# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_w11_final
_database_code_depnum_ccdc_archive 'CCDC 2249036'
_audit_update_record             
;
2023-03-15 deposited with the CCDC.	2024-09-06 downloaded from the CCDC.
;
_audit_creation_date             2022-03-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'(C72 H24 Cu12 O48) (O40 P V W11)4- 2*(C4 H12 N+) 12*(H2O)@Cu 10(H2O) 2(H3O+)'
_chemical_formula_sum            'C80 H98 Cu12 N2 O112 P V W11'
_chemical_formula_weight         5746.34
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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 0.1857 0.4707 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0015 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0013 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0229 0.0309 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.1100 0.1867 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -1.1497 2.7769 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   26.2682(12)
_cell_length_b                   26.2682(12)
_cell_length_c                   26.2682(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18126(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4079
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      10.61
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.905
_shelx_estimated_absorpt_T_min   0.822
_exptl_absorpt_coefficient_mu    2.037
_exptl_absorpt_correction_T_max  0.9683
_exptl_absorpt_correction_T_min  0.8780
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1482 before and 0.1047 after correction.
The Ratio of minimum to maximum transmission is 0.9067.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_description       bulk
_exptl_crystal_F_000             10752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1620
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            99252
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        13.896
_diffrn_reflns_theta_max         13.896
_diffrn_reflns_theta_min         0.901
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'huber 3-circle'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   'synchrotron at Advanced Photo Source'
_diffrn_source_current           103.0
_diffrn_source_power             103.0
_diffrn_source_voltage           1000.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                631
_reflns_number_total             812
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.585
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         812
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1122P)²+54.9215P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1594
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{W1, V1}
{O2W, O2U}
2. Restrained distances
 N1S-C1S
 1.5 with sigma of 0.01
 O2U-H2UA = O2U-H2UB = O2U-H2UC
 0.95 with sigma of 0.05
 H2UC-H2UA = H2UC-H2UB
 1.52 with sigma of 0.05
 H2UC-H2UA \\sim H2UC-H2UB \\sim H2UA-H2UB
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(W1) = Uanis(V1)
Uanis(O2W) = Uanis(O2U)
4. Others
 Fixed Sof: W1(0.229175) V1(0.020825) O4(0.083333) H1SA(0.08335) H1SB(0.08335)
 H1SC(0.08335) O1W(0.25) H1WA(0.125) H1WB(0.25) O2W(0.20835) H(0.2083)
 HA(0.10415) O2U(0.04165) H2UA(0.0417) H2UB(0.04165) H2UC(0.0417)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H,HA)
5.b Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
W1 W 0.40427(2) 0.500000 0.40427(2) 0.0761(4) Uani 0.9167 4 d S T P . .
V1 V 0.40427(2) 0.500000 0.40427(2) 0.0761(4) Uani 0.0833 4 d S T P . .
Cu1 Cu 0.21448(5) 0.500000 0.28552(5) 0.0731(6) Uani 1 4 d S T P . .
P1 P 0.500000 0.500000 0.500000 0.067(3) Uani 1 48 d S T P . .
O1 O 0.2561(2) 0.4475(2) 0.3173(2) 0.0875(16) Uani 1 1 d . . . . .
O3 O 0.4499(3) 0.5501(3) 0.3800(4) 0.113(3) Uani 1 2 d S T P . .
O2 O 0.3590(3) 0.500000 0.3590(3) 0.107(4) Uani 1 4 d S T P . .
C1 C 0.2975(3) 0.4300(6) 0.2975(3) 0.084(3) Uani 1 2 d S T P . .
C2 C 0.3219(3) 0.3886(5) 0.3219(3) 0.086(3) Uani 1 2 d S T P . .
C3 C 0.3660(3) 0.3660(3) 0.3001(5) 0.085(3) Uani 1 2 d S T P . .
H3 H 0.380536 0.380535 0.270397 0.102 Uiso 1 2 calc R U P . .
O4 O 0.4667(6) 0.5333(6) 0.4667(6) 0.079(7) Uani 0.5 6 d S T P . .
N1S N 0.250000 0.250000 0.250000 0.19(3) Uani 1 24 d DS T P . .
C1S C 0.2169(2) 0.2169(2) 0.2169(2) 0.28(3) Uiso 1 6 d DS . P . .
H1SA H 0.238437 0.195358 0.195358 0.415 Uiso 0.1667 1 calc R U P A -1
H1SB H 0.195358 0.195358 0.238437 0.415 Uiso 0.1667 1 calc R U P A -1
H1SC H 0.195358 0.238437 0.195358 0.415 Uiso 0.1667 1 calc R U P A -1
O1W O 0.1452(6) 0.500000 0.3317(7) 0.128(9) Uani 0.5 2 d S T P . .
