# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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data_eu

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H36 Cu5 Eu2 N20 O88 Si2 W22'
_chemical_formula_sum            'C44 H70 Cu5 Eu2 N20 O95 Si2 W22'
_chemical_formula_weight         7121.70

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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.378(5)
_cell_length_b                   12.184(5)
_cell_length_c                   23.328(5)
_cell_angle_alpha                83.715(5)
_cell_angle_beta                 81.990(5)
_cell_angle_gamma                70.714(5)
_cell_volume                     3015.7(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22639
_cell_measurement_theta_min      0.88
_cell_measurement_theta_max      28.32

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3161
_exptl_absorpt_coefficient_mu    22.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_T_max  0.003
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22639
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         28.32
_reflns_number_total             14898
_reflns_number_gt                11332
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
During the refinement, the non-H atoms W, Si, Cu, Eu, C, N and O were 
refined anisotropically. Since most O atoms on the polyanion and lattice 
water molecules as well as some C and N atoms exhibit obvious ADP and
NPD problems with the anisotropic parameters, they are just refined 
isotropically. But this treatment didn't influence the precise of the 
polyanion structure and the final R values.
The restraint command 'isor' was employed to restrain several C, 0 and
N atoms so as to avoid the ADP and NPD problems on them. This command
led to a restraint number 168.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0432P)²+60.3424P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14898
_refine_ls_number_parameters     889
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1312
_refine_ls_wR_factor_gt          0.1091
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.08841(6) 0.50950(5) 0.23553(3) 0.01402(13) Uani 1 1 d . . .
W2 W 0.98897(6) 0.65679(5) 0.36914(3) 0.01443(13) Uani 1 1 d . . .
W3 W 0.98256(6) 1.01434(5) 0.25484(3) 0.01458(13) Uani 1 1 d . . .
W4 W 0.76538(6) 0.92133(6) 0.36919(3) 0.01661(13) Uani 1 1 d . . .
W5 W 0.68367(6) 0.68620(5) 0.35466(3) 0.01461(13) Uani 1 1 d . . .
W6 W 0.78866(6) 0.53435(5) 0.21813(3) 0.01567(13) Uani 1 1 d . . .
W7 W 0.97035(6) 0.62909(5) 0.11102(3) 0.01465(13) Uani 1 1 d . . .
W8 W 0.74210(6) 0.92476(5) 0.10777(3) 0.01447(13) Uani 1 1 d . . .
W9 W 0.64914(6) 1.06816(5) 0.23091(3) 0.01807(14) Uani 1 1 d . . .
W10 W 1.07163(5) 0.88243(5) 0.13298(2) 0.01209(12) Uani 1 1 d . . .
W11 W 0.56206(5) 0.83379(5) 0.21687(3) 0.01429(13) Uani 1 1 d . . .
Cu1 Cu 1.10846(17) 0.24324(16) 0.25486(7) 0.0132(4) Uani 1 1 d . . .
Cu2 Cu 1.69184(17) 0.13081(17) -0.02764(8) 0.0171(4) Uani 1 1 d . . .
Cu3 Cu 0.5000 0.5000 0.5000 0.0292(7) Uani 1 2 d S . .
Eu1 Eu 1.26236(7) 0.73370(7) 0.25992(4) 0.01802(17) Uani 1 1 d . . .
Si1 Si 0.8722(4) 0.7867(3) 0.23780(17) 0.0096(8) Uani 1 1 d . . .
O1 O 1.1949(10) 0.3685(9) 0.2438(5) 0.016(2) Uani 1 1 d . . .
O2 O 1.0586(11) 0.5740(11) 0.4260(5) 0.028(3) Uani 1 1 d . . .
O3 O 0.9880(11) 1.1528(9) 0.2683(5) 0.021(2) Uani 1 1 d . . .
O4 O 0.7168(12) 1.0191(11) 0.4227(5) 0.032(3) Uani 1 1 d . . .
O5 O 0.5741(11) 0.6356(10) 0.3951(5) 0.026(3) Uani 1 1 d . . .
O6 O 0.7103(11) 0.4354(10) 0.2159(5) 0.028(3) Uani 1 1 d . . .
O7 O 1.0184(10) 0.5839(11) 0.0428(5) 0.026(3) Uani 1 1 d . . .
O8 O 0.7074(10) 0.9788(9) 0.0387(5) 0.019(2) Uani 1 1 d U . .
O9 O 0.5562(11) 1.2062(11) 0.2417(6) 0.035(3) Uani 1 1 d . . .
O10 O 1.1364(9) 0.9310(9) 0.0660(5) 0.015(2) Uani 1 1 d . . .
O11 O 0.4101(9) 0.8306(10) 0.2184(5) 0.019(2) Uani 1 1 d . . .
O12 O 0.7469(9) 0.8687(8) 0.2083(4) 0.010(2) Uani 1 1 d U . .
O13 O 0.6546(10) 0.8286(9) 0.3905(5) 0.019(2) Uani 1 1 d . . .
O14 O 0.8930(10) 0.7983(9) 0.4061(5) 0.018(2) Uani 1 1 d . . .
O15 O 0.8241(10) 0.6179(10) 0.3897(5) 0.023(3) Uani 1 1 d . . .
O16 O 0.6661(10) 1.0012(10) 0.3103(5) 0.026(3) Uani 1 1 d . . .
O17 O 0.7409(11) 0.5768(9) 0.2953(5) 0.021(2) Uani 1 1 d . . .
O18 O 1.0213(10) 0.5410(9) 0.3128(4) 0.016(2) Uani 1 1 d . . .
O19 O 1.1029(10) 0.7128(10) 0.3323(5) 0.023(3) Uani 1 1 d . . .
O20 O 0.8049(10) 1.0740(9) 0.2299(5) 0.018(2) Uani 1 1 d . . .
O21 O 1.1355(11) 0.9307(9) 0.2693(5) 0.021(2) Uani 1 1 d . . .
O22 O 1.1838(10) 0.5964(9) 0.2313(5) 0.020(2) Uani 1 1 d . . .
O23 O 1.2110(10) 0.8121(10) 0.1654(5) 0.021(2) Uani 1 1 d . . .
O24 O 1.0307(9) 1.0215(8) 0.1717(4) 0.012(2) Uani 1 1 d U . .
O25 O 0.8923(9) 0.9467(9) 0.1109(5) 0.017(2) Uani 1 1 d . . .
O26 O 0.6582(10) 1.0641(8) 0.1475(5) 0.019(2) Uani 1 1 d . . .
O27 O 0.8291(9) 0.7652(8) 0.0968(4) 0.012(2) Uani 1 1 d . . .
O28 O 1.0918(9) 0.5100(9) 0.1517(4) 0.014(2) Uani 1 1 d U . .
O29 O 0.9424(10) 0.4382(9) 0.2372(5) 0.020(2) Uani 1 1 d U . .
O30 O 0.5198(10) 0.9952(9) 0.2337(5) 0.021(2) Uani 1 1 d . . .
O31 O 0.8549(10) 0.5471(10) 0.1381(4) 0.021(2) Uani 1 1 d . . .
O32 O 0.6602(10) 0.6791(10) 0.1987(5) 0.021(2) Uani 1 1 d . . .
O33 O 1.0566(10) 0.7383(9) 0.1147(5) 0.018(2) Uani 1 1 d . . .
O34 O 0.5861(10) 0.7900(9) 0.2949(5) 0.018(2) Uani 1 1 d . . .
O35 O 0.8963(9) 0.9718(9) 0.3246(5) 0.017(2) Uani 1 1 d U . .
O36 O 0.5903(10) 0.8819(10) 0.1362(5) 0.020(2) Uani 1 1 d . . .
O37 O 0.8400(10) 0.7733(9) 0.3069(5) 0.020(2) Uani 1 1 d . . .
O38 O 0.9166(9) 0.6566(9) 0.2121(4) 0.012(2) Uani 1 1 d . . .
O39 O 0.9791(9) 0.8517(9) 0.2217(4) 0.014(2) Uani 1 1 d . . .
O1W O 1.4299(13) 0.5985(13) 0.1959(8) 0.055(4) Uani 1 1 d . . .
O2W O 1.4016(17) 0.5830(13) 0.3189(7) 0.060(5) Uani 1 1 d . . .
O3W O 1.3245(15) 0.8156(15) 0.3405(6) 0.055(4) Uani 1 1 d . . .
O4W O 1.2737(11) 0.0880(11) 0.2591(6) 0.039(3) Uani 1 1 d . . .
O5W O 1.6381(10) 0.0701(9) -0.0932(5) 0.021(2) Uani 1 1 d U . .
O6W O 1.425(2) 0.385(3) 0.1594(15) 0.053(9) Uani 0.50 1 d P . .
O8W O 1.409(3) -0.033(2) 0.4520(14) 0.048(8) Uani 0.50 1 d PU . .
O9W O 1.345(4) 0.581(3) 0.0949(18) 0.080(12) Uani 0.50 1 d PU . .
O11W O 1.179(4) 0.996(3) 0.3995(18) 0.088(13) Uani 0.50 1 d PU . .
O12W O 0.969(4) 0.025(4) 0.4600(19) 0.090(13) Uani 0.50 1 d PU . .
C1 C 0.9955(16) 0.2722(16) 0.3748(8) 0.030(4) Uani 1 1 d . . .
H1 H 0.9270 0.2613 0.3615 0.036 Uiso 1 1 calc R . .
C2 C 0.9899(15) 0.3014(14) 0.4309(7) 0.022(3) Uani 1 1 d U . .
C3 C 1.0914(15) 0.3067(15) 0.4543(6) 0.022(4) Uani 1 1 d . . .
H3 H 1.0870 0.3194 0.4932 0.026 Uiso 1 1 calc R . .
C4 C 1.2013(13) 0.2924(12) 0.4174(6) 0.012(3) Uani 1 1 d U . .
C5 C 1.2043(14) 0.2703(13) 0.3610(7) 0.019(3) Uani 1 1 d U . .
H5 H 1.2779 0.2621 0.3363 0.023 Uiso 1 1 calc R . .
C6 C 0.7618(15) 0.3910(13) 0.4509(7) 0.020(3) Uani 1 1 d . . .
H6 H 0.7512 0.4370 0.4162 0.024 Uiso 1 1 calc R . .
C7 C 0.7240(16) 0.3038(15) 0.5335(8) 0.027(4) Uani 1 1 d U . .
H7 H 0.6805 0.2783 0.5661 0.033 Uiso 1 1 calc R . .
C8 C 0.8508(17) 0.2621(18) 0.5182(8) 0.038(5) Uani 1 1 d . . .
H8 H 0.9100 0.2082 0.5396 0.045 Uiso 1 1 calc R . .
C9 C 1.428(2) 0.220(2) 0.4305(12) 0.062(7) Uani 1 1 d U . .
H9 H 1.4504 0.1449 0.4176 0.074 Uiso 1 1 calc R . .
C10 C 1.4998(17) 0.2747(16) 0.4510(8) 0.029(4) Uani 1 1 d U . .
H10 H 1.5848 0.2393 0.4542 0.035 Uiso 1 1 calc R . .
C11 C 1.3204(16) 0.3995(16) 0.4561(8) 0.026(4) Uani 1 1 d U . .
H11 H 1.2529 0.4666 0.4634 0.032 Uiso 1 1 calc R . .
C12 C 0.9994(15) 0.2507(13) 0.1485(6) 0.018(3) Uani 1 1 d . . .
H12 H 0.9285 0.2506 0.1737 0.022 Uiso 1 1 calc R . .
C13 C 0.9985(14) 0.2544(14) 0.0898(7) 0.017(3) Uani 1 1 d . . .
C14 C 1.1085(14) 0.2490(14) 0.0504(6) 0.018(3) Uani 1 1 d U . .
H14 H 1.1085 0.2519 0.0104 0.022 Uiso 1 1 calc R . .
C15 C 1.2112(15) 0.2395(14) 0.0750(7) 0.020(3) Uani 1 1 d . . .
C16 C 1.2112(14) 0.2387(12) 0.1344(6) 0.012(3) Uani 1 1 d U . .
H16 H 1.2848 0.2321 0.1495 0.015 Uiso 1 1 calc R . .
C17 C 1.4404(17) 0.1790(16) 0.0382(8) 0.028(4) Uani 1 1 d . . .
H17 H 1.4661 0.1190 0.0666 0.033 Uiso 1 1 calc R . .
C18 C 1.3174(18) 0.3281(17) -0.0092(9) 0.034(5) Uani 1 1 d . . .
H18 H 1.2463 0.3839 -0.0219 0.041 Uiso 1 1 calc R . .
C19 C 1.4414(17) 0.311(2) -0.0343(9) 0.052(7) Uani 1 1 d . . .
H19 H 1.4714 0.3556 -0.0638 0.062 Uiso 1 1 calc R . .
C20 C 0.8710(13) 0.1928(13) 0.0311(6) 0.013(3) Uani 1 1 d U . .
H20 H 0.9379 0.1367 0.0125 0.016 Uiso 1 1 calc R . .
C21 C 0.7670(17) 0.332(2) 0.0852(10) 0.049(7) Uani 1 1 d . . .
H21 H 0.7460 0.3871 0.1129 0.059 Uiso 1 1 calc R . .
C22 C 0.6910(18) 0.310(2) 0.0552(11) 0.059(8) Uani 1 1 d . . .
H22 H 0.6064 0.3524 0.0552 0.071 Uiso 1 1 calc R . .
N1 N 1.1045(11) 0.2598(10) 0.3397(5) 0.010(2) Uani 1 1 d U . .
N2 N 0.8721(11) 0.3155(11) 0.4656(5) 0.015(3) Uani 1 1 d U . .
N3 N 0.6719(13) 0.3900(14) 0.4925(6) 0.030(4) Uani 1 1 d . . .
N4 N 1.3109(12) 0.3059(12) 0.4342(6) 0.023(3) Uani 1 1 d U . .
N5 N 1.4355(13) 0.3865(14) 0.4663(6) 0.033(4) Uani 1 1 d . . .
N6 N 1.1089(10) 0.2470(10) 0.1694(5) 0.011(2) Uani 1 1 d . . .
N7 N 1.3194(12) 0.2505(13) 0.0362(6) 0.026(3) Uani 1 1 d . . .
N8 N 1.5113(13) 0.2044(12) -0.0025(6) 0.023(3) Uani 1 1 d . . .
N9 N 0.8838(13) 0.2594(12) 0.0684(5) 0.020(3) Uani 1 1 d . . .
N10 N 0.7537(12) 0.2132(13) 0.0226(6) 0.027(3) Uani 1 1 d . . .
O7W O 1.559(3) 0.376(3) 0.3155(14) 0.054(8) Uani 0.50 1 d PU A 1
O7W' O 0.725(4) 0.262(3) 0.3377(17) 0.078(11) Uani 0.50 1 d PU B 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O22 1.736(11) . ?
W1 O1 1.753(10) . ?
W1 O18 1.885(11) . ?
W1 O28 1.949(10) . ?
W1 O29 2.109(10) . ?
W1 O38 2.258(10) . ?
W2 O2 1.696(11) . ?
W2 O19 1.740(11) . ?
W2 O14 1.931(11) . ?
W2 O18 1.945(10) . ?
W2 O15 2.064(12) . ?
W2 O37 2.374(11) . ?
W3 O21 1.760(11) . ?
W3 O3 1.772(11) . ?
W3 O35 1.894(10) . ?
W3 O24 1.940(10) . ?
W3 O20 2.054(10) . ?
W3 O39 2.218(10) . ?
W3 Eu1 3.8297(16) . ?
W4 O4 1.726(12) . ?
W4 O16 1.877(12) . ?
W4 O35 1.927(10) . ?
W4 O14 1.931(11) . ?
W4 O13 1.938(10) . ?
W4 O37 2.302(11) . ?
W5 O5 1.696(12) . ?
W5 O15 1.803(10) . ?
W5 O13 1.917(11) . ?
W5 O17 1.923(11) . ?
W5 O34 1.974(11) . ?
W5 O37 2.443(11) . ?
W6 O6 1.729(10) . ?
W6 O29 1.838(11) . ?
W6 O17 1.883(11) . ?
W6 O31 1.923(10) . ?
W6 O32 1.939(11) . ?
W6 O38 2.384(9) . ?
W7 O7 1.698(11) . ?
W7 O31 1.902(11) . ?
W7 O33 1.911(11) . ?
W7 O28 1.912(10) . ?
W7 O27 1.926(9) . ?
W7 O38 2.384(10) . ?
W8 O8 1.721(11) . ?
W8 O25 1.827(10) . ?
W8 O27 1.896(10) . ?
W8 O26 1.918(10) . ?
W8 O36 1.974(10) . ?
W8 O12 2.372(9) . ?
W9 O9 1.689(12) . ?
W9 O20 1.793(10) . ?
W9 O26 1.939(11) . ?
W9 O30 1.946(11) . ?
W9 O16 1.949(12) . ?
W9 O12 2.399(10) . ?
W10 O10 1.761(10) . ?
W10 O23 1.766(11) . ?
W10 O24 1.898(10) . ?
W10 O33 1.917(11) . ?
W10 O25 2.047(10) . ?
W10 O39 2.240(10) . ?
W10 Eu1 3.8446(12) . ?
W11 O11 1.737(10) . ?
W11 O34 1.871(11) . ?
W11 O32 1.906(11) . ?
W11 O36 1.923(11) . ?
W11 O30 1.935(11) . ?
W11 O12 2.257(9) . ?
Cu1 N6 1.989(12) . ?
Cu1 O3 1.998(11) 1_545 ?
Cu1 N1 2.004(12) . ?
Cu1 O1 2.049(10) . ?
Cu1 O4W 2.188(12) . ?
Cu2 N10 1.958(14) 1_655 ?
Cu2 O10 1.968(10) 2_865 ?
Cu2 N8 1.982(14) . ?
Cu2 O5W 2.017(11) . ?
Cu2 O8 2.255(10) 1_645 ?
Cu3 N3 1.968(13) . ?
Cu3 N3 1.968(13) 2_666 ?
Cu3 N5 2.034(16) 2_766 ?
Cu3 N5 2.034(16) 1_455 ?
Eu1 O22 2.333(11) . ?
Eu1 O19 2.359(11) . ?
Eu1 O21 2.373(11) . ?
Eu1 O23 2.375(11) . ?
Eu1 O11 2.401(10) 1_655 ?
Eu1 O2W 2.431(15) . ?
Eu1 O1W 2.500(14) . ?
Eu1 O3W 2.505(15) . ?
Si1 O37 1.606(11) . ?
Si1 O12 1.640(10) . ?
Si1 O39 1.640(10) . ?
Si1 O38 1.650(11) . ?
O3 Cu1 1.998(11) 1_565 ?
O8 Cu2 2.255(10) 1_465 ?
O10 Cu2 1.968(10) 2_865 ?
O11 Eu1 2.401(10) 1_455 ?
C1 N1 1.36(2) . ?
C1 C2 1.38(2) . ?
C2 C3 1.37(2) . ?
C2 N2 1.43(2) . ?
C3 C4 1.39(2) . ?
C4 C5 1.37(2) . ?
C4 N4 1.422(18) . ?
C5 N1 1.348(18) . ?
C6 N3 1.31(2) . ?
C6 N2 1.352(19) . ?
C7 C8 1.37(2) . ?
C7 N3 1.38(2) . ?
C8 N2 1.36(2) . ?
C9 C10 1.38(3) . ?
C9 N4 1.39(3) . ?
C10 N5 1.38(2) . ?
C11 N5 1.32(2) . ?
C11 N4 1.34(2) . ?
C12 C13 1.36(2) . ?
C12 N6 1.386(18) . ?
C13 C14 1.43(2) . ?
C13 N9 1.443(19) . ?
C14 C15 1.34(2) . ?
C15 C16 1.38(2) . ?
C15 N7 1.457(19) . ?
C16 N6 1.306(17) . ?
C17 N8 1.24(2) . ?
C17 N7 1.37(2) . ?
C18 N7 1.34(2) . ?
C18 C19 1.41(2) . ?
C19 N8 1.46(2) . ?
C20 N9 1.306(19) . ?
C20 N10 1.314(19) . ?
C21 C22 1.30(3) . ?
C21 N9 1.36(2) . ?
C22 N10 1.40(2) . ?
N5 Cu3 2.034(16) 1_655 ?
N10 Cu2 1.958(14) 1_455 ?

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
O22 W1 O1 102.5(5) . . ?
O22 W1 O18 94.3(5) . . ?
O1 W1 O18 102.2(5) . . ?
O22 W1 O28 94.5(5) . . ?
O1 W1 O28 95.4(5) . . ?
O18 W1 O28 158.2(4) . . ?
O22 W1 O29 167.7(5) . . ?
O1 W1 O29 89.7(4) . . ?
O18 W1 O29 83.9(4) . . ?
O28 W1 O29 83.3(4) . . ?
O22 W1 O38 95.1(4) . . ?
O1 W1 O38 160.4(4) . . ?
O18 W1 O38 84.7(4) . . ?
O28 W1 O38 74.6(4) . . ?
O29 W1 O38 72.6(4) . . ?
O2 W2 O19 104.0(6) . . ?
O2 W2 O14 100.4(5) . . ?
O19 W2 O14 95.1(5) . . ?
O2 W2 O18 101.5(5) . . ?
O19 W2 O18 92.1(5) . . ?
O14 W2 O18 154.4(4) . . ?
O2 W2 O15 94.7(5) . . ?
O19 W2 O15 161.2(5) . . ?
O14 W2 O15 82.8(4) . . ?
O18 W2 O15 82.5(4) . . ?
O2 W2 O37 163.9(5) . . ?
O19 W2 O37 90.8(5) . . ?
O14 W2 O37 71.6(4) . . ?
O18 W2 O37 83.8(4) . . ?
O15 W2 O37 70.8(4) . . ?
O21 W3 O3 98.3(5) . . ?
O21 W3 O35 97.7(5) . . ?
O3 W3 O35 102.5(5) . . ?
O21 W3 O24 92.5(5) . . ?
O3 W3 O24 97.8(5) . . ?
O35 W3 O24 155.6(4) . . ?
O21 W3 O20 165.6(5) . . ?
O3 W3 O20 95.8(5) . . ?
O35 W3 O20 81.8(4) . . ?
O24 W3 O20 82.8(4) . . ?
O21 W3 O39 84.3(4) . . ?
O3 W3 O39 170.0(4) . . ?
O35 W3 O39 86.7(4) . . ?
O24 W3 O39 72.3(4) . . ?
O20 W3 O39 81.3(4) . . ?
O21 W3 Eu1 25.8(3) . . ?
O3 W3 Eu1 123.9(4) . . ?
O35 W3 Eu1 94.0(3) . . ?
O24 W3 Eu1 85.7(3) . . ?
O20 W3 Eu1 139.8(3) . . ?
O39 W3 Eu1 58.5(3) . . ?
O4 W4 O16 102.3(5) . . ?
O4 W4 O35 100.9(5) . . ?
O16 W4 O35 85.7(5) . . ?
O4 W4 O14 99.9(5) . . ?
O16 W4 O14 157.7(5) . . ?
O35 W4 O14 88.5(4) . . ?
O4 W4 O13 101.5(5) . . ?
O16 W4 O13 89.3(5) . . ?
O35 W4 O13 157.6(5) . . ?
O14 W4 O13 87.9(4) . . ?
O4 W4 O37 172.8(5) . . ?
O16 W4 O37 84.6(4) . . ?
O35 W4 O37 81.8(4) . . ?
O14 W4 O37 73.3(4) . . ?
O13 W4 O37 76.0(4) . . ?
O5 W5 O15 104.5(5) . . ?
O5 W5 O13 100.3(5) . . ?
O15 W5 O13 90.9(5) . . ?
O5 W5 O17 100.6(5) . . ?
O15 W5 O17 91.5(5) . . ?
O13 W5 O17 157.6(4) . . ?
O5 W5 O34 101.8(5) . . ?
O15 W5 O34 153.7(5) . . ?
O13 W5 O34 83.8(4) . . ?
O17 W5 O34 84.2(5) . . ?
O5 W5 O37 172.7(5) . . ?
O15 W5 O37 73.2(5) . . ?
O13 W5 O37 73.0(4) . . ?
O17 W5 O37 86.5(4) . . ?
O34 W5 O37 80.6(4) . . ?
O6 W6 O29 101.6(5) . . ?
O6 W6 O17 101.2(5) . . ?
