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

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H80 Cu4 N16 Nb12 O59 P V6'
_chemical_formula_weight         3146.65

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'
Cu Cu 0.3201 1.2651 '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'
Nb Nb -2.0727 0.6215 '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'
P P 0.1023 0.0942 '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/m

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

_cell_length_a                   15.141(2)
_cell_length_b                   15.141(2)
_cell_length_c                   19.257(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4414.7(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2014
_cell_measurement_theta_min      3.19
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3042
_exptl_absorpt_coefficient_mu    3.151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4972
_exptl_absorpt_correction_T_max  0.7055
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            17424
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2014
_reflns_number_gt                1697
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       auto
_computing_cell_refinement       auto
_computing_data_reduction        auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1487P)²+82.8862P] 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         2014
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.2145
_refine_ls_wR_factor_gt          0.2049
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
Nb1 Nb 0.27973(8) 0.60024(8) 0.0000 0.0324(4) Uani 1 2 d S . .
Nb2 Nb 0.33897(6) 0.43958(6) 0.13475(5) 0.0345(4) Uani 1 1 d . . .
P1 P 0.5000 0.5000 0.0000 0.0141(11) Uani 1 8 d S . .
V1 V 0.5000 0.5000 0.21145(14) 0.0275(7) Uani 1 4 d S . .
V2 V 0.24909(15) 0.40726(17) 0.0000 0.0374(6) Uani 1 2 d S . .
Cu1 Cu 0.2500 0.2500 0.2500 0.0568(6) Uani 1 2 d S . .
O1 O 0.3900(4) 0.5504(4) 0.1722(3) 0.0323(15) Uani 1 1 d . . .
O2 O 0.2664(5) 0.5037(4) 0.0672(3) 0.0382(16) Uani 1 1 d . . .
O3 O 0.3252(4) 0.3433(5) 0.0679(3) 0.0350(15) Uani 1 1 d . . .
O4 O 0.2647(4) 0.4110(4) 0.1967(3) 0.0337(15) Uani 1 1 d . . .
O5 O 0.1781(6) 0.6462(7) 0.0000 0.042(2) Uani 1 2 d S . .
O6 O 0.1456(7) 0.3725(8) 0.0000 0.056(3) Uani 1 2 d S . .
O7 O 0.5000 0.5000 0.2960(7) 0.045(3) Uani 1 4 d S . .
O8 O 0.4246(7) 0.5326(7) -0.0460(5) 0.019(2) Uani 0.50 1 d P . .
C1 C 0.1540(19) 0.1698(17) 0.1415(11) 0.120(8) Uani 1 1 d . . .
H1A H 0.1378 0.1175 0.1676 0.145 Uiso 1 1 calc R . .
H1B H 0.1446 0.1586 0.0925 0.145 Uiso 1 1 calc R . .
N2 N 0.2472(10) 0.1953(9) 0.1554(6) 0.082(4) Uani 1 1 d . . .
H2A H 0.2660 0.2342 0.1233 0.099 Uiso 1 1 calc R . .
H2B H 0.2824 0.1475 0.1540 0.099 Uiso 1 1 calc R . .
C2 C 0.1035(15) 0.247(2) 0.1646(14) 0.137(10) Uani 1 1 d . . .
H2C H 0.1211 0.2986 0.1388 0.164 Uiso 1 1 calc R . .
H2D H 0.0409 0.2368 0.1572 0.164 Uiso 1 1 calc R . .
N1 N 0.1212(8) 0.2583(10) 0.2367(8) 0.080(4) Uani 1 1 d . . .
H1C H 0.0936 0.2163 0.2616 0.096 Uiso 1 1 calc R . .
H1D H 0.1016 0.3115 0.2508 0.096 Uiso 1 1 calc R . .
O1W O -0.0199(12) 0.4394(13) 0.0000 0.100(5) Uiso 1 2 d S . .
O2W O 0.4537(15) 0.0971(15) 0.1383(11) 0.169(8) Uiso 1 1 d . . .
O3W O 0.0000 0.5000 0.2500 0.13(2) Uiso 0.50 4 d SP . .


_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
Nb1 O5 1.689(9) . ?
Nb1 O2 1.963(6) 11 ?
Nb1 O2 1.963(6) . ?
Nb1 O3 1.978(6) 4_565 ?
Nb1 O3 1.978(6) 10_565 ?
Nb1 O8 2.578(10) 11 ?
Nb1 O8 2.578(10) . ?
Nb1 V2 2.958(3) . ?
Nb1 V2 2.989(3) 10_565 ?
Nb2 O4 1.696(6) . ?
Nb2 O2 1.960(6) . ?
Nb2 O3 1.956(6) . ?
Nb2 O1 1.973(6) 2_655 ?
Nb2 O1 1.983(6) . ?
Nb2 O8 2.567(10) 11 ?
Nb2 V2 2.9707(15) . ?
Nb2 V1 2.9938(17) . ?
P1 O8 1.526(10) 10_565 ?
P1 O8 1.526(10) 9_665 ?
P1 O8 1.526(10) 4_565 ?
P1 O8 1.526(10) . ?
