#------------------------------------------------------------------------------
#$Date: 2019-11-24 00:35:08 +0200 (Sun, 24 Nov 2019) $
#$Revision: 235786 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/97/4349746.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_4349746
loop_
_publ_author_name
'Zhang, Ting-Ting'
'Zhang, Xiao'
'Lü, Ying'
'Li, Guo-Dong'
'Xiao, Li-Na'
'Cui, Xiao-Bing'
'Xu, Ji-Qing'
_publ_section_title
;
 New organic--inorganic hybrid compounds based on [SiNb12V2O42]12−
 with high catalytic activity for styrene epoxidation
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1397
_journal_paper_doi               10.1039/C7QI00318H
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C24 H138 Cu6 N24 Nb12 O63 Si V2'
_chemical_formula_weight         3397.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.742(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.2503(7)
_cell_length_b                   20.5402(6)
_cell_length_c                   20.6527(7)
_cell_measurement_reflns_used    12028
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8800
_cell_measurement_theta_min      3.6240
_cell_volume                     9829.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23698
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         3.102
_exptl_absorpt_coefficient_mu    2.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74360
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_description       block
_exptl_crystal_F_000             6720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.827
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         11280
_refine_ls_number_restraints     602
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0801
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0262P)²+576.3777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9778
_reflns_number_total             11280
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7qi00318h2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4349746
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Nb1 Nb 0.38082(3) 0.65212(4) 0.67522(4) 0.02315(17) Uani 1 1 d . . .
Nb2 Nb 0.5000 0.56242(5) 0.7500 0.0262(2) Uani 1 2 d S T P
Nb3 Nb 0.5000 0.92432(5) 0.7500 0.0223(2) Uani 1 2 d S T P
Nb4 Nb 0.46825(3) 0.74386(4) 0.57290(3) 0.02219(16) Uani 1 1 d . . .
Nb5 Nb 0.58609(3) 0.65134(4) 0.64519(4) 0.02616(18) Uani 1 1 d . . .
Nb6 Nb 0.58642(3) 0.83556(4) 0.64460(4) 0.02202(17) Uani 1 1 d . . .
Nb7 Nb 0.38079(3) 0.83434(4) 0.67536(4) 0.02489(18) Uani 1 1 d . . .
V1 V 0.67070(5) 0.74285(7) 0.72433(6) 0.0178(3) Uani 1 1 d . . .
Si1 Si 0.5000 0.74303(13) 0.7500 0.0086(5) Uani 1 2 d S T P
O1 O 0.4496(7) 0.7434(7) 0.6903(7) 0.0391(17) Uani 0.5 1 d . U P
O2 O 0.5264(7) 0.7437(7) 0.6782(7) 0.0397(16) Uani 0.5 1 d . U P
O3 O 0.5401(6) 0.8096(7) 0.7444(6) 0.0342(18) Uani 0.5 1 d . U P
O4 O 0.4589(6) 0.6767(7) 0.7551(7) 0.0350(18) Uani 0.5 1 d . U P
O5 O 0.5449(4) 0.9076(4) 0.6747(4) 0.0541(16) Uani 1 1 d . U .
O6 O 0.3184(3) 0.6146(4) 0.6398(4) 0.053(2) Uani 1 1 d . U .
O7 O 0.5454(4) 0.5772(5) 0.6744(5) 0.0632(17) Uani 1 1 d . U .
O8 O 0.4293(4) 0.9071(4) 0.6933(4) 0.0543(17) Uani 1 1 d . U .
O9 O 0.6399(4) 0.8309(3) 0.7289(3) 0.0403(14) Uani 1 1 d . U .
O10 O 0.5000 1.0086(5) 0.7500 0.050(3) Uani 1 2 d S TU P
O11 O 0.4289(4) 0.5788(5) 0.6948(4) 0.0620(18) Uani 1 1 d . U .
O12 O 0.5287(4) 0.6769(4) 0.5798(5) 0.0599(17) Uani 1 1 d . U .
O13 O 0.4145(4) 0.6773(4) 0.5997(5) 0.0590(15) Uani 1 1 d . U .
O14 O 0.6322(3) 0.6101(4) 0.5954(4) 0.0415(17) Uani 1 1 d . U .
O15 O 0.4501(5) 0.7409(4) 0.4898(4) 0.065(2) Uani 1 1 d . U .
O16 O 0.4124(4) 0.8093(4) 0.5971(4) 0.0536(15) Uani 1 1 d . U .
O17 O 0.3455(3) 0.7430(3) 0.6852(3) 0.0406(14) Uani 1 1 d . U .
O18 O 0.5276(4) 0.8104(4) 0.5799(5) 0.0574(16) Uani 1 1 d . U .
O19 O 0.6394(4) 0.6548(4) 0.7294(3) 0.0429(15) Uani 1 1 d . U .
