#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/04/7220447.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7220447
loop_
_publ_author_name
'Lan, Qing'
'Zhang, Zhi-Ming'
'Li, Yang-Guang'
'Wang, Enbo'
_publ_section_title
;
 Extended Structural Materials Composed of Transition-Metal-Substituted
 Arsenicniobates and Their Photocatalytic Activity
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA08262E
_journal_year                    2015
_chemical_formula_sum            'C20 H104 As Cu5 N20 Nb8 O56 V8'
_chemical_formula_weight         3064.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-04 deposited with the CCDC.
2015-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                89.48(3)
_cell_angle_beta                 80.34(3)
_cell_angle_gamma                63.81(3)
_cell_formula_units_Z            1
_cell_length_a                   12.907(3)
_cell_length_b                   14.153(3)
_cell_length_c                   14.277(3)
_cell_measurement_reflns_used    7927
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.03
_cell_volume                     2300.9(11)
_computing_cell_refinement       auto
_computing_data_collection       auto
_computing_data_reduction        auto
_computing_molecular_graphics    auto
_computing_publication_material  auto
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17789
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.306
_exptl_absorpt_correction_T_max  0.467
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1502
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.864
_refine_diff_density_min         -2.878
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7927
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1106P)²+51.5411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2230
_refine_ls_wR_factor_ref         0.2378
_reflns_number_gt                6159
_reflns_number_total             7927
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra08262e2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2300.9(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7220447
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Nb1 Nb 1.21916(9) -0.17434(8) -0.20126(7) 0.0285(3) Uani 1 1 d .
Nb2 Nb 0.86583(11) -0.10386(10) 0.19728(8) 0.0364(3) Uani 1 1 d .
Nb3 Nb 1.30126(11) -0.18576(8) 0.02847(9) 0.0414(3) Uani 1 1 d .
Nb4 Nb 0.78165(14) -0.09171(11) -0.03254(11) 0.0581(5) Uani 1 1 d .
V1 V 1.08544(15) -0.28198(12) -0.00721(13) 0.0208(4) Uani 1 1 d .
V2 V 0.9130(2) 0.01063(14) -0.23427(12) 0.0292(5) Uani 1 1 d U
V3 V 0.9998(2) -0.21265(17) -0.18818(16) 0.0394(5) Uani 1 1 d .
V4 V 1.1313(2) -0.23073(17) 0.17964(16) 0.0381(5) Uani 1 1 d .
As1 As 1.0000 0.0000 0.0000 0.0428(5) Uani 1 2 d S
Cu1 Cu 1.44842(17) -0.0151(2) 0.25401(14) 0.0644(6) Uani 1 1 d D
Cu2 Cu 1.0000 0.0000 -0.5000 0.0527(7) Uani 1 2 d S
Cu3 Cu 1.5000 -0.5000 0.0000 0.0833(11) Uani 1 2 d S
Cu4 Cu 1.0000 0.5000 0.0000 0.0397(5) Uani 1 2 d S
O1 O 1.1839(10) -0.3242(8) 0.2494(7) 0.056(3) Uani 1 1 d .
O2 O 1.2125(7) -0.2745(7) 0.0484(6) 0.0351(19) Uani 1 1 d .
O3 O 1.0038(8) -0.1018(6) 0.2474(6) 0.039(2) Uani 1 1 d .
O4 O 0.6865(8) -0.1417(7) -0.0492(7) 0.045(2) Uani 1 1 d .
O5 O 0.8072(10) -0.1559(8) 0.2896(8) 0.066(3) Uani 1 1 d U
O6 O 0.9375(8) -0.2270(9) -0.0577(7) 0.054(3) Uani 1 1 d .
O7 O 1.0636(10) -0.1216(8) -0.2507(7) 0.050(3) Uani 1 1 d .
O8 O 1.0024(9) -0.2342(10) 0.1269(8) 0.066(3) Uani 1 1 d .
O9 O 0.8765(8) 0.0123(7) -0.3394(6) 0.041(2) Uani 1 1 d .
O10 O 1.1451(8) -0.2651(8) -0.1382(8) 0.057(3) Uani 1 1 d .
O11 O 1.4377(9) -0.2782(9) 0.0470(7) 0.057(3) Uani 1 1 d .
O12 O 1.2114(11) -0.1403(9) 0.1646(9) 0.072(3) Uani 1 1 d U
O13 O 1.1265(10) -0.4090(7) -0.0114(7) 0.050(3) Uani 1 1 d .
