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

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

data_shelxl
_audit_block_doi                 10.5517/cc11m0b0
_database_code_depnum_ccdc_archive 'CCDC 971581'
_audit_update_record             
;
2014-08-23 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'H2 Nb12 O40 Sb2 Si, 4(C4 H18 Cu N4 O), 22(H2 O)'
_chemical_formula_sum            'C16 H118 Cu4 N16 Nb12 O66 Sb2 Si'
_chemical_formula_weight         3231.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   25.6450(5)
_cell_length_b                   25.6450(5)
_cell_length_c                   16.2100(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10660.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6312
_exptl_absorpt_coefficient_mu    2.617
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35081
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         28.37
_reflns_number_total             6678
_reflns_number_gt                4008
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0972P)²+16.4811P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6678
_refine_ls_number_parameters     287
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1889
_refine_ls_wR_factor_gt          0.1581
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.0000 0.2500 0.1250 0.0163(9) Uani 1 4 d S . .
Cu1 Cu 0.08465(5) 0.97883(5) 0.17086(8) 0.0371(3) Uani 1 1 d . . .
Nb1 Nb 0.13674(3) 0.20957(3) 0.13052(5) 0.0212(2) Uani 1 1 d . . .
Nb2 Nb 0.05513(3) 0.16154(3) 0.27550(5) 0.0215(2) Uani 1 1 d . . .
Nb3 Nb 0.09396(3) 0.29452(3) 0.27651(5) 0.0218(2) Uani 1 1 d . . .
Sb1 Sb 0.0000 0.2500 0.39416(5) 0.0262(2) Uani 1 2 d S . .
C1 C 0.0205(7) 0.9623(6) 0.3103(10) 0.087(5) Uani 1 1 d U . .
H1A H 0.0404 0.9627 0.3612 0.105 Uiso 1 1 calc R . .
H1B H -0.0158 0.9676 0.3248 0.105 Uiso 1 1 calc R . .
C2 C 0.0253(7) 0.9132(7) 0.2754(11) 0.097(5) Uani 1 1 d U . .
H2A H -0.0074 0.9043 0.2488 0.117 Uiso 1 1 calc R . .
H2B H 0.0311 0.8881 0.3191 0.117 Uiso 1 1 calc R . .
C3 C 0.1454(6) 0.9952(5) 0.0287(8) 0.066(4) Uani 1 1 d . . .
H3A H 0.1177 0.9984 -0.0116 0.079 Uiso 1 1 calc R . .
H3B H 0.1776 0.9884 -0.0007 0.079 Uiso 1 1 calc R . .
C4 C 0.1502(5) 1.0437(5) 0.0739(10) 0.066(4) Uani 1 1 d . . .
H4A H 0.1503 1.0728 0.0356 0.080 Uiso 1 1 calc R . .
H4B H 0.1829 1.0441 0.1040 0.080 Uiso 1 1 calc R . .
N1 N 0.0372(4) 1.0058(3) 0.2605(5) 0.046(2) Uani 1 1 d . . .
H1C H 0.0543 1.0291 0.2920 0.055 Uiso 1 1 calc R . .
H1D H 0.0093 1.0217 0.2380 0.055 Uiso 1 1 calc R . .
N2 N 0.0671(4) 0.9084(3) 0.2153(6) 0.047(2) Uani 1 1 d . . .
H2C H 0.0569 0.8873 0.1739 0.056 Uiso 1 1 calc R . .
H2D H 0.0954 0.8942 0.2394 0.056 Uiso 1 1 calc R . .
N3 N 0.1343(4) 0.9523(3) 0.0830(6) 0.047(2) Uani 1 1 d . . .
H3C H 0.1639 0.9406 0.1064 0.057 Uiso 1 1 calc R . .
H3D H 0.1195 0.9260 0.0548 0.057 Uiso 1 1 calc R . .
N4 N 0.1067(3) 1.0492(3) 0.1315(6) 0.041(2) Uani 1 1 d . . .
H4C H 0.0798 1.0652 0.1063 0.049 Uiso 1 1 calc R . .
H4D H 0.1166 1.0689 0.1748 0.049 Uiso 1 1 calc R . .
O1 O 0.2015(2) 0.1917(3) 0.1055(4) 0.0331(16) Uani 1 1 d . . .
O2 O 0.0668(3) 0.1148(3) 0.3541(4) 0.0356(16) Uani 1 1 d . . .
O3 O 0.1253(3) 0.3303(3) 0.3555(4) 0.0343(16) Uani 1 1 d . . .
O4 O 0.1504(2) 0.2616(2) 0.2207(4) 0.0234(13) Uani 1 1 d . . .
O5 O 0.1220(2) 0.1598(2) 0.2225(4) 0.0258(14) Uani 1 1 d . . .
O6 O 0.0747(2) 0.2284(2) 0.3442(4) 0.0230(13) Uani 1 1 d . . .
O7 O -0.0168(2) 0.1921(2) 0.3167(4) 0.0236(13) Uani 1 1 d . . .
O8 O 0.0970(2) 0.1670(2) 0.0539(4) 0.0279(14) Uani 1 1 d . . .
O9 O 0.1278(2) 0.2678(2) 0.0541(4) 0.0241(13) Uani 1 1 d . . .
O10 O 0.0502(2) 0.2354(2) 0.1824(3) 0.0206(12) Uani 1 1 d . . .
O1W O 0.0143(3) 0.9748(3) 0.0842(5) 0.047(2) Uani 1 1 d . . .
O2W O 0.7870(3) 0.1298(4) 0.4287(7) 0.085(3) Uani 1 1 d . . .
O3W O 0.9052(5) 0.0600(4) 0.3221(7) 0.102(4) Uani 1 1 d . . .
O4W O 0.1227(7) 0.0343(6) 0.4182(12) 0.065(5) Uani 0.50 1 d P . .
O5W O 0.9201(7) 0.1529(8) 0.5078(9) 0.067(6) Uani 0.50 1 d P . .
O6W O 0.0174(7) 0.1098(8) 0.5003(11) 0.080(6) Uani 0.50 1 d PU . .
O7W O 0.1685(7) 0.9833(7) 0.2823(12) 0.183(7) Uani 1 1 d U . .
O8W O 0.1454(10) 0.8555(10) 0.3580(14) 0.107(8) Uani 0.50 1 d PU . .
O9W O 0.0585(12) 0.9753(11) 0.5272(18) 0.132(10) Uani 0.50 1 d PU . .


_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
Si1 O10 1.631(6) . ?
Si1 O10 1.631(6) 2 ?
Si1 O10 1.631(6) 16 ?
Si1 O10 1.631(6) 15 ?
Cu1 N2 1.997(9) . ?
Cu1 N4 1.997(9) . ?
Cu1 N1 2.018(9) . ?
Cu1 N3 2.027(9) . ?
Cu1 O1W 2.289(7) . ?
Nb1 O1 1.770(6) . ?
Nb1 O8 1.943(6) . ?
Nb1 O9 1.953(6) . ?
Nb1 O5 2.000(6) . ?
Nb1 O4 2.011(6) . ?
Nb1 O10 2.465(6) . ?
Nb2 O2 1.776(6) . ?
Nb2 O9 1.898(6) 15 ?
Nb2 O5 1.919(6) . ?
Nb2 O6 2.105(6) . ?
Nb2 O7 2.112(6) . ?
Nb2 O10 2.425(6) . ?
Nb2 Sb1 3.2931(9) . ?
Nb3 O3 1.768(6) . ?
Nb3 O8 1.894(6) 16 ?
Nb3 O4 1.904(6) . ?
Nb3 O6 2.080(6) . ?
Nb3 O7 2.112(6) 2 ?
Nb3 O10 2.427(6) . ?
Nb3 Sb1 3.2782(9) . ?
Sb1 O7 1.992(6) . ?
Sb1 O7 1.992(6) 2 ?
Sb1 O6 2.152(6) 2 ?
Sb1 O6 2.152(6) . ?
Sb1 Nb3 3.2783(9) 2 ?
Sb1 Nb2 3.2932(9) 2 ?
C1 C2 1.39(2) . ?
C1 N1 1.441(16) . ?
C2 N2 1.452(17) . ?
C3 N3 1.438(15) . ?
C3 C4 1.449(17) . ?
C4 N4 1.462(15) . ?
O7 Nb3 2.112(6) 2 ?
O8 Nb3 1.894(6) 15 ?
O9 Nb2 1.898(6) 16 ?

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
O10 Si1 O10 110.4(4) . 2 ?
O10 Si1 O10 108.99(19) . 16 ?
O10 Si1 O10 108.99(19) 2 16 ?
O10 Si1 O10 108.99(19) . 15 ?
O10 Si1 O10 108.99(19) 2 15 ?
O10 Si1 O10 110.4(4) 16 15 ?
N2 Cu1 N4 175.9(4) . . ?
N2 Cu1 N1 85.0(4) . . ?
N4 Cu1 N1 95.3(4) . . ?
N2 Cu1 N3 95.3(4) . . ?
N4 Cu1 N3 84.3(4) . . ?
N1 Cu1 N3 178.2(4) . . ?
N2 Cu1 O1W 90.1(3) . . ?
N4 Cu1 O1W 94.0(3) . . ?
N1 Cu1 O1W 89.0(3) . . ?
N3 Cu1 O1W 92.8(3) . . ?
O1 Nb1 O8 101.6(3) . . ?
O1 Nb1 O9 99.4(3) . . ?
O8 Nb1 O9 87.8(3) . . ?
O1 Nb1 O5 100.5(3) . . ?
O8 Nb1 O5 91.1(3) . . ?
O9 Nb1 O5 159.9(2) . . ?
O1 Nb1 O4 100.0(3) . . ?
O8 Nb1 O4 158.4(2) . . ?
O9 Nb1 O4 88.5(2) . . ?
O5 Nb1 O4 85.1(3) . . ?
O1 Nb1 O10 173.2(3) . . ?
O8 Nb1 O10 84.0(2) . . ?
O9 Nb1 O10 84.6(2) . . ?
O5 Nb1 O10 75.3(2) . . ?
O4 Nb1 O10 74.4(2) . . ?
O2 Nb2 O9 102.3(3) . 15 ?
O2 Nb2 O5 98.9(3) . . ?
O9 Nb2 O5 97.7(3) 15 . ?
O2 Nb2 O6 97.5(3) . . ?
O9 Nb2 O6 155.9(2) 15 . ?
O5 Nb2 O6 92.5(2) . . ?
O2 Nb2 O7 99.8(3) . . ?
O9 Nb2 O7 88.4(2) 15 . ?
O5 Nb2 O7 158.6(2) . . ?
O6 Nb2 O7 74.8(2) . . ?
O2 Nb2 O10 169.5(3) . . ?
O9 Nb2 O10 88.0(2) 15 . ?
O5 Nb2 O10 77.7(2) . . ?
O6 Nb2 O10 72.9(2) . . ?
O7 Nb2 O10 82.0(2) . . ?
O2 Nb2 Sb1 96.8(2) . . ?
O9 Nb2 Sb1 123.14(18) 15 . ?
O5 Nb2 Sb1 131.42(18) . . ?
O6 Nb2 Sb1 39.83(16) . . ?
O7 Nb2 Sb1 35.41(16) . . ?
O10 Nb2 Sb1 78.63(13) . . ?
O3 Nb3 O8 101.4(3) . 16 ?
O3 Nb3 O4 103.1(3) . . ?
O8 Nb3 O4 95.8(3) 16 . ?
O3 Nb3 O6 98.5(3) . . ?
O8 Nb3 O6 155.1(2) 16 . ?
O4 Nb3 O6 94.0(2) . . ?
O3 Nb3 O7 96.8(3) . 2 ?
O8 Nb3 O7 87.6(2) 16 2 ?
O4 Nb3 O7 158.6(2) . 2 ?
O6 Nb3 O7 75.3(2) . 2 ?
O3 Nb3 O10 171.8(3) . . ?
O8 Nb3 O10 86.7(2) 16 . ?
O4 Nb3 O10 77.1(2) . . ?
O6 Nb3 O10 73.3(2) . . ?
O7 Nb3 O10 82.0(2) 2 . ?
O3 Nb3 Sb1 95.4(2) . . ?
O8 Nb3 Sb1 122.59(19) 16 . ?
O4 Nb3 Sb1 132.93(18) . . ?
O6 Nb3 Sb1 40.02(16) . . ?
O7 Nb3 Sb1 35.74(16) 2 . ?
O10 Nb3 Sb1 78.92(13) . . ?
O7 Sb1 O7 101.8(3) . 2 ?
O7 Sb1 O6 76.3(2) . 2 ?
O7 Sb1 O6 76.3(2) 2 2 ?
O7 Sb1 O6 76.3(2) . . ?
O7 Sb1 O6 76.3(2) 2 . ?
O6 Sb1 O6 135.8(3) 2 . ?
O7 Sb1 Nb3 92.97(17) . . ?
O7 Sb1 Nb3 38.25(17) 2 . ?
O6 Sb1 Nb3 110.22(16) 2 . ?
O6 Sb1 Nb3 38.43(16) . . ?
O7 Sb1 Nb3 38.26(17) . 2 ?
O7 Sb1 Nb3 92.97(17) 2 2 ?
O6 Sb1 Nb3 38.43(16) 2 2 ?
O6 Sb1 Nb3 110.22(16) . 2 ?
Nb3 Sb1 Nb3 108.86(4) . 2 ?
O7 Sb1 Nb2 37.90(17) . . ?
O7 Sb1 Nb2 93.01(17) 2 . ?
O6 Sb1 Nb2 109.86(16) 2 . ?
O6 Sb1 Nb2 38.80(15) . . ?
Nb3 Sb1 Nb2 65.45(2) . . ?
Nb3 Sb1 Nb2 74.69(2) 2 . ?
O7 Sb1 Nb2 93.02(17) . 2 ?
O7 Sb1 Nb2 37.91(17) 2 2 ?
O6 Sb1 Nb2 38.80(15) 2 2 ?
O6 Sb1 Nb2 109.86(16) . 2 ?
Nb3 Sb1 Nb2 74.69(2) . 2 ?
Nb3 Sb1 Nb2 65.45(2) 2 2 ?
Nb2 Sb1 Nb2 108.53(4) . 2 ?
C2 C1 N1 116.6(14) . . ?
C1 C2 N2 114.6(14) . . ?
N3 C3 C4 111.4(11) . . ?
C3 C4 N4 109.9(11) . . ?
C1 N1 Cu1 108.5(8) . . ?
C2 N2 Cu1 109.3(9) . . ?
C3 N3 Cu1 107.3(7) . . ?
C4 N4 Cu1 109.5(7) . . ?
Nb3 O4 Nb1 120.4(3) . . ?
Nb2 O5 Nb1 119.2(3) . . ?
Nb3 O6 Nb2 116.2(3) . . ?
Nb3 O6 Sb1 101.6(2) . . ?
Nb2 O6 Sb1 101.4(2) . . ?
Sb1 O7 Nb3 106.0(3) . 2 ?
Sb1 O7 Nb2 106.7(3) . . ?
Nb3 O7 Nb2 141.4(3) 2 . ?
Nb3 O8 Nb1 153.7(3) 15 . ?
Nb2 O9 Nb1 151.6(3) 16 . ?
Si1 O10 Nb2 125.2(3) . . ?
Si1 O10 Nb3 125.5(3) . . ?
Nb2 O10 Nb3 94.2(2) . . ?
Si1 O10 Nb1 125.3(3) . . ?
Nb2 O10 Nb1 87.43(18) . . ?
Nb3 O10 Nb1 88.02(19) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.214
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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_shelxl
_audit_block_doi                 10.5517/cc138bnc
_database_code_depnum_ccdc_archive 'CCDC 1020912'
_audit_update_record             
;
2014-08-23 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'H2 Ge Nb12 O40 Sb2, 4(C4 H18 Cu N4 O), 22(H2 O)'
_chemical_formula_sum            'C16 H118 Cu4 Ge N16 Nb12 O66 Sb2'
_chemical_formula_weight         3276.43

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'
Cu Cu 0.3201 1.2651 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   25.5410(4)
_cell_length_b                   25.5410(4)
_cell_length_c                   16.1450(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10532.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6384
_exptl_absorpt_coefficient_mu    2.917
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19047
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4616
_reflns_number_gt                3894
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0529P)²+167.4637P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4616
_refine_ls_number_parameters     282
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.1202
_refine_ls_wR_factor_gt          0.1134
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.0000 0.2500 0.1250 0.0114(3) Uani 1 4 d S . .
Nb1 Nb 0.13806(2) 0.29090(2) 0.13014(4) 0.01862(16) Uani 1 1 d . . .
Nb2 Nb 0.09508(2) 0.20473(2) 0.27798(4) 0.01911(16) Uani 1 1 d . . .
Nb3 Nb 0.05573(2) 0.33956(2) 0.27703(4) 0.01899(16) Uani 1 1 d . . .
Sb1 Sb 0.0000 0.2500 0.39349(4) 0.02393(17) Uani 1 2 d S . .
Cu1 Cu 0.08570(4) 0.52143(3) 0.17235(6) 0.0353(2) Uani 1 1 d . . .
O1 O 0.05851(19) 0.04757(18) 0.1454(3) 0.0310(11) Uani 1 1 d . . .
O2 O 0.12663(19) 0.1690(2) 0.3562(3) 0.0319(11) Uani 1 1 d . . .
O3 O 0.0667(2) 0.38654(19) 0.3546(3) 0.0320(11) Uani 1 1 d . . .
O4 O 0.12159(16) 0.34049(16) 0.2218(3) 0.0222(9) Uani 1 1 d . . .
O5 O 0.15073(16) 0.23850(17) 0.2208(3) 0.0223(10) Uani 1 1 d . . .
O6 O 0.07522(17) 0.27206(16) 0.3442(3) 0.0225(10) Uani 1 1 d . . .
O7 O 0.01783(17) 0.37698(17) 0.1961(3) 0.0229(10) Uani 1 1 d . . .
O8 O -0.01663(17) 0.30777(17) 0.3148(3) 0.0221(9) Uani 1 1 d . . .
O9 O 0.08232(16) 0.15317(17) 0.1965(3) 0.0234(10) Uani 1 1 d . . .
O10 O 0.05266(16) 0.26542(15) 0.1850(3) 0.0188(9) Uani 1 1 d . . .
O1W O 0.0154(2) 0.5250(2) 0.0846(4) 0.0441(14) Uani 1 1 d . . .
C1 C 0.0229(6) 0.5860(4) 0.2733(8) 0.087(4) Uani 1 1 d . . .
H1A H 0.0252 0.6126 0.3160 0.105 Uiso 1 1 calc R . .
H1B H -0.0090 0.5923 0.2423 0.105 Uiso 1 1 calc R . .
C2 C 0.0193(6) 0.5386(4) 0.3102(9) 0.091(4) Uani 1 1 d . . .
H2A H -0.0170 0.5324 0.3246 0.110 Uiso 1 1 calc R . .
H2B H 0.0391 0.5397 0.3614 0.110 Uiso 1 1 calc R . .
C3 C 0.1465(5) 0.5046(4) 0.0300(7) 0.072(3) Uani 1 1 d . . .
H3A H 0.1188 0.5014 -0.0107 0.087 Uiso 1 1 calc R . .
H3B H 0.1789 0.5118 0.0007 0.087 Uiso 1 1 calc R . .
C4 C 0.1516(4) 0.4558(4) 0.0755(7) 0.062(3) Uani 1 1 d . . .
H4A H 0.1839 0.4559 0.1071 0.074 Uiso 1 1 calc R . .
H4B H 0.1527 0.4267 0.0371 0.074 Uiso 1 1 calc R . .
N1 N 0.0677(3) 0.5922(3) 0.2170(5) 0.0480(18) Uani 1 1 d . . .
H1C H 0.0953 0.6057 0.2445 0.058 Uiso 1 1 calc R . .
H1D H 0.0594 0.6141 0.1753 0.058 Uiso 1 1 calc R . .
N2 N 0.0378(3) 0.4946(3) 0.2614(4) 0.0456(17) Uani 1 1 d . . .
H2C H 0.0104 0.4779 0.2384 0.055 Uiso 1 1 calc R . .
H2D H 0.0550 0.4719 0.2940 0.055 Uiso 1 1 calc R . .
N3 N 0.1348(3) 0.5478(3) 0.0857(5) 0.0459(17) Uani 1 1 d . . .
H3C H 0.1200 0.5743 0.0575 0.055 Uiso 1 1 calc R . .
H3D H 0.1645 0.5597 0.1094 0.055 Uiso 1 1 calc R . .
N4 N 0.1069(3) 0.4500(3) 0.1314(4) 0.0387(15) Uani 1 1 d . . .
H4C H 0.1157 0.4295 0.1745 0.046 Uiso 1 1 calc R . .
H4D H 0.0800 0.4349 0.1045 0.046 Uiso 1 1 calc R . .
O2W O 0.2139(3) 0.1270(3) 0.4284(6) 0.094(3) Uani 1 1 d . . .
O3W O 0.0948(5) 0.0587(4) 0.3254(7) 0.120(4) Uani 1 1 d . . .
O4W O 0.1253(6) 0.4670(6) 0.4192(11) 0.078(5) Uani 0.50 1 d P . .
O5W O 0.0766(6) 0.1561(8) 0.5086(7) 0.085(5) Uani 0.50 1 d P . .
O6W O 0.0145(7) 0.3974(7) 0.4987(11) 0.089(5) Uiso 0.50 1 d P . .
O7W O 0.1676(6) 0.5177(6) 0.2798(10) 0.176(6) Uani 1 1 d U . .
O8W O 0.1398(9) 0.1475(8) 0.6462(10) 0.109(7) Uani 0.50 1 d P . .
O9W O 0.0568(10) 0.5210(10) 0.5275(15) 0.134(8) Uani 0.50 1 d PU . .


_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
Ge1 O10 1.704(4) 16 ?
Ge1 O10 1.704(4) 2 ?
Ge1 O10 1.704(4) 15 ?
Ge1 O10 1.704(4) . ?
Nb1 O1 1.754(5) 16 ?
Nb1 O9 1.939(4) 16 ?
Nb1 O7 1.961(4) 15 ?
Nb1 O4 1.992(4) . ?
Nb1 O5 2.009(4) . ?
Nb1 O10 2.443(4) . ?
Nb2 O2 1.754(5) . ?
Nb2 O9 1.890(4) . ?
Nb2 O5 1.902(4) . ?
Nb2 O6 2.088(4) . ?
Nb2 O8 2.114(4) 2 ?
Nb2 O10 2.414(4) . ?
Nb2 Sb1 3.2728(7) . ?
Nb3 O3 1.757(5) . ?
Nb3 O7 1.886(4) . ?
Nb3 O4 1.904(4) . ?
Nb3 O6 2.097(4) . ?
Nb3 O8 2.109(4) . ?
Nb3 O10 2.408(4) . ?
Nb3 Sb1 3.2854(7) . ?
Sb1 O8 1.993(4) . ?
Sb1 O8 1.993(4) 2 ?
Sb1 O6 2.154(4) . ?
Sb1 O6 2.154(4) 2 ?
Sb1 Nb2 3.2728(7) 2 ?
Sb1 Nb3 3.2854(7) 2 ?
Cu1 N3 1.997(7) . ?
Cu1 N1 2.000(7) . ?
Cu1 N2 2.009(7) . ?
Cu1 N4 2.014(7) . ?
Cu1 O1W 2.289(5) . ?
O1 Nb1 1.754(5) 15 ?
O7 Nb1 1.961(4) 16 ?
O8 Nb2 2.114(4) 2 ?
O9 Nb1 1.939(4) 15 ?
C1 C2 1.353(15) . ?
C1 N1 1.471(14) . ?
C2 N2 1.450(13) . ?
C3 C4 1.452(13) . ?
C3 N3 1.454(13) . ?
C4 N4 1.462(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Ge1 O10 108.86(14) 16 2 ?
O10 Ge1 O10 110.7(3) 16 15 ?
O10 Ge1 O10 108.86(14) 2 15 ?
O10 Ge1 O10 108.86(14) 16 . ?
O10 Ge1 O10 110.7(3) 2 . ?
O10 Ge1 O10 108.86(14) 15 . ?
O1 Nb1 O9 102.6(2) 16 16 ?
O1 Nb1 O7 100.6(2) 16 15 ?
O9 Nb1 O7 86.46(18) 16 15 ?
O1 Nb1 O4 102.1(2) 16 . ?
O9 Nb1 O4 90.70(19) 16 . ?
O7 Nb1 O4 157.20(18) 15 . ?
O1 Nb1 O5 101.0(2) 16 . ?
O9 Nb1 O5 156.30(18) 16 . ?
O7 Nb1 O5 88.34(18) 15 . ?
O4 Nb1 O5 85.22(18) . . ?
O1 Nb1 O10 172.3(2) 16 . ?
O9 Nb1 O10 83.78(16) 16 . ?
O7 Nb1 O10 83.97(16) 15 . ?
O4 Nb1 O10 73.24(15) . . ?
O5 Nb1 O10 72.68(15) . . ?
O2 Nb2 O9 102.6(2) . . ?
O2 Nb2 O5 104.0(2) . . ?
O9 Nb2 O5 96.14(19) . . ?
O2 Nb2 O6 99.9(2) . . ?
O9 Nb2 O6 152.73(18) . . ?
O5 Nb2 O6 93.26(18) . . ?
O2 Nb2 O8 98.9(2) . 2 ?
O9 Nb2 O8 85.82(18) . 2 ?
O5 Nb2 O8 155.99(18) . 2 ?
O6 Nb2 O8 75.52(17) . 2 ?
O2 Nb2 O10 171.0(2) . . ?
O9 Nb2 O10 86.40(17) . . ?
O5 Nb2 O10 75.08(16) . . ?
O6 Nb2 O10 71.39(16) . . ?
O8 Nb2 O10 81.18(16) 2 . ?
O2 Nb2 Sb1 96.58(17) . . ?
O9 Nb2 Sb1 120.99(13) . . ?
O5 Nb2 Sb1 132.15(13) . . ?
O6 Nb2 Sb1 40.25(12) . . ?
O8 Nb2 Sb1 35.90(12) 2 . ?
O10 Nb2 Sb1 78.15(10) . . ?
O3 Nb3 O7 103.3(2) . . ?
O3 Nb3 O4 100.6(2) . . ?
O7 Nb3 O4 97.04(19) . . ?
O3 Nb3 O6 98.9(2) . . ?
O7 Nb3 O6 153.75(18) . . ?
O4 Nb3 O6 92.46(18) . . ?
O3 Nb3 O8 101.4(2) . . ?
O7 Nb3 O8 86.89(18) . . ?
O4 Nb3 O8 156.14(18) . . ?
O6 Nb3 O8 75.04(17) . . ?
O3 Nb3 O10 169.10(19) . . ?
O7 Nb3 O10 87.39(17) . . ?
O4 Nb3 O10 75.49(16) . . ?
O6 Nb3 O10 71.37(16) . . ?
O8 Nb3 O10 81.21(16) . . ?
O3 Nb3 Sb1 97.88(17) . . ?
O7 Nb3 Sb1 121.79(13) . . ?
O4 Nb3 Sb1 131.26(13) . . ?
O6 Nb3 Sb1 40.03(12) . . ?
O8 Nb3 Sb1 35.57(12) . . ?
O10 Nb3 Sb1 77.97(10) . . ?
O8 Sb1 O8 100.8(3) . 2 ?
O8 Sb1 O6 76.18(17) . . ?
O8 Sb1 O6 76.61(17) 2 . ?
O8 Sb1 O6 76.61(17) . 2 ?
O8 Sb1 O6 76.19(17) 2 2 ?
O6 Sb1 O6 136.7(2) . 2 ?
O8 Sb1 Nb2 38.47(12) . 2 ?
O8 Sb1 Nb2 93.24(13) 2 2 ?
O6 Sb1 Nb2 111.04(12) . 2 ?
O6 Sb1 Nb2 38.77(11) 2 2 ?
O8 Sb1 Nb2 93.24(13) . . ?
O8 Sb1 Nb2 38.47(12) 2 . ?
O6 Sb1 Nb2 38.77(11) . . ?
O6 Sb1 Nb2 111.04(12) 2 . ?
Nb2 Sb1 Nb2 110.52(3) 2 . ?
O8 Sb1 Nb3 38.00(12) . . ?
O8 Sb1 Nb3 93.36(13) 2 . ?
O6 Sb1 Nb3 38.77(11) . . ?
O6 Sb1 Nb3 110.93(12) 2 . ?
Nb2 Sb1 Nb3 75.484(17) 2 . ?
Nb2 Sb1 Nb3 66.323(16) . . ?
O8 Sb1 Nb3 93.36(13) . 2 ?
O8 Sb1 Nb3 38.00(12) 2 2 ?
O6 Sb1 Nb3 110.93(12) . 2 ?
O6 Sb1 Nb3 38.77(11) 2 2 ?
Nb2 Sb1 Nb3 66.324(16) 2 2 ?
Nb2 Sb1 Nb3 75.486(17) . 2 ?
Nb3 Sb1 Nb3 110.18(3) . 2 ?
N3 Cu1 N1 95.2(3) . . ?
N3 Cu1 N2 178.6(3) . . ?
N1 Cu1 N2 84.9(3) . . ?
N3 Cu1 N4 84.6(3) . . ?
N1 Cu1 N4 177.1(3) . . ?
N2 Cu1 N4 95.2(3) . . ?
N3 Cu1 O1W 92.6(3) . . ?
N1 Cu1 O1W 90.4(3) . . ?
N2 Cu1 O1W 88.8(3) . . ?
N4 Cu1 O1W 92.5(2) . . ?
Nb3 O4 Nb1 121.8(2) . . ?
Nb2 O5 Nb1 122.4(2) . . ?
Nb2 O6 Nb3 118.0(2) . . ?
Nb2 O6 Sb1 100.98(18) . . ?
Nb3 O6 Sb1 101.20(18) . . ?
Nb3 O7 Nb1 154.2(2) . 16 ?
Sb1 O8 Nb3 106.43(19) . . ?
Sb1 O8 Nb2 105.63(19) . 2 ?
Nb3 O8 Nb2 143.8(2) . 2 ?
Nb2 O9 Nb1 156.5(3) . 15 ?
Ge1 O10 Nb3 123.9(2) . . ?
Ge1 O10 Nb2 124.0(2) . . ?
Nb3 O10 Nb2 96.12(15) . . ?
Ge1 O10 Nb1 124.1(2) . . ?
Nb3 O10 Nb1 89.15(14) . . ?
Nb2 O10 Nb1 89.76(14) . . ?
C2 C1 N1 114.9(10) . . ?
C1 C2 N2 115.6(10) . . ?
C4 C3 N3 110.9(9) . . ?
C3 C4 N4 109.3(8) . . ?
C1 N1 Cu1 107.7(6) . . ?
C2 N2 Cu1 108.9(6) . . ?
C3 N3 Cu1 107.8(5) . . ?
C4 N4 Cu1 108.7(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.633
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.156
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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_shelxl
_audit_block_doi                 10.5517/cc138bpd
_database_code_depnum_ccdc_archive 'CCDC 1020913'
_audit_update_record             
;
2014-08-23 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H Nb12 O40 P Sb2, 4(C4 H18 Cu N4 O), 22(H2 O)'
_chemical_formula_sum            'C16 H117 Cu4 N16 Nb12 O66 P Sb2'
_chemical_formula_weight         3233.81

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   25.6100(5)
_cell_length_b                   25.6100(5)
_cell_length_c                   16.1860(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10615.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6312
_exptl_absorpt_coefficient_mu    2.632
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19856
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4655
_reflns_number_gt                3446
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0643P)²+159.6516P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4655
_refine_ls_number_parameters     286
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1451
_refine_ls_wR_factor_gt          0.1313
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.58590(5) 0.97838(4) 0.32825(8) 0.0363(3) Uani 1 1 d . . .
Nb1 Nb 0.63826(3) 0.20926(3) 0.37039(5) 0.0193(2) Uani 1 1 d . . .
Nb2 Nb 0.59453(3) 0.29576(3) 0.22221(5) 0.0198(2) Uani 1 1 d . . .
Nb3 Nb 0.55519(3) 0.16046(3) 0.22321(5) 0.0195(2) Uani 1 1 d . . .
Sb1 Sb 0.5000 0.2500 0.10621(5) 0.0243(2) Uani 1 2 d S . .
P1 P 0.5000 0.2500 0.3750 0.0001(6) Uiso 1 4 d S . .
O1 O 0.4415(2) 0.0471(2) 0.3557(4) 0.0321(15) Uani 1 1 d . . .
O2 O 0.6264(2) 0.3305(2) 0.1440(4) 0.0309(15) Uani 1 1 d . . .
O3 O 0.5674(2) 0.1136(2) 0.1453(4) 0.0315(15) Uani 1 1 d . . .
O4 O 0.6210(2) 0.1600(2) 0.2785(4) 0.0238(13) Uani 1 1 d . . .
O5 O 0.6497(2) 0.2617(2) 0.2801(4) 0.0228(13) Uani 1 1 d . . .
O6 O 0.5747(2) 0.2285(2) 0.1570(4) 0.0228(13) Uani 1 1 d . . .
O7 O 0.5166(2) 0.3084(2) 0.1836(4) 0.0217(13) Uani 1 1 d . . .
O8 O 0.5825(2) 0.3480(2) 0.3024(4) 0.0239(13) Uani 1 1 d . . .
O9 O 0.5177(2) 0.1221(2) 0.3028(4) 0.0224(13) Uani 1 1 d . . .
O10 O 0.5488(2) 0.2355(2) 0.3187(4) 0.0212(13) Uani 1 1 d . . .
O1W O 0.5151(3) 0.9744(3) 0.4166(5) 0.0464(19) Uani 1 1 d . . .
C1 C 0.5202(7) 0.9616(6) 0.1890(11) 0.088(5) Uani 1 1 d U . .
H1A H 0.4840 0.9676 0.1739 0.106 Uiso 1 1 calc R . .
H1B H 0.5405 0.9608 0.1385 0.106 Uiso 1 1 calc R . .
C2 C 0.5238(7) 0.9131(5) 0.2269(10) 0.087(5) Uani 1 1 d . . .
H2A H 0.5268 0.8866 0.1844 0.104 Uiso 1 1 calc R . .
H2B H 0.4918 0.9066 0.2571 0.104 Uiso 1 1 calc R . .
C3 C 0.6514(5) 1.0435(4) 0.4252(9) 0.060(3) Uani 1 1 d . . .
H3A H 0.6837 1.0436 0.3938 0.072 Uiso 1 1 calc R . .
H3B H 0.6522 1.0727 0.4632 0.072 Uiso 1 1 calc R . .
C4 C 0.6474(6) 0.9958(5) 0.4706(9) 0.073(4) Uani 1 1 d . . .
H4A H 0.6202 0.9991 0.5120 0.087 Uiso 1 1 calc R . .
H4B H 0.6801 0.9891 0.4989 0.087 Uiso 1 1 calc R . .
N1 N 0.5379(4) 1.0051(3) 0.2390(5) 0.047(2) Uani 1 1 d . . .
H1C H 0.5104 1.0214 0.2619 0.056 Uiso 1 1 calc R . .
H1D H 0.5550 1.0283 0.2070 0.056 Uiso 1 1 calc R . .
N2 N 0.5675(4) 0.9077(3) 0.2833(6) 0.050(2) Uani 1 1 d . . .
H2C H 0.5951 0.8940 0.2565 0.060 Uiso 1 1 calc R . .
H2D H 0.5588 0.8861 0.3249 0.060 Uiso 1 1 calc R . .
N3 N 0.6072(3) 1.0492(3) 0.3690(5) 0.037(2) Uani 1 1 d . . .
H3C H 0.6162 1.0696 0.3260 0.044 Uiso 1 1 calc R . .
H3D H 0.5803 1.0645 0.3955 0.044 Uiso 1 1 calc R . .
N4 N 0.6352(3) 0.9518(3) 0.4152(6) 0.044(2) Uani 1 1 d . . .
H4C H 0.6202 0.9256 0.4438 0.053 Uiso 1 1 calc R . .
H4D H 0.6646 0.9396 0.3916 0.053 Uiso 1 1 calc R . .
O2W O 0.7140(3) 0.3724(4) 0.0710(8) 0.094(4) Uani 1 1 d . . .
O3W O 0.5949(6) 0.4421(5) 0.1743(9) 0.129(5) Uani 1 1 d . . .
O4W O 0.5773(6) 0.3456(7) -0.0078(10) 0.065(5) Uani 0.50 1 d PU . .
O5W O 0.6245(7) 0.0324(7) 0.0808(13) 0.079(6) Uani 0.50 1 d P . .
O6W O 0.6404(8) 0.8528(8) 0.1439(13) 0.087(6) Uani 0.50 1 d PU . .
O7W O 0.6690(7) 0.9829(7) 0.2203(12) 0.181(7) Uani 1 1 d . . .
O8W O 0.5150(8) 0.1051(9) 0.0003(13) 0.090(6) Uani 0.50 1 d PU . .
O9W O 0.5591(13) -0.0209(13) -0.030(2) 0.159(12) Uani 0.50 1 d PU . .