O29 W6 O17 90.8(5) . . ?
O6 W6 O31 101.0(5) . . ?
O29 W6 O31 90.9(5) . . ?
O17 W6 O31 156.9(5) . . ?
O6 W6 O32 100.7(5) . . ?
O29 W6 O32 157.7(5) . . ?
O17 W6 O32 85.1(5) . . ?
O31 W6 O32 84.6(5) . . ?
O6 W6 O38 172.6(5) . . ?
O29 W6 O38 74.4(4) . . ?
O17 W6 O38 85.3(4) . . ?
O31 W6 O38 73.0(4) . . ?
O32 W6 O38 83.4(4) . . ?
O7 W7 O31 101.4(5) . . ?
O7 W7 O33 102.8(5) . . ?
O31 W7 O33 155.6(5) . . ?
O7 W7 O28 99.0(5) . . ?
O31 W7 O28 87.6(5) . . ?
O33 W7 O28 91.4(4) . . ?
O7 W7 O27 100.8(5) . . ?
O31 W7 O27 88.0(4) . . ?
O33 W7 O27 84.8(4) . . ?
O28 W7 O27 160.2(4) . . ?
O7 W7 O38 169.8(5) . . ?
O31 W7 O38 73.4(4) . . ?
O33 W7 O38 83.1(4) . . ?
O28 W7 O38 72.3(4) . . ?
O27 W7 O38 88.0(4) . . ?
O8 W8 O25 103.0(5) . . ?
O8 W8 O27 101.9(5) . . ?
O25 W8 O27 88.9(4) . . ?
O8 W8 O26 98.7(5) . . ?
O25 W8 O26 89.7(5) . . ?
O27 W8 O26 159.1(4) . . ?
O8 W8 O36 99.3(4) . . ?
O25 W8 O36 157.6(5) . . ?
O27 W8 O36 88.5(4) . . ?
O26 W8 O36 84.9(5) . . ?
O8 W8 O12 168.6(4) . . ?
O25 W8 O12 85.7(4) . . ?
O27 W8 O12 85.3(4) . . ?
O26 W8 O12 73.8(4) . . ?
O36 W8 O12 71.9(4) . . ?
O9 W9 O20 104.1(5) . . ?
O9 W9 O26 101.9(6) . . ?
O20 W9 O26 94.9(5) . . ?
O9 W9 O30 98.8(5) . . ?
O20 W9 O30 156.6(4) . . ?
O26 W9 O30 84.7(5) . . ?
O9 W9 O16 101.7(6) . . ?
O20 W9 O16 86.1(5) . . ?
O26 W9 O16 155.4(4) . . ?
O30 W9 O16 84.9(5) . . ?
O9 W9 O12 168.9(5) . . ?
O20 W9 O12 86.2(4) . . ?
O26 W9 O12 72.8(4) . . ?
O30 W9 O12 71.3(4) . . ?
O16 W9 O12 82.7(4) . . ?
O10 W10 O23 99.1(5) . . ?
O10 W10 O24 98.1(4) . . ?
O23 W10 O24 94.8(5) . . ?
O10 W10 O33 101.9(5) . . ?
O23 W10 O33 93.0(5) . . ?
O24 W10 O33 157.1(4) . . ?
O10 W10 O25 93.5(4) . . ?
O23 W10 O25 167.2(5) . . ?
O24 W10 O25 85.5(4) . . ?
O33 W10 O25 82.3(4) . . ?
O10 W10 O39 170.5(4) . . ?
O23 W10 O39 83.6(4) . . ?
O24 W10 O39 72.5(4) . . ?
O33 W10 O39 87.1(4) . . ?
O25 W10 O39 84.3(4) . . ?
O10 W10 Eu1 124.0(3) . . ?
O23 W10 Eu1 25.5(4) . . ?
O24 W10 Eu1 85.8(3) . . ?
O33 W10 Eu1 92.3(3) . . ?
O25 W10 Eu1 142.3(3) . . ?
O39 W10 Eu1 58.2(3) . . ?
O11 W11 O34 99.5(5) . . ?
O11 W11 O32 102.4(5) . . ?
O34 W11 O32 88.6(5) . . ?
O11 W11 O36 98.9(5) . . ?
O34 W11 O36 161.6(4) . . ?
O32 W11 O36 88.2(5) . . ?
O11 W11 O30 97.5(5) . . ?
O34 W11 O30 89.1(5) . . ?
O32 W11 O30 160.1(5) . . ?
O36 W11 O30 87.9(5) . . ?
O11 W11 O12 170.4(4) . . ?
O34 W11 O12 86.3(4) . . ?
O32 W11 O12 85.4(4) . . ?
O36 W11 O12 75.4(4) . . ?
O30 W11 O12 74.8(4) . . ?
N6 Cu1 O3 91.2(5) . 1_545 ?
N6 Cu1 N1 173.2(5) . . ?
O3 Cu1 N1 93.2(5) 1_545 . ?
N6 Cu1 O1 90.0(5) . . ?
O3 Cu1 O1 166.7(4) 1_545 . ?
N1 Cu1 O1 84.5(4) . . ?
N6 Cu1 O4W 94.7(5) . . ?
O3 Cu1 O4W 94.0(5) 1_545 . ?
N1 Cu1 O4W 90.1(5) . . ?
O1 Cu1 O4W 99.2(5) . . ?
N10 Cu2 O10 88.8(5) 1_655 2_865 ?
N10 Cu2 N8 96.3(6) 1_655 . ?
O10 Cu2 N8 170.2(5) 2_865 . ?
N10 Cu2 O5W 167.5(6) 1_655 . ?
O10 Cu2 O5W 86.2(4) 2_865 . ?
N8 Cu2 O5W 87.0(5) . . ?
N10 Cu2 O8 92.3(5) 1_655 1_645 ?
O10 Cu2 O8 95.5(4) 2_865 1_645 ?
N8 Cu2 O8 92.6(5) . 1_645 ?
O5W Cu2 O8 99.6(4) . 1_645 ?
N3 Cu3 N3 180.000 . 2_666 ?
N3 Cu3 N5 89.0(6) . 2_766 ?
N3 Cu3 N5 91.0(6) 2_666 2_766 ?
N3 Cu3 N5 91.0(6) . 1_455 ?
N3 Cu3 N5 89.0(6) 2_666 1_455 ?
N5 Cu3 N5 180.0 2_766 1_455 ?
O22 Eu1 O19 72.4(4) . . ?
O22 Eu1 O21 121.5(4) . . ?
O19 Eu1 O21 78.6(4) . . ?
O22 Eu1 O23 78.5(4) . . ?
O19 Eu1 O23 119.6(4) . . ?
O21 Eu1 O23 73.5(4) . . ?
O22 Eu1 O11 136.3(4) . 1_655 ?
O19 Eu1 O11 150.9(4) . 1_655 ?
O21 Eu1 O11 80.1(4) . 1_655 ?
O23 Eu1 O11 72.0(4) . 1_655 ?
O22 Eu1 O2W 90.4(5) . . ?
O19 Eu1 O2W 84.7(5) . . ?
O21 Eu1 O2W 136.3(5) . . ?
O23 Eu1 O2W 147.5(5) . . ?
O11 Eu1 O2W 97.5(5) 1_655 . ?
O22 Eu1 O1W 71.1(5) . . ?
O19 Eu1 O1W 135.0(5) . . ?
O21 Eu1 O1W 144.2(5) . . ?
O23 Eu1 O1W 77.3(5) . . ?
O11 Eu1 O1W 71.5(5) 1_655 . ?
O2W Eu1 O1W 70.2(6) . . ?
O22 Eu1 O3W 148.1(5) . . ?
O19 Eu1 O3W 82.2(5) . . ?
O21 Eu1 O3W 70.0(5) . . ?
O23 Eu1 O3W 132.1(5) . . ?
O11 Eu1 O3W 72.0(4) 1_655 . ?
O2W Eu1 O3W 67.9(5) . . ?
O1W Eu1 O3W 118.7(5) . . ?
O22 Eu1 W3 102.7(3) . . ?
O19 Eu1 W3 71.7(3) . . ?
O21 Eu1 W3 18.8(3) . . ?
O23 Eu1 W3 64.8(3) . . ?
O11 Eu1 W3 93.2(3) 1_655 . ?
O2W Eu1 W3 147.6(4) . . ?
O1W Eu1 W3 142.0(4) . . ?
O3W Eu1 W3 86.8(4) . . ?
O22 Eu1 W10 73.6(3) . . ?
O19 Eu1 W10 101.3(3) . . ?
O21 Eu1 W10 63.7(3) . . ?
O23 Eu1 W10 18.6(3) . . ?
O11 Eu1 W10 86.6(2) 1_655 . ?
O2W Eu1 W10 159.9(4) . . ?
O1W Eu1 W10 92.8(4) . . ?
O3W Eu1 W10 131.6(4) . . ?
W3 Eu1 W10 50.74(2) . . ?
O37 Si1 O12 109.8(6) . . ?
O37 Si1 O39 110.0(6) . . ?
O12 Si1 O39 107.3(5) . . ?
O37 Si1 O38 108.8(6) . . ?
O12 Si1 O38 108.4(5) . . ?
O39 Si1 O38 112.5(5) . . ?
W1 O1 Cu1 112.3(5) . . ?
W3 O3 Cu1 138.9(6) . 1_565 ?
W8 O8 Cu2 145.3(6) . 1_465 ?
W10 O10 Cu2 128.2(6) . 2_865 ?
W11 O11 Eu1 145.3(6) . 1_455 ?
Si1 O12 W11 125.7(5) . . ?
Si1 O12 W8 124.4(5) . . ?
W11 O12 W8 93.3(3) . . ?
Si1 O12 W9 120.8(5) . . ?
W11 O12 W9 92.9(3) . . ?
W8 O12 W9 90.4(3) . . ?
W5 O13 W4 120.9(6) . . ?
W4 O14 W2 122.3(6) . . ?
W5 O15 W2 125.1(6) . . ?
W4 O16 W9 151.0(7) . . ?
W6 O17 W5 154.1(6) . . ?
W1 O18 W2 142.0(5) . . ?
W2 O19 Eu1 158.6(6) . . ?
W9 O20 W3 153.0(6) . . ?
W3 O21 Eu1 135.3(5) . . ?
W1 O22 Eu1 157.3(6) . . ?
W10 O23 Eu1 135.9(6) . . ?
W10 O24 W3 117.9(5) . . ?
W8 O25 W10 149.0(6) . . ?
W8 O26 W9 122.7(5) . . ?
W8 O27 W7 148.7(5) . . ?
W7 O28 W1 120.4(5) . . ?
W6 O29 W1 118.9(5) . . ?
W11 O30 W9 121.0(5) . . ?
W7 O31 W6 123.5(5) . . ?
W11 O32 W6 149.3(6) . . ?
W7 O33 W10 155.1(6) . . ?
W11 O34 W5 150.3(6) . . ?
W3 O35 W4 154.0(6) . . ?
W11 O36 W8 119.5(5) . . ?
Si1 O37 W4 126.8(6) . . ?
Si1 O37 W2 122.7(6) . . ?
W4 O37 W2 92.7(4) . . ?
Si1 O37 W5 123.8(6) . . ?
W4 O37 W5 89.9(4) . . ?
W2 O37 W5 90.9(4) . . ?
Si1 O38 W1 123.9(5) . . ?
Si1 O38 W7 122.1(5) . . ?
W1 O38 W7 92.4(4) . . ?
Si1 O38 W6 125.1(5) . . ?
W1 O38 W6 94.1(4) . . ?
W7 O38 W6 89.9(3) . . ?
Si1 O39 W3 128.1(6) . . ?
Si1 O39 W10 126.4(5) . . ?
W3 O39 W10 95.1(4) . . ?
N1 C1 C2 117.7(15) . . ?
C3 C2 C1 123.2(16) . . ?
C3 C2 N2 121.2(14) . . ?
C1 C2 N2 115.3(15) . . ?
C2 C3 C4 117.1(14) . . ?
C5 C4 C3 119.3(14) . . ?
C5 C4 N4 117.3(13) . . ?
C3 C4 N4 123.4(13) . . ?
N1 C5 C4 122.4(14) . . ?
N3 C6 N2 110.2(14) . . ?
C8 C7 N3 108.5(16) . . ?
N2 C8 C7 105.9(15) . . ?
C10 C9 N4 101(2) . . ?
N5 C10 C9 114.4(19) . . ?
N5 C11 N4 112.9(16) . . ?
C13 C12 N6 118.1(14) . . ?
C12 C13 C14 121.8(14) . . ?
C12 C13 N9 117.8(13) . . ?
C14 C13 N9 120.4(14) . . ?
C15 C14 C13 115.4(14) . . ?
C14 C15 C16 122.6(14) . . ?
C14 C15 N7 116.7(15) . . ?
C16 C15 N7 119.8(13) . . ?
N6 C16 C15 120.8(13) . . ?
N8 C17 N7 111.5(16) . . ?
N7 C18 C19 108.2(17) . . ?
C18 C19 N8 102.6(16) . . ?
N9 C20 N10 113.0(14) . . ?
C22 C21 N9 106.5(18) . . ?
C21 C22 N10 110.7(17) . . ?
C5 N1 C1 119.9(13) . . ?
C5 N1 Cu1 120.7(10) . . ?
C1 N1 Cu1 119.1(10) . . ?
C6 N2 C8 108.3(13) . . ?
C6 N2 C2 124.0(13) . . ?
C8 N2 C2 127.7(14) . . ?
C6 N3 C7 106.6(14) . . ?
C6 N3 Cu3 127.3(12) . . ?
C7 N3 Cu3 125.8(12) . . ?
C11 N4 C9 109.3(16) . . ?
C11 N4 C4 127.1(14) . . ?
C9 N4 C4 123.6(16) . . ?
C11 N5 C10 102.4(15) . . ?
C11 N5 Cu3 128.7(12) . 1_655 ?
C10 N5 Cu3 128.8(12) . 1_655 ?
C16 N6 C12 121.1(13) . . ?
C16 N6 Cu1 121.1(9) . . ?
C12 N6 Cu1 117.7(10) . . ?
C18 N7 C17 108.0(15) . . ?
C18 N7 C15 126.3(14) . . ?
C17 N7 C15 125.7(15) . . ?
C17 N8 C19 109.0(15) . . ?
C17 N8 Cu2 132.0(13) . . ?
C19 N8 Cu2 119.0(11) . . ?
C20 N9 C21 107.0(14) . . ?
C20 N9 C13 126.9(14) . . ?
C21 N9 C13 126.1(14) . . ?
C20 N10 C22 102.2(14) . . ?
C20 N10 Cu2 126.6(11) . 1_455 ?
C22 N10 Cu2 131.1(12) . 1_455 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         2.681
_refine_diff_density_min         -2.677
_refine_diff_density_rms         0.496
_database_code_depnum_ccdc_archive 'CCDC 1005803'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_sm

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H36 Cu5 N20 O93 Si2 Sm2 W22'
_chemical_formula_sum            'C44 H66 Cu5 N20 O93 Si2 Sm2 W22'
_chemical_formula_weight         7082.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.384(5)
_cell_length_b                   12.189(5)
_cell_length_c                   23.331(5)
_cell_angle_alpha                83.750(5)
_cell_angle_beta                 82.022(5)
_cell_angle_gamma                70.697(5)
_cell_volume                     3019.0(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17435
_cell_measurement_theta_min      0.88
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3139
_exptl_absorpt_coefficient_mu    22.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_T_max  0.003
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17435
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10604
_reflns_number_gt                8015
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
During the refinement, the non-H atoms W, Si, Cu, Sm, C, N and O were 
refined anisotropically. Since most O atoms on the polyanion and lattice 
water molecules as well as some C and N atoms exhibit obvious ADP and
NPD problems with the anisotropic parameters, they are just refined 
isotropically. But this treatment didn't influence the precise of the 
polyanion structure and the final R values.
The 'omit 0 50' command was used to omit the weak reflections above 50
degree.
The restraint command 'isor' was employed to restrain several C, 0 and
N atoms so as to avoid the ADP and NPD problems on them. This command
led to a restraint number 252.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1157P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10604
_refine_ls_number_parameters     871
_refine_ls_number_restraints     252
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1850
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W -0.08883(8) 0.49088(7) 0.76447(4) 0.0145(2) Uani 1 1 d . . .
W2 W 0.01059(8) 0.34366(7) 0.63091(4) 0.0139(2) Uani 1 1 d . . .
W3 W 0.01731(8) -0.01425(7) 0.74517(4) 0.0146(2) Uani 1 1 d . . .
W4 W 0.23396(8) 0.07845(7) 0.63100(4) 0.0164(2) Uani 1 1 d . . .
W5 W 0.31600(8) 0.31348(7) 0.64562(4) 0.0145(2) Uani 1 1 d . . .
W6 W 0.21112(8) 0.46532(7) 0.78200(4) 0.0160(2) Uani 1 1 d . . .
W7 W 0.02890(8) 0.37080(7) 0.88917(4) 0.0143(2) Uani 1 1 d . . .
W8 W 0.25684(8) 0.07533(7) 0.89234(4) 0.0142(2) Uani 1 1 d . . .
W9 W 0.35001(8) -0.06832(7) 0.76910(5) 0.0180(2) Uani 1 1 d . . .
W10 W -0.07242(7) 0.11811(7) 0.86721(4) 0.0116(2) Uani 1 1 d . . .
W11 W 0.43711(8) 0.16576(7) 0.78342(4) 0.0148(2) Uani 1 1 d . . .
Cu1 Cu -0.1086(2) 0.7575(2) 0.74498(12) 0.0134(6) Uani 1 1 d . . .
Cu2 Cu -0.6916(2) 0.8695(2) 1.02778(12) 0.0157(6) Uani 1 1 d . . .
Cu3 Cu 0.5000 0.5000 0.5000 0.0286(11) Uani 1 2 d S . .
Sm1 Sm -0.26350(10) 0.26703(9) 0.73989(6) 0.0176(3) Uani 1 1 d . . .
Si1 Si 0.1264(5) 0.2127(4) 0.7627(3) 0.0115(13) Uani 1 1 d . . .
O1 O -0.1927(14) 0.6301(13) 0.7575(7) 0.023(4) Uani 1 1 d U . .
O2 O -0.0578(15) 0.4268(12) 0.5730(8) 0.027(4) Uani 1 1 d . . .
O3 O 0.0123(14) -0.1516(12) 0.7339(7) 0.019(3) Uani 1 1 d U . .
O4 O 0.2816(16) -0.0179(13) 0.5773(7) 0.026(4) Uani 1 1 d . . .
O5 O 0.4248(13) 0.3675(12) 0.6042(7) 0.018(3) Uani 1 1 d U . .
O6 O 0.2908(14) 0.5636(12) 0.7848(8) 0.023(4) Uani 1 1 d . . .
O7 O -0.0194(17) 0.4168(15) 0.9578(8) 0.033(4) Uani 1 1 d . . .
O8 O 0.2945(14) 0.0203(13) 0.9625(7) 0.019(4) Uani 1 1 d . . .
O9 O 0.4450(15) -0.2116(13) 0.7606(9) 0.032(5) Uani 1 1 d . . .
O10 O -0.1398(13) 0.0722(12) 0.9335(7) 0.017(3) Uani 1 1 d U . .
O11 O 0.5934(12) 0.1623(11) 0.7818(7) 0.016(4) Uani 1 1 d . . .
O12 O 0.2483(12) 0.1350(12) 0.7920(7) 0.013(3) Uani 1 1 d U . .
O13 O 0.3472(13) 0.1660(13) 0.6061(8) 0.024(4) Uani 1 1 d . . .
O14 O 0.1050(15) 0.2030(14) 0.5950(8) 0.027(4) Uani 1 1 d . . .
O15 O 0.1773(13) 0.3811(12) 0.6105(7) 0.016(3) Uani 1 1 d . . .
O16 O 0.3282(16) 0.0005(14) 0.6907(8) 0.029(4) Uani 1 1 d . . .
O17 O 0.2587(14) 0.4189(12) 0.7043(7) 0.021(3) Uani 1 1 d U . .
O18 O -0.0228(13) 0.4610(11) 0.6867(7) 0.015(3) Uani 1 1 d U . .
O19 O -0.1023(13) 0.2850(12) 0.6678(7) 0.016(3) Uani 1 1 d U . .
O20 O 0.1875(15) -0.0703(14) 0.7714(7) 0.024(4) Uani 1 1 d . . .
O21 O -0.1362(13) 0.0716(11) 0.7311(7) 0.013(3) Uani 1 1 d U . .
O22 O -0.1831(13) 0.4046(12) 0.7682(7) 0.017(3) Uani 1 1 d U . .
O23 O -0.2090(12) 0.1877(11) 0.8353(7) 0.012(3) Uani 1 1 d U . .
O24 O -0.0326(13) -0.0214(12) 0.8265(7) 0.018(3) Uani 1 1 d . . .
O25 O 0.1054(13) 0.0559(13) 0.8903(8) 0.023(4) Uani 1 1 d . . .
O26 O 0.3390(14) -0.0651(11) 0.8521(7) 0.015(3) Uani 1 1 d U . .
O27 O 0.1707(12) 0.2395(12) 0.9027(7) 0.014(3) Uani 1 1 d U . .
O28 O -0.0927(14) 0.4895(12) 0.8486(7) 0.017(3) Uani 1 1 d U . .
O29 O 0.0582(13) 0.5600(12) 0.7631(7) 0.019(3) Uani 1 1 d U . .
O30 O 0.4767(15) 0.0099(14) 0.7661(8) 0.025(4) Uani 1 1 d U . .
O31 O 0.1438(13) 0.4568(11) 0.8624(7) 0.014(3) Uani 1 1 d . . .
O32 O 0.3374(17) 0.3215(17) 0.7998(8) 0.035(5) Uani 1 1 d . . .
O33 O -0.0538(13) 0.2589(12) 0.8859(7) 0.017(3) Uani 1 1 d U . .
O34 O 0.4116(16) 0.2131(15) 0.7054(8) 0.034(5) Uani 1 1 d . . .
O35 O 0.1055(13) 0.0217(11) 0.6742(7) 0.020(4) Uani 1 1 d . . .
O36 O 0.4112(13) 0.1157(13) 0.8640(7) 0.019(3) Uani 1 1 d U . .
O37 O 0.1631(12) 0.2297(11) 0.6918(6) 0.010(3) Uani 1 1 d U . .
O38 O 0.0857(14) 0.3356(12) 0.7885(7) 0.019(4) Uani 1 1 d . . .
O39 O 0.0220(13) 0.1510(11) 0.7788(6) 0.012(3) Uani 1 1 d U . .
O1W O -0.4364(17) 0.4061(19) 0.8065(10) 0.053(6) Uani 1 1 d . . .
O2W O -0.402(2) 0.420(2) 0.6798(11) 0.073(8) Uani 1 1 d . . .
O3W O -0.3227(19) 0.1821(17) 0.6586(9) 0.044(5) Uani 1 1 d . . .
O4W O -0.2662(19) 0.9070(18) 0.7401(10) 0.054(6) Uani 1 1 d . . .
O5W O -0.6372(14) 0.9307(15) 1.0933(8) 0.029(4) Uani 1 1 d . . .
O6W O -0.343(4) 0.436(4) 0.905(2) 0.062(12) Uani 0.50 1 d PU . .
O7W O 0.576(3) -0.366(4) 0.840(2) 0.070(16) Uani 0.50 1 d P . .
O9W O -0.573(5) 0.632(4) 0.689(3) 0.080(16) Uani 0.50 1 d PU . .
O10W O -0.089(7) -0.009(6) 0.594(3) 0.12(2) Uani 0.50 1 d PU . .
O11W O -0.413(4) 0.049(3) 0.551(2) 0.062(14) Uani 0.50 1 d P . .
C1 C -0.0036(19) 0.7317(18) 0.6264(10) 0.016(5) Uani 1 1 d U . .
H1 H 0.0625 0.7448 0.6408 0.020 Uiso 1 1 calc R . .
C2 C 0.0122(19) 0.7004(17) 0.5687(10) 0.017(5) Uani 1 1 d U . .
C3 C -0.088(2) 0.688(2) 0.5415(12) 0.026(6) Uani 1 1 d . . .
H3 H -0.0820 0.6690 0.5035 0.031 Uiso 1 1 calc R . .
C4 C -0.2028(18) 0.7119(16) 0.5842(10) 0.014(5) Uani 1 1 d . . .