H1WA H 0.142599 0.479660 0.357430 0.153 Uiso 0.25 1 d R U P B -1
H1WB H 0.121039 0.520340 0.324800 0.153 Uiso 0.25 1 d R U P B -1
O2W O 0.2538(7) 0.500000 0.4266(8) 0.113(6) Uani 0.4167 2 d S T P C 1
H H 0.255334 0.528970 0.440891 0.169 Uiso 0.2083 1 d R U P C -1
HA H 0.281354 0.500000 0.409741 0.169 Uiso 0.2083 1 d R U P C -1
O2U O 0.2538(7) 0.500000 0.4266(8) 0.113(6) Uani 0.0833 2 d DS T P D 2
H2UA H 0.269(16) 0.529(9) 0.443(10) 0.169 Uiso 0.0417 1 d D U P E 2
H2UB H 0.27(2) 0.500000 0.393(7) 0.169 Uiso 0.0833 2 d DS U P F 2
H2UC H 0.269(16) 0.471(9) 0.443(10) 0.169 Uiso 0.0417 1 d D U P G 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
W1 O3 1.890(4) . ?
W1 O3 1.891(4) 99_565 ?
W1 O3 1.891(4) 103_556 ?
W1 O3 1.891(4) 6_566 ?
W1 O2 1.681(13) . ?
W1 O4 2.478(14) 99_565 ?
W1 O4 2.478(14) . ?
Cu1 Cu1 2.639(4) 145_565 ?
Cu1 O1 1.948(6) 99_565 ?
Cu1 O1 1.948(6) 72_565 ?
Cu1 O1 1.948(6) . ?
Cu1 O1 1.948(6) 166 ?
Cu1 O1W 2.187(15) . ?
Cu1 O1W 2.187(15) 166 ?
P1 O4 1.52(3) . ?
P1 O4 1.52(3) 97_666 ?
P1 O4 1.52(3) 3_656 ?
P1 O4 1.52(3) 100_655 ?
P1 O4 1.52(3) 2_665 ?
P1 O4 1.52(3) 99_565 ?
P1 O4 1.52(3) 98_556 ?
P1 O4 1.52(3) 4_566 ?
O1 C1 1.290(9) . ?
C1 C2 1.415(18) . ?
C2 C3 1.422(8) . ?
C2 C3 1.422(8) 5 ?
C3 H3 0.9500 . ?
O4 O4 1.75(3) 100_655 ?
O4 O4 1.75(3) 99_565 ?
O4 O4 1.75(3) 98_556 ?
N1S C1S 1.506(10) 28 ?
N1S C1S 1.506(10) . ?
N1S C1S 1.506(10) 51 ?
N1S C1S 1.506(10) 74 ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
O1W O1W 0.86(4) 166 ?
O1W H1WA 0.8637 . ?
O1W H1WB 0.8497 . ?
O2U H2UA 0.96(5) . ?
O2U H2UB 0.95(5) . ?
O2U H2UC 0.96(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
O3 W1 O3 86.8(5) . 6_566 ?
O3 W1 O3 155.7(8) . 103_556 ?
O3 W1 O3 88.2(6) 6_566 103_556 ?
O3 W1 O3 88.2(6) . 99_565 ?
O3 W1 O3 155.7(8) 6_566 99_565 ?
O3 W1 O3 86.8(5) 103_556 99_565 ?
O3 W1 O4 63.7(4) . . ?
O3 W1 O4 63.7(4) 6_566 . ?
O3 W1 O4 92.8(5) 99_565 . ?
O3 W1 O4 63.7(4) 99_565 99_565 ?
O3 W1 O4 92.8(5) 103_556 . ?
O3 W1 O4 92.8(5) . 99_565 ?
O3 W1 O4 92.8(5) 6_566 99_565 ?
O3 W1 O4 63.7(4) 103_556 99_565 ?
O2 W1 O3 102.1(4) . . ?
O2 W1 O3 102.1(4) . 99_565 ?
O2 W1 O3 102.1(4) . 103_556 ?
O2 W1 O3 102.1(4) . 6_566 ?
O2 W1 O4 159.3(5) . 99_565 ?
O2 W1 O4 159.3(5) . . ?
O4 W1 O4 41.4(10) 99_565 . ?
O1 Cu1 Cu1 84.61(19) 166 145_565 ?
O1 Cu1 Cu1 84.61(19) 99_565 145_565 ?
O1 Cu1 Cu1 84.61(19) . 145_565 ?
O1 Cu1 Cu1 84.61(19) 72_565 145_565 ?
O1 Cu1 O1 90.2(4) 166 72_565 ?