P1 O8 1.526(10) 11 ?
P1 O8 1.526(10) 3_665 ?
P1 O8 1.526(10) 2_655 ?
P1 O8 1.526(10) 12_655 ?
V1 O7 1.628(14) . ?
V1 O1 1.981(6) 4_565 ?
V1 O1 1.981(6) . ?
V1 O1 1.981(6) 2_655 ?
V1 O1 1.981(6) 3_665 ?
V1 Nb2 2.9938(17) 4_565 ?
V1 Nb2 2.9938(17) 2_655 ?
V1 Nb2 2.9938(17) 3_665 ?
V2 O6 1.653(10) . ?
V2 O2 1.968(7) . ?
V2 O2 1.968(7) 11 ?
V2 O3 1.995(6) . ?
V2 O3 1.995(6) 11 ?
V2 Nb2 2.9707(15) 11 ?
V2 Nb1 2.989(3) 2_655 ?
Cu1 N1 1.971(12) 13 ?
Cu1 N1 1.971(12) . ?
Cu1 N2 2.001(13) 13 ?
Cu1 N2 2.001(13) . ?
O1 Nb2 1.973(6) 4_565 ?
O3 Nb1 1.978(6) 2_655 ?
O8 O8 1.758(14) 4_565 ?
O8 O8 1.758(14) 2_655 ?
O8 O8 1.77(2) 11 ?
O8 Nb2 2.567(10) 11 ?
C1 N2 1.49(3) . ?
C1 C2 1.46(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
C2 N1 1.42(3) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Nb1 O2 102.3(3) . 11 ?
O5 Nb1 O2 102.3(3) . . ?
O2 Nb1 O2 82.5(4) 11 . ?
O5 Nb1 O3 102.0(3) . 4_565 ?
O2 Nb1 O3 155.7(3) 11 4_565 ?
O2 Nb1 O3 92.2(3) . 4_565 ?
O5 Nb1 O3 102.0(3) . 10_565 ?
O2 Nb1 O3 92.2(3) 11 10_565 ?
O2 Nb1 O3 155.7(3) . 10_565 ?
O3 Nb1 O3 82.8(4) 4_565 10_565 ?
O5 Nb1 O8 159.9(2) . 11 ?
O2 Nb1 O8 91.0(3) 11 11 ?
O2 Nb1 O8 64.2(3) . 11 ?
O3 Nb1 O8 65.5(3) 4_565 11 ?
O3 Nb1 O8 92.3(3) 10_565 11 ?
O5 Nb1 O8 159.9(2) . . ?
O2 Nb1 O8 64.2(3) 11 . ?
O2 Nb1 O8 91.0(3) . . ?
O3 Nb1 O8 92.3(3) 4_565 . ?
O3 Nb1 O8 65.5(3) 10_565 . ?
O8 Nb1 O8 40.2(4) 11 . ?
O5 Nb1 V2 105.3(4) . . ?
O2 Nb1 V2 41.2(2) 11 . ?
O2 Nb1 V2 41.2(2) . . ?
O3 Nb1 V2 129.78(18) 4_565 . ?
O3 Nb1 V2 129.78(18) 10_565 . ?
O8 Nb1 V2 75.0(3) 11 . ?
O8 Nb1 V2 75.0(3) . . ?
O5 Nb1 V2 105.9(4) . 10_565 ?
O2 Nb1 V2 129.42(19) 11 10_565 ?
O2 Nb1 V2 129.42(19) . 10_565 ?
O3 Nb1 V2 41.42(18) 4_565 10_565 ?
O3 Nb1 V2 41.42(18) 10_565 10_565 ?
O8 Nb1 V2 75.7(3) 11 10_565 ?
O8 Nb1 V2 75.7(3) . 10_565 ?
V2 Nb1 V2 148.78(9) . 10_565 ?
O4 Nb2 O2 102.8(3) . . ?
O4 Nb2 O3 101.7(3) . . ?
O2 Nb2 O3 82.7(3) . . ?
O4 Nb2 O1 102.0(3) . 2_655 ?
O2 Nb2 O1 155.1(3) . 2_655 ?
O3 Nb2 O1 92.7(3) . 2_655 ?
O4 Nb2 O1 102.6(3) . . ?
O2 Nb2 O1 92.4(3) . . ?
O3 Nb2 O1 155.7(3) . . ?
O1 Nb2 O1 81.8(3) 2_655 . ?
O4 Nb2 O8 160.7(3) . 11 ?
O2 Nb2 O8 64.5(3) . 11 ?
O3 Nb2 O8 91.4(3) . 11 ?
O1 Nb2 O8 91.3(3) 2_655 11 ?
O1 Nb2 O8 65.3(3) . 11 ?
O4 Nb2 V2 105.6(2) . . ?
O2 Nb2 V2 41.0(2) . . ?
O3 Nb2 V2 41.73(19) . . ?
O1 Nb2 V2 130.24(18) 2_655 . ?
O1 Nb2 V2 129.48(18) . . ?
O8 Nb2 V2 74.9(2) 11 . ?
O4 Nb2 V1 105.7(2) . . ?
