(3) Uani 1 d . . . .
O40 O 0.4099(9) 0.4578(5) 0.5880(5) 0.027(3) Uani 1 d . . . .
O41 O 0.3032(10) 0.4613(5) 0.4982(5) 0.028(3) Uani 1 d . . . .
O42 O 0.4593(9) 0.5656(5) 0.5212(5) 0.028(3) Uani 1 d . . . .
O43 O 0.5627(10) 0.5757(5) 0.6070(5) 0.038(3) Uani 1 d . . . .
N1 N 0.2415(13) 0.4160(8) 0.6549(7) 0.052(5) Uani 1 d . . . .
H1C H 0.1803 0.4006 0.6728 0.078 Uiso 1 calc . . R .
H1D H 0.2591 0.4525 0.6717 0.078 Uiso 1 calc . . R .
H1E H 0.3008 0.3905 0.6608 0.078 Uiso 1 calc . . R .
N2 N 0.3686(12) 0.6821(7) 0.5296(6) 0.043(4) Uani 1 d . . D .
H2A H 0.3561 0.7224 0.5329 0.064 Uiso 1 calc . . R .
H2B H 0.3059 0.6616 0.5397 0.064 Uiso 1 calc . . R .
H2C H 0.3850 0.6731 0.4905 0.064 Uiso 1 calc . . R .
C1 C 0.2156(14) 0.4236(10) 0.5871(8) 0.041(5) Uani 1 d . . . .
H1A H 0.1518 0.4519 0.5805 0.049 Uiso 1 calc . . R .
H1B H 0.1935 0.3842 0.5689 0.049 Uiso 1 calc . . R .
C2 C 0.3218(14) 0.4485(7) 0.5552(8) 0.024(4) Uani 1 d . . . .
C3 C 0.4947(13) 0.5978(7) 0.5649(7) 0.018(4) Uani 1 d . . . U
C4 C 0.4653(15) 0.6643(8) 0.5717(9) 0.044(5) Uani 1 d . . D .
H4A H 0.4457 0.6723 0.6144 0.053 Uiso 1 calc . . R .
H4B H 0.5319 0.6891 0.5627 0.053 Uiso 1 calc . . R .


_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
Tm1 K1 4.211(4) . ?
Tm1 K2 4.035(4) . ?
Tm1 O18 2.420(11) . ?
Tm1 O21 2.360(11) . ?
Tm1 O30 2.364(10) . ?
Tm1 O38 2.400(10) . ?
Tm1 O40 2.363(10) 3_666 ?
Tm1 O41 2.368(10) . ?
Tm1 O42 2.838(11) 3_666 ?
Tm1 O42 2.342(11) . ?
Tm1 O43 2.367(12) 3_666 ?
Tm1 C3 2.985(15) 3_666 ?
B1 O5 1.53(2) . ?
B1 O6 1.544(19) . ?
B1 O14 1.473(19) . ?
B1 O35 1.506(19) . ?
W1 K1 3.612(4) . ?
W1 K2 3.860(4) . ?
W1 O6 2.448(9) . ?
W1 O19 1.734(10) . ?
W1 O23 1.924(11) . ?
W1 O24 2.037(11) . ?
W1 O25 1.900(11) . ?
W1 O30 1.793(10) . ?
W2 O1 1.719(12) . ?
W2 O10 1.918(11) . ?
W2 O12 1.950(11) . ?
W2 O13 1.887(11) . ?
W2 O14 2.390(9) . ?
W2 O26 1.844(11) . ?
W3 K2 3.650(4) . ?
W3 O7 1.933(11) . ?
W3 O9 2.061(10) . ?
W3 O18 1.745(11) . ?
W3 O33 1.916(10) . ?
W3 O35 2.383(10) . ?
W3 O39 1.715(11) . ?
W4 K2 3.853(4) . ?
W4 O4 1.703(11) . ?
W4 O7 1.914(11) . ?
W4 O20 1.904(11) . ?
W4 O25 1.910(12) . ?
W4 O35 2.403(11) . ?
W4 O36 1.888(10) . ?
W5 O3 1.710(11) . ?
W5 O5 2.397(10) . ?
W5 O16 1.947(10) . ?
W5 O17 2.018(10) . ?
W5 O21 1.784(11) . ?
W5 O33 1.894(10) . ?
W6 O8 1.907(11) . ?
W6 O9 1.823(10) . ?
W6 O20 1.946(11) . ?
W6 O31 1.911(11) . ?
W6 O35 2.310(10) . ?
W6 O37 1.732(11) . ?
W7 O2 1.724(11) . ?
W7 O5 2.378(11) . ?
W7 O11 1.922(11) . ?
W7 O13 1.906(11) . ?
W7 O16 1.884(11) . ?
W7 O34 1.888(10) . ?
W8 O6 2.449(10) . ?
W8 O23 1.890(11) . ?
W8 O26 2.009(11) . ?
W8 O32 1.703(10) . ?
W8 O34 1.930(11) . ?
W8 O38 1.757(10) . ?
W9 O5 2.313(10) . ?
W9 O8 1.887(11) . ?
W9 O11 1.936(10) . ?
W9 O15 1.701(11) . ?
W9 O17 1.879(11) . ?
W9 O22 1.925(10) . ?
W10 O12 1.920(11) . ?
W10 O14 2.378(10) . ?
W10 O24 1.827(11) . ?
W10 O28 1.948(11) . ?
W10 O29 1.722(11) . ?
W10 O36 1.913(10) . ?
W11 O10 1.941(11) . ?
W11 O14 2.272(10) . ?
W11 O22 1.892(11) . ?
W11 O27 1.730(11) . ?
W11 O28 1.915(10) . ?
W11 O31 1.920(10) . ?
Na1 O1W 2.609(19) . ?
Na1 O5W 2.97(2) . ?
Na1 O13W 3.02(3) 4_576 ?
Na1 O11 2.931(16) . ?
Na1 O13 2.965(16) . ?
Na1 O19 2.721(16) 2 ?
Na2 O7W 2.67(2) . ?
Na2 O13W 2.95(4) . ?
Na2 O14W 2.99(3) 1_455 ?
Na2 O2 2.762(13) 4_575 ?
Na2 O20 2.891(13) . ?
Na2 O28 3.008(13) . ?
Na2 O31 3.008(14) . ?
Na2 O36 2.849(12) . ?
K1 K2 4.270(6) . ?
K1 O6W 2.76(3) . ?
K1 O10W 2.752(14) . ?
K1 O19 2.936(11) . ?
K1 O27 2.876(12) 2_545 ?
K1 O30 2.819(10) . ?
K1 O32 2.791(11) 3_566 ?
K1 O41 2.907(12) . ?
K2 O2W 2.716(17) . ?
K2 O10W 2.678(13) . ?
K2 O7 2.855(12) . ?
K2 O15 2.873(12) 2_645 ?
K2 O18 2.891(12) . ?
K2 O25 2.991(12) . ?
K2 O30 3.080(11) . ?
K2 O43 2.680(13) 3_666 ?
O11W O12W 1.81(4) 1_655 ?
O12W O11W 1.81(4) 1_455 ?
O13W Na1 3.02(3) 4_575 ?
O14W Na2 2.99(3) 1_655 ?
O2 Na2 2.762(13) 4_576 ?
O15 K2 2.873(12) 2_655 ?
O19 Na1 2.721(16) 2_545 ?
O27 K1 2.876(12) 2 ?
O32 K1 2.791(11) 3_566 ?
O40 Tm1 2.363(10) 3_666 ?
O40 C2 1.236(19) . ?
O41 C2 1.263(19) . ?
O42 Tm1 2.838(11) 3_666 ?
O42 C3 1.226(17) . ?
O43 Tm1 2.367(12) 3_666 ?
O43 K2 2.680(13) 3_666 ?
O43 C3 1.271(18) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N1 C1 1.48(2) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.465(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.54(2) . ?
C3 Tm1 2.985(15) 3_666 ?
C3 C4 1.49(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
K2 Tm1 K1 62.32(8) . . ?
O18 Tm1 K1 101.5(3) . . ?
O18 Tm1 K2 45.1(3) . . ?
O18 Tm1 O42 114.1(3) . 3_666 ?
O18 Tm1 C3 97.5(4) . 3_666 ?
O21 Tm1 K1 141.7(3) . . ?
O21 Tm1 K2 112.0(3) . . ?
O21 Tm1 O18 67.3(4) . . ?
O21 Tm1 O30 105.8(3) . . ?
O21 Tm1 O38 69.4(3) . . ?
O21 Tm1 O40 74.0(4) . 3_666 ?
O21 Tm1 O41 140.7(4) . . ?
O21 Tm1 O42 135.3(3) . 3_666 ?
O21 Tm1 O43 143.3(4) . 3_666 ?
O21 Tm1 C3 147.0(4) . 3_666 ?
O30 Tm1 K1 39.4(2) . . ?
O30 Tm1 K2 49.5(3) . . ?
O30 Tm1 O18 69.4(3) . . ?
O30 Tm1 O38 71.2(3) . . ?
O30 Tm1 O41 77.6(4) . . ?
O30 Tm1 O42 116.5(3) . 3_666 ?
O30 Tm1 O43 73.9(4) . 3_666 ?
O30 Tm1 C3 94.8(4) . 3_666 ?
O38 Tm1 K1 81.0(2) . . ?
O38 Tm1 K2 119.4(3) . . ?
O38 Tm1 O18 108.3(4) . . ?
O38 Tm1 O42 136.9(3) . 3_666 ?
O38 Tm1 C3 143.1(4) . 3_666 ?
O40 Tm1 K1 140.3(3) 3_666 . ?
O40 Tm1 K2 91.8(3) 3_666 . ?
O40 Tm1 O18 73.6(4) 3_666 . ?
O40 Tm1 O30 139.3(4) 3_666 . ?
O40 Tm1 O38 138.5(4) 3_666 . ?
O40 Tm1 O41 128.8(4) 3_666 . ?
O40 Tm1 O42 64.9(3) 3_666 3_666 ?
O40 Tm1 O43 83.0(4) 3_666 3_666 ?
O40 Tm1 C3 73.6(4) 3_666 3_666 ?
O41 Tm1 K1 41.7(3) . . ?
O41 Tm1 K2 100.0(3) . . ?
O41 Tm1 O18 142.9(4) . . ?
O41 Tm1 O38 75.3(4) . . ?
O41 Tm1 O42 66.3(3) . 3_666 ?
O41 Tm1 C3 68.3(4) . 3_666 ?
O42 Tm1 K1 118.6(3) . . ?
O42 Tm1 K1 83.0(2) 3_666 . ?
O42 Tm1 K2 86.8(2) 3_666 . ?
O42 Tm1 K2 160.4(3) . . ?
O42 Tm1 O18 140.0(4) . . ?
O42 Tm1 O21 79.7(4) . . ?
O42 Tm1 O30 144.8(3) . . ?
O42 Tm1 O38 78.9(4) . . ?
O42 Tm1 O40 75.9(4) . 3_666 ?
O42 Tm1 O41 77.0(4) . . ?
O42 Tm1 O42 74.2(4) . 3_666 ?
O42 Tm1 O43 122.2(4) . 3_666 ?
O42 Tm1 C3 98.1(4) . 3_666 ?
O42 Tm1 C3 24.1(3) 3_666 3_666 ?
O43 Tm1 K1 57.7(3) 3_666 . ?
O43 Tm1 K2 39.7(3) 3_666 . ?
O43 Tm1 O18 79.0(4) 3_666 . ?
O43 Tm1 O38 138.5(4) 3_666 . ?
O43 Tm1 O41 75.9(4) 3_666 . ?
O43 Tm1 O42 48.2(4) 3_666 3_666 ?
O43 Tm1 C3 24.1(4) 3_666 3_666 ?
C3 Tm1 K1 68.0(3) 3_666 . ?
C3 Tm1 K2 63.3(3) 3_666 . ?
O5 B1 O6 105.1(12) . . ?
O14 B1 O5 111.8(12) . . ?
O14 B1 O6 109.0(12) . . ?
O14 B1 O35 113.2(13) . . ?
O35 B1 O5 110.5(12) . . ?
O35 B1 O6 106.8(12) . . ?
K1 W1 K2 69.62(9) . . ?
O6 W1 K1 127.0(2) . . ?
O6 W1 K2 97.3(2) . . ?
O19 W1 K1 53.6(4) . . ?
O19 W1 K2 88.0(3) . . ?
O19 W1 O6 174.5(4) . . ?
O19 W1 O23 100.7(5) . . ?
O19 W1 O24 99.1(5) . . ?
O19 W1 O25 100.5(5) . . ?
O19 W1 O30 101.3(5) . . ?
O23 W1 K1 87.8(3) . . ?
O23 W1 K2 144.3(3) . . ?
O23 W1 O6 74.1(4) . . ?
O23 W1 O24 82.2(4) . . ?
O24 W1 K1 148.6(3) . . ?
O24 W1 K2 130.9(3) . . ?
O24 W1 O6 78.6(4) . . ?
O25 W1 K1 115.4(3) . . ?
O25 W1 K2 49.3(3) . . ?
O25 W1 O6 84.1(4) . . ?
O25 W1 O23 155.1(5) . . ?
O25 W1 O24 81.7(4) . . ?
O30 W1 K1 50.1(3) . . ?
O30 W1 K2 51.4(3) . . ?
O30 W1 O6 81.0(4) . . ?
O30 W1 O23 92.9(5) . . ?
O30 W1 O24 159.6(4) . . ?
O30 W1 O25 95.6(5) . . ?
O1 W2 O10 98.9(5) . . ?
O1 W2 O12 98.1(5) . . ?
O1 W2 O13 100.7(5) . . ?
O1 W2 O14 169.0(5) . . ?
O1 W2 O26 102.3(5) . . ?
O10 W2 O12 86.4(5) . . ?
O10 W2 O14 72.4(4) . . ?
O12 W2 O14 75.0(4) . . ?
O13 W2 O10 86.8(5) . . ?
O13 W2 O12 160.8(4) . . ?
O13 W2 O14 85.8(4) . . ?
O26 W2 O10 158.8(5) . . ?
O26 W2 O12 90.5(5) . . ?
O26 W2 O13 89.4(5) . . ?
O26 W2 O14 86.5(4) . . ?
O7 W3 K2 50.9(3) . . ?
O7 W3 O9 82.4(4) . . ?
O7 W3 O35 74.9(4) . . ?
O9 W3 K2 132.4(3) . . ?
O9 W3 O35 70.4(4) . . ?
O18 W3 K2 51.0(4) . . ?
O18 W3 O7 94.6(5) . . ?
O18 W3 O9 161.5(4) . . ?
O18 W3 O33 93.1(5) . . ?
O18 W3 O35 91.2(4) . . ?
O33 W3 K2 143.3(3) . . ?
O33 W3 O7 158.8(5) . . ?
O33 W3 O9 84.0(4) . . ?
O33 W3 O35 85.3(4) . . ?
O35 W3 K2 101.1(2) . . ?
O39 W3 K2 83.2(4) . . ?
O39 W3 O7 97.0(5) . . ?
O39 W3 O9 95.4(5) . . ?
O39 W3 O18 103.1(5) . . ?
O39 W3 O33 100.4(5) . . ?
O39 W3 O35 164.2(5) . . ?
O4 W4 K2 85.2(4) . . ?
O4 W4 O7 99.2(5) . . ?
O4 W4 O20 97.8(5) . . ?
O4 W4 O25 102.0(5) . . ?
O4 W4 O35 170.3(4) . . ?
O4 W4 O36 100.8(5) . . ?
O7 W4 K2 45.4(3) . . ?
O7 W4 O35 74.7(4) . . ?
O20 W4 K2 133.3(3) . . ?
O20 W4 O7 88.6(5) . . ?
O20 W4 O25 160.2(5) . . ?
O20 W4 O35 74.8(4) . . ?
O25 W4 K2 49.6(3) . . ?
O25 W4 O7 88.3(5) . . ?
O25 W4 O35 85.6(4) . . ?
O35 W4 K2 95.3(3) . . ?
O36 W4 K2 137.3(3) . . ?
O36 W4 O7 160.0(5) . . ?
O36 W4 O20 88.1(4) . . ?
O36 W4 O25 88.1(4) . . ?
O36 W4 O35 85.4(4) . . ?
O3 W5 O5 167.2(5) . . ?
O3 W5 O16 98.7(5) . . ?
O3 W5 O17 97.3(5) . . ?
O3 W5 O21 102.8(5) . . ?
O3 W5 O33 99.5(5) . . ?
O16 W5 O5 73.9(4) . . ?
O16 W5 O17 82.5(4) . . ?
O17 W5 O5 71.6(4) . . ?
O21 W5 O5 88.1(4) . . ?
O21 W5 O16 91.4(4) . . ?
O21 W5 O17 159.7(5) . . ?
O21 W5 O33 94.8(5) . . ?
O33 W5 O5 86.1(4) . . ?
O33 W5 O16 158.9(4) . . ?
O33 W5 O17 84.7(5) . . ?
O8 W6 O20 161.4(4) . . ?
O8 W6 O31 86.9(5) . . ?
O8 W6 O35 86.1(4) . . ?
O9 W6 O8 91.8(5) . . ?
O9 W6 O20 89.7(5) . . ?
O9 W6 O31 159.6(4) . . ?
O9 W6 O35 76.0(4) . . ?
O20 W6 O35 76.3(4) . . ?
O31 W6 O20 85.4(5) . . ?
O31 W6 O35 83.6(4) . . ?
O37 W6 O8 100.1(5) . . ?
O37 W6 O9 101.5(5) . . ?
O37 W6 O20 97.7(5) . . ?
O37 W6 O31 98.7(5) . . ?
O37 W6 O35 173.4(4) . . ?
O2 W7 O5 171.3(5) . . ?
O2 W7 O11 98.9(5) . . ?
O2 W7 O13 101.2(5) . . ?
O2 W7 O16 98.9(5) . . ?
O2 W7 O34 100.4(5) . . ?
O11 W7 O5 74.5(4) . . ?
O13 W7 O5 84.4(4) . . ?
O13 W7 O11 87.9(5) . . ?
O16 W7 O5 75.4(4) . . ?
O16 W7 O11 87.6(5) . . ?
O16 W7 O13 159.8(5) . . ?
O16 W7 O34 90.8(4) . . ?
O34 W7 O5 86.4(4) . . ?
O34 W7 O11 160.7(5) . . ?
O34 W7 O13 87.1(5) . . ?
O23 W8 O6 74.7(4) . . ?
O23 W8 O26 83.7(5) . . ?
O23 W8 O34 154.9(4) . . ?
O26 W8 O6 78.9(4) . . ?
O32 W8 O6 174.1(4) . . ?
O32 W8 O23 100.5(5) . . ?
O32 W8 O26 97.4(5) . . ?
O32 W8 O34 101.4(5) . . ?
O32 W8 O38 101.3(5) . . ?
O34 W8 O6 82.7(4) . . ?
O34 W8 O26 81.3(4) . . ?
O38 W8 O6 82.7(4) . . ?
O38 W8 O23 94.8(5) . . ?
O38 W8 O26 161.2(4) . . ?
O38 W8 O34 93.0(4) . . ?
O8 W9 O5 86.3(4) . . ?
O8 W9 O11 161.5(4) . . ?
O8 W9 O22 85.1(5) . . ?
O11 W9 O5 75.8(4) . . ?
O15 W9 O5 171.7(5) . . ?
O15 W9 O8 100.8(5) . . ?
O15 W9 O11 97.4(5) . . ?
O15 W9 O17 99.4(5) . . ?
O15 W9 O22 101.6(5) . . ?
O17 W9 O5 75.9(4) . . ?
O17 W9 O8 90.8(5) . . ?
O17 W9 O11 89.2(5) . . ?
O17 W9 O22 159.0(4) . . ?
O22 W9 O5 83.2(4) . . ?
O22 W9 O11 88.3(5) . . ?
O12 W10 O14 75.9(4) . . ?
O12 W10 O28 86.7(5) . . ?
O24 W10 O12 91.8(5) . . ?
O24 W10 O14 86.7(4) . . ?
O24 W10 O28 158.5(5) . . ?
O24 W10 O36 89.3(4) . . ?
O28 W10 O14 72.1(4) . . ?
O29 W10 O12 97.6(5) . . ?
O29 W10 O14 168.9(5) . . ?
O29 W10 O24 102.7(5) . . ?
O29 W10 O28 98.8(5) . . ?
O29 W10 O36 100.5(5) . . ?
O36 W10 O12 161.2(5) . . ?
O36 W10 O14 85.4(4) . . ?
O36 W10 O28 85.4(4) . . ?
O10 W11 O14 74.8(4) . . ?
O22 W11 O10 88.7(5) . . ?
O22 W11 O14 85.2(4) . . ?
O22 W11 O28 160.2(4) . . ?
O22 W11 O31 87.4(5) . . ?
O27 W11 O10 98.2(5) . . ?
O27 W11 O14 170.3(5) . . ?
O27 W11 O22 101.5(5) . . ?
O27 W11 O28 98.3(6) . . ?
O27 W11 O31 102.1(5) . . ?
O28 W11 O10 89.0(5) . . ?
O28 W11 O14 75.2(4) . . ?
O28 W11 O31 88.0(5) . . ?
O31 W11 O10 159.7(4) . . ?
O31 W11 O14 85.0(4) . . ?
O1W Na1 O5W 59.1(6) . . ?
O1W Na1 O13W 96.1(9) . 4_576 ?
O1W Na1 O11 62.5(4) . . ?
O1W Na1 O13 109.0(5) . . ?
O1W Na1 O19 116.5(6) . 2 ?
O5W Na1 O13W 151.1(9) . 4_576 ?
O11 Na1 O5W 88.4(6) . . ?
O11 Na1 O13W 92.6(7) . 4_576 ?
O11 Na1 O13 53.6(4) . . ?
O13 Na1 O5W 136.6(6) . . ?
O13 Na1 O13W 61.8(7) . 4_576 ?
O19 Na1 O5W 65.5(5) 2 . ?
O19 Na1 O13W 122.6(8) 2 4_576 ?
O19 Na1 O11 143.6(7) 2 . ?
O19 Na1 O13 132.8(6) 2 . ?
O7W Na2 O13W 68.5(8) . . ?
O7W Na2 O14W 81.4(8) . 1_455 ?
O7W Na2 O2 76.0(5) . 4_575 ?
O7W Na2 O20 138.0(6) . . ?
O7W Na2 O28 75.4(5) . . ?
O7W Na2 O31 88.8(6) . . ?
O7W Na2 O36 128.3(6) . . ?
O13W Na2 O14W 62.3(9) . 1_455 ?
O13W Na2 O28 133.1(7) . . ?
O13W Na2 O31 149.5(7) . . ?
O14W Na2 O28 83.9(6) 1_455 . ?
O14W Na2 O31 136.4(7) 1_455 . ?
O2 Na2 O13W 67.4(7) 4_575 . ?
O2 Na2 O14W 129.5(7) 4_575 1_455 ?
O2 Na2 O20 85.6(4) 4_575 . ?
O2 Na2 O28 130.9(4) 4_575 . ?
O2 Na2 O31 88.0(4) 4_575 . ?
O2 Na2 O36 139.9(4) 4_575 . ?
O20 Na2 O13W 137.1(7) . . ?
O20 Na2 O14W 136.7(7) . 1_455 ?
O20 Na2 O28 89.8(4) . . ?
O20 Na2 O31 52.6(3) . . ?
O31 Na2 O28 52.6(3) . . ?
O36 Na2 O13W 145.8(7) . . ?
O36 Na2 O14W 88.9(7) . 1_455 ?
O36 Na2 O20 54.7(3) . . ?
O36 Na2 O28 53.0(3) . . ?
O36 Na2 O31 64.5(3) . . ?
Tm1 K1 K2 56.82(7) . . ?
W1 K1 Tm1 60.52(6) . . ?
W1 K1 K2 57.92(8) . . ?
O6W K1 Tm1 104.8(6) . . ?
O6W K1 W1 161.4(6) . . ?
O6W K1 K2 105.2(6) . . ?
O6W K1 O19 158.5(6) . . ?
O6W K1 O27 93.6(6) . 2_545 ?
O6W K1 O30 133.8(6) . . ?
O6W K1 O32 87.4(6) . 3_566 ?
O6W K1 O41 84.4(6) . . ?
O10W K1 Tm1 93.4(3) . . ?
O10W K1 W1 81.1(3) . . ?
O10W K1 K2 37.6(3) . . ?
O10W K1 O6W 89.0(7) . . ?
O10W K1 O19 73.3(4) . . ?
O10W K1 O27 77.6(4) . 2_545 ?
O10W K1 O30 81.3(4) . . ?
O10W K1 O32 141.9(4) . 3_566 ?
O10W K1 O41 118.9(4) . . ?
O19 K1 Tm1 88.6(2) . . ?
O19 K1 W1 28.4(2) . . ?
O19 K1 K2 67.9(2) . . ?
O27 K1 Tm1 159.4(3) 2_545 . ?
O27 K1 W1 99.5(3) 2_545 . ?
O27 K1 K2 109.9(3) 2_545 . ?
O27 K1 O19 71.2(3) 2_545 . ?
O27 K1 O41 163.2(4) 2_545 . ?
O30 K1 Tm1 32.2(2) . . ?
O30 K1 W1 29.2(2) . . ?
O30 K1 K2 46.1(2) . . ?
O30 K1 O19 56.6(3) . . ?
O30 K1 O27 127.3(4) . 2_545 ?
O30 K1 O41 62.4(3) . . ?
O32 K1 Tm1 124.1(3) 3_566 . ?
O32 K1 W1 110.1(3) 3_566 . ?
O32 K1 K2 166.9(3) 3_566 . ?
O32 K1 O19 99.0(3) 3_566 . ?
O32 K1 O27 64.8(3) 3_566 2_545 ?
O32 K1 O30 126.3(3) 3_566 . ?
O32 K1 O41 98.5(3) 3_566 . ?
O41 K1 Tm1 32.8(2) . . ?
O41 K1 W1 86.7(2) . . ?
O41 K1 K2 86.6(2) . . ?
O41 K1 O19 114.5(3) . . ?
W1 K2 Tm1 60.43(6) . . ?
W3 K2 Tm1 64.09(7) . . ?
W3 K2 W1 78.66(8) . . ?
W3 K2 W4 53.00(6) . . ?
W4 K2 Tm1 95.47(9) . . ?
W4 K2 W1 57.34(6) . . ?
O2W K2 Tm1 175.7(3) . . ?
O2W K2 W1 116.4(3) . . ?
O2W K2 W3 113.0(4) . . ?
O2W K2 W4 80.3(3) . . ?
O2W K2 O7 84.5(4) . . ?
O2W K2 O15 81.5(4) . 2_645 ?
O2W K2 O18 140.4(4) . . ?
O2W K2 O25 95.9(4) . . ?
O2W K2 O30 141.9(4) . . ?
O10W K2 Tm1 98.6(3) . . ?
O10W K2 W1 77.4(3) . . ?
O10W K2 W3 155.3(3) . . ?
O10W K2 W4 116.0(4) . . ?
O10W K2 O2W 83.1(5) . . ?
O10W K2 O7 144.3(4) . . ?
O10W K2 O15 105.2(4) . 2_645 ?
O10W K2 O18 131.1(4) . . ?
O10W K2 O25 94.1(4) . . ?
O10W K2 O30 77.8(3) . . ?
O10W K2 O43 82.4(4) . 3_666 ?
O7 K2 Tm1 91.9(2) . . ?
O7 K2 W1 78.5(2) . . ?
O7 K2 W3 31.7(2) . . ?
O7 K2 W4 28.5(2) . . ?
O7 K2 O15 105.8(3) . 2_645 ?
O7 K2 O18 56.2(3) . . ?
O7 K2 O25 54.2(3) . . ?
O7 K2 O30 92.1(3) . . ?
O15 K2 Tm1 101.8(3) 2_645 . ?
O15 K2 W1 162.1(3) 2_645 . ?
O15 K2 W3 95.9(3) 2_645 . ?
O15 K2 W4 132.0(3) 2_645 . ?
O15 K2 O18 103.1(3) 2_645 . ?
O15 K2 O25 160.0(4) 2_645 . ?
O15 K2 O30 135.3(3) 2_645 . ?
O18 K2 Tm1 36.4(2) . . ?
O18 K2 W1 64.4(2) . . ?
O18 K2 W3 28.0(2) . . ?
O18 K2 W4 67.4(2) . . ?
O18 K2 O25 66.4(3) . . ?
O18 K2 O30 54.2(3) . . ?
O25 K2 Tm1 80.0(2) . . ?
O25 K2 W1 28.8(2) . . ?
O25 K2 W3 66.7(2) . . ?
O25 K2 W4 29.1(2) . . ?
O25 K2 O30 53.5(3) . . ?
O30 K2 Tm1 35.71(19) . . ?
O30 K2 W1 27.08(19) . . ?
O30 K2 W3 78.2(2) . . ?
O30 K2 W4 79.1(2) . . ?
O43 K2 Tm1 34.3(3) 3_666 . ?
O43 K2 W1 85.7(3) 3_666 . ?
O43 K2 W3 90.2(3) 3_666 . ?
O43 K2 W4 129.8(3) 3_666 . ?
O43 K2 O2W 149.9(4) 3_666 . ?
O43 K2 O7 121.6(4) 3_666 . ?
O43 K2 O15 77.2(4) 3_666 2_645 ?
O43 K2 O18 66.2(3) 3_666 . ?
O43 K2 O25 111.2(4) 3_666 . ?
O43 K2 O30 58.7(3) 3_666 . ?
K2 O10W K1 103.7(4) . . ?
Na2 O13W Na1 132.8(12) . 4_575 ?
W7 O2 Na2 147.3(6) . 4_576 ?
B1 O5 W5 124.2(9) . . ?
B1 O5 W7 126.9(8) . . ?
B1 O5 W9 124.0(9) . . ?
W7 O5 W5 88.9(4) . . ?
W9 O5 W5 91.9(4) . . ?
W9 O5 W7 90.3(4) . . ?
B1 O6 W1 129.0(9) . . ?
B1 O6 W8 131.0(8) . . ?
W1 O6 W8 85.9(3) . . ?
W3 O7 K2 97.4(4) . . ?
W4 O7 W3 121.3(5) . . ?
W4 O7 K2 106.1(4) . . ?
W9 O8 W6 149.7(6) . . ?
W6 O9 W3 121.2(5) . . ?
W2 O10 W11 120.7(6) . . ?
W7 O11 W9 119.1(5) . . ?
W7 O11 Na1 104.5(5) . . ?
W9 O11 Na1 105.1(6) . . ?
W10 O12 W2 119.7(5) . . ?
W2 O13 W7 146.0(6) . . ?
W2 O13 Na1 107.9(5) . . ?
W7 O13 Na1 103.8(5) . . ?
B1 O14 W2 124.5(9) . . ?
B1 O14 W10 124.4(9) . . ?
B1 O14 W11 124.5(9) . . ?
W10 O14 W2 89.1(3) . . ?
W11 O14 W2 92.0(3) . . ?
W11 O14 W10 92.2(4) . . ?
W9 O15 K2 134.8(6) . 2_655 ?
W7 O16 W5 121.5(5) . . ?
W9 O17 W5 120.5(5) . . ?
Tm1 O18 K2 98.5(4) . . ?
W3 O18 Tm1 158.1(6) . . ?
W3 O18 K2 101.0(4) . . ?
W1 O19 Na1 122.7(6) . 2_545 ?
W1 O19 K1 98.0(4) . . ?
Na1 O19 K1 132.5(5) 2_545 . ?
W4 O20 W6 119.1(6) . . ?
W4 O20 Na2 101.9(4) . . ?
W6 O20 Na2 108.2(4) . . ?
W5 O21 Tm1 154.8(5) . . ?
W11 O22 W9 149.6(6) . . ?
W8 O23 W1 122.0(5) . . ?
W10 O24 W1 151.2(6) . . ?
W1 O25 W4 152.4(6) . . ?
W1 O25 K2 101.9(4) . . ?
W4 O25 K2 101.4(4) . . ?
W2 O26 W8 151.3(6) . . ?
W11 O27 K1 142.2(6) . 2 ?
W10 O28 Na2 102.1(4) . . ?
W11 O28 W10 120.4(6) . . ?
W11 O28 Na2 105.2(4) . . ?
Tm1 O30 K1 108.4(4) . . ?
Tm1 O30 K2 94.8(3) . . ?
W1 O30 Tm1 145.8(5) . . ?
W1 O30 K1 100.8(4) . . ?
W1 O30 K2 101.5(4) . . ?
K1 O30 K2 92.7(3) . . ?
W6 O31 W11 147.2(6) . . ?
W6 O31 Na2 105.0(4) . . ?
W11 O31 Na2 105.1(5) . . ?
W8 O32 K1 162.1(6) . 3_566 ?
W5 O33 W3 138.3(5) . . ?
W7 O34 W8 153.0(6) . . ?
B1 O35 W3 125.5(9) . . ?
B1 O35 W4 125.4(9) . . ?
B1 O35 W6 124.3(9) . . ?
W3 O35 W4 88.9(3) . . ?
W6 O35 W3 92.4(3) . . ?
W6 O35 W4 89.5(4) . . ?
W4 O36 W10 145.3(6) . . ?
W4 O36 Na2 103.8(4) . . ?
W10 O36 Na2 108.8(5) . . ?
W8 O38 Tm1 143.9(6) . . ?
C2 O40 Tm1 138.3(10) . 3_666 ?
Tm1 O41 K1 105.5(4) . . ?
C2 O41 Tm1 135.0(10) . . ?
C2 O41 K1 118.1(9) . . ?
Tm1 O42 Tm1 105.8(4) . 3_666 ?
C3 O42 Tm1 84.7(10) . 3_666 ?
C3 O42 Tm1 166.9(12) . . ?
Tm1 O43 K2 106.0(4) 3_666 3_666 ?
C3 O43 Tm1 106.4(10) . 3_666 ?
C3 O43 K2 145.0(10) . 3_666 ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
N1 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
N1 C1 C2 110.1(14) . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
O40 C2 O41 128.4(15) . . ?
O40 C2 C1 117.8(15) . . ?
O41 C2 C1 113.6(15) . . ?
O42 C3 Tm1 71.2(9) . 3_666 ?
O42 C3 O43 120.5(15) . . ?
O42 C3 C4 123.7(15) . . ?
O43 C3 Tm1 49.5(8) . 3_666 ?
O43 C3 C4 115.7(13) . . ?
C4 C3 Tm1 164.2(10) . 3_666 ?
N2 C4 C3 111.6(14) . . ?
N2 C4 H4A 109.3 . . ?
N2 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?

