# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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. 
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data_mo_60722b
_database_code_depnum_ccdc_archive 'CCDC 1554237'
_audit_update_record             
;
2017-11-20 deposited with the CCDC.
2017-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_mo_60722b           
;
PROBLEM: Check Calcd Resid. Dens.  1.68A   From O14             4.20 eA-3
RESPONSE: The compound containing highly disordered lattice water molecules. The number of lattice water molecules could be determined by TG analysis. O14 is from coordination water molecule, therefore, the lattice water molecules and coordination water molecules may form hydrogen bonds among them. The residual density could be the lattice water molecules since the distance is possible for hydrogen bond but the position could not be determined.
;
_vrf_PLAT971_mo_60722b_2         
;
PROBLEM: Check Calcd Resid. Dens.  2.03A   From O4              3.63 eA-3
RESPONSE: The compound containing highly disordered lattice water molecules. The number of lattice water molecules could be determined by TG analysis. O4 is from terminal oxygen atom of Keggin anion, therefore, the lattice water molecules and terminal oxygen atom may form hydrogen bonds among them. The residual density could be the lattice water molecules since the distance is possible for hydrogen bond but the position could not be determined.
;
_vrf_PLAT975_mo_60722b           
;
PROBLEM: Check Calcd Resid. Dens.  0.87A   From O2W             2.56 eA-3
RESPONSE: O2W is from lattice water molecule. The residual density could be the H atoms since the distance is within normal O-H distance but the position could not be determined.
;
_vrf_PLAT975_mo_60722b_2         
;
PROBLEM: Check Calcd Resid. Dens.  0.71A   From O1              2.05 eA-3
RESPONSE: O1 is from the hydroxide ion according to BVS calculation. The residual density could be the H atoms since the distance is within normal O-H distance but the position could not be determined.
;
_vrf_PLAT975_mo_60722b_3         
;
PROBLEM: Check Calcd Resid. Dens.  0.64A   From O2W             2.03 eA-3
RESPONSE: O2W is from lattice water molecule. The residual density could be the H atoms since the distance is within normal O-H distance but the position could not be determined.
;
_vrf_PLAT430_mo_60722b           
;
PROBLEM: Short Inter D...A Contact O2W      ..O13       .       2.74 Ang.
RESPONSE: O2W is from lattice water molecule. O13 is from coordination water molecule. The distance is reasonable for the hydrogen bond between them, but the position of H atom could not be determined.
;
_vrf_PLAT971_mo_60722b_3         
;
PROBLEM: Check Calcd Resid. Dens.  1.47A   From O1W             3.25 eA-3
RESPONSE: The compound containing highly disordered lattice water molecules. The number of lattice water molecules could be determined by TG analysis. O1W is from the lattice water molecule and may form hydrogen bonds among them. The residual density could be the lattice water molecules since the distance is possible for hydrogen bond but the position could not be determined.
;
_vrf_PLAT971_mo_60722b_4         
;
PROBLEM: Check Calcd Resid. Dens.  1.43A   From O15             2.91 eA-3
RESPONSE: The compound containing highly disordered lattice water molecules. The number of lattice water molecules could be determined by TG analysis. O15 is from coordination water molecules, therefore, the lattice water molecules and coordination water molecule may form hydrogen bonds among them. The residual density could be the lattice water molecules since the distance is possible for hydrogen bond but the position could not be determined.
;
_vrf_PLAT971_mo_60722b_5         
;
PROBLEM: Check Calcd Resid. Dens.  0.87A   From O2W             2.56 eA-3
RESPONSE: O2W is from lattice water molecules, the residual density could be the H atoms since the distance is within normal O-H distance but the position could not be determined.
;
# Added during the CSD deposition process: Monday 20 November 2017 06:09 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H12 Cu8 N18 Nb3 O56.50 P W9'
_chemical_formula_weight         3785.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_H-M_alt        'I 41/a c d'
_space_group_name_Hall           '-I 4bd 2c'

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

_cell_length_a                   17.588(2)
_cell_length_b                   17.588(2)
_cell_length_c                   47.567(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14714(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    36495
_cell_measurement_theta_min      1.848
_cell_measurement_theta_max      25.999

_exptl_crystal_description       slice
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.417
_exptl_crystal_F_000             13584
_exptl_transmission_factor_min   0.320
_exptl_transmission_factor_max   0.603
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    16.843
_shelx_estimated_absorpt_T_min   0.3962
_shelx_estimated_absorpt_T_max   0.5635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker AXS)'
_exptl_absorpt_special_details   
'wR2(int)=0.1014 before and 0.0662 after the adsorption correction process.'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36495
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_theta_min         1.848
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3616
_reflns_number_gt                2793
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0560P)²+1412.7617P] 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         3616
_refine_ls_number_parameters     244
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0521
_refine_ls_wR_factor_ref         0.1363
_refine_ls_wR_factor_gt          0.1225
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
P1 P 0.500000 0.250000 0.125000 0.0048(13) Uani 1 4 d S TU P . .
W1 W 0.30723(3) 0.31895(4) 0.12682(2) 0.01096(18) Uani 0.875 1 d . U P . .
W2 W 0.43375(4) 0.37605(4) 0.17838(2) 0.01394(19) Uani 0.875 1 d . U P . .