O1 Cu1 O1 88.8(4) 99_565 72_565 ?
O1 Cu1 O1 169.2(4) 166 99_565 ?
O1 Cu1 O1 169.2(4) 72_565 . ?
O1 Cu1 O1 88.8(4) 166 . ?
O1 Cu1 O1 90.2(4) 99_565 . ?
O1 Cu1 O1W 87.4(4) 166 . ?
O1 Cu1 O1W 103.2(4) . . ?
O1 Cu1 O1W 87.4(4) 99_565 166 ?
O1 Cu1 O1W 87.4(4) . 166 ?
O1 Cu1 O1W 103.2(4) 166 166 ?
O1 Cu1 O1W 103.2(4) 99_565 . ?
O1 Cu1 O1W 103.2(4) 72_565 166 ?
O1 Cu1 O1W 87.4(4) 72_565 . ?
O1W Cu1 Cu1 168.7(5) 166 145_565 ?
O1W Cu1 Cu1 168.7(5) . 145_565 ?
O1W Cu1 O1W 22.6(10) 166 . ?
O4 P1 O4 109.471(2) . 2_665 ?
O4 P1 O4 70.529(3) 2_665 97_666 ?
O4 P1 O4 180.0(9) . 97_666 ?
O4 P1 O4 109.471(4) 99_565 100_655 ?
O4 P1 O4 180.0(9) 100_655 4_566 ?
O4 P1 O4 109.471(8) . 3_656 ?
O4 P1 O4 109.471(1) 99_565 98_556 ?
O4 P1 O4 70.529(9) 99_565 4_566 ?
O4 P1 O4 70.529(2) 3_656 100_655 ?
O4 P1 O4 109.471(2) 2_665 4_566 ?
O4 P1 O4 109.471(10) 3_656 2_665 ?
O4 P1 O4 70.529(1) 100_655 2_665 ?
O4 P1 O4 109.471(4) 100_655 98_556 ?
O4 P1 O4 109.471(1) 99_565 97_666 ?
O4 P1 O4 70.529(4) . 98_556 ?
O4 P1 O4 70.5 3_656 97_666 ?
O4 P1 O4 109.471(10) 100_655 97_666 ?
O4 P1 O4 70.529(2) 3_656 98_556 ?
O4 P1 O4 180.0(9) 99_565 3_656 ?
O4 P1 O4 70.529(7) 97_666 4_566 ?
O4 P1 O4 180.0(9) 98_556 2_665 ?
O4 P1 O4 109.471(2) 98_556 97_666 ?
O4 P1 O4 70.529(3) . 100_655 ?
O4 P1 O4 109.5 . 4_566 ?
O4 P1 O4 70.529(1) 99_565 2_665 ?
O4 P1 O4 109.471(1) 3_656 4_566 ?
O4 P1 O4 70.529(8) . 99_565 ?
O4 P1 O4 70.529(8) 98_556 4_566 ?
C1 O1 Cu1 123.6(7) . . ?
W1 O3 W1 140.3(7) . 106_565 ?
O1 C1 O1 123.5(12) . 120 ?
O1 C1 C2 118.2(6) 120 . ?
O1 C1 C2 118.2(6) . . ?
C1 C2 C3 120.5(7) . . ?
C1 C2 C3 120.5(7) . 5 ?
C3 C2 C3 118.7(14) . 5 ?
C2 C3 C2 121.3(14) 9 . ?
C2 C3 H3 119.3 . . ?
C2 C3 H3 119.3 9 . ?
W1 O4 W1 91.7(7) . 106_565 ?
W1 O4 W1 91.7(7) . 6_566 ?
W1 O4 W1 91.7(7) 6_566 106_565 ?
P1 O4 W1 124.0(5) . 6_566 ?
P1 O4 W1 124.0(5) . . ?
P1 O4 W1 124.0(5) . 106_565 ?
P1 O4 O4 54.736(3) . 100_655 ?
P1 O4 O4 54.736(3) . 98_556 ?
P1 O4 O4 54.736(2) . 99_565 ?
O4 O4 W1 131.41(16) 100_655 6_566 ?
O4 O4 W1 131.41(16) 99_565 106_565 ?
O4 O4 W1 131.41(16) 98_556 . ?
O4 O4 W1 131.41(16) 98_556 106_565 ?
O4 O4 W1 69.3(5) 100_655 106_565 ?
O4 O4 W1 131.41(16) 100_655 . ?
O4 O4 W1 131.41(17) 99_565 6_566 ?
O4 O4 W1 69.3(5) 98_556 6_566 ?
O4 O4 W1 69.3(5) 99_565 . ?
O4 O4 O4 90.001(4) 100_655 99_565 ?