_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
Cu1 N3 2.006(8) . ?
Cu1 N2 2.007(9) . ?
Cu1 N4 2.010(9) . ?
Cu1 N1 2.017(9) . ?
Cu1 O1W 2.312(7) . ?
Nb1 O1 1.760(6) 12_656 ?
Nb1 O8 1.940(6) 11_666 ?
Nb1 O9 1.963(6) 12_656 ?
Nb1 O4 1.999(6) . ?
Nb1 O5 2.006(6) . ?
Nb1 O10 2.530(5) . ?
Nb2 O2 1.749(6) . ?
Nb2 O8 1.890(6) . ?
Nb2 O5 1.906(5) . ?
Nb2 O6 2.082(6) . ?
Nb2 O7 2.116(5) . ?
Nb2 O10 2.489(6) . ?
Nb2 Sb1 3.2802(9) . ?
Nb3 O3 1.769(6) . ?
Nb3 O9 1.884(6) . ?
Nb3 O4 1.909(6) . ?
Nb3 O7 2.105(5) 2_655 ?
Nb3 O6 2.106(6) . ?
Nb3 O10 2.471(5) . ?
Nb3 Sb1 3.2927(9) . ?
Sb1 O7 1.996(5) . ?
Sb1 O7 1.996(5) 2_655 ?
Sb1 O6 2.153(6) . ?
Sb1 O6 2.153(6) 2_655 ?
Sb1 Nb2 3.2802(9) 2_655 ?
Sb1 Nb3 3.2927(9) 2_655 ?
P1 O10 1.590(6) 12_656 ?
P1 O10 1.590(5) 2_655 ?
P1 O10 1.590(6) . ?
P1 O10 1.590(5) 11_666 ?
O1 Nb1 1.760(6) 11_666 ?
O7 Nb3 2.105(5) 2_655 ?
O8 Nb1 1.940(6) 12_656 ?
O9 Nb1 1.963(6) 11_666 ?
C1 C2 1.387(19) . ?
C1 N1 1.450(16) . ?
C2 N2 1.450(16) . ?
C3 C4 1.429(16) . ?
C3 N3 1.460(14) . ?
C4 N4 1.475(16) . ?

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
N3 Cu1 N2 177.1(4) . . ?
N3 Cu1 N4 84.6(3) . . ?
N2 Cu1 N4 95.5(4) . . ?
N3 Cu1 N1 95.4(3) . . ?
N2 Cu1 N1 84.4(4) . . ?
N4 Cu1 N1 178.5(4) . . ?
N3 Cu1 O1W 92.8(3) . . ?
N2 Cu1 O1W 90.1(3) . . ?
N4 Cu1 O1W 92.6(3) . . ?
N1 Cu1 O1W 88.9(3) . . ?
O1 Nb1 O8 102.5(3) 12_656 11_666 ?
O1 Nb1 O9 100.6(3) 12_656 12_656 ?
O8 Nb1 O9 86.6(2) 11_666 12_656 ?
O1 Nb1 O4 102.0(3) 12_656 . ?
O8 Nb1 O4 90.8(2) 11_666 . ?
O9 Nb1 O4 157.2(2) 12_656 . ?
O1 Nb1 O5 101.3(3) 12_656 . ?
O8 Nb1 O5 156.2(2) 11_666 . ?
O9 Nb1 O5 88.3(2) 12_656 . ?
O4 Nb1 O5 85.0(2) . . ?
O1 Nb1 O10 173.3(3) 12_656 . ?
O8 Nb1 O10 83.0(2) 11_666 . ?
O9 Nb1 O10 83.4(2) 12_656 . ?
O4 Nb1 O10 73.8(2) . . ?
O5 Nb1 O10 73.35(19) . . ?
O2 Nb2 O8 102.3(3) . . ?
O2 Nb2 O5 104.0(3) . . ?
O8 Nb2 O5 96.2(2) . . ?
O2 Nb2 O6 99.6(3) . . ?
O8 Nb2 O6 153.3(2) . . ?
O5 Nb2 O6 93.0(2) . . ?
O2 Nb2 O7 98.5(3) . . ?
O8 Nb2 O7 86.6(2) . . ?
O5 Nb2 O7 156.1(2) . . ?
O6 Nb2 O7 75.3(2) . . ?
O2 Nb2 O10 171.5(2) . . ?
O8 Nb2 O10 86.1(2) . . ?
O5 Nb2 O10 75.9(2) . . ?
O6 Nb2 O10 71.9(2) . . ?
O7 Nb2 O10 80.6(2) . . ?
O2 Nb2 Sb1 96.4(2) . . ?
O8 Nb2 Sb1 121.71(17) . . ?
O5 Nb2 Sb1 131.67(17) . . ?
O6 Nb2 Sb1 40.04(15) . . ?
O7 Nb2 Sb1 35.85(15) . . ?
O10 Nb2 Sb1 77.88(13) . . ?
O3 Nb3 O9 102.9(3) . . ?
O3 Nb3 O4 100.0(3) . . ?
O9 Nb3 O4 97.3(2) . . ?
O3 Nb3 O7 101.2(3) . 2_655 ?
O9 Nb3 O7 87.7(2) . 2_655 ?
O4 Nb3 O7 156.5(2) . 2_655 ?
O3 Nb3 O6 99.1(3) . . ?
O9 Nb3 O6 154.2(2) . . ?
O4 Nb3 O6 92.0(2) . . ?
O7 Nb3 O6 74.8(2) 2_655 . ?
O3 Nb3 O10 170.1(2) . . ?
O9 Nb3 O10 86.8(2) . . ?
O4 Nb3 O10 76.7(2) . . ?
O7 Nb3 O10 80.7(2) 2_655 . ?
O6 Nb3 O10 72.0(2) . . ?
O3 Nb3 Sb1 98.0(2) . . ?
O9 Nb3 Sb1 122.52(17) . . ?
O4 Nb3 Sb1 130.76(17) . . ?
O7 Nb3 Sb1 35.48(15) 2_655 . ?
O6 Nb3 Sb1 39.90(15) . . ?
O10 Nb3 Sb1 77.87(13) . . ?
O7 Sb1 O7 102.3(3) . 2_655 ?
O7 Sb1 O6 76.2(2) . . ?
O7 Sb1 O6 76.0(2) 2_655 . ?
O7 Sb1 O6 76.0(2) . 2_655 ?
O7 Sb1 O6 76.2(2) 2_655 2_655 ?
O6 Sb1 O6 135.1(3) . 2_655 ?
O7 Sb1 Nb2 38.37(15) . . ?
O7 Sb1 Nb2 93.78(16) 2_655 . ?
O6 Sb1 Nb2 38.46(15) . . ?
O6 Sb1 Nb2 110.22(15) 2_655 . ?
O7 Sb1 Nb2 93.78(16) . 2_655 ?
O7 Sb1 Nb2 38.37(15) 2_655 2_655 ?
O6 Sb1 Nb2 110.22(15) . 2_655 ?
O6 Sb1 Nb2 38.46(15) 2_655 2_655 ?
Nb2 Sb1 Nb2 110.16(4) . 2_655 ?
O7 Sb1 Nb3 37.74(15) . 2_655 ?
O7 Sb1 Nb3 93.98(16) 2_655 2_655 ?
O6 Sb1 Nb3 109.83(15) . 2_655 ?
O6 Sb1 Nb3 38.86(15) 2_655 2_655 ?
Nb2 Sb1 Nb3 74.86(2) . 2_655 ?
Nb2 Sb1 Nb3 66.59(2) 2_655 2_655 ?
O7 Sb1 Nb3 93.98(16) . . ?
O7 Sb1 Nb3 37.73(15) 2_655 . ?
O6 Sb1 Nb3 38.85(15) . . ?
O6 Sb1 Nb3 109.83(15) 2_655 . ?
Nb2 Sb1 Nb3 66.60(2) . . ?
Nb2 Sb1 Nb3 74.86(2) 2_655 . ?
Nb3 Sb1 Nb3 109.78(4) 2_655 . ?
O10 P1 O10 109.2(2) 12_656 2_655 ?
O10 P1 O10 109.2(2) 12_656 . ?
O10 P1 O10 110.1(4) 2_655 . ?
O10 P1 O10 110.1(4) 12_656 11_666 ?
O10 P1 O10 109.2(2) 2_655 11_666 ?
O10 P1 O10 109.2(2) . 11_666 ?
Nb3 O4 Nb1 122.7(3) . . ?
Nb2 O5 Nb1 123.8(3) . . ?
Nb2 O6 Nb3 119.0(3) . . ?
Nb2 O6 Sb1 101.5(2) . . ?
Nb3 O6 Sb1 101.3(2) . . ?
Sb1 O7 Nb3 106.8(2) . 2_655 ?
Sb1 O7 Nb2 105.8(2) . . ?
Nb3 O7 Nb2 142.3(3) 2_655 . ?
Nb2 O8 Nb1 155.3(3) . 12_656 ?
Nb3 O9 Nb1 153.2(3) . 11_666 ?
P1 O10 Nb3 126.3(3) . . ?
P1 O10 Nb2 125.7(3) . . ?
Nb3 O10 Nb2 93.3(2) . . ?
P1 O10 Nb1 125.7(3) . . ?
Nb3 O10 Nb1 86.58(17) . . ?
Nb2 O10 Nb1 86.88(17) . . ?
C2 C1 N1 114.9(13) . . ?
C1 C2 N2 114.6(12) . . ?
C4 C3 N3 110.6(10) . . ?
C3 C4 N4 110.8(12) . . ?
C1 N1 Cu1 109.2(8) . . ?
C2 N2 Cu1 108.8(7) . . ?
C3 N3 Cu1 108.9(6) . . ?
C4 N4 Cu1 107.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.276
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.183
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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_shelxl
_audit_block_doi                 10.5517/cc138bqf
_database_code_depnum_ccdc_archive 'CCDC 1020914'
_audit_update_record             
;
2014-08-23 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'H As Nb12 O40 Sb2, 4(C4 H18 Cu N4 O), 22(H2 O)'
_chemical_formula_sum            'C16 H117 As Cu4 N16 Nb12 O66 Sb2'
_chemical_formula_weight         3277.76

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'
As As 0.0499 2.0058 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   25.6050(5)
_cell_length_b                   25.6050(5)
_cell_length_c                   16.1890(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10613.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6384
_exptl_absorpt_coefficient_mu    2.927
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18769
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4641
_reflns_number_gt                3861
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0598P)²+167.8265P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4641
_refine_ls_number_parameters     287
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1295
_refine_ls_wR_factor_gt          0.1207
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.91415(4) 0.47851(4) 0.82796(6) 0.0375(3) Uani 1 1 d . . .
As1 As 0.0000 0.2500 0.1250 0.0154(3) Uani 1 4 d S . .
Nb1 Nb -0.04088(2) 0.38821(2) 0.12001(4) 0.01998(17) Uani 1 1 d . . .
Nb2 Nb 0.04556(2) 0.34489(2) -0.02810(4) 0.02032(17) Uani 1 1 d . . .
Nb3 Nb -0.08965(2) 0.30549(2) -0.02720(4) 0.02043(17) Uani 1 1 d . . .
Sb1 Sb 0.0000 0.2500 -0.14455(4) 0.02414(18) Uani 1 2 d S . .
O1 O -0.0584(2) 0.45264(19) 0.1448(3) 0.0326(12) Uani 1 1 d . . .
O2 O 0.0810(2) 0.3767(2) -0.1063(3) 0.0348(12) Uani 1 1 d . . .
O3 O -0.1366(2) 0.3169(2) -0.1045(3) 0.0339(12) Uani 1 1 d . . .
O4 O -0.09013(18) 0.37141(17) 0.0283(3) 0.0249(10) Uani 1 1 d . . .
O5 O 0.01149(17) 0.40042(17) 0.0289(3) 0.0234(10) Uani 1 1 d . . .
O6 O -0.02202(17) 0.32503(17) -0.0942(3) 0.0241(10) Uani 1 1 d . . .
O7 O -0.05809(17) 0.23326(17) -0.0655(3) 0.0237(10) Uani 1 1 d . . .
O8 O 0.01791(17) 0.37736(17) 0.1964(3) 0.0240(10) Uani 1 1 d . . .
O9 O -0.08251(18) 0.34724(18) 0.1969(3) 0.0255(10) Uani 1 1 d . . .
O10 O -0.01538(16) 0.30203(16) 0.0658(3) 0.0192(9) Uani 1 1 d . . .
O1W O 0.9845(2) 0.4747(2) 0.9158(4) 0.0459(15) Uani 1 1 d . . .
C1 C 0.9770(6) 0.4138(5) 0.7261(9) 0.096(5) Uani 1 1 d . . .
H1A H 1.0089 0.4075 0.7567 0.115 Uiso 1 1 calc R . .
H1B H 0.9746 0.3874 0.6833 0.115 Uiso 1 1 calc R . .
C2 C 0.9803(6) 0.4614(4) 0.6896(9) 0.091(5) Uani 1 1 d . . .
H2A H 0.9604 0.4604 0.6387 0.109 Uiso 1 1 calc R . .
H2B H 1.0165 0.4677 0.6750 0.109 Uiso 1 1 calc R . .
C3 C 0.8531(5) 0.4953(4) 0.9712(8) 0.076(3) Uani 1 1 d . . .
H3A H 0.8807 0.4987 1.0120 0.091 Uiso 1 1 calc R . .
H3B H 0.8207 0.4882 1.0000 0.091 Uiso 1 1 calc R . .
C4 C 0.8483(4) 0.5442(4) 0.9242(8) 0.068(3) Uani 1 1 d . . .
H4A H 0.8163 0.5437 0.8922 0.082 Uiso 1 1 calc R . .
H4B H 0.8468 0.5735 0.9620 0.082 Uiso 1 1 calc R . .
N1 N 0.9322(3) 0.4076(3) 0.7828(5) 0.051(2) Uani 1 1 d . . .
H1C H 0.9406 0.3857 0.8243 0.062 Uiso 1 1 calc R . .
H1D H 0.9046 0.3941 0.7555 0.062 Uiso 1 1 calc R . .
N2 N 0.9619(3) 0.5054(3) 0.7386(4) 0.0482(19) Uani 1 1 d . . .
H2C H 0.9446 0.5281 0.7062 0.058 Uiso 1 1 calc R . .
H2D H 0.9893 0.5222 0.7614 0.058 Uiso 1 1 calc R . .
N3 N 0.8652(3) 0.4522(3) 0.9152(5) 0.0490(19) Uani 1 1 d . . .
H3C H 0.8357 0.4402 0.8917 0.059 Uiso 1 1 calc R . .
H3D H 0.8802 0.4258 0.9433 0.059 Uiso 1 1 calc R . .
N4 N 0.8930(3) 0.5501(3) 0.8690(4) 0.0405(17) Uani 1 1 d . . .
H4C H 0.9198 0.5651 0.8962 0.049 Uiso 1 1 calc R . .
H4D H 0.8844 0.5707 0.8261 0.049 Uiso 1 1 calc R . .
O2W O 0.8771(3) 0.5358(3) 0.1788(6) 0.088(3) Uani 1 1 d U . .
O3W O 0.1916(4) 0.3451(5) 0.9244(7) 0.130(4) Uani 1 1 d . . .
O4W O 1.0931(9) 0.3264(6) 0.7416(8) 0.094(6) Uani 0.50 1 d P . .
O5W O 0.7829(6) 0.3750(7) 0.8311(12) 0.083(5) Uani 0.50 1 d P . .
O6W O 0.8530(8) 0.2644(7) 0.7516(11) 0.094(5) Uani 0.50 1 d PU . .
O7W O 0.8323(6) 0.4832(7) 0.7199(11) 0.185(6) Uani 1 1 d U . .
O8W O 0.1023(8) 0.3895(8) 0.6046(12) 0.100(6) Uani 0.50 1 d PU . .
O9W O 0.7713(10) 0.1919(10) 0.7764(16) 0.140(9) Uani 0.50 1 d PU . .


_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
Cu1 N3 2.005(7) . ?
Cu1 N1 2.012(7) . ?
Cu1 N2 2.016(7) . ?
Cu1 N4 2.024(7) . ?
Cu1 O1W 2.297(6) . ?
As1 O10 1.688(4) 2 ?
As1 O10 1.688(4) 15 ?
As1 O10 1.688(4) 16 ?
As1 O10 1.688(4) . ?
Nb1 O1 1.756(5) . ?
Nb1 O9 1.946(5) . ?
Nb1 O8 1.967(5) . ?
Nb1 O4 1.995(5) . ?
Nb1 O5 2.017(5) . ?
Nb1 O10 2.463(4) . ?
Nb2 O2 1.759(5) . ?
Nb2 O9 1.892(5) 15 ?
Nb2 O5 1.907(5) . ?
Nb2 O6 2.097(5) . ?
Nb2 O7 2.115(5) 2 ?
Nb2 O10 2.439(4) . ?
Nb2 Sb1 3.2891(7) . ?
Nb3 O3 1.760(5) . ?
Nb3 O8 1.890(5) 16 ?
Nb3 O4 1.912(5) . ?
Nb3 O6 2.104(5) . ?
Nb3 O7 2.111(5) . ?
Nb3 O10 2.427(4) . ?
Nb3 Sb1 3.3011(7) . ?
Sb1 O7 2.009(5) . ?
Sb1 O7 2.009(5) 2 ?
Sb1 O6 2.162(5) 2 ?
Sb1 O6 2.162(5) . ?
Sb1 Nb2 3.2891(7) 2 ?
Sb1 Nb3 3.3010(7) 2 ?
O7 Nb2 2.115(5) 2 ?
O8 Nb3 1.890(5) 15 ?
O9 Nb2 1.892(5) 16 ?
C1 C2 1.356(16) . ?
C1 N1 1.479(14) . ?
C2 N2 1.456(13) . ?
C3 N3 1.462(14) . ?
C3 C4 1.470(14) . ?
C4 N4 1.459(12) . ?

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
N3 Cu1 N1 95.5(3) . . ?
N3 Cu1 N2 178.7(3) . . ?
N1 Cu1 N2 84.8(3) . . ?
N3 Cu1 N4 84.6(3) . . ?
N1 Cu1 N4 177.0(3) . . ?
N2 Cu1 N4 95.1(3) . . ?
N3 Cu1 O1W 92.3(3) . . ?
N1 Cu1 O1W 90.4(3) . . ?
N2 Cu1 O1W 89.0(3) . . ?
N4 Cu1 O1W 92.6(3) . . ?
O10 As1 O10 108.83(15) 2 15 ?
O10 As1 O10 108.83(15) 2 16 ?
O10 As1 O10 110.8(3) 15 16 ?
O10 As1 O10 110.8(3) 2 . ?
O10 As1 O10 108.82(15) 15 . ?
O10 As1 O10 108.82(15) 16 . ?
O1 Nb1 O9 102.7(2) . . ?
O1 Nb1 O8 100.6(2) . . ?
O9 Nb1 O8 86.62(19) . . ?
O1 Nb1 O4 102.2(2) . . ?
O9 Nb1 O4 90.8(2) . . ?
O8 Nb1 O4 157.04(19) . . ?
O1 Nb1 O5 101.0(2) . . ?
O9 Nb1 O5 156.24(19) . . ?
O8 Nb1 O5 88.42(19) . . ?
O4 Nb1 O5 84.82(19) . . ?
O1 Nb1 O10 172.2(2) . . ?
O9 Nb1 O10 83.71(17) . . ?
O8 Nb1 O10 83.96(17) . . ?
O4 Nb1 O10 73.08(16) . . ?
O5 Nb1 O10 72.66(16) . . ?
O2 Nb2 O9 102.5(2) . 15 ?
O2 Nb2 O5 103.9(2) . . ?
O9 Nb2 O5 96.2(2) 15 . ?
O2 Nb2 O6 99.9(2) . . ?
O9 Nb2 O6 153.01(18) 15 . ?
O5 Nb2 O6 92.90(19) . . ?
O2 Nb2 O7 98.9(2) . 2 ?
O9 Nb2 O7 86.21(19) 15 2 ?
O5 Nb2 O7 155.99(19) . 2 ?
O6 Nb2 O7 75.51(17) . 2 ?
O2 Nb2 O10 171.0(2) . . ?
O9 Nb2 O10 86.51(17) 15 . ?
O5 Nb2 O10 74.99(17) . . ?
O6 Nb2 O10 71.41(16) . . ?
O7 Nb2 O10 81.34(16) 2 . ?
O2 Nb2 Sb1 96.49(18) . . ?
O9 Nb2 Sb1 121.50(14) 15 . ?
O5 Nb2 Sb1 131.78(14) . . ?
O6 Nb2 Sb1 40.16(12) . . ?
O7 Nb2 Sb1 36.00(12) 2 . ?
O10 Nb2 Sb1 78.33(10) . . ?
O3 Nb3 O8 103.2(2) . 16 ?
O3 Nb3 O4 100.6(2) . . ?
O8 Nb3 O4 96.9(2) 16 . ?
O3 Nb3 O6 99.0(2) . . ?
O8 Nb3 O6 154.01(18) 16 . ?
O4 Nb3 O6 92.16(19) . . ?
O3 Nb3 O7 101.4(2) . . ?
O8 Nb3 O7 87.29(19) 16 . ?
O4 Nb3 O7 156.00(19) . . ?
O6 Nb3 O7 75.05(17) . . ?
O3 Nb3 O10 169.3(2) . . ?
O8 Nb3 O10 87.27(17) 16 . ?
O4 Nb3 O10 75.27(17) . . ?
O6 Nb3 O10 71.55(16) . . ?
O7 Nb3 O10 81.37(16) . . ?
O3 Nb3 Sb1 97.88(18) . . ?
O8 Nb3 Sb1 122.33(14) 16 . ?
O4 Nb3 Sb1 130.90(14) . . ?
O6 Nb3 Sb1 39.93(12) . . ?
O7 Nb3 Sb1 35.70(12) . . ?
O10 Nb3 Sb1 78.24(10) . . ?
O7 Sb1 O7 100.8(3) . 2 ?
O7 Sb1 O6 76.31(17) . 2 ?
O7 Sb1 O6 75.90(17) 2 2 ?
O7 Sb1 O6 75.90(17) . . ?
O7 Sb1 O6 76.31(17) 2 . ?
O6 Sb1 O6 135.7(3) 2 . ?
O7 Sb1 Nb2 38.23(13) . 2 ?
O7 Sb1 Nb2 93.15(13) 2 2 ?
O6 Sb1 Nb2 38.74(12) 2 2 ?
O6 Sb1 Nb2 110.37(12) . 2 ?
O7 Sb1 Nb2 93.15(13) . . ?
O7 Sb1 Nb2 38.23(13) 2 . ?
O6 Sb1 Nb2 110.37(12) 2 . ?
O6 Sb1 Nb2 38.74(12) . . ?
Nb2 Sb1 Nb2 110.06(3) 2 . ?
O7 Sb1 Nb3 93.22(13) . 2 ?
O7 Sb1 Nb3 37.83(13) 2 2 ?
O6 Sb1 Nb3 38.67(12) 2 2 ?
O6 Sb1 Nb3 110.31(13) . 2 ?
Nb2 Sb1 Nb3 66.349(17) 2 2 ?
Nb2 Sb1 Nb3 75.016(18) . 2 ?
O7 Sb1 Nb3 37.83(13) . . ?
O7 Sb1 Nb3 93.22(13) 2 . ?
O6 Sb1 Nb3 110.31(13) 2 . ?
O6 Sb1 Nb3 38.67(12) . . ?
Nb2 Sb1 Nb3 75.016(18) 2 . ?
Nb2 Sb1 Nb3 66.350(17) . . ?
Nb3 Sb1 Nb3 109.73(3) 2 . ?
Nb3 O4 Nb1 122.4(2) . . ?
Nb2 O5 Nb1 122.9(2) . . ?
Nb2 O6 Nb3 118.3(2) . . ?
Nb2 O6 Sb1 101.10(19) . . ?
Nb3 O6 Sb1 101.40(18) . . ?
Sb1 O7 Nb3 106.5(2) . . ?
Sb1 O7 Nb2 105.8(2) . 2 ?
Nb3 O7 Nb2 143.4(2) . 2 ?
Nb3 O8 Nb1 153.7(3) 15 . ?
Nb2 O9 Nb1 156.0(3) 16 . ?
As1 O10 Nb3 124.3(2) . . ?
As1 O10 Nb2 124.0(2) . . ?
Nb3 O10 Nb2 95.66(16) . . ?
As1 O10 Nb1 124.5(2) . . ?
Nb3 O10 Nb1 88.89(14) . . ?
Nb2 O10 Nb1 89.35(14) . . ?
C2 C1 N1 114.6(10) . . ?
C1 C2 N2 116.0(11) . . ?
N3 C3 C4 109.8(10) . . ?
N4 C4 C3 109.9(8) . . ?
C1 N1 Cu1 107.8(6) . . ?
C2 N2 Cu1 108.8(6) . . ?
C3 N3 Cu1 108.4(6) . . ?
C4 N4 Cu1 108.5(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.238
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.164
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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_shelx
_audit_block_doi                 10.5517/cc13dvcq
_database_code_depnum_ccdc_archive 'CCDC 1025243'
_audit_update_record             
;
2014-11-18 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(H Nb12 O40 Sb2 Ge), 9(C4 H16 Cu N4), 17(H2 O)'
_chemical_formula_sum            'C36 H180 Cu9 Ge2 N36 Nb24 O97 Sb4'
_chemical_formula_weight         6104.04

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'
Cu Cu 0.3201 1.2651 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.8930(8)
_cell_length_b                   39.874(2)
_cell_length_c                   19.3320(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.0520(10)
_cell_angle_gamma                90.00
_cell_volume                     11435.6(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5874
_exptl_absorpt_coefficient_mu    2.759
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            78111
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         27.24
_reflns_number_total             25520
_reflns_number_gt                16441
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. The ISOR instruction was 
 used on atoms of c15 c16 c15' c16' c13 c14 c1 c2 c3 c4 because of the 
ADP 
 or NPD Alert. The Anis instruction was not used on atoms O7w and the 
 occupancy of atoms O6w O7w is changed because of the 
ADP or NPD Alert. 
 17 H2O molecules is add to molecular formula based on Elemental Analysis 
 and Thermogravimetric Analysis.