O20 O 0.5000 0.4788(6) 0.7500 0.061(3) Uani 1 2 d S TU P
O21 O 0.6226(3) 0.7427(3) 0.6426(4) 0.0402(14) Uani 1 1 d . U .
O22 O 0.3165(3) 0.8725(3) 0.6441(3) 0.0362(15) Uani 1 1 d . U .
O23 O 0.7390(3) 0.7420(3) 0.7134(3) 0.0298(13) Uani 1 1 d . U .
O24 O 0.6344(3) 0.8753(4) 0.5963(4) 0.0408(16) Uani 1 1 d . U .
Cu1 Cu 0.75145(7) 0.98883(7) 0.74595(8) 0.0442(3) Uani 1 1 d . . .
N1 N 0.6655(5) 0.9915(6) 0.7393(9) 0.083(4) Uani 1 1 d . . .
H1C H 0.6520 0.9832 0.6985 0.100 Uiso 1 1 calc R U .
H1D H 0.6523 0.9608 0.7646 0.100 Uiso 1 1 calc R U .
C1 C 0.6454(10) 1.0530(11) 0.7582(13) 0.128(8) Uani 1 1 d D U .
H1A H 0.6294 1.0482 0.7998 0.154 Uiso 1 1 calc R U .
H1B H 0.6142 1.0663 0.7269 0.154 Uiso 1 1 calc R U .
C2 C 0.6871(8) 1.1040(8) 0.7637(14) 0.118(9) Uani 1 1 d D U .
H2A H 0.6795 1.1312 0.8005 0.141 Uiso 1 1 calc R U .
H2B H 0.6823 1.1308 0.7250 0.141 Uiso 1 1 calc R U .
N2 N 0.7462(5) 1.0820(6) 0.7720(7) 0.070(4) Uani 1 1 d . . .
H2C H 0.7596 1.0865 0.8134 0.084 Uiso 1 1 calc R U .
H2D H 0.7678 1.1063 0.7479 0.084 Uiso 1 1 calc R U .
N3 N 0.7570(6) 0.8942(6) 0.7317(8) 0.081(4) Uani 1 1 d . . .
H3C H 0.7323 0.8736 0.7553 0.097 Uiso 1 1 calc R U .
H3D H 0.7475 0.8852 0.6900 0.097 Uiso 1 1 calc R U .
C3 C 0.8147(7) 0.8718(8) 0.7497(12) 0.099(7) Uani 1 1 d . . .
H3A H 0.8174 0.8579 0.7947 0.119 Uiso 1 1 calc R U .
H3B H 0.8228 0.8344 0.7232 0.119 Uiso 1 1 calc R U .
C4 C 0.8557(7) 0.9199(8) 0.7417(13) 0.104(7) Uani 1 1 d . . .
H4A H 0.8635 0.9218 0.6963 0.124 Uiso 1 1 calc R U .
H4B H 0.8914 0.9083 0.7668 0.124 Uiso 1 1 calc R U .
N4 N 0.8373(5) 0.9842(6) 0.7622(7) 0.068(3) Uani 1 1 d . . .
H4C H 0.8537 1.0151 0.7398 0.082 Uiso 1 1 calc R U .
H4D H 0.8477 0.9902 0.8042 0.082 Uiso 1 1 calc R U .
Cu2 Cu 0.5000 1.0000 0.5000 0.0386(4) Uani 1 2 d S . P
N5 N 0.4421(4) 1.0705(5) 0.5163(5) 0.048(2) Uani 1 1 d . . .
H5C H 0.4600 1.1054 0.5336 0.057 Uiso 1 1 calc R U .
H5D H 0.4226 1.0822 0.4791 0.057 Uiso 1 1 calc R U .
C5 C 0.4025(7) 1.0435(8) 0.5612(8) 0.072(5) Uani 1 1 d . . .
H5A H 0.3659 1.0662 0.5554 0.086 Uiso 1 1 calc R U .
H5B H 0.4185 1.0506 0.6056 0.086 Uiso 1 1 calc R U .
C6 C 0.3930(6) 0.9734(7) 0.5503(8) 0.071(4) Uani 1 1 d . . .
H6A H 0.3727 0.9550 0.5852 0.085 Uiso 1 1 calc R U .
H6B H 0.3697 0.9664 0.5097 0.085 Uiso 1 1 calc R U .
N6 N 0.4494(4) 0.9421(5) 0.5480(5) 0.050(3) Uani 1 1 d . . .
H6C H 0.4453 0.9038 0.5280 0.060 Uiso 1 1 calc R U .
H6D H 0.4653 0.9353 0.5882 0.060 Uiso 1 1 calc R U .