O14 O 1.2244(11) -0.0445(9) -0.2323(10) 0.073(3) Uani 1 1 d U
O15 O 0.8524(12) -0.0833(8) -0.1699(9) 0.084(5) Uani 1 1 d .
O16 O 0.9982(10) -0.2989(8) -0.2617(7) 0.054(3) Uani 1 1 d .
O17 O 1.3146(10) -0.2590(10) -0.2967(9) 0.069(3) Uani 1 1 d U
O18 O 1.3151(10) -0.2037(12) -0.1068(8) 0.076(4) Uani 1 1 d .
O19 O 1.3173(16) -0.0573(13) 0.0229(13) 0.109(5) Uani 1 1 d U
O20 O 0.7755(11) -0.1033(13) 0.1033(9) 0.090(4) Uani 1 1 d U
O21 O 1.1205(13) -0.0239(12) 0.0619(9) 0.024(3) Uani 0.50 1 d P
O22 O 1.0417(13) 0.0940(10) -0.0342(11) 0.024(3) Uani 0.50 1 d P
O23 O 0.9412(13) 0.0149(11) 0.1146(11) 0.026(3) Uani 0.50 1 d P
O24 O 1.1026(13) -0.1175(12) -0.0373(10) 0.025(3) Uani 0.50 1 d P
N1 N 0.8763(11) 0.6125(9) 0.0965(9) 0.049(3) Uani 1 1 d .
H1C H 0.8852 0.6721 0.0927 0.059 Uiso 1 1 calc R
H1D H 0.8043 0.6270 0.0855 0.059 Uiso 1 1 calc R
N2 N 1.0764(10) 0.4388(8) 0.1135(9) 0.046(3) Uani 1 1 d .
H2C H 1.0687 0.3800 0.1282 0.056 Uiso 1 1 calc R
H2D H 1.1535 0.4220 0.1001 0.056 Uiso 1 1 calc R
N3 N 0.9703(17) -0.1195(14) -0.5405(10) 0.084(5) Uani 1 1 d .
H3C H 0.8966 -0.1079 -0.5150 0.100 Uiso 1 1 calc R
H3D H 0.9787 -0.1253 -0.6044 0.100 Uiso 1 1 calc R
N4 N 1.506(2) 0.0825(17) 0.1868(15) 0.138(9) Uani 1 1 d DU
H4C H 1.5836 0.0574 0.1869 0.166 Uiso 1 1 calc R
H4D H 1.4966 0.0832 0.1257 0.166 Uiso 1 1 calc R
N5 N 1.1450(15) -0.1120(15) -0.4615(10) 0.087(6) Uani 1 1 d .
H5C H 1.2069 -0.0983 -0.4799 0.105 Uiso 1 1 calc R
H5D H 1.1344 -0.1159 -0.3979 0.105 Uiso 1 1 calc R
N6 N 1.3110(17) 0.1257(17) 0.3098(14) 0.110(7) Uani 1 1 d DU
H6C H 1.2435 0.1255 0.3015 0.133 Uiso 1 1 calc R
H6D H 1.3087 0.1320 0.3729 0.133 Uiso 1 1 calc R
N7 N 1.3862(18) -0.1027(17) 0.3229(14) 0.114(7) Uani 1 1 d DU
H7C H 1.3811 -0.0901 0.3856 0.137 Uiso 1 1 calc R
H7D H 1.3128 -0.0825 0.3124 0.137 Uiso 1 1 calc R
N8 N 1.6164(15) -0.4942(13) -0.1062(17) 0.106(8) Uani 1 1 d .
H8C H 1.6392 -0.4452 -0.0924 0.128 Uiso 1 1 calc R
H8D H 1.6800 -0.5573 -0.1193 0.128 Uiso 1 1 calc R
N9 N 1.3978(19) -0.4771(15) -0.096(2) 0.123(9) Uani 1 1 d .
H9C H 1.3583 -0.5162 -0.0853 0.148 Uiso 1 1 calc R
H9D H 1.3457 -0.4086 -0.0934 0.148 Uiso 1 1 calc R
N10 N 1.571(3) -0.141(2) 0.194(2) 0.177(12) Uani 1 1 d DU
H10C H 1.5660 -0.1443 0.1322 0.212 Uiso 1 1 calc R
H10D H 1.6396 -0.1410 0.1975 0.212 Uiso 1 1 calc R
C1 C 1.0177(16) 0.5190(14) 0.1934(12) 0.062(4) Uani 1 1 d .