;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.010 0.000 -0.001 2210 1475 ' '
2 -0.071 0.500 0.429 2210 1480 ' '
_platon_squeeze_details          
;
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1104P)²+31.1482P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         25520
_refine_ls_number_parameters     928
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.2111
_refine_ls_wR_factor_gt          0.1960
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.59298(5) 0.126984(19) 0.27255(4) 0.01626(17) Uani 1 1 d . . .
Nb1 Nb 0.59622(6) 0.059945(19) 0.39830(4) 0.03082(19) Uani 1 1 d . . .
Nb2 Nb 0.77500(6) 0.06473(2) 0.30211(4) 0.0316(2) Uani 1 1 d . . .
Nb3 Nb 0.75659(5) 0.124884(19) 0.42274(4) 0.02486(17) Uani 1 1 d . . .
Nb4 Nb 0.60484(6) 0.06031(2) 0.14629(4) 0.03172(19) Uani 1 1 d . . .
Nb5 Nb 0.42539(6) 0.059814(19) 0.24263(4) 0.02952(19) Uani 1 1 d . . .
Nb6 Nb 0.42959(5) 0.120645(18) 0.12248(4) 0.02394(17) Uani 1 1 d . . .
Nb7 Nb 0.78718(5) 0.13414(2) 0.17302(4) 0.02666(18) Uani 1 1 d . . .
Nb8 Nb 0.76285(5) 0.194172(18) 0.29200(4) 0.02279(17) Uani 1 1 d . . .
Nb9 Nb 0.61265(5) 0.194153(18) 0.15065(4) 0.02305(17) Uani 1 1 d . . .
Nb10 Nb 0.55930(5) 0.193237(18) 0.39417(4) 0.02256(17) Uani 1 1 d . . .
Nb11 Nb 0.39702(5) 0.128128(19) 0.37189(4) 0.02538(17) Uani 1 1 d . . .
Nb12 Nb 0.40944(5) 0.189161(18) 0.25274(4) 0.02195(16) Uani 1 1 d . . .
Sb1 Sb 0.56354(4) 0.126734(15) 0.49311(3) 0.03132(15) Uani 1 1 d . . .
Sb2 Sb 0.62086(4) 0.127801(15) 0.05154(3) 0.03174(15) Uani 1 1 d . . .
Cu1 Cu 0.83181(9) 0.25124(4) 0.01999(7) 0.0510(4) Uani 1 1 d . . .
Cu2 Cu 0.32993(8) 0.24622(3) 0.02278(6) 0.0422(3) Uani 1 1 d . . .
Cu3 Cu 0.32133(10) 0.99632(4) 0.45006(8) 0.0595(4) Uani 1 1 d . . .
Cu4 Cu 0.09077(8) 0.12661(4) 0.27512(7) 0.0487(4) Uani 1 1 d . . .
Cu5 Cu 0.5000 0.0000 0.0000 0.0839(8) Uani 1 2 d S . .
O1 O 0.5697(5) 0.03057(16) 0.4608(3) 0.0422(17) Uani 1 1 d . . .
O2 O 0.8655(5) 0.03642(19) 0.2932(4) 0.056(2) Uani 1 1 d . . .
O3 O 0.8218(4) 0.13537(17) 0.5009(3) 0.0394(16) Uani 1 1 d . . .
O4 O 0.6367(5) 0.03197(15) 0.0813(4) 0.0437(17) Uani 1 1 d . . .
O5 O 0.3447(5) 0.02787(17) 0.2515(4) 0.0490(19) Uani 1 1 d . . .
O6 O 0.3618(5) 0.12886(16) 0.0444(3) 0.0412(16) Uani 1 1 d . . .
O7 O 0.8752(4) 0.12547(19) 0.1183(4) 0.0470(18) Uani 1 1 d . . .
O8 O 0.8376(4) 0.22522(16) 0.3246(3) 0.0394(16) Uani 1 1 d . . .
O9 O 0.5933(4) 0.22263(14) 0.0801(3) 0.0318(14) Uani 1 1 d . . .
O10 O 0.5729(4) 0.22233(15) 0.4645(3) 0.0331(14) Uani 1 1 d . . .
O11 O 0.3132(5) 0.11700(18) 0.4267(3) 0.0422(16) Uani 1 1 d . . .
O12 O 0.3269(4) 0.21831(15) 0.2209(3) 0.0339(14) Uani 1 1 d . . .
O13 O 0.6995(4) 0.03864(14) 0.3656(3) 0.0354(15) Uani 1 1 d . . .
O14 O 0.8261(4) 0.08948(15) 0.3881(3) 0.0323(14) Uani 1 1 d . . .
O15 O 0.6689(4) 0.09177(14) 0.4680(3) 0.0298(13) Uani 1 1 d . . .
O16 O 0.5059(5) 0.03628(15) 0.1798(3) 0.0380(16) Uani 1 1 d . . .
O17 O 0.3708(4) 0.08207(15) 0.1572(3) 0.0321(14) Uani 1 1 d . . .
O18 O 0.5232(4) 0.09073(15) 0.0772(3) 0.0296(13) Uani 1 1 d . . .
O19 O 0.8393(4) 0.17126(15) 0.2260(3) 0.0302(13) Uani 1 1 d . . .
O20 O 0.7086(4) 0.16524(14) 0.1045(3) 0.0255(12) Uani 1 1 d . . .
O21 O 0.7033(4) 0.21764(14) 0.2080(3) 0.0283(13) Uani 1 1 d . . .
O22 O 0.4698(4) 0.16129(14) 0.4401(3) 0.0272(13) Uani 1 1 d . . .
O23 O 0.4649(4) 0.21420(13) 0.3366(3) 0.0250(12) Uani 1 1 d . . .
O24 O 0.3398(4) 0.16382(15) 0.3198(3) 0.0281(13) Uani 1 1 d . . .
O25 O 0.5026(4) 0.09821(14) 0.4189(3) 0.0260(12) Uani 1 1 d . . .
O26 O 0.5133(4) 0.04877(14) 0.3213(3) 0.0338(14) Uani 1 1 d . . .
O27 O 0.6897(4) 0.05112(14) 0.2235(3) 0.0342(15) Uani 1 1 d . . .
O28 O 0.8118(4) 0.10163(14) 0.2445(3) 0.0318(14) Uani 1 1 d . . .
O29 O 0.7890(4) 0.15872(14) 0.3612(3) 0.0267(13) Uani 1 1 d . . .
O30 O 0.6420(4) 0.15473(14) 0.4391(3) 0.0264(13) Uani 1 1 d . . .
O31 O 0.3795(4) 0.09536(14) 0.3015(3) 0.0300(14) Uani 1 1 d . . .
O32 O 0.6895(4) 0.10161(14) 0.1266(3) 0.0303(14) Uani 1 1 d . . .
O33 O 0.6554(4) 0.20477(13) 0.3422(3) 0.0240(12) Uani 1 1 d . . .
O34 O 0.5367(3) 0.15365(13) 0.1063(3) 0.0225(12) Uani 1 1 d . . .
O35 O 0.3893(4) 0.15326(14) 0.1838(3) 0.0257(12) Uani 1 1 d . . .
O36 O 0.5128(4) 0.20286(14) 0.2026(3) 0.0244(12) Uani 1 1 d . . .
O37 O 0.6581(3) 0.10244(13) 0.3322(3) 0.0208(11) Uani 1 1 d . . .
O38 O 0.5333(4) 0.10060(13) 0.2130(3) 0.0215(12) Uani 1 1 d . . .
O39 O 0.6657(3) 0.15395(13) 0.2317(3) 0.0202(11) Uani 1 1 d . . .
O40 O 0.5151(3) 0.15166(13) 0.3127(3) 0.0187(11) Uani 1 1 d . . .
C1 C 0.9101(14) 0.2565(5) 0.1578(10) 0.122(7) Uani 1 1 d U . .
H1A H 0.8716 0.2667 0.1898 0.146 Uiso 1 1 calc R . .
H1B H 0.9561 0.2439 0.1855 0.146 Uiso 1 1 calc R . .
C2 C 0.9538(12) 0.2827(5) 0.1234(9) 0.105(6) Uani 1 1 d U . .
H2A H 1.0160 0.2765 0.1191 0.126 Uiso 1 1 calc R . .
H2B H 0.9537 0.3030 0.1512 0.126 Uiso 1 1 calc R . .
C3 C 0.7154(14) 0.2208(5) -0.0830(11) 0.124(7) Uani 1 1 d U . .
H3A H 0.7139 0.2007 -0.1112 0.149 Uiso 1 1 calc R . .
H3B H 0.6534 0.2272 -0.0780 0.149 Uiso 1 1 calc R . .
C4 C 0.7545(12) 0.2457(4) -0.1183(9) 0.099(5) Uani 1 1 d U . .
H4A H 0.7077 0.2572 -0.1474 0.119 Uiso 1 1 calc R . .
H4B H 0.7952 0.2356 -0.1488 0.119 Uiso 1 1 calc R . .
C5 C 0.4432(8) 0.2922(3) 0.1033(6) 0.056(3) Uani 1 1 d . . .
H5A H 0.4990 0.2951 0.1324 0.068 Uiso 1 1 calc R . .
H5B H 0.3989 0.3077 0.1187 0.068 Uiso 1 1 calc R . .
C6 C 0.4583(8) 0.2990(3) 0.0285(7) 0.062(3) Uani 1 1 d . . .
H6A H 0.4719 0.3226 0.0221 0.075 Uiso 1 1 calc R . .
H6B H 0.5083 0.2858 0.0147 0.075 Uiso 1 1 calc R . .
C7 C 0.2075(9) 0.1930(3) 0.0173(6) 0.063(3) Uani 1 1 d . . .
H7A H 0.1563 0.2052 0.0323 0.076 Uiso 1 1 calc R . .
H7B H 0.1960 0.1692 0.0225 0.076 Uiso 1 1 calc R . .
C8 C 0.2168(8) 0.2007(3) -0.0585(6) 0.059(3) Uani 1 1 d . . .
H8A H 0.2609 0.1859 -0.0765 0.071 Uiso 1 1 calc R . .
H8B H 0.1595 0.1975 -0.0856 0.071 Uiso 1 1 calc R . .
C9 C 0.3166(12) 0.9411(4) 0.3561(8) 0.091(5) Uani 1 1 d . . .
H9A H 0.3135 0.9168 0.3517 0.109 Uiso 1 1 calc R . .
H9B H 0.2871 0.9508 0.3140 0.109 Uiso 1 1 calc R . .
C10 C 0.4105(11) 0.9515(3) 0.3637(8) 0.079(4) Uani 1 1 d . . .
H10A H 0.4379 0.9477 0.3207 0.095 Uiso 1 1 calc R . .
H10B H 0.4434 0.9386 0.4002 0.095 Uiso 1 1 calc R . .
C11 C 0.2399(11) 1.0409(4) 0.5440(9) 0.097(6) Uani 1 1 d . . .
H11A H 0.2063 1.0557 0.5114 0.116 Uiso 1 1 calc R . .
H11B H 0.2156 1.0430 0.5887 0.116 Uiso 1 1 calc R . .
C12 C 0.3340(11) 1.0500(4) 0.5501(8) 0.086(5) Uani 1 1 d . . .
H12A H 0.3660 1.0380 0.5884 0.103 Uiso 1 1 calc R . .
H12B H 0.3407 1.0739 0.5587 0.103 Uiso 1 1 calc R . .
C13 C 0.0985(18) 0.0791(6) 0.1598(14) 0.170(10) Uani 1 1 d U . .
H13A H 0.1345 0.0610 0.1815 0.204 Uiso 1 1 calc R A .
H13B H 0.0706 0.0713 0.1154 0.204 Uiso 1 1 calc R . .
C14 C 0.1585(15) 0.1109(6) 0.1497(12) 0.138(8) Uani 1 1 d U A .
H14A H 0.2073 0.1054 0.1216 0.166 Uiso 1 1 calc R . .
H14B H 0.1226 0.1287 0.1270 0.166 Uiso 1 1 calc R . .
C17 C 0.5355(19) 0.0478(5) -0.1010(12) 0.142(9) Uani 1 1 d . . .
H17A H 0.5707 0.0642 -0.0732 0.171 Uiso 1 1 calc R . .
H17B H 0.5455 0.0513 -0.1494 0.171 Uiso 1 1 calc R . .
C18 C 0.4400(16) 0.0515(5) -0.0912(12) 0.126(8) Uani 1 1 d . . .
H18A H 0.4038 0.0372 -0.1233 0.151 Uiso 1 1 calc R . .
H18B H 0.4209 0.0745 -0.0986 0.151 Uiso 1 1 calc R . .
N1 N 0.8561(6) 0.2328(3) 0.1152(5) 0.071(3) Uani 1 1 d . . .
H1C H 0.8037 0.2291 0.1338 0.085 Uiso 1 1 calc R . .
H1D H 0.8856 0.2132 0.1135 0.085 Uiso 1 1 calc R . .
N2 N 0.9091(7) 0.2894(3) 0.0545(5) 0.063(3) Uani 1 1 d . . .
H2C H 0.9511 0.2933 0.0247 0.076 Uiso 1 1 calc R . .
H2D H 0.8751 0.3080 0.0562 0.076 Uiso 1 1 calc R . .
N3 N 0.7570(7) 0.2129(3) -0.0164(5) 0.072(3) Uani 1 1 d . . .
H3C H 0.7918 0.1946 -0.0190 0.086 Uiso 1 1 calc R . .
H3D H 0.7145 0.2083 0.0127 0.086 Uiso 1 1 calc R . .
N4 N 0.8035(8) 0.2701(3) -0.0757(5) 0.078(4) Uani 1 1 d . . .
H4C H 0.7704 0.2889 -0.0735 0.094 Uiso 1 1 calc R . .
H4D H 0.8550 0.2754 -0.0943 0.094 Uiso 1 1 calc R . .
N5 N 0.4112(6) 0.2580(2) 0.1088(5) 0.049(2) Uani 1 1 d . . .
H5C H 0.3806 0.2559 0.1467 0.059 Uiso 1 1 calc R . .
H5D H 0.4584 0.2438 0.1132 0.059 Uiso 1 1 calc R . .
N6 N 0.3733(6) 0.2897(2) -0.0138(5) 0.052(2) Uani 1 1 d . . .
H6C H 0.3837 0.2875 -0.0588 0.063 Uiso 1 1 calc R . .
H6D H 0.3314 0.3058 -0.0106 0.063 Uiso 1 1 calc R . .
N7 N 0.2856(7) 0.2019(2) 0.0599(4) 0.050(2) Uani 1 1 d . . .
H7C H 0.3281 0.1859 0.0582 0.060 Uiso 1 1 calc R . .
H7D H 0.2726 0.2042 0.1042 0.060 Uiso 1 1 calc R . .
N8 N 0.2458(6) 0.2357(2) -0.0626(4) 0.045(2) Uani 1 1 d . . .
H8C H 0.1977 0.2494 -0.0645 0.054 Uiso 1 1 calc R . .
H8D H 0.2745 0.2389 -0.1012 0.054 Uiso 1 1 calc R . .
N9 N 0.2680(7) 0.9519(2) 0.4176(6) 0.067(3) Uani 1 1 d . . .
H9C H 0.2755 0.9366 0.4518 0.080 Uiso 1 1 calc R . .
H9D H 0.2086 0.9542 0.4052 0.080 Uiso 1 1 calc R . .
N10 N 0.4133(7) 0.9878(2) 0.3815(5) 0.059(3) Uani 1 1 d . . .
H10C H 0.4004 1.0002 0.3430 0.070 Uiso 1 1 calc R . .
H10D H 0.4687 0.9935 0.4002 0.070 Uiso 1 1 calc R . .
N11 N 0.2312(7) 1.0054(2) 0.5192(5) 0.064(3) Uani 1 1 d . . .
H11C H 0.1751 1.0019 0.4992 0.076 Uiso 1 1 calc R . .
H11D H 0.2408 0.9914 0.5554 0.076 Uiso 1 1 calc R . .
N12 N 0.3730(8) 1.0406(2) 0.4806(6) 0.071(3) Uani 1 1 d . . .
H12C H 0.4335 1.0393 0.4868 0.086 Uiso 1 1 calc R . .
H12D H 0.3580 1.0563 0.4482 0.086 Uiso 1 1 calc R . .
N13 N 0.0237(12) 0.0909(4) 0.2086(9) 0.149(7) Uani 1 1 d . A .
H13C H 0.0041 0.0736 0.2330 0.179 Uiso 1 1 calc R . .
H13D H -0.0236 0.1002 0.1835 0.179 Uiso 1 1 calc R . .
N14 N 0.1920(7) 0.1207(3) 0.2152(6) 0.080(4) Uani 1 1 d . A .
H14C H 0.2224 0.1401 0.2127 0.096 Uiso 1 1 calc R . .
H14D H 0.2305 0.1050 0.2338 0.096 Uiso 1 1 calc R . .
N15 N -0.0138(7) 0.1320(3) 0.3309(6) 0.072(3) Uani 0.60 1 d P A 1
H15A H -0.0633 0.1368 0.3025 0.086 Uiso 0.60 1 calc PR A 1
H15B H -0.0236 0.1127 0.3530 0.086 Uiso 0.60 1 calc PR A 1
C15 C 0.0015(13) 0.1578(6) 0.3797(11) 0.064(6) Uani 0.60 1 d PU A 1
H15C H -0.0243 0.1512 0.4220 0.077 Uiso 0.60 1 calc PR A 1
H15D H -0.0305 0.1776 0.3621 0.077 Uiso 0.60 1 calc PR A 1
C16 C 0.101(2) 0.1672(9) 0.3981(17) 0.121(11) Uani 0.60 1 d PU A 1
H16A H 0.1041 0.1890 0.4203 0.145 Uiso 0.60 1 calc PR A 1
H16B H 0.1284 0.1509 0.4306 0.145 Uiso 0.60 1 calc PR A 1
N16 N 0.1516(9) 0.1680(4) 0.3330(8) 0.055(4) Uani 0.60 1 d P A 1
H16C H 0.2111 0.1648 0.3432 0.066 Uiso 0.60 1 calc PR A 1
H16D H 0.1428 0.1875 0.3098 0.066 Uiso 0.60 1 calc PR A 1
N15' N -0.0138(7) 0.1320(3) 0.3309(6) 0.072(3) Uani 0.40 1 d PD A 2
H15E H -0.0303 0.1537 0.3330 0.086 Uiso 0.40 1 calc PR A 2
H15F H -0.0612 0.1198 0.3132 0.086 Uiso 0.40 1 calc PR A 2
C15' C 0.021(4) 0.1195(15) 0.3993(16) 0.19(3) Uiso 0.40 1 d PD A 2
H15G H 0.0579 0.1372 0.4212 0.232 Uiso 0.40 1 calc PR A 2
H15H H -0.0307 0.1171 0.4263 0.232 Uiso 0.40 1 calc PR A 2
C16' C 0.073(3) 0.0886(14) 0.408(3) 0.17(3) Uiso 0.40 1 d PD A 2
H16E H 0.0344 0.0696 0.3951 0.209 Uiso 0.40 1 calc PR A 2
H16F H 0.0950 0.0860 0.4566 0.209 Uiso 0.40 1 calc PR A 2
N16' N 0.1490(8) 0.0893(3) 0.3651(7) 0.105(4) Uani 0.40 1 d PD A 2
H16G H 0.1606 0.0688 0.3483 0.127 Uiso 0.40 1 calc PR A 2
H16H H 0.1991 0.0975 0.3885 0.127 Uiso 0.40 1 calc PR A 2
O6W O 0.1490(8) 0.0893(3) 0.3651(7) 0.105(4) Uani 0.60 1 d P A 3
N17 N 0.5634(10) 0.0125(3) -0.0787(7) 0.108(5) Uani 1 1 d . . .
H17C H 0.6233 0.0117 -0.0672 0.130 Uiso 1 1 calc R . .
H17D H 0.5500 -0.0020 -0.1139 0.130 Uiso 1 1 calc R . .
N18 N 0.4308(10) 0.0411(3) -0.0176(7) 0.094(4) Uani 1 1 d . . .
H18C H 0.3724 0.0374 -0.0112 0.112 Uiso 1 1 calc R . .
H18D H 0.4519 0.0573 0.0119 0.112 Uiso 1 1 calc R . .
O1W O 0.6918(7) 0.2803(2) 0.0566(6) 0.096(3) Uani 1 1 d U . .
O2W O 0.9730(7) 0.2204(3) 0.9726(7) 0.106(4) Uani 1 1 d . . .
O3W O 0.4664(5) 0.2149(2) 0.9703(4) 0.070(3) Uani 1 1 d . . .
O4W O 0.1977(5) 0.2791(2) 0.0752(4) 0.065(2) Uani 1 1 d . . .
O5W O 0.2112(8) 0.0249(3) 0.3416(7) 0.118(4) Uani 1 1 d . . .
O7W O 0.0267(14) 0.1779(5) 0.1985(11) 0.090(6) Uiso 0.50 1 d P . .


_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
Ge1 O37 1.741(5) . ?
Ge1 O38 1.744(5) . ?
Ge1 O40 1.753(5) . ?
Ge1 O39 1.762(5) . ?
Nb1 O1 1.753(6) . ?
Nb1 O26 1.902(6) . ?
Nb1 O13 1.912(6) . ?
Nb1 O15 2.083(6) . ?
Nb1 O25 2.128(6) . ?
Nb1 O37 2.358(5) . ?
Nb1 Sb1 3.2932(11) . ?
Nb2 O2 1.779(7) . ?
Nb2 O28 1.952(6) . ?
Nb2 O27 1.970(6) . ?
Nb2 O14 2.023(6) . ?
Nb2 O13 2.025(6) . ?
Nb2 O37 2.410(5) . ?
Nb3 O3 1.772(6) . ?
Nb3 O29 1.889(6) . ?
Nb3 O14 1.906(6) . ?
Nb3 O15 2.102(6) . ?
Nb3 O30 2.127(5) . ?
Nb3 O37 2.358(5) . ?
Nb3 Sb1 3.2880(10) . ?
Nb4 O4 1.785(6) . ?
Nb4 O27 1.904(6) . ?
Nb4 O16 1.918(7) . ?
Nb4 O18 2.109(6) . ?
Nb4 O32 2.128(6) . ?
Nb4 O38 2.370(5) . ?
Nb4 Sb2 3.2760(10) . ?
Nb5 O5 1.769(7) . ?
Nb5 O26 1.966(6) . ?
Nb5 O31 1.976(6) . ?
Nb5 O17 1.985(6) . ?
Nb5 O16 2.012(7) . ?
Nb5 O38 2.392(5) . ?
Nb6 O6 1.770(6) . ?
Nb6 O35 1.892(6) . ?
Nb6 O17 1.919(6) . ?
Nb6 O18 2.085(6) . ?
Nb6 O34 2.113(5) . ?
Nb6 O38 2.369(5) . ?
Nb6 Sb2 3.2810(10) . ?
Nb7 O7 1.789(7) . ?
Nb7 O28 1.907(6) . ?
Nb7 O19 1.924(6) . ?
Nb7 O32 2.091(6) . ?
Nb7 O20 2.094(5) . ?
Nb7 O39 2.354(5) . ?
Nb7 Sb2 3.2695(10) . ?
Nb8 O8 1.745(6) . ?
Nb8 O29 1.962(6) . ?
Nb8 O33 1.989(5) . ?
Nb8 O19 2.003(6) . ?
Nb8 O21 2.011(6) . ?
Nb8 O39 2.393(5) . ?
Nb9 O9 1.778(6) . ?
Nb9 O36 1.897(6) . ?
Nb9 O21 1.915(5) . ?
Nb9 O20 2.096(5) . ?
Nb9 O34 2.110(5) . ?
Nb9 O39 2.330(5) . ?
Nb9 Sb2 3.2753(10) . ?
Nb10 O10 1.785(6) . ?
Nb10 O33 1.877(6) . ?
Nb10 O23 1.908(5) . ?
Nb10 O22 2.097(6) . ?
Nb10 O30 2.107(5) . ?
Nb10 O40 2.341(5) . ?
Nb10 Sb1 3.2669(10) . ?
Nb11 O11 1.763(7) . ?
Nb11 O31 1.888(6) . ?
Nb11 O24 1.901(6) . ?
Nb11 O22 2.101(6) . ?
Nb11 O25 2.114(6) . ?
Nb11 O40 2.374(5) . ?
Nb11 Sb1 3.2591(9) . ?
Nb12 O12 1.763(6) . ?
Nb12 O35 1.961(6) . ?
Nb12 O36 1.968(5) . ?
Nb12 O24 2.003(6) . ?
Nb12 O23 2.017(5) . ?
Nb12 O40 2.394(5) . ?
Sb1 O30 1.979(6) . ?
Sb1 O25 1.987(5) . ?
Sb1 O22 2.155(6) . ?
Sb1 O15 2.185(6) . ?
Sb2 O32 1.995(6) . ?
Sb2 O34 1.996(5) . ?
Sb2 O18 2.162(6) . ?
Sb2 O20 2.179(6) . ?
Cu1 N3 1.985(11) . ?
Cu1 N1 1.985(9) . ?
Cu1 N2 1.989(10) . ?
Cu1 N4 2.007(9) . ?
Cu2 N6 2.001(9) . ?
Cu2 N5 2.024(9) . ?
Cu2 N8 2.026(8) . ?
Cu2 N7 2.040(8) . ?
Cu3 N12 1.993(10) . ?
Cu3 N11 2.008(11) . ?
Cu3 N9 2.017(10) . ?
Cu3 N10 2.017(11) . ?
Cu4 N15 1.982(11) . ?
Cu4 N14 1.995(10) . ?
Cu4 N13 2.108(16) . ?
Cu4 N16 2.149(16) . ?
Cu4 N16' 2.393(13) . ?
Cu5 N17 1.925(15) . ?
Cu5 N17 1.925(15) 3_655 ?
Cu5 N18 1.948(13) 3_655 ?
Cu5 N18 1.948(13) . ?
C1 C2 1.43(2) . ?
C1 N1 1.448(19) . ?
C2 N2 1.459(18) . ?
C3 C4 1.36(2) . ?
C3 N3 1.42(2) . ?
C4 N4 1.431(18) . ?
C5 N5 1.452(14) . ?
C5 C6 1.507(16) . ?
C6 N6 1.493(14) . ?
C7 N7 1.409(14) . ?
C7 C8 1.514(16) . ?
C8 N8 1.468(14) . ?
C9 C10 1.45(2) . ?
C9 N9 1.510(19) . ?
C10 N10 1.490(15) . ?
C11 C12 1.44(2) . ?
C11 N11 1.494(18) . ?
C12 N12 1.554(18) . ?
C13 C14 1.57(3) . ?
C13 N13 1.59(3) . ?
C14 N14 1.38(2) . ?
C17 C18 1.46(3) . ?
C17 N17 1.52(2) . ?
C18 N18 1.50(2) . ?
N15 C15 1.40(2) . ?
C15 C16 1.53(3) . ?
C16 N16 1.53(3) . ?
C15' C16' 1.459(10) . ?
C16' N16' 1.466(10) . ?

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
O37 Ge1 O38 108.6(3) . . ?
O37 Ge1 O40 112.0(2) . . ?
O38 Ge1 O40 108.2(2) . . ?
O37 Ge1 O39 108.1(2) . . ?
O38 Ge1 O39 111.7(2) . . ?
O40 Ge1 O39 108.2(2) . . ?
O1 Nb1 O26 102.3(3) . . ?
O1 Nb1 O13 99.6(3) . . ?
O26 Nb1 O13 97.1(3) . . ?
O1 Nb1 O15 95.6(3) . . ?
O26 Nb1 O15 156.0(2) . . ?
O13 Nb1 O15 95.6(3) . . ?
O1 Nb1 O25 99.2(3) . . ?
O26 Nb1 O25 85.6(2) . . ?
O13 Nb1 O25 160.0(2) . . ?
O15 Nb1 O25 75.8(2) . . ?
O1 Nb1 O37 167.5(2) . . ?
O26 Nb1 O37 90.1(2) . . ?
O13 Nb1 O37 77.1(2) . . ?
O15 Nb1 O37 73.0(2) . . ?
O25 Nb1 O37 83.1(2) . . ?
O1 Nb1 Sb1 95.9(2) . . ?
O26 Nb1 Sb1 120.49(19) . . ?
O13 Nb1 Sb1 134.88(19) . . ?
O15 Nb1 Sb1 40.65(17) . . ?
O25 Nb1 Sb1 35.38(14) . . ?
O37 Nb1 Sb1 78.72(13) . . ?
O2 Nb2 O28 99.8(3) . . ?
O2 Nb2 O27 101.1(3) . . ?
O28 Nb2 O27 87.8(3) . . ?
O2 Nb2 O14 99.0(3) . . ?
O28 Nb2 O14 89.8(2) . . ?
O27 Nb2 O14 159.9(2) . . ?
O2 Nb2 O13 101.5(3) . . ?
O28 Nb2 O13 158.7(2) . . ?
O27 Nb2 O13 88.4(3) . . ?
O14 Nb2 O13 86.6(3) . . ?
O2 Nb2 O37 171.6(3) . . ?
O28 Nb2 O37 85.0(2) . . ?
O27 Nb2 O37 85.9(2) . . ?
O14 Nb2 O37 74.0(2) . . ?
O13 Nb2 O37 73.9(2) . . ?
O3 Nb3 O29 102.5(3) . . ?
O3 Nb3 O14 101.5(3) . . ?
O29 Nb3 O14 97.5(3) . . ?
O3 Nb3 O15 96.2(3) . . ?
O29 Nb3 O15 156.0(2) . . ?
O14 Nb3 O15 93.3(3) . . ?
O3 Nb3 O30 97.4(3) . . ?
O29 Nb3 O30 86.9(2) . . ?
O14 Nb3 O30 159.1(2) . . ?
O15 Nb3 O30 75.7(2) . . ?
O3 Nb3 O37 168.6(3) . . ?
O29 Nb3 O37 88.9(2) . . ?
O14 Nb3 O37 77.3(2) . . ?
O15 Nb3 O37 72.6(2) . . ?
O30 Nb3 O37 82.4(2) . . ?
O3 Nb3 Sb1 94.3(2) . . ?
O29 Nb3 Sb1 121.70(17) . . ?
O14 Nb3 Sb1 133.11(19) . . ?
O15 Nb3 Sb1 40.86(16) . . ?
O30 Nb3 Sb1 35.28(15) . . ?
O37 Nb3 Sb1 78.82(13) . . ?
O4 Nb4 O27 103.3(3) . . ?
O4 Nb4 O16 100.5(3) . . ?
O27 Nb4 O16 96.6(3) . . ?
O4 Nb4 O18 95.3(3) . . ?
O27 Nb4 O18 155.9(2) . . ?
O16 Nb4 O18 94.8(3) . . ?
O4 Nb4 O32 99.6(3) . . ?
O27 Nb4 O32 85.8(2) . . ?
O16 Nb4 O32 158.7(2) . . ?
O18 Nb4 O32 76.1(2) . . ?
O4 Nb4 O38 166.4(3) . . ?
O27 Nb4 O38 90.2(2) . . ?
O16 Nb4 O38 76.1(2) . . ?
O18 Nb4 O38 72.1(2) . . ?
O32 Nb4 O38 82.8(2) . . ?
O4 Nb4 Sb2 95.1(2) . . ?
O27 Nb4 Sb2 121.35(19) . . ?
O16 Nb4 Sb2 134.05(19) . . ?
O18 Nb4 Sb2 40.52(16) . . ?
O32 Nb4 Sb2 36.00(15) . . ?
O38 Nb4 Sb2 78.80(13) . . ?
O5 Nb5 O26 100.1(3) . . ?
O5 Nb5 O31 100.9(3) . . ?
O26 Nb5 O31 87.5(2) . . ?
O5 Nb5 O17 99.8(3) . . ?
O26 Nb5 O17 159.9(2) . . ?
O31 Nb5 O17 91.2(2) . . ?
O5 Nb5 O16 99.7(3) . . ?
O26 Nb5 O16 88.3(3) . . ?
O31 Nb5 O16 159.4(2) . . ?
O17 Nb5 O16 85.9(3) . . ?
O5 Nb5 O38 171.5(3) . . ?
O26 Nb5 O38 85.5(2) . . ?
O31 Nb5 O38 85.6(2) . . ?
O17 Nb5 O38 74.4(2) . . ?
O16 Nb5 O38 74.0(2) . . ?
O6 Nb6 O35 102.6(3) . . ?
O6 Nb6 O17 101.7(3) . . ?
O35 Nb6 O17 98.8(3) . . ?
O6 Nb6 O18 95.7(3) . . ?
O35 Nb6 O18 156.5(2) . . ?
O17 Nb6 O18 91.7(3) . . ?
O6 Nb6 O34 98.0(3) . . ?
O35 Nb6 O34 87.2(2) . . ?
O17 Nb6 O34 157.6(2) . . ?
O18 Nb6 O34 75.7(2) . . ?
O6 Nb6 O38 167.9(3) . . ?
O35 Nb6 O38 89.5(2) . . ?
O17 Nb6 O38 76.1(2) . . ?
O18 Nb6 O38 72.6(2) . . ?
O34 Nb6 O38 82.40(19) . . ?
O6 Nb6 Sb2 94.5(2) . . ?
O35 Nb6 Sb2 122.48(17) . . ?
O17 Nb6 Sb2 130.91(19) . . ?
O18 Nb6 Sb2 40.28(16) . . ?
O34 Nb6 Sb2 35.80(14) . . ?
O38 Nb6 Sb2 78.71(13) . . ?
O7 Nb7 O28 101.1(3) . . ?
O7 Nb7 O19 100.5(3) . . ?
O28 Nb7 O19 95.4(2) . . ?
O7 Nb7 O32 98.3(3) . . ?
O28 Nb7 O32 88.4(2) . . ?
O19 Nb7 O32 159.7(2) . . ?
O7 Nb7 O20 97.9(3) . . ?
O28 Nb7 O20 157.2(2) . . ?
O19 Nb7 O20 93.3(2) . . ?
O32 Nb7 O20 76.5(2) . . ?
O7 Nb7 O39 169.6(3) . . ?
O28 Nb7 O39 89.2(2) . . ?
O19 Nb7 O39 77.1(2) . . ?
O32 Nb7 O39 83.1(2) . . ?
O20 Nb7 O39 72.29(19) . . ?
O7 Nb7 Sb2 96.2(2) . . ?
O28 Nb7 Sb2 123.61(18) . . ?
O19 Nb7 Sb2 133.34(17) . . ?
O32 Nb7 Sb2 35.86(16) . . ?
O20 Nb7 Sb2 41.06(16) . . ?
O39 Nb7 Sb2 78.84(12) . . ?
O8 Nb8 O29 100.5(3) . . ?
O8 Nb8 O33 100.8(3) . . ?
O29 Nb8 O33 86.6(2) . . ?
O8 Nb8 O19 100.0(3) . . ?
O29 Nb8 O19 90.9(2) . . ?
O33 Nb8 O19 159.1(2) . . ?
O8 Nb8 O21 100.6(3) . . ?
O29 Nb8 O21 158.9(2) . . ?
O33 Nb8 O21 88.8(2) . . ?
O19 Nb8 O21 86.1(2) . . ?
O8 Nb8 O39 172.0(3) . . ?
O29 Nb8 O39 85.7(2) . . ?
O33 Nb8 O39 84.4(2) . . ?
O19 Nb8 O39 74.7(2) . . ?
O21 Nb8 O39 73.4(2) . . ?
O9 Nb9 O36 101.9(3) . . ?
O9 Nb9 O21 101.0(3) . . ?
O36 Nb9 O21 98.6(2) . . ?
O9 Nb9 O20 95.5(3) . . ?
O36 Nb9 O20 157.1(2) . . ?
O21 Nb9 O20 92.5(2) . . ?
O9 Nb9 O34 97.6(2) . . ?
O36 Nb9 O34 86.5(2) . . ?
O21 Nb9 O34 159.3(2) . . ?
O20 Nb9 O34 76.5(2) . . ?
O9 Nb9 O39 167.7(2) . . ?
O36 Nb9 O39 90.3(2) . . ?
O21 Nb9 O39 76.5(2) . . ?
O20 Nb9 O39 72.8(2) . . ?
O34 Nb9 O39 83.38(19) . . ?
O9 Nb9 Sb2 94.5(2) . . ?
O36 Nb9 Sb2 121.91(17) . . ?
O21 Nb9 Sb2 132.30(18) . . ?
O20 Nb9 Sb2 40.95(16) . . ?
O34 Nb9 Sb2 35.91(14) . . ?
O39 Nb9 Sb2 79.02(13) . . ?
O10 Nb10 O33 102.0(3) . . ?
O10 Nb10 O23 100.8(3) . . ?
O33 Nb10 O23 97.9(2) . . ?
O10 Nb10 O22 96.1(3) . . ?
O33 Nb10 O22 156.7(2) . . ?
O23 Nb10 O22 92.9(2) . . ?
O10 Nb10 O30 97.9(2) . . ?
O33 Nb10 O30 87.3(2) . . ?
O23 Nb10 O30 159.0(2) . . ?
O22 Nb10 O30 75.7(2) . . ?
O10 Nb10 O40 168.2(2) . . ?
O33 Nb10 O40 89.8(2) . . ?
O23 Nb10 O40 76.6(2) . . ?
O22 Nb10 O40 72.7(2) . . ?
O30 Nb10 O40 83.1(2) . . ?
O10 Nb10 Sb1 95.0(2) . . ?
O33 Nb10 Sb1 122.41(17) . . ?
O23 Nb10 Sb1 132.26(17) . . ?
O22 Nb10 Sb1 40.44(16) . . ?
O30 Nb10 Sb1 35.59(16) . . ?
O40 Nb10 Sb1 78.98(12) . . ?
O11 Nb11 O31 101.5(3) . . ?
O11 Nb11 O24 101.5(3) . . ?
O31 Nb11 O24 96.3(3) . . ?
O11 Nb11 O22 97.7(3) . . ?
O31 Nb11 O22 156.8(2) . . ?
O24 Nb11 O22 92.5(2) . . ?
O11 Nb11 O25 98.0(3) . . ?
O31 Nb11 O25 88.2(2) . . ?
O24 Nb11 O25 158.7(2) . . ?
O22 Nb11 O25 76.2(2) . . ?
O11 Nb11 O40 169.2(3) . . ?
O31 Nb11 O40 89.3(2) . . ?
O24 Nb11 O40 76.4(2) . . ?
O22 Nb11 O40 72.0(2) . . ?
O25 Nb11 O40 82.85(19) . . ?
O11 Nb11 Sb1 95.6(2) . . ?
O31 Nb11 Sb1 123.67(18) . . ?
O24 Nb11 Sb1 132.13(17) . . ?
O22 Nb11 Sb1 40.63(16) . . ?
O25 Nb11 Sb1 36.03(15) . . ?
O40 Nb11 Sb1 78.72(12) . . ?
O12 Nb12 O35 100.6(3) . . ?
O12 Nb12 O36 101.3(3) . . ?
O35 Nb12 O36 87.0(2) . . ?
O12 Nb12 O24 100.0(3) . . ?
O35 Nb12 O24 90.8(2) . . ?
O36 Nb12 O24 158.6(2) . . ?
O12 Nb12 O23 100.2(2) . . ?
O35 Nb12 O23 159.2(2) . . ?
O36 Nb12 O23 88.6(2) . . ?
O24 Nb12 O23 85.9(2) . . ?
O12 Nb12 O40 171.5(2) . . ?
O35 Nb12 O40 85.9(2) . . ?
O36 Nb12 O40 84.4(2) . . ?
O24 Nb12 O40 74.2(2) . . ?
O23 Nb12 O40 73.46(19) . . ?
O30 Sb1 O25 101.2(2) . . ?
O30 Sb1 O22 77.1(2) . . ?
O25 Sb1 O22 77.7(2) . . ?
O30 Sb1 O15 76.9(2) . . ?
O25 Sb1 O15 76.4(2) . . ?
O22 Sb1 O15 138.6(2) . . ?
O30 Sb1 Nb11 93.32(16) . . ?
O25 Sb1 Nb11 38.75(16) . . ?
O22 Sb1 Nb11 39.41(15) . . ?
O15 Sb1 Nb11 111.52(14) . . ?
O30 Sb1 Nb10 38.28(16) . . ?
O25 Sb1 Nb10 93.31(16) . . ?
O22 Sb1 Nb10 39.14(15) . . ?
O15 Sb1 Nb10 111.41(15) . . ?
Nb11 Sb1 Nb10 65.85(2) . . ?
O30 Sb1 Nb3 38.37(16) . . ?
O25 Sb1 Nb3 92.79(17) . . ?
O22 Sb1 Nb3 111.78(15) . . ?
O15 Sb1 Nb3 38.99(15) . . ?
Nb11 Sb1 Nb3 109.92(3) . . ?
Nb10 Sb1 Nb3 75.43(2) . . ?
O30 Sb1 Nb1 92.25(16) . . ?
O25 Sb1 Nb1 38.33(17) . . ?
O22 Sb1 Nb1 111.95(15) . . ?
O15 Sb1 Nb1 38.39(15) . . ?
Nb11 Sb1 Nb1 75.76(2) . . ?
Nb10 Sb1 Nb1 109.07(3) . . ?
Nb3 Sb1 Nb1 64.79(2) . . ?
O32 Sb2 O34 100.9(2) . . ?
O32 Sb2 O18 77.7(2) . . ?
O34 Sb2 O18 76.4(2) . . ?
O32 Sb2 O20 76.6(2) . . ?
O34 Sb2 O20 77.0(2) . . ?
O18 Sb2 O20 138.4(2) . . ?
O32 Sb2 Nb7 37.88(17) . . ?
O34 Sb2 Nb7 92.90(15) . . ?
O18 Sb2 Nb7 111.74(15) . . ?
O20 Sb2 Nb7 39.14(14) . . ?
O32 Sb2 Nb9 92.30(17) . . ?
O34 Sb2 Nb9 38.31(15) . . ?
O18 Sb2 Nb9 110.94(15) . . ?
O20 Sb2 Nb9 39.07(14) . . ?
Nb7 Sb2 Nb9 65.31(2) . . ?
O32 Sb2 Nb4 38.83(17) . . ?
O34 Sb2 Nb4 92.74(16) . . ?
O18 Sb2 Nb4 39.32(15) . . ?
O20 Sb2 Nb4 111.72(14) . . ?
Nb7 Sb2 Nb4 75.51(2) . . ?
Nb9 Sb2 Nb4 109.16(3) . . ?
O32 Sb2 Nb6 93.33(18) . . ?
O34 Sb2 Nb6 38.27(15) . . ?
O18 Sb2 Nb6 38.57(16) . . ?
O20 Sb2 Nb6 111.71(14) . . ?
Nb7 Sb2 Nb6 109.70(3) . . ?
Nb9 Sb2 Nb6 75.35(2) . . ?
Nb4 Sb2 Nb6 65.55(2) . . ?
N3 Cu1 N1 95.4(4) . . ?
N3 Cu1 N2 178.4(4) . . ?
N1 Cu1 N2 85.3(4) . . ?
N3 Cu1 N4 84.0(4) . . ?
N1 Cu1 N4 178.3(4) . . ?
N2 Cu1 N4 95.2(4) . . ?
N6 Cu2 N5 84.4(3) . . ?
N6 Cu2 N8 94.9(3) . . ?
N5 Cu2 N8 178.1(3) . . ?
N6 Cu2 N7 179.9(4) . . ?
N5 Cu2 N7 95.8(4) . . ?
N8 Cu2 N7 84.9(3) . . ?
N12 Cu3 N11 84.6(5) . . ?
N12 Cu3 N9 179.0(4) . . ?
N11 Cu3 N9 95.6(5) . . ?
N12 Cu3 N10 94.4(4) . . ?
N11 Cu3 N10 178.9(4) . . ?
N9 Cu3 N10 85.4(4) . . ?
N15 Cu4 N14 177.4(4) . . ?
N15 Cu4 N13 93.0(6) . . ?
N14 Cu4 N13 84.7(6) . . ?
N15 Cu4 N16 87.1(5) . . ?
N14 Cu4 N16 95.0(5) . . ?
N13 Cu4 N16 172.2(7) . . ?
N15 Cu4 N16' 85.7(5) . . ?
N14 Cu4 N16' 96.0(5) . . ?
N13 Cu4 N16' 98.4(6) . . ?
N16 Cu4 N16' 89.4(5) . . ?
N17 Cu5 N17 179.997(2) . 3_655 ?
N17 Cu5 N18 93.8(6) . 3_655 ?
N17 Cu5 N18 86.2(6) 3_655 3_655 ?
N17 Cu5 N18 86.2(6) . . ?
N17 Cu5 N18 93.8(6) 3_655 . ?
N18 Cu5 N18 179.998(2) 3_655 . ?
Nb1 O13 Nb2 118.6(3) . . ?
Nb3 O14 Nb2 118.3(3) . . ?
Nb1 O15 Nb3 114.8(3) . . ?
Nb1 O15 Sb1 101.0(2) . . ?
Nb3 O15 Sb1 100.2(2) . . ?
Nb4 O16 Nb5 119.2(3) . . ?
Nb6 O17 Nb5 118.9(3) . . ?
Nb6 O18 Nb4 115.7(3) . . ?
Nb6 O18 Sb2 101.1(2) . . ?
Nb4 O18 Sb2 100.2(2) . . ?
Nb7 O19 Nb8 117.7(3) . . ?
Nb7 O20 Nb9 114.9(2) . . ?
Nb7 O20 Sb2 99.8(2) . . ?
Nb9 O20 Sb2 100.0(2) . . ?
Nb9 O21 Nb8 118.6(3) . . ?
Nb10 O22 Nb11 115.4(3) . . ?
Nb10 O22 Sb1 100.4(2) . . ?
Nb11 O22 Sb1 100.0(2) . . ?
Nb10 O23 Nb12 118.7(3) . . ?
Nb11 O24 Nb12 119.2(3) . . ?
Sb1 O25 Nb11 105.2(3) . . ?
Sb1 O25 Nb1 106.3(2) . . ?
Nb11 O25 Nb1 143.0(3) . . ?
Nb1 O26 Nb5 153.5(3) . . ?
Nb4 O27 Nb2 152.9(3) . . ?
Nb7 O28 Nb2 151.6(3) . . ?
Nb3 O29 Nb8 153.9(3) . . ?
Sb1 O30 Nb10 106.1(2) . . ?
Sb1 O30 Nb3 106.3(2) . . ?
Nb10 O30 Nb3 142.6(3) . . ?
Nb11 O31 Nb5 151.5(3) . . ?
Sb2 O32 Nb7 106.3(3) . . ?
Sb2 O32 Nb4 105.2(3) . . ?
Nb7 O32 Nb4 143.5(3) . . ?
Nb10 O33 Nb8 153.3(3) . . ?
Sb2 O34 Nb9 105.8(2) . . ?
Sb2 O34 Nb6 105.9(2) . . ?
Nb9 O34 Nb6 143.2(3) . . ?
Nb6 O35 Nb12 152.8(3) . . ?
Nb9 O36 Nb12 153.3(3) . . ?
Ge1 O37 Nb1 122.8(3) . . ?
Ge1 O37 Nb3 123.5(3) . . ?
Nb1 O37 Nb3 96.78(19) . . ?
Ge1 O37 Nb2 124.2(3) . . ?
Nb1 O37 Nb2 90.45(17) . . ?
Nb3 O37 Nb2 90.04(17) . . ?
Ge1 O38 Nb6 123.0(3) . . ?
Ge1 O38 Nb4 122.8(3) . . ?
Nb6 O38 Nb4 97.00(18) . . ?
Ge1 O38 Nb5 124.5(3) . . ?
Nb6 O38 Nb5 89.88(18) . . ?
Nb4 O38 Nb5 90.76(17) . . ?
Ge1 O39 Nb9 122.4(2) . . ?
Ge1 O39 Nb7 122.7(3) . . ?
Nb9 O39 Nb7 97.9(2) . . ?
Ge1 O39 Nb8 124.0(3) . . ?
Nb9 O39 Nb8 91.22(18) . . ?
Nb7 O39 Nb8 90.16(18) . . ?
Ge1 O40 Nb10 122.5(2) . . ?
Ge1 O40 Nb11 122.6(3) . . ?
Nb10 O40 Nb11 97.57(19) . . ?
Ge1 O40 Nb12 124.6(3) . . ?
Nb10 O40 Nb12 90.99(18) . . ?
Nb11 O40 Nb12 89.84(17) . . ?
C2 C1 N1 117.7(16) . . ?
C1 C2 N2 111.7(15) . . ?
C4 C3 N3 116.5(17) . . ?
C3 C4 N4 115.1(16) . . ?
N5 C5 C6 108.6(10) . . ?
N6 C6 C5 106.8(10) . . ?
N7 C7 C8 112.0(10) . . ?
N8 C8 C7 107.3(10) . . ?
C10 C9 N9 111.2(12) . . ?
C9 C10 N10 108.0(13) . . ?
C12 C11 N11 108.6(12) . . ?
C11 C12 N12 107.6(14) . . ?
C14 C13 N13 105.5(19) . . ?
N14 C14 C13 106.2(19) . . ?
C18 C17 N17 107.5(17) . . ?
C17 C18 N18 105.6(18) . . ?
C1 N1 Cu1 109.5(10) . . ?
C2 N2 Cu1 111.7(9) . . ?
C3 N3 Cu1 109.7(11) . . ?
C4 N4 Cu1 109.4(9) . . ?
C5 N5 Cu2 109.5(6) . . ?
C6 N6 Cu2 107.8(7) . . ?
C7 N7 Cu2 106.7(7) . . ?
C8 N8 Cu2 108.4(6) . . ?
C9 N9 Cu3 107.1(8) . . ?
C10 N10 Cu3 107.9(8) . . ?
C11 N11 Cu3 110.0(8) . . ?
C12 N12 Cu3 107.8(8) . . ?
C13 N13 Cu4 104.1(14) . . ?
C14 N14 Cu4 109.7(11) . . ?
C15 N15 Cu4 111.0(10) . . ?
N15 C15 C16 115.5(19) . . ?
N16 C16 C15 111(2) . . ?
C16 N16 Cu4 101.2(15) . . ?
C15' C16' N16' 110(4) . . ?
C16' N16' Cu4 100(2) . . ?
C17 N17 Cu5 108.8(13) . . ?
C18 N18 Cu5 107.8(11) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.24
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.045
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.234
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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_shelx
_audit_block_doi                 10.5517/cc13qs0m
_database_code_depnum_ccdc_archive 'CCDC 1034780'
_audit_update_record             
;
2014-11-18 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Nb12 O39 Sb2 Ge, 4(C4 H16 Cu N4), 6(H2 O)'
_chemical_formula_sum            'C16 H76 Cu4 N16 Nb12 O45 Sb2 Ge'
_chemical_formula_weight         2898.10