O2 Nb2 V1 129.26(19) . . ?
O3 Nb2 V1 129.72(18) . . ?
O1 Nb2 V1 40.89(17) 2_655 . ?
O1 Nb2 V1 40.94(17) . . ?
O8 Nb2 V1 75.5(2) 11 . ?
V2 Nb2 V1 148.69(7) . . ?
O8 P1 O8 70.3(4) 10_565 9_665 ?
O8 P1 O8 70.9(8) 10_565 4_565 ?
O8 P1 O8 109.7(4) 9_665 4_565 ?
O8 P1 O8 109.7(4) 10_565 . ?
O8 P1 O8 180.0(11) 9_665 . ?
O8 P1 O8 70.3(4) 4_565 . ?
O8 P1 O8 70.3(4) 10_565 11 ?
O8 P1 O8 109.1(8) 9_665 11 ?
O8 P1 O8 109.7(4) 4_565 11 ?
O8 P1 O8 70.9(8) . 11 ?
O8 P1 O8 109.7(4) 10_565 3_665 ?
O8 P1 O8 70.9(8) 9_665 3_665 ?
O8 P1 O8 70.3(4) 4_565 3_665 ?
O8 P1 O8 109.1(8) . 3_665 ?
O8 P1 O8 180.0(10) 11 3_665 ?
O8 P1 O8 180.0(8) 10_565 2_655 ?
O8 P1 O8 109.7(4) 9_665 2_655 ?
O8 P1 O8 109.1(8) 4_565 2_655 ?
O8 P1 O8 70.3(4) . 2_655 ?
O8 P1 O8 109.7(4) 11 2_655 ?
O8 P1 O8 70.3(4) 3_665 2_655 ?
O8 P1 O8 109.1(8) 10_565 12_655 ?
O8 P1 O8 70.3(4) 9_665 12_655 ?
O8 P1 O8 180.0(6) 4_565 12_655 ?
O8 P1 O8 109.7(4) . 12_655 ?
O8 P1 O8 70.3(4) 11 12_655 ?
O8 P1 O8 109.7(4) 3_665 12_655 ?
O8 P1 O8 70.9(8) 2_655 12_655 ?
O7 V1 O1 112.4(2) . 4_565 ?
O7 V1 O1 112.4(2) . . ?
O1 V1 O1 81.64(15) 4_565 . ?
O7 V1 O1 112.4(2) . 2_655 ?
O1 V1 O1 135.2(4) 4_565 2_655 ?
O1 V1 O1 81.64(15) . 2_655 ?
O7 V1 O1 112.4(2) . 3_665 ?
O1 V1 O1 81.64(15) 4_565 3_665 ?
O1 V1 O1 135.2(4) . 3_665 ?
O1 V1 O1 81.64(15) 2_655 3_665 ?
O7 V1 Nb2 119.56(5) . . ?
O1 V1 Nb2 112.5(2) 4_565 . ?
O1 V1 Nb2 40.97(17) . . ?
O1 V1 Nb2 40.68(17) 2_655 . ?
O1 V1 Nb2 112.3(2) 3_665 . ?
O7 V1 Nb2 119.56(5) . 4_565 ?
O1 V1 Nb2 40.97(17) 4_565 4_565 ?
O1 V1 Nb2 40.68(17) . 4_565 ?
O1 V1 Nb2 112.3(2) 2_655 4_565 ?
O1 V1 Nb2 112.5(2) 3_665 4_565 ?
Nb2 V1 Nb2 75.91(4) . 4_565 ?
O7 V1 Nb2 119.56(5) . 2_655 ?
O1 V1 Nb2 112.3(2) 4_565 2_655 ?
O1 V1 Nb2 112.5(2) . 2_655 ?
O1 V1 Nb2 40.97(17) 2_655 2_655 ?
O1 V1 Nb2 40.68(17) 3_665 2_655 ?
Nb2 V1 Nb2 75.91(4) . 2_655 ?
Nb2 V1 Nb2 120.88(10) 4_565 2_655 ?
O7 V1 Nb2 119.56(5) . 3_665 ?
O1 V1 Nb2 40.68(17) 4_565 3_665 ?
O1 V1 Nb2 112.3(2) . 3_665 ?
O1 V1 Nb2 112.5(2) 2_655 3_665 ?
O1 V1 Nb2 40.97(17) 3_665 3_665 ?
Nb2 V1 Nb2 120.88(10) . 3_665 ?
Nb2 V1 Nb2 75.91(4) 4_565 3_665 ?
Nb2 V1 Nb2 75.91(4) 2_655 3_665 ?
O6 V2 O2 111.3(4) . . ?
O6 V2 O2 111.3(4) . 11 ?
O2 V2 O2 82.2(4) . 11 ?
O6 V2 O3 113.1(4) . . ?
O2 V2 O3 81.5(3) . . ?
O2 V2 O3 135.6(3) 11 . ?
O6 V2 O3 113.1(4) . 11 ?
O2 V2 O3 135.6(3) . 11 ?
O2 V2 O3 81.5(3) 11 11 ?
O3 V2 O3 82.0(4) . 11 ?
