# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2017

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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1554472'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;

_vrf_PLAT043_4                   
;
PROBLEM:  Calculated and Reported Mol. Weight Differ by .. 36.29 Check
RESPONSE: the hydrogen atoms attached to water molecules are not added. 
therefore, the Calculated and Reported Mol. Weight are different.
;

_vrf_PLAT306_4                   
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?) .......   O1W Check
RESPONSE:  the hydrogen atoms attached to water molecules are not added 
;

_vrf_PLAT934_4                   
;
PROBLEM:  Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....       2 Check
RESPONSE: only 2, nothing was done.
;

_vrf_PLAT910_4                   
;
PROBLEM:  Missing # of FCF Reflection(s) Below Theta(Min)       18 Note
RESPONSE: Data completeness of is 99.8% which guarantees a correct
structural elucidation of compound 3.
;

_vrf_PLAT972_4                   
;
PROBLEM: Check Calcd Residual Density  0.59A From      K1    -2.83 eA-3
RESPONSE: the Residual Density possibly can be considered to be due to
the poor crystal quality or other effects.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H36 K6 Nb6 O36'
_chemical_formula_weight         1404.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

_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'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.102(2)
_cell_length_b                   12.703(3)
_cell_length_c                   10.068(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1547.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14010
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      27.45

_exptl_crystal_description       Pale-green
_exptl_crystal_colour            rhombus
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.013
_exptl_crystal_F_000             1368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.085
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7802
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14180
_diffrn_reflns_av_unetI/netI     0.0091
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.082
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1855
_reflns_number_gt                1772
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0997P)²+48.8347P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1855
_refine_ls_number_parameters     127
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1818
_refine_ls_wR_factor_gt          0.1808
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.051
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.95810(8) 0.31773(7) 0.0000 0.0105(3) Uani 1 2 d S T P . .
Nb2 Nb 1.13408(6) 0.47247(5) 0.17047(7) 0.0125(3) Uani 1 1 d . . . . .
K1 K 0.7319(4) 0.2433(4) 0.5000 0.0606(12) Uani 1 2 d S T P . .
O7 O 1.2259(7) 0.4538(7) 0.0000 0.0144(16) Uani 1 2 d S T P . .
O6 O 1.0000 0.5000 0.0000 0.011(2) Uani 1 4 d S TU P . .
O5 O 1.1447(5) 0.6259(4) 0.1386(6) 0.0141(11) Uani 1 1 d . . . . .
O4 O 1.0807(5) 0.3277(4) 0.1348(6) 0.0130(11) Uani 1 1 d . . . . .
O3 O 1.2363(5) 0.4489(5) 0.2948(6) 0.0195(12) Uani 1 1 d . . . . .
O2 O 1.0000 0.5000 0.2782(8) 0.0142(15) Uani 1 2 d S T P . .
K3 K 1.0010(5) 0.1867(4) 0.5000 0.0623(12) Uani 1 2 d S T P . .
K2 K 0.7178(5) 0.1573(5) 0.0000 0.0687(14) Uani 1 2 d S T P . .
O3W O 0.9799(10) 0.6284(8) 0.5000 0.030(2) Uani 1 2 d S T P . .
O2W O 0.8650(6) 0.2150(6) 0.6683(7) 0.0267(15) Uani 1 1 d . . . . .
O1W O 1.0000 0.0000 0.0000 0.039(4) Uani 1 4 d S T P . .
O6W O 0.6928(11) 0.4216(9) 0.5000 0.038(3) Uani 1 2 d S T P . .
O1 O 0.9200(8) 0.1834(7) 0.0000 0.0200(18) Uani 1 2 d S T P . .
O9W O 1.1403(7) 0.1952(8) 0.6599(9) 0.047(3) Uani 1 1 d . . . . .
O8W O 1.0000 0.0000 0.200(2) 0.070(4) Uani 1 2 d S T P . .
O7W O 0.941(2) 0.007(3) 0.5000 0.136(10) Uani 1 2 d S TU 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 O1 1.767(8) . ?
Nb1 O5 2.002(6) 5_765 ?
Nb1 O5 2.002(6) 2_765 ?
Nb1 O4 2.015(6) . ?
Nb1 O4 2.015(6) 6 ?
Nb1 O6 2.3704(10) . ?
Nb1 K1 3.403(5) 7_665 ?
Nb1 K2 3.551(6) . ?
Nb2 O3 1.785(6) . ?
Nb2 O5 1.979(6) . ?
Nb2 O4 1.981(5) . ?
Nb2 O2 1.983(4) . ?
Nb2 O7 2.059(5) . ?
Nb2 O6 2.3877(8) . ?
Nb2 Nb2 3.3199(15) 2_765 ?
Nb2 K1 3.444(5) 7_665 ?
Nb2 K2 3.841(3) 7_666 ?
K1 O6W 2.313(12) . ?
K1 O2W 2.366(8) 6_556 ?
K1 O2W 2.366(8) . ?
K1 O4 2.450(7) 4_455 ?
K1 O4 2.450(7) 7_566 ?
K1 O7 2.505(10) 7_566 ?
K1 K3 3.335(8) . ?
K1 Nb1 3.403(5) 7_566 ?
K1 Nb2 3.444(5) 4_455 ?
K1 Nb2 3.444(5) 7_566 ?
O7 Nb2 2.059(5) 6 ?
O7 K1 2.505(10) 7_665 ?
O6 Nb1 2.3704(10) 5_765 ?
O6 Nb2 2.3876(8) 5_765 ?
O6 Nb2 2.3876(8) 6 ?
O6 Nb2 2.3876(8) 2_765 ?
O5 Nb1 2.002(6) 5_765 ?
O4 K1 2.450(7) 7_665 ?
O3 K2 2.478(7) 7_666 ?
O2 Nb2 1.983(4) 2_765 ?
K3 O9W 2.334(9) . ?
K3 O9W 2.334(9) 6_556 ?
K3 O3W 2.361(11) 5_766 ?
K3 O2W 2.389(8) . ?
K3 O2W 2.389(8) 6_556 ?
K3 O7W 2.39(3) . ?
K3 O7W 2.56(3) 5_756 ?
K3 K2 3.288(8) 7_666 ?
K3 K3 4.742(10) 5_756 ?
K2 O3W 2.421(13) 3_645 ?
K2 O1 2.470(11) . ?
K2 O3 2.478(7) 7_565 ?
K2 O3 2.478(7) 4_455 ?
K2 O9W 2.642(13) 7_565 ?
K2 O9W 2.642(13) 4_455 ?
K2 O6W 3.184(12) 3_645 ?
K2 K3 3.288(8) 7_565 ?
K2 Nb2 3.841(3) 7_565 ?
K2 Nb2 3.841(3) 4_455 ?
O3W K3 2.361(11) 5_766 ?
O3W K2 2.421(13) 3_655 ?
O6W K2 3.184(12) 3_655 ?
O9W K2 2.642(13) 7_666 ?
O7W O7W 1.45(6) 5_756 ?
O7W K3 2.56(3) 5_756 ?