O4 O4 O4 90.001(3) 100_655 98_556 ?
O4 O4 O4 90.001(2) 99_565 98_556 ?
C1S N1S C1S 109.471(1) 28 . ?
C1S N1S C1S 109.471(1) 51 . ?
C1S N1S C1S 109.471(3) 51 74 ?
C1S N1S C1S 109.471(1) 74 . ?
C1S N1S C1S 109.5 28 51 ?
C1S N1S C1S 109.471(2) 28 74 ?
N1S C1S H1SA 109.5 . . ?
N1S C1S H1SB 109.5 . . ?
N1S C1S H1SC 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
Cu1 O1W H1WA 120.0 . . ?
Cu1 O1W H1WB 120.2 . . ?
O1W O1W Cu1 78.7(5) 166 . ?
O1W O1W H1WA 60.2 166 . ?
O1W O1W H1WB 132.8 166 . ?
H1WA O1W H1WB 119.8 . . ?
H2UA O2U H2UB 105(7) . . ?
H2UA O2U H2UC 105(7) . . ?
H2UB O2U H2UC 105(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C1 O1 4.0(17) . . . 120 ?
Cu1 O1 C1 C2 -174.3(8) . . . . ?
O1 C1 C2 C3 176.2(11) . . . . ?
O1 C1 C2 C3 2.1(18) . . . 5 ?
O1 C1 C2 C3 -2.1(18) 120 . . . ?
O1 C1 C2 C3 -176.2(11) 120 . . 5 ?
O3 W1 O3 W1 53.7(11) 6_566 . . 106_565 ?
O3 W1 O3 W1 -24.5(8) 103_556 . . 106_565 ?
O3 W1 O3 W1 -102.5(8) 99_565 . . 106_565 ?
O2 W1 O3 W1 155.5(8) . . . 106_565 ?
C1 C2 C3 C2 -175.0(9) . . . 9 ?
C3 C2 C3 C2 -1(2) 5 . . 9 ?
O4 W1 O3 W1 -8.4(8) . . . 106_565 ?
O4 W1 O3 W1 -38.9(10) 99_565 . . 106_565 ?
O4 P1 O4 W1 60.000(0) 3_656 . . 106_565 ?
O4 P1 O4 W1 180.000(1) 3_656 . . . ?
O4 P1 O4 W1 -60.0 4_566 . . . ?
O4 P1 O4 W1 60.000(3) 2_665 . . . ?
O4 P1 O4 W1 180.000(1) 4_566 . . 106_565 ?
O4 P1 O4 W1 0.000(1) 100_655 . . 106_565 ?
O4 P1 O4 W1 120.000(1) 98_556 . . 106_565 ?
O4 P1 O4 W1 -60.000(3) 3_656 . . 6_566 ?
O4 P1 O4 W1 120.0 100_655 . . . ?
O4 P1 O4 W1 -120.000(1) 99_565 . . 106_565 ?
O4 P1 O4 W1 -120.000(3) 98_556 . . . ?
O4 P1 O4 W1 60.000(1) 4_566 . . 6_566 ?
O4 P1 O4 W1 120.000(3) 99_565 . . 6_566 ?
O4 P1 O4 W1 -120.000(1) 100_655 . . 6_566 ?
O4 P1 O4 W1 -60.000(1) 2_665 . . 106_565 ?
O4 P1 O4 W1 180.000(0) 2_665 . . 6_566 ?
O4 P1 O4 W1 0.000(1) 99_565 . . . ?
O4 P1 O4 W1 0.000(0) 98_556 . . 6_566 ?
O4 P1 O4 O4 -120.000(1) 99_565 . . 100_655 ?
O4 P1 O4 O4 180.000(2) 4_566 . . 100_655 ?
O4 P1 O4 O4 60.000(2) 3_656 . . 100_655 ?
O4 P1 O4 O4 120.000(1) 99_565 . . 98_556 ?
O4 P1 O4 O4 60.000(2) 2_665 . . 99_565 ?
O4 P1 O4 O4 120.000(1) 100_655 . . 99_565 ?
O4 P1 O4 O4 -120.000(3) 98_556 . . 99_565 ?
O4 P1 O4 O4 -60.000(0) 2_665 . . 100_655 ?
O4 P1 O4 O4 180.000(4) 3_656 . . 99_565 ?
O4 P1 O4 O4 -60.0 3_656 . . 98_556 ?
O4 P1 O4 O4 -120.000(2) 100_655 . . 98_556 ?
O4 P1 O4 O4 180.000(2) 2_665 . . 98_556 ?
O4 P1 O4 O4 60.000(2) 4_566 . . 98_556 ?