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
N1 H1C O12 0.89 2.26 3.025(18) 143.7 3_566
N1 H1C O24 0.89 2.51 3.236(17) 139.6 3_566
N1 H1D O5W 0.89 1.92 2.76(2) 157.4 4_576
N1 H1D O39 0.89 2.51 3.06(2) 120.8 3_666
N1 H1E O3 0.89 2.60 3.32(2) 138.6 3_666
N1 H1E O33 0.89 2.55 3.38(2) 156.1 3_666
N2 H2A O37 0.89 1.94 2.755(19) 150.9 4_576
N2 H2B O3W 0.89 2.06 2.90(2) 157.0 4_576
N2 H2B O38 0.89 2.63 3.112(18) 115.1 .
N2 H2C O16 0.89 2.43 2.998(17) 121.6 .
N2 H2C O21 0.89 2.21 3.084(18) 167.0 .

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1495661'
_audit_update_record             
;
2016-09-05 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT201_2                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......    1 Report 
RESPONSE: Due to the large structure and the existence of a large 
 amount of weight atoms, the intensity data are not very good, 
 leading to the ADP max/min ratio of some water molecules, 
 and it is very difficult to refine this large structure. Therefore,
 in the final refinement, all the W, B, lanthanoid, Na and K atoms 
 were refined anisotropically and some water molecules
 were refined isotropically.
;

_vrf_PLAT220_2                   
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range   8.3 Ratio 
RESPONSE: In polyoxometalate (POM) compounds, the Ueq of oxygen atoms in
 the POM skeleton is small due to multiple covalent bonds, whereas
 the Ueq of these discrete water oxygen atoms is biggish 
 without the constraint of covalent bonds. 
;

_vrf_PLAT306_2                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check  
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

_vrf_PLAT430_2                   
;
PROBLEM:  Short Inter D...A Contact  O3W    ..  O5W     ..       2.80 Ang.  
RESPONSE: In the crystal structure, there are a number of short connections
 between  OW(H2O) and O(POM) or OW(H2O) atoms in the range 2.75-2.81 Ang,
 which indicate extensive H bonding interactions among them. 
 
;

# end Validation Reply Form

_audit_creation_date             2016-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C16 H40 B4 K8 N8 Na8 O200 Pr4 W44), 9(O)'
_chemical_formula_sum            'C8 H70 B2 K4 N4 Na4 O109 Pr2 W22'
_chemical_formula_weight         6563.18
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        P2(1)/c
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.7518(9)
_cell_length_b                   21.4795(16)
_cell_length_c                   21.3507(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9080(10)
_cell_angle_gamma                90.00
_cell_volume                     5386.4(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4870
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.138
_cell_measurement_theta_min      2.220
_exptl_absorpt_coefficient_mu    24.559
_exptl_absorpt_correction_T_max  0.1199
_exptl_absorpt_correction_T_min  0.0839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0954 before and 0.0585 after correction. The Ratio of minimum to maximum transmission is 0.6445. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    4.047
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5788
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 Thanks to the large structure of 2 and the existence of a 
large amount of weight atoms, the intensity data are not 
very good, leading to the ADP max/min ratio of some atoms,
and it is very difficult to refine this large structure,
therefore, some unit-occupancy atoms have been refined 
isotropically and restrainedly refined. The ISOR 
instruction is used for C3, O10, O31, O6, O26, C2 and B1. 
O6W-O9W and O11W-O14W are refined isostropicallly. 
680 parameters and 42 restraints are used in the 
refinement. 
;
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27048
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         27048
_reflns_number_gt                6892
_reflns_number_total             9363
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         2.146
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.355
_refine_ls_extinction_coef       0.000063(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         9363
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0405
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0176P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0780
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(B1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O8W(0.5) O9W(0.5) O11W(0.5) O13W(0.5) O14W(0.5)
 Fixed Uiso: O8W(0.08474) O13W(0.08046)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
4.b Me refined with riding coordinates:
 N1(H1C,H1D,H1E), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pr1 Pr 0.39252(6) 0.52134(4) 0.42485(4) 0.01242(18) Uani 1 d . . . .
B1 B 0.2176(14) 0.6541(7) 0.2707(7) 0.013(4) Uani 1 d . . . U
W1 W 0.10207(5) 0.50598(3) 0.31883(3) 0.01442(14) Uani 1 d . . . .
W2 W -0.03235(5) 0.72872(3) 0.30628(3) 0.01824(15) Uani 1 d . . . .
W3 W 0.46258(5) 0.56937(3) 0.24143(3) 0.01644(15) Uani 1 d . . . .
W4 W 0.22091(5) 0.53259(3) 0.16261(3) 0.01675(15) Uani 1 d . . . .
W5 W 0.46974(5) 0.69323(3) 0.35337(3) 0.01714(15) Uani 1 d . . . .
W6 W 0.34891(5) 0.66619(3) 0.13118(3) 0.01796(15) Uani 1 d . . . .
W7 W 0.23448(5) 0.77319(3) 0.38385(3) 0.01787(15) Uani 1 d . . . .
W8 W 0.10336(5) 0.62160(3) 0.42396(3) 0.01497(14) Uani 1 d . . . .
W9 W 0.35479(5) 0.79272(3) 0.24651(3) 0.01851(15) Uani 1 d . . . .
W10 W -0.03910(5) 0.61275(3) 0.20144(3) 0.01772(15) Uani 1 d . . . .
W11 W 0.08451(5) 0.74849(3) 0.16679(3) 0.01866(15) Uani 1 d . . . .
Na1 Na 0.0979(7) 0.8957(4) 0.2783(4) 0.078(3) Uani 1 d . . . .
Na2 Na 0.0739(5) 0.6244(3) 0.0298(3) 0.0281(15) Uani 1 d . . . .
K1 K 0.1519(3) 0.37626(17) 0.42748(17) 0.0322(9) Uani 1 d . . . .
K2 K 0.3652(3) 0.41089(17) 0.27173(18) 0.0354(9) Uani 1 d . . . .
O1W O 0.2626(12) 0.9585(5) 0.3362(7) 0.063(4) Uani 1 d . . . .
O2W O 0.3401(12) 0.3451(6) 0.1604(6) 0.063(4) Uani 1 d . . . .
O3W O 0.2077(10) 0.8961(6) 0.0856(5) 0.048(3) Uani 1 d . . . .
O4W O -0.3276(11) 0.7093(6) 0.1922(7) 0.068(4) Uani 1 d . . . .
O5W O 0.2345(10) 0.9581(6) 0.2005(6) 0.051(4) Uani 1 d . . . .
O6W O 0.2577(16) 0.2851(8) 0.5004(9) 0.108(6) Uiso 1 d . . . .
O7W O -0.039(2) 0.7291(10) -0.0152(11) 0.144(8) Uiso 1 d . . . .
O8W O 0.364(3) 0.5727(15) -0.0160(15) 0.085 Uiso 0.50 d . . . .
O9W O 0.549(2) 0.6510(12) -0.0408(12) 0.057(7) Uiso 0.50 d . . . .
O10W O 0.2244(10) 0.3259(5) 0.3178(6) 0.043(3) Uani 1 d . . . .
O11W O 0.646(3) 0.5766(18) 0.0882(16) 0.094(11) Uiso 0.50 d . . . .
O12W O -0.3406(17) 0.6349(10) 0.0842(9) 0.115(7) Uiso 1 d . . . .
O13W O -0.011(3) 0.6086(14) -0.1049(15) 0.080 Uiso 0.50 d . . . .
O14W O -0.158(2) 0.5786(12) 0.0169(13) 0.062(8) Uiso 0.50 d . . . .
O1 O -0.1448(9) 0.7685(5) 0.3375(5) 0.033(3) Uani 1 d . . . .
O2 O 0.2125(9) 0.8267(5) 0.4393(5) 0.031(3) Uani 1 d . . . .
O3 O 0.6036(9) 0.7006(5) 0.3890(5) 0.033(3) Uani 1 d . . . .
O4 O 0.1945(9) 0.4706(4) 0.1137(5) 0.026(3) Uani 1 d . . . .
O5 O 0.2879(7) 0.7074(4) 0.3000(4) 0.013(2) Uani 1 d . . . .
O6 O 0.1963(7) 0.6075(4) 0.3237(4) 0.014(2) Uani 1 d . . . U
O7 O 0.3756(8) 0.5137(4) 0.1860(4) 0.019(2) Uani 1 d . . . .
O8 O 0.3905(8) 0.7366(4) 0.1817(4) 0.020(2) Uani 1 d . . . .
O9 O 0.4734(8) 0.6211(4) 0.1613(4) 0.020(2) Uani 1 d . . . .
O10 O -0.0191(8) 0.7759(4) 0.2296(4) 0.020(2) Uani 1 d . . . U
O11 O 0.2891(8) 0.8285(4) 0.3190(5) 0.021(2) Uani 1 d . . . .
O12 O -0.1196(8) 0.6686(4) 0.2553(4) 0.017(2) Uani 1 d . . . .
O13 O 0.0908(8) 0.7761(4) 0.3404(4) 0.016(2) Uani 1 d . . . .
O14 O 0.1082(7) 0.6768(4) 0.2461(4) 0.016(2) Uani 1 d . . . .
O15 O 0.4089(9) 0.8601(5) 0.2175(5) 0.033(3) Uani 1 d . . . .
O16 O 0.3885(8) 0.7527(4) 0.4046(4) 0.018(2) Uani 1 d . . . .
O17 O 0.4799(8) 0.7660(4) 0.2946(5) 0.024(2) Uani 1 d . . . .
O18 O 0.4116(8) 0.5357(5) 0.3104(4) 0.024(3) Uani 1 d . . . .
O19 O 0.0221(8) 0.4388(5) 0.3181(5) 0.027(3) Uani 1 d . . . .
O20 O 0.2773(8) 0.5903(4) 0.1027(4) 0.020(2) Uani 1 d . . . .
O21 O 0.4070(8) 0.6302(4) 0.3946(5) 0.022(2) Uani 1 d . . . .
O22 O 0.2030(8) 0.7933(4) 0.2096(5) 0.021(2) Uani 1 d . . . .
O23 O 0.0362(8) 0.5490(4) 0.3877(5) 0.020(2) Uani 1 d . . . .
O24 O -0.0072(8) 0.5590(4) 0.2659(4) 0.017(2) Uani 1 d . . . .
O25 O 0.1756(8) 0.5001(4) 0.2402(4) 0.023(2) Uani 1 d . . . .
O26 O -0.0034(7) 0.6695(4) 0.3646(4) 0.017(2) Uani 1 d . . . U
O27 O 0.0431(9) 0.8015(5) 0.1103(5) 0.028(3) Uani 1 d . . . .
O28 O -0.0227(8) 0.6846(5) 0.1456(4) 0.023(2) Uani 1 d . . . .
O29 O -0.1571(9) 0.5785(5) 0.1655(5) 0.035(3) Uani 1 d . . . .
O30 O 0.2227(8) 0.4838(4) 0.3657(4) 0.019(2) Uani 1 d . . . .
O31 O 0.1980(8) 0.7023(4) 0.1270(4) 0.018(2) Uani 1 d . . . U
O32 O 0.0235(8) 0.6293(5) 0.4892(4) 0.023(2) Uani 1 d . . . .
O33 O 0.5071(8) 0.6440(5) 0.2837(5) 0.025(3) Uani 1 d . . . .
O34 O 0.1834(8) 0.6998(4) 0.4241(4) 0.020(2) Uani 1 d . . . .
O35 O 0.2851(8) 0.6216(4) 0.2219(4) 0.020(2) Uani 1 d . . . .
O36 O 0.0797(8) 0.5738(4) 0.1567(4) 0.022(2) Uani 1 d . . . .
O37 O 0.3980(8) 0.6908(4) 0.0602(5) 0.024(3) Uani 1 d . . . .
O38 O 0.2262(7) 0.5823(4) 0.4541(4) 0.014(2) Uani 1 d . . . .
O39 O 0.5941(8) 0.5345(5) 0.2335(5) 0.029(3) Uani 1 d . . . .
O40 O 0.4051(8) 0.4586(4) 0.5927(4) 0.020(2) Uani 1 d . . . .
O41 O 0.2949(8) 0.4560(5) 0.5046(5) 0.024(2) Uani 1 d . . . .
O42 O 0.4638(8) 0.5681(4) 0.5239(4) 0.019(2) Uani 1 d . . . .
O43 O 0.5730(9) 0.5883(5) 0.6055(5) 0.029(3) Uani 1 d . . . .
N1 N 0.2449(11) 0.4139(7) 0.6628(6) 0.042(4) Uani 1 d . . . .
H1C H 0.1850 0.3985 0.6820 0.063 Uiso 1 calc . . R .
H1D H 0.2625 0.4510 0.6789 0.063 Uiso 1 calc . . R .
H1E H 0.3039 0.3883 0.6684 0.063 Uiso 1 calc . . R .
N2 N 0.3645(11) 0.6846(6) 0.5258(6) 0.031(3) Uani 1 d . . . .
H2A H 0.3476 0.7250 0.5269 0.046 Uiso 1 calc . . R .
H2B H 0.3081 0.6628 0.5419 0.046 Uiso 1 calc . . R .
H2C H 0.3736 0.6729 0.4863 0.046 Uiso 1 calc . . R .
C1 C 0.2177(13) 0.4203(8) 0.5963(7) 0.030(4) Uani 1 d . . . .
H1A H 0.1516 0.4470 0.5904 0.036 Uiso 1 calc . . R .
H1B H 0.1988 0.3798 0.5788 0.036 Uiso 1 calc . . R .
C2 C 0.3162(12) 0.4476(6) 0.5619(7) 0.016(3) Uani 1 d . . . U
C3 C 0.5020(12) 0.6058(7) 0.5633(7) 0.016(3) Uani 1 d . . . U
C4 C 0.4709(14) 0.6732(8) 0.5627(9) 0.039(5) Uani 1 d . . . .
H4A H 0.4617 0.6873 0.6054 0.047 Uiso 1 calc . . R .
H4B H 0.5322 0.6970 0.5450 0.047 Uiso 1 calc . . R .