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
O1 Nb1 O5 100.6(3) . 5_765 ?
O1 Nb1 O5 100.6(3) . 2_765 ?
O5 Nb1 O5 88.4(3) 5_765 2_765 ?
O1 Nb1 O4 104.7(3) . . ?
O5 Nb1 O4 154.8(2) 5_765 . ?
O5 Nb1 O4 88.0(2) 2_765 . ?
O1 Nb1 O4 104.7(3) . 6 ?
O5 Nb1 O4 88.0(2) 5_765 6 ?
O5 Nb1 O4 154.8(2) 2_765 6 ?
O4 Nb1 O4 84.7(3) . 6 ?
O1 Nb1 O6 177.2(3) . . ?
O5 Nb1 O6 77.48(16) 5_765 . ?
O5 Nb1 O6 77.48(16) 2_765 . ?
O4 Nb1 O6 77.34(15) . . ?
O4 Nb1 O6 77.34(15) 6 . ?
O1 Nb1 K1 92.0(3) . 7_665 ?
O5 Nb1 K1 133.35(17) 5_765 7_665 ?
O5 Nb1 K1 133.35(17) 2_765 7_665 ?
O4 Nb1 K1 45.36(16) . 7_665 ?
O4 Nb1 K1 45.36(16) 6 7_665 ?
O6 Nb1 K1 90.82(9) . 7_665 ?
O1 Nb1 K2 39.9(3) . . ?
O5 Nb1 K2 72.34(17) 5_765 . ?
O5 Nb1 K2 72.34(17) 2_765 . ?
O4 Nb1 K2 129.74(16) . . ?
O4 Nb1 K2 129.74(16) 6 . ?
O6 Nb1 K2 137.37(10) . . ?
K1 Nb1 K2 131.81(14) 7_665 . ?
O3 Nb2 O5 103.5(3) . . ?
O3 Nb2 O4 101.4(3) . . ?
O5 Nb2 O4 154.9(2) . . ?
O3 Nb2 O2 102.3(3) . . ?
O5 Nb2 O2 88.16(18) . . ?
O4 Nb2 O2 89.77(17) . . ?
O3 Nb2 O7 101.0(3) . . ?
O5 Nb2 O7 86.8(3) . . ?
O4 Nb2 O7 85.3(3) . . ?
O2 Nb2 O7 156.7(3) . . ?
O3 Nb2 O6 178.2(2) . . ?
O5 Nb2 O6 77.48(16) . . ?
O4 Nb2 O6 77.54(16) . . ?
O2 Nb2 O6 79.12(19) . . ?
O7 Nb2 O6 77.56(19) . . ?
O3 Nb2 Nb2 135.5(2) . 2_765 ?
O5 Nb2 Nb2 81.70(17) . 2_765 ?
O4 Nb2 Nb2 82.93(16) . 2_765 ?
O2 Nb2 Nb2 33.16(19) . 2_765 ?
O7 Nb2 Nb2 123.52(19) . 2_765 ?
O6 Nb2 Nb2 45.955(19) . 2_765 ?
O3 Nb2 K1 88.7(2) . 7_665 ?
O5 Nb2 K1 132.91(19) . 7_665 ?
O4 Nb2 K1 44.21(18) . 7_665 ?
O2 Nb2 K1 133.97(10) . 7_665 ?
O7 Nb2 K1 46.1(2) . 7_665 ?
O6 Nb2 K1 89.54(7) . 7_665 ?
Nb2 Nb2 K1 120.25(9) 2_765 7_665 ?
O3 Nb2 K2 30.7(2) . 7_666 ?
O5 Nb2 K2 123.07(19) . 7_666 ?
O4 Nb2 K2 81.03(18) . 7_666 ?
O2 Nb2 K2 79.57(19) . 7_666 ?
O7 Nb2 K2 121.9(2) . 7_666 ?
O6 Nb2 K2 149.65(9) . 7_666 ?
Nb2 Nb2 K2 110.38(8) 2_765 7_666 ?
K1 Nb2 K2 89.89(9) 7_665 7_666 ?
O6W K1 O2W 106.7(3) . 6_556 ?
O6W K1 O2W 106.7(3) . . ?
O2W K1 O2W 91.5(4) 6_556 . ?
O6W K1 O4 102.0(3) . 4_455 ?
O2W K1 O4 93.2(2) 6_556 4_455 ?
O2W K1 O4 148.1(3) . 4_455 ?
O6W K1 O4 102.0(3) . 7_566 ?
O2W K1 O4 148.1(3) 6_556 7_566 ?
O2W K1 O4 93.2(2) . 7_566 ?
O4 K1 O4 67.3(3) 4_455 7_566 ?
O6W K1 O7 166.6(4) . 7_566 ?
O2W K1 O7 82.4(3) 6_556 7_566 ?
O2W K1 O7 82.4(3) . 7_566 ?
O4 K1 O7 67.1(2) 4_455 7_566 ?
O4 K1 O7 67.1(2) 7_566 7_566 ?
O6W K1 K3 114.3(4) . . ?
O2W K1 K3 45.75(19) 6_556 . ?
O2W K1 K3 45.75(19) . . ?
O4 K1 K3 130.5(2) 4_455 . ?
O4 K1 K3 130.5(2) 7_566 . ?
O7 K1 K3 79.2(3) 7_566 . ?
O6W K1 Nb1 91.4(3) . 7_566 ?
O2W K1 Nb1 128.9(2) 6_556 7_566 ?
O2W K1 Nb1 128.9(2) . 7_566 ?
O4 K1 Nb1 35.81(15) 4_455 7_566 ?
O4 K1 Nb1 35.81(15) 7_566 7_566 ?
O7 K1 Nb1 75.2(2) 7_566 7_566 ?
K3 K1 Nb1 154.4(2) . 7_566 ?
O6W K1 Nb2 135.1(3) . 4_455 ?
O2W K1 Nb2 75.9(2) 6_556 4_455 ?
O2W K1 Nb2 118.0(3) . 4_455 ?
O4 K1 Nb2 34.32(14) 4_455 4_455 ?
O4 K1 Nb2 74.11(18) 7_566 4_455 ?
O7 K1 Nb2 36.34(12) 7_566 4_455 ?
K3 K1 Nb2 99.43(15) . 4_455 ?
Nb1 K1 Nb2 58.93(8) 7_566 4_455 ?
O6W K1 Nb2 135.1(3) . 7_566 ?
O2W K1 Nb2 118.0(3) 6_556 7_566 ?
O2W K1 Nb2 75.9(2) . 7_566 ?
O4 K1 Nb2 74.11(18) 4_455 7_566 ?
O4 K1 Nb2 34.32(14) 7_566 7_566 ?
O7 K1 Nb2 36.34(12) 7_566 7_566 ?
K3 K1 Nb2 99.43(15) . 7_566 ?
Nb1 K1 Nb2 58.93(8) 7_566 7_566 ?
Nb2 K1 Nb2 59.78(9) 4_455 7_566 ?
Nb2 O7 Nb2 113.0(4) 6 . ?
Nb2 O7 K1 97.5(3) 6 7_665 ?
Nb2 O7 K1 97.5(3) . 7_665 ?
Nb1 O6 Nb1 180.0 5_765 . ?
Nb1 O6 Nb2 90.13(2) 5_765 5_765 ?
Nb1 O6 Nb2 89.87(2) . 5_765 ?
Nb1 O6 Nb2 89.87(2) 5_765 6 ?
Nb1 O6 Nb2 90.13(2) . 6 ?
Nb2 O6 Nb2 88.09(4) 5_765 6 ?
Nb1 O6 Nb2 90.13(2) 5_765 2_765 ?
Nb1 O6 Nb2 89.87(2) . 2_765 ?
Nb2 O6 Nb2 91.91(4) 5_765 2_765 ?
Nb2 O6 Nb2 180.0 6 2_765 ?
Nb1 O6 Nb2 89.87(2) 5_765 . ?
Nb1 O6 Nb2 90.13(2) . . ?
Nb2 O6 Nb2 180.0 5_765 . ?
Nb2 O6 Nb2 91.91(4) 6 . ?
Nb2 O6 Nb2 88.09(4) 2_765 . ?
Nb2 O5 Nb1 115.2(3) . 5_765 ?
Nb2 O4 Nb1 114.9(3) . . ?
Nb2 O4 K1 101.5(3) . 7_665 ?
Nb1 O4 K1 98.8(2) . 7_665 ?
Nb2 O3 K2 127.8(3) . 7_666 ?
Nb2 O2 Nb2 113.7(4) 2_765 . ?
O9W K3 O9W 87.2(5) . 6_556 ?
O9W K3 O3W 83.3(4) . 5_766 ?
O9W K3 O3W 83.3(4) 6_556 5_766 ?
O9W K3 O2W 90.1(3) . . ?
O9W K3 O2W 168.5(4) 6_556 . ?
O3W K3 O2W 85.3(3) 5_766 . ?
O9W K3 O2W 168.5(4) . 6_556 ?
O9W K3 O2W 90.1(3) 6_556 6_556 ?
O3W K3 O2W 85.3(3) 5_766 6_556 ?
O2W K3 O2W 90.4(4) . 6_556 ?
O9W K3 O7W 105.3(6) . . ?
O9W K3 O7W 105.3(6) 6_556 . ?
O3W K3 O7W 167.9(8) 5_766 . ?
O2W K3 O7W 86.2(5) . . ?
O2W K3 O7W 86.2(5) 6_556 . ?
O9W K3 O7W 81.1(5) . 5_756 ?
O9W K3 O7W 81.1(5) 6_556 5_756 ?
O3W K3 O7W 158.4(7) 5_766 5_756 ?
O2W K3 O7W 109.5(5) . 5_756 ?
O2W K3 O7W 109.5(5) 6_556 5_756 ?
O7W K3 O7W 33.7(12) . 5_756 ?
O9W K3 K2 52.8(3) . 7_666 ?
O9W K3 K2 52.8(3) 6_556 7_666 ?
O3W K3 K2 47.3(3) 5_766 7_666 ?
O2W K3 K2 117.3(2) . 7_666 ?
O2W K3 K2 117.3(2) 6_556 7_666 ?
O7W K3 K2 144.8(7) . 7_666 ?
O7W K3 K2 111.1(7) 5_756 7_666 ?
O9W K3 K1 134.1(2) . . ?
O9W K3 K1 134.1(2) 6_556 . ?
O3W K3 K1 83.1(3) 5_766 . ?
O2W K3 K1 45.18(19) . . ?
O2W K3 K1 45.18(19) 6_556 . ?
O7W K3 K1 84.7(7) . . ?
O7W K3 K1 118.5(7) 5_756 . ?
K2 K3 K1 130.5(2) 7_666 . ?
O9W K3 K3 92.9(3) . 5_756 ?
O9W K3 K3 92.9(3) 6_556 5_756 ?
O3W K3 K3 174.7(4) 5_766 5_756 ?
O2W K3 K3 98.5(2) . 5_756 ?
O2W K3 K3 98.5(2) 6_556 5_756 ?
O7W K3 K3 17.5(7) . 5_756 ?
O7W K3 K3 16.3(6) 5_756 5_756 ?
K2 K3 K3 127.4(2) 7_666 5_756 ?
K1 K3 K3 102.2(2) . 5_756 ?
O3W K2 O1 179.0(4) 3_645 . ?
O3W K2 O3 90.4(2) 3_645 7_565 ?
O1 K2 O3 89.0(2) . 7_565 ?
O3W K2 O3 90.4(2) 3_645 4_455 ?
O1 K2 O3 89.0(2) . 4_455 ?
O3 K2 O3 113.0(4) 7_565 4_455 ?
O3W K2 O9W 75.9(3) 3_645 7_565 ?
O1 K2 O9W 104.8(3) . 7_565 ?
O3 K2 O9W 157.9(3) 7_565 7_565 ?
O3 K2 O9W 84.9(2) 4_455 7_565 ?
O3W K2 O9W 75.9(3) 3_645 4_455 ?
O1 K2 O9W 104.8(3) . 4_455 ?
O3 K2 O9W 84.9(2) 7_565 4_455 ?
O3 K2 O9W 157.9(3) 4_455 4_455 ?
O9W K2 O9W 75.1(4) 7_565 4_455 ?
O3W K2 O6W 101.1(4) 3_645 3_645 ?
O1 K2 O6W 77.8(3) . 3_645 ?
O3 K2 O6W 57.11(19) 7_565 3_645 ?
O3 K2 O6W 57.11(19) 4_455 3_645 ?
O9W K2 O6W 142.0(2) 7_565 3_645 ?
O9W K2 O6W 142.0(2) 4_455 3_645 ?
O3W K2 K3 45.8(3) 3_645 7_565 ?
O1 K2 K3 135.2(3) . 7_565 ?
O3 K2 K3 113.6(2) 7_565 7_565 ?
O3 K2 K3 113.6(2) 4_455 7_565 ?
O9W K2 K3 44.7(2) 7_565 7_565 ?
O9W K2 K3 44.7(2) 4_455 7_565 ?
O6W K2 K3 146.9(3) 3_645 7_565 ?
O3W K2 Nb1 153.7(3) 3_645 . ?
O1 K2 Nb1 27.3(2) . . ?
O3 K2 Nb1 103.8(2) 7_565 . ?
O3 K2 Nb1 103.8(2) 4_455 . ?
O9W K2 Nb1 83.3(2) 7_565 . ?
O9W K2 Nb1 83.3(2) 4_455 . ?
O6W K2 Nb1 105.1(3) 3_645 . ?
K3 K2 Nb1 107.9(2) 7_565 . ?
O3W K2 Nb2 70.98(14) 3_645 7_565 ?
O1 K2 Nb2 108.60(14) . 7_565 ?
O3 K2 Nb2 21.55(15) 7_565 7_565 ?
O3 K2 Nb2 120.7(2) 4_455 7_565 ?
O9W K2 Nb2 137.5(3) 7_565 7_565 ?
O9W K2 Nb2 71.62(18) 4_455 7_565 ?
O6W K2 Nb2 71.69(14) 3_645 7_565 ?
K3 K2 Nb2 92.77(11) 7_565 7_565 ?
Nb1 K2 Nb2 117.53(8) . 7_565 ?
O3W K2 Nb2 70.98(14) 3_645 4_455 ?
O1 K2 Nb2 108.60(14) . 4_455 ?
O3 K2 Nb2 120.7(2) 7_565 4_455 ?
O3 K2 Nb2 21.55(15) 4_455 4_455 ?
O9W K2 Nb2 71.62(18) 7_565 4_455 ?
O9W K2 Nb2 137.5(3) 4_455 4_455 ?
O6W K2 Nb2 71.69(14) 3_645 4_455 ?
K3 K2 Nb2 92.77(11) 7_565 4_455 ?
Nb1 K2 Nb2 117.53(8) . 4_455 ?
Nb2 K2 Nb2 119.49(16) 7_565 4_455 ?
K3 O3W K2 86.9(4) 5_766 3_655 ?
K1 O2W K3 89.1(3) . . ?
K1 O6W K2 148.3(6) . 3_655 ?
Nb1 O1 K2 112.8(4) . . ?
K3 O9W K2 82.5(3) . 7_666 ?
O7W O7W K3 80(3) 5_756 . ?
O7W O7W K3 67(2) 5_756 5_756 ?
K3 O7W K3 146.3(12) . 5_756 ?