O4 P1 O4 O4 -60.000(1) 4_566 . . 99_565 ?
O4 P1 O4 O4 120.000(1) 98_556 . . 100_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT601_w11_final           
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        309 Ang**3
RESPONSE: 
This is a structure of Metal-organic framework containing polyoxometalate cages. 
MOF materials typically possess solvent-accessible voids if PLATON/SQUEEZE 
routine is not applied.
;
####################################################################### 
# 
# 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_w10_a8
_database_code_depnum_ccdc_archive 'CCDC 2249037'
_audit_update_record             
;
2023-03-15 deposited with the CCDC.	2024-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C72H24Cu12O48) (O40 P V2 W10)5- 12*(H2O)@Cu 9*(H2O) 2*(C4 H12 N+) 3*(H3O+) 2*(O)'
_chemical_formula_sum            'C80 H99 Cu12 N2 O114 P V2 W10'
_chemical_formula_weight         5646.44


_vrf_PLAT601_w10_a8              
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        741 Ang**3
RESPONSE: 
This is a structure of Metal-organic framework containing polyoxometalate cages. 
MOF materials typically possess solvent-accessible voids if PLATON/SQUEEZE 
routine is not applied.
  
;


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0011 0.0005 '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 0.1857 0.4707 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0015 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0013 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0229 0.0309 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.1100 0.1867 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -1.1497 2.7769 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'

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

_cell_length_a                   26.2682(12)
_cell_length_b                   26.2682(12)
_cell_length_c                   26.2682(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18126(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7408
_cell_measurement_theta_max      12.592
_cell_measurement_theta_min      2.208

_exptl_crystal_description       bulk
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_F_000             10616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.895
_shelx_estimated_absorpt_T_min   0.833
_shelx_estimated_absorpt_T_max   0.911

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.41328
_diffrn_radiation_type           synchrotron
_diffrn_source                   'synchrotron at Advanced Photo Source'
_diffrn_measurement_device_type  'huber 3-circle'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            87447
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         0.901
_diffrn_reflns_theta_max         13.896
_diffrn_reflns_theta_full        13.896
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             812
_reflns_number_gt                674
_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       ?
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1189P)²+254.9259P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         812
_refine_ls_number_parameters     77
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1911
_refine_ls_wR_factor_gt          0.1709
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.163
_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
W1 W 0.40438(2) 0.500000 0.40438(2) 0.0679(5) Uani 0.8333 4 d S T P . .
V1 V 0.40438(2) 0.500000 0.40438(2) 0.0679(5) Uani 0.1667 4 d S T P . .
Cu1 Cu 0.21451(6) 0.500000 0.28549(6) 0.0643(7) Uani 1 4 d S T P . .
P1 P 0.500000 0.500000 0.500000 0.056(3) Uani 1 48 d S T P . .
O1 O 0.2560(3) 0.4476(3) 0.3177(3) 0.0785(18) Uani 1 1 d . . . . .
O3 O 0.4497(4) 0.5503(4) 0.3793(5) 0.107(4) Uani 1 2 d S T P . .
O2 O 0.3592(4) 0.500000 0.3592(4) 0.100(5) Uani 1 4 d S T P . .
C1 C 0.2976(4) 0.4297(6) 0.2976(4) 0.077(4) Uani 1 2 d S T P . .
C2 C 0.3216(4) 0.3890(5) 0.3216(4) 0.073(3) Uani 1 2 d S T P . .
C3 C 0.3667(4) 0.3667(4) 0.2995(6) 0.075(3) Uani 1 2 d S T P . .
H3 H 0.381799 0.381801 0.270265 0.090 Uiso 1 2 calc R U P . .
O4 O 0.4655(7) 0.5345(7) 0.4655(7) 0.080(9) Uani 0.5 6 d S T P . .
N1S N 0.250000 0.250000 0.250000 0.14(3) Uani 1 24 d DS T P . .
C1S C 0.2169(2) 0.2169(2) 0.2169(2) 0.25(4) Uani 1 6 d DS T P . .
H1SA H 0.238458 0.195379 0.195379 0.380 Uiso 0.1667 1 calc R U P A -1
H1SB H 0.195379 0.195379 0.238458 0.380 Uiso 0.1667 1 calc R U P A -1
H1SC H 0.195379 0.238458 0.195379 0.380 Uiso 0.1667 1 calc R U P A -1
O1W O 0.1467(11) 0.500000 0.3315(11) 0.130(16) Uani 0.5 2 d S T P . .