C5 C -0.2043(19) 0.7347(16) 0.6391(10) 0.014(4) Uani 1 1 d U . .
H5 H -0.2783 0.7452 0.6637 0.017 Uiso 1 1 calc R . .
C6 C 0.241(2) 0.6032(19) 0.5487(11) 0.023(6) Uani 1 1 d . . .
H6 H 0.2521 0.5511 0.5813 0.028 Uiso 1 1 calc R . .
C7 C 0.280(2) 0.687(2) 0.4661(12) 0.034(7) Uani 1 1 d . . .
H7 H 0.3237 0.7019 0.4310 0.041 Uiso 1 1 calc R . .
C8 C 0.152(2) 0.740(2) 0.4824(11) 0.029(6) Uani 1 1 d . . .
H8 H 0.0953 0.8007 0.4625 0.034 Uiso 1 1 calc R . .
C9 C -0.429(3) 0.777(3) 0.5704(15) 0.045(7) Uani 1 1 d U . .
H9 H -0.4537 0.8502 0.5854 0.054 Uiso 1 1 calc R . .
C10 C -0.500(4) 0.725(3) 0.548(2) 0.083(15) Uani 1 1 d . . .
H10 H -0.5845 0.7613 0.5432 0.099 Uiso 1 1 calc R . .
C11 C -0.321(3) 0.598(2) 0.5452(13) 0.036(7) Uani 1 1 d U . .
H11 H -0.2554 0.5288 0.5405 0.043 Uiso 1 1 calc R . .
C12 C -0.005(2) 0.7511(17) 0.8516(10) 0.020(5) Uani 1 1 d . . .
H12 H 0.0663 0.7489 0.8264 0.024 Uiso 1 1 calc R . .
C13 C -0.0009(18) 0.7487(16) 0.9110(10) 0.013(5) Uani 1 1 d . . .
C14 C -0.108(2) 0.7535(18) 0.9497(11) 0.018(5) Uani 1 1 d U . .
H14 H -0.1080 0.7521 0.9896 0.022 Uiso 1 1 calc R . .
C15 C -0.214(2) 0.7602(19) 0.9257(11) 0.020(5) Uani 1 1 d U . .
C16 C -0.214(2) 0.7604(18) 0.8663(10) 0.017(5) Uani 1 1 d U . .
H16 H -0.2867 0.7632 0.8512 0.020 Uiso 1 1 calc R . .
C17 C -0.434(2) 0.818(2) 0.9586(13) 0.033(7) Uani 1 1 d . . .
H17 H -0.4586 0.8762 0.9296 0.039 Uiso 1 1 calc R . .
C18 C -0.317(2) 0.676(2) 1.0097(13) 0.036(6) Uani 1 1 d U . .
H18 H -0.2452 0.6228 1.0233 0.043 Uiso 1 1 calc R . .
C19 C -0.438(2) 0.692(2) 1.0327(13) 0.033(7) Uani 1 1 d . . .
H19 H -0.4650 0.6475 1.0629 0.040 Uiso 1 1 calc R . .
C20 C 0.126(2) 0.8110(19) 0.9689(11) 0.020(5) Uani 1 1 d U . .
H20 H 0.0600 0.8699 0.9860 0.024 Uiso 1 1 calc R . .
C21 C 0.237(2) 0.663(2) 0.9128(12) 0.031(6) Uani 1 1 d U . .
H21 H 0.2570 0.6087 0.8849 0.037 Uiso 1 1 calc R . .
C22 C 0.313(3) 0.689(2) 0.9452(13) 0.037(7) Uani 1 1 d U . .
H22 H 0.3976 0.6474 0.9457 0.044 Uiso 1 1 calc R . .
N1 N -0.1067(16) 0.7430(14) 0.6600(8) 0.014(4) Uani 1 1 d U . .
N2 N 0.1285(15) 0.6829(14) 0.5348(8) 0.011(4) Uani 1 1 d U . .
N3 N 0.3269(16) 0.6137(15) 0.5084(9) 0.019(4) Uani 1 1 d U . .
N4 N -0.3136(18) 0.6978(15) 0.5653(10) 0.028(6) Uani 1 1 d . . .
N5 N -0.4366(18) 0.6166(16) 0.5338(10) 0.029(5) Uani 1 1 d . . .
N6 N -0.1096(15) 0.7566(13) 0.8301(8) 0.008(3) Uani 1 1 d U . .
N7 N -0.3221(16) 0.7531(15) 0.9633(8) 0.018(4) Uani 1 1 d U . .
N8 N -0.5114(18) 0.7883(17) 1.0025(9) 0.025(5) Uani 1 1 d U . .
N9 N 0.1158(19) 0.7408(17) 0.9329(9) 0.026(5) Uani 1 1 d . . .
N10 N 0.2486(17) 0.7856(15) 0.9777(9) 0.020(4) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O22 1.722(14) . ?
W1 O1 1.723(15) . ?
W1 O18 1.889(15) . ?
W1 O28 1.956(15) . ?
W1 O29 2.103(14) . ?
W1 O38 2.332(13) . ?
W2 O2 1.711(15) . ?
W2 O19 1.753(15) . ?
W2 O14 1.908(17) . ?
W2 O18 1.948(15) . ?
W2 O15 2.076(15) . ?
W2 O37 2.372(12) . ?
W3 O3 1.743(14) . ?
W3 O21 1.770(13) . ?
W3 O35 1.900(16) . ?
W3 O24 1.904(16) . ?
W3 O20 1.990(15) . ?
W3 O39 2.258(14) . ?
W4 O4 1.719(17) . ?
W4 O16 1.857(16) . ?
W4 O13 1.925(15) . ?
W4 O35 1.934(15) . ?
W4 O14 1.938(16) . ?
W4 O37 2.309(14) . ?
W5 O5 1.723(15) . ?
W5 O15 1.787(13) . ?
W5 O17 1.879(17) . ?
W5 O34 1.949(17) . ?
W5 O13 2.014(16) . ?
W5 O37 2.376(13) . ?
W6 O6 1.736(14) . ?
W6 O29 1.825(13) . ?
W6 O17 1.910(17) . ?
W6 O32 1.911(19) . ?
W6 O31 1.930(16) . ?
W6 O38 2.437(15) . ?
W7 O7 1.710(19) . ?
W7 O27 1.895(13) . ?
W7 O33 1.909(14) . ?
W7 O28 1.910(13) . ?
W7 O31 1.933(14) . ?
W7 O38 2.394(17) . ?
W8 O8 1.754(15) . ?
W8 O25 1.824(14) . ?
W8 O26 1.932(14) . ?
W8 O27 1.940(14) . ?
W8 O36 1.986(15) . ?
W8 O12 2.380(15) . ?
W9 O9 1.740(15) . ?
W9 O20 1.851(15) . ?
W9 O26 1.927(15) . ?
W9 O16 1.939(17) . ?
W9 O30 1.966(14) . ?
W9 O12 2.447(14) . ?
W10 O23 1.733(13) . ?
W10 O10 1.750(16) . ?
W10 O33 1.899(14) . ?
W10 O24 1.930(15) . ?
W10 O25 2.040(14) . ?
W10 O39 2.250(15) . ?
W11 O11 1.760(13) . ?
W11 O30 1.877(16) . ?
W11 O34 1.881(18) . ?
W11 O32 1.91(2) . ?
W11 O36 1.926(15) . ?
W11 O12 2.280(13) . ?
Cu1 N6 1.983(18) . ?
Cu1 N1 2.006(19) . ?
Cu1 O3 2.010(14) 1_565 ?
Cu1 O1 2.054(15) . ?
Cu1 O4W 2.10(2) . ?
Cu2 O10 1.939(15) 2_467 ?
Cu2 N10 1.954(19) 1_455 ?
Cu2 N8 2.00(2) . ?
Cu2 O5W 2.024(16) . ?
Cu2 O8 2.234(15) 1_465 ?
Cu3 N3 1.997(17) 2_666 ?
Cu3 N3 1.997(17) . ?
Cu3 N5 2.059(19) 2_566 ?
Cu3 N5 2.059(19) 1_655 ?
Sm1 O22 2.347(14) . ?
Sm1 O21 2.358(13) . ?
Sm1 O19 2.360(16) . ?
Sm1 O23 2.408(14) . ?
Sm1 O11 2.429(14) 1_455 ?
Sm1 O2W 2.46(2) . ?
Sm1 O3W 2.524(19) . ?
Sm1 O1W 2.59(2) . ?
Si1 O38 1.576(15) . ?
Si1 O39 1.590(14) . ?
Si1 O12 1.595(14) . ?
Si1 O37 1.656(16) . ?
O3 Cu1 2.010(14) 1_545 ?
O8 Cu2 2.234(15) 1_645 ?
O10 Cu2 1.939(15) 2_467 ?
O11 Sm1 2.429(13) 1_655 ?
C1 N1 1.29(3) . ?
C1 C2 1.41(3) . ?
C2 N2 1.41(3) . ?
C2 C3 1.43(3) . ?
C3 C4 1.50(3) . ?
C4 C5 1.34(3) . ?
C4 N4 1.46(3) . ?
C5 N1 1.31(3) . ?
C6 N3 1.29(3) . ?
C6 N2 1.38(3) . ?
C7 N3 1.30(3) . ?
C7 C8 1.40(4) . ?
C8 N2 1.38(3) . ?
C9 N4 1.35(3) . ?
C9 C10 1.37(4) . ?
C10 N5 1.33(4) . ?
C11 N5 1.32(3) . ?
C11 N4 1.38(3) . ?
C12 N6 1.33(3) . ?
C12 C13 1.39(3) . ?
C13 C14 1.41(3) . ?
C13 N9 1.46(2) . ?
C14 C15 1.37(3) . ?
C15 C16 1.39(3) . ?
C15 N7 1.43(3) . ?
C16 N6 1.35(3) . ?
C17 N7 1.27(3) . ?
C17 N8 1.35(3) . ?
C18 N7 1.35(3) . ?
C18 C19 1.36(4) . ?
C19 N8 1.38(3) . ?
C20 N9 1.30(3) . ?
C20 N10 1.36(3) . ?
C21 C22 1.36(3) . ?
C21 N9 1.44(3) . ?
C22 N10 1.41(3) . ?
N5 Cu3 2.059(19) 1_455 ?
N10 Cu2 1.954(19) 1_655 ?

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
O22 W1 O1 103.1(7) . . ?
O22 W1 O18 94.1(7) . . ?
O1 W1 O18 102.4(7) . . ?
O22 W1 O28 94.4(7) . . ?
O1 W1 O28 94.6(7) . . ?
O18 W1 O28 158.8(6) . . ?
O22 W1 O29 167.0(6) . . ?
O1 W1 O29 89.8(6) . . ?
O18 W1 O29 83.8(6) . . ?
O28 W1 O29 83.5(6) . . ?
O22 W1 O38 93.6(6) . . ?
O1 W1 O38 160.9(6) . . ?
O18 W1 O38 85.2(6) . . ?
O28 W1 O38 74.8(6) . . ?
O29 W1 O38 73.4(5) . . ?
O2 W2 O19 105.2(7) . . ?
O2 W2 O14 100.5(8) . . ?
O19 W2 O14 93.8(7) . . ?
O2 W2 O18 101.2(7) . . ?
O19 W2 O18 92.9(6) . . ?
O14 W2 O18 154.8(6) . . ?
O2 W2 O15 94.5(7) . . ?
O19 W2 O15 160.3(6) . . ?
O14 W2 O15 82.8(6) . . ?
O18 W2 O15 82.8(6) . . ?
O2 W2 O37 161.9(7) . . ?
O19 W2 O37 91.7(5) . . ?
O14 W2 O37 71.3(6) . . ?
O18 W2 O37 84.2(5) . . ?
O15 W2 O37 68.8(5) . . ?
O3 W3 O21 99.7(6) . . ?
O3 W3 O35 101.4(7) . . ?
O21 W3 O35 98.7(6) . . ?
O3 W3 O24 95.9(7) . . ?
O21 W3 O24 91.4(7) . . ?
O35 W3 O24 158.1(6) . . ?
O3 W3 O20 95.9(6) . . ?
O21 W3 O20 163.7(7) . . ?
O35 W3 O20 82.7(6) . . ?
O24 W3 O20 82.3(6) . . ?
O3 W3 O39 168.5(6) . . ?
O21 W3 O39 83.7(5) . . ?
O35 W3 O39 88.9(6) . . ?
O24 W3 O39 72.9(5) . . ?
O20 W3 O39 80.1(6) . . ?
O4 W4 O16 103.9(8) . . ?
O4 W4 O13 98.2(7) . . ?
O16 W4 O13 91.3(7) . . ?
O4 W4 O35 98.7(7) . . ?
O16 W4 O35 84.1(6) . . ?
O13 W4 O35 163.0(7) . . ?
O4 W4 O14 100.2(7) . . ?
O16 W4 O14 155.7(8) . . ?
O13 W4 O14 88.2(6) . . ?
O35 W4 O14 89.3(6) . . ?
O4 W4 O37 171.3(6) . . ?
O16 W4 O37 83.9(7) . . ?
O13 W4 O37 77.4(6) . . ?
O35 W4 O37 85.9(6) . . ?
O14 W4 O37 72.3(6) . . ?
O5 W5 O15 103.2(7) . . ?
O5 W5 O17 100.9(7) . . ?
O15 W5 O17 91.7(6) . . ?
O5 W5 O34 102.9(7) . . ?
O15 W5 O34 154.0(7) . . ?
O17 W5 O34 83.0(7) . . ?
O5 W5 O13 99.9(7) . . ?
O15 W5 O13 90.2(6) . . ?
O17 W5 O13 158.1(7) . . ?
O34 W5 O13 85.8(7) . . ?
O5 W5 O37 172.8(6) . . ?
O15 W5 O37 73.1(6) . . ?
O17 W5 O37 85.5(6) . . ?
O34 W5 O37 81.0(6) . . ?
O13 W5 O37 74.2(6) . . ?
O6 W6 O29 102.6(7) . . ?
O6 W6 O17 102.6(7) . . ?
O29 W6 O17 91.0(7) . . ?
O6 W6 O32 100.7(7) . . ?
O29 W6 O32 156.7(7) . . ?
O17 W6 O32 83.4(7) . . ?
O6 W6 O31 99.6(7) . . ?
O29 W6 O31 90.2(6) . . ?
O17 W6 O31 157.0(6) . . ?
O32 W6 O31 86.6(7) . . ?
O6 W6 O38 173.4(7) . . ?
O29 W6 O38 75.6(5) . . ?
O17 W6 O38 83.8(6) . . ?
O32 W6 O38 81.3(6) . . ?
O31 W6 O38 74.2(6) . . ?
O7 W7 O27 101.0(7) . . ?
O7 W7 O33 103.2(7) . . ?
O27 W7 O33 85.0(6) . . ?
O7 W7 O28 98.9(7) . . ?
O27 W7 O28 160.1(7) . . ?
O33 W7 O28 92.5(6) . . ?
O7 W7 O31 100.4(7) . . ?
O27 W7 O31 87.4(5) . . ?
O33 W7 O31 156.2(7) . . ?
O28 W7 O31 87.1(6) . . ?
O7 W7 O38 171.7(6) . . ?
O27 W7 O38 86.0(6) . . ?
O33 W7 O38 81.8(6) . . ?
O28 W7 O38 74.1(6) . . ?
O31 W7 O38 75.2(6) . . ?
O8 W8 O25 103.4(7) . . ?
O8 W8 O26 98.8(7) . . ?
O25 W8 O26 90.2(7) . . ?
O8 W8 O27 102.5(7) . . ?
O25 W8 O27 88.8(6) . . ?
O26 W8 O27 158.3(6) . . ?
O8 W8 O36 98.0(6) . . ?
O25 W8 O36 158.5(7) . . ?
O26 W8 O36 84.9(6) . . ?
O27 W8 O36 88.2(6) . . ?
O8 W8 O12 168.9(6) . . ?
O25 W8 O12 85.8(6) . . ?
O26 W8 O12 74.7(5) . . ?
O27 W8 O12 83.6(6) . . ?
O36 W8 O12 72.8(5) . . ?
O9 W9 O20 105.5(8) . . ?
O9 W9 O26 100.0(8) . . ?
O20 W9 O26 93.1(7) . . ?
O9 W9 O16 104.8(9) . . ?
O20 W9 O16 85.1(7) . . ?
O26 W9 O16 154.7(7) . . ?
O9 W9 O30 100.8(7) . . ?
O20 W9 O30 153.5(7) . . ?
O26 W9 O30 85.6(7) . . ?
O16 W9 O30 85.0(7) . . ?
O9 W9 O12 168.8(6) . . ?
O20 W9 O12 84.0(6) . . ?
O26 W9 O12 73.2(5) . . ?
O16 W9 O12 81.6(6) . . ?
O30 W9 O12 70.2(6) . . ?
O23 W10 O10 98.1(6) . . ?
O23 W10 O33 94.1(6) . . ?
O10 W10 O33 101.5(7) . . ?
O23 W10 O24 94.0(6) . . ?
O10 W10 O24 99.4(7) . . ?
O33 W10 O24 156.3(6) . . ?
O23 W10 O25 167.3(7) . . ?
O10 W10 O25 94.2(6) . . ?
O33 W10 O25 80.2(6) . . ?
O24 W10 O25 87.2(6) . . ?
O23 W10 O39 84.0(6) . . ?
O10 W10 O39 172.0(6) . . ?
O33 W10 O39 86.1(6) . . ?
O24 W10 O39 72.7(6) . . ?
O25 W10 O39 84.3(6) . . ?
O11 W11 O30 95.5(6) . . ?
O11 W11 O34 99.9(7) . . ?
O30 W11 O34 89.5(8) . . ?
O11 W11 O32 105.4(6) . . ?
O30 W11 O32 159.1(7) . . ?
O34 W11 O32 86.0(8) . . ?
O11 W11 O36 97.9(7) . . ?
O30 W11 O36 87.9(7) . . ?
O34 W11 O36 162.2(6) . . ?
O32 W11 O36 90.1(7) . . ?
O11 W11 O12 169.3(5) . . ?
O30 W11 O12 75.6(6) . . ?
O34 W11 O12 86.1(6) . . ?
O32 W11 O12 83.7(6) . . ?
O36 W11 O12 76.2(5) . . ?
N6 Cu1 N1 174.8(6) . . ?
N6 Cu1 O3 89.0(6) . 1_565 ?
N1 Cu1 O3 94.8(7) . 1_565 ?
N6 Cu1 O1 89.8(6) . . ?
N1 Cu1 O1 85.7(7) . . ?
O3 Cu1 O1 165.9(6) 1_565 . ?
N6 Cu1 O4W 94.5(8) . . ?
N1 Cu1 O4W 88.8(8) . . ?
O3 Cu1 O4W 93.7(6) 1_565 . ?
O1 Cu1 O4W 100.5(6) . . ?
O10 Cu2 N10 89.2(7) 2_467 1_455 ?
O10 Cu2 N8 168.4(7) 2_467 . ?
N10 Cu2 N8 93.7(8) 1_455 . ?
O10 Cu2 O5W 86.3(7) 2_467 . ?
N10 Cu2 O5W 167.5(8) 1_455 . ?
N8 Cu2 O5W 88.5(7) . . ?
O10 Cu2 O8 96.9(6) 2_467 1_465 ?
N10 Cu2 O8 93.2(7) 1_455 1_465 ?
N8 Cu2 O8 94.1(7) . 1_465 ?
O5W Cu2 O8 98.9(6) . 1_465 ?
N3 Cu3 N3 180.000 2_666 . ?
N3 Cu3 N5 89.2(7) 2_666 2_566 ?
N3 Cu3 N5 90.8(8) . 2_566 ?
N3 Cu3 N5 90.8(8) 2_666 1_655 ?
N3 Cu3 N5 89.2(8) . 1_655 ?
N5 Cu3 N5 180.0 2_566 1_655 ?
O22 Sm1 O21 120.7(5) . . ?
O22 Sm1 O19 72.3(5) . . ?
O21 Sm1 O19 77.7(5) . . ?
O22 Sm1 O23 78.3(5) . . ?
O21 Sm1 O23 72.9(5) . . ?
O19 Sm1 O23 118.4(5) . . ?
O22 Sm1 O11 137.7(6) . 1_455 ?
O21 Sm1 O11 78.2(5) . 1_455 ?
O19 Sm1 O11 149.1(5) . 1_455 ?
O23 Sm1 O11 71.8(5) . 1_455 ?
O22 Sm1 O2W 89.9(7) . . ?
O21 Sm1 O2W 136.8(7) . . ?
O19 Sm1 O2W 84.8(7) . . ?
O23 Sm1 O2W 148.1(7) . . ?
O11 Sm1 O2W 99.9(7) 1_455 . ?
O22 Sm1 O3W 147.9(6) . . ?
O21 Sm1 O3W 69.7(5) . . ?
O19 Sm1 O3W 81.6(6) . . ?
O23 Sm1 O3W 132.0(5) . . ?
O11 Sm1 O3W 72.0(6) 1_455 . ?
O2W Sm1 O3W 68.9(7) . . ?
O22 Sm1 O1W 71.6(6) . . ?
O21 Sm1 O1W 143.8(6) . . ?
O19 Sm1 O1W 136.0(6) . . ?
O23 Sm1 O1W 77.5(6) . . ?
O11 Sm1 O1W 73.1(6) 1_455 . ?
O2W Sm1 O1W 70.7(8) . . ?
O3W Sm1 O1W 119.7(7) . . ?
O38 Si1 O39 111.9(9) . . ?
O38 Si1 O12 106.0(8) . . ?
O39 Si1 O12 108.1(7) . . ?
O38 Si1 O37 108.3(8) . . ?
O39 Si1 O37 112.8(8) . . ?
O12 Si1 O37 109.4(8) . . ?
W1 O1 Cu1 113.7(7) . . ?
W3 O3 Cu1 140.0(9) . 1_545 ?
W8 O8 Cu2 144.5(8) . 1_645 ?
W10 O10 Cu2 130.5(7) . 2_467 ?
W11 O11 Sm1 141.8(7) . 1_655 ?
Si1 O12 W11 127.3(7) . . ?
Si1 O12 W8 125.9(8) . . ?
W11 O12 W8 92.4(5) . . ?
Si1 O12 W9 120.2(8) . . ?
W11 O12 W9 91.1(5) . . ?
W8 O12 W9 89.1(4) . . ?
W4 O13 W5 116.9(8) . . ?
W2 O14 W4 123.5(9) . . ?
W5 O15 W2 125.4(8) . . ?
W4 O16 W9 154.1(10) . . ?
W5 O17 W6 156.0(8) . . ?
W1 O18 W2 141.2(7) . . ?
W2 O19 Sm1 157.4(8) . . ?
W9 O20 W3 153.0(9) . . ?
W3 O21 Sm1 136.6(7) . . ?
W1 O22 Sm1 158.0(9) . . ?
W10 O23 Sm1 136.6(8) . . ?
W3 O24 W10 118.5(7) . . ?
W8 O25 W10 149.8(9) . . ?
W9 O26 W8 122.8(7) . . ?
W7 O27 W8 147.1(8) . . ?
W7 O28 W1 120.5(8) . . ?
W6 O29 W1 119.9(7) . . ?
W11 O30 W9 123.0(9) . . ?
W6 O31 W7 121.8(7) . . ?
W11 O32 W6 151.7(10) . . ?
W10 O33 W7 157.2(9) . . ?
W11 O34 W5 152.0(12) . . ?
W3 O35 W4 151.6(9) . . ?
W11 O36 W8 118.7(7) . . ?
Si1 O37 W4 123.9(7) . . ?
Si1 O37 W2 120.9(7) . . ?
W4 O37 W2 92.7(5) . . ?
Si1 O37 W5 126.0(7) . . ?
W4 O37 W5 91.5(5) . . ?
W2 O37 W5 92.7(5) . . ?
Si1 O38 W1 123.8(8) . . ?
Si1 O38 W7 125.3(9) . . ?
W1 O38 W7 90.5(5) . . ?
Si1 O38 W6 126.6(9) . . ?
W1 O38 W6 91.0(5) . . ?
W7 O38 W6 88.7(5) . . ?
Si1 O39 W10 127.9(8) . . ?
Si1 O39 W3 127.7(9) . . ?
W10 O39 W3 93.9(5) . . ?
N1 C1 C2 122.4(19) . . ?
N2 C2 C1 120.3(18) . . ?
N2 C2 C3 117(2) . . ?