H1A H 1.0495 0.5699 0.1886 0.075 Uiso 1 1 calc R
H1B H 1.0301 0.4863 0.2532 0.075 Uiso 1 1 calc R
C2 C 0.8898(17) 0.5730(15) 0.1903(12) 0.069(5) Uani 1 1 d .
H2A H 0.8562 0.5238 0.2018 0.082 Uiso 1 1 calc R
H2B H 0.8495 0.6310 0.2391 0.082 Uiso 1 1 calc R
C3 C 1.4463(18) 0.1887(16) 0.2298(17) 0.088(6) Uani 1 1 d D
H3A H 1.4503 0.2376 0.1830 0.105 Uiso 1 1 calc R
H3B H 1.4835 0.1955 0.2814 0.105 Uiso 1 1 calc R
C4 C 1.4532(17) -0.217(2) 0.2992(15) 0.096(8) Uani 1 1 d D
H4A H 1.4100 -0.2422 0.2657 0.116 Uiso 1 1 calc R
H4B H 1.4674 -0.2537 0.3568 0.116 Uiso 1 1 calc R
C5 C 1.3180(18) 0.2145(18) 0.2684(14) 0.078(6) Uani 1 1 d .
H5A H 1.2840 0.2739 0.3158 0.093 Uiso 1 1 calc R
H5B H 1.2737 0.2342 0.2169 0.093 Uiso 1 1 calc R
C6 C 1.164(2) -0.212(2) -0.5108(19) 0.110(8) Uani 1 1 d U
H6A H 1.2003 -0.2159 -0.5769 0.132 Uiso 1 1 calc R
H6B H 1.2174 -0.2715 -0.4812 0.132 Uiso 1 1 calc R
C7 C 1.057(2) -0.219(2) -0.5069(19) 0.107(8) Uani 1 1 d U
H7A H 1.0269 -0.2272 -0.4420 0.128 Uiso 1 1 calc R
H7B H 1.0696 -0.2790 -0.5470 0.128 Uiso 1 1 calc R
C8 C 1.551(3) -0.464(2) -0.190(2) 0.115(9) Uani 1 1 d U
H8A H 1.5071 -0.3883 -0.1883 0.138 Uiso 1 1 calc R
H8B H 1.6067 -0.4889 -0.2493 0.138 Uiso 1 1 calc R
C9 C 1.475(3) -0.509(2) -0.185(3) 0.138(12) Uani 1 1 d .
H9A H 1.5194 -0.5854 -0.1917 0.165 Uiso 1 1 calc R
H9B H 1.4309 -0.4868 -0.2361 0.165 Uiso 1 1 calc R
C10 C 1.570(2) -0.236(2) 0.2359(18) 0.114(8) Uani 1 1 d DU
H10A H 1.6313 -0.2644 0.2734 0.136 Uiso 1 1 calc R
H10B H 1.5875 -0.2882 0.1848 0.136 Uiso 1 1 calc R
O1W O 1.6652(9) -0.3237(8) -0.0130(9) 0.061(3) Uani 1 1 d .
O2W O 1.257(2) -0.4279(19) -0.3409(18) 0.159(9) Uiso 1 1 d .
O3W O 1.559(2) -0.019(2) 0.3677(19) 0.171(9) Uiso 1 1 d .
O4W O 1.200(2) -0.492(2) 0.3668(19) 0.174(10) Uiso 1 1 d .
O5W O 0.782(3) -0.230(3) 0.462(2) 0.160(11) Uiso 0.75 1 d P
O6W O 0.938(3) -0.385(2) -0.413(2) 0.154(11) Uiso 0.75 1 d P
O7W O 1.592(5) 0.139(4) 0.441(4) 0.174(19) Uiso 0.50 1 d P
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'
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'
As As 0.0499 2.0058 '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'
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
O17 Nb1 O18 102.5(6) . .
O17 Nb1 O14 101.8(6) . .
O18 Nb1 O14 95.3(5) . .
O17 Nb1 O10 100.6(5) . .
O18 Nb1 O10 90.2(5) . .
O14 Nb1 O10 155.1(5) . .
O17 Nb1 O7 100.2(5) . .
O18 Nb1 O7 155.5(5) . .
O14 Nb1 O7 89.0(4) . .
O10 Nb1 O7 76.6(4) . .
