# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1891064'
loop_
_audit_author_name
_audit_author_address
'Junwei Zhao'
;Henan University
China
;
_audit_update_record             
;
2019-02-11 deposited with the CCDC.	2019-02-14 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT201_4                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......   4 Report 
RESPONSE: Due to the large structure and the existence of a large 
 amount of weight atoms, the intensity data are not very good, 
 leading to the ADP max/min ratio of some water molecules, and it is 
very difficult to refine this large structure, therefore, 
 in the final refinement, the W, Ge, Cu and Dy atoms were refined 
anisotropically, some O atoms and water molecules were
 refined isotropically.
;


_vrf_PLAT220_4                   
;
PROBLEM:  Non-Solvent  Resd 1  O   Ueq(max)/Ueq(min) Range   9.1 Ratio 
RESPONSE: In polyoxometalate compounds, the Ueq of oxygen atoms in
 the POM skeleton is small due to multiple covalent bonds, whereas the 
Ueq of these dissociative water oxygen atoms is biggish without 
the constraint of covalent bonds, which lead to the 
non-solvent O Ueq(max)/Ueq(min) range. 
;


_vrf_PLAT306_4                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O10W Check
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

_vrf_PLAT342_4                   
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0304 Ang.
RESPONSE: The alert derives from shading of reciprocal space
 by the pressure cell, and it is unavoidable in high pressure
 crystal structure determinations.
;

_vrf_PLAT430_4                   
;
PROBLEM: Short Inter D...A Contact  O5W     ..O16W   .  2.40 Ang. 
RESPONSE: In the crystal structure, there are a number of 
short contacts between Ow(H2O) and O(POM) or Ow(H2O) in the range
 of 2.40-2.87 Ang, which indicate extensive hydrogen bonding 
interactions among them. 
;


# end Validation Reply Form


_audit_creation_date             2019-02-09
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'Ge O40 W12, C6 H4 Cu0.5 Dy N O9, C18 H12 Cu2 N3 O8, C6 H4 Cu0.5 N O2, 7(O)'
_chemical_formula_sum            'C30 H52 Cu3 Dy Ge N5 O66 W12'
_chemical_formula_weight         4170.68
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ge Ge 0.1547 1.8001 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.241(4)
_cell_length_b                   16.539(4)
_cell_length_c                   35.111(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.086(4)
_cell_angle_gamma                90.00
_cell_volume                     7570(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4730
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.955
_cell_measurement_theta_min      2.447
_exptl_absorpt_coefficient_mu    20.455
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1664 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.3472.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            mazarine
_exptl_crystal_density_diffrn    3.659
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            37973
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                9046
_reflns_number_total             13124
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         4.647
_refine_diff_density_min         -2.712
_refine_diff_density_rms         0.335
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         13124
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0498
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0329P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1127
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 W6-O1
 1.9 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(O27)
\\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(O34) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: W5(0.95) W5'(0.05) W8(0.95) W8'(0.05) W12(0.95) W12'(0.05)
 Fixed Uiso: O13W(0.15858) O14W(0.1508) O15W(0.16819) O16W(0.16599)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C7(H7A), C8(H8A), C9(H9A), C10(H10A),
 C13(H13A), C14(H14A), C15(H15A), C16(H16A), C19(H19A), C20(H20A), C21(H21A),
 C22(H22A), C25(H25A), C26(H26A), C27(H27A), C28(H28A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
W1 W 0.75378(5) 1.15295(4) 0.320958(18) 0.01943(15) Uani 1 d . . 1 . . .
W2 W 0.75686(5) 1.35450(4) 0.32829(2) 0.02587(17) Uani 1 d . . 1 . . .
W3 W 0.80854(5) 1.12463(4) 0.425987(19) 0.02130(16) Uani 1 d . . 1 . . .
W4 W 0.54919(5) 1.26084(4) 0.279534(19) 0.02308(16) Uani 1 d . . 1 . . .
W5 W 0.81245(8) 1.35120(6) 0.43374(3) 0.0232(2) Uani 0.95 d . . 1 . . .
W5' W 0.7851(19) 1.3344(15) 0.4383(8) 0.041(8) Uiso 0.05 d . . 1 . . .
W6 W 0.59156(5) 1.11842(4) 0.46271(2) 0.02814(18) Uani 1 d . . 1 D . .
W7 W 0.36533(5) 1.23755(4) 0.41753(2) 0.02675(17) Uani 1 d . . 1 . . .
W8 W 0.37648(6) 1.15030(6) 0.33200(3) 0.0231(2) Uani 0.95 d . . 1 . . .
W8' W 0.3756(14) 1.1336(11) 0.3188(5) 0.016(5) Uiso 0.05 d . . 1 . . .
W9 W 0.59538(5) 1.34210(4) 0.47062(2) 0.02894(18) Uani 1 d . . 1 . . .
W10 W 0.37628(5) 1.34892(4) 0.338964(19) 0.02478(17) Uani 1 d . . 1 . . .
W11 W 0.60513(5) 1.02968(4) 0.37780(2) 0.02569(17) Uani 1 d . . 1 . . .
W12 W 0.60925(8) 1.45626(5) 0.39292(3) 0.0253(2) Uani 0.95 d . . 1 . . .
W12' W 0.5712(16) 1.4448(14) 0.3940(7) 0.034(7) Uiso 0.05 d . . 1 . . .
Ge1 Ge 0.60002(12) 1.24353(9) 0.38176(4) 0.0162(3) Uani 1 d . . 1 . . .
Dy1 Dy 1.14682(8) 0.77558(6) 0.39711(3) 0.0452(3) Uani 1 d . . 1 . . .
Cu1 Cu 1.0000 1.0000 0.5000 0.0337(7) Uani 1 d . . 2 S T P
Cu2 Cu 0.08697(18) 1.20906(14) 0.26735(7) 0.0413(6) Uani 1 d . . 1 . . .
Cu3 Cu 0.21737(16) 1.49517(12) 0.25723(6) 0.0309(5) Uani 1 d . . 1 . . .
Cu4 Cu 1.0000 1.5000 0.5000 0.0336(7) Uani 1 d . . 2 S T P
O1W O 1.2264(16) 0.8394(13) 0.4542(6) 0.111(7) Uiso 1 d . . 1 . . .
O2W O 1.0357(14) 0.8542(11) 0.3519(5) 0.095(6) Uani 1 d . . 1 . . .
O3W O 1.2503(19) 0.8730(14) 0.3737(7) 0.136(8) Uiso 1 d . . 1 . . .
O4W O 1.1879(14) 0.7251(12) 0.3406(5) 0.093(6) Uani 1 d . . 1 . . .
O5W O 1.3155(19) 0.7246(13) 0.4135(7) 0.128(8) Uiso 1 d . . 1 . . .
O6W O 1.0224(13) 0.6838(10) 0.3738(4) 0.074(5) Uani 1 d . . 1 . . .
O7W O 1.1474(11) 0.6753(9) 0.4469(4) 0.066(4) Uani 1 d . . 1 . . .
O8W O -0.0801(12) 1.2300(9) 0.2381(4) 0.070(5) Uani 1 d . . 1 . . .
O9W O 0.0747(10) 1.4925(8) 0.2651(4) 0.054(4) Uani 1 d . . 1 . . .
O1 O 0.6231(7) 1.2238(4) 0.4789(3) 0.015(2) Uiso 1 d . . 1 D . .
O2 O 0.4786(8) 1.4166(6) 0.3699(3) 0.033(3) Uani 1 d . . 1 . . .
O3 O 0.6513(8) 1.2512(5) 0.3405(3) 0.017(2) Uani 1 d . . 1 . . .
O4 O 0.8168(8) 1.2537(6) 0.3152(3) 0.025(3) Uani 1 d . . 1 . . .
O5 O 0.6573(9) 1.0767(6) 0.3363(3) 0.031(3) Uani 1 d . . 1 . . .
O6 O 0.8223(8) 1.2376(6) 0.4388(3) 0.025(3) Uani 1 d . . 1 . . .
O7 O 0.3181(8) 1.1601(7) 0.3781(3) 0.032(3) Uani 1 d . . 1 . . .
O8 O 0.6538(8) 1.1819(6) 0.2772(3) 0.025(3) Uani 1 d . . 1 . . .
O9 O 0.9272(8) 1.0876(7) 0.4445(3) 0.030(3) Uani 1 d . . 1 . . .
O10W O 0.1298(15) 0.4367(10) 0.1379(5) 0.096(6) Uani 1 d . . 1 . . .
O11W O 1.124(2) 0.8922(15) 0.2641(7) 0.147(9) Uiso 1 d . . 1 . . .
O12W O -0.6698(15) 0.9989(11) 0.4212(5) 0.098(6) Uiso 1 d . . 1 . . .
O13W O 0.505(2) 0.7682(16) 0.3699(8) 0.159 Uiso 1 d . . 1 . . .
O14W O 1.358(2) 0.5664(16) 0.4058(7) 0.151 Uiso 1 d . . 1 . . .
O15W O 1.089(2) 0.5423(17) 0.3454(8) 0.168 Uiso 1 d . . 1 . . .
O16W O 0.442(2) 0.8285(17) 0.4290(8) 0.166 Uiso 1 d . . 1 . . .
O10 O 0.8357(10) 1.4213(7) 0.3124(4) 0.046(4) Uani 1 d . . 1 . . .
O11 O 0.4689(8) 1.2468(6) 0.3713(3) 0.023(2) Uani 1 d . . 1 . . .
O12 O 0.7431(8) 1.3565(6) 0.4781(3) 0.028(3) Uani 1 d . . 1 . . .
O13 O 0.6639(8) 1.4218(6) 0.3482(3) 0.027(3) Uani 1 d . . 1 . . .
O14 O 0.8219(8) 1.3386(6) 0.3811(3) 0.028(3) Uani 1 d . . 1 . . .
O15 O 0.2921(9) 1.4198(7) 0.3176(3) 0.038(3) Uani 1 d . . 1 . . .
O16 O 0.6552(8) 1.3408(7) 0.2823(3) 0.032(3) Uani 1 d . . 1 . . .
O17 O 0.2715(9) 1.2320(7) 0.4447(3) 0.041(3) Uani 1 d . . 1 . . .
O18 O 0.4748(9) 1.0756(7) 0.3578(3) 0.035(3) Uani 1 d . . 1 . . .
O19 O 0.7377(8) 1.1041(7) 0.4677(3) 0.028(3) Uani 1 d . . 1 . . .
O20 O 0.7454(7) 1.0266(6) 0.4039(3) 0.021(2) Uani 1 d . . 1 . U .
O21 O 0.4570(8) 1.3115(6) 0.4453(3) 0.025(3) Uani 1 d . . 1 . U .
O22 O 0.4599(8) 1.1534(7) 0.4401(3) 0.032(3) Uani 1 d . . 1 . U .
O23 O 0.7490(9) 1.4544(7) 0.4193(3) 0.036(3) Uani 1 d . . 1 . . .
O24 O 0.3173(8) 1.3247(7) 0.3835(3) 0.028(3) Uani 1 d . . 1 . . .
O25 O 0.4715(8) 1.3358(6) 0.3039(3) 0.029(3) Uani 1 d . . 1 . . .
O26 O 0.1188(9) 1.3226(7) 0.2586(3) 0.039(3) Uani 1 d . . 1 . . .
O27 O 0.6422(7) 1.3256(6) 0.4115(3) 0.019(2) Uani 1 d . . 1 . U .
O28 O 0.9300(9) 1.3829(7) 0.4551(3) 0.039(3) Uani 1 d . . 1 . . .
O29 O 0.2058(9) 1.4007(7) 0.2244(3) 0.034(3) Uani 1 d . . 1 . . .
O30 O 0.5746(8) 1.4420(6) 0.4441(3) 0.026(3) Uani 1 d . . 1 . . .
O31 O 1.0579(10) 0.9270(8) 0.4655(4) 0.046(3) Uani 1 d . . 1 . . .
O32 O 0.8186(8) 1.1511(6) 0.3746(3) 0.025(3) Uani 1 d . . 1 . . .
O33 O 0.6400(8) 1.1543(6) 0.4056(3) 0.021(2) Uani 1 d . . 1 . . .
O34 O 0.8300(8) 1.0894(6) 0.2995(3) 0.028(3) Uani 1 d . . 1 . U .
O35 O 0.3129(8) 1.2521(7) 0.3159(3) 0.030(3) Uani 1 d . . 1 . . .
O36 O 0.5886(9) 0.9307(6) 0.3625(3) 0.037(3) Uani 1 d . . 1 . . .
O37 O 0.5936(9) 1.5575(7) 0.3867(3) 0.040(3) Uani 1 d . . 1 . . .
O38 O 1.0086(11) 0.8206(8) 0.4264(4) 0.057(4) Uani 1 d . . 1 . . .
O39 O 0.4679(7) 1.1791(6) 0.2969(3) 0.019(2) Uani 1 d . . 1 . . .
O43 O 0.2945(9) 1.0868(7) 0.3044(3) 0.038(3) Uani 1 d . . 1 . . .
O44 O 0.5704(8) 1.0267(7) 0.4289(3) 0.035(3) Uani 1 d . . 1 . . .
O45 O 0.9883(9) 1.5668(8) 0.4539(4) 0.043(3) Uani 1 d . . 1 . . .
O46 O 0.5723(8) 1.0779(7) 0.5047(3) 0.032(3) Uani 1 d . . 1 . U .
O47 O 0.0599(10) 1.0934(9) 0.2750(5) 0.064(4) Uani 1 d . . 1 . . .
O50 O 0.5770(9) 1.3699(8) 0.5161(3) 0.042(3) Uani 1 d . . 1 . . .
O52 O 0.4939(9) 1.2690(7) 0.2319(3) 0.033(3) Uani 1 d . . 1 . . .
O53 O 0.2380(10) 1.5890(7) 0.2895(4) 0.042(3) Uani 1 d . . 1 . . .
O61 O 0.8787(12) 1.6456(9) 0.4160(4) 0.061(4) Uani 1 d . . 1 . . .
O64 O 0.0692(14) 1.0038(10) 0.3227(6) 0.109(7) Uani 1 d . . 1 . . .
O68 O 0.3634(10) 1.6589(9) 0.3248(4) 0.057(4) Uani 1 d . . 1 . . .
N1 N 0.8752(11) 0.9307(9) 0.4875(4) 0.033(4) Uani 1 d . . 1 . . .
N2 N 0.0705(12) 1.2181(12) 0.3213(6) 0.060(5) Uani 1 d . . 1 . . .
N3 N 0.1508(11) 1.1913(10) 0.2209(4) 0.038(4) Uani 1 d . . 1 . . .
N4 N 0.3636(11) 1.5058(7) 0.2547(4) 0.026(3) Uani 1 d . . 1 . . .
N5 N 0.8598(12) 1.5412(8) 0.5021(4) 0.036(4) Uani 1 d . . 1 . . .
C1 C 0.7871(14) 0.9391(11) 0.5017(6) 0.041(5) Uani 1 d . . 1 . . .
H1A H 0.7814 0.9753 0.5215 0.049 Uiso 1 calc . . 1 R . .
C2 C 0.7047(18) 0.8898(12) 0.4847(7) 0.056(6) Uani 1 d . . 1 . . .
H2A H 0.6422 0.8923 0.4934 0.068 Uiso 1 calc . . 1 R . .
C3 C 0.7172(18) 0.8390(13) 0.4559(7) 0.065(7) Uani 1 d . . 1 . . .
H3A H 0.6616 0.8084 0.4440 0.078 Uiso 1 calc . . 1 R . .
C4 C 0.8057(15) 0.8313(12) 0.4438(7) 0.049(6) Uani 1 d . . 1 . . .
H4A H 0.8142 0.7942 0.4248 0.059 Uiso 1 calc . . 1 R . .
C5 C 0.8818(14) 0.8785(11) 0.4599(6) 0.037(5) Uani 1 d . . 1 . . .
C6 C 0.9908(15) 0.8733(13) 0.4493(6) 0.046(5) Uani 1 d . . 1 . . .
C7 C 0.0690(16) 1.2859(17) 0.3406(7) 0.061(6) Uani 1 d . . 1 . . .
H7A H 0.0695 1.3351 0.3279 0.074 Uiso 1 calc . . 1 R . .
C8 C 0.0667(17) 1.2844(16) 0.3820(7) 0.067(7) Uani 1 d . . 1 . U .
H8A H 0.0675 1.3318 0.3963 0.081 Uiso 1 calc . . 1 R . .
C9 C 0.0634(19) 1.2122(17) 0.3983(8) 0.072(8) Uani 1 d . . 1 . U .
H9A H 0.0615 1.2080 0.4246 0.087 Uiso 1 calc . . 1 R . .
C10 C 0.0629(17) 1.146(2) 0.3768(8) 0.095(11) Uani 1 d . . 1 . . .
H10A H 0.0586 1.0967 0.3890 0.114 Uiso 1 calc . . 1 R . .
C11 C 0.0684(18) 1.0765(17) 0.3108(9) 0.071(7) Uani 1 d . . 1 . U .
C12 C 0.0681(16) 1.1447(14) 0.3384(6) 0.053(6) Uani 1 d . . 1 . U .
C13 C 0.1643(15) 1.1235(11) 0.2013(6) 0.043(5) Uani 1 d . . 1 . . .
H13A H 0.1358 1.0758 0.2086 0.051 Uiso 1 calc . . 1 R . .
C14 C 0.2140(17) 1.1206(12) 0.1732(6) 0.049(6) Uani 1 d . . 1 . . .
H14A H 0.2215 1.0720 0.1607 0.059 Uiso 1 calc . . 1 R . .
C15 C 0.2568(15) 1.1914(13) 0.1615(6) 0.048(5) Uani 1 d . . 1 . . .
H15A H 0.2909 1.1899 0.1405 0.057 Uiso 1 calc . . 1 R . .
C16 C 0.2498(13) 1.2644(11) 0.1805(5) 0.034(4) Uani 1 d . . 1 . . .
H16A H 0.2827 1.3114 0.1747 0.041 Uiso 1 calc . . 1 R . .
C17 C 0.1883(14) 1.2609(10) 0.2094(6) 0.036(5) Uani 1 d . . 1 . . .
C18 C 0.1716(13) 1.3299(9) 0.2326(5) 0.028(4) Uani 1 d . . 1 . . .
C19 C 0.4207(14) 1.4654(10) 0.2341(4) 0.029(4) Uani 1 d . . 1 . . .
H19A H 0.3887 1.4279 0.2162 0.035 Uiso 1 calc . . 1 R . .
C20 C 0.5275(16) 1.4759(11) 0.2376(5) 0.043(5) Uani 1 d . . 1 . . .
H20A H 0.5659 1.4464 0.2227 0.051 Uiso 1 calc . . 1 R . .
C21 C 0.5723(17) 1.5321(12) 0.2644(6) 0.051(6) Uani 1 d . . 1 . . .
H21A H 0.6422 1.5426 0.2672 0.061 Uiso 1 calc . . 1 R . .
C22 C 0.5130(13) 1.5734(11) 0.2875(5) 0.033(4) Uani 1 d . . 1 . . .
H22A H 0.5431 1.6097 0.3063 0.040 Uiso 1 calc . . 1 R . .
C23 C 0.4124(11) 1.5593(9) 0.2818(4) 0.023(4) Uani 1 d . . 1 . . .
C24 C 0.3391(15) 1.6067(12) 0.3010(6) 0.039(5) Uani 1 d . . 1 . . .
C25 C 0.8012(16) 1.5297(13) 0.5280(6) 0.052(6) Uani 1 d . . 1 . . .
H25A H 0.8254 1.4977 0.5494 0.062 Uiso 1 calc . . 1 R . .
C26 C 0.7054(19) 1.5631(15) 0.5246(9) 0.078(8) Uani 1 d . . 1 . . .
H26A H 0.6641 1.5560 0.5432 0.093 Uiso 1 calc . . 1 R . .
C27 C 0.6746(18) 1.6083(13) 0.4913(8) 0.061(6) Uani 1 d . . 1 . . .
H27A H 0.6094 1.6311 0.4870 0.073 Uiso 1 calc . . 1 R . .
C28 C 0.7336(16) 1.6200(14) 0.4659(6) 0.056(6) Uani 1 d . . 1 . . .
H28A H 0.7103 1.6505 0.4438 0.067 Uiso 1 calc . . 1 R . .
C29 C 0.8250(13) 1.5891(10) 0.4713(4) 0.027(4) Uani 1 d . . 1 . . .
C30 C 0.9039(16) 1.6068(11) 0.4462(5) 0.039(5) Uani 1 d . . 1 . . .