C1 C2 C3 123(2) . . ?
C2 C3 C4 109(2) . . ?
C5 C4 N4 120(2) . . ?
C5 C4 C3 123.0(19) . . ?
N4 C4 C3 117(2) . . ?
N1 C5 C4 123(2) . . ?
N3 C6 N2 108(2) . . ?
N3 C7 C8 108(2) . . ?
N2 C8 C7 104.2(19) . . ?
N4 C9 C10 103(3) . . ?
N5 C10 C9 113(3) . . ?
N5 C11 N4 109(2) . . ?
N6 C12 C13 121(2) . . ?
C12 C13 C14 120.1(19) . . ?
C12 C13 N9 120(2) . . ?
C14 C13 N9 120(2) . . ?
C15 C14 C13 117(2) . . ?
C14 C15 C16 122(2) . . ?
C14 C15 N7 119(2) . . ?
C16 C15 N7 119.3(18) . . ?
N6 C16 C15 120.5(18) . . ?
N7 C17 N8 110(2) . . ?
N7 C18 C19 106(2) . . ?
C18 C19 N8 107(2) . . ?
N9 C20 N10 110(2) . . ?
C22 C21 N9 102(2) . . ?
C21 C22 N10 112(2) . . ?
C1 N1 C5 120(2) . . ?
C1 N1 Cu1 118.9(14) . . ?
C5 N1 Cu1 121.1(16) . . ?
C8 N2 C6 107.7(19) . . ?
C8 N2 C2 127.0(17) . . ?
C6 N2 C2 125.2(19) . . ?
C6 N3 C7 111(2) . . ?
C6 N3 Cu3 123.7(15) . . ?
C7 N3 Cu3 122.6(19) . . ?
C9 N4 C11 109(2) . . ?
C9 N4 C4 125(2) . . ?
C11 N4 C4 126.2(18) . . ?
C11 N5 C10 106(2) . . ?
C11 N5 Cu3 125.9(17) . 1_455 ?
C10 N5 Cu3 128.5(18) . 1_455 ?
C12 N6 C16 120(2) . . ?
C12 N6 Cu1 119.3(16) . . ?
C16 N6 Cu1 120.8(13) . . ?
C17 N7 C18 111(2) . . ?
C17 N7 C15 126(2) . . ?
C18 N7 C15 123.4(19) . . ?
C17 N8 C19 106(2) . . ?
C17 N8 Cu2 130.1(16) . . ?
C19 N8 Cu2 123.7(18) . . ?
C20 N9 C21 110.9(18) . . ?
C20 N9 C13 125(2) . . ?
C21 N9 C13 124(2) . . ?
C20 N10 C22 104.7(19) . . ?
C20 N10 Cu2 124.3(16) . 1_655 ?
C22 N10 Cu2 131.0(16) . 1_655 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         4.344
_refine_diff_density_min         -5.425
_refine_diff_density_rms         0.760
_database_code_depnum_ccdc_archive 'CCDC 1005804'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ho

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H36 Cu5 Ho2 N20 O88 Si2 W22'
_chemical_formula_sum            'C44 H70 Cu5 Ho2 N20 O95 Si2 W22'
_chemical_formula_weight         7147.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4580(16)
_cell_length_b                   12.2630(18)
_cell_length_c                   24.833(4)
_cell_angle_alpha                94.768(2)
_cell_angle_beta                 100.812(2)
_cell_angle_gamma                114.139(2)
_cell_volume                     3077.5(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22381
_cell_measurement_theta_min      0.85
_cell_measurement_theta_max      28.41

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3169
_exptl_absorpt_coefficient_mu    22.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_T_max  0.003
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22381
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         0.85
_diffrn_reflns_theta_max         28.41
_reflns_number_total             15242
_reflns_number_gt                10876
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
During the refinement, the non-H atoms W, Si, Cu, Ho, C, N and O were 
refined anisotropically. Since most O atoms on the polyanion and lattice 
water molecules as well as some C and N atoms exhibit obvious ADP and
NPD problems with the anisotropic parameters, they are just refined 
isotropically. But this treatment didn't influence the precise of the 
polyanion structure and the final R values.
The restraint command 'isor' was employed to restrain several C, 0 and
N atoms so as to avoid the ADP and NPD problems on them. This command
led to a restraint number 162.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0776P)²+52.5738P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15242
_refine_ls_number_parameters     893
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1669
_refine_ls_wR_factor_gt          0.1436
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.15564(7) 0.02771(6) 0.74267(3) 0.01139(15) Uani 1 1 d . . .
W2 W 0.16963(7) 0.14340(6) 0.62805(3) 0.00960(14) Uani 1 1 d . . .
W3 W 0.30133(7) 0.54583(6) 0.73210(3) 0.01295(15) Uani 1 1 d . . .
W4 W 0.08201(7) 0.40217(6) 0.60925(3) 0.01158(15) Uani 1 1 d . . .
W5 W -0.18067(7) 0.09836(6) 0.60226(3) 0.01032(15) Uani 1 1 d . . .
W6 W -0.20050(8) -0.03388(6) 0.71634(3) 0.01399(16) Uani 1 1 d . . .
W7 W 0.03075(8) 0.14203(7) 0.85140(3) 0.01616(17) Uani 1 1 d . . .
W8 W -0.03071(8) 0.38679(7) 0.84094(3) 0.01535(16) Uani 1 1 d . . .
W9 W -0.01964(7) 0.51217(6) 0.71056(3) 0.01252(15) Uani 1 1 d . . .
W10 W 0.28413(8) 0.41494(7) 0.85742(3) 0.01692(17) Uani 1 1 d . . .
W11 W -0.27436(7) 0.20435(6) 0.70821(3) 0.01078(15) Uani 1 1 d . . .
Cu1 Cu 0.2850(2) -0.20152(18) 0.74284(9) 0.0126(4) Uani 1 1 d . . .
Cu2 Cu -0.3266(2) -0.1393(2) 0.47334(9) 0.0137(4) Uani 1 1 d . . .
Cu3 Cu 1.0000 0.0000 1.0000 0.0332(9) Uani 1 2 d S . .
Ho1 Ho 0.47150(10) 0.32030(9) 0.75224(4) 0.0201(2) Uani 0.95 1 d P . .
Ho1' Ho 0.374(2) 0.2916(16) 0.7499(7) 0.018(3) Uani 0.05 1 d PU . .
Si1 Si 0.0571(5) 0.2600(4) 0.72797(18) 0.0063(8) Uani 1 1 d . . .
O1 O 0.1549(13) -0.1108(11) 0.7541(5) 0.016(3) Uani 1 1 d . . .
O2 O 0.1821(12) 0.0825(10) 0.5631(5) 0.010(2) Uani 1 1 d U . .
O3 O 0.4218(14) 0.6918(12) 0.7408(6) 0.021(3) Uani 1 1 d . . .
O4 O 0.0788(16) 0.4327(13) 0.5443(5) 0.027(3) Uani 1 1 d . . .
O5 O -0.2670(14) 0.0351(11) 0.5347(5) 0.020(3) Uani 1 1 d . . .
O6 O -0.2974(15) -0.1756(13) 0.7214(7) 0.030(4) Uani 1 1 d . . .
O7 O 0.0098(16) 0.0543(14) 0.9030(6) 0.028(4) Uani 1 1 d . . .
O8 O -0.1079(16) 0.4422(15) 0.8821(6) 0.034(4) Uani 1 1 d . . .
O9 O -0.0918(13) 0.6088(12) 0.7093(6) 0.017(3) Uani 1 1 d . . .
O10 O 0.4070(16) 0.5068(14) 0.9144(6) 0.031(4) Uani 1 1 d . . .
O11 O 0.5756(12) 0.2100(11) 0.7112(5) 0.013(3) Uani 1 1 d U . .
O12 O 0.0952(11) 0.3884(10) 0.7058(5) 0.009(2) Uani 1 1 d . . .
O13 O -0.0870(12) 0.2605(10) 0.5950(5) 0.012(2) Uani 1 1 d U . .
O14 O 0.1555(14) 0.2900(11) 0.6106(6) 0.019(3) Uani 1 1 d . . .
O15 O -0.0325(13) 0.0746(11) 0.6072(6) 0.020(3) Uani 1 1 d . . .
O16 O -0.0061(13) 0.4924(11) 0.6351(5) 0.016(3) Uani 1 1 d . . .
O17 O -0.2509(13) -0.0438(10) 0.6375(5) 0.015(3) Uani 1 1 d U . .
O18 O 0.1406(12) 0.0031(10) 0.6631(5) 0.010(2) Uani 1 1 d . . .
O19 O 0.3391(13) 0.2231(11) 0.6589(5) 0.016(3) Uani 1 1 d . . .
O20 O 0.1619(14) 0.6179(10) 0.7318(5) 0.017(3) Uani 1 1 d . . .
O21 O 0.3854(13) 0.4538(11) 0.7256(6) 0.017(3) Uani 1 1 d . . .
O22 O 0.3313(13) 0.1185(12) 0.7599(5) 0.019(3) Uani 1 1 d . . .
O23 O 0.3597(14) 0.3482(12) 0.8206(6) 0.022(3) Uani 1 1 d . . .
O24 O 0.2866(14) 0.5236(12) 0.8051(6) 0.021(3) Uani 1 1 d U . .
O25 O 0.1440(13) 0.4636(12) 0.8780(6) 0.019(3) Uani 1 1 d . . .
O26 O -0.0057(12) 0.4871(11) 0.7882(5) 0.015(3) Uani 1 1 d U . .
O27 O -0.0487(14) 0.2409(12) 0.8731(6) 0.019(3) Uani 1 1 d . . .
O28 O 0.1253(14) 0.0830(11) 0.8102(5) 0.019(3) Uani 1 1 d . . .
O29 O -0.0453(14) -0.0407(12) 0.7158(6) 0.020(3) Uani 1 1 d . . .
O30 O -0.1768(13) 0.3618(10) 0.6921(5) 0.014(3) Uani 1 1 d . . .
O31 O -0.1212(13) 0.0440(11) 0.7936(5) 0.017(3) Uani 1 1 d U . .
O32 O -0.3202(13) 0.0458(11) 0.7221(5) 0.015(3) Uani 1 1 d U . .
O33 O 0.1990(16) 0.2719(13) 0.8901(6) 0.030(3) Uani 1 1 d . . .
O34 O -0.3094(13) 0.1461(11) 0.6288(5) 0.016(3) Uani 1 1 d . . .
O35 O 0.2443(14) 0.5252(11) 0.6516(6) 0.022(3) Uani 1 1 d . . .
O36 O -0.1840(13) 0.2677(11) 0.7809(5) 0.017(3) Uani 1 1 d . . .
O37 O 0.0795(12) 0.2900(10) 0.7963(5) 0.011(2) Uani 1 1 d U . .
O38 O 0.1459(13) 0.1955(11) 0.7120(5) 0.013(3) Uani 1 1 d U . .
O39 O -0.0999(12) 0.1682(10) 0.6997(5) 0.012(2) Uani 1 1 d . . .
O1W O 0.660(2) 0.4937(17) 0.8142(9) 0.075(7) Uani 1 1 d . . .
O2W O 0.6045(16) 0.4468(14) 0.6896(7) 0.034(4) Uani 1 1 d . . .
O3W O 0.5829(18) 0.2644(17) 0.8325(7) 0.044(5) Uani 1 1 d . . .
O4W O 0.4444(14) -0.0379(11) 0.7526(7) 0.027(3) Uani 1 1 d . . .
O5W O -0.4240(14) -0.0907(14) 0.4105(6) 0.027(3) Uani 1 1 d . . .
O6W O 0.387(4) 0.122(5) 0.9010(16) 0.075(15) Uani 0.50 1 d P . .
O7W O 0.5241(19) 0.6041(17) 0.6391(9) 0.057(6) Uani 1 1 d . . .
O8W O 0.672(3) 0.085(3) 0.8574(12) 0.093(9) Uani 1 1 d . . .
O9W O 0.842(3) 0.714(3) 0.8007(13) 0.029(7) Uani 0.50 1 d PU . .
O10W O 0.600(6) 0.393(5) 0.937(2) 0.10(2) Uani 0.50 1 d P . .
N1 N 0.3293(17) -0.1952(14) 0.8238(6) 0.017(3) Uani 1 1 d . . .
N2 N 0.602(2) -0.1907(17) 0.9299(10) 0.042(6) Uani 1 1 d . . .
N3 N 0.8121(19) -0.1220(18) 0.9669(8) 0.030(4) Uani 1 1 d . . .
N4 N 0.184(2) -0.1978(18) 0.9419(7) 0.029(5) Uani 1 1 d . . .
N5 N 0.0608(19) -0.1242(17) 0.9785(8) 0.030(4) Uani 1 1 d U . .
N6 N 0.2343(15) -0.2129(13) 0.6603(6) 0.013(3) Uani 1 1 d U . .
N7 N -0.0654(15) -0.2464(12) 0.5636(6) 0.011(3) Uani 1 1 d . . .
N8 N -0.2274(17) -0.2117(14) 0.5200(6) 0.017(3) Uani 1 1 d . . .
N9 N 0.3423(15) -0.2501(14) 0.5319(7) 0.017(3) Uani 1 1 d U . .
N10 N 0.5064(18) -0.2203(16) 0.4960(7) 0.024(4) Uani 1 1 d . . .
C1 C 0.448(2) -0.1892(18) 0.8509(8) 0.023(4) Uani 1 1 d . . .
H1 H 0.5105 -0.1801 0.8305 0.027 Uiso 1 1 calc R B .
C2 C 0.479(2) -0.1955(17) 0.9044(9) 0.023(4) Uani 1 1 d . . .
C3 C 0.392(2) -0.2020(17) 0.9389(8) 0.020(4) Uani 1 1 d U . .
H3 H 0.4118 -0.2057 0.9766 0.024 Uiso 1 1 calc R B .
C4 C 0.273(2) -0.2025(19) 0.9116(9) 0.025(5) Uani 1 1 d . . .
C5 C 0.240(2) -0.2063(18) 0.8560(8) 0.024(5) Uani 1 1 d . . .
H5 H 0.1556 -0.2166 0.8391 0.028 Uiso 1 1 calc R B .
C6 C 0.469(2) -0.177(2) 0.5348(9) 0.025(5) Uani 1 1 d . . .
H6 H 0.5211 -0.1060 0.5607 0.030 Uiso 1 1 calc R . .
C7 C 0.715(4) -0.107(3) 0.9462(15) 0.069(9) Uani 1 1 d U B .
H7 H 0.7269 -0.0288 0.9425 0.083 Uiso 1 1 calc R A 1
C8 C 0.304(3) -0.3439(19) 0.4904(10) 0.036(6) Uani 1 1 d . . .
H8 H 0.2237 -0.4124 0.4810 0.043 Uiso 1 1 calc R . .
C9 C 0.140(3) -0.267(3) 0.9825(11) 0.046(7) Uiso 1 1 d . . .
H9 H 0.1564 -0.3319 0.9925 0.055 Uiso 1 1 calc R . .
C10 C 0.070(4) -0.218(3) 1.0035(15) 0.071(10) Uani 1 1 d U . .
H10 H 0.0314 -0.2447 1.0325 0.085 Uiso 1 1 calc R . .
C11 C 0.136(2) -0.1135(19) 0.9416(9) 0.029(5) Uani 1 1 d U . .
H11 H 0.1531 -0.0552 0.9188 0.035 Uiso 1 1 calc R . .
C12 C 0.313(2) -0.2191(17) 0.6262(8) 0.017(4) Uani 1 1 d . . .
H12 H 0.3986 -0.2099 0.6402 0.021 Uiso 1 1 calc R . .
C13 C 0.2603(19) -0.2393(15) 0.5716(8) 0.016(4) Uani 1 1 d U . .
C14 C 0.138(2) -0.2426(18) 0.5462(8) 0.020(4) Uani 1 1 d U . .
H14 H 0.1098 -0.2466 0.5081 0.024 Uiso 1 1 calc R . .
C15 C 0.064(2) -0.2395(16) 0.5833(8) 0.018(4) Uani 1 1 d . . .
C16 C 0.1088(19) -0.2298(14) 0.6386(8) 0.017(4) Uani 1 1 d . . .
H16 H 0.0531 -0.2348 0.6621 0.020 Uiso 1 1 calc R . .
C17 C -0.105(2) -0.1876(17) 0.5256(8) 0.020(4) Uani 1 1 d U . .
H17 H -0.0506 -0.1364 0.5060 0.024 Uiso 1 1 calc R . .
C18 C -0.168(3) -0.310(2) 0.5853(10) 0.040(6) Uani 1 1 d . . .
H18 H -0.1695 -0.3561 0.6133 0.048 Uiso 1 1 calc R . .
C19 C -0.270(3) -0.290(2) 0.5558(10) 0.044(7) Uani 1 1 d . . .
H19 H -0.3558 -0.3245 0.5597 0.053 Uiso 1 1 calc R . .
C20 C 0.761(5) -0.214(4) 0.9909(19) 0.034(11) Uani 0.50 1 d P B 1
H20 H 0.8064 -0.2422 1.0166 0.041 Uiso 0.50 1 calc PR B 1
C20' C 0.792(10) -0.201(8) 0.914(4) 0.11(3) Uani 0.50 1 d PU B 2
H20' H 0.8549 -0.2125 0.8982 0.130 Uiso 0.50 1 calc PR B 2
C21 C 0.635(6) -0.258(5) 0.973(2) 0.043(12) Uani 0.50 1 d PU B 1
H21 H 0.5739 -0.3218 0.9849 0.051 Uiso 0.50 1 calc PR B 1
C21' C 0.648(6) -0.257(6) 0.893(3) 0.055(15) Uani 0.50 1 d PU B 2
H21' H 0.5975 -0.3194 0.8626 0.066 Uiso 0.50 1 calc PR B 2
C22 C 0.407(2) -0.320(2) 0.4640(11) 0.044(7) Uani 1 1 d . . .
H22 H 0.4061 -0.3644 0.4315 0.053 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
W1 O1 1.742(12) . ?
W1 O22 1.800(14) . ?
W1 O28 1.902(12) . ?
W1 O18 1.937(11) . ?
W1 O29 2.050(14) . ?
W1 O38 2.289(12) . ?
W1 Ho1' 3.144(19) . ?
W2 O19 1.754(13) . ?
W2 O2 1.775(11) . ?
W2 O18 1.929(11) . ?
W2 O14 1.945(12) . ?
W2 O15 2.055(14) . ?
W2 O38 2.227(11) . ?
W2 Ho1' 3.302(19) . ?
W3 O3 1.720(14) . ?
W3 O21 1.773(12) . ?
W3 O24 1.885(14) . ?
W3 O35 1.943(14) . ?
W3 O20 2.118(13) . ?
W3 O12 2.283(12) . ?
W3 Ho1' 3.583(18) . ?
W4 O4 1.683(14) . ?
W4 O35 1.884(13) . ?
W4 O14 1.884(12) . ?
W4 O16 1.922(12) . ?
W4 O13 1.945(12) . ?
W4 O12 2.399(12) . ?
W5 O5 1.711(13) . ?
W5 O15 1.821(14) . ?
W5 O13 1.877(12) . ?
W5 O17 1.955(12) . ?
W5 O34 1.990(12) . ?
W5 O39 2.368(12) . ?
W6 O6 1.667(14) . ?
W6 O29 1.817(13) . ?
W6 O17 1.914(13) . ?
W6 O31 1.936(13) . ?
W6 O32 2.000(12) . ?
W6 O39 2.378(11) . ?
W7 O7 1.729(13) . ?
W7 O27 1.889(12) . ?
W7 O31 1.898(14) . ?
W7 O28 1.917(12) . ?
W7 O33 1.927(16) . ?
W7 O37 2.313(11) . ?
W8 O8 1.733(15) . ?
W8 O25 1.834(13) . ?
W8 O26 1.853(13) . ?
W8 O27 1.970(12) . ?
W8 O36 2.000(15) . ?
W8 O37 2.402(12) . ?
W9 O9 1.699(13) . ?
W9 O20 1.885(14) . ?
W9 O16 1.912(12) . ?
W9 O30 1.920(13) . ?
W9 O26 1.964(13) . ?
W9 O12 2.390(11) . ?
W10 O10 1.716(15) . ?
W10 O23 1.734(12) . ?
W10 O24 1.932(14) . ?
W10 O33 1.955(15) . ?
W10 O25 2.059(12) . ?
W10 O37 2.343(13) . ?
W10 Ho1' 3.481(17) . ?
W11 O11 1.763(12) 1_455 ?
W11 O36 1.827(14) . ?
W11 O32 1.876(12) . ?
W11 O30 1.915(11) . ?
W11 O34 1.947(12) . ?
W11 O39 2.259(12) . ?
Cu1 N1 1.967(15) . ?
Cu1 N6 1.999(15) . ?
Cu1 O20 2.041(12) 1_545 ?
Cu1 O4W 2.043(14) . ?
Cu1 O1 2.235(12) . ?
Cu1 O3 2.422(13) 1_545 ?
Cu2 O2 1.942(12) 2_556 ?
Cu2 N10 1.977(18) 1_455 ?
Cu2 N8 1.982(16) . ?
Cu2 O5W 2.021(14) . ?
Cu2 O5 2.289(13) . ?
Cu3 N5 1.991(18) 1_655 ?
Cu3 N5 1.991(18) 2_657 ?
Cu3 N3 2.01(2) 2_757 ?
Cu3 N3 2.01(2) . ?
Ho1 Ho1' 1.01(2) . ?
Ho1 O21 2.312(12) . ?
Ho1 O22 2.384(14) . ?
Ho1 O23 2.391(12) . ?
Ho1 O19 2.416(13) . ?
Ho1 O11 2.417(12) . ?
Ho1 O1W 2.451(19) . ?
Ho1 O3W 2.461(16) . ?
Ho1 O2W 2.551(14) . ?
Ho1' O23 1.90(2) . ?
Ho1' O22 2.02(2) . ?
Ho1' O21 2.09(2) . ?
Ho1' O19 2.25(2) . ?
Ho1' O38 2.34(2) . ?
Si1 O38 1.606(12) . ?
Si1 O12 1.626(12) . ?
Si1 O37 1.653(12) . ?
Si1 O39 1.653(13) . ?
O2 Cu2 1.942(11) 2_556 ?
O3 Cu1 2.422(13) 1_565 ?
O11 W11 1.763(12) 1_655 ?
O20 Cu1 2.041(12) 1_565 ?
N1 C1 1.37(3) . ?
N1 C5 1.38(2) . ?
N2 C7 1.24(4) . ?
N2 C2 1.41(3) . ?
N2 C21' 1.48(6) . ?
N2 C21 1.48(5) . ?
N3 C7 1.22(4) . ?
N3 C20 1.29(5) . ?
N3 C20' 1.49(10) . ?
N4 C11 1.36(3) . ?
N4 C4 1.39(2) . ?
N4 C9 1.41(3) . ?
N5 C11 1.35(3) . ?
N5 C10 1.39(4) . ?
N5 Cu3 1.991(18) 1_455 ?
N6 C16 1.36(2) . ?
N6 C12 1.37(2) . ?
N7 C17 1.35(2) . ?
N7 C18 1.36(3) . ?
N7 C15 1.44(2) . ?
N8 C17 1.29(2) . ?
N8 C19 1.36(3) . ?
N9 C8 1.34(2) . ?
N9 C6 1.34(2) . ?
N9 C13 1.52(2) . ?
N10 C6 1.29(2) . ?
N10 C22 1.34(3) . ?
N10 Cu2 1.977(18) 1_655 ?
C1 C2 1.33(3) . ?
C2 C3 1.42(3) . ?
C3 C4 1.40(3) . ?
C4 C5 1.35(3) . ?
C7 C20' 1.92(10) . ?
C7 C21 1.93(7) . ?
C7 C21' 1.94(7) . ?
C7 C20 1.95(6) . ?
C8 C22 1.39(3) . ?
C9 C10 1.33(4) . ?
C12 C13 1.34(3) . ?
C13 C14 1.41(3) . ?
C14 C15 1.37(2) . ?
C15 C16 1.35(3) . ?
C18 C19 1.38(4) . ?
C20 C21 1.28(7) . ?
C20' C21' 1.47(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 O22 98.4(6) . . ?
O1 W1 O28 101.7(5) . . ?
O22 W1 O28 96.9(6) . . ?
O1 W1 O18 97.4(5) . . ?
O22 W1 O18 94.1(6) . . ?