O17 Nb1 O23 158.8(6) . 2_755
O18 Nb1 O23 95.0(6) . 2_755
O14 Nb1 O23 64.3(6) . 2_755
O10 Nb1 O23 91.1(5) . 2_755
O7 Nb1 O23 65.2(5) . 2_755
O17 Nb1 O24 158.3(6) . .
O18 Nb1 O24 67.3(5) . .
O14 Nb1 O24 98.2(6) . .
O10 Nb1 O24 61.7(5) . .
O7 Nb1 O24 88.2(5) . .
O23 Nb1 O24 41.8(5) 2_755 .
O17 Nb1 V3 103.0(4) . .
O18 Nb1 V3 125.5(3) . .
O14 Nb1 V3 124.7(4) . .
O10 Nb1 V3 38.2(3) . .
O7 Nb1 V3 38.4(3) . .
O23 Nb1 V3 75.5(3) 2_755 .
O24 Nb1 V3 71.4(3) . .
O5 Nb2 O20 100.3(7) . .
O5 Nb2 O14 100.9(6) . 2_755
O20 Nb2 O14 93.8(6) . 2_755
O5 Nb2 O8 102.5(5) . .
O20 Nb2 O8 89.2(5) . .
O14 Nb2 O8 155.5(5) 2_755 .
O5 Nb2 O3 101.7(5) . .
O20 Nb2 O3 156.5(5) . .
O14 Nb2 O3 90.0(4) 2_755 .
O8 Nb2 O3 78.2(4) . .
O5 Nb2 O22 157.3(5) . 2_755
O20 Nb2 O22 66.9(6) . 2_755
O14 Nb2 O22 98.7(5) 2_755 2_755
O8 Nb2 O22 60.3(5) . 2_755
O3 Nb2 O22 89.6(4) . 2_755
O5 Nb2 O23 158.9(6) . .
O20 Nb2 O23 94.9(6) . .
O14 Nb2 O23 63.3(5) 2_755 .
O8 Nb2 O23 92.2(5) . .
O3 Nb2 O23 66.2(4) . .
O22 Nb2 O23 43.6(5) 2_755 .
O5 Nb2 V4 104.8(4) . .
O20 Nb2 V4 125.9(4) . .
O14 Nb2 V4 126.3(4) 2_755 .
O8 Nb2 V4 39.1(3) . .
O3 Nb2 V4 39.1(2) . .
O22 Nb2 V4 71.9(3) 2_755 .
O23 Nb2 V4 77.2(3) . .
O11 Nb3 O18 102.3(5) . .
O11 Nb3 O19 103.0(7) . .
O18 Nb3 O19 94.0(7) . .
O11 Nb3 O2 99.6(4) . .
O18 Nb3 O2 90.1(4) . .
O19 Nb3 O2 155.6(6) . .
O11 Nb3 O12 101.4(5) . .
O18 Nb3 O12 154.5(5) . .
O19 Nb3 O12 89.7(6) . .
O2 Nb3 O12 76.8(4) . .
O11 Nb3 O21 155.6(5) . .
O18 Nb3 O21 99.3(5) . .
O19 Nb3 O21 64.0(6) . .
O2 Nb3 O21 91.6(4) . .
O12 Nb3 O21 60.0(5) . .
O11 Nb3 V4 102.7(3) . .
O18 Nb3 V4 125.3(3) . .
O19 Nb3 V4 125.8(5) . .
O2 Nb3 V4 38.2(2) . .
O12 Nb3 V4 38.6(3) . .
O21 Nb3 V4 73.2(3) . .
O4 Nb4 O19 102.0(6) . 2_755
O4 Nb4 O20 99.4(5) . .
O19 Nb4 O20 95.3(7) 2_755 .
O4 Nb4 O15 101.7(6) . .
O19 Nb4 O15 90.0(6) 2_755 .
O20 Nb4 O15 156.7(6) . .
O4 Nb4 O6 100.2(4) . .
O19 Nb4 O6 156.0(6) 2_755 .
O20 Nb4 O6 89.9(5) . .
O15 Nb4 O6 76.7(4) . .
O4 Nb4 O21 155.9(5) . 2_755
O19 Nb4 O21 63.0(6) 2_755 2_755
O20 Nb4 O21 100.7(6) . 2_755
O15 Nb4 O21 61.7(5) . 2_755
O6 Nb4 O21 93.1(4) . 2_755
O4 Nb4 V3 104.3(3) . .
O19 Nb4 V3 125.5(5) 2_755 .
O20 Nb4 V3 125.6(4) . .