_refine_diff_density_max         1.728
_refine_diff_density_min         -2.977
_refine_diff_density_rms         0.402



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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1554470'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_2                   
;
PROBLEM: Check Calcd Residual Density   1.76A From      O6   3.62 eA-3
RESPONSE:  the Residual Density possibly can be considered to be due to
the poor crystal quality or other effects.
;

_vrf_PLAT430_2                   
;
PROBLEM:  Short Inter D...A Contact  O2W    ..  O6      ..     2.83 Ang.  
RESPONSE: there should be a strong hydrogen bond between the two atoms.
;

_vrf_PLAT043_2                   
;
PROBLEM:  Calculated and Reported Mol. Weight Differ by .. 43.82 Check
RESPONSE: Some carbon and nitrogen atoms are disorderedly distributed.
thus the hydrogen atoms attached to them are not added. in addition, 
the hydrogen atoms attached to water molecules are not added too.
therefore, the Calculated and Reported Mol. Weight are different.
;

_vrf_PLAT094_2                   
;
PROBLEM:Ratio of Maximum / Minimum Residual Density ....    4.21 Report
RESPONSE:  Please see our answer to _vrf_PLAT971_2.
;

_vrf_PLAT306_2                   
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?) .......   O1W Check
RESPONSE:  the hydrogen atoms attached to water molecules are not added 
;

_vrf_PLAT342_2                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............  0.06 Ang
RESPONSE: The quality of this crystal was poor, however, it represents the
 best possible data after multiple crystallization attempts
;

_vrf_PLAT601_2                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        117 Ang3
RESPONSE: The existance of large voids containing loosely bound
water solvent is typical for POM structures 
;

_vrf_PLAT975_2                   
;
PROBLEM: Check Calcd Residual Density  0.88A From      N4       1.75 eA-3  
RESPONSE:  the Residual Density possibly can be considered to be due to
the poor crystal quality or other effects. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H112 Cu6 N24 Nb12 O50 Si V2'
_chemical_formula_weight         3163.50

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'
V V 0.3005 0.5294 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_H-M_alt        'P 4/m n c'
_space_group_name_Hall           '-P 4 2n'

_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'
'-y, x, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, z'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'-x-1/2, y-1/2, z-1/2'
'x, y, -z'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.5357(4)
_cell_length_b                   14.5357(4)
_cell_length_c                   22.999(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4859.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3077
_cell_measurement_theta_min      3.5910
_cell_measurement_theta_max      26.7130

_exptl_crystal_description       block
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_F_000             3100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.922
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14332
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.004
_diffrn_reflns_theta_max         28.925
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2982
_reflns_number_gt                2096
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1058P)²+126.0086P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2982
_refine_ls_number_parameters     173
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0994
_refine_ls_wR_factor_ref         0.2746
_refine_ls_wR_factor_gt          0.2499
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.20791(10) 0.14705(10) 0.5000 0.0410(5) Uani 1 2 d S T P . .
Nb2 Nb 0.18004(8) -0.03080(9) 0.39448(6) 0.0463(4) Uani 1 1 d . . . . .
Cu2 Cu 0.5000 0.0000 0.5000 0.0591(10) Uani 1 4 d S T P . .
N3 N 0.6109(19) 0.0767(18) 0.5216(11) 0.068(7) Uani 0.5 1 d . U P . .
C3 C 0.579(3) 0.174(3) 0.5000 0.104(9) Uani 1 2 d S TU P . .
C4 C 0.538(3) 0.178(3) 0.4539(18) 0.083(10) Uani 0.5 1 d . U P . .
N4 N 0.456(2) 0.100(2) 0.4395(15) 0.087(9) Uani 0.5 1 d . U P . .
Cu1 Cu 0.2932(15) 0.2220(17) 0.2575(14) 0.092(7) Uani 0.5 1 d . . P . .
N1 N 0.379(2) 0.314(2) 0.2569(15) 0.202(11) Uani 1 1 d . U . . .
H1A H 0.4274 0.2964 0.2360 0.243 Uiso 1 1 calc R U . . .
H1B H 0.3552 0.3640 0.2407 0.243 Uiso 1 1 calc R U . . .
C1 C 0.411(3) 0.337(3) 0.325(2) 0.217(12) Uani 1 1 d . U . . .
H1C H 0.4693 0.3065 0.3335 0.261 Uiso 1 1 calc R U . . .
H1D H 0.4185 0.4023 0.3304 0.261 Uiso 1 1 calc R U . . .
C2 C 0.333(3) 0.298(3) 0.3642(17) 0.187(11) Uani 1 1 d . U . . .
H2A H 0.3588 0.2777 0.4009 0.224 Uiso 1 1 calc R U . . .
H2B H 0.2892 0.3468 0.3725 0.224 Uiso 1 1 calc R U . . .
N2 N 0.2826(19) 0.2188(19) 0.3363(11) 0.146(8) Uani 1 1 d . U . . .
H2C H 0.2233 0.2212 0.3460 0.175 Uiso 1 1 calc R U . . .
H2D H 0.3054 0.1661 0.3496 0.175 Uiso 1 1 calc R U . . .
V1 V 0.0000 0.0000 0.32496(19) 0.0490(11) Uani 1 4 d S T P . .
Si1 Si 0.0000 0.0000 0.5000 0.0162(13) Uani 1 8 d S T P . .
O7 O 0.2444(10) 0.0561(9) 0.4396(6) 0.087(4) Uani 1 1 d . U . . .
O6 O 0.2566(9) -0.0448(9) 0.3364(6) 0.086(4) Uani 1 1 d . . . . .
O5 O 0.0702(8) -0.1006(7) 0.3574(5) 0.068(3) Uani 1 1 d . . . . .
O4 O 0.0000 0.0000 0.2522(9) 0.076(7) Uani 1 4 d S T P . .
O3 O 0.0524(10) -0.0747(9) 0.4587(7) 0.032(3) Uani 0.5 1 d . . P . .
O2 O 0.2076(9) -0.1337(10) 0.4416(7) 0.100(5) Uani 1 1 d . . . . .
O1W O 0.4280(18) 0.379(2) 0.5000 0.191(16) Uani 1 2 d S T P . .
O1 O 0.3062(9) 0.2148(9) 0.5000 0.072(5) Uani 1 2 d S T P . .
O2W O 0.180(5) 0.360(5) 0.277(3) 0.26(3) Uani 0.5 1 d . U 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 O1 1.736(13) . ?
Nb1 O2 1.935(12) 2 ?
Nb1 O2 1.935(12) 15_556 ?
Nb1 O7 1.990(13) . ?
Nb1 O7 1.990(13) 12_556 ?
Nb1 O3 2.559(14) 2 ?
Nb1 O3 2.559(14) 15_556 ?
Nb2 O6 1.750(11) . ?
Nb2 O7 1.883(13) . ?
Nb2 O2 1.890(13) . ?
Nb2 O5 2.053(11) 2 ?
Nb2 O5 2.075(11) . ?
Nb2 O3 2.447(15) 2 ?
Nb2 O3 2.457(16) . ?
Nb2 V1 3.099(3) . ?
Cu2 N3 2.02(3) . ?
Cu2 N3 2.02(3) 9_656 ?
Cu2 N3 2.02(3) 12_556 ?
Cu2 N3 2.02(3) 4_655 ?
Cu2 N4 2.12(3) . ?
Cu2 N4 2.12(3) 12_556 ?
Cu2 N4 2.12(3) 4_655 ?
Cu2 N4 2.12(3) 9_656 ?
N3 N3 1.00(5) 12_556 ?
N3 C3 1.57(4) . ?
N3 C4 1.91(5) 12_556 ?
C3 C4 1.22(4) . ?
C3 C4 1.22(4) 12_556 ?
C3 N3 1.57(4) 12_556 ?
C4 N4 1.68(5) . ?
C4 N3 1.91(5) 12_556 ?
Cu1 Cu1 0.46(6) 5 ?
Cu1 N2 1.82(4) . ?
Cu1 N1 1.82(5) . ?
Cu1 N2 2.17(4) 5 ?
Cu1 N1 2.16(5) 5 ?
N1 C1 1.66(5) . ?
N1 Cu1 2.16(5) 5 ?
C1 C2 1.56(5) . ?
C2 N2 1.51(4) . ?
N2 Cu1 2.17(4) 5 ?
V1 O4 1.67(2) . ?
V1 O5 1.933(11) 2 ?
V1 O5 1.933(11) 7 ?
V1 O5 1.933(11) 4 ?
V1 O5 1.933(11) . ?
V1 Nb2 3.099(3) 2 ?
V1 Nb2 3.099(3) 7 ?
V1 Nb2 3.099(3) 4 ?
Si1 O3 1.630(14) . ?
Si1 O3 1.630(14) 15_556 ?
Si1 O3 1.630(14) 7 ?
Si1 O3 1.630(14) 9_556 ?
Si1 O3 1.630(14) 10_556 ?
Si1 O3 1.630(14) 2 ?
Si1 O3 1.630(14) 4 ?
Si1 O3 1.630(14) 12_556 ?
O5 Nb2 2.053(11) 7 ?
O3 Nb2 2.447(15) 7 ?
O3 Nb1 2.559(13) 10_556 ?
O2 Nb1 1.935(12) 10_556 ?
O2W O2W 1.50(12) 5 ?