O6 V2 Nb1 117.6(5) . . ?
O2 V2 Nb1 41.11(19) . . ?
O2 V2 Nb1 41.11(19) 11 . ?
O3 V2 Nb1 112.9(2) . . ?
O3 V2 Nb1 112.9(2) 11 . ?
O6 V2 Nb2 119.12(4) . . ?
O2 V2 Nb2 40.76(18) . . ?
O2 V2 Nb2 113.0(2) 11 . ?
O3 V2 Nb2 40.74(18) . . ?
O3 V2 Nb2 112.8(2) 11 . ?
Nb1 V2 Nb2 76.44(5) . . ?
O6 V2 Nb2 119.12(4) . 11 ?
O2 V2 Nb2 113.0(2) . 11 ?
O2 V2 Nb2 40.76(18) 11 11 ?
O3 V2 Nb2 112.8(2) . 11 ?
O3 V2 Nb2 40.74(18) 11 11 ?
Nb1 V2 Nb2 76.44(5) . 11 ?
Nb2 V2 Nb2 121.74(9) . 11 ?
O6 V2 Nb1 121.2(5) . 2_655 ?
O2 V2 Nb1 112.2(2) . 2_655 ?
O2 V2 Nb1 112.2(2) 11 2_655 ?
O3 V2 Nb1 40.99(18) . 2_655 ?
O3 V2 Nb1 40.99(18) 11 2_655 ?
Nb1 V2 Nb1 121.22(9) . 2_655 ?
Nb2 V2 Nb1 75.92(5) . 2_655 ?
Nb2 V2 Nb1 75.92(5) 11 2_655 ?
N1 Cu1 N1 180.000(1) 13 . ?
N1 Cu1 N2 83.5(7) 13 13 ?
N1 Cu1 N2 96.5(7) . 13 ?
N1 Cu1 N2 96.5(7) 13 . ?
N1 Cu1 N2 83.5(7) . . ?
N2 Cu1 N2 180.000(1) 13 . ?
Nb2 O1 Nb2 137.2(3) 4_565 . ?
Nb2 O1 V1 98.4(3) 4_565 . ?
Nb2 O1 V1 98.1(3) . . ?
Nb2 O2 V2 98.3(3) . . ?
Nb2 O2 Nb1 138.5(4) . . ?
V2 O2 Nb1 97.6(3) . . ?
Nb2 O3 Nb1 137.5(4) . 2_655 ?
Nb2 O3 V2 97.5(3) . . ?
Nb1 O3 V2 97.6(3) 2_655 . ?
P1 O8 O8 54.83(19) . 4_565 ?
P1 O8 O8 54.83(19) . 2_655 ?
O8 O8 O8 90.000(2) 4_565 2_655 ?
P1 O8 O8 54.6(4) . 11 ?
O8 O8 O8 90.000(1) 4_565 11 ?
O8 O8 O8 90.000(1) 2_655 11 ?
P1 O8 Nb2 125.9(6) . 11 ?
O8 O8 Nb2 132.2(3) 4_565 11 ?
O8 O8 Nb2 71.1(5) 2_655 11 ?
O8 O8 Nb2 131.8(2) 11 11 ?
P1 O8 Nb1 124.5(5) . . ?
O8 O8 Nb1 130.2(7) 4_565 . ?
O8 O8 Nb1 133.0(7) 2_655 . ?
O8 O8 Nb1 69.9(2) 11 . ?
Nb2 O8 Nb1 91.0(3) 11 . ?
N2 C1 C2 103.6(18) . . ?
N2 C1 H1A 111.0 . . ?
C2 C1 H1A 111.0 . . ?
N2 C1 H1B 111.0 . . ?
C2 C1 H1B 111.0 . . ?
H1A C1 H1B 109.0 . . ?
C1 N2 Cu1 107.0(12) . . ?
C1 N2 H2A 110.3 . . ?
Cu1 N2 H2A 110.3 . . ?
C1 N2 H2B 110.3 . . ?
Cu1 N2 H2B 110.3 . . ?
H2A N2 H2B 108.6 . . ?
N1 C2 C1 107.3(19) . . ?
N1 C2 H2C 110.3 . . ?
C1 C2 H2C 110.3 . . ?
N1 C2 H2D 110.3 . . ?
C1 C2 H2D 110.3 . . ?
H2C C2 H2D 108.5 . . ?
C2 N1 Cu1 107.8(13) . . ?
C2 N1 H1C 110.1 . . ?
Cu1 N1 H1C 110.1 . . ?
C2 N1 H1D 110.1 . . ?
Cu1 N1 H1D 110.1 . . ?