O15 Nb4 V3 38.4(3) . .
O6 Nb4 V3 38.3(3) . .
O21 Nb4 V3 74.2(3) 2_755 .
O13 V1 O10 101.0(5) . .
O13 V1 O6 102.6(5) . .
O10 V1 O6 80.8(4) . .
O13 V1 O2 100.7(5) . .
O10 V1 O2 95.9(4) . .
O6 V1 O2 156.6(4) . .
O13 V1 O8 103.2(5) . .
O10 V1 O8 155.8(5) . .
O6 V1 O8 93.2(4) . .
O2 V1 O8 80.3(4) . .
O13 V1 O22 158.2(5) . 2_755
O10 V1 O22 95.5(5) . 2_755
O6 V1 O22 66.0(5) . 2_755
O2 V1 O22 91.5(4) . 2_755
O8 V1 O22 61.0(5) . 2_755
O13 V1 O24 157.3(5) . .
O10 V1 O24 63.0(5) . .
O6 V1 O24 91.1(5) . .
O2 V1 O24 67.2(4) . .
O8 V1 O24 93.9(5) . .
O22 V1 O24 44.5(5) 2_755 .
O13 V1 V3 105.2(4) . .
O10 V1 V3 40.3(3) . .
O6 V1 V3 40.5(3) . .
O2 V1 V3 132.3(2) . .
O8 V1 V3 129.8(4) . .
O22 V1 V3 78.6(4) 2_755 .
O24 V1 V3 73.8(3) . .
O13 V1 V4 105.0(4) . .
O10 V1 V4 131.9(4) . .
O6 V1 V4 130.1(3) . .
O2 V1 V4 39.9(3) . .
O8 V1 V4 40.3(3) . .
O22 V1 V4 73.3(4) 2_755 .
O24 V1 V4 78.6(3) . .
V3 V1 V4 149.88(8) . .
O9 V2 O12 104.2(5) . 2_755
O9 V2 O15 101.3(6) . .
O12 V2 O15 95.0(4) 2_755 .
O9 V2 O7 101.3(4) . .
O12 V2 O7 154.4(5) 2_755 .
O15 V2 O7 81.6(4) . .
O9 V2 O3 102.7(4) . 2_755
O12 V2 O3 80.4(4) 2_755 2_755
O15 V2 O3 156.0(6) . 2_755
O7 V2 O3 92.4(4) . 2_755
O9 V2 O21 155.4(5) . 2_755
O12 V2 O21 60.8(5) 2_755 2_755
O15 V2 O21 63.5(6) . 2_755
O7 V2 O21 95.6(5) . 2_755
O3 V2 O21 94.2(4) 2_755 2_755
O9 V2 V3 104.5(3) . .
O12 V2 V3 131.1(3) 2_755 .
O15 V2 V3 40.8(3) . .
O7 V2 V3 40.8(3) . .
O3 V2 V3 129.4(3) 2_755 .
O21 V2 V3 77.2(4) 2_755 .
O9 V2 V4 107.0(3) . 2_755
O12 V2 V4 40.2(3) 2_755 2_755
O15 V2 V4 131.3(3) . 2_755
O7 V2 V4 128.5(3) . 2_755
O3 V2 V4 40.2(3) 2_755 2_755
O21 V2 V4 74.9(4) 2_755 2_755
V3 V2 V4 148.49(10) . 2_755
O16 V3 O10 112.7(6) . .
O16 V3 O6 111.1(5) . .
O10 V3 O6 81.8(4) . .
O16 V3 O7 113.3(5) . .
O10 V3 O7 81.2(4) . .
O6 V3 O7 135.6(5) . .
O16 V3 O15 111.2(6) . .
O10 V3 O15 136.1(6) . .
O6 V3 O15 81.4(5) . .
O7 V3 O15 83.2(5) . .
O16 V3 V2 119.8(4) . .
O10 V3 V2 113.0(3) . .
O6 V3 V2 112.4(4) . .
O7 V3 V2 42.0(3) . .
O15 V3 V2 41.2(3) . .
O16 V3 V1 119.1(4) . .
O10 V3 V1 40.6(3) . .
O6 V3 V1 41.2(3) . .
O7 V3 V1 111.9(3) . .
O15 V3 V1 112.8(4) . .
V2 V3 V1 121.12(9) . .
O16 V3 Nb4 118.8(4) . .
O10 V3 Nb4 112.2(3) . .
O6 V3 Nb4 40.8(3) . .