_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 O3 2.298(9) . ?
W1 O4 1.891(10) . ?
W1 O5 1.938(11) . ?
W1 O8 1.905(11) . ?
W1 O32 1.929(10) . ?
W1 O34 1.721(10) . ?
W2 O3 2.296(9) . ?
W2 O4 1.936(10) . ?
W2 O10 1.680(11) . ?
W2 O13 1.883(10) . ?
W2 O14 1.920(11) . ?
W2 O16 1.925(12) . ?
W3 O6 1.923(10) . ?
W3 O9 1.705(11) . ?
W3 O19 1.903(10) . ?
W3 O20 1.924(10) . ?
W3 O32 1.882(10) . ?
W3 O33 2.274(10) . ?
W4 O3 2.330(10) . ?
W4 O8 1.915(11) . ?
W4 O16 1.919(11) . ?
W4 O25 1.906(10) . ?
W4 O39 1.894(10) . ?
W4 O52 1.709(11) . ?
W5 W5' 0.50(2) . ?
W5 O6 1.889(10) . ?
W5 O12 1.943(11) . ?
W5 O14 1.887(11) . ?
W5 O23 1.930(12) . ?
W5 O27 2.292(10) . ?
W5 O28 1.690(12) . ?
W5' W9 2.94(2) . ?
W5' O6 1.67(3) . ?
W5' O12 1.63(3) . ?
W5' O14 2.15(3) . ?
W5' O23 2.12(3) . ?
W5' O27 1.97(3) . ?
W5' O28 2.07(3) . ?
W6 O1 1.858(7) . ?
W6 O19 1.927(11) . ?
W6 O22 1.876(11) . ?
W6 O33 2.289(9) . ?
W6 O44 1.916(12) . ?
W6 O46 1.680(10) . ?
W7 O7 1.909(11) . ?
W7 O11 2.305(10) . ?
W7 O17 1.697(11) . ?
W7 O21 1.873(11) . ?
W7 O22 1.946(11) . ?
W7 O24 1.909(11) . ?
W8 W8' 0.538(16) . ?
W8 O7 1.919(11) . ?
W8 O11 2.315(11) . ?
W8 O18 1.905(11) . ?
W8 O35 1.923(10) . ?
W8 O39 1.932(9) . ?
W8 O43 1.689(11) . ?
W8' O7 2.379(19) . ?
W8' O18 1.97(2) . ?
W8' O35 2.12(2) . ?
W8' O39 1.73(2) . ?
W8' O43 1.35(2) . ?
W9 W12' 3.15(2) . ?
W9 O1 2.003(8) . ?
W9 O12 1.942(10) . ?
W9 O21 1.958(11) . ?
W9 O27 2.286(10) . ?
W9 O30 1.893(11) . ?
W9 O50 1.719(12) . ?
W10 O2 1.937(12) . ?
W10 O11 2.271(10) . ?
W10 O15 1.698(11) . ?
W10 O24 1.908(10) . ?
W10 O25 1.923(10) . ?
W10 O35 1.919(11) . ?
W11 O5 1.886(11) . ?
W11 O18 1.904(11) . ?
W11 O20 1.922(10) . ?
W11 O33 2.292(10) . ?
W11 O36 1.725(11) . ?
W11 O44 1.930(10) . ?
W12 W12' 0.55(2) . ?
W12 O2 1.894(12) . ?
W12 O13 1.927(10) . ?
W12 O23 1.919(12) . ?
W12 O27 2.276(10) . ?
W12 O30 1.944(10) . ?
W12 O37 1.696(12) . ?
W12' O2 1.44(2) . ?
W12' O13 2.22(2) . ?
W12' O23 2.37(2) . ?
W12' O27 2.22(3) . ?
W12' O30 1.75(2) . ?
W12' O37 1.91(3) . ?
Ge1 O3 1.707(9) . ?
Ge1 O11 1.712(10) . ?
Ge1 O27 1.744(10) . ?
Ge1 O33 1.733(10) . ?
Dy1 O1W 2.35(2) . ?
Dy1 O2W 2.358(17) . ?
Dy1 O3W 2.35(2) . ?
Dy1 O4W 2.303(16) . ?
Dy1 O5W 2.36(2) . ?
Dy1 O6W 2.284(15) . ?
Dy1 O7W 2.408(14) . ?
Dy1 O38 2.370(13) . ?
Cu1 O31 1.959(12) . ?
Cu1 O31 1.959(12) 3_776 ?
Cu1 N1 1.996(15) . ?
Cu1 N1 1.996(15) 3_776 ?
Cu2 O8W 2.297(15) . ?
Cu2 O26 1.961(12) . ?
Cu2 O47 1.973(14) . ?
Cu2 N2 1.95(2) . ?
Cu2 N3 1.987(15) . ?
Cu3 O9W 1.958(13) . ?
Cu3 O29 1.932(11) . ?
Cu3 O53 1.914(12) . ?
Cu3 N4 1.962(14) . ?
Cu4 O45 1.943(12) . ?
Cu4 O45 1.943(12) 3_786 ?
Cu4 N5 1.991(15) 3_786 ?
Cu4 N5 1.991(15) . ?
O26 C18 1.248(19) . ?
O29 C18 1.305(19) . ?
O31 C6 1.31(2) . ?
O38 C6 1.24(2) . ?
O45 C30 1.29(2) . ?
O47 C11 1.27(3) . ?
O53 C24 1.36(2) . ?
O61 C30 1.23(2) . ?
O64 C11 1.27(3) . ?
O68 C24 1.21(2) . ?
N1 C1 1.35(2) . ?
N1 C5 1.31(2) . ?
N2 C7 1.31(3) . ?
N2 C12 1.36(2) . ?
N3 C13 1.34(2) . ?
N3 C17 1.34(2) . ?
N4 C19 1.316(18) . ?
N4 C23 1.38(2) . ?
N5 C25 1.31(2) . ?
N5 C29 1.36(2) . ?
C1 C2 1.41(3) . ?
C2 C3 1.35(3) . ?
C3 C4 1.32(3) . ?
C4 C5 1.32(3) . ?
C5 C6 1.56(2) . ?
C7 C8 1.46(3) . ?
C8 C9 1.33(3) . ?
C9 C10 1.33(4) . ?
C10 C12 1.36(3) . ?
C11 C12 1.49(3) . ?
C13 C14 1.28(3) . ?
C14 C15 1.39(3) . ?
C15 C16 1.39(3) . ?
C16 C17 1.41(2) . ?
C17 C18 1.44(2) . ?
C19 C20 1.41(3) . ?
C20 C21 1.38(3) . ?
C21 C22 1.40(2) . ?
C22 C23 1.33(2) . ?
C23 C24 1.50(2) . ?
C25 C26 1.37(3) . ?
C26 C27 1.39(3) . ?
C27 C28 1.30(3) . ?
C28 C29 1.30(2) . ?
C29 C30 1.51(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 W1 O3 72.8(4) . . ?
O4 W1 O5 158.2(4) . . ?
O4 W1 O8 87.1(5) . . ?
O4 W1 O32 89.4(5) . . ?
O5 W1 O3 85.7(4) . . ?
O8 W1 O3 72.5(4) . . ?
O8 W1 O5 89.4(5) . . ?
O8 W1 O32 156.8(4) . . ?
O32 W1 O3 84.5(4) . . ?
O32 W1 O5 85.4(4) . . ?
O34 W1 O3 170.3(4) . . ?
O34 W1 O4 100.8(5) . . ?
O34 W1 O5 101.0(5) . . ?
O34 W1 O8 100.3(5) . . ?
O34 W1 O32 102.9(5) . . ?
O4 W2 O3 72.1(4) . . ?
O10 W2 O3 170.2(5) . . ?
O10 W2 O4 100.6(5) . . ?
O10 W2 O13 102.6(5) . . ?
O10 W2 O14 102.2(6) . . ?
O10 W2 O16 100.6(6) . . ?
O13 W2 O3 84.9(4) . . ?
O13 W2 O4 156.8(4) . . ?
O13 W2 O14 86.2(4) . . ?
O13 W2 O16 88.5(5) . . ?
O14 W2 O3 84.3(4) . . ?
O14 W2 O4 88.7(4) . . ?
O14 W2 O16 157.3(4) . . ?
O16 W2 O3 73.2(4) . . ?
O16 W2 O4 87.4(5) . . ?
O6 W3 O20 158.4(4) . . ?
O6 W3 O33 85.0(4) . . ?
O9 W3 O6 102.5(5) . . ?
O9 W3 O19 100.9(5) . . ?
O9 W3 O20 99.0(5) . . ?
O9 W3 O32 103.5(5) . . ?
O9 W3 O33 170.1(4) . . ?
O19 W3 O6 91.9(5) . . ?
O19 W3 O20 85.6(4) . . ?
O19 W3 O33 72.1(4) . . ?
O20 W3 O33 73.8(4) . . ?
O32 W3 O6 88.8(4) . . ?
O32 W3 O19 154.9(4) . . ?
O32 W3 O20 84.7(4) . . ?
O32 W3 O33 83.0(4) . . ?
O8 W4 O3 71.6(4) . . ?
O8 W4 O16 86.8(5) . . ?
O16 W4 O3 72.5(4) . . ?
O25 W4 O3 84.5(4) . . ?
O25 W4 O8 156.0(4) . . ?
O25 W4 O16 88.6(5) . . ?
O39 W4 O3 85.7(4) . . ?
O39 W4 O8 89.0(4) . . ?
O39 W4 O16 158.0(4) . . ?
O39 W4 O25 86.5(4) . . ?
O52 W4 O3 170.1(4) . . ?
O52 W4 O8 101.6(5) . . ?
O52 W4 O16 100.4(5) . . ?
O52 W4 O25 102.4(5) . . ?
O52 W4 O39 101.6(5) . . ?
W5' W5 O6 58(3) . . ?
W5' W5 O12 46(3) . . ?
W5' W5 O14 115(3) . . ?
W5' W5 O23 106(3) . . ?
W5' W5 O27 45(3) . . ?
W5' W5 O28 133(3) . . ?
O6 W5 O12 90.2(4) . . ?
O6 W5 O23 157.4(5) . . ?
O6 W5 O27 84.1(4) . . ?
O12 W5 O27 73.0(4) . . ?
O14 W5 O6 88.1(4) . . ?
O14 W5 O12 155.8(5) . . ?
O14 W5 O23 86.6(4) . . ?
O14 W5 O27 82.8(4) . . ?
O23 W5 O12 85.8(5) . . ?
O23 W5 O27 73.5(4) . . ?
O28 W5 O6 102.9(5) . . ?
O28 W5 O12 99.1(5) . . ?
O28 W5 O14 104.9(5) . . ?
O28 W5 O23 99.6(6) . . ?
O28 W5 O27 169.6(5) . . ?
W5 W5' W9 144(4) . . ?
W5 W5' O6 108(4) . . ?
W5 W5' O12 121(4) . . ?
W5 W5' O14 53(3) . . ?
W5 W5' O23 61(3) . . ?
W5 W5' O27 125(4) . . ?
W5 W5' O28 36(3) . . ?
O6 W5' W9 107.9(10) . . ?
O6 W5' O14 85.8(12) . . ?
O6 W5' O23 161.4(16) . . ?
O6 W5' O27 101.1(13) . . ?
O6 W5' O28 96.4(13) . . ?
O12 W5' W9 38.4(7) . . ?
O12 W5' O6 110.4(15) . . ?
O12 W5' O14 163.6(17) . . ?
O12 W5' O23 88.2(12) . . ?
O12 W5' O27 89.0(12) . . ?
O12 W5' O28 96.1(13) . . ?
O14 W5' W9 135.2(12) . . ?
O23 W5' W9 85.4(9) . . ?
O23 W5' O14 75.6(9) . . ?
O27 W5' W9 51.0(6) . . ?
O27 W5' O14 84.9(11) . . ?
O27 W5' O23 76.9(11) . . ?
O27 W5' O28 158.8(15) . . ?
O28 W5' W9 133.3(12) . . ?
O28 W5' O14 84.5(9) . . ?
O28 W5' O23 82.7(10) . . ?
O1 W6 O19 85.3(4) . . ?
O1 W6 O22 89.0(5) . . ?
O1 W6 O33 86.7(4) . . ?
O1 W6 O44 158.9(4) . . ?
O19 W6 O33 71.4(4) . . ?
O22 W6 O19 157.0(4) . . ?
O22 W6 O33 86.1(4) . . ?
O22 W6 O44 87.6(5) . . ?
O44 W6 O19 89.7(5) . . ?
O44 W6 O33 72.3(4) . . ?
O46 W6 O1 99.6(5) . . ?
O46 W6 O19 100.1(5) . . ?
O46 W6 O22 102.8(5) . . ?
O46 W6 O33 169.1(5) . . ?
O46 W6 O44 101.5(5) . . ?
O7 W7 O11 72.2(4) . . ?
O7 W7 O22 85.5(5) . . ?
O7 W7 O24 91.2(5) . . ?
O17 W7 O7 101.1(5) . . ?
O17 W7 O11 169.7(5) . . ?
O17 W7 O21 102.4(5) . . ?
O17 W7 O22 102.4(5) . . ?
O17 W7 O24 101.4(5) . . ?
O21 W7 O7 156.4(4) . . ?
O21 W7 O11 85.0(4) . . ?
O21 W7 O22 86.7(5) . . ?
O21 W7 O24 87.0(5) . . ?
O22 W7 O11 85.1(4) . . ?
O24 W7 O11 71.5(4) . . ?
O24 W7 O22 156.3(4) . . ?
W8' W8 O7 145(2) . . ?
W8' W8 O11 143(2) . . ?
W8' W8 O18 89(2) . . ?
W8' W8 O35 105(2) . . ?
W8' W8 O39 60(2) . . ?
W8' W8 O43 43(2) . . ?
O7 W8 O11 71.8(4) . . ?
O7 W8 O35 87.3(5) . . ?
O7 W8 O39 155.1(4) . . ?
O18 W8 O7 89.8(5) . . ?
O18 W8 O11 85.3(4) . . ?
O18 W8 O35 159.3(5) . . ?
O18 W8 O39 90.6(5) . . ?
O35 W8 O11 74.3(4) . . ?
O35 W8 O39 83.5(4) . . ?
O39 W8 O11 83.4(4) . . ?
O43 W8 O7 102.9(5) . . ?
O43 W8 O11 172.1(5) . . ?
O43 W8 O18 100.7(5) . . ?
O43 W8 O35 99.9(5) . . ?
O43 W8 O39 101.5(5) . . ?
W8 W8' O7 27.5(16) . . ?
W8 W8' O18 75(2) . . ?
W8 W8' O35 61.1(19) . . ?
W8 W8' O39 104(2) . . ?
W8 W8' O43 121(2) . . ?
O18 W8' O7 76.0(7) . . ?
O18 W8' O35 133.6(10) . . ?
O35 W8' O7 71.9(6) . . ?
O39 W8' O7 132.0(10) . . ?
O39 W8' O18 94.8(10) . . ?
O39 W8' O35 83.0(9) . . ?
O43 W8' O7 94.5(10) . . ?
O43 W8' O18 111.7(13) . . ?
O43 W8' O35 103.5(12) . . ?
O43 W8' O39 131.5(13) . . ?
W5' W9 W12' 70.1(7) . . ?
O1 W9 W5' 82.3(6) . . ?
O1 W9 W12' 129.8(5) . . ?
O1 W9 O27 86.8(3) . . ?
O12 W9 W5' 31.5(6) . . ?
O12 W9 W12' 89.9(5) . . ?
O12 W9 O1 86.8(4) . . ?
O12 W9 O21 159.0(4) . . ?
O12 W9 O27 73.2(4) . . ?
O21 W9 W5' 127.6(6) . . ?
O21 W9 W12' 78.7(5) . . ?
O21 W9 O1 87.0(4) . . ?
O21 W9 O27 86.5(4) . . ?
O27 W9 W5' 42.0(6) . . ?
O27 W9 W12' 44.9(5) . . ?
O30 W9 W5' 84.7(6) . . ?
O30 W9 W12' 28.9(5) . . ?
O30 W9 O1 158.6(4) . . ?
O30 W9 O12 90.9(5) . . ?
O30 W9 O21 87.6(5) . . ?
O30 W9 O27 72.3(4) . . ?
O50 W9 W5' 129.9(7) . . ?
O50 W9 W12' 129.7(6) . . ?
O50 W9 O1 100.3(5) . . ?
O50 W9 O12 98.3(5) . . ?
O50 W9 O21 102.5(5) . . ?
O50 W9 O27 168.8(5) . . ?
O50 W9 O30 101.1(5) . . ?
O2 W10 O11 83.5(4) . . ?
O15 W10 O2 100.9(5) . . ?
O15 W10 O11 171.4(5) . . ?
O15 W10 O24 100.1(5) . . ?
O15 W10 O25 104.4(5) . . ?
O15 W10 O35 100.7(5) . . ?
O24 W10 O2 90.5(5) . . ?
O24 W10 O11 72.3(4) . . ?
O24 W10 O25 155.4(4) . . ?
O24 W10 O35 87.6(5) . . ?
O25 W10 O2 87.2(5) . . ?
O25 W10 O11 83.1(4) . . ?
O35 W10 O2 158.4(4) . . ?
O35 W10 O11 75.4(4) . . ?
O35 W10 O25 85.6(5) . . ?
O5 W11 O18 88.9(5) . . ?
O5 W11 O20 85.7(4) . . ?
O5 W11 O33 83.3(4) . . ?
O5 W11 O44 155.3(5) . . ?
O18 W11 O20 157.6(4) . . ?
O18 W11 O33 84.3(4) . . ?
O18 W11 O44 90.3(5) . . ?
O20 W11 O33 73.4(4) . . ?
O20 W11 O44 85.7(4) . . ?
O36 W11 O5 101.2(5) . . ?
O36 W11 O18 101.9(5) . . ?
O36 W11 O20 100.5(5) . . ?
O36 W11 O33 172.3(5) . . ?
O36 W11 O44 103.2(5) . . ?
O44 W11 O33 72.0(4) . . ?
W12' W12 O2 29(2) . . ?
W12' W12 O13 116(2) . . ?
W12' W12 O23 142(3) . . ?
W12' W12 O27 78(3) . . ?
W12' W12 O30 62(2) . . ?
W12' W12 O37 105(3) . . ?
O2 W12 O13 89.7(5) . . ?
O2 W12 O23 158.7(5) . . ?
O2 W12 O27 84.8(4) . . ?
O2 W12 O30 90.4(5) . . ?
O13 W12 O27 82.7(4) . . ?
O13 W12 O30 154.2(4) . . ?
O23 W12 O13 85.4(5) . . ?
O23 W12 O27 74.1(4) . . ?
O23 W12 O30 85.2(5) . . ?
O30 W12 O27 71.6(4) . . ?
O37 W12 O2 101.8(5) . . ?
O37 W12 O13 104.0(5) . . ?
O37 W12 O23 99.4(6) . . ?
O37 W12 O27 170.5(5) . . ?
O37 W12 O30 101.3(5) . . ?
W12 W12' W9 107(3) . . ?
W12 W12' O2 141(3) . . ?
W12 W12' O13 51(2) . . ?
W12 W12' O23 30(2) . . ?
W12 W12' O27 89(3) . . ?
W12 W12' O30 103(3) . . ?
W12 W12' O37 59(2) . . ?
O2 W12' W9 106.0(11) . . ?
O2 W12' O13 92.3(12) . . ?
O2 W12' O23 158.2(15) . . ?
O2 W12' O27 98.6(12) . . ?
O2 W12' O30 116.8(14) . . ?
O2 W12' O37 111.9(15) . . ?
O13 W12' W9 122.7(9) . . ?
O13 W12' O23 69.1(7) . . ?
O13 W12' O27 77.7(8) . . ?
O23 W12' W9 76.7(7) . . ?
O27 W12' W9 46.5(5) . . ?
O27 W12' O23 67.1(7) . . ?
O30 W12' W9 31.5(6) . . ?
O30 W12' O13 143.3(13) . . ?
O30 W12' O23 77.1(9) . . ?
O30 W12' O27 76.4(10) . . ?
O30 W12' O37 100.6(12) . . ?
O37 W12' W9 130.2(11) . . ?
O37 W12' O13 87.2(9) . . ?
O37 W12' O23 79.5(9) . . ?
O37 W12' O27 146.5(12) . . ?
O3 Ge1 O11 110.8(5) . . ?
O3 Ge1 O27 108.4(4) . . ?
O3 Ge1 O33 109.8(5) . . ?
O11 Ge1 O27 108.1(5) . . ?
O11 Ge1 O33 110.1(5) . . ?
O33 Ge1 O27 109.6(5) . . ?
O1W Dy1 O2W 117.5(7) . . ?
O1W Dy1 O3W 77.8(8) . . ?
O1W Dy1 O5W 71.8(8) . . ?
O1W Dy1 O7W 75.3(6) . . ?
O1W Dy1 O38 75.7(6) . . ?
O2W Dy1 O5W 144.4(7) . . ?
O2W Dy1 O7W 142.2(6) . . ?
O2W Dy1 O38 71.4(5) . . ?
O3W Dy1 O2W 73.8(7) . . ?
O3W Dy1 O5W 75.3(8) . . ?
O3W Dy1 O7W 142.8(7) . . ?
O3W Dy1 O38 118.5(7) . . ?
O4W Dy1 O1W 139.5(7) . . ?
O4W Dy1 O2W 80.4(6) . . ?
O4W Dy1 O3W 73.0(8) . . ?
O4W Dy1 O5W 74.1(7) . . ?
O4W Dy1 O7W 113.9(6) . . ?
O4W Dy1 O38 143.5(6) . . ?
O5W Dy1 O7W 72.2(6) . . ?
O5W Dy1 O38 140.8(7) . . ?
O6W Dy1 O1W 142.5(6) . . ?
O6W Dy1 O2W 78.4(7) . . ?
O6W Dy1 O3W 139.2(7) . . ?
O6W Dy1 O4W 73.4(6) . . ?
O6W Dy1 O5W 116.2(7) . . ?
O6W Dy1 O7W 73.3(5) . . ?
O6W Dy1 O38 78.6(5) . . ?
O38 Dy1 O7W 78.8(5) . . ?
O31 Cu1 O31 180.0(6) 3_776 . ?
O31 Cu1 N1 84.8(6) 3_776 3_776 ?
O31 Cu1 N1 95.2(6) 3_776 . ?
O31 Cu1 N1 84.8(6) . . ?
O31 Cu1 N1 95.2(6) . 3_776 ?
N1 Cu1 N1 180.0(7) . 3_776 ?
O26 Cu2 O8W 90.1(5) . . ?
O26 Cu2 O47 177.5(6) . . ?
O26 Cu2 N3 83.0(6) . . ?
O47 Cu2 O8W 91.3(6) . . ?
O47 Cu2 N3 94.7(7) . . ?
N2 Cu2 O8W 99.2(6) . . ?
N2 Cu2 O26 98.2(7) . . ?
N2 Cu2 O47 83.6(8) . . ?
N2 Cu2 N3 161.0(7) . . ?
N3 Cu2 O8W 99.8(6) . . ?
O9W Cu3 N4 173.4(6) . . ?
O29 Cu3 O9W 95.1(5) . . ?
O29 Cu3 N4 91.2(5) . . ?
O53 Cu3 O9W 88.6(6) . . ?
O53 Cu3 O29 176.3(5) . . ?
O53 Cu3 N4 85.1(6) . . ?
O45 Cu4 O45 180.0(4) . 3_786 ?
O45 Cu4 N5 95.9(5) 3_786 . ?
O45 Cu4 N5 84.1(5) . . ?
O45 Cu4 N5 84.1(5) 3_786 3_786 ?
O45 Cu4 N5 95.9(5) . 3_786 ?
N5 Cu4 N5 180.0(8) . 3_786 ?
W6 O1 W9 147.8(5) . . ?
W12 O2 W10 159.4(6) . . ?
W12' O2 W10 163.0(12) . . ?
W12' O2 W12 10.5(9) . . ?
W1 O3 W4 92.9(3) . . ?
W2 O3 W1 93.4(3) . . ?
W2 O3 W4 92.9(3) . . ?
Ge1 O3 W1 123.0(5) . . ?
Ge1 O3 W2 124.0(5) . . ?
Ge1 O3 W4 122.1(5) . . ?
W1 O4 W2 121.8(5) . . ?
W11 O5 W1 146.3(6) . . ?
W5 O6 W3 160.4(6) . . ?
W5' O6 W3 155.6(11) . . ?
W5' O6 W5 14.7(8) . . ?
W7 O7 W8 122.6(5) . . ?
W7 O7 W8' 130.1(7) . . ?
W8 O7 W8' 7.4(5) . . ?
W1 O8 W4 122.9(5) . . ?
W7 O11 W8 93.2(4) . . ?
W10 O11 W7 93.8(4) . . ?
W10 O11 W8 91.8(4) . . ?
Ge1 O11 W7 123.6(5) . . ?
Ge1 O11 W8 121.1(5) . . ?
Ge1 O11 W10 124.7(5) . . ?
W5' O12 W5 12.8(8) . . ?
W5' O12 W9 110.0(11) . . ?
W9 O12 W5 119.5(6) . . ?
W2 O13 W12 147.2(6) . . ?
W2 O13 W12' 148.3(8) . . ?
W12 O13 W12' 12.8(6) . . ?
W2 O14 W5' 140.4(9) . . ?
W5 O14 W2 146.7(6) . . ?
W5 O14 W5' 12.3(6) . . ?
W4 O16 W2 121.5(5) . . ?
W8 O18 W8' 15.8(5) . . ?
W11 O18 W8 159.1(6) . . ?
W11 O18 W8' 154.3(8) . . ?
W3 O19 W6 122.0(5) . . ?
W11 O20 W3 119.0(5) . . ?
W7 O21 W9 151.0(6) . . ?
W6 O22 W7 151.3(7) . . ?
W5 O23 W5' 13.2(6) . . ?
W5 O23 W12' 113.4(8) . . ?
W5' O23 W12' 102.1(10) . . ?
W12 O23 W5 118.7(6) . . ?
W12 O23 W5' 108.2(9) . . ?
W12 O23 W12' 8.2(6) . . ?
W10 O24 W7 122.2(5) . . ?
W4 O25 W10 145.7(6) . . ?
C18 O26 Cu2 111.7(11) . . ?
W5' O27 W5 10.4(7) . . ?
W5' O27 W9 87.0(8) . . ?
W5' O27 W12 100.8(8) . . ?
W5' O27 W12' 113.1(10) . . ?
W9 O27 W5 94.3(4) . . ?
W12 O27 W5 92.9(3) . . ?
W12 O27 W9 94.5(3) . . ?
W12' O27 W5 105.9(7) . . ?
W12' O27 W9 88.6(7) . . ?
W12' O27 W12 13.9(5) . . ?
Ge1 O27 W5 122.7(5) . . ?
Ge1 O27 W5' 121.6(9) . . ?
Ge1 O27 W9 121.8(5) . . ?
Ge1 O27 W12 122.9(5) . . ?
Ge1 O27 W12' 116.7(8) . . ?
W5 O28 W5' 10.2(7) . . ?
C18 O29 Cu3 126.0(11) . . ?
W9 O30 W12 121.6(5) . . ?
W12' O30 W9 119.6(9) . . ?
W12' O30 W12 15.9(7) . . ?
C6 O31 Cu1 112.1(11) . . ?
W3 O32 W1 147.7(6) . . ?
W3 O33 W6 94.5(4) . . ?
W3 O33 W11 93.1(4) . . ?
W6 O33 W11 94.2(3) . . ?
Ge1 O33 W3 122.4(5) . . ?
Ge1 O33 W6 122.3(5) . . ?
Ge1 O33 W11 122.6(5) . . ?
W8 O35 W8' 14.2(5) . . ?
W10 O35 W8 118.1(5) . . ?
W10 O35 W8' 127.7(7) . . ?
W12 O37 W12' 16.0(6) . . ?
C6 O38 Dy1 138.9(13) . . ?
W4 O39 W8 146.7(5) . . ?
W8' O39 W4 160.2(8) . . ?
W8' O39 W8 15.6(6) . . ?
W8' O43 W8 15.9(7) . . ?
W6 O44 W11 121.5(6) . . ?
C30 O45 Cu4 114.0(11) . . ?
C11 O47 Cu2 111.2(17) . . ?
C24 O53 Cu3 112.3(11) . . ?
C1 N1 Cu1 126.4(13) . . ?
C5 N1 Cu1 112.4(11) . . ?
C5 N1 C1 120.9(17) . . ?
C7 N2 Cu2 125.6(17) . . ?
C7 N2 C12 122(2) . . ?
C12 N2 Cu2 112.1(16) . . ?
C13 N3 Cu2 131.1(13) . . ?
C17 N3 Cu2 110.6(12) . . ?
C17 N3 C13 118.3(16) . . ?
C19 N4 Cu3 130.2(12) . . ?
C19 N4 C23 117.5(15) . . ?
C23 N4 Cu3 111.9(10) . . ?
C25 N5 Cu4 130.3(14) . . ?
C25 N5 C29 118.7(17) . . ?
C29 N5 Cu4 111.0(11) . . ?
N1 C1 C2 116.0(19) . . ?
C3 C2 C1 119(2) . . ?
C4 C3 C2 122(2) . . ?
C5 C4 C3 117(2) . . ?
N1 C5 C4 124.1(17) . . ?
N1 C5 C6 113.4(18) . . ?
C4 C5 C6 122.4(19) . . ?
O31 C6 C5 116.4(18) . . ?
O38 C6 O31 124.5(17) . . ?
O38 C6 C5 119.1(19) . . ?
N2 C7 C8 120(2) . . ?
C9 C8 C7 117(3) . . ?
C10 C9 C8 119(3) . . ?
C9 C10 C12 126(3) . . ?
O47 C11 C12 118(2) . . ?
O64 C11 O47 122(3) . . ?
O64 C11 C12 120(3) . . ?
N2 C12 C10 116(3) . . ?
N2 C12 C11 113(2) . . ?
C10 C12 C11 132(3) . . ?
C14 C13 N3 123.9(19) . . ?
C13 C14 C15 119.1(19) . . ?
C16 C15 C14 121.6(17) . . ?
C15 C16 C17 113.9(17) . . ?
N3 C17 C16 122.8(17) . . ?
N3 C17 C18 114.1(16) . . ?
C16 C17 C18 122.6(16) . . ?
O26 C18 O29 120.5(15) . . ?
O26 C18 C17 119.8(16) . . ?
O29 C18 C17 119.4(15) . . ?
N4 C19 C20 123.6(17) . . ?
C21 C20 C19 116.5(18) . . ?
C20 C21 C22 120(2) . . ?
C23 C22 C21 118.4(18) . . ?
N4 C23 C24 112.7(15) . . ?
C22 C23 N4 123.5(16) . . ?
C22 C23 C24 123.4(17) . . ?
O53 C24 C23 115.9(16) . . ?
O68 C24 O53 119.1(16) . . ?
O68 C24 C23 124.9(18) . . ?
N5 C25 C26 122(2) . . ?
C25 C26 C27 115(2) . . ?
C28 C27 C26 122(2) . . ?
C29 C28 C27 120(2) . . ?
N5 C29 C30 114.0(16) . . ?
C28 C29 N5 121.7(18) . . ?
C28 C29 C30 124.2(18) . . ?
O45 C30 C29 116.4(16) . . ?
O61 C30 O45 122.8(17) . . ?
O61 C30 C29 119.4(18) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1891067'
loop_
_audit_author_name
_audit_author_address
'Junwei Zhao'
;Henan University
China
;
_audit_update_record             
;
2019-02-11 deposited with the CCDC.	2019-02-14 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT201_3                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......   5 Report 
RESPONSE: Due to the large structure and the existence of a large 
 amount of weight atoms, the intensity data are not very good, 
 leading to the ADP max/min ratio of some water molecules, and it is 
very difficult to refine this large structure, therefore, 
 in the final refinement, the W, Ge, Cu and Tb atoms were refined 
anisotropically, some O atoms and water molecules were
 refined isotropically.
;