Cu3 Cu 0.2500 0.7500 0.5000 0.0450(5) Uani 1 2 d S . P
N7 N 0.3118(5) 0.8177(6) 0.4983(5) 0.057(3) Uani 1 1 d . . .
H7C H 0.3005 0.8538 0.5174 0.069 Uiso 1 1 calc R U .
H7D H 0.3438 0.8035 0.5205 0.069 Uiso 1 1 calc R U .
C7 C 0.3239(8) 0.8322(9) 0.4327(7) 0.078(5) Uani 1 1 d . . .
H7A H 0.3648 0.8411 0.4318 0.094 Uiso 1 1 calc R U .
H7B H 0.3030 0.8711 0.4184 0.094 Uiso 1 1 calc R U .
C8 C 0.3081(6) 0.7796(8) 0.3884(7) 0.066(4) Uani 1 1 d . . .
H8A H 0.3008 0.7971 0.3448 0.079 Uiso 1 1 calc R U .
H8B H 0.3402 0.7494 0.3880 0.079 Uiso 1 1 calc R U .
N8 N 0.2578(5) 0.7453(6) 0.4058(5) 0.059(3) Uani 1 1 d . . .
H8C H 0.2602 0.7038 0.3940 0.071 Uiso 1 1 calc R U .
H8D H 0.2266 0.7623 0.3845 0.071 Uiso 1 1 calc R U .
Cu4 Cu 0.7500 0.7500 0.5000 0.0510(6) Uani 1 2 d S . P
N9 N 0.7164(5) 0.7850(5) 0.4143(5) 0.059(3) Uani 1 1 d . . .
H9C H 0.7180 0.8283 0.4144 0.071 Uiso 1 1 calc R U .
H9D H 0.7365 0.7704 0.3824 0.071 Uiso 1 1 calc R U .
C9 C 0.6555(8) 0.7630(13) 0.4038(9) 0.112(8) Uani 1 1 d . . .
H9A H 0.6337 0.7942 0.3763 0.134 Uiso 1 1 calc R U .
H9B H 0.6541 0.7214 0.3815 0.134 Uiso 1 1 calc R U .
C10 C 0.6299(7) 0.7567(9) 0.4638(8) 0.078(5) Uani 1 1 d . . .
H10A H 0.6171 0.7993 0.4770 0.093 Uiso 1 1 calc R U .
H10B H 0.5962 0.7290 0.4573 0.093 Uiso 1 1 calc R U .
N10 N 0.6679(5) 0.7303(6) 0.5146(6) 0.063(3) Uani 1 1 d . . .
H10C H 0.6629 0.6874 0.5163 0.075 Uiso 1 1 calc R U .
H10D H 0.6595 0.7471 0.5524 0.075 Uiso 1 1 calc R U .
Cu5 Cu 0.5000 0.5000 0.5000 0.0374(4) Uani 1 2 d S . P
N11 N 0.4591(5) 0.4183(5) 0.5236(5) 0.052(3) Uani 1 1 d . . .
H11C H 0.4397 0.4016 0.4884 0.062 Uiso 1 1 calc R U .
H11D H 0.4846 0.3888 0.5394 0.062 Uiso 1 1 calc R U .
C11 C 0.4189(9) 0.4344(9) 0.5726(9) 0.094(6) Uani 1 1 d . . .
H11A H 0.3858 0.4057 0.5676 0.113 Uiso 1 1 calc R U .
H11B H 0.4379 0.4277 0.6157 0.113 Uiso 1 1 calc R U .
C12 C 0.4007(9) 0.4983(10) 0.5664(12) 0.125(10) Uani 1 1 d . . .
H12A H 0.3828 0.5106 0.6054 0.150 Uiso 1 1 calc R U .
H12B H 0.3715 0.5012 0.5302 0.150 Uiso 1 1 calc R U .
N12 N 0.4461(5) 0.5439(5) 0.5562(6) 0.062(3) Uani 1 1 d . . .
H12C H 0.4646 0.5551 0.5941 0.074 Uiso 1 1 calc R U .
H12D H 0.4316 0.5797 0.5369 0.074 Uiso 1 1 calc R U .
O1W O 0.7522(6) 1.0127(7) 0.6332(6) 0.099(4) Uani 1 1 d . U .
O2W O 0.5782(5) 0.4743(5) 0.6004(6) 0.079(3) Uani 1 1 d . U .
O3W O 0.7367(4) 0.5745(5) 0.5638(5) 0.060(2) Uani 1 1 d . U .
O4W O 0.7443(5) 0.8743(8) 0.5598(6) 0.097(4) Uani 1 1 d . U .
O5W O 0.5593(5) 1.0313(6) 0.6070(6) 0.085(3) Uani 1 1 d . U .
O6W O 0.4825(6) 0.8327(6) 0.4011(6) 0.098(3) Uani 1 1 d . U .