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'
Cu Cu 0.3201 1.2651 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   13.8690(6)
_cell_length_b                   14.6210(6)
_cell_length_c                   22.1360(9)
_cell_angle_alpha                84.6380(10)
_cell_angle_beta                 80.6320(10)
_cell_angle_gamma                62.3180(10)
_cell_volume                     3921.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2772
_exptl_absorpt_coefficient_mu    3.882
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29267
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         28.31
_reflns_number_total             19381
_reflns_number_gt                15413
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. The ISOR instruction was 
 used on atoms of C2 N4 N2 because of the 
ADP or NPD Alert. The Anis 
 instruction was not used on atoms O5w O6w O7w O8w O9w O10w O11w 
 O12w because of the 
 ADP or NPD Alert. The occupancy of water molecules 
 is changed based on Elemental Analysis and Thermogravimetric Analysis.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0822P)²+38.6019P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         19381
_refine_ls_number_parameters     889
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1612
_refine_ls_wR_factor_gt          0.1485
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.05013(12) 0.61340(11) 0.78685(8) 0.0568(4) Uani 1 1 d . . .
Cu2 Cu -0.44300(10) 1.56212(8) 0.80002(5) 0.0343(3) Uani 1 1 d . . .
Cu3 Cu 0.32993(11) 0.95607(10) 0.54363(5) 0.0379(3) Uani 1 1 d . . .
Cu4 Cu 0.05960(12) 0.11501(12) 0.83752(7) 0.0527(4) Uani 1 1 d . . .
Ge1 Ge -0.44105(6) 1.09195(5) 0.79047(3) 0.01241(14) Uani 1 1 d . . .
Nb1 Nb -0.51203(5) 0.92921(5) 0.89556(3) 0.01377(12) Uani 1 1 d . . .
Nb2 Nb -0.49973(5) 0.88589(5) 0.74819(3) 0.01697(13) Uani 1 1 d . . .
Nb3 Nb -0.25652(5) 0.81283(5) 0.80322(3) 0.01745(13) Uani 1 1 d . . .
Nb4 Nb -0.70148(5) 1.16607(5) 0.73806(3) 0.01852(14) Uani 1 1 d . . .
Nb5 Nb -0.71274(5) 1.21370(5) 0.88390(3) 0.01714(13) Uani 1 1 d . . .
Nb6 Nb -0.63936(6) 1.36204(5) 0.78084(3) 0.01895(14) Uani 1 1 d . . .
Nb7 Nb -0.41001(6) 1.04124(5) 0.62975(3) 0.01840(14) Uani 1 1 d . . .
Nb8 Nb -0.34725(6) 1.23319(5) 0.66992(3) 0.02020(14) Uani 1 1 d . . .
Nb9 Nb -0.17458(6) 0.97878(5) 0.68779(3) 0.02120(14) Uani 1 1 d . . .
Nb10 Nb -0.44462(5) 1.14755(5) 0.94195(3) 0.01471(13) Uani 1 1 d . . .
Nb11 Nb -0.18534(5) 1.03512(5) 0.85140(3) 0.01835(13) Uani 1 1 d . . .
Nb12 Nb -0.36979(6) 1.28856(5) 0.83539(3) 0.01863(14) Uani 1 1 d . . .
Sb1 Sb -0.28285(4) 0.89732(4) 0.94086(2) 0.01935(11) Uani 1 1 d . . .
Sb2 Sb -0.59436(5) 1.28684(4) 0.64022(2) 0.02328(12) Uani 1 1 d . . .
O1 O -0.4573(4) 1.1354(4) 1.0298(2) 0.0177(10) Uani 1 1 d . . .
O2 O -0.5452(5) 0.8096(5) 0.7155(3) 0.0290(13) Uani 1 1 d . . .
O3 O -0.1444(5) 0.6903(4) 0.8128(3) 0.0295(13) Uani 1 1 d . . .
O4 O -0.7996(5) 1.1813(5) 0.6921(3) 0.0337(14) Uani 1 1 d . . .
O5 O -0.8214(5) 1.2480(5) 0.9442(3) 0.0295(13) Uani 1 1 d . . .
O6 O -0.7099(5) 1.4950(4) 0.7640(3) 0.0322(13) Uani 1 1 d . . .
O7 O -0.4356(5) 1.0272(5) 0.5560(2) 0.0283(12) Uani 1 1 d . . .
O8 O -0.3361(6) 1.3320(5) 0.6222(3) 0.0351(14) Uani 1 1 d . . .
O9 O -0.0371(5) 0.9081(5) 0.6544(3) 0.0351(14) Uani 1 1 d . . .
O11 O -0.0520(5) 0.9778(5) 0.8709(3) 0.0345(14) Uani 1 1 d . . .
O12 O -0.3560(5) 1.4008(4) 0.8446(3) 0.0278(12) Uani 1 1 d . . .
O13 O -0.5434(4) 0.8625(4) 0.8396(2) 0.0193(10) Uani 1 1 d . . .
O14 O -0.3484(4) 0.7786(4) 0.7629(2) 0.0201(10) Uani 1 1 d . . .
O15 O -0.3456(4) 0.8201(4) 0.8897(2) 0.0181(10) Uani 1 1 d . . .
O16 O -0.7858(4) 1.1990(4) 0.8184(2) 0.0217(11) Uani 1 1 d . . .
O17 O -0.7348(4) 1.3507(4) 0.8522(2) 0.0238(11) Uani 1 1 d . . .
O18 O -0.7110(4) 1.3155(4) 0.7215(2) 0.0207(11) Uani 1 1 d . . .
O19 O -0.4203(5) 1.1882(4) 0.6114(2) 0.0221(11) Uani 1 1 d . . .
O20 O -0.2072(5) 1.1198(4) 0.6516(3) 0.0251(11) Uani 1 1 d . . .
O21 O -0.2534(4) 0.9684(4) 0.6210(2) 0.0234(11) Uani 1 1 d . . .
O22 O -0.4227(5) 1.2642(4) 0.9262(2) 0.0213(11) Uani 1 1 d . . .
O23 O -0.2765(4) 1.0413(4) 0.9368(2) 0.0178(10) Uani 1 1 d . . .
O24 O -0.2248(4) 1.1803(4) 0.8526(3) 0.0238(11) Uani 1 1 d . . .
O25 O -0.6357(4) 1.0569(4) 0.8964(2) 0.0190(10) Uani 1 1 d . . .
O26 O -0.6300(4) 1.0197(4) 0.7525(2) 0.0232(11) Uani 1 1 d . . .
O27 O -0.4374(5) 0.9371(4) 0.6766(2) 0.0216(11) Uani 1 1 d . . .
O28 O -0.2003(5) 0.8679(4) 0.7337(2) 0.0232(11) Uani 1 1 d . . .
O29 O -0.2145(4) 0.9021(4) 0.8549(2) 0.0208(10) Uani 1 1 d . . .
O30 O -0.4380(4) 1.0019(4) 0.9344(2) 0.0163(10) Uani 1 1 d . . .
O31 O -0.5895(4) 1.2032(4) 0.9285(2) 0.0212(11) Uani 1 1 d . . .
O32 O -0.1580(5) 1.0203(5) 0.7649(3) 0.0267(12) Uani 1 1 d . . .
O33 O -0.5731(4) 1.1453(4) 0.6662(2) 0.0215(11) Uani 1 1 d . . .
O34 O -0.5219(5) 1.3146(4) 0.7013(2) 0.0221(11) Uani 1 1 d . . .
O35 O -0.3320(5) 1.2687(4) 0.7482(2) 0.0246(11) Uani 1 1 d . . .
O36 O -0.5255(5) 1.3512(4) 0.8228(2) 0.0229(11) Uani 1 1 d . . .
O37 O -0.4313(4) 0.9676(4) 0.8089(2) 0.0149(9) Uani 1 1 d . . .
O38 O -0.5802(4) 1.1810(4) 0.7961(2) 0.0162(10) Uani 1 1 d . . .
O39 O -0.3695(4) 1.0888(4) 0.7177(2) 0.0166(10) Uani 1 1 d . . .
O40 O -0.3839(4) 1.1289(4) 0.8432(2) 0.0156(9) Uani 1 1 d . . .
C1 C 0.1197(13) 0.6094(12) 0.9029(10) 0.092(6) Uani 1 1 d . . .
H1A H 0.1984 0.5829 0.8919 0.110 Uiso 1 1 calc R . .
H1B H 0.1035 0.6021 0.9469 0.110 Uiso 1 1 calc R . .
C2 C 0.0599(16) 0.7200(14) 0.8824(10) 0.098(5) Uani 1 1 d U . .
H2A H -0.0153 0.7490 0.9026 0.117 Uiso 1 1 calc R . .
H2B H 0.0940 0.7582 0.8955 0.117 Uiso 1 1 calc R . .
C3 C 0.0109(14) 0.5230(17) 0.6963(8) 0.093(6) Uani 1 1 d . . .
H3A H 0.0284 0.4632 0.6727 0.112 Uiso 1 1 calc R . .
H3B H -0.0685 0.5619 0.7044 0.112 Uiso 1 1 calc R . .
C4 C 0.0513(14) 0.5818(16) 0.6635(8) 0.092(5) Uani 1 1 d . . .
H4A H 0.0147 0.6092 0.6274 0.110 Uiso 1 1 calc R . .
H4B H 0.1292 0.5406 0.6503 0.110 Uiso 1 1 calc R . .
C5 C -0.6298(11) 1.6550(11) 0.8909(7) 0.064(4) Uani 1 1 d . . .
H5A H -0.6840 1.6453 0.9208 0.077 Uiso 1 1 calc R . .
H5B H -0.6635 1.7252 0.8747 0.077 Uiso 1 1 calc R . .
C6 C -0.5330(11) 1.6367(11) 0.9205(6) 0.058(3) Uani 1 1 d . . .
H6A H -0.5537 1.6907 0.9495 0.070 Uiso 1 1 calc R . .
H6B H -0.5068 1.5709 0.9425 0.070 Uiso 1 1 calc R . .
C7 C -0.3961(11) 1.5582(8) 0.6709(5) 0.052(3) Uani 1 1 d . . .
H7A H -0.4349 1.6326 0.6655 0.063 Uiso 1 1 calc R . .
H7B H -0.3856 1.5266 0.6322 0.063 Uiso 1 1 calc R . .
C8 C -0.2859(11) 1.5265(10) 0.6922(6) 0.061(3) Uani 1 1 d . . .
H8A H -0.2432 1.4518 0.6924 0.073 Uiso 1 1 calc R . .
H8B H -0.2447 1.5557 0.6650 0.073 Uiso 1 1 calc R . .
C9 C 0.4357(11) 0.7357(9) 0.5488(5) 0.055(3) Uani 1 1 d . . .
H9A H 0.4126 0.7223 0.5910 0.066 Uiso 1 1 calc R . .
H9B H 0.4626 0.6729 0.5261 0.066 Uiso 1 1 calc R . .
C10 C 0.5231(10) 0.7659(8) 0.5460(5) 0.047(3) Uani 1 1 d . . .
H10A H 0.5537 0.7701 0.5038 0.057 Uiso 1 1 calc R . .
H10B H 0.5815 0.7156 0.5680 0.057 Uiso 1 1 calc R . .
C11 C 0.1471(10) 1.1521(10) 0.5289(6) 0.059(3) Uani 1 1 d . . .
H11A H 0.1043 1.1646 0.5693 0.071 Uiso 1 1 calc R . .
H11B H 0.1005 1.1986 0.4998 0.071 Uiso 1 1 calc R . .
C12 C 0.2446(10) 1.1710(10) 0.5287(6) 0.056(3) Uani 1 1 d . . .
H12A H 0.2807 1.1698 0.4872 0.068 Uiso 1 1 calc R . .
H12B H 0.2217 1.2378 0.5459 0.068 Uiso 1 1 calc R . .
C13 C 0.1285(17) 0.0324(14) 0.9524(8) 0.104(7) Uani 1 1 d . . .
H13A H 0.1840 0.0473 0.9642 0.125 Uiso 1 1 calc R . .
H13B H 0.0942 0.0121 0.9893 0.125 Uiso 1 1 calc R . .
C14 C 0.1819(12) -0.0533(12) 0.9121(7) 0.075(4) Uani 1 1 d . . .
H14A H 0.1417 -0.0935 0.9183 0.090 Uiso 1 1 calc R . .
H14B H 0.2554 -0.0974 0.9222 0.090 Uiso 1 1 calc R . .
C15 C -0.0635(12) 0.2795(10) 0.7618(7) 0.068(4) Uani 1 1 d . . .
H15A H -0.1336 0.3369 0.7547 0.082 Uiso 1 1 calc R . .
H15B H -0.0059 0.2990 0.7463 0.082 Uiso 1 1 calc R . .
C16 C -0.0455(10) 0.1885(11) 0.7304(6) 0.057(3) Uani 1 1 d . . .
H16A H -0.1107 0.1781 0.7393 0.068 Uiso 1 1 calc R . .
H16B H -0.0318 0.1985 0.6865 0.068 Uiso 1 1 calc R . .
N1 N 0.0779(8) 0.5549(8) 0.8701(5) 0.063(3) Uani 1 1 d . . .
H1C H 0.0150 0.5590 0.8915 0.076 Uiso 1 1 calc R . .
H1D H 0.1272 0.4877 0.8674 0.076 Uiso 1 1 calc R . .
N2 N 0.0588(12) 0.7344(10) 0.8173(7) 0.088(4) Uani 1 1 d U . .
H2C H 0.1203 0.7372 0.7990 0.106 Uiso 1 1 calc R . .
H2D H 0.0004 0.7938 0.8089 0.106 Uiso 1 1 calc R . .
N3 N 0.0553(7) 0.4887(7) 0.7538(5) 0.054(2) Uani 1 1 d . . .
H3C H 0.1249 0.4380 0.7478 0.065 Uiso 1 1 calc R . .
H3D H 0.0144 0.4652 0.7799 0.065 Uiso 1 1 calc R . .
N4 N 0.0331(10) 0.6718(10) 0.7033(6) 0.088(4) Uani 1 1 d U . .
H4C H -0.0345 0.7247 0.7020 0.105 Uiso 1 1 calc R . .
H4D H 0.0832 0.6946 0.6900 0.105 Uiso 1 1 calc R . .
N5 N -0.5920(7) 1.5809(7) 0.8408(4) 0.046(2) Uani 1 1 d . . .
H5C H -0.6400 1.6051 0.8134 0.055 Uiso 1 1 calc R . .
H5D H -0.5874 1.5199 0.8559 0.055 Uiso 1 1 calc R . .
N6 N -0.4454(8) 1.6364(7) 0.8725(4) 0.047(2) Uani 1 1 d . . .
H6C H -0.3800 1.6042 0.8866 0.056 Uiso 1 1 calc R . .
H6D H -0.4587 1.7017 0.8616 0.056 Uiso 1 1 calc R . .
N7 N -0.4589(9) 1.5225(8) 0.7187(4) 0.051(2) Uani 1 1 d . . .
H7C H -0.4323 1.4535 0.7172 0.061 Uiso 1 1 calc R . .
H7D H -0.5301 1.5525 0.7132 0.061 Uiso 1 1 calc R . .
N8 N -0.3081(8) 1.5653(6) 0.7544(4) 0.044(2) Uani 1 1 d . . .
H8C H -0.3171 1.6305 0.7523 0.053 Uiso 1 1 calc R . .
H8D H -0.2504 1.5262 0.7745 0.053 Uiso 1 1 calc R . .
N9 N 0.3420(8) 0.8193(7) 0.5223(4) 0.046(2) Uani 1 1 d . . .
H9C H 0.2797 0.8155 0.5375 0.055 Uiso 1 1 calc R . .
H9D H 0.3522 0.8135 0.4814 0.055 Uiso 1 1 calc R . .
N10 N 0.4726(8) 0.8687(7) 0.5749(4) 0.048(2) Uani 1 1 d . . .
H10C H 0.5175 0.8984 0.5653 0.058 Uiso 1 1 calc R . .
H10D H 0.4617 0.8616 0.6159 0.058 Uiso 1 1 calc R . .
N11 N 0.1871(7) 1.0443(7) 0.5121(4) 0.0409(19) Uani 1 1 d . . .
H11C H 0.1962 1.0398 0.4711 0.049 Uiso 1 1 calc R . .
H11D H 0.1375 1.0222 0.5282 0.049 Uiso 1 1 calc R . .
N12 N 0.3191(8) 1.0885(7) 0.5659(4) 0.044(2) Uani 1 1 d . . .
H12C H 0.2934 1.1002 0.6060 0.053 Uiso 1 1 calc R . .
H12D H 0.3860 1.0862 0.5590 0.053 Uiso 1 1 calc R . .
N13 N 0.0466(9) 0.1255(8) 0.9281(5) 0.059(3) Uani 1 1 d . . .
H13C H 0.0557 0.1798 0.9366 0.071 Uiso 1 1 calc R . .
H13D H -0.0208 0.1356 0.9456 0.071 Uiso 1 1 calc R . .
N14 N 0.1891(8) -0.0206(8) 0.8479(5) 0.059(3) Uani 1 1 d . . .
H14C H 0.1900 -0.0677 0.8241 0.071 Uiso 1 1 calc R . .
H14D H 0.2515 -0.0149 0.8366 0.071 Uiso 1 1 calc R . .
N15 N -0.0626(7) 0.2539(7) 0.8285(5) 0.049(2) Uani 1 1 d . . .
H15C H -0.1267 0.2550 0.8453 0.059 Uiso 1 1 calc R . .
H15D H -0.0532 0.3004 0.8475 0.059 Uiso 1 1 calc R . .
N16 N 0.0467(10) 0.0993(9) 0.7504(5) 0.068(3) Uani 1 1 d . . .
H16C H 0.1087 0.0914 0.7260 0.081 Uiso 1 1 calc R . .
H16D H 0.0383 0.0425 0.7474 0.081 Uiso 1 1 calc R . .
O1W O 0.7812(8) 0.7484(8) 0.6328(5) 0.019(2) Uiso 0.50 1 d P . .
O2W O 0.8617(9) 0.4987(7) 0.8432(5) 0.022(2) Uani 0.50 1 d P . .
O3W O 0.7418(10) 0.4178(9) 0.9407(6) 0.030(3) Uani 0.50 1 d P . .
O4W O 0.3634(10) 0.4365(8) 0.9551(6) 0.037(3) Uani 0.50 1 d P . .
O5W O 0.8115(9) 0.2142(9) 0.9806(5) 0.026(2) Uani 0.50 1 d P . .
O6W O 0.3071(13) 0.6075(12) 0.6625(7) 0.055(5) Uani 0.50 1 d P . .
O7W O 0.4760(12) 0.4665(12) 0.5642(7) 0.047(3) Uiso 0.50 1 d P . .
O8W O 0.8659(15) 0.6008(11) 0.5445(8) 0.069(6) Uani 0.50 1 d P . .
O9W O 0.2520(16) 0.9475(15) 0.6561(9) 0.067(5) Uiso 0.50 1 d P . .
O10W O 0.2788(13) 0.3661(12) 0.0528(7) 0.049(4) Uiso 0.50 1 d P . .
O11W O 0.0885(14) 0.4107(13) 0.0180(8) 0.054(4) Uiso 0.50 1 d P . .
O12W O -0.1688(18) 1.3307(17) 0.5355(10) 0.082(6) Uiso 0.50 1 d P . .


_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
Cu1 N4 1.966(13) . ?
Cu1 N1 1.976(11) . ?
Cu1 N3 1.993(10) . ?
Cu1 N2 2.011(13) . ?
Cu1 O3 2.381(6) . ?
Cu2 N8 1.995(9) . ?
Cu2 N6 2.008(9) . ?
Cu2 N7 2.017(9) . ?
Cu2 N5 2.018(9) . ?
Cu2 O12 2.302(6) . ?
Cu3 N12 1.974(8) . ?
Cu3 N10 1.990(9) . ?
Cu3 N11 1.996(9) . ?
Cu3 N9 2.022(8) . ?
Cu4 N15 1.968(9) . ?
Cu4 N14 1.987(10) . ?
Cu4 N13 1.998(11) . ?
Cu4 N16 2.010(11) . ?
Ge1 O39 1.741(5) . ?
Ge1 O38 1.747(5) . ?
Ge1 O40 1.760(5) . ?
Ge1 O37 1.772(5) . ?
Nb1 O25 1.857(5) . ?
Nb1 O13 1.863(5) . ?
Nb1 O1 1.912(5) 2_477 ?
Nb1 O30 2.095(5) . ?
Nb1 O15 2.099(5) . ?
Nb1 O37 2.221(5) . ?
Nb1 Sb1 3.3013(8) . ?
Nb1 Nb2 3.3431(9) . ?
Nb2 O2 1.766(5) . ?
Nb2 O27 1.937(5) . ?
Nb2 O26 1.948(6) . ?
Nb2 O14 2.010(5) . ?
Nb2 O13 2.060(5) . ?
Nb2 O37 2.430(5) . ?
Nb3 O3 1.767(5) . ?
Nb3 O28 1.894(5) . ?
Nb3 O14 1.928(5) . ?
Nb3 O15 2.085(5) . ?
Nb3 O29 2.134(5) . ?
Nb3 O37 2.423(5) . ?
Nb3 Sb1 3.2961(8) . ?
Nb4 O4 1.749(6) . ?
Nb4 O26 1.916(6) . ?
Nb4 O16 1.930(5) . ?
Nb4 O33 2.111(5) . ?
Nb4 O18 2.127(5) . ?
Nb4 O38 2.372(5) . ?
Nb4 Sb2 3.2697(9) . ?
Nb4 Nb5 3.3297(9) . ?
Nb5 O5 1.753(6) . ?
Nb5 O17 1.958(5) . ?
Nb5 O16 1.977(5) . ?
Nb5 O25 2.044(5) . ?
Nb5 O31 2.049(5) . ?
Nb5 O38 2.361(5) . ?
Nb6 O6 1.758(6) . ?
Nb6 O36 1.897(6) . ?
Nb6 O17 1.937(5) . ?
Nb6 O18 2.096(5) . ?
Nb6 O34 2.116(5) . ?
Nb6 O38 2.388(5) . ?
Nb6 Sb2 3.2644(8) . ?
Nb7 O7 1.775(6) . ?
Nb7 O21 1.909(6) . ?
Nb7 O27 1.911(5) . ?
Nb7 O19 2.092(5) . ?
Nb7 O33 2.126(5) . ?
Nb7 O39 2.360(5) . ?
Nb7 Sb2 3.3041(8) . ?
Nb8 O8 1.760(6) . ?
Nb8 O20 1.888(6) . ?
Nb8 O35 1.925(5) . ?
Nb8 O19 2.083(5) . ?
Nb8 O34 2.167(6) . ?
Nb8 O39 2.398(5) . ?
Nb8 Sb2 3.3064(9) . ?
Nb9 O9 1.762(6) . ?
Nb9 O32 1.945(6) . ?
Nb9 O28 1.975(5) . ?
Nb9 O20 2.010(5) . ?
Nb9 O21 2.031(5) . ?
Nb9 O39 2.431(5) . ?
Nb10 O31 1.849(5) . ?
Nb10 O22 1.860(5) . ?
Nb10 O1 1.923(5) . ?
Nb10 O23 2.108(5) . ?
Nb10 O30 2.111(5) . ?
Nb10 O40 2.205(5) . ?
Nb10 Sb1 3.2851(8) . ?
Nb10 Nb12 3.3428(9) . ?
Nb11 O11 1.749(6) . ?
Nb11 O32 1.904(6) . ?
Nb11 O24 1.932(5) . ?
Nb11 O23 2.081(5) . ?
Nb11 O29 2.155(5) . ?
Nb11 O40 2.471(5) . ?
Nb11 Sb1 3.2747(8) . ?
Nb12 O12 1.772(5) . ?
Nb12 O35 1.928(5) . ?
Nb12 O24 1.968(6) . ?
Nb12 O36 1.972(6) . ?
Nb12 O22 2.081(5) . ?
Nb12 O40 2.420(5) . ?
Sb1 O29 1.993(5) . ?
Sb1 O30 1.998(5) . ?
Sb1 O23 2.140(5) . ?
Sb1 O15 2.189(5) . ?
Sb2 O34 1.981(5) . ?
Sb2 O33 1.992(5) . ?
Sb2 O18 2.143(5) . ?
Sb2 O19 2.180(5) . ?
O1 Nb1 1.912(5) 2_477 ?
C1 N1 1.474(18) . ?
C1 C2 1.50(2) . ?
C2 N2 1.44(2) . ?
C3 C4 1.33(2) . ?
C3 N3 1.451(18) . ?
C4 N4 1.55(2) . ?
C5 N5 1.479(14) . ?
C5 C6 1.491(17) . ?
C6 N6 1.477(15) . ?
C7 N7 1.473(15) . ?
C7 C8 1.520(18) . ?
C8 N8 1.469(15) . ?
C9 C10 1.462(17) . ?
C9 N9 1.471(15) . ?
C10 N10 1.488(13) . ?
C11 N11 1.471(14) . ?
C11 C12 1.499(17) . ?
C12 N12 1.462(14) . ?
C13 C14 1.43(2) . ?
C13 N13 1.435(18) . ?
C14 N14 1.461(17) . ?
C15 C16 1.457(18) . ?
C15 N15 1.490(17) . ?
C16 N16 1.435(16) . ?