O28 W1 O18 156.3(5) . . ?
O1 W1 O29 94.8(6) . . ?
O22 W1 O29 166.5(5) . . ?
O28 W1 O29 83.1(6) . . ?
O18 W1 O29 81.4(5) . . ?
O1 W1 O38 170.3(5) . . ?
O22 W1 O38 84.6(5) . . ?
O28 W1 O38 87.1(5) . . ?
O18 W1 O38 73.1(4) . . ?
O29 W1 O38 82.0(5) . . ?
O1 W1 Ho1' 135.4(6) . . ?
O22 W1 Ho1' 37.0(5) . . ?
O28 W1 Ho1' 88.5(5) . . ?
O18 W1 Ho1' 87.7(5) . . ?
O29 W1 Ho1' 129.7(5) . . ?
O38 W1 Ho1' 48.0(5) . . ?
O19 W2 O2 97.5(6) . . ?
O19 W2 O18 96.6(5) . . ?
O2 W2 O18 97.9(5) . . ?
O19 W2 O14 92.5(6) . . ?
O2 W2 O14 100.8(5) . . ?
O18 W2 O14 158.0(5) . . ?
O19 W2 O15 166.5(5) . . ?
O2 W2 O15 95.6(5) . . ?
O18 W2 O15 84.8(5) . . ?
O14 W2 O15 81.8(6) . . ?
O19 W2 O38 84.6(5) . . ?
O2 W2 O38 172.5(5) . . ?
O18 W2 O38 74.8(4) . . ?
O14 W2 O38 86.2(5) . . ?
O15 W2 O38 82.8(5) . . ?
O19 W2 Ho1' 39.5(5) . . ?
O2 W2 Ho1' 136.2(5) . . ?
O18 W2 Ho1' 83.4(5) . . ?
O14 W2 Ho1' 91.2(5) . . ?
O15 W2 Ho1' 127.9(5) . . ?
O38 W2 Ho1' 45.2(5) . . ?
O3 W3 O21 104.2(6) . . ?
O3 W3 O24 103.9(6) . . ?
O21 W3 O24 94.9(6) . . ?
O3 W3 O35 95.5(6) . . ?
O21 W3 O35 91.2(6) . . ?
O24 W3 O35 157.5(6) . . ?
O3 W3 O20 88.4(6) . . ?
O21 W3 O20 166.8(6) . . ?
O24 W3 O20 85.6(5) . . ?
O35 W3 O20 83.7(5) . . ?
O3 W3 O12 158.0(5) . . ?
O21 W3 O12 95.1(5) . . ?
O24 W3 O12 84.6(5) . . ?
O35 W3 O12 73.3(5) . . ?
O20 W3 O12 71.8(4) . . ?
O3 W3 Ho1' 122.8(6) . . ?
O21 W3 Ho1' 23.8(5) . . ?
O24 W3 Ho1' 76.3(4) . . ?
O35 W3 Ho1' 102.7(5) . . ?
O20 W3 Ho1' 146.6(5) . . ?
O12 W3 Ho1' 78.7(4) . . ?
O4 W4 O35 103.2(7) . . ?
O4 W4 O14 102.4(6) . . ?
O35 W4 O14 90.1(6) . . ?
O4 W4 O16 100.5(6) . . ?
O35 W4 O16 89.3(6) . . ?
O14 W4 O16 156.6(5) . . ?
O4 W4 O13 99.7(6) . . ?
O35 W4 O13 157.2(6) . . ?
O14 W4 O13 85.5(6) . . ?
O16 W4 O13 86.1(5) . . ?
O4 W4 O12 171.9(5) . . ?
O35 W4 O12 71.5(5) . . ?
O14 W4 O12 83.9(5) . . ?
O16 W4 O12 73.8(5) . . ?
O13 W4 O12 85.7(4) . . ?
O5 W5 O15 103.2(6) . . ?
O5 W5 O13 100.5(6) . . ?
O15 W5 O13 90.4(6) . . ?
O5 W5 O17 99.6(6) . . ?
O15 W5 O17 87.7(6) . . ?
O13 W5 O17 159.7(5) . . ?
O5 W5 O34 99.3(6) . . ?
O15 W5 O34 157.3(6) . . ?
O13 W5 O34 88.1(5) . . ?
O17 W5 O34 85.9(5) . . ?
O5 W5 O39 169.3(5) . . ?
O15 W5 O39 84.8(5) . . ?
O13 W5 O39 86.3(5) . . ?
O17 W5 O39 73.4(5) . . ?
O34 W5 O39 72.5(5) . . ?
O6 W6 O29 102.4(7) . . ?
O6 W6 O17 99.7(7) . . ?
O29 W6 O17 94.7(6) . . ?
O6 W6 O31 102.6(7) . . ?
O29 W6 O31 86.4(6) . . ?
O17 W6 O31 157.0(5) . . ?
O6 W6 O32 100.7(6) . . ?
O29 W6 O32 156.4(6) . . ?
O17 W6 O32 86.6(5) . . ?
O31 W6 O32 83.5(5) . . ?
O6 W6 O39 169.1(6) . . ?
O29 W6 O39 87.0(5) . . ?
O17 W6 O39 73.9(5) . . ?
O31 W6 O39 83.3(5) . . ?
O32 W6 O39 70.6(4) . . ?
O7 W7 O27 99.1(6) . . ?
O7 W7 O31 101.6(7) . . ?
O27 W7 O31 91.6(6) . . ?
O7 W7 O28 102.3(6) . . ?
O27 W7 O28 158.5(5) . . ?
O31 W7 O28 86.3(6) . . ?
O7 W7 O33 97.6(7) . . ?
O27 W7 O33 87.9(6) . . ?
O31 W7 O33 160.6(6) . . ?
O28 W7 O33 87.1(6) . . ?
O7 W7 O37 169.2(6) . . ?
O27 W7 O37 75.2(5) . . ?
O31 W7 O37 87.9(5) . . ?
O28 W7 O37 83.4(5) . . ?
O33 W7 O37 73.2(5) . . ?
O8 W8 O25 104.0(7) . . ?
O8 W8 O26 102.5(7) . . ?
O25 W8 O26 92.4(6) . . ?
O8 W8 O27 98.9(7) . . ?
O25 W8 O27 90.1(6) . . ?
O26 W8 O27 157.2(5) . . ?
O8 W8 O36 101.8(6) . . ?
O25 W8 O36 154.2(5) . . ?
O26 W8 O36 84.6(5) . . ?
O27 W8 O36 83.4(6) . . ?
O8 W8 O37 170.1(6) . . ?
O25 W8 O37 73.5(5) . . ?
O26 W8 O37 87.3(4) . . ?
O27 W8 O37 71.7(4) . . ?
O36 W8 O37 80.7(5) . . ?
O9 W9 O20 103.1(6) . . ?
O9 W9 O16 101.1(6) . . ?
O20 W9 O16 88.8(5) . . ?
O9 W9 O30 98.3(6) . . ?
O20 W9 O30 158.5(5) . . ?
O16 W9 O30 89.3(5) . . ?
O9 W9 O26 100.8(5) . . ?
O20 W9 O26 87.5(5) . . ?
O16 W9 O26 158.1(5) . . ?
O30 W9 O26 86.4(5) . . ?
O9 W9 O12 173.9(5) . . ?
O20 W9 O12 73.3(5) . . ?
O16 W9 O12 74.2(5) . . ?
O30 W9 O12 85.6(4) . . ?
O26 W9 O12 84.1(4) . . ?
O10 W10 O23 104.2(7) . . ?
O10 W10 O24 103.6(7) . . ?
O23 W10 O24 91.9(6) . . ?
O10 W10 O33 99.7(7) . . ?
O23 W10 O33 93.9(6) . . ?
O24 W10 O33 153.8(6) . . ?
O10 W10 O25 94.8(6) . . ?
O23 W10 O25 160.9(6) . . ?
O24 W10 O25 81.8(5) . . ?
O33 W10 O25 84.4(6) . . ?
O10 W10 O37 164.2(6) . . ?
O23 W10 O37 90.1(6) . . ?
O24 W10 O37 82.4(5) . . ?
O33 W10 O37 72.1(5) . . ?
O25 W10 O37 71.3(5) . . ?
O10 W10 Ho1' 117.7(6) . . ?
O23 W10 Ho1' 17.2(6) . . ?
O24 W10 Ho1' 78.6(5) . . ?
O33 W10 Ho1' 101.1(5) . . ?
O25 W10 Ho1' 145.1(5) . . ?
O37 W10 Ho1' 77.7(4) . . ?
O11 W11 O36 99.3(6) 1_455 . ?
O11 W11 O32 97.5(6) 1_455 . ?
O36 W11 O32 91.0(5) . . ?
O11 W11 O30 101.0(5) 1_455 . ?
O36 W11 O30 86.7(6) . . ?
O32 W11 O30 161.5(5) . . ?
O11 W11 O34 100.2(6) 1_455 . ?
O36 W11 O34 160.0(5) . . ?
O32 W11 O34 90.3(5) . . ?
O30 W11 O34 85.7(5) . . ?
O11 W11 O39 171.7(5) 1_455 . ?
O36 W11 O39 85.3(5) . . ?
O32 W11 O39 75.5(5) . . ?
O30 W11 O39 86.0(5) . . ?
O34 W11 O39 75.8(5) . . ?
N1 Cu1 N6 178.1(7) . . ?
N1 Cu1 O20 90.1(6) . 1_545 ?
N6 Cu1 O20 88.2(6) . 1_545 ?
N1 Cu1 O4W 89.3(7) . . ?
N6 Cu1 O4W 92.6(6) . . ?
O20 Cu1 O4W 164.8(5) 1_545 . ?
N1 Cu1 O1 89.3(6) . . ?
N6 Cu1 O1 90.4(5) . . ?
O20 Cu1 O1 103.6(5) 1_545 . ?
O4W Cu1 O1 91.6(5) . . ?
N1 Cu1 O3 84.6(6) . 1_545 ?
N6 Cu1 O3 95.6(5) . 1_545 ?
O20 Cu1 O3 73.6(5) 1_545 1_545 ?
O4W Cu1 O3 91.2(5) . 1_545 ?
O1 Cu1 O3 173.2(5) . 1_545 ?
O2 Cu2 N10 168.4(6) 2_556 1_455 ?
O2 Cu2 N8 87.2(6) 2_556 . ?
N10 Cu2 N8 96.4(7) 1_455 . ?
O2 Cu2 O5W 85.2(6) 2_556 . ?
N10 Cu2 O5W 88.9(7) 1_455 . ?
N8 Cu2 O5W 166.1(6) . . ?
O2 Cu2 O5 98.9(5) 2_556 . ?
N10 Cu2 O5 91.5(6) 1_455 . ?
N8 Cu2 O5 98.5(5) . . ?
O5W Cu2 O5 94.2(5) . . ?
N5 Cu3 N5 180.0 1_655 2_657 ?
N5 Cu3 N3 90.4(8) 1_655 2_757 ?
N5 Cu3 N3 89.6(8) 2_657 2_757 ?
N5 Cu3 N3 89.6(8) 1_655 . ?
N5 Cu3 N3 90.4(8) 2_657 . ?
N3 Cu3 N3 180.000 2_757 . ?
Ho1' Ho1 O21 64.5(10) . . ?
Ho1' Ho1 O22 57.1(10) . . ?
O21 Ho1 O22 121.0(4) . . ?
Ho1' Ho1 O23 49.3(11) . . ?
O21 Ho1 O23 72.8(4) . . ?
O22 Ho1 O23 76.2(5) . . ?
Ho1' Ho1 O19 68.2(10) . . ?
O21 Ho1 O19 77.1(4) . . ?
O22 Ho1 O19 74.6(4) . . ?
O23 Ho1 O19 117.3(5) . . ?
Ho1' Ho1 O11 127.2(10) . . ?
O21 Ho1 O11 136.3(4) . . ?
O22 Ho1 O11 79.8(4) . . ?
O23 Ho1 O11 150.0(4) . . ?
O19 Ho1 O11 72.3(4) . . ?
Ho1' Ho1 O1W 129.1(12) . . ?
O21 Ho1 O1W 87.9(7) . . ?
O22 Ho1 O1W 135.8(6) . . ?
O23 Ho1 O1W 82.9(7) . . ?
O19 Ho1 O1W 148.9(6) . . ?
O11 Ho1 O1W 102.6(7) . . ?
Ho1' Ho1 O3W 112.2(11) . . ?
O21 Ho1 O3W 144.1(6) . . ?
O22 Ho1 O3W 71.7(5) . . ?
O23 Ho1 O3W 79.3(5) . . ?
O19 Ho1 O3W 137.1(5) . . ?
O11 Ho1 O3W 76.2(5) . . ?
O1W Ho1 O3W 66.3(7) . . ?
Ho1' Ho1 O2W 127.7(11) . . ?
O21 Ho1 O2W 71.5(4) . . ?
O22 Ho1 O2W 143.5(5) . . ?
O23 Ho1 O2W 137.5(5) . . ?
O19 Ho1 O2W 75.8(5) . . ?
O11 Ho1 O2W 71.2(4) . . ?
O1W Ho1 O2W 73.6(7) . . ?
O3W Ho1 O2W 120.0(6) . . ?
Ho1 Ho1' O23 106.8(14) . . ?
Ho1 Ho1' O22 98.1(13) . . ?
O23 Ho1' O22 97.5(9) . . ?
Ho1 Ho1' O21 89.6(12) . . ?
O23 Ho1' O21 88.8(9) . . ?
O22 Ho1' O21 168.2(12) . . ?
Ho1 Ho1' O19 87.1(11) . . ?
O23 Ho1' O19 165.0(12) . . ?
O22 Ho1' O19 85.8(8) . . ?
O21 Ho1' O19 85.7(8) . . ?
Ho1 Ho1' O38 159.1(14) . . ?
O23 Ho1' O38 94.1(9) . . ?
O22 Ho1' O38 78.5(8) . . ?
O21 Ho1' O38 91.1(9) . . ?
O19 Ho1' O38 72.1(7) . . ?
Ho1 Ho1' W1 129.5(12) . . ?
O23 Ho1' W1 93.4(8) . . ?
O22 Ho1' W1 32.4(5) . . ?
O21 Ho1' W1 137.7(9) . . ?
O19 Ho1' W1 81.5(6) . . ?
O38 Ho1' W1 46.5(4) . . ?
Ho1 Ho1' W2 116.8(12) . . ?
O23 Ho1' W2 136.3(10) . . ?
O22 Ho1' W2 79.7(7) . . ?
O21 Ho1' W2 88.9(7) . . ?
O19 Ho1' W2 29.8(4) . . ?
O38 Ho1' W2 42.4(4) . . ?
W1 Ho1' W2 61.2(3) . . ?
Ho1 Ho1' W10 117.8(12) . . ?
O23 Ho1' W10 15.7(5) . . ?
O22 Ho1' W10 105.7(7) . . ?
O21 Ho1' W10 78.3(6) . . ?
O19 Ho1' W10 149.8(9) . . ?
O38 Ho1' W10 82.7(6) . . ?
W1 Ho1' W10 93.4(5) . . ?
W2 Ho1' W10 123.5(6) . . ?
Ho1 Ho1' W3 107.0(11) . . ?
O23 Ho1' W3 74.6(7) . . ?
O22 Ho1' W3 154.9(9) . . ?
O21 Ho1' W3 20.1(4) . . ?
O19 Ho1' W3 96.3(6) . . ?
O38 Ho1' W3 78.3(6) . . ?
W1 Ho1' W3 123.0(6) . . ?
W2 Ho1' W3 89.8(4) . . ?
W10 Ho1' W3 61.6(3) . . ?
O38 Si1 O12 111.2(6) . . ?
O38 Si1 O37 111.0(6) . . ?
O12 Si1 O37 107.1(6) . . ?
O38 Si1 O39 108.9(7) . . ?
O12 Si1 O39 109.5(6) . . ?
O37 Si1 O39 109.1(6) . . ?
W1 O1 Cu1 134.6(7) . . ?
W2 O2 Cu2 129.7(7) . 2_556 ?
W3 O3 Cu1 98.5(6) . 1_565 ?
W5 O5 Cu2 138.1(7) . . ?
W11 O11 Ho1 146.1(7) 1_655 . ?
Si1 O12 W3 123.4(6) . . ?
Si1 O12 W9 125.1(6) . . ?
W3 O12 W9 95.5(4) . . ?
Si1 O12 W4 122.4(6) . . ?
W3 O12 W4 91.9(4) . . ?
W9 O12 W4 89.3(4) . . ?
W5 O13 W4 147.9(7) . . ?
W4 O14 W2 154.9(8) . . ?
W5 O15 W2 149.5(7) . . ?
W9 O16 W4 122.8(7) . . ?
W6 O17 W5 121.7(6) . . ?
W2 O18 W1 116.4(6) . . ?
W2 O19 Ho1' 110.7(8) . . ?
W2 O19 Ho1 135.2(7) . . ?
Ho1' O19 Ho1 24.7(5) . . ?
W9 O20 Cu1 139.9(7) . 1_565 ?
W9 O20 W3 119.4(6) . . ?
Cu1 O20 W3 99.4(6) 1_565 . ?
W3 O21 Ho1' 136.1(9) . . ?
W3 O21 Ho1 155.9(7) . . ?
Ho1' O21 Ho1 25.9(6) . . ?
W1 O22 Ho1' 110.6(8) . . ?
W1 O22 Ho1 134.6(6) . . ?
Ho1' O22 Ho1 24.8(6) . . ?
W10 O23 Ho1' 147.1(10) . . ?
W10 O23 Ho1 158.0(7) . . ?
Ho1' O23 Ho1 23.8(6) . . ?
W3 O24 W10 143.0(7) . . ?
W8 O25 W10 122.9(7) . . ?
W8 O26 W9 151.4(7) . . ?
W7 O27 W8 121.7(6) . . ?
W1 O28 W7 152.5(8) . . ?
W6 O29 W1 151.5(7) . . ?
W11 O30 W9 149.0(7) . . ?
W7 O31 W6 149.9(7) . . ?
W11 O32 W6 120.6(6) . . ?
W7 O33 W10 121.4(8) . . ?
W11 O34 W5 118.0(7) . . ?
W4 O35 W3 123.2(7) . . ?
W11 O36 W8 153.4(7) . . ?
Si1 O37 W7 123.5(6) . . ?
Si1 O37 W10 123.7(6) . . ?
W7 O37 W10 93.3(4) . . ?
Si1 O37 W8 123.7(6) . . ?
W7 O37 W8 91.2(4) . . ?
W10 O37 W8 92.3(4) . . ?
Si1 O38 W2 128.4(7) . . ?
Si1 O38 W1 126.3(7) . . ?
W2 O38 W1 93.3(4) . . ?
Si1 O38 Ho1' 119.1(8) . . ?
W2 O38 Ho1' 92.5(6) . . ?
W1 O38 Ho1' 85.5(6) . . ?
Si1 O39 W11 126.2(6) . . ?
Si1 O39 W5 121.7(6) . . ?
W11 O39 W5 93.7(5) . . ?
Si1 O39 W6 122.3(7) . . ?
W11 O39 W6 93.1(4) . . ?
W5 O39 W6 90.7(4) . . ?
C1 N1 C5 116.0(17) . . ?
C1 N1 Cu1 121.3(12) . . ?
C5 N1 Cu1 122.5(14) . . ?
C7 N2 C2 133(2) . . ?
C7 N2 C21' 91(3) . . ?
C2 N2 C21' 112(3) . . ?
C7 N2 C21 90(3) . . ?
C2 N2 C21 130(3) . . ?
C21' N2 C21 86(3) . . ?
C7 N3 C20 101(3) . . ?
C7 N3 C20' 90(4) . . ?
C20 N3 C20' 93(4) . . ?
C7 N3 Cu3 130(2) . . ?
C20 N3 Cu3 119(2) . . ?
C20' N3 Cu3 114(4) . . ?
C11 N4 C4 124.6(18) . . ?
C11 N4 C9 107.3(18) . . ?
C4 N4 C9 127.7(19) . . ?
C11 N5 C10 102(2) . . ?
C11 N5 Cu3 123.6(15) . 1_455 ?
C10 N5 Cu3 132.2(18) . 1_455 ?
C16 N6 C12 120.7(16) . . ?
C16 N6 Cu1 115.9(12) . . ?
C12 N6 Cu1 122.9(13) . . ?
C17 N7 C18 108.8(17) . . ?
C17 N7 C15 128.5(16) . . ?
C18 N7 C15 122.5(17) . . ?
C17 N8 C19 105.4(19) . . ?
C17 N8 Cu2 126.4(13) . . ?
C19 N8 Cu2 128.1(17) . . ?
C8 N9 C6 107.0(17) . . ?
C8 N9 C13 125.2(16) . . ?
C6 N9 C13 127.4(17) . . ?
C6 N10 C22 111.0(19) . . ?
C6 N10 Cu2 126.8(15) . 1_655 ?
C22 N10 Cu2 120.9(14) . 1_655 ?
C2 C1 N1 124.3(19) . . ?
C1 C2 N2 122(2) . . ?
C1 C2 C3 120.9(19) . . ?
N2 C2 C3 117(2) . . ?
C4 C3 C2 114.5(19) . . ?
C5 C4 N4 117(2) . . ?
C5 C4 C3 122.7(19) . . ?
N4 C4 C3 120(2) . . ?
C4 C5 N1 121(2) . . ?
N10 C6 N9 109(2) . . ?
N3 C7 N2 124(3) . . ?
N3 C7 C20' 51(3) . . ?
N2 C7 C20' 93(4) . . ?
N3 C7 C21 79(3) . . ?
N2 C7 C21 50(2) . . ?
C20' C7 C21 79(4) . . ?
N3 C7 C21' 90(3) . . ?
N2 C7 C21' 50(2) . . ?
C20' C7 C21' 45(3) . . ?
C21 C7 C21' 63(3) . . ?
N3 C7 C20 41(2) . . ?
N2 C7 C20 88(3) . . ?
C20' C7 C20 63(3) . . ?
C21 C7 C20 39(2) . . ?
C21' C7 C20 78(3) . . ?
N9 C8 C22 107.9(19) . . ?
C10 C9 N4 104(3) . . ?
C9 C10 N5 114(3) . . ?
N5 C11 N4 111.9(17) . . ?
C13 C12 N6 115.9(18) . . ?
C12 C13 C14 126.5(17) . . ?
C12 C13 N9 118.1(18) . . ?
C14 C13 N9 115.3(16) . . ?
C15 C14 C13 113.2(17) . . ?
C16 C15 C14 122.1(19) . . ?
C16 C15 N7 118.0(16) . . ?
C14 C15 N7 119.9(17) . . ?
C15 C16 N6 120.8(18) . . ?
N8 C17 N7 111.4(17) . . ?
N7 C18 C19 103(2) . . ?
N8 C19 C18 111(3) . . ?
C21 C20 N3 107(4) . . ?
C21 C20 C7 70(3) . . ?
N3 C20 C7 38.0(19) . . ?
C21' C20' N3 102(7) . . ?
C21' C20' C7 69(5) . . ?
N3 C20' C7 40(3) . . ?
C20 C21 N2 110(5) . . ?
C20 C21 C7 71(4) . . ?
N2 C21 C7 39.9(18) . . ?
C20' C21' N2 105(6) . . ?
C20' C21' C7 67(5) . . ?
N2 C21' C7 40(2) . . ?
N10 C22 C8 104.4(19) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        28.41
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         3.702
_refine_diff_density_min         -3.986
_refine_diff_density_rms         0.588
_database_code_depnum_ccdc_archive 'CCDC 1005805'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_y

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H36 Cu5 N20 O88 Si2 W22 Y2'
_chemical_formula_sum            'C44 H70 Cu5 N20 O95 Si2 W22 Y2'
_chemical_formula_weight         6995.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.335(5)
_cell_length_b                   12.152(5)
_cell_length_c                   23.319(5)
_cell_angle_alpha                83.543(5)
_cell_angle_beta                 81.741(5)
_cell_angle_gamma                71.112(5)
_cell_volume                     3000.1(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17333
_cell_measurement_theta_min      0.88
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3113
_exptl_absorpt_coefficient_mu    22.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_T_max  0.064
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17333
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         25.03
_reflns_number_total             10583
_reflns_number_gt                7624
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
During the refinement, the non-H atoms W, Si, Cu, Y, C, N and O were 
refined anisotropically. Since most O atoms on the polyanion and lattice 
water molecules as well as some C and N atoms exhibit obvious ADP and
NPD problems with the anisotropic parameters, they are just refined 
isotropically. But this treatment didn't influence the precise of the 
polyanion structure and the final R values.
