# Electronic Supplementary Material (ESI) 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_a2014200_ar624ht_reh10dias
_database_code_depnum_ccdc_archive 'CCDC 2336816'
loop_
_audit_author_name
_audit_author_address
'Leire San Felices'
;Universidad del Pais Vasco UPV EHU
Spain
;
_audit_update_record             
;
2024-05-02 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;


_audit_creation_date             2023-11-30T18:17:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         
'Cu1 O39 P W11, C6 H4 Cu0.5 N O2, O, 4(C H6 N3), C H5 N2.5'
_chemical_formula_sum            'C11 H36 Cu1.50 N16 O42 P W11'
_chemical_formula_weight         3213.19

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.1291(5)
_cell_length_b                   19.1015(7)
_cell_length_c                   20.7513(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.490(4)
_cell_angle_gamma                90
_cell_volume                     5194.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(3)
_cell_measurement_reflns_used    7680
_cell_measurement_theta_min      2.163
_cell_measurement_theta_max      27.819

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prismatic
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.3126
_exptl_crystal_size_mid          0.2396
_exptl_crystal_size_min          0.1993
_exptl_crystal_density_diffrn    4.109
_exptl_crystal_F_000             5690
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -25 10 0.1045
-18 5 5 0.0773
7 17 19 0.0476
17 -3 -11 0.1378
-1 18 -22 0.132
-6 -20 -16 0.1511
2 -3 -29 0.0685


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    24.996
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.35544
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_ambient_temperature      100.0(3)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      -0.0399123
_diffrn_orient_matrix_ub_12      0.0249079
_diffrn_orient_matrix_ub_13      0.0015327
_diffrn_orient_matrix_ub_21      -0.0311805
_diffrn_orient_matrix_ub_22      -0.020553
_diffrn_orient_matrix_ub_23      -0.021804
_diffrn_orient_matrix_ub_31      -0.0191563
_diffrn_orient_matrix_ub_32      -0.0183361
_diffrn_orient_matrix_ub_33      0.0263409
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_number            23098
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.885
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             10213
_reflns_number_gt                6861
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     iterative
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1064P)²+352.9782P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10213
_refine_ls_number_parameters     605
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0869
_refine_ls_wR_factor_ref         0.2437
_refine_ls_wR_factor_gt          0.2104
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         5.832
_refine_diff_density_min         -2.561
_refine_diff_density_rms         0.527

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 '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'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.26877(10) -0.03895(7) 0.36044(6) 0.0459(3) Uani 1 1 d . . . . .
W2 W 0.12275(10) 0.10640(7) 0.32275(8) 0.0520(4) Uani 1 1 d . . . . .
W3 W 0.37371(10) 0.12614(7) 0.36863(7) 0.0483(4) Uani 1 1 d . . . . .
W4 W 0.19375(10) -0.11396(6) 0.20286(6) 0.0425(3) Uani 1 1 d . . . . .
W5 W 0.04711(9) 0.03021(7) 0.16234(7) 0.0481(4) Uani 1 1 d . . . . .
W6 W 0.16293(10) 0.20735(6) 0.17353(8) 0.0504(4) Uani 1 1 d . . . . .
W8 W 0.56720(9) 0.06979(7) 0.26095(7) 0.0479(4) Uani 1 1 d . . . . .
W10 W 0.50222(10) -0.00411(6) 0.11630(6) 0.0434(3) Uani 1 1 d . . . . .
W11 W 0.23012(10) -0.02102(6) 0.06331(6) 0.0402(3) Uani 1 1 d . . . . .
W12 W 0.34600(10) 0.15463(6) 0.07498(6) 0.0412(3) Uani 1 1 d . . . . .
P1 P 0.3061(4) 0.0550(3) 0.2147(3) 0.0135(11) Uani 1 1 d . . . . .
O1T O 0.254(2) -0.0978(13) 0.4207(12) 0.069(7) Uani 1 1 d . . . . .
O2T O 0.018(2) 0.1377(15) 0.3560(15) 0.078(8) Uani 1 1 d . . . . .
O3T O 0.4213(18) 0.1669(12) 0.4366(10) 0.055(6) Uani 1 1 d . . . . .
O4T O 0.1490(16) -0.1976(10) 0.2093(11) 0.052(6) Uani 1 1 d . . . . .
O5T O -0.0796(19) 0.0353(13) 0.1481(15) 0.079(8) Uani 1 1 d . . . . .
O6T O 0.066(2) 0.2689(13) 0.1577(15) 0.076(8) Uani 1 1 d . . . . .
O8T O 0.6864(15) 0.0932(11) 0.2906(10) 0.045(5) Uani 1 1 d . . . . .
O9T O 0.521(2) -0.1849(16) 0.2682(14) 0.090(10) Uani 1 1 d . . . . .
O10T O 0.5812(16) -0.0253(11) 0.0556(10) 0.052(6) Uani 1 1 d . . . . .
O11T O 0.2096(18) -0.0500(10) -0.0148(10) 0.051(6) Uani 1 1 d . . . . .
O12 O 0.1549(17) 0.0136(11) 0.3651(9) 0.050(6) Uani 1 1 d . . . . .
O12T O 0.370(2) 0.1845(10) 0.0031(11) 0.062(7) Uani 1 1 d . . . . .
O13 O 0.3414(17) 0.0346(10) 0.4052(10) 0.046(5) Uani 1 1 d . . . . .
O14 O 0.1927(15) -0.0810(9) 0.2888(10) 0.042(5) Uani 1 1 d . . . . .
O19 O 0.3885(15) -0.0719(8) 0.3222(11) 0.044(5) Uani 1 1 d . U . . .
O23 O 0.2359(17) 0.1480(10) 0.3749(10) 0.049(5) Uani 1 1 d . U . . .
O25 O 0.0587(16) 0.0546(11) 0.2520(11) 0.050(5) Uani 1 1 d . . . . .
O26 O 0.1384(17) 0.1786(11) 0.2604(14) 0.068(7) Uani 1 1 d . . . . .
O37 O 0.3763(15) 0.1978(9) 0.3058(12) 0.052(6) Uani 1 1 d . . . . .
O38 O 0.4872(13) 0.0832(9) 0.3300(8) 0.034(4) Uani 1 1 d . U . . .
O45 O 0.0648(17) -0.0669(10) 0.1861(10) 0.049(5) Uani 1 1 d . U . . .
O49 O 0.3306(15) -0.1259(10) 0.2117(11) 0.049(5) Uani 1 1 d . . . . .
O56 O 0.0881(15) 0.1241(11) 0.1450(11) 0.050(6) Uani 1 1 d . . . . .
O67 O 0.2742(17) 0.2622(10) 0.2036(10) 0.048(5) Uani 1 1 d . . . . .
O78 O 0.5177(16) 0.1563(10) 0.2282(9) 0.042(5) Uani 1 1 d . . . . .
O89 O 0.5713(15) -0.0271(12) 0.2813(9) 0.048(5) Uani 1 1 d . . . . .
O101 O 0.3699(16) -0.0349(9) 0.0843(9) 0.042(5) Uani 1 1 d . U . . .
O102 O 0.4506(15) 0.0880(10) 0.0895(9) 0.041(5) Uani 1 1 d . . . . .
O112 O 0.2551(15) 0.0745(9) 0.0531(10) 0.040(5) Uani 1 1 d . . . . .
O123 O 0.2793(13) 0.0603(10) 0.2856(10) 0.038(5) Uani 1 1 d . . . . .
O411 O 0.2007(15) -0.1054(8) 0.1088(9) 0.037(5) Uani 1 1 d . . . . .
O451 O 0.2268(14) 0.0072(9) 0.1765(10) 0.040(5) Uani 1 1 d . . . . .
O511 O 0.0928(18) 0.0039(10) 0.0828(11) 0.057(6) Uani 1 1 d . . . . .
O612 O 0.2232(17) 0.2047(10) 0.0914(14) 0.067(7) Uani 1 1 d . . . . .
O672 O 0.3024(14) 0.1279(9) 0.1832(9) 0.034(4) Uani 1 1 d . . . . .
O712 O 0.4137(15) 0.2207(8) 0.1284(10) 0.039(5) Uani 1 1 d . . . . .
O810 O 0.5965(16) 0.0439(12) 0.1763(12) 0.055(6) Uani 1 1 d . . . . .
O890 O 0.4103(12) 0.0248(10) 0.2106(10) 0.036(4) Uani 1 1 d . . . . .
O910 O 0.5125(16) -0.0835(9) 0.1658(10) 0.041(5) Uani 1 1 d . . . . .
Cu7 Cu 0.40985(13) 0.22309(8) 0.22267(9) 0.0394(6) Uani 0.450(6) 1 d . . P A 1
Cu9 Cu 0.46277(14) -0.09122(9) 0.25214(9) 0.0365(6) Uani 0.550(6) 1 d . . P B 1
W7 W 0.40985(13) 0.22309(8) 0.22267(9) 0.0394(6) Uani 0.550(6) 1 d . . P A 2
W9 W 0.46277(14) -0.09122(9) 0.25214(9) 0.0365(6) Uani 0.450(6) 1 d . . P B 2
Cu1A Cu 0 0 0.5 0.113(4) Uani 1 2 d S . P . .
O8 O 0.051(2) -0.0924(15) 0.5168(15) 0.082(8) Uiso 1 1 d . . . . .
O9 O 0.182(2) -0.1470(14) 0.5600(14) 0.071(7) Uiso 1 1 d . . . . .
N1 N 0.135(3) 0.024(2) 0.5270(19) 0.087(11) Uiso 1 1 d . . . . .
C2 C 0.191(3) 0.092(2) 0.529(2) 0.085(13) Uiso 1 1 d . . . . .
H2 H 0.153204 0.13315 0.516439 0.102 Uiso 1 1 calc R U . . .
C3 C 0.302(4) 0.101(3) 0.548(3) 0.101(16) Uiso 1 1 d . . . . .
H3 H 0.33675 0.144581 0.550409 0.121 Uiso 1 1 calc R U . . .
C4 C 0.344(4) 0.042(3) 0.560(3) 0.106(17) Uiso 1 1 d . . . . .
H4 H 0.415779 0.040891 0.568289 0.128 Uiso 1 1 calc R U . . .
C5 C 0.292(4) -0.017(3) 0.563(3) 0.098(15) Uiso 1 1 d . . . . .
H5 H 0.329098 -0.05638 0.580193 0.118 Uiso 1 1 calc R U . . .
C6 C 0.201(3) -0.028(2) 0.545(2) 0.073(11) Uiso 1 1 d . . . . .
C7 C 0.133(3) -0.094(2) 0.537(2) 0.067(10) Uiso 1 1 d . . . . .
O1W O 0.459(3) -0.185(2) 0.421(2) 0.132(14) Uiso 1 1 d . . . . .
N1G N 0.363(3) -0.289(2) 0.030(2) 0.108(14) Uiso 1 1 d . . . . .
H1GA H 0.315162 -0.321132 0.029796 0.13 Uiso 1 1 calc R U . . .
H1GB H 0.395775 -0.280854 -0.004899 0.13 Uiso 1 1 calc R U . . .
N2G N 0.454(3) -0.2014(19) 0.080(2) 0.088(11) Uiso 1 1 d . . . . .
H2GA H 0.483807 -0.192753 0.044325 0.105 Uiso 1 1 calc R U . . .
H2GB H 0.46902 -0.176401 0.115038 0.105 Uiso 1 1 calc R U . . .
N3G N 0.338(3) -0.2620(17) 0.1347(17) 0.074(9) Uiso 1 1 d . . . . .
H3GA H 0.289953 -0.293956 0.136257 0.089 Uiso 1 1 calc R U . . .
H3GB H 0.354745 -0.236382 0.168956 0.089 Uiso 1 1 calc R U . . .
C1G C 0.384(3) -0.253(2) 0.082(2) 0.080(12) Uiso 1 1 d . . . . .
N4G N -0.222(2) -0.0860(15) 0.3011(14) 0.055(7) Uiso 1 1 d . . . . .
H4GA H -0.279493 -0.063376 0.293174 0.066 Uiso 1 1 calc R U . . .
H4GB H -0.221661 -0.13199 0.303895 0.066 Uiso 1 1 calc R U . . .
N5G N -0.137(3) 0.0143(17) 0.3045(16) 0.074(9) Uiso 1 1 d . . . . .
H5GA H -0.080113 0.03829 0.308611 0.088 Uiso 1 1 calc R U . . .
H5GB H -0.195914 0.036344 0.297531 0.088 Uiso 1 1 calc R U . . .
N6G N -0.048(3) -0.0835(18) 0.3192(16) 0.073(9) Uiso 1 1 d . . . . .
H6GA H 0.00878 -0.059304 0.323186 0.088 Uiso 1 1 calc R U . . .
H6GB H -0.046536 -0.129487 0.322136 0.088 Uiso 1 1 calc R U . . .
C2G C -0.136(3) -0.051(2) 0.3087(19) 0.062(9) Uiso 1 1 d . . . . .
N7G N -0.093(3) 0.2184(18) -0.0475(17) 0.079(10) Uiso 1 1 d . . . . .
H7GA H -0.138938 0.186018 -0.057521 0.094 Uiso 1 1 calc R U . . .
H7GB H -0.106823 0.262705 -0.05543 0.094 Uiso 1 1 calc R U . . .
N8G N 0.053(4) 0.257(2) 0.001(2) 0.121(15) Uiso 1 1 d . . . . .
H8GA H 0.109627 0.249991 0.025105 0.145 Uiso 1 1 calc R U . . .
H8GB H 0.032279 0.299308 -0.008667 0.145 Uiso 1 1 calc R U . . .
N9G N 0.025(2) 0.1368(15) -0.0070(15) 0.061(8) Uiso 1 1 d . . . . .
H9GA H -0.017021 0.101653 -0.015662 0.073 Uiso 1 1 calc R U . . .
H9GB H 0.086356 0.128751 0.010921 0.073 Uiso 1 1 calc R U . . .
C3G C -0.004(3) 0.200(2) -0.021(2) 0.069(10) Uiso 1 1 d . . . . .
N2 N 0.110(2) 0.3384(16) 0.3284(15) 0.064(8) Uiso 1 1 d . . . . .
H2A H 0.060817 0.369236 0.321349 0.077 Uiso 1 1 calc R U . . .
H2B H 0.103966 0.296154 0.311742 0.077 Uiso 1 1 calc R U . . .
N3 N 0.211(2) 0.4144(13) 0.3907(13) 0.047(6) Uiso 1 1 d . . . . .
H3A H 0.269112 0.422844 0.412155 0.056 Uiso 1 1 calc R U . . .
H3B H 0.16327 0.447134 0.387404 0.056 Uiso 1 1 calc R U . . .
N15G N 0.265(3) 0.308(2) 0.370(2) 0.104(13) Uiso 1 1 d . . . . .
H15A H 0.323364 0.31679 0.391543 0.125 Uiso 1 1 calc R U . . .
H15B H 0.254383 0.266629 0.351936 0.125 Uiso 1 1 calc R U . . .
C5G C 0.194(3) 0.356(2) 0.365(2) 0.076(11) Uiso 1 1 d . . . . .
C4G C -0.235(4) 0.192(3) 0.137(2) 0.18(3) Uiso 1 1 d D U . . .
N12G N -0.206(8) 0.253(4) 0.113(5) 0.20(4) Uiso 0.5 1 d D U P C 1
H12A H -0.230876 0.267042 0.074946 0.243 Uiso 0.5 1 calc R U P C 1
H12B H -0.162101 0.279502 0.135707 0.243 Uiso 0.5 1 calc R U P C 1
N10G N -0.193(8) 0.173(5) 0.193(4) 0.19(4) Uiso 0.5 1 d D U P C 1
H10A H -0.207984 0.132715 0.209795 0.222 Uiso 0.5 1 calc R U P C 1
H10B H -0.148846 0.201391 0.214079 0.222 Uiso 0.5 1 calc R U P C 1
N11G N -0.300(6) 0.152(4) 0.104(4) 0.15(4) Uiso 0.5 1 d D U P C .
H11A H -0.277998 0.118339 0.080122 0.184 Uiso 0.5 1 calc R U P . .
H11B H -0.365984 0.15912 0.106711 0.184 Uiso 0.5 1 calc R U P . .
N13G N -0.274(6) 0.242(4) 0.171(4) 0.14(3) Uiso 0.5 1 d D U P C 2
H13A H -0.233789 0.270742 0.194098 0.163 Uiso 0.5 1 calc R U P C 2
H13B H -0.340817 0.246389 0.171973 0.163 Uiso 0.5 1 calc R U P C 2
N14G N -0.137(4) 0.184(6) 0.134(6) 0.21(4) Uiso 0.5 1 d D U P C 2
H14A H -0.113926 0.149999 0.110161 0.255 Uiso 0.5 1 calc R U P C 2
H14B H -0.094741 0.211342 0.156285 0.255 Uiso 0.5 1 calc R U P C 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O1T 1.70(2) . ?
W1 O12 1.81(3) . ?
W1 O13 1.91(2) . ?
W1 O14 1.917(18) . ?
W1 O19 1.91(2) . ?
W1 O123 2.46(2) . ?
W2 O2T 1.69(2) . ?
W2 O12 2.01(2) . ?
W2 O23 1.95(2) . ?
W2 O25 1.92(2) . ?
W2 O26 1.91(3) . ?
W2 O123 2.406(18) . ?
W3 O3T 1.70(2) . ?
W3 O13 1.963(19) . ?
W3 O23 1.87(2) . ?
W3 O37 1.89(2) . ?
W3 O38 1.918(18) . ?
W3 O123 2.414(18) . ?
W4 O4T 1.711(17) . ?
W4 O14 1.89(2) . ?
W4 O45 1.93(2) . ?
W4 O49 1.81(2) . ?
W4 O411 1.966(19) . ?
W4 O451 2.423(16) . ?
W5 O5T 1.67(2) . ?
W5 O25 1.91(2) . ?
W5 O45 1.93(2) . ?
W5 O56 1.91(2) . ?
W5 O451 2.401(19) . ?
W5 O511 1.86(3) . ?
W6 O6T 1.75(2) . ?
W6 O26 1.93(3) . ?
W6 O56 1.94(2) . ?
W6 O67 1.87(2) . ?
W6 O612 1.92(3) . ?
W6 O672 2.378(18) . ?
W8 O8T 1.71(2) . ?
W8 O38 1.846(19) . ?
W8 O78 1.89(2) . ?
W8 O89 1.90(2) . ?
W8 O810 1.89(2) . ?
W8 O890 2.411(16) . ?
W10 O10T 1.73(2) . ?
W10 O101 1.91(2) . ?
W10 O102 1.95(2) . ?
W10 O810 1.93(2) . ?
W10 O890 2.423(19) . ?
W10 O910 1.833(19) . ?
W11 O11T 1.719(19) . ?
W11 O101 1.88(2) . ?
W11 O112 1.869(17) . ?
W11 O411 1.919(17) . ?
W11 O451 2.41(2) . ?
W11 O511 1.93(3) . ?
W12 O12T 1.64(2) . ?
W12 O102 1.88(2) . ?
W12 O112 1.976(17) . ?
W12 O612 1.92(2) . ?
W12 O672 2.406(18) . ?
W12 O712 1.868(18) . ?
P1 O123 1.53(2) . ?
P1 O451 1.564(17) . ?
P1 O672 1.537(17) . ?
P1 O890 1.493(18) . ?
O9T Cu7 1.98(3) 2_645 ?
O9T Cu9 1.97(3) . ?
O9T W9 1.97(3) . ?
O19 Cu9 1.84(2) . ?
O19 W9 1.84(2) . ?
O37 Cu7 1.87(3) . ?
O37 W7 1.87(3) . ?
O49 Cu9 1.99(2) . ?
O49 W9 1.99(2) . ?
O67 Cu7 1.95(2) . ?
O67 W7 1.95(2) . ?
O78 Cu7 1.90(2) . ?
O78 W7 1.90(2) . ?
O89 Cu9 1.95(2) . ?
O89 W9 1.95(2) . ?
O672 Cu7 2.415(17) . ?
O672 W7 2.415(17) . ?
O712 Cu7 1.96(2) . ?
O712 W7 1.96(2) . ?
O890 W9 2.462(19) . ?
O910 Cu9 1.949(19) . ?
O910 W9 1.949(19) . ?
Cu1A O8 1.91(3) . ?
Cu1A O8 1.91(3) 3_556 ?
Cu1A N1 1.88(4) 3_556 ?
Cu1A N1 1.88(4) . ?
O8 C7 1.13(4) . ?
O9 C7 1.28(4) . ?
N1 C2 1.49(6) . ?
N1 C6 1.36(5) . ?
C2 H2 0.95 . ?
C2 C3 1.50(7) . ?
C3 H3 0.95 . ?
C3 C4 1.27(7) . ?
C4 H4 0.95 . ?
C4 C5 1.32(7) . ?
C5 H5 0.95 . ?
C5 C6 1.25(6) . ?
C6 C7 1.55(6) . ?
N1G H1GA 0.88 . ?
N1G H1GB 0.88 . ?
N1G C1G 1.29(6) . ?
N2G H2GA 0.88 . ?
N2G H2GB 0.88 . ?
N2G C1G 1.34(5) . ?
N3G H3GA 0.88 . ?
N3G H3GB 0.88 . ?
N3G C1G 1.30(5) . ?
N4G H4GA 0.88 . ?
N4G H4GB 0.88 . ?
N4G C2G 1.31(4) . ?
N5G H5GA 0.88 . ?
N5G H5GB 0.88 . ?
N5G C2G 1.26(4) . ?
N6G H6GA 0.88 . ?
N6G H6GB 0.88 . ?
N6G C2G 1.31(5) . ?
N7G H7GA 0.88 . ?
N7G H7GB 0.88 . ?
N7G C3G 1.31(5) . ?
N8G H8GA 0.88 . ?
N8G H8GB 0.88 . ?
N8G C3G 1.36(6) . ?
N9G H9GA 0.88 . ?
N9G H9GB 0.88 . ?
N9G C3G 1.30(5) . ?
N2 H2A 0.88 . ?
N2 H2B 0.88 . ?
N2 C5G 1.34(5) . ?
N3 H3A 0.88 . ?
N3 H3B 0.88 . ?
N3 C5G 1.25(5) . ?
N15G H15A 0.88 . ?
N15G H15B 0.88 . ?
N15G C5G 1.30(5) . ?
C4G N12G 1.321(14) . ?
C4G N10G 1.316(14) . ?
C4G N11G 1.304(13) . ?
C4G N13G 1.312(19) . ?
C4G N14G 1.296(19) . ?
N12G H12A 0.88 . ?
N12G H12B 0.88 . ?
N10G H10A 0.88 . ?
N10G H10B 0.88 . ?
N11G H11A 0.88 . ?
N11G H11B 0.88 . ?
N13G H13A 0.88 . ?
N13G H13B 0.88 . ?
N14G H14A 0.88 . ?
N14G H14B 0.88 . ?