_vrf_PLAT220_3                   
;
PROBLEM:  Non-Solvent  Resd 1  O   Ueq(max)/Ueq(min) Range   7.8 Ratio 
RESPONSE: In polyoxometalate compounds, the Ueq of oxygen atoms in
 the POM skeleton is small due to multiple covalent bonds, whereas the 
Ueq of these dissociative water oxygen atoms is biggish without 
the constraint of covalent bonds, which lead to the 
non-solvent O Ueq(max)/Ueq(min) range. 
;


_vrf_PLAT306_3                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O10W Check
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

_vrf_PLAT342_3                   
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0344 Ang.
RESPONSE: The alert derives from shading of reciprocal space
 by the pressure cell, and it is unavoidable in high pressure
 crystal structure determinations.
;

_vrf_PLAT430_3                   
;
PROBLEM: Short Inter D...A Contact  O2W     ..O10W   .  2.61 Ang. 
RESPONSE: In the crystal structure, there are a number of 
short contacts between Ow(H2O) and O(POM) or Ow(H2O) in the range
 of 2.61-2.89 Ang, which indicate extensive hydrogen bonding 
interactions among them. 
;

_vrf_PLAT242_3                   
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of Tb1 Check  
RESPONSE: Due to the large structure and the existence of a large 
 amount of weight atoms, the intensity data are not very good, 
 leading to this alert, and it is very difficult to refine this large structure.
;


# end Validation Reply Form

_audit_creation_date             2019-02-09
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'Ge O40 W12, C6 H4 Cu0.5 N O9 Tb, C18 H12 Cu2 N3 O8, C6 H4 Cu0.5 N O2, 7(O)'
_chemical_formula_sum            'C30 H52 Cu3 Ge N5 O66 Tb W12'
_chemical_formula_weight         4167.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ge Ge 0.1547 1.8001 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.2757(5)
_cell_length_b                   16.5995(6)
_cell_length_c                   35.2571(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.0500(10)
_cell_angle_gamma                90.00
_cell_volume                     7650.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9496
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.150
_cell_measurement_theta_min      2.439
_exptl_absorpt_coefficient_mu    20.189
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1568 before and 0.0758 after correction.
The Ratio of minimum to maximum transmission is 0.3559.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            mazarine
_exptl_crystal_density_diffrn    3.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7468
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            37659
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                9727
_reflns_number_total             13226
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         5.019
_refine_diff_density_min         -3.361
_refine_diff_density_rms         0.429
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         13226
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0610
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0886P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1666
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 W6-O1
 1.89 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O68)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: W5(0.95) W5'(0.05) W8(0.95) W8'(0.05) W11(0.95) W11'(0.05)
 W12(0.95) W12'(0.05)
 Fixed Uiso: O13W(0.15858) O14W(0.1508) O15W(0.16819) O16W(0.16599)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C7(H7A), C8(H8A), C9(H9A), C10(H10A),
 C13(H13A), C14(H14A), C15(H15A), C16(H16A), C19(H19A), C20(H20A), C21(H21A),
 C22(H22A), C25(H25A), C26(H26A), C27(H27A), C28(H28A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
W1 W 0.75437(5) 1.15276(4) 0.32109(2) 0.02281(17) Uani 1 d . . 1 . . .
W2 W 0.75727(6) 1.35418(4) 0.32840(2) 0.03016(19) Uani 1 d . . 1 . . .
W3 W 0.80871(5) 1.12463(4) 0.42596(2) 0.02546(18) Uani 1 d . . 1 . . .
W4 W 0.54962(6) 1.26066(4) 0.27960(2) 0.02657(18) Uani 1 d . . 1 . . .
W5 W 0.81247(7) 1.35086(5) 0.43367(3) 0.0277(2) Uani 0.95 d . . 1 . . .
W5' W 0.7774(18) 1.3304(12) 0.4384(7) 0.043(6) Uiso 0.05 d . . 1 . . .
W6 W 0.59169(6) 1.11854(4) 0.46256(2) 0.0336(2) Uani 1 d . . 1 D . .
W7 W 0.36560(6) 1.23767(4) 0.41734(2) 0.0321(2) Uani 1 d . . 1 . . .
W8 W 0.37706(6) 1.14998(5) 0.33183(3) 0.0277(2) Uani 0.95 d . . 1 . . .
W8' W 0.3758(13) 1.1275(10) 0.3147(5) 0.029(4) Uiso 0.05 d . . 1 . . .
W9 W 0.59542(6) 1.34225(4) 0.47031(2) 0.0345(2) Uani 1 d . . 1 . . .
W10 W 0.37672(6) 1.34845(4) 0.33883(2) 0.02932(19) Uani 1 d . . 1 . . .
W11 W 0.60550(6) 1.02983(5) 0.37809(3) 0.0271(2) Uani 0.95 d . . 1 . . .
W11' W 0.5972(15) 1.0206(12) 0.3619(6) 0.029(5) Uiso 0.05 d . . 1 . . .
W12 W 0.60907(7) 1.45582(4) 0.39274(2) 0.0297(2) Uani 0.95 d . . 1 . . .
W12' W 0.5587(17) 1.4345(11) 0.3922(5) 0.035(4) Uiso 0.05 d . . 1 . . .
Ge1 Ge 0.60014(13) 1.24323(9) 0.38177(5) 0.0204(4) Uani 1 d . . 1 . . .
Tb1 Tb 1.14669(8) 0.77524(6) 0.39699(3) 0.0478(3) Uani 1 d . . 1 . . .
Cu1 Cu 1.0000 1.0000 0.5000 0.0362(8) Uani 1 d . . 2 S T P
Cu2 Cu 0.0875(2) 1.20838(14) 0.26760(8) 0.0460(6) Uani 1 d . . 1 . . .
Cu3 Cu 0.21690(17) 1.49471(12) 0.25722(7) 0.0352(5) Uani 1 d . . 1 . . .
Cu4 Cu 1.0000 1.5000 0.5000 0.0385(8) Uani 1 d . . 2 S T P
O1W O 1.220(2) 0.8397(16) 0.4521(7) 0.135(9) Uiso 1 d . . 1 . . .
O2W O 1.0285(16) 0.8499(13) 0.3506(6) 0.100(7) Uani 1 d . . 1 . . .
O3W O 1.254(2) 0.8758(19) 0.3708(9) 0.163(11) Uiso 1 d . . 1 . . .
O4W O 1.1820(18) 0.7260(13) 0.3374(7) 0.104(7) Uani 1 d . . 1 . . .
O5W O 1.314(2) 0.7274(15) 0.4135(8) 0.124(8) Uiso 1 d . . 1 . . .
O6W O 1.0196(13) 0.6809(10) 0.3753(5) 0.077(5) Uani 1 d . . 1 . . .
O7W O 1.1474(13) 0.6732(11) 0.4474(5) 0.081(5) Uani 1 d . . 1 . . .
O8W O -0.0824(13) 1.2282(10) 0.2368(6) 0.073(5) Uani 1 d . . 1 . . .
O9W O 0.0732(12) 1.4916(8) 0.2659(5) 0.063(4) Uani 1 d . . 1 . . .
O10W O 0.1285(16) 0.4350(11) 0.1377(5) 0.096(7) Uani 1 d . . 1 . . .
O11W O 1.123(2) 0.8916(18) 0.2629(9) 0.164(11) Uiso 1 d . . 1 . . .
O12W O -0.6661(16) 1.0003(13) 0.4218(6) 0.102(7) Uiso 1 d . . 1 . . .
O13W O 0.520(3) 0.7622(17) 0.3666(10) 0.159 Uiso 1 d . . 1 . . .
O14W O 1.366(2) 0.5722(17) 0.4025(8) 0.151 Uiso 1 d . . 1 . . .
O15W O 1.086(2) 0.5368(19) 0.3436(9) 0.168 Uiso 1 d . . 1 . . .
O16W O 0.438(2) 0.8503(19) 0.4212(9) 0.166 Uiso 1 d . . 1 . . .
O1 O 0.6208(8) 1.2235(4) 0.4778(3) 0.021(2) Uiso 1 d . . 1 D . .
O2 O 0.4791(10) 1.4172(7) 0.3695(4) 0.043(3) Uani 1 d . . 1 . . .
O3 O 0.6510(8) 1.2507(6) 0.3396(3) 0.022(2) Uani 1 d . . 1 . . .
O4 O 0.8193(9) 1.2536(6) 0.3151(3) 0.028(3) Uani 1 d . . 1 . . .
O5 O 0.6593(8) 1.0778(6) 0.3371(3) 0.028(3) Uani 1 d . . 1 . . .
O6 O 0.8233(9) 1.2362(6) 0.4389(4) 0.031(3) Uani 1 d . . 1 . . .
O7 O 0.3152(9) 1.1599(7) 0.3779(4) 0.035(3) Uani 1 d . . 1 . U .
O8 O 0.6543(9) 1.1823(7) 0.2773(3) 0.031(3) Uani 1 d . . 1 . . .
O9 O 0.9275(10) 1.0882(7) 0.4449(4) 0.040(3) Uani 1 d . . 1 . . .
O10 O 0.8353(10) 1.4231(7) 0.3127(4) 0.045(3) Uani 1 d . . 1 . . .
O11 O 0.4686(8) 1.2452(6) 0.3710(3) 0.023(2) Uani 1 d . . 1 . . .
O12 O 0.7437(10) 1.3550(7) 0.4781(4) 0.038(3) Uani 1 d . . 1 . . .
O13 O 0.6649(10) 1.4226(7) 0.3492(4) 0.038(3) Uani 1 d . . 1 . . .
O14 O 0.8237(9) 1.3379(7) 0.3813(4) 0.034(3) Uani 1 d . . 1 . . .
O15 O 0.2917(9) 1.4185(7) 0.3162(4) 0.038(3) Uani 1 d . . 1 . . .
O16 O 0.6533(9) 1.3398(6) 0.2819(4) 0.038(3) Uani 1 d . . 1 . . .
O17 O 0.2747(12) 1.2326(9) 0.4450(4) 0.056(4) Uani 1 d . . 1 . . .
O18 O 0.4740(9) 1.0758(6) 0.3587(4) 0.036(3) Uani 1 d . . 1 . . .
O19 O 0.7381(9) 1.1021(7) 0.4674(3) 0.031(3) Uani 1 d . . 1 . . .
O20 O 0.7455(8) 1.0262(6) 0.4044(3) 0.027(3) Uani 1 d . . 1 . . .
O21 O 0.4549(9) 1.3117(7) 0.4446(3) 0.032(3) Uani 1 d . . 1 . U .
O22 O 0.4593(10) 1.1545(7) 0.4412(4) 0.041(3) Uiso 1 d . . 1 . . .
O23 O 0.7484(9) 1.4535(6) 0.4187(3) 0.035(3) Uani 1 d . . 1 . . .
O24 O 0.3157(8) 1.3250(8) 0.3831(3) 0.034(3) Uani 1 d . . 1 . . .
O25 O 0.4698(9) 1.3341(6) 0.3039(4) 0.033(3) Uani 1 d . . 1 . . .
O26 O 0.1198(11) 1.3229(7) 0.2586(4) 0.045(3) Uani 1 d . . 1 . . .
O27 O 0.6427(9) 1.3251(6) 0.4115(3) 0.031(3) Uani 1 d . . 1 . . .
O28 O 0.9297(10) 1.3829(8) 0.4551(4) 0.047(4) Uani 1 d . . 1 . . .
O29 O 0.2057(10) 1.3996(7) 0.2242(4) 0.039(3) Uani 1 d . . 1 . . .
O30 O 0.5748(10) 1.4428(7) 0.4439(4) 0.041(3) Uani 1 d . . 1 . . .
O31 O 1.0552(10) 0.9262(7) 0.4654(4) 0.047(3) Uani 1 d . . 1 . . .
O32 O 0.8202(9) 1.1519(6) 0.3744(3) 0.026(3) Uani 1 d . . 1 . U .
O33 O 0.6403(9) 1.1557(6) 0.4062(4) 0.031(3) Uani 1 d . . 1 . . .
O34 O 0.8305(9) 1.0906(7) 0.2995(4) 0.039(3) Uani 1 d . . 1 . . .
O35 O 0.3130(9) 1.2519(6) 0.3149(4) 0.033(3) Uani 1 d . . 1 . . .
O36 O 0.5901(10) 0.9320(6) 0.3617(4) 0.051(4) Uani 1 d . . 1 . . .
O37 O 0.5933(11) 1.5575(7) 0.3860(4) 0.045(3) Uani 1 d . . 1 . . .
O38 O 1.0110(12) 0.8215(9) 0.4268(5) 0.061(4) Uani 1 d . . 1 . . .
O39 O 0.4680(9) 1.1798(6) 0.2977(3) 0.034(3) Uani 1 d . . 1 . . .
O43 O 0.2926(9) 1.0872(7) 0.3042(3) 0.038(3) Uani 1 d . . 1 . . .
O44 O 0.5684(9) 1.0269(6) 0.4279(4) 0.037(3) Uani 1 d . . 1 . . .
O46 O 0.5741(10) 1.0778(8) 0.5044(4) 0.050(4) Uani 1 d . . 1 . . .
O47 O 0.0615(12) 1.0971(9) 0.2774(5) 0.065(5) Uani 1 d . . 1 . . .
O50 O 0.5796(12) 1.3713(9) 0.5150(4) 0.056(4) Uani 1 d . . 1 . . .
O52 O 0.4957(11) 1.2696(7) 0.2324(4) 0.043(3) Uani 1 d . . 1 . . .
O53 O 0.2417(12) 1.5887(7) 0.2904(4) 0.051(4) Uani 1 d . . 1 . . .
O64 O 0.0682(18) 1.0078(12) 0.3251(8) 0.139(10) Uani 1 d . . 1 . . .
O68 O 0.3651(12) 1.6572(8) 0.3250(4) 0.055(4) Uani 1 d . . 1 . U .
N1 N 0.8759(12) 0.9317(8) 0.4881(5) 0.037(4) Uani 1 d . . 1 . . .
N2 N 0.0712(13) 1.2213(13) 0.3199(6) 0.052(5) Uani 1 d . . 1 . . .
N3 N 0.1517(13) 1.1909(8) 0.2216(4) 0.039(4) Uani 1 d . . 1 . . .
N4 N 0.3622(11) 1.5059(7) 0.2542(5) 0.035(4) Uani 1 d . . 1 . . .
N5 N 0.8627(12) 1.5427(8) 0.5029(5) 0.035(4) Uani 1 d . . 1 . . .
C1 C 0.7884(16) 0.9378(11) 0.5011(6) 0.039(5) Uani 1 d . . 1 . . .
H1A H 0.7826 0.9747 0.5205 0.047 Uiso 1 calc . . 1 R . .
C2 C 0.708(2) 0.8914(12) 0.4865(8) 0.072(9) Uani 1 d . . 1 . . .
H2A H 0.6470 0.8950 0.4961 0.086 Uiso 1 calc . . 1 R . .
C3 C 0.7174(19) 0.8358(13) 0.4559(8) 0.066(7) Uani 1 d . . 1 . . .
H3A H 0.6622 0.8050 0.4440 0.079 Uiso 1 calc . . 1 R . .
C4 C 0.808(2) 0.8308(11) 0.4455(8) 0.071(8) Uani 1 d . . 1 . . .
H4A H 0.8170 0.7923 0.4272 0.085 Uiso 1 calc . . 1 R . .
C5 C 0.8858(15) 0.8782(11) 0.4597(6) 0.040(5) Uani 1 d . . 1 . . .
C6 C 0.9889(13) 0.8734(10) 0.4493(6) 0.037(5) Uani 1 d . . 1 . . .
C7 C 0.0719(17) 1.284(2) 0.3409(7) 0.073(9) Uani 1 d . . 1 . . .
H7A H 0.0752 1.3337 0.3290 0.087 Uiso 1 calc . . 1 R . .
C8 C 0.068(2) 1.284(2) 0.3810(10) 0.099(10) Uani 1 d . . 1 . U .
H8A H 0.0686 1.3313 0.3951 0.119 Uiso 1 calc . . 1 R . .
C9 C 0.0638(17) 1.208(2) 0.3978(7) 0.080(9) Uani 1 d . . 1 . . .
H9A H 0.0623 1.2041 0.4240 0.096 Uiso 1 calc . . 1 R . .
C10 C 0.062(2) 1.141(2) 0.3770(9) 0.084(8) Uani 1 d . . 1 . U .
H10A H 0.0552 1.0915 0.3883 0.101 Uiso 1 calc . . 1 R . .
C11 C 0.067(2) 1.0769(17) 0.3123(9) 0.077(8) Uani 1 d . . 1 . U .
C12 C 0.0689(19) 1.1454(15) 0.3391(8) 0.065(6) Uani 1 d . . 1 . U .
C13 C 0.1642(16) 1.1237(11) 0.2034(7) 0.048(6) Uani 1 d . . 1 . . .
H13A H 0.1374 1.0764 0.2116 0.058 Uiso 1 calc . . 1 R . .
C14 C 0.2157(16) 1.1202(11) 0.1726(7) 0.052(6) Uani 1 d . . 1 . . .
H14A H 0.2217 1.0719 0.1598 0.063 Uiso 1 calc . . 1 R . .
C15 C 0.2596(17) 1.1932(16) 0.1609(7) 0.063(7) Uani 1 d . . 1 . . .
H15A H 0.2942 1.1927 0.1401 0.076 Uiso 1 calc . . 1 R . .
C16 C 0.2508(17) 1.2629(12) 0.1801(6) 0.044(5) Uani 1 d . . 1 . . .
H16A H 0.2821 1.3102 0.1741 0.053 Uiso 1 calc . . 1 R . .
C17 C 0.1937(15) 1.2601(9) 0.2087(6) 0.040(5) Uani 1 d . . 1 . . .
C18 C 0.1726(15) 1.3341(11) 0.2319(6) 0.043(5) Uani 1 d . . 1 . . .
C19 C 0.4180(15) 1.4647(11) 0.2330(6) 0.042(5) Uani 1 d . . 1 . . .
H19A H 0.3863 1.4276 0.2151 0.050 Uiso 1 calc . . 1 R . .
C20 C 0.5263(16) 1.4769(10) 0.2374(6) 0.042(5) Uani 1 d . . 1 . . .
H20A H 0.5649 1.4495 0.2219 0.051 Uiso 1 calc . . 1 R . .
C21 C 0.5703(15) 1.5284(12) 0.2642(7) 0.048(6) Uani 1 d . . 1 . . .
H21A H 0.6407 1.5358 0.2676 0.057 Uiso 1 calc . . 1 R . .
C22 C 0.5133(15) 1.5721(11) 0.2877(7) 0.050(6) Uani 1 d . . 1 . . .
H22A H 0.5444 1.6070 0.3069 0.060 Uiso 1 calc . . 1 R . .
C23 C 0.4095(13) 1.5600(10) 0.2806(6) 0.033(4) Uani 1 d . . 1 . . .
C24 C 0.3360(16) 1.6075(11) 0.3011(6) 0.037(5) Uani 1 d . . 1 . . .
C25 C 0.8045(17) 1.5301(13) 0.5267(8) 0.065(7) Uani 1 d . . 1 . . .
H25A H 0.8300 1.4980 0.5478 0.078 Uiso 1 calc . . 1 R . .
C26 C 0.705(2) 1.5596(18) 0.5248(8) 0.082(9) Uani 1 d . . 1 . . .
H26A H 0.6643 1.5476 0.5430 0.099 Uiso 1 calc . . 1 R . .
C27 C 0.675(2) 1.6063(16) 0.4944(9) 0.081(9) Uani 1 d . . 1 . . .
H27A H 0.6103 1.6298 0.4920 0.098 Uiso 1 calc . . 1 R . .
C28 C 0.733(2) 1.6230(13) 0.4653(8) 0.064(7) Uani 1 d . . 1 . . .
H28A H 0.7099 1.6554 0.4440 0.077 Uiso 1 calc . . 1 R . .
C29 C 0.8242(16) 1.5881(11) 0.4712(7) 0.048(6) Uani 1 d . . 1 . . .
C30 C 0.9018(15) 1.6033(11) 0.4460(6) 0.041(5) Uani 1 d . . 1 . . .
O45 O 0.9904(11) 1.5686(8) 0.4546(4) 0.048(4) Uani 1 d . . 1 . . .
O61 O 0.8770(11) 1.6456(10) 0.4163(4) 0.060(4) Uani 1 d . . 1 . . .