W3 W 0.44346(5) 0.38500(5) 0.07204(2) 0.0166(2) Uani 0.5 1 d . U P . .
Nb1 Nb 0.30723(3) 0.31895(4) 0.12682(2) 0.01096(18) Uani 0.125 1 d . U P . .
Nb2 Nb 0.43375(4) 0.37605(4) 0.17838(2) 0.01394(19) Uani 0.125 1 d . U P . .
Nb3 Nb 0.44346(5) 0.38500(5) 0.07204(2) 0.0166(2) Uani 0.5 1 d . U P . .
Cu1 Cu 0.32580(11) 0.49951(10) 0.02269(4) 0.0176(4) Uani 1 1 d D U . . .
Cu2 Cu 0.250000 0.66987(14) 0.000000 0.0118(5) Uani 1 2 d S TU P . .
Cu3 Cu 0.5121(4) 0.7342(3) 0.07811(9) 0.0270(13) Uani 0.5 1 d . U P . .
C1 C 0.3897(9) 0.7181(9) 0.0326(4) 0.021(4) Uani 1 1 d . . . . .
H1 H 0.382818 0.769425 0.028745 0.025 Uiso 1 1 calc R U . . .
C2 C 0.4234(11) 0.6164(9) 0.0506(4) 0.025(4) Uani 1 1 d . . . . .
H2 H 0.447108 0.581306 0.062242 0.030 Uiso 1 1 calc R U . . .
C3 C 0.2936(10) 0.3344(9) 0.0147(3) 0.020(4) Uani 1 1 d . U . . .
H3 H 0.331184 0.319862 0.027350 0.025 Uiso 1 1 calc R U . . .
N1 N 0.3494(7) 0.6626(7) 0.0211(3) 0.015(2) Uani 1 1 d . . . . .
N2 N 0.3710(7) 0.5983(7) 0.0332(3) 0.015(2) Uani 1 1 d . . . . .
N3 N 0.4413(10) 0.6910(10) 0.0504(3) 0.035(4) Uani 1 1 d . U . . .
N4 N 0.2784(8) 0.4027(7) 0.0096(3) 0.015(3) Uani 1 1 d . U . . .
N5 N 0.250000 0.2826(10) 0.000000 0.012(3) Uani 1 2 d S TU P . .
O1 O 0.250000 0.5543(9) 0.000000 0.023(2) Uani 1 2 d S TU P . .
O2 O 0.3969(7) 0.4424(6) 0.0462(3) 0.023(2) Uani 1 1 d . . . . .
O3 O 0.3661(6) 0.3780(5) 0.1008(2) 0.010(2) Uani 1 1 d . . . . .
O4 O 0.2191(6) 0.3525(7) 0.1200(2) 0.022(3) Uani 1 1 d . . . . .
O5 O 0.3420(6) 0.3871(6) 0.1564(2) 0.0100(15) Uani 1 1 d . . . . .
O6 O 0.3849(5) 0.2906(6) 0.1965(2) 0.013(2) Uani 1 1 d . . . . .
O7 O 0.5305(5) 0.3372(6) 0.1879(2) 0.013(2) Uani 1 1 d . . . . .
O8 O 0.4320(6) 0.2706(6) 0.1437(2) 0.0100(15) Uani 1 1 d . U . . .
O9 O 0.2859(5) 0.2457(6) 0.1562(2) 0.013(2) Uani 1 1 d . . . . .
O10 O 0.3192(6) 0.2366(5) 0.1012(2) 0.010(2) Uani 1 1 d . . . . .
O11 O 0.4185(7) 0.4458(6) 0.2037(2) 0.020(3) Uani 1 1 d . . . . .
O12 O 0.2486(9) 0.4928(8) 0.0689(3) 0.045(4) Uani 1 1 d . . . . .
O13 O 0.4248(14) 0.5057(12) -0.0178(4) 0.055(7) Uani 0.8 1 d D U P . .
O13' O 0.386(6) 0.496(6) -0.0276(13) 0.055(7) Uani 0.2 1 d D . P . .
O14 O 0.3978(18) 0.7440(17) 0.1038(7) 0.048(7) Uani 0.5 1 d . U P . .
O15 O 0.4789(19) 0.6535(16) 0.1055(7) 0.052(8) Uani 0.5 1 d . U P . .
O1W O 0.361(6) 0.611(6) 0.125000 0.10(4) Uiso 0.25 2 d S . P . .
O2W O 0.122(2) 0.396(2) 0.0549(8) 0.060(10) Uiso 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O8 1.534(10) 20_656 ?
P1 O8 1.534(10) 10_554 ?
P1 O8 1.534(10) 27_565 ?
P1 O8 1.534(10) . ?
W1 O4 1.691(11) . ?
W1 O10 1.903(9) . ?
W1 O3 1.919(10) . ?
W1 O9 1.938(10) . ?
W1 O5 1.946(10) . ?
W1 O8 2.486(10) . ?
W2 O11 1.739(10) . ?
W2 O7 1.888(10) . ?
W2 O6 1.932(10) . ?
W2 O5 1.933(10) . ?
W2 O10 1.943(10) 27_565 ?
W2 O8 2.482(10) . ?
W3 O2 1.788(11) . ?
W3 O3 1.934(10) . ?