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
O1T W1 O12 101.2(11) . . ?
O1T W1 O13 101.9(11) . . ?
O1T W1 O14 102.4(11) . . ?
O1T W1 O19 102.9(11) . . ?
O1T W1 O123 170.5(10) . . ?
O12 W1 O13 87.4(9) . . ?
O12 W1 O14 83.1(8) . . ?
O12 W1 O19 155.4(8) . . ?
O12 W1 O123 71.6(7) . . ?
O13 W1 O14 155.2(8) . . ?
O13 W1 O19 92.6(8) . . ?
O13 W1 O123 72.2(7) . . ?
O14 W1 O123 83.1(7) . . ?
O19 W1 O14 86.7(8) . . ?
O19 W1 O123 85.0(7) . . ?
O2T W2 O12 106.7(11) . . ?
O2T W2 O23 104.0(12) . . ?
O2T W2 O25 99.5(12) . . ?
O2T W2 O26 98.4(12) . . ?
O2T W2 O123 174.6(11) . . ?
O12 W2 O123 70.0(8) . . ?
O23 W2 O12 89.1(8) . . ?
O23 W2 O123 72.0(7) . . ?
O25 W2 O12 87.2(9) . . ?
O25 W2 O23 156.3(9) . . ?
O25 W2 O123 84.8(8) . . ?
O26 W2 O12 154.6(9) . . ?
O26 W2 O23 88.4(10) . . ?
O26 W2 O25 85.0(10) . . ?
O26 W2 O123 85.3(8) . . ?
O3T W3 O13 99.5(10) . . ?
O3T W3 O23 98.5(10) . . ?
O3T W3 O37 102.7(10) . . ?
O3T W3 O38 106.7(9) . . ?
O3T W3 O123 168.4(9) . . ?
O13 W3 O123 72.5(8) . . ?
O23 W3 O13 86.5(9) . . ?
O23 W3 O37 86.9(9) . . ?
O23 W3 O38 154.7(7) . . ?
O23 W3 O123 73.1(7) . . ?
O37 W3 O13 157.6(9) . . ?
O37 W3 O38 88.5(8) . . ?
O37 W3 O123 85.1(8) . . ?
O38 W3 O13 88.4(8) . . ?
O38 W3 O123 81.8(6) . . ?
O4T W4 O14 102.4(10) . . ?
O4T W4 O45 98.5(9) . . ?
O4T W4 O49 102.6(10) . . ?
O4T W4 O411 101.1(9) . . ?
O4T W4 O451 167.6(9) . . ?
O14 W4 O45 87.6(8) . . ?
O14 W4 O411 155.7(7) . . ?
O14 W4 O451 84.6(8) . . ?
O45 W4 O411 82.9(8) . . ?
O45 W4 O451 71.4(7) . . ?
O49 W4 O14 90.6(9) . . ?
O49 W4 O45 158.7(8) . . ?
O49 W4 O411 90.3(9) . . ?
O49 W4 O451 87.3(8) . . ?
O411 W4 O451 71.1(7) . . ?
O5T W5 O25 100.2(12) . . ?
O5T W5 O45 101.8(11) . . ?
O5T W5 O56 101.6(11) . . ?
O5T W5 O451 172.1(10) . . ?
O5T W5 O511 103.3(13) . . ?
O25 W5 O45 89.1(9) . . ?
O25 W5 O451 84.6(8) . . ?
O45 W5 O451 72.0(7) . . ?
O56 W5 O25 87.0(9) . . ?
O56 W5 O45 156.7(9) . . ?
O56 W5 O451 84.8(7) . . ?
O511 W5 O25 156.5(9) . . ?
O511 W5 O45 85.8(8) . . ?
O511 W5 O56 88.7(9) . . ?
O511 W5 O451 72.0(8) . . ?
O6T W6 O26 101.9(12) . . ?
O6T W6 O56 98.4(11) . . ?
O6T W6 O67 103.2(11) . . ?
O6T W6 O612 100.6(12) . . ?
O6T W6 O672 173.1(11) . . ?
O26 W6 O56 86.6(9) . . ?
O26 W6 O672 84.9(8) . . ?
O56 W6 O672 82.9(7) . . ?
O67 W6 O26 91.1(9) . . ?
O67 W6 O56 158.3(9) . . ?
O67 W6 O612 87.4(10) . . ?
O67 W6 O672 75.4(8) . . ?
O612 W6 O26 157.1(9) . . ?
O612 W6 O56 86.3(10) . . ?
O612 W6 O672 72.6(7) . . ?
O8T W8 O38 103.7(8) . . ?
O8T W8 O78 100.8(9) . . ?
O8T W8 O89 99.4(9) . . ?
O8T W8 O810 99.8(9) . . ?
O8T W8 O890 172.2(8) . . ?
O38 W8 O78 87.6(8) . . ?
O38 W8 O89 88.4(8) . . ?
O38 W8 O810 156.5(8) . . ?
O38 W8 O890 82.8(7) . . ?
O78 W8 O89 159.8(8) . . ?
O78 W8 O890 83.7(7) . . ?
O89 W8 O890 76.2(7) . . ?
O810 W8 O78 88.8(9) . . ?
O810 W8 O89 87.0(9) . . ?
O810 W8 O890 73.8(8) . . ?
O10T W10 O101 104.3(8) . . ?
O10T W10 O102 102.5(10) . . ?
O10T W10 O810 101.1(9) . . ?
O10T W10 O890 172.8(8) . . ?
O10T W10 O910 100.8(10) . . ?
O101 W10 O102 83.5(8) . . ?
O101 W10 O810 154.4(8) . . ?
O101 W10 O890 82.2(7) . . ?
O102 W10 O890 81.0(7) . . ?
O810 W10 O102 87.3(9) . . ?
O810 W10 O890 72.7(8) . . ?
O910 W10 O101 88.5(9) . . ?
O910 W10 O102 156.5(8) . . ?
O910 W10 O810 90.5(10) . . ?
O910 W10 O890 76.1(8) . . ?
O11T W11 O101 105.5(10) . . ?
O11T W11 O112 103.1(9) . . ?
O11T W11 O411 99.7(8) . . ?
O11T W11 O451 168.3(8) . . ?
O11T W11 O511 100.5(10) . . ?
O101 W11 O411 89.5(8) . . ?
O101 W11 O451 83.2(7) . . ?
O101 W11 O511 153.8(9) . . ?
O112 W11 O101 89.3(8) . . ?
O112 W11 O411 156.7(8) . . ?
O112 W11 O451 84.6(7) . . ?
O112 W11 O511 87.5(8) . . ?
O411 W11 O451 72.1(7) . . ?
O411 W11 O511 83.4(8) . . ?
O511 W11 O451 70.6(8) . . ?
O12T W12 O102 101.7(11) . . ?
O12T W12 O112 101.9(9) . . ?
O12T W12 O612 101.3(12) . . ?
O12T W12 O672 171.6(8) . . ?
O12T W12 O712 101.2(9) . . ?
O102 W12 O112 86.4(8) . . ?
O102 W12 O612 156.8(9) . . ?
O102 W12 O672 85.4(7) . . ?
O112 W12 O672 82.9(7) . . ?
O612 W12 O112 85.7(9) . . ?
O612 W12 O672 72.0(9) . . ?
O712 W12 O102 92.6(8) . . ?
O712 W12 O112 156.7(8) . . ?
O712 W12 O612 86.2(10) . . ?
O712 W12 O672 73.8(7) . . ?
O123 P1 O451 109.9(11) . . ?
O123 P1 O672 110.1(10) . . ?
O672 P1 O451 108.1(10) . . ?
O890 P1 O123 110.2(11) . . ?
O890 P1 O451 109.2(10) . . ?
O890 P1 O672 109.3(10) . . ?
Cu9 O9T Cu7 173.9(17) . 2_645 ?
W1 O12 W2 128.2(9) . . ?
W1 O13 W3 125.5(11) . . ?
W4 O14 W1 146.8(12) . . ?
Cu9 O19 W1 152.2(11) . . ?
W9 O19 W1 152.2(11) . . ?
W3 O23 W2 125.3(10) . . ?
W5 O25 W2 150.8(11) . . ?
W2 O26 W6 150.3(12) . . ?
Cu7 O37 W3 146.9(11) . . ?
W7 O37 W3 146.9(11) . . ?
W8 O38 W3 151.3(10) . . ?
W5 O45 W4 125.8(10) . . ?
W4 O49 Cu9 146.5(11) . . ?
W4 O49 W9 146.5(11) . . ?
W5 O56 W6 148.6(12) . . ?
W6 O67 Cu7 122.5(10) . . ?
W6 O67 W7 122.5(10) . . ?
W8 O78 Cu7 147.9(12) . . ?
W8 O78 W7 147.9(12) . . ?
W8 O89 Cu9 122.3(10) . . ?
W8 O89 W9 122.3(10) . . ?
W11 O101 W10 152.8(9) . . ?
W12 O102 W10 153.0(11) . . ?
W11 O112 W12 146.9(11) . . ?
W2 O123 W1 89.8(7) . . ?
W2 O123 W3 89.5(6) . . ?
W3 O123 W1 89.8(6) . . ?
P1 O123 W1 125.3(10) . . ?
P1 O123 W2 125.5(10) . . ?
P1 O123 W3 125.5(10) . . ?
W11 O411 W4 125.5(9) . . ?
W5 O451 W4 90.8(6) . . ?
W5 O451 W11 89.9(6) . . ?
W11 O451 W4 91.2(6) . . ?
P1 O451 W4 124.5(11) . . ?
P1 O451 W5 125.0(11) . . ?
P1 O451 W11 125.0(11) . . ?
W5 O511 W11 127.5(11) . . ?
W12 O612 W6 124.4(12) . . ?
W6 O672 W12 90.6(6) . . ?
W6 O672 Cu7 88.8(6) . . ?
W6 O672 W7 88.8(6) . . ?
W12 O672 Cu7 89.4(6) . . ?
W12 O672 W7 89.4(6) . . ?
P1 O672 W6 128.2(10) . . ?
P1 O672 W12 125.9(10) . . ?
P1 O672 Cu7 122.3(10) . . ?
P1 O672 W7 122.3(10) . . ?
W12 O712 Cu7 124.6(9) . . ?
W12 O712 W7 124.6(9) . . ?
W8 O810 W10 124.4(11) . . ?
W8 O890 W10 88.7(6) . . ?
W8 O890 W9 87.4(6) . . ?
W10 O890 W9 86.3(6) . . ?
P1 O890 W8 126.8(10) . . ?
P1 O890 W10 129.7(11) . . ?
P1 O890 W9 124.4(10) . . ?
W10 O910 Cu9 124.1(10) . . ?
W10 O910 W9 124.1(10) . . ?
O9T Cu7 O672 162.8(9) 2_655 . ?
O37 Cu7 O9T 105.9(10) . 2_655 ?
O37 Cu7 O67 91.3(9) . . ?
O37 Cu7 O78 89.3(8) . . ?
O37 Cu7 O672 87.3(7) . . ?
O37 Cu7 O712 159.5(7) . . ?
O67 Cu7 O9T 95.0(10) . 2_655 ?
O67 Cu7 O672 73.3(7) . . ?
O67 Cu7 O712 83.4(9) . . ?
O78 Cu7 O9T 104.7(10) . 2_655 ?
O78 Cu7 O67 159.3(8) . . ?
O78 Cu7 O672 86.2(7) . . ?
O78 Cu7 O712 88.8(8) . . ?
O712 Cu7 O9T 94.4(10) . 2_655 ?
O712 Cu7 O672 72.2(7) . . ?
O9T Cu9 O49 95.1(10) . . ?
O19 Cu9 O9T 105.6(10) . . ?
O19 Cu9 O49 84.8(8) . . ?
O19 Cu9 O89 92.4(8) . . ?
O19 Cu9 O910 159.4(8) . . ?
O89 Cu9 O9T 104.5(10) . . ?
O89 Cu9 O49 160.3(8) . . ?
O89 Cu9 O910 87.6(9) . . ?
O910 Cu9 O9T 94.3(11) . . ?
O910 Cu9 O49 88.3(9) . . ?
O9T W7 O672 162.8(9) 2_655 . ?
O37 W7 O9T 105.9(10) . 2_655 ?
O37 W7 O67 91.3(9) . . ?
O37 W7 O78 89.3(8) . . ?
O37 W7 O672 87.3(7) . . ?
O37 W7 O712 159.5(7) . . ?
O67 W7 O9T 95.0(10) . 2_655 ?
O67 W7 O672 73.3(7) . . ?
O67 W7 O712 83.4(9) . . ?
O78 W7 O9T 104.7(10) . 2_655 ?
O78 W7 O67 159.3(8) . . ?
O78 W7 O672 86.2(7) . . ?
O78 W7 O712 88.8(8) . . ?
O712 W7 O9T 94.4(10) . 2_655 ?
O712 W7 O672 72.2(7) . . ?
O9T W9 O49 95.1(10) . . ?
O9T W9 O890 167.5(10) . . ?
O19 W9 O9T 105.6(10) . . ?
O19 W9 O49 84.8(8) . . ?
O19 W9 O89 92.4(8) . . ?
O19 W9 O890 86.9(7) . . ?
O19 W9 O910 159.4(8) . . ?
O49 W9 O890 86.2(7) . . ?
O89 W9 O9T 104.5(10) . . ?
O89 W9 O49 160.3(8) . . ?
O89 W9 O890 74.1(7) . . ?
O89 W9 O910 87.6(9) . . ?
O910 W9 O9T 94.3(11) . . ?
O910 W9 O49 88.3(9) . . ?
O910 W9 O890 73.3(7) . . ?
O8 Cu1A O8 180 3_556 . ?
N1 Cu1A O8 82.0(15) 3_556 3_556 ?
N1 Cu1A O8 98.0(15) . 3_556 ?
N1 Cu1A O8 82.0(15) . . ?
N1 Cu1A O8 98.0(15) 3_556 . ?
N1 Cu1A N1 180 . 3_556 ?
C7 O8 Cu1A 114(3) . . ?
C2 N1 Cu1A 133(3) . . ?
C6 N1 Cu1A 118(3) . . ?
C6 N1 C2 109(4) . . ?
N1 C2 H2 117.5 . . ?
N1 C2 C3 125(4) . . ?
C3 C2 H2 117.5 . . ?
C2 C3 H3 124.5 . . ?
C4 C3 C2 111(5) . . ?
C4 C3 H3 124.5 . . ?
C3 C4 H4 118.3 . . ?
C3 C4 C5 123(6) . . ?
C5 C4 H4 118.3 . . ?
C4 C5 H5 116.2 . . ?
C6 C5 C4 128(6) . . ?
C6 C5 H5 116.2 . . ?
N1 C6 C7 102(4) . . ?
C5 C6 N1 123(5) . . ?
C5 C6 C7 134(5) . . ?
O8 C7 O9 127(4) . . ?
O8 C7 C6 123(4) . . ?
O9 C7 C6 109(3) . . ?
H1GA N1G H1GB 120 . . ?
C1G N1G H1GA 120 . . ?
C1G N1G H1GB 120 . . ?
H2GA N2G H2GB 120 . . ?
C1G N2G H2GA 120 . . ?
C1G N2G H2GB 120 . . ?
H3GA N3G H3GB 120 . . ?
C1G N3G H3GA 120 . . ?
C1G N3G H3GB 120 . . ?
N1G C1G N2G 119(5) . . ?
N1G C1G N3G 123(5) . . ?
N3G C1G N2G 118(4) . . ?
H4GA N4G H4GB 120 . . ?
C2G N4G H4GA 120 . . ?
C2G N4G H4GB 120 . . ?
H5GA N5G H5GB 120 . . ?
C2G N5G H5GA 120 . . ?
C2G N5G H5GB 120 . . ?
H6GA N6G H6GB 120 . . ?
C2G N6G H6GA 120 . . ?
C2G N6G H6GB 120 . . ?
N5G C2G N4G 119(4) . . ?
N5G C2G N6G 120(4) . . ?
N6G C2G N4G 121(4) . . ?
H7GA N7G H7GB 120 . . ?
C3G N7G H7GA 120 . . ?
C3G N7G H7GB 120 . . ?
H8GA N8G H8GB 120 . . ?
C3G N8G H8GA 120 . . ?
C3G N8G H8GB 120 . . ?
H9GA N9G H9GB 120 . . ?
C3G N9G H9GA 120 . . ?
C3G N9G H9GB 120 . . ?
N7G C3G N8G 113(4) . . ?
N9G C3G N7G 125(4) . . ?
N9G C3G N8G 121(4) . . ?
H2A N2 H2B 120 . . ?
C5G N2 H2A 120 . . ?
C5G N2 H2B 120 . . ?
H3A N3 H3B 120 . . ?
C5G N3 H3A 120 . . ?
C5G N3 H3B 120 . . ?
H15A N15G H15B 120 . . ?
C5G N15G H15A 120 . . ?
C5G N15G H15B 120 . . ?
N3 C5G N2 125(4) . . ?
N3 C5G N15G 119(4) . . ?
N15G C5G N2 116(4) . . ?
N10G C4G N12G 117(3) . . ?
N11G C4G N12G 121(3) . . ?
N11G C4G N10G 122(3) . . ?
N11G C4G N13G 116(3) . . ?
N14G C4G N11G 121(3) . . ?
N14G C4G N13G 123(3) . . ?
C4G N12G H12A 120 . . ?
C4G N12G H12B 120 . . ?
H12A N12G H12B 120 . . ?
C4G N10G H10A 120 . . ?
C4G N10G H10B 120 . . ?
H10A N10G H10B 120 . . ?
C4G N11G H11A 120 . . ?
C4G N11G H11B 120 . . ?
H11A N11G H11B 120 . . ?
C4G N13G H13A 120 . . ?
C4G N13G H13B 120 . . ?
H13A N13G H13B 120 . . ?
C4G N14G H14A 120 . . ?
C4G N14G H14B 120 . . ?
H14A N14G H14B 120 . . ?