H1WA H 0.144234 0.479730 0.356634 0.156 Uiso 0.25 1 d R U P B -1
H1WB H 0.122464 0.520270 0.324664 0.156 Uiso 0.25 1 d R U P B -1
O2W O 0.2541(10) 0.500000 0.4247(10) 0.125(9) Uani 0.375 2 d S T P C 1
H H 0.255608 0.528970 0.439003 0.187 Uiso 0.1875 1 d R U P C -1
HA H 0.281598 0.500000 0.407853 0.187 Uiso 0.1875 1 d R U P C -1
O2U O 0.2541(10) 0.500000 0.4247(10) 0.125(9) Uani 0.125 2 d DS T P D 2
H2UA H 0.274(14) 0.529(9) 0.434(10) 0.187 Uiso 0.0625 1 d D U P E 2
H2UB H 0.253(18) 0.500000 0.388(2) 0.187 Uiso 0.125 2 d DS U P F 2
H2UC H 0.274(14) 0.471(9) 0.434(10) 0.187 Uiso 0.0625 1 d D U P G 2
O3W O 0.176(2) 0.500000 0.500000 0.12(2) Uani 0.3334 8 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
W1 O2 1.679(14) . ?
W1 O3 1.896(5) 6_566 ?
W1 O3 1.896(5) 99_565 ?
W1 O3 1.896(5) 103_556 ?
W1 O3 1.896(5) . ?
W1 O4 2.445(17) 99_565 ?
W1 O4 2.445(17) . ?
Cu1 O1 1.950(7) . ?
Cu1 O1 1.950(7) 99_565 ?
Cu1 O1 1.950(7) 166 ?
Cu1 O1 1.950(7) 72_565 ?
Cu1 O1W 2.15(2) . ?
Cu1 O1W 2.15(2) 166 ?
Cu1 Cu1 2.637(4) 145_565 ?
P1 O4 1.57(3) . ?
P1 O4 1.57(3) 99_565 ?
P1 O4 1.57(3) 3_656 ?
P1 O4 1.57(3) 100_655 ?
P1 O4 1.57(3) 98_556 ?
P1 O4 1.57(3) 2_665 ?
P1 O4 1.57(3) 97_666 ?
P1 O4 1.57(3) 4_566 ?
O1 C1 1.301(10) . ?
C1 C2 1.39(2) . ?
C2 C3 1.443(9) . ?
C2 C3 1.443(9) 5 ?
C3 H3 0.9500 . ?
O4 O4 1.81(4) 100_655 ?
O4 O4 1.81(4) 99_565 ?
O4 O4 1.81(4) 98_556 ?
N1S C1S 1.505(10) . ?
N1S C1S 1.505(10) 28 ?
N1S C1S 1.505(10) 74 ?
N1S C1S 1.505(10) 51 ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
O1W O1W 0.81(7) 166 ?
O1W H1WA 0.8510 . ?
O1W H1WB 0.8491 . ?
O2U H2UA 0.96(5) . ?
O2U H2UB 0.96(5) . ?
O2U H2UC 0.96(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
O2 W1 O3 101.5(4) . 6_566 ?
O2 W1 O3 101.5(4) . 99_565 ?
O3 W1 O3 157.0(9) 6_566 99_565 ?
O2 W1 O3 101.5(4) . 103_556 ?
O3 W1 O3 88.2(7) 6_566 103_556 ?
O3 W1 O3 87.2(7) 99_565 103_556 ?
O2 W1 O3 101.5(4) . . ?
O3 W1 O3 87.2(7) 6_566 . ?
O3 W1 O3 88.2(7) 99_565 . ?
O3 W1 O3 157.0(9) 103_556 . ?
O2 W1 O4 158.3(6) . 99_565 ?
O3 W1 O4 94.2(6) 6_566 99_565 ?
O3 W1 O4 63.7(5) 99_565 99_565 ?
O3 W1 O4 63.7(5) 103_556 99_565 ?
O3 W1 O4 94.2(6) . 99_565 ?
O2 W1 O4 158.3(6) . . ?
O3 W1 O4 63.7(5) 6_566 . ?
O3 W1 O4 94.2(6) 99_565 . ?
O3 W1 O4 94.2(6) 103_556 . ?
O3 W1 O4 63.7(5) . . ?
O4 W1 O4 43.5(12) 99_565 . ?
O1 Cu1 O1 89.9(4) . 99_565 ?
O1 Cu1 O1 89.2(4) . 166 ?
O1 Cu1 O1 169.8(4) 99_565 166 ?
O1 Cu1 O1 169.8(4) . 72_565 ?
O1 Cu1 O1 89.2(4) 99_565 72_565 ?
O1 Cu1 O1 89.9(4) 166 72_565 ?
O1 Cu1 O1W 102.7(7) . . ?
O1 Cu1 O1W 102.7(7) 99_565 . ?