The restraint command 'isor' was employed to restrain several C, 0 and
N atoms so as to avoid the ADP and NPD problems on them. This command
led to a restraint number 276.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0570P)²+43.7044P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10583
_refine_ls_number_parameters     889
_refine_ls_number_restraints     276
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1439
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.08615(8) 0.01098(7) 0.23558(4) 0.0146(2) Uani 1 1 d . . .
W2 W 0.98687(8) 0.15729(7) 0.36891(4) 0.0136(2) Uani 1 1 d . . .
W3 W 0.98008(8) 0.51458(7) 0.25469(4) 0.0139(2) Uani 1 1 d . . .
W4 W 0.76239(8) 0.42068(7) 0.36972(4) 0.0154(2) Uani 1 1 d . . .
W5 W 0.68097(8) 0.18445(7) 0.35560(4) 0.0136(2) Uani 1 1 d . . .
W6 W 0.78609(8) 0.03283(7) 0.21918(4) 0.0162(2) Uani 1 1 d . . .
W7 W 0.96737(8) 0.12952(7) 0.11126(4) 0.0140(2) Uani 1 1 d . . .
W8 W 0.73909(7) 0.42428(7) 0.10830(4) 0.0133(2) Uani 1 1 d . . .
W9 W 0.64621(8) 0.56719(7) 0.23155(4) 0.0177(2) Uani 1 1 d . . .
W10 W 1.06895(7) 0.38338(7) 0.13301(4) 0.01115(19) Uani 1 1 d . . .
W11 W 0.55873(7) 0.33143(7) 0.21797(4) 0.0142(2) Uani 1 1 d . . .
Cu1 Cu 1.1078(2) -0.2560(2) 0.25484(11) 0.0124(5) Uani 1 1 d . . .
Cu2 Cu 1.6925(2) -0.3702(2) -0.02826(11) 0.0167(6) Uani 1 1 d . . .
Cu3 Cu 0.5000 0.0000 0.5000 0.0291(10) Uani 1 2 d S . .
Y1 Y 1.2555(2) 0.23653(18) 0.25890(10) 0.0191(5) Uani 1 1 d . . .
Si1 Si 0.8688(5) 0.2868(5) 0.2377(2) 0.0093(11) Uani 1 1 d . . .
O1 O 1.1939(11) -0.1308(10) 0.2426(6) 0.009(3) Uani 1 1 d U . .
O2 O 1.0543(14) 0.0786(11) 0.4268(7) 0.021(3) Uani 1 1 d U . .
O3 O 0.9846(13) 0.6547(11) 0.2678(6) 0.018(3) Uani 1 1 d . . .
O4 O 0.7131(14) 0.5176(12) 0.4224(7) 0.023(4) Uani 1 1 d . . .
O5 O 0.5738(14) 0.1254(12) 0.3975(6) 0.020(3) Uani 1 1 d . . .
O5W O 1.6401(14) -0.4292(15) -0.0940(8) 0.033(4) Uani 1 1 d U . .
O6 O 0.7084(14) -0.0671(15) 0.2168(7) 0.031(4) Uani 1 1 d U . .
O7 O 1.0167(13) 0.0849(13) 0.0432(7) 0.026(4) Uani 1 1 d . . .
O8 O 0.7034(13) 0.4753(13) 0.0385(7) 0.024(4) Uani 1 1 d . . .
O9 O 0.5511(15) 0.7077(13) 0.2424(9) 0.038(5) Uani 1 1 d . . .
O10 O 1.1374(13) 0.4310(13) 0.0657(7) 0.021(4) Uani 1 1 d . . .
O11 O 0.4082(12) 0.3241(12) 0.2197(6) 0.016(3) Uani 1 1 d U . .
O12 O 0.7445(12) 0.3663(13) 0.2088(6) 0.017(3) Uani 1 1 d . . .
O13 O 0.6533(12) 0.3296(13) 0.3917(7) 0.020(3) Uani 1 1 d U . .
O14 O 0.8935(13) 0.2978(12) 0.4051(7) 0.022(4) Uani 1 1 d . . .
O15 O 0.8226(11) 0.1130(10) 0.3913(6) 0.007(3) Uani 1 1 d U . .
O16 O 0.6605(12) 0.5035(11) 0.3115(6) 0.014(3) Uani 1 1 d U . .
O17 O 0.7429(13) 0.0712(12) 0.2980(7) 0.022(4) Uani 1 1 d . . .
O18 O 1.0162(11) 0.0432(10) 0.3126(6) 0.007(3) Uani 1 1 d U . .
O19 O 1.1012(13) 0.2178(11) 0.3311(7) 0.019(3) Uani 1 1 d . . .
O20 O 0.8037(13) 0.5775(11) 0.2297(6) 0.016(3) Uani 1 1 d U . .
O21 O 1.1337(13) 0.4256(12) 0.2688(6) 0.018(3) Uani 1 1 d . . .
O22 O 1.1832(14) 0.0996(13) 0.2315(7) 0.023(4) Uani 1 1 d . . .
O23 O 1.2061(12) 0.3146(12) 0.1660(6) 0.016(3) Uani 1 1 d U . .
O24 O 1.0318(12) 0.5206(12) 0.1705(6) 0.015(3) Uani 1 1 d . . .
O25 O 0.8908(13) 0.4446(12) 0.1111(6) 0.016(3) Uani 1 1 d . . .
O26 O 0.6556(13) 0.5634(14) 0.1501(7) 0.024(4) Uani 1 1 d U . .
O27 O 0.8220(12) 0.2655(11) 0.0988(6) 0.014(3) Uani 1 1 d U . .
O28 O 1.0894(11) 0.0125(11) 0.1516(6) 0.010(3) Uani 1 1 d U . .
O29 O 0.9379(13) -0.0583(13) 0.2373(7) 0.023(4) Uani 1 1 d U . .
O30 O 0.5166(12) 0.4910(13) 0.2355(6) 0.019(3) Uani 1 1 d . . .
O31 O 0.8522(12) 0.0428(13) 0.1380(6) 0.018(3) Uani 1 1 d U . .
O32 O 0.6532(13) 0.1798(11) 0.2004(7) 0.019(4) Uani 1 1 d . . .
O33 O 1.0507(13) 0.2411(12) 0.1155(6) 0.019(3) Uani 1 1 d . . .
O34 O 0.5819(12) 0.2855(11) 0.2966(6) 0.012(3) Uani 1 1 d U . .
O35 O 0.8942(12) 0.4738(11) 0.3247(6) 0.014(3) Uani 1 1 d . . .
O36 O 0.5884(13) 0.3782(12) 0.1368(6) 0.017(3) Uani 1 1 d U . .
O37 O 0.8361(13) 0.2681(12) 0.3079(6) 0.017(3) Uani 1 1 d U . .
O38 O 0.9154(11) 0.1588(10) 0.2117(6) 0.006(3) Uani 1 1 d U . .
O39 O 0.9773(12) 0.3475(11) 0.2209(6) 0.011(3) Uani 1 1 d U . .
O1W O 1.388(3) 0.087(3) 0.3174(13) 0.099(9) Uani 1 1 d U . .
O2W O 1.4242(16) 0.1039(15) 0.1971(10) 0.053(6) Uani 1 1 d . . .
O3W O 1.3175(17) 0.307(2) 0.3390(8) 0.052(6) Uani 1 1 d . . .
O4W O 1.2699(15) -0.4120(14) 0.2583(9) 0.043(5) Uani 1 1 d . . .
O6W O 0.718(5) -0.232(4) 0.338(2) 0.084(17) Uani 0.50 1 d P . .
O8W O 0.404(4) 0.464(4) 0.453(2) 0.064(13) Uani 0.50 1 d P . .
O9W O 0.200(5) 0.499(3) 0.397(2) 0.070(14) Uani 0.50 1 d P . .
C1 C 0.9986(18) -0.2276(16) 0.3738(9) 0.012(4) Uani 1 1 d U . .
H1 H 0.9272 -0.2310 0.3599 0.015 Uiso 1 1 calc R . .
C2 C 0.9919(19) -0.2087(19) 0.4300(9) 0.017(5) Uani 1 1 d U . .
C3 C 1.091(2) -0.192(2) 0.4548(12) 0.037(6) Uani 1 1 d U . .
H3 H 1.0836 -0.1691 0.4922 0.044 Uiso 1 1 calc R . .
C4 C 1.2038(18) -0.2140(17) 0.4164(9) 0.013(4) Uani 1 1 d U . .
C5 C 1.2030(19) -0.2347(18) 0.3599(9) 0.017(5) Uani 1 1 d . . .
H5 H 1.2774 -0.2447 0.3353 0.020 Uiso 1 1 calc R . .
C6 C 0.763(2) -0.114(2) 0.4539(10) 0.023(5) Uani 1 1 d . . .
H6 H 0.7521 -0.0729 0.4180 0.027 Uiso 1 1 calc R . .
C7 C 0.719(2) -0.1854(17) 0.5345(11) 0.023(5) Uani 1 1 d U . .
H7 H 0.6753 -0.2016 0.5696 0.028 Uiso 1 1 calc R . .
C8 C 0.848(2) -0.239(2) 0.5181(11) 0.034(6) Uani 1 1 d U . .
H8 H 0.9052 -0.3001 0.5371 0.041 Uiso 1 1 calc R . .
C9 C 1.431(3) -0.279(3) 0.4283(18) 0.081(14) Uani 1 1 d . . .
H9 H 1.4541 -0.3509 0.4127 0.097 Uiso 1 1 calc R . .
C10 C 1.507(3) -0.232(2) 0.4493(13) 0.040(7) Uani 1 1 d U . .
H10 H 1.5921 -0.2692 0.4525 0.048 Uiso 1 1 calc R . .
C11 C 1.322(2) -0.107(2) 0.4555(12) 0.038(7) Uani 1 1 d . . .
H11 H 1.2540 -0.0396 0.4623 0.046 Uiso 1 1 calc R . .
C12 C 1.0020(19) -0.2476(18) 0.1474(10) 0.019(5) Uani 1 1 d U . .
H12 H 0.9297 -0.2455 0.1723 0.023 Uiso 1 1 calc R . .
C13 C 0.9983(17) -0.2446(16) 0.0893(9) 0.010(4) Uani 1 1 d U . .
C14 C 1.1028(19) -0.2483(17) 0.0501(10) 0.018(5) Uani 1 1 d U . .
H14 H 1.1015 -0.2472 0.0103 0.021 Uiso 1 1 calc R . .
C15 C 1.2117(17) -0.2537(16) 0.0745(9) 0.011(4) Uani 1 1 d U . .
C16 C 1.2114(18) -0.2583(15) 0.1344(9) 0.010(4) Uani 1 1 d . . .
H16 H 1.2852 -0.2650 0.1495 0.011 Uiso 1 1 calc R . .
C17 C 1.4397(19) -0.3238(17) 0.0386(10) 0.019(5) Uani 1 1 d U . .
H17 H 1.4624 -0.3856 0.0664 0.023 Uiso 1 1 calc R . .
C18 C 1.318(3) -0.163(3) -0.0078(12) 0.043(7) Uani 1 1 d U . .
H18 H 1.2532 -0.0965 -0.0177 0.052 Uiso 1 1 calc R . .
C19 C 1.443(2) -0.2024(19) -0.0337(11) 0.028(6) Uani 1 1 d U . .
H19 H 1.4722 -0.1679 -0.0681 0.033 Uiso 1 1 calc R . .
C20 C 0.8726(19) -0.3123(17) 0.0309(10) 0.017(5) Uani 1 1 d U . .
H20 H 0.9390 -0.3707 0.0135 0.021 Uiso 1 1 calc R . .
C21 C 0.768(2) -0.1643(19) 0.0854(10) 0.023(5) Uani 1 1 d U . .
H21 H 0.7500 -0.1052 0.1104 0.027 Uiso 1 1 calc R . .
C22 C 0.685(2) -0.193(3) 0.0577(11) 0.048(9) Uani 1 1 d . . .
H22 H 0.5980 -0.1584 0.0610 0.058 Uiso 1 1 calc R . .
N1 N 1.1039(16) -0.2417(16) 0.3371(8) 0.021(4) Uani 1 1 d . . .
N2 N 0.8677(16) -0.1755(15) 0.4662(7) 0.014(4) Uani 1 1 d . . .
N3 N 0.6689(18) -0.110(2) 0.4930(9) 0.041(6) Uani 1 1 d . . .
N4 N 1.3118(17) -0.1999(19) 0.4343(9) 0.031(5) Uani 1 1 d U . .
N5 N 1.4377(16) -0.1183(17) 0.4659(9) 0.025(5) Uani 1 1 d . . .
N6 N 1.1081(15) -0.2534(14) 0.1705(8) 0.014(4) Uani 1 1 d U . .
N7 N 1.3183(16) -0.2480(15) 0.0358(8) 0.017(4) Uani 1 1 d . . .
N8 N 1.5187(16) -0.2964(15) -0.0038(9) 0.021(4) Uani 1 1 d . . .
N9 N 0.8854(14) -0.2429(13) 0.0677(7) 0.010(3) Uani 1 1 d U . .
N10 N 0.7567(16) -0.2895(16) 0.0220(8) 0.021(4) Uani 1 1 d U . .
O7W O 0.420(3) -0.104(3) 0.1638(16) 0.033(8) Uani 0.50 1 d PU A 1
O10W O 1.075(7) 0.506(6) 0.409(3) 0.12(2) Uani 0.50 1 d PU . 1
O11W O 0.952(5) -0.473(5) 0.467(3) 0.096(17) Uani 0.50 1 d PU B 2
O12W O 0.342(5) 0.051(5) 0.095(3) 0.101(19) Uani 0.50 1 d PU C 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O22 1.758(13) . ?
W1 O1 1.766(12) . ?
W1 O18 1.885(12) . ?
W1 O28 1.951(14) . ?
W1 O29 2.103(13) . ?
W1 O38 2.262(12) . ?
W2 O2 1.690(16) . ?
W2 O19 1.772(14) . ?
W2 O14 1.910(14) . ?
W2 O18 1.935(12) . ?
W2 O15 2.083(12) . ?
W2 O37 2.353(15) . ?
W3 O3 1.781(12) . ?
W3 O21 1.781(15) . ?
W3 O35 1.879(13) . ?
W3 O24 1.968(14) . ?
W3 O20 2.042(14) . ?
W3 O39 2.270(12) . ?
W4 O4 1.707(13) . ?
W4 O16 1.893(14) . ?
W4 O13 1.895(13) . ?
W4 O14 1.938(15) . ?
W4 O35 1.942(13) . ?
W4 O37 2.337(12) . ?
W5 O5 1.734(14) . ?
W5 O15 1.829(13) . ?
W5 O17 1.927(14) . ?
W5 O13 1.954(14) . ?
W5 O34 1.958(14) . ?
W5 O37 2.388(13) . ?
W6 O6 1.724(15) . ?
W6 O29 1.799(15) . ?
W6 O17 1.902(15) . ?
W6 O31 1.938(15) . ?
W6 O32 1.981(14) . ?
W6 O38 2.417(11) . ?
W7 O7 1.694(16) . ?
W7 O28 1.902(14) . ?
W7 O33 1.904(13) . ?
W7 O31 1.927(13) . ?
W7 O27 1.949(13) . ?
W7 O38 2.370(13) . ?
W8 O8 1.731(16) . ?
W8 O25 1.825(13) . ?
W8 O27 1.876(12) . ?
W8 O26 1.943(15) . ?
W8 O36 1.970(12) . ?
W8 O12 2.373(14) . ?
W9 O9 1.723(14) . ?
W9 O20 1.823(13) . ?
W9 O26 1.892(16) . ?
W9 O16 1.944(14) . ?
W9 O30 1.961(13) . ?
W9 O12 2.417(14) . ?
W10 O23 1.751(14) . ?
W10 O10 1.770(15) . ?
W10 O24 1.868(13) . ?
W10 O33 1.901(13) . ?
W10 O25 2.033(14) . ?
W10 O39 2.225(13) . ?
W11 O11 1.732(12) . ?
W11 O32 1.864(13) . ?
W11 O34 1.886(14) . ?
W11 O30 1.917(14) . ?
W11 O36 1.929(15) . ?
W11 O12 2.255(13) . ?
Cu1 N1 1.938(19) . ?
Cu1 N6 1.962(18) . ?
Cu1 O3 2.001(13) 1_545 ?
Cu1 O1 2.033(12) . ?
Cu1 O4W 2.175(16) . ?
Cu2 N8 1.913(17) . ?
Cu2 O10 1.941(14) 2_855 ?
Cu2 N10 1.956(17) 1_655 ?
Cu2 O5W 2.000(16) . ?
Cu2 O8 2.284(16) 1_645 ?
Cu3 N3 1.94(2) . ?
Cu3 N3 1.94(2) 2_656 ?
Cu3 N5 2.068(18) 2_756 ?
Cu3 N5 2.068(18) 1_455 ?
Y1 O22 2.264(13) . ?
Y1 O21 2.283(15) . ?
Y1 O19 2.296(14) . ?
Y1 O23 2.334(15) . ?
Y1 O11 2.341(13) 1_655 ?
Y1 O1W 2.39(3) . ?
Y1 O3W 2.418(18) . ?
Y1 O2W 2.463(16) . ?
Si1 O39 1.610(13) . ?
Si1 O12 1.618(15) . ?
Si1 O38 1.629(12) . ?
Si1 O37 1.634(15) . ?
O3 Cu1 2.001(13) 1_565 ?
O8 Cu2 2.284(16) 1_465 ?
O10 Cu2 1.941(14) 2_855 ?
O11 Y1 2.341(13) 1_455 ?
O9W O10W 1.38(7) 1_455 ?
C1 N1 1.34(2) . ?
C1 C2 1.34(3) . ?
C2 C3 1.42(3) . ?
C2 N2 1.49(2) . ?
C3 C4 1.41(3) . ?
C4 C5 1.37(3) . ?
C4 N4 1.41(3) . ?
C5 N1 1.34(3) . ?
C6 N2 1.24(3) . ?
C6 N3 1.29(3) . ?
C7 N3 1.31(3) . ?
C7 C8 1.41(3) . ?
C8 N2 1.39(3) . ?
C9 C10 1.34(4) . ?
C9 N4 1.38(4) . ?
C10 N5 1.42(3) . ?
C11 N4 1.33(3) . ?
C11 N5 1.33(3) . ?
C12 C13 1.36(3) . ?
C12 N6 1.37(3) . ?
C13 C14 1.38(3) . ?
C13 N9 1.43(2) . ?
C14 C15 1.41(3) . ?
C15 C16 1.39(3) . ?
C15 N7 1.42(2) . ?
C16 N6 1.33(2) . ?
C17 N8 1.32(3) . ?
C17 N7 1.39(3) . ?
C18 N7 1.37(3) . ?
C18 C19 1.41(3) . ?
C19 N8 1.37(3) . ?
C20 N10 1.30(3) . ?
C20 N9 1.32(2) . ?
C21 C22 1.37(3) . ?
C21 N9 1.40(3) . ?
C22 N10 1.46(3) . ?
N5 Cu3 2.068(18) 1_655 ?
N10 Cu2 1.956(17) 1_455 ?
O10W O9W 1.38(7) 1_655 ?

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
O22 W1 O1 102.4(6) . . ?
O22 W1 O18 94.4(6) . . ?
O1 W1 O18 103.9(6) . . ?
O22 W1 O28 94.7(6) . . ?
O1 W1 O28 94.7(6) . . ?
O18 W1 O28 157.1(5) . . ?
O22 W1 O29 166.8(7) . . ?
O1 W1 O29 90.7(6) . . ?
O18 W1 O29 83.2(5) . . ?
O28 W1 O29 83.2(5) . . ?
O22 W1 O38 94.7(6) . . ?
O1 W1 O38 160.4(5) . . ?
O18 W1 O38 84.1(5) . . ?
O28 W1 O38 74.1(5) . . ?
O29 W1 O38 72.2(5) . . ?
O2 W2 O19 104.8(7) . . ?
O2 W2 O14 98.9(6) . . ?
O19 W2 O14 93.4(6) . . ?
O2 W2 O18 104.0(6) . . ?
O19 W2 O18 93.2(6) . . ?
O14 W2 O18 153.7(6) . . ?
O2 W2 O15 93.3(6) . . ?
O19 W2 O15 161.9(6) . . ?
O14 W2 O15 84.4(5) . . ?
O18 W2 O15 81.5(5) . . ?
O2 W2 O37 162.1(6) . . ?
O19 W2 O37 91.5(6) . . ?
O14 W2 O37 72.3(6) . . ?
O18 W2 O37 82.1(5) . . ?
O15 W2 O37 70.7(5) . . ?
O3 W3 O21 101.0(6) . . ?
O3 W3 O35 101.6(6) . . ?
O21 W3 O35 97.1(6) . . ?
O3 W3 O24 97.9(6) . . ?
O21 W3 O24 91.4(6) . . ?
O35 W3 O24 156.7(5) . . ?
O3 W3 O20 93.9(6) . . ?
O21 W3 O20 164.8(5) . . ?
O35 W3 O20 82.8(6) . . ?
O24 W3 O20 83.3(6) . . ?
O3 W3 O39 169.7(6) . . ?
O21 W3 O39 81.9(5) . . ?
O35 W3 O39 87.7(5) . . ?
O24 W3 O39 72.0(5) . . ?
O20 W3 O39 82.9(5) . . ?
O4 W4 O16 100.7(7) . . ?
O4 W4 O13 100.7(6) . . ?
O16 W4 O13 89.8(6) . . ?
O4 W4 O14 101.1(7) . . ?
O16 W4 O14 158.0(6) . . ?
O13 W4 O14 88.8(6) . . ?
O4 W4 O35 100.7(6) . . ?
O16 W4 O35 85.9(6) . . ?
O13 W4 O35 158.6(6) . . ?
O14 W4 O35 87.4(6) . . ?
O4 W4 O37 172.1(7) . . ?
O16 W4 O37 86.3(5) . . ?
O13 W4 O37 75.4(5) . . ?
O14 W4 O37 72.2(6) . . ?
O35 W4 O37 83.4(5) . . ?
O5 W5 O15 101.4(6) . . ?
O5 W5 O17 98.8(6) . . ?
O15 W5 O17 88.9(6) . . ?
O5 W5 O13 102.8(6) . . ?
O15 W5 O13 91.5(6) . . ?
O17 W5 O13 157.9(6) . . ?
O5 W5 O34 102.8(6) . . ?
O15 W5 O34 155.7(5) . . ?
O17 W5 O34 86.1(6) . . ?
O13 W5 O34 84.5(6) . . ?
O5 W5 O37 173.6(6) . . ?
O15 W5 O37 74.0(5) . . ?
O17 W5 O37 85.7(5) . . ?
O13 W5 O37 73.2(5) . . ?
O34 W5 O37 82.0(5) . . ?
O6 W6 O29 102.5(7) . . ?
O6 W6 O17 101.6(7) . . ?
O29 W6 O17 88.9(7) . . ?
O6 W6 O31 99.3(6) . . ?
O29 W6 O31 90.4(6) . . ?
O17 W6 O31 158.8(6) . . ?
O6 W6 O32 100.5(7) . . ?
O29 W6 O32 157.0(6) . . ?
O17 W6 O32 86.4(6) . . ?
O31 W6 O32 86.0(6) . . ?
O6 W6 O38 172.0(6) . . ?
O29 W6 O38 73.7(5) . . ?
O17 W6 O38 85.5(5) . . ?
O31 W6 O38 74.0(5) . . ?
O32 W6 O38 83.6(5) . . ?
O7 W7 O28 98.8(7) . . ?
O7 W7 O33 103.3(6) . . ?
O28 W7 O33 91.3(6) . . ?
O7 W7 O31 100.8(6) . . ?
O28 W7 O31 87.7(6) . . ?
O33 W7 O31 155.7(6) . . ?
O7 W7 O27 102.1(7) . . ?
O28 W7 O27 159.1(6) . . ?
O33 W7 O27 84.6(6) . . ?
O31 W7 O27 87.7(6) . . ?
O7 W7 O38 170.3(6) . . ?
O28 W7 O38 72.4(5) . . ?
O33 W7 O38 81.3(5) . . ?