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
W1 O19 Cu9 O9T -134(2) . . . . ?
W1 O19 Cu9 O49 -41(2) . . . . ?
W1 O19 Cu9 O89 120(2) . . . . ?
W1 O19 Cu9 O910 30(4) . . . . ?
W1 O19 W9 O9T -134(2) . . . . ?
W1 O19 W9 O49 -41(2) . . . . ?
W1 O19 W9 O89 120(2) . . . . ?
W1 O19 W9 O890 46(2) . . . . ?
W1 O19 W9 O910 30(4) . . . . ?
W3 O37 Cu7 O9T -135(2) . . . 2_655 ?
W3 O37 Cu7 O67 129(2) . . . . ?
W3 O37 Cu7 O78 -30(2) . . . . ?
W3 O37 Cu7 O672 56(2) . . . . ?
W3 O37 Cu7 O712 54(4) . . . . ?
W3 O37 W7 O9T -135(2) . . . 2_655 ?
W3 O37 W7 O67 129(2) . . . . ?
W3 O37 W7 O78 -30(2) . . . . ?
W3 O37 W7 O672 56(2) . . . . ?
W3 O37 W7 O712 54(4) . . . . ?
O1T W1 O12 W2 167.3(14) . . . . ?
O3T W3 O23 W2 -168.4(15) . . . . ?
O3T W3 O37 Cu7 134(2) . . . . ?
O3T W3 O37 W7 134(2) . . . . ?
O4T W4 O14 W1 126.3(19) . . . . ?
O4T W4 O49 Cu9 -136(2) . . . . ?
O4T W4 O49 W9 -136(2) . . . . ?
O5T W5 O511 W11 -173.6(13) . . . . ?
O6T W6 O67 Cu7 -174.8(14) . . . . ?
O6T W6 O67 W7 -174.8(14) . . . . ?
O8T W8 O38 W3 122(2) . . . . ?
O8T W8 O78 Cu7 -132(2) . . . . ?
O8T W8 O78 W7 -132(2) . . . . ?
O8T W8 O89 Cu9 -173.0(12) . . . . ?
O8T W8 O89 W9 -173.0(12) . . . . ?
O8T W8 O810 W10 169.1(14) . . . . ?
O10T W10 O910 Cu9 168.3(12) . . . . ?
O10T W10 O910 W9 168.3(12) . . . . ?
O11T W11 O101 W10 129(3) . . . . ?
O11T W11 O112 W12 -129(2) . . . . ?
O12T W12 O102 W10 -134(2) . . . . ?
O12T W12 O712 Cu7 175.0(13) . . . . ?
O12T W12 O712 W7 175.0(13) . . . . ?
O13 W1 O12 W2 65.7(13) . . . . ?
O13 W3 O23 W2 -69.3(14) . . . . ?
O13 W3 O37 Cu7 -55(3) . . . . ?
O13 W3 O37 W7 -55(3) . . . . ?
O14 W1 O12 W2 -91.3(13) . . . . ?
O14 W4 O49 Cu9 -34(2) . . . . ?
O14 W4 O49 W9 -34(2) . . . . ?
O19 W1 O12 W2 -25(3) . . . . ?
O23 W3 O37 Cu7 -128(2) . . . . ?
O23 W3 O37 W7 -128(2) . . . . ?
O25 W5 O511 W11 5(3) . . . . ?
O26 W6 O67 Cu7 82.7(13) . . . . ?
O26 W6 O67 W7 82.7(13) . . . . ?
O37 W3 O23 W2 89.2(15) . . . . ?
O38 W3 O23 W2 9(3) . . . . ?
O38 W3 O37 Cu7 27(2) . . . . ?
O38 W3 O37 W7 27(2) . . . . ?
O38 W8 O78 Cu7 -28(2) . . . . ?
O38 W8 O78 W7 -28(2) . . . . ?
O38 W8 O89 Cu9 83.4(12) . . . . ?
O38 W8 O89 W9 83.4(12) . . . . ?
O38 W8 O810 W10 -9(3) . . . . ?
O45 W4 O14 W1 -135.6(19) . . . . ?
O45 W4 O49 Cu9 51(4) . . . . ?
O45 W4 O49 W9 51(4) . . . . ?
O45 W5 O511 W11 -72.5(13) . . . . ?
O49 W4 O14 W1 23(2) . . . . ?
O56 W5 O511 W11 84.8(12) . . . . ?
O56 W6 O67 Cu7 -1(3) . . . . ?
O56 W6 O67 W7 -1(3) . . . . ?
O78 W8 O38 W3 22(2) . . . . ?
O78 W8 O89 Cu9 5(3) . . . . ?
O78 W8 O89 W9 5(3) . . . . ?
O78 W8 O810 W10 -90.1(14) . . . . ?
O89 W8 O38 W3 -139(2) . . . . ?
O89 W8 O78 Cu7 50(4) . . . . ?
O89 W8 O78 W7 50(4) . . . . ?
O89 W8 O810 W10 70.1(14) . . . . ?
O101 W10 O910 Cu9 -87.4(13) . . . . ?
O101 W10 O910 W9 -87.4(13) . . . . ?
O101 W11 O112 W12 -23(2) . . . . ?
O102 W10 O910 Cu9 -18(3) . . . . ?
O102 W10 O910 W9 -18(3) . . . . ?
O102 W12 O712 Cu7 -82.6(13) . . . . ?
O102 W12 O712 W7 -82.6(13) . . . . ?
O112 W11 O101 W10 25(3) . . . . ?
O112 W12 O102 W10 -33(2) . . . . ?
O112 W12 O712 Cu7 4(3) . . . . ?
O112 W12 O712 W7 4(3) . . . . ?
O123 W1 O12 W2 -6.4(11) . . . . ?
O123 W3 O23 W2 3.4(12) . . . . ?
O123 W3 O37 Cu7 -55(2) . . . . ?
O123 W3 O37 W7 -55(2) . . . . ?
O123 P1 O451 W4 -58.9(15) . . . . ?
O123 P1 O451 W5 61.2(15) . . . . ?
O123 P1 O451 W11 -179.7(11) . . . . ?
O123 P1 O672 W6 -57.7(15) . . . . ?
O123 P1 O672 W12 176.3(10) . . . . ?
O123 P1 O672 Cu7 60.1(14) . . . . ?
O123 P1 O672 W7 60.1(14) . . . . ?
O123 P1 O890 W8 -57.2(16) . . . . ?
O123 P1 O890 W10 177.1(11) . . . . ?
O123 P1 O890 W9 59.3(14) . . . . ?
O411 W4 O14 W1 -69(3) . . . . ?
O411 W4 O49 Cu9 122(2) . . . . ?
O411 W4 O49 W9 122(2) . . . . ?
O411 W11 O101 W10 -131(3) . . . . ?
O411 W11 O112 W12 64(3) . . . . ?
O451 W4 O14 W1 -64.0(19) . . . . ?
O451 W4 O49 Cu9 51(2) . . . . ?
O451 W4 O49 W9 51(2) . . . . ?
O451 W5 O511 W11 -0.1(10) . . . . ?
O451 W11 O101 W10 -59(3) . . . . ?
O451 W11 O112 W12 60(2) . . . . ?
O451 P1 O123 W1 59.6(14) . . . . ?
O451 P1 O123 W2 -60.5(15) . . . . ?
O451 P1 O123 W3 179.6(11) . . . . ?
O451 P1 O672 W6 62.4(15) . . . . ?
O451 P1 O672 W12 -63.6(14) . . . . ?
O451 P1 O672 Cu7 -179.9(11) . . . . ?
O451 P1 O672 W7 -179.9(11) . . . . ?
O451 P1 O890 W8 -178.0(12) . . . . ?
O451 P1 O890 W10 56.2(15) . . . . ?
O451 P1 O890 W9 -61.6(15) . . . . ?
O511 W11 O101 W10 -57(4) . . . . ?
O511 W11 O112 W12 131(2) . . . . ?
O612 W6 O67 Cu7 -74.5(13) . . . . ?
O612 W6 O67 W7 -74.5(13) . . . . ?
O612 W12 O102 W10 38(4) . . . . ?
O612 W12 O712 Cu7 74.2(13) . . . . ?
O612 W12 O712 W7 74.2(13) . . . . ?
O672 W6 O67 Cu7 -1.7(11) . . . . ?
O672 W6 O67 W7 -1.7(11) . . . . ?
O672 W12 O102 W10 51(2) . . . . ?
O672 W12 O712 Cu7 1.9(10) . . . . ?
O672 W12 O712 W7 1.9(10) . . . . ?
O672 P1 O123 W1 178.6(10) . . . . ?
O672 P1 O123 W2 58.4(14) . . . . ?
O672 P1 O123 W3 -61.4(14) . . . . ?
O672 P1 O451 W4 -179.1(11) . . . . ?
O672 P1 O451 W5 -59.0(15) . . . . ?
O672 P1 O451 W11 60.1(14) . . . . ?
O672 P1 O890 W8 64.0(15) . . . . ?
O672 P1 O890 W10 -61.8(14) . . . . ?
O672 P1 O890 W9 -179.6(10) . . . . ?
O712 W12 O102 W10 124(2) . . . . ?
O810 W8 O38 W3 -60(3) . . . . ?
O810 W8 O78 Cu7 128(2) . . . . ?
O810 W8 O78 W7 128(2) . . . . ?
O810 W8 O89 Cu9 -73.6(13) . . . . ?
O810 W8 O89 W9 -73.6(13) . . . . ?
O810 W10 O910 Cu9 67.0(13) . . . . ?
O810 W10 O910 W9 67.0(13) . . . . ?
O890 W8 O38 W3 -62(2) . . . . ?
O890 W8 O78 Cu7 55(2) . . . . ?
O890 W8 O78 W7 55(2) . . . . ?
O890 W8 O89 Cu9 0.4(11) . . . . ?
O890 W8 O89 W9 0.4(11) . . . . ?
O890 W8 O810 W10 -6.4(12) . . . . ?
O890 W10 O910 Cu9 -5.1(11) . . . . ?
O890 W10 O910 W9 -5.1(11) . . . . ?
O890 P1 O123 W1 -60.8(14) . . . . ?
O890 P1 O123 W2 179.1(11) . . . . ?
O890 P1 O123 W3 59.2(14) . . . . ?
O890 P1 O451 W4 62.1(16) . . . . ?
O890 P1 O451 W5 -177.8(12) . . . . ?
O890 P1 O451 W11 -58.7(15) . . . . ?
O890 P1 O672 W6 -178.9(11) . . . . ?
O890 P1 O672 W12 55.1(14) . . . . ?
O890 P1 O672 Cu7 -61.1(14) . . . . ?
O890 P1 O672 W7 -61.1(14) . . . . ?
Cu1A O8 C7 O9 171(3) . . . . ?
Cu1A O8 C7 C6 -5(6) . . . . ?
Cu1A N1 C2 C3 -176(4) . . . . ?
Cu1A N1 C6 C5 179(4) . . . . ?
Cu1A N1 C6 C7 -1(4) . . . . ?
O8 Cu1A N1 C2 174(4) . . . . ?
O8 Cu1A N1 C2 -6(4) 3_556 . . . ?
O8 Cu1A N1 C6 179(3) 3_556 . . . ?
O8 Cu1A N1 C6 -1(3) . . . . ?
N1 C2 C3 C4 3(7) . . . . ?
N1 C6 C7 O8 4(6) . . . . ?
N1 C6 C7 O9 -172(4) . . . . ?
C2 N1 C6 C5 3(7) . . . . ?
C2 N1 C6 C7 -177(3) . . . . ?
C2 C3 C4 C5 -7(8) . . . . ?
C3 C4 C5 C6 11(10) . . . . ?
C4 C5 C6 N1 -8(9) . . . . ?
C4 C5 C6 C7 172(5) . . . . ?
C5 C6 C7 O8 -176(6) . . . . ?
C5 C6 C7 O9 8(8) . . . . ?
C6 N1 C2 C3 -1(6) . . . . ?

# start Validation Reply Form
_vrf_PLAT971_a2014200_ar624ht_reh10dias 
;
PROBLEM: Check Calcd Resid. Dens. 0.85Ang From W11 5.82 eA-3
RESPONSE: The crystal used in the sc-XRD measurement 
was previously heated to 423 K, let to air exposure for 1 day and 
cooled down to 100 K for data collection.
All of the structures show large maxima of residual electron
density, which are located close to the W atoms according to the final
difference density map. Large residual maxima in the final Fourier map is a
common fact found in the refinement of polyoxotungstate structures due to the
high absorption of heavy atoms such as W.
;
_vrf_PLAT973_a2014200_ar624ht_reh10dias 
;
PROBLEM: Check Calcd Positive Resid. Density on W11 3.98 eA-3
RESPONSE: The crystal used in the sc-XRD measurement 
was previously heated to 423 K, let to air exposure for 1 day and 
cooled down to 100 K for data collection.
All of the structures show large maxima of residual electron
density, which are located close to the W atoms according to the final
difference density map. Large residual maxima in the final Fourier map is a
common fact found in the refinement of polyoxotungstate structures due to the
high absorption of heavy atoms such as W.
;
_vrf_PLAT234_a2014200_ar624ht_reh10dias 
;
PROBLEM: Large Hirshfeld Difference W7 --O9T_b . 0.30 Ang.
RESPONSE: The crystal used in the sc-XRD measurement 
was previously heated to 423 K let to air exposure for 1 day and 
subsequently cooled to 100 K for data 
collection. In this compound some thermal ellipsoids from
the POM O atoms had to be restricted, 
as indicated in the manuscript. 
This modelling sometimes involves the presence of such incongruities.
;
_vrf_PLAT241_a2014200_ar624ht_reh10dias 
;
PROBLEM: High MainMol Ueq as Compared to Neighbors of O9T Check
RESPONSE: The crystal used in the sc-XRD measurement 
was previously heated to 423 K let to air exposure for 1 day and 
subsequently cooled to 100 K for data 
collection. In this compound some thermal ellipsoids from
the POM O atoms had to be restricted, 
as indicated in the manuscript. 
This modelling sometimes involves the presence of such incongruities.
;
_vrf_PLAT306_a2014200_ar624ht_reh10dias 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check
RESPONSE: No hydrogen atom was added to water molecules and therefore, 
isolated O atoms can be found in the structure.     
This is a common fact found in the refinement of polyoxotungstate structures 
due to the presence of a large amount of heavy atoms such as W.
;
_vrf_PLAT342_a2014200_ar624ht_reh10dias 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.07 Ang.
RESPONSE: The presence of a large amount of heavy atoms such as W and their
high absorption of radiation does not allow the precise location of lighter
atoms like C and therefore low precision bonds can be found in the structure.
;
_vrf_PLAT430_a2014200_ar624ht_reh10dias 
;
PROBLEM: Short Inter D...A Contact O1W ..O712 . 2.70 Ang.
RESPONSE: These two atoms belong to molecules involved in the
formation of a hydrogen bond. Distances below 2.8 Ang. imply that 
the two atoms are not coexisting in the structure; that is, the sum of
their partial occupancies is less than 1.
;
_vrf_PLAT976_a2014200_ar624ht_reh10dias 
;
PROBLEM: Check Calcd Resid. Dens. 1.04Ang From N15G . -1.72 eA-3
RESPONSE: The crystal used in the sc-XRD measurement 
was previously heated to 393 K, let to air exposure for 1 day and 
cooled down to 100 K for data collection.
In this compound some disorder is observed in one of the guanidinium cations
and thus its atomic positions as well as thermal ellipsoids had 
to be restricted, 
as indicated in the manuscript. 
;
# end Validation Reply Form

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_a2014166_ar624ht_100ktras165
_database_code_depnum_ccdc_archive 'CCDC 2336817'
loop_
_audit_author_name
_audit_author_address
'Leire San Felices'
;Universidad del Pais Vasco UPV EHU
Spain
;
_audit_update_record             
;
2024-05-02 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        ?
_chemical_formula_moiety         'Cu1 O39 P W11, C6 H4 Cu0.5 N O2, 5(C H6 N3)'
_chemical_formula_sum            'C11 H34 Cu1.50 N16 O41 P W11'
_chemical_formula_weight         3195.17
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.0736(3)
_cell_length_b                   19.0786(6)
_cell_length_c                   20.5732(7)
_cell_angle_alpha                90
_cell_angle_beta                 93.780(3)
_cell_angle_gamma                90
_cell_volume                     5120.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14269
_cell_measurement_theta_min      2.072
_cell_measurement_theta_max      28.203
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prismatic
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.2518
_exptl_crystal_size_min          0.2351
_exptl_crystal_density_diffrn    4.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5650
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -25 8 0.0745
0 -2 -29 0.0881
-18 5 5 0.0743
5 18 20 0.071
-1 16 -23 0.1422
17 -8 4 0.1297

_exptl_special_details           ?