O1 Cu1 O1W 87.4(7) 166 . ?
O1 Cu1 O1W 87.4(7) 72_565 . ?
O1 Cu1 O1W 87.4(7) . 166 ?
O1 Cu1 O1W 87.4(7) 99_565 166 ?
O1 Cu1 O1W 102.7(7) 166 166 ?
O1 Cu1 O1W 102.7(7) 72_565 166 ?
O1W Cu1 O1W 21.7(18) . 166 ?
O1 Cu1 Cu1 84.9(2) . 145_565 ?
O1 Cu1 Cu1 84.9(2) 99_565 145_565 ?
O1 Cu1 Cu1 84.9(2) 166 145_565 ?
O1 Cu1 Cu1 84.9(2) 72_565 145_565 ?
O1W Cu1 Cu1 169.2(9) . 145_565 ?
O1W Cu1 Cu1 169.2(9) 166 145_565 ?
O4 P1 O4 70.529(10) . 99_565 ?
O4 P1 O4 109.471(10) . 3_656 ?
O4 P1 O4 180(2) 99_565 3_656 ?
O4 P1 O4 70.529(3) . 100_655 ?
O4 P1 O4 109.471(4) 99_565 100_655 ?
O4 P1 O4 70.529(2) 3_656 100_655 ?
O4 P1 O4 70.529(5) . 98_556 ?
O4 P1 O4 109.471(1) 99_565 98_556 ?
O4 P1 O4 70.529(2) 3_656 98_556 ?
O4 P1 O4 109.471(6) 100_655 98_556 ?
O4 P1 O4 109.471(3) . 2_665 ?
O4 P1 O4 70.529(1) 99_565 2_665 ?
O4 P1 O4 109.471(11) 3_656 2_665 ?
O4 P1 O4 70.529(1) 100_655 2_665 ?
O4 P1 O4 180.0(11) 98_556 2_665 ?
O4 P1 O4 180.0(11) . 97_666 ?
O4 P1 O4 109.471(1) 99_565 97_666 ?
O4 P1 O4 70.5 3_656 97_666 ?
O4 P1 O4 109.471(11) 100_655 97_666 ?
O4 P1 O4 109.471(2) 98_556 97_666 ?
O4 P1 O4 70.529(3) 2_665 97_666 ?
O4 P1 O4 109.471(1) . 4_566 ?
O4 P1 O4 70.529(11) 99_565 4_566 ?
O4 P1 O4 109.471(1) 3_656 4_566 ?
O4 P1 O4 180.0(11) 100_655 4_566 ?
O4 P1 O4 70.529(10) 98_556 4_566 ?
O4 P1 O4 109.471(2) 2_665 4_566 ?
O4 P1 O4 70.529(8) 97_666 4_566 ?
C1 O1 Cu1 123.3(7) . . ?
W1 O3 W1 139.0(8) 106_565 . ?
O1 C1 O1 123.4(13) 120 . ?
O1 C1 C2 118.3(6) 120 . ?
O1 C1 C2 118.3(6) . . ?
C1 C2 C3 120.0(8) . . ?
C1 C2 C3 120.0(8) . 5 ?
C3 C2 C3 119.9(15) . 5 ?
C2 C3 C2 120.1(15) . 9 ?
C2 C3 H3 119.9 . . ?
C2 C3 H3 119.9 9 . ?
P1 O4 O4 54.738(3) . 100_655 ?
P1 O4 O4 54.738(3) . 99_565 ?
O4 O4 O4 90.004(4) 100_655 99_565 ?
P1 O4 O4 54.738(4) . 98_556 ?
O4 O4 O4 90.004(4) 100_655 98_556 ?
O4 O4 O4 90.004(3) 99_565 98_556 ?
P1 O4 W1 123.0(6) . 106_565 ?
O4 O4 W1 68.3(6) 100_655 106_565 ?
O4 O4 W1 131.1(2) 99_565 106_565 ?
O4 O4 W1 131.1(2) 98_556 106_565 ?
P1 O4 W1 123.0(6) . 6_566 ?
O4 O4 W1 131.1(2) 100_655 6_566 ?
O4 O4 W1 131.1(2) 99_565 6_566 ?
O4 O4 W1 68.3(6) 98_556 6_566 ?
W1 O4 W1 93.2(9) 106_565 6_566 ?
P1 O4 W1 123.0(6) . . ?
O4 O4 W1 131.1(2) 100_655 . ?
O4 O4 W1 68.3(6) 99_565 . ?
O4 O4 W1 131.1(2) 98_556 . ?
W1 O4 W1 93.2(9) 106_565 . ?
W1 O4 W1 93.2(9) 6_566 . ?