_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
Pr1 Pr1 4.1206(15) 3_666 ?
Pr1 K2 4.043(4) . ?
Pr1 O18 2.480(10) . ?
Pr1 O21 2.433(9) . ?
Pr1 O30 2.462(9) . ?
Pr1 O38 2.451(9) . ?
Pr1 O40 2.458(9) 3_666 ?
Pr1 O41 2.513(10) . ?
Pr1 O42 2.760(9) 3_666 ?
Pr1 O42 2.464(10) . ?
Pr1 O43 2.480(10) 3_666 ?
Pr1 C3 3.006(14) 3_666 ?
B1 O5 1.533(17) . ?
B1 O6 1.537(17) . ?
B1 O14 1.457(18) . ?
B1 O35 1.503(18) . ?
W1 K1 3.660(4) . ?
W1 K2 3.867(4) . ?
W1 O6 2.447(8) . ?
W1 O19 1.721(9) . ?
W1 O23 1.922(9) . ?
W1 O24 2.031(9) . ?
W1 O25 1.918(10) . ?
W1 O30 1.773(9) . ?
W2 O1 1.726(10) . ?
W2 O10 1.936(10) . ?
W2 O12 1.957(9) . ?
W2 O13 1.895(9) . ?
W2 O14 2.401(9) . ?
W2 O26 1.805(9) . ?
W3 K2 3.656(4) . ?
W3 O7 1.948(9) . ?
W3 O9 2.047(9) . ?
W3 O18 1.764(9) . ?
W3 O33 1.905(10) . ?
W3 O35 2.392(9) . ?
W3 O39 1.731(10) . ?
W4 K2 3.856(4) . ?
W4 O4 1.714(9) . ?
W4 O7 1.912(9) . ?
W4 O20 1.916(9) . ?
W4 O25 1.890(9) . ?
W4 O35 2.400(10) . ?
W4 O36 1.882(10) . ?
W5 O3 1.731(10) . ?
W5 O5 2.406(9) . ?
W5 O16 1.952(9) . ?
W5 O17 2.010(9) . ?
W5 O21 1.788(9) . ?
W5 O33 1.888(10) . ?
W6 O8 1.911(9) . ?
W6 O9 1.852(10) . ?
W6 O20 1.924(9) . ?
W6 O31 1.936(9) . ?
W6 O35 2.308(9) . ?
W6 O37 1.722(10) . ?
W7 O2 1.676(10) . ?
W7 O5 2.381(9) . ?
W7 O11 1.949(9) . ?
W7 O13 1.901(9) . ?
W7 O16 1.901(9) . ?
W7 O34 1.902(9) . ?
W8 O6 2.455(9) . ?
W8 O23 1.900(9) . ?
W8 O26 2.033(9) . ?
W8 O32 1.714(9) . ?
W8 O34 1.925(9) . ?
W8 O38 1.775(9) . ?
W9 O5 2.312(9) . ?
W9 O8 1.893(10) . ?
W9 O11 1.915(10) . ?
W9 O15 1.707(10) . ?
W9 O17 1.856(10) . ?
W9 O22 1.926(10) . ?
W10 O12 1.931(9) . ?
W10 O14 2.384(9) . ?
W10 O24 1.827(9) . ?
W10 O28 1.964(10) . ?
W10 O29 1.726(10) . ?
W10 O36 1.910(9) . ?
W11 O10 1.933(9) . ?
W11 O14 2.299(9) . ?
W11 O22 1.902(10) . ?
W11 O27 1.718(9) . ?
W11 O28 1.907(10) . ?
W11 O31 1.886(9) . ?
Na1 O1W 2.633(17) . ?
Na1 O5W 2.705(15) . ?
Na1 O13W 2.84(3) 4_576 ?
Na1 O11 2.785(12) . ?
Na1 O13 2.892(12) . ?
Na1 O19 2.625(13) 2 ?
Na1 O22 2.938(14) . ?
Na2 O7W 2.77(2) . ?
Na2 O14W 2.90(3) . ?
Na2 O2 2.775(11) 4_575 ?
Na2 O20 2.902(11) . ?
Na2 O31 3.006(11) . ?
Na2 O36 2.917(11) . ?
K1 K2 4.295(5) . ?
K1 O6W 2.771(19) . ?
K1 O10W 2.742(12) . ?
K1 O19 3.058(11) . ?
K1 O27 2.890(11) 2_545 ?
K1 O30 2.800(10) . ?
K1 O32 2.769(10) 3_566 ?
K1 O41 2.879(11) . ?
K1 O43 3.418(11) 3_666 ?
K2 O2W 2.773(14) . ?
K2 O10W 2.674(12) . ?
K2 O7 2.874(10) . ?
K2 O15 2.872(11) 2_645 ?
K2 O18 2.852(10) . ?
K2 O25 2.998(10) . ?
K2 O30 3.083(10) . ?
K2 O43 2.696(11) 3_666 ?
O11W O12W 1.27(3) 1_655 ?
O12W O11W 1.27(3) 1_455 ?
O13W Na1 2.84(3) 4_575 ?
O2 Na2 2.775(11) 4_576 ?
O15 K2 2.872(11) 2_655 ?
O19 Na1 2.625(13) 2_545 ?
O27 K1 2.890(11) 2 ?
O32 K1 2.769(10) 3_566 ?
O40 Pr1 2.458(9) 3_666 ?
O40 C2 1.239(16) . ?
O41 C2 1.253(16) . ?
O42 Pr1 2.760(9) 3_666 ?
O42 C3 1.240(16) . ?
O43 Pr1 2.480(10) 3_666 ?
O43 K1 3.418(11) 3_666 ?
O43 K2 2.696(11) 3_666 ?
O43 C3 1.265(17) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N1 C1 1.453(19) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.477(18) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.510(19) . ?
C3 Pr1 3.006(14) 3_666 ?
C3 C4 1.49(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
K2 Pr1 Pr1 121.96(6) . 3_666 ?
O18 Pr1 Pr1 136.2(2) . 3_666 ?
O18 Pr1 K2 44.2(2) . . ?
O18 Pr1 O41 142.7(3) . . ?
O18 Pr1 O42 113.7(3) . 3_666 ?
O18 Pr1 O43 80.7(3) . 3_666 ?
O18 Pr1 C3 98.3(4) . 3_666 ?
O21 Pr1 Pr1 111.9(2) . 3_666 ?
O21 Pr1 K2 110.7(2) . . ?
O21 Pr1 O18 67.0(3) . . ?
O21 Pr1 O30 104.0(3) . . ?
O21 Pr1 O38 67.5(3) . . ?
O21 Pr1 O40 73.4(3) . 3_666 ?
O21 Pr1 O41 138.9(3) . . ?
O21 Pr1 O42 136.6(3) . 3_666 ?
O21 Pr1 O42 79.1(3) . . ?
O21 Pr1 O43 146.1(3) . 3_666 ?
O21 Pr1 C3 149.6(3) . 3_666 ?
O30 Pr1 Pr1 142.4(2) . 3_666 ?
O30 Pr1 K2 49.6(2) . . ?
O30 Pr1 O18 68.5(3) . . ?
O30 Pr1 O41 77.5(3) . . ?
O30 Pr1 O42 116.7(3) . 3_666 ?
O30 Pr1 O42 145.2(3) . . ?
O30 Pr1 O43 72.0(3) . 3_666 ?
O30 Pr1 C3 94.0(3) . 3_666 ?
O38 Pr1 Pr1 113.2(2) . 3_666 ?
O38 Pr1 K2 118.5(2) . . ?
O38 Pr1 O18 106.5(3) . . ?
O38 Pr1 O30 70.5(3) . . ?
O38 Pr1 O40 136.8(3) . 3_666 ?
O38 Pr1 O41 74.9(3) . . ?
O38 Pr1 O42 138.9(3) . 3_666 ?
O38 Pr1 O42 79.3(3) . . ?
O38 Pr1 O43 135.5(3) . 3_666 ?
O38 Pr1 C3 142.6(3) . 3_666 ?
O40 Pr1 Pr1 65.6(2) 3_666 3_666 ?
O40 Pr1 K2 91.7(2) 3_666 . ?
O40 Pr1 O18 73.0(3) 3_666 . ?
O40 Pr1 O30 138.7(3) 3_666 . ?
O40 Pr1 O41 131.9(3) 3_666 . ?
O40 Pr1 O42 75.9(3) 3_666 . ?
O40 Pr1 O42 66.4(3) 3_666 3_666 ?
O40 Pr1 O43 87.7(3) 3_666 3_666 ?
O40 Pr1 C3 76.9(3) 3_666 3_666 ?
O41 Pr1 Pr1 68.3(2) . 3_666 ?
O41 Pr1 K2 101.2(2) . . ?
O41 Pr1 O42 68.3(3) . 3_666 ?
O41 Pr1 C3 68.4(3) . 3_666 ?
O42 Pr1 Pr1 40.5(2) . 3_666 ?
O42 Pr1 Pr1 35.5(2) 3_666 3_666 ?
O42 Pr1 K2 161.7(2) . . ?
O42 Pr1 K2 86.7(2) 3_666 . ?
O42 Pr1 O18 139.1(3) . . ?
O42 Pr1 O41 78.2(3) . . ?
O42 Pr1 O42 76.0(3) . 3_666 ?
O42 Pr1 O43 123.9(3) . 3_666 ?
O42 Pr1 C3 99.8(4) . 3_666 ?
O42 Pr1 C3 24.4(3) 3_666 3_666 ?
O43 Pr1 Pr1 83.8(2) 3_666 3_666 ?
O43 Pr1 K2 40.6(2) 3_666 . ?
O43 Pr1 O41 74.3(3) 3_666 . ?
O43 Pr1 O42 48.6(3) 3_666 3_666 ?
O43 Pr1 C3 24.3(3) 3_666 3_666 ?
C3 Pr1 Pr1 59.5(3) 3_666 3_666 ?
C3 Pr1 K2 63.7(3) 3_666 . ?
O5 B1 O6 106.5(11) . . ?
O14 B1 O5 110.8(11) . . ?
O14 B1 O6 108.6(11) . . ?
O14 B1 O35 112.7(12) . . ?
O35 B1 O5 109.9(11) . . ?
O35 B1 O6 108.1(11) . . ?
K1 W1 K2 69.53(8) . . ?
O6 W1 K1 126.1(2) . . ?
O6 W1 K2 96.7(2) . . ?
O19 W1 K1 56.2(3) . . ?
O19 W1 K2 89.8(3) . . ?
O19 W1 O6 173.5(4) . . ?
O19 W1 O23 100.2(4) . . ?
O19 W1 O24 97.4(4) . . ?
O19 W1 O25 101.4(4) . . ?
O19 W1 O30 101.9(5) . . ?
O23 W1 K1 86.6(3) . . ?
O23 W1 K2 143.0(3) . . ?
O23 W1 O6 74.5(3) . . ?
O23 W1 O24 83.8(4) . . ?
O24 W1 K1 149.8(3) . . ?
O24 W1 K2 130.4(3) . . ?
O24 W1 O6 78.5(3) . . ?
O25 W1 K1 115.9(3) . . ?
O25 W1 K2 49.5(3) . . ?
O25 W1 O6 83.0(4) . . ?
O25 W1 O23 155.0(4) . . ?
O25 W1 O24 81.1(4) . . ?
O30 W1 K1 47.9(3) . . ?
O30 W1 K2 51.2(3) . . ?
O30 W1 O6 82.2(4) . . ?
O30 W1 O23 91.8(4) . . ?
O30 W1 O24 160.7(4) . . ?
O30 W1 O25 95.8(4) . . ?
O1 W2 O10 98.7(5) . . ?
O1 W2 O12 98.5(4) . . ?
O1 W2 O13 99.8(4) . . ?
O1 W2 O14 170.3(4) . . ?
O1 W2 O26 102.2(5) . . ?
O10 W2 O12 86.0(4) . . ?
O10 W2 O14 73.4(3) . . ?
O12 W2 O14 75.7(3) . . ?
O13 W2 O10 87.8(4) . . ?
O13 W2 O12 161.4(4) . . ?
O13 W2 O14 85.7(3) . . ?
O26 W2 O10 159.1(4) . . ?
O26 W2 O12 90.1(4) . . ?
O26 W2 O13 89.4(4) . . ?
O26 W2 O14 85.7(4) . . ?
O7 W3 K2 51.3(3) . . ?
O7 W3 O9 82.6(4) . . ?
O7 W3 O35 75.2(4) . . ?
O9 W3 K2 133.0(3) . . ?
O9 W3 O35 71.2(3) . . ?
O18 W3 K2 49.7(3) . . ?
O18 W3 O7 94.0(4) . . ?
O18 W3 O9 162.3(4) . . ?
O18 W3 O33 92.6(4) . . ?
O18 W3 O35 91.1(4) . . ?
O33 W3 K2 141.5(3) . . ?
O33 W3 O7 159.2(4) . . ?
O33 W3 O9 85.1(4) . . ?
O33 W3 O35 85.0(4) . . ?
O35 W3 K2 101.0(2) . . ?
O39 W3 K2 84.3(3) . . ?
O39 W3 O7 97.3(4) . . ?
O39 W3 O9 94.2(4) . . ?
O39 W3 O18 103.5(5) . . ?
O39 W3 O33 100.3(5) . . ?
O39 W3 O35 164.1(4) . . ?
O4 W4 K2 84.7(4) . . ?
O4 W4 O7 98.4(4) . . ?
O4 W4 O20 99.0(4) . . ?
O4 W4 O25 101.3(4) . . ?
O4 W4 O35 170.9(4) . . ?
O4 W4 O36 100.6(5) . . ?
O7 W4 K2 45.9(3) . . ?
O7 W4 O20 88.0(4) . . ?
O7 W4 O35 75.6(4) . . ?
O20 W4 K2 133.4(3) . . ?
O20 W4 O35 74.2(4) . . ?
O25 W4 K2 49.6(3) . . ?
O25 W4 O7 89.2(4) . . ?
O25 W4 O20 159.7(4) . . ?
O25 W4 O35 85.7(4) . . ?
O35 W4 K2 95.6(2) . . ?
O36 W4 K2 136.8(3) . . ?
O36 W4 O7 161.1(4) . . ?
O36 W4 O20 88.5(4) . . ?
O36 W4 O25 87.7(4) . . ?
O36 W4 O35 85.5(4) . . ?
O3 W5 O5 167.3(4) . . ?
O3 W5 O16 98.5(5) . . ?
O3 W5 O17 97.5(4) . . ?
O3 W5 O21 103.7(5) . . ?
O3 W5 O33 99.5(5) . . ?
O16 W5 O5 74.9(3) . . ?
O16 W5 O17 83.2(4) . . ?
O17 W5 O5 71.1(3) . . ?
O21 W5 O5 87.4(4) . . ?
O21 W5 O16 90.2(4) . . ?
O21 W5 O17 158.5(4) . . ?
O21 W5 O33 94.3(4) . . ?
O33 W5 O5 85.7(4) . . ?
O33 W5 O16 159.9(4) . . ?
O33 W5 O17 85.6(4) . . ?
O8 W6 O20 161.8(4) . . ?
O8 W6 O31 85.7(4) . . ?
O8 W6 O35 86.5(4) . . ?
O9 W6 O8 91.9(4) . . ?
O9 W6 O20 90.0(4) . . ?
O9 W6 O31 159.7(4) . . ?
O9 W6 O35 76.5(4) . . ?
O20 W6 O31 86.2(4) . . ?
O20 W6 O35 76.3(4) . . ?
O31 W6 O35 83.3(4) . . ?
O37 W6 O8 99.6(4) . . ?
O37 W6 O9 100.5(4) . . ?
O37 W6 O20 97.9(4) . . ?
O37 W6 O31 99.8(4) . . ?
O37 W6 O35 173.3(4) . . ?
O2 W7 O5 171.3(4) . . ?
O2 W7 O11 98.4(4) . . ?
O2 W7 O13 99.6(5) . . ?
O2 W7 O16 99.3(5) . . ?
O2 W7 O34 101.0(4) . . ?
O11 W7 O5 74.2(3) . . ?
O13 W7 O5 84.6(3) . . ?
O13 W7 O11 86.6(4) . . ?
O13 W7 O16 161.0(4) . . ?
O13 W7 O34 87.7(4) . . ?
O16 W7 O5 76.4(3) . . ?
O16 W7 O11 88.4(4) . . ?
O16 W7 O34 90.9(4) . . ?
O34 W7 O5 86.7(3) . . ?
O34 W7 O11 160.5(4) . . ?
O23 W8 O6 74.6(3) . . ?
O23 W8 O26 85.5(4) . . ?
O23 W8 O34 155.9(4) . . ?
O26 W8 O6 78.6(3) . . ?
O32 W8 O6 173.1(4) . . ?
O32 W8 O23 100.3(4) . . ?
O32 W8 O26 96.6(4) . . ?
O32 W8 O34 101.3(4) . . ?
O32 W8 O38 102.2(4) . . ?
O34 W8 O6 82.9(3) . . ?
O34 W8 O26 81.4(4) . . ?
O38 W8 O6 83.0(4) . . ?
O38 W8 O23 94.6(4) . . ?
O38 W8 O26 160.9(4) . . ?
O38 W8 O34 91.3(4) . . ?
O8 W9 O5 86.8(3) . . ?
O8 W9 O11 162.3(4) . . ?
O8 W9 O22 86.0(4) . . ?
O11 W9 O5 76.5(3) . . ?
O11 W9 O22 86.3(4) . . ?
O15 W9 O5 171.7(4) . . ?
O15 W9 O8 100.4(5) . . ?
O15 W9 O11 96.8(4) . . ?
O15 W9 O17 99.5(5) . . ?
O15 W9 O22 101.3(5) . . ?
O17 W9 O5 75.9(3) . . ?
O17 W9 O8 90.9(4) . . ?
O17 W9 O11 90.6(4) . . ?
O17 W9 O22 159.1(4) . . ?
O22 W9 O5 83.3(4) . . ?
O12 W10 O14 76.5(3) . . ?
O12 W10 O28 86.1(4) . . ?
O24 W10 O12 92.1(4) . . ?
O24 W10 O14 86.3(4) . . ?
O24 W10 O28 158.9(4) . . ?
O24 W10 O36 88.0(4) . . ?
O28 W10 O14 72.8(3) . . ?
O29 W10 O12 97.3(5) . . ?
O29 W10 O14 170.0(4) . . ?
O29 W10 O24 102.0(5) . . ?
O29 W10 O28 99.1(4) . . ?
O29 W10 O36 100.4(5) . . ?
O36 W10 O12 161.9(4) . . ?
O36 W10 O14 85.4(4) . . ?
O36 W10 O28 87.3(4) . . ?
O10 W11 O14 75.9(4) . . ?
O22 W11 O10 88.9(4) . . ?
O22 W11 O14 85.2(4) . . ?
O22 W11 O28 161.0(4) . . ?
O27 W11 O10 96.6(4) . . ?
O27 W11 O14 170.4(4) . . ?
O27 W11 O22 100.8(5) . . ?
O27 W11 O28 98.1(5) . . ?
O27 W11 O31 102.7(4) . . ?
O28 W11 O10 87.5(4) . . ?
O28 W11 O14 75.8(4) . . ?
O31 W11 O10 160.7(4) . . ?
O31 W11 O14 84.8(3) . . ?
O31 W11 O22 88.0(4) . . ?
O31 W11 O28 89.2(4) . . ?
O1W Na1 O5W 66.0(4) . . ?
O1W Na1 O13W 87.2(8) . 4_576 ?
O1W Na1 O11 63.0(4) . . ?
O1W Na1 O13 105.8(4) . . ?
O1W Na1 O22 107.6(4) . . ?
O5W Na1 O13W 148.1(8) . 4_576 ?
O5W Na1 O11 87.7(4) . . ?
O5W Na1 O13 138.5(5) . . ?
O5W Na1 O22 78.2(4) . . ?
O13W Na1 O13 63.2(7) 4_576 . ?
O13W Na1 O22 128.6(7) 4_576 . ?
O11 Na1 O13W 95.3(7) . 4_576 ?
O11 Na1 O13 55.4(3) . . ?
O11 Na1 O22 54.6(3) . . ?
O13 Na1 O22 65.4(3) . . ?
O19 Na1 O1W 123.7(5) 2 . ?
O19 Na1 O5W 70.0(4) 2 . ?
O19 Na1 O13W 116.9(7) 2 4_576 ?
O19 Na1 O11 146.6(5) 2 . ?
O19 Na1 O13 130.5(5) 2 . ?
O19 Na1 O22 95.5(4) 2 . ?
O7W Na2 O14W 78.6(7) . . ?
O7W Na2 O2 74.8(5) . 4_575 ?
O7W Na2 O20 140.2(6) . . ?
O7W Na2 O31 90.2(5) . . ?
O7W Na2 O36 128.3(6) . . ?
O14W Na2 O31 133.3(6) . . ?
O14W Na2 O36 87.4(6) . . ?
O2 Na2 O14W 129.3(6) 4_575 . ?
O2 Na2 O20 88.7(3) 4_575 . ?
O2 Na2 O31 89.3(3) 4_575 . ?
O2 Na2 O36 142.3(4) 4_575 . ?
O20 Na2 O14W 136.0(6) . . ?
O20 Na2 O31 53.0(3) . . ?
O20 Na2 O36 54.2(3) . . ?
O36 Na2 O31 64.5(3) . . ?
Pr1 K1 K2 56.76(7) . . ?
W1 K1 Pr1 61.41(5) . . ?
W1 K1 K2 57.50(7) . . ?
O6W K1 Pr1 104.0(4) . . ?
O6W K1 W1 162.5(4) . . ?
O6W K1 K2 107.2(4) . . ?
O6W K1 O19 160.6(4) . . ?
O6W K1 O27 95.8(4) . 2_545 ?
O6W K1 O30 135.5(4) . . ?
O6W K1 O41 81.8(4) . . ?
O6W K1 O43 82.1(4) . 3_666 ?
O10W K1 Pr1 93.0(2) . . ?
O10W K1 W1 78.9(3) . . ?
O10W K1 K2 37.0(2) . . ?
O10W K1 O6W 93.1(5) . . ?
O10W K1 O19 71.5(3) . . ?
O10W K1 O27 78.9(3) . 2_545 ?
O10W K1 O30 79.5(3) . . ?
O10W K1 O32 142.3(3) . 3_566 ?
O10W K1 O41 122.1(3) . . ?
O10W K1 O43 65.7(3) . 3_666 ?
O19 K1 Pr1 89.00(19) . . ?
O19 K1 W1 27.89(18) . . ?
O19 K1 K2 67.8(2) . . ?
O19 K1 O43 101.3(3) . 3_666 ?
O27 K1 Pr1 159.1(2) 2_545 . ?
O27 K1 W1 97.9(2) 2_545 . ?
O27 K1 K2 111.0(2) 2_545 . ?
O27 K1 O19 70.1(3) 2_545 . ?
O27 K1 O43 144.3(3) 2_545 3_666 ?
O30 K1 Pr1 34.2(2) . . ?
O30 K1 W1 28.0(2) . . ?
O30 K1 K2 45.7(2) . . ?
O30 K1 O19 55.0(3) . . ?
O30 K1 O27 124.9(3) . 2_545 ?
O30 K1 O41 66.5(3) . . ?
O30 K1 O43 54.6(3) . 3_666 ?
O32 K1 Pr1 123.7(2) 3_566 . ?
O32 K1 W1 109.4(2) 3_566 . ?
O32 K1 K2 166.1(2) 3_566 . ?
O32 K1 O6W 86.5(4) 3_566 . ?
O32 K1 O19 98.4(3) 3_566 . ?
O32 K1 O27 63.6(3) 3_566 2_545 ?
O32 K1 O30 125.2(3) 3_566 . ?
O32 K1 O41 95.2(3) 3_566 . ?
O32 K1 O43 150.6(3) 3_566 3_666 ?
O41 K1 Pr1 35.7(2) . . ?
O41 K1 W1 89.3(2) . . ?
O41 K1 K2 89.7(2) . . ?
O41 K1 O19 116.2(3) . . ?
O41 K1 O27 158.8(3) . 2_545 ?
O41 K1 O43 56.5(3) . 3_666 ?
O43 K1 Pr1 36.09(17) 3_666 . ?
O43 K1 W1 80.34(19) 3_666 . ?
O43 K1 K2 38.86(19) 3_666 . ?
W1 K2 Pr1 61.48(6) . . ?
W3 K2 Pr1 65.16(6) . . ?
W3 K2 W1 79.16(7) . . ?
W3 K2 W4 52.84(5) . . ?
W4 K2 Pr1 96.45(8) . . ?
W4 K2 W1 57.30(5) . . ?
O2W K2 Pr1 174.6(3) . . ?
O2W K2 W1 115.4(3) . . ?
O2W K2 W3 110.4(3) . . ?
O2W K2 W4 78.2(3) . . ?
O2W K2 O7 81.4(4) . . ?
O2W K2 O15 87.0(4) . 2_645 ?
O2W K2 O18 137.8(4) . . ?
O2W K2 O25 94.4(4) . . ?
O2W K2 O30 140.5(4) . . ?
O10W K2 Pr1 97.9(3) . . ?
O10W K2 W1 75.8(3) . . ?
O10W K2 W3 154.5(3) . . ?
O10W K2 W4 114.8(3) . . ?
O10W K2 O2W 85.3(4) . . ?
O10W K2 O7 143.0(4) . . ?
O10W K2 O15 107.0(4) . 2_645 ?
O10W K2 O18 130.6(3) . . ?
O10W K2 O25 93.1(3) . . ?
O10W K2 O30 75.6(3) . . ?
O10W K2 O43 78.3(4) . 3_666 ?
O7 K2 Pr1 93.5(2) . . ?
O7 K2 W1 79.1(2) . . ?
O7 K2 W3 31.96(19) . . ?
O7 K2 W4 28.52(18) . . ?
O7 K2 O25 54.0(3) . . ?
O7 K2 O30 93.4(3) . . ?
O15 K2 Pr1 96.3(2) 2_645 . ?
O15 K2 W1 157.6(3) 2_645 . ?
O15 K2 W3 94.2(2) 2_645 . ?
O15 K2 W4 133.8(2) 2_645 . ?
O15 K2 O7 106.5(3) 2_645 . ?
O15 K2 O25 159.8(3) 2_645 . ?
O15 K2 O30 131.4(3) 2_645 . ?
O18 K2 Pr1 37.4(2) . . ?
O18 K2 W1 64.9(2) . . ?
O18 K2 W3 28.14(19) . . ?
O18 K2 W4 67.3(2) . . ?
O18 K2 O7 56.7(3) . . ?
O18 K2 O15 99.6(3) . 2_645 ?
O18 K2 O25 66.3(3) . . ?
O18 K2 O30 55.7(3) . . ?
O25 K2 Pr1 81.1(2) . . ?
O25 K2 W1 29.09(19) . . ?
O25 K2 W3 66.41(19) . . ?
O25 K2 W4 28.67(18) . . ?
O25 K2 O30 53.6(3) . . ?
O30 K2 Pr1 37.45(18) . . ?
O30 K2 W1 26.63(18) . . ?
O30 K2 W3 79.76(19) . . ?
O30 K2 W4 79.13(19) . . ?
O43 K2 Pr1 36.8(2) 3_666 . ?
O43 K2 W1 86.3(2) 3_666 . ?
O43 K2 W3 95.2(2) 3_666 . ?
O43 K2 W4 133.0(2) 3_666 . ?
O43 K2 O2W 148.7(4) 3_666 . ?
O43 K2 O7 126.8(3) 3_666 . ?
O43 K2 O15 72.9(3) 3_666 2_645 ?
O43 K2 O18 70.7(3) 3_666 . ?
O43 K2 O25 112.9(3) 3_666 . ?
O43 K2 O30 59.9(3) 3_666 . ?
K2 O10W K1 105.0(4) . . ?
W7 O2 Na2 149.3(6) . 4_576 ?
B1 O5 W5 123.9(8) . . ?
B1 O5 W7 126.7(8) . . ?
B1 O5 W9 125.2(8) . . ?
W7 O5 W5 88.4(3) . . ?
W9 O5 W5 91.3(3) . . ?
W9 O5 W7 90.2(3) . . ?
B1 O6 W1 129.3(8) . . ?
B1 O6 W8 130.5(8) . . ?
W1 O6 W8 86.1(3) . . ?
W3 O7 K2 96.7(4) . . ?
W4 O7 W3 120.2(5) . . ?
W4 O7 K2 105.6(4) . . ?
W9 O8 W6 149.0(5) . . ?
W6 O9 W3 120.2(5) . . ?
W11 O10 W2 119.8(5) . . ?
W7 O11 Na1 104.8(4) . . ?
W9 O11 W7 118.7(4) . . ?
W9 O11 Na1 107.4(5) . . ?
W10 O12 W2 118.9(5) . . ?
W2 O13 W7 145.5(5) . . ?
W2 O13 Na1 109.5(4) . . ?
W7 O13 Na1 102.4(4) . . ?
B1 O14 W2 125.2(8) . . ?
B1 O14 W10 124.9(8) . . ?
B1 O14 W11 125.0(8) . . ?
W10 O14 W2 88.8(3) . . ?
W11 O14 W2 90.8(3) . . ?
W11 O14 W10 91.4(3) . . ?
W9 O15 K2 130.4(5) . 2_655 ?
W7 O16 W5 120.0(5) . . ?
W9 O17 W5 121.6(5) . . ?
Pr1 O18 K2 98.4(3) . . ?
W3 O18 Pr1 156.6(5) . . ?
W3 O18 K2 102.2(4) . . ?
W1 O19 Na1 125.6(6) . 2_545 ?
W1 O19 K1 95.9(4) . . ?
Na1 O19 K1 133.2(4) 2_545 . ?
W4 O20 W6 119.6(5) . . ?
W4 O20 Na2 103.0(4) . . ?
W6 O20 Na2 107.5(4) . . ?
W5 O21 Pr1 153.2(5) . . ?
W9 O22 Na1 101.5(4) . . ?
W11 O22 W9 147.8(5) . . ?
W11 O22 Na1 107.8(4) . . ?
W8 O23 W1 122.3(5) . . ?
W10 O24 W1 152.1(5) . . ?
W1 O25 K2 101.5(4) . . ?
W4 O25 W1 153.0(5) . . ?
W4 O25 K2 101.8(4) . . ?
W2 O26 W8 152.3(5) . . ?
W11 O27 K1 140.2(5) . 2 ?
W11 O28 W10 119.9(5) . . ?
Pr1 O30 K1 106.1(3) . . ?
Pr1 O30 K2 93.0(3) . . ?
W1 O30 Pr1 145.2(5) . . ?
W1 O30 K1 104.1(4) . . ?
W1 O30 K2 102.2(4) . . ?
K1 O30 K2 93.7(3) . . ?
W6 O31 Na2 103.4(4) . . ?
W11 O31 W6 148.3(5) . . ?
W11 O31 Na2 105.7(4) . . ?
W8 O32 K1 163.3(5) . 3_566 ?
W5 O33 W3 141.0(5) . . ?
W7 O34 W8 152.1(5) . . ?
B1 O35 W3 125.0(8) . . ?
B1 O35 W4 124.9(8) . . ?
B1 O35 W6 125.6(8) . . ?
W3 O35 W4 88.6(3) . . ?
W6 O35 W3 92.0(3) . . ?
W6 O35 W4 89.6(3) . . ?
W4 O36 W10 146.1(6) . . ?
W4 O36 Na2 103.3(4) . . ?
W10 O36 Na2 107.9(4) . . ?
W8 O38 Pr1 143.8(5) . . ?
C2 O40 Pr1 139.0(9) . 3_666 ?
Pr1 O41 K1 102.4(4) . . ?
C2 O41 Pr1 131.4(9) . . ?
C2 O41 K1 124.5(9) . . ?
Pr1 O42 Pr1 104.0(3) . 3_666 ?
C3 O42 Pr1 162.4(9) . . ?
C3 O42 Pr1 89.0(8) . 3_666 ?
Pr1 O43 K1 89.6(3) 3_666 3_666 ?
Pr1 O43 K2 102.7(4) 3_666 3_666 ?
K2 O43 K1 88.5(3) 3_666 3_666 ?
C3 O43 Pr1 101.8(9) . 3_666 ?
C3 O43 K1 113.1(9) . 3_666 ?
C3 O43 K2 147.2(9) . 3_666 ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C2 111.4(13) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
O40 C2 O41 128.9(14) . . ?
O40 C2 C1 117.5(14) . . ?
O41 C2 C1 113.5(13) . . ?
O42 C3 Pr1 66.6(8) . 3_666 ?
O42 C3 O43 120.3(13) . . ?
O42 C3 C4 122.9(14) . . ?
O43 C3 Pr1 53.8(7) . 3_666 ?
O43 C3 C4 116.7(13) . . ?
C4 C3 Pr1 169.0(10) . 3_666 ?
N2 C4 C3 111.6(13) . . ?
N2 C4 H4A 109.3 . . ?
N2 C4 H4B 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?