O7 V3 Nb4 112.8(3) . .
O15 V3 Nb4 40.6(3) . .
V2 V3 Nb4 75.56(8) . .
V1 V3 Nb4 76.00(7) . .
O16 V3 Nb1 120.6(4) . .
O10 V3 Nb1 40.3(3) . .
O6 V3 Nb1 112.1(3) . .
O7 V3 Nb1 40.9(3) . .
O15 V3 Nb1 113.8(4) . .
V2 V3 Nb1 76.99(7) . .
V1 V3 Nb1 75.07(7) . .
Nb4 V3 Nb1 120.59(8) . .
O1 V4 O2 111.5(5) . .
O1 V4 O3 112.7(5) . .
O2 V4 O3 135.7(4) . .
O1 V4 O8 112.6(6) . .
O2 V4 O8 82.1(4) . .
O3 V4 O8 81.9(4) . .
O1 V4 O12 113.5(6) . .
O2 V4 O12 80.6(4) . .
O3 V4 O12 81.5(4) . .
O8 V4 O12 133.9(6) . .
O1 V4 V1 119.1(4) . .
O2 V4 V1 40.8(3) . .
O3 V4 V1 113.1(3) . .
O8 V4 V1 41.2(3) . .
O12 V4 V1 111.0(4) . .
O1 V4 V2 120.4(4) . 2_755
O2 V4 V2 111.5(3) . 2_755
O3 V4 V2 41.4(3) . 2_755
O8 V4 V2 112.4(4) . 2_755
O12 V4 V2 40.1(3) . 2_755
V1 V4 V2 120.44(9) . 2_755
O1 V4 Nb2 119.7(4) . .
O2 V4 Nb2 113.0(3) . .
O3 V4 Nb2 41.2(3) . .
O8 V4 Nb2 40.7(3) . .
O12 V4 Nb2 112.1(4) . .
V1 V4 Nb2 76.41(8) . .
V2 V4 Nb2 76.51(8) 2_755 .
O1 V4 Nb3 119.3(4) . .
O2 V4 Nb3 40.2(3) . .
O3 V4 Nb3 112.5(3) . .
O8 V4 Nb3 111.9(4) . .
O12 V4 Nb3 40.4(3) . .
V1 V4 Nb3 75.15(7) . .
V2 V4 Nb3 75.31(7) 2_755 .
Nb2 V4 Nb3 120.98(8) . .
O24 As1 O24 180(2) . 2_755
O24 As1 O23 115.1(7) . .
O24 As1 O23 64.9(7) 2_755 .
O24 As1 O23 64.9(7) . 2_755
O24 As1 O23 115.1(7) 2_755 2_755
O23 As1 O23 180.0(13) . 2_755
O24 As1 O22 111.7(7) . .
O24 As1 O22 68.3(7) 2_755 .
O23 As1 O22 113.1(7) . .
O23 As1 O22 66.9(7) 2_755 .
O24 As1 O22 68.3(7) . 2_755
O24 As1 O22 111.7(7) 2_755 2_755
O23 As1 O22 66.9(7) . 2_755
O23 As1 O22 113.1(7) 2_755 2_755
O22 As1 O22 180.0(14) . 2_755
O24 As1 O21 73.1(7) . .
O24 As1 O21 106.9(7) 2_755 .
O23 As1 O21 75.3(7) . .
O23 As1 O21 104.7(7) 2_755 .
O22 As1 O21 75.7(7) . .
O22 As1 O21 104.3(7) 2_755 .
O24 As1 O21 106.9(7) . 2_755
O24 As1 O21 73.1(7) 2_755 2_755
O23 As1 O21 104.7(7) . 2_755
O23 As1 O21 75.3(7) 2_755 2_755
O22 As1 O21 104.3(7) . 2_755
O22 As1 O21 75.7(7) 2_755 2_755
O21 As1 O21 180.0(8) . 2_755
N10 Cu1 N7 86.1(12) . .
N10 Cu1 N6 175.7(8) . .
N7 Cu1 N6 95.7(9) . .
N10 Cu1 N4 96.9(12) . .
N7 Cu1 N4 177.0(9) . .
N6 Cu1 N4 81.4(9) . .
N10 Cu1 O3W 90.0(10) . .
N7 Cu1 O3W 93.1(9) . .
N6 Cu1 O3W 93.8(8) . .
N4 Cu1 O3W 86.6(8) . .
N3 Cu2 N3 180.0(9) 2_754 .