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
O1 Nb1 O2 101.6(6) . 2 ?
O1 Nb1 O2 101.6(6) . 15_556 ?
O2 Nb1 O2 87.9(9) 2 15_556 ?
O1 Nb1 O7 99.0(5) . . ?
O2 Nb1 O7 88.0(5) 2 . ?
O2 Nb1 O7 159.3(7) 15_556 . ?
O1 Nb1 O7 99.0(5) . 12_556 ?
O2 Nb1 O7 159.3(7) 2 12_556 ?
O2 Nb1 O7 88.0(5) 15_556 12_556 ?
O7 Nb1 O7 88.6(8) . 12_556 ?
O1 Nb1 O3 158.2(3) . 2 ?
O2 Nb1 O3 64.2(6) 2 2 ?
O2 Nb1 O3 94.6(6) 15_556 2 ?
O7 Nb1 O3 65.5(5) . 2 ?
O7 Nb1 O3 96.0(6) 12_556 2 ?
O1 Nb1 O3 158.2(3) . 15_556 ?
O2 Nb1 O3 94.6(6) 2 15_556 ?
O2 Nb1 O3 64.2(6) 15_556 15_556 ?
O7 Nb1 O3 96.0(6) . 15_556 ?
O7 Nb1 O3 65.5(5) 12_556 15_556 ?
O3 Nb1 O3 43.6(7) 2 15_556 ?
O6 Nb2 O7 100.5(7) . . ?
O6 Nb2 O2 102.2(7) . . ?
O7 Nb2 O2 96.3(6) . . ?
O6 Nb2 O5 97.1(6) . 2 ?
O7 Nb2 O5 91.6(5) . 2 ?
O2 Nb2 O5 157.4(5) . 2 ?
O6 Nb2 O5 96.8(6) . . ?
O7 Nb2 O5 159.5(5) . . ?
O2 Nb2 O5 90.7(5) . . ?
O5 Nb2 O5 75.3(6) 2 . ?
O6 Nb2 O3 156.3(6) . 2 ?
O7 Nb2 O3 69.3(5) . 2 ?
O2 Nb2 O3 100.2(7) . 2 ?
O5 Nb2 O3 63.0(5) 2 2 ?
O5 Nb2 O3 90.5(5) . 2 ?
O6 Nb2 O3 155.4(6) . . ?
O7 Nb2 O3 102.6(6) . . ?
O2 Nb2 O3 67.0(6) . . ?
O5 Nb2 O3 90.6(5) 2 . ?
O5 Nb2 O3 62.6(5) . . ?
O3 Nb2 O3 45.0(6) 2 . ?
O6 Nb2 V1 99.2(5) . . ?
O7 Nb2 V1 127.3(4) . . ?
O2 Nb2 V1 126.1(3) . . ?
O5 Nb2 V1 37.6(3) 2 . ?
O5 Nb2 V1 37.7(3) . . ?
O3 Nb2 V1 73.2(3) 2 . ?
O3 Nb2 V1 73.1(3) . . ?
N3 Cu2 N3 180.0(12) . 9_656 ?
N3 Cu2 N3 28.5(14) . 12_556 ?
N3 Cu2 N3 151.5(14) 9_656 12_556 ?
N3 Cu2 N3 151.5(14) . 4_655 ?
N3 Cu2 N3 28.5(14) 9_656 4_655 ?
N3 Cu2 N3 180.0(9) 12_556 4_655 ?
N3 Cu2 N4 91.3(12) . . ?
N3 Cu2 N4 88.7(12) 9_656 . ?
N3 Cu2 N4 72.5(12) 12_556 . ?
N3 Cu2 N4 107.5(12) 4_655 . ?
N3 Cu2 N4 72.5(12) . 12_556 ?
N3 Cu2 N4 107.5(12) 9_656 12_556 ?
N3 Cu2 N4 91.3(12) 12_556 12_556 ?
N3 Cu2 N4 88.7(12) 4_655 12_556 ?
N4 Cu2 N4 82.2(19) . 12_556 ?
N3 Cu2 N4 107.5(12) . 4_655 ?
N3 Cu2 N4 72.5(12) 9_656 4_655 ?
N3 Cu2 N4 88.7(12) 12_556 4_655 ?
N3 Cu2 N4 91.3(12) 4_655 4_655 ?
N4 Cu2 N4 97.8(19) . 4_655 ?
N4 Cu2 N4 180.0(14) 12_556 4_655 ?
N3 Cu2 N4 88.7(12) . 9_656 ?
N3 Cu2 N4 91.3(12) 9_656 9_656 ?
N3 Cu2 N4 107.5(12) 12_556 9_656 ?
N3 Cu2 N4 72.5(12) 4_655 9_656 ?
N4 Cu2 N4 180.0 . 9_656 ?
N4 Cu2 N4 97.8(19) 12_556 9_656 ?
N4 Cu2 N4 82.2(19) 4_655 9_656 ?
N3 N3 C3 71.5(10) 12_556 . ?
N3 N3 C4 107.2(15) 12_556 12_556 ?
C3 N3 C4 39.6(15) . 12_556 ?
N3 N3 Cu2 75.8(7) 12_556 . ?
C3 N3 Cu2 100.6(19) . . ?
C4 N3 Cu2 93.2(17) 12_556 . ?
C4 C3 C4 121(5) . 12_556 ?
C4 C3 N3 85(3) . 12_556 ?
C4 C3 N3 118(3) 12_556 12_556 ?
C4 C3 N3 118(3) . . ?
C4 C3 N3 85(3) 12_556 . ?
N3 C3 N3 37(2) 12_556 . ?
C3 C4 N4 119(4) . . ?
C3 C4 N3 55(2) . 12_556 ?
N4 C4 N3 86(2) . 12_556 ?
C4 N4 Cu2 97(2) . . ?
Cu1 Cu1 N2 133(9) 5 . ?
Cu1 Cu1 N1 132(9) 5 . ?
N2 Cu1 N1 95(2) . . ?
Cu1 Cu1 N2 38(7) 5 5 ?
N2 Cu1 N2 170.0(17) . 5 ?
N1 Cu1 N2 94.0(19) . 5 ?
Cu1 Cu1 N1 39(7) 5 5 ?
N2 Cu1 N1 94.3(19) . 5 ?
N1 Cu1 N1 170.1(19) . 5 ?
N2 Cu1 N1 76.6(16) 5 5 ?
C1 N1 Cu1 109(3) . . ?
C1 N1 Cu1 119(3) . 5 ?
Cu1 N1 Cu1 9.2(19) . 5 ?
C2 C1 N1 105(3) . . ?
N2 C2 C1 112(3) . . ?
C2 N2 Cu1 111(3) . . ?
C2 N2 Cu1 120(2) . 5 ?
Cu1 N2 Cu1 9.0(19) . 5 ?
O4 V1 O5 112.7(4) . 2 ?
O4 V1 O5 112.7(4) . 7 ?
O5 V1 O5 134.6(8) 2 7 ?
O4 V1 O5 112.7(4) . 4 ?
O5 V1 O5 81.4(3) 2 4 ?
O5 V1 O5 81.4(3) 7 4 ?
O4 V1 O5 112.7(4) . . ?
O5 V1 O5 81.4(3) 2 . ?
O5 V1 O5 81.4(3) 7 . ?
O5 V1 O5 134.6(8) 4 . ?
O4 V1 Nb2 121.06(7) . . ?
O5 V1 Nb2 40.4(3) 2 . ?
O5 V1 Nb2 111.3(4) 7 . ?
O5 V1 Nb2 110.9(4) 4 . ?
O5 V1 Nb2 41.0(3) . . ?
O4 V1 Nb2 121.06(7) . 2 ?
O5 V1 Nb2 41.0(3) 2 2 ?
O5 V1 Nb2 110.9(4) 7 2 ?
O5 V1 Nb2 40.4(3) 4 2 ?
O5 V1 Nb2 111.3(4) . 2 ?
Nb2 V1 Nb2 74.57(7) . 2 ?
O4 V1 Nb2 121.06(7) . 7 ?
O5 V1 Nb2 110.9(4) 2 7 ?
O5 V1 Nb2 41.0(3) 7 7 ?
O5 V1 Nb2 111.3(4) 4 7 ?
O5 V1 Nb2 40.4(3) . 7 ?
Nb2 V1 Nb2 74.57(7) . 7 ?
Nb2 V1 Nb2 117.89(15) 2 7 ?
O4 V1 Nb2 121.06(7) . 4 ?
O5 V1 Nb2 111.3(4) 2 4 ?
O5 V1 Nb2 40.4(3) 7 4 ?
O5 V1 Nb2 41.0(3) 4 4 ?
O5 V1 Nb2 110.9(4) . 4 ?
Nb2 V1 Nb2 117.89(15) . 4 ?
Nb2 V1 Nb2 74.57(7) 2 4 ?
Nb2 V1 Nb2 74.57(7) 7 4 ?
O3 Si1 O3 109.8(5) . 15_556 ?
O3 Si1 O3 70.2(5) . 7 ?
O3 Si1 O3 180.0 15_556 7 ?
O3 Si1 O3 180.0(9) . 9_556 ?
O3 Si1 O3 70.2(5) 15_556 9_556 ?
O3 Si1 O3 109.8(5) 7 9_556 ?
O3 Si1 O3 109.8(5) . 10_556 ?
O3 Si1 O3 108.8(10) 15_556 10_556 ?
O3 Si1 O3 71.2(10) 7 10_556 ?
O3 Si1 O3 70.2(5) 9_556 10_556 ?
O3 Si1 O3 70.2(5) . 2 ?
O3 Si1 O3 71.2(10) 15_556 2 ?
O3 Si1 O3 108.8(10) 7 2 ?
O3 Si1 O3 109.8(5) 9_556 2 ?
O3 Si1 O3 180.0(9) 10_556 2 ?
O3 Si1 O3 108.8(10) . 4 ?
O3 Si1 O3 109.8(5) 15_556 4 ?
O3 Si1 O3 70.2(5) 7 4 ?
O3 Si1 O3 71.2(10) 9_556 4 ?
O3 Si1 O3 109.8(5) 10_556 4 ?
O3 Si1 O3 70.2(5) 2 4 ?
O3 Si1 O3 71.2(10) . 12_556 ?
O3 Si1 O3 70.2(5) 15_556 12_556 ?
O3 Si1 O3 109.8(5) 7 12_556 ?
O3 Si1 O3 108.8(10) 9_556 12_556 ?
O3 Si1 O3 70.2(5) 10_556 12_556 ?
O3 Si1 O3 109.8(5) 2 12_556 ?
O3 Si1 O3 180.0(9) 4 12_556 ?
Nb2 O7 Nb1 134.2(8) . . ?
V1 O5 Nb2 102.0(5) . 7 ?
V1 O5 Nb2 101.2(5) . . ?
Nb2 O5 Nb2 130.9(6) 7 . ?
Si1 O3 Nb2 122.5(8) . 7 ?
Si1 O3 Nb2 122.0(7) . . ?
Nb2 O3 Nb2 99.9(5) 7 . ?
Si1 O3 Nb1 122.6(8) . 10_556 ?
Nb2 O3 Nb1 90.9(4) 7 10_556 ?
Nb2 O3 Nb1 90.8(5) . 10_556 ?
Nb2 O2 Nb1 138.0(9) . 10_556 ?