H1C N1 H1D 108.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.254
_database_code_depnum_ccdc_archive 'CCDC 973046'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H97 Cu4 N16 Nb12 O57 P V6'
_chemical_formula_weight         3227.87

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'
Nb Nb -2.0727 0.6215 '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'
P P 0.1023 0.0942 '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'
Cu Cu 0.3201 1.2651 '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/m

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

_cell_length_a                   15.229(2)
_cell_length_b                   15.229(2)
_cell_length_c                   19.207(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4454.5(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2029
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3140
_exptl_absorpt_coefficient_mu    3.125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4972
_exptl_absorpt_correction_T_max  0.7055
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            16922
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2029
_reflns_number_gt                1658
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       auto
_computing_cell_refinement       auto
_computing_data_reduction        auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1522P)²+47.2889P] 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         2029
_refine_ls_number_parameters     154
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.2226
_refine_ls_wR_factor_gt          0.2105
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.036
_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
Nb1 Nb 0.56225(6) -0.34079(6) 0.63454(5) 0.0424(4) Uani 1 1 d . . .
Nb2 Nb 0.40376(8) -0.27914(8) 0.5000 0.0405(4) Uani 1 2 d S . .
V1 V 0.5000 -0.5000 0.71175(14) 0.0351(7) Uani 1 4 d S . .
V2 V 0.59646(17) -0.25258(16) 0.5000 0.0453(6) Uani 1 2 d S . .
P1 P 0.5000 -0.5000 0.5000 0.0184(11) Uani 1 8 d S . .
O1 O 0.5000 -0.5000 0.7953(7) 0.055(4) Uani 1 4 d S . .
O2 O 0.6329(9) -0.1518(8) 0.5000 0.069(3) Uani 1 2 d S . .
O3 O 0.4522(4) -0.3901(4) 0.6721(3) 0.0411(16) Uani 1 1 d . . .
O4 O 0.5000(4) -0.2680(5) 0.5672(4) 0.0477(17) Uani 1 1 d . . .
O5 O 0.6586(4) -0.3292(4) 0.5682(3) 0.0395(15) Uani 1 1 d . . .
O6 O 0.5925(5) -0.2686(4) 0.6973(3) 0.0418(15) Uani 1 1 d . . .
O7 O 0.3601(7) -0.1780(6) 0.5000 0.053(3) Uani 1 2 d S . .
O8 O 0.4688(7) -0.4240(6) 0.5451(5) 0.024(2) Uani 0.50 1 d P . .
Cu1 Cu 0.2500 0.2500 0.2500 0.0642(7) Uani 1 2 d S . .
C1 C 0.1706(17) 0.1572(17) 0.3568(12) 0.121(7) Uani 1 1 d U . .
H1A H 0.1197 0.1438 0.3275 0.145 Uiso 1 1 calc R . .
C2 C 0.150(3) 0.139(3) 0.424(2) 0.30(2) Uani 1 1 d DU . .
H2A H 0.1328 0.0782 0.4273 0.451 Uiso 1 1 calc R . .
H2B H 0.1018 0.1755 0.4380 0.451 Uiso 1 1 calc R . .
H2C H 0.1997 0.1495 0.4528 0.451 Uiso 1 1 calc R . .
C3 C 0.238(2) 0.1039(15) 0.3372(14) 0.148(11) Uani 1 1 d D . .
H3A H 0.2220 0.0427 0.3429 0.177 Uiso 1 1 calc R . .
H3B H 0.2899 0.1156 0.3651 0.177 Uiso 1 1 calc R . .
N1 N 0.1974(9) 0.2502(10) 0.3437(6) 0.091(4) Uani 1 1 d . . .
H1B H 0.2367 0.2681 0.3756 0.109 Uiso 1 1 calc R . .
H1C H 0.1505 0.2861 0.3452 0.109 Uiso 1 1 calc R . .
N2 N 0.2543(11) 0.1231(9) 0.2667(9) 0.103(5) Uani 1 1 d . . .
H2D H 0.2138 0.0962 0.2401 0.123 Uiso 1 1 calc R . .
H2E H 0.3075 0.1024 0.2546 0.123 Uiso 1 1 calc R . .
O1W O 0.446(4) -0.006(4) 0.5000 0.20(3) Uiso 0.50 2 d SP . 1
O2W O 0.354(5) -0.017(5) 0.563(4) 0.15(2) Uiso 0.25 1 d P A 2
O3W O 0.447(2) -0.099(2) 0.6387(15) 0.112(9) Uiso 0.50 1 d P . .
O4W O 0.5000 0.0000 0.2500 0.15(2) Uiso 0.50 4 d SP . .
O5W O 0.492(4) -0.108(4) 0.671(3) 0.120(18) Uiso 0.25 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
Nb1 O6 1.695(6) . ?
Nb1 O5 1.952(6) . ?
Nb1 O4 1.949(7) . ?
Nb1 O3 1.973(6) . ?
Nb1 O3 1.981(6) 4_655 ?
Nb1 O8 2.565(10) . ?
Nb1 V2 2.9586(16) . ?
Nb1 V1 2.9961(17) . ?
Nb2 O7 1.678(9) . ?
Nb2 O4 1.960(7) . ?
Nb2 O4 1.960(7) 11_556 ?
Nb2 O5 1.976(6) 12_546 ?
Nb2 O5 1.976(6) 2_545 ?
Nb2 O8 2.568(10) 11_556 ?
Nb2 O8 2.568(10) . ?
Nb2 V2 2.962(3) . ?
Nb2 V2 2.982(3) 2_545 ?
V1 O1 1.604(13) . ?