_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 O3 2.294(10) . ?
W1 O4 1.911(10) . ?
W1 O5 1.925(10) . ?
W1 O8 1.916(12) . ?
W1 O32 1.931(11) . ?
W1 O34 1.713(11) . ?
W2 O3 2.300(10) . ?
W2 O4 1.955(10) . ?
W2 O10 1.699(12) . ?
W2 O13 1.909(12) . ?
W2 O14 1.938(12) . ?
W2 O16 1.966(13) . ?
W3 O6 1.909(10) . ?
W3 O9 1.713(13) . ?
W3 O19 1.905(11) . ?
W3 O20 1.931(10) . ?
W3 O32 1.904(11) . ?
W3 O33 2.282(11) . ?
W4 O3 2.305(11) . ?
W4 O8 1.915(11) . ?
W4 O16 1.895(12) . ?
W4 O25 1.913(11) . ?
W4 O39 1.904(11) . ?
W4 O52 1.701(14) . ?
W5 W5' 0.62(2) . ?
W5 O6 1.915(10) . ?
W5 O12 1.947(13) . ?
W5 O14 1.890(12) . ?
W5 O23 1.936(11) . ?
W5 O27 2.292(12) . ?
W5 O28 1.692(13) . ?
W5' W9 2.84(2) . ?
W5' O6 1.68(2) . ?
W5' O12 1.59(2) . ?
W5' O14 2.21(3) . ?
W5' O23 2.17(2) . ?
W5' O27 1.87(3) . ?
W5' O28 2.19(3) . ?
W6 O1 1.844(7) . ?
W6 O19 1.941(11) . ?
W6 O22 1.884(13) . ?
W6 O33 2.278(12) . ?
W6 O44 1.943(12) . ?
W6 O46 1.676(13) . ?
W7 O7 1.930(13) . ?
W7 O11 2.310(11) . ?
W7 O17 1.682(13) . ?
W7 O21 1.855(12) . ?
W7 O22 1.949(13) . ?
W7 O24 1.929(11) . ?
W8 W8' 0.708(19) . ?
W8 O7 1.950(13) . ?
W8 O11 2.301(11) . ?
W8 O18 1.909(12) . ?
W8 O35 1.939(11) . ?
W8 O39 1.912(12) . ?
W8 O43 1.706(11) . ?
W8' O18 2.03(2) . ?
W8' O35 2.227(19) . ?
W8' O39 1.69(2) . ?
W8' O43 1.29(2) . ?
W9 W12' 3.113(17) . ?
W9 O1 2.010(8) . ?
W9 O12 1.951(13) . ?
W9 O21 1.992(12) . ?
W9 O27 2.285(11) . ?
W9 O30 1.906(12) . ?
W9 O50 1.694(14) . ?
W10 W12' 3.14(2) . ?
W10 O2 1.949(14) . ?
W10 O11 2.286(10) . ?
W10 O15 1.717(11) . ?
W10 O24 1.918(12) . ?
W10 O25 1.906(11) . ?
W10 O35 1.935(11) . ?
W11 W11' 0.584(19) . ?
W11 O5 1.896(11) . ?
W11 O18 1.918(12) . ?
W11 O20 1.928(10) . ?
W11 O33 2.325(11) . ?
W11 O36 1.725(11) . ?
W11 O44 1.904(13) . ?
W11' O5 1.61(2) . ?
W11' O18 1.86(2) . ?
W11' O20 2.26(2) . ?
W11' O36 1.47(2) . ?
W11' O44 2.43(2) . ?
W12 W12' 0.75(2) . ?
W12 O2 1.889(14) . ?
W12 O13 1.899(12) . ?
W12 O23 1.916(12) . ?
W12 O27 2.290(11) . ?
W12 O30 1.949(13) . ?
W12 O37 1.712(11) . ?
W12' O2 1.24(2) . ?
W12' O13 2.25(2) . ?
W12' O27 2.18(2) . ?
W12' O30 1.80(2) . ?
W12' O37 2.11(2) . ?
Ge1 O3 1.742(12) . ?
Ge1 O11 1.721(11) . ?
Ge1 O27 1.750(11) . ?
Ge1 O33 1.725(10) . ?
Tb1 O1W 2.28(3) . ?
Tb1 O2W 2.404(18) . ?
Tb1 O3W 2.48(3) . ?
Tb1 O4W 2.38(2) . ?
Tb1 O5W 2.34(3) . ?
Tb1 O6W 2.331(17) . ?
Tb1 O7W 2.455(16) . ?
Tb1 O38 2.366(14) . ?
Cu1 O31 1.960(13) . ?
Cu1 O31 1.960(13) 3_776 ?
Cu1 N1 1.983(16) . ?
Cu1 N1 1.983(16) 3_776 ?
Cu2 O8W 2.350(16) . ?
Cu2 O26 1.986(12) . ?
Cu2 O47 1.922(14) . ?
Cu2 N2 1.91(2) . ?
Cu2 N3 1.981(16) . ?
Cu3 O9W 1.984(14) . ?
Cu3 O29 1.951(12) . ?
Cu3 O53 1.944(14) . ?
Cu3 N4 1.958(15) . ?
Cu4 N5 1.975(15) 3_786 ?
Cu4 N5 1.975(15) . ?
Cu4 O45 1.950(13) . ?
Cu4 O45 1.950(13) 3_786 ?
O26 C18 1.28(2) . ?
O29 C18 1.22(2) . ?
O31 C6 1.30(2) . ?
O38 C6 1.24(2) . ?
O47 C11 1.27(3) . ?
O53 C24 1.28(2) . ?
O64 C11 1.23(3) . ?
O68 C24 1.19(2) . ?
N1 C1 1.32(2) . ?
N1 C5 1.36(2) . ?
N2 C7 1.28(3) . ?
N2 C12 1.43(3) . ?
N3 C13 1.31(2) . ?
N3 C17 1.39(2) . ?
N4 C19 1.33(2) . ?
N4 C23 1.36(2) . ?
N5 C25 1.26(3) . ?
N5 C29 1.37(3) . ?
C1 C2 1.34(3) . ?
C2 C3 1.44(3) . ?
C3 C4 1.31(3) . ?
C4 C5 1.33(3) . ?
C5 C6 1.48(3) . ?
C7 C8 1.42(4) . ?
C8 C9 1.40(4) . ?
C9 C10 1.33(4) . ?
C10 C12 1.35(4) . ?
C11 C12 1.48(4) . ?
C13 C14 1.38(3) . ?
C14 C15 1.44(3) . ?
C15 C16 1.36(3) . ?
C16 C17 1.36(3) . ?
C17 C18 1.53(3) . ?
C19 C20 1.43(3) . ?
C20 C21 1.33(3) . ?
C21 C22 1.42(3) . ?
C22 C23 1.37(3) . ?
C23 C24 1.53(2) . ?
C25 C26 1.40(3) . ?
C26 C27 1.33(4) . ?
C27 C28 1.42(4) . ?
C28 C29 1.32(3) . ?
C29 C30 1.49(3) . ?
C30 O45 1.30(2) . ?
C30 O61 1.26(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 W1 O3 73.4(4) . . ?
O4 W1 O5 158.4(5) . . ?
O4 W1 O8 87.1(5) . . ?
O4 W1 O32 88.7(5) . . ?
O5 W1 O3 85.4(4) . . ?
O5 W1 O32 85.3(5) . . ?
O8 W1 O3 71.5(4) . . ?
O8 W1 O5 90.2(5) . . ?
O8 W1 O32 156.7(5) . . ?
O32 W1 O3 85.4(4) . . ?
O34 W1 O3 169.0(5) . . ?
O34 W1 O4 99.6(5) . . ?
O34 W1 O5 102.0(5) . . ?
O34 W1 O8 100.2(6) . . ?
O34 W1 O32 103.1(6) . . ?
O4 W2 O3 72.5(4) . . ?
O4 W2 O16 87.7(5) . . ?
O10 W2 O3 170.3(5) . . ?
O10 W2 O4 101.0(6) . . ?
O10 W2 O13 101.1(6) . . ?
O10 W2 O14 101.9(6) . . ?
O10 W2 O16 100.9(6) . . ?
O13 W2 O3 85.7(5) . . ?
O13 W2 O4 157.8(5) . . ?
O13 W2 O14 85.9(5) . . ?
O13 W2 O16 89.3(5) . . ?
O14 W2 O3 85.5(5) . . ?
O14 W2 O4 88.4(5) . . ?
O14 W2 O16 157.2(5) . . ?
O16 W2 O3 71.9(4) . . ?
O6 W3 O20 159.0(5) . . ?
O6 W3 O33 84.6(5) . . ?
O9 W3 O6 101.6(6) . . ?
O9 W3 O19 100.0(5) . . ?
O9 W3 O20 99.3(5) . . ?
O9 W3 O32 103.6(5) . . ?
O9 W3 O33 170.3(5) . . ?
O19 W3 O6 92.9(5) . . ?
O19 W3 O20 84.2(5) . . ?
O19 W3 O33 72.0(4) . . ?
O20 W3 O33 74.7(4) . . ?
O32 W3 O6 88.6(5) . . ?
O32 W3 O19 155.5(5) . . ?
O32 W3 O20 85.8(5) . . ?
O32 W3 O33 83.8(5) . . ?
O8 W4 O3 71.2(4) . . ?
O16 W4 O3 73.0(5) . . ?
O16 W4 O8 86.9(5) . . ?
O16 W4 O25 89.7(5) . . ?
O16 W4 O39 157.9(5) . . ?
O25 W4 O3 85.1(5) . . ?
O25 W4 O8 156.1(5) . . ?
O39 W4 O3 85.3(5) . . ?
O39 W4 O8 89.7(5) . . ?
O39 W4 O25 84.7(5) . . ?
O52 W4 O3 169.4(6) . . ?
O52 W4 O8 101.7(6) . . ?
O52 W4 O16 99.1(6) . . ?
O52 W4 O25 102.2(6) . . ?
O52 W4 O39 102.9(6) . . ?
W5' W5 O6 59(2) . . ?
W5' W5 O12 48(2) . . ?
W5' W5 O14 113(2) . . ?
W5' W5 O23 104(2) . . ?
W5' W5 O27 42(2) . . ?
W5' W5 O28 136(2) . . ?
O6 W5 O12 89.8(5) . . ?
O6 W5 O23 157.3(5) . . ?
O6 W5 O27 84.2(4) . . ?
O12 W5 O27 73.1(5) . . ?
O14 W5 O6 87.9(5) . . ?
O14 W5 O12 156.6(5) . . ?
O14 W5 O23 86.5(5) . . ?
O14 W5 O27 83.5(5) . . ?
O23 W5 O12 86.7(5) . . ?
O23 W5 O27 73.3(4) . . ?
O28 W5 O6 102.8(6) . . ?
O28 W5 O12 98.8(6) . . ?
O28 W5 O14 104.4(6) . . ?
O28 W5 O23 99.9(6) . . ?
O28 W5 O27 169.4(5) . . ?
W5 W5' W9 143(2) . . ?
W5 W5' O6 103(2) . . ?
W5 W5' O12 116(3) . . ?
W5 W5' O14 52.0(18) . . ?
W5 W5' O23 59.9(18) . . ?
W5 W5' O27 126(3) . . ?
W5 W5' O28 32.3(18) . . ?
O6 W5' W9 113.2(11) . . ?
O6 W5' O14 84.4(10) . . ?
O6 W5' O23 157.5(14) . . ?
O6 W5' O27 105.9(13) . . ?
O6 W5' O28 93.0(11) . . ?
O12 W5' W9 41.2(7) . . ?
O12 W5' O6 112.8(14) . . ?
O12 W5' O14 161.9(14) . . ?
O12 W5' O23 88.8(11) . . ?
O12 W5' O27 93.8(12) . . ?
O12 W5' O28 92.8(12) . . ?
O14 W5' W9 138.3(11) . . ?
O23 W5' W9 86.9(8) . . ?
O23 W5' O14 73.5(8) . . ?
O23 W5' O28 79.3(9) . . ?
O27 W5' W9 53.3(6) . . ?
O27 W5' O14 86.2(10) . . ?
O27 W5' O23 77.4(9) . . ?
O27 W5' O28 155.6(13) . . ?
O28 W5' W9 132.5(10) . . ?
O28 W5' O14 80.3(9) . . ?
O1 W6 O19 87.2(5) . . ?
O1 W6 O22 87.2(5) . . ?
O1 W6 O33 85.5(4) . . ?
O1 W6 O44 157.7(5) . . ?
O19 W6 O33 71.5(4) . . ?
O19 W6 O44 89.6(5) . . ?
O22 W6 O19 158.4(5) . . ?
O22 W6 O33 87.2(5) . . ?
O22 W6 O44 87.8(5) . . ?
O44 W6 O33 72.6(4) . . ?
O46 W6 O1 100.3(6) . . ?
O46 W6 O19 99.0(6) . . ?
O46 W6 O22 102.5(6) . . ?
O46 W6 O33 168.8(5) . . ?
O46 W6 O44 101.9(6) . . ?
O7 W7 O11 72.5(4) . . ?
O7 W7 O22 87.2(5) . . ?
O17 W7 O7 101.0(7) . . ?
O17 W7 O11 170.7(6) . . ?
O17 W7 O21 101.0(7) . . ?
O17 W7 O22 100.6(6) . . ?
O17 W7 O24 101.4(6) . . ?
O21 W7 O7 157.9(5) . . ?
O21 W7 O11 85.9(4) . . ?
O21 W7 O22 86.8(5) . . ?
O21 W7 O24 86.9(5) . . ?
O22 W7 O11 86.0(4) . . ?
O24 W7 O7 90.7(6) . . ?
O24 W7 O11 72.4(4) . . ?
O24 W7 O22 157.9(5) . . ?
W8' W8 O7 143.5(14) . . ?
W8' W8 O11 143.7(14) . . ?
W8' W8 O18 89.8(14) . . ?
W8' W8 O35 104.7(14) . . ?
W8' W8 O39 61.5(14) . . ?
W8' W8 O43 43.5(14) . . ?
O7 W8 O11 72.4(4) . . ?
O18 W8 O7 89.3(5) . . ?
O18 W8 O11 84.6(4) . . ?
O18 W8 O35 159.5(5) . . ?
O18 W8 O39 91.9(5) . . ?
O35 W8 O7 87.5(5) . . ?
O35 W8 O11 75.1(5) . . ?
O39 W8 O7 154.9(5) . . ?
O39 W8 O11 82.8(5) . . ?
O39 W8 O35 82.7(5) . . ?
O43 W8 O7 101.3(6) . . ?
O43 W8 O11 171.0(5) . . ?
O43 W8 O18 102.0(5) . . ?
O43 W8 O35 98.5(6) . . ?
O43 W8 O39 102.9(6) . . ?
W8 W8' O18 69.8(14) . . ?
W8 W8' O35 57.4(12) . . ?
W8 W8' O39 96.9(16) . . ?
W8 W8' O43 114.2(19) . . ?
O18 W8' O35 125.3(11) . . ?
O39 W8' O18 94.5(10) . . ?
O39 W8' O35 79.6(8) . . ?
O43 W8' O18 113.8(12) . . ?
O43 W8' O35 100.4(11) . . ?
O43 W8' O39 143.2(16) . . ?
W5' W9 W12' 72.4(6) . . ?
O1 W9 W5' 81.3(5) . . ?
O1 W9 W12' 126.5(4) . . ?
O1 W9 O27 86.0(4) . . ?
O12 W9 W5' 32.6(6) . . ?
O12 W9 W12' 94.0(6) . . ?
O12 W9 O1 86.9(5) . . ?
O12 W9 O21 159.0(5) . . ?
O12 W9 O27 73.2(5) . . ?
O21 W9 W5' 126.6(6) . . ?
O21 W9 W12' 74.6(5) . . ?
O21 W9 O1 86.1(4) . . ?
O21 W9 O27 86.6(4) . . ?
O27 W9 W5' 41.1(6) . . ?
O27 W9 W12' 44.4(4) . . ?
O30 W9 W5' 85.8(5) . . ?
O30 W9 W12' 32.0(5) . . ?
O30 W9 O1 158.3(5) . . ?
O30 W9 O12 91.7(5) . . ?
O30 W9 O21 87.6(5) . . ?
O30 W9 O27 72.9(4) . . ?
O50 W9 W5' 129.7(7) . . ?
O50 W9 W12' 131.0(6) . . ?
O50 W9 O1 101.6(6) . . ?
O50 W9 O12 97.1(7) . . ?
O50 W9 O21 103.7(6) . . ?
O50 W9 O27 167.5(6) . . ?
O50 W9 O30 100.0(6) . . ?
O2 W10 W12' 8.7(5) . . ?
O2 W10 O11 84.5(5) . . ?
O11 W10 W12' 75.8(4) . . ?
O15 W10 W12' 110.2(5) . . ?
O15 W10 O2 101.5(6) . . ?
O15 W10 O11 171.3(5) . . ?
O15 W10 O24 100.3(5) . . ?
O15 W10 O25 103.5(5) . . ?
O15 W10 O35 99.0(6) . . ?
O24 W10 W12' 89.7(5) . . ?
O24 W10 O2 91.2(5) . . ?
O24 W10 O11 73.1(4) . . ?
O24 W10 O35 88.4(5) . . ?
O25 W10 W12' 85.8(5) . . ?
O25 W10 O2 87.9(5) . . ?
O25 W10 O11 82.9(5) . . ?
O25 W10 O24 156.0(5) . . ?
O25 W10 O35 84.2(5) . . ?
O35 W10 W12' 150.6(5) . . ?
O35 W10 O2 159.2(5) . . ?
O35 W10 O11 75.5(5) . . ?
W11' W11 O5 53(2) . . ?
W11' W11 O18 76(2) . . ?
W11' W11 O20 118(2) . . ?
W11' W11 O33 130(2) . . ?
W11' W11 O36 55(2) . . ?
W11' W11 O44 149(2) . . ?
O5 W11 O18 90.1(5) . . ?
O5 W11 O20 85.4(5) . . ?
O5 W11 O33 82.8(4) . . ?
O5 W11 O44 155.0(5) . . ?
O18 W11 O20 157.7(4) . . ?
O18 W11 O33 84.0(4) . . ?
O20 W11 O33 73.7(4) . . ?
O36 W11 O5 100.3(6) . . ?
O36 W11 O18 102.0(6) . . ?
O36 W11 O20 100.3(5) . . ?
O36 W11 O33 173.2(6) . . ?
O36 W11 O44 104.5(6) . . ?
O44 W11 O18 88.5(5) . . ?
O44 W11 O20 86.5(5) . . ?
O44 W11 O33 72.2(4) . . ?
W11 W11' O5 110(2) . . ?
W11 W11' O18 87(2) . . ?
W11 W11' O20 49.1(17) . . ?
W11 W11' O36 106(2) . . ?
W11 W11' O44 23.6(16) . . ?
O5 W11' O18 101.8(11) . . ?
O5 W11' O20 82.3(10) . . ?
O5 W11' O44 132.5(11) . . ?
O18 W11' O20 132.5(11) . . ?
O18 W11' O44 75.7(8) . . ?
O20 W11' O44 68.1(7) . . ?
O36 W11' O5 128.6(15) . . ?
O36 W11' O18 115.9(13) . . ?
O36 W11' O20 95.2(11) . . ?
O36 W11' O44 91.5(11) . . ?
W12' W12 O2 24.7(14) . . ?
W12' W12 O13 108.3(14) . . ?
W12' W12 O23 141.3(14) . . ?
W12' W12 O27 71.9(13) . . ?
W12' W12 O30 67.7(14) . . ?
W12' W12 O37 111.9(14) . . ?
O2 W12 O13 90.3(6) . . ?
O2 W12 O23 159.0(5) . . ?
O2 W12 O27 85.5(5) . . ?
O2 W12 O30 91.2(6) . . ?
O13 W12 O23 84.2(5) . . ?
O13 W12 O27 82.8(4) . . ?
O13 W12 O30 154.6(5) . . ?
O23 W12 O27 73.7(4) . . ?
O23 W12 O30 85.3(5) . . ?
O30 W12 O27 72.1(4) . . ?
O37 W12 O2 101.2(6) . . ?
O37 W12 O13 103.2(6) . . ?
O37 W12 O23 99.8(6) . . ?
O37 W12 O27 170.8(5) . . ?
O37 W12 O30 101.3(5) . . ?
W9 W12' W10 107.0(6) . . ?
W12 W12' W9 102.0(15) . . ?
W12 W12' W10 144.6(16) . . ?
W12 W12' O2 141(2) . . ?
W12 W12' O13 53.2(12) . . ?
W12 W12' O27 88.9(15) . . ?
W12 W12' O30 89.5(16) . . ?
W12 W12' O37 48.7(11) . . ?
O2 W12' W9 116.2(13) . . ?
O2 W12' W10 13.8(7) . . ?
O2 W12' O13 96.1(12) . . ?
O2 W12' O27 109.9(13) . . ?
O2 W12' O30 127.4(16) . . ?
O2 W12' O37 109.4(12) . . ?
O13 W12' W9 122.2(8) . . ?
O13 W12' W10 93.6(7) . . ?
O27 W12' W9 47.2(4) . . ?
O27 W12' W10 96.2(7) . . ?
O27 W12' O13 78.0(7) . . ?
O30 W12' W9 34.0(5) . . ?
O30 W12' W10 125.8(10) . . ?
O30 W12' O13 135.2(12) . . ?
O30 W12' O27 77.5(8) . . ?
O30 W12' O37 92.4(10) . . ?
O37 W12' W9 124.3(9) . . ?
O37 W12' W10 122.4(8) . . ?
O37 W12' O13 80.9(8) . . ?
O37 W12' O27 136.9(12) . . ?
O3 Ge1 O27 108.9(5) . . ?
O11 Ge1 O3 109.8(5) . . ?
O11 Ge1 O27 109.1(5) . . ?
O11 Ge1 O33 109.8(5) . . ?
O33 Ge1 O3 110.8(5) . . ?
O33 Ge1 O27 108.3(6) . . ?
O1W Tb1 O2W 118.0(9) . . ?
O1W Tb1 O3W 79.1(10) . . ?
O1W Tb1 O4W 142.4(9) . . ?
O1W Tb1 O5W 72.6(9) . . ?
O1W Tb1 O6W 140.5(8) . . ?
O1W Tb1 O7W 76.1(8) . . ?
O1W Tb1 O38 73.5(8) . . ?
O2W Tb1 O3W 75.5(9) . . ?
O2W Tb1 O7W 140.2(6) . . ?
O4W Tb1 O2W 77.4(7) . . ?
O4W Tb1 O3W 71.8(9) . . ?
O4W Tb1 O7W 115.3(7) . . ?
O5W Tb1 O2W 145.5(8) . . ?
O5W Tb1 O3W 74.6(10) . . ?
O5W Tb1 O4W 77.1(9) . . ?
O5W Tb1 O7W 72.7(7) . . ?
O5W Tb1 O38 139.9(8) . . ?
O6W Tb1 O2W 76.9(7) . . ?
O6W Tb1 O3W 139.7(8) . . ?
O6W Tb1 O4W 73.9(7) . . ?
O6W Tb1 O5W 117.1(7) . . ?
O6W Tb1 O7W 71.6(6) . . ?
O6W Tb1 O38 78.5(6) . . ?
O7W Tb1 O3W 143.6(9) . . ?
O38 Tb1 O2W 71.2(6) . . ?
O38 Tb1 O3W 118.7(8) . . ?
O38 Tb1 O4W 141.9(7) . . ?
O38 Tb1 O7W 79.0(6) . . ?
O31 Cu1 O31 180.0(6) 3_776 . ?
O31 Cu1 N1 95.8(6) 3_776 . ?
O31 Cu1 N1 84.2(6) 3_776 3_776 ?
O31 Cu1 N1 84.2(6) . . ?
O31 Cu1 N1 95.8(6) . 3_776 ?
N1 Cu1 N1 180.000(2) 3_776 . ?
O26 Cu2 O8W 90.5(6) . . ?
O47 Cu2 O8W 91.7(6) . . ?
O47 Cu2 O26 177.8(7) . . ?
O47 Cu2 N3 97.1(7) . . ?
N2 Cu2 O8W 99.7(7) . . ?
N2 Cu2 O26 96.4(8) . . ?
N2 Cu2 O47 83.1(8) . . ?
N2 Cu2 N3 161.2(7) . . ?
N3 Cu2 O8W 99.1(7) . . ?
N3 Cu2 O26 82.7(6) . . ?
O29 Cu3 O9W 95.5(6) . . ?
O29 Cu3 N4 91.0(6) . . ?
O53 Cu3 O9W 89.7(6) . . ?
O53 Cu3 O29 174.7(6) . . ?
O53 Cu3 N4 83.8(6) . . ?
N4 Cu3 O9W 173.1(7) . . ?
N5 Cu4 N5 180.0(9) 3_786 . ?
O45 Cu4 N5 84.5(6) 3_786 3_786 ?
O45 Cu4 N5 84.5(6) . . ?
O45 Cu4 N5 95.5(6) . 3_786 ?
O45 Cu4 N5 95.5(6) 3_786 . ?
O45 Cu4 O45 180.0(5) 3_786 . ?
W6 O1 W9 150.1(6) . . ?
W12 O2 W10 159.2(7) . . ?
W12' O2 W10 157.5(11) . . ?
W12' O2 W12 14.6(9) . . ?
W1 O3 W2 93.7(4) . . ?
W1 O3 W4 94.2(4) . . ?
W2 O3 W4 93.8(4) . . ?
Ge1 O3 W1 122.2(5) . . ?
Ge1 O3 W2 122.7(5) . . ?
Ge1 O3 W4 122.5(6) . . ?
W1 O4 W2 120.3(6) . . ?
W11 O5 W1 148.0(7) . . ?
W11' O5 W1 164.4(11) . . ?
W11' O5 W11 16.8(7) . . ?
W3 O6 W5 159.8(8) . . ?
W5' O6 W3 151.7(11) . . ?
W5' O6 W5 18.5(8) . . ?
W7 O7 W8 120.9(6) . . ?
W4 O8 W1 123.1(6) . . ?
W8 O11 W7 94.1(4) . . ?
W10 O11 W7 93.5(4) . . ?
W10 O11 W8 92.1(4) . . ?
Ge1 O11 W7 123.1(6) . . ?
Ge1 O11 W8 121.9(5) . . ?
Ge1 O11 W10 123.8(5) . . ?
W5 O12 W9 119.1(6) . . ?
W5' O12 W5 16.8(8) . . ?
W5' O12 W9 106.2(11) . . ?
W2 O13 W12' 146.1(8) . . ?
W12 O13 W2 148.2(7) . . ?
W12 O13 W12' 18.5(5) . . ?
W2 O14 W5' 137.2(9) . . ?
W5 O14 W2 145.5(6) . . ?
W5 O14 W5' 15.0(6) . . ?
W4 O16 W2 121.2(6) . . ?
W8 O18 W8' 20.4(5) . . ?
W8 O18 W11 157.8(7) . . ?
W11 O18 W8' 149.6(9) . . ?
W11' O18 W8 149.0(9) . . ?
W11' O18 W8' 133.9(11) . . ?
W11' O18 W11 17.7(6) . . ?
W3 O19 W6 121.6(6) . . ?
W3 O20 W11' 124.4(7) . . ?
W11 O20 W3 118.6(5) . . ?
W11 O20 W11' 13.2(5) . . ?
W7 O21 W9 150.2(6) . . ?
W6 O22 W7 151.4(7) . . ?
W5 O23 W5' 16.2(6) . . ?
W12 O23 W5 119.3(6) . . ?
W12 O23 W5' 105.9(8) . . ?
W10 O24 W7 121.0(6) . . ?
W10 O25 W4 147.3(6) . . ?
C18 O26 Cu2 114.7(12) . . ?
W5' O27 W5 12.8(7) . . ?
W5' O27 W9 85.7(8) . . ?
W5' O27 W12 102.9(8) . . ?
W5' O27 W12' 120.7(10) . . ?
W9 O27 W5 94.5(4) . . ?
W9 O27 W12 94.2(4) . . ?
W12 O27 W5 93.0(4) . . ?
W12' O27 W5 111.7(8) . . ?
W12' O27 W9 88.4(6) . . ?
W12' O27 W12 19.2(6) . . ?
Ge1 O27 W5 123.0(6) . . ?
Ge1 O27 W5' 121.3(9) . . ?
Ge1 O27 W9 122.0(6) . . ?
Ge1 O27 W12 122.4(6) . . ?
Ge1 O27 W12' 111.4(8) . . ?
W5 O28 W5' 11.3(6) . . ?
C18 O29 Cu3 125.6(14) . . ?
W9 O30 W12 120.8(5) . . ?
W12' O30 W9 114.0(8) . . ?
W12' O30 W12 22.8(7) . . ?
C6 O31 Cu1 113.2(12) . . ?
W3 O32 W1 146.5(6) . . ?
W3 O33 W11 92.2(4) . . ?
W6 O33 W3 94.8(4) . . ?
W6 O33 W11 93.6(4) . . ?
Ge1 O33 W3 123.0(6) . . ?
Ge1 O33 W6 123.6(6) . . ?
Ge1 O33 W11 121.5(6) . . ?
W8 O35 W8' 17.9(5) . . ?
W10 O35 W8 117.0(7) . . ?
W10 O35 W8' 129.4(8) . . ?
W11' O36 W11 19.0(8) . . ?
W12 O37 W12' 19.3(6) . . ?
C6 O38 Tb1 142.5(14) . . ?
W4 O39 W8 148.4(6) . . ?
W8' O39 W4 165.7(9) . . ?
W8' O39 W8 21.6(7) . . ?
W8' O43 W8 22.3(8) . . ?
W6 O44 W11' 127.1(7) . . ?
W11 O44 W6 121.4(5) . . ?
W11 O44 W11' 7.0(5) . . ?
C11 O47 Cu2 116.6(17) . . ?
C24 O53 Cu3 115.2(11) . . ?
C1 N1 Cu1 129.0(12) . . ?
C1 N1 C5 120.4(17) . . ?
C5 N1 Cu1 110.2(12) . . ?
C7 N2 Cu2 131.5(19) . . ?
C7 N2 C12 116(2) . . ?
C12 N2 Cu2 112.0(17) . . ?
C13 N3 Cu2 129.4(14) . . ?
C13 N3 C17 116.8(18) . . ?
C17 N3 Cu2 113.7(12) . . ?
C19 N4 Cu3 129.2(14) . . ?
C19 N4 C23 119.1(17) . . ?
C23 N4 Cu3 111.5(11) . . ?
C25 N5 Cu4 131.1(16) . . ?
C25 N5 C29 116.9(19) . . ?
C29 N5 Cu4 111.8(13) . . ?
N1 C1 C2 120.7(18) . . ?
C1 C2 C3 119(2) . . ?
C4 C3 C2 117(2) . . ?
C3 C4 C5 123(2) . . ?
N1 C5 C6 115.4(17) . . ?
C4 C5 N1 119.7(18) . . ?
C4 C5 C6 124.7(19) . . ?
O31 C6 C5 116.2(17) . . ?
O38 C6 O31 121.9(17) . . ?
O38 C6 C5 122.0(17) . . ?
N2 C7 C8 125(3) . . ?
C9 C8 C7 116(3) . . ?
C10 C9 C8 121(3) . . ?
C9 C10 C12 120(3) . . ?
O47 C11 C12 114(2) . . ?
O64 C11 O47 127(3) . . ?
O64 C11 C12 119(3) . . ?
N2 C12 C11 112(2) . . ?
C10 C12 N2 121(3) . . ?
C10 C12 C11 126(2) . . ?
N3 C13 C14 122.9(19) . . ?
C13 C14 C15 118.2(18) . . ?
C16 C15 C14 120(2) . . ?
C15 C16 C17 117(2) . . ?
N3 C17 C18 111.6(18) . . ?
C16 C17 N3 125.3(17) . . ?
C16 C17 C18 123.0(16) . . ?
O26 C18 C17 116.8(16) . . ?
O29 C18 O26 123.8(19) . . ?
O29 C18 C17 119.4(18) . . ?
N4 C19 C20 121(2) . . ?
C21 C20 C19 118.3(19) . . ?
C20 C21 C22 122(2) . . ?
C23 C22 C21 116(2) . . ?
N4 C23 C22 123.3(17) . . ?
N4 C23 C24 113.9(15) . . ?
C22 C23 C24 122.8(19) . . ?
O53 C24 C23 114.0(16) . . ?
O68 C24 O53 123.7(18) . . ?
O68 C24 C23 122.3(19) . . ?
N5 C25 C26 127(3) . . ?
C27 C26 C25 113(3) . . ?
C26 C27 C28 125(3) . . ?
C29 C28 C27 114(2) . . ?
N5 C29 C30 112.3(18) . . ?
C28 C29 N5 125(2) . . ?
C28 C29 C30 123(2) . . ?
O45 C30 C29 118.5(19) . . ?
O61 C30 C29 118.8(18) . . ?
O61 C30 O45 122.6(19) . . ?
C30 O45 Cu4 112.2(12) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1891066'
loop_
_audit_author_name
_audit_author_address
'Junwei Zhao'
;Henan University
China
;
_audit_update_record             
;
2019-02-11 deposited with the CCDC.	2019-02-14 downloaded from the CCDC.
;
# start Validation Reply Form