O31 W7 O38 75.3(5) . . ?
O27 W7 O38 86.7(5) . . ?
O8 W8 O25 104.4(6) . . ?
O8 W8 O27 101.4(7) . . ?
O25 W8 O27 89.0(6) . . ?
O8 W8 O26 101.1(7) . . ?
O25 W8 O26 90.2(6) . . ?
O27 W8 O26 157.0(7) . . ?
O8 W8 O36 98.4(6) . . ?
O25 W8 O36 157.3(6) . . ?
O27 W8 O36 86.3(6) . . ?
O26 W8 O36 85.7(6) . . ?
O8 W8 O12 168.7(6) . . ?
O25 W8 O12 85.5(5) . . ?
O27 W8 O12 83.9(6) . . ?
O26 W8 O12 73.1(6) . . ?
O36 W8 O12 71.9(5) . . ?
O9 W9 O20 103.1(7) . . ?
O9 W9 O26 101.8(8) . . ?
O20 W9 O26 94.5(6) . . ?
O9 W9 O16 100.5(8) . . ?
O20 W9 O16 87.1(6) . . ?
O26 W9 O16 156.6(6) . . ?
O9 W9 O30 99.2(7) . . ?
O20 W9 O30 157.2(6) . . ?
O26 W9 O30 85.4(6) . . ?
O16 W9 O30 84.3(6) . . ?
O9 W9 O12 168.7(7) . . ?
O20 W9 O12 87.4(5) . . ?
O26 W9 O12 72.8(6) . . ?
O16 W9 O12 84.0(5) . . ?
O30 W9 O12 70.8(5) . . ?
O23 W10 O10 98.7(7) . . ?
O23 W10 O24 93.7(6) . . ?
O10 W10 O24 97.6(6) . . ?
O23 W10 O33 94.0(6) . . ?
O10 W10 O33 102.2(6) . . ?
O24 W10 O33 157.3(6) . . ?
O23 W10 O25 166.4(6) . . ?
O10 W10 O25 94.7(6) . . ?
O24 W10 O25 86.9(6) . . ?
O33 W10 O25 80.8(6) . . ?
O23 W10 O39 82.6(6) . . ?
O10 W10 O39 172.4(5) . . ?
O24 W10 O39 74.9(5) . . ?
O33 W10 O39 85.0(5) . . ?
O25 W10 O39 84.4(5) . . ?
O11 W11 O32 100.5(6) . . ?
O11 W11 O34 98.7(6) . . ?
O32 W11 O34 88.0(6) . . ?
O11 W11 O30 98.6(6) . . ?
O32 W11 O30 160.9(6) . . ?
O34 W11 O30 89.1(6) . . ?
O11 W11 O36 99.3(6) . . ?
O32 W11 O36 87.8(6) . . ?
O34 W11 O36 162.1(5) . . ?
O30 W11 O36 89.2(6) . . ?
O11 W11 O12 171.7(6) . . ?
O32 W11 O12 85.6(6) . . ?
O34 W11 O12 87.0(5) . . ?
O30 W11 O12 75.3(5) . . ?
O36 W11 O12 75.3(5) . . ?
N1 Cu1 N6 174.3(7) . . ?
N1 Cu1 O3 93.3(6) . 1_545 ?
N6 Cu1 O3 90.2(6) . 1_545 ?
N1 Cu1 O1 85.7(6) . . ?
N6 Cu1 O1 89.8(6) . . ?
O3 Cu1 O1 165.9(5) 1_545 . ?
N1 Cu1 O4W 90.4(8) . . ?
N6 Cu1 O4W 93.9(7) . . ?
O3 Cu1 O4W 93.7(6) 1_545 . ?
O1 Cu1 O4W 100.4(6) . . ?
N8 Cu2 O10 170.3(8) . 2_855 ?
N8 Cu2 N10 96.0(8) . 1_655 ?
O10 Cu2 N10 88.0(7) 2_855 1_655 ?
N8 Cu2 O5W 88.1(7) . . ?
O10 Cu2 O5W 86.1(6) 2_855 . ?
N10 Cu2 O5W 166.9(8) 1_655 . ?
N8 Cu2 O8 92.6(7) . 1_645 ?
O10 Cu2 O8 96.0(6) 2_855 1_645 ?
N10 Cu2 O8 92.9(7) 1_655 1_645 ?
O5W Cu2 O8 99.3(6) . 1_645 ?
N3 Cu3 N3 180.000 . 2_656 ?
N3 Cu3 N5 90.8(8) . 2_756 ?
N3 Cu3 N5 89.2(8) 2_656 2_756 ?
N3 Cu3 N5 89.2(8) . 1_455 ?
N3 Cu3 N5 90.8(8) 2_656 1_455 ?
N5 Cu3 N5 180.000 2_756 1_455 ?
O22 Y1 O21 123.0(5) . . ?
O22 Y1 O19 74.3(5) . . ?
O21 Y1 O19 77.7(5) . . ?
O22 Y1 O23 79.5(5) . . ?
O21 Y1 O23 73.8(5) . . ?
O19 Y1 O23 120.7(5) . . ?
O22 Y1 O11 135.4(5) . 1_655 ?
O21 Y1 O11 82.6(5) . 1_655 ?
O19 Y1 O11 150.2(5) . 1_655 ?
O23 Y1 O11 73.7(5) . 1_655 ?
O22 Y1 O1W 88.2(8) . . ?
O21 Y1 O1W 136.2(8) . . ?
O19 Y1 O1W 83.3(8) . . ?
O23 Y1 O1W 147.9(8) . . ?
O11 Y1 O1W 96.1(8) 1_655 . ?
O22 Y1 O3W 145.3(7) . . ?
O21 Y1 O3W 71.7(6) . . ?
O19 Y1 O3W 79.7(6) . . ?
O23 Y1 O3W 134.3(6) . . ?
O11 Y1 O3W 73.0(6) 1_655 . ?
O1W Y1 O3W 66.1(9) . . ?
O22 Y1 O2W 71.0(5) . . ?
O21 Y1 O2W 144.9(6) . . ?
O19 Y1 O2W 136.1(6) . . ?
O23 Y1 O2W 78.4(7) . . ?
O11 Y1 O2W 69.2(5) 1_655 . ?
O1W Y1 O2W 69.6(9) . . ?
O3W Y1 O2W 116.7(7) . . ?
O39 Si1 O12 109.0(8) . . ?
O39 Si1 O38 109.4(7) . . ?
O12 Si1 O38 108.6(7) . . ?
O39 Si1 O37 112.1(7) . . ?
O12 Si1 O37 110.2(8) . . ?
O38 Si1 O37 107.5(7) . . ?
W1 O1 Cu1 112.3(6) . . ?
W3 O3 Cu1 138.1(7) . 1_565 ?
W8 O8 Cu2 142.7(8) . 1_465 ?
W10 O10 Cu2 128.9(9) . 2_855 ?
W11 O11 Y1 149.0(8) . 1_455 ?
Si1 O12 W11 126.4(8) . . ?
Si1 O12 W8 124.5(7) . . ?
W11 O12 W8 93.3(5) . . ?
Si1 O12 W9 120.4(7) . . ?
W11 O12 W9 92.6(5) . . ?
W8 O12 W9 89.9(5) . . ?
W4 O13 W5 120.9(7) . . ?
W2 O14 W4 123.1(8) . . ?
W5 O15 W2 122.5(7) . . ?
W4 O16 W9 149.4(7) . . ?
W6 O17 W5 151.0(9) . . ?
W1 O18 W2 141.9(7) . . ?
W2 O19 Y1 156.6(7) . . ?
W9 O20 W3 150.4(8) . . ?
W3 O21 Y1 137.2(7) . . ?
W1 O22 Y1 156.9(8) . . ?
W10 O23 Y1 136.4(7) . . ?
W10 O24 W3 117.6(7) . . ?
W8 O25 W10 150.4(8) . . ?
W9 O26 W8 123.9(9) . . ?
W8 O27 W7 148.2(8) . . ?
W7 O28 W1 120.7(6) . . ?
W6 O29 W1 121.0(8) . . ?
W11 O30 W9 121.2(7) . . ?
W7 O31 W6 121.2(7) . . ?
W11 O32 W6 149.4(9) . . ?
W10 O33 W7 157.3(8) . . ?
W11 O34 W5 150.2(7) . . ?
W3 O35 W4 153.2(8) . . ?
W11 O36 W8 119.4(7) . . ?
Si1 O37 W4 123.7(8) . . ?
Si1 O37 W2 122.7(7) . . ?
W4 O37 W2 92.3(5) . . ?
Si1 O37 W5 125.6(7) . . ?
W4 O37 W5 90.3(4) . . ?
W2 O37 W5 92.7(5) . . ?
Si1 O38 W1 124.7(7) . . ?
Si1 O38 W7 123.5(7) . . ?
W1 O38 W7 92.6(4) . . ?
Si1 O38 W6 123.9(6) . . ?
W1 O38 W6 93.1(4) . . ?
W7 O38 W6 89.4(4) . . ?
Si1 O39 W10 128.2(8) . . ?
Si1 O39 W3 126.1(7) . . ?
W10 O39 W3 93.8(5) . . ?
N1 C1 C2 122.7(19) . . ?
C1 C2 C3 123.5(19) . . ?
C1 C2 N2 119.9(18) . . ?
C3 C2 N2 115.1(19) . . ?
C4 C3 C2 113(2) . . ?
C5 C4 C3 120(2) . . ?
C5 C4 N4 120.1(18) . . ?
C3 C4 N4 120(2) . . ?
N1 C5 C4 125.4(19) . . ?
N2 C6 N3 117(2) . . ?
N3 C7 C8 110(2) . . ?
N2 C8 C7 102(2) . . ?
C10 C9 N4 107(3) . . ?
C9 C10 N5 109(2) . . ?
N4 C11 N5 113(2) . . ?
C13 C12 N6 122.4(19) . . ?
C12 C13 C14 121.5(19) . . ?
C12 C13 N9 119.8(17) . . ?
C14 C13 N9 118.6(19) . . ?
C13 C14 C15 116(2) . . ?
C16 C15 C14 120.7(18) . . ?
C16 C15 N7 121.5(17) . . ?
C14 C15 N7 117.7(19) . . ?
N6 C16 C15 121.6(18) . . ?
N8 C17 N7 111(2) . . ?
N7 C18 C19 101(2) . . ?
N8 C19 C18 114(2) . . ?
N10 C20 N9 112.0(18) . . ?
C22 C21 N9 105(2) . . ?
C21 C22 N10 107(2) . . ?
C1 N1 C5 115.6(19) . . ?
C1 N1 Cu1 122.0(14) . . ?
C5 N1 Cu1 122.1(14) . . ?
C6 N2 C8 106.4(19) . . ?
C6 N2 C2 131(2) . . ?
C8 N2 C2 120.6(18) . . ?
C6 N3 C7 103(2) . . ?
C6 N3 Cu3 131(2) . . ?
C7 N3 Cu3 125.0(17) . . ?
C11 N4 C9 107(2) . . ?
C11 N4 C4 128(2) . . ?
C9 N4 C4 126(2) . . ?
C11 N5 C10 103(2) . . ?
C11 N5 Cu3 128.1(16) . 1_655 ?
C10 N5 Cu3 128.6(16) . 1_655 ?
C16 N6 C12 118.1(19) . . ?
C16 N6 Cu1 121.2(14) . . ?
C12 N6 Cu1 120.7(14) . . ?
C18 N7 C17 109.9(19) . . ?
C18 N7 C15 124.7(19) . . ?
C17 N7 C15 125.3(19) . . ?
C17 N8 C19 103.4(18) . . ?
C17 N8 Cu2 132.3(16) . . ?
C19 N8 Cu2 124.0(16) . . ?
C20 N9 C21 109.5(17) . . ?
C20 N9 C13 127.8(16) . . ?
C21 N9 C13 122.6(16) . . ?
C20 N10 C22 106.0(17) . . ?
C20 N10 Cu2 126.6(15) . 1_455 ?
C22 N10 Cu2 127.5(14) . 1_455 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.956
_refine_diff_density_min         -2.755
_refine_diff_density_rms         0.585
_database_code_depnum_ccdc_archive 'CCDC 1005806'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_ce

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H36 Ce2 Cu5 N20 O88 Si2 W22'
_chemical_formula_sum            'C44 H68 Ce2 Cu5 N20 O94 Si2 W22'
_chemical_formula_weight         7080.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.322(5)
_cell_length_b                   12.139(5)
_cell_length_c                   23.311(5)
_cell_angle_alpha                83.586(5)
_cell_angle_beta                 81.753(5)
_cell_angle_gamma                71.169(5)
_cell_volume                     2993.6(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18673
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3141
_exptl_absorpt_coefficient_mu    22.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_T_max  0.001
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18673
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10514
_reflns_number_gt                8246
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis (Oxford Diffraction,2006)'
_computing_cell_refinement       CrysAlis
_computing_data_reduction        CrysAlis
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0464P)²+116.7797P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10514
_refine_ls_number_parameters     880
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1254
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.91485(7) 0.98821(6) 0.26460(3) 0.01210(17) Uani 1 1 d . . .
W2 W 1.01340(7) 0.84185(6) 0.13138(3) 0.01194(17) Uani 1 1 d . . .
W3 W 1.01865(7) 0.48595(6) 0.24556(3) 0.01204(17) Uani 1 1 d . . .
W4 W 1.23697(7) 0.57908(6) 0.13061(3) 0.01392(18) Uani 1 1 d . . .
W5 W 1.31911(6) 0.81499(6) 0.14462(3) 0.01211(17) Uani 1 1 d . . .
W6 W 1.21480(7) 0.96647(6) 0.28099(4) 0.01372(18) Uani 1 1 d . . .
W7 W 1.03331(7) 0.87031(6) 0.38876(3) 0.01221(17) Uani 1 1 d . . .
W8 W 1.26055(6) 0.57560(6) 0.39177(3) 0.01196(17) Uani 1 1 d . . .
W9 W 1.35263(7) 0.43296(6) 0.26886(4) 0.01563(18) Uani 1 1 d . . .
W10 W 0.93043(6) 0.61678(6) 0.36715(3) 0.00964(17) Uani 1 1 d . . .
W11 W 1.44112(6) 0.66786(6) 0.28220(3) 0.01233(17) Uani 1 1 d . . .
Cu1 Cu 0.89232(19) 1.25578(18) 0.24516(9) 0.0115(5) Uani 1 1 d . . .
Cu2 Cu 1.3081(2) 1.3697(2) 0.52783(10) 0.0147(5) Uani 1 1 d . . .
Cu3 Cu 0.5000 1.0000 0.0000 0.0278(9) Uani 1 2 d S . .
Ce1 Ce 0.74382(17) 0.76358(16) 0.24117(9) 0.0599(5) Uani 1 1 d . . .
Si1 Si 1.1307(4) 0.7133(4) 0.2624(2) 0.0079(10) Uani 1 1 d . . .
O1 O 0.8070(11) 1.1300(10) 0.2574(6) 0.017(3) Uani 1 1 d . . .
O2 O 0.9424(12) 0.9253(11) 0.0742(6) 0.021(3) Uani 1 1 d . . .
O3 O 1.0132(11) 0.3487(10) 0.2329(6) 0.014(3) Uani 1 1 d . . .
O4 O 1.2848(12) 0.4830(12) 0.0781(6) 0.024(3) Uani 1 1 d . . .
O5 O 1.4302(12) 0.8686(11) 0.1034(6) 0.020(3) Uani 1 1 d U . .
O6 O 1.2926(12) 1.0654(12) 0.2830(6) 0.024(3) Uani 1 1 d . . .
O7 O 0.9850(13) 0.9134(12) 0.4565(6) 0.023(3) Uani 1 1 d . . .
O8 O 1.2962(11) 0.5236(12) 0.4616(6) 0.020(3) Uani 1 1 d . . .
O9 O 1.4477(12) 0.2940(12) 0.2584(7) 0.031(4) Uani 1 1 d . . .
O10 O 0.8647(11) 0.5680(11) 0.4336(5) 0.016(3) Uani 1 1 d . . .
O11 O 1.5955(11) 0.6715(10) 0.2803(5) 0.014(3) Uani 1 1 d U . .
O12 O 1.2554(11) 0.6319(10) 0.2914(5) 0.012(3) Uani 1 1 d . . .
O13 O 1.3466(11) 0.6703(11) 0.1081(6) 0.017(3) Uani 1 1 d . . .
O14 O 1.1075(11) 0.7014(10) 0.0940(6) 0.016(3) Uani 1 1 d . . .
O15 O 1.1801(11) 0.8821(10) 0.1086(6) 0.015(3) Uani 1 1 d U . .
O16 O 1.3368(11) 0.4975(10) 0.1897(5) 0.015(3) Uani 1 1 d U . .
O17 O 1.2610(11) 0.9236(11) 0.2028(6) 0.018(3) Uani 1 1 d . . .
O18 O 0.9829(11) 0.9565(10) 0.1868(6) 0.015(3) Uani 1 1 d . . .
O19 O 0.8963(11) 0.7854(11) 0.1698(6) 0.022(3) Uani 1 1 d . . .
O20 O 1.1941(12) 0.4247(12) 0.2705(6) 0.020(3) Uani 1 1 d . . .
O21 O 0.8652(12) 0.5741(11) 0.2317(6) 0.021(3) Uani 1 1 d . . .
O22 O 0.8197(11) 0.8981(11) 0.2688(6) 0.018(3) Uani 1 1 d . . .
O23 O 0.7918(11) 0.6872(10) 0.3330(6) 0.015(3) Uani 1 1 d . . .
O24 O 0.9698(11) 0.4786(10) 0.3284(6) 0.015(3) Uani 1 1 d . . .
O25 O 1.1095(11) 0.5551(11) 0.3885(6) 0.018(3) Uani 1 1 d . . .
O26 O 1.3449(11) 0.4346(10) 0.3513(6) 0.020(3) Uani 1 1 d . . .
O27 O 1.1764(10) 0.7358(10) 0.4022(6) 0.014(3) Uani 1 1 d . . .
O28 O 0.9127(11) 0.9858(11) 0.3474(6) 0.016(3) Uani 1 1 d . . .
O29 O 1.0605(11) 1.0599(10) 0.2636(6) 0.015(3) Uani 1 1 d . . .
O30 O 1.4833(11) 0.5088(11) 0.2642(6) 0.017(3) Uani 1 1 d . . .
O31 O 1.1498(11) 0.9545(11) 0.3614(6) 0.017(3) Uani 1 1 d . . .
O32 O 1.3462(11) 0.8206(10) 0.2988(6) 0.014(3) Uani 1 1 d . . .
O33 O 0.9472(10) 0.7598(11) 0.3858(6) 0.015(3) Uani 1 1 d . . .
O34 O 1.4174(11) 0.7142(11) 0.2043(5) 0.016(3) Uani 1 1 d . . .
O35 O 1.1047(11) 0.5277(11) 0.1765(6) 0.017(3) Uani 1 1 d . . .
O36 O 1.4148(11) 0.6175(11) 0.3621(6) 0.016(3) Uani 1 1 d . . .
O37 O 1.1631(11) 0.7306(10) 0.1931(5) 0.011(3) Uani 1 1 d . . .
O38 O 1.0850(10) 0.8408(10) 0.2887(5) 0.009(3) Uani 1 1 d . . .
O39 O 1.0213(11) 0.6503(10) 0.2796(5) 0.012(3) Uani 1 1 d . . .
O1W O 0.6811(16) 0.6905(17) 0.1615(7) 0.049(5) Uani 1 1 d . . .
O2W O 0.616(2) 0.9101(19) 0.1832(10) 0.082(8) Uani 1 1 d . . .
O3W O 0.5768(14) 0.8948(14) 0.3048(9) 0.051(5) Uani 1 1 d . . .
O4W O 0.7289(13) 1.4120(12) 0.2419(8) 0.036(4) Uani 1 1 d . . .
O5W O 1.3609(12) 1.4297(12) 0.5939(6) 0.024(3) Uani 1 1 d U . .
O6W O 0.592(3) 0.541(3) 0.0470(15) 0.042(9) Uani 0.50 1 d P . .
O7W O 0.802(4) 0.507(4) 0.106(2) 0.074(13) Uani 0.50 1 d PU . .
O8W O 0.574(3) 0.118(4) 0.337(2) 0.077(15) Uani 0.50 1 d P . .
O10W O 0.659(4) 0.924(4) 0.404(2) 0.078(13) Uani 0.50 1 d PU . .
C1 C 0.7954(17) 1.2338(16) 0.1405(9) 0.018(4) Uani 1 1 d . . .
H1 H 0.7203 1.2468 0.1648 0.022 Uiso 1 1 calc R . .
C2 C 0.7996(16) 1.2086(16) 0.0835(8) 0.015(4) Uani 1 1 d U . .
C3 C 0.9095(16) 1.1899(16) 0.0468(8) 0.015(4) Uani 1 1 d U . .
H3 H 0.9147 1.1705 0.0088 0.018 Uiso 1 1 calc R . .
C4 C 1.0113(17) 1.2011(16) 0.0685(9) 0.018(4) Uani 1 1 d U . .
C5 C 1.0035(16) 1.2243(16) 0.1254(8) 0.016(4) Uani 1 1 d . . .
H5 H 1.0743 1.2294 0.1395 0.019 Uiso 1 1 calc R . .
C6 C 0.6825(18) 1.100(2) 0.0437(10) 0.031(5) Uani 1 1 d . . .
H6 H 0.7504 1.0339 0.0364 0.038 Uiso 1 1 calc R . .
C7 C 0.497(2) 1.226(2) 0.0506(14) 0.051(8) Uani 1 1 d . . .
H7 H 0.4110 1.2615 0.0488 0.062 Uiso 1 1 calc R . .
C8 C 0.573(2) 1.276(2) 0.0690(14) 0.049(8) Uani 1 1 d . . .
H8 H 0.5497 1.3507 0.0820 0.058 Uiso 1 1 calc R . .
C9 C 1.1529(18) 1.237(2) -0.0202(9) 0.028(5) Uani 1 1 d . . .
H9 H 1.0955 1.2918 -0.0422 0.033 Uiso 1 1 calc R . .
C10 C 1.2775(18) 1.192(2) -0.0345(10) 0.029(5) Uani 1 1 d . . .
H10 H 1.3216 1.2135 -0.0683 0.034 Uiso 1 1 calc R . .
C11 C 1.2382(17) 1.1079(18) 0.0489(10) 0.025(5) Uani 1 1 d . . .
H11 H 1.2470 1.0608 0.0833 0.030 Uiso 1 1 calc R . .
C12 C 0.7899(18) 1.2565(17) 0.3670(8) 0.018(4) Uani 1 1 d . . .
H12 H 0.7167 1.2606 0.3520 0.022 Uiso 1 1 calc R . .
C13 C 0.7885(16) 1.2563(17) 0.4250(8) 0.015(4) Uani 1 1 d . . .
C14 C 0.8928(18) 1.2539(16) 0.4484(8) 0.019(4) Uani 1 1 d . . .
H14 H 0.8917 1.2581 0.4881 0.022 Uiso 1 1 calc R . .
C15 C 1.0000(15) 1.2451(14) 0.4104(8) 0.008(3) Uani 1 1 d U . .
C16 C 1.0002(17) 1.2443(15) 0.3522(8) 0.014(4) Uani 1 1 d U . .
H16 H 1.0735 1.2392 0.3274 0.017 Uiso 1 1 calc R . .
C17 C 1.1276(18) 1.3096(16) 0.4681(8) 0.019(4) Uani 1 1 d . . .
H17 H 1.0612 1.3685 0.4852 0.022 Uiso 1 1 calc R . .
C18 C 1.2319(19) 1.168(2) 0.4148(11) 0.039(6) Uani 1 1 d . . .
H18 H 1.2531 1.1107 0.3882 0.047 Uiso 1 1 calc R . .
C19 C 1.311(2) 1.194(2) 0.4451(11) 0.036(6) Uani 1 1 d U . .
H19 H 1.3968 1.1560 0.4434 0.043 Uiso 1 1 calc R . .
C20 C 0.5629(17) 1.3226(17) 0.4621(9) 0.021(5) Uani 1 1 d . . .
H20 H 0.5388 1.3865 0.4356 0.025 Uiso 1 1 calc R . .
C21 C 0.683(2) 1.168(2) 0.5076(10) 0.034(6) Uani 1 1 d . . .
H21 H 0.7514 1.1045 0.5171 0.041 Uiso 1 1 calc R . .