N3 Cu2 N5 94.3(8) 2_754 .
N3 Cu2 N5 85.7(8) . .
N3 Cu2 N5 85.7(8) 2_754 2_754
N3 Cu2 N5 94.3(8) . 2_754
N5 Cu2 N5 180.0(8) . 2_754
N8 Cu3 N8 180.0(9) 2_845 .
N8 Cu3 N9 86.1(10) 2_845 2_845
N8 Cu3 N9 93.9(10) . 2_845
N8 Cu3 N9 93.9(10) 2_845 .
N8 Cu3 N9 86.1(10) . .
N9 Cu3 N9 180.0(12) 2_845 .
N1 Cu4 N1 180.0(12) 2_765 .
N1 Cu4 N2 95.5(5) 2_765 .
N1 Cu4 N2 84.5(5) . .
N1 Cu4 N2 84.5(5) 2_765 2_765
N1 Cu4 N2 95.5(5) . 2_765
N2 Cu4 N2 180.0(7) . 2_765
V4 O2 V1 99.2(4) . .
V4 O2 Nb3 101.6(4) . .
V1 O2 Nb3 134.7(4) . .
V4 O3 V2 98.4(4) . 2_755
V4 O3 Nb2 99.7(4) . .
V2 O3 Nb2 135.8(4) 2_755 .
V3 O6 V1 98.3(4) . .
V3 O6 Nb4 100.9(5) . .
V1 O6 Nb4 135.3(5) . .
V3 O7 V2 97.2(5) . .
V3 O7 Nb1 100.7(4) . .
V2 O7 Nb1 136.5(5) . .
V4 O8 V1 98.4(4) . .
V4 O8 Nb2 100.2(4) . .
V1 O8 Nb2 137.2(8) . .
V3 O10 V1 99.1(4) . .
V3 O10 Nb1 101.6(4) . .
V1 O10 Nb1 135.2(7) . .
V2 O12 V4 99.7(5) 2_755 .
V2 O12 Nb3 136.7(7) 2_755 .
V4 O12 Nb3 100.9(5) . .
Nb1 O14 Nb2 139.0(8) . 2_755
V3 O15 V2 98.0(5) . .
V3 O15 Nb4 101.0(6) . .
V2 O15 Nb4 134.6(7) . .
Nb1 O18 Nb3 140.3(7) . .
Nb3 O19 Nb4 138.5(10) . 2_755
Nb2 O20 Nb4 138.6(8) . .
As1 O21 Nb3 121.0(7) . .
As1 O21 V2 120.1(7) . 2_755
Nb3 O21 V2 100.2(5) . 2_755
As1 O21 Nb4 117.5(7) . 2_755
Nb3 O21 Nb4 94.4(5) . 2_755
V2 O21 Nb4 98.6(5) 2_755 2_755
As1 O22 V1 122.7(7) . 2_755
As1 O22 Nb2 124.7(7) . 2_755
V1 O22 Nb2 99.2(5) 2_755 2_755
As1 O23 O24 56.7(7) . 2_755
As1 O23 Nb1 126.9(8) . 2_755
O24 O23 Nb1 70.3(7) 2_755 2_755
As1 O23 Nb2 124.8(7) . .
O24 O23 Nb2 138.9(9) 2_755 .
Nb1 O23 Nb2 93.4(5) 2_755 .
As1 O24 O23 58.4(7) . 2_755
As1 O24 V1 124.6(7) . .
O23 O24 V1 138.8(9) 2_755 .
As1 O24 Nb1 126.3(7) . .
O23 O24 Nb1 67.9(6) 2_755 .
V1 O24 Nb1 96.5(5) . .
C2 N1 Cu4 107.7(10) . .
C1 N2 Cu4 107.5(9) . .
C7 N3 Cu2 108.1(15) . .
C3 N4 Cu1 113.0(17) . .
C6 N5 Cu2 105.1(14) . .
C5 N6 Cu1 113.5(15) . .
C4 N7 Cu1 116.2(15) . .
C8 N8 Cu3 104.0(15) . .
C9 N9 Cu3 105.1(19) . .
C10 N10 Cu1 114(2) . .
N2 C1 C2 108.2(14) . .
N1 C2 C1 108.0(14) . .
N4 C3 C5 108.9(19) . .
N7 C4 C10 107(2) . .
N6 C5 C3 110.0(19) . .
C7 C6 N5 111(2) . .
C6 C7 N3 109(2) . .