_refine_diff_density_max         3.565
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.242



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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1554471'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT430_3                   
;
PROBLEM:  Short Inter D...A Contact   O10W   ..  O10W  ..   1.26 Ang. 
RESPONSE: O10w (O11w) is disorderedly distributed over two positions with
occupancy factors of 0.5 respectively.
As for other ALERTs about water molecules and terminal oxygens, 
there should be a strong hydrogen bond between the two atoms.
;

_vrf_PLAT975_3                   
;
PROBLEM: Check Calcd Residual Density  0.61A From      O7    3.38 eA-3
RESPONSE: the Residual Density possibly can be considered to be due to
the poor crystal quality or other effects.
;

_vrf_PLAT043_3                   
;
PROBLEM:  Calculated and Reported Mol. Weight Differ by .. 42.27 Check
RESPONSE: Some carbon and nitrogen atoms are disorderedly distributed.
thus the hydrogen atoms attached to them are not added. in addition, 
the hydrogen atoms attached to water molecules are not added too.
therefore, the Calculated and Reported Mol. Weight are different.
;

_vrf_PLAT306_3                   
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?) .......   O2W Check
RESPONSE:  the hydrogen atoms attached to water molecules are not added 
;

_vrf_PLAT342_3                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ............... 0.02333 Ang.
RESPONSE: The quality of this crystal was poor, however, it represents the
 best possible data after multiple crystallization attempts
;

_vrf_PLAT910_3                   
;
PROBLEM:  Missing # of FCF Reflection(s) Below Theta(Min)       18 Note
RESPONSE: Data completeness of is 99.8% which guarantees a correct
structural elucidation of compound 3.
;

_vrf_PLAT976_3                   
;
PROBLEM: Check Calcd Residual Density  0.61A From      O7    3.38 eA-3
RESPONSE: Please see our answer to _vrf_PLAT975_3.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H138 Cu6 N24 Nb12 O63 Si V2'
_chemical_formula_weight         3397.71

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'

_cell_length_a                   23.2503(7)
_cell_length_b                   20.5402(6)
_cell_length_c                   20.6527(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.742(3)
_cell_angle_gamma                90
_cell_volume                     9829.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12028
_cell_measurement_theta_min      3.6240
_cell_measurement_theta_max      28.8800

_exptl_crystal_description       block
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_F_000             6720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    2.907
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23698
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.102
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11280
_reflns_number_gt                9778
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0262P)²+576.3777P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11280
_refine_ls_number_parameters     635
_refine_ls_number_restraints     602
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0801
_refine_ls_wR_factor_ref         0.1648
_refine_ls_wR_factor_gt          0.1590
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . .


_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 1.750(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 ?

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 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) . . ?

_refine_diff_density_max         3.827
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.199



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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1554469'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT430_1                   
;
PROBLEM:  Short Inter D...A Contact  O4W    ..  O4W    ..   1.43 Ang. 
RESPONSE: O4w is disorderedly distributed over two positions with
occupancy factors of 0.5 respectively.
As for other ALERTs about water molecules and terminal oxygens, 
there should be a strong hydrogen bond between the two atoms.
;

_vrf_PLAT043_1                   
;
PROBLEM:  Calculated and Reported Mol. Weight Differ by .. 60.41 Check
RESPONSE: Some carbon and nitrogen atoms are disorderedly distributed.
thus the hydrogen atoms attached to them are not added. in addition, 
the hydrogen atoms attached to water molecules are not added too.
therefore, the Calculated and Reported Mol. Weight are different.
;

_vrf_PLAT306_1                   
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?) .......   O2W Check
RESPONSE:  the hydrogen atoms attached to water molecules are not added 
;

_vrf_PLAT342_1                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............  0.03 Ang
RESPONSE: The quality of this crystal was poor, however, it represents the
 best possible data after multiple crystallization attempts
;

_vrf_PLAT971_1                   
;
PROBLEM: Check Calcd Residual Density  1.31A From     O1W       2.70 eA-3
RESPONSE: the Residual Density possibly can be considered to be due to
the poor crystal quality or other effects.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H132 Cu6 N24 Nb12 O60 Si V2'
_chemical_formula_weight         3343.66

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 2/m'
_space_group_name_Hall           '-I 2y'

_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'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   14.8976(5)
_cell_length_b                   20.6011(8)
_cell_length_c                   16.2057(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.757(3)
_cell_angle_gamma                90
_cell_volume                     4939.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6942
_cell_measurement_theta_min      3.9180
_cell_measurement_theta_max      28.7580