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    25.356
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47538

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Nova (Mo) X-ray micro-source'
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_source_voltage           50
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      -0.0327133
_diffrn_orient_matrix_ub_12      0.0285901
_diffrn_orient_matrix_ub_13      0.0064369
_diffrn_orient_matrix_ub_21      -0.0391422
_diffrn_orient_matrix_ub_22      -0.0148255
_diffrn_orient_matrix_ub_23      -0.0212723
_diffrn_orient_matrix_ub_31      -0.0188378
_diffrn_orient_matrix_ub_32      -0.018636
_diffrn_orient_matrix_ub_33      0.0264145
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_number            36597
_diffrn_reflns_theta_min         1.561
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             10054
_reflns_number_gt                7458
_reflns_threshold_expression     >2sigma(I)
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   40.00  118.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767 -178.0000  150.0000 78

#__ type_ start__ end____ width___ exp.time_
  2 omega  -40.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -19.0000  120.0000 133

#__ type_ start__ end____ width___ exp.time_
  3 omega   11.00   80.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  -99.0000 -120.0000 69

#__ type_ start__ end____ width___ exp.time_
  4 omega   73.00  100.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   19.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
  5 omega   37.00   90.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000 -150.0000 53

#__ type_ start__ end____ width___ exp.time_
  6 omega   66.00  110.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000  -90.0000 44

#__ type_ start__ end____ width___ exp.time_
  7 omega   41.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767  178.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
  8 omega  -32.00   35.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7767   19.0000   30.0000 67

;
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_diff_density_max         7.727
_refine_diff_density_min         -4.213
_refine_diff_density_rms         0.520
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         10054
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0740
_refine_ls_restrained_S_all      1.014
_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)+(0.0790P)²+476.9914P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.1971

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 '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'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 0.27460(8) -0.04407(6) 0.36120(5) 0.0368(3) Uani 1 1 d . . . . .
W2 W 0.12533(8) 0.10138(6) 0.32615(6) 0.0403(3) Uani 1 1 d . . . . .
W3 W 0.37764(9) 0.12236(6) 0.37255(6) 0.0396(3) Uani 1 1 d . . . . .
W4 W 0.19822(8) -0.11682(5) 0.20125(5) 0.0331(3) Uani 1 1 d . . . . .
W5 W 0.04788(7) 0.02743(5) 0.16341(6) 0.0351(3) Uani 1 1 d . . . . .
W6 W 0.16180(8) 0.20545(5) 0.17648(6) 0.0381(3) Uani 1 1 d . . . . .
W8 W 0.57157(8) 0.06988(6) 0.26246(5) 0.0371(3) Uani 1 1 d . . . . .
W10 W 0.50614(8) -0.00260(5) 0.11535(5) 0.0319(2) Uani 1 1 d . . . . .
W11 W 0.23209(8) -0.02062(5) 0.06214(5) 0.0308(2) Uani 1 1 d . . . . .
W12 W 0.34740(8) 0.15610(5) 0.07629(5) 0.0299(2) Uani 1 1 d . . . . .
P1 P 0.3082(3) 0.0534(2) 0.2158(2) 0.0091(9) Uani 1 1 d . . . . .
O1T O 0.2577(16) -0.1050(11) 0.4212(9) 0.050(5) Uani 1 1 d . . . . .
O2T O 0.0208(16) 0.1288(12) 0.3612(14) 0.068(7) Uani 1 1 d . . . . .
O3T O 0.4298(16) 0.1624(11) 0.4410(9) 0.047(5) Uani 1 1 d . . . . .
O4T O 0.1546(16) -0.2008(9) 0.2045(9) 0.045(5) Uani 1 1 d . . . . .
O5T O -0.0819(13) 0.0309(9) 0.1483(11) 0.048(5) Uani 1 1 d . . . . .
O6T O 0.0653(15) 0.2662(10) 0.1638(12) 0.055(5) Uani 1 1 d . U . . .
O8T O 0.6917(14) 0.0957(9) 0.2935(9) 0.042(5) Uani 1 1 d . . . . .
O9T O 0.524(2) -0.1874(15) 0.2648(12) 0.079(8) Uani 1 1 d . . . . .
O10T O 0.5848(14) -0.0229(10) 0.0548(9) 0.041(4) Uani 1 1 d . . . . .
O11T O 0.2115(15) -0.0484(9) -0.0161(9) 0.042(5) Uani 1 1 d . . . . .
O12 O 0.1526(13) 0.0120(9) 0.3681(9) 0.038(4) Uani 1 1 d . U . . .
O12T O 0.3715(16) 0.1870(9) 0.0018(9) 0.044(5) Uani 1 1 d . . . . .
O13 O 0.3486(15) 0.0291(10) 0.4074(9) 0.045(5) Uani 1 1 d . . . . .
O14 O 0.1975(13) -0.0849(8) 0.2885(9) 0.035(4) Uani 1 1 d . . . . .
O19 O 0.3932(13) -0.0734(9) 0.3243(9) 0.037(4) Uani 1 1 d . U . . .
O23 O 0.2357(16) 0.1432(9) 0.3800(9) 0.043(5) Uani 1 1 d . . . . .
O25 O 0.0610(12) 0.0506(9) 0.2542(10) 0.042(5) Uani 1 1 d . . . . .
O26 O 0.1401(14) 0.1752(9) 0.2622(11) 0.049(5) Uani 1 1 d . . . . .
O37 O 0.3794(13) 0.1932(9) 0.3092(9) 0.037(4) Uani 1 1 d . . . . .
O38 O 0.4949(12) 0.0828(8) 0.3347(8) 0.029(4) Uani 1 1 d . U . . .
O45 O 0.0672(12) -0.0685(9) 0.1866(9) 0.035(4) Uani 1 1 d . U . . .
O49 O 0.3374(14) -0.1269(8) 0.2109(9) 0.035(4) Uani 1 1 d . . . . .
O56 O 0.0876(13) 0.1210(9) 0.1494(9) 0.041(5) Uani 1 1 d . . . . .
O67 O 0.2705(14) 0.2605(8) 0.2084(10) 0.041(5) Uani 1 1 d . . . . .
O78 O 0.5191(12) 0.1587(8) 0.2297(8) 0.029(4) Uani 1 1 d . . . . .
O89 O 0.5745(14) -0.0296(10) 0.2813(8) 0.038(4) Uani 1 1 d . . . . .
O101 O 0.3729(12) -0.0329(9) 0.0800(8) 0.030(4) Uani 1 1 d . U . . .
O102 O 0.4541(12) 0.0904(8) 0.0898(8) 0.027(3) Uani 1 1 d . U . . .
O123 O 0.2821(12) 0.0566(8) 0.2884(8) 0.031(4) Uani 1 1 d . . . . .
O411 O 0.2064(14) -0.1056(8) 0.1077(9) 0.037(4) Uani 1 1 d . . . . .
O451 O 0.2305(11) 0.0059(8) 0.1779(8) 0.028(4) Uani 1 1 d . . . . .
O511 O 0.0915(12) 0.0038(8) 0.0803(9) 0.036(4) Uani 1 1 d . . . . .
O612 O 0.2187(13) 0.2029(8) 0.0925(9) 0.034(4) Uani 1 1 d . U . . .
O672 O 0.3018(12) 0.1271(8) 0.1849(8) 0.028(4) Uani 1 1 d . . . . .
O712 O 0.4170(13) 0.2204(9) 0.1303(9) 0.038(4) Uani 1 1 d . . . . .
O810 O 0.5993(14) 0.0444(9) 0.1758(9) 0.036(4) Uani 1 1 d . . . . .
O890 O 0.4169(12) 0.0246(8) 0.2119(8) 0.027(3) Uani 1 1 d . U . . .
O910 O 0.5184(13) -0.0838(9) 0.1645(9) 0.035(4) Uani 1 1 d . . . . .
O911 O 0.2588(14) 0.0760(9) 0.0549(8) 0.036(4) Uani 1 1 d . . . . .
Cu7 Cu 0.40969(11) 0.22278(7) 0.22562(8) 0.0301(5) Uani 0.449(5) 1 d . . P A 1
Cu9 Cu 0.46818(12) -0.09236(7) 0.25125(8) 0.0284(5) Uani 0.551(5) 1 d . . P B 1
W7 W 0.40969(11) 0.22278(7) 0.22562(8) 0.0301(5) Uani 0.551(5) 1 d . . P A 2
W9 W 0.46818(12) -0.09236(7) 0.25125(8) 0.0284(5) Uani 0.449(5) 1 d . . P B 2
Cu1A Cu 0.000000 0.000000 0.500000 0.078(2) Uani 1 2 d S . P . .
O8A O 0.0519(18) -0.0934(10) 0.5106(11) 0.059(6) Uani 1 1 d . . . . .
O9A O 0.1847(15) -0.1521(9) 0.5536(10) 0.042(4) Uani 1 1 d . . . . .
N1A N 0.144(3) 0.0269(13) 0.5257(14) 0.066(8) Uani 1 1 d . . . . .
C2A C 0.189(3) 0.0894(18) 0.5295(19) 0.082(13) Uani 1 1 d . . . . .
H2A H 0.147891 0.128709 0.516352 0.098 Uiso 1 1 calc R U . . .
C3A C 0.284(4) 0.1022(18) 0.5496(19) 0.083(13) Uani 1 1 d . . . . .
H3A H 0.309345 0.148760 0.554231 0.099 Uiso 1 1 calc R U . . .
C4A C 0.350(4) 0.042(2) 0.5646(14) 0.077(12) Uani 1 1 d . . . . .
H4A H 0.421383 0.047107 0.576963 0.093 Uiso 1 1 calc R U . . .
C5A C 0.303(3) -0.0230(15) 0.5595(12) 0.053(9) Uani 1 1 d . . . . .
H5A H 0.342746 -0.064155 0.567823 0.063 Uiso 1 1 calc R U . . .
C6A C 0.201(2) -0.0293(13) 0.5431(13) 0.047(7) Uani 1 1 d D U . . .
C7A C 0.140(2) -0.0976(12) 0.5354(15) 0.048(7) Uani 1 1 d D . . . .
N1G N 0.633(2) 0.2777(15) -0.0186(14) 0.064(8) Uiso 1 1 d . . . . .
H1GA H 0.682252 0.308650 -0.012824 0.077 Uiso 1 1 calc R U . . .
H1GB H 0.596083 0.265972 0.014178 0.077 Uiso 1 1 calc R U . . .
N2G N 0.543(2) 0.1963(14) -0.0765(14) 0.056(7) Uiso 1 1 d . . . . .
H2GA H 0.531139 0.171150 -0.112052 0.068 Uiso 1 1 calc R U . . .
H2GB H 0.509429 0.187248 -0.041712 0.068 Uiso 1 1 calc R U . . .
N3G N 0.6630(19) 0.2640(13) -0.1241(12) 0.050(6) Uiso 1 1 d . . . . .
H3GA H 0.713280 0.294755 -0.120444 0.060 Uiso 1 1 calc R U . . .
H3GB H 0.647342 0.243566 -0.161774 0.060 Uiso 1 1 calc R U . . .
C1G C 0.613(2) 0.2494(15) -0.0752(14) 0.040(6) Uiso 1 1 d . . . . .
N4G N -0.2172(18) -0.0891(13) 0.2989(11) 0.042(5) Uiso 1 1 d . . . . .
H4GA H -0.217343 -0.135123 0.302038 0.050 Uiso 1 1 calc R U . . .
H4GB H -0.275230 -0.066402 0.290655 0.050 Uiso 1 1 calc R U . . .
N5G N -0.134(2) 0.0150(16) 0.3088(14) 0.069(8) Uiso 1 1 d . . . . .
H5GA H -0.192960 0.037101 0.305210 0.083 Uiso 1 1 calc R U . . .
H5GB H -0.076304 0.038927 0.313910 0.083 Uiso 1 1 calc R U . . .
N6G N -0.045(2) -0.0891(14) 0.3189(12) 0.051(6) Uiso 1 1 d . . . . .
H6GA H -0.045030 -0.135069 0.321963 0.061 Uiso 1 1 calc R U . . .
H6GB H 0.013694 -0.066003 0.324044 0.061 Uiso 1 1 calc R U . . .
C2G C -0.131(2) -0.0547(15) 0.3065(14) 0.043(7) Uiso 1 1 d . . . . .
N7G N -0.094(2) 0.2146(15) -0.0459(13) 0.059(7) Uiso 1 1 d . . . . .
H7GA H -0.111690 0.257919 -0.055851 0.071 Uiso 1 1 calc R U . . .
H7GB H -0.135574 0.179716 -0.056472 0.071 Uiso 1 1 calc R U . . .
N8G N 0.056(3) 0.256(2) -0.0006(18) 0.096(11) Uiso 1 1 d . . . . .
H8GA H 0.036071 0.298336 -0.011160 0.116 Uiso 1 1 calc R U . . .
H8GB H 0.116701 0.248769 0.019825 0.116 Uiso 1 1 calc R U . . .
N9G N 0.0292(19) 0.1354(13) -0.0025(11) 0.045(6) Uiso 1 1 d . . . . .
H9GA H 0.091109 0.128267 0.015839 0.054 Uiso 1 1 calc R U . . .
H9GB H -0.011206 0.099605 -0.012395 0.054 Uiso 1 1 calc R U . . .
C3G C -0.004(2) 0.2019(16) -0.0154(14) 0.047(7) Uiso 1 1 d . . . . .
N10G N 0.664(2) 0.2415(18) 0.1465(15) 0.074(9) Uiso 1 1 d . . . . .
H10A H 0.607472 0.217337 0.151477 0.089 Uiso 1 1 calc R U . . .
H10B H 0.661732 0.287603 0.146061 0.089 Uiso 1 1 calc R U . . .
N11G N 0.831(3) 0.254(2) 0.124(2) 0.110(13) Uiso 1 1 d . . . . .
H11A H 0.890143 0.237129 0.114299 0.133 Uiso 1 1 calc R U . . .
H11B H 0.820261 0.299507 0.124761 0.133 Uiso 1 1 calc R U . . .
N12G N 0.764(3) 0.1448(19) 0.1396(16) 0.083(10) Uiso 1 1 d . . . . .
H12A H 0.711301 0.116872 0.144288 0.099 Uiso 1 1 calc R U . . .
H12B H 0.825020 0.126873 0.134793 0.099 Uiso 1 1 calc R U . . .
C4G C 0.752(3) 0.2082(19) 0.1397(17) 0.058(8) Uiso 1 1 d . . . . .
N13G N 0.1052(19) 0.3349(14) 0.3291(12) 0.048(6) Uiso 1 1 d . . . . .
H13A H 0.093068 0.291905 0.315242 0.058 Uiso 1 1 calc R U . . .
H13B H 0.060062 0.368278 0.319760 0.058 Uiso 1 1 calc R U . . .
N14G N 0.2106(18) 0.4122(12) 0.3904(11) 0.042(5) Uiso 1 1 d . . . . .
H14A H 0.266333 0.418771 0.416041 0.050 Uiso 1 1 calc R U . . .
H14B H 0.167543 0.447002 0.382245 0.050 Uiso 1 1 calc R U . . .
N15G N 0.256(3) 0.2988(19) 0.3769(16) 0.085(10) Uiso 1 1 d . . . . .
H15A H 0.241924 0.256215 0.362405 0.102 Uiso 1 1 calc R U . . .
H15B H 0.313760 0.306971 0.400034 0.102 Uiso 1 1 calc R U . . .
C5G C 0.191(2) 0.3495(14) 0.3641(13) 0.037(6) Uiso 1 1 d . . . . .