C22 C 0.5587(19) 1.198(2) 0.5359(11) 0.034(6) Uani 1 1 d . . .
H22 H 0.5319 1.1613 0.5701 0.041 Uiso 1 1 calc R . .
N1 N 0.8971(13) 1.2399(12) 0.1612(6) 0.011(3) Uani 1 1 d . . .
N2 N 0.6894(14) 1.1973(15) 0.0649(7) 0.021(4) Uani 1 1 d . . .
N3 N 0.5638(15) 1.1138(15) 0.0345(8) 0.025(4) Uani 1 1 d . . .
N4 N 1.1284(13) 1.1845(14) 0.0343(7) 0.019(4) Uani 1 1 d . . .
N5 N 1.3313(14) 1.1088(14) 0.0076(7) 0.020(4) Uani 1 1 d . . .
N6 N 0.8936(13) 1.2511(12) 0.3307(7) 0.012(3) Uani 1 1 d . . .
N7 N 1.1157(14) 1.2404(13) 0.4305(7) 0.016(3) Uani 1 1 d U . .
N8 N 1.2463(15) 1.2839(14) 0.4784(8) 0.023(4) Uani 1 1 d . . .
N9 N 0.6797(13) 1.2511(15) 0.4634(7) 0.019(4) Uani 1 1 d . . .
N10 N 0.4843(13) 1.2898(15) 0.5045(7) 0.021(4) Uani 1 1 d . . .
O9W O 0.281(4) 0.231(4) 0.167(2) 0.082(16) Uani 0.50 1 d P A 1
O11W O 0.457(4) 1.113(4) 0.184(2) 0.077(13) Uani 0.50 1 d PU B 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O22 1.753(11) . ?
W1 O1 1.766(12) . ?
W1 O18 1.895(13) . ?
W1 O28 1.925(13) . ?
W1 O29 2.094(12) . ?
W1 O38 2.256(11) . ?
W2 O2 1.712(12) . ?
W2 O19 1.772(11) . ?
W2 O18 1.921(13) . ?
W2 O14 1.923(12) . ?
W2 O15 2.082(11) . ?
W2 O37 2.356(12) . ?
W3 O3 1.745(12) . ?
W3 O21 1.775(13) . ?
W3 O35 1.868(12) . ?
W3 O24 1.932(13) . ?
W3 O20 2.029(13) . ?
W3 O39 2.238(12) . ?
W4 O4 1.695(14) . ?
W4 O16 1.891(13) . ?
W4 O13 1.901(12) . ?
W4 O14 1.938(12) . ?
W4 O35 1.941(12) . ?
W4 O37 2.337(13) . ?
W5 O5 1.723(11) . ?
W5 O15 1.801(12) . ?
W5 O17 1.895(13) . ?
W5 O13 1.953(13) . ?
W5 O34 1.964(12) . ?
W5 O37 2.404(11) . ?
W6 O6 1.711(12) . ?
W6 O29 1.823(12) . ?
W6 O17 1.906(13) . ?
W6 O31 1.922(13) . ?
W6 O32 1.958(12) . ?
W6 O38 2.414(11) . ?
W7 O7 1.679(14) . ?
W7 O28 1.897(12) . ?
W7 O33 1.908(11) . ?
W7 O31 1.917(11) . ?
W7 O27 1.927(11) . ?
W7 O38 2.360(12) . ?
W8 O8 1.734(13) . ?
W8 O25 1.819(12) . ?
W8 O27 1.895(12) . ?
W8 O26 1.944(13) . ?
W8 O36 1.984(11) . ?
W8 O12 2.368(12) . ?
W9 O9 1.705(14) . ?
W9 O20 1.824(12) . ?
W9 O26 1.913(15) . ?
W9 O16 1.932(13) . ?
W9 O30 1.964(12) . ?
W9 O12 2.392(12) . ?
W10 O10 1.747(12) . ?
W10 O23 1.779(12) . ?
W10 O24 1.889(12) . ?
W10 O33 1.909(12) . ?
W10 O25 2.036(12) . ?
W10 O39 2.207(12) . ?
W11 O11 1.756(11) . ?
W11 O32 1.870(12) . ?
W11 O34 1.871(12) . ?
W11 O36 1.907(13) . ?
W11 O30 1.914(13) . ?
W11 O12 2.258(11) . ?
Cu1 N1 1.979(15) . ?
Cu1 N6 1.991(16) . ?
Cu1 O3 2.010(11) 1_565 ?
Cu1 O1 2.029(12) . ?
Cu1 O4W 2.183(14) . ?
Cu2 N10 1.942(15) 1_655 ?
Cu2 N8 1.968(18) . ?
Cu2 O10 1.975(12) 2_776 ?
Cu2 O5W 2.013(14) . ?
Cu2 O8 2.268(13) 1_565 ?
Cu3 N5 1.936(15) 2_775 ?
Cu3 N5 1.936(15) 1_455 ?
Cu3 N3 2.033(17) 2_675 ?
Cu3 N3 2.033(17) . ?
Ce1 O22 2.263(13) . ?
Ce1 O19 2.278(12) . ?
Ce1 O21 2.284(13) . ?
Ce1 O23 2.303(13) . ?
Ce1 O11 2.334(11) 1_455 ?
Ce1 O2W 2.335(18) . ?
Ce1 O1W 2.427(17) . ?
Ce1 O3W 2.468(18) . ?
Si1 O37 1.610(13) . ?
Si1 O38 1.626(12) . ?
Si1 O12 1.628(12) . ?
Si1 O39 1.638(12) . ?
O3 Cu1 2.010(11) 1_545 ?
O8 Cu2 2.268(13) 1_545 ?
O10 Cu2 1.975(12) 2_776 ?
O11 Ce1 2.334(11) 1_655 ?
C1 N1 1.34(2) . ?
C1 C2 1.39(3) . ?
C2 C3 1.37(3) . ?
C2 N2 1.43(2) . ?
C3 C4 1.37(3) . ?
C4 C5 1.37(3) . ?
C4 N4 1.41(2) . ?
C5 N1 1.34(2) . ?
C6 N3 1.35(2) . ?
C6 N2 1.35(3) . ?
C7 C8 1.34(3) . ?
C7 N3 1.39(3) . ?
C8 N2 1.36(3) . ?
C9 C10 1.34(3) . ?
C9 N4 1.39(3) . ?
C10 N5 1.38(3) . ?
C11 N5 1.32(2) . ?
C11 N4 1.35(2) . ?
C12 N6 1.33(2) . ?
C12 C13 1.35(3) . ?
C13 C14 1.36(3) . ?
C13 N9 1.43(2) . ?
C14 C15 1.38(3) . ?
C15 C16 1.36(3) . ?
C15 N7 1.44(2) . ?
C16 N6 1.35(2) . ?
C17 N8 1.33(2) . ?
C17 N7 1.33(2) . ?
C18 C19 1.35(3) . ?
C18 N7 1.35(3) . ?
C19 N8 1.36(3) . ?
C20 N9 1.33(2) . ?
C20 N10 1.35(2) . ?
C21 N9 1.36(2) . ?
C21 C22 1.41(3) . ?
C22 N10 1.37(3) . ?
N5 Cu3 1.936(15) 1_655 ?
N10 Cu2 1.942(15) 1_455 ?

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
O22 W1 O1 103.1(5) . . ?
O22 W1 O18 93.7(6) . . ?
O1 W1 O18 103.1(6) . . ?
O22 W1 O28 94.6(6) . . ?
O1 W1 O28 95.3(6) . . ?
O18 W1 O28 157.5(5) . . ?
O22 W1 O29 166.9(5) . . ?
O1 W1 O29 89.9(5) . . ?
O18 W1 O29 84.5(5) . . ?
O28 W1 O29 82.7(5) . . ?
O22 W1 O38 93.9(5) . . ?
O1 W1 O38 160.4(5) . . ?
O18 W1 O38 85.1(5) . . ?
O28 W1 O38 73.5(5) . . ?
O29 W1 O38 73.0(4) . . ?
O2 W2 O19 103.8(6) . . ?
O2 W2 O18 101.5(6) . . ?
O19 W2 O18 91.8(6) . . ?
O2 W2 O14 100.1(6) . . ?
O19 W2 O14 95.6(6) . . ?
O18 W2 O14 154.8(5) . . ?
O2 W2 O15 94.2(5) . . ?
O19 W2 O15 162.0(6) . . ?
O18 W2 O15 82.8(5) . . ?
O14 W2 O15 82.7(5) . . ?
O2 W2 O37 163.6(5) . . ?
O19 W2 O37 91.8(5) . . ?
O18 W2 O37 82.7(5) . . ?
O14 W2 O37 73.0(5) . . ?
O15 W2 O37 70.5(4) . . ?
O3 W3 O21 100.5(6) . . ?
O3 W3 O35 102.5(6) . . ?
O21 W3 O35 97.5(6) . . ?
O3 W3 O24 97.4(5) . . ?
O21 W3 O24 92.0(6) . . ?
O35 W3 O24 155.8(5) . . ?
O3 W3 O20 94.6(6) . . ?
O21 W3 O20 164.6(6) . . ?
O35 W3 O20 82.4(5) . . ?
O24 W3 O20 82.6(5) . . ?
O3 W3 O39 169.1(5) . . ?
O21 W3 O39 82.2(5) . . ?
O35 W3 O39 87.5(5) . . ?
O24 W3 O39 71.8(5) . . ?
O20 W3 O39 82.4(5) . . ?
O4 W4 O16 101.8(6) . . ?
O4 W4 O13 100.6(6) . . ?
O16 W4 O13 90.3(5) . . ?
O4 W4 O14 100.0(6) . . ?
O16 W4 O14 158.1(5) . . ?
O13 W4 O14 88.3(5) . . ?
O4 W4 O35 101.3(6) . . ?
O16 W4 O35 85.1(5) . . ?
O13 W4 O35 158.1(6) . . ?
O14 W4 O35 88.0(5) . . ?
O4 W4 O37 172.4(6) . . ?
O16 W4 O37 85.2(5) . . ?
O13 W4 O37 76.1(5) . . ?
O14 W4 O37 73.3(5) . . ?
O35 W4 O37 82.2(5) . . ?
O5 W5 O15 103.5(6) . . ?
O5 W5 O17 100.2(6) . . ?
O15 W5 O17 91.6(6) . . ?
O5 W5 O13 101.2(6) . . ?
O15 W5 O13 89.8(5) . . ?
O17 W5 O13 157.6(5) . . ?
O5 W5 O34 101.4(6) . . ?
O15 W5 O34 155.1(5) . . ?
O17 W5 O34 84.2(5) . . ?
O13 W5 O34 85.1(5) . . ?
O5 W5 O37 173.9(6) . . ?
O15 W5 O37 73.8(5) . . ?
O17 W5 O37 85.4(5) . . ?
O13 W5 O37 73.6(4) . . ?
O34 W5 O37 81.4(4) . . ?
O6 W6 O29 102.3(6) . . ?
O6 W6 O17 101.8(6) . . ?
O29 W6 O17 91.0(6) . . ?
O6 W6 O31 100.1(6) . . ?
O29 W6 O31 90.1(5) . . ?
O17 W6 O31 157.2(5) . . ?
O6 W6 O32 100.6(6) . . ?
O29 W6 O32 157.2(5) . . ?
O17 W6 O32 84.3(5) . . ?
O31 W6 O32 85.9(5) . . ?
O6 W6 O38 172.1(6) . . ?
O29 W6 O38 73.9(4) . . ?
O17 W6 O38 85.2(5) . . ?
O31 W6 O38 73.3(5) . . ?
O32 W6 O38 83.4(4) . . ?
O7 W7 O28 100.2(6) . . ?
O7 W7 O33 101.9(6) . . ?
O28 W7 O33 90.8(5) . . ?
O7 W7 O31 101.8(6) . . ?
O28 W7 O31 88.0(5) . . ?
O33 W7 O31 156.1(6) . . ?
O7 W7 O27 100.9(6) . . ?
O28 W7 O27 158.9(6) . . ?
O33 W7 O27 85.2(5) . . ?
O31 W7 O27 87.3(5) . . ?
O7 W7 O38 170.9(5) . . ?
O28 W7 O38 71.5(5) . . ?
O33 W7 O38 82.3(5) . . ?
O31 W7 O38 74.7(5) . . ?
O27 W7 O38 87.4(5) . . ?
O8 W8 O25 104.4(6) . . ?
O8 W8 O27 101.3(6) . . ?
O25 W8 O27 89.0(5) . . ?
O8 W8 O26 99.7(6) . . ?
O25 W8 O26 90.1(5) . . ?
O27 W8 O26 158.6(5) . . ?
O8 W8 O36 98.7(5) . . ?
O25 W8 O36 156.8(6) . . ?
O27 W8 O36 88.2(5) . . ?
O26 W8 O36 84.2(5) . . ?
O8 W8 O12 168.6(5) . . ?
O25 W8 O12 85.1(5) . . ?
O27 W8 O12 84.9(5) . . ?
O26 W8 O12 73.7(5) . . ?
O36 W8 O12 71.7(5) . . ?
O9 W9 O20 104.2(6) . . ?
O9 W9 O26 100.7(6) . . ?
O20 W9 O26 94.9(5) . . ?
O9 W9 O16 101.3(6) . . ?
O20 W9 O16 86.4(5) . . ?
O26 W9 O16 156.9(5) . . ?
O9 W9 O30 98.5(6) . . ?
O20 W9 O30 156.7(6) . . ?
O26 W9 O30 85.9(5) . . ?
O16 W9 O30 84.1(5) . . ?
O9 W9 O12 168.3(6) . . ?
O20 W9 O12 86.7(5) . . ?
O26 W9 O12 73.7(5) . . ?
O16 W9 O12 83.4(5) . . ?
O30 W9 O12 71.2(5) . . ?
O10 W10 O23 100.0(6) . . ?
O10 W10 O24 97.9(6) . . ?
O23 W10 O24 93.9(5) . . ?
O10 W10 O33 101.8(6) . . ?
O23 W10 O33 93.7(5) . . ?
O24 W10 O33 157.3(5) . . ?
O10 W10 O25 94.3(5) . . ?
O23 W10 O25 165.6(5) . . ?
O24 W10 O25 86.2(5) . . ?
O33 W10 O25 81.2(5) . . ?
O10 W10 O39 171.2(5) . . ?
O23 W10 O39 82.0(5) . . ?
O24 W10 O39 73.3(5) . . ?
O33 W10 O39 86.6(5) . . ?
O25 W10 O39 84.2(5) . . ?
O11 W11 O32 102.0(5) . . ?
O11 W11 O34 99.0(5) . . ?
O32 W11 O34 87.0(5) . . ?
O11 W11 O36 98.6(5) . . ?
O32 W11 O36 90.0(5) . . ?
O34 W11 O36 162.4(5) . . ?
O11 W11 O30 97.1(5) . . ?
O32 W11 O30 160.8(5) . . ?
O34 W11 O30 89.0(6) . . ?
O36 W11 O30 88.2(5) . . ?
O11 W11 O12 170.3(5) . . ?
O32 W11 O12 85.9(5) . . ?
O34 W11 O12 86.9(5) . . ?
O36 W11 O12 75.6(5) . . ?
O30 W11 O12 75.1(5) . . ?
N1 Cu1 N6 173.2(6) . . ?
N1 Cu1 O3 94.0(5) . 1_565 ?
N6 Cu1 O3 89.9(5) . 1_565 ?
N1 Cu1 O1 85.4(6) . . ?
N6 Cu1 O1 89.5(6) . . ?
O3 Cu1 O1 166.8(5) 1_565 . ?
N1 Cu1 O4W 90.8(6) . . ?
N6 Cu1 O4W 94.6(6) . . ?
O3 Cu1 O4W 92.8(5) 1_565 . ?
O1 Cu1 O4W 100.4(5) . . ?
N10 Cu2 N8 94.5(7) 1_655 . ?
N10 Cu2 O10 168.5(6) 1_655 2_776 ?
N8 Cu2 O10 89.1(6) . 2_776 ?
N10 Cu2 O5W 88.3(7) 1_655 . ?
N8 Cu2 O5W 165.9(6) . . ?
O10 Cu2 O5W 85.7(5) 2_776 . ?
N10 Cu2 O8 94.9(6) 1_655 1_565 ?
N8 Cu2 O8 94.3(6) . 1_565 ?
O10 Cu2 O8 95.8(5) 2_776 1_565 ?
O5W Cu2 O8 99.2(5) . 1_565 ?
N5 Cu3 N5 180.000 2_775 1_455 ?
N5 Cu3 N3 90.2(7) 2_775 2_675 ?
N5 Cu3 N3 89.8(7) 1_455 2_675 ?
N5 Cu3 N3 89.8(7) 2_775 . ?
N5 Cu3 N3 90.2(7) 1_455 . ?
N3 Cu3 N3 180.0 2_675 . ?
O22 Ce1 O19 73.1(5) . . ?
O22 Ce1 O21 122.0(5) . . ?
O19 Ce1 O21 78.9(5) . . ?
O22 Ce1 O23 79.0(4) . . ?
O19 Ce1 O23 121.0(5) . . ?
O21 Ce1 O23 73.8(5) . . ?
O22 Ce1 O11 136.6(5) . 1_455 ?
O19 Ce1 O11 150.3(5) . 1_455 ?
O21 Ce1 O11 80.9(4) . 1_455 ?
O23 Ce1 O11 72.9(4) . 1_455 ?
O22 Ce1 O2W 88.9(7) . . ?
O19 Ce1 O2W 82.2(7) . . ?
O21 Ce1 O2W 136.0(7) . . ?
O23 Ce1 O2W 148.2(6) . . ?
O11 Ce1 O2W 97.8(7) 1_455 . ?
O22 Ce1 O1W 146.3(5) . . ?
O19 Ce1 O1W 80.7(5) . . ?
O21 Ce1 O1W 71.4(6) . . ?
O23 Ce1 O1W 133.7(5) . . ?
O11 Ce1 O1W 72.3(5) 1_455 . ?
O2W Ce1 O1W 66.5(8) . . ?
O22 Ce1 O3W 71.5(5) . . ?
O19 Ce1 O3W 135.6(5) . . ?
O21 Ce1 O3W 143.8(5) . . ?
O23 Ce1 O3W 77.0(6) . . ?
O11 Ce1 O3W 70.3(5) 1_455 . ?
O2W Ce1 O3W 71.2(7) . . ?
O1W Ce1 O3W 117.6(6) . . ?
O37 Si1 O38 108.3(6) . . ?
O37 Si1 O12 110.1(7) . . ?
O38 Si1 O12 108.8(7) . . ?
O37 Si1 O39 111.9(7) . . ?
O38 Si1 O39 110.0(6) . . ?
O12 Si1 O39 107.9(6) . . ?
W1 O1 Cu1 112.6(6) . . ?
W3 O3 Cu1 139.8(7) . 1_545 ?
W8 O8 Cu2 143.1(8) . 1_545 ?
W10 O10 Cu2 128.2(7) . 2_776 ?
W11 O11 Ce1 146.8(6) . 1_655 ?
Si1 O12 W11 125.6(6) . . ?
Si1 O12 W8 124.4(6) . . ?
W11 O12 W8 93.2(4) . . ?
Si1 O12 W9 121.1(7) . . ?
W11 O12 W9 92.9(4) . . ?
W8 O12 W9 90.3(4) . . ?
W4 O13 W5 120.4(6) . . ?
W2 O14 W4 121.7(7) . . ?
W5 O15 W2 123.7(6) . . ?
W4 O16 W9 150.7(7) . . ?
W5 O17 W6 153.8(7) . . ?
W1 O18 W2 141.8(6) . . ?
W2 O19 Ce1 158.8(8) . . ?
W9 O20 W3 151.4(7) . . ?
W3 O21 Ce1 137.0(7) . . ?
W1 O22 Ce1 157.7(8) . . ?
W10 O23 Ce1 136.8(7) . . ?
W10 O24 W3 118.0(6) . . ?
W8 O25 W10 150.4(7) . . ?
W9 O26 W8 122.0(6) . . ?
W8 O27 W7 147.7(7) . . ?
W7 O28 W1 122.0(7) . . ?
W6 O29 W1 119.9(6) . . ?
W11 O30 W9 120.8(6) . . ?
W7 O31 W6 122.4(7) . . ?
W11 O32 W6 150.5(8) . . ?
W7 O33 W10 155.5(7) . . ?
W11 O34 W5 151.0(7) . . ?
W3 O35 W4 154.4(7) . . ?
W11 O36 W8 119.5(6) . . ?
Si1 O37 W4 124.6(6) . . ?
Si1 O37 W2 123.1(6) . . ?
W4 O37 W2 91.9(4) . . ?
Si1 O37 W5 125.5(7) . . ?
W4 O37 W5 89.7(4) . . ?
W2 O37 W5 92.1(4) . . ?
Si1 O38 W1 124.1(7) . . ?
Si1 O38 W7 123.9(6) . . ?
W1 O38 W7 92.8(4) . . ?
Si1 O38 W6 123.8(6) . . ?
W1 O38 W6 93.2(4) . . ?
W7 O38 W6 89.5(4) . . ?
Si1 O39 W10 127.6(7) . . ?
Si1 O39 W3 126.2(7) . . ?
W10 O39 W3 94.9(4) . . ?
N1 C1 C2 121.4(17) . . ?
C3 C2 C1 120.3(17) . . ?
C3 C2 N2 121.0(17) . . ?
C1 C2 N2 118.6(16) . . ?
C2 C3 C4 117.2(18) . . ?
C5 C4 C3 120.6(17) . . ?
C5 C4 N4 117.6(17) . . ?
C3 C4 N4 121.8(18) . . ?
N1 C5 C4 121.8(17) . . ?
N3 C6 N2 110.7(18) . . ?
C8 C7 N3 110.6(19) . . ?
C7 C8 N2 107(2) . . ?
C10 C9 N4 105.1(18) . . ?
C9 C10 N5 111.1(18) . . ?
N5 C11 N4 111.0(18) . . ?
N6 C12 C13 121.6(18) . . ?
C12 C13 C14 120.8(17) . . ?
C12 C13 N9 120.6(16) . . ?
C14 C13 N9 118.5(17) . . ?
C13 C14 C15 116.7(18) . . ?
C16 C15 C14 121.7(17) . . ?
C16 C15 N7 116.9(15) . . ?
C14 C15 N7 121.4(17) . . ?
N6 C16 C15 119.6(17) . . ?
N8 C17 N7 111.5(17) . . ?
C19 C18 N7 107(2) . . ?
C18 C19 N8 110(2) . . ?
N9 C20 N10 110.8(16) . . ?
N9 C21 C22 104.6(18) . . ?
N10 C22 C21 108.9(19) . . ?
C5 N1 C1 118.7(17) . . ?
C5 N1 Cu1 121.2(12) . . ?
C1 N1 Cu1 119.8(12) . . ?
C6 N2 C8 107.9(17) . . ?
C6 N2 C2 125.0(16) . . ?
C8 N2 C2 127.0(18) . . ?
C6 N3 C7 104.0(18) . . ?
C6 N3 Cu3 127.8(15) . . ?
C7 N3 Cu3 128.1(14) . . ?
C11 N4 C9 107.5(16) . . ?
C11 N4 C4 124.5(17) . . ?
C9 N4 C4 127.9(16) . . ?
C11 N5 C10 105.2(16) . . ?
C11 N5 Cu3 128.0(14) . 1_655 ?
C10 N5 Cu3 126.0(14) . 1_655 ?
C12 N6 C16 119.5(17) . . ?
C12 N6 Cu1 120.9(12) . . ?
C16 N6 Cu1 119.6(12) . . ?
C17 N7 C18 107.1(17) . . ?
C17 N7 C15 125.4(16) . . ?
C18 N7 C15 127.5(17) . . ?
C17 N8 C19 104.9(18) . . ?
C17 N8 Cu2 125.2(14) . . ?
C19 N8 Cu2 129.8(14) . . ?
C20 N9 C21 109.7(16) . . ?
C20 N9 C13 127.3(16) . . ?
C21 N9 C13 123.0(17) . . ?
C20 N10 C22 105.7(16) . . ?
C20 N10 Cu2 128.7(13) . 1_455 ?
C22 N10 Cu2 124.7(13) . 1_455 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.533
_refine_diff_density_min         -7.334
_refine_diff_density_rms         0.422
_database_code_depnum_ccdc_archive 'CCDC 1005807'