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
N4 Cu1 N1 175.7(5) . . ?
N4 Cu1 N3 86.0(6) . . ?
N1 Cu1 N3 95.7(5) . . ?
N4 Cu1 N2 93.3(6) . . ?
N1 Cu1 N2 84.6(6) . . ?
N3 Cu1 N2 175.0(5) . . ?
N4 Cu1 O3 90.2(4) . . ?
N1 Cu1 O3 93.6(3) . . ?
N3 Cu1 O3 92.3(3) . . ?
N2 Cu1 O3 92.6(4) . . ?
N8 Cu2 N6 94.1(4) . . ?
N8 Cu2 N7 84.2(4) . . ?
N6 Cu2 N7 166.1(4) . . ?
N8 Cu2 N5 171.2(4) . . ?
N6 Cu2 N5 85.0(4) . . ?
N7 Cu2 N5 94.6(4) . . ?
N8 Cu2 O12 96.8(3) . . ?
N6 Cu2 O12 93.9(3) . . ?
N7 Cu2 O12 100.0(3) . . ?
N5 Cu2 O12 92.0(3) . . ?
N12 Cu3 N10 95.1(4) . . ?
N12 Cu3 N11 84.7(4) . . ?
N10 Cu3 N11 179.7(4) . . ?
N12 Cu3 N9 178.9(4) . . ?
N10 Cu3 N9 84.1(4) . . ?
N11 Cu3 N9 96.1(4) . . ?
N15 Cu4 N14 176.0(4) . . ?
N15 Cu4 N13 93.5(4) . . ?
N14 Cu4 N13 85.2(4) . . ?
N15 Cu4 N16 84.1(4) . . ?
N14 Cu4 N16 97.9(5) . . ?
N13 Cu4 N16 168.7(5) . . ?
O39 Ge1 O38 113.4(2) . . ?
O39 Ge1 O40 108.8(2) . . ?
O38 Ge1 O40 106.8(2) . . ?
O39 Ge1 O37 108.5(2) . . ?
O38 Ge1 O37 108.1(2) . . ?
O40 Ge1 O37 111.3(2) . . ?
O25 Nb1 O13 99.5(2) . . ?
O25 Nb1 O1 102.9(2) . 2_477 ?
O13 Nb1 O1 100.2(2) . 2_477 ?
O25 Nb1 O30 87.1(2) . . ?
O13 Nb1 O30 161.2(2) . . ?
O1 Nb1 O30 95.4(2) 2_477 . ?
O25 Nb1 O15 159.4(2) . . ?
O13 Nb1 O15 94.0(2) . . ?
O1 Nb1 O15 89.9(2) 2_477 . ?
O30 Nb1 O15 75.51(19) . . ?
O25 Nb1 O37 92.5(2) . . ?
O13 Nb1 O37 79.7(2) . . ?
O1 Nb1 O37 164.3(2) 2_477 . ?
O30 Nb1 O37 82.48(18) . . ?
O15 Nb1 O37 74.51(18) . . ?
O25 Nb1 Sb1 122.26(16) . . ?
O13 Nb1 Sb1 133.92(17) . . ?
O1 Nb1 Sb1 89.40(15) 2_477 . ?
O30 Nb1 Sb1 35.25(13) . . ?
O15 Nb1 Sb1 40.65(14) . . ?
O37 Nb1 Sb1 79.90(13) . . ?
O25 Nb1 Nb2 95.03(16) . . ?
O13 Nb1 Nb2 33.35(15) . . ?
O1 Nb1 Nb2 132.91(15) 2_477 . ?
O30 Nb1 Nb2 129.05(14) . . ?
O15 Nb1 Nb2 87.64(14) . . ?
O37 Nb1 Nb2 46.59(12) . . ?
Sb1 Nb1 Nb2 116.84(2) . . ?
O2 Nb2 O27 102.3(2) . . ?
O2 Nb2 O26 101.5(3) . . ?
O27 Nb2 O26 88.4(2) . . ?
O2 Nb2 O14 100.5(2) . . ?
O27 Nb2 O14 90.2(2) . . ?
O26 Nb2 O14 157.7(2) . . ?
O2 Nb2 O13 99.7(2) . . ?
O27 Nb2 O13 158.0(2) . . ?
O26 Nb2 O13 88.3(2) . . ?
O14 Nb2 O13 84.7(2) . . ?
O2 Nb2 O37 169.3(2) . . ?
O27 Nb2 O37 86.8(2) . . ?
O26 Nb2 O37 84.1(2) . . ?
O14 Nb2 O37 73.63(18) . . ?
O13 Nb2 O37 71.22(18) . . ?
O2 Nb2 Nb1 129.5(2) . . ?
O27 Nb2 Nb1 128.23(16) . . ?
O26 Nb2 Nb1 82.83(16) . . ?
O14 Nb2 Nb1 80.59(15) . . ?
O13 Nb2 Nb1 29.81(14) . . ?
O37 Nb2 Nb1 41.62(11) . . ?
O3 Nb3 O28 102.3(3) . . ?
O3 Nb3 O14 102.0(3) . . ?
O28 Nb3 O14 97.4(2) . . ?
O3 Nb3 O15 97.4(2) . . ?
O28 Nb3 O15 154.6(2) . . ?
O14 Nb3 O15 94.0(2) . . ?
O3 Nb3 O29 98.9(2) . . ?
O28 Nb3 O29 85.3(2) . . ?
O14 Nb3 O29 157.8(2) . . ?
O15 Nb3 O29 75.9(2) . . ?
O3 Nb3 O37 167.2(2) . . ?
O28 Nb3 O37 90.5(2) . . ?
O14 Nb3 O37 75.12(18) . . ?
O15 Nb3 O37 70.53(18) . . ?
O29 Nb3 O37 82.84(18) . . ?
O3 Nb3 Sb1 96.5(2) . . ?
O28 Nb3 Sb1 120.20(17) . . ?
O14 Nb3 Sb1 133.10(16) . . ?
O15 Nb3 Sb1 40.69(14) . . ?
O29 Nb3 Sb1 35.56(14) . . ?
O37 Nb3 Sb1 77.44(11) . . ?
O4 Nb4 O26 102.4(3) . . ?
O4 Nb4 O16 102.8(3) . . ?
O26 Nb4 O16 95.5(2) . . ?
O4 Nb4 O33 96.9(3) . . ?
O26 Nb4 O33 88.0(2) . . ?
O16 Nb4 O33 158.8(2) . . ?
O4 Nb4 O18 97.2(3) . . ?
O26 Nb4 O18 155.7(2) . . ?
O16 Nb4 O18 94.0(2) . . ?
O33 Nb4 O18 75.5(2) . . ?
O4 Nb4 O38 168.6(2) . . ?
O26 Nb4 O38 88.9(2) . . ?
O16 Nb4 O38 77.1(2) . . ?
O33 Nb4 O38 82.04(19) . . ?
O18 Nb4 O38 71.46(18) . . ?
O4 Nb4 Sb2 93.7(2) . . ?
O26 Nb4 Sb2 123.43(16) . . ?
O16 Nb4 Sb2 133.29(17) . . ?
O33 Nb4 Sb2 35.92(14) . . ?
O18 Nb4 Sb2 40.20(14) . . ?
O38 Nb4 Sb2 78.74(12) . . ?
O4 Nb4 Nb5 134.2(2) . . ?
O26 Nb4 Nb5 92.23(16) . . ?
O16 Nb4 Nb5 31.98(16) . . ?
O33 Nb4 Nb5 127.15(15) . . ?
O18 Nb4 Nb5 84.06(14) . . ?
O38 Nb4 Nb5 45.16(12) . . ?
Sb2 Nb4 Nb5 113.91(2) . . ?
O5 Nb5 O17 100.4(3) . . ?
O5 Nb5 O16 99.3(3) . . ?
O17 Nb5 O16 91.3(2) . . ?
O5 Nb5 O25 100.4(2) . . ?
O17 Nb5 O25 158.6(2) . . ?
O16 Nb5 O25 90.2(2) . . ?
O5 Nb5 O31 100.8(3) . . ?
O17 Nb5 O31 89.4(2) . . ?
O16 Nb5 O31 159.4(2) . . ?
O25 Nb5 O31 81.9(2) . . ?
O5 Nb5 O38 173.8(2) . . ?
O17 Nb5 O38 75.3(2) . . ?
O16 Nb5 O38 76.52(19) . . ?
O25 Nb5 O38 84.35(18) . . ?
O31 Nb5 O38 83.78(19) . . ?
O5 Nb5 Nb4 130.4(2) . . ?
O17 Nb5 Nb4 84.28(16) . . ?
O16 Nb5 Nb4 31.13(15) . . ?
O25 Nb5 Nb4 85.99(15) . . ?
O31 Nb5 Nb4 128.75(15) . . ?
O38 Nb5 Nb4 45.42(12) . . ?
O6 Nb6 O36 103.3(3) . . ?
O6 Nb6 O17 100.4(3) . . ?
O36 Nb6 O17 97.1(2) . . ?
O6 Nb6 O18 96.2(3) . . ?
O36 Nb6 O18 156.0(2) . . ?
O17 Nb6 O18 92.9(2) . . ?
O6 Nb6 O34 99.5(2) . . ?
O36 Nb6 O34 87.5(2) . . ?
O17 Nb6 O34 157.9(2) . . ?
O18 Nb6 O34 75.6(2) . . ?
O6 Nb6 O38 166.4(2) . . ?
O36 Nb6 O38 90.0(2) . . ?
O17 Nb6 O38 75.01(19) . . ?
O18 Nb6 O38 71.63(18) . . ?
O34 Nb6 O38 83.44(18) . . ?
O6 Nb6 Sb2 96.0(2) . . ?
O36 Nb6 Sb2 122.63(17) . . ?
O17 Nb6 Sb2 131.84(17) . . ?
O18 Nb6 Sb2 40.16(15) . . ?
O34 Nb6 Sb2 35.78(15) . . ?
O38 Nb6 Sb2 78.64(12) . . ?
O7 Nb7 O21 101.4(3) . . ?
O7 Nb7 O27 102.0(3) . . ?
O21 Nb7 O27 97.1(2) . . ?
O7 Nb7 O19 95.1(2) . . ?
O21 Nb7 O19 96.0(2) . . ?
O27 Nb7 O19 155.9(2) . . ?
O7 Nb7 O33 98.5(2) . . ?
O21 Nb7 O33 159.0(2) . . ?
O27 Nb7 O33 85.6(2) . . ?
O19 Nb7 O33 75.2(2) . . ?
O7 Nb7 O39 167.9(2) . . ?
O21 Nb7 O39 77.3(2) . . ?
O27 Nb7 O39 90.1(2) . . ?
O19 Nb7 O39 73.25(19) . . ?
O33 Nb7 O39 81.86(19) . . ?
O7 Nb7 Sb2 94.34(19) . . ?
O21 Nb7 Sb2 135.00(17) . . ?
O27 Nb7 Sb2 120.57(16) . . ?
O19 Nb7 Sb2 40.31(15) . . ?
O33 Nb7 Sb2 35.27(14) . . ?
O39 Nb7 Sb2 78.88(12) . . ?
O8 Nb8 O20 102.5(3) . . ?
O8 Nb8 O35 101.5(3) . . ?
O20 Nb8 O35 99.5(2) . . ?
O8 Nb8 O19 96.8(3) . . ?
O20 Nb8 O19 94.1(2) . . ?
O35 Nb8 O19 154.1(2) . . ?
O8 Nb8 O34 97.8(3) . . ?
O20 Nb8 O34 158.0(2) . . ?
O35 Nb8 O34 84.4(2) . . ?
O19 Nb8 O34 75.1(2) . . ?
O8 Nb8 O39 169.1(2) . . ?
O20 Nb8 O39 76.3(2) . . ?
O35 Nb8 O39 89.4(2) . . ?
O19 Nb8 O39 72.58(18) . . ?
O34 Nb8 O39 82.21(18) . . ?
O8 Nb8 Sb2 95.3(2) . . ?
O20 Nb8 Sb2 132.95(18) . . ?
O35 Nb8 Sb2 119.16(17) . . ?
O19 Nb8 Sb2 40.21(15) . . ?
O34 Nb8 Sb2 35.25(14) . . ?
O39 Nb8 Sb2 78.34(12) . . ?
O9 Nb9 O32 102.2(3) . . ?
O9 Nb9 O28 100.7(3) . . ?
O32 Nb9 O28 88.0(2) . . ?
O9 Nb9 O20 100.0(3) . . ?
O32 Nb9 O20 90.0(2) . . ?
O28 Nb9 O20 159.1(2) . . ?
O9 Nb9 O21 100.0(3) . . ?
O32 Nb9 O21 157.8(2) . . ?
O28 Nb9 O21 88.6(2) . . ?
O20 Nb9 O21 85.4(2) . . ?
O9 Nb9 O39 170.9(2) . . ?
O32 Nb9 O39 84.4(2) . . ?
O28 Nb9 O39 85.6(2) . . ?
O20 Nb9 O39 73.4(2) . . ?
O21 Nb9 O39 73.49(19) . . ?
O31 Nb10 O22 99.6(2) . . ?
O31 Nb10 O1 102.1(2) . . ?
O22 Nb10 O1 102.6(2) . . ?
O31 Nb10 O23 158.4(2) . . ?
O22 Nb10 O23 95.5(2) . . ?
O1 Nb10 O23 89.4(2) . . ?
O31 Nb10 O30 86.3(2) . . ?
O22 Nb10 O30 162.6(2) . . ?
O1 Nb10 O30 92.1(2) . . ?
O23 Nb10 O30 75.00(19) . . ?
O31 Nb10 O40 92.5(2) . . ?
O22 Nb10 O40 80.4(2) . . ?
O1 Nb10 O40 164.3(2) . . ?
O23 Nb10 O40 74.95(19) . . ?
O30 Nb10 O40 83.02(18) . . ?
O31 Nb10 Sb1 121.97(16) . . ?
O22 Nb10 Sb1 134.74(18) . . ?
O1 Nb10 Sb1 86.64(15) . . ?
O23 Nb10 Sb1 39.70(13) . . ?
O30 Nb10 Sb1 35.74(13) . . ?
O40 Nb10 Sb1 80.69(13) . . ?
O31 Nb10 Nb12 97.01(16) . . ?
O22 Nb10 Nb12 34.07(16) . . ?
O1 Nb10 Nb12 135.45(15) . . ?
O23 Nb10 Nb12 86.96(14) . . ?
O30 Nb10 Nb12 129.27(14) . . ?
O40 Nb10 Nb12 46.34(12) . . ?
Sb1 Nb10 Nb12 116.13(2) . . ?
O11 Nb11 O32 101.9(3) . . ?
O11 Nb11 O24 101.8(3) . . ?
O32 Nb11 O24 97.8(2) . . ?
O11 Nb11 O23 101.0(3) . . ?
O32 Nb11 O23 152.7(2) . . ?
O24 Nb11 O23 91.9(2) . . ?
O11 Nb11 O29 100.5(3) . . ?
O32 Nb11 O29 85.9(2) . . ?
O24 Nb11 O29 156.1(2) . . ?
O23 Nb11 O29 75.46(19) . . ?
O11 Nb11 O40 169.4(2) . . ?
O32 Nb11 O40 88.4(2) . . ?
O24 Nb11 O40 73.94(19) . . ?
O23 Nb11 O40 69.84(18) . . ?
O29 Nb11 O40 82.63(18) . . ?
O11 Nb11 Sb1 99.0(2) . . ?
O32 Nb11 Sb1 121.14(17) . . ?
O24 Nb11 Sb1 130.40(17) . . ?
O23 Nb11 Sb1 39.77(13) . . ?
O29 Nb11 Sb1 36.16(14) . . ?
O40 Nb11 Sb1 77.44(11) . . ?
O12 Nb12 O35 102.5(3) . . ?
O12 Nb12 O24 100.5(3) . . ?
O35 Nb12 O24 93.0(2) . . ?
O12 Nb12 O36 100.5(3) . . ?
O35 Nb12 O36 87.7(2) . . ?
O24 Nb12 O36 158.3(2) . . ?
O12 Nb12 O22 98.8(2) . . ?
O35 Nb12 O22 158.6(2) . . ?
O24 Nb12 O22 84.9(2) . . ?
O36 Nb12 O22 86.5(2) . . ?
O12 Nb12 O40 169.1(2) . . ?
O35 Nb12 O40 87.6(2) . . ?
O24 Nb12 O40 74.57(19) . . ?
O36 Nb12 O40 83.77(19) . . ?
O22 Nb12 O40 71.23(18) . . ?
O12 Nb12 Nb10 128.84(19) . . ?
O35 Nb12 Nb10 128.64(17) . . ?
O24 Nb12 Nb10 79.51(16) . . ?
O36 Nb12 Nb10 83.08(16) . . ?
O22 Nb12 Nb10 30.04(14) . . ?
O40 Nb12 Nb10 41.22(11) . . ?
O29 Sb1 O30 99.9(2) . . ?
O29 Sb1 O23 77.6(2) . . ?
O30 Sb1 O23 76.65(19) . . ?
O29 Sb1 O15 76.6(2) . . ?
O30 Sb1 O15 75.53(19) . . ?
O23 Sb1 O15 137.72(19) . . ?
O29 Sb1 Nb11 39.65(15) . . ?
O30 Sb1 Nb11 92.17(14) . . ?
O23 Sb1 Nb11 38.47(14) . . ?
O15 Sb1 Nb11 112.17(13) . . ?
O29 Sb1 Nb10 92.90(15) . . ?
O30 Sb1 Nb10 38.11(14) . . ?
O23 Sb1 Nb10 38.99(13) . . ?
O15 Sb1 Nb10 110.23(13) . . ?
Nb11 Sb1 Nb10 65.014(18) . . ?
O29 Sb1 Nb3 38.51(15) . . ?
O30 Sb1 Nb3 90.88(14) . . ?
O23 Sb1 Nb3 111.86(14) . . ?
O15 Sb1 Nb3 38.39(13) . . ?
Nb11 Sb1 Nb3 76.77(2) . . ?
Nb10 Sb1 Nb3 108.49(2) . . ?
O29 Sb1 Nb1 92.02(15) . . ?
O30 Sb1 Nb1 37.25(14) . . ?
O23 Sb1 Nb1 110.43(13) . . ?
O15 Sb1 Nb1 38.68(13) . . ?
Nb11 Sb1 Nb1 109.04(2) . . ?
Nb10 Sb1 Nb1 74.289(18) . . ?
Nb3 Sb1 Nb1 64.287(18) . . ?
O34 Sb2 O33 101.1(2) . . ?
O34 Sb2 O18 77.4(2) . . ?
O33 Sb2 O18 77.6(2) . . ?
O34 Sb2 O19 76.9(2) . . ?
O33 Sb2 O19 76.0(2) . . ?
O18 Sb2 O19 138.46(19) . . ?
O34 Sb2 Nb6 38.63(16) . . ?
O33 Sb2 Nb6 93.27(15) . . ?
O18 Sb2 Nb6 39.12(14) . . ?
O19 Sb2 Nb6 111.64(14) . . ?
O34 Sb2 Nb4 94.40(15) . . ?
O33 Sb2 Nb4 38.45(16) . . ?
O18 Sb2 Nb4 39.85(14) . . ?
O19 Sb2 Nb4 111.31(14) . . ?
Nb6 Sb2 Nb4 66.736(19) . . ?
O34 Sb2 Nb7 92.92(15) . . ?
O33 Sb2 Nb7 38.06(16) . . ?
O18 Sb2 Nb7 112.10(13) . . ?
O19 Sb2 Nb7 38.38(14) . . ?
Nb6 Sb2 Nb7 109.88(2) . . ?
Nb4 Sb2 Nb7 75.58(2) . . ?
O34 Sb2 Nb8 39.15(16) . . ?
O33 Sb2 Nb8 91.82(15) . . ?
O18 Sb2 Nb8 112.47(14) . . ?
O19 Sb2 Nb8 38.10(14) . . ?
Nb6 Sb2 Nb8 76.43(2) . . ?
Nb4 Sb2 Nb8 110.42(2) . . ?
Nb7 Sb2 Nb8 64.413(19) . . ?
Nb1 O1 Nb10 150.1(3) 2_477 . ?
Nb3 O3 Cu1 136.5(3) . . ?
Nb12 O12 Cu2 128.7(3) . . ?
Nb1 O13 Nb2 116.8(3) . . ?
Nb3 O14 Nb2 121.0(2) . . ?
Nb3 O15 Nb1 114.1(2) . . ?
Nb3 O15 Sb1 100.9(2) . . ?
Nb1 O15 Sb1 100.7(2) . . ?
Nb4 O16 Nb5 116.9(3) . . ?
Nb6 O17 Nb5 119.5(3) . . ?
Nb6 O18 Nb4 116.6(2) . . ?
Nb6 O18 Sb2 100.7(2) . . ?
Nb4 O18 Sb2 99.9(2) . . ?
Nb8 O19 Nb7 115.1(2) . . ?
Nb8 O19 Sb2 101.7(2) . . ?
Nb7 O19 Sb2 101.3(2) . . ?
Nb8 O20 Nb9 120.7(3) . . ?
Nb7 O21 Nb9 119.0(3) . . ?
Nb10 O22 Nb12 115.9(3) . . ?
Nb11 O23 Nb10 114.6(2) . . ?
Nb11 O23 Sb1 101.8(2) . . ?
Nb10 O23 Sb1 101.3(2) . . ?
Nb11 O24 Nb12 122.1(3) . . ?
Nb1 O25 Nb5 153.0(3) . . ?
Nb4 O26 Nb2 151.8(3) . . ?
Nb7 O27 Nb2 153.6(3) . . ?
Nb3 O28 Nb9 153.3(3) . . ?
Sb1 O29 Nb3 105.9(2) . . ?
Sb1 O29 Nb11 104.2(2) . . ?
Nb3 O29 Nb11 144.0(3) . . ?
Sb1 O30 Nb1 107.5(2) . . ?
Sb1 O30 Nb10 106.2(2) . . ?
Nb1 O30 Nb10 142.0(3) . . ?
Nb10 O31 Nb5 153.5(3) . . ?
Nb11 O32 Nb9 154.3(3) . . ?
Sb2 O33 Nb4 105.6(2) . . ?
Sb2 O33 Nb7 106.7(2) . . ?
Nb4 O33 Nb7 143.9(3) . . ?
Sb2 O34 Nb6 105.6(3) . . ?
Sb2 O34 Nb8 105.6(2) . . ?
Nb6 O34 Nb8 143.3(3) . . ?
Nb8 O35 Nb12 154.3(3) . . ?
Nb6 O36 Nb12 151.8(3) . . ?
Ge1 O37 Nb1 123.7(2) . . ?
Ge1 O37 Nb3 122.3(2) . . ?
Nb1 O37 Nb3 98.09(17) . . ?
Ge1 O37 Nb2 122.5(2) . . ?
Nb1 O37 Nb2 91.80(17) . . ?
Nb3 O37 Nb2 89.88(15) . . ?
Ge1 O38 Nb5 126.7(2) . . ?
Ge1 O38 Nb4 121.9(2) . . ?
Nb5 O38 Nb4 89.42(17) . . ?
Ge1 O38 Nb6 121.8(2) . . ?
Nb5 O38 Nb6 90.19(16) . . ?
Nb4 O38 Nb6 98.06(17) . . ?
Ge1 O39 Nb7 123.1(3) . . ?
Ge1 O39 Nb8 123.7(2) . . ?
Nb7 O39 Nb8 95.55(17) . . ?
Ge1 O39 Nb9 125.4(2) . . ?
Nb7 O39 Nb9 90.23(16) . . ?
Nb8 O39 Nb9 89.14(16) . . ?
Ge1 O40 Nb10 124.2(3) . . ?
Ge1 O40 Nb12 124.0(2) . . ?
Nb10 O40 Nb12 92.44(17) . . ?
Ge1 O40 Nb11 121.1(2) . . ?
Nb10 O40 Nb11 97.71(18) . . ?
Nb12 O40 Nb11 88.47(16) . . ?
N1 C1 C2 104.2(13) . . ?
N2 C2 C1 114.2(15) . . ?
C4 C3 N3 111.6(15) . . ?
C3 C4 N4 109.4(16) . . ?
N5 C5 C6 108.5(10) . . ?
N6 C6 C5 108.7(10) . . ?
N7 C7 C8 106.7(9) . . ?
N8 C8 C7 107.5(10) . . ?
C10 C9 N9 109.3(9) . . ?
C9 C10 N10 106.8(10) . . ?
N11 C11 C12 108.3(10) . . ?
N12 C12 C11 107.0(11) . . ?
C14 C13 N13 115.7(14) . . ?
C13 C14 N14 112.3(13) . . ?
C16 C15 N15 108.2(10) . . ?
N16 C16 C15 109.8(10) . . ?
C1 N1 Cu1 112.0(11) . . ?
C2 N2 Cu1 107.2(10) . . ?
C3 N3 Cu1 105.1(10) . . ?
C4 N4 Cu1 105.3(10) . . ?
C5 N5 Cu2 108.5(7) . . ?
C6 N6 Cu2 108.1(7) . . ?
C7 N7 Cu2 107.1(7) . . ?
C8 N8 Cu2 110.6(7) . . ?
C9 N9 Cu3 108.5(7) . . ?
C10 N10 Cu3 108.1(7) . . ?
C11 N11 Cu3 109.4(7) . . ?
C12 N12 Cu3 108.4(7) . . ?
C13 N13 Cu4 109.7(9) . . ?
C14 N14 Cu4 108.6(8) . . ?
C15 N15 Cu4 107.7(7) . . ?
C16 N16 Cu4 110.2(8) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         3.738
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.263
####################################################################### 
# 
# 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_shelx
_audit_block_doi                 10.5517/cc13qs1n
_database_code_depnum_ccdc_archive 'CCDC 1034781'
_audit_update_record             
;
2014-11-18 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Nb12 O39 Sb2 Si, 4(C4 H16 Cu N4), 6(H2 O)'
_chemical_formula_sum            'C16 H76 Cu4 N16 Nb12 O45 Sb2 Si'
_chemical_formula_weight         2853.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   13.9137(7)
_cell_length_b                   14.4730(7)
_cell_length_c                   21.9355(10)
_cell_angle_alpha                84.8190(10)
_cell_angle_beta                 79.8390(10)
_cell_angle_gamma                61.3420(10)
_cell_volume                     3815.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2736
_exptl_absorpt_coefficient_mu    3.619
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28356
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         28.31
_reflns_number_total             18856
_reflns_number_gt                13511
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. The ISOR instruction was 
 used on atoms of C6 C14 C3 C13 Cu4 N14 because of the 
ADP or NPD Alert. 
 The Anis instruction was not used on atoms O5w O6w O7w O8w O9w O10w O11w 
 O12w O13w because of the 
 ADP or NPD Alert. The occupancy of water 
 molecules is changed based on Elemental Analysis and Thermogravimetric 
 Analysis.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0835P)²+23.5327P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         18856
_refine_ls_number_parameters     892
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1707
_refine_ls_wR_factor_gt          0.1461
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 1.05138(13) -0.39635(11) 0.78170(8) 0.0540(4) Uani 1 1 d . A .
Cu2 Cu 0.56815(13) 0.55889(10) 0.80080(7) 0.0443(4) Uani 1 1 d . . .
Cu3 Cu 0.68069(14) 0.02451(15) 0.45804(6) 0.0525(4) Uani 1 1 d . . .
Cu4 Cu -0.06764(17) 0.9137(2) 1.17263(12) 0.1097(10) Uani 1 1 d DU . .
Nb1 Nb 0.48889(6) -0.07097(5) 0.89539(3) 0.01439(15) Uani 1 1 d . . .
Nb2 Nb 0.50270(7) -0.11961(6) 0.74729(3) 0.02029(16) Uani 1 1 d . . .
Nb3 Nb 0.74751(6) -0.19732(6) 0.80175(3) 0.01806(16) Uani 1 1 d . . .
Nb4 Nb 0.30458(7) 0.16678(7) 0.73783(3) 0.02315(17) Uani 1 1 d . . .
Nb5 Nb 0.29064(6) 0.21825(6) 0.88499(3) 0.02075(17) Uani 1 1 d . . .
Nb6 Nb 0.36886(7) 0.36370(6) 0.77973(4) 0.02362(18) Uani 1 1 d . . .
Nb7 Nb 0.59693(7) 0.03279(6) 0.62867(3) 0.02021(16) Uani 1 1 d . . .
Nb8 Nb 0.66189(7) 0.22594(6) 0.66798(3) 0.02080(17) Uani 1 1 d . . .
Nb9 Nb 0.83397(6) -0.03549(6) 0.68536(3) 0.01974(16) Uani 1 1 d . . .
Nb10 Nb 0.55889(6) 0.14421(5) 0.94099(3) 0.01526(15) Uani 1 1 d . . .
Nb11 Nb 0.82168(6) 0.02252(6) 0.85012(3) 0.01830(16) Uani 1 1 d . . .
Nb12 Nb 0.63791(7) 0.28375(6) 0.83442(3) 0.02064(17) Uani 1 1 d . . .
Sb1 Sb 0.71944(5) -0.11209(4) 0.94095(2) 0.01925(13) Uani 1 1 d . . .
Sb2 Sb 0.41486(5) 0.28469(5) 0.63806(3) 0.02811(15) Uani 1 1 d . . .
Si1 Si 0.56354(18) 0.08711(16) 0.79007(9) 0.0130(4) Uani 1 1 d . . .
O1 O 0.4552(5) -0.1350(4) 0.9703(2) 0.0184(12) Uani 1 1 d . . .
O2 O 0.4581(6) -0.1965(6) 0.7151(3) 0.0367(17) Uani 1 1 d . . .
O3 O 0.8590(5) -0.3242(5) 0.8097(3) 0.0311(15) Uani 1 1 d . . .
O4 O 0.2029(6) 0.1894(6) 0.6930(3) 0.0414(18) Uani 1 1 d . . .
O5 O 0.1786(5) 0.2609(5) 0.9449(3) 0.0337(16) Uani 1 1 d . . .
O6 O 0.2974(6) 0.5006(5) 0.7626(3) 0.0394(18) Uani 1 1 d . . .
O7 O 0.5733(6) 0.0183(6) 0.5540(3) 0.0326(16) Uani 1 1 d . . .
O8 O 0.6757(6) 0.3228(5) 0.6179(3) 0.0341(16) Uani 1 1 d . . .
O9 O 0.9722(5) -0.1107(5) 0.6500(3) 0.0331(15) Uani 1 1 d . . .
O11 O 0.9543(5) -0.0349(6) 0.8697(3) 0.0337(16) Uani 1 1 d . . .
O12 O 0.6539(6) 0.3959(5) 0.8433(3) 0.0311(15) Uani 1 1 d . . .
O13 O 0.4571(5) -0.1374(5) 0.8394(3) 0.0221(13) Uani 1 1 d . . .
O14 O 0.6562(5) -0.2296(5) 0.7622(3) 0.0252(13) Uani 1 1 d . . .
O15 O 0.6560(5) -0.1859(4) 0.8887(2) 0.0184(12) Uani 1 1 d . . .
O16 O 0.2205(5) 0.2044(5) 0.8192(3) 0.0300(15) Uani 1 1 d . . .
O17 O 0.2727(5) 0.3548(5) 0.8519(3) 0.0318(16) Uani 1 1 d . . .
O18 O 0.2975(5) 0.3162(5) 0.7210(3) 0.0294(15) Uani 1 1 d . . .
O19 O 0.5889(5) 0.1798(5) 0.6102(3) 0.0234(13) Uani 1 1 d . . .
O20 O 0.8027(5) 0.1060(5) 0.6491(3) 0.0246(13) Uani 1 1 d . . .
O21 O 0.7544(5) -0.0434(5) 0.6194(2) 0.0219(13) Uani 1 1 d . . .
O22 O 0.5827(5) 0.2601(4) 0.9250(3) 0.0223(13) Uani 1 1 d . . .
O23 O 0.7268(5) 0.0334(4) 0.9357(2) 0.0183(12) Uani 1 1 d . . .
O24 O 0.7821(5) 0.1692(5) 0.8501(3) 0.0260(14) Uani 1 1 d . . .
O25 O 0.3633(5) 0.0601(5) 0.8980(3) 0.0233(13) Uani 1 1 d . . .
O26 O 0.3704(5) 0.0188(5) 0.7515(3) 0.0276(14) Uani 1 1 d . . .
O27 O 0.5680(5) -0.0715(5) 0.6746(3) 0.0244(13) Uani 1 1 d . . .
O28 O 0.8074(5) -0.1464(5) 0.7316(3) 0.0255(13) Uani 1 1 d . . .
O29 O 0.7929(5) -0.1099(4) 0.8538(2) 0.0193(12) Uani 1 1 d . . .
O30 O 0.5639(5) -0.0031(4) 0.9360(2) 0.0151(11) Uani 1 1 d . . .
O31 O 0.4126(5) 0.2047(4) 0.9306(3) 0.0213(12) Uani 1 1 d . . .
O32 O 0.8528(5) 0.0048(5) 0.7629(3) 0.0252(13) Uani 1 1 d . . .
O33 O 0.4334(5) 0.1418(5) 0.6636(3) 0.0244(13) Uani 1 1 d . . .
O34 O 0.4868(5) 0.3140(5) 0.6987(3) 0.0263(14) Uani 1 1 d . . .
O35 O 0.6765(5) 0.2639(5) 0.7456(3) 0.0277(14) Uani 1 1 d . . .
O36 O 0.4823(5) 0.3528(5) 0.8220(3) 0.0257(14) Uani 1 1 d . . .
O37 O 0.5700(4) -0.0288(4) 0.8083(2) 0.0144(11) Uani 1 1 d . . .
O38 O 0.4317(5) 0.1759(4) 0.7949(2) 0.0185(12) Uani 1 1 d . . .
O39 O 0.6330(5) 0.0808(4) 0.7208(2) 0.0174(11) Uani 1 1 d . . .
O40 O 0.6169(5) 0.1206(4) 0.8403(2) 0.0172(11) Uani 1 1 d . . .
C1 C 1.0678(15) -0.4409(15) 0.6547(8) 0.093(6) Uani 1 1 d . . .
H1A H 1.1477 -0.4784 0.6434 0.111 Uiso 1 1 calc R . .
H1B H 1.0347 -0.4177 0.6171 0.111 Uiso 1 1 calc R . .
C2 C 1.0266(15) -0.5118(15) 0.6926(9) 0.093(6) Uani 1 1 d . . .
H2A H 0.9464 -0.4789 0.6971 0.111 Uiso 1 1 calc R . .
H2B H 1.0571 -0.5786 0.6718 0.111 Uiso 1 1 calc R . .
C3 C 1.084(2) -0.288(2) 0.8720(14) 0.132(9) Uani 0.50 1 d PU A 1
H3A H 1.1627 -0.3136 0.8717 0.159 Uiso 0.50 1 calc PR A 1
H3B H 1.0450 -0.2203 0.8928 0.159 Uiso 0.50 1 calc PR A 1
C4 C 1.053(3) -0.358(3) 0.9071(16) 0.081(14) Uani 0.50 1 d P A 1
H4A H 0.9758 -0.3203 0.9249 0.097 Uiso 0.50 1 calc PR A 1
H4B H 1.0967 -0.3863 0.9408 0.097 Uiso 0.50 1 calc PR A 1
C3' C 1.084(2) -0.288(2) 0.8720(14) 0.132(9) Uani 0.50 1 d P A 2
H3'1 H 1.1414 -0.2687 0.8743 0.159 Uiso 0.50 1 calc PR A 2
H3'2 H 1.0173 -0.2373 0.8970 0.159 Uiso 0.50 1 calc PR A 2
C4' C 1.115(3) -0.386(3) 0.901(2) 0.087(13) Uani 0.50 1 d P A 2
H4'1 H 1.0835 -0.3766 0.9449 0.105 Uiso 0.50 1 calc PR A 2
H4'2 H 1.1955 -0.4253 0.8984 0.105 Uiso 0.50 1 calc PR A 2
C5 C 0.6212(16) 0.5485(11) 0.6694(6) 0.079(6) Uani 1 1 d . . .
H5A H 0.5876 0.6239 0.6624 0.095 Uiso 1 1 calc R . .
H5B H 0.6318 0.5143 0.6309 0.095 Uiso 1 1 calc R . .
C6 C 0.7287(16) 0.5098(14) 0.6920(8) 0.083(5) Uani 1 1 d U . .
H6A H 0.7749 0.5335 0.6640 0.100 Uiso 1 1 calc R . .
H6B H 0.7669 0.4334 0.6923 0.100 Uiso 1 1 calc R . .
C7 C 0.3810(15) 0.6573(12) 0.8933(7) 0.081(5) Uani 1 1 d . . .
H7A H 0.3240 0.6494 0.9222 0.097 Uiso 1 1 calc R . .
H7B H 0.3512 0.7302 0.8798 0.097 Uiso 1 1 calc R . .
C8 C 0.4831(15) 0.6247(13) 0.9238(6) 0.075(5) Uani 1 1 d . . .
H8A H 0.4654 0.6730 0.9569 0.090 Uiso 1 1 calc R . .
H8B H 0.5072 0.5546 0.9413 0.090 Uiso 1 1 calc R . .
C9 C 0.7576(14) -0.1908(15) 0.4717(7) 0.079(5) Uani 1 1 d . . .
H9A H 0.7770 -0.2588 0.4556 0.094 Uiso 1 1 calc R . .
H9B H 0.7199 -0.1855 0.5138 0.094 Uiso 1 1 calc R . .
C10 C 0.8612(13) -0.1821(16) 0.4712(7) 0.090(6) Uani 1 1 d . . .
H10A H 0.9038 -0.2290 0.5020 0.107 Uiso 1 1 calc R . .
H10B H 0.9070 -0.2008 0.4309 0.107 Uiso 1 1 calc R . .
C11 C 0.4967(13) 0.2210(12) 0.4527(6) 0.064(4) Uani 1 1 d . . .
H11A H 0.4655 0.2177 0.4955 0.077 Uiso 1 1 calc R . .
H11B H 0.4386 0.2748 0.4315 0.077 Uiso 1 1 calc R . .
C12 C 0.5882(15) 0.2467(13) 0.4496(7) 0.077(5) Uani 1 1 d . . .
H12A H 0.6134 0.2579 0.4068 0.092 Uiso 1 1 calc R . .
H12B H 0.5623 0.3110 0.4722 0.092 Uiso 1 1 calc R . .
C13 C -0.169(2) 1.044(2) 1.0757(12) 0.141(9) Uani 1 1 d U . .
H13A H -0.2361 1.0833 1.0575 0.169 Uiso 1 1 calc R B .
H13B H -0.1253 1.0808 1.0678 0.169 Uiso 1 1 calc R . .
C14 C -0.106(2) 0.9374(19) 1.0519(11) 0.129(8) Uani 1 1 d DU B .
H14A H -0.1565 0.9088 1.0535 0.154 Uiso 1 1 calc R . .
H14B H -0.0774 0.9414 1.0086 0.154 Uiso 1 1 calc R . .
N15 N -0.069(3) 0.927(3) 1.2567(17) 0.150(13) Uiso 0.60 1 d P B 1
H15A H -0.0664 0.9874 1.2614 0.180 Uiso 0.50 1 calc PR B 1
H15B H -0.1337 0.9349 1.2774 0.180 Uiso 0.50 1 calc PR B 1
C15 C 0.025(2) 0.838(2) 1.2884(15) 0.072(7) Uiso 0.60 1 d P B 1
H15C H -0.0009 0.8256 1.3309 0.086 Uiso 0.50 1 calc PR B 1
H15D H 0.0886 0.8490 1.2864 0.086 Uiso 0.50 1 calc PR B 1
C16 C 0.046(4) 0.749(3) 1.243(2) 0.124(14) Uiso 0.60 1 d P B 1
H16A H 0.1057 0.6847 1.2570 0.149 Uiso 0.50 1 calc PR B 1
H16B H -0.0194 0.7395 1.2518 0.149 Uiso 0.50 1 calc PR B 1
N16 N 0.070(3) 0.749(3) 1.1834(18) 0.155(14) Uiso 0.60 1 d P B 1
H16C H 0.0618 0.6999 1.1655 0.186 Uiso 0.50 1 calc PR B 1
H16D H 0.1378 0.7425 1.1702 0.186 Uiso 0.50 1 calc PR B 1
N15' N -0.176(3) 1.026(4) 1.235(2) 0.20(3) Uiso 0.40 1 d PD B 2
H15E H -0.2166 1.0865 1.2160 0.243 Uiso 0.50 1 calc PR B 2
H15F H -0.2227 1.0047 1.2583 0.243 Uiso 0.50 1 calc PR B 2
C15' C -0.109(4) 1.039(3) 1.273(2) 0.110(16) Uiso 0.40 1 d PDU B 2
H15G H -0.1532 1.0988 1.3002 0.132 Uiso 0.50 1 calc PR B 2
H15H H -0.0499 1.0484 1.2476 0.132 Uiso 0.50 1 calc PR B 2
C16' C -0.062(3) 0.939(2) 1.3100(16) 0.058(8) Uiso 0.40 1 d PDU B 2
H16E H -0.1210 0.9254 1.3319 0.070 Uiso 0.50 1 calc PR B 2
H16F H -0.0212 0.9438 1.3400 0.070 Uiso 0.50 1 calc PR B 2
N16' N 0.035(4) 0.829(4) 1.252(2) 0.105(14) Uiso 0.40 1 d P B 2
H16G H 0.0360 0.7668 1.2625 0.126 Uiso 0.50 1 calc PR B 2
H16H H 0.1041 0.8206 1.2436 0.126 Uiso 0.50 1 calc PR B 2
N1 N 1.0353(10) -0.3501(10) 0.6937(6) 0.083(5) Uani 1 1 d . . .
H1C H 0.9645 -0.3023 0.6914 0.099 Uiso 1 1 calc R . .
H1D H 1.0783 -0.3196 0.6798 0.099 Uiso 1 1 calc R . .
N2 N 1.0614(9) -0.5286(8) 0.7529(6) 0.063(3) Uani 1 1 d . . .
H2C H 1.1317 -0.5808 0.7506 0.076 Uiso 1 1 calc R . .
H2D H 1.0179 -0.5481 0.7802 0.076 Uiso 1 1 calc R . .
N3 N 1.0638(11) -0.2710(9) 0.8094(8) 0.090(5) Uani 1 1 d . . .
H3C H 1.1196 -0.2650 0.7848 0.108 Uiso 1 1 calc R A 1
H3D H 1.0005 -0.2110 0.8064 0.108 Uiso 1 1 calc R A 1
N4 N 1.0718(9) -0.4447(8) 0.8682(5) 0.061(3) Uani 1 1 d . . .
H4C H 1.0238 -0.4690 0.8839 0.074 Uiso 1 1 calc R A 1
H4D H 1.1410 -0.4979 0.8687 0.074 Uiso 1 1 calc R A 1
N5 N 0.5511(11) 0.5225(9) 0.7179(5) 0.063(3) Uani 1 1 d . . .
H5C H 0.5715 0.4534 0.7167 0.075 Uiso 1 1 calc R . .
H5D H 0.4798 0.5593 0.7119 0.075 Uiso 1 1 calc R . .
N6 N 0.7112(11) 0.5495(9) 0.7562(5) 0.072(4) Uani 1 1 d . . .
H6C H 0.7080 0.6133 0.7542 0.086 Uiso 1 1 calc R . .
H6D H 0.7676 0.5051 0.7763 0.086 Uiso 1 1 calc R . .
N7 N 0.4172(9) 0.5883(8) 0.8407(5) 0.053(3) Uani 1 1 d . . .
H7C H 0.3698 0.6189 0.8131 0.063 Uiso 1 1 calc R . .
H7D H 0.4170 0.5275 0.8534 0.063 Uiso 1 1 calc R . .
N8 N 0.5709(11) 0.6262(8) 0.8777(5) 0.066(4) Uani 1 1 d . . .
H8C H 0.6369 0.5893 0.8910 0.079 Uiso 1 1 calc R . .
H8D H 0.5586 0.6927 0.8695 0.079 Uiso 1 1 calc R . .
N9 N 0.6862(9) -0.1096(10) 0.4349(4) 0.057(3) Uani 1 1 d . . .
H9C H 0.6180 -0.1042 0.4426 0.069 Uiso 1 1 calc R . .
H9D H 0.7125 -0.1232 0.3944 0.069 Uiso 1 1 calc R . .
N10 N 0.8257(9) -0.0707(10) 0.4858(4) 0.061(3) Uani 1 1 d . . .
H10C H 0.8770 -0.0526 0.4666 0.073 Uiso 1 1 calc R . .
H10D H 0.8197 -0.0640 0.5269 0.073 Uiso 1 1 calc R . .
N11 N 0.5408(9) 0.1199(9) 0.4234(4) 0.054(3) Uani 1 1 d . . .
H11C H 0.5554 0.1259 0.3820 0.065 Uiso 1 1 calc R . .
H11D H 0.4921 0.0945 0.4321 0.065 Uiso 1 1 calc R . .
N12 N 0.6800(11) 0.1602(11) 0.4765(5) 0.067(4) Uani 1 1 d . . .
H12C H 0.6705 0.1687 0.5176 0.081 Uiso 1 1 calc R . .
H12D H 0.7447 0.1584 0.4595 0.081 Uiso 1 1 calc R . .
N13 N -0.1943(13) 1.0272(13) 1.1429(8) 0.102(5) Uani 1 1 d . B .
H13C H -0.2512 1.0124 1.1501 0.122 Uiso 1 1 calc R . .
H13D H -0.2147 1.0865 1.1633 0.122 Uiso 1 1 calc R . .
N14 N -0.0154(18) 0.8644(17) 1.0816(10) 0.154(8) Uani 1 1 d DU B .
H14C H 0.0470 0.8678 1.0657 0.185 Uiso 1 1 calc R . .
H14D H -0.0036 0.7982 1.0782 0.185 Uiso 1 1 calc R . .
O1W O 0.7913(10) 0.7269(10) 0.6281(5) 0.026(3) Uani 0.50 1 d P . .
O2W O 0.4870(11) 0.4611(10) 0.5634(6) 0.030(3) Uani 0.50 1 d P . .
O3W O 0.3532(12) 0.4429(9) 0.9548(7) 0.037(3) Uani 0.50 1 d P . .
O4W O 0.3211(12) 0.6012(11) 0.6571(6) 0.037(4) Uani 0.50 1 d P . .
O5W O 0.9406(15) 0.0964(14) 0.5420(8) 0.058(5) Uiso 0.50 1 d P . .
O6W O -0.2875(15) 1.2380(14) 1.2498(8) 0.058(5) Uiso 0.50 1 d P . .
O7W O 0.8690(19) -0.5191(17) 0.8420(10) 0.082(6) Uiso 0.50 1 d P . .
O8W O 1.1638(18) -0.2579(16) 0.5867(10) 0.075(6) Uiso 0.50 1 d P . .
O9W O 0.127(3) 0.418(3) 1.0194(15) 0.067(9) Uiso 0.30 1 d P . .
O9W' O 0.273(3) 0.377(3) 1.0573(18) 0.046(10) Uiso 0.20 1 d P . .
O10W O 0.7520(18) 0.4026(17) 0.9453(10) 0.076(6) Uiso 0.50 1 d P . .
O11W O 0.892(3) 0.537(3) 0.5434(16) 0.053(9) Uiso 0.25 1 d P . .
O12W O 0.190(3) 0.807(2) 1.0144(14) 0.041(7) Uiso 0.25 1 d P . .
O13W O 0.8264(17) 0.3477(15) 0.5289(9) 0.065(5) Uiso 0.50 1 d P . .