O7W O 0.2312(6) 0.9445(6) 0.5887(7) 0.104(4) Uani 1 1 d . U .
O8W O 0.3283(6) 0.6485(6) 0.5000(6) 0.092(3) Uani 1 1 d . U .
O9W O 0.4383(7) 0.6625(7) 0.3873(7) 0.105(3) Uani 1 1 d . U .
O10W O 0.5075(12) 0.3489(13) 0.7799(12) 0.098(7) Uani 0.5 1 d . U P
O11W O 0.5057(13) 1.1380(13) 0.7796(12) 0.103(7) Uani 0.5 1 d . U P
O12W O 0.9226(16) 0.7433(18) 0.7649(18) 0.141(12) Uani 0.5 1 d . U 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'
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'
Si Si 0.0817 0.0704 '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'
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
O6 Nb1 O13 99.4(4) . .
O6 Nb1 O11 101.2(5) . .
O13 Nb1 O11 96.7(4) . .
O6 Nb1 O17 96.8(4) . .
O13 Nb1 O17 91.8(3) . .
O11 Nb1 O17 158.6(4) . .
O6 Nb1 O19 99.4(4) . 2_656
O13 Nb1 O19 158.6(4) . 2_656
O11 Nb1 O19 89.7(3) . 2_656
O17 Nb1 O19 75.8(3) . 2_656
O6 Nb1 O4 158.9(5) . .
O13 Nb1 O4 99.8(5) . .
O11 Nb1 O4 67.8(4) . .
O17 Nb1 O4 91.4(4) . .
O19 Nb1 O4 63.8(4) 2_656 .
O6 Nb1 O1 153.5(5) . .
O13 Nb1 O1 65.5(5) . .
O11 Nb1 O1 102.2(5) . .
O17 Nb1 O1 63.7(4) . .
O19 Nb1 O1 93.2(4) 2_656 .
O4 Nb1 O1 46.3(5) . .
O6 Nb1 V1 101.0(3) . 2_656
O13 Nb1 V1 127.0(3) . 2_656
O11 Nb1 V1 125.9(3) . 2_656
O17 Nb1 V1 37.63(19) . 2_656
O19 Nb1 V1 38.2(2) 2_656 2_656
O4 Nb1 V1 74.1(3) . 2_656
O1 Nb1 V1 75.0(3) . 2_656
O20 Nb2 O11 99.9(3) . 2_656
O20 Nb2 O11 99.9(3) . .
O11 Nb2 O11 160.2(6) 2_656 .
O20 Nb2 O7 98.8(3) . .
O11 Nb2 O7 87.3(4) 2_656 .
O11 Nb2 O7 89.7(4) . .
O20 Nb2 O7 98.8(3) . 2_656
O11 Nb2 O7 89.7(4) 2_656 2_656
O11 Nb2 O7 87.3(4) . 2_656
O7 Nb2 O7 162.3(6) . 2_656
O20 Nb2 O4 157.6(3) . 2_656
O11 Nb2 O4 64.1(4) 2_656 2_656
O11 Nb2 O4 96.8(5) . 2_656
O7 Nb2 O4 66.3(4) . 2_656
O7 Nb2 O4 96.8(4) 2_656 2_656
O20 Nb2 O4 157.6(3) . .
O11 Nb2 O4 96.8(5) 2_656 .
O11 Nb2 O4 64.1(4) . .
O7 Nb2 O4 96.8(4) . .
O7 Nb2 O4 66.3(4) 2_656 .
O4 Nb2 O4 44.9(6) 2_656 .
O10 Nb3 O8 100.4(3) . 2_656
O10 Nb3 O8 100.4(3) . .
O8 Nb3 O8 159.3(6) 2_656 .
O10 Nb3 O5 100.0(3) . 2_656
O8 Nb3 O5 88.3(4) 2_656 2_656
O8 Nb3 O5 88.1(3) . 2_656
O10 Nb3 O5 100.0(3) . .
O8 Nb3 O5 88.1(3) 2_656 .
O8 Nb3 O5 88.3(4) . .
O5 Nb3 O5 159.9(6) 2_656 .
O10 Nb3 O3 158.0(3) . .
O8 Nb3 O3 64.5(4) 2_656 .
O8 Nb3 O3 95.6(4) . .
O5 Nb3 O3 95.4(4) 2_656 .
O5 Nb3 O3 65.3(4) . .
O10 Nb3 O3 158.0(3) . 2_656
O8 Nb3 O3 95.6(4) 2_656 2_656
O8 Nb3 O3 64.5(4) . 2_656
O5 Nb3 O3 65.3(4) 2_656 2_656
O5 Nb3 O3 95.4(4) . 2_656
O3 Nb3 O3 43.9(7) . 2_656
O15 Nb4 O18 102.2(4) . .
O15 Nb4 O12 99.2(5) . .