W3 O6 1.954(11) 27_565 ?
W3 O9 1.962(10) 27_565 ?
W3 O7 1.973(10) 20_656 ?
W3 O8 2.426(10) 27_565 ?
Cu1 O2 1.956(11) . ?
Cu1 O1 1.968(8) . ?
Cu1 N2 1.976(13) . ?
Cu1 N4 1.996(13) . ?
Cu1 O12 2.585(14) . ?
Cu1 O13 2.598(18) . ?
Cu2 N5 1.982(17) 26 ?
Cu2 N1 2.021(12) . ?
Cu2 N1 2.021(12) 5 ?
Cu2 O1 2.032(16) . ?
Cu2 O11 2.401(10) 15_444 ?
Cu2 O11 2.401(10) 11_544 ?
Cu3 Cu3 0.700(8) 10_564 ?
Cu3 N3 1.963(16) . ?
Cu3 O15 2.01(3) . ?
Cu3 N3 2.033(17) 10_564 ?
Cu3 O14 2.04(3) 10_564 ?
Cu3 O14 2.36(3) . ?
Cu3 O15 2.37(3) 10_564 ?
C1 N1 1.32(2) . ?
C1 N3 1.33(2) . ?
C2 N2 1.28(2) . ?
C2 N3 1.35(2) . ?
C3 N4 1.25(2) . ?
C3 N5 1.381(19) . ?
N1 N2 1.324(18) . ?
N4 N4 1.35(2) 5 ?
O13 O13' 0.84(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 P1 O8 109.6(4) 20_656 10_554 ?
O8 P1 O8 109.1(7) 20_656 27_565 ?
O8 P1 O8 109.6(4) 10_554 27_565 ?
O8 P1 O8 109.6(4) 20_656 . ?
O8 P1 O8 109.1(7) 10_554 . ?
O8 P1 O8 109.6(4) 27_565 . ?
O4 W1 O10 104.1(5) . . ?
O4 W1 O3 100.4(5) . . ?
O10 W1 O3 86.5(4) . . ?
O4 W1 O9 101.2(5) . . ?
O10 W1 O9 88.7(4) . . ?
O3 W1 O9 158.4(4) . . ?
O4 W1 O5 102.3(5) . . ?
O10 W1 O5 153.6(4) . . ?
O3 W1 O5 87.9(4) . . ?
O9 W1 O5 87.0(4) . . ?
O4 W1 O8 172.3(5) . . ?
O10 W1 O8 81.3(4) . . ?
O3 W1 O8 85.3(4) . . ?
O9 W1 O8 73.2(4) . . ?
O5 W1 O8 72.5(4) . . ?
O11 W2 O7 103.2(5) . . ?
O11 W2 O6 99.9(5) . . ?
O7 W2 O6 90.7(4) . . ?
O11 W2 O5 100.1(5) . . ?
O7 W2 O5 156.6(4) . . ?
O6 W2 O5 87.0(4) . . ?
O11 W2 O10 103.1(5) . 27_565 ?
O7 W2 O10 85.5(4) . 27_565 ?
O6 W2 O10 157.0(4) . 27_565 ?
O5 W2 O10 87.6(4) . 27_565 ?
O11 W2 O8 170.0(4) . . ?
O7 W2 O8 84.3(4) . . ?
O6 W2 O8 73.1(4) . . ?
O5 W2 O8 72.8(4) . . ?
O10 W2 O8 83.9(4) 27_565 . ?
O2 W3 O3 101.5(5) . . ?
O2 W3 O6 101.1(5) . 27_565 ?
O3 W3 O6 157.4(4) . 27_565 ?
O2 W3 O9 100.1(5) . 27_565 ?
O3 W3 O9 90.1(4) . 27_565 ?
O6 W3 O9 87.4(4) 27_565 27_565 ?
O2 W3 O7 103.7(5) . 20_656 ?
O3 W3 O7 85.3(4) . 20_656 ?
O6 W3 O7 87.9(4) 27_565 20_656 ?
O9 W3 O7 156.2(4) 27_565 20_656 ?
O2 W3 O8 172.6(4) . 27_565 ?
O3 W3 O8 83.6(4) . 27_565 ?
O6 W3 O8 74.1(4) 27_565 27_565 ?
O9 W3 O8 74.3(4) 27_565 27_565 ?
O7 W3 O8 82.0(4) 20_656 27_565 ?
O2 Cu1 O1 177.1(4) . . ?
O2 Cu1 N2 92.8(5) . . ?
O1 Cu1 N2 88.9(5) . . ?
O2 Cu1 N4 90.5(5) . . ?
O1 Cu1 N4 87.9(6) . . ?
N2 Cu1 N4 176.2(5) . . ?
O2 Cu1 O12 80.0(5) . . ?
O1 Cu1 O12 97.6(4) . . ?
N2 Cu1 O12 92.1(5) . . ?
N4 Cu1 O12 90.4(5) . . ?
O2 Cu1 O13 91.0(7) . . ?
O1 Cu1 O13 91.5(5) . . ?
N2 Cu1 O13 83.2(6) . . ?
N4 Cu1 O13 94.8(6) . . ?
O12 Cu1 O13 169.6(7) . . ?
N5 Cu2 N1 93.6(4) 26 . ?