_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
Cu1 N4 1.983(11) . ?
Cu1 N1 2.000(12) . ?
Cu1 N2 2.004(11) . ?
Cu1 N3 2.055(13) . ?
Cu1 O3 2.342(7) . ?
Cu2 N7 1.980(11) . ?
Cu2 N6 2.004(12) . ?
Cu2 N5 2.022(11) . ?
Cu2 N8 2.036(11) . ?
Cu2 O12 2.270(7) . ?
Cu3 N10 1.989(11) . ?
Cu3 N11 2.007(11) . ?
Cu3 N9 2.012(11) . ?
Cu3 N12 2.036(11) . ?
Cu3 O7 2.379(6) . ?
Cu4 N15 1.87(4) . ?
Cu4 N13 1.915(15) . ?
Cu4 N15' 2.03(2) . ?
Cu4 N14 2.07(2) . ?
Cu4 N16 2.26(4) . ?
Cu4 N16' 2.31(5) . ?
Nb1 O13 1.856(6) . ?
Nb1 O25 1.861(6) . ?
Nb1 O1 1.909(5) . ?
Nb1 O30 2.079(5) . ?
Nb1 O15 2.099(6) . ?
Nb1 O37 2.233(5) . ?
Nb1 Sb1 3.2918(9) . ?
Nb1 Nb2 3.3390(10) . ?
Nb2 O2 1.755(7) . ?
Nb2 O27 1.935(6) . ?
Nb2 O26 1.961(7) . ?
Nb2 O14 2.023(6) . ?
Nb2 O13 2.040(6) . ?
Nb2 O37 2.517(5) . ?
Nb3 O3 1.765(6) . ?
Nb3 O28 1.881(6) . ?
Nb3 O14 1.902(6) . ?
Nb3 O15 2.071(5) . ?
Nb3 O29 2.141(6) . ?
Nb3 O37 2.496(5) . ?
Nb3 Sb1 3.2857(9) . ?
Nb4 O4 1.751(7) . ?
Nb4 O26 1.901(7) . ?
Nb4 O16 1.918(6) . ?
Nb4 O33 2.110(6) . ?
Nb4 O18 2.118(7) . ?
Nb4 O38 2.398(6) . ?
Nb4 Sb2 3.2724(10) . ?
Nb4 Nb5 3.3297(11) . ?
Nb5 O5 1.744(6) . ?
Nb5 O16 1.953(7) . ?
Nb5 O17 1.956(6) . ?
Nb5 O25 2.026(6) . ?
Nb5 O31 2.039(6) . ?
Nb5 O38 2.414(6) . ?
Nb6 O6 1.779(6) . ?
Nb6 O36 1.903(7) . ?
Nb6 O17 1.922(6) . ?
Nb6 O18 2.093(7) . ?
Nb6 O34 2.107(6) . ?
Nb6 O38 2.433(5) . ?
Nb6 Sb2 3.2577(10) . ?
Nb7 O7 1.775(6) . ?
Nb7 O27 1.903(6) . ?
Nb7 O21 1.903(6) . ?
Nb7 O19 2.082(6) . ?
Nb7 O33 2.101(6) . ?
Nb7 O39 2.401(6) . ?
Nb7 Sb2 3.2930(10) . ?
Nb8 O8 1.764(6) . ?
Nb8 O20 1.898(6) . ?
Nb8 O35 1.907(6) . ?
Nb8 O19 2.083(6) . ?
Nb8 O34 2.148(6) . ?
Nb8 O39 2.475(5) . ?
Nb8 Sb2 3.2954(11) . ?
Nb9 O9 1.762(6) . ?
Nb9 O32 1.945(6) . ?
Nb9 O28 1.971(6) . ?
Nb9 O20 1.997(6) . ?
Nb9 O21 2.013(6) . ?
Nb9 O39 2.492(6) . ?
Nb10 O31 1.839(6) . ?
Nb10 O22 1.852(6) . ?
Nb10 O1 1.921(5) 2_657 ?
Nb10 O23 2.095(6) . ?
Nb10 O30 2.111(5) . ?
Nb10 O40 2.211(5) . ?
Nb10 Sb1 3.2866(9) . ?
Nb10 Nb12 3.3351(10) . ?
Nb11 O11 1.739(6) . ?
Nb11 O32 1.898(6) . ?
Nb11 O24 1.921(6) . ?
Nb11 O23 2.066(5) . ?
Nb11 O29 2.130(6) . ?
Nb11 O40 2.541(6) . ?
Nb11 Sb1 3.2782(9) . ?
Nb12 O12 1.772(6) . ?
Nb12 O35 1.938(6) . ?
Nb12 O36 1.961(7) . ?
Nb12 O24 1.960(7) . ?
Nb12 O22 2.061(6) . ?
Nb12 O40 2.504(5) . ?
Sb1 O30 1.990(5) . ?
Sb1 O29 2.008(5) . ?
Sb1 O23 2.148(6) . ?
Sb1 O15 2.172(6) . ?
Sb2 O34 1.982(7) . ?
Sb2 O33 1.997(6) . ?
Sb2 O18 2.139(6) . ?
Sb2 O19 2.159(6) . ?
Si1 O39 1.635(5) . ?
Si1 O38 1.650(6) . ?
Si1 O37 1.652(6) . ?
Si1 O40 1.653(6) . ?
O1 Nb10 1.921(5) 2_657 ?
C1 N1 1.47(2) . ?
C1 C2 1.52(3) . ?
C2 N2 1.45(2) . ?
C3 C4 1.40(5) . ?
C3 N3 1.43(3) . ?
C4 N4 1.48(4) . ?
C4' N4 1.55(4) . ?
C5 N5 1.462(17) . ?
C5 C6 1.48(2) . ?
C6 N6 1.505(19) . ?
C7 N7 1.450(16) . ?
C7 C8 1.52(2) . ?
C8 N8 1.449(16) . ?
C9 N9 1.417(19) . ?
C9 C10 1.50(2) . ?
C10 N10 1.49(2) . ?
C11 N11 1.450(17) . ?
C11 C12 1.48(2) . ?
C12 N12 1.46(2) . ?
C13 C14 1.45(3) . ?
C13 N13 1.48(3) . ?
C14 N14 1.417(17) . ?
N15 C15 1.54(4) . ?
C15 C16 1.58(5) . ?
C16 N16 1.29(4) . ?
N15' C15' 1.44(2) . ?
C15' C16' 1.493(19) . ?
C16' N16' 1.92(6) . ?

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
N4 Cu1 N1 178.4(5) . . ?
N4 Cu1 N2 95.8(5) . . ?
N1 Cu1 N2 83.8(6) . . ?
N4 Cu1 N3 83.2(6) . . ?
N1 Cu1 N3 97.0(7) . . ?
N2 Cu1 N3 172.4(5) . . ?
N4 Cu1 O3 90.1(4) . . ?
N1 Cu1 O3 91.4(4) . . ?
N2 Cu1 O3 91.0(4) . . ?
N3 Cu1 O3 96.5(4) . . ?
N7 Cu2 N6 172.1(5) . . ?
N7 Cu2 N5 94.5(5) . . ?
N6 Cu2 N5 84.9(5) . . ?
N7 Cu2 N8 84.9(5) . . ?
N6 Cu2 N8 94.2(5) . . ?
N5 Cu2 N8 168.3(5) . . ?
N7 Cu2 O12 94.9(3) . . ?
N6 Cu2 O12 92.9(4) . . ?
N5 Cu2 O12 100.6(4) . . ?
N8 Cu2 O12 91.0(4) . . ?
N10 Cu3 N11 175.5(4) . . ?
N10 Cu3 N9 84.6(5) . . ?
N11 Cu3 N9 94.9(5) . . ?
N10 Cu3 N12 95.3(5) . . ?
N11 Cu3 N12 84.9(5) . . ?
N9 Cu3 N12 176.7(4) . . ?
N10 Cu3 O7 94.7(3) . . ?
N11 Cu3 O7 89.7(3) . . ?
N9 Cu3 O7 87.9(3) . . ?
N12 Cu3 O7 95.4(3) . . ?
N15 Cu4 N13 112.1(13) . . ?
N15 Cu4 N15' 48.5(19) . . ?
N13 Cu4 N15' 63.6(17) . . ?
N15 Cu4 N14 161.9(14) . . ?
N13 Cu4 N14 85.5(8) . . ?
N15' Cu4 N14 148.7(19) . . ?
N15 Cu4 N16 85.0(15) . . ?
N13 Cu4 N16 159.3(12) . . ?
N15' Cu4 N16 132(2) . . ?
N14 Cu4 N16 78.8(12) . . ?
N15 Cu4 N16' 38.9(14) . . ?
N13 Cu4 N16' 151.0(13) . . ?
N15' Cu4 N16' 87(2) . . ?
N14 Cu4 N16' 123.4(13) . . ?
N16 Cu4 N16' 47.1(15) . . ?
O13 Nb1 O25 99.3(3) . . ?
O13 Nb1 O1 99.3(2) . . ?
O25 Nb1 O1 101.9(2) . . ?
O13 Nb1 O30 162.3(2) . . ?
O25 Nb1 O30 88.4(2) . . ?
O1 Nb1 O30 94.6(2) . . ?
O13 Nb1 O15 93.9(2) . . ?
O25 Nb1 O15 160.5(2) . . ?
O1 Nb1 O15 89.9(2) . . ?
O30 Nb1 O15 75.2(2) . . ?
O13 Nb1 O37 81.5(2) . . ?
O25 Nb1 O37 91.8(2) . . ?
O1 Nb1 O37 165.9(2) . . ?
O30 Nb1 O37 82.3(2) . . ?
O15 Nb1 O37 76.0(2) . . ?
O13 Nb1 Sb1 133.73(19) . . ?
O25 Nb1 Sb1 123.37(19) . . ?
O1 Nb1 Sb1 89.33(18) . . ?
O30 Nb1 Sb1 35.10(15) . . ?
O15 Nb1 Sb1 40.39(15) . . ?
O37 Nb1 Sb1 80.28(14) . . ?
O13 Nb1 Nb2 32.69(17) . . ?
O25 Nb1 Nb2 95.97(18) . . ?
O1 Nb1 Nb2 131.33(17) . . ?
O30 Nb1 Nb2 131.08(14) . . ?
O15 Nb1 Nb2 87.43(15) . . ?
O37 Nb1 Nb2 48.92(14) . . ?
Sb1 Nb1 Nb2 117.31(3) . . ?
O2 Nb2 O27 102.4(3) . . ?
O2 Nb2 O26 101.5(3) . . ?
O27 Nb2 O26 88.8(3) . . ?
O2 Nb2 O14 101.1(3) . . ?
O27 Nb2 O14 89.5(3) . . ?
O26 Nb2 O14 157.2(3) . . ?
O2 Nb2 O13 100.6(3) . . ?
O27 Nb2 O13 157.0(2) . . ?
O26 Nb2 O13 87.8(2) . . ?
O14 Nb2 O13 85.0(2) . . ?
O2 Nb2 O37 170.8(3) . . ?
O27 Nb2 O37 85.7(2) . . ?
O26 Nb2 O37 83.0(2) . . ?
O14 Nb2 O37 74.3(2) . . ?
O13 Nb2 O37 71.3(2) . . ?
O2 Nb2 Nb1 130.0(2) . . ?
O27 Nb2 Nb1 127.60(18) . . ?
O26 Nb2 Nb1 83.02(18) . . ?
O14 Nb2 Nb1 80.07(17) . . ?
O13 Nb2 Nb1 29.42(17) . . ?
O37 Nb2 Nb1 41.97(12) . . ?
O3 Nb3 O28 101.2(3) . . ?
O3 Nb3 O14 100.9(3) . . ?
O28 Nb3 O14 97.7(3) . . ?
O3 Nb3 O15 98.4(3) . . ?
O28 Nb3 O15 155.0(2) . . ?
O14 Nb3 O15 93.7(3) . . ?
O3 Nb3 O29 99.1(3) . . ?
O28 Nb3 O29 85.3(2) . . ?
O14 Nb3 O29 158.8(2) . . ?
O15 Nb3 O29 76.3(2) . . ?
O3 Nb3 O37 168.6(2) . . ?
O28 Nb3 O37 90.2(2) . . ?
O14 Nb3 O37 76.7(2) . . ?
O15 Nb3 O37 70.84(19) . . ?
O29 Nb3 O37 82.29(19) . . ?
O3 Nb3 Sb1 97.3(2) . . ?
O28 Nb3 Sb1 120.90(19) . . ?
O14 Nb3 Sb1 132.77(19) . . ?
O15 Nb3 Sb1 40.37(16) . . ?
O29 Nb3 Sb1 36.24(15) . . ?
O37 Nb3 Sb1 77.02(12) . . ?
O4 Nb4 O26 102.7(3) . . ?
O4 Nb4 O16 102.3(3) . . ?
O26 Nb4 O16 95.7(3) . . ?
O4 Nb4 O33 96.9(3) . . ?
O26 Nb4 O33 89.1(3) . . ?
O16 Nb4 O33 158.6(3) . . ?
O4 Nb4 O18 95.7(3) . . ?
O26 Nb4 O18 157.3(3) . . ?
O16 Nb4 O18 93.2(3) . . ?
O33 Nb4 O18 75.4(2) . . ?
O4 Nb4 O38 167.4(3) . . ?
O26 Nb4 O38 89.9(2) . . ?
O16 Nb4 O38 77.4(2) . . ?
O33 Nb4 O38 81.9(2) . . ?
O18 Nb4 O38 71.9(2) . . ?
O4 Nb4 Sb2 93.1(2) . . ?
O26 Nb4 Sb2 124.64(19) . . ?
O16 Nb4 Sb2 132.3(2) . . ?
O33 Nb4 Sb2 35.98(17) . . ?
O18 Nb4 Sb2 39.99(17) . . ?
O38 Nb4 Sb2 78.49(13) . . ?
O4 Nb4 Nb5 132.5(2) . . ?
O26 Nb4 Nb5 93.35(18) . . ?
O16 Nb4 Nb5 30.97(19) . . ?
O33 Nb4 Nb5 128.14(17) . . ?
O18 Nb4 Nb5 83.76(17) . . ?
O38 Nb4 Nb5 46.41(13) . . ?
Sb2 Nb4 Nb5 113.83(3) . . ?
O5 Nb5 O16 99.7(3) . . ?
O5 Nb5 O17 99.4(3) . . ?
O16 Nb5 O17 90.9(3) . . ?
O5 Nb5 O25 101.5(3) . . ?
O16 Nb5 O25 89.7(3) . . ?
O17 Nb5 O25 158.6(2) . . ?
O5 Nb5 O31 100.6(3) . . ?
O16 Nb5 O31 159.4(2) . . ?
O17 Nb5 O31 89.7(3) . . ?
O25 Nb5 O31 82.4(2) . . ?
O5 Nb5 O38 173.3(3) . . ?
O16 Nb5 O38 76.3(2) . . ?
O17 Nb5 O38 75.4(2) . . ?
O25 Nb5 O38 84.0(2) . . ?
O31 Nb5 O38 83.9(2) . . ?
O5 Nb5 Nb4 129.9(2) . . ?
O16 Nb5 Nb4 30.35(18) . . ?
O17 Nb5 Nb4 84.0(2) . . ?
O25 Nb5 Nb4 85.83(17) . . ?
O31 Nb5 Nb4 129.48(16) . . ?
O38 Nb5 Nb4 46.01(14) . . ?
O6 Nb6 O36 102.8(3) . . ?
O6 Nb6 O17 100.6(3) . . ?
O36 Nb6 O17 96.8(3) . . ?
O6 Nb6 O18 96.5(3) . . ?
O36 Nb6 O18 156.5(3) . . ?
O17 Nb6 O18 92.5(3) . . ?
O6 Nb6 O34 98.9(3) . . ?
O36 Nb6 O34 88.2(3) . . ?
O17 Nb6 O34 158.2(3) . . ?
O18 Nb6 O34 75.7(3) . . ?
O6 Nb6 O38 167.0(3) . . ?
O36 Nb6 O38 90.0(2) . . ?
O17 Nb6 O38 75.5(2) . . ?
O18 Nb6 O38 71.5(2) . . ?
O34 Nb6 O38 83.3(2) . . ?
O6 Nb6 Sb2 95.9(2) . . ?
O36 Nb6 Sb2 123.39(18) . . ?
O17 Nb6 Sb2 131.5(2) . . ?
O18 Nb6 Sb2 40.18(17) . . ?
O34 Nb6 Sb2 35.87(18) . . ?
O38 Nb6 Sb2 78.32(13) . . ?
O7 Nb7 O27 101.3(3) . . ?
O7 Nb7 O21 101.2(3) . . ?
O27 Nb7 O21 97.4(3) . . ?
O7 Nb7 O19 95.0(3) . . ?
O27 Nb7 O19 157.0(2) . . ?
O21 Nb7 O19 95.3(2) . . ?
O7 Nb7 O33 97.6(3) . . ?
O27 Nb7 O33 86.7(3) . . ?
O21 Nb7 O33 159.6(2) . . ?
O19 Nb7 O33 75.0(2) . . ?
O7 Nb7 O39 169.0(3) . . ?
O27 Nb7 O39 89.7(2) . . ?
O21 Nb7 O39 78.2(2) . . ?
O19 Nb7 O39 74.1(2) . . ?
O33 Nb7 O39 81.8(2) . . ?
O7 Nb7 Sb2 94.0(2) . . ?
O27 Nb7 Sb2 121.8(2) . . ?
O21 Nb7 Sb2 134.06(18) . . ?
O19 Nb7 Sb2 39.92(17) . . ?
O33 Nb7 Sb2 35.45(17) . . ?
O39 Nb7 Sb2 79.03(14) . . ?
O8 Nb8 O20 102.4(3) . . ?
O8 Nb8 O35 101.9(3) . . ?
O20 Nb8 O35 100.0(3) . . ?
O8 Nb8 O19 96.6(3) . . ?
O20 Nb8 O19 93.3(3) . . ?
O35 Nb8 O19 154.2(3) . . ?
O8 Nb8 O34 97.4(3) . . ?
O20 Nb8 O34 158.0(2) . . ?
O35 Nb8 O34 85.0(3) . . ?
O19 Nb8 O34 74.9(2) . . ?
O8 Nb8 O39 169.0(3) . . ?
O20 Nb8 O39 76.9(2) . . ?
O35 Nb8 O39 89.0(2) . . ?
O19 Nb8 O39 72.5(2) . . ?
O34 Nb8 O39 81.9(2) . . ?
O8 Nb8 Sb2 95.0(2) . . ?
O20 Nb8 Sb2 131.95(19) . . ?
O35 Nb8 Sb2 119.8(2) . . ?
O19 Nb8 Sb2 39.88(16) . . ?
O34 Nb8 Sb2 35.36(17) . . ?
O39 Nb8 Sb2 78.02(14) . . ?
O9 Nb9 O32 102.1(3) . . ?
O9 Nb9 O28 100.5(3) . . ?
O32 Nb9 O28 88.1(3) . . ?
O9 Nb9 O20 100.0(3) . . ?
O32 Nb9 O20 90.5(3) . . ?
O28 Nb9 O20 159.4(3) . . ?
O9 Nb9 O21 99.7(3) . . ?
O32 Nb9 O21 158.2(2) . . ?
O28 Nb9 O21 88.7(2) . . ?
O20 Nb9 O21 85.1(2) . . ?
O9 Nb9 O39 172.1(3) . . ?
O32 Nb9 O39 84.1(2) . . ?
O28 Nb9 O39 84.6(2) . . ?
O20 Nb9 O39 74.8(2) . . ?
O21 Nb9 O39 74.1(2) . . ?
O31 Nb10 O22 99.7(3) . . ?
O31 Nb10 O1 100.6(3) . 2_657 ?
O22 Nb10 O1 101.8(2) . 2_657 ?
O31 Nb10 O23 159.8(2) . . ?
O22 Nb10 O23 95.5(3) . . ?
O1 Nb10 O23 89.2(2) 2_657 . ?
O31 Nb10 O30 87.1(2) . . ?
O22 Nb10 O30 163.8(2) . . ?
O1 Nb10 O30 91.3(2) 2_657 . ?
O23 Nb10 O30 75.0(2) . . ?
O31 Nb10 O40 92.4(2) . . ?
O22 Nb10 O40 82.1(2) . . ?
O1 Nb10 O40 165.5(2) 2_657 . ?
O23 Nb10 O40 76.4(2) . . ?
O30 Nb10 O40 82.9(2) . . ?
O31 Nb10 Sb1 122.50(18) . . ?
O22 Nb10 Sb1 134.9(2) . . ?
O1 Nb10 Sb1 86.57(17) 2_657 . ?
O23 Nb10 Sb1 39.82(16) . . ?
O30 Nb10 Sb1 35.49(15) . . ?
O40 Nb10 Sb1 80.97(14) . . ?
O31 Nb10 Nb12 98.23(18) . . ?
O22 Nb10 Nb12 33.47(17) . . ?
O1 Nb10 Nb12 134.07(17) 2_657 . ?
O23 Nb10 Nb12 87.13(15) . . ?
O30 Nb10 Nb12 131.32(14) . . ?
O40 Nb10 Nb12 48.66(14) . . ?
Sb1 Nb10 Nb12 116.93(3) . . ?
O11 Nb11 O32 101.6(3) . . ?
O11 Nb11 O24 101.1(3) . . ?
O32 Nb11 O24 97.1(3) . . ?
O11 Nb11 O23 101.5(3) . . ?
O32 Nb11 O23 152.8(2) . . ?
O24 Nb11 O23 92.2(2) . . ?
O11 Nb11 O29 101.4(3) . . ?
O32 Nb11 O29 85.9(2) . . ?
O24 Nb11 O29 156.2(2) . . ?
O23 Nb11 O29 75.7(2) . . ?
O11 Nb11 O40 169.9(3) . . ?
O32 Nb11 O40 88.1(2) . . ?
O24 Nb11 O40 74.7(2) . . ?
O23 Nb11 O40 69.82(19) . . ?
O29 Nb11 O40 81.8(2) . . ?
O11 Nb11 Sb1 100.0(2) . . ?
O32 Nb11 Sb1 121.33(19) . . ?
O24 Nb11 Sb1 130.63(18) . . ?
O23 Nb11 Sb1 39.84(16) . . ?
O29 Nb11 Sb1 36.33(15) . . ?
O40 Nb11 Sb1 76.83(12) . . ?
O12 Nb12 O35 101.6(3) . . ?
O12 Nb12 O36 100.0(3) . . ?
O35 Nb12 O36 87.1(3) . . ?
O12 Nb12 O24 101.4(3) . . ?
O35 Nb12 O24 92.9(3) . . ?
O36 Nb12 O24 158.1(2) . . ?
O12 Nb12 O22 100.1(3) . . ?
O35 Nb12 O22 158.2(2) . . ?
O36 Nb12 O22 86.7(2) . . ?
O24 Nb12 O22 85.2(3) . . ?
O12 Nb12 O40 170.7(2) . . ?
O35 Nb12 O40 87.3(2) . . ?
O36 Nb12 O40 83.2(2) . . ?
O24 Nb12 O40 75.0(2) . . ?
O22 Nb12 O40 71.2(2) . . ?
O12 Nb12 Nb10 129.7(2) . . ?
O35 Nb12 Nb10 128.69(19) . . ?
O36 Nb12 Nb10 83.72(17) . . ?
O24 Nb12 Nb10 79.21(17) . . ?
O22 Nb12 Nb10 29.71(16) . . ?
O40 Nb12 Nb10 41.53(12) . . ?
O30 Sb1 O29 101.2(2) . . ?
O30 Sb1 O23 76.3(2) . . ?
O29 Sb1 O23 76.5(2) . . ?
O30 Sb1 O15 75.4(2) . . ?
O29 Sb1 O15 76.9(2) . . ?
O23 Sb1 O15 136.1(2) . . ?
O30 Sb1 Nb11 92.66(15) . . ?
O29 Sb1 Nb11 38.93(16) . . ?
O23 Sb1 Nb11 38.04(14) . . ?
O15 Sb1 Nb11 111.38(14) . . ?
O30 Sb1 Nb3 91.32(15) . . ?
O29 Sb1 Nb3 39.07(17) . . ?
O23 Sb1 Nb3 110.73(14) . . ?
O15 Sb1 Nb3 38.14(14) . . ?
Nb11 Sb1 Nb3 76.35(2) . . ?
O30 Sb1 Nb10 38.02(15) . . ?
O29 Sb1 Nb10 92.35(16) . . ?
O23 Sb1 Nb10 38.64(15) . . ?
O15 Sb1 Nb10 109.22(15) . . ?
Nb11 Sb1 Nb10 64.67(2) . . ?
Nb3 Sb1 Nb10 107.54(2) . . ?
O30 Sb1 Nb1 36.91(15) . . ?
O29 Sb1 Nb1 92.68(17) . . ?
O23 Sb1 Nb1 109.13(15) . . ?
O15 Sb1 Nb1 38.79(15) . . ?
Nb11 Sb1 Nb1 108.42(2) . . ?
Nb3 Sb1 Nb1 64.36(2) . . ?
Nb10 Sb1 Nb1 73.42(2) . . ?
O34 Sb2 O33 102.9(2) . . ?
O34 Sb2 O18 77.3(3) . . ?
O33 Sb2 O18 77.3(2) . . ?
O34 Sb2 O19 76.7(2) . . ?
O33 Sb2 O19 75.5(2) . . ?
O18 Sb2 O19 136.7(2) . . ?
O34 Sb2 Nb6 38.53(18) . . ?
O33 Sb2 Nb6 94.04(17) . . ?
O18 Sb2 Nb6 39.16(19) . . ?
O19 Sb2 Nb6 110.67(16) . . ?
O34 Sb2 Nb4 95.07(17) . . ?
O33 Sb2 Nb4 38.37(17) . . ?
O18 Sb2 Nb4 39.53(18) . . ?
O19 Sb2 Nb4 110.12(15) . . ?
Nb6 Sb2 Nb4 66.96(2) . . ?
O34 Sb2 Nb7 93.57(18) . . ?
O33 Sb2 Nb7 37.61(17) . . ?
O18 Sb2 Nb7 110.79(17) . . ?
O19 Sb2 Nb7 38.22(16) . . ?
Nb6 Sb2 Nb7 109.35(2) . . ?
Nb4 Sb2 Nb7 74.73(2) . . ?
O34 Sb2 Nb8 38.84(18) . . ?
O33 Sb2 Nb8 92.59(18) . . ?
O18 Sb2 Nb8 111.53(18) . . ?
O19 Sb2 Nb8 38.21(16) . . ?
Nb6 Sb2 Nb8 75.70(2) . . ?
Nb4 Sb2 Nb8 110.03(2) . . ?
Nb7 Sb2 Nb8 64.93(2) . . ?
O39 Si1 O38 112.8(3) . . ?
O39 Si1 O37 108.9(3) . . ?
O38 Si1 O37 108.1(3) . . ?
O39 Si1 O40 109.4(3) . . ?
O38 Si1 O40 107.1(3) . . ?
O37 Si1 O40 110.6(3) . . ?
Nb1 O1 Nb10 148.6(3) . 2_657 ?
Nb3 O3 Cu1 133.2(4) . . ?
Nb7 O7 Cu3 126.1(3) . . ?
Nb12 O12 Cu2 129.0(4) . . ?
Nb1 O13 Nb2 117.9(3) . . ?
Nb3 O14 Nb2 122.2(3) . . ?
Nb3 O15 Nb1 114.3(3) . . ?
Nb3 O15 Sb1 101.5(2) . . ?
Nb1 O15 Sb1 100.8(2) . . ?
Nb4 O16 Nb5 118.7(3) . . ?
Nb6 O17 Nb5 120.8(3) . . ?
Nb6 O18 Nb4 117.6(3) . . ?
Nb6 O18 Sb2 100.7(3) . . ?
Nb4 O18 Sb2 100.5(3) . . ?
Nb8 O19 Nb7 116.2(3) . . ?
Nb8 O19 Sb2 101.9(2) . . ?
Nb7 O19 Sb2 101.9(3) . . ?
Nb8 O20 Nb9 121.6(3) . . ?
Nb7 O21 Nb9 119.9(3) . . ?
Nb10 O22 Nb12 116.8(3) . . ?
Nb11 O23 Nb10 115.1(2) . . ?
Nb11 O23 Sb1 102.1(2) . . ?
Nb10 O23 Sb1 101.5(2) . . ?
Nb11 O24 Nb12 124.1(3) . . ?
Nb1 O25 Nb5 150.9(3) . . ?
Nb4 O26 Nb2 149.8(4) . . ?
Nb7 O27 Nb2 152.3(4) . . ?
Nb3 O28 Nb9 152.3(4) . . ?
Sb1 O29 Nb11 104.7(2) . . ?
Sb1 O29 Nb3 104.7(3) . . ?
Nb11 O29 Nb3 143.6(3) . . ?
Sb1 O30 Nb1 108.0(2) . . ?
Sb1 O30 Nb10 106.5(3) . . ?
Nb1 O30 Nb10 139.6(3) . . ?
Nb10 O31 Nb5 151.5(3) . . ?
Nb11 O32 Nb9 153.3(4) . . ?
Sb2 O33 Nb7 106.9(3) . . ?
Sb2 O33 Nb4 105.6(3) . . ?
Nb7 O33 Nb4 142.3(3) . . ?
Sb2 O34 Nb6 105.6(3) . . ?
Sb2 O34 Nb8 105.8(3) . . ?
Nb6 O34 Nb8 141.9(3) . . ?
Nb8 O35 Nb12 153.4(4) . . ?
Nb6 O36 Nb12 150.6(4) . . ?
Si1 O37 Nb1 126.7(3) . . ?
Si1 O37 Nb3 123.4(3) . . ?
Nb1 O37 Nb3 95.43(18) . . ?
Si1 O37 Nb2 124.4(3) . . ?
Nb1 O37 Nb2 89.12(18) . . ?
Nb3 O37 Nb2 86.57(17) . . ?
Si1 O38 Nb4 123.6(3) . . ?
Si1 O38 Nb5 127.2(3) . . ?
Nb4 O38 Nb5 87.58(19) . . ?
Si1 O38 Nb6 123.4(3) . . ?
Nb4 O38 Nb6 96.42(19) . . ?
Nb5 O38 Nb6 88.20(19) . . ?
Si1 O39 Nb7 125.0(3) . . ?
Si1 O39 Nb8 125.1(3) . . ?
Nb7 O39 Nb8 92.99(18) . . ?
Si1 O39 Nb9 127.7(3) . . ?
Nb7 O39 Nb9 87.72(18) . . ?
Nb8 O39 Nb9 86.42(17) . . ?
Si1 O40 Nb10 126.9(3) . . ?
Si1 O40 Nb12 125.4(3) . . ?
Nb10 O40 Nb12 89.81(19) . . ?
Si1 O40 Nb11 122.7(3) . . ?
Nb10 O40 Nb11 95.0(2) . . ?
Nb12 O40 Nb11 85.61(18) . . ?
N1 C1 C2 106.9(14) . . ?
N2 C2 C1 108.4(16) . . ?
C4 C3 N3 116(2) . . ?
C3 C4 N4 111(3) . . ?
N5 C5 C6 106.2(13) . . ?
C5 C6 N6 110.8(14) . . ?
N7 C7 C8 106.3(12) . . ?
N8 C8 C7 109.1(13) . . ?
N9 C9 C10 110.3(15) . . ?
N10 C10 C9 107.0(13) . . ?
N11 C11 C12 108.2(14) . . ?
N12 C12 C11 109.6(12) . . ?
C14 C13 N13 103(2) . . ?
N14 C14 C13 118(2) . . ?
C15 N15 Cu4 118(3) . . ?
N15 C15 C16 95(3) . . ?
N16 C16 C15 127(4) . . ?
C16 N16 Cu4 94(3) . . ?
C15' N15' Cu4 105(3) . . ?
N15' C15' C16' 105(4) . . ?
C15' C16' N16' 106(3) . . ?
C16' N16' Cu4 93(2) . . ?
C1 N1 Cu1 110.2(10) . . ?
C2 N2 Cu1 110.1(10) . . ?
C3 N3 Cu1 108.9(13) . . ?
C4 N4 C4' 28.5(18) . . ?
C4 N4 Cu1 110.8(17) . . ?
C4' N4 Cu1 113.3(16) . . ?
C5 N5 Cu2 108.4(10) . . ?
C6 N6 Cu2 107.5(10) . . ?
C7 N7 Cu2 110.5(10) . . ?
C8 N8 Cu2 105.7(8) . . ?
C9 N9 Cu3 106.6(9) . . ?
C10 N10 Cu3 110.4(8) . . ?
C11 N11 Cu3 105.8(8) . . ?
C12 N12 Cu3 107.1(8) . . ?
C13 N13 Cu4 110.5(15) . . ?
C14 N14 Cu4 102.7(16) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         2.200
_refine_diff_density_min         -2.341
_refine_diff_density_rms         0.313
####################################################################### 
# 
# 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_shelx
_audit_block_doi                 10.5517/cc13qs2p
_database_code_depnum_ccdc_archive 'CCDC 1034782'
_audit_update_record             
;
2014-11-18 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(H Nb12 O40 Sb2 Si), 9(C4 H16 Cu N4), 17(H2 O)'
_chemical_formula_sum            'C36 H180 Cu9 N36 Nb24 O97 Sb4 Si2'
_chemical_formula_weight         6015.04