O18 Nb4 O12 89.3(4) . .
O15 Nb4 O16 99.5(5) . .
O18 Nb4 O16 88.9(4) . .
O12 Nb4 O16 161.2(4) . .
O15 Nb4 O13 98.4(5) . .
O18 Nb4 O13 159.4(4) . .
O12 Nb4 O13 87.7(4) . .
O16 Nb4 O13 87.4(3) . .
O15 Nb4 O2 160.8(5) . .
O18 Nb4 O2 66.4(4) . .
O12 Nb4 O2 66.3(4) . .
O16 Nb4 O2 95.9(4) . .
O13 Nb4 O2 93.8(5) . .
O15 Nb4 O1 155.9(5) . .
O18 Nb4 O1 96.3(5) . .
O12 Nb4 O1 96.2(5) . .
O16 Nb4 O1 65.4(4) . .
O13 Nb4 O1 63.8(4) . .
O2 Nb4 O1 43.1(5) . .
O14 Nb5 O12 98.3(4) . .
O14 Nb5 O7 98.1(4) . .
O12 Nb5 O7 96.2(4) . .
O14 Nb5 O19 99.0(4) . .
O12 Nb5 O19 159.4(4) . .
O7 Nb5 O19 92.3(4) . .
O14 Nb5 O21 98.7(3) . .
O12 Nb5 O21 89.8(3) . .
O7 Nb5 O21 161.1(4) . .
O19 Nb5 O21 76.7(3) . .
O14 Nb5 O4 156.7(4) . 2_656
O12 Nb5 O4 102.5(5) . 2_656
O7 Nb5 O4 69.3(4) . 2_656
O19 Nb5 O4 63.2(4) . 2_656
O21 Nb5 O4 91.9(4) . 2_656
O14 Nb5 O2 155.5(4) . .
O12 Nb5 O2 66.8(4) . .
O7 Nb5 O2 102.7(5) . .
O19 Nb5 O2 93.0(4) . .
O21 Nb5 O2 63.4(4) . .
O4 Nb5 O2 46.8(5) 2_656 .
O14 Nb5 V1 102.1(3) . .
O12 Nb5 V1 126.1(3) . .
O7 Nb5 V1 128.8(3) . .
O19 Nb5 V1 38.4(2) . .
O21 Nb5 V1 38.26(19) . .
O4 Nb5 V1 73.9(3) 2_656 .
O2 Nb5 V1 74.6(4) . .
O24 Nb6 O5 100.8(4) . .
O24 Nb6 O18 100.4(4) . .
O5 Nb6 O18 94.9(4) . .
O24 Nb6 O9 97.7(3) . .
O5 Nb6 O9 92.7(3) . .
O18 Nb6 O9 158.6(4) . .
O24 Nb6 O21 97.9(3) . .
O5 Nb6 O21 159.3(4) . .
O18 Nb6 O21 90.3(3) . .
O9 Nb6 O21 76.0(3) . .
O24 Nb6 O3 156.6(4) . .
O5 Nb6 O3 68.0(4) . .
O18 Nb6 O3 101.0(5) . .
O9 Nb6 O3 63.7(4) . .
O21 Nb6 O3 91.4(4) . .
O24 Nb6 O2 155.6(4) . .
O5 Nb6 O2 100.9(5) . .
O18 Nb6 O2 66.5(5) . .
O9 Nb6 O2 92.4(4) . .
O21 Nb6 O2 63.1(4) . .
O3 Nb6 O2 46.0(5) . .
O24 Nb6 V1 100.6(2) . .
O5 Nb6 V1 128.3(2) . .
O18 Nb6 V1 126.2(3) . .
O9 Nb6 V1 37.96(19) . .
O21 Nb6 V1 38.04(19) . .
O3 Nb6 V1 74.0(3) . .
O2 Nb6 V1 74.3(3) . .
O22 Nb7 O8 101.3(4) . .
O22 Nb7 O16 100.6(4) . .
O8 Nb7 O16 96.6(4) . .
O22 Nb7 O17 96.2(3) . .
O8 Nb7 O17 159.1(3) . .
O16 Nb7 O17 91.3(3) . .
O22 Nb7 O9 96.2(3) . 2_656
O8 Nb7 O9 91.3(3) . 2_656
O16 Nb7 O9 159.7(3) . 2_656
O17 Nb7 O9 75.5(3) . 2_656
O22 Nb7 O3 156.3(4) . 2_656
O8 Nb7 O3 68.0(4) . 2_656
O16 Nb7 O3 101.6(4) . 2_656
O17 Nb7 O3 91.6(4) . 2_656
O9 Nb7 O3 64.2(4) 2_656 2_656
O22 Nb7 O1 154.9(4) . .
O8 Nb7 O1 101.8(5) . .