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
N1 H1C O12 0.89 2.13 2.922(16) 148.1 3_566
N1 H1C O24 0.89 2.57 3.277(16) 137.3 3_566
N1 H1D O5W 0.89 2.03 2.868(19) 155.4 4_576
N1 H1D O39 0.89 2.49 3.071(17) 122.9 3_666
N1 H1E O3 0.89 2.53 3.252(18) 138.4 3_666
N1 H1E O33 0.89 2.51 3.334(17) 154.0 3_666
N2 H2A O37 0.89 2.03 2.800(15) 144.8 4_576
N2 H2B O3W 0.89 1.98 2.861(18) 168.4 4_576
N2 H2C O16 0.89 2.46 2.994(16) 119.3 .
N2 H2C O21 0.89 2.21 3.091(16) 170.9 .

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1495662'
_audit_update_record             
;
2016-09-05 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT220_4                   
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range   6.5 Ratio 
RESPONSE: In polyoxometalate (POM) compounds, the Ueq of oxygen atoms in
 the POM skeleton is small due to multiple covalent bonds, whereas
 the Ueq of these discrete water oxygen atoms is biggish 
 without the constraint of covalent bonds. 
;

_vrf_PLAT306_4                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......   O3W Check  
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

_vrf_PLAT430_4                   
;
PROBLEM: Short Inter D...A Contact O1W    ..  O39     ..       2.75 Ang.
RESPONSE: In the crystal structure, there are a number of short connections
 between  OW(H2O) and O(POM) or OW(H2O) atoms in the range 2.70-2.83 Ang,
 which indicate extensive H bonding interactions among them. 
;