C1S N1S C1S 109.471(1) . 28 ?
C1S N1S C1S 109.471(1) . 74 ?
C1S N1S C1S 109.471(3) 28 74 ?
C1S N1S C1S 109.471(1) . 51 ?
C1S N1S C1S 109.5 28 51 ?
C1S N1S C1S 109.471(3) 74 51 ?
N1S C1S H1SA 109.5 . . ?
N1S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
N1S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
O1W O1W Cu1 79.2(9) 166 . ?
O1W O1W H1WA 60.3 166 . ?
Cu1 O1W H1WA 119.9 . . ?
O1W O1W H1WB 132.8 166 . ?
Cu1 O1W H1WB 120.1 . . ?
H1WA O1W H1WB 119.9 . . ?
H2UA O2U H2UB 105(7) . . ?
H2UA O2U H2UC 105(7) . . ?
H2UB O2U H2UC 105(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 W1 O3 W1 156.0(10) . . . 106_565 ?
O3 W1 O3 W1 54.8(14) 6_566 . . 106_565 ?
O3 W1 O3 W1 -102.6(9) 99_565 . . 106_565 ?
O3 W1 O3 W1 -24.0(10) 103_556 . . 106_565 ?
O4 W1 O3 W1 -39.2(11) 99_565 . . 106_565 ?
O4 W1 O3 W1 -7.1(10) . . . 106_565 ?
Cu1 O1 C1 O1 5(2) . . . 120 ?
Cu1 O1 C1 C2 -174.0(10) . . . . ?
O1 C1 C2 C3 -2(2) 120 . . . ?
O1 C1 C2 C3 177.5(13) . . . . ?
O1 C1 C2 C3 -177.5(13) 120 . . 5 ?
O1 C1 C2 C3 2(2) . . . 5 ?
C1 C2 C3 C2 -174.3(10) . . . 9 ?
C3 C2 C3 C2 2(3) 5 . . 9 ?
O4 P1 O4 O4 -120.000(3) 99_565 . . 100_655 ?
O4 P1 O4 O4 60.000(1) 3_656 . . 100_655 ?
O4 P1 O4 O4 120.000(1) 98_556 . . 100_655 ?
O4 P1 O4 O4 -60.000(1) 2_665 . . 100_655 ?
O4 P1 O4 O4 180.000(3) 4_566 . . 100_655 ?
O4 P1 O4 O4 180.000(5) 3_656 . . 99_565 ?
O4 P1 O4 O4 120.000(2) 100_655 . . 99_565 ?
O4 P1 O4 O4 -120.000(3) 98_556 . . 99_565 ?
O4 P1 O4 O4 60.000(3) 2_665 . . 99_565 ?
O4 P1 O4 O4 -60.000(2) 4_566 . . 99_565 ?
O4 P1 O4 O4 120.000(1) 99_565 . . 98_556 ?
O4 P1 O4 O4 -60.000(0) 3_656 . . 98_556 ?
O4 P1 O4 O4 -120.000(3) 100_655 . . 98_556 ?
O4 P1 O4 O4 180.000(2) 2_665 . . 98_556 ?
O4 P1 O4 O4 60.000(3) 4_566 . . 98_556 ?
O4 P1 O4 W1 -120.000(0) 99_565 . . 106_565 ?
O4 P1 O4 W1 60.0 3_656 . . 106_565 ?
O4 P1 O4 W1 0.000(1) 100_655 . . 106_565 ?
O4 P1 O4 W1 120.000(1) 98_556 . . 106_565 ?
O4 P1 O4 W1 -60.000(1) 2_665 . . 106_565 ?
O4 P1 O4 W1 180.0 4_566 . . 106_565 ?
O4 P1 O4 W1 120.000(3) 99_565 . . 6_566 ?
O4 P1 O4 W1 -60.000(3) 3_656 . . 6_566 ?
O4 P1 O4 W1 -120.000(1) 100_655 . . 6_566 ?
O4 P1 O4 W1 0.000(1) 98_556 . . 6_566 ?
O4 P1 O4 W1 180.000(0) 2_665 . . 6_566 ?
O4 P1 O4 W1 60.000(1) 4_566 . . 6_566 ?
O4 P1 O4 W1 0.000(1) 99_565 . . . ?
O4 P1 O4 W1 180.000(0) 3_656 . . . ?
O4 P1 O4 W1 120.000(0) 100_655 . . . ?
O4 P1 O4 W1 -120.000(3) 98_556 . . . ?
O4 P1 O4 W1 60.000(4) 2_665 . . . ?
O4 P1 O4 W1 -60.000(0) 4_566 . . . ?

_refine_diff_density_max         1.189
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.210