_vrf_PLAT201_1                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......    14 Report 
RESPONSE: Due to the large structure and the existence of a large 
 amount of weight atoms, the intensity data are not very good, 
 leading to the ADP max/min ratio of some water molecules, and it is 
very difficult to refine this large structure, therefore, 
 in the final refinement, the W, Ge, Cu and La atoms were refined 
anisotropically, some O atoms and water molecules were
 refined isotropically.
;


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


_vrf_PLAT306_1                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O15W Check
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

_vrf_PLAT342_1                   
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02867 Ang.
RESPONSE: The alert derives from shading of reciprocal space
 by the pressure cell, and it is unavoidable in high pressure
 crystal structure determinations.
;


# end Validation Reply Form


_audit_creation_date             2019-02-09
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'Ge O40 W12, C18 H12 Cu2 La0.5 N3 Na0.5 O16, C18 H12 Cu2 N3 O8, 8(O)'
_chemical_formula_sum            'C36 H64 Cu4 Ge La0.50 N6 Na0.50 O72 W12'
_chemical_formula_weight         4346.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   18.7617(9)
_cell_length_b                   14.7533(7)
_cell_length_c                   31.1104(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.9910(10)
_cell_angle_gamma                90.00
_cell_volume                     8578.6(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9539
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.988
_cell_measurement_theta_min      2.407
_exptl_absorpt_coefficient_mu    17.694
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1302 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.4529.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            mazarine
_exptl_crystal_density_diffrn    3.366
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7872
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43205
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                11706
_reflns_number_total             15057
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         2.419
_refine_diff_density_min         -2.842
_refine_diff_density_rms         0.321
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         15057
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0502
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0385P)²+149.0722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1159
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{La1, Na1}
3. Restrained distances
 La1-O14W
 2.8 with sigma of 0.01
4. Rigid bond restraints
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(La1) = Uanis(Na1)
6. Others
 Fixed Sof: La1(0.5) Na1(0.5)
 Fixed Uiso: O3W(0.08902) O4W(0.08428) O5W(0.0863) O6W(0.08905) O7W(0.08352)
 O9W(0.09367) O14W(0.13141) O19W(0.14921) O45(0.05872)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C7(H7A), C8(H8A), C9(H9A), C10(H10A),
 C13(H13A), C14(H14A), C15(H15A), C16(H16A), C19(H19A), C20(H20A), C21(H21A),
 C22(H22A), C25(H25A), C26(H26A), C27(H27A), C28(H28A), C31(H31A), C32(H32A),
 C33(H33A), C34(H34A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
W1 W 0.38168(3) -0.58257(4) -0.32433(2) 0.02444(15) Uani 1 d . . . .
W2 W 0.39795(3) -0.56451(4) -0.16383(2) 0.02170(14) Uani 1 d . . . .
W3 W 0.60489(3) -0.39704(4) -0.32518(2) 0.02399(15) Uani 1 d . . . .
W4 W 0.45755(3) -0.72037(4) -0.24770(2) 0.02240(15) Uani 1 d . . . .
W5 W 0.55533(3) -0.64063(4) -0.32485(2) 0.02564(15) Uani 1 d . . . .
W6 W 0.44497(3) -0.34471(4) -0.16419(2) 0.02133(14) Uani 1 d . . . .
W7 W 0.32394(3) -0.42595(4) -0.24016(2) 0.02329(15) Uani 1 d . . . .
W8 W 0.63667(3) -0.40824(4) -0.16476(2) 0.02308(15) Uani 1 d . . . .
W9 W 0.55172(3) -0.25591(4) -0.24981(2) 0.02123(14) Uani 1 d . . . .
W10 W 0.43112(3) -0.33848(4) -0.32602(2) 0.02364(15) Uani 1 d . . . .
W11 W 0.58988(3) -0.62762(4) -0.16308(2) 0.02090(14) Uani 1 d . . . .
W12 W 0.68815(3) -0.55045(4) -0.24020(2) 0.02398(15) Uani 1 d . . . .
Ge1 Ge 0.50506(7) -0.48836(9) -0.24472(5) 0.0131(3) Uani 1 d . . . .
La1 La 0.10428(11) -1.15596(13) 0.00745(7) 0.0481(5) Uani 0.50 d A 1 D .
Na1 Na 0.10428(11) -1.15596(13) 0.00745(7) 0.0481(5) Uani 0.50 d A 2 . .
Cu1 Cu 0.59483(10) -0.72309(12) -0.04208(7) 0.0317(5) Uani 1 d . . . .
Cu2 Cu 0.34676(11) -0.88790(16) -0.00556(7) 0.0438(6) Uani 1 d A . . .
Cu3 Cu 0.48910(11) -0.99640(13) -0.23748(7) 0.0351(5) Uani 1 d . . . .
Cu4 Cu 0.44035(12) -1.00866(18) -0.40257(8) 0.0521(6) Uani 1 d . . . .
N1 N 0.5801(7) -0.5912(9) -0.0413(4) 0.033(3) Uani 1 d . . . .
N2 N 0.3395(7) -0.8824(9) -0.0686(5) 0.035(3) Uani 1 d . . . .
N3 N 0.3439(7) -0.8869(9) 0.0575(5) 0.035(3) Uani 1 d A . . .
N4 N 0.5801(7) -0.9299(9) -0.2327(5) 0.036(3) Uani 1 d . . . .
N5 N 0.3992(7) -1.0667(8) -0.2402(5) 0.033(3) Uani 1 d . . . .
N6 N 0.5432(7) -1.0396(9) -0.3883(4) 0.031(3) Uani 1 d . . . .
O1W O 0.5787(8) -0.7509(10) 0.0288(5) 0.069(4) Uani 1 d . . . .
O2W O 0.6248(6) -0.8500(7) -0.0507(4) 0.040(3) Uani 1 d . . . .
O3W O 0.0675(9) -1.2197(12) -0.0667(6) 0.089 Uiso 1 d . . . .
O4W O 0.0910(9) -1.0178(11) -0.0523(6) 0.084 Uiso 1 d . . . .
O5W O 0.0474(9) -1.0385(11) 0.0519(6) 0.086 Uiso 1 d . . . .
O6W O 0.0413(9) -1.2268(12) 0.0653(6) 0.089 Uiso 1 d . . . .
O7W O 0.2068(9) -1.2082(11) 0.0638(6) 0.084 Uiso 1 d . . . .
O8W O 0.1102(9) -1.3336(12) 0.0051(7) 0.096(6) Uiso 1 d . . . .
O9W O 0.2191(9) -1.1578(12) -0.0279(7) 0.094 Uiso 1 d . . . .
O10W O 0.2713(10) -0.7523(13) -0.0079(7) 0.105(6) Uiso 1 d . . . .
O11W O 0.3360(10) -0.9890(13) -0.4266(7) 0.103(6) Uiso 1 d . . . .
O12W O 0.4287(9) -1.1490(11) -0.4441(6) 0.088(5) Uiso 1 d . . . .
O13W O 0.4357(11) -0.8544(14) -0.3695(8) 0.117(7) Uiso 1 d . . . .
O14W O -0.0404(6) -1.1579(15) -0.0245(8) 0.131 Uiso 1 d . . D .
O15W O 0.9435(10) -0.4321(13) 0.4056(7) 0.101(6) Uiso 1 d . . . .
O16W O 0.7339(9) 0.1654(12) 0.4155(7) 0.096(6) Uiso 1 d . . . .
O17W O -0.1324(13) -1.1575(17) 0.0384(9) 0.150(9) Uiso 1 d . . . .
O18W O -0.2022(11) -1.2784(14) -0.0619(8) 0.121(7) Uiso 1 d . . . .
O19W O 0.7971(13) 0.3478(17) 0.1566(9) 0.149 Uiso 1 d . . . .
O1 O 0.5963(6) -0.6995(7) -0.3629(4) 0.036(3) Uani 1 d . . . .
O2 O 0.7723(5) -0.5799(8) -0.2515(4) 0.042(3) Uani 1 d . . . .
O3 O 0.4380(6) -0.8304(7) -0.2370(4) 0.036(3) Uani 1 d . . . .
O4 O 0.5721(5) -0.1450(6) -0.2396(4) 0.031(3) Uani 1 d . . . .
O5 O 0.3116(6) -0.6021(7) -0.3616(4) 0.038(3) Uani 1 d . . . .
O6 O 0.6733(5) -0.6346(6) -0.1950(4) 0.029(3) Uani 1 d . . . .
O7 O 0.4604(5) -0.6302(6) -0.3542(3) 0.022(2) Uani 1 d . . . U
O8 O 0.3586(5) -0.6233(7) -0.1252(4) 0.031(3) Uani 1 d . . . .
O9 O 0.3517(5) -0.3402(6) -0.1957(3) 0.024(2) Uani 1 d . . . .
O10 O 0.3160(5) -0.5137(6) -0.1953(3) 0.022(2) Uani 1 d . . . .
O11 O 0.5186(5) -0.7400(6) -0.2929(3) 0.025(2) Uani 1 d . . . .
O12 O 0.4988(5) -0.5889(6) -0.1495(3) 0.022(2) Uani 1 d . . . .
O13 O 0.6152(5) -0.3212(6) -0.2094(3) 0.024(2) Uani 1 d . . . .
O14 O 0.3774(6) -0.2829(7) -0.3649(4) 0.036(3) Uani 1 d . . . .
O15 O 0.3818(5) -0.6932(7) -0.2922(3) 0.026(2) Uani 1 d . . . .
O16 O 0.5382(5) -0.6978(6) -0.2082(3) 0.021(2) Uani 1 d . . . .
O17 O 0.6625(6) -0.3756(7) -0.3631(4) 0.037(3) Uani 1 d . . . .
O18 O 0.5172(5) -0.3488(6) -0.3548(3) 0.027(2) Uani 1 d . . . .
O19 O 0.4806(5) -0.2791(6) -0.2096(4) 0.027(2) Uani 1 d . . . .
O20 O 0.6296(5) -0.6222(6) -0.2791(3) 0.024(2) Uani 1 d . . . .
O21 O 0.5826(5) -0.5120(6) -0.2118(3) 0.017(2) Uani 1 d . . . .
O22 O 0.6650(5) -0.4543(7) -0.2801(3) 0.025(2) Uani 1 d . . . .
O23 O 0.6316(5) -0.5217(6) -0.1339(3) 0.020(2) Uani 1 d . . . .
O24 O 0.4048(5) -0.6540(6) -0.2077(3) 0.024(2) Uani 1 d . . . .
O25 O 0.3366(5) -0.5220(6) -0.2794(3) 0.023(2) Uani 1 d . . . .
O26 O 0.4755(5) -0.2385(6) -0.2948(3) 0.025(2) Uani 1 d . . . .
O27 O 0.6115(5) -0.7059(6) -0.1231(3) 0.026(2) Uani 1 d . . . .
O28 O 0.5709(5) -0.5178(6) -0.3397(4) 0.030(3) Uani 1 d . . . .
O29 O 0.2353(6) -0.3971(8) -0.2511(4) 0.039(3) Uani 1 d . . . .
O30 O 0.5188(4) -0.3972(5) -0.2775(3) 0.016(2) Uani 1 d . . . .
O31 O 0.7097(5) -0.4593(6) -0.1963(3) 0.024(2) Uani 1 d . . . .
O32 O 0.4379(5) -0.4634(6) -0.2118(3) 0.019(2) Uani 1 d . . . .
O33 O 0.4814(5) -0.5815(6) -0.2769(3) 0.019(2) Uani 1 d . . . .
O34 O 0.4364(6) -0.2630(7) -0.1267(3) 0.032(3) Uani 1 d . . . U
O35 O 0.4107(5) -0.4624(6) -0.3388(4) 0.027(2) Uani 1 d . . . .
O36 O 0.3698(5) -0.3540(6) -0.2802(3) 0.023(2) Uani 1 d . . . .
O37 O 0.4119(5) -0.4487(7) -0.1336(3) 0.023(2) Uani 1 d . . . .
O38 O 0.5404(5) -0.3831(6) -0.1502(3) 0.022(2) Uani 1 d . . . .
O39 O 0.6146(5) -0.2837(6) -0.2935(3) 0.025(2) Uani 1 d . . . .
O40 O 0.6866(5) -0.3481(7) -0.1268(4) 0.032(3) Uani 1 d . . . .
O41 O 0.7640(7) -0.5717(10) -0.0080(6) 0.074(5) Uani 1 d . . . .
O42 O 0.6947(6) -0.6892(8) -0.0270(5) 0.047(3) Uani 1 d . . . .
O43 O 0.4966(5) -0.7536(8) -0.0631(4) 0.038(3) Uani 1 d . . . .
O44 O 0.4376(6) -0.8154(7) -0.0117(4) 0.033(3) Uani 1 d . . . .
O45 O 0.1850(7) -1.0150(9) 0.0402(5) 0.059 Uiso 1 d . . . .
O46 O 0.2602(8) -0.9644(13) -0.0035(5) 0.093(6) Uani 1 d . . . .
O47 O 0.5019(7) -0.9936(8) -0.1761(4) 0.047(3) Uani 1 d . . . .
O48 O 0.5700(8) -0.9334(9) -0.1213(5) 0.063(4) Uani 1 d . . . .
O49 O 0.4726(6) -0.9992(7) -0.3012(4) 0.036(3) Uani 1 d . . . .
O50 O 0.3997(6) -1.0616(8) -0.3532(4) 0.041(3) Uani 1 d . . . .
O51 O 0.5791(8) -0.8863(10) -0.4702(5) 0.073(5) Uani 1 d . . . .
O52 O 0.4776(7) -0.9415(10) -0.4495(5) 0.065(4) Uani 1 d . . . .
C1 C 0.5205(12) -0.5431(12) -0.0518(6) 0.051(5) Uani 1 d . . . .
H1A H 0.4787 -0.5737 -0.0611 0.061 Uiso 1 calc . . R .
C2 C 0.5192(13) -0.4482(12) -0.0493(6) 0.052(6) Uani 1 d . . . .
H2A H 0.4770 -0.4162 -0.0560 0.063 Uiso 1 calc . . R .
C3 C 0.5803(13) -0.4050(13) -0.0369(8) 0.063(6) Uani 1 d . . . .
H3A H 0.5803 -0.3421 -0.0345 0.076 Uiso 1 calc . . R .
C4 C 0.6441(13) -0.4527(13) -0.0274(7) 0.063(6) Uani 1 d . . . .
H4A H 0.6872 -0.4230 -0.0200 0.075 Uiso 1 calc . . R .
C5 C 0.6400(10) -0.5440(12) -0.0296(6) 0.043(4) Uani 1 d . . . U
C6 C 0.7062(9) -0.6067(12) -0.0195(7) 0.044(5) Uani 1 d . . . .
C7 C 0.2910(10) -0.9196(12) -0.0964(6) 0.045(5) Uani 1 d . . . .
H7A H 0.2541 -0.9524 -0.0856 0.054 Uiso 1 calc . . R .
C8 C 0.2921(9) -0.9124(13) -0.1402(6) 0.044(5) Uani 1 d . . . .
H8A H 0.2561 -0.9384 -0.1586 0.053 Uiso 1 calc . . R .
C9 C 0.3481(9) -0.8655(12) -0.1570(6) 0.039(4) Uani 1 d . . . .
H9A H 0.3514 -0.8605 -0.1865 0.047 Uiso 1 calc . . R .
C10 C 0.3986(9) -0.8267(10) -0.1272(6) 0.035(4) Uani 1 d . . . .
H10A H 0.4365 -0.7943 -0.1370 0.042 Uiso 1 calc . . R .
C11 C 0.3935(8) -0.8355(10) -0.0836(5) 0.027(4) Uani 1 d . . . .
C12 C 0.4457(9) -0.7999(10) -0.0494(7) 0.035(4) Uani 1 d . . . .
C13 C 0.3907(11) -0.8473(11) 0.0877(6) 0.047(5) Uani 1 d . . . .
H13A H 0.4323 -0.8201 0.0798 0.056 Uiso 1 calc . . R .
C14 C 0.3756(14) -0.8482(12) 0.1296(7) 0.059(6) Uani 1 d . . . .
H14A H 0.4083 -0.8211 0.1498 0.071 Uiso 1 calc . . R .
C15 C 0.3180(15) -0.8848(15) 0.1436(8) 0.071(8) Uani 1 d . . . .
H15A H 0.3088 -0.8821 0.1724 0.086 Uiso 1 calc . . R .
C16 C 0.2720(12) -0.9274(18) 0.1130(9) 0.071(7) Uani 1 d A . . .
H16A H 0.2318 -0.9574 0.1213 0.085 Uiso 1 calc . . R .
C17 C 0.2851(10) -0.9258(14) 0.0705(7) 0.052(5) Uani 1 d . . . .
C18 C 0.2412(11) -0.966(2) 0.0347(9) 0.085(9) Uani 1 d A . . .
C19 C 0.6154(9) -0.8994(10) -0.2659(6) 0.038(4) Uani 1 d . . . .
H19A H 0.5982 -0.9142 -0.2940 0.046 Uiso 1 calc . . R .
C20 C 0.6746(10) -0.8482(11) -0.2596(9) 0.056(6) Uani 1 d . . . .
H20A H 0.6969 -0.8248 -0.2827 0.067 Uiso 1 calc . . R .
C21 C 0.7014(9) -0.8314(12) -0.2168(10) 0.068(7) Uani 1 d . . . U
H21A H 0.7437 -0.7991 -0.2111 0.082 Uiso 1 calc . . R .
C22 C 0.6641(10) -0.8633(12) -0.1830(9) 0.058(6) Uani 1 d . . . U
H22A H 0.6803 -0.8509 -0.1545 0.070 Uiso 1 calc . . R .
C23 C 0.6046(9) -0.9122(11) -0.1923(7) 0.042(5) Uani 1 d . . . .
C24 C 0.5548(11) -0.9477(11) -0.1595(6) 0.042(5) Uani 1 d . . . .
C25 C 0.5719(11) -1.0965(12) -0.3593(7) 0.052(5) Uani 1 d . . . .
H25A H 0.5425 -1.1289 -0.3422 0.062 Uiso 1 calc . . R .
C26 C 0.3055(9) -1.1470(12) -0.2149(7) 0.042(5) Uani 1 d . . . .
H26A H 0.2819 -1.1677 -0.1917 0.050 Uiso 1 calc . . R .
C27 C 0.2786(8) -1.1676(11) -0.2567(7) 0.042(5) Uani 1 d . . . .
H27A H 0.2376 -1.2028 -0.2619 0.051 Uiso 1 calc . . R .
C28 C 0.3131(8) -1.1355(10) -0.2892(6) 0.035(4) Uani 1 d . . . .
H28A H 0.2958 -1.1469 -0.3176 0.043 Uiso 1 calc . . R .
C29 C 0.3733(9) -1.0866(10) -0.2807(6) 0.031(4) Uani 1 d . . . .
C30 C 0.4188(9) -1.0436(10) -0.3140(6) 0.034(4) Uani 1 d . . . .
C31 C 0.3647(9) -1.0979(12) -0.2076(6) 0.041(4) Uani 1 d . . . .
H31A H 0.3822 -1.0852 -0.1793 0.049 Uiso 1 calc . . R .
C32 C 0.6470(10) -1.1092(13) -0.3538(8) 0.056(6) Uani 1 d . . . .
H32A H 0.6679 -1.1482 -0.3329 0.068 Uiso 1 calc . . R .
C33 C 0.6874(9) -1.0615(15) -0.3805(8) 0.064(7) Uani 1 d . . . .
H33A H 0.7366 -1.0705 -0.3789 0.077 Uiso 1 calc . . R .
C34 C 0.6569(10) -1.0019(12) -0.4092(7) 0.048(5) Uani 1 d . . . .
H34A H 0.6854 -0.9678 -0.4262 0.057 Uiso 1 calc . . R .
C35 C 0.5851(9) -0.9913(12) -0.4134(6) 0.040(4) Uani 1 d . . . .
C36 C 0.5459(13) -0.9356(15) -0.4468(7) 0.061(6) Uani 1 d . . . .
O20W O 0.4266(7) -1.0232(9) -0.0077(5) 0.062(4) Uiso 1 d . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O5 1.700(11) . ?
W1 O7 1.943(9) . ?
W1 O15 1.913(10) . ?
W1 O25 1.917(10) . ?
W1 O33 2.280(9) . ?
W1 O35 1.920(9) . ?
W2 O8 1.702(10) . ?
W2 O10 1.902(9) . ?
W2 O12 1.939(9) . ?
W2 O24 1.912(10) . ?
W2 O32 2.282(9) . ?
W2 O37 1.957(10) . ?
W3 O17 1.698(11) . ?
W3 O18 1.948(10) . ?
W3 O22 1.919(10) . ?
W3 O28 1.933(10) . ?
W3 O30 2.286(9) . ?