N5 Cu2 N1 93.6(4) 26 5 ?
N1 Cu2 N1 172.7(7) . 5 ?
N5 Cu2 O1 180.0 26 . ?
N1 Cu2 O1 86.4(4) . . ?
N1 Cu2 O1 86.4(4) 5 . ?
N5 Cu2 O11 90.6(3) 26 15_444 ?
N1 Cu2 O11 83.5(5) . 15_444 ?
N1 Cu2 O11 96.5(5) 5 15_444 ?
O1 Cu2 O11 89.4(3) . 15_444 ?
N5 Cu2 O11 90.6(3) 26 11_544 ?
N1 Cu2 O11 96.5(5) . 11_544 ?
N1 Cu2 O11 83.5(5) 5 11_544 ?
O1 Cu2 O11 89.4(3) . 11_544 ?
O11 Cu2 O11 178.9(6) 15_444 11_544 ?
Cu3 Cu3 N3 85.6(10) 10_564 . ?
Cu3 Cu3 O15 112.6(14) 10_564 . ?
N3 Cu3 O15 88.7(10) . . ?
Cu3 Cu3 N3 74.3(9) 10_564 10_564 ?
N3 Cu3 N3 94.1(10) . 10_564 ?
O15 Cu3 N3 172.7(12) . 10_564 ?
Cu3 Cu3 O14 108.8(13) 10_564 10_564 ?
N3 Cu3 O14 165.4(11) . 10_564 ?
O15 Cu3 O14 88.3(12) . 10_564 ?
N3 Cu3 O14 87.3(10) 10_564 10_564 ?
Cu3 Cu3 O14 54.9(11) 10_564 . ?
N3 Cu3 O14 80.6(9) . . ?
O15 Cu3 O14 57.9(13) . . ?
N3 Cu3 O14 129.2(10) 10_564 . ?
O14 Cu3 O14 109.7(17) 10_564 . ?
Cu3 Cu3 O15 51.5(12) 10_564 10_564 ?
N3 Cu3 O15 137.1(11) . 10_564 ?
O15 Cu3 O15 104.5(16) . 10_564 ?
N3 Cu3 O15 77.9(9) 10_564 10_564 ?
O14 Cu3 O15 57.4(13) 10_564 10_564 ?
O14 Cu3 O15 73.2(10) . 10_564 ?
N1 C1 N3 111.4(15) . . ?
N2 C2 N3 114.2(16) . . ?
N4 C3 N5 114.6(15) . . ?
C1 N1 N2 107.2(12) . . ?
C1 N1 Cu2 128.5(11) . . ?
N2 N1 Cu2 121.2(9) . . ?
C2 N2 N1 105.9(13) . . ?
C2 N2 Cu1 132.4(11) . . ?
N1 N2 Cu1 121.6(10) . . ?
C1 N3 C2 101.0(15) . . ?
C1 N3 Cu3 136.2(14) . . ?
C2 N3 Cu3 121.4(13) . . ?
C1 N3 Cu3 117.1(13) . 10_564 ?
C2 N3 Cu3 136.1(13) . 10_564 ?
Cu3 N3 Cu3 20.1(3) . 10_564 ?
C3 N4 N4 106.8(9) . 5 ?
C3 N4 Cu1 131.9(11) . . ?
N4 N4 Cu1 121.3(4) 5 . ?
C3 N5 C3 97.4(18) 5 . ?
C3 N5 Cu2 131.3(9) 5 26_545 ?
C3 N5 Cu2 131.3(9) . 26_545 ?
Cu1 O1 Cu1 121.3(8) . 5 ?
Cu1 O1 Cu2 119.3(4) . . ?
Cu1 O1 Cu2 119.3(4) 5 . ?
W3 O2 Cu1 167.3(8) . . ?
W1 O3 W3 150.5(5) . . ?
W2 O5 W1 126.3(5) . . ?
W2 O6 W3 124.0(5) . 20_656 ?
W2 O7 W3 151.7(6) . 27_565 ?
P1 O8 W3 129.5(5) . 20_656 ?
P1 O8 W2 123.5(5) . . ?
W3 O8 W2 88.7(3) 20_656 . ?
P1 O8 W1 125.6(5) . . ?
W3 O8 W1 88.8(3) 20_656 . ?
W2 O8 W1 88.3(3) . . ?
W1 O9 W3 123.6(5) . 20_656 ?
W1 O10 W2 152.0(6) . 20_656 ?
W2 O11 Cu2 156.0(6) . 12_454 ?
O13' O13 Cu1 82(4) . . ?
Cu3 O14 Cu3 16.3(3) 10_564 . ?
Cu3 O15 Cu3 15.8(3) . 10_564 ?

_refine_diff_density_max         3.880
_refine_diff_density_min         -1.829
_refine_diff_density_rms         0.372

####################################################################### 
# 
# 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_142
_database_code_depnum_ccdc_archive 'CCDC 1554238'
_audit_update_record             
;
2017-11-20 deposited with the CCDC.
2017-11-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT410_142                 
;
PROBLEM: Short Intra H...H Contact H2       ..H4'       .       1.57 Ang.
RESPONSE: H4' is from the positional disordered ligand and H2 is from the stable ligand, the distance is somewhat meaningless.