# end Validation Reply Form


_audit_creation_date             2016-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C16 H40 B4 K8 N8 Na8 O194 Sm4 W44), 12(O)'
_chemical_formula_sum            'C8 H70 B2 K4 N4 Na4 O109 Sm2 W22'
_chemical_formula_weight         6582.06
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        P2(1)/c
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.7598(7)
_cell_length_b                   21.7014(14)
_cell_length_c                   21.7560(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.4250(10)
_cell_angle_gamma                90.00
_cell_volume                     5547.2(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3286
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.969
_cell_measurement_theta_min      2.213
_exptl_absorpt_coefficient_mu    24.028
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1455 before and 0.0572 after correction. 
The Ratio of minimum to maximum transmission is 0.4419. 
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'Pale yellow '
_exptl_crystal_density_diffrn    3.941
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5800
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
Thanks to the large structure of 4 and the existence of a 
large amount of weight atoms, the intensity data are not 
very good, leading to the ADP max/min ratio of some atoms,
and it is very difficult to refine this large structure,
therefore, some unit-occupancy atoms have been refined 
isotropically and restrainedly refined. The ISOR 
instruction is used for O14, B1, N2, O14, O12, O13W, 
O3, O43, O23, O1, and Na1. O8W-O9W, O11W, O12W and
O14W are refined isostropicallly. 
692 parameters and 66 restraints are used in the 
refinement.
;
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27769
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.97
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         27946
_reflns_number_gt                6604
_reflns_number_total             9609
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         3.961
_refine_diff_density_min         -2.173
_refine_diff_density_rms         0.359
_refine_ls_extinction_coef       0.000037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         9609
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0429
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0008P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0717
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13W) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(O43) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Na1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O8W(0.5) O11W(0.5) O12W(0.5) O13W(0.5) O14W(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
4.b Me refined with riding coordinates:
 N1(H1C,H1D,H1E), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.39137(6) 0.52526(4) 0.42659(4) 0.01447(19) Uani 1 1 d . . .
B1 B 0.2124(15) 0.6594(8) 0.2776(8) 0.017(4) Uani 1 1 d U . .
W1 W 0.10058(5) 0.51086(3) 0.32398(3) 0.01798(16) Uani 1 1 d . . .
W2 W -0.03552(5) 0.73110(3) 0.31340(3) 0.02138(17) Uani 1 1 d . . .
W3 W 0.45901(5) 0.57443(3) 0.24866(3) 0.01811(16) Uani 1 1 d . . .
W4 W 0.21565(5) 0.53845(3) 0.17035(3) 0.02016(16) Uani 1 1 d . . .
W5 W 0.46802(5) 0.69571(3) 0.35938(3) 0.01872(16) Uani 1 1 d . . .
W6 W 0.34338(5) 0.67141(3) 0.14096(3) 0.02023(16) Uani 1 1 d . . .
W7 W 0.23261(5) 0.77508(3) 0.38975(3) 0.02083(16) Uani 1 1 d . . .
W8 W 0.10379(5) 0.62438(3) 0.42824(3) 0.01831(16) Uani 1 1 d . . .
W9 W 0.35079(5) 0.79578(3) 0.25493(3) 0.02068(16) Uani 1 1 d . . .
W10 W -0.04393(5) 0.61713(3) 0.20955(3) 0.02082(16) Uani 1 1 d . . .
W11 W 0.07929(5) 0.75204(3) 0.17627(3) 0.02079(16) Uani 1 1 d . . .
Na1 Na 0.0737(6) 0.9156(3) 0.3011(3) 0.046(2) Uani 1 1 d U . .
Na2 Na 0.0681(7) 0.6299(4) 0.0395(3) 0.060(2) Uani 1 1 d . . .
K1 K 0.1509(3) 0.37914(18) 0.42486(18) 0.0368(10) Uani 1 1 d . . .
K2 K 0.3674(3) 0.41649(17) 0.27386(17) 0.0349(10) Uani 1 1 d . . .
O1W O 0.2727(7) 0.9631(4) 0.3234(4) 0.014(2) Uiso 1 1 d . . .
O2W O 0.3405(10) 0.3490(6) 0.1666(6) 0.049(4) Uani 1 1 d . . .
O3W O 0.2057(10) 0.8932(6) 0.0892(6) 0.055(4) Uani 1 1 d . . .
O4W O -0.3317(10) 0.7168(6) 0.2025(7) 0.064(4) Uani 1 1 d . . .
O5W O 0.2324(11) 0.9657(6) 0.1958(6) 0.059(4) Uani 1 1 d . . .
O6W O 0.2699(15) 0.2917(8) 0.4944(7) 0.098(6) Uani 1 1 d . . .
O7W O -0.0310(13) 0.7229(7) -0.0033(6) 0.077(5) Uani 1 1 d . . .
O8W O 0.362(3) 0.5620(16) -0.0049(16) 0.097(11) Uiso 0.50 1 d P . .
O9W O 0.5378(17) 0.6579(10) -0.0336(10) 0.131(7) Uiso 1 1 d . . .
O10W O 0.2222(9) 0.3294(5) 0.3157(6) 0.042(3) Uani 1 1 d . . .
O11W O 0.627(2) 0.5713(12) 0.0929(11) 0.049(7) Uiso 0.50 1 d P . .
O12W O -0.245(2) 0.6956(13) 0.0841(13) 0.066(8) Uiso 0.50 1 d P . .
O13W O -0.0327(18) 0.6165(9) -0.0860(9) 0.029(5) Uani 0.50 1 d PU . .
O14W O 0.485(3) 0.5624(16) -0.1231(15) 0.090(10) Uiso 0.50 1 d P . .
O1 O -0.1460(8) 0.7697(5) 0.3434(5) 0.030(3) Uani 1 1 d U . .
O2 O 0.2109(9) 0.8270(5) 0.4465(5) 0.035(3) Uani 1 1 d . . .
O3 O 0.5992(8) 0.7045(5) 0.3945(5) 0.032(3) Uani 1 1 d U . .
O4 O 0.1878(9) 0.4780(5) 0.1213(5) 0.036(3) Uani 1 1 d . . .
O5 O 0.2866(8) 0.7102(4) 0.3077(5) 0.021(3) Uani 1 1 d . . .
O6 O 0.1937(8) 0.6120(5) 0.3287(4) 0.022(3) Uani 1 1 d . . .
O7 O 0.3705(8) 0.5190(5) 0.1947(4) 0.023(3) Uani 1 1 d . . .
O8 O 0.3852(8) 0.7397(5) 0.1908(5) 0.025(3) Uani 1 1 d . . .
O9 O 0.4676(8) 0.6262(5) 0.1702(5) 0.025(3) Uani 1 1 d . . .
O10 O -0.0216(8) 0.7786(4) 0.2403(5) 0.024(3) Uani 1 1 d . . .
O11 O 0.2861(8) 0.8287(5) 0.3281(5) 0.030(3) Uani 1 1 d . . .
O12 O -0.1230(8) 0.6718(5) 0.2624(4) 0.021(3) Uani 1 1 d U . .
O13 O 0.0892(8) 0.7780(5) 0.3466(5) 0.024(3) Uani 1 1 d . . .
O14 O 0.1040(8) 0.6813(4) 0.2543(4) 0.016(2) Uani 1 1 d U . .
O15 O 0.4048(9) 0.8616(5) 0.2266(5) 0.032(3) Uani 1 1 d . . .
O16 O 0.3846(8) 0.7547(5) 0.4093(5) 0.023(3) Uani 1 1 d . . .
O17 O 0.4778(8) 0.7683(4) 0.3015(4) 0.023(3) Uani 1 1 d . . .
O18 O 0.4081(8) 0.5411(4) 0.3154(5) 0.022(3) Uani 1 1 d . . .
O19 O 0.0222(9) 0.4439(5) 0.3258(5) 0.029(3) Uani 1 1 d . . .
O20 O 0.2712(8) 0.5954(5) 0.1121(5) 0.024(3) Uani 1 1 d . . .
O21 O 0.4118(8) 0.6330(4) 0.3992(5) 0.026(3) Uani 1 1 d . . .
O22 O 0.1992(8) 0.7962(4) 0.2170(4) 0.015(2) Uani 1 1 d . . .
O23 O 0.0358(7) 0.5534(5) 0.3911(4) 0.020(2) Uani 1 1 d U . .
O24 O -0.0092(8) 0.5641(5) 0.2731(5) 0.025(3) Uani 1 1 d . . .
O25 O 0.1708(9) 0.5037(5) 0.2466(5) 0.027(3) Uani 1 1 d . . .
O26 O -0.0030(8) 0.6714(5) 0.3719(5) 0.030(3) Uani 1 1 d . . .
O27 O 0.0381(8) 0.8033(5) 0.1212(4) 0.022(3) Uani 1 1 d . . .
O28 O -0.0272(8) 0.6884(5) 0.1549(5) 0.024(3) Uani 1 1 d . . .
O29 O -0.1616(8) 0.5837(5) 0.1743(5) 0.032(3) Uani 1 1 d . . .
O30 O 0.2238(8) 0.4881(5) 0.3687(4) 0.023(3) Uani 1 1 d . . .
O31 O 0.1910(8) 0.7067(4) 0.1362(4) 0.022(3) Uani 1 1 d . . .
O32 O 0.0258(9) 0.6307(5) 0.4935(5) 0.030(3) Uani 1 1 d . . .
O33 O 0.5068(8) 0.6487(4) 0.2903(4) 0.020(2) Uani 1 1 d . . .
O34 O 0.1814(8) 0.7028(5) 0.4265(4) 0.023(3) Uani 1 1 d . . .
O35 O 0.2806(8) 0.6263(4) 0.2289(4) 0.019(2) Uani 1 1 d . . .
O36 O 0.0737(8) 0.5788(5) 0.1647(4) 0.022(3) Uani 1 1 d . . .
O37 O 0.3887(9) 0.6956(5) 0.0703(5) 0.030(3) Uani 1 1 d . . .
O38 O 0.2283(8) 0.5834(4) 0.4575(4) 0.018(2) Uani 1 1 d . . .
O39 O 0.5879(8) 0.5399(5) 0.2403(5) 0.028(3) Uani 1 1 d . . .
O40 O 0.4102(8) 0.4568(5) 0.5890(5) 0.024(3) Uani 1 1 d . . .
O41 O 0.2980(8) 0.4599(5) 0.5003(5) 0.025(3) Uani 1 1 d . . .
O42 O 0.4639(8) 0.5676(5) 0.5234(5) 0.024(3) Uani 1 1 d . . .
O43 O 0.5674(9) 0.5798(5) 0.6078(5) 0.031(3) Uani 1 1 d U . .
N1 N 0.2456(11) 0.4114(7) 0.6555(6) 0.039(4) Uani 1 1 d . . .
H1C H 0.1840 0.3961 0.6723 0.058 Uiso 1 1 calc R . .
H1D H 0.2626 0.4478 0.6724 0.058 Uiso 1 1 calc R . .
H1E H 0.3038 0.3857 0.6620 0.058 Uiso 1 1 calc R . .
N2 N 0.3712(11) 0.6820(6) 0.5286(6) 0.034(4) Uani 1 1 d U . .
H2A H 0.3573 0.7222 0.5311 0.050 Uiso 1 1 calc R . .
H2B H 0.3104 0.6610 0.5396 0.050 Uiso 1 1 calc R . .
H2C H 0.3866 0.6724 0.4900 0.050 Uiso 1 1 calc R . .
C1 C 0.2236(13) 0.4190(8) 0.5898(7) 0.031(4) Uani 1 1 d . . .
H1A H 0.1564 0.4446 0.5832 0.037 Uiso 1 1 calc R . .
H1B H 0.2068 0.3790 0.5718 0.037 Uiso 1 1 calc R . .
C2 C 0.3186(13) 0.4471(8) 0.5572(8) 0.024(4) Uani 1 1 d . . .
C3 C 0.4999(12) 0.5997(8) 0.5668(8) 0.025(4) Uani 1 1 d . . .
C4 C 0.4690(15) 0.6662(8) 0.5696(8) 0.043(5) Uani 1 1 d . . .
H4A H 0.4514 0.6766 0.6115 0.051 Uiso 1 1 calc R . .
H4B H 0.5339 0.6908 0.5586 0.051 Uiso 1 1 calc R . .