V1 O3 1.978(6) 4_655 ?
V1 O3 1.978(6) 2_545 ?
V1 O3 1.978(6) 3_645 ?
V1 O3 1.978(6) . ?
V1 Nb1 2.9961(17) 3_645 ?
V1 Nb1 2.9961(17) 4_655 ?
V1 Nb1 2.9961(17) 2_545 ?
V2 O2 1.632(11) . ?
V2 O4 1.969(7) 11_556 ?
V2 O4 1.969(7) . ?
V2 O5 1.993(6) 11_556 ?
V2 O5 1.993(6) . ?
V2 Nb1 2.9586(16) 11_556 ?
V2 Nb2 2.982(3) 10_656 ?
P1 O8 1.522(9) 4_655 ?
P1 O8 1.522(9) 10_656 ?
P1 O8 1.522(9) 12_546 ?
P1 O8 1.522(9) . ?
P1 O8 1.522(9) 9_646 ?
P1 O8 1.522(9) 3_645 ?
P1 O8 1.522(9) 2_545 ?
P1 O8 1.522(9) 11_556 ?
O3 Nb1 1.981(6) 2_545 ?
O5 Nb2 1.976(6) 10_656 ?
O8 O8 1.732(19) 11_556 ?
O8 O8 1.770(14) 4_655 ?
O8 O8 1.770(14) 2_545 ?
Cu1 N2 1.960(14) 13 ?
Cu1 N2 1.960(14) . ?
Cu1 N1 1.970(13) 13 ?
Cu1 N1 1.970(13) . ?
C1 C3 1.36(3) . ?
C1 C2 1.35(4) . ?
C1 N1 1.50(3) . ?
C1 H1A 0.9800 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N2 1.41(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N2 H2D 0.9000 . ?
N2 H2E 0.9000 . ?
O1W O1W 1.66(13) 9_656 ?
O3W O5W 0.94(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
O6 Nb1 O5 101.6(3) . . ?
O6 Nb1 O4 103.6(3) . . ?
O5 Nb1 O4 83.2(3) . . ?
O6 Nb1 O3 102.6(3) . . ?
O5 Nb1 O3 155.8(3) . . ?
O4 Nb1 O3 92.6(3) . . ?
O6 Nb1 O3 101.4(3) . 4_655 ?
O5 Nb1 O3 92.3(3) . 4_655 ?
O4 Nb1 O3 155.0(3) . 4_655 ?
O3 Nb1 O3 81.5(4) . 4_655 ?
O6 Nb1 O8 161.3(3) . . ?
O5 Nb1 O8 91.4(3) . . ?
O4 Nb1 O8 64.3(3) . . ?
O3 Nb1 O8 65.5(3) . . ?
O3 Nb1 O8 91.4(3) 4_655 . ?
O6 Nb1 V2 106.2(2) . . ?
O5 Nb1 V2 41.94(19) . . ?
O4 Nb1 V2 41.2(2) . . ?
O3 Nb1 V2 129.92(19) . . ?
O3 Nb1 V2 129.97(19) 4_655 . ?
O8 Nb1 V2 74.7(2) . . ?
O6 Nb1 V1 105.0(2) . . ?
O5 Nb1 V1 129.37(19) . . ?
O4 Nb1 V1 129.4(2) . . ?
O3 Nb1 V1 40.73(19) . . ?
O3 Nb1 V1 40.77(18) 4_655 . ?
O8 Nb1 V1 75.9(2) . . ?
V2 Nb1 V1 148.81(7) . . ?
O7 Nb2 O4 102.5(3) . . ?
O7 Nb2 O4 102.5(3) . 11_556 ?
O4 Nb2 O4 82.4(4) . 11_556 ?
O7 Nb2 O5 102.3(3) . 12_546 ?
O4 Nb2 O5 155.2(3) . 12_546 ?
O4 Nb2 O5 92.0(3) 11_556 12_546 ?
O7 Nb2 O5 102.3(3) . 2_545 ?
O4 Nb2 O5 92.0(3) . 2_545 ?
O4 Nb2 O5 155.2(3) 11_556 2_545 ?
O5 Nb2 O5 83.0(4) 12_546 2_545 ?
O7 Nb2 O8 160.3(2) . 11_556 ?
O4 Nb2 O8 90.5(3) . 11_556 ?
O4 Nb2 O8 64.1(3) 11_556 11_556 ?
O5 Nb2 O8 65.6(3) 12_546 11_556 ?
O5 Nb2 O8 91.9(3) 2_545 11_556 ?
O7 Nb2 O8 160.3(2) . . ?
O4 Nb2 O8 64.1(3) . . ?
O4 Nb2 O8 90.5(3) 11_556 . ?
O5 Nb2 O8 91.9(3) 12_546 . ?
O5 Nb2 O8 65.6(3) 2_545 . ?
O8 Nb2 O8 39.4(4) 11_556 . ?
O7 Nb2 V2 105.5(4) . . ?
O4 Nb2 V2 41.2(2) . . ?
O4 Nb2 V2 41.2(2) 11_556 . ?
O5 Nb2 V2 129.41(18) 12_546 . ?