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.7450(5)
_cell_length_b                   40.0530(14)
_cell_length_c                   19.1580(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.8120(10)
_cell_angle_gamma                90.00
_cell_volume                     11274.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5802
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48284
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         23.28
_reflns_number_total             16230
_reflns_number_gt                11844
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 0.000 -0.001 2173 844 ' '
2 -0.020 0.500 0.571 2173 845 ' '
_platon_squeeze_details          
;
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0792P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16230
_refine_ls_number_parameters     925
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1413
_refine_ls_wR_factor_gt          0.1337
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.91013(15) 0.37334(5) 0.22773(11) 0.0131(5) Uani 1 1 d . . .
Cu1 Cu 0.67649(8) 0.24703(3) 0.47993(6) 0.0324(3) Uani 1 1 d . . .
Cu2 Cu 0.17847(7) 0.25544(3) 0.47680(5) 0.0269(3) Uani 1 1 d . . .
Cu3 Cu 0.81822(9) 0.49531(3) 0.94828(6) 0.0387(3) Uani 1 1 d . . .
Cu4 Cu 0.41322(7) 0.37371(3) 0.22724(6) 0.0322(3) Uani 1 1 d . . .
Cu5 Cu 0.0000 0.5000 0.5000 0.0745(8) Uani 1 2 d S . .
Nb1 Nb 0.90492(5) 0.439470(19) 0.10062(4) 0.0245(2) Uani 1 1 d . . .
Nb2 Nb 0.72276(5) 0.433813(18) 0.19826(4) 0.02063(19) Uani 1 1 d . . .
Nb3 Nb 0.74663(5) 0.374352(17) 0.07604(4) 0.01683(18) Uani 1 1 d . . .
Nb4 Nb 0.89396(6) 0.438736(18) 0.35578(4) 0.0231(2) Uani 1 1 d . . .
Nb5 Nb 1.07667(5) 0.440715(18) 0.25794(4) 0.02081(19) Uani 1 1 d . . .
Nb6 Nb 1.07309(5) 0.380141(17) 0.37927(4) 0.01714(18) Uani 1 1 d . . .
Nb7 Nb 0.71525(5) 0.365058(18) 0.32904(4) 0.02040(19) Uani 1 1 d . . .
Nb8 Nb 0.74171(5) 0.305595(17) 0.20800(4) 0.01740(18) Uani 1 1 d . . .
Nb9 Nb 0.89317(5) 0.306872(18) 0.35100(4) 0.02027(19) Uani 1 1 d . . .
Nb10 Nb 0.94693(5) 0.308524(17) 0.10411(4) 0.01773(18) Uani 1 1 d . . .
Nb11 Nb 1.10755(5) 0.373908(17) 0.12673(4) 0.01828(19) Uani 1 1 d . . .
Nb12 Nb 1.09811(5) 0.312887(17) 0.24736(4) 0.01530(18) Uani 1 1 d . . .
Sb1 Sb 0.94125(4) 0.374098(15) 0.00488(3) 0.02967(17) Uani 1 1 d . . .
Sb2 Sb 0.88115(5) 0.371920(15) 0.45141(3) 0.03100(17) Uani 1 1 d . . .
O1 O 0.9310(4) 0.46960(12) 0.0379(3) 0.0270(14) Uani 1 1 d . . .
O2 O 0.6302(4) 0.46116(14) 0.2059(3) 0.0375(16) Uani 1 1 d . . .
O3 O 0.6806(4) 0.36333(13) -0.0021(3) 0.0248(14) Uani 1 1 d . . .
O4 O 0.8614(4) 0.46739(13) 0.4197(3) 0.0306(15) Uani 1 1 d . . .
O5 O 1.1550(4) 0.47395(13) 0.2501(3) 0.0327(16) Uani 1 1 d . . .
O6 O 1.1442(4) 0.37213(12) 0.4572(3) 0.0244(14) Uani 1 1 d . . .
O7 O 0.6258(4) 0.37260(13) 0.3838(3) 0.0257(14) Uani 1 1 d . . .
O8 O 0.6681(4) 0.27410(12) 0.1750(3) 0.0251(14) Uani 1 1 d . . .
O9 O 0.9135(4) 0.27812(13) 0.4216(3) 0.0225(13) Uani 1 1 d . . .
O10 O 0.9357(4) 0.27889(12) 0.0336(3) 0.0207(13) Uani 1 1 d . . .
O11 O 1.1960(4) 0.38477(14) 0.0733(3) 0.0266(14) Uani 1 1 d . . .
O12 O 1.1830(4) 0.28412(13) 0.2782(3) 0.0248(14) Uani 1 1 d . . .
O13 O 0.7991(4) 0.45985(13) 0.1354(3) 0.0249(14) Uani 1 1 d . . .
O14 O 0.6741(3) 0.40936(12) 0.1125(3) 0.0178(12) Uani 1 1 d . . .
O15 O 0.8316(4) 0.40786(12) 0.0315(3) 0.0188(13) Uani 1 1 d . . .
O16 O 0.9923(4) 0.46348(12) 0.3194(3) 0.0233(14) Uani 1 1 d . . .
O17 O 1.1315(4) 0.41849(12) 0.3445(3) 0.0205(13) Uani 1 1 d . . .
O18 O 0.9784(4) 0.40995(13) 0.4241(3) 0.0229(13) Uani 1 1 d . . .
O19 O 0.6644(3) 0.32792(12) 0.2749(3) 0.0168(12) Uani 1 1 d . . .
O20 O 0.7949(4) 0.33412(12) 0.3968(3) 0.0189(13) Uani 1 1 d . . .
O21 O 0.8044(4) 0.28288(12) 0.2922(3) 0.0187(13) Uani 1 1 d . . .
O22 O 1.0371(4) 0.34020(13) 0.0592(3) 0.0219(13) Uani 1 1 d . . .
O23 O 1.0424(4) 0.28816(12) 0.1628(3) 0.0186(13) Uani 1 1 d . . .
O24 O 1.1654(4) 0.33829(12) 0.1800(3) 0.0176(12) Uani 1 1 d . . .
O25 O 1.0030(4) 0.40322(12) 0.0787(3) 0.0192(13) Uani 1 1 d . . .
O26 O 0.9877(4) 0.45169(12) 0.1787(3) 0.0221(13) Uani 1 1 d . . .
O27 O 0.8080(4) 0.44870(12) 0.2776(3) 0.0252(14) Uani 1 1 d . . .
O28 O 0.6877(4) 0.39710(13) 0.2570(3) 0.0225(13) Uani 1 1 d . . .
O29 O 0.7145(3) 0.34028(12) 0.1382(3) 0.0175(12) Uani 1 1 d . . .
O30 O 0.8612(4) 0.34493(12) 0.0584(3) 0.0200(13) Uani 1 1 d . . .
O31 O 1.1246(4) 0.40660(12) 0.1985(3) 0.0186(13) Uani 1 1 d . . .
O32 O 0.8107(4) 0.39846(13) 0.3762(3) 0.0228(13) Uani 1 1 d . . .
O33 O 0.8501(4) 0.29487(12) 0.1575(3) 0.0177(12) Uani 1 1 d . . .
O34 O 0.9687(4) 0.34684(12) 0.3965(3) 0.0191(13) Uani 1 1 d . . .
O35 O 1.1176(4) 0.34837(13) 0.3177(3) 0.0184(12) Uani 1 1 d . . .
O36 O 0.9945(4) 0.29765(12) 0.2980(3) 0.0177(12) Uani 1 1 d . . .
O37 O 0.8469(4) 0.39623(12) 0.1708(3) 0.0160(12) Uani 1 1 d . . .
O38 O 0.9645(3) 0.39791(12) 0.2850(3) 0.0145(12) Uani 1 1 d . . .
O39 O 0.8430(4) 0.34760(11) 0.2669(3) 0.0171(12) Uani 1 1 d . . .
O40 O 0.9848(4) 0.35082(12) 0.1887(3) 0.0176(12) Uani 1 1 d . . .
C1 C 0.5999(11) 0.2423(4) 0.3428(8) 0.098(5) Uani 1 1 d U . .
H1A H 0.6394 0.2338 0.3088 0.117 Uiso 1 1 calc R . .
H1B H 0.5511 0.2543 0.3166 0.117 Uiso 1 1 calc R . .
C2 C 0.5604(10) 0.2144(3) 0.3733(7) 0.078(4) Uani 1 1 d U . .
H2A H 0.5694 0.1948 0.3451 0.093 Uiso 1 1 calc R . .
H2B H 0.4954 0.2180 0.3738 0.093 Uiso 1 1 calc R . .
C3 C 0.8029(11) 0.2749(4) 0.5795(7) 0.090(5) Uani 1 1 d U . .
H3A H 0.8161 0.2944 0.6087 0.108 Uiso 1 1 calc R . .
H3B H 0.8605 0.2658 0.5675 0.108 Uiso 1 1 calc R . .
C4 C 0.7568(9) 0.2500(3) 0.6201(7) 0.077(4) Uani 1 1 d . . .
H4A H 0.8018 0.2374 0.6493 0.093 Uiso 1 1 calc R . .
H4B H 0.7172 0.2612 0.6506 0.093 Uiso 1 1 calc R . .
C5 C 0.2916(7) 0.3014(2) 0.5588(5) 0.039(2) Uani 1 1 d . . .
H5A H 0.3480 0.3051 0.5876 0.046 Uiso 1 1 calc R . .
H5B H 0.2449 0.3157 0.5755 0.046 Uiso 1 1 calc R . .
C6 C 0.3043(7) 0.3089(2) 0.4812(5) 0.045(3) Uani 1 1 d . . .
H6A H 0.3169 0.3325 0.4750 0.054 Uiso 1 1 calc R . .
H6B H 0.3546 0.2961 0.4657 0.054 Uiso 1 1 calc R . .
C7 C 0.0488(6) 0.2028(2) 0.4717(5) 0.035(2) Uani 1 1 d . . .
H7A H -0.0020 0.2157 0.4859 0.042 Uiso 1 1 calc R . .
H7B H 0.0358 0.1793 0.4782 0.042 Uiso 1 1 calc R . .
C8 C 0.0635(6) 0.2097(2) 0.3955(5) 0.034(2) Uani 1 1 d . . .
H8A H 0.1075 0.1941 0.3793 0.041 Uiso 1 1 calc R . .
H8B H 0.0067 0.2071 0.3666 0.041 Uiso 1 1 calc R . .
C9 C 0.8156(9) 0.4409(3) 0.8527(6) 0.055(3) Uani 1 1 d . . .
H9A H 0.7872 0.4511 0.8105 0.066 Uiso 1 1 calc R . .
H9B H 0.8118 0.4168 0.8472 0.066 Uiso 1 1 calc R . .
C10 C 0.9146(8) 0.4516(2) 0.8640(6) 0.048(3) Uani 1 1 d . . .
H10A H 0.9455 0.4391 0.9024 0.058 Uiso 1 1 calc R . .
H10B H 0.9455 0.4476 0.8221 0.058 Uiso 1 1 calc R . .
C11 C 0.7340(8) 0.5377(3) 1.0434(6) 0.053(3) Uani 1 1 d . . .
H11A H 0.7107 0.5394 1.0891 0.064 Uiso 1 1 calc R . .
H11B H 0.6984 0.5523 1.0114 0.064 Uiso 1 1 calc R . .
C12 C 0.8331(8) 0.5481(3) 1.0482(6) 0.058(3) Uani 1 1 d . . .
H12A H 0.8388 0.5718 1.0579 0.070 Uiso 1 1 calc R . .
H12B H 0.8677 0.5359 1.0852 0.070 Uiso 1 1 calc R . .
C13 C 0.4072(9) 0.4230(3) 0.3307(7) 0.082(4) Uani 1 1 d . . .
H13A H 0.3723 0.4398 0.3036 0.098 Uiso 1 1 calc R . .
H13B H 0.4368 0.4336 0.3721 0.098 Uiso 1 1 calc R . .
C14 C 0.3459(9) 0.3959(4) 0.3515(6) 0.073(4) Uani 1 1 d U . .
H14A H 0.3794 0.3797 0.3812 0.087 Uiso 1 1 calc R . .
H14B H 0.2968 0.4049 0.3764 0.087 Uiso 1 1 calc R . .
C15 C 0.5042(7) 0.3384(3) 0.1219(6) 0.050(3) Uani 1 1 d . . .
H15A H 0.5324 0.3182 0.1413 0.060 Uiso 1 1 calc R . .
H15B H 0.5322 0.3438 0.0792 0.060 Uiso 1 1 calc R . .
C16 C 0.4036(9) 0.3325(4) 0.1049(7) 0.082(4) Uani 1 1 d U . .
H16A H 0.3795 0.3487 0.0706 0.099 Uiso 1 1 calc R . .
H16B H 0.3938 0.3104 0.0852 0.099 Uiso 1 1 calc R . .
C17 C -0.0213(11) 0.4504(3) 0.6047(8) 0.091(5) Uani 1 1 d U . .
H17A H -0.0264 0.4459 0.6539 0.110 Uiso 1 1 calc R . .
H17B H -0.0571 0.4338 0.5776 0.110 Uiso 1 1 calc R . .
C18 C 0.0690(11) 0.4482(3) 0.5902(8) 0.089(5) Uani 1 1 d U . .
H18A H 0.0901 0.4253 0.5955 0.106 Uiso 1 1 calc R . .
H18B H 0.1066 0.4621 0.6224 0.106 Uiso 1 1 calc R . .
N1 N 0.6499(6) 0.2655(2) 0.3841(4) 0.044(2) Uani 1 1 d . . .
H1C H 0.6181 0.2846 0.3862 0.053 Uiso 1 1 calc R . .
H1D H 0.7024 0.2701 0.3652 0.053 Uiso 1 1 calc R . .
N2 N 0.6000(5) 0.20871(18) 0.4448(4) 0.035(2) Uani 1 1 d . . .
H2C H 0.6343 0.1901 0.4458 0.042 Uiso 1 1 calc R . .
H2D H 0.5551 0.2055 0.4731 0.042 Uiso 1 1 calc R . .
N3 N 0.7515(6) 0.28515(19) 0.5166(4) 0.048(2) Uani 1 1 d . . .
H3C H 0.7893 0.2917 0.4847 0.058 Uiso 1 1 calc R . .
H3D H 0.7154 0.3025 0.5255 0.058 Uiso 1 1 calc R . .
N4 N 0.7047(5) 0.2277(2) 0.5751(4) 0.041(2) Uani 1 1 d . . .
H4C H 0.6524 0.2228 0.5939 0.049 Uiso 1 1 calc R . .
H4D H 0.7358 0.2085 0.5714 0.049 Uiso 1 1 calc R . .
N5 N 0.2642(5) 0.26598(17) 0.5613(4) 0.0286(18) Uani 1 1 d . . .
H5C H 0.2366 0.2621 0.6006 0.034 Uiso 1 1 calc R . .
H5D H 0.3137 0.2528 0.5617 0.034 Uiso 1 1 calc R . .
N6 N 0.2190(5) 0.29958(17) 0.4412(4) 0.0316(19) Uani 1 1 d . . .
H6C H 0.2276 0.2980 0.3953 0.038 Uiso 1 1 calc R . .
H6D H 0.1761 0.3152 0.4464 0.038 Uiso 1 1 calc R . .
N7 N 0.1331(5) 0.21217(16) 0.5137(4) 0.0257(17) Uani 1 1 d . . .
H7C H 0.1753 0.1961 0.5108 0.031 Uiso 1 1 calc R . .
H7D H 0.1221 0.2145 0.5589 0.031 Uiso 1 1 calc R . .
N8 N 0.0972(5) 0.24415(17) 0.3904(4) 0.0318(19) Uani 1 1 d . . .
H8C H 0.0499 0.2584 0.3860 0.038 Uiso 1 1 calc R . .
H8D H 0.1285 0.2462 0.3522 0.038 Uiso 1 1 calc R . .
N9 N 0.7677(6) 0.45145(19) 0.9146(4) 0.050(2) Uani 1 1 d . . .
H9C H 0.7760 0.4361 0.9489 0.060 Uiso 1 1 calc R . .
H9D H 0.7076 0.4533 0.9025 0.060 Uiso 1 1 calc R . .
N10 N 0.9147(5) 0.48754(17) 0.8805(4) 0.038(2) Uani 1 1 d . . .
H10C H 0.9020 0.4995 0.8411 0.046 Uiso 1 1 calc R . .
H10D H 0.9697 0.4938 0.9000 0.046 Uiso 1 1 calc R . .
N11 N 0.7261(6) 0.50288(19) 1.0182(4) 0.042(2) Uani 1 1 d . . .
H11C H 0.6697 0.4992 0.9980 0.051 Uiso 1 1 calc R . .
H11D H 0.7362 0.4887 1.0544 0.051 Uiso 1 1 calc R . .
N12 N 0.8663(6) 0.54032(18) 0.9798(4) 0.040(2) Uani 1 1 d . . .
H12C H 0.9275 0.5401 0.9834 0.048 Uiso 1 1 calc R . .
H12D H 0.8472 0.5560 0.9483 0.048 Uiso 1 1 calc R . .
N13 N 0.4749(6) 0.4084(2) 0.2890(4) 0.047(2) Uani 1 1 d . . .
H13C H 0.5200 0.3991 0.3171 0.057 Uiso 1 1 calc R . .
H13D H 0.4991 0.4243 0.2629 0.057 Uiso 1 1 calc R . .
N14 N 0.3105(6) 0.3805(2) 0.2853(4) 0.049(2) Uani 1 1 d . . .
H14C H 0.2686 0.3939 0.2629 0.059 Uiso 1 1 calc R . .
H14D H 0.2839 0.3608 0.2935 0.059 Uiso 1 1 calc R . .
N15 N 0.5201(5) 0.36566(19) 0.1721(4) 0.040(2) Uani 1 1 d . . .
H15C H 0.5325 0.3844 0.1489 0.047 Uiso 1 1 calc R . .
H15D H 0.5690 0.3608 0.2016 0.047 Uiso 1 1 calc R . .
N16 N 0.3557(5) 0.33565(18) 0.1699(4) 0.043(2) Uani 1 1 d . . .
H16C H 0.3608 0.3165 0.1946 0.052 Uiso 1 1 calc R . .
H16D H 0.2962 0.3398 0.1590 0.052 Uiso 1 1 calc R . .
N17 N -0.0583(8) 0.4856(2) 0.5862(5) 0.084(4) Uani 1 1 d . . .
H17C H -0.0438 0.4999 0.6217 0.101 Uiso 1 1 calc R . .
H17D H -0.1193 0.4851 0.5778 0.101 Uiso 1 1 calc R . .
N18 N 0.0760(8) 0.4598(2) 0.5157(5) 0.066(3) Uani 1 1 d . . .
H18C H 0.0566 0.4437 0.4855 0.079 Uiso 1 1 calc R . .
H18D H 0.1343 0.4646 0.5089 0.079 Uiso 1 1 calc R . .
O1W O 0.8192(5) 0.21916(15) 0.4457(4) 0.0483(19) Uani 1 1 d . . .
O2W O 0.5345(5) 0.27835(17) 0.5305(5) 0.071(3) Uani 1 1 d . . .
O3W O 0.3087(4) 0.22165(16) 0.4233(3) 0.0430(17) Uani 1 1 d . . .
O4W O 0.0440(4) 0.28630(16) 0.5280(3) 0.0388(16) Uani 1 1 d . . .
O5W O 0.7123(5) 0.52311(16) 0.8422(3) 0.0494(19) Uani 1 1 d . . .
O6W O 0.4760(9) 0.3192(3) 0.3086(7) 0.047(4) Uani 0.50 1 d PU . .
O7W O 0.3535(4) 0.41394(16) 0.1341(4) 0.0465(18) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 O38 1.633(5) . ?
Si1 O40 1.650(5) . ?
Si1 O39 1.652(5) . ?
Si1 O37 1.652(5) . ?
Cu1 N3 1.979(8) . ?
Cu1 N1 1.987(8) . ?
Cu1 N2 1.988(8) . ?
Cu1 N4 1.993(7) . ?
Cu2 N6 2.004(7) . ?
Cu2 N7 2.008(6) . ?
Cu2 N5 2.013(7) . ?
Cu2 N8 2.012(8) . ?
Cu3 N9 1.994(8) . ?
Cu3 N11 2.009(8) . ?
Cu3 N12 2.012(7) . ?
Cu3 N10 2.030(8) . ?
Cu4 N14 1.972(8) . ?
Cu4 N13 1.995(8) . ?
Cu4 N15 1.996(8) . ?
Cu4 N16 2.023(8) . ?
Cu5 N18 1.969(9) 3_566 ?
Cu5 N18 1.969(9) . ?
Cu5 N17 2.009(11) 3_566 ?
Cu5 N17 2.009(11) . ?
Nb1 O1 1.768(5) . ?
Nb1 O26 1.913(5) . ?
Nb1 O13 1.929(6) . ?
Nb1 O15 2.070(5) . ?
Nb1 O25 2.116(5) . ?
Nb1 O37 2.394(5) . ?
Nb1 Sb1 3.2668(10) . ?
Nb2 O2 1.766(6) . ?
Nb2 O28 1.948(5) . ?
Nb2 O27 1.982(6) . ?
Nb2 O14 1.994(5) . ?
Nb2 O13 2.008(5) . ?
Nb2 O37 2.461(5) . ?
Nb3 O3 1.771(5) . ?
Nb3 O29 1.897(5) . ?
Nb3 O14 1.930(5) . ?
Nb3 O15 2.069(5) . ?
Nb3 O30 2.110(5) . ?
Nb3 O37 2.408(5) . ?
Nb3 Sb1 3.2787(10) . ?
Nb4 O4 1.773(5) . ?
Nb4 O27 1.920(6) . ?
Nb4 O16 1.933(5) . ?
Nb4 O18 2.079(6) . ?
Nb4 O32 2.084(5) . ?
Nb4 O38 2.415(5) . ?
Nb4 Sb2 3.2577(10) . ?
Nb5 O5 1.777(5) . ?
Nb5 O31 1.949(5) . ?
Nb5 O26 1.971(5) . ?
Nb5 O17 1.992(5) . ?
Nb5 O16 2.003(5) . ?
Nb5 O38 2.467(5) . ?
Nb6 O6 1.781(6) . ?
Nb6 O35 1.890(5) . ?
Nb6 O17 1.908(5) . ?
Nb6 O18 2.077(5) . ?
Nb6 O34 2.084(5) . ?
Nb6 O38 2.418(5) . ?
Nb6 Sb2 3.2688(10) . ?
Nb7 O7 1.778(5) . ?
Nb7 O28 1.904(5) . ?
Nb7 O19 1.928(5) . ?
Nb7 O20 2.084(5) . ?
Nb7 O32 2.091(5) . ?
Nb7 O39 2.415(5) . ?
Nb7 Sb2 3.2547(10) . ?
Nb8 O8 1.748(5) . ?
Nb8 O29 1.946(5) . ?
Nb8 O33 1.983(5) . ?
Nb8 O19 1.997(5) . ?
Nb8 O21 2.009(5) . ?
Nb8 O39 2.460(5) . ?
Nb9 O9 1.782(5) . ?
Nb9 O36 1.911(5) . ?
Nb9 O21 1.913(5) . ?
Nb9 O20 2.067(5) . ?
Nb9 O34 2.098(5) . ?
Nb9 O39 2.368(5) . ?
Nb9 Sb2 3.2522(10) . ?
Nb10 O10 1.795(5) . ?
Nb10 O33 1.905(5) . ?
Nb10 O23 1.909(5) . ?
Nb10 O30 2.075(5) . ?
Nb10 O22 2.076(5) . ?
Nb10 O40 2.378(5) . ?
Nb10 Sb1 3.2392(9) . ?
Nb11 O11 1.778(5) . ?
Nb11 O31 1.900(5) . ?
Nb11 O24 1.913(5) . ?
Nb11 O22 2.085(5) . ?
Nb11 O25 2.089(5) . ?
Nb11 O40 2.429(5) . ?
Nb11 Sb1 3.2407(10) . ?
Nb12 O12 1.766(5) . ?
Nb12 O35 1.963(5) . ?
Nb12 O24 1.974(5) . ?
Nb12 O36 1.975(5) . ?
Nb12 O23 2.014(5) . ?
Nb12 O40 2.459(5) . ?
Sb1 O25 1.993(5) . ?
Sb1 O30 2.003(5) . ?
Sb1 O22 2.163(6) . ?
Sb1 O15 2.200(5) . ?
Sb2 O34 2.003(5) . ?
Sb2 O32 2.009(5) . ?
Sb2 O18 2.186(5) . ?
Sb2 O20 2.187(5) . ?
C1 N1 1.393(15) . ?
C1 C2 1.407(16) . ?
C2 N2 1.462(13) . ?
C3 N3 1.429(15) . ?
C3 C4 1.468(16) . ?
C4 N4 1.422(14) . ?
C5 N5 1.477(11) . ?
C5 C6 1.542(13) . ?
C6 N6 1.467(12) . ?
C7 N7 1.470(11) . ?
C7 C8 1.520(12) . ?
C8 N8 1.472(11) . ?
C9 N9 1.492(13) . ?
C9 C10 1.520(15) . ?
C10 N10 1.474(11) . ?
C11 N11 1.477(12) . ?
C11 C12 1.515(15) . ?
C12 N12 1.470(13) . ?
C13 N13 1.452(14) . ?
C13 C14 1.488(17) . ?
C14 N14 1.466(14) . ?
C15 N15 1.460(12) . ?
C15 C16 1.511(16) . ?
C16 N16 1.487(14) . ?
C17 C18 1.387(19) . ?
C17 N17 1.544(16) . ?
C18 N18 1.512(16) . ?