_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
Sm1 K1 4.248(4) . ?
Sm1 K2 4.076(4) . ?
Sm1 O18 2.459(10) . ?
Sm1 O21 2.427(10) . ?
Sm1 O30 2.430(10) . ?
Sm1 O38 2.414(9) . ?
Sm1 O40 2.404(10) 3_666 ?
Sm1 O41 2.437(10) . ?
Sm1 O42 2.420(11) . ?
Sm1 O42 2.826(10) 3_666 ?
Sm1 O43 2.455(10) 3_666 ?
Sm1 C3 2.999(17) 3_666 ?
B1 O5 1.536(19) . ?
B1 O6 1.539(19) . ?
B1 O14 1.433(19) . ?
B1 O35 1.534(19) . ?
W1 K1 3.637(4) . ?
W1 K2 3.939(4) . ?
W1 O6 2.452(10) . ?
W1 O19 1.722(10) . ?
W1 O23 1.913(10) . ?
W1 O24 2.025(10) . ?
W1 O25 1.913(10) . ?
W1 O30 1.782(9) . ?
W2 O1 1.700(9) . ?
W2 O10 1.909(10) . ?
W2 O12 1.963(10) . ?
W2 O13 1.903(10) . ?
W2 O14 2.386(9) . ?
W2 O26 1.845(11) . ?
W3 K2 3.641(4) . ?
W3 O7 1.950(10) . ?
W3 O9 2.049(10) . ?
W3 O18 1.750(10) . ?
W3 O33 1.921(10) . ?
W3 O35 2.403(9) . ?
W3 O39 1.708(9) . ?
W4 K2 3.863(4) . ?
W4 O4 1.715(11) . ?
W4 O7 1.922(10) . ?
W4 O20 1.906(10) . ?
W4 O25 1.916(10) . ?
W4 O35 2.399(10) . ?
W4 O36 1.885(10) . ?
W5 O3 1.704(10) . ?
W5 O5 2.390(10) . ?
W5 O16 1.967(9) . ?
W5 O17 2.023(10) . ?
W5 O21 1.758(9) . ?
W5 O33 1.888(9) . ?
W6 O8 1.889(10) . ?
W6 O9 1.850(10) . ?
W6 O20 1.946(10) . ?
W6 O31 1.948(10) . ?
W6 O35 2.298(9) . ?
W6 O37 1.729(10) . ?
W7 O2 1.700(10) . ?
W7 O5 2.380(10) . ?
W7 O11 1.903(11) . ?
W7 O13 1.896(9) . ?
W7 O16 1.873(9) . ?
W7 O34 1.871(10) . ?
W8 O6 2.465(9) . ?
W8 O23 1.900(10) . ?
W8 O26 1.998(11) . ?
W8 O32 1.728(10) . ?
W8 O34 1.933(10) . ?
W8 O38 1.806(10) . ?
W9 O5 2.326(10) . ?
W9 O8 1.908(10) . ?
W9 O11 1.929(10) . ?
W9 O15 1.690(10) . ?
W9 O17 1.867(10) . ?
W9 O22 1.933(9) . ?
W10 O12 1.919(10) . ?
W10 O14 2.402(10) . ?
W10 O24 1.833(10) . ?
W10 O28 1.965(10) . ?
W10 O29 1.715(11) . ?
W10 O36 1.916(10) . ?
W11 O10 1.954(10) . ?
W11 O14 2.297(9) . ?
W11 O22 1.893(9) . ?
W11 O27 1.691(10) . ?
W11 O28 1.909(10) . ?
W11 O31 1.884(9) . ?
Na1 O1W 2.585(11) . ?
Na1 O13W 2.89(2) 4_576 ?
Na1 O19 3.000(13) 2 ?
Na2 O7W 2.491(19) . ?
Na2 O13W 2.95(2) . ?
Na2 O2 2.841(12) 4_575 ?
Na2 O20 2.905(13) . ?
Na2 O31 3.005(13) . ?
Na2 O36 2.938(12) . ?
K1 K2 4.317(5) . ?
K1 O6W 2.769(16) . ?
K1 O10W 2.771(12) . ?
K1 O19 2.939(12) . ?
K1 O27 2.910(11) 2_545 ?
K1 O30 2.812(11) . ?
K1 O32 2.798(10) 3_566 ?
K1 O41 2.918(11) . ?
K2 O2W 2.761(13) . ?
K2 O10W 2.729(11) . ?
K2 O7 2.815(11) . ?
K2 O15 2.932(11) 2_645 ?
K2 O18 2.886(10) . ?
K2 O25 3.028(11) . ?
K2 O30 3.134(10) . ?
K2 O43 2.655(11) 3_666 ?
O13W Na1 2.89(2) 4_575 ?
O2 Na2 2.841(12) 4_576 ?
O15 K2 2.932(11) 2_655 ?
O19 Na1 3.000(13) 2_545 ?
O27 K1 2.910(11) 2 ?
O32 K1 2.798(10) 3_566 ?
O40 Sm1 2.404(10) 3_666 ?
O40 C2 1.273(18) . ?
O41 C2 1.282(18) . ?
O42 Sm1 2.826(10) 3_666 ?
O42 C3 1.233(17) . ?
O43 Sm1 2.455(10) 3_666 ?
O43 K2 2.655(11) 3_666 ?
O43 C3 1.247(17) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N1 C1 1.451(19) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.466(19) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.480(19) . ?
C3 Sm1 2.999(17) 3_666 ?
C3 C4 1.49(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
K2 Sm1 K1 62.45(7) . . ?
O18 Sm1 K1 100.2(2) . . ?
O18 Sm1 K2 44.4(2) . . ?
O18 Sm1 O42 114.0(3) . 3_666 ?
O18 Sm1 C3 97.0(4) . 3_666 ?
O21 Sm1 K1 142.1(2) . . ?
O21 Sm1 K2 111.2(3) . . ?
O21 Sm1 O18 67.1(3) . . ?
O21 Sm1 O30 106.2(3) . . ?
O21 Sm1 O41 140.7(3) . . ?
O21 Sm1 O42 135.8(3) . 3_666 ?
O21 Sm1 O43 142.9(3) . 3_666 ?
O21 Sm1 C3 146.8(4) . 3_666 ?
O30 Sm1 K1 39.0(2) . . ?
O30 Sm1 K2 50.1(2) . . ?
O30 Sm1 O18 68.5(3) . . ?
O30 Sm1 O41 76.7(3) . . ?
O30 Sm1 O42 115.1(3) . 3_666 ?
O30 Sm1 O43 72.5(3) . 3_666 ?
O30 Sm1 C3 93.4(4) . 3_666 ?
O38 Sm1 K1 81.7(2) . . ?
O38 Sm1 K2 120.1(2) . . ?
O38 Sm1 O18 107.3(3) . . ?
O38 Sm1 O21 69.7(3) . . ?
O38 Sm1 O30 71.4(3) . . ?
O38 Sm1 O41 74.7(3) . . ?
O38 Sm1 O42 79.3(3) . . ?
O38 Sm1 O42 137.6(3) . 3_666 ?
O38 Sm1 O43 137.7(3) . 3_666 ?
O38 Sm1 C3 143.2(4) . 3_666 ?
O40 Sm1 K1 140.3(3) 3_666 . ?
O40 Sm1 K2 90.7(3) 3_666 . ?
O40 Sm1 O18 73.7(3) 3_666 . ?
O40 Sm1 O21 72.7(3) 3_666 . ?
O40 Sm1 O30 138.7(3) 3_666 . ?
O40 Sm1 O38 137.9(3) 3_666 . ?
O40 Sm1 O41 130.9(3) 3_666 . ?
O40 Sm1 O42 66.3(3) 3_666 3_666 ?
O40 Sm1 O42 75.7(3) 3_666 . ?
O40 Sm1 O43 84.4(4) 3_666 3_666 ?
O40 Sm1 C3 74.9(4) 3_666 3_666 ?
O41 Sm1 K1 41.7(3) . . ?
O41 Sm1 K2 100.5(3) . . ?
O41 Sm1 O18 141.8(3) . . ?
O41 Sm1 O42 67.2(3) . 3_666 ?
O41 Sm1 O43 76.1(3) . 3_666 ?
O41 Sm1 C3 69.2(4) . 3_666 ?
O42 Sm1 K1 82.0(2) 3_666 . ?
O42 Sm1 K1 120.1(2) . . ?
O42 Sm1 K2 159.9(2) . . ?
O42 Sm1 K2 85.4(2) 3_666 . ?
O42 Sm1 O18 139.7(3) . . ?
O42 Sm1 O21 79.2(4) . . ?
O42 Sm1 O30 145.6(3) . . ?
O42 Sm1 O41 78.5(4) . . ?
O42 Sm1 O42 75.6(4) . 3_666 ?
O42 Sm1 O43 123.5(3) . 3_666 ?
O42 Sm1 C3 99.7(4) . 3_666 ?
O42 Sm1 C3 24.2(3) 3_666 3_666 ?
O43 Sm1 K1 56.2(3) 3_666 . ?
O43 Sm1 K2 38.8(3) 3_666 . ?
O43 Sm1 O18 78.8(3) 3_666 . ?
O43 Sm1 O42 48.1(3) 3_666 3_666 ?
O43 Sm1 C3 23.9(4) 3_666 3_666 ?
C3 Sm1 K1 66.9(3) 3_666 . ?
C3 Sm1 K2 62.0(3) 3_666 . ?
O6 B1 O5 105.5(11) . . ?
O14 B1 O5 113.2(13) . . ?
O14 B1 O6 109.0(12) . . ?
O14 B1 O35 113.2(12) . . ?
O35 B1 O5 109.1(12) . . ?
O35 B1 O6 106.3(12) . . ?
K1 W1 K2 69.35(8) . . ?
O6 W1 K1 128.1(2) . . ?
O6 W1 K2 96.7(2) . . ?
O19 W1 K1 52.9(4) . . ?
O19 W1 K2 90.1(3) . . ?
O19 W1 O6 173.0(4) . . ?
O19 W1 O23 99.1(4) . . ?
O19 W1 O24 99.4(5) . . ?
O19 W1 O25 101.7(5) . . ?
O19 W1 O30 100.2(5) . . ?
O23 W1 K1 88.7(3) . . ?
O23 W1 K2 144.1(3) . . ?
O23 W1 O6 74.2(4) . . ?
O23 W1 O24 83.0(4) . . ?
O24 W1 K1 149.5(3) . . ?
O24 W1 K2 129.9(3) . . ?
O24 W1 O6 77.6(4) . . ?
O25 W1 K1 113.7(3) . . ?
O25 W1 K2 48.4(3) . . ?
O25 W1 O6 84.3(4) . . ?
O25 W1 O23 155.8(4) . . ?
O25 W1 O24 81.6(4) . . ?
O30 W1 K1 49.0(3) . . ?
O30 W1 K2 50.8(3) . . ?
O30 W1 O6 82.7(4) . . ?
O30 W1 O23 93.3(4) . . ?
O30 W1 O24 160.3(4) . . ?
O30 W1 O25 95.0(4) . . ?
O1 W2 O10 98.5(5) . . ?
O1 W2 O12 98.6(5) . . ?
O1 W2 O13 100.3(5) . . ?
O1 W2 O14 169.9(4) . . ?
O1 W2 O26 102.8(5) . . ?
O10 W2 O12 86.8(4) . . ?
O10 W2 O14 73.1(4) . . ?
O12 W2 O14 75.8(3) . . ?
O13 W2 O10 86.3(4) . . ?
O13 W2 O12 160.6(4) . . ?
O13 W2 O14 84.9(4) . . ?
O26 W2 O10 158.7(4) . . ?
O26 W2 O12 91.0(4) . . ?
O26 W2 O13 88.8(4) . . ?
O26 W2 O14 85.8(4) . . ?
O7 W3 K2 49.9(3) . . ?
O7 W3 O9 83.1(4) . . ?
O7 W3 O35 75.0(4) . . ?
O9 W3 K2 131.8(3) . . ?
O9 W3 O35 70.6(4) . . ?
O18 W3 K2 51.2(3) . . ?
O18 W3 O7 93.0(4) . . ?
O18 W3 O9 161.4(4) . . ?
O18 W3 O33 93.3(4) . . ?
O18 W3 O35 90.9(4) . . ?
O33 W3 K2 143.2(3) . . ?
O33 W3 O7 159.9(4) . . ?
O33 W3 O9 84.8(4) . . ?
O33 W3 O35 85.8(4) . . ?
O35 W3 K2 101.9(2) . . ?
O39 W3 K2 82.7(4) . . ?
O39 W3 O7 96.8(5) . . ?
O39 W3 O9 94.4(4) . . ?
O39 W3 O18 104.1(5) . . ?
O39 W3 O33 100.1(5) . . ?
O39 W3 O35 163.5(4) . . ?
O4 W4 K2 84.8(4) . . ?
O4 W4 O7 99.1(5) . . ?
O4 W4 O20 98.3(5) . . ?
O4 W4 O25 100.7(5) . . ?
O4 W4 O35 170.6(4) . . ?
O4 W4 O36 99.8(5) . . ?
O7 W4 K2 43.9(3) . . ?
O7 W4 O35 75.6(4) . . ?
O20 W4 K2 132.0(3) . . ?
O20 W4 O7 88.8(4) . . ?
O20 W4 O25 161.0(4) . . ?
O20 W4 O35 74.2(4) . . ?
O25 W4 K2 50.4(3) . . ?
O25 W4 O7 88.1(4) . . ?
O25 W4 O35 86.9(4) . . ?
O35 W4 K2 96.1(2) . . ?
O36 W4 K2 138.0(3) . . ?
O36 W4 O7 161.1(4) . . ?
O36 W4 O20 89.0(4) . . ?
O36 W4 O25 87.9(4) . . ?
O36 W4 O35 85.8(4) . . ?
O3 W5 O5 165.9(4) . . ?
O3 W5 O16 98.2(5) . . ?
O3 W5 O17 96.8(5) . . ?
O3 W5 O21 102.6(5) . . ?
O3 W5 O33 100.0(5) . . ?
O16 W5 O5 73.6(4) . . ?
O16 W5 O17 83.1(4) . . ?
O17 W5 O5 71.2(4) . . ?
O21 W5 O5 89.3(4) . . ?
O21 W5 O16 91.4(4) . . ?
O21 W5 O17 160.5(4) . . ?
O21 W5 O33 94.8(4) . . ?
O33 W5 O5 86.4(4) . . ?
O33 W5 O16 159.0(4) . . ?
O33 W5 O17 84.4(4) . . ?
O8 W6 O20 161.7(4) . . ?
O8 W6 O31 86.5(4) . . ?
O8 W6 O35 86.6(4) . . ?
O9 W6 O8 92.1(4) . . ?
O9 W6 O20 89.3(4) . . ?
O9 W6 O31 159.7(4) . . ?
O9 W6 O35 76.4(4) . . ?
O20 W6 O31 85.9(4) . . ?
O20 W6 O35 75.9(4) . . ?
O31 W6 O35 83.4(4) . . ?
O37 W6 O8 100.9(5) . . ?
O37 W6 O9 101.4(5) . . ?
O37 W6 O20 96.7(5) . . ?
O37 W6 O31 98.7(5) . . ?
O37 W6 O35 172.3(4) . . ?
O2 W7 O5 172.0(4) . . ?
O2 W7 O11 99.9(5) . . ?
O2 W7 O13 100.3(5) . . ?
O2 W7 O16 99.4(5) . . ?
O2 W7 O34 100.6(5) . . ?
O11 W7 O5 74.1(4) . . ?
O13 W7 O5 84.8(4) . . ?
O13 W7 O11 86.8(4) . . ?
O16 W7 O5 75.4(4) . . ?
O16 W7 O11 87.9(4) . . ?
O16 W7 O13 160.2(4) . . ?
O34 W7 O5 85.7(4) . . ?
O34 W7 O11 159.3(4) . . ?
O34 W7 O13 86.8(4) . . ?
O34 W7 O16 91.5(4) . . ?
O23 W8 O6 74.1(4) . . ?
O23 W8 O26 84.9(4) . . ?
O23 W8 O34 153.7(4) . . ?
O26 W8 O6 78.4(4) . . ?
O32 W8 O6 173.2(4) . . ?
O32 W8 O23 100.6(5) . . ?
O32 W8 O26 97.0(5) . . ?
O32 W8 O34 102.4(5) . . ?
O32 W8 O38 101.6(5) . . ?
O34 W8 O6 81.9(3) . . ?
O34 W8 O26 79.8(4) . . ?
O38 W8 O6 83.3(4) . . ?
O38 W8 O23 94.0(4) . . ?
O38 W8 O26 161.3(4) . . ?
O38 W8 O34 93.7(4) . . ?
O8 W9 O5 86.3(4) . . ?
O8 W9 O11 160.4(4) . . ?
O8 W9 O22 84.9(4) . . ?
O11 W9 O5 74.9(4) . . ?
O11 W9 O22 87.8(4) . . ?
O15 W9 O5 171.7(4) . . ?
O15 W9 O8 100.3(5) . . ?
O15 W9 O11 99.0(5) . . ?
O15 W9 O17 99.4(5) . . ?
O15 W9 O22 101.2(5) . . ?
O17 W9 O5 75.3(4) . . ?
O17 W9 O8 90.2(4) . . ?
O17 W9 O11 90.3(4) . . ?
O17 W9 O22 159.3(4) . . ?
O22 W9 O5 84.3(4) . . ?
O12 W10 O14 76.1(4) . . ?
O12 W10 O28 86.5(4) . . ?
O24 W10 O12 92.0(4) . . ?
O24 W10 O14 85.7(4) . . ?
O24 W10 O28 157.8(4) . . ?
O24 W10 O36 88.2(4) . . ?
O28 W10 O14 72.5(3) . . ?
O29 W10 O12 97.3(5) . . ?
O29 W10 O14 169.6(4) . . ?
O29 W10 O24 102.8(5) . . ?
O29 W10 O28 99.3(5) . . ?
O29 W10 O36 100.1(5) . . ?
O36 W10 O12 162.1(4) . . ?
O36 W10 O14 86.1(4) . . ?
O36 W10 O28 86.6(4) . . ?
O10 W11 O14 74.5(4) . . ?
O22 W11 O10 88.9(4) . . ?
O22 W11 O14 85.6(4) . . ?
O22 W11 O28 161.4(4) . . ?
O27 W11 O10 98.5(4) . . ?
O27 W11 O14 170.6(4) . . ?
O27 W11 O22 100.6(4) . . ?
O27 W11 O28 98.0(5) . . ?
O27 W11 O31 101.5(4) . . ?
O28 W11 O10 88.6(4) . . ?
O28 W11 O14 75.9(4) . . ?
O31 W11 O10 160.0(4) . . ?
O31 W11 O14 85.6(4) . . ?
O31 W11 O22 87.7(4) . . ?
O31 W11 O28 88.4(4) . . ?
O1W Na1 O13W 111.0(5) . 4_576 ?
O1W Na1 O19 113.1(4) . 2 ?
O13W Na1 O19 132.2(5) 4_576 2 ?
O7W Na2 O13W 64.5(6) . . ?
O7W Na2 O2 75.5(4) . 4_575 ?
O7W Na2 O20 140.6(5) . . ?
O7W Na2 O31 90.9(5) . . ?
O7W Na2 O36 130.1(5) . . ?
O13W Na2 O31 150.1(5) . . ?
O2 Na2 O13W 66.3(5) 4_575 . ?
O2 Na2 O20 88.5(4) 4_575 . ?
O2 Na2 O31 92.0(4) 4_575 . ?
O2 Na2 O36 142.5(4) 4_575 . ?
O20 Na2 O13W 140.2(5) . . ?
O20 Na2 O31 53.3(3) . . ?
O20 Na2 O36 54.1(3) . . ?
O36 Na2 O13W 144.5(5) . . ?
O36 Na2 O31 64.5(3) . . ?
Sm1 K1 K2 56.83(7) . . ?
W1 K1 Sm1 60.65(6) . . ?
W1 K1 K2 58.63(7) . . ?
O6W K1 Sm1 100.7(4) . . ?
O6W K1 W1 159.0(4) . . ?
O6W K1 K2 104.1(4) . . ?
O6W K1 O10W 92.2(4) . . ?
O6W K1 O19 164.0(4) . . ?
O6W K1 O27 99.3(4) . 2_545 ?
O6W K1 O30 131.1(5) . . ?
O6W K1 O32 88.4(5) . 3_566 ?
O6W K1 O41 80.2(4) . . ?
O10W K1 Sm1 94.2(2) . . ?
O10W K1 W1 80.6(3) . . ?
O10W K1 K2 37.9(2) . . ?
O10W K1 O19 73.9(3) . . ?
O10W K1 O27 74.9(3) . 2_545 ?
O10W K1 O30 81.2(3) . . ?
O10W K1 O32 140.7(3) . 3_566 ?
O10W K1 O41 121.5(3) . . ?
O19 K1 Sm1 88.4(2) . . ?
O19 K1 W1 27.9(2) . . ?
O19 K1 K2 69.8(2) . . ?
O27 K1 Sm1 157.5(2) 2_545 . ?
O27 K1 W1 97.7(2) 2_545 . ?
O27 K1 K2 108.1(2) 2_545 . ?
O27 K1 O19 69.9(3) 2_545 . ?
O27 K1 O41 163.6(3) 2_545 . ?
O30 K1 Sm1 33.0(2) . . ?
O30 K1 W1 28.58(19) . . ?
O30 K1 K2 46.5(2) . . ?
O30 K1 O19 55.7(3) . . ?
O30 K1 O27 124.7(3) . 2_545 ?
O30 K1 O41 63.6(3) . . ?
O32 K1 Sm1 124.3(3) 3_566 . ?
O32 K1 W1 109.7(3) 3_566 . ?
O32 K1 K2 167.1(3) 3_566 . ?
O32 K1 O19 97.4(3) 3_566 . ?
O32 K1 O27 66.3(3) 3_566 2_545 ?
O32 K1 O30 126.0(3) 3_566 . ?
O32 K1 O41 97.3(3) 3_566 . ?
O41 K1 Sm1 33.7(2) . . ?
O41 K1 W1 86.8(2) . . ?
O41 K1 K2 87.7(2) . . ?
O41 K1 O19 113.6(3) . . ?
W1 K2 Sm1 60.11(6) . . ?
W3 K2 Sm1 64.34(6) . . ?
W3 K2 W1 78.26(7) . . ?
W3 K2 W4 53.10(5) . . ?
W4 K2 Sm1 95.32(8) . . ?
W4 K2 W1 56.73(6) . . ?
O2W K2 Sm1 175.9(3) . . ?
O2W K2 W1 116.4(3) . . ?
O2W K2 W3 113.3(3) . . ?
O2W K2 W4 80.6(3) . . ?
O2W K2 O7 84.6(3) . . ?
O2W K2 O15 81.6(3) . 2_645 ?
O2W K2 O18 140.7(4) . . ?
O2W K2 O25 96.1(3) . . ?
O2W K2 O30 140.7(3) . . ?
O10W K2 Sm1 98.7(3) . . ?
O10W K2 W1 75.6(3) . . ?
O10W K2 W3 153.5(3) . . ?
O10W K2 W4 112.9(3) . . ?
O10W K2 O2W 82.2(4) . . ?
O10W K2 O7 140.9(4) . . ?
O10W K2 O15 107.7(4) . 2_645 ?
O10W K2 O18 130.0(3) . . ?
O10W K2 O25 90.8(3) . . ?
O10W K2 O30 76.2(3) . . ?
O7 K2 Sm1 92.2(2) . . ?
O7 K2 W1 77.8(2) . . ?
O7 K2 W3 32.0(2) . . ?
O7 K2 W4 28.3(2) . . ?
O7 K2 O15 106.5(3) . 2_645 ?
O7 K2 O18 56.2(3) . . ?
O7 K2 O25 54.2(3) . . ?
O7 K2 O30 91.8(3) . . ?
O15 K2 Sm1 101.9(2) 2_645 . ?
O15 K2 W1 161.9(2) 2_645 . ?
O15 K2 W3 96.1(2) 2_645 . ?
O15 K2 W4 132.5(2) 2_645 . ?
O15 K2 O25 160.7(3) 2_645 . ?
O15 K2 O30 136.2(3) 2_645 . ?
O18 K2 Sm1 36.6(2) . . ?
O18 K2 W1 63.2(2) . . ?
O18 K2 W3 28.2(2) . . ?
O18 K2 W4 66.8(2) . . ?
O18 K2 O15 104.0(3) . 2_645 ?
O18 K2 O25 65.8(3) . . ?
O18 K2 O30 54.2(3) . . ?
O25 K2 Sm1 79.8(2) . . ?
O25 K2 W1 28.2(2) . . ?
O25 K2 W3 67.1(2) . . ?
O25 K2 W4 29.2(2) . . ?
O25 K2 O30 52.5(3) . . ?
O30 K2 Sm1 36.53(18) . . ?
O30 K2 W1 26.14(17) . . ?
O30 K2 W3 78.7(2) . . ?
O30 K2 W4 78.22(19) . . ?
O43 K2 Sm1 35.4(2) 3_666 . ?
O43 K2 W1 85.2(2) 3_666 . ?
O43 K2 W3 92.4(3) 3_666 . ?
O43 K2 W4 130.7(3) 3_666 . ?
O43 K2 O2W 148.5(4) 3_666 . ?
O43 K2 O10W 81.8(4) 3_666 . ?
O43 K2 O7 123.9(3) 3_666 . ?
O43 K2 O15 77.8(3) 3_666 2_645 ?
O43 K2 O18 68.3(3) 3_666 . ?
O43 K2 O25 111.0(3) 3_666 . ?
O43 K2 O30 59.2(3) 3_666 . ?
K2 O10W K1 103.4(4) . . ?
Na1 O13W Na2 129.8(8) 4_575 . ?
W7 O2 Na2 147.9(6) . 4_576 ?
B1 O5 W5 125.8(9) . . ?
B1 O5 W7 125.5(8) . . ?
B1 O5 W9 123.5(8) . . ?
W7 O5 W5 89.2(3) . . ?
W9 O5 W5 92.0(3) . . ?
W9 O5 W7 90.0(3) . . ?
B1 O6 W1 130.2(8) . . ?
B1 O6 W8 129.9(8) . . ?
W1 O6 W8 85.8(3) . . ?
W3 O7 K2 98.0(4) . . ?
W4 O7 W3 120.4(5) . . ?
W4 O7 K2 107.8(4) . . ?
W6 O8 W9 149.5(6) . . ?
W6 O9 W3 120.8(5) . . ?
W2 O10 W11 120.7(5) . . ?
W7 O11 W9 120.6(5) . . ?
W10 O12 W2 119.2(4) . . ?
W7 O13 W2 145.6(6) . . ?
B1 O14 W2 125.5(9) . . ?
B1 O14 W10 124.7(9) . . ?
B1 O14 W11 124.4(9) . . ?
W2 O14 W10 88.7(3) . . ?
W11 O14 W2 91.6(3) . . ?
W11 O14 W10 91.2(3) . . ?
W9 O15 K2 134.6(6) . 2_655 ?
W7 O16 W5 121.5(5) . . ?
W9 O17 W5 121.4(5) . . ?
Sm1 O18 K2 99.1(3) . . ?
W3 O18 Sm1 156.7(5) . . ?
W3 O18 K2 100.6(4) . . ?
W1 O19 Na1 109.5(5) . 2_545 ?
W1 O19 K1 99.2(5) . . ?
K1 O19 Na1 137.6(4) . 2_545 ?
W4 O20 W6 119.5(5) . . ?
W4 O20 Na2 103.4(4) . . ?
W6 O20 Na2 107.1(4) . . ?
W5 O21 Sm1 155.5(5) . . ?
W11 O22 W9 148.6(5) . . ?
W8 O23 W1 122.8(5) . . ?
W10 O24 W1 152.5(5) . . ?
W1 O25 W4 151.0(6) . . ?
W1 O25 K2 103.4(4) . . ?
W4 O25 K2 100.4(4) . . ?
W2 O26 W8 152.7(6) . . ?
W11 O27 K1 143.9(5) . 2 ?
W11 O28 W10 120.3(5) . . ?
Sm1 O30 K1 108.0(3) . . ?
Sm1 O30 K2 93.3(3) . . ?
W1 O30 Sm1 144.5(5) . . ?
W1 O30 K1 102.4(4) . . ?
W1 O30 K2 103.1(4) . . ?
K1 O30 K2 93.0(3) . . ?
W6 O31 Na2 103.5(4) . . ?
W11 O31 W6 147.0(6) . . ?
W11 O31 Na2 106.8(4) . . ?
W8 O32 K1 161.8(6) . 3_566 ?
W5 O33 W3 138.9(5) . . ?
W7 O34 W8 155.1(6) . . ?
B1 O35 W3 125.0(8) . . ?
B1 O35 W4 125.1(8) . . ?
B1 O35 W6 124.8(8) . . ?
W4 O35 W3 88.8(3) . . ?
W6 O35 W3 92.3(3) . . ?
W6 O35 W4 90.2(3) . . ?
W4 O36 W10 145.6(6) . . ?
W4 O36 Na2 102.8(4) . . ?
W10 O36 Na2 108.7(4) . . ?
W8 O38 Sm1 143.3(5) . . ?
C2 O40 Sm1 138.9(9) . 3_666 ?
Sm1 O41 K1 104.6(4) . . ?
C2 O41 Sm1 133.6(10) . . ?
C2 O41 K1 119.8(10) . . ?
Sm1 O42 Sm1 104.4(4) . 3_666 ?
C3 O42 Sm1 85.8(9) . 3_666 ?
C3 O42 Sm1 167.8(11) . . ?
Sm1 O43 K2 105.7(4) 3_666 3_666 ?
C3 O43 Sm1 103.3(10) . 3_666 ?
C3 O43 K2 146.4(10) . 3_666 ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
N1 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
N1 C1 C2 114.3(14) . . ?
H1A C1 H1B 107.6 . . ?
C2 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
O40 C2 O41 127.6(14) . . ?
O40 C2 C1 116.5(14) . . ?
O41 C2 C1 115.9(14) . . ?
O42 C3 Sm1 70.0(9) . 3_666 ?
O42 C3 O43 122.7(16) . . ?
O42 C3 C4 120.1(15) . . ?
O43 C3 Sm1 52.8(8) . 3_666 ?
O43 C3 C4 117.0(14) . . ?
C4 C3 Sm1 168.0(11) . 3_666 ?
N2 C4 C3 112.9(14) . . ?
N2 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
C3 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?

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
N1 H1C O12 0.89 2.19 2.959(16) 144.4 3_566
N1 H1C O24 0.89 2.57 3.286(16) 138.3 3_566
N1 H1D O5W 0.89 1.98 2.815(19) 155.1 4_576
N1 H1D O39 0.89 2.55 3.116(18) 122.5 3_666
N1 H1E O3 0.89 2.60 3.319(19) 138.2 3_666
N1 H1E O33 0.89 2.53 3.359(17) 155.3 3_666
N2 H2A O37 0.89 2.00 2.811(17) 150.2 4_576
N2 H2B O3W 0.89 2.04 2.901(18) 161.2 4_576
N2 H2B O38 0.89 2.61 3.095(17) 115.0 .
N2 H2C O16 0.89 2.50 3.047(17) 119.9 .
N2 H2C O21 0.89 2.18 3.064(17) 169.8 .