;
_vrf_PLAT430_142                 
;
PROBLEM: Short Inter D...A Contact O7       ..O12       .       2.02 Ang.
RESPONSE: O12 is from lattice water molecule and H atoms could not be refined to stable model. O7 is the terminal oxygen atom, the distance is reasonable for hydrogen bond between them.
;
_vrf_PLAT430_142_2               
;
PROBLEM: Short Inter D...A Contact O12      ..N4'       .       2.45 Ang.
RESPONSE: O12 is from lattice water molecule and H atoms could not be refined to stable model. N4' is from the ligand, the distance is reasonable for hydrogen bond between them.
;
_vrf_PLAT430_142_3               
;
PROBLEM: Short Inter D...A Contact O12      ..N4'       .       2.45 Ang.
RESPONSE: O12 is from lattice water molecule and H atoms could not be refined to stable model. N4' is from the ligand, the distance is reasonable for hydrogen bond between them.
;
_vrf_PLAT971_142                 
;
PROBLEM: Check Calcd Resid. Dens.  2.38A   From O12             4.09 eA-3
RESPONSE: The compound containing highly disordered lattice water molecules. The number of lattice water molecules could be determined by TG analysis. O12 is from the lattice water molecules and may form hydrogen bonds among them. The residual density could be the lattice water molecules since the distance is possible for hydrogen bond but the position could not be determined.
;
_vrf_PLAT972_142                 
;
PROBLEM: Check Calcd Resid. Dens.  0.36A   From W3             -4.49 eA-3
RESPONSE: It is series terminal errors caused by heavy atoms (Nb,W) in the position.
;
_vrf_PLAT972_142_2               
;
PROBLEM: Check Calcd Resid. Dens.  0.35A   From W3             -4.49 eA-3
RESPONSE: It is series terminal errors caused by heavy atoms (Nb,W) in the position.
;
_vrf_PLAT972_142_3               
;
PROBLEM: Check Calcd Resid. Dens.  0.43A   From W3             -4.43 eA-3
RESPONSE: It is series terminal errors caused by heavy atoms (Nb,W) in the position.
;
_vrf_PLAT972_142_4               
;
PROBLEM: Check Calcd Resid. Dens.  0.61A   From W3             -4.33 eA-3
RESPONSE: It is series terminal errors caused by heavy atoms (Nb,W) in the position.
;
_vrf_PLAT975_142                 
;
PROBLEM: Check Calcd Resid. Dens.  0.71A   From O14             2.45 eA-3
RESPONSE: O14 is from coordination water molecule, the residual density could be the H atoms since the distance is within normal O-H distance but the position could not be determined.
;
_vrf_PLAT201_142                 
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          2 Report
RESPONSE:  The two atoms are O13 and O14. They are from coordination water molecules and could not be refined anistropically due to the stability of the structure.
;
_vrf_PLAT306_142                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O12 Check
RESPONSE: O12 is from lattice water molecule and refined isotropically, H atom could not be stably refined.
;
_vrf_PLAT430_142_4               
;
PROBLEM: Short Inter D...A Contact O12      ..N4        .       2.65 Ang.
RESPONSE: O12 is from lattice water molecule and H atoms could not be refined to stable model. N4 is from the ligand, the distance is reasonable for hydrogen bond between them.
;
_vrf_PLAT430_142_5               
;
PROBLEM: Short Inter D...A Contact O12      ..N4        .       2.65 Ang.
RESPONSE: O12 is from lattice water molecule and H atoms could not be refined to stable model. N4 is from the ligand, the distance is reasonable for hydrogen bond between them.
;
_vrf_PLAT976_142                 
;
PROBLEM: Check Calcd Resid. Dens.  0.58A   From O12            -1.59 eA-3
RESPONSE: O14 is from lattice water molecule, the residual density could be the H atoms since the distance is within normal O-H distance but the position could not be determined.
;
# Added during the CSD deposition process: Monday 20 November 2017 06:18 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            
'C12.80 H14.40 Cu6.40 N19.20 Nb2.40 O41.60 P0.80 W7.20'
_chemical_formula_weight         3080.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_H-M_alt        'I 41/a c d'
_space_group_name_Hall           '-I 4bd 2c'

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

_cell_length_a                   17.5009(8)
_cell_length_b                   17.5009(8)
_cell_length_c                   47.384(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14513.0(19)
_cell_formula_units_Z            10
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4405
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.29

_exptl_crystal_description       slice
_exptl_crystal_colour            green
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.525
_exptl_crystal_F_000             13872
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    17.077
_shelx_estimated_absorpt_T_min   0.4780
_shelx_estimated_absorpt_T_max   0.7452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_process_details   'SADABS-2008/1,(Bruker AXS)'
_exptl_absorpt_special_details   
'wR2(int)=0.1130 before and 0.0607 after the adsorption correction process.'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42896
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_theta_min         1.719
_diffrn_reflns_theta_max         25.384
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3334
_reflns_number_gt                2624
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0510P)²+3596.5210P] 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         3334
_refine_ls_number_parameters     268
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.1706
_refine_ls_wR_factor_gt          0.1634
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
O14 O 0.0850(16) -0.0003(17) -0.0217(6) 0.084(8) Uiso 1 1 d . . . . .