O5 Nb2 V2 129.41(18) 2_545 . ?
O8 Nb2 V2 74.6(3) 11_556 . ?
O8 Nb2 V2 74.6(3) . . ?
O7 Nb2 V2 106.1(4) . 2_545 ?
O4 Nb2 V2 129.2(2) . 2_545 ?
O4 Nb2 V2 129.2(2) 11_556 2_545 ?
O5 Nb2 V2 41.52(18) 12_546 2_545 ?
O5 Nb2 V2 41.52(18) 2_545 2_545 ?
O8 Nb2 V2 75.7(3) 11_556 2_545 ?
O8 Nb2 V2 75.7(3) . 2_545 ?
V2 Nb2 V2 148.40(9) . 2_545 ?
O1 V1 O3 112.6(2) . 4_655 ?
O1 V1 O3 112.6(2) . 2_545 ?
O3 V1 O3 134.7(4) 4_655 2_545 ?
O1 V1 O3 112.6(2) . 3_645 ?
O3 V1 O3 81.47(15) 4_655 3_645 ?
O3 V1 O3 81.47(15) 2_545 3_645 ?
O1 V1 O3 112.6(2) . . ?
O3 V1 O3 81.47(15) 4_655 . ?
O3 V1 O3 81.47(15) 2_545 . ?
O3 V1 O3 134.7(4) 3_645 . ?
O1 V1 Nb1 119.67(5) . 3_645 ?
O3 V1 Nb1 112.0(2) 4_655 3_645 ?
O3 V1 Nb1 40.86(18) 2_545 3_645 ?
O3 V1 Nb1 40.62(18) 3_645 3_645 ?
O3 V1 Nb1 112.2(2) . 3_645 ?
O1 V1 Nb1 119.67(5) . . ?
O3 V1 Nb1 40.86(18) 4_655 . ?
O3 V1 Nb1 112.0(2) 2_545 . ?
O3 V1 Nb1 112.2(2) 3_645 . ?
O3 V1 Nb1 40.62(18) . . ?
Nb1 V1 Nb1 120.66(10) 3_645 . ?
O1 V1 Nb1 119.67(5) . 4_655 ?
O3 V1 Nb1 40.62(18) 4_655 4_655 ?
O3 V1 Nb1 112.2(2) 2_545 4_655 ?
O3 V1 Nb1 40.86(18) 3_645 4_655 ?
O3 V1 Nb1 112.0(2) . 4_655 ?
Nb1 V1 Nb1 75.82(4) 3_645 4_655 ?
Nb1 V1 Nb1 75.82(4) . 4_655 ?
O1 V1 Nb1 119.67(5) . 2_545 ?
O3 V1 Nb1 112.2(2) 4_655 2_545 ?
O3 V1 Nb1 40.62(18) 2_545 2_545 ?
O3 V1 Nb1 112.0(2) 3_645 2_545 ?
O3 V1 Nb1 40.86(18) . 2_545 ?
Nb1 V1 Nb1 75.82(4) 3_645 2_545 ?
Nb1 V1 Nb1 75.82(4) . 2_545 ?
Nb1 V1 Nb1 120.66(10) 4_655 2_545 ?
O2 V2 O4 111.5(4) . 11_556 ?
O2 V2 O4 111.5(4) . . ?
O4 V2 O4 81.9(4) 11_556 . ?
O2 V2 O5 112.9(4) . 11_556 ?
O4 V2 O5 81.6(3) 11_556 11_556 ?
O4 V2 O5 135.6(3) . 11_556 ?
O2 V2 O5 112.9(4) . . ?
O4 V2 O5 135.6(3) 11_556 . ?
O4 V2 O5 81.6(3) . . ?
O5 V2 O5 82.2(3) 11_556 . ?
O2 V2 Nb1 119.13(4) . 11_556 ?
O4 V2 Nb1 40.7(2) 11_556 11_556 ?
O4 V2 Nb1 112.8(2) . 11_556 ?
O5 V2 Nb1 40.88(18) 11_556 11_556 ?
O5 V2 Nb1 113.1(2) . 11_556 ?
O2 V2 Nb1 119.13(4) . . ?
O4 V2 Nb1 112.8(2) 11_556 . ?
O4 V2 Nb1 40.7(2) . . ?
O5 V2 Nb1 113.1(2) 11_556 . ?
O5 V2 Nb1 40.88(18) . . ?
Nb1 V2 Nb1 121.72(9) 11_556 . ?
O2 V2 Nb2 117.7(5) . . ?
O4 V2 Nb2 41.0(2) 11_556 . ?
O4 V2 Nb2 41.0(2) . . ?
O5 V2 Nb2 113.0(2) 11_556 . ?
O5 V2 Nb2 113.0(2) . . ?
Nb1 V2 Nb2 76.32(5) 11_556 . ?
Nb1 V2 Nb2 76.32(5) . . ?
O2 V2 Nb2 120.7(5) . 10_656 ?
O4 V2 Nb2 112.4(2) 11_556 10_656 ?
O4 V2 Nb2 112.4(2) . 10_656 ?
O5 V2 Nb2 41.08(17) 11_556 10_656 ?