W3 O39 1.941(10) . ?
W4 O3 1.704(10) . ?
W4 O11 1.911(10) . ?
W4 O15 1.937(10) . ?
W4 O16 1.895(10) . ?
W4 O24 1.923(10) . ?
W4 O33 2.300(9) . ?
W5 O1 1.704(11) . ?
W5 O7 1.935(9) . ?
W5 O11 1.932(10) . ?
W5 O20 1.924(10) . ?
W5 O28 1.900(9) . ?
W5 O33 2.295(9) . ?
W6 O9 1.932(9) . ?
W6 O19 1.883(11) . ?
W6 O32 2.289(9) . ?
W6 O34 1.694(11) . ?
W6 O37 1.936(10) . ?
W6 O38 1.893(9) . ?
W7 O9 1.912(10) . ?
W7 O10 1.920(10) . ?
W7 O25 1.899(10) . ?
W7 O29 1.722(10) . ?
W7 O32 2.309(9) . ?
W7 O36 1.898(10) . ?
W8 O13 1.909(10) . ?
W8 O21 2.293(9) . ?
W8 O23 1.937(9) . ?
W8 O31 1.908(10) . ?
W8 O38 1.935(9) . ?
W8 O40 1.694(11) . ?
W9 O4 1.704(10) . ?
W9 O13 1.914(10) . ?
W9 O19 1.936(11) . ?
W9 O26 1.929(10) . ?
W9 O30 2.319(9) . ?
W9 O39 1.921(10) . ?
W10 O14 1.716(11) . ?
W10 O18 1.920(10) . ?
W10 O26 1.916(10) . ?
W10 O30 2.303(9) . ?
W10 O35 1.903(9) . ?
W10 O36 1.923(10) . ?
W11 O6 1.928(10) . ?
W11 O12 1.884(9) . ?
W11 O16 1.935(10) . ?
W11 O21 2.279(9) . ?
W11 O23 1.939(9) . ?
W11 O27 1.721(10) . ?
W12 O2 1.703(10) . ?
W12 O6 1.914(11) . ?
W12 O20 1.886(10) . ?
W12 O21 2.308(9) . ?
W12 O22 1.909(10) . ?
W12 O31 1.934(10) . ?
Ge1 O21 1.739(9) . ?
Ge1 O30 1.720(9) . ?
Ge1 O32 1.731(9) . ?
Ge1 O33 1.735(9) . ?
La1 O3W 2.532(19) . ?
La1 O4W 2.755(18) . ?
La1 O5W 2.512(18) . ?
La1 O6W 2.468(19) . ?
La1 O7W 2.604(17) . ?
La1 O8W 2.624(18) . ?
La1 O9W 2.502(18) . ?
La1 O14W 2.808(9) . ?
La1 O45 2.717(14) . ?
Cu1 N1 1.966(14) . ?
Cu1 O1W 2.288(15) . ?
Cu1 O2W 1.980(11) . ?
Cu1 O42 1.957(11) . ?
Cu1 O43 1.954(10) . ?
Cu2 N2 1.954(15) . ?
Cu2 N3 1.966(15) . ?
Cu2 O44 2.035(11) . ?
Cu2 O46 1.983(13) . ?
Cu3 N4 1.963(14) . ?
Cu3 N5 1.976(13) . ?
Cu3 O47 1.904(13) . ?
Cu3 O49 1.981(12) . ?
Cu4 N6 1.996(14) . ?
Cu4 O11W 2.054(19) . ?
Cu4 O12W 2.440(18) . ?
Cu4 O50 1.938(12) . ?
Cu4 O52 1.944(15) . ?
N1 C1 1.34(2) . ?
N1 C5 1.34(2) . ?
N2 C7 1.32(2) . ?
N2 C11 1.345(19) . ?
N3 C13 1.36(2) . ?
N3 C17 1.34(2) . ?
N4 C19 1.35(2) . ?
N4 C23 1.33(2) . ?
N5 C29 1.34(2) . ?
N5 C31 1.33(2) . ?
N6 C25 1.31(2) . ?
N6 C35 1.36(2) . ?
O41 C6 1.225(19) . ?
O42 C6 1.254(19) . ?
O43 C12 1.276(18) . ?
O44 C12 1.22(2) . ?
O45 C18 1.30(2) . ?
O46 C18 1.27(3) . ?
O47 C24 1.27(2) . ?
O48 C24 1.21(2) . ?
O49 C30 1.241(19) . ?
O50 C30 1.27(2) . ?
O51 C36 1.23(2) . ?
O52 C36 1.28(2) . ?
C1 C2 1.40(2) . ?
C2 C3 1.34(3) . ?
C3 C4 1.40(3) . ?
C4 C5 1.35(2) . ?
C5 C6 1.56(3) . ?
C7 C8 1.37(3) . ?
C8 C9 1.40(2) . ?
C9 C10 1.39(2) . ?
C10 C11 1.37(2) . ?
C11 C12 1.48(2) . ?
C13 C14 1.36(3) . ?
C14 C15 1.32(3) . ?
C15 C16 1.38(3) . ?
C16 C17 1.37(3) . ?
C17 C18 1.45(3) . ?
C19 C20 1.34(2) . ?
C20 C21 1.40(3) . ?
C21 C22 1.40(3) . ?
C22 C23 1.34(2) . ?
C23 C24 1.53(3) . ?
C25 C32 1.42(3) . ?
C26 C27 1.39(3) . ?
C26 C31 1.33(2) . ?
C27 C28 1.34(3) . ?
C28 C29 1.35(2) . ?
C29 C30 1.54(2) . ?
C32 C33 1.37(3) . ?
C33 C34 1.34(3) . ?
C34 C35 1.35(2) . ?
C35 C36 1.47(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 W1 O7 100.8(5) . . ?
O5 W1 O15 100.2(5) . . ?
O5 W1 O25 102.2(5) . . ?
O5 W1 O33 170.0(4) . . ?
O5 W1 O35 102.4(5) . . ?
O7 W1 O33 72.3(4) . . ?
O15 W1 O7 88.5(4) . . ?
O15 W1 O25 89.9(4) . . ?
O15 W1 O33 72.8(4) . . ?
O15 W1 O35 157.3(4) . . ?
O25 W1 O7 156.8(4) . . ?
O25 W1 O33 85.1(4) . . ?
O25 W1 O35 83.9(4) . . ?
O35 W1 O7 88.8(4) . . ?
O35 W1 O33 85.0(4) . . ?
O8 W2 O10 100.5(4) . . ?
O8 W2 O12 102.6(4) . . ?
O8 W2 O24 102.3(5) . . ?
O8 W2 O32 169.2(4) . . ?
O8 W2 O37 98.8(5) . . ?
O10 W2 O12 156.9(4) . . ?
O10 W2 O24 90.4(4) . . ?
O10 W2 O32 72.8(4) . . ?
O10 W2 O37 88.4(4) . . ?
O12 W2 O32 84.4(4) . . ?
O12 W2 O37 88.0(4) . . ?
O24 W2 O12 84.9(4) . . ?
O24 W2 O32 86.5(4) . . ?
O24 W2 O37 158.7(4) . . ?
O37 W2 O32 72.9(4) . . ?
O17 W3 O18 99.6(5) . . ?
O17 W3 O22 102.7(5) . . ?
O17 W3 O28 103.0(5) . . ?
O17 W3 O30 168.4(4) . . ?
O17 W3 O39 98.9(5) . . ?
O18 W3 O30 72.1(4) . . ?
O22 W3 O18 157.7(4) . . ?
O22 W3 O28 85.8(4) . . ?
O22 W3 O30 85.9(4) . . ?
O22 W3 O39 89.2(4) . . ?
O28 W3 O18 88.7(4) . . ?
O28 W3 O30 85.1(4) . . ?
O28 W3 O39 158.1(4) . . ?
O39 W3 O18 87.9(4) . . ?
O39 W3 O30 73.3(4) . . ?
O3 W4 O11 98.8(5) . . ?
O3 W4 O15 100.4(5) . . ?
O3 W4 O16 102.3(5) . . ?
O3 W4 O24 103.1(5) . . ?
O3 W4 O33 168.0(5) . . ?
O11 W4 O15 87.4(4) . . ?
O11 W4 O24 158.1(4) . . ?
O11 W4 O33 72.2(4) . . ?
O15 W4 O33 71.9(4) . . ?
O16 W4 O11 90.4(4) . . ?
O16 W4 O15 157.2(4) . . ?
O16 W4 O24 85.3(4) . . ?
O16 W4 O33 85.9(4) . . ?
O24 W4 O15 88.3(4) . . ?
O24 W4 O33 86.1(4) . . ?
O1 W5 O7 99.5(5) . . ?
O1 W5 O11 100.0(5) . . ?
O1 W5 O20 104.2(5) . . ?
O1 W5 O28 103.2(5) . . ?
O1 W5 O33 168.4(4) . . ?
O7 W5 O33 72.1(4) . . ?
O11 W5 O7 87.0(4) . . ?
O11 W5 O33 72.0(4) . . ?
O20 W5 O7 156.3(4) . . ?
O20 W5 O11 89.6(4) . . ?
O20 W5 O33 84.5(4) . . ?
O28 W5 O7 87.9(4) . . ?
O28 W5 O11 156.8(4) . . ?
O28 W5 O20 85.9(4) . . ?
O28 W5 O33 84.9(4) . . ?
O9 W6 O32 72.5(4) . . ?
O9 W6 O37 87.8(4) . . ?
O19 W6 O9 88.1(4) . . ?
O19 W6 O32 85.0(4) . . ?
O19 W6 O37 157.9(4) . . ?
O19 W6 O38 86.3(4) . . ?
O34 W6 O9 100.9(5) . . ?
O34 W6 O19 102.2(5) . . ?
O34 W6 O32 170.2(4) . . ?
O34 W6 O37 99.9(5) . . ?
O34 W6 O38 101.5(5) . . ?
O37 W6 O32 73.1(4) . . ?
O38 W6 O9 157.6(4) . . ?
O38 W6 O32 85.4(4) . . ?
O38 W6 O37 89.3(4) . . ?
O9 W7 O10 87.4(4) . . ?
O9 W7 O32 72.4(4) . . ?
O10 W7 O32 71.8(3) . . ?
O25 W7 O9 156.5(4) . . ?
O25 W7 O10 89.2(4) . . ?
O25 W7 O32 84.5(4) . . ?
O29 W7 O9 100.2(5) . . ?
O29 W7 O10 100.1(5) . . ?
O29 W7 O25 103.3(5) . . ?
O29 W7 O32 168.9(5) . . ?
O29 W7 O36 102.5(5) . . ?
O36 W7 O9 89.6(4) . . ?
O36 W7 O10 157.3(4) . . ?
O36 W7 O25 84.6(4) . . ?
O36 W7 O32 85.9(4) . . ?
O13 W8 O21 86.0(4) . . ?
O13 W8 O23 157.9(4) . . ?
O13 W8 O38 84.2(4) . . ?
O23 W8 O21 72.7(4) . . ?
O31 W8 O13 90.4(4) . . ?
O31 W8 O21 72.9(4) . . ?
O31 W8 O23 89.0(4) . . ?
O31 W8 O38 157.2(4) . . ?
O38 W8 O21 84.7(4) . . ?
O38 W8 O23 87.9(4) . . ?
O40 W8 O13 103.0(5) . . ?
O40 W8 O21 169.2(4) . . ?
O40 W8 O23 98.9(4) . . ?
O40 W8 O31 100.8(5) . . ?
O40 W8 O38 101.9(5) . . ?
O4 W9 O13 104.2(5) . . ?
O4 W9 O19 101.9(4) . . ?
O4 W9 O26 98.4(5) . . ?
O4 W9 O30 168.7(5) . . ?
O4 W9 O39 101.3(5) . . ?
O13 W9 O19 84.9(4) . . ?
O13 W9 O26 157.3(4) . . ?
O13 W9 O30 85.5(4) . . ?
O13 W9 O39 88.4(4) . . ?
O19 W9 O30 84.5(4) . . ?
O26 W9 O19 89.1(4) . . ?
O26 W9 O30 72.1(3) . . ?
O39 W9 O19 156.9(4) . . ?
O39 W9 O26 88.7(4) . . ?
O39 W9 O30 72.9(4) . . ?
O14 W10 O18 100.1(5) . . ?
O14 W10 O26 101.1(5) . . ?
O14 W10 O30 170.1(4) . . ?
O14 W10 O35 102.5(5) . . ?
O14 W10 O36 103.1(5) . . ?
O18 W10 O30 72.1(4) . . ?
O18 W10 O36 156.7(4) . . ?
O26 W10 O18 87.2(4) . . ?
O26 W10 O30 72.7(4) . . ?
O26 W10 O36 88.7(4) . . ?
O35 W10 O18 89.3(4) . . ?
O35 W10 O26 156.4(4) . . ?
O35 W10 O30 84.0(4) . . ?
O35 W10 O36 85.3(4) . . ?
O36 W10 O30 84.8(4) . . ?
O6 W11 O16 88.6(4) . . ?
O6 W11 O21 72.6(4) . . ?
O6 W11 O23 88.4(4) . . ?
O12 W11 O6 157.6(4) . . ?
O12 W11 O16 85.3(4) . . ?
O12 W11 O21 85.4(4) . . ?
O12 W11 O23 89.3(4) . . ?
O16 W11 O21 85.5(4) . . ?
O16 W11 O23 158.1(4) . . ?
O23 W11 O21 73.0(4) . . ?
O27 W11 O6 100.7(4) . . ?
O27 W11 O12 101.7(4) . . ?
O27 W11 O16 103.7(4) . . ?
O27 W11 O21 168.8(4) . . ?
O27 W11 O23 98.1(4) . . ?
O2 W12 O6 100.5(5) . . ?
O2 W12 O20 102.9(5) . . ?
O2 W12 O21 169.5(5) . . ?
O2 W12 O22 102.6(5) . . ?
O2 W12 O31 100.5(5) . . ?
O6 W12 O21 72.2(4) . . ?
O6 W12 O31 88.2(4) . . ?
O20 W12 O6 89.6(4) . . ?
O20 W12 O21 84.9(4) . . ?
O20 W12 O22 85.0(4) . . ?
O20 W12 O31 156.5(4) . . ?
O22 W12 O6 156.9(4) . . ?
O22 W12 O21 85.0(4) . . ?
O22 W12 O31 87.9(4) . . ?
O31 W12 O21 72.1(4) . . ?
O30 Ge1 O21 110.2(4) . . ?
O30 Ge1 O32 109.8(4) . . ?
O30 Ge1 O33 108.7(5) . . ?
O32 Ge1 O21 108.0(4) . . ?
O32 Ge1 O33 110.3(4) . . ?
O33 Ge1 O21 109.8(4) . . ?
O3W La1 O4W 70.0(5) . . ?
O3W La1 O7W 129.1(5) . . ?
O3W La1 O8W 67.2(6) . . ?
O3W La1 O14W 59.7(6) . . ?
O3W La1 O45 136.4(5) . . ?
O4W La1 O14W 75.0(6) . . ?
O5W La1 O3W 131.5(6) . . ?
O5W La1 O4W 81.0(6) . . ?
O5W La1 O7W 99.1(6) . . ?
O5W La1 O8W 136.5(6) . . ?
O5W La1 O14W 76.0(6) . . ?
O5W La1 O45 61.0(5) . . ?
O6W La1 O3W 113.4(6) . . ?
O6W La1 O4W 141.6(5) . . ?
O6W La1 O5W 68.8(6) . . ?
O6W La1 O7W 75.9(6) . . ?
O6W La1 O8W 67.8(6) . . ?
O6W La1 O9W 143.2(6) . . ?
O6W La1 O14W 75.2(7) . . ?
O6W La1 O45 109.7(5) . . ?
O7W La1 O4W 133.7(5) . . ?
O7W La1 O8W 72.1(5) . . ?
O7W La1 O14W 150.5(6) . . ?
O7W La1 O45 67.6(5) . . ?
O8W La1 O4W 136.2(6) . . ?
O8W La1 O14W 91.2(6) . . ?
O8W La1 O45 138.7(5) . . ?
O9W La1 O3W 76.8(6) . . ?
O9W La1 O4W 75.1(5) . . ?
O9W La1 O5W 132.3(6) . . ?
O9W La1 O7W 71.3(6) . . ?
O9W La1 O8W 86.4(6) . . ?
O9W La1 O14W 133.4(7) . . ?
O9W La1 O45 72.6(5) . . ?
O45 La1 O4W 72.6(5) . . ?
O45 La1 O14W 129.1(5) . . ?
N1 Cu1 O1W 97.7(5) . . ?
N1 Cu1 O2W 168.4(5) . . ?
O2W Cu1 O1W 91.3(5) . . ?
O42 Cu1 N1 82.9(5) . . ?
O42 Cu1 O1W 91.1(6) . . ?
O42 Cu1 O2W 89.8(5) . . ?
O43 Cu1 N1 95.9(5) . . ?
O43 Cu1 O1W 94.6(5) . . ?
O43 Cu1 O2W 90.5(5) . . ?
O43 Cu1 O42 174.2(6) . . ?
N2 Cu2 N3 173.8(6) . . ?
N2 Cu2 O44 82.6(5) . . ?
N2 Cu2 O46 94.0(6) . . ?
N3 Cu2 O44 100.7(5) . . ?
N3 Cu2 O46 83.0(6) . . ?
O46 Cu2 O44 175.5(7) . . ?
N4 Cu3 N5 177.5(6) . . ?
N4 Cu3 O49 98.4(6) . . ?
N5 Cu3 O49 83.6(5) . . ?
O47 Cu3 N4 83.1(6) . . ?
O47 Cu3 N5 95.0(6) . . ?
O47 Cu3 O49 178.3(5) . . ?
N6 Cu4 O11W 170.3(7) . . ?
N6 Cu4 O12W 87.9(5) . . ?
O11W Cu4 O12W 83.6(7) . . ?
O50 Cu4 N6 99.9(5) . . ?
O50 Cu4 O11W 85.2(7) . . ?
O50 Cu4 O12W 93.1(6) . . ?
O50 Cu4 O52 173.1(6) . . ?
O52 Cu4 N6 83.1(5) . . ?
O52 Cu4 O11W 92.7(7) . . ?
O52 Cu4 O12W 93.2(7) . . ?
C1 N1 Cu1 129.5(13) . . ?
C1 N1 C5 116.8(16) . . ?
C5 N1 Cu1 113.6(11) . . ?
C7 N2 Cu2 128.6(11) . . ?
C7 N2 C11 118.9(15) . . ?
C11 N2 Cu2 112.5(11) . . ?
C13 N3 Cu2 128.3(12) . . ?
C17 N3 Cu2 113.2(13) . . ?
C17 N3 C13 118.4(16) . . ?
C19 N4 Cu3 126.0(13) . . ?
C23 N4 Cu3 113.5(13) . . ?
C23 N4 C19 120.4(16) . . ?
C29 N5 Cu3 113.1(12) . . ?
C31 N5 Cu3 128.2(13) . . ?
C31 N5 C29 118.6(15) . . ?
C25 N6 Cu4 129.0(12) . . ?
C25 N6 C35 120.6(15) . . ?
C35 N6 Cu4 110.4(11) . . ?
W12 O6 W11 121.4(5) . . ?
W5 O7 W1 120.7(5) . . ?
W7 O9 W6 121.4(5) . . ?
W2 O10 W7 122.0(5) . . ?
W4 O11 W5 121.8(5) . . ?
W11 O12 W2 152.9(6) . . ?
W8 O13 W9 153.7(6) . . ?
W1 O15 W4 121.2(5) . . ?
W4 O16 W11 152.4(5) . . ?
W10 O18 W3 121.3(5) . . ?
W6 O19 W9 152.3(5) . . ?
W12 O20 W5 153.9(5) . . ?
W8 O21 W12 93.5(3) . . ?
W11 O21 W8 94.4(3) . . ?
W11 O21 W12 93.8(3) . . ?
Ge1 O21 W8 122.9(4) . . ?
Ge1 O21 W11 122.7(4) . . ?
Ge1 O21 W12 121.7(5) . . ?
W12 O22 W3 152.7(6) . . ?
W8 O23 W11 119.9(5) . . ?
W2 O24 W4 152.1(5) . . ?
W7 O25 W1 154.8(5) . . ?
W10 O26 W9 121.8(5) . . ?
W5 O28 W3 151.3(7) . . ?
W3 O30 W9 93.4(3) . . ?
W3 O30 W10 94.5(3) . . ?
W10 O30 W9 93.3(3) . . ?
Ge1 O30 W3 122.4(4) . . ?
Ge1 O30 W9 122.1(5) . . ?
Ge1 O30 W10 123.2(4) . . ?
W8 O31 W12 121.5(5) . . ?
W2 O32 W6 94.7(4) . . ?
W2 O32 W7 93.5(3) . . ?
W6 O32 W7 93.6(3) . . ?
Ge1 O32 W2 123.1(4) . . ?
Ge1 O32 W6 122.8(4) . . ?
Ge1 O32 W7 121.4(5) . . ?
W1 O33 W4 94.2(3) . . ?
W1 O33 W5 94.9(4) . . ?
W5 O33 W4 93.9(3) . . ?
Ge1 O33 W1 122.2(4) . . ?
Ge1 O33 W4 121.7(5) . . ?
Ge1 O33 W5 122.5(5) . . ?
W10 O35 W1 153.4(6) . . ?
W7 O36 W10 152.6(5) . . ?
W6 O37 W2 119.4(5) . . ?
W6 O38 W8 152.5(6) . . ?
W9 O39 W3 120.4(5) . . ?
C6 O42 Cu1 116.0(11) . . ?
C12 O43 Cu1 136.3(12) . . ?
C12 O44 Cu2 111.4(11) . . ?
C18 O45 La1 143.7(17) . . ?
C18 O46 Cu2 109.9(14) . . ?
C24 O47 Cu3 116.4(12) . . ?
C30 O49 Cu3 112.6(11) . . ?
C30 O50 Cu4 125.4(11) . . ?
C36 O52 Cu4 114.2(12) . . ?
N1 C1 C2 122(2) . . ?
C3 C2 C1 118(2) . . ?
C2 C3 C4 121.2(18) . . ?
C5 C4 C3 117(2) . . ?
N1 C5 C4 124.9(19) . . ?
N1 C5 C6 112.4(14) . . ?
C4 C5 C6 122.7(18) . . ?
O41 C6 O42 126.6(18) . . ?
O41 C6 C5 118.6(16) . . ?
O42 C6 C5 114.6(15) . . ?
N2 C7 C8 123.4(16) . . ?
C7 C8 C9 119.2(16) . . ?
C10 C9 C8 116.5(16) . . ?
C11 C10 C9 121.1(14) . . ?
N2 C11 C10 120.8(15) . . ?
N2 C11 C12 113.8(15) . . ?
C10 C11 C12 125.3(14) . . ?
O43 C12 C11 114.7(16) . . ?
O44 C12 O43 125.5(17) . . ?
O44 C12 C11 119.8(14) . . ?
C14 C13 N3 118.8(18) . . ?
C15 C14 C13 125(2) . . ?
C14 C15 C16 116(2) . . ?
C17 C16 C15 120(2) . . ?
N3 C17 C16 122(2) . . ?
N3 C17 C18 111.9(18) . . ?
C16 C17 C18 126(2) . . ?
O45 C18 C17 123(2) . . ?
O46 C18 O45 116(2) . . ?
O46 C18 C17 121.3(17) . . ?
C20 C19 N4 122(2) . . ?
C19 C20 C21 118(2) . . ?
C22 C21 C20 119.5(18) . . ?
C23 C22 C21 119(2) . . ?
N4 C23 C22 122(2) . . ?
N4 C23 C24 112.4(15) . . ?
C22 C23 C24 126(2) . . ?
O47 C24 C23 114.2(16) . . ?
O48 C24 O47 127(2) . . ?
O48 C24 C23 119.0(18) . . ?
N6 C25 C32 120.7(19) . . ?
C31 C26 C27 120.8(18) . . ?
C28 C27 C26 118.1(16) . . ?
C27 C28 C29 119.6(18) . . ?
N5 C29 C28 122.1(16) . . ?
N5 C29 C30 111.5(14) . . ?
C28 C29 C30 126.4(17) . . ?
O49 C30 O50 125.0(17) . . ?
O49 C30 C29 119.1(15) . . ?
O50 C30 C29 115.8(15) . . ?
C26 C31 N5 120.8(19) . . ?
C33 C32 C25 117.2(18) . . ?
C34 C33 C32 120.9(17) . . ?
C33 C34 C35 120.2(18) . . ?
N6 C35 C36 114.9(16) . . ?
C34 C35 N6 120.3(17) . . ?
C34 C35 C36 124.6(18) . . ?
O51 C36 O52 124(2) . . ?
O51 C36 C35 120(2) . . ?
O52 C36 C35 116.4(17) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1891065'
loop_
_audit_author_name
_audit_author_address
'Junwei Zhao'
;Henan University
China
;
_audit_update_record             
;
2019-02-11 deposited with the CCDC.	2019-02-14 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT201_2                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......    14 Report 
RESPONSE: Due to the large structure and the existence of a large 
 amount of weight atoms, the intensity data are not very good, 
 leading to the ADP max/min ratio of some water molecules, and it is 
very difficult to refine this large structure, therefore, 
 in the final refinement, the W, Ge, Cu and Ce atoms were refined 
anisotropically, some O atoms and water molecules were
 refined isotropically.
;