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1495663'
_audit_update_record             
;
2016-09-05 deposited with the CCDC.
2016-09-13 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT430_3                   
;
PROBLEM: Short Inter D...A Contact O1W .. O14W .. 2.36 Ang.
RESPONSE: In the crystal structure, there are a number of short connections
 between  OW(H2O) and O(POM) or OW(H2O) atoms in the range 2.36-2.84 Ang,
 which indicate extensive H bonding interactions among them. 
 Some shorter connections between OW(H2O) or OW(H2O) atoms result from
 the disordered water molecules. 
;

_vrf_PLAT220_3                   
;
PROBLEM: Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range   10.0 Ratio 
RESPONSE: In polyoxometalate (POM) compounds, the Ueq of oxygen atoms in
 the POM skeleton is small due to multiple covalent bonds, whereas
 the Ueq of these discrete water oxygen atoms is biggish 
 without the constraint of covalent bonds. 
;

_vrf_PLAT306_3                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O3W Check  
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

# end Validation Reply Form


_audit_creation_date             2016-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C16 H40 B4 K8 N8 Na8 Nd4 O198 W44), 10(O)'
_chemical_formula_sum            'C8 H70 B2 K4 N4 Na4 Nd2 O109 W22'
_chemical_formula_weight         6569.84
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 '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'
W W -0.8490 6.8722 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        P2(1)/c
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.7456(8)
_cell_length_b                   21.6247(15)
_cell_length_c                   21.5977(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.4380(10)
_cell_angle_gamma                90.00
_cell_volume                     5480.7(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.154
_cell_measurement_theta_min      2.220
_exptl_absorpt_coefficient_mu    24.195
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.1233 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.5072.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    3.981
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             5792
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_special_details           
;
 Thanks to the large structure of 3 and the existence of a 
large amount of weight atoms, the intensity data are not 
very good, leading to the ADP max/min ratio of some atoms,
and it is very difficult to refine this large structure,
therefore, some unit-occupancy atoms have been refined 
isotropically and restrainedly refined. The ISOR 
instruction is used for O29, N1, C2, O1W, O35, O30, 
O13W, O29, O26, N1, C1, B1, O14 and O6. 
O8W-O9W, O11W, O12W and O14W are refined isostropicallly. 
697 parameters and 84 restraints are used in the 
refinement.
;
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27696
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.89
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         27696
_reflns_number_gt                8086
_reflns_number_total             9600
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         2.132
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.319
_refine_ls_extinction_coef       0.000133(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         9600
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0323P)²+31.8085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0827
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O29) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O1W)
\\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O13W) \\sim Ueq,
Uanis(O29) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B1) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O8W(0.5) O11W(0.5) O12W(0.5) O13W(0.5) O14W(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
4.b Me refined with riding coordinates:
 N1(H1C,H1D,H1E), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Nd1 Nd 0.39249(5) 0.52337(3) 0.42599(3) 0.00817(13) Uani 1 d . . . .
B1 B 0.2183(10) 0.6593(5) 0.2751(5) 0.005(2) Uani 1 d . . . U
W1 W 0.10097(4) 0.50985(2) 0.32107(2) 0.01105(11) Uani 1 d . . . .
W2 W -0.03258(4) 0.73089(2) 0.31002(2) 0.01523(12) Uani 1 d . . . .
W3 W 0.46093(4) 0.57287(2) 0.24605(2) 0.01211(11) Uani 1 d . . . .
W4 W 0.21804(4) 0.53750(2) 0.16721(2) 0.01359(11) Uani 1 d . . . .
W5 W 0.46971(4) 0.69441(2) 0.35752(2) 0.01274(11) Uani 1 d . . . .
W6 W 0.34676(4) 0.67024(2) 0.13759(2) 0.01426(12) Uani 1 d . . . .
W7 W 0.23504(4) 0.77428(2) 0.38766(2) 0.01434(12) Uani 1 d . . . .
W8 W 0.10442(4) 0.62365(2) 0.42594(2) 0.01138(11) Uani 1 d . . . .
W9 W 0.35458(4) 0.79472(2) 0.25238(2) 0.01476(12) Uani 1 d . . . .
W10 W -0.04117(4) 0.61687(2) 0.20564(2) 0.01461(12) Uani 1 d . . . .
W11 W 0.08319(4) 0.75176(2) 0.17258(2) 0.01494(12) Uani 1 d . . . .
Na1 Na 0.0999(6) 0.8987(3) 0.2790(3) 0.0515(17) Uani 1 d . . . .
Na2 Na 0.0697(5) 0.6302(3) 0.0364(3) 0.0466(17) Uani 1 d . . . .
K1 K 0.1487(3) 0.37909(14) 0.42565(13) 0.0294(7) Uani 1 d . . . .
K2 K 0.3638(3) 0.41487(13) 0.27258(13) 0.0286(7) Uani 1 d . . . .
O1W O 0.2747(9) 0.9624(4) 0.3310(5) 0.045(3) Uani 1 d . . . U
O2W O 0.3405(10) 0.3466(5) 0.1654(5) 0.050(3) Uani 1 d . . . .
O3W O 0.2072(9) 0.8951(6) 0.0873(4) 0.050(3) Uani 1 d . . . .
O4W O -0.3312(10) 0.7158(6) 0.1987(6) 0.061(3) Uani 1 d . . . .
O5W O 0.2378(10) 0.9632(5) 0.1969(5) 0.054(3) Uani 1 d . . . .
O6W O 0.2599(16) 0.2905(8) 0.4977(7) 0.103(6) Uani 1 d . . . .
O7W O -0.0380(17) 0.7285(8) -0.0097(9) 0.118(6) Uani 1 d . . . .
O8W O 0.343(2) 0.5589(12) -0.0088(12) 0.067(7) Uiso 0.50 d . . . .
O9W O 0.542(2) 0.6555(11) -0.0353(10) 0.152(8) Uiso 1 d . . . .
O10W O 0.2223(8) 0.3294(5) 0.3174(5) 0.041(3) Uani 1 d . . . .
O11W O 0.618(3) 0.5771(15) 0.0781(15) 0.100(10) Uiso 0.50 d . . . .
O12W O -0.250(3) 0.6960(15) 0.0801(15) 0.096(10) Uiso 0.50 d . . . .
O13W O -0.019(2) 0.6119(12) -0.1033(13) 0.076(8) Uani 0.50 d . . . U
O14W O -0.241(3) 0.5198(14) 0.0788(14) 0.086(9) Uiso 0.50 d . . . .
O1 O -0.1444(7) 0.7695(4) 0.3401(4) 0.030(2) Uani 1 d . . . .
O2 O 0.2150(8) 0.8269(4) 0.4443(4) 0.029(2) Uani 1 d . . . .
O3 O 0.6018(8) 0.7019(4) 0.3926(4) 0.033(2) Uani 1 d . . . .
O4 O 0.1901(8) 0.4764(4) 0.1183(4) 0.025(2) Uani 1 d . . . .
O5 O 0.2903(6) 0.7090(3) 0.3049(3) 0.0113(16) Uani 1 d . . . .
O6 O 0.1974(6) 0.6113(3) 0.3267(3) 0.0084(15) Uani 1 d . . . U
O7 O 0.3716(6) 0.5173(3) 0.1917(3) 0.0149(17) Uani 1 d . . . .
O8 O 0.3911(7) 0.7392(3) 0.1879(4) 0.0188(18) Uani 1 d . . . .
O9 O 0.4704(7) 0.6258(4) 0.1667(4) 0.0185(18) Uani 1 d . . . .
O10 O -0.0191(7) 0.7783(4) 0.2348(4) 0.0173(18) Uani 1 d . . . .
O11 O 0.2898(7) 0.8286(4) 0.3260(4) 0.0177(18) Uani 1 d . . . .
O12 O -0.1221(6) 0.6726(3) 0.2597(3) 0.0145(17) Uani 1 d . . . .
O13 O 0.0899(7) 0.7773(4) 0.3443(4) 0.0190(18) Uani 1 d . . . .
O14 O 0.1054(6) 0.6794(3) 0.2507(3) 0.0124(16) Uani 1 d . . . U
O15 O 0.4105(8) 0.8618(4) 0.2236(4) 0.026(2) Uani 1 d . . . .
O16 O 0.3878(7) 0.7539(3) 0.4076(3) 0.0138(17) Uani 1 d . . . .
O17 O 0.4806(7) 0.7675(4) 0.3000(4) 0.0191(19) Uani 1 d . . . .
O18 O 0.4095(7) 0.5391(4) 0.3135(3) 0.0184(18) Uani 1 d . . . .
O19 O 0.0215(7) 0.4423(4) 0.3215(4) 0.0193(19) Uani 1 d . . . .
O20 O 0.2750(7) 0.5942(4) 0.1085(4) 0.0210(19) Uani 1 d . . . .
O21 O 0.4097(7) 0.6314(3) 0.3962(4) 0.0182(18) Uani 1 d . . . .
O22 O 0.2010(7) 0.7955(4) 0.2147(4) 0.0192(19) Uani 1 d . . . .
O23 O 0.0350(7) 0.5526(4) 0.3878(3) 0.0180(18) Uani 1 d . . . .
O24 O -0.0090(6) 0.5628(4) 0.2705(3) 0.0147(17) Uani 1 d . . . .
O25 O 0.1736(6) 0.5043(3) 0.2441(3) 0.0124(16) Uani 1 d . . . .
O26 O -0.0031(6) 0.6709(4) 0.3681(4) 0.0175(18) Uani 1 d . . . U
O27 O 0.0415(7) 0.8047(4) 0.1161(4) 0.023(2) Uani 1 d . . . .
O28 O -0.0247(6) 0.6878(4) 0.1505(4) 0.0167(18) Uani 1 d . . . .
O29 O -0.1596(7) 0.5840(4) 0.1689(4) 0.026(2) Uani 1 d . . . U
O30 O 0.2227(6) 0.4869(3) 0.3662(3) 0.0126(17) Uani 1 d . . . U
O31 O 0.1962(6) 0.7066(3) 0.1317(4) 0.0157(17) Uani 1 d . . . .
O32 O 0.0258(7) 0.6300(4) 0.4901(4) 0.0216(19) Uani 1 d . . . .
O33 O 0.5082(7) 0.6466(4) 0.2883(4) 0.0208(19) Uani 1 d . . . .
O34 O 0.1847(7) 0.7020(4) 0.4252(3) 0.0172(18) Uani 1 d . . . .
O35 O 0.2823(6) 0.6242(3) 0.2265(3) 0.0113(16) Uani 1 d . . . U
O36 O 0.0764(7) 0.5791(4) 0.1615(4) 0.0186(18) Uani 1 d . . . .
O37 O 0.3958(7) 0.6938(4) 0.0674(4) 0.023(2) Uani 1 d . . . .
O38 O 0.2255(6) 0.5837(3) 0.4557(3) 0.0140(17) Uani 1 d . . . .
O39 O 0.5907(7) 0.5374(4) 0.2384(4) 0.029(2) Uani 1 d . . . .
O40 O 0.4051(7) 0.4571(4) 0.5901(4) 0.0202(19) Uani 1 d . . . .
O41 O 0.2975(7) 0.4577(4) 0.5028(4) 0.0206(19) Uani 1 d . . . .
O42 O 0.4644(7) 0.5669(4) 0.5238(3) 0.0186(19) Uani 1 d . . . .
O43 O 0.5692(8) 0.5840(4) 0.6086(4) 0.026(2) Uani 1 d . . . .
N1 N 0.2444(10) 0.4131(5) 0.6586(5) 0.030(3) Uani 1 d . . . U
H1C H 0.1845 0.3978 0.6772 0.044 Uiso 1 calc . . R .
H1D H 0.2629 0.4496 0.6750 0.044 Uiso 1 calc . . R .
H1E H 0.3031 0.3873 0.6637 0.044 Uiso 1 calc . . R .
N2 N 0.3676(10) 0.6811(5) 0.5269(5) 0.037(3) Uani 1 d . . . .
H2A H 0.3509 0.7212 0.5281 0.055 Uiso 1 calc . . R .
H2B H 0.3089 0.6592 0.5397 0.055 Uiso 1 calc . . R .
H2C H 0.3820 0.6703 0.4882 0.055 Uiso 1 calc . . R .
C1 C 0.2159(10) 0.4207(6) 0.5915(5) 0.023(3) Uani 1 d . . . U
H1A H 0.1511 0.4483 0.5859 0.027 Uiso 1 calc . . R .
H1B H 0.1949 0.3810 0.5736 0.027 Uiso 1 calc . . R .
C2 C 0.3169(10) 0.4471(5) 0.5583(5) 0.013(2) Uani 1 d . . . U
C3 C 0.4997(11) 0.6017(5) 0.5658(5) 0.020(3) Uani 1 d . . . .
C4 C 0.4657(13) 0.6690(6) 0.5664(6) 0.035(4) Uani 1 d . . . .
H4A H 0.4498 0.6811 0.6084 0.043 Uiso 1 calc . . R .
H4B H 0.5288 0.6940 0.5531 0.043 Uiso 1 calc . . R .