O13 O 0.2562(13) -0.0121(13) 0.0672(4) 0.060(6) Uiso 1 1 d . . . . .
P1 P 0.500000 0.250000 0.125000 0.0103(18) Uani 1 4 d S T P . .
W1 W 0.30598(5) 0.31741(5) 0.12680(2) 0.0160(3) Uani 0.75 1 d . . P . .
W2 W 0.37343(5) 0.18240(5) 0.07159(2) 0.0163(3) Uani 0.75 1 d . . P . .
W3 W 0.44275(7) 0.38423(7) 0.07187(3) 0.0329(3) Uani 0.75 1 d . . P . .
Nb1 Nb 0.30598(5) 0.31741(5) 0.12680(2) 0.0160(3) Uani 0.25 1 d . . P . .
Nb2 Nb 0.37343(5) 0.18240(5) 0.07159(2) 0.0163(3) Uani 0.25 1 d . . P . .
Nb3 Nb 0.44275(7) 0.38423(7) 0.07187(3) 0.0329(3) Uani 0.25 1 d . . P . .
Cu3 Cu 0.000000 0.250000 0.08010(14) 0.0586(15) Uani 1 2 d DS TU P . .
Cu1 Cu 0.17328(17) -0.00170(15) 0.02197(6) 0.0288(7) Uani 1 1 d . . . . .
Cu2 Cu 0.250000 0.16828(18) 0.000000 0.0180(8) Uani 1 2 d S T P . .
O5 O 0.3171(9) 0.2341(8) 0.1012(3) 0.025(3) Uani 1 1 d . . . . .
O3 O 0.4586(8) 0.1341(8) 0.0530(3) 0.018(3) Uani 1 1 d . . . . .
O4 O 0.4128(8) 0.2797(7) 0.0618(3) 0.016(3) Uani 1 1 d . . . . .
O8 O 0.3388(7) 0.3874(8) 0.1560(3) 0.016(3) Uani 1 1 d . . . . .
O9 O 0.3646(8) 0.3768(8) 0.1005(3) 0.018(3) Uani 1 1 d . . . . .
O10 O 0.3973(8) 0.4391(8) 0.0461(3) 0.023(3) Uani 1 1 d . . . . .
O2 O 0.3054(8) 0.1678(8) 0.0464(3) 0.022(3) Uani 1 1 d . . . . .
O7 O 0.2138(8) 0.3483(9) 0.1201(3) 0.027(4) Uani 1 1 d . . . . .
O6 O 0.2862(7) 0.2434(8) 0.1559(3) 0.017(3) Uani 1 1 d . . . . .
O11 O 0.5223(8) 0.3188(7) 0.1063(3) 0.015(3) Uani 1 1 d . . . . .
O1 O 0.250000 0.0536(11) 0.000000 0.025(3) Uani 1 2 d S T P . .
N6 N 0.250000 0.2830(13) 0.000000 0.024(6) Uani 1 2 d S T P . .
N7 N 0.2190(10) -0.0975(10) 0.0088(4) 0.022(4) Uani 1 1 d . . . . .
O12 O 0.0989(11) 0.3489(11) 0.125000 0.046(7) Uiso 1 2 d S . P . .
C1 C 0.1084(15) 0.2172(16) 0.0334(6) 0.042(7) Uani 1 1 d . . . . .
H1 H 0.112485 0.269084 0.029439 0.050 Uiso 1 1 calc R U . . .
C2 C 0.0746(18) 0.1121(15) 0.0497(7) 0.056(9) Uani 1 1 d . . . . .
H2 H 0.049544 0.074956 0.060215 0.067 Uiso 1 1 calc R U . . .
C3 C 0.2049(14) -0.1688(12) 0.0142(5) 0.028(5) Uani 1 1 d . . . . .
H3 H 0.167258 -0.184761 0.026757 0.034 Uiso 1 1 calc R U . . .
N1 N 0.1524(10) 0.1637(10) 0.0218(4) 0.026(4) Uani 1 1 d . . . . .
N2 N 0.1277(12) 0.0965(11) 0.0324(5) 0.038(5) Uani 1 1 d . . . . .
N3 N 0.0576(16) 0.1874(13) 0.0514(7) 0.070(9) Uani 1 1 d . . . . .
C4 C 0.139(3) 0.170(4) 0.1059(14) 0.103(17) Uani 0.75(6) 1 d D U P A 1
H4 H 0.174549 0.184966 0.092575 0.124 Uiso 0.75(6) 1 calc R U P A 1
N4 N 0.069(3) 0.205(3) 0.1115(10) 0.100(14) Uani 0.75(6) 1 d D U P A 1
N5 N 0.145(3) 0.105(3) 0.125000 0.10(2) Uani 0.75(6) 2 d DS TU P A 1
H5 H 0.179359 0.070643 0.125001 0.126 Uiso 0.75(6) 2 calc R U P A 1
C4' C 0.099(7) 0.121(7) 0.0992(18) 0.09(3) Uani 0.25(6) 1 d D U P A 2
H4' H 0.112025 0.105024 0.081091 0.109 Uiso 0.25(6) 1 calc R U P A 2
N4' N 0.033(5) 0.162(5) 0.108(2) 0.08(2) Uani 0.25(6) 1 d D U P A 2
N5' N 0.142(3) 0.108(3) 0.125000 0.09(3) Uani 0.25(6) 2 d DGS TU P A 2
H5' H 0.177110 0.072893 0.125000 0.107 Uiso 0.25(6) 2 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O14 Cu1 2.58(3) . ?