C9 C8 N8 110(3) . .
C8 C9 N9 109(3) . .
N10 C10 C4 114(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O17 1.724(10) .
Nb1 O18 1.903(10) .
Nb1 O14 1.913(11) .
Nb1 O10 2.036(9) .
Nb1 O7 2.057(10) .
Nb1 O23 2.445(14) 2_755
Nb1 O24 2.484(15) .
Nb1 V3 3.085(3) .
Nb2 O5 1.730(9) .
Nb2 O20 1.917(12) .
Nb2 O14 1.919(12) 2_755
Nb2 O8 2.022(10) .
Nb2 O3 2.039(9) .
Nb2 O22 2.465(15) 2_755
Nb2 O23 2.487(15) .
Nb2 V4 3.052(3) .
Nb3 O11 1.732(10) .
Nb3 O18 1.918(12) .
Nb3 O19 1.919(16) .
Nb3 O2 2.032(8) .
Nb3 O12 2.036(11) .
Nb3 O21 2.418(15) .
Nb3 V4 3.082(3) .
Nb4 O4 1.713(9) .
Nb4 O19 1.914(17) 2_755
Nb4 O20 1.936(14) .
Nb4 O15 2.045(11) .
Nb4 O6 2.052(11) .
Nb4 O21 2.465(14) 2_755
Nb4 V3 3.084(3) .
V1 O13 1.633(8) .
V1 O10 1.955(10) .
V1 O6 1.978(10) .
V1 O2 1.981(9) .
V1 O8 1.992(10) .
V1 O22 2.444(13) 2_755
V1 O24 2.461(14) .
V1 V3 2.969(3) .
V1 V4 2.989(3) .
V2 O9 1.644(9) .
V2 O12 1.957(11) 2_755
V2 O15 1.969(11) .
V2 O7 1.995(11) .
V2 O3 2.001(9) 2_755
V2 O21 2.420(13) 2_755
V2 V3 2.959(3) .
V2 V4 2.994(3) 2_755
V3 O16 1.627(10) .
V3 O10 1.946(11) .
V3 O6 1.947(10) .
V3 O7 1.950(9) .
V3 O15 1.951(12) .
V4 O1 1.617(9) .
V4 O2 1.945(9) .
V4 O3 1.954(9) .
V4 O8 1.956(10) .
V4 O12 1.960(11) .
V4 V2 2.994(3) 2_755
As1 O24 1.624(15) .
As1 O24 1.624(15) 2_755
As1 O23 1.657(15) .
As1 O23 1.657(15) 2_755
As1 O22 1.682(14) .
As1 O22 1.682(14) 2_755
As1 O21 1.819(15) .
As1 O21 1.819(15) 2_755
Cu1 N10 1.87(3) .
Cu1 N7 1.935(19) .
Cu1 N6 2.05(2) .
Cu1 N4 2.01(2) .
Cu1 O3W 2.32(3) .
Cu2 N3 2.002(16) 2_754
Cu2 N3 2.002(16) .
Cu2 N5 2.008(16) .
Cu2 N5 2.008(16) 2_754
Cu3 N8 1.976(18) 2_845
Cu3 N8 1.976(18) .
Cu3 N9 1.98(2) 2_845
Cu3 N9 1.98(2) .
Cu4 N1 2.010(12) 2_765
Cu4 N1 2.010(12) .
Cu4 N2 2.027(12) .
Cu4 N2 2.027(12) 2_765
O3 V2 2.001(9) 2_755
O12 V2 1.957(11) 2_755
O14 Nb2 1.919(12) 2_755
O19 Nb4 1.914(17) 2_755
O21 V2 2.420(13) 2_755
O21 Nb4 2.465(14) 2_755
O22 V1 2.444(13) 2_755
O22 Nb2 2.465(15) 2_755
O23 O24 1.76(2) 2_755
O23 Nb1 2.445(14) 2_755
O24 O23 1.76(2) 2_755
N1 C2 1.46(2) .
N2 C1 1.46(2) .
N3 C7 1.49(3) .
N4 C3 1.438(10) .
N5 C6 1.49(3) .
N6 C5 1.42(3) .
N7 C4 1.46(3) .
N8 C8 1.53(3) .
N9 C9 1.42(4) .
N10 C10 1.46(4) .
C1 C2 1.49(3) .
C3 C5 1.53(3) .
C4 C10 1.53(3) .
C6 C7 1.42(4) .
C8 C9 1.37(4) .