_exptl_crystal_description       block
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.248
_exptl_crystal_F_000             3300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.888
_shelx_estimated_absorpt_T_min   0.596
_shelx_estimated_absorpt_T_max   0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12063
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.057
_diffrn_reflns_theta_max         29.038
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             5712
_reflns_number_gt                5001
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0654P)²+87.8145P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5712
_refine_ls_number_parameters     356
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1604
_refine_ls_wR_factor_gt          0.1531
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.128
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb4 Nb 0.70805(5) 0.5000 0.14557(5) 0.0291(2) Uani 1 2 d S T P . .
Nb3 Nb 0.51825(4) 0.40840(3) 0.19114(3) 0.03152(17) Uani 1 1 d . . . . .
Nb2 Nb 0.5000 0.31992(4) 0.0000 0.0329(2) Uani 1 2 d S T P . .
Nb1 Nb 0.69379(4) 0.40908(3) -0.04412(4) 0.03236(17) Uani 1 1 d . . . . .
Cu1 Cu 0.7500 0.2500 0.2500 0.0466(4) Uani 1 2 d S . P . .
Cu3 Cu 0.0000 0.5000 0.0000 0.0511(5) Uani 1 4 d S T P . .
Cu2 Cu 0.0000 0.0000 0.0000 0.0591(6) Uani 1 4 d S T P . .
Cu4 Cu 0.2500 0.2500 0.2500 0.0702(5) Uani 1 2 d S . P . .
Si1 Si 0.5000 0.5000 0.0000 0.0157(5) Uani 1 4 d S T P . .
V1 V 0.35450(10) 0.5000 0.19598(9) 0.0264(3) Uani 1 2 d S T P . .
O1 O 0.3897(7) 0.5000 -0.0096(7) 0.024(2) Uani 0.5 2 d S T P . .
O2 O 0.5355(5) 0.4337(4) -0.0460(5) 0.0232(16) Uani 0.5 1 d . . P . .
O3 O 0.5447(7) 0.5000 0.0978(7) 0.022(2) Uani 0.5 2 d S T P . .
O4 O 0.8090(7) 0.5000 0.2112(8) 0.090(4) Uani 1 2 d S T P . .
O5 O 0.5306(4) 0.3371(4) 0.1195(4) 0.080(2) Uani 1 1 d . U . . .
O6 O 0.6259(5) 0.3377(4) -0.0134(4) 0.081(2) Uani 1 1 d . U . . .
O7 O 0.7377(7) 0.4342(3) 0.0649(4) 0.080(2) Uani 1 1 d . U . . .
O8 O 0.6417(5) 0.4336(3) 0.1973(6) 0.077(2) Uani 1 1 d . U . . .
O9 O 0.5000 0.2366(4) 0.0000 0.062(2) Uani 1 2 d S T P . .
O10 O 0.5196(4) 0.3685(3) 0.2871(3) 0.0499(14) Uani 1 1 d . . . . .
O11 O 0.7906(4) 0.3719(3) -0.0740(4) 0.0529(15) Uani 1 1 d . . . . .
O12 O 0.3812(4) 0.4126(3) 0.1593(4) 0.0562(17) Uani 1 1 d . . . . .
O13 O 0.4838(4) 0.5000 0.2292(6) 0.049(2) Uani 1 2 d S T P . .
O14 O 0.2968(5) 0.5000 0.2749(4) 0.0415(17) Uani 1 2 d S T P . .
O15 O 0.2806(6) 0.5000 0.0897(5) 0.050(2) Uani 1 2 d S T P . .
N4 N 0.7813(7) 0.1749(4) 0.1800(5) 0.075(3) Uani 1 1 d . . . . .
H4C H 0.8369 0.1609 0.1968 0.090 Uiso 1 1 calc R U . . .
H4D H 0.7427 0.1424 0.1837 0.090 Uiso 1 1 calc R U . . .
C4 C 0.7754(12) 0.1989(9) 0.0934(8) 0.117(6) Uani 1 1 d . . . . .
H4A H 0.8154 0.1735 0.0630 0.141 Uiso 1 1 calc R U . . .
H4B H 0.7142 0.1930 0.0667 0.141 Uiso 1 1 calc R U . . .
C3 C 0.7996(12) 0.2665(9) 0.0900(10) 0.113(5) Uani 1 1 d . U . . .
H3A H 0.7850 0.2829 0.0340 0.136 Uiso 1 1 calc R U . . .
H3B H 0.8641 0.2717 0.1059 0.136 Uiso 1 1 calc R U . . .
N3 N 0.7497(6) 0.3020(5) 0.1467(5) 0.073(3) Uani 1 1 d . . . . .
H3C H 0.6932 0.3086 0.1237 0.087 Uiso 1 1 calc R U . . .
H3D H 0.7754 0.3404 0.1583 0.087 Uiso 1 1 calc R U . . .
N10 N 0.2360(9) 0.1567(6) 0.2262(8) 0.107(4) Uani 1 1 d . . . . .
H10C H 0.2410 0.1347 0.2738 0.128 Uiso 1 1 calc R U . . .
H10D H 0.1812 0.1493 0.1996 0.128 Uiso 1 1 calc R U . . .
N9 N 0.3460(9) 0.2460(6) 0.1736(8) 0.108(4) Uani 1 1 d . . . . .
H9C H 0.3347 0.2750 0.1330 0.129 Uiso 1 1 calc R U . . .
H9D H 0.3997 0.2551 0.2015 0.129 Uiso 1 1 calc R U . . .
N7 N -0.0665(9) 0.4208(10) 0.0692(9) 0.070(6) Uani 0.5 1 d D . P . .
H7C H -0.1221 0.4319 0.0789 0.084 Uiso 0.5 1 calc R U P . .
H7D H -0.0683 0.3832 0.0421 0.084 Uiso 0.5 1 calc R U P . .
C7 C -0.0051(13) 0.4190(11) 0.1438(12) 0.100(10) Uani 0.5 1 d D . P . .
H7A H 0.0327 0.3811 0.1393 0.120 Uiso 0.5 1 calc R U P . .
H7B H -0.0414 0.4101 0.1884 0.120 Uiso 0.5 1 calc R U P . .
C8 C 0.0550(14) 0.4709(10) 0.1726(10) 0.079(7) Uani 0.5 1 d D . P . .
N8 N 0.0880(8) 0.5000 0.1013(8) 0.070(3) Uani 1 2 d DS T P . .
C6 C -0.1567(16) 0.0000 0.0835(12) 0.105(7) Uani 1 2 d S T P . .
N6 N -0.0650(13) 0.0000 0.0992(9) 0.138(9) Uani 1 2 d S T P . .
C10 C 0.3042(15) 0.1344(10) 0.1756(14) 0.163(10) Uani 1 1 d . . . . .
H10A H 0.3488 0.1091 0.2102 0.195 Uiso 1 1 calc R U . . .
H10B H 0.2757 0.1061 0.1325 0.195 Uiso 1 1 calc R U . . .
O1W O 0.0703(16) 0.3015(11) 0.1001(15) 0.120(7) Uani 0.5 1 d . U P . .
O2W O 0.8893(14) 0.4150(10) 0.3193(14) 0.225(8) Uani 1 1 d . U . . .
O3W O 1.060(3) 0.5000 0.409(3) 0.332(19) Uani 1 2 d S TU P . .
O4W O 0.958(2) 0.3924(9) 0.4734(14) 0.139(11) Uani 0.5 1 d . . P . .
O5W O 0.0543(8) 0.1573(12) 0.0737(7) 0.222(10) Uani 1 1 d . . . . .
O6W O 0.5776(7) 0.2221(6) 0.2141(8) 0.130(4) Uani 1 1 d . . . . .
C9 C 0.3467(18) 0.1825(10) 0.1398(15) 0.175(11) Uani 1 1 d . . . . .
H9A H 0.3206 0.1851 0.0821 0.210 Uiso 1 1 calc R U . . .
H9B H 0.4093 0.1696 0.1398 0.210 Uiso 1 1 calc R U . . .
N5 N -0.1200(14) -0.0353(8) -0.0528(9) 0.069(5) Uani 0.5 1 d . . P . .
C5 C -0.1928(18) 0.0000 -0.0024(14) 0.163(14) Uani 1 2 d S T 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
Nb4 O4 1.737(8) . ?
Nb4 O8 1.936(7) 6_565 ?
Nb4 O8 1.936(7) . ?
Nb4 O7 1.969(7) 6_565 ?
Nb4 O7 1.969(7) . ?
Nb4 O3 2.465(11) . ?
Nb4 O1 2.494(12) 5_665 ?
Nb3 O10 1.756(5) . ?
Nb3 O5 1.895(6) . ?