O16 Nb7 O1 67.0(4) . .
O17 Nb7 O1 63.7(4) . .
O9 Nb7 O1 93.1(4) 2_656 .
O3 Nb7 O1 46.2(5) 2_656 .
O22 Nb7 V1 98.7(2) . 2_656
O8 Nb7 V1 127.1(2) . 2_656
O16 Nb7 V1 126.9(2) . 2_656
O17 Nb7 V1 37.51(19) . 2_656
O9 Nb7 V1 37.98(19) 2_656 2_656
O3 Nb7 V1 74.3(3) 2_656 2_656
O1 Nb7 V1 74.9(3) . 2_656
O23 V1 O17 113.9(3) . 2_656
O23 V1 O21 112.3(3) . .
O17 V1 O21 133.9(4) 2_656 .
O23 V1 O9 112.6(4) . .
O17 V1 O9 81.4(3) 2_656 .
O21 V1 O9 81.8(3) . .
O23 V1 O19 111.7(4) . .
O17 V1 O19 81.2(3) 2_656 .
O21 V1 O19 81.7(3) . .
O9 V1 O19 135.7(4) . .
O23 V1 Nb5 120.5(2) . .
O17 V1 Nb5 110.2(2) 2_656 .
O21 V1 Nb5 41.0(2) . .
O9 V1 Nb5 111.7(2) . .
O19 V1 Nb5 40.7(2) . .
O23 V1 Nb1 121.5(2) . 2_656
O17 V1 Nb1 40.5(2) 2_656 2_656
O21 V1 Nb1 110.7(2) . 2_656
O9 V1 Nb1 111.2(2) . 2_656
O19 V1 Nb1 40.8(2) . 2_656
Nb5 V1 Nb1 73.99(4) . 2_656
O23 V1 Nb6 121.0(2) . .
O17 V1 Nb6 110.2(2) 2_656 .
O21 V1 Nb6 41.3(2) . .
O9 V1 Nb6 40.4(2) . .
O19 V1 Nb6 112.0(2) . .
Nb5 V1 Nb6 75.30(4) . .
Nb1 V1 Nb6 117.48(4) 2_656 .
O23 V1 Nb7 122.3(2) . 2_656
O17 V1 Nb7 40.5(2) 2_656 2_656
O21 V1 Nb7 110.7(2) . 2_656
O9 V1 Nb7 40.9(2) . 2_656
O19 V1 Nb7 111.0(2) . 2_656
Nb5 V1 Nb7 117.19(4) . 2_656
Nb1 V1 Nb7 74.11(4) 2_656 2_656
Nb6 V1 Nb7 73.85(4) . 2_656
O1 Si1 O1 179.5(10) . 2_656
O1 Si1 O2 67.6(7) . .
O1 Si1 O2 112.4(7) 2_656 .
O1 Si1 O2 112.4(7) . 2_656
O1 Si1 O2 67.6(7) 2_656 2_656
O2 Si1 O2 179.1(10) . 2_656
O1 Si1 O3 108.4(7) . .
O1 Si1 O3 71.2(7) 2_656 .
O2 Si1 O3 71.3(7) . .
O2 Si1 O3 107.9(7) 2_656 .
O1 Si1 O3 71.2(7) . 2_656
O1 Si1 O3 108.4(7) 2_656 2_656
O2 Si1 O3 107.9(7) . 2_656
O2 Si1 O3 71.3(7) 2_656 2_656
O3 Si1 O3 69.5(10) . 2_656
O1 Si1 O4 70.9(7) . .
O1 Si1 O4 109.6(7) 2_656 .
O2 Si1 O4 108.7(7) . .
O2 Si1 O4 72.1(7) 2_656 .
O3 Si1 O4 179.2(8) . .
O3 Si1 O4 109.8(7) 2_656 .
O1 Si1 O4 109.6(7) . 2_656
O1 Si1 O4 70.9(7) 2_656 2_656
O2 Si1 O4 72.1(7) . 2_656
O2 Si1 O4 108.7(7) 2_656 2_656
O3 Si1 O4 109.8(7) . 2_656
O3 Si1 O4 179.2(8) 2_656 2_656
O4 Si1 O4 70.9(10) . 2_656
Si1 O1 Nb7 121.1(7) . .
Si1 O1 Nb1 120.7(7) . .
Nb7 O1 Nb1 98.8(5) . .
Si1 O1 Nb4 124.2(8) . .
Nb7 O1 Nb4 92.2(5) . .
Nb1 O1 Nb4 92.5(5) . .
Si1 O2 Nb4 125.1(8) . .
Si1 O2 Nb5 120.0(7) . .
Nb4 O2 Nb5 92.1(5) . .
Si1 O2 Nb6 121.2(7) . .
Nb4 O2 Nb6 91.8(5) . .