O13 Cu1 2.60(2) . ?
P1 O11 1.544(13) . ?
P1 O11 1.544(13) 10_554 ?
P1 O11 1.544(13) 27_565 ?
P1 O11 1.544(13) 20_656 ?
W1 O7 1.730(14) . ?
W1 O5 1.906(15) . ?
W1 O9 1.920(14) . ?
W1 O6 1.922(14) . ?
W1 O8 1.934(13) . ?
W1 O11 2.463(13) 20_656 ?
W2 O2 1.704(14) . ?
W2 O4 1.894(13) . ?
W2 O3 1.926(15) . ?
W2 O5 1.940(14) . ?
W2 O8 1.962(14) 20_656 ?
W2 O11 2.457(13) 10_554 ?
W3 O10 1.746(15) . ?
W3 O9 1.931(14) . ?
W3 O6 1.959(13) 27_565 ?
W3 O4 1.962(13) . ?
W3 O3 1.971(14) 10_554 ?
W3 O11 2.433(13) . ?
Cu3 N3 2.02(3) 10_454 ?
Cu3 N3 2.02(3) . ?
Cu3 N4 2.07(5) . ?
Cu3 N4 2.07(5) 10_454 ?
Cu3 N4' 2.10(5) 10_454 ?
Cu3 N4' 2.10(5) . ?
Cu1 O1 1.955(10) . ?
Cu1 N2 1.96(2) . ?
Cu1 N7 1.960(17) . ?
Cu1 O10 1.976(15) 30_545 ?
Cu2 N1 1.997(18) 5 ?
Cu2 N1 1.997(18) . ?
Cu2 O1 2.01(2) . ?
Cu2 N6 2.01(2) . ?
Cu2 O2 2.404(14) . ?
Cu2 O2 2.404(14) 5 ?
N6 C3 1.34(3) 30 ?
N6 C3 1.34(3) 26 ?
N7 C3 1.30(3) . ?
N7 N7 1.37(3) 5 ?
C1 N1 1.33(3) . ?
C1 N3 1.34(4) . ?
C2 N2 1.27(3) . ?
C2 N3 1.35(3) . ?
N1 N2 1.35(3) . ?
C4 N4 1.39(7) . ?
C4 N5 1.45(6) . ?
N4 N4 1.41(9) 8 ?
C4' N4' 1.42(7) . ?
C4' N5' 1.45(7) . ?

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
O11 P1 O11 110.1(10) . 10_554 ?
O11 P1 O11 109.2(5) . 27_565 ?
O11 P1 O11 109.2(5) 10_554 27_565 ?
O11 P1 O11 109.2(5) . 20_656 ?
O11 P1 O11 109.2(5) 10_554 20_656 ?
O11 P1 O11 110.1(10) 27_565 20_656 ?
O7 W1 O5 102.6(7) . . ?
O7 W1 O9 102.1(7) . . ?
O5 W1 O9 87.0(6) . . ?
O7 W1 O6 100.0(7) . . ?
O5 W1 O6 87.6(6) . . ?
O9 W1 O6 157.9(6) . . ?
O7 W1 O8 102.1(7) . . ?
O5 W1 O8 155.3(6) . . ?
O9 W1 O8 87.8(5) . . ?
O6 W1 O8 88.2(6) . . ?
O7 W1 O11 171.5(6) . 20_656 ?
O5 W1 O11 82.6(6) . 20_656 ?
O9 W1 O11 84.8(5) . 20_656 ?
O6 W1 O11 73.2(5) . 20_656 ?
O8 W1 O11 72.9(5) . 20_656 ?
O2 W2 O4 102.6(6) . . ?
O2 W2 O3 98.9(6) . . ?
O4 W2 O3 90.0(6) . . ?
O2 W2 O5 102.7(7) . . ?
O4 W2 O5 86.8(6) . . ?
O3 W2 O5 158.3(6) . . ?
O2 W2 O8 100.8(6) . 20_656 ?
O4 W2 O8 156.7(6) . 20_656 ?
O3 W2 O8 87.5(6) . 20_656 ?
O5 W2 O8 87.0(6) . 20_656 ?
O2 W2 O11 170.4(6) . 10_554 ?
O4 W2 O11 84.4(5) . 10_554 ?
O3 W2 O11 74.2(5) . 10_554 ?
O5 W2 O11 84.1(6) . 10_554 ?
O8 W2 O11 72.6(5) 20_656 10_554 ?
O10 W3 O9 101.8(7) . . ?
O10 W3 O6 101.1(6) . 27_565 ?
O9 W3 O6 89.4(6) . 27_565 ?
O10 W3 O4 102.8(6) . . ?
O9 W3 O4 85.4(6) . . ?
O6 W3 O4 156.1(6) 27_565 . ?
O10 W3 O3 99.9(6) . 10_554 ?
O9 W3 O3 158.2(6) . 10_554 ?
O6 W3 O3 87.9(6) 27_565 10_554 ?
O4 W3 O3 88.4(6) . 10_554 ?