Nb3 O8 1.902(7) . ?
Nb3 O12 2.048(6) . ?
Nb3 O13 2.068(3) . ?
Nb3 O2 2.450(8) 2_655 ?
Nb3 O3 2.479(7) . ?
Nb3 V1 3.0926(13) . ?
Nb2 O9 1.716(8) . ?
Nb2 O6 1.949(7) . ?
Nb2 O6 1.949(7) 2_655 ?
Nb2 O5 1.969(6) . ?
Nb2 O5 1.969(6) 2_655 ?
Nb2 O2 2.533(9) . ?
Nb2 O2 2.533(9) 2_655 ?
Nb1 O11 1.750(5) . ?
Nb1 O7 1.882(7) . ?
Nb1 O6 1.884(7) . ?
Nb1 O12 2.061(5) 2_655 ?
Nb1 O15 2.065(4) 5_665 ?
Nb1 O2 2.409(8) . ?
Nb1 O1 2.463(7) 5_665 ?
Nb1 V1 3.1090(13) 5_665 ?
Cu1 N3 1.988(7) . ?
Cu1 N3 1.988(7) 7_655 ?
Cu1 N4 2.005(9) . ?
Cu1 N4 2.005(9) 7_655 ?
Cu3 N8 1.976(12) 5_565 ?
Cu3 N8 1.976(12) . ?
Cu3 N7 2.27(2) . ?
Cu3 N7 2.27(2) 6_565 ?
Cu3 N7 2.27(2) 2 ?
Cu3 N7 2.27(2) 5_565 ?
Cu2 N6 1.972(16) . ?
Cu2 N6 1.972(16) 5 ?
Cu2 N5 2.024(18) . ?
Cu2 N5 2.024(18) 5 ?
Cu2 N5 2.024(18) 6 ?
Cu2 N5 2.024(18) 2 ?
Cu4 N10 1.966(12) . ?
Cu4 N10 1.966(12) 7 ?
Cu4 N9 2.001(11) . ?
Cu4 N9 2.001(11) 7 ?
Si1 O1 1.633(11) . ?
Si1 O1 1.633(11) 5_665 ?
Si1 O3 1.645(11) . ?
Si1 O3 1.645(11) 5_665 ?
Si1 O2 1.672(8) 5_665 ?
Si1 O2 1.672(8) 6_565 ?
Si1 O2 1.672(8) 2_655 ?
Si1 O2 1.672(8) . ?
V1 O14 1.623(7) . ?
V1 O15 1.932(7) . ?
V1 O13 1.938(7) . ?
V1 O12 1.952(5) 6_565 ?
V1 O12 1.952(5) . ?
V1 Nb3 3.0926(13) 6_565 ?
V1 Nb1 3.1091(13) 2_655 ?
V1 Nb1 3.1091(13) 5_665 ?
O1 Nb1 2.463(7) 2_655 ?
O1 Nb1 2.463(7) 5_665 ?
O1 Nb4 2.494(12) 5_665 ?
O2 Nb3 2.450(8) 2_655 ?
O3 Nb3 2.479(7) 6_565 ?
O12 Nb1 2.061(5) 2_655 ?
O13 Nb3 2.068(3) 6_565 ?
O15 Nb1 2.065(4) 2_655 ?
O15 Nb1 2.065(4) 5_665 ?
N4 C4 1.480(15) . ?
N4 H4C 0.8900 . ?
N4 H4D 0.8900 . ?
C4 C3 1.44(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 N3 1.446(17) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N10 C10 1.454(19) . ?
N10 H10C 0.8900 . ?
N10 H10D 0.8900 . ?
N9 C9 1.42(2) . ?
N9 H9C 0.8900 . ?
N9 H9D 0.8900 . ?
N7 C7 1.429(10) . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
C7 C8 1.437(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C8 1.20(4) 6_565 ?
C8 N8 1.439(9) . ?
N8 C8 1.439(9) 6_565 ?
C6 N6 1.36(3) . ?
C6 C5 1.43(3) . ?
C10 C9 1.34(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
O4W O4W 1.43(5) 2_756 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N5 N5 1.45(3) 6 ?
N5 C5 1.61(3) . ?
C5 N5 1.61(3) 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
O4 Nb4 O8 100.6(4) . 6_565 ?
O4 Nb4 O8 100.6(4) . . ?
O8 Nb4 O8 90.0(4) 6_565 . ?
O4 Nb4 O7 99.3(4) . 6_565 ?
O8 Nb4 O7 88.1(3) 6_565 6_565 ?
O8 Nb4 O7 160.0(4) . 6_565 ?
O4 Nb4 O7 99.3(4) . . ?
O8 Nb4 O7 160.0(4) 6_565 . ?
O8 Nb4 O7 88.1(3) . . ?
O7 Nb4 O7 87.0(4) 6_565 . ?
O4 Nb4 O3 160.7(6) . . ?
O8 Nb4 O3 66.5(3) 6_565 . ?
O8 Nb4 O3 66.5(3) . . ?
O7 Nb4 O3 94.7(3) 6_565 . ?
O7 Nb4 O3 94.7(3) . . ?
O4 Nb4 O1 156.1(6) . 5_665 ?
O8 Nb4 O1 96.2(3) 6_565 5_665 ?
O8 Nb4 O1 96.2(3) . 5_665 ?
O7 Nb4 O1 64.3(3) 6_565 5_665 ?
O7 Nb4 O1 64.3(3) . 5_665 ?
O3 Nb4 O1 43.2(4) . 5_665 ?
O10 Nb3 O5 100.8(4) . . ?
O10 Nb3 O8 99.8(3) . . ?
O5 Nb3 O8 94.6(3) . . ?
O10 Nb3 O12 98.6(3) . . ?
O5 Nb3 O12 92.5(2) . . ?
O8 Nb3 O12 158.6(3) . . ?
O10 Nb3 O13 98.1(3) . . ?
O5 Nb3 O13 159.3(3) . . ?
O8 Nb3 O13 90.4(3) . . ?
O12 Nb3 O13 76.2(2) . . ?
O10 Nb3 O2 156.6(3) . 2_655 ?
O5 Nb3 O2 67.7(3) . 2_655 ?
O8 Nb3 O2 101.4(3) . 2_655 ?
O12 Nb3 O2 63.0(3) . 2_655 ?
O13 Nb3 O2 91.6(3) . 2_655 ?
O10 Nb3 O3 155.5(3) . . ?
O5 Nb3 O3 100.5(3) . . ?
O8 Nb3 O3 66.6(4) . . ?
O12 Nb3 O3 92.3(3) . . ?
O13 Nb3 O3 63.3(3) . . ?
O2 Nb3 O3 46.4(3) 2_655 . ?
O10 Nb3 V1 100.94(19) . . ?
O5 Nb3 V1 128.51(18) . . ?
O8 Nb3 V1 126.4(2) . . ?
O12 Nb3 V1 38.26(15) . . ?
O13 Nb3 V1 37.97(19) . . ?
O2 Nb3 V1 74.05(19) 2_655 . ?
O3 Nb3 V1 74.5(2) . . ?
O9 Nb2 O6 100.9(3) . . ?
O9 Nb2 O6 100.9(3) . 2_655 ?
O6 Nb2 O6 158.3(5) . 2_655 ?
O9 Nb2 O5 100.3(3) . . ?
O6 Nb2 O5 87.8(3) . . ?
O6 Nb2 O5 88.3(3) 2_655 . ?
O9 Nb2 O5 100.3(3) . 2_655 ?
O6 Nb2 O5 88.4(3) . 2_655 ?
O6 Nb2 O5 87.8(3) 2_655 2_655 ?
O5 Nb2 O5 159.3(5) . 2_655 ?
O9 Nb2 O2 157.65(17) . . ?
O6 Nb2 O2 63.7(3) . . ?
O6 Nb2 O2 95.5(3) 2_655 . ?
O5 Nb2 O2 95.2(3) . . ?
O5 Nb2 O2 65.0(3) 2_655 . ?
O9 Nb2 O2 157.65(17) . 2_655 ?
O6 Nb2 O2 95.5(3) . 2_655 ?
O6 Nb2 O2 63.7(3) 2_655 2_655 ?
O5 Nb2 O2 65.0(3) . 2_655 ?
O5 Nb2 O2 95.2(3) 2_655 2_655 ?
O2 Nb2 O2 44.7(3) . 2_655 ?
O11 Nb1 O7 100.0(3) . . ?
O11 Nb1 O6 102.5(4) . . ?
O7 Nb1 O6 96.0(3) . . ?
O11 Nb1 O12 98.1(3) . 2_655 ?
O7 Nb1 O12 158.7(3) . 2_655 ?
O6 Nb1 O12 90.9(2) . 2_655 ?
O11 Nb1 O15 96.0(3) . 5_665 ?
O7 Nb1 O15 91.6(3) . 5_665 ?
O6 Nb1 O15 158.4(3) . 5_665 ?
O12 Nb1 O15 75.4(3) 2_655 5_665 ?
O11 Nb1 O2 157.8(3) . . ?
O7 Nb1 O2 100.7(3) . . ?
O6 Nb1 O2 67.2(3) . . ?
O12 Nb1 O2 63.6(3) 2_655 . ?
O15 Nb1 O2 91.5(3) 5_665 . ?
O11 Nb1 O1 153.7(3) . 5_665 ?
O7 Nb1 O1 66.0(4) . 5_665 ?
O6 Nb1 O1 101.0(4) . 5_665 ?
O12 Nb1 O1 92.9(3) 2_655 5_665 ?
O15 Nb1 O1 63.8(3) 5_665 5_665 ?
O2 Nb1 O1 46.4(3) . 5_665 ?
O11 Nb1 V1 99.55(19) . 5_665 ?
O7 Nb1 V1 126.8(2) . 5_665 ?
O6 Nb1 V1 126.71(18) . 5_665 ?
O12 Nb1 V1 37.98(15) 2_655 5_665 ?
O15 Nb1 V1 37.4(2) 5_665 5_665 ?
O2 Nb1 V1 74.2(2) . 5_665 ?
O1 Nb1 V1 75.1(2) 5_665 5_665 ?
N3 Cu1 N3 180.0 . 7_655 ?
N3 Cu1 N4 85.2(4) . . ?
N3 Cu1 N4 94.8(4) 7_655 . ?
N3 Cu1 N4 94.8(4) . 7_655 ?
N3 Cu1 N4 85.2(4) 7_655 7_655 ?
N4 Cu1 N4 180.0 . 7_655 ?
N8 Cu3 N8 180.0(5) 5_565 . ?
N8 Cu3 N7 97.2(4) 5_565 . ?
N8 Cu3 N7 82.8(4) . . ?
N8 Cu3 N7 97.2(4) 5_565 6_565 ?
N8 Cu3 N7 82.8(4) . 6_565 ?
N7 Cu3 N7 91.8(8) . 6_565 ?
N8 Cu3 N7 82.8(4) 5_565 2 ?
N8 Cu3 N7 97.2(4) . 2 ?
N7 Cu3 N7 88.2(8) . 2 ?