_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 O1T 1.719(19) . ?
W1 O12 1.932(19) . ?
W1 O13 1.915(18) . ?
W1 O14 1.914(18) . ?
W1 O19 1.857(17) . ?
W1 O123 2.441(17) . ?
W2 O2T 1.67(2) . ?
W2 O12 1.935(18) . ?
W2 O23 1.932(19) . ?
W2 O25 1.92(2) . ?
W2 O26 1.94(2) . ?
W2 O123 2.397(16) . ?
W3 O3T 1.705(19) . ?
W3 O13 1.96(2) . ?
W3 O23 1.91(2) . ?
W3 O37 1.880(19) . ?
W3 O38 1.919(16) . ?
W3 O123 2.417(16) . ?
W4 O4T 1.703(17) . ?
W4 O14 1.895(19) . ?
W4 O45 1.951(17) . ?
W4 O49 1.828(18) . ?
W4 O411 1.946(18) . ?
W4 O451 2.433(15) . ?
W5 O5T 1.706(17) . ?
W5 O25 1.92(2) . ?
W5 O45 1.904(16) . ?
W5 O56 1.887(17) . ?
W5 O451 2.421(14) . ?
W5 O511 1.893(19) . ?
W6 O6T 1.721(17) . ?
W6 O26 1.90(2) . ?
W6 O56 1.943(17) . ?
W6 O67 1.852(19) . ?
W6 O612 1.927(19) . ?
W6 O672 2.362(16) . ?
W8 O8T 1.728(17) . ?
W8 O38 1.863(15) . ?
W8 O78 1.933(16) . ?
W8 O89 1.937(18) . ?
W8 O810 1.905(18) . ?
W8 O890 2.375(16) . ?
W10 O10T 1.712(18) . ?
W10 O101 1.932(17) . ?
W10 O102 1.960(16) . ?
W10 O810 1.906(19) . ?
W10 O890 2.425(15) . ?
W10 O910 1.851(17) . ?
W11 O11T 1.700(18) . ?
W11 O101 1.868(16) . ?
W11 O411 1.914(16) . ?
W11 O451 2.437(17) . ?
W11 O511 1.956(17) . ?
W11 O911 1.883(17) . ?
W12 O12T 1.690(17) . ?
W12 O102 1.882(16) . ?
W12 O612 1.953(17) . ?
W12 O672 2.415(16) . ?
W12 O712 1.854(17) . ?
W12 O911 1.951(17) . ?
P1 O123 1.555(18) . ?
P1 O451 1.535(16) . ?
P1 O672 1.542(16) . ?
P1 O890 1.531(16) . ?
O9T Cu7 1.92(3) 2_645 ?
O9T Cu9 1.97(3) . ?
O9T W9 1.97(3) . ?
O19 Cu9 1.883(17) . ?
O19 W9 1.883(17) . ?
O37 Cu7 1.876(18) . ?
O37 W7 1.876(18) . ?
O49 Cu9 1.965(18) . ?
O49 W9 1.965(18) . ?
O67 Cu7 1.967(17) . ?
O67 W7 1.967(17) . ?
O78 Cu7 1.879(16) . ?
O78 W7 1.879(16) . ?
O89 Cu9 1.906(19) . ?
O89 W9 1.906(19) . ?
O672 Cu7 2.423(15) . ?
O672 W7 2.423(15) . ?
O712 Cu7 1.970(19) . ?
O712 W7 1.970(19) . ?
O890 W9 2.452(16) . ?
O910 Cu9 1.948(18) . ?
O910 W9 1.948(18) . ?
Cu1A O8A 1.915(19) 3_556 ?
Cu1A O8A 1.915(19) . ?
Cu1A N1A 1.99(3) . ?
Cu1A N1A 1.99(3) 3_556 ?
O8A C7A 1.23(3) . ?
O9A C7A 1.24(3) . ?
N1A C2A 1.33(4) . ?
N1A C6A 1.34(4) . ?
C2A H2A 0.9500 . ?
C2A C3A 1.31(6) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.46(6) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.39(5) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.36(4) . ?
C6A C7A 1.532(19) . ?
N1G H1GA 0.8800 . ?
N1G H1GB 0.8800 . ?
N1G C1G 1.29(4) . ?
N2G H2GA 0.8800 . ?
N2G H2GB 0.8800 . ?
N2G C1G 1.37(4) . ?
N3G H3GA 0.8800 . ?
N3G H3GB 0.8800 . ?
N3G C1G 1.26(3) . ?
N4G H4GA 0.8800 . ?
N4G H4GB 0.8800 . ?
N4G C2G 1.30(4) . ?
N5G H5GA 0.8800 . ?
N5G H5GB 0.8800 . ?
N5G C2G 1.33(4) . ?
N6G H6GA 0.8800 . ?
N6G H6GB 0.8800 . ?
N6G C2G 1.32(4) . ?
N7G H7GA 0.8800 . ?
N7G H7GB 0.8800 . ?
N7G C3G 1.32(4) . ?
N8G H8GA 0.8800 . ?
N8G H8GB 0.8800 . ?
N8G C3G 1.31(5) . ?
N9G H9GA 0.8800 . ?
N9G H9GB 0.8800 . ?
N9G C3G 1.36(4) . ?
N10G H10A 0.8800 . ?
N10G H10B 0.8800 . ?
N10G C4G 1.33(4) . ?
N11G H11A 0.8800 . ?
N11G H11B 0.8800 . ?
N11G C4G 1.40(5) . ?
N12G H12A 0.8800 . ?
N12G H12B 0.8800 . ?
N12G C4G 1.22(4) . ?
N13G H13A 0.8800 . ?
N13G H13B 0.8800 . ?
N13G C5G 1.33(4) . ?
N14G H14A 0.8800 . ?
N14G H14B 0.8800 . ?
N14G C5G 1.33(3) . ?
N15G H15A 0.8800 . ?
N15G H15B 0.8800 . ?
N15G C5G 1.30(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1T W1 O12 100.1(9) . . ?
O1T W1 O13 102.8(9) . . ?
O1T W1 O14 101.5(9) . . ?
O1T W1 O19 103.9(9) . . ?
O1T W1 O123 169.7(8) . . ?
O12 W1 O123 71.1(6) . . ?
O13 W1 O12 87.3(8) . . ?
O13 W1 O123 72.0(7) . . ?
O14 W1 O12 83.6(7) . . ?
O14 W1 O13 155.2(8) . . ?
O14 W1 O123 83.2(6) . . ?
O19 W1 O12 155.8(7) . . ?
O19 W1 O13 90.8(8) . . ?
O19 W1 O14 88.2(8) . . ?
O19 W1 O123 85.3(7) . . ?
O2T W2 O12 102.5(10) . . ?
O2T W2 O23 103.0(10) . . ?
O2T W2 O25 99.3(10) . . ?
O2T W2 O26 100.7(10) . . ?
O2T W2 O123 173.1(11) . . ?
O12 W2 O26 156.4(7) . . ?
O12 W2 O123 72.2(6) . . ?
O23 W2 O12 90.0(7) . . ?
O23 W2 O26 89.2(8) . . ?
O23 W2 O123 73.2(7) . . ?
O25 W2 O12 87.6(7) . . ?
O25 W2 O23 157.6(8) . . ?
O25 W2 O26 84.3(8) . . ?
O25 W2 O123 84.9(6) . . ?
O26 W2 O123 85.1(6) . . ?
O3T W3 O13 100.4(8) . . ?
O3T W3 O23 100.3(9) . . ?
O3T W3 O37 103.2(9) . . ?
O3T W3 O38 103.0(9) . . ?
O3T W3 O123 169.6(8) . . ?
O13 W3 O123 71.8(7) . . ?
O23 W3 O13 86.9(8) . . ?
O23 W3 O38 156.7(7) . . ?
O23 W3 O123 73.0(6) . . ?
O37 W3 O13 156.4(8) . . ?
O37 W3 O23 87.8(7) . . ?
O37 W3 O38 87.4(7) . . ?
O37 W3 O123 84.6(7) . . ?
O38 W3 O13 88.4(7) . . ?
O38 W3 O123 83.9(6) . . ?
O4T W4 O14 104.0(8) . . ?
O4T W4 O45 99.1(8) . . ?
O4T W4 O49 103.3(9) . . ?
O4T W4 O411 100.5(8) . . ?
O4T W4 O451 167.4(7) . . ?
O14 W4 O45 86.3(7) . . ?
O14 W4 O411 154.8(6) . . ?
O14 W4 O451 83.6(6) . . ?
O45 W4 O451 71.1(6) . . ?
O49 W4 O14 89.9(8) . . ?
O49 W4 O45 157.6(7) . . ?
O49 W4 O411 90.0(8) . . ?
O49 W4 O451 86.5(6) . . ?
O411 W4 O45 84.3(8) . . ?
O411 W4 O451 71.2(6) . . ?
O5T W5 O25 101.1(9) . . ?
O5T W5 O45 101.3(7) . . ?
O5T W5 O56 102.5(8) . . ?
O5T W5 O451 171.8(7) . . ?
O5T W5 O511 101.5(9) . . ?
O25 W5 O451 83.9(6) . . ?
O45 W5 O25 88.6(8) . . ?
O45 W5 O451 72.1(6) . . ?
O56 W5 O25 85.6(8) . . ?
O56 W5 O45 156.2(7) . . ?
O56 W5 O451 84.3(6) . . ?
O56 W5 O511 89.1(8) . . ?
O511 W5 O25 157.4(7) . . ?
O511 W5 O45 87.4(7) . . ?
O511 W5 O451 73.6(6) . . ?
O6T W6 O26 101.1(9) . . ?
O6T W6 O56 99.7(9) . . ?
O6T W6 O67 102.1(9) . . ?
O6T W6 O612 101.8(9) . . ?
O6T W6 O672 174.3(9) . . ?
O26 W6 O56 84.9(8) . . ?
O26 W6 O612 156.6(7) . . ?
O26 W6 O672 84.4(6) . . ?
O56 W6 O672 82.3(6) . . ?
O67 W6 O26 90.1(8) . . ?
O67 W6 O56 158.2(7) . . ?
O67 W6 O612 90.0(8) . . ?
O67 W6 O672 76.1(6) . . ?
O612 W6 O56 86.4(8) . . ?
O612 W6 O672 72.9(6) . . ?
O8T W8 O38 101.0(8) . . ?
O8T W8 O78 99.9(7) . . ?
O8T W8 O89 101.5(8) . . ?
O8T W8 O810 101.2(9) . . ?
O8T W8 O890 173.0(8) . . ?
O38 W8 O78 88.0(7) . . ?
O38 W8 O89 88.6(7) . . ?
O38 W8 O810 157.8(7) . . ?
O38 W8 O890 84.9(6) . . ?
O78 W8 O89 158.6(7) . . ?
O78 W8 O890 83.9(6) . . ?
O89 W8 O890 74.7(6) . . ?
O810 W8 O78 89.0(7) . . ?
O810 W8 O89 86.2(7) . . ?
O810 W8 O890 72.9(7) . . ?
O10T W10 O101 103.2(8) . . ?
O10T W10 O102 102.9(8) . . ?
O10T W10 O810 101.1(8) . . ?
O10T W10 O890 171.7(7) . . ?
O10T W10 O910 100.1(8) . . ?
O101 W10 O102 83.2(7) . . ?
O101 W10 O890 84.4(6) . . ?
O102 W10 O890 81.3(6) . . ?
O810 W10 O101 155.2(7) . . ?
O810 W10 O102 86.8(7) . . ?
O810 W10 O890 71.7(6) . . ?
O910 W10 O101 90.0(7) . . ?
O910 W10 O102 156.9(7) . . ?
O910 W10 O810 90.5(7) . . ?
O910 W10 O890 76.1(7) . . ?
O11T W11 O101 103.8(8) . . ?
O11T W11 O411 100.2(8) . . ?
O11T W11 O451 168.5(7) . . ?
O11T W11 O511 99.4(8) . . ?
O11T W11 O911 104.4(8) . . ?
O101 W11 O411 90.0(7) . . ?
O101 W11 O451 84.6(6) . . ?
O101 W11 O511 156.8(7) . . ?
O101 W11 O911 87.3(7) . . ?
O411 W11 O451 71.6(6) . . ?
O411 W11 O511 84.9(7) . . ?
O511 W11 O451 72.3(6) . . ?
O911 W11 O411 155.1(7) . . ?
O911 W11 O451 83.5(6) . . ?
O911 W11 O511 87.9(7) . . ?
O12T W12 O102 100.7(8) . . ?
O12T W12 O612 102.1(8) . . ?
O12T W12 O672 172.2(7) . . ?
O12T W12 O712 101.5(9) . . ?
O12T W12 O911 102.2(8) . . ?
O102 W12 O612 156.6(7) . . ?
O102 W12 O672 86.3(6) . . ?
O102 W12 O911 86.3(7) . . ?
O612 W12 O672 71.3(6) . . ?
O712 W12 O102 91.3(7) . . ?
O712 W12 O612 89.4(7) . . ?
O712 W12 O672 74.8(7) . . ?
O712 W12 O911 156.2(8) . . ?
O911 W12 O612 83.8(7) . . ?
O911 W12 O672 81.4(6) . . ?
O451 P1 O123 109.3(9) . . ?
O451 P1 O672 108.2(9) . . ?
O672 P1 O123 110.6(9) . . ?
O890 P1 O123 109.1(9) . . ?
O890 P1 O451 110.3(9) . . ?
O890 P1 O672 109.3(9) . . ?
Cu7 O9T Cu9 174.7(15) 2_645 . ?
W1 O12 W2 125.7(8) . . ?
W1 O13 W3 125.6(10) . . ?
W4 O14 W1 146.7(10) . . ?
W1 O19 Cu9 151.2(11) . . ?
W1 O19 W9 151.2(11) . . ?
W3 O23 W2 124.1(9) . . ?
W5 O25 W2 151.2(9) . . ?
W6 O26 W2 151.3(10) . . ?
Cu7 O37 W3 149.8(10) . . ?
W7 O37 W3 149.8(10) . . ?
W8 O38 W3 149.6(9) . . ?
W5 O45 W4 126.4(8) . . ?
W4 O49 Cu9 147.5(10) . . ?
W4 O49 W9 147.5(10) . . ?
W5 O56 W6 151.4(10) . . ?
W6 O67 Cu7 122.4(8) . . ?
W6 O67 W7 122.4(8) . . ?
Cu7 O78 W8 146.9(9) . . ?
W7 O78 W8 146.9(9) . . ?
Cu9 O89 W8 123.1(9) . . ?
W9 O89 W8 123.1(9) . . ?
W11 O101 W10 152.8(10) . . ?
W12 O102 W10 152.0(9) . . ?
W2 O123 W1 90.7(6) . . ?
W2 O123 W3 89.8(5) . . ?
W3 O123 W1 90.5(6) . . ?
P1 O123 W1 125.3(9) . . ?
P1 O123 W2 124.8(9) . . ?
P1 O123 W3 124.9(9) . . ?
W11 O411 W4 126.9(9) . . ?
W4 O451 W11 90.3(5) . . ?
W5 O451 W4 90.3(5) . . ?
W5 O451 W11 89.2(5) . . ?
P1 O451 W4 125.8(9) . . ?
P1 O451 W5 125.3(9) . . ?
P1 O451 W11 124.8(9) . . ?
W5 O511 W11 124.9(8) . . ?
W6 O612 W12 123.5(8) . . ?
W6 O672 W12 91.4(6) . . ?
W6 O672 Cu7 88.8(5) . . ?
W6 O672 W7 88.8(5) . . ?
W12 O672 Cu7 88.5(5) . . ?
W12 O672 W7 88.5(5) . . ?
P1 O672 W6 128.9(9) . . ?
P1 O672 W12 125.5(9) . . ?
P1 O672 Cu7 122.0(9) . . ?
P1 O672 W7 122.0(9) . . ?
W12 O712 Cu7 123.9(9) . . ?
W12 O712 W7 123.9(9) . . ?
W8 O810 W10 125.3(9) . . ?
W8 O890 W10 89.7(5) . . ?
W8 O890 W9 88.9(5) . . ?
W10 O890 W9 86.6(5) . . ?
P1 O890 W8 127.8(9) . . ?
P1 O890 W10 128.2(9) . . ?
P1 O890 W9 123.0(8) . . ?
W10 O910 Cu9 123.2(9) . . ?
W10 O910 W9 123.2(9) . . ?
W11 O911 W12 149.3(10) . . ?
O9T Cu7 O67 95.5(9) 2_655 . ?
O9T Cu7 O672 162.6(9) 2_655 . ?
O9T Cu7 O712 94.1(9) 2_655 . ?
O37 Cu7 O9T 107.1(10) . 2_655 ?
O37 Cu7 O67 91.5(8) . . ?
O37 Cu7 O78 88.3(7) . . ?
O37 Cu7 O672 86.4(7) . . ?
O37 Cu7 O712 158.8(7) . . ?
O67 Cu7 O672 72.7(6) . . ?
O67 Cu7 O712 86.2(8) . . ?
O78 Cu7 O9T 103.9(9) . 2_655 ?
O78 Cu7 O67 159.8(7) . . ?
O78 Cu7 O672 87.1(6) . . ?
O78 Cu7 O712 86.7(7) . . ?
O712 Cu7 O672 72.8(6) . . ?
O19 Cu9 O9T 105.8(9) . . ?
O19 Cu9 O49 85.3(8) . . ?
O19 Cu9 O89 91.6(8) . . ?
O19 Cu9 O910 160.0(7) . . ?
O49 Cu9 O9T 93.3(9) . . ?
O89 Cu9 O9T 106.0(9) . . ?
O89 Cu9 O49 160.6(7) . . ?
O89 Cu9 O910 87.8(7) . . ?
O910 Cu9 O9T 93.6(9) . . ?
O910 Cu9 O49 88.7(7) . . ?
O9T W7 O67 95.5(9) 2_655 . ?
O9T W7 O672 162.6(9) 2_655 . ?
O9T W7 O712 94.1(9) 2_655 . ?
O37 W7 O9T 107.1(10) . 2_655 ?
O37 W7 O67 91.5(8) . . ?
O37 W7 O78 88.3(7) . . ?
O37 W7 O672 86.4(7) . . ?
O37 W7 O712 158.8(7) . . ?
O67 W7 O672 72.7(6) . . ?
O67 W7 O712 86.2(8) . . ?
O78 W7 O9T 103.9(9) . 2_655 ?
O78 W7 O67 159.8(7) . . ?
O78 W7 O672 87.1(6) . . ?
O78 W7 O712 86.7(7) . . ?
O712 W7 O672 72.8(6) . . ?
O9T W9 O890 167.4(8) . . ?
O19 W9 O9T 105.8(9) . . ?
O19 W9 O49 85.3(8) . . ?
O19 W9 O89 91.6(8) . . ?
O19 W9 O890 86.8(7) . . ?
O19 W9 O910 160.0(7) . . ?
O49 W9 O9T 93.3(9) . . ?
O49 W9 O890 87.4(6) . . ?
O89 W9 O9T 106.0(9) . . ?
O89 W9 O49 160.6(7) . . ?
O89 W9 O890 73.4(6) . . ?
O89 W9 O910 87.8(7) . . ?
O910 W9 O9T 93.6(9) . . ?
O910 W9 O49 88.7(7) . . ?
O910 W9 O890 73.9(6) . . ?
O8A Cu1A O8A 180.0 3_556 . ?
O8A Cu1A N1A 83.6(10) . . ?
O8A Cu1A N1A 96.4(10) 3_556 . ?
O8A Cu1A N1A 83.6(10) 3_556 3_556 ?
O8A Cu1A N1A 96.4(10) . 3_556 ?
N1A Cu1A N1A 180.0 . 3_556 ?
C7A O8A Cu1A 114.9(18) . . ?
C2A N1A Cu1A 131(3) . . ?
C2A N1A C6A 118(3) . . ?
C6A N1A Cu1A 111(2) . . ?
N1A C2A H2A 116.8 . . ?
C3A C2A N1A 126(4) . . ?
C3A C2A H2A 116.8 . . ?
C2A C3A H3A 121.3 . . ?
C2A C3A C4A 117(3) . . ?
C4A C3A H3A 121.3 . . ?
C3A C4A H4A 122.2 . . ?
C5A C4A C3A 116(4) . . ?
C5A C4A H4A 122.2 . . ?
C4A C5A H5A 119.2 . . ?
C6A C5A C4A 122(3) . . ?
C6A C5A H5A 119.2 . . ?
N1A C6A C5A 121(3) . . ?
N1A C6A C7A 112(2) . . ?
C5A C6A C7A 127(3) . . ?
O8A C7A O9A 126(2) . . ?
O8A C7A C6A 117(2) . . ?
O9A C7A C6A 117(2) . . ?
H1GA N1G H1GB 120.0 . . ?
C1G N1G H1GA 120.0 . . ?
C1G N1G H1GB 120.0 . . ?
H2GA N2G H2GB 120.0 . . ?
C1G N2G H2GA 120.0 . . ?
C1G N2G H2GB 120.0 . . ?
H3GA N3G H3GB 120.0 . . ?
C1G N3G H3GA 120.0 . . ?
C1G N3G H3GB 120.0 . . ?
N1G C1G N2G 115(3) . . ?
N3G C1G N1G 123(3) . . ?
N3G C1G N2G 122(3) . . ?
H4GA N4G H4GB 120.0 . . ?
C2G N4G H4GA 120.0 . . ?
C2G N4G H4GB 120.0 . . ?
H5GA N5G H5GB 120.0 . . ?
C2G N5G H5GA 120.0 . . ?
C2G N5G H5GB 120.0 . . ?
H6GA N6G H6GB 120.0 . . ?
C2G N6G H6GA 120.0 . . ?
C2G N6G H6GB 120.0 . . ?
N4G C2G N5G 119(3) . . ?
N4G C2G N6G 120(3) . . ?
N6G C2G N5G 121(3) . . ?
H7GA N7G H7GB 120.0 . . ?
C3G N7G H7GA 120.0 . . ?
C3G N7G H7GB 120.0 . . ?
H8GA N8G H8GB 120.0 . . ?
C3G N8G H8GA 120.0 . . ?
C3G N8G H8GB 120.0 . . ?
H9GA N9G H9GB 120.0 . . ?
C3G N9G H9GA 120.0 . . ?
C3G N9G H9GB 120.0 . . ?
N7G C3G N9G 122(3) . . ?
N8G C3G N7G 118(3) . . ?
N8G C3G N9G 120(3) . . ?
H10A N10G H10B 120.0 . . ?
C4G N10G H10A 120.0 . . ?
C4G N10G H10B 120.0 . . ?
H11A N11G H11B 120.0 . . ?
C4G N11G H11A 120.0 . . ?
C4G N11G H11B 120.0 . . ?
H12A N12G H12B 120.0 . . ?
C4G N12G H12A 120.0 . . ?
C4G N12G H12B 120.0 . . ?
N10G C4G N11G 112(4) . . ?
N12G C4G N10G 126(4) . . ?
N12G C4G N11G 122(4) . . ?
H13A N13G H13B 120.0 . . ?
C5G N13G H13A 120.0 . . ?
C5G N13G H13B 120.0 . . ?
H14A N14G H14B 120.0 . . ?
C5G N14G H14A 120.0 . . ?
C5G N14G H14B 120.0 . . ?
H15A N15G H15B 120.0 . . ?
C5G N15G H15A 120.0 . . ?
C5G N15G H15B 120.0 . . ?
N13G C5G N14G 123(3) . . ?
N15G C5G N13G 118(3) . . ?
N15G C5G N14G 119(3) . . ?