Nb5 O2 Nb6 99.5(5) . .
Si1 O3 Nb7 121.5(7) . 2_656
Si1 O3 Nb6 121.5(7) . .
Nb7 O3 Nb6 99.7(5) 2_656 .
Si1 O3 Nb3 123.3(7) . .
Nb7 O3 Nb3 92.0(5) 2_656 .
Nb6 O3 Nb3 91.5(4) . .
Si1 O4 Nb1 122.1(7) . .
Si1 O4 Nb5 120.9(7) . 2_656
Nb1 O4 Nb5 100.5(5) . 2_656
Si1 O4 Nb2 122.1(7) . .
Nb1 O4 Nb2 92.4(5) . .
Nb5 O4 Nb2 91.5(4) 2_656 .
Nb6 O5 Nb3 135.2(5) . .
Nb5 O7 Nb2 132.8(5) . .
Nb7 O8 Nb3 135.5(5) . .
V1 O9 Nb6 101.6(3) . .
V1 O9 Nb7 101.1(3) . 2_656
Nb6 O9 Nb7 129.3(4) . 2_656
Nb1 O11 Nb2 135.6(6) . .
Nb5 O12 Nb4 134.8(5) . .
Nb1 O13 Nb4 138.2(5) . .
Nb7 O16 Nb4 135.4(5) . .
V1 O17 Nb1 101.9(3) 2_656 .
V1 O17 Nb7 102.0(3) 2_656 .
Nb1 O17 Nb7 130.5(4) . .
Nb6 O18 Nb4 135.2(5) . .
V1 O19 Nb5 100.9(3) . .
V1 O19 Nb1 101.0(3) . 2_656
Nb5 O19 Nb1 129.7(4) . 2_656
V1 O21 Nb5 100.8(3) . .
V1 O21 Nb6 100.6(3) . .
Nb5 O21 Nb6 131.6(4) . .
N3 Cu1 N1 95.4(5) . .
N3 Cu1 N2 172.9(7) . .
N1 Cu1 N2 84.8(5) . .
N3 Cu1 N4 84.4(5) . .
N1 Cu1 N4 174.2(7) . .
N2 Cu1 N4 94.7(5) . .
N3 Cu1 O1W 92.9(6) . .
N1 Cu1 O1W 90.9(6) . .
N2 Cu1 O1W 94.1(5) . .
N4 Cu1 O1W 94.9(5) . .
C1 N1 Cu1 110.9(11) . .
N1 C1 C2 116.2(19) . .
C1 C2 N2 114.5(17) . .
C2 N2 Cu1 110.3(9) . .
C3 N3 Cu1 110.4(10) . .
C4 C3 N3 112.0(16) . .
C3 C4 N4 112.8(14) . .
C4 N4 Cu1 107.8(9) . .
N6 Cu2 N6 180.0 . 5_676
N6 Cu2 N5 94.8(4) . 5_676
N6 Cu2 N5 85.2(4) 5_676 5_676
N6 Cu2 N5 85.2(4) . .
N6 Cu2 N5 94.8(4) 5_676 .
N5 Cu2 N5 180.0 5_676 .
C5 N5 Cu2 107.1(8) . .
N5 C5 C6 111.6(12) . .
N6 C6 C5 108.1(12) . .
C6 N6 Cu2 108.7(7) . .
N8 Cu3 N8 180.0 . 7_566
N8 Cu3 N7 83.8(4) . .
N8 Cu3 N7 96.2(4) 7_566 .
N8 Cu3 N7 96.2(4) . 7_566
N8 Cu3 N7 83.8(4) 7_566 7_566
N7 Cu3 N7 180.0 . 7_566
C7 N7 Cu3 110.9(8) . .
N7 C7 C8 112.6(12) . .
N8 C8 C7 112.2(12) . .
C8 N8 Cu3 111.5(8) . .
N10 Cu4 N10 180.0 . 7_666
N10 Cu4 N9 84.2(5) . .
N10 Cu4 N9 95.8(5) 7_666 .
N10 Cu4 N9 95.8(5) . 7_666
N10 Cu4 N9 84.2(5) 7_666 7_666
N9 Cu4 N9 180.0 . 7_666
C9 N9 Cu4 108.5(9) . .
C10 C9 N9 111.2(16) . .
N10 C10 C9 113.5(15) . .
C10 N10 Cu4 110.7(8) . .
N12 Cu5 N12 180.0 5_666 .
N12 Cu5 N11 95.5(4) 5_666 .
N12 Cu5 N11 84.5(4) . .
N12 Cu5 N11 84.5(4) 5_666 5_666
N12 Cu5 N11 95.5(4) . 5_666
N11 Cu5 N11 180.0 . 5_666
C11 N11 Cu5 108.6(9) . .
C12 C11 N11 111.0(14) . .