N7 Cu3 N7 180.0(6) 6_565 2 ?
N8 Cu3 N7 82.8(4) 5_565 5_565 ?
N8 Cu3 N7 97.2(4) . 5_565 ?
N7 Cu3 N7 180.0 . 5_565 ?
N7 Cu3 N7 88.2(8) 6_565 5_565 ?
N7 Cu3 N7 91.8(8) 2 5_565 ?
N6 Cu2 N6 180.0 . 5 ?
N6 Cu2 N5 81.4(7) . . ?
N6 Cu2 N5 98.6(7) 5 . ?
N6 Cu2 N5 98.6(7) . 5 ?
N6 Cu2 N5 81.4(7) 5 5 ?
N5 Cu2 N5 180.0 . 5 ?
N6 Cu2 N5 81.4(7) . 6 ?
N6 Cu2 N5 98.6(7) 5 6 ?
N5 Cu2 N5 42.1(10) . 6 ?
N5 Cu2 N5 137.9(10) 5 6 ?
N6 Cu2 N5 98.6(7) . 2 ?
N6 Cu2 N5 81.4(7) 5 2 ?
N5 Cu2 N5 137.9(10) . 2 ?
N5 Cu2 N5 42.1(10) 5 2 ?
N5 Cu2 N5 180.0(13) 6 2 ?
N10 Cu4 N10 180.0 . 7 ?
N10 Cu4 N9 84.6(5) . . ?
N10 Cu4 N9 95.4(5) 7 . ?
N10 Cu4 N9 95.4(5) . 7 ?
N10 Cu4 N9 84.6(5) 7 7 ?
N9 Cu4 N9 180.0 . 7 ?
O1 Si1 O1 180.0 . 5_665 ?
O1 Si1 O3 112.4(6) . . ?
O1 Si1 O3 67.6(6) 5_665 . ?
O1 Si1 O3 67.6(6) . 5_665 ?
O1 Si1 O3 112.4(6) 5_665 5_665 ?
O3 Si1 O3 180.0 . 5_665 ?
O1 Si1 O2 71.0(3) . 5_665 ?
O1 Si1 O2 109.0(3) 5_665 5_665 ?
O3 Si1 O2 71.6(3) . 5_665 ?
O3 Si1 O2 108.4(3) 5_665 5_665 ?
O1 Si1 O2 109.0(3) . 6_565 ?
O1 Si1 O2 71.0(3) 5_665 6_565 ?
O3 Si1 O2 108.4(3) . 6_565 ?
O3 Si1 O2 71.6(3) 5_665 6_565 ?
O2 Si1 O2 70.3(5) 5_665 6_565 ?
O1 Si1 O2 71.0(3) . 2_655 ?
O1 Si1 O2 109.0(3) 5_665 2_655 ?
O3 Si1 O2 71.6(3) . 2_655 ?
O3 Si1 O2 108.4(3) 5_665 2_655 ?
O2 Si1 O2 109.7(5) 5_665 2_655 ?
O2 Si1 O2 180.0(5) 6_565 2_655 ?
O1 Si1 O2 109.0(3) . . ?
O1 Si1 O2 71.0(3) 5_665 . ?
O3 Si1 O2 108.4(3) . . ?
O3 Si1 O2 71.6(3) 5_665 . ?
O2 Si1 O2 180.0 5_665 . ?
O2 Si1 O2 109.7(5) 6_565 . ?
O2 Si1 O2 70.3(5) 2_655 . ?
O14 V1 O15 113.8(4) . . ?
O14 V1 O13 112.5(4) . . ?
O15 V1 O13 133.7(4) . . ?
O14 V1 O12 112.7(2) . 6_565 ?
O15 V1 O12 81.0(2) . 6_565 ?
O13 V1 O12 81.5(2) . 6_565 ?
O14 V1 O12 112.7(2) . . ?
O15 V1 O12 81.0(2) . . ?
O13 V1 O12 81.5(2) . . ?
O12 V1 O12 134.6(5) 6_565 . ?
O14 V1 Nb3 120.8(2) . 6_565 ?
O15 V1 Nb3 110.2(2) . 6_565 ?
O13 V1 Nb3 41.04(11) . 6_565 ?
O12 V1 Nb3 40.50(17) 6_565 6_565 ?
O12 V1 Nb3 111.4(2) . 6_565 ?
O14 V1 Nb3 120.8(2) . . ?
O15 V1 Nb3 110.2(2) . . ?
O13 V1 Nb3 41.04(11) . . ?
O12 V1 Nb3 111.4(2) 6_565 . ?
O12 V1 Nb3 40.50(17) . . ?
Nb3 V1 Nb3 75.21(4) 6_565 . ?
O14 V1 Nb1 121.9(2) . 2_655 ?
O15 V1 Nb1 40.52(11) . 2_655 ?
O13 V1 Nb1 110.5(2) . 2_655 ?
O12 V1 Nb1 110.6(2) 6_565 2_655 ?
O12 V1 Nb1 40.50(16) . 2_655 ?
Nb3 V1 Nb1 117.21(5) 6_565 2_655 ?
Nb3 V1 Nb1 73.86(3) . 2_655 ?
O14 V1 Nb1 121.9(2) . 5_665 ?
O15 V1 Nb1 40.52(11) . 5_665 ?
O13 V1 Nb1 110.5(2) . 5_665 ?
O12 V1 Nb1 40.50(16) 6_565 5_665 ?
O12 V1 Nb1 110.6(2) . 5_665 ?
Nb3 V1 Nb1 73.86(3) 6_565 5_665 ?
Nb3 V1 Nb1 117.21(5) . 5_665 ?
Nb1 V1 Nb1 74.09(4) 2_655 5_665 ?
Si1 O1 Nb1 120.7(3) . 2_655 ?
Si1 O1 Nb1 120.7(3) . 5_665 ?
Nb1 O1 Nb1 99.0(4) 2_655 5_665 ?
Si1 O1 Nb4 124.1(6) . 5_665 ?
Nb1 O1 Nb4 92.6(3) 2_655 5_665 ?
Nb1 O1 Nb4 92.6(3) 5_665 5_665 ?
Si1 O2 Nb1 121.8(4) . . ?
Si1 O2 Nb3 121.1(4) . 2_655 ?
Nb1 O2 Nb3 100.2(3) . 2_655 ?
Si1 O2 Nb2 122.5(4) . . ?
Nb1 O2 Nb2 92.3(3) . . ?
Nb3 O2 Nb2 91.7(3) 2_655 . ?
Si1 O3 Nb4 125.1(6) . . ?
Si1 O3 Nb3 120.8(3) . . ?
Nb4 O3 Nb3 91.7(3) . . ?
Si1 O3 Nb3 120.8(3) . 6_565 ?
Nb4 O3 Nb3 91.7(3) . 6_565 ?
Nb3 O3 Nb3 99.1(4) . 6_565 ?
Nb3 O5 Nb2 135.6(4) . . ?
Nb1 O6 Nb2 136.9(5) . . ?
Nb1 O7 Nb4 137.1(5) . . ?
Nb3 O8 Nb4 135.2(5) . . ?
V1 O12 Nb3 101.2(3) . . ?
V1 O12 Nb1 101.5(3) . 2_655 ?
Nb3 O12 Nb1 130.2(4) . 2_655 ?
V1 O13 Nb3 101.0(2) . . ?
V1 O13 Nb3 101.0(2) . 6_565 ?
Nb3 O13 Nb3 131.7(4) . 6_565 ?
V1 O15 Nb1 102.1(2) . 2_655 ?
V1 O15 Nb1 102.1(2) . 5_665 ?
Nb1 O15 Nb1 130.1(4) 2_655 5_665 ?
C4 N4 Cu1 106.7(8) . . ?
C4 N4 H4C 110.4 . . ?
Cu1 N4 H4C 110.4 . . ?
C4 N4 H4D 110.4 . . ?
Cu1 N4 H4D 110.4 . . ?
H4C N4 H4D 108.6 . . ?
C3 C4 N4 111.7(13) . . ?
C3 C4 H4A 109.3 . . ?
N4 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
N4 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C4 C3 N3 108.3(13) . . ?
C4 C3 H3A 110.0 . . ?
N3 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
N3 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
C3 N3 Cu1 108.1(8) . . ?
C3 N3 H3C 110.1 . . ?
Cu1 N3 H3C 110.1 . . ?
C3 N3 H3D 110.1 . . ?
Cu1 N3 H3D 110.1 . . ?
H3C N3 H3D 108.4 . . ?
C10 N10 Cu4 110.7(9) . . ?
C10 N10 H10C 109.5 . . ?
Cu4 N10 H10C 109.5 . . ?
C10 N10 H10D 109.5 . . ?
Cu4 N10 H10D 109.5 . . ?
H10C N10 H10D 108.1 . . ?
C9 N9 Cu4 108.3(9) . . ?
C9 N9 H9C 110.0 . . ?
Cu4 N9 H9C 110.0 . . ?
C9 N9 H9D 110.0 . . ?
Cu4 N9 H9D 110.0 . . ?
H9C N9 H9D 108.4 . . ?
C7 N7 Cu3 99.4(12) . . ?
C7 N7 H7C 111.9 . . ?
Cu3 N7 H7C 111.9 . . ?
C7 N7 H7D 111.9 . . ?
Cu3 N7 H7D 111.9 . . ?
H7C N7 H7D 109.6 . . ?
N7 C7 C8 124.6(18) . . ?
N7 C7 H7A 106.2 . . ?
C8 C7 H7A 106.2 . . ?
N7 C7 H7B 106.2 . . ?
C8 C7 H7B 106.2 . . ?
H7A C7 H7B 106.4 . . ?
C8 C8 C7 138.1(13) 6_565 . ?
C8 C8 N8 65.4(9) 6_565 . ?
C7 C8 N8 107.9(14) . . ?
C8 N8 C8 49.2(18) 6_565 . ?
C8 N8 Cu3 114.3(10) 6_565 . ?
C8 N8 Cu3 114.3(10) . . ?
N6 C6 C5 115.9(19) . . ?
C6 N6 Cu2 115.2(13) . . ?
C9 C10 N10 114.1(18) . . ?
C9 C10 H10A 108.7 . . ?
N10 C10 H10A 108.7 . . ?
C9 C10 H10B 108.7 . . ?
N10 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C10 C9 N9 119.2(15) . . ?
C10 C9 H9A 107.5 . . ?
N9 C9 H9A 107.5 . . ?
C10 C9 H9B 107.5 . . ?
N9 C9 H9B 107.5 . . ?
H9A C9 H9B 107.0 . . ?
N5 N5 C5 63.1(7) 6 . ?
N5 N5 Cu2 68.9(5) 6 . ?
C5 N5 Cu2 103.7(11) . . ?
C6 C5 N5 107.2(18) . 6 ?
C6 C5 N5 107.2(18) . . ?
N5 C5 N5 53.8(15) 6 . ?

_refine_diff_density_max         2.809
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.172