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
W1 O19 Cu9 O9T -129(2) . . . . ?
W1 O19 Cu9 O49 -37(2) . . . . ?
W1 O19 Cu9 O89 123(2) . . . . ?
W1 O19 Cu9 O910 36(4) . . . . ?
W1 O19 W9 O9T -129(2) . . . . ?
W1 O19 W9 O49 -37(2) . . . . ?
W1 O19 W9 O89 123(2) . . . . ?
W1 O19 W9 O890 50(2) . . . . ?
W1 O19 W9 O910 36(4) . . . . ?
W3 O37 Cu7 O9T -135(2) . . . 2_655 ?
W3 O37 Cu7 O67 128(2) . . . . ?
W3 O37 Cu7 O78 -31(2) . . . . ?
W3 O37 Cu7 O672 56(2) . . . . ?
W3 O37 Cu7 O712 45(3) . . . . ?
W3 O37 W7 O9T -135(2) . . . 2_655 ?
W3 O37 W7 O67 128(2) . . . . ?
W3 O37 W7 O78 -31(2) . . . . ?
W3 O37 W7 O672 56(2) . . . . ?
W3 O37 W7 O712 45(3) . . . . ?
W8 O78 Cu7 O9T 138.6(17) . . . 2_655 ?
W8 O78 Cu7 O37 31.4(17) . . . . ?
W8 O78 Cu7 O67 -58(3) . . . . ?
W8 O78 Cu7 O672 -55.1(17) . . . . ?
W8 O78 Cu7 O712 -128.0(17) . . . . ?
W8 O78 W7 O9T 138.6(17) . . . 2_655 ?
W8 O78 W7 O37 31.4(17) . . . . ?
W8 O78 W7 O67 -58(3) . . . . ?
W8 O78 W7 O672 -55.1(17) . . . . ?
W8 O78 W7 O712 -128.0(17) . . . . ?
O1T W1 O19 Cu9 135(2) . . . . ?
O1T W1 O19 W9 135(2) . . . . ?
O3T W3 O37 Cu7 132(2) . . . . ?
O3T W3 O37 W7 132(2) . . . . ?
O4T W4 O14 W1 125.6(16) . . . . ?
O4T W4 O49 Cu9 -138.0(18) . . . . ?
O4T W4 O49 W9 -138.0(18) . . . . ?
O5T W5 O56 W6 130(2) . . . . ?
O5T W5 O511 W11 -172.1(10) . . . . ?
O6T W6 O26 W2 132(2) . . . . ?
O6T W6 O67 Cu7 -174.5(12) . . . . ?
O6T W6 O67 W7 -174.5(12) . . . . ?
O8T W8 O38 W3 127.7(18) . . . . ?
O10T W10 O910 Cu9 168.6(11) . . . . ?
O10T W10 O910 W9 168.6(11) . . . . ?
O11T W11 O101 W10 136(2) . . . . ?
O11T W11 O911 W12 -127(2) . . . . ?
O12 W1 O19 Cu9 -36(3) . . . . ?
O12 W1 O19 W9 -36(3) . . . . ?
O12T W12 O102 W10 -132.7(19) . . . . ?
O12T W12 O712 Cu7 173.0(11) . . . . ?
O12T W12 O712 W7 173.0(11) . . . . ?
O13 W1 O19 Cu9 -122(2) . . . . ?
O13 W1 O19 W9 -122(2) . . . . ?
O13 W3 O37 Cu7 -51(3) . . . . ?
O13 W3 O37 W7 -51(3) . . . . ?
O14 W1 O19 Cu9 34(2) . . . . ?
O14 W1 O19 W9 34(2) . . . . ?
O14 W4 O49 Cu9 -33.6(18) . . . . ?
O14 W4 O49 W9 -33.6(18) . . . . ?
O23 W3 O37 Cu7 -128(2) . . . . ?
O23 W3 O37 W7 -128(2) . . . . ?
O25 W5 O56 W6 30(2) . . . . ?
O25 W5 O511 W11 9(2) . . . . ?
O26 W6 O67 Cu7 84.2(12) . . . . ?
O26 W6 O67 W7 84.2(12) . . . . ?
O38 W3 O37 Cu7 29(2) . . . . ?
O38 W3 O37 W7 29(2) . . . . ?
O45 W4 O14 W1 -136.0(16) . . . . ?
O45 W4 O49 Cu9 46(3) . . . . ?
O45 W4 O49 W9 46(3) . . . . ?
O45 W5 O56 W6 -46(4) . . . . ?
O45 W5 O511 W11 -71.0(10) . . . . ?
O49 W4 O14 W1 21.9(16) . . . . ?
O56 W5 O511 W11 85.4(10) . . . . ?
O56 W6 O26 W2 33(2) . . . . ?
O56 W6 O67 Cu7 8(3) . . . . ?
O56 W6 O67 W7 8(3) . . . . ?
O67 W6 O26 W2 -125(2) . . . . ?
O78 W8 O38 W3 28.0(18) . . . . ?
O89 W8 O38 W3 -130.8(19) . . . . ?
O101 W10 O910 Cu9 -88.0(11) . . . . ?
O101 W10 O910 W9 -88.0(11) . . . . ?
O101 W11 O911 W12 -24(2) . . . . ?
O102 W10 O910 Cu9 -16(2) . . . . ?
O102 W10 O910 W9 -16(2) . . . . ?
O102 W12 O712 Cu7 -85.8(11) . . . . ?
O102 W12 O712 W7 -85.8(11) . . . . ?
O123 W1 O19 Cu9 -50(2) . . . . ?
O123 W1 O19 W9 -50(2) . . . . ?
O123 W3 O37 Cu7 -55(2) . . . . ?
O123 W3 O37 W7 -55(2) . . . . ?
O123 P1 O451 W4 -58.7(12) . . . . ?
O123 P1 O451 W5 62.5(12) . . . . ?
O123 P1 O451 W11 -179.4(9) . . . . ?
O123 P1 O672 W6 -57.4(13) . . . . ?
O123 P1 O672 W12 174.8(9) . . . . ?
O123 P1 O672 Cu7 60.7(12) . . . . ?
O123 P1 O672 W7 60.7(12) . . . . ?
O123 P1 O890 W8 -57.5(13) . . . . ?
O123 P1 O890 W10 175.6(9) . . . . ?
O123 P1 O890 W9 60.7(12) . . . . ?
O411 W4 O14 W1 -68(2) . . . . ?
O411 W4 O49 Cu9 121.2(18) . . . . ?
O411 W4 O49 W9 121.2(18) . . . . ?
O411 W11 O101 W10 -123(2) . . . . ?
O411 W11 O911 W12 61(3) . . . . ?
O451 W4 O14 W1 -64.5(15) . . . . ?
O451 W4 O49 Cu9 50.0(18) . . . . ?
O451 W4 O49 W9 50.0(18) . . . . ?
O451 W5 O56 W6 -54(2) . . . . ?
O451 W5 O511 W11 1.1(9) . . . . ?
O451 W11 O101 W10 -52(2) . . . . ?
O451 W11 O911 W12 61.3(19) . . . . ?
O451 P1 O123 W1 59.0(12) . . . . ?
O451 P1 O123 W2 -61.8(12) . . . . ?
O451 P1 O123 W3 179.6(9) . . . . ?
O451 P1 O672 W6 62.3(13) . . . . ?
O451 P1 O672 W12 -65.5(12) . . . . ?
O451 P1 O672 Cu7 -179.6(9) . . . . ?
O451 P1 O672 W7 -179.6(9) . . . . ?
O451 P1 O890 W8 -177.6(10) . . . . ?
O451 P1 O890 W10 55.4(13) . . . . ?
O451 P1 O890 W9 -59.4(12) . . . . ?
O511 W5 O56 W6 -128(2) . . . . ?
O511 W11 O101 W10 -46(3) . . . . ?
O511 W11 O911 W12 134(2) . . . . ?
O612 W6 O26 W2 -35(4) . . . . ?
O612 W6 O67 Cu7 -72.4(12) . . . . ?
O612 W6 O67 W7 -72.4(12) . . . . ?
O612 W12 O102 W10 34(3) . . . . ?
O612 W12 O712 Cu7 70.8(11) . . . . ?
O612 W12 O712 W7 70.8(11) . . . . ?
O672 W6 O26 W2 -49(2) . . . . ?
O672 W6 O67 Cu7 0.0(10) . . . . ?
O672 W6 O67 W7 0.0(10) . . . . ?
O672 W12 O102 W10 50.7(19) . . . . ?
O672 W12 O712 Cu7 0.0(9) . . . . ?
O672 W12 O712 W7 0.0(9) . . . . ?
O672 P1 O123 W1 178.0(9) . . . . ?
O672 P1 O123 W2 57.3(12) . . . . ?
O672 P1 O123 W3 -61.4(12) . . . . ?
O672 P1 O451 W4 -179.2(9) . . . . ?
O672 P1 O451 W5 -58.0(13) . . . . ?
O672 P1 O451 W11 60.1(12) . . . . ?
O672 P1 O890 W8 63.6(13) . . . . ?
O672 P1 O890 W10 -63.4(13) . . . . ?
O672 P1 O890 W9 -178.2(9) . . . . ?
O712 W12 O102 W10 125.4(19) . . . . ?
O810 W8 O38 W3 -54(3) . . . . ?
O810 W10 O910 Cu9 67.2(11) . . . . ?
O810 W10 O910 W9 67.2(11) . . . . ?
O890 W8 O38 W3 -56.1(18) . . . . ?
O890 W10 O910 Cu9 -3.8(9) . . . . ?
O890 W10 O910 W9 -3.8(9) . . . . ?
O890 P1 O123 W1 -61.7(12) . . . . ?
O890 P1 O123 W2 177.5(9) . . . . ?
O890 P1 O123 W3 58.9(12) . . . . ?
O890 P1 O451 W4 61.3(12) . . . . ?
O890 P1 O451 W5 -177.5(9) . . . . ?
O890 P1 O451 W11 -59.4(12) . . . . ?
O890 P1 O672 W6 -177.6(10) . . . . ?
O890 P1 O672 W12 54.6(12) . . . . ?
O890 P1 O672 Cu7 -59.4(12) . . . . ?
O890 P1 O672 W7 -59.4(12) . . . . ?
O911 W11 O101 W10 32(2) . . . . ?
O911 W12 O102 W10 -30.9(19) . . . . ?
O911 W12 O712 Cu7 -2(3) . . . . ?
O911 W12 O712 W7 -2(3) . . . . ?
Cu1A O8A C7A O9A 171(3) . . . . ?
Cu1A O8A C7A C6A -10(4) . . . . ?
Cu1A N1A C2A C3A 177(3) . . . . ?
Cu1A N1A C6A C5A 177(2) . . . . ?
Cu1A N1A C6A C7A 2(3) . . . . ?
N1A C2A C3A C4A 5(7) . . . . ?
N1A C6A C7A O8A 5(4) . . . . ?
N1A C6A C7A O9A -176(3) . . . . ?
C2A N1A C6A C5A -4(5) . . . . ?
C2A N1A C6A C7A -179(3) . . . . ?
C2A C3A C4A C5A -4(5) . . . . ?
C3A C4A C5A C6A -1(5) . . . . ?
C4A C5A C6A N1A 6(5) . . . . ?
C4A C5A C6A C7A 179(3) . . . . ?
C5A C6A C7A O8A -169(3) . . . . ?
C5A C6A C7A O9A 9(5) . . . . ?
C6A N1A C2A C3A -1(7) . . . . ?

# start Validation Reply Form
_vrf_PLAT971_a2014166_ar624ht_100ktras165 
;
PROBLEM: Check Calcd Resid. Dens. 0.94Ang From O19 7.50 eA-3
RESPONSE: All of the structures show large maxima of residual electron
density, which are located close to the heavy metal atoms according to 
the final difference density map. Large residual maxima in the final
Fourier map is a common fact found in the refinement of polyoxotungstate 
structures due to the high absorption of heavy atoms such as W or Cu.
It is worth mentioning that the crystal used in the data collection 
was previously heated to 423 K and subsequently cooled down to 100 K.
;
_vrf_PLAT972_a2014166_ar624ht_100ktras165 
;
PROBLEM: Check Calcd Resid. Dens. 0.77Ang From W1 -4.26 eA-3
RESPONSE: All of the structures show large maxima of residual electron
density, which are located close to the heavy metal atoms according to 
the final difference density map. Large residual maxima in the final
Fourier map is a common fact found in the refinement of polyoxotungstate 
structures due to the high absorption of heavy atoms such as W or Cu.
It is worth mentioning that the crystal used in the data collection 
was previously heated to 423 K and subsequently cooled down to 100 K.
;
_vrf_PLAT973_a2014166_ar624ht_100ktras165 
;
PROBLEM: Check Calcd Positive Resid. Density on W4 2.55 eA-3
RESPONSE: All of the structures show large maxima of residual electron
density, which are located close to the heavy metal atoms according to 
the final difference density map. Large residual maxima in the final
Fourier map is a common fact found in the refinement of polyoxotungstate 
structures due to the high absorption of heavy atoms such as W or Cu.
It is worth mentioning that the crystal used in the data collection 
was previously heated to 423 K and subsequently cooled down to 100 K.
;
_vrf_PLAT097_a2014166_ar624ht_100ktras165 
;
PROBLEM: Large Reported Max. (Positive) Residual Density 7.73 eA-3
RESPONSE: All of the structures show large maxima of residual electron
density, which are located close to the heavy metal atoms according to 
the final difference density map. Large residual maxima in the final
Fourier map is a common fact found in the refinement of polyoxotungstate 
structures due to the high absorption of heavy atoms such as W or Cu.
It is worth mentioning that the crystal used in the data collection 
was previously heated to 423 K and subsequently cooled down to 100 K.
;
_vrf_PLAT234_a2014166_ar624ht_100ktras165 
;
PROBLEM: Large Hirshfeld Difference W7 --O9T_b . 0.28 Ang.
RESPONSE: The crystal used in the sc-XRD measurement 
was previously heated to 423 K and subsequently cooled to 100 K for data 
collection. In this compound some thermal ellipsoids from
the POm O atoms had to be restricted, 
as indicated in the manuscript. 
This modelling sometimes involves the presence of such incongruities.
;
_vrf_PLAT241_a2014166_ar624ht_100ktras165 
;
PROBLEM: High MainMol Ueq as Compared to Neighbors of O9T Check
RESPONSE: The crystal used in the sc-XRD measurement 
was previously heated to 423 K and subsequently cooled to 100 K for data 
collection. In this compound some thermal ellipsoids from
the POm O atoms had to be restricted, 
as indicated in the manuscript. 
This modelling sometimes involves the presence of such incongruities.
;
_vrf_PLAT342_a2014166_ar624ht_100ktras165 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.05 Ang.
RESPONSE: The presence of a large amount of heavy atoms such as W and their
high absorption of radiation does not allow the precise location of lighter
atoms like C and therefore low precision bonds can be found in the structure.
;
# end Validation Reply Form

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF

####################################################################### 
# 
# 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_b20240088_p2agudumo_auto
_database_code_depnum_ccdc_archive 'CCDC 2336818'
loop_
_audit_author_name
_audit_author_address
'Leire San Felices'
;Universidad del Pais Vasco UPV EHU
Spain
;
_audit_update_record             
;
2024-05-02 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;


_audit_creation_date             2024-05-02T12:57:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         
'C6 H4 Cu1.5 N O42 P W11, 5(O), 4.5(C H6 N3), C0.5 H2.5 N1.5'
_chemical_formula_sum            'C11 H46 Cu1.50 N16 O47 P W11'
_chemical_formula_weight         3303.27

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.96551(18)
_cell_length_b                   21.5917(3)
_cell_length_c                   22.2169(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.8906(14)
_cell_angle_gamma                90
_cell_volume                     5726.65(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.15
_cell_measurement_reflns_used    46463
_cell_measurement_theta_min      2.055
_cell_measurement_theta_max      30.038

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prismatic
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.063
_exptl_crystal_density_diffrn    3.831
_exptl_crystal_F_000             5890
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-16 3 -7 0.0352
9 23 12 0.069
-10 25 3 0.0674
-5 4 -29 0.0318
-7 -2 29 0.0345
4 -4 30 0.0306
17 -3 4 0.0296
9 2 -28 0.0327
-16 -3 -8 0.0339
9 -25 -1 0.0561
-5 -27 -8 0.0577


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    22.685
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
        Numerical absorption correction based on gaussian integration over
        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.069
_exptl_absorpt_correction_T_max  0.374

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_ambient_temperature      150.15
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      0.0141268
_diffrn_orient_matrix_ub_12      0.0182367
_diffrn_orient_matrix_ub_13      -0.0249297
_diffrn_orient_matrix_ub_21      0.002553
_diffrn_orient_matrix_ub_22      -0.0271334
_diffrn_orient_matrix_ub_23      -0.0178547
_diffrn_orient_matrix_ub_31      -0.0576562
_diffrn_orient_matrix_ub_32      0.0032693
_diffrn_orient_matrix_ub_33      -0.0091307
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_number            71075
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.886
_diffrn_reflns_theta_max         26.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_Friedel_coverage         0
_reflns_number_total             11677
_reflns_number_gt                10170
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     iterative
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0107P)²+64.5108P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         11677
_refine_ls_number_parameters     761
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.032
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.198