O5 V2 Nb2 41.08(17) . 10_656 ?
Nb1 V2 Nb2 76.19(5) 11_556 10_656 ?
Nb1 V2 Nb2 76.19(5) . 10_656 ?
Nb2 V2 Nb2 121.60(9) . 10_656 ?
O8 P1 O8 69.4(8) 4_655 10_656 ?
O8 P1 O8 180.0(7) 4_655 12_546 ?
O8 P1 O8 110.6(8) 10_656 12_546 ?
O8 P1 O8 71.1(4) 4_655 . ?
O8 P1 O8 108.9(4) 10_656 . ?
O8 P1 O8 108.9(4) 12_546 . ?
O8 P1 O8 108.9(4) 4_655 9_646 ?
O8 P1 O8 71.1(4) 10_656 9_646 ?
O8 P1 O8 71.1(4) 12_546 9_646 ?
O8 P1 O8 180.000(2) . 9_646 ?
O8 P1 O8 71.1(4) 4_655 3_645 ?
O8 P1 O8 108.9(4) 10_656 3_645 ?
O8 P1 O8 108.9(4) 12_546 3_645 ?
O8 P1 O8 110.6(8) . 3_645 ?
O8 P1 O8 69.4(8) 9_646 3_645 ?
O8 P1 O8 110.6(8) 4_655 2_545 ?
O8 P1 O8 180.0(6) 10_656 2_545 ?
O8 P1 O8 69.4(8) 12_546 2_545 ?
O8 P1 O8 71.1(4) . 2_545 ?
O8 P1 O8 108.9(4) 9_646 2_545 ?
O8 P1 O8 71.1(4) 3_645 2_545 ?
O8 P1 O8 108.9(4) 4_655 11_556 ?
O8 P1 O8 71.1(4) 10_656 11_556 ?
O8 P1 O8 71.1(4) 12_546 11_556 ?
O8 P1 O8 69.4(8) . 11_556 ?
O8 P1 O8 110.6(8) 9_646 11_556 ?
O8 P1 O8 180.0(10) 3_645 11_556 ?
O8 P1 O8 108.9(4) 2_545 11_556 ?
Nb1 O3 V1 98.6(3) . . ?
Nb1 O3 Nb1 137.2(4) . 2_545 ?
V1 O3 Nb1 98.4(3) . 2_545 ?
Nb1 O4 Nb2 138.7(4) . . ?
Nb1 O4 V2 98.0(3) . . ?
Nb2 O4 V2 97.8(3) . . ?
Nb1 O5 Nb2 137.9(4) . 10_656 ?
Nb1 O5 V2 97.2(3) . . ?
Nb2 O5 V2 97.4(3) 10_656 . ?
P1 O8 O8 55.3(4) . 11_556 ?
P1 O8 O8 54.45(19) . 4_655 ?
O8 O8 O8 90.000(1) 11_556 4_655 ?
P1 O8 O8 54.45(19) . 2_545 ?
O8 O8 O8 90.000(1) 11_556 2_545 ?
O8 O8 O8 90.000(1) 4_655 2_545 ?
P1 O8 Nb1 125.7(6) . . ?
O8 O8 Nb1 132.0(2) 11_556 . ?
O8 O8 Nb1 71.3(5) 4_655 . ?
O8 O8 Nb1 132.0(3) 2_545 . ?
P1 O8 Nb2 125.6(5) . . ?
O8 O8 Nb2 70.3(2) 11_556 . ?
O8 O8 Nb2 133.4(7) 4_655 . ?
O8 O8 Nb2 130.0(7) 2_545 . ?
Nb1 O8 Nb2 90.9(3) . . ?
N2 Cu1 N2 180.0(10) 13 . ?
N2 Cu1 N1 82.3(7) 13 13 ?
N2 Cu1 N1 97.7(7) . 13 ?
N2 Cu1 N1 97.7(7) 13 . ?
N2 Cu1 N1 82.3(7) . . ?
N1 Cu1 N1 180.000(1) 13 . ?
C3 C1 C2 108(2) . . ?
C3 C1 N1 108(2) . . ?
C2 C1 N1 115(3) . . ?
C3 C1 H1A 108.4 . . ?
C2 C1 H1A 108.4 . . ?
N1 C1 H1A 108.4 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 N2 106(2) . . ?
C1 C3 H3A 110.6 . . ?
N2 C3 H3A 110.6 . . ?
C1 C3 H3B 110.6 . . ?
N2 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
C1 N1 Cu1 105.3(12) . . ?
C1 N1 H1B 110.7 . . ?
Cu1 N1 H1B 110.7 . . ?
C1 N1 H1C 110.7 . . ?
Cu1 N1 H1C 110.7 . . ?
H1B N1 H1C 108.8 . . ?
C3 N2 Cu1 110.9(13) . . ?
C3 N2 H2D 109.5 . . ?
Cu1 N2 H2D 109.5 . . ?
C3 N2 H2E 109.5 . . ?
Cu1 N2 H2E 109.5 . . ?
H2D N2 H2E 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.222
_database_code_depnum_ccdc_archive 'CCDC 973047'