_vrf_PLAT220_2                   
;
PROBLEM:  Non-Solvent  Resd 1  O   Ueq(max)/Ueq(min) Range   8.4 Ratio 
RESPONSE: In polyoxometalate compounds, the Ueq of oxygen atoms in
 the POM skeleton is small due to multiple covalent bonds, whereas the 
Ueq of these dissociative water oxygen atoms is biggish without 
the constraint of covalent bonds, which lead to the 
non-solvent O Ueq(max)/Ueq(min) range. 
;


_vrf_PLAT306_2                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O15W Check
RESPONSE: The hydrogen atoms of the water molecules could not be directly 
 located from the difference Fourier maps because of the presence of too many
 heavy atoms in the structure.
;

_vrf_PLAT342_2                   
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.034 Ang.
RESPONSE: The alert derives from shading of reciprocal space
 by the pressure cell, and it is unavoidable in high pressure
 crystal structure determinations.
;


# end Validation Reply Form

_audit_creation_date             2019-02-09
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'Ge O40 W12, C18 H12 Ce0.5 Cu2 N3 Na0.5 O16, C18 H12 Cu2 N3 O8, 8(O)'
_chemical_formula_sum            'C36 H64 Ce0.50 Cu4 Ge N6 Na0.50 O72 W12'
_chemical_formula_weight         4347.44
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   18.7986(7)
_cell_length_b                   14.7548(4)
_cell_length_c                   31.1802(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.0180(10)
_cell_angle_gamma                90.00
_cell_volume                     8615.3(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.62
_exptl_absorpt_coefficient_mu    17.635
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1182 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.6553.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            mazarine
_exptl_crystal_density_diffrn    3.352
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7874
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            74790
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                13833
_reflns_number_total             15104
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         3.003
_refine_diff_density_min         -3.111
_refine_diff_density_rms         0.343
_refine_ls_extinction_coef       0.000099(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         15104
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0540
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0433P)²+559.5684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1378
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Ce1, Na1}
3. Rigid bond restraints
 C32, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Ce1) = Uanis(Na1)
5. Others
 Fixed Sof: Ce1(0.5) Na1(0.5)
 Fixed Uiso: O3W(0.08902) O4W(0.08428) O5W(0.0863) O6W(0.08905) O7W(0.08352)
 O8W(0.08123) O9W(0.09367) O14W(0.15141) O19W(0.14921) O45(0.05872)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C7(H7A), C8(H8A), C9(H9A), C10(H10A),
 C13(H13A), C14(H14A), C15(H15A), C16(H16A), C19(H19A), C20(H20A), C21(H21A),
 C22(H22A), C25(H25A), C26(H26A), C27(H27A), C28(H28A), C31(H31A), C32(H32A),
 C33(H33A), C34(H34A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
W1 W 0.38176(4) -0.58254(5) -0.32405(2) 0.02782(17) Uani 1 d . . . .
W2 W 0.39804(4) -0.56461(5) -0.16401(2) 0.02490(16) Uani 1 d . . . .
W3 W 0.60478(4) -0.39723(5) -0.32498(2) 0.02717(16) Uani 1 d . . . .
W4 W 0.45758(4) -0.72042(4) -0.24767(2) 0.02554(16) Uani 1 d . . . .
W5 W 0.55490(4) -0.64061(5) -0.32476(2) 0.02923(17) Uani 1 d . . . .
W6 W 0.44527(4) -0.34490(4) -0.16425(2) 0.02475(16) Uani 1 d . . . .
W7 W 0.32424(3) -0.42566(5) -0.24017(2) 0.02660(16) Uani 1 d . . . .
W8 W 0.63652(4) -0.40853(5) -0.16493(2) 0.02599(16) Uani 1 d . . . .
W9 W 0.55174(4) -0.25613(4) -0.24980(2) 0.02453(16) Uani 1 d . . . .
W10 W 0.43137(4) -0.33852(5) -0.32591(2) 0.02650(16) Uani 1 d . . . .
W11 W 0.58965(3) -0.62776(4) -0.16315(2) 0.02410(16) Uani 1 d . . . .
W12 W 0.68777(3) -0.55090(5) -0.24020(2) 0.02743(17) Uani 1 d . . . .
Ge1 Ge 0.50533(8) -0.48839(10) -0.24463(5) 0.0175(3) Uani 1 d . . . .
Ce1 Ce 0.10578(13) -1.15639(16) 0.00760(7) 0.0506(5) Uani 0.50 d A 1 . .
Na1 Na 0.10578(13) -1.15639(16) 0.00760(7) 0.0506(5) Uani 0.50 d A 2 . .
Cu1 Cu 0.59422(12) -0.72305(15) -0.04230(7) 0.0341(5) Uani 1 d . . . .
Cu2 Cu 0.34674(14) -0.8876(2) -0.00537(8) 0.0476(7) Uani 1 d A . . .
Cu3 Cu 0.48924(14) -0.99694(17) -0.23768(8) 0.0415(6) Uani 1 d . . . .
Cu4 Cu 0.44065(15) -1.0101(2) -0.40283(9) 0.0564(7) Uani 1 d . . . .
N1 N 0.5798(9) -0.5896(10) -0.0414(5) 0.036(4) Uani 1 d . . . .
N2 N 0.3397(8) -0.8831(11) -0.0688(5) 0.037(4) Uani 1 d . . . .
N3 N 0.3447(9) -0.8862(12) 0.0583(5) 0.041(4) Uani 1 d A . . .
N4 N 0.5784(8) -0.9306(11) -0.2340(6) 0.046(4) Uani 1 d . . . .
N5 N 0.3990(8) -1.0670(11) -0.2411(5) 0.037(4) Uani 1 d . . . .
N6 N 0.5419(9) -1.0400(11) -0.3887(5) 0.039(4) Uani 1 d . . . .
O1W O 0.5769(10) -0.7511(12) 0.0289(5) 0.068(5) Uani 1 d . . . .
O2W O 0.6248(8) -0.8500(9) -0.0512(4) 0.045(3) Uani 1 d . . . .
O3W O 0.0712(12) -1.2181(15) -0.0677(7) 0.089 Uiso 1 d . . . .
O4W O 0.0884(11) -1.0193(14) -0.0496(7) 0.084 Uiso 1 d . . . .
O5W O 0.0477(11) -1.0384(15) 0.0497(7) 0.086 Uiso 1 d . . . .
O6W O 0.0398(12) -1.2249(15) 0.0671(7) 0.089 Uiso 1 d . . . .
O7W O 0.2029(11) -1.2118(14) 0.0643(7) 0.084 Uiso 1 d . . . .
O8W O 0.1093(11) -1.3303(14) 0.0046(7) 0.081 Uiso 1 d . . . .
O9W O 0.2204(12) -1.1626(16) -0.0290(7) 0.094 Uiso 1 d . . . .
O10W O 0.2721(12) -0.7497(16) -0.0068(8) 0.097(7) Uiso 1 d . . . .
O11W O 0.3385(13) -0.9907(17) -0.4258(8) 0.103(7) Uiso 1 d . . . .
O12W O 0.4288(11) -1.1499(15) -0.4432(7) 0.088(6) Uiso 1 d . . . .
O13W O 0.4353(15) -0.857(2) -0.3683(9) 0.125(9) Uiso 1 d . . . .
O14W O -0.0349(18) -1.164(2) -0.0263(11) 0.151 Uiso 1 d . . . .
O15W O 0.9443(13) -0.4319(17) 0.4059(8) 0.107(8) Uiso 1 d . . . .
O16W O 0.7343(13) 0.1639(17) 0.4148(8) 0.108(8) Uiso 1 d . . . .
O17W O -0.1320(15) -1.159(2) 0.0377(9) 0.129(9) Uiso 1 d . . . .
O18W O -0.2032(12) -1.2803(16) -0.0618(8) 0.096(7) Uiso 1 d . . . .
O19W O 0.8086(17) 0.350(2) 0.1608(11) 0.149 Uiso 1 d . . . .
O1 O 0.5954(7) -0.6989(9) -0.3622(4) 0.041(3) Uani 1 d . . . .
O2 O 0.7711(7) -0.5809(9) -0.2520(5) 0.047(4) Uani 1 d . . . .
O3 O 0.4378(7) -0.8295(8) -0.2361(4) 0.033(3) Uani 1 d . . . .
O4 O 0.5720(7) -0.1445(8) -0.2393(4) 0.033(3) Uani 1 d . . . .
O5 O 0.3126(7) -0.6022(10) -0.3615(4) 0.042(3) Uani 1 d . . . .
O6 O 0.6722(6) -0.6347(8) -0.1951(4) 0.028(3) Uani 1 d . . . .
O7 O 0.4593(6) -0.6293(8) -0.3536(4) 0.030(3) Uani 1 d . . . .
O8 O 0.3582(7) -0.6231(9) -0.1258(4) 0.036(3) Uani 1 d . . . .
O9 O 0.3516(6) -0.3394(8) -0.1963(4) 0.030(3) Uani 1 d . . . .
O10 O 0.3144(6) -0.5148(8) -0.1955(4) 0.029(3) Uani 1 d . . . .
O11 O 0.5183(7) -0.7410(8) -0.2931(4) 0.031(3) Uani 1 d . . . .
O12 O 0.4974(6) -0.5886(8) -0.1497(3) 0.026(2) Uani 1 d . . . .
O13 O 0.6160(6) -0.3220(8) -0.2094(4) 0.031(3) Uani 1 d . . . .
O14 O 0.3779(7) -0.2837(9) -0.3645(4) 0.037(3) Uani 1 d . . . .
O15 O 0.3810(6) -0.6941(8) -0.2926(4) 0.031(3) Uani 1 d . . . .
O16 O 0.5382(6) -0.6972(8) -0.2080(3) 0.026(2) Uani 1 d . . . .
O17 O 0.6623(7) -0.3762(9) -0.3628(4) 0.038(3) Uani 1 d . . . .
O18 O 0.5182(7) -0.3504(8) -0.3546(4) 0.033(3) Uani 1 d . . . .
O19 O 0.4806(6) -0.2783(8) -0.2104(4) 0.029(3) Uani 1 d . . . .
O20 O 0.6289(6) -0.6231(8) -0.2796(4) 0.031(3) Uani 1 d . . . .
O21 O 0.5820(5) -0.5126(7) -0.2123(3) 0.018(2) Uani 1 d . . . .
O22 O 0.6641(6) -0.4542(8) -0.2796(4) 0.029(3) Uani 1 d . . . .
O23 O 0.6306(6) -0.5228(8) -0.1345(4) 0.028(3) Uani 1 d . . . .
O24 O 0.4046(6) -0.6544(8) -0.2080(4) 0.029(3) Uani 1 d . . . .
O25 O 0.3364(6) -0.5233(8) -0.2797(4) 0.029(3) Uani 1 d . . . .
O26 O 0.4762(6) -0.2382(7) -0.2944(4) 0.027(3) Uani 1 d . . . .
O27 O 0.6105(6) -0.7065(8) -0.1239(4) 0.036(3) Uani 1 d . . . .
O28 O 0.5704(6) -0.5165(8) -0.3398(4) 0.031(3) Uani 1 d . . . .
O29 O 0.2368(6) -0.3978(9) -0.2512(4) 0.039(3) Uani 1 d . . . .
O30 O 0.5193(5) -0.3969(7) -0.2768(3) 0.021(2) Uani 1 d . . . .
O31 O 0.7099(6) -0.4588(9) -0.1965(4) 0.031(3) Uani 1 d . . . .
O32 O 0.4375(5) -0.4630(7) -0.2121(3) 0.020(2) Uani 1 d . . . .
O33 O 0.4814(6) -0.5816(7) -0.2766(4) 0.023(2) Uani 1 d . . . .
O34 O 0.4369(7) -0.2621(9) -0.1268(4) 0.040(3) Uani 1 d . . . .
O35 O 0.4106(6) -0.4620(8) -0.3393(3) 0.028(3) Uani 1 d . . . .
O36 O 0.3702(6) -0.3535(8) -0.2812(4) 0.028(3) Uani 1 d . . . .
O37 O 0.4112(6) -0.4489(8) -0.1345(4) 0.028(3) Uani 1 d . . . .
O38 O 0.5398(6) -0.3846(8) -0.1506(3) 0.025(2) Uani 1 d . . . .
O39 O 0.6137(6) -0.2838(8) -0.2944(4) 0.027(3) Uani 1 d . . . .
O40 O 0.6864(6) -0.3487(8) -0.1273(4) 0.032(3) Uani 1 d . . . .
O41 O 0.7632(9) -0.5725(12) -0.0089(6) 0.072(5) Uani 1 d . . . .
O42 O 0.6951(8) -0.6888(10) -0.0276(5) 0.053(4) Uani 1 d . . . .
O43 O 0.4974(6) -0.7535(9) -0.0637(4) 0.036(3) Uani 1 d . . . .
O44 O 0.4357(7) -0.8162(10) -0.0114(4) 0.040(3) Uani 1 d . . . .
O45 O 0.1884(9) -1.0188(11) 0.0394(5) 0.059 Uiso 1 d . . . .
O46 O 0.2590(11) -0.9608(19) -0.0031(6) 0.106(9) Uani 1 d . . . .
O47 O 0.5008(8) -0.9936(10) -0.1754(4) 0.047(4) Uani 1 d . . . .
O48 O 0.5704(10) -0.9350(11) -0.1210(5) 0.067(5) Uani 1 d . . . .
O49 O 0.4738(8) -1.0000(10) -0.3004(4) 0.042(3) Uani 1 d . . . .
O50 O 0.3988(7) -1.0633(10) -0.3515(5) 0.043(3) Uani 1 d . . . .
O51 O 0.5797(11) -0.8872(15) -0.4696(6) 0.088(7) Uani 1 d . . . .
O52 O 0.4780(9) -0.9426(13) -0.4503(5) 0.066(5) Uani 1 d . . . .
C1 C 0.5197(12) -0.5417(15) -0.0508(6) 0.047(5) Uani 1 d . . . .
H1A H 0.4770 -0.5720 -0.0583 0.056 Uiso 1 calc . . R .
C2 C 0.5202(15) -0.4498(15) -0.0496(6) 0.056(6) Uani 1 d . . . .
H2A H 0.4784 -0.4180 -0.0577 0.067 Uiso 1 calc . . R .
C3 C 0.5798(17) -0.4047(17) -0.0371(8) 0.068(8) Uani 1 d . . . .
H3A H 0.5794 -0.3418 -0.0355 0.081 Uiso 1 calc . . R .
C4 C 0.6410(16) -0.4516(16) -0.0267(8) 0.062(7) Uani 1 d . . . .
H4A H 0.6830 -0.4210 -0.0178 0.074 Uiso 1 calc . . R .
C5 C 0.6403(11) -0.5466(13) -0.0295(7) 0.041(5) Uani 1 d . . . .
C6 C 0.7047(11) -0.6055(16) -0.0207(7) 0.048(5) Uani 1 d . . . .
C7 C 0.2913(10) -0.9189(15) -0.0960(6) 0.043(5) Uani 1 d . . . .
H7A H 0.2545 -0.9510 -0.0849 0.052 Uiso 1 calc . . R .
C8 C 0.2908(12) -0.9128(16) -0.1395(7) 0.053(6) Uani 1 d . . . .
H8A H 0.2546 -0.9392 -0.1576 0.064 Uiso 1 calc . . R .
C9 C 0.3480(11) -0.8639(16) -0.1566(7) 0.047(5) Uani 1 d . . . .
H9A H 0.3504 -0.8572 -0.1861 0.057 Uiso 1 calc . . R .
C10 C 0.3999(9) -0.8270(13) -0.1270(6) 0.032(4) Uani 1 d . . . .
H10A H 0.4391 -0.7973 -0.1366 0.039 Uiso 1 calc . . R .
C11 C 0.3929(10) -0.8347(12) -0.0837(6) 0.031(4) Uani 1 d . . . .
C12 C 0.4452(10) -0.7987(12) -0.0492(7) 0.036(4) Uani 1 d . . . .
C13 C 0.3906(13) -0.8483(16) 0.0871(7) 0.051(5) Uani 1 d . . . .
H13A H 0.4320 -0.8219 0.0786 0.061 Uiso 1 calc . . R .
C14 C 0.3772(17) -0.8477(14) 0.1302(7) 0.065(8) Uani 1 d . . . .
H14A H 0.4089 -0.8170 0.1497 0.078 Uiso 1 calc . . R .
C15 C 0.322(2) -0.888(2) 0.1446(10) 0.080(9) Uani 1 d . . . .
H15A H 0.3163 -0.8913 0.1739 0.096 Uiso 1 calc . . R .
C16 C 0.2714(15) -0.928(2) 0.1122(12) 0.088(11) Uani 1 d A . . .
H16A H 0.2292 -0.9548 0.1193 0.106 Uiso 1 calc . . R .
C17 C 0.2888(14) -0.924(2) 0.0711(8) 0.068(7) Uani 1 d . . . .
C18 C 0.2399(16) -0.966(3) 0.0340(10) 0.097(12) Uani 1 d A . . .
C19 C 0.6140(10) -0.8992(12) -0.2666(8) 0.045(5) Uani 1 d . . . .
H19A H 0.5972 -0.9115 -0.2949 0.053 Uiso 1 calc . . R .
C20 C 0.6756(12) -0.8483(13) -0.2578(9) 0.056(7) Uani 1 d . . . .
H20A H 0.6998 -0.8254 -0.2802 0.067 Uiso 1 calc . . R .
C21 C 0.7017(13) -0.8314(15) -0.2142(10) 0.065(7) Uani 1 d . . . U
H21A H 0.7434 -0.7986 -0.2076 0.078 Uiso 1 calc . . R .
C22 C 0.6636(12) -0.8648(15) -0.1824(9) 0.057(6) Uani 1 d . . . U
H22A H 0.6805 -0.8551 -0.1539 0.069 Uiso 1 calc . . R .
C23 C 0.6046(9) -0.9096(12) -0.1907(8) 0.041(5) Uani 1 d . . . .
C24 C 0.5553(11) -0.9485(14) -0.1600(7) 0.042(5) Uani 1 d . . . .
C25 C 0.5741(12) -1.0955(16) -0.3591(8) 0.053(6) Uani 1 d . . . .
H25A H 0.5446 -1.1269 -0.3418 0.064 Uiso 1 calc . . R .
C26 C 0.3062(12) -1.1491(14) -0.2152(7) 0.046(5) Uani 1 d . . . .
H26A H 0.2842 -1.1727 -0.1921 0.055 Uiso 1 calc . . R .
C27 C 0.2781(11) -1.1662(15) -0.2575(9) 0.058(7) Uani 1 d . . . .
H27A H 0.2356 -1.1982 -0.2628 0.070 Uiso 1 calc . . R .
C28 C 0.3133(11) -1.1357(14) -0.2903(7) 0.044(5) Uani 1 d . . . .
H28A H 0.2967 -1.1485 -0.3186 0.053 Uiso 1 calc . . R .
C29 C 0.3751(9) -1.0849(12) -0.2813(6) 0.031(4) Uani 1 d . . . .
C30 C 0.4187(10) -1.0456(14) -0.3148(7) 0.041(5) Uani 1 d . . . .
C31 C 0.3649(12) -1.0984(14) -0.2084(8) 0.049(6) Uani 1 d . . . .
H31A H 0.3824 -1.0847 -0.1803 0.059 Uiso 1 calc . . R .
C32 C 0.6431(15) -1.1104(16) -0.3518(7) 0.063(7) Uani 1 d . . . U
H32A H 0.6616 -1.1499 -0.3304 0.076 Uiso 1 calc . . R .
C33 C 0.6865(13) -1.0640(17) -0.3778(9) 0.065(7) Uani 1 d . . . U
H33A H 0.7357 -1.0723 -0.3744 0.078 Uiso 1 calc . . R .
C34 C 0.6568(11) -1.0053(15) -0.4089(7) 0.048(5) Uani 1 d . . . .
H34A H 0.6857 -0.9745 -0.4267 0.057 Uiso 1 calc . . R .
C35 C 0.5870(12) -0.9933(14) -0.4130(7) 0.046(5) Uani 1 d . . . .
C36 C 0.5473(16) -0.9361(17) -0.4466(7) 0.062(7) Uani 1 d . . . .
O20W O 0.4270(10) -1.0234(13) -0.0077(6) 0.072(5) Uiso 1 d . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O5 1.695(12) . ?