O10 W3 O11 171.7(6) . . ?
O9 W3 O11 84.4(5) . . ?
O6 W3 O11 73.4(5) 27_565 . ?
O4 W3 O11 82.9(5) . . ?
O3 W3 O11 74.1(5) 10_554 . ?
N3 Cu3 N3 95(2) 10_454 . ?
N3 Cu3 N4 169.2(17) 10_454 . ?
N3 Cu3 N4 89.2(17) . . ?
N3 Cu3 N4 89.2(17) 10_454 10_454 ?
N3 Cu3 N4 169.2(17) . 10_454 ?
N4 Cu3 N4 88(3) . 10_454 ?
N3 Cu3 N4' 83(3) 10_454 10_454 ?
N3 Cu3 N4' 163(3) . 10_454 ?
N4 Cu3 N4' 90(3) . 10_454 ?
N4 Cu3 N4' 28(3) 10_454 10_454 ?
N3 Cu3 N4' 163(3) 10_454 . ?
N3 Cu3 N4' 83(3) . . ?
N4' Cu3 N4' 103(6) 10_454 . ?
O1 Cu1 N2 88.9(8) . . ?
O1 Cu1 N7 88.5(7) . . ?
N2 Cu1 N7 176.0(9) . . ?
O1 Cu1 O10 175.3(5) . 30_545 ?
N2 Cu1 O10 93.4(7) . 30_545 ?
N7 Cu1 O10 89.5(7) . 30_545 ?
O1 Cu1 O14 88.9(6) . . ?
N2 Cu1 O14 87.2(10) . . ?
N7 Cu1 O14 89.8(9) . . ?
O10 Cu1 O14 95.4(8) 30_545 . ?
O1 Cu1 O13 95.2(5) . . ?
N2 Cu1 O13 94.6(9) . . ?
N7 Cu1 O13 88.6(8) . . ?
O10 Cu1 O13 80.5(7) 30_545 . ?
O14 Cu1 O13 175.6(8) . . ?
N1 Cu2 N1 175.4(10) 5 . ?
N1 Cu2 O1 87.7(5) 5 . ?
N1 Cu2 O1 87.7(5) . . ?
N1 Cu2 N6 92.3(5) 5 . ?
N1 Cu2 N6 92.3(5) . . ?
O1 Cu2 N6 180.0 . . ?
N1 Cu2 O2 97.4(7) 5 . ?
N1 Cu2 O2 82.6(7) . . ?
O1 Cu2 O2 89.8(4) . . ?
N6 Cu2 O2 90.2(4) . . ?
N1 Cu2 O2 82.6(7) 5 5 ?
N1 Cu2 O2 97.4(7) . 5 ?
O1 Cu2 O2 89.8(4) . 5 ?
N6 Cu2 O2 90.2(4) . 5 ?
O2 Cu2 O2 179.6(7) . 5 ?
W1 O5 W2 150.3(8) . . ?
W2 O3 W3 122.8(7) . 10_554 ?
W2 O4 W3 151.1(8) . . ?
W1 O8 W2 125.0(7) . 27_565 ?
W1 O9 W3 150.5(8) . . ?
W3 O10 Cu1 168.0(9) . 30 ?
W2 O2 Cu2 157.1(8) . . ?
W1 O6 W3 124.3(7) . 20_656 ?
P1 O11 W3 127.3(7) . . ?
P1 O11 W2 124.4(7) . 10_554 ?
W3 O11 W2 88.8(4) . 10_554 ?
P1 O11 W1 126.1(7) . 27_565 ?
W3 O11 W1 89.0(4) . 27_565 ?
W2 O11 W1 89.3(4) 10_554 27_565 ?
Cu1 O1 Cu1 120.7(10) 5 . ?
Cu1 O1 Cu2 119.7(5) 5 . ?
Cu1 O1 Cu2 119.7(5) . . ?
C3 N6 C3 102(3) 30 26 ?
C3 N6 Cu2 129.1(13) 30 . ?
C3 N6 Cu2 129.1(13) 26 . ?
C3 N7 N7 105.8(13) . 5 ?
C3 N7 Cu1 132.9(16) . . ?
N7 N7 Cu1 121.2(5) 5 . ?
N1 C1 N3 112(2) . . ?
N2 C2 N3 114(2) . . ?
N7 C3 N6 113(2) . 26_545 ?
C1 N1 N2 105.8(19) . . ?
C1 N1 Cu2 132.8(17) . . ?
N2 N1 Cu2 120.2(13) . . ?
C2 N2 N1 107(2) . . ?
C2 N2 Cu1 130.6(18) . . ?
N1 N2 Cu1 122.6(15) . . ?
C1 N3 C2 101(2) . . ?
C1 N3 Cu3 123.4(19) . . ?
C2 N3 Cu3 133(2) . . ?
N4 C4 N5 107(5) . . ?
C4 N4 N4 108(4) . 8 ?
C4 N4 Cu3 123(4) . . ?
N4 N4 Cu3 126(3) 8 . ?
C4 N5 C4 106(7) 8 . ?
N4' C4' N5' 106(6) . . ?
C4' N4' Cu3 115(5) . . ?

_refine_diff_density_max         3.770
_refine_diff_density_min         -4.832
_refine_diff_density_rms         0.427