C11 C12 N12 114.0(16) . .
C12 N12 Cu5 107.1(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O6 1.750(8) .
Nb1 O13 1.875(9) .
Nb1 O11 1.899(9) .
Nb1 O17 2.057(7) .
Nb1 O19 2.064(7) 2_656
Nb1 O4 2.404(15) .
Nb1 O1 2.466(15) .
Nb1 V1 3.1021(15) 2_656
Nb2 O20 1.717(12) .
Nb2 O11 1.957(10) 2_656
Nb2 O11 1.957(9) .
Nb2 O7 1.979(10) .
Nb2 O7 1.979(10) 2_656
Nb2 O4 2.540(14) 2_656
Nb2 O4 2.540(13) .
Nb3 O10 1.732(11) .
Nb3 O8 1.969(8) 2_656
Nb3 O8 1.969(8) .
Nb3 O5 1.975(8) 2_656
Nb3 O5 1.975(8) .
Nb3 O3 2.540(13) .
Nb3 O3 2.540(13) 2_656
Nb4 O15 1.734(8) .
Nb4 O18 1.938(9) .
Nb4 O12 1.962(9) .
Nb4 O16 1.963(8) .
Nb4 O13 1.963(9) .
Nb4 O2 2.465(15) .
Nb4 O1 2.498(14) .
Nb5 O14 1.763(7) .
Nb5 O12 1.894(9) .
Nb5 O7 1.917(10) .
Nb5 O19 2.052(7) .
Nb5 O21 2.062(7) .
Nb5 O4 2.442(13) 2_656
Nb5 O2 2.479(14) .
Nb5 V1 3.0890(16) .
Nb6 O24 1.757(7) .
Nb6 O5 1.898(8) .
Nb6 O18 1.904(9) .
Nb6 O9 2.056(7) .
Nb6 O21 2.087(7) .
Nb6 O3 2.461(14) .
Nb6 O2 2.480(15) .
Nb6 V1 3.1054(15) .
Nb7 O22 1.762(7) .
Nb7 O8 1.891(8) .
Nb7 O16 1.900(8) .
Nb7 O17 2.063(7) .
Nb7 O9 2.075(7) 2_656
Nb7 O3 2.425(14) 2_656
Nb7 O1 2.463(15) .
Nb7 V1 3.1092(15) 2_656
V1 O23 1.623(6) .
V1 O17 1.936(7) 2_656
V1 O21 1.947(7) .
V1 O9 1.950(7) .
V1 O19 1.955(7) .
V1 Nb1 3.1021(15) 2_656
V1 Nb7 3.1092(15) 2_656
Si1 O1 1.629(15) .
Si1 O1 1.629(15) 2_656
Si1 O2 1.650(15) .
Si1 O2 1.650(15) 2_656
Si1 O3 1.666(14) .
Si1 O3 1.666(14) 2_656
Si1 O4 1.671(14) .
Si1 O4 1.671(14) 2_656
O3 Nb7 2.425(14) 2_656
O4 Nb5 2.443(13) 2_656
O9 Nb7 2.075(7) 2_656
O17 V1 1.936(7) 2_656
O19 Nb1 2.064(7) 2_656
Cu1 N3 1.971(12) .
Cu1 N1 1.992(12) .
Cu1 N2 1.995(11) .
Cu1 N4 1.999(12) .
Cu1 O1W 2.382(13) .
N1 C1 1.41(3) .
C1 C2 1.424(10) .
C2 N2 1.44(2) .
N3 C3 1.44(2) .
C3 C4 1.39(2) .
C4 N4 1.46(2) .
Cu2 N6 1.994(9) .
Cu2 N6 1.994(9) 5_676
Cu2 N5 2.025(10) 5_676
Cu2 N5 2.025(10) .
N5 C5 1.468(16) .
C5 C6 1.47(2) .
C6 N6 1.467(17) .
Cu3 N8 1.971(10) .
Cu3 N8 1.971(10) 7_566
Cu3 N7 2.002(10) .
Cu3 N7 2.002(10) 7_566
N7 C7 1.437(17) .
C7 C8 1.44(2) .
C8 N8 1.438(17) .
Cu4 N10 1.999(11) .
Cu4 N10 1.999(11) 7_666
Cu4 N9 2.008(11) .
Cu4 N9 2.008(11) 7_666
N9 C9 1.48(2) .
C9 C10 1.42(2) .
C10 N10 1.421(19) .
Cu5 N12 1.993(9) 5_666
Cu5 N12 1.993(9) .
Cu5 N11 2.010(10) .
Cu5 N11 2.010(10) 5_666
N11 C11 1.470(18) .
C11 C12 1.38(3) .
C12 N12 1.441(19) .
O10W O10W 1.26(5) 2_656
O11W O11W 1.23(5) 2_656