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 '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'
W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.35151(3) 0.53180(2) 0.64725(2) 0.02315(7) Uani 1 1 d . . . . .
W3 W 0.22379(3) 0.67218(2) 0.62763(2) 0.02482(12) Uani 0.921(2) 1 d . . P . .
Cu3 Cu 0.22379(3) 0.67218(2) 0.62763(2) 0.02482(12) Uani 0.079(2) 1 d . . P . .
W2 W 0.48110(3) 0.66212(2) 0.70513(2) 0.02438(12) Uani 0.952(2) 1 d . . P . .
Cu2 Cu 0.48110(3) 0.66212(2) 0.70513(2) 0.02438(12) Uani 0.048(2) 1 d . . P . .
W8 W -0.02779(3) 0.61058(2) 0.69299(2) 0.02528(13) Uani 0.814(2) 1 d . . P . .
Cu8 Cu -0.02779(3) 0.61058(2) 0.69299(2) 0.02528(13) Uani 0.186(2) 1 d . . P .
.
W7 W 0.10955(3) 0.75052(2) 0.75711(2) 0.02447(12) Uani 0.894(2) 1 d . . P . .
Cu7 Cu 0.10955(3) 0.75052(2) 0.75711(2) 0.02447(12) Uani 0.106(2) 1 d . . P . .
W6 W 0.36506(3) 0.74017(2) 0.83497(2) 0.02322(11) Uani 0.968(2) 1 d . . P . .
Cu6 Cu 0.36506(3) 0.74017(2) 0.83497(2) 0.02322(11) Uani 0.032(2) 1 d . . P . .
W5 W 0.50281(3) 0.58707(2) 0.85505(2) 0.02225(12) Uani 0.921(2) 1 d . . P . .
Cu5 Cu 0.50281(3) 0.58707(2) 0.85505(2) 0.02225(12) Uani 0.079(2) 1 d . . P . .
W4 W 0.37082(3) 0.45713(2) 0.79748(2) 0.02125(12) Uani 0.910(2) 1 d . . P . .
Cu4 Cu 0.37082(3) 0.45713(2) 0.79748(2) 0.02125(12) Uani 0.090(2) 1 d . . P . .
W9 W 0.09859(3) 0.47099(2) 0.71176(2) 0.02198(13) Uani 0.816(2) 1 d . . P . .
Cu9 Cu 0.09859(3) 0.47099(2) 0.71176(2) 0.02198(13) Uani 0.184(2) 1 d . . P . .
W10 W -0.00601(3) 0.54351(2) 0.83232(2) 0.02309(12) Uani 0.958(2) 1 d . . P . .
Cu10 Cu -0.00601(3) 0.54351(2) 0.83232(2) 0.02309(12) Uani 0.042(2) 1 d . . P .
.
W12 W 0.13175(3) 0.68389(2) 0.89694(2) 0.02196(12) Uani 0.916(2) 1 d . . P . .
Cu12 Cu 0.13175(3) 0.68389(2) 0.89694(2) 0.02196(12) Uani 0.084(2) 1 d . . P .
.
W11 W 0.26860(3) 0.53206(2) 0.91813(2) 0.02161(12) Uani 0.930(2) 1 d . . P . .
Cu11 Cu 0.26860(3) 0.53206(2) 0.91813(2) 0.02161(12) Uani 0.070(2) 1 d . . P .
.
Cu1A Cu 0.5 0.5 0.5 0.0229(3) Uani 1 2 d S . P . .
P1 P 0.23969(15) 0.60325(9) 0.77340(8) 0.0157(4) Uani 1 1 d . . . . .
O1T O 0.3992(5) 0.4826(3) 0.5939(2) 0.0265(12) Uani 1 1 d . . . . .
O8A O 0.5427(5) 0.5839(3) 0.5235(3) 0.0277(13) Uani 1 1 d . . . . .
O3T O 0.1939(6) 0.7134(3) 0.5622(3) 0.0416(16) Uani 1 1 d . . . . .
O9A O 0.4817(6) 0.6807(3) 0.5184(3) 0.0455(17) Uani 1 1 d . . . . .
O2T O 0.6057(5) 0.6944(3) 0.6871(3) 0.0404(16) Uani 1 1 d . . . . .
O8T O -0.1506(6) 0.6284(3) 0.6495(3) 0.0481(18) Uani 1 1 d . . . . .
O7T O 0.0401(5) 0.8182(3) 0.7356(3) 0.0377(15) Uani 1 1 d . . . . .
O6T O 0.4497(5) 0.7998(3) 0.8610(3) 0.0321(14) Uani 1 1 d . . . . .
O5T O 0.6364(5) 0.5935(3) 0.8894(3) 0.0400(16) Uani 1 1 d . . . . .
O4T O 0.4281(5) 0.3829(3) 0.7957(3) 0.0336(14) Uani 1 1 d . . . . .
O9T O 0.0557(5) 0.4016(3) 0.6769(3) 0.0415(16) Uani 1 1 d . . . . .
O10T O -0.1107(5) 0.5192(3) 0.8751(3) 0.0359(15) Uani 1 1 d . . . . .
O12T O 0.0714(5) 0.7093(3) 0.9611(3) 0.0358(14) Uani 1 1 d . . . . .
O11T O 0.2579(5) 0.5030(3) 0.9894(3) 0.0367(15) Uani 1 1 d . . . . .
O13 O 0.2820(5) 0.5951(3) 0.5982(2) 0.0285(13) Uani 1 1 d . . . . .
O23 O 0.3795(5) 0.6957(3) 0.6449(3) 0.0293(13) Uani 1 1 d . . . . .
O12 O 0.4784(4) 0.5866(3) 0.6602(3) 0.0265(12) Uani 1 1 d . . . . .
O38 O 0.0867(5) 0.6323(3) 0.6408(2) 0.0302(13) Uani 1 1 d . . . . .
O37 O 0.1876(5) 0.7316(2) 0.6868(3) 0.0281(13) Uani 1 1 d . . . . .
O26 O 0.4267(5) 0.7208(3) 0.7611(3) 0.0290(13) Uani 1 1 d . . . . .
O25 O 0.5246(5) 0.6132(3) 0.7751(3) 0.0282(13) Uani 1 1 d . . . . .
O14 O 0.4024(4) 0.4899(3) 0.7203(2) 0.0253(12) Uani 1 1 d . . . . .
O19 O 0.2085(4) 0.4989(3) 0.6587(2) 0.0244(12) Uani 1 1 d . . . . .
O78 O 0.0057(4) 0.6884(3) 0.7332(3) 0.0285(13) Uani 1 1 d . . . . .
O67 O 0.2502(5) 0.7863(2) 0.7911(3) 0.0293(13) Uani 1 1 d . . . . .
O56 O 0.4435(4) 0.6683(3) 0.8665(2) 0.0271(13) Uani 1 1 d . . . . .
O45 O 0.5022(4) 0.5028(3) 0.8296(3) 0.0270(13) Uani 1 1 d . . . . .
O49 O 0.2239(4) 0.4451(3) 0.7661(2) 0.0258(12) Uani 1 1 d . . . . .
O89 O -0.0068(5) 0.5261(3) 0.6732(3) 0.0276(13) Uani 1 1 d . . . . .
O810 O -0.0904(5) 0.5825(3) 0.7670(3) 0.0278(13) Uani 1 1 d . . . . .
O712 O 0.0682(5) 0.7420(3) 0.8391(3) 0.0279(13) Uani 1 1 d . . . . .
O612 O 0.2669(4) 0.7319(2) 0.8989(2) 0.0257(12) Uani 1 1 d . . . . .
O511 O 0.4213(4) 0.5607(2) 0.9231(2) 0.0236(12) Uani 1 1 d . . . . .
O411 O 0.3211(4) 0.4592(2) 0.8772(2) 0.0242(12) Uani 1 1 d . . . . .
O910 O 0.0082(4) 0.4729(3) 0.7807(2) 0.0256(12) Uani 1 1 d . . . . .
O102 O 0.0271(5) 0.6240(3) 0.8660(3) 0.0277(13) Uani 1 1 d . . . . .
O112 O 0.2216(4) 0.6151(3) 0.9258(3) 0.0284(13) Uani 1 1 d . . . . .
O101 O 0.1236(4) 0.5163(3) 0.8797(2) 0.0254(12) Uani 1 1 d . . . . .
O123 O 0.2978(4) 0.6119(2) 0.7147(2) 0.0220(11) Uani 1 1 d . . . . .
O890 O 0.1270(4) 0.5718(2) 0.7611(2) 0.0224(12) Uani 1 1 d . . . . .
O39 O 0.2221(4) 0.6668(2) 0.8023(2) 0.0212(11) Uani 1 1 d . . . . .
O451 O 0.3133(4) 0.5632(2) 0.8166(2) 0.0223(11) Uani 1 1 d . . . . .
N1A N 0.3656(5) 0.5402(3) 0.4639(3) 0.0243(15) Uani 1 1 d . . . . .
C6A C 0.3657(7) 0.6015(4) 0.4740(3) 0.0254(17) Uani 1 1 d . . . . .
C5A C 0.2769(7) 0.6389(4) 0.4537(4) 0.031(2) Uani 1 1 d . . . . .
H5A H 0.27772 0.681982 0.462227 0.038 Uiso 1 1 calc R U . . .
C4A C 0.1879(8) 0.6126(5) 0.4211(4) 0.039(2) Uani 1 1 d . . . . .
H4A H 0.127523 0.637602 0.405318 0.046 Uiso 1 1 calc R U . . .
C3A C 0.1870(8) 0.5496(5) 0.4116(4) 0.038(2) Uani 1 1 d . . . . .
H3A H 0.124388 0.530567 0.390478 0.046 Uiso 1 1 calc R U . . .
C2A C 0.2769(7) 0.5144(4) 0.4328(4) 0.0277(18) Uani 1 1 d . . . . .
H2A H 0.276507 0.471082 0.425288 0.033 Uiso 1 1 calc R U . . .
C7A C 0.4698(8) 0.6242(4) 0.5084(4) 0.0286(19) Uani 1 1 d . . . . .
O1W O 0.7203(7) 0.6767(4) 0.5513(4) 0.062(2) Uiso 1 1 d . . . . .
O2W O 0.0097(8) 0.5663(4) 1.0216(4) 0.077(3) Uiso 1 1 d . . . . .
O3W O -0.1650(9) 0.6320(5) 0.9571(5) 0.095(3) Uiso 1 1 d . . . . .
O4W O -0.0340(11) 0.6756(6) 0.5070(6) 0.109(4) Uiso 0.9 1 d . . P . .
O5W O 0.2620(13) 0.3760(7) 0.5629(7) 0.119(5) Uiso 0.8 1 d . . P . .
N1G N -0.1766(12) 0.7977(7) 0.5593(6) 0.102(5) Uiso 0.9 1 d D . P . .
H1GA H -0.149667 0.816443 0.528254 0.122 Uiso 0.9 1 calc R U P . .
H1GB H -0.217151 0.763878 0.553754 0.122 Uiso 0.9 1 calc R U P . .
N2G N -0.0960(8) 0.8711(4) 0.6278(5) 0.050(2) Uiso 0.9 1 d D . P . .
H2GA H -0.086307 0.883875 0.665442 0.059 Uiso 0.9 1 calc R U P . .
H2GB H -0.065933 0.891849 0.598905 0.059 Uiso 0.9 1 calc R U P . .
N3G N -0.1957(14) 0.7944(8) 0.6633(7) 0.128(6) Uiso 0.9 1 d D . P . .
H3GA H -0.180986 0.811112 0.69911 0.153 Uiso 0.9 1 calc R U P . .
H3GB H -0.23668 0.760625 0.65961 0.153 Uiso 0.9 1 calc R U P . .
C1G C -0.1561(14) 0.8204(6) 0.6147(6) 0.099(6) Uiso 0.9 1 d D . P . .
N4G N 0.7936(6) 0.4227(3) 0.7330(3) 0.0300(16) Uani 1 1 d . . . . .
H4GA H 0.796198 0.38267 0.725691 0.036 Uiso 1 1 calc R U . . .
H4GB H 0.853354 0.441981 0.748779 0.036 Uiso 1 1 calc R U . . .
N5G N 0.6945(6) 0.5141(3) 0.7310(4) 0.0356(18) Uani 1 1 d . . . . .
H5GA H 0.631711 0.534441 0.72247 0.043 Uiso 1 1 calc R U . . .
H5GB H 0.753903 0.533673 0.746814 0.043 Uiso 1 1 calc R U . . .
N6G N 0.6114(6) 0.4244(3) 0.6965(4) 0.0343(18) Uani 1 1 d . . . . .
H6GA H 0.548417 0.444481 0.68789 0.041 Uiso 1 1 calc R U . . .
H6GB H 0.615289 0.384355 0.689345 0.041 Uiso 1 1 calc R U . . .
C2G C 0.6995(6) 0.4539(4) 0.7201(4) 0.0260(18) Uani 1 1 d . . . . .
N7G N 0.5495(7) 0.7980(4) 0.5856(3) 0.044(2) Uani 1 1 d . . . . .
H7GA H 0.528703 0.759191 0.589216 0.053 Uiso 1 1 calc R U . . .
H7GB H 0.600463 0.813971 0.611476 0.053 Uiso 1 1 calc R U . . .
N8G N 0.4284(7) 0.8071(3) 0.5034(4) 0.044(2) Uani 1 1 d . . . . .
H8GA H 0.3958 0.829351 0.47402 0.053 Uiso 1 1 calc R U . . .
H8GB H 0.4103 0.767866 0.507343 0.053 Uiso 1 1 calc R U . . .
N9G N 0.5332(7) 0.8909(3) 0.5364(3) 0.0372(19) Uani 1 1 d . . . . .
H9GA H 0.501546 0.913968 0.507417 0.045 Uiso 1 1 calc R U . . .
H9GB H 0.584183 0.90694 0.562287 0.045 Uiso 1 1 calc R U . . .
C3G C 0.5042(7) 0.8324(4) 0.5412(4) 0.0315(19) Uani 1 1 d . . . . .
N10G N -0.1534(12) 0.7860(7) 0.8677(6) 0.051(4) Uiso 0.6 1 d D . P A 1
H10A H -0.165455 0.825127 0.87626 0.061 Uiso 0.6 1 calc R U P A 1
H10B H -0.090368 0.768065 0.880866 0.061 Uiso 0.6 1 calc R U P A 1
N11G N -0.3239(17) 0.7831(12) 0.8161(11) 0.116(8) Uiso 0.6 1 d D . P A 1
H11A H -0.333664 0.822234 0.825335 0.14 Uiso 0.6 1 calc R U P A 1
H11B H -0.37642 0.763065 0.794239 0.14 Uiso 0.6 1 calc R U P A 1
N12G N -0.2078(16) 0.6970(8) 0.8170(9) 0.079(5) Uiso 0.6 1 d D . P A 1
H12A H -0.141963 0.680268 0.826855 0.095 Uiso 0.6 1 calc R U P A 1
H12B H -0.25882 0.675844 0.79528 0.095 Uiso 0.6 1 calc R U P A 1
C4G C -0.2301(17) 0.7541(9) 0.8350(12) 0.108(9) Uiso 0.6 1 d D . P A 1
N13G N 0.3370(7) 0.8437(4) 0.6591(4) 0.044(2) Uani 1 1 d . . . . .
H13A H 0.317671 0.804945 0.664882 0.052 Uiso 1 1 calc R U . . .
H13B H 0.397755 0.858868 0.678233 0.052 Uiso 1 1 calc R U . . .
N14G N 0.3057(6) 0.9370(4) 0.6141(4) 0.0407(19) Uani 1 1 d . . . . .
H14A H 0.265155 0.961301 0.589457 0.049 Uiso 1 1 calc R U . . .
H14B H 0.366666 0.951313 0.63363 0.049 Uiso 1 1 calc R U . . .
N15G N 0.1840(8) 0.8578(4) 0.5924(6) 0.076(4) Uani 1 1 d . . . . .
H15A H 0.143642 0.882264 0.567786 0.092 Uiso 1 1 calc R U . . .
H15B H 0.163328 0.819139 0.597336 0.092 Uiso 1 1 calc R U . . .
C5G C 0.2750(8) 0.8790(4) 0.6216(5) 0.040(2) Uani 1 1 d . . . . .
N16G N 0.0756(16) 0.479(3) 0.5418(12) 0.054(11) Uiso 0.25 1 d D . P B 1
H16A H 0.103653 0.504228 0.570171 0.064 Uiso 0.25 1 calc R U P B 1
H16B H 0.097593 0.440279 0.541078 0.064 Uiso 0.25 1 calc R U P B 1
N17G N 0.063(2) 0.4556(17) 0.5267(19) 0.059(12) Uiso 0.25 1 d D . P B -1
N18G N 0.027(4) 0.4426(7) 0.485(2) 0.047(11) Uiso 0.2 1 d D . P B 2
H18A H 0.084004 0.42379 0.504547 0.057 Uiso 0.2 1 calc R U P B 2
H18B H -0.011599 0.423337 0.455583 0.057 Uiso 0.2 1 calc R U P B 2
N19G N -0.023(2) 0.4509(8) 0.4653(9) 0.041(5) Uiso 0.4 1 d D . P B 1
H19A H 0.010125 0.415348 0.473474 0.049 Uiso 0.4 1 calc R U P B 1
H19B H -0.072469 0.454008 0.43405 0.049 Uiso 0.4 1 calc R U P B 1
C6G C 0 0.5 0.5 0.062(4) Uiso 1 2 d DS . P . .
O6W O -0.319(2) 0.7459(14) 0.8897(14) 0.073(8) Uiso 0.3 1 d . . P C 2
N20G N 0.058(2) 0.5170(16) 0.5379(11) 0.055(6) Uiso 0.4 1 d . . P B 2
H20A H 0.111566 0.492935 0.553326 0.066 Uiso 0.4 1 calc R U P B 2
H20B H 0.049147 0.5545 0.552427 0.066 Uiso 0.4 1 calc R U P B 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O1T 1.719(5) . ?
W1 O13 1.904(5) . ?
W1 O12 1.932(5) . ?
W1 O14 1.921(5) . ?
W1 O19 1.886(5) . ?
W1 O123 2.405(5) . ?
W3 O3T 1.721(6) . ?
W3 O13 1.936(6) . ?
W3 O23 1.944(6) . ?
W3 O38 1.893(6) . ?
W3 O37 1.908(6) . ?
W3 O123 2.447(5) . ?
W2 O2T 1.718(6) . ?
W2 O23 1.890(6) . ?
W2 O12 1.910(6) . ?
W2 O26 1.920(6) . ?
W2 O25 1.921(6) . ?
W2 O123 2.469(5) . ?
W8 O8T 1.745(7) . ?
W8 O38 1.913(6) . ?
W8 O78 1.932(6) . ?
W8 O89 1.896(6) . ?
W8 O810 1.949(6) . ?
W8 O890 2.458(5) . ?
W7 O7T 1.731(6) . ?
W7 O37 1.918(6) . ?
W7 O78 1.880(6) . ?
W7 O67 1.956(6) . ?
W7 O712 1.928(6) . ?
W7 O39 2.430(5) . ?
W6 O6T 1.714(6) . ?
W6 O26 1.891(6) . ?
W6 O67 1.910(6) . ?
W6 O56 1.921(5) . ?
W6 O612 1.911(6) . ?
W6 O39 2.407(5) . ?
W5 O5T 1.730(6) . ?
W5 O25 1.899(6) . ?
W5 O56 1.915(5) . ?
W5 O45 1.905(6) . ?
W5 O511 1.939(5) . ?
W5 O451 2.423(5) . ?
W4 O4T 1.745(6) . ?
W4 O14 1.916(5) . ?
W4 O45 1.949(5) . ?
W4 O49 1.865(5) . ?
W4 O411 1.907(5) . ?
W4 O451 2.436(5) . ?
W9 O9T 1.748(7) . ?
W9 O19 1.921(5) . ?
W9 O49 1.942(5) . ?
W9 O89 1.897(6) . ?
W9 O910 1.934(5) . ?
W9 O890 2.450(5) . ?
W10 O10T 1.705(6) . ?
W10 O810 1.906(6) . ?
W10 O910 1.923(5) . ?
W10 O102 1.923(5) . ?
W10 O101 1.907(5) . ?
W10 O890 2.398(5) . ?
W12 O12T 1.730(6) . ?
W12 O712 1.916(6) . ?
W12 O612 1.918(5) . ?
W12 O102 1.896(6) . ?
W12 O112 1.917(6) . ?
W12 O39 2.457(5) . ?
W11 O11T 1.716(6) . ?
W11 O511 1.925(5) . ?
W11 O411 1.942(5) . ?
W11 O112 1.891(6) . ?
W11 O101 1.912(5) . ?
W11 O451 2.447(5) . ?
Cu1A O1T 2.507(5) . ?
Cu1A O8A 1.945(5) 3_666 ?
Cu1A O8A 1.945(5) . ?
Cu1A N1A 1.951(6) . ?
Cu1A N1A 1.951(7) 3_666 ?
P1 O123 1.530(5) . ?
P1 O890 1.518(5) . ?
P1 O39 1.535(5) . ?
P1 O451 1.528(5) . ?
O8A C7A 1.261(10) . ?
O9A C7A 1.245(10) . ?
N1A C6A 1.343(10) . ?
N1A C2A 1.348(10) . ?
C6A C5A 1.385(11) . ?
C6A C7A 1.499(11) . ?
C5A H5A 0.95 . ?
C5A C4A 1.368(13) . ?
C4A H4A 0.95 . ?
C4A C3A 1.377(14) . ?
C3A H3A 0.95 . ?
C3A C2A 1.374(13) . ?
C2A H2A 0.95 . ?
N1G H1GA 0.88 . ?
N1G H1GB 0.88 . ?
N1G C1G 1.332(2) . ?
N2G H2GA 0.88 . ?
N2G H2GB 0.88 . ?
N2G C1G 1.331(2) . ?
N3G H3GA 0.88 . ?
N3G H3GB 0.88 . ?
N3G C1G 1.332(2) . ?
N4G H4GA 0.88 . ?
N4G H4GB 0.88 . ?
N4G C2G 1.327(10) . ?
N5G H5GA 0.88 . ?
N5G H5GB 0.88 . ?
N5G C2G 1.323(10) . ?
N6G H6GA 0.88 . ?
N6G H6GB 0.88 . ?
N6G C2G 1.311(10) . ?
N7G H7GA 0.88 . ?
N7G H7GB 0.88 . ?
N7G C3G 1.319(11) . ?
N8G H8GA 0.88 . ?
N8G H8GB 0.88 . ?
N8G C3G 1.313(11) . ?
N9G H9GA 0.88 . ?
N9G H9GB 0.88 . ?
N9G C3G 1.317(11) . ?
N10G H10A 0.88 . ?
N10G H10B 0.88 . ?
N10G C4G 1.324(10) . ?
N11G H11A 0.88 . ?
N11G H11B 0.88 . ?
N11G C4G 1.329(10) . ?
N12G H12A 0.88 . ?
N12G H12B 0.88 . ?
N12G C4G 1.330(2) . ?
N13G H13A 0.88 . ?
N13G H13B 0.88 . ?
N13G C5G 1.319(12) . ?
N14G H14A 0.88 . ?
N14G H14B 0.88 . ?
N14G C5G 1.317(12) . ?
N15G H15A 0.88 . ?
N15G H15B 0.88 . ?
N15G C5G 1.313(12) . ?
N16G H16A 0.88 . ?
N16G H16B 0.88 . ?
N16G N17G 0.62(5) . ?
N16G N19G 1.64(4) 3_566 ?
N16G C6G 1.330(2) . ?
N17G N19G 1.66(4) . ?
N17G C6G 1.331(2) . ?
N18G H18A 0.88 . ?
N18G H18B 0.88 . ?
N18G C6G 1.330(2) . ?
N18G N20G 1.41(4) 3_566 ?
N18G H20B 1.19(6) 3_566 ?
N19G H19A 0.88 . ?
N19G H19B 0.88 . ?
N19G C6G 1.330(2) . ?
N19G H20B 0.50(3) 3_566 ?
C6G N20G 1.11(2) . ?
C6G N20G 1.11(2) 3_566 ?
N20G H20A 0.88 . ?
N20G H20B 0.88 . ?