_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 Nd1 4.1152(11) 3_666 ?
Nd1 K2 4.062(3) . ?
Nd1 O18 2.470(7) . ?
Nd1 O21 2.434(7) . ?
Nd1 O30 2.459(7) . ?
Nd1 O38 2.464(7) . ?
Nd1 O40 2.454(8) 3_666 ?
Nd1 O41 2.484(8) . ?
Nd1 O42 2.767(8) 3_666 ?
Nd1 O42 2.431(7) . ?
Nd1 O43 2.485(8) 3_666 ?
Nd1 C3 2.989(11) 3_666 ?
B1 O5 1.494(13) . ?
B1 O6 1.549(13) . ?
B1 O14 1.473(13) . ?
B1 O35 1.521(13) . ?
W1 K1 3.647(3) . ?
W1 K2 3.888(3) . ?
W1 O6 2.470(7) . ?
W1 O19 1.734(8) . ?
W1 O23 1.905(8) . ?
W1 O24 2.014(8) . ?
W1 O25 1.904(7) . ?
W1 O30 1.767(7) . ?
W2 O1 1.707(9) . ?
W2 O10 1.934(8) . ?
W2 O12 1.944(7) . ?
W2 O13 1.880(8) . ?
W2 O14 2.384(7) . ?
W2 O26 1.827(8) . ?
W3 K2 3.655(3) . ?
W3 O7 1.954(7) . ?
W3 O9 2.067(8) . ?
W3 O18 1.759(7) . ?
W3 O33 1.908(8) . ?
W3 O35 2.395(7) . ?
W3 O39 1.721(9) . ?
W4 K2 3.848(3) . ?
W4 O4 1.715(8) . ?
W4 O7 1.908(7) . ?
W4 O20 1.905(8) . ?
W4 O25 1.902(7) . ?
W4 O35 2.375(7) . ?
W4 O36 1.891(8) . ?
W5 O3 1.705(8) . ?
W5 O5 2.373(7) . ?
W5 O16 1.959(8) . ?
W5 O17 2.017(8) . ?
W5 O21 1.761(8) . ?
W5 O33 1.888(8) . ?
W6 O8 1.904(8) . ?
W6 O9 1.830(8) . ?
W6 O20 1.940(8) . ?
W6 O31 1.934(8) . ?
W6 O35 2.319(7) . ?
W6 O37 1.722(8) . ?
W7 O2 1.694(8) . ?
W7 O5 2.390(7) . ?
W7 O11 1.908(8) . ?
W7 O13 1.911(8) . ?
W7 O16 1.880(8) . ?
W7 O34 1.868(8) . ?
W8 O6 2.462(7) . ?
W8 O23 1.909(8) . ?
W8 O26 2.017(8) . ?
W8 O32 1.703(8) . ?
W8 O34 1.939(8) . ?
W8 O38 1.761(7) . ?
W9 O5 2.317(7) . ?
W9 O8 1.902(8) . ?
W9 O11 1.936(8) . ?
W9 O15 1.719(8) . ?
W9 O17 1.862(8) . ?
W9 O22 1.948(8) . ?
W10 O12 1.953(8) . ?
W10 O14 2.366(7) . ?
W10 O24 1.850(7) . ?
W10 O28 1.957(8) . ?
W10 O29 1.726(8) . ?
W10 O36 1.895(8) . ?
W11 O10 1.928(8) . ?
W11 O14 2.307(7) . ?
W11 O22 1.879(8) . ?
W11 O27 1.728(7) . ?
W11 O28 1.922(8) . ?
W11 O31 1.897(8) . ?
Na1 O1W 2.679(12) . ?
Na1 O5W 2.821(14) . ?
Na1 O13W 2.96(3) 4_576 ?
Na1 O11 2.847(10) . ?
Na1 O13 2.983(10) . ?
Na1 O19 2.715(10) 2 ?
Na1 O22 2.908(11) . ?
Na2 O7W 2.646(18) . ?
Na2 O2 2.832(10) 4_575 ?
Na2 O20 2.920(10) . ?
Na2 O28 3.013(10) . ?
Na2 O31 2.985(10) . ?
Na2 O36 2.918(9) . ?
K1 K2 4.315(4) . ?
K1 O6W 2.761(15) . ?
K1 O10W 2.746(11) . ?
K1 O19 2.978(8) . ?
K1 O27 2.867(8) 2_545 ?
K1 O30 2.817(8) . ?
K1 O32 2.804(9) 3_566 ?
K1 O41 2.911(9) . ?
K2 O2W 2.749(11) . ?
K2 O10W 2.694(10) . ?
K2 O7 2.825(8) . ?
K2 O15 2.887(9) 2_645 ?
K2 O18 2.871(8) . ?
K2 O25 2.999(8) . ?
K2 O30 3.089(8) . ?
K2 O43 2.653(8) 3_666 ?
O13W Na1 2.96(3) 4_575 ?
O2 Na2 2.832(10) 4_576 ?
O15 K2 2.887(9) 2_655 ?
O19 Na1 2.715(10) 2_545 ?
O27 K1 2.867(8) 2 ?
O32 K1 2.804(9) 3_566 ?
O40 Nd1 2.454(8) 3_666 ?
O40 C2 1.237(13) . ?
O41 C2 1.233(13) . ?
O42 Nd1 2.767(8) 3_666 ?
O42 C3 1.238(13) . ?
O43 Nd1 2.485(8) 3_666 ?
O43 K2 2.653(8) 3_666 ?
O43 C3 1.266(13) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N1 C1 1.482(15) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.428(17) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.524(15) . ?
C3 Nd1 2.989(11) 3_666 ?
C3 C4 1.510(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
K2 Nd1 Nd1 121.24(5) . 3_666 ?
O18 Nd1 Nd1 136.5(2) . 3_666 ?
O18 Nd1 K2 44.31(19) . . ?
O18 Nd1 O41 142.5(3) . . ?
O18 Nd1 O42 114.2(3) . 3_666 ?
O18 Nd1 O43 79.0(3) . 3_666 ?
O18 Nd1 C3 97.5(3) . 3_666 ?
O21 Nd1 Nd1 112.71(19) . 3_666 ?
O21 Nd1 K2 110.1(2) . . ?
O21 Nd1 O18 66.2(3) . . ?
O21 Nd1 O30 104.1(2) . . ?
O21 Nd1 O38 68.7(3) . . ?
O21 Nd1 O40 72.9(3) . 3_666 ?
O21 Nd1 O41 140.4(3) . . ?
O21 Nd1 O42 136.4(2) . 3_666 ?
O21 Nd1 O43 143.0(3) . 3_666 ?
O21 Nd1 C3 147.6(3) . 3_666 ?
O30 Nd1 Nd1 141.84(16) . 3_666 ?
O30 Nd1 K2 49.38(19) . . ?
O30 Nd1 O18 68.0(3) . . ?
O30 Nd1 O38 70.7(2) . . ?
O30 Nd1 O41 77.9(2) . . ?
O30 Nd1 O42 116.4(2) . 3_666 ?
O30 Nd1 O43 72.3(3) . 3_666 ?
O30 Nd1 C3 94.2(3) . 3_666 ?
O38 Nd1 Nd1 113.38(17) . 3_666 ?
O38 Nd1 K2 118.63(18) . . ?
O38 Nd1 O18 106.4(3) . . ?
O38 Nd1 O41 75.2(3) . . ?
O38 Nd1 O42 138.5(2) . 3_666 ?
O38 Nd1 O43 136.8(3) . 3_666 ?
O38 Nd1 C3 143.5(3) . 3_666 ?
O40 Nd1 Nd1 65.54(18) 3_666 3_666 ?
O40 Nd1 K2 91.8(2) 3_666 . ?
O40 Nd1 O18 73.6(3) 3_666 . ?
O40 Nd1 O30 138.6(3) 3_666 . ?
O40 Nd1 O38 137.1(3) 3_666 . ?
O40 Nd1 O41 131.2(3) 3_666 . ?
O40 Nd1 O42 66.5(2) 3_666 3_666 ?
O40 Nd1 O43 86.0(3) 3_666 3_666 ?
O40 Nd1 C3 75.7(3) 3_666 3_666 ?
O41 Nd1 Nd1 67.61(18) . 3_666 ?
O41 Nd1 K2 101.0(2) . . ?
O41 Nd1 O42 67.5(3) . 3_666 ?
O41 Nd1 O43 76.0(3) . 3_666 ?
O41 Nd1 C3 69.2(3) . 3_666 ?
O42 Nd1 Nd1 34.89(15) 3_666 3_666 ?
O42 Nd1 Nd1 40.61(19) . 3_666 ?
O42 Nd1 K2 161.1(2) . . ?
O42 Nd1 K2 86.57(16) 3_666 . ?
O42 Nd1 O18 139.7(3) . . ?
O42 Nd1 O21 80.1(3) . . ?
O42 Nd1 O30 145.5(3) . . ?
O42 Nd1 O38 79.6(3) . . ?
O42 Nd1 O40 75.7(3) . 3_666 ?
O42 Nd1 O41 77.9(3) . . ?
O42 Nd1 O42 75.5(3) . 3_666 ?
O42 Nd1 O43 124.2(3) . 3_666 ?
O42 Nd1 C3 24.4(3) 3_666 3_666 ?
O42 Nd1 C3 99.7(3) . 3_666 ?
O43 Nd1 Nd1 83.73(17) 3_666 3_666 ?
O43 Nd1 K2 39.23(18) 3_666 . ?
O43 Nd1 O42 49.0(2) 3_666 3_666 ?
O43 Nd1 C3 24.6(3) 3_666 3_666 ?
C3 Nd1 Nd1 59.2(2) 3_666 3_666 ?
C3 Nd1 K2 63.0(2) 3_666 . ?
O5 B1 O6 106.1(8) . . ?
O5 B1 O35 111.6(8) . . ?
O14 B1 O5 115.2(8) . . ?
O14 B1 O6 106.8(8) . . ?
O14 B1 O35 111.3(8) . . ?
O35 B1 O6 105.0(8) . . ?
K1 W1 K2 69.79(7) . . ?
O6 W1 K1 126.88(16) . . ?
O6 W1 K2 96.58(17) . . ?
O19 W1 K1 54.0(3) . . ?
O19 W1 K2 89.4(3) . . ?
O19 W1 O6 173.8(3) . . ?
O19 W1 O23 99.7(4) . . ?
O19 W1 O24 98.6(3) . . ?
O19 W1 O25 102.3(4) . . ?
O19 W1 O30 100.5(3) . . ?
O23 W1 K1 88.0(2) . . ?
O23 W1 K2 144.4(2) . . ?
O23 W1 O6 74.5(3) . . ?
O23 W1 O24 82.1(3) . . ?
O24 W1 K1 148.8(2) . . ?
O24 W1 K2 130.7(2) . . ?
O24 W1 O6 78.7(3) . . ?
O25 W1 K1 115.4(2) . . ?
O25 W1 K2 48.8(2) . . ?
O25 W1 O6 83.0(3) . . ?
O25 W1 O23 154.5(3) . . ?
O25 W1 O24 82.1(3) . . ?
O30 W1 K1 48.8(2) . . ?
O30 W1 K2 50.7(2) . . ?
O30 W1 O6 82.2(3) . . ?
O30 W1 O23 93.7(3) . . ?
O30 W1 O24 160.8(3) . . ?
O30 W1 O25 94.7(3) . . ?
O1 W2 O10 98.8(4) . . ?
O1 W2 O12 97.1(4) . . ?
O1 W2 O13 100.2(4) . . ?
O1 W2 O14 169.7(3) . . ?
O1 W2 O26 102.2(4) . . ?
O10 W2 O12 86.3(3) . . ?
O10 W2 O14 73.4(3) . . ?
O12 W2 O14 76.1(3) . . ?
O13 W2 O10 87.6(3) . . ?
O13 W2 O12 162.4(3) . . ?
O13 W2 O14 86.3(3) . . ?
O26 W2 O10 159.0(3) . . ?
O26 W2 O12 90.3(3) . . ?
O26 W2 O13 89.4(3) . . ?
O26 W2 O14 85.7(3) . . ?
O7 W3 K2 49.9(2) . . ?
O7 W3 O9 83.6(3) . . ?
O7 W3 O35 74.6(3) . . ?
O9 W3 K2 132.5(2) . . ?
O9 W3 O35 71.0(3) . . ?
O18 W3 K2 50.3(3) . . ?
O18 W3 O7 92.7(3) . . ?
O18 W3 O9 161.5(4) . . ?
O18 W3 O33 93.1(3) . . ?
O18 W3 O35 90.5(3) . . ?
O33 W3 K2 142.4(2) . . ?
O33 W3 O7 159.9(3) . . ?
O33 W3 O9 84.8(3) . . ?
O33 W3 O35 86.1(3) . . ?
O35 W3 K2 100.58(18) . . ?
O39 W3 K2 83.2(3) . . ?
O39 W3 O7 97.1(4) . . ?
O39 W3 O9 95.1(4) . . ?
O39 W3 O18 103.3(4) . . ?
O39 W3 O33 100.2(4) . . ?
O39 W3 O35 164.3(3) . . ?
O4 W4 K2 84.4(3) . . ?
O4 W4 O7 98.5(4) . . ?
O4 W4 O20 98.6(4) . . ?
O4 W4 O25 101.2(4) . . ?
O4 W4 O35 171.3(3) . . ?
O4 W4 O36 100.5(4) . . ?
O7 W4 K2 44.5(2) . . ?
O7 W4 O35 75.9(3) . . ?
O20 W4 K2 132.6(3) . . ?
O20 W4 O7 88.7(3) . . ?
O20 W4 O35 74.8(3) . . ?
O25 W4 K2 49.9(2) . . ?
O25 W4 O7 87.9(3) . . ?
O25 W4 O20 160.2(3) . . ?
O25 W4 O35 85.4(3) . . ?
O35 W4 K2 95.84(17) . . ?
O36 W4 K2 137.3(2) . . ?
O36 W4 O7 161.0(3) . . ?
O36 W4 O20 89.0(3) . . ?
O36 W4 O25 87.9(3) . . ?
O36 W4 O35 85.3(3) . . ?
O3 W5 O5 166.7(4) . . ?
O3 W5 O16 98.7(4) . . ?
O3 W5 O17 96.8(4) . . ?
O3 W5 O21 103.8(4) . . ?
O3 W5 O33 99.2(4) . . ?
O16 W5 O5 74.4(3) . . ?
O16 W5 O17 82.5(3) . . ?
O17 W5 O5 71.3(3) . . ?
O21 W5 O5 88.0(3) . . ?
O21 W5 O16 91.8(3) . . ?
O21 W5 O17 159.3(3) . . ?
O21 W5 O33 93.8(4) . . ?
O33 W5 O5 86.0(3) . . ?
O33 W5 O16 159.4(3) . . ?
O33 W5 O17 85.3(3) . . ?
O8 W6 O20 162.3(3) . . ?
O8 W6 O31 86.9(3) . . ?
O8 W6 O35 87.4(3) . . ?
O9 W6 O8 91.2(3) . . ?
O9 W6 O20 89.6(3) . . ?
O9 W6 O31 161.0(3) . . ?
O9 W6 O35 76.8(3) . . ?
O20 W6 O35 75.6(3) . . ?
O31 W6 O20 86.5(3) . . ?
O31 W6 O35 84.2(3) . . ?
O37 W6 O8 100.2(4) . . ?
O37 W6 O9 99.7(4) . . ?
O37 W6 O20 97.0(4) . . ?
O37 W6 O31 99.3(4) . . ?
O37 W6 O35 171.7(3) . . ?
O2 W7 O5 170.9(4) . . ?
O2 W7 O11 98.7(4) . . ?
O2 W7 O13 100.5(4) . . ?
O2 W7 O16 98.8(4) . . ?
O2 W7 O34 101.1(4) . . ?
O11 W7 O5 74.4(3) . . ?
O11 W7 O13 87.5(3) . . ?
O13 W7 O5 85.3(3) . . ?
O16 W7 O5 75.3(3) . . ?
O16 W7 O11 87.5(3) . . ?
O16 W7 O13 160.6(3) . . ?
O34 W7 O5 86.1(3) . . ?
O34 W7 O11 160.1(3) . . ?
O34 W7 O13 87.1(3) . . ?
O34 W7 O16 91.2(3) . . ?
O23 W8 O6 74.6(3) . . ?
O23 W8 O26 84.0(3) . . ?
O23 W8 O34 153.9(3) . . ?
O26 W8 O6 78.8(3) . . ?
O32 W8 O6 173.4(3) . . ?
O32 W8 O23 100.3(4) . . ?
O32 W8 O26 96.7(3) . . ?
O32 W8 O34 102.6(4) . . ?
O32 W8 O38 101.5(4) . . ?
O34 W8 O6 81.6(3) . . ?
O34 W8 O26 81.0(3) . . ?
O38 W8 O6 83.3(3) . . ?
O38 W8 O23 95.0(3) . . ?
O38 W8 O26 161.6(3) . . ?
O38 W8 O34 92.6(3) . . ?
O8 W9 O5 86.6(3) . . ?
O8 W9 O11 161.7(3) . . ?
O8 W9 O22 86.2(3) . . ?
O11 W9 O5 75.7(3) . . ?
O11 W9 O22 87.2(3) . . ?
O15 W9 O5 171.8(3) . . ?
O15 W9 O8 99.6(4) . . ?
O15 W9 O11 98.5(4) . . ?
O15 W9 O17 99.2(4) . . ?
O15 W9 O22 101.7(4) . . ?
O17 W9 O5 75.2(3) . . ?
O17 W9 O8 90.4(3) . . ?
O17 W9 O11 89.8(3) . . ?
O17 W9 O22 159.1(3) . . ?
O22 W9 O5 84.1(3) . . ?
O12 W10 O14 76.4(3) . . ?
O12 W10 O28 86.8(3) . . ?
O24 W10 O12 91.5(3) . . ?
O24 W10 O14 85.9(3) . . ?
O24 W10 O28 159.0(3) . . ?
O24 W10 O36 88.8(3) . . ?
O28 W10 O14 73.3(3) . . ?
O29 W10 O12 97.2(4) . . ?
O29 W10 O14 169.4(3) . . ?
O29 W10 O24 102.9(4) . . ?
O29 W10 O28 98.1(4) . . ?
O29 W10 O36 100.5(4) . . ?
O36 W10 O12 161.8(3) . . ?
O36 W10 O14 85.4(3) . . ?
O36 W10 O28 86.5(3) . . ?
O10 W11 O14 75.3(3) . . ?
O22 W11 O10 88.9(3) . . ?
O22 W11 O14 86.0(3) . . ?
O22 W11 O28 161.2(3) . . ?
O22 W11 O31 88.2(3) . . ?
O27 W11 O10 97.4(4) . . ?
O27 W11 O14 170.0(3) . . ?
O27 W11 O22 100.8(4) . . ?
O27 W11 O28 97.9(4) . . ?
O27 W11 O31 101.3(4) . . ?
O28 W11 O10 87.9(3) . . ?
O28 W11 O14 75.3(3) . . ?
O31 W11 O10 161.3(3) . . ?
O31 W11 O14 86.1(3) . . ?
O31 W11 O28 88.9(3) . . ?
O1W Na1 O5W 63.8(4) . . ?
O1W Na1 O13W 93.5(6) . 4_576 ?
O1W Na1 O11 63.2(3) . . ?
O1W Na1 O13 107.4(3) . . ?
O1W Na1 O19 121.6(4) . 2 ?
O1W Na1 O22 105.9(4) . . ?
O5W Na1 O13W 151.9(6) . 4_576 ?
O5W Na1 O11 91.4(3) . . ?
O5W Na1 O13 140.1(4) . . ?
O5W Na1 O22 79.7(3) . . ?
O13W Na1 O13 59.8(5) 4_576 . ?
O11 Na1 O13W 92.5(5) . 4_576 ?
O11 Na1 O13 53.8(2) . . ?
O11 Na1 O22 55.4(2) . . ?
O19 Na1 O5W 67.8(3) 2 . ?
O19 Na1 O13W 117.6(6) 2 4_576 ?
O19 Na1 O11 147.8(4) 2 . ?
O19 Na1 O13 130.8(3) 2 . ?
O19 Na1 O22 95.5(3) 2 . ?
O22 Na1 O13W 124.6(6) . 4_576 ?
O22 Na1 O13 64.9(3) . . ?
O7W Na2 O2 76.4(5) . 4_575 ?
O7W Na2 O20 141.8(5) . . ?
O7W Na2 O28 77.8(5) . . ?
O7W Na2 O31 91.8(5) . . ?
O7W Na2 O36 130.3(5) . . ?
O2 Na2 O20 87.3(3) 4_575 . ?
O2 Na2 O28 133.9(3) 4_575 . ?
O2 Na2 O31 90.4(3) 4_575 . ?
O2 Na2 O36 141.4(3) 4_575 . ?
O20 Na2 O28 89.9(3) . . ?
O20 Na2 O31 53.4(2) . . ?
O31 Na2 O28 52.9(2) . . ?
O36 Na2 O20 54.3(2) . . ?
O36 Na2 O28 52.8(2) . . ?
O36 Na2 O31 65.0(2) . . ?
Nd1 K1 K2 56.72(5) . . ?
W1 K1 Nd1 61.05(4) . . ?
W1 K1 K2 57.73(6) . . ?
O6W K1 Nd1 101.9(4) . . ?
O6W K1 W1 160.6(4) . . ?
O6W K1 K2 106.1(4) . . ?
O6W K1 O19 162.5(4) . . ?
O6W K1 O27 97.6(4) . 2_545 ?
O6W K1 O30 133.1(4) . . ?
O6W K1 O32 85.8(4) . 3_566 ?
O6W K1 O41 79.9(4) . . ?
O10W K1 Nd1 93.0(2) . . ?
O10W K1 W1 79.7(2) . . ?
O10W K1 K2 37.1(2) . . ?
O10W K1 O6W 92.9(4) . . ?
O10W K1 O19 72.7(3) . . ?
O10W K1 O27 77.4(3) . 2_545 ?
O10W K1 O30 79.7(3) . . ?
O10W K1 O32 142.2(3) . 3_566 ?
O10W K1 O41 120.8(3) . . ?
O19 K1 Nd1 88.89(16) . . ?
O19 K1 W1 28.10(15) . . ?
O19 K1 K2 68.31(17) . . ?
O27 K1 Nd1 158.68(19) 2_545 . ?
O27 K1 W1 98.21(18) 2_545 . ?
O27 K1 K2 109.46(19) 2_545 . ?
O27 K1 O19 70.2(2) 2_545 . ?
O27 K1 O41 161.6(3) 2_545 . ?
O30 K1 Nd1 33.82(15) . . ?
O30 K1 W1 28.16(15) . . ?
O30 K1 K2 45.58(17) . . ?
O30 K1 O19 55.3(2) . . ?
O30 K1 O27 124.9(2) . 2_545 ?
O30 K1 O41 65.7(2) . . ?
O32 K1 Nd1 124.3(2) 3_566 . ?
O32 K1 W1 111.03(19) 3_566 . ?
O32 K1 K2 167.78(19) 3_566 . ?
O32 K1 O19 99.5(2) 3_566 . ?
O32 K1 O27 65.4(2) 3_566 2_545 ?
O32 K1 O30 127.0(3) 3_566 . ?
O32 K1 O41 96.1(2) 3_566 . ?
O41 K1 Nd1 34.83(15) . . ?
O41 K1 W1 88.53(17) . . ?
O41 K1 K2 88.67(17) . . ?
O41 K1 O19 115.7(2) . . ?
W1 K2 Nd1 60.96(4) . . ?
W3 K2 Nd1 64.68(5) . . ?
W3 K2 W1 78.76(6) . . ?
W3 K2 W4 52.92(4) . . ?
W4 K2 Nd1 95.95(6) . . ?
W4 K2 W1 57.11(4) . . ?
O2W K2 Nd1 177.1(3) . . ?
O2W K2 W1 117.3(3) . . ?
O2W K2 W3 113.0(3) . . ?
O2W K2 W4 81.1(2) . . ?
O2W K2 O7 84.5(3) . . ?
O2W K2 O15 82.5(3) . 2_645 ?
O2W K2 O18 140.5(3) . . ?
O2W K2 O25 97.3(3) . . ?
O2W K2 O30 141.7(3) . . ?
O10W K2 Nd1 97.7(2) . . ?
O10W K2 W1 75.9(2) . . ?
O10W K2 W3 154.1(2) . . ?
O10W K2 W4 114.8(2) . . ?
O10W K2 O2W 83.9(3) . . ?
O10W K2 O7 142.9(3) . . ?
O10W K2 O15 107.3(3) . 2_645 ?
O10W K2 O18 129.9(3) . . ?
O10W K2 O25 92.9(3) . . ?
O10W K2 O30 75.8(3) . . ?
O7 K2 Nd1 92.73(16) . . ?
O7 K2 W1 78.43(17) . . ?
O7 K2 W3 31.95(15) . . ?
O7 K2 W4 28.28(16) . . ?
O7 K2 O15 106.0(3) . 2_645 ?
O7 K2 O18 56.4(2) . . ?
O7 K2 O25 53.9(2) . . ?
O7 K2 O30 92.4(2) . . ?
O15 K2 Nd1 99.31(18) 2_645 . ?
O15 K2 W1 160.19(19) 2_645 . ?
O15 K2 W3 94.80(19) 2_645 . ?
O15 K2 W4 132.5(2) 2_645 . ?
O15 K2 O25 159.6(2) 2_645 . ?
O15 K2 O30 134.3(2) 2_645 . ?
O18 K2 Nd1 36.94(15) . . ?
O18 K2 W1 64.10(18) . . ?
O18 K2 W3 28.13(15) . . ?
O18 K2 W4 67.04(16) . . ?
O18 K2 O15 101.7(3) . 2_645 ?
O18 K2 O25 65.7(2) . . ?
O18 K2 O30 54.9(2) . . ?
O25 K2 Nd1 80.22(15) . . ?
O25 K2 W1 28.55(15) . . ?
O25 K2 W3 66.41(15) . . ?
O25 K2 W4 29.02(14) . . ?
O25 K2 O30 52.7(2) . . ?
O30 K2 Nd1 37.18(14) . . ?
O30 K2 W1 26.28(13) . . ?
O30 K2 W3 79.11(15) . . ?
O30 K2 W4 78.59(14) . . ?
O43 K2 Nd1 36.33(18) 3_666 . ?
O43 K2 W1 86.6(2) 3_666 . ?
O43 K2 W3 93.5(2) 3_666 . ?
O43 K2 W4 132.2(2) 3_666 . ?
O43 K2 O2W 146.6(3) 3_666 . ?
O43 K2 O10W 79.7(3) 3_666 . ?
O43 K2 O7 125.1(3) 3_666 . ?
O43 K2 O15 75.0(3) 3_666 2_645 ?
O43 K2 O18 69.5(2) 3_666 . ?
O43 K2 O25 112.3(2) 3_666 . ?
O43 K2 O30 60.5(2) 3_666 . ?
K2 O10W K1 105.0(3) . . ?
W7 O2 Na2 146.4(5) . 4_576 ?
B1 O5 W5 125.8(6) . . ?
B1 O5 W7 125.4(6) . . ?
B1 O5 W9 123.7(6) . . ?
W5 O5 W7 89.1(2) . . ?
W9 O5 W5 92.2(3) . . ?
W9 O5 W7 89.9(2) . . ?
B1 O6 W1 130.3(6) . . ?
B1 O6 W8 130.0(6) . . ?
W8 O6 W1 85.4(2) . . ?
W3 O7 K2 98.1(3) . . ?
W4 O7 W3 120.2(4) . . ?
W4 O7 K2 107.2(3) . . ?
W9 O8 W6 147.9(5) . . ?
W6 O9 W3 120.4(4) . . ?
W11 O10 W2 120.2(4) . . ?
W7 O11 W9 119.7(4) . . ?
W7 O11 Na1 107.1(4) . . ?
W9 O11 Na1 103.8(3) . . ?
W2 O12 W10 118.0(4) . . ?
W2 O13 W7 145.7(4) . . ?
W2 O13 Na1 109.2(3) . . ?
W7 O13 Na1 102.1(3) . . ?
B1 O14 W2 124.6(6) . . ?
B1 O14 W10 127.4(6) . . ?
B1 O14 W11 122.3(6) . . ?
W10 O14 W2 89.4(2) . . ?
W11 O14 W2 91.1(3) . . ?
W11 O14 W10 91.7(2) . . ?
W9 O15 K2 133.6(4) . 2_655 ?
W7 O16 W5 120.9(4) . . ?
W9 O17 W5 121.2(4) . . ?
Nd1 O18 K2 98.7(3) . . ?
W3 O18 Nd1 156.4(4) . . ?
W3 O18 K2 101.6(3) . . ?
W1 O19 Na1 123.5(4) . 2_545 ?
W1 O19 K1 97.9(3) . . ?
Na1 O19 K1 132.4(3) 2_545 . ?
W4 O20 W6 119.3(4) . . ?
W4 O20 Na2 102.8(4) . . ?
W6 O20 Na2 106.5(3) . . ?
W5 O21 Nd1 155.2(4) . . ?
W9 O22 Na1 101.3(3) . . ?
W11 O22 W9 148.0(4) . . ?
W11 O22 Na1 108.1(4) . . ?
W1 O23 W8 122.5(4) . . ?
W10 O24 W1 151.1(4) . . ?
W1 O25 K2 102.6(3) . . ?
W4 O25 W1 152.6(4) . . ?
W4 O25 K2 101.1(3) . . ?
W2 O26 W8 151.7(4) . . ?
W11 O27 K1 141.9(4) . 2 ?
W10 O28 Na2 102.9(3) . . ?
W11 O28 W10 119.6(4) . . ?
W11 O28 Na2 103.8(3) . . ?
Nd1 O30 K1 106.6(2) . . ?
Nd1 O30 K2 93.4(2) . . ?
W1 O30 Nd1 144.9(4) . . ?
W1 O30 K1 103.0(3) . . ?
W1 O30 K2 103.0(3) . . ?
K1 O30 K2 93.8(2) . . ?
W6 O31 Na2 104.3(3) . . ?
W11 O31 W6 146.6(4) . . ?
W11 O31 Na2 105.6(3) . . ?
W8 O32 K1 163.5(4) . 3_566 ?
W5 O33 W3 139.6(4) . . ?
W7 O34 W8 153.8(4) . . ?
B1 O35 W3 124.4(6) . . ?
B1 O35 W4 127.7(6) . . ?
B1 O35 W6 123.1(6) . . ?
W4 O35 W3 89.2(2) . . ?
W6 O35 W3 91.8(3) . . ?
W6 O35 W4 90.0(2) . . ?
W4 O36 W10 146.1(4) . . ?
W4 O36 Na2 103.3(3) . . ?
W10 O36 Na2 108.1(3) . . ?
W8 O38 Nd1 143.5(4) . . ?
C2 O40 Nd1 138.2(7) . 3_666 ?
Nd1 O41 K1 103.2(3) . . ?
C2 O41 Nd1 133.3(7) . . ?
C2 O41 K1 122.0(7) . . ?
Nd1 O42 Nd1 104.5(3) . 3_666 ?
C3 O42 Nd1 165.1(8) . . ?
C3 O42 Nd1 87.9(7) . 3_666 ?
Nd1 O43 K2 104.4(3) 3_666 3_666 ?
C3 O43 Nd1 100.6(7) . 3_666 ?
C3 O43 K2 149.1(8) . 3_666 ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 C2 110.7(10) . . ?
H1A C1 H1B 108.1 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
O40 C2 C1 117.1(10) . . ?
O41 C2 O40 128.6(11) . . ?
O41 C2 C1 114.3(10) . . ?
O42 C3 Nd1 67.7(6) . 3_666 ?
O42 C3 O43 122.4(11) . . ?
O42 C3 C4 120.8(10) . . ?
O43 C3 Nd1 54.8(6) . 3_666 ?
O43 C3 C4 116.7(10) . . ?
C4 C3 Nd1 169.7(9) . 3_666 ?
N2 C4 C3 112.2(11) . . ?
N2 C4 H4A 109.2 . . ?
N2 C4 H4B 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?

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
N1 H1C O12 0.89 2.19 2.971(13) 146.4 3_566
N1 H1C O24 0.89 2.54 3.260(13) 138.5 3_566
N1 H1D O5W 0.89 1.97 2.802(16) 155.5 4_576
N1 H1D O39 0.89 2.50 3.079(14) 123.1 3_666
N1 H1E O3 0.89 2.56 3.291(15) 139.8 3_666
N1 H1E O33 0.89 2.52 3.338(14) 153.8 3_666
N2 H2A O37 0.89 2.08 2.859(14) 145.0 4_576
N2 H2B O3W 0.89 1.99 2.860(18) 164.4 4_576
N2 H2B O38 0.89 2.60 3.060(14) 113.0 .
N2 H2C O16 0.89 2.51 3.038(14) 118.3 .
N2 H2C O21 0.89 2.20 3.079(14) 172.4 .

_olex2_submission_special_instructions 'No special instructions were received'