W1 O7 1.920(12) . ?
W1 O15 1.917(12) . ?
W1 O25 1.900(12) . ?
W1 O33 2.284(11) . ?
W1 O35 1.931(12) . ?
W2 O8 1.698(12) . ?
W2 O10 1.924(12) . ?
W2 O12 1.916(11) . ?
W2 O24 1.919(11) . ?
W2 O32 2.289(10) . ?
W2 O37 1.945(12) . ?
W3 O17 1.697(12) . ?
W3 O18 1.927(12) . ?
W3 O22 1.918(11) . ?
W3 O28 1.918(12) . ?
W3 O30 2.294(10) . ?
W3 O39 1.925(12) . ?
W4 O3 1.698(12) . ?
W4 O11 1.921(12) . ?
W4 O15 1.956(12) . ?
W4 O16 1.902(11) . ?
W4 O24 1.920(11) . ?
W4 O33 2.298(11) . ?
W5 O1 1.683(12) . ?
W5 O7 1.945(11) . ?
W5 O11 1.939(12) . ?
W5 O20 1.909(12) . ?
W5 O28 1.918(12) . ?
W5 O33 2.299(11) . ?
W6 O9 1.948(12) . ?
W6 O19 1.909(12) . ?
W6 O32 2.290(11) . ?
W6 O34 1.706(12) . ?
W6 O37 1.931(11) . ?
W6 O38 1.884(11) . ?
W7 O9 1.906(12) . ?
W7 O10 1.937(12) . ?
W7 O25 1.922(12) . ?
W7 O29 1.701(11) . ?
W7 O32 2.298(10) . ?
W7 O36 1.927(12) . ?
W8 O13 1.900(12) . ?
W8 O21 2.308(10) . ?
W8 O23 1.943(12) . ?
W8 O31 1.913(12) . ?
W8 O38 1.943(11) . ?
W8 O40 1.686(12) . ?
W9 O4 1.715(11) . ?
W9 O13 1.929(12) . ?
W9 O19 1.922(12) . ?
W9 O26 1.917(12) . ?
W9 O30 2.304(11) . ?
W9 O39 1.935(12) . ?
W10 O14 1.703(12) . ?
W10 O18 1.937(12) . ?
W10 O26 1.929(12) . ?
W10 O30 2.320(10) . ?
W10 O35 1.903(12) . ?
W10 O36 1.896(12) . ?
W11 O6 1.918(11) . ?
W11 O12 1.908(11) . ?
W11 O16 1.925(11) . ?
W11 O21 2.285(10) . ?
W11 O23 1.916(12) . ?
W11 O27 1.709(12) . ?
W12 O2 1.699(13) . ?
W12 O6 1.915(11) . ?
W12 O20 1.905(12) . ?
W12 O21 2.310(10) . ?
W12 O22 1.910(12) . ?
W12 O31 1.944(12) . ?
Ge1 O21 1.722(9) . ?
Ge1 O30 1.715(10) . ?
Ge1 O32 1.738(10) . ?
Ge1 O33 1.734(10) . ?
Ce1 O3W 2.55(2) . ?
Ce1 O4W 2.70(2) . ?
Ce1 O5W 2.49(2) . ?
Ce1 O6W 2.53(2) . ?
Ce1 O7W 2.56(2) . ?
Ce1 O8W 2.57(2) . ?
Ce1 O9W 2.53(2) . ?
Ce1 O14W 2.76(3) . ?
Ce1 O45 2.693(17) . ?
Cu1 N1 1.988(16) . ?
Cu1 O1W 2.309(17) . ?
Cu1 O2W 1.985(14) . ?
Cu1 O42 1.978(14) . ?
Cu1 O43 1.936(12) . ?
Cu2 N2 1.972(16) . ?
Cu2 N3 1.989(17) . ?
Cu2 O44 2.000(13) . ?
Cu2 O46 1.977(16) . ?
Cu3 N4 1.935(16) . ?
Cu3 N5 1.981(15) . ?
Cu3 O47 1.935(14) . ?
Cu3 O49 1.951(12) . ?
Cu4 N6 1.966(17) . ?
Cu4 O11W 2.01(2) . ?
Cu4 O12W 2.42(2) . ?
Cu4 O50 2.004(15) . ?
Cu4 O52 1.963(16) . ?
N1 C1 1.34(3) . ?
N1 C5 1.33(2) . ?
N2 C7 1.30(2) . ?
N2 C11 1.35(2) . ?
N3 C13 1.31(3) . ?
N3 C17 1.29(3) . ?
N4 C19 1.35(3) . ?
N4 C23 1.43(3) . ?
N5 C29 1.32(2) . ?
N5 C31 1.33(2) . ?
N6 C25 1.34(3) . ?
N6 C35 1.37(2) . ?
O41 C6 1.23(2) . ?
O42 C6 1.26(3) . ?
O43 C12 1.30(2) . ?
O44 C12 1.23(2) . ?
O45 C18 1.26(3) . ?
O46 C18 1.25(3) . ?
O47 C24 1.28(2) . ?
O48 C24 1.24(3) . ?
O49 C30 1.28(2) . ?
O50 C30 1.20(2) . ?
O51 C36 1.22(3) . ?
O52 C36 1.30(3) . ?
C1 C2 1.36(3) . ?
C2 C3 1.33(4) . ?
C3 C4 1.36(4) . ?
C4 C5 1.41(3) . ?
C5 C6 1.49(3) . ?
C7 C8 1.36(3) . ?
C8 C9 1.43(3) . ?
C9 C10 1.39(3) . ?
C10 C11 1.37(2) . ?
C11 C12 1.49(3) . ?
C13 C14 1.39(3) . ?
C14 C15 1.30(4) . ?
C15 C16 1.46(5) . ?
C16 C17 1.35(4) . ?
C17 C18 1.54(4) . ?
C19 C20 1.39(3) . ?
C20 C21 1.43(4) . ?
C21 C22 1.36(4) . ?
C22 C23 1.30(3) . ?
C23 C24 1.50(3) . ?
C25 C32 1.32(3) . ?
C26 C27 1.40(3) . ?
C26 C31 1.33(3) . ?
C27 C28 1.34(3) . ?
C28 C29 1.39(3) . ?
C29 C30 1.50(3) . ?
C32 C33 1.38(4) . ?
C33 C34 1.38(3) . ?
C34 C35 1.32(3) . ?
C35 C36 1.50(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 W1 O7 100.2(6) . . ?
O5 W1 O15 99.6(6) . . ?
O5 W1 O25 102.4(6) . . ?
O5 W1 O33 169.7(5) . . ?
O5 W1 O35 101.7(6) . . ?
O7 W1 O33 72.5(4) . . ?
O7 W1 O35 88.3(5) . . ?
O15 W1 O7 88.7(5) . . ?
O15 W1 O33 73.5(4) . . ?
O15 W1 O35 158.7(5) . . ?
O25 W1 O7 157.3(5) . . ?
O25 W1 O15 89.9(5) . . ?
O25 W1 O33 85.4(4) . . ?
O25 W1 O35 84.8(5) . . ?
O35 W1 O33 85.5(4) . . ?
O8 W2 O10 99.3(6) . . ?
O8 W2 O12 102.9(5) . . ?
O8 W2 O24 102.2(6) . . ?
O8 W2 O32 168.8(5) . . ?
O8 W2 O37 99.2(6) . . ?
O10 W2 O32 73.3(4) . . ?
O10 W2 O37 88.3(5) . . ?
O12 W2 O10 157.8(5) . . ?
O12 W2 O24 85.2(5) . . ?
O12 W2 O32 84.7(4) . . ?
O12 W2 O37 88.4(5) . . ?
O24 W2 O10 90.0(5) . . ?
O24 W2 O32 86.5(4) . . ?
O24 W2 O37 158.6(5) . . ?
O37 W2 O32 72.5(4) . . ?
O17 W3 O18 99.4(6) . . ?
O17 W3 O22 103.2(6) . . ?
O17 W3 O28 102.8(6) . . ?
O17 W3 O30 168.6(5) . . ?
O17 W3 O39 98.7(6) . . ?
O18 W3 O30 72.7(4) . . ?
O22 W3 O18 157.3(5) . . ?
O22 W3 O28 86.4(5) . . ?
O22 W3 O30 85.0(4) . . ?
O22 W3 O39 89.7(5) . . ?
O28 W3 O18 87.8(5) . . ?
O28 W3 O30 85.4(4) . . ?
O28 W3 O39 158.4(5) . . ?
O39 W3 O18 87.6(5) . . ?
O39 W3 O30 73.2(4) . . ?
O3 W4 O11 99.4(5) . . ?
O3 W4 O15 100.3(6) . . ?
O3 W4 O16 102.1(6) . . ?
O3 W4 O24 102.0(5) . . ?
O3 W4 O33 169.2(5) . . ?
O11 W4 O15 87.2(5) . . ?
O11 W4 O33 72.7(4) . . ?
O15 W4 O33 72.5(4) . . ?
O16 W4 O11 91.0(5) . . ?
O16 W4 O15 157.5(5) . . ?
O16 W4 O24 85.3(5) . . ?
O16 W4 O33 85.6(4) . . ?
O24 W4 O11 158.6(5) . . ?
O24 W4 O15 88.2(5) . . ?
O24 W4 O33 86.0(4) . . ?
O1 W5 O7 100.3(6) . . ?
O1 W5 O11 99.4(6) . . ?
O1 W5 O20 103.6(6) . . ?
O1 W5 O28 103.3(6) . . ?
O1 W5 O33 168.5(5) . . ?
O7 W5 O33 71.7(4) . . ?
O11 W5 O7 86.9(5) . . ?
O11 W5 O33 72.4(4) . . ?
O20 W5 O7 156.1(5) . . ?
O20 W5 O11 89.8(5) . . ?
O20 W5 O28 86.3(5) . . ?
O20 W5 O33 84.7(4) . . ?
O28 W5 O7 87.6(5) . . ?
O28 W5 O11 157.2(5) . . ?
O28 W5 O33 84.9(4) . . ?
O9 W6 O32 72.2(4) . . ?
O19 W6 O9 87.1(5) . . ?
O19 W6 O32 84.7(4) . . ?
O19 W6 O37 157.3(5) . . ?
O34 W6 O9 100.8(6) . . ?
O34 W6 O19 101.9(6) . . ?
O34 W6 O32 170.4(5) . . ?
O34 W6 O37 100.7(6) . . ?
O34 W6 O38 102.1(6) . . ?
O37 W6 O9 87.5(5) . . ?
O37 W6 O32 72.7(4) . . ?
O38 W6 O9 157.1(5) . . ?
O38 W6 O19 87.0(5) . . ?
O38 W6 O32 85.2(4) . . ?
O38 W6 O37 89.4(5) . . ?
O9 W7 O10 88.5(5) . . ?
O9 W7 O25 157.0(5) . . ?
O9 W7 O32 72.7(4) . . ?
O9 W7 O36 89.9(5) . . ?
O10 W7 O32 72.9(4) . . ?
O25 W7 O10 88.7(5) . . ?
O25 W7 O32 84.6(4) . . ?
O25 W7 O36 84.4(5) . . ?
O29 W7 O9 100.3(5) . . ?
O29 W7 O10 99.1(6) . . ?
O29 W7 O25 102.7(5) . . ?
O29 W7 O32 169.3(5) . . ?
O29 W7 O36 102.3(6) . . ?
O36 W7 O10 158.4(5) . . ?
O36 W7 O32 86.1(4) . . ?
O13 W8 O21 85.9(4) . . ?
O13 W8 O23 157.4(5) . . ?
O13 W8 O31 89.7(5) . . ?
O13 W8 O38 84.9(5) . . ?
O23 W8 O21 72.2(4) . . ?
O31 W8 O21 73.3(4) . . ?
O31 W8 O23 89.4(5) . . ?
O31 W8 O38 157.0(5) . . ?
O38 W8 O21 84.0(4) . . ?
O38 W8 O23 87.1(5) . . ?
O40 W8 O13 102.8(5) . . ?
O40 W8 O21 169.3(5) . . ?
O40 W8 O23 99.6(5) . . ?
O40 W8 O31 100.3(6) . . ?
O40 W8 O38 102.6(5) . . ?
O4 W9 O13 104.1(5) . . ?
O4 W9 O19 101.4(5) . . ?
O4 W9 O26 98.3(5) . . ?
O4 W9 O30 169.4(5) . . ?
O4 W9 O39 101.7(5) . . ?
O13 W9 O30 85.1(4) . . ?
O13 W9 O39 88.9(5) . . ?
O19 W9 O13 85.9(5) . . ?
O19 W9 O30 84.4(4) . . ?
O19 W9 O39 157.0(5) . . ?
O26 W9 O13 157.6(5) . . ?
O26 W9 O19 88.5(5) . . ?
O26 W9 O30 72.8(4) . . ?
O26 W9 O39 87.8(5) . . ?
O39 W9 O30 72.8(4) . . ?
O14 W10 O18 100.7(6) . . ?
O14 W10 O26 101.5(6) . . ?
O14 W10 O30 170.3(5) . . ?
O14 W10 O35 101.7(6) . . ?
O14 W10 O36 102.5(6) . . ?
O18 W10 O30 71.9(4) . . ?
O26 W10 O18 87.5(5) . . ?
O26 W10 O30 72.2(4) . . ?
O35 W10 O18 88.7(5) . . ?
O35 W10 O26 156.8(5) . . ?
O35 W10 O30 84.8(4) . . ?
O36 W10 O18 156.8(5) . . ?
O36 W10 O26 88.9(5) . . ?
O36 W10 O30 85.1(4) . . ?
O36 W10 O35 85.6(5) . . ?
O6 W11 O16 88.4(5) . . ?
O6 W11 O21 72.4(4) . . ?
O12 W11 O6 157.2(5) . . ?
O12 W11 O16 84.9(5) . . ?
O12 W11 O21 85.2(4) . . ?
O12 W11 O23 89.3(5) . . ?
O16 W11 O21 84.9(4) . . ?
O23 W11 O6 88.6(5) . . ?
O23 W11 O16 157.7(5) . . ?
O23 W11 O21 73.2(4) . . ?
O27 W11 O6 101.0(5) . . ?
O27 W11 O12 101.8(5) . . ?
O27 W11 O16 103.2(6) . . ?
O27 W11 O21 169.7(5) . . ?
O27 W11 O23 99.1(6) . . ?
O2 W12 O6 101.2(6) . . ?
O2 W12 O20 102.0(6) . . ?
O2 W12 O21 170.5(6) . . ?
O2 W12 O22 102.9(6) . . ?
O2 W12 O31 100.9(6) . . ?
O6 W12 O21 71.9(4) . . ?
O6 W12 O31 88.5(5) . . ?
O20 W12 O6 89.7(5) . . ?
O20 W12 O21 84.8(4) . . ?
O20 W12 O22 85.1(5) . . ?
O20 W12 O31 156.9(5) . . ?
O22 W12 O6 155.9(5) . . ?
O22 W12 O21 84.2(4) . . ?
O22 W12 O31 87.3(5) . . ?
O31 W12 O21 72.8(4) . . ?
O21 Ge1 O32 108.7(5) . . ?
O21 Ge1 O33 109.5(5) . . ?
O30 Ge1 O21 110.0(5) . . ?
O30 Ge1 O32 109.3(5) . . ?
O30 Ge1 O33 109.5(5) . . ?
O33 Ge1 O32 109.9(5) . . ?
O3W Ce1 O4W 69.7(7) . . ?
O3W Ce1 O7W 129.1(7) . . ?
O3W Ce1 O8W 67.4(7) . . ?
O3W Ce1 O14W 58.3(9) . . ?
O3W Ce1 O45 134.5(6) . . ?
O4W Ce1 O14W 73.8(8) . . ?
O5W Ce1 O3W 130.4(7) . . ?
O5W Ce1 O4W 78.0(7) . . ?
O5W Ce1 O6W 68.1(7) . . ?
O5W Ce1 O7W 100.2(7) . . ?
O5W Ce1 O8W 137.0(7) . . ?
O5W Ce1 O9W 134.0(7) . . ?
O5W Ce1 O14W 77.4(9) . . ?
O5W Ce1 O45 62.9(6) . . ?
O6W Ce1 O3W 115.5(7) . . ?
O6W Ce1 O4W 138.2(7) . . ?
O6W Ce1 O7W 74.4(7) . . ?
O6W Ce1 O8W 69.1(7) . . ?
O6W Ce1 O14W 75.6(9) . . ?
O6W Ce1 O45 109.6(6) . . ?
O7W Ce1 O4W 137.2(7) . . ?
O7W Ce1 O8W 71.8(7) . . ?
O7W Ce1 O14W 148.4(9) . . ?
O7W Ce1 O45 68.5(6) . . ?
O8W Ce1 O4W 136.7(7) . . ?
O8W Ce1 O14W 88.4(8) . . ?
O8W Ce1 O45 138.6(6) . . ?
O9W Ce1 O3W 74.3(7) . . ?
O9W Ce1 O4W 77.7(7) . . ?
O9W Ce1 O6W 143.9(7) . . ?
O9W Ce1 O7W 73.5(7) . . ?
O9W Ce1 O8W 85.5(7) . . ?
O9W Ce1 O14W 130.6(9) . . ?
O9W Ce1 O45 72.9(6) . . ?
O45 Ce1 O4W 73.2(6) . . ?
O45 Ce1 O14W 132.3(8) . . ?
N1 Cu1 O1W 97.6(6) . . ?
O2W Cu1 N1 167.9(7) . . ?
O2W Cu1 O1W 91.8(6) . . ?
O42 Cu1 N1 82.7(7) . . ?
O42 Cu1 O1W 92.0(7) . . ?
O42 Cu1 O2W 89.4(6) . . ?
O43 Cu1 N1 96.3(6) . . ?
O43 Cu1 O1W 94.7(6) . . ?
O43 Cu1 O2W 90.5(6) . . ?
O43 Cu1 O42 173.2(6) . . ?
N2 Cu2 N3 174.4(7) . . ?
N2 Cu2 O44 82.6(6) . . ?
N2 Cu2 O46 94.1(7) . . ?
N3 Cu2 O44 100.2(6) . . ?
O46 Cu2 N3 83.2(7) . . ?
O46 Cu2 O44 176.5(7) . . ?
N4 Cu3 N5 178.8(7) . . ?
N4 Cu3 O49 97.1(7) . . ?
O47 Cu3 N4 84.7(8) . . ?
O47 Cu3 N5 95.0(7) . . ?
O47 Cu3 O49 177.9(6) . . ?
O49 Cu3 N5 83.3(6) . . ?
N6 Cu4 O11W 171.0(9) . . ?
N6 Cu4 O12W 88.2(7) . . ?
N6 Cu4 O50 100.0(6) . . ?
O11W Cu4 O12W 83.9(9) . . ?
O50 Cu4 O11W 84.9(8) . . ?
O50 Cu4 O12W 93.3(7) . . ?
O52 Cu4 N6 83.1(7) . . ?
O52 Cu4 O11W 93.0(9) . . ?
O52 Cu4 O12W 93.7(8) . . ?
O52 Cu4 O50 172.5(7) . . ?
C1 N1 Cu1 129.1(15) . . ?
C5 N1 Cu1 111.2(14) . . ?
C5 N1 C1 119.6(18) . . ?
C7 N2 Cu2 128.5(13) . . ?
C7 N2 C11 119.2(17) . . ?
C11 N2 Cu2 112.2(12) . . ?
C13 N3 Cu2 128.1(15) . . ?
C17 N3 Cu2 113.1(16) . . ?
C17 N3 C13 119(2) . . ?
C19 N4 Cu3 127.9(15) . . ?
C19 N4 C23 119.0(17) . . ?
C23 N4 Cu3 113.0(14) . . ?
C29 N5 Cu3 111.9(13) . . ?
C29 N5 C31 120.7(18) . . ?
C31 N5 Cu3 127.4(15) . . ?
C25 N6 Cu4 131.4(15) . . ?
C25 N6 C35 115.1(19) . . ?
C35 N6 Cu4 113.4(14) . . ?
W12 O6 W11 122.0(6) . . ?
W1 O7 W5 121.2(6) . . ?
W7 O9 W6 121.0(6) . . ?
W2 O10 W7 120.1(6) . . ?
W4 O11 W5 121.0(6) . . ?
W11 O12 W2 153.1(6) . . ?
W8 O13 W9 152.9(7) . . ?
W1 O15 W4 120.0(6) . . ?
W4 O16 W11 152.9(6) . . ?
W3 O18 W10 121.5(6) . . ?
W6 O19 W9 151.3(6) . . ?
W12 O20 W5 153.6(7) . . ?
W8 O21 W12 93.1(3) . . ?
W11 O21 W8 93.8(4) . . ?
W11 O21 W12 93.7(4) . . ?
Ge1 O21 W8 122.6(5) . . ?
Ge1 O21 W11 123.2(5) . . ?
Ge1 O21 W12 122.3(5) . . ?
W12 O22 W3 152.9(7) . . ?
W11 O23 W8 120.7(6) . . ?
W2 O24 W4 151.6(7) . . ?
W1 O25 W7 153.9(7) . . ?
W9 O26 W10 121.8(5) . . ?
W3 O28 W5 150.7(7) . . ?
W3 O30 W9 93.6(4) . . ?
W3 O30 W10 93.9(4) . . ?
W9 O30 W10 93.2(4) . . ?
Ge1 O30 W3 122.3(5) . . ?
Ge1 O30 W9 123.0(6) . . ?
Ge1 O30 W10 122.8(5) . . ?
W8 O31 W12 120.8(6) . . ?
W2 O32 W6 94.5(4) . . ?
W2 O32 W7 93.6(4) . . ?
W6 O32 W7 94.0(4) . . ?
Ge1 O32 W2 122.5(5) . . ?
Ge1 O32 W6 122.4(5) . . ?
Ge1 O32 W7 122.1(5) . . ?
W1 O33 W4 94.1(4) . . ?
W1 O33 W5 94.6(4) . . ?
W4 O33 W5 93.9(4) . . ?
Ge1 O33 W1 122.3(5) . . ?
Ge1 O33 W4 122.1(6) . . ?
Ge1 O33 W5 122.4(6) . . ?
W10 O35 W1 152.2(6) . . ?
W10 O36 W7 152.7(7) . . ?
W6 O37 W2 120.3(6) . . ?
W6 O38 W8 152.6(6) . . ?
W3 O39 W9 120.5(5) . . ?
C6 O42 Cu1 114.1(14) . . ?
C12 O43 Cu1 135.6(13) . . ?
C12 O44 Cu2 113.1(11) . . ?
C18 O45 Ce1 147(2) . . ?
C18 O46 Cu2 112.3(17) . . ?
C24 O47 Cu3 113.9(14) . . ?
C30 O49 Cu3 114.2(12) . . ?
C30 O50 Cu4 124.3(13) . . ?
C36 O52 Cu4 113.1(14) . . ?
N1 C1 C2 121(2) . . ?
C3 C2 C1 121(2) . . ?
C2 C3 C4 119(2) . . ?
C3 C4 C5 119(3) . . ?
N1 C5 C4 120(2) . . ?
N1 C5 C6 115.7(17) . . ?
C4 C5 C6 124(2) . . ?
O41 C6 O42 123(2) . . ?
O41 C6 C5 121(2) . . ?
O42 C6 C5 115.9(17) . . ?
N2 C7 C8 124.6(18) . . ?
C7 C8 C9 117.6(19) . . ?
C10 C9 C8 117.1(19) . . ?
C11 C10 C9 119.8(18) . . ?
N2 C11 C10 121.5(17) . . ?
N2 C11 C12 113.7(16) . . ?
C10 C11 C12 124.6(17) . . ?
O43 C12 C11 113.7(17) . . ?
O44 C12 O43 128.0(18) . . ?
O44 C12 C11 118.3(16) . . ?
N3 C13 C14 120(2) . . ?
C15 C14 C13 123(3) . . ?
C14 C15 C16 116(2) . . ?
C17 C16 C15 116(3) . . ?
N3 C17 C16 126(3) . . ?
N3 C17 C18 113(2) . . ?
C16 C17 C18 121(3) . . ?
O45 C18 C17 124(2) . . ?
O46 C18 O45 117(3) . . ?
O46 C18 C17 118(2) . . ?
N4 C19 C20 120(2) . . ?
C19 C20 C21 120(2) . . ?
C22 C21 C20 118(2) . . ?
C23 C22 C21 122(3) . . ?
N4 C23 C24 109.7(16) . . ?
C22 C23 N4 121(2) . . ?
C22 C23 C24 129(2) . . ?
O47 C24 C23 118.6(19) . . ?
O48 C24 O47 124(2) . . ?
O48 C24 C23 117(2) . . ?
C32 C25 N6 127(2) . . ?
C31 C26 C27 119(2) . . ?
C28 C27 C26 119(2) . . ?
C27 C28 C29 119(2) . . ?
N5 C29 C28 120.5(18) . . ?
N5 C29 C30 115.0(17) . . ?
C28 C29 C30 124.5(17) . . ?
O49 C30 C29 115.5(18) . . ?
O50 C30 O49 128.6(18) . . ?
O50 C30 C29 115.8(18) . . ?
N5 C31 C26 121(2) . . ?
C25 C32 C33 116(2) . . ?
C32 C33 C34 120(2) . . ?
C35 C34 C33 119(2) . . ?
N6 C35 C36 112(2) . . ?
C34 C35 N6 123(2) . . ?
C34 C35 C36 125(2) . . ?
O51 C36 O52 123(2) . . ?
O51 C36 C35 120(3) . . ?
O52 C36 C35 117.1(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