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
O38 Si1 O40 109.0(3) . . ?
O38 Si1 O39 110.5(3) . . ?
O40 Si1 O39 108.2(3) . . ?
O38 Si1 O37 109.1(3) . . ?
O40 Si1 O37 111.4(3) . . ?
O39 Si1 O37 108.6(3) . . ?
N3 Cu1 N1 95.8(3) . . ?
N3 Cu1 N2 178.9(3) . . ?
N1 Cu1 N2 85.0(3) . . ?
N3 Cu1 N4 84.7(3) . . ?
N1 Cu1 N4 178.7(4) . . ?
N2 Cu1 N4 94.5(3) . . ?
N6 Cu2 N7 177.6(3) . . ?
N6 Cu2 N5 84.5(3) . . ?
N7 Cu2 N5 96.0(3) . . ?
N6 Cu2 N8 95.3(3) . . ?
N7 Cu2 N8 84.4(3) . . ?
N5 Cu2 N8 177.6(3) . . ?
N9 Cu3 N11 95.4(4) . . ?
N9 Cu3 N12 178.1(3) . . ?
N11 Cu3 N12 84.6(3) . . ?
N9 Cu3 N10 85.4(3) . . ?
N11 Cu3 N10 178.0(3) . . ?
N12 Cu3 N10 94.7(3) . . ?
N14 Cu4 N13 84.4(3) . . ?
N14 Cu4 N15 177.4(4) . . ?
N13 Cu4 N15 94.9(3) . . ?
N14 Cu4 N16 95.9(3) . . ?
N13 Cu4 N16 175.3(3) . . ?
N15 Cu4 N16 84.5(3) . . ?
N18 Cu5 N18 179.998(3) 3_566 . ?
N18 Cu5 N17 85.3(4) 3_566 3_566 ?
N18 Cu5 N17 94.7(4) . 3_566 ?
N18 Cu5 N17 94.7(4) 3_566 . ?
N18 Cu5 N17 85.3(4) . . ?
N17 Cu5 N17 179.999(3) 3_566 . ?
O1 Nb1 O26 101.3(2) . . ?
O1 Nb1 O13 100.0(2) . . ?
O26 Nb1 O13 95.9(2) . . ?
O1 Nb1 O15 96.6(2) . . ?
O26 Nb1 O15 157.1(2) . . ?
O13 Nb1 O15 94.9(2) . . ?
O1 Nb1 O25 98.2(2) . . ?
O26 Nb1 O25 85.9(2) . . ?
O13 Nb1 O25 160.9(2) . . ?
O15 Nb1 O25 77.4(2) . . ?
O1 Nb1 O37 169.7(2) . . ?
O26 Nb1 O37 88.9(2) . . ?
O13 Nb1 O37 77.0(2) . . ?
O15 Nb1 O37 74.01(18) . . ?
O25 Nb1 O37 84.11(18) . . ?
O1 Nb1 Sb1 96.34(18) . . ?
O26 Nb1 Sb1 121.33(15) . . ?
O13 Nb1 Sb1 135.13(17) . . ?
O15 Nb1 Sb1 41.58(15) . . ?
O25 Nb1 Sb1 36.06(14) . . ?
O37 Nb1 Sb1 79.54(12) . . ?
O2 Nb2 O28 100.1(3) . . ?
O2 Nb2 O27 101.2(3) . . ?
O28 Nb2 O27 88.1(2) . . ?
O2 Nb2 O14 98.4(3) . . ?
O28 Nb2 O14 90.6(2) . . ?
O27 Nb2 O14 160.3(2) . . ?
O2 Nb2 O13 101.7(3) . . ?
O28 Nb2 O13 158.1(2) . . ?
O27 Nb2 O13 87.3(2) . . ?
O14 Nb2 O13 86.7(2) . . ?
O2 Nb2 O37 172.4(2) . . ?
O28 Nb2 O37 84.26(19) . . ?
O27 Nb2 O37 85.0(2) . . ?
O14 Nb2 O37 75.27(18) . . ?
O13 Nb2 O37 74.03(19) . . ?
O3 Nb3 O29 101.7(2) . . ?
O3 Nb3 O14 101.8(2) . . ?
O29 Nb3 O14 96.9(2) . . ?
O3 Nb3 O15 97.0(2) . . ?
O29 Nb3 O15 156.5(2) . . ?
O14 Nb3 O15 92.9(2) . . ?
O3 Nb3 O30 96.7(2) . . ?
O29 Nb3 O30 86.8(2) . . ?
O14 Nb3 O30 159.9(2) . . ?
O15 Nb3 O30 77.0(2) . . ?
O3 Nb3 O37 170.7(2) . . ?
O29 Nb3 O37 87.60(19) . . ?
O14 Nb3 O37 77.67(19) . . ?
O15 Nb3 O37 73.73(18) . . ?
O30 Nb3 O37 82.79(19) . . ?
O3 Nb3 Sb1 94.95(19) . . ?
O29 Nb3 Sb1 122.14(16) . . ?
O14 Nb3 Sb1 133.14(15) . . ?
O15 Nb3 Sb1 41.31(14) . . ?
O30 Nb3 Sb1 36.03(13) . . ?
O37 Nb3 Sb1 79.11(12) . . ?
O4 Nb4 O27 101.8(3) . . ?
O4 Nb4 O16 99.9(2) . . ?
O27 Nb4 O16 94.5(2) . . ?
O4 Nb4 O18 96.1(2) . . ?
O27 Nb4 O18 158.0(2) . . ?
O16 Nb4 O18 94.8(2) . . ?
O4 Nb4 O32 100.0(2) . . ?
O27 Nb4 O32 86.9(2) . . ?
O16 Nb4 O32 159.3(2) . . ?
O18 Nb4 O32 77.5(2) . . ?
O4 Nb4 O38 168.6(2) . . ?
O27 Nb4 O38 89.4(2) . . ?
O16 Nb4 O38 76.90(19) . . ?
O18 Nb4 O38 73.40(18) . . ?
O32 Nb4 O38 82.49(18) . . ?
O4 Nb4 Sb2 96.40(18) . . ?
O27 Nb4 Sb2 122.93(16) . . ?
O16 Nb4 Sb2 134.77(16) . . ?
O18 Nb4 Sb2 41.42(15) . . ?
O32 Nb4 Sb2 36.45(15) . . ?
O38 Nb4 Sb2 78.90(11) . . ?
O5 Nb5 O31 101.9(3) . . ?
O5 Nb5 O26 99.4(2) . . ?
O31 Nb5 O26 87.5(2) . . ?
O5 Nb5 O17 100.6(2) . . ?
O31 Nb5 O17 91.8(2) . . ?
O26 Nb5 O17 159.7(2) . . ?
O5 Nb5 O16 98.6(2) . . ?
O31 Nb5 O16 159.4(2) . . ?
O26 Nb5 O16 86.9(2) . . ?
O17 Nb5 O16 86.7(2) . . ?
O5 Nb5 O38 172.0(2) . . ?
O31 Nb5 O38 85.29(19) . . ?
O26 Nb5 O38 84.40(19) . . ?
O17 Nb5 O38 75.36(19) . . ?
O16 Nb5 O38 74.48(18) . . ?
O6 Nb6 O35 101.1(2) . . ?
O6 Nb6 O17 100.8(2) . . ?
O35 Nb6 O17 97.7(2) . . ?
O6 Nb6 O18 97.2(2) . . ?
O35 Nb6 O18 157.8(2) . . ?
O17 Nb6 O18 91.2(2) . . ?
O6 Nb6 O34 98.2(2) . . ?
O35 Nb6 O34 88.1(2) . . ?
O17 Nb6 O34 158.7(2) . . ?
O18 Nb6 O34 76.8(2) . . ?
O6 Nb6 O38 170.4(2) . . ?
O35 Nb6 O38 88.5(2) . . ?
O17 Nb6 O38 78.01(19) . . ?
O18 Nb6 O38 73.37(19) . . ?
O34 Nb6 O38 81.67(19) . . ?
O6 Nb6 Sb2 95.55(19) . . ?
O35 Nb6 Sb2 123.66(16) . . ?
O17 Nb6 Sb2 131.38(16) . . ?
O18 Nb6 Sb2 41.16(15) . . ?
O34 Nb6 Sb2 36.03(14) . . ?
O38 Nb6 Sb2 78.64(12) . . ?
O7 Nb7 O28 100.9(2) . . ?
O7 Nb7 O19 100.0(2) . . ?
O28 Nb7 O19 94.6(2) . . ?
O7 Nb7 O20 98.1(2) . . ?
O28 Nb7 O20 158.0(2) . . ?
O19 Nb7 O20 92.8(2) . . ?
O7 Nb7 O32 98.2(2) . . ?
O28 Nb7 O32 88.7(2) . . ?
O19 Nb7 O32 160.5(2) . . ?
O20 Nb7 O32 77.7(2) . . ?
O7 Nb7 O39 171.0(2) . . ?
O28 Nb7 O39 88.0(2) . . ?
O19 Nb7 O39 78.20(19) . . ?
O20 Nb7 O39 73.30(18) . . ?
O32 Nb7 O39 82.73(19) . . ?
O7 Nb7 Sb2 96.4(2) . . ?
O28 Nb7 Sb2 124.57(17) . . ?
O19 Nb7 Sb2 133.39(16) . . ?
O20 Nb7 Sb2 41.54(14) . . ?
O32 Nb7 Sb2 36.58(14) . . ?
O39 Nb7 Sb2 79.02(13) . . ?
O8 Nb8 O29 100.4(2) . . ?
O8 Nb8 O33 99.7(2) . . ?
O29 Nb8 O33 87.0(2) . . ?
O8 Nb8 O19 100.7(2) . . ?
O29 Nb8 O19 91.5(2) . . ?
O33 Nb8 O19 159.5(2) . . ?
O8 Nb8 O21 101.2(2) . . ?
O29 Nb8 O21 158.3(2) . . ?
O33 Nb8 O21 87.6(2) . . ?
O19 Nb8 O21 86.3(2) . . ?
O8 Nb8 O39 174.0(2) . . ?
O29 Nb8 O39 84.77(19) . . ?
O33 Nb8 O39 83.61(19) . . ?
O19 Nb8 O39 75.92(19) . . ?
O21 Nb8 O39 73.79(18) . . ?
O9 Nb9 O36 100.9(2) . . ?
O9 Nb9 O21 100.7(2) . . ?
O36 Nb9 O21 96.7(2) . . ?
O9 Nb9 O20 95.7(2) . . ?
O36 Nb9 O20 159.1(2) . . ?
O21 Nb9 O20 92.6(2) . . ?
O9 Nb9 O34 97.4(2) . . ?
O36 Nb9 O34 87.5(2) . . ?
O21 Nb9 O34 160.3(2) . . ?
O20 Nb9 O34 77.7(2) . . ?
O9 Nb9 O39 170.0(2) . . ?
O36 Nb9 O39 89.1(2) . . ?
O21 Nb9 O39 77.65(19) . . ?
O20 Nb9 O39 74.63(19) . . ?
O34 Nb9 O39 83.21(19) . . ?
O9 Nb9 Sb2 94.77(17) . . ?
O36 Nb9 Sb2 123.55(15) . . ?
O21 Nb9 Sb2 133.01(16) . . ?
O20 Nb9 Sb2 41.51(14) . . ?
O34 Nb9 Sb2 36.51(14) . . ?
O39 Nb9 Sb2 79.71(12) . . ?
O10 Nb10 O33 100.8(2) . . ?
O10 Nb10 O23 100.2(2) . . ?
O33 Nb10 O23 96.3(2) . . ?
O10 Nb10 O30 97.6(2) . . ?
O33 Nb10 O30 88.3(2) . . ?
O23 Nb10 O30 160.3(2) . . ?
O10 Nb10 O22 96.6(2) . . ?
O33 Nb10 O22 158.9(2) . . ?
O23 Nb10 O22 92.2(2) . . ?
O30 Nb10 O22 77.5(2) . . ?
O10 Nb10 O40 170.1(2) . . ?
O33 Nb10 O40 89.0(2) . . ?
O23 Nb10 O40 77.52(19) . . ?
O30 Nb10 O40 83.48(19) . . ?
O22 Nb10 O40 74.02(19) . . ?
O10 Nb10 Sb1 95.64(16) . . ?
O33 Nb10 Sb1 124.33(15) . . ?
O23 Nb10 Sb1 132.34(16) . . ?
O30 Nb10 Sb1 36.65(14) . . ?
O22 Nb10 Sb1 41.16(16) . . ?
O40 Nb10 Sb1 79.35(12) . . ?
O11 Nb11 O31 100.9(2) . . ?
O11 Nb11 O24 100.0(2) . . ?
O31 Nb11 O24 95.8(2) . . ?
O11 Nb11 O22 98.8(2) . . ?
O31 Nb11 O22 157.5(2) . . ?
O24 Nb11 O22 91.4(2) . . ?
O11 Nb11 O25 99.1(2) . . ?
O31 Nb11 O25 88.8(2) . . ?
O24 Nb11 O25 159.0(2) . . ?
O22 Nb11 O25 77.3(2) . . ?
O11 Nb11 O40 170.7(2) . . ?
O31 Nb11 O40 88.2(2) . . ?
O24 Nb11 O40 76.85(19) . . ?
O22 Nb11 O40 72.75(18) . . ?
O25 Nb11 O40 82.91(19) . . ?
O11 Nb11 Sb1 97.59(19) . . ?
O31 Nb11 Sb1 124.46(16) . . ?
O24 Nb11 Sb1 131.52(15) . . ?
O22 Nb11 Sb1 41.18(15) . . ?
O25 Nb11 Sb1 36.44(14) . . ?
O40 Nb11 Sb1 78.64(12) . . ?
O12 Nb12 O35 100.6(2) . . ?
O12 Nb12 O24 100.0(2) . . ?
O35 Nb12 O24 91.3(2) . . ?
O12 Nb12 O36 100.9(2) . . ?
O35 Nb12 O36 87.8(2) . . ?
O24 Nb12 O36 158.8(2) . . ?
O12 Nb12 O23 100.3(2) . . ?
O35 Nb12 O23 159.1(2) . . ?
O24 Nb12 O23 85.5(2) . . ?
O36 Nb12 O23 87.9(2) . . ?
O12 Nb12 O40 172.4(2) . . ?
O35 Nb12 O40 85.47(19) . . ?
O24 Nb12 O40 75.08(19) . . ?
O36 Nb12 O40 83.77(19) . . ?
O23 Nb12 O40 73.76(18) . . ?
O25 Sb1 O30 103.4(2) . . ?
O25 Sb1 O22 77.6(2) . . ?
O30 Sb1 O22 77.1(2) . . ?
O25 Sb1 O15 77.1(2) . . ?
O30 Sb1 O15 76.3(2) . . ?
O22 Sb1 O15 137.50(19) . . ?
O25 Sb1 Nb10 94.03(14) . . ?
O30 Sb1 Nb10 38.18(16) . . ?
O22 Sb1 Nb10 39.17(14) . . ?
O15 Sb1 Nb10 110.22(13) . . ?
O25 Sb1 Nb11 38.49(15) . . ?
O30 Sb1 Nb11 94.15(16) . . ?
O22 Sb1 Nb11 39.41(14) . . ?
O15 Sb1 Nb11 111.14(13) . . ?
Nb10 Sb1 Nb11 66.08(2) . . ?
O25 Sb1 Nb1 38.67(15) . . ?
O30 Sb1 Nb1 92.78(14) . . ?
O22 Sb1 Nb1 111.35(14) . . ?
O15 Sb1 Nb1 38.64(13) . . ?
Nb10 Sb1 Nb1 108.53(2) . . ?
Nb11 Sb1 Nb1 75.36(2) . . ?
O25 Sb1 Nb3 93.83(15) . . ?
O30 Sb1 Nb3 38.29(15) . . ?
O22 Sb1 Nb3 111.16(14) . . ?
O15 Sb1 Nb3 38.37(13) . . ?
Nb10 Sb1 Nb3 74.87(2) . . ?
Nb11 Sb1 Nb3 109.65(3) . . ?
Nb1 Sb1 Nb3 64.76(2) . . ?
O34 Sb2 O32 101.9(2) . . ?
O34 Sb2 O18 76.0(2) . . ?
O32 Sb2 O18 76.7(2) . . ?
O34 Sb2 O20 77.0(2) . . ?
O32 Sb2 O20 77.2(2) . . ?
O18 Sb2 O20 137.3(2) . . ?
O34 Sb2 Nb9 38.55(15) . . ?
O32 Sb2 Nb9 92.87(15) . . ?
O18 Sb2 Nb9 110.32(14) . . ?
O20 Sb2 Nb9 38.79(14) . . ?
O34 Sb2 Nb7 93.33(15) . . ?
O32 Sb2 Nb7 38.35(15) . . ?
O18 Sb2 Nb7 110.80(15) . . ?
O20 Sb2 Nb7 39.19(13) . . ?
Nb9 Sb2 Nb7 65.24(2) . . ?
O34 Sb2 Nb4 92.65(14) . . ?
O32 Sb2 Nb4 38.05(16) . . ?
O18 Sb2 Nb4 38.98(15) . . ?
O20 Sb2 Nb4 110.99(14) . . ?
Nb9 Sb2 Nb4 108.47(3) . . ?
Nb7 Sb2 Nb4 74.92(2) . . ?
O34 Sb2 Nb6 37.74(15) . . ?
O32 Sb2 Nb6 93.27(16) . . ?
O18 Sb2 Nb6 38.71(14) . . ?
O20 Sb2 Nb6 110.89(14) . . ?
Nb9 Sb2 Nb6 74.84(2) . . ?
Nb7 Sb2 Nb6 109.21(3) . . ?
Nb4 Sb2 Nb6 65.57(2) . . ?
Nb1 O13 Nb2 119.9(3) . . ?
Nb3 O14 Nb2 118.9(3) . . ?
Nb3 O15 Nb1 115.8(2) . . ?
Nb3 O15 Sb1 100.3(2) . . ?
Nb1 O15 Sb1 99.8(2) . . ?
Nb4 O16 Nb5 120.0(2) . . ?
Nb6 O17 Nb5 119.1(3) . . ?
Nb6 O18 Nb4 116.5(2) . . ?
Nb6 O18 Sb2 100.1(2) . . ?
Nb4 O18 Sb2 99.6(2) . . ?
Nb7 O19 Nb8 118.3(2) . . ?
Nb9 O20 Nb7 115.4(2) . . ?
Nb9 O20 Sb2 99.7(2) . . ?
Nb7 O20 Sb2 99.3(2) . . ?
Nb9 O21 Nb8 119.4(2) . . ?
Nb10 O22 Nb11 116.2(2) . . ?
Nb10 O22 Sb1 99.7(2) . . ?
Nb11 O22 Sb1 99.4(2) . . ?
Nb10 O23 Nb12 119.6(2) . . ?
Nb11 O24 Nb12 120.5(3) . . ?
Sb1 O25 Nb11 105.1(2) . . ?
Sb1 O25 Nb1 105.3(2) . . ?
Nb11 O25 Nb1 142.1(3) . . ?
Nb1 O26 Nb5 152.2(3) . . ?
Nb4 O27 Nb2 150.5(3) . . ?
Nb7 O28 Nb2 151.3(3) . . ?
Nb3 O29 Nb8 153.7(3) . . ?
Sb1 O30 Nb10 105.2(2) . . ?
Sb1 O30 Nb3 105.7(2) . . ?
Nb10 O30 Nb3 142.4(3) . . ?
Nb11 O31 Nb5 150.9(3) . . ?
Sb2 O32 Nb4 105.5(3) . . ?
Sb2 O32 Nb7 105.1(2) . . ?
Nb4 O32 Nb7 143.1(3) . . ?
Nb10 O33 Nb8 150.5(3) . . ?
Sb2 O34 Nb6 106.2(2) . . ?
Sb2 O34 Nb9 104.9(2) . . ?
Nb6 O34 Nb9 142.8(3) . . ?
Nb6 O35 Nb12 151.4(3) . . ?
Nb9 O36 Nb12 150.8(3) . . ?
Si1 O37 Nb1 124.3(3) . . ?
Si1 O37 Nb3 124.9(3) . . ?
Nb1 O37 Nb3 93.78(17) . . ?
Si1 O37 Nb2 125.9(3) . . ?
Nb1 O37 Nb2 89.13(16) . . ?
Nb3 O37 Nb2 87.89(18) . . ?
Si1 O38 Nb4 125.1(3) . . ?
Si1 O38 Nb6 125.6(3) . . ?
Nb4 O38 Nb6 93.97(17) . . ?
Si1 O38 Nb5 125.3(3) . . ?
Nb4 O38 Nb5 88.58(16) . . ?
Nb6 O38 Nb5 87.01(17) . . ?
Si1 O39 Nb9 125.0(3) . . ?
Si1 O39 Nb7 124.4(3) . . ?
Nb9 O39 Nb7 94.34(17) . . ?
Si1 O39 Nb8 125.6(3) . . ?
Nb9 O39 Nb8 89.08(16) . . ?
Nb7 O39 Nb8 87.44(17) . . ?
Si1 O40 Nb10 124.8(3) . . ?
Si1 O40 Nb11 124.5(3) . . ?
Nb10 O40 Nb11 94.61(18) . . ?
Si1 O40 Nb12 125.7(3) . . ?
Nb10 O40 Nb12 89.03(17) . . ?
Nb11 O40 Nb12 87.30(17) . . ?
N1 C1 C2 120.7(12) . . ?
C1 C2 N2 111.5(11) . . ?
N3 C3 C4 113.9(12) . . ?
N4 C4 C3 110.9(11) . . ?
N5 C5 C6 106.0(8) . . ?
N6 C6 C5 106.6(8) . . ?
N7 C7 C8 107.2(7) . . ?
N8 C8 C7 108.2(7) . . ?
N9 C9 C10 108.6(9) . . ?
N10 C10 C9 106.9(9) . . ?
N11 C11 C12 109.3(9) . . ?
N12 C12 C11 106.2(10) . . ?
N13 C13 C14 108.3(10) . . ?
N14 C14 C13 104.7(10) . . ?
N15 C15 C16 111.1(9) . . ?
N16 C16 C15 109.5(10) . . ?
C18 C17 N17 109.8(13) . . ?
C17 C18 N18 108.2(13) . . ?
C1 N1 Cu1 109.3(7) . . ?
C2 N2 Cu1 111.6(6) . . ?
C3 N3 Cu1 108.7(7) . . ?
C4 N4 Cu1 111.8(6) . . ?
C5 N5 Cu2 109.3(5) . . ?
C6 N6 Cu2 108.3(6) . . ?
C7 N7 Cu2 108.7(5) . . ?
C8 N8 Cu2 109.7(5) . . ?
C9 N9 Cu3 108.6(6) . . ?
C10 N10 Cu3 107.4(6) . . ?
C11 N11 Cu3 108.7(6) . . ?
C12 N12 Cu3 108.9(6) . . ?
C13 N13 Cu4 107.8(7) . . ?
C14 N14 Cu4 108.1(7) . . ?
C15 N15 Cu4 112.3(6) . . ?
C16 N16 Cu4 108.1(7) . . ?
C17 N17 Cu5 106.5(8) . . ?
C18 N18 Cu5 108.3(8) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        23.28
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         4.015
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.168
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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_shelx
_audit_block_doi                 10.5517/cc13qs3q
_database_code_depnum_ccdc_archive 'CCDC 1034783'
_audit_update_record             
;
2014-11-18 deposited with the CCDC.
2015-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'H V Nb12 O40 Sb2, 4(C4 H18 Cu N4 O), 22(H2 O)'
_chemical_formula_sum            'C16 H117 Cu4 N16 Nb12 O66 Sb2 V'
_chemical_formula_weight         3253.78

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   25.7020(5)
_cell_length_b                   25.7020(5)
_cell_length_c                   16.2360(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10725.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       platelet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6344
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18533
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4724
_reflns_number_gt                3864
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0696P)²+134.8337P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4724
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1407
_refine_ls_wR_factor_gt          0.1326
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.77145(4) 0.33506(4) 0.42218(6) 0.0368(3) Uani 1 1 d . . .
Nb1 Nb 0.63788(2) 0.20895(2) 0.36969(4) 0.02036(19) Uani 1 1 d . . .
Nb2 Nb 0.54511(2) 0.15508(2) 0.52770(4) 0.02071(19) Uani 1 1 d . . .
Nb3 Nb 0.58950(2) 0.30548(2) 0.52677(4) 0.02061(19) Uani 1 1 d . . .
Sb1 Sb 0.5000 0.2500 0.64291(4) 0.0265(2) Uani 1 2 d S . .
V1 V 0.5000 0.2500 0.3750 0.0082(4) Uani 1 4 d S . .
C1 C 0.7877(4) 0.2687(6) 0.5591(9) 0.096(5) Uani 1 1 d . . .
H1A H 0.7885 0.2881 0.6104 0.115 Uiso 1 1 calc R . .
H1B H 0.7813 0.2326 0.5729 0.115 Uiso 1 1 calc R . .
C2 C 0.8365(4) 0.2722(6) 0.5227(9) 0.098(5) Uani 1 1 d . . .
H2A H 0.8430 0.2405 0.4919 0.117 Uiso 1 1 calc R . .
H2B H 0.8626 0.2746 0.5657 0.117 Uiso 1 1 calc R . .
C3 C 0.7059(4) 0.4009(4) 0.3251(8) 0.067(3) Uani 1 1 d . . .
H3A H 0.6775 0.4009 0.2857 0.081 Uiso 1 1 calc R . .
H3B H 0.7045 0.4333 0.3559 0.081 Uiso 1 1 calc R . .
C4 C 0.7556(4) 0.3969(5) 0.2818(8) 0.077(4) Uani 1 1 d . . .
H4A H 0.7528 0.3703 0.2395 0.092 Uiso 1 1 calc R . .
H4B H 0.7630 0.4297 0.2547 0.092 Uiso 1 1 calc R . .
N1 N 0.7448(3) 0.2872(3) 0.5113(5) 0.0489(19) Uani 1 1 d . . .
H1C H 0.7223 0.3044 0.5439 0.059 Uiso 1 1 calc R . .
H1D H 0.7279 0.2601 0.4885 0.059 Uiso 1 1 calc R . .
N2 N 0.8425(3) 0.3172(3) 0.4666(5) 0.0502(19) Uani 1 1 d . . .
H2C H 0.8642 0.3091 0.4250 0.060 Uiso 1 1 calc R . .
H2D H 0.8559 0.3446 0.4940 0.060 Uiso 1 1 calc R . .
N3 N 0.7004(3) 0.3562(3) 0.3820(5) 0.0404(17) Uani 1 1 d . . .
H3C H 0.6852 0.3294 0.3558 0.048 Uiso 1 1 calc R . .
H3D H 0.6803 0.3652 0.4251 0.048 Uiso 1 1 calc R . .
N4 N 0.7978(3) 0.3841(3) 0.3356(5) 0.0464(18) Uani 1 1 d . . .
H4C H 0.8103 0.4132 0.3593 0.056 Uiso 1 1 calc R . .
H4D H 0.8237 0.3690 0.3068 0.056 Uiso 1 1 calc R . .
O1 O 0.70218(18) 0.1913(2) 0.3956(3) 0.0323(12) Uani 1 1 d . . .
O2 O 0.5807(2) 0.1234(2) 0.6054(3) 0.0347(12) Uani 1 1 d . . .
O3 O 0.6365(2) 0.3166(2) 0.6039(3) 0.0338(12) Uani 1 1 d . . .
O4 O 0.59046(18) 0.37162(18) 0.4718(3) 0.0250(10) Uani 1 1 d . . .
O5 O 0.65069(17) 0.26138(17) 0.2792(3) 0.0239(10) Uani 1 1 d . . .
O6 O 0.47786(17) 0.17498(17) 0.5939(3) 0.0238(10) Uani 1 1 d . . .
O7 O 0.55767(18) 0.23351(17) 0.5643(3) 0.0236(10) Uani 1 1 d . . .
O8 O 0.62654(17) 0.26778(18) 0.4462(3) 0.0239(10) Uani 1 1 d . . .
O9 O 0.59666(18) 0.16788(18) 0.4459(3) 0.0257(11) Uani 1 1 d . . .
O10 O 0.55284(17) 0.23409(16) 0.3147(3) 0.0198(10) Uani 1 1 d . . .
O1W O 0.7751(2) 0.2647(2) 0.3341(4) 0.0472(16) Uani 1 1 d . . .
O2W O 0.6233(3) 0.0359(3) 0.6768(6) 0.087(3) Uani 1 1 d . . .
O3W O 0.6912(4) 0.1539(5) 0.5741(7) 0.119(4) Uani 1 1 d . . .
O4W O 0.7170(6) 0.3753(6) 0.6698(10) 0.175(6) Uiso 1 1 d . . .
O5W O 0.6466(7) 0.2629(7) 0.7476(11) 0.086(5) Uiso 0.50 1 d P . .
O6W O 0.5941(6) 0.1728(6) 0.7577(11) 0.080(5) Uiso 0.50 1 d P . .
O8W O 0.7678(7) 0.4173(6) 0.5271(11) 0.082(5) Uani 0.50 1 d P . .
O9W O 0.7273(11) 0.1904(11) 0.7240(19) 0.066(8) Uiso 0.25 1 d P . .
O7W O 0.8983(8) 0.3873(8) 0.6022(13) 0.104(6) Uiso 0.50 1 d P A 1
O10W O 0.8557(14) 0.4655(14) 0.654(2) 0.089(10) Uiso 0.25 1 d P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N4 2.007(7) . ?
Cu1 N3 2.013(7) . ?
Cu1 N2 2.016(7) . ?
Cu1 N1 2.020(7) . ?
Cu1 O1W 2.308(6) . ?
Nb1 O1 1.764(5) . ?
Nb1 O9 1.942(5) . ?
Nb1 O8 1.978(5) . ?
Nb1 O4 1.998(5) 11_666 ?
Nb1 O5 2.021(5) . ?
Nb1 O10 2.448(4) . ?
Nb2 O2 1.758(5) . ?
Nb2 O9 1.904(5) . ?
Nb2 O5 1.913(5) 11_666 ?
Nb2 O6 2.099(5) . ?
Nb2 O7 2.127(4) . ?
Nb2 O10 2.425(4) 11_666 ?
Nb2 Sb1 3.2857(7) . ?
Nb3 O3 1.764(5) . ?
Nb3 O8 1.886(5) . ?
Nb3 O4 1.920(5) . ?
Nb3 O6 2.107(5) 2_655 ?
Nb3 O7 2.113(4) . ?
Nb3 O10 2.406(4) 12_656 ?
Nb3 Sb1 3.2986(7) . ?
Sb1 O7 2.001(5) . ?
Sb1 O7 2.001(5) 2_655 ?
Sb1 O6 2.162(5) 2_655 ?
Sb1 O6 2.162(5) . ?
Sb1 Nb2 3.2857(7) 2_655 ?
Sb1 Nb3 3.2986(7) 2_655 ?
V1 O10 1.724(4) 11_666 ?
V1 O10 1.724(4) 12_656 ?
V1 O10 1.724(4) . ?
V1 O10 1.724(4) 2_655 ?
C1 C2 1.391(16) . ?
C1 N1 1.429(13) . ?
C2 N2 1.481(15) . ?
C3 C4 1.462(14) . ?
C3 N3 1.481(12) . ?
C4 N4 1.431(13) . ?
O4 Nb1 1.999(5) 12_656 ?
O5 Nb2 1.913(5) 12_656 ?
O6 Nb3 2.107(5) 2_655 ?
O10 Nb3 2.406(4) 11_666 ?
O10 Nb2 2.425(4) 12_656 ?

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
N4 Cu1 N3 84.8(3) . . ?
N4 Cu1 N2 95.0(3) . . ?
N3 Cu1 N2 176.9(3) . . ?
N4 Cu1 N1 178.6(3) . . ?
N3 Cu1 N1 95.1(3) . . ?
N2 Cu1 N1 85.0(3) . . ?
N4 Cu1 O1W 92.5(3) . . ?
N3 Cu1 O1W 92.7(3) . . ?
N2 Cu1 O1W 90.4(3) . . ?
N1 Cu1 O1W 88.9(3) . . ?
O1 Nb1 O9 102.7(2) . . ?
O1 Nb1 O8 100.6(2) . . ?
O9 Nb1 O8 86.27(19) . . ?
O1 Nb1 O4 102.1(2) . 11_666 ?
O9 Nb1 O4 90.8(2) . 11_666 ?
O8 Nb1 O4 157.14(19) . 11_666 ?
O1 Nb1 O5 101.1(2) . . ?
O9 Nb1 O5 156.22(19) . . ?
O8 Nb1 O5 88.32(19) . . ?
O4 Nb1 O5 85.26(19) 11_666 . ?
O1 Nb1 O10 172.3(2) . . ?
O9 Nb1 O10 83.62(17) . . ?
O8 Nb1 O10 84.01(17) . . ?
O4 Nb1 O10 73.13(16) 11_666 . ?
O5 Nb1 O10 72.78(16) . . ?
O2 Nb2 O9 102.6(2) . . ?
O2 Nb2 O5 103.6(2) . 11_666 ?
O9 Nb2 O5 96.2(2) . 11_666 ?
O2 Nb2 O6 100.0(2) . . ?
O9 Nb2 O6 152.63(18) . . ?
O5 Nb2 O6 93.25(19) 11_666 . ?
O2 Nb2 O7 99.1(2) . . ?
O9 Nb2 O7 85.74(19) . . ?
O5 Nb2 O7 156.10(19) 11_666 . ?
O6 Nb2 O7 75.56(18) . . ?
O2 Nb2 O10 170.7(2) . 11_666 ?
O9 Nb2 O10 86.66(18) . 11_666 ?
O5 Nb2 O10 75.08(17) 11_666 11_666 ?
O6 Nb2 O10 71.06(16) . 11_666 ?
O7 Nb2 O10 81.28(16) . 11_666 ?
O2 Nb2 Sb1 96.80(18) . . ?
O9 Nb2 Sb1 120.94(14) . . ?
O5 Nb2 Sb1 132.17(14) 11_666 . ?
O6 Nb2 Sb1 40.26(12) . . ?
O7 Nb2 Sb1 35.94(12) . . ?
O10 Nb2 Sb1 78.03(11) 11_666 . ?
O3 Nb3 O8 103.3(2) . . ?
O3 Nb3 O4 100.2(2) . . ?
O8 Nb3 O4 97.2(2) . . ?
O3 Nb3 O6 99.1(2) . 2_655 ?
O8 Nb3 O6 153.67(18) . 2_655 ?
O4 Nb3 O6 92.29(19) . 2_655 ?
O3 Nb3 O7 101.7(2) . . ?
O8 Nb3 O7 86.91(19) . . ?
O4 Nb3 O7 156.11(19) . . ?
O6 Nb3 O7 74.99(18) 2_655 . ?
O3 Nb3 O10 169.0(2) . 12_656 ?
O8 Nb3 O10 87.37(17) . 12_656 ?
O4 Nb3 O10 75.41(17) . 12_656 ?
O6 Nb3 O10 71.34(17) 2_655 12_656 ?
O7 Nb3 O10 81.32(17) . 12_656 ?
O3 Nb3 Sb1 98.18(18) . . ?
O8 Nb3 Sb1 121.77(14) . . ?
O4 Nb3 Sb1 131.10(14) . . ?
O6 Nb3 Sb1 40.01(12) 2_655 . ?
O7 Nb3 Sb1 35.54(13) . . ?
O10 Nb3 Sb1 78.01(10) 12_656 . ?
O7 Sb1 O7 100.8(3) . 2_655 ?
O7 Sb1 O6 76.07(17) . 2_655 ?
O7 Sb1 O6 76.80(18) 2_655 2_655 ?
O7 Sb1 O6 76.80(18) . . ?
O7 Sb1 O6 76.08(17) 2_655 . ?
O6 Sb1 O6 136.8(3) 2_655 . ?
O7 Sb1 Nb2 38.59(13) . . ?
O7 Sb1 Nb2 93.19(13) 2_655 . ?
O6 Sb1 Nb2 111.09(12) 2_655 . ?
O6 Sb1 Nb2 38.85(12) . . ?
O7 Sb1 Nb2 93.19(13) . 2_655 ?
O7 Sb1 Nb2 38.59(13) 2_655 2_655 ?
O6 Sb1 Nb2 38.85(12) 2_655 2_655 ?
O6 Sb1 Nb2 111.09(12) . 2_655 ?
Nb2 Sb1 Nb2 110.59(3) . 2_655 ?
O7 Sb1 Nb3 37.86(13) . . ?
O7 Sb1 Nb3 93.48(14) 2_655 . ?
O6 Sb1 Nb3 38.79(12) 2_655 . ?
O6 Sb1 Nb3 111.03(13) . . ?
Nb2 Sb1 Nb3 75.490(19) . . ?
Nb2 Sb1 Nb3 66.399(17) 2_655 . ?
O7 Sb1 Nb3 93.48(14) . 2_655 ?
O7 Sb1 Nb3 37.86(13) 2_655 2_655 ?
O6 Sb1 Nb3 111.03(13) 2_655 2_655 ?
O6 Sb1 Nb3 38.79(12) . 2_655 ?
Nb2 Sb1 Nb3 66.400(17) . 2_655 ?
Nb2 Sb1 Nb3 75.492(19) 2_655 2_655 ?
Nb3 Sb1 Nb3 110.27(3) . 2_655 ?
O10 V1 O10 110.8(3) 11_666 12_656 ?
O10 V1 O10 108.84(14) 11_666 . ?
O10 V1 O10 108.83(15) 12_656 . ?
O10 V1 O10 108.83(15) 11_666 2_655 ?
O10 V1 O10 108.84(14) 12_656 2_655 ?
O10 V1 O10 110.7(3) . 2_655 ?
C2 C1 N1 116.3(11) . . ?
C1 C2 N2 114.0(10) . . ?
C4 C3 N3 109.1(8) . . ?
N4 C4 C3 112.7(9) . . ?
C1 N1 Cu1 109.2(6) . . ?
C2 N2 Cu1 107.6(6) . . ?
C3 N3 Cu1 109.1(5) . . ?
C4 N4 Cu1 108.4(6) . . ?
Nb3 O4 Nb1 121.5(2) . 12_656 ?
Nb2 O5 Nb1 122.1(2) 12_656 . ?
Nb2 O6 Nb3 118.0(2) . 2_655 ?
Nb2 O6 Sb1 100.89(19) . . ?
Nb3 O6 Sb1 101.19(18) 2_655 . ?
Sb1 O7 Nb3 106.6(2) . . ?
Sb1 O7 Nb2 105.5(2) . . ?
Nb3 O7 Nb2 143.9(2) . . ?
Nb3 O8 Nb1 154.5(3) . . ?
Nb2 O9 Nb1 156.7(3) . . ?
V1 O10 Nb3 124.0(2) . 11_666 ?
V1 O10 Nb2 123.3(2) . 12_656 ?
Nb3 O10 Nb2 96.56(16) 11_666 12_656 ?
V1 O10 Nb1 124.0(2) . . ?
Nb3 O10 Nb1 89.57(14) 11_666 . ?
Nb2 O10 Nb1 89.89(14) 12_656 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.511
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.169
_chemical_properties_physical    Efflorescent