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
O1T W1 O13 101.6(3) . . ?
O1T W1 O12 100.8(2) . . ?
O1T W1 O14 101.0(2) . . ?
O1T W1 O19 101.9(2) . . ?
O1T W1 O123 172.0(2) . . ?
O13 W1 O12 87.3(2) . . ?
O13 W1 O14 157.4(2) . . ?
O13 W1 O123 73.5(2) . . ?
O12 W1 O123 73.0(2) . . ?
O14 W1 O12 87.8(2) . . ?
O14 W1 O123 83.9(2) . . ?
O19 W1 O13 89.0(2) . . ?
O19 W1 O12 157.2(2) . . ?
O19 W1 O14 87.0(2) . . ?
O19 W1 O123 84.5(2) . . ?
O3T W3 O13 102.6(3) . . ?
O3T W3 O23 100.0(3) . . ?
O3T W3 O38 103.4(3) . . ?
O3T W3 O37 101.0(3) . . ?
O3T W3 O123 170.4(3) . . ?
O13 W3 O23 85.9(2) . . ?
O13 W3 O123 72.0(2) . . ?
O23 W3 O123 72.1(2) . . ?
O38 W3 O13 89.8(2) . . ?
O38 W3 O23 156.5(2) . . ?
O38 W3 O37 87.7(2) . . ?
O38 W3 O123 84.7(2) . . ?
O37 W3 O13 156.2(2) . . ?
O37 W3 O23 87.0(2) . . ?
O37 W3 O123 84.2(2) . . ?
O2T W2 O23 101.9(3) . . ?
O2T W2 O12 102.0(3) . . ?
O2T W2 O26 102.8(3) . . ?
O2T W2 O25 102.7(3) . . ?
O2T W2 O123 171.4(3) . . ?
O23 W2 O12 88.3(2) . . ?
O23 W2 O26 88.6(2) . . ?
O23 W2 O25 155.4(2) . . ?
O23 W2 O123 72.3(2) . . ?
O12 W2 O26 155.1(2) . . ?
O12 W2 O25 87.0(2) . . ?
O12 W2 O123 71.8(2) . . ?
O26 W2 O25 85.7(2) . . ?
O26 W2 O123 83.8(2) . . ?
O25 W2 O123 83.2(2) . . ?
O8T W8 O38 102.8(3) . . ?
O8T W8 O78 101.8(3) . . ?
O8T W8 O89 101.7(3) . . ?
O8T W8 O810 100.3(3) . . ?
O8T W8 O890 170.6(3) . . ?
O38 W8 O78 86.1(2) . . ?
O38 W8 O810 156.9(2) . . ?
O38 W8 O890 85.2(2) . . ?
O78 W8 O810 87.7(2) . . ?
O78 W8 O890 83.5(2) . . ?
O89 W8 O38 89.1(2) . . ?
O89 W8 O78 156.5(2) . . ?
O89 W8 O810 87.8(2) . . ?
O89 W8 O890 73.1(2) . . ?
O810 W8 O890 72.0(2) . . ?
O7T W7 O37 101.9(3) . . ?
O7T W7 O78 103.2(3) . . ?
O7T W7 O67 99.0(3) . . ?
O7T W7 O712 101.1(3) . . ?
O7T W7 O39 169.6(2) . . ?
O37 W7 O67 86.8(2) . . ?
O37 W7 O712 156.8(2) . . ?
O37 W7 O39 83.7(2) . . ?
O78 W7 O37 88.1(2) . . ?
O78 W7 O67 157.7(2) . . ?
O78 W7 O712 89.5(2) . . ?
O78 W7 O39 85.6(2) . . ?
O67 W7 O39 72.3(2) . . ?
O712 W7 O67 86.7(2) . . ?
O712 W7 O39 73.1(2) . . ?
O6T W6 O26 101.7(3) . . ?
O6T W6 O67 99.7(3) . . ?
O6T W6 O56 102.8(3) . . ?
O6T W6 O612 101.5(3) . . ?
O6T W6 O39 171.0(2) . . ?
O26 W6 O67 89.0(2) . . ?
O26 W6 O56 85.8(2) . . ?
O26 W6 O612 156.8(2) . . ?
O26 W6 O39 84.5(2) . . ?
O67 W6 O56 157.5(2) . . ?
O67 W6 O612 88.3(2) . . ?
O67 W6 O39 73.6(2) . . ?
O56 W6 O39 84.1(2) . . ?
O612 W6 O56 87.9(2) . . ?
O612 W6 O39 72.7(2) . . ?
O5T W5 O25 102.0(3) . . ?
O5T W5 O56 102.0(3) . . ?
O5T W5 O45 101.1(3) . . ?
O5T W5 O511 100.3(3) . . ?
O5T W5 O451 170.8(2) . . ?
O25 W5 O56 85.8(2) . . ?
O25 W5 O45 90.2(2) . . ?
O25 W5 O511 157.6(2) . . ?
O25 W5 O451 85.3(2) . . ?
O56 W5 O511 87.4(2) . . ?
O56 W5 O451 84.0(2) . . ?
O45 W5 O56 156.9(2) . . ?
O45 W5 O511 87.7(2) . . ?
O45 W5 O451 73.0(2) . . ?
O511 W5 O451 72.8(2) . . ?
O4T W4 O14 102.6(3) . . ?
O4T W4 O45 99.5(3) . . ?
O4T W4 O49 103.0(3) . . ?
O4T W4 O411 100.9(2) . . ?
O4T W4 O451 169.5(2) . . ?
O14 W4 O45 86.4(2) . . ?
O14 W4 O451 83.3(2) . . ?
O45 W4 O451 72.0(2) . . ?
O49 W4 O14 87.4(2) . . ?
O49 W4 O45 157.5(2) . . ?
O49 W4 O411 90.3(2) . . ?
O49 W4 O451 85.8(2) . . ?
O411 W4 O14 156.2(2) . . ?
O411 W4 O45 86.7(2) . . ?
O411 W4 O451 72.9(2) . . ?
O9T W9 O19 100.9(3) . . ?
O9T W9 O49 102.7(3) . . ?
O9T W9 O89 99.9(3) . . ?
O9T W9 O910 101.9(3) . . ?
O9T W9 O890 170.9(2) . . ?
O19 W9 O49 86.5(2) . . ?
O19 W9 O910 157.2(2) . . ?
O19 W9 O890 85.2(2) . . ?
O49 W9 O890 84.3(2) . . ?
O89 W9 O19 89.3(2) . . ?
O89 W9 O49 157.4(2) . . ?
O89 W9 O910 87.3(2) . . ?
O89 W9 O890 73.3(2) . . ?
O910 W9 O49 87.9(2) . . ?
O910 W9 O890 72.3(2) . . ?
O10T W10 O810 100.9(3) . . ?
O10T W10 O910 100.7(3) . . ?
O10T W10 O102 101.6(3) . . ?
O10T W10 O101 101.4(3) . . ?
O10T W10 O890 172.4(2) . . ?
O810 W10 O910 87.7(2) . . ?
O810 W10 O102 88.9(2) . . ?
O810 W10 O101 157.7(2) . . ?
O810 W10 O890 74.1(2) . . ?
O910 W10 O890 73.7(2) . . ?
O102 W10 O910 157.6(2) . . ?
O102 W10 O890 84.1(2) . . ?
O101 W10 O910 89.1(2) . . ?
O101 W10 O102 85.7(2) . . ?
O101 W10 O890 83.8(2) . . ?
O12T W12 O712 100.2(3) . . ?
O12T W12 O612 102.1(3) . . ?
O12T W12 O102 102.3(3) . . ?
O12T W12 O112 103.0(3) . . ?
O12T W12 O39 170.2(2) . . ?
O712 W12 O612 87.5(2) . . ?
O712 W12 O112 156.8(2) . . ?
O712 W12 O39 72.6(2) . . ?
O612 W12 O39 71.4(2) . . ?
O102 W12 O712 88.9(2) . . ?
O102 W12 O612 155.6(2) . . ?
O102 W12 O112 86.3(2) . . ?
O102 W12 O39 84.5(2) . . ?
O112 W12 O612 87.6(2) . . ?
O112 W12 O39 84.3(2) . . ?
O11T W11 O511 101.2(3) . . ?
O11T W11 O411 100.5(3) . . ?
O11T W11 O112 102.8(3) . . ?
O11T W11 O101 103.0(3) . . ?
O11T W11 O451 170.2(2) . . ?
O511 W11 O411 87.2(2) . . ?
O511 W11 O451 72.4(2) . . ?
O411 W11 O451 72.1(2) . . ?
O112 W11 O511 88.7(2) . . ?
O112 W11 O411 156.6(2) . . ?
O112 W11 O101 86.7(2) . . ?
O112 W11 O451 84.7(2) . . ?
O101 W11 O511 155.8(2) . . ?
O101 W11 O411 87.7(2) . . ?
O101 W11 O451 83.5(2) . . ?
O8A Cu1A O1T 92.8(2) . . ?
O8A Cu1A O1T 87.2(2) 3_666 . ?
O8A Cu1A O8A 180.0(3) 3_666 . ?
O8A Cu1A N1A 96.3(3) 3_666 . ?
O8A Cu1A N1A 83.7(3) 3_666 3_666 ?
O8A Cu1A N1A 96.3(3) . 3_666 ?
O8A Cu1A N1A 83.7(3) . . ?
N1A Cu1A O1T 91.2(2) 3_666 . ?
N1A Cu1A O1T 88.8(2) . . ?
N1A Cu1A N1A 180.0(4) 3_666 . ?
O123 P1 O39 109.3(3) . . ?
O890 P1 O123 110.5(3) . . ?
O890 P1 O39 109.3(3) . . ?
O890 P1 O451 109.1(3) . . ?
O451 P1 O123 109.2(3) . . ?
O451 P1 O39 109.5(3) . . ?
W1 O1T Cu1A 133.0(3) . . ?
C7A O8A Cu1A 114.0(5) . . ?
W1 O13 W3 125.2(3) . . ?
W2 O23 W3 127.0(3) . . ?
W2 O12 W1 125.9(3) . . ?
W3 O38 W8 150.4(3) . . ?
W3 O37 W7 148.2(3) . . ?
W6 O26 W2 151.3(3) . . ?
W5 O25 W2 150.8(3) . . ?
W4 O14 W1 149.3(3) . . ?
W1 O19 W9 150.0(3) . . ?
W7 O78 W8 149.7(3) . . ?
W6 O67 W7 124.2(3) . . ?
W5 O56 W6 150.2(3) . . ?
W5 O45 W4 125.4(3) . . ?
W4 O49 W9 149.4(3) . . ?
W9 O89 W8 126.4(3) . . ?
W10 O810 W8 124.5(3) . . ?
W12 O712 W7 125.5(3) . . ?
W6 O612 W12 126.4(3) . . ?
W11 O511 W5 125.1(3) . . ?
W4 O411 W11 125.8(3) . . ?
W10 O910 W9 124.5(3) . . ?
W12 O102 W10 150.6(3) . . ?
W11 O112 W12 150.2(3) . . ?
W10 O101 W11 150.6(3) . . ?
W1 O123 W3 89.27(17) . . ?
W1 O123 W2 89.15(17) . . ?
W3 O123 W2 88.51(16) . . ?
P1 O123 W1 126.8(3) . . ?
P1 O123 W3 125.3(3) . . ?
P1 O123 W2 125.8(3) . . ?
W9 O890 W8 87.21(17) . . ?
W10 O890 W8 89.25(17) . . ?
W10 O890 W9 89.47(17) . . ?
P1 O890 W8 125.6(3) . . ?
P1 O890 W9 124.9(3) . . ?
P1 O890 W10 128.1(3) . . ?
W7 O39 W12 88.73(17) . . ?
W6 O39 W7 89.86(17) . . ?
W6 O39 W12 89.29(17) . . ?
P1 O39 W7 125.5(3) . . ?
P1 O39 W6 126.9(3) . . ?
P1 O39 W12 124.9(3) . . ?
W5 O451 W4 89.61(17) . . ?
W5 O451 W11 89.53(17) . . ?
W4 O451 W11 89.15(17) . . ?
P1 O451 W5 125.9(3) . . ?
P1 O451 W4 125.5(3) . . ?
P1 O451 W11 125.6(3) . . ?
C6A N1A Cu1A 112.2(5) . . ?
C6A N1A C2A 119.0(7) . . ?
C2A N1A Cu1A 128.7(6) . . ?
N1A C6A C5A 121.8(8) . . ?
N1A C6A C7A 113.6(7) . . ?
C5A C6A C7A 124.6(8) . . ?
C6A C5A H5A 120.6 . . ?
C4A C5A C6A 118.9(9) . . ?
C4A C5A H5A 120.6 . . ?
C5A C4A H4A 120.4 . . ?
C5A C4A C3A 119.2(8) . . ?
C3A C4A H4A 120.4 . . ?
C4A C3A H3A 120.1 . . ?
C2A C3A C4A 119.7(9) . . ?
C2A C3A H3A 120.1 . . ?
N1A C2A C3A 121.2(8) . . ?
N1A C2A H2A 119.4 . . ?
C3A C2A H2A 119.4 . . ?
O8A C7A C6A 116.4(7) . . ?
O9A C7A O8A 124.0(8) . . ?
O9A C7A C6A 119.5(8) . . ?
H1GA N1G H1GB 120 . . ?
C1G N1G H1GA 120 . . ?
C1G N1G H1GB 120 . . ?
H2GA N2G H2GB 120 . . ?
C1G N2G H2GA 120 . . ?
C1G N2G H2GB 120 . . ?
H3GA N3G H3GB 120 . . ?
C1G N3G H3GA 120 . . ?
C1G N3G H3GB 120 . . ?
N2G C1G N1G 124.6(13) . . ?
N2G C1G N3G 112.7(13) . . ?
N3G C1G N1G 122.7(13) . . ?
H4GA N4G H4GB 120 . . ?
C2G N4G H4GA 120 . . ?
C2G N4G H4GB 120 . . ?
H5GA N5G H5GB 120 . . ?
C2G N5G H5GA 120 . . ?
C2G N5G H5GB 120 . . ?
H6GA N6G H6GB 120 . . ?
C2G N6G H6GA 120 . . ?
C2G N6G H6GB 120 . . ?
N5G C2G N4G 120.5(8) . . ?
N6G C2G N4G 119.1(8) . . ?
N6G C2G N5G 120.4(8) . . ?
H7GA N7G H7GB 120 . . ?
C3G N7G H7GA 120 . . ?
C3G N7G H7GB 120 . . ?
H8GA N8G H8GB 120 . . ?
C3G N8G H8GA 120 . . ?
C3G N8G H8GB 120 . . ?
H9GA N9G H9GB 120 . . ?
C3G N9G H9GA 120 . . ?
C3G N9G H9GB 120 . . ?
N8G C3G N7G 118.4(8) . . ?
N8G C3G N9G 121.4(8) . . ?
N9G C3G N7G 120.2(8) . . ?
H10A N10G H10B 120 . . ?
C4G N10G H10A 120 . . ?
C4G N10G H10B 120 . . ?
H11A N11G H11B 120 . . ?
C4G N11G H11A 120 . . ?
C4G N11G H11B 120 . . ?
H12A N12G H12B 120 . . ?
C4G N12G H12A 120 . . ?
C4G N12G H12B 120 . . ?
N10G C4G N11G 118.0(18) . . ?
N10G C4G N12G 120.1(18) . . ?
N11G C4G N12G 121.6(19) . . ?
H13A N13G H13B 120 . . ?
C5G N13G H13A 120 . . ?
C5G N13G H13B 120 . . ?
H14A N14G H14B 120 . . ?
C5G N14G H14A 120 . . ?
C5G N14G H14B 120 . . ?
H15A N15G H15B 120 . . ?
C5G N15G H15A 120 . . ?
C5G N15G H15B 120 . . ?
N14G C5G N13G 118.7(9) . . ?
N15G C5G N13G 121.5(9) . . ?
N15G C5G N14G 119.8(10) . . ?
H16A N16G H16B 120 . . ?
N17G N16G H16A 163.2 . . ?
N17G N16G H16B 43.6 . . ?
N17G N16G N19G 128.4(11) . 3_566 ?
N17G N16G C6G 76.5(12) . . ?
N19G N16G H16A 68 3_566 . ?
N19G N16G H16B 172 3_566 . ?
C6G N16G H16A 120 . . ?
C6G N16G H16B 120 . . ?
C6G N16G N19G 52.0(12) . 3_566 ?
N16G N17G N19G 127.8(12) . . ?
N16G N17G C6G 76.4(12) . . ?
C6G N17G N19G 51.5(11) . . ?
H18A N18G H18B 120 . . ?
C6G N18G H18A 120 . . ?
C6G N18G H18B 120 . . ?
C6G N18G N20G 47.9(12) . 3_566 ?
C6G N18G H20B 86(2) . 3_566 ?
N20G N18G H18A 167.9 3_566 . ?
N20G N18G H18B 72.1 3_566 . ?
N17G N19G H19A 68.5 . . ?
N17G N19G H19B 171.4 . . ?
N17G N19G H20B 170(4) . 3_566 ?
H19A N19G H19B 120 . . ?
H19A N19G H20B 102 . 3_566 ?
H19B N19G H20B 18.1 . 3_566 ?
C6G N19G N17G 51.5(11) . . ?
C6G N19G H19A 120 . . ?
C6G N19G H19B 120 . . ?
C6G N19G H20B 138(4) . 3_566 ?
N16G C6G N16G 180 . 3_566 ?
N16G C6G N17G 153(2) 3_566 . ?
N16G C6G N17G 27(2) 3_566 3_566 ?
N16G C6G N17G 27(2) . . ?
N16G C6G N17G 153(2) . 3_566 ?
N17G C6G N17G 180(3) . 3_566 ?
N19G C6G N16G 104(2) . . ?
N19G C6G N16G 76(2) 3_566 . ?
N19G C6G N16G 104(2) 3_566 3_566 ?
N19G C6G N16G 76(2) . 3_566 ?
N19G C6G N17G 103(2) 3_566 . ?
N19G C6G N17G 77(2) 3_566 3_566 ?
N19G C6G N17G 77(2) . . ?
N19G C6G N17G 103(2) . 3_566 ?
N19G C6G N18G 147(2) . 3_566 ?
N19G C6G N18G 33(2) 3_566 3_566 ?
N19G C6G N19G 180 3_566 . ?
N20G C6G N18G 70(2) 3_566 . ?
N20G C6G N18G 110(2) . . ?
N20G C6G N20G 180 . 3_566 ?
C6G N20G H18B 99(3) . 3_566 ?
C6G N20G H20A 120 . . ?
C6G N20G H20B 120 . . ?
H20A N20G H20B 120 . . ?

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
Cu1A O8A C7A O9A -178.7(7) . . . . ?
Cu1A O8A C7A C6A -1.7(9) . . . . ?
Cu1A N1A C6A C5A -178.3(6) . . . . ?
Cu1A N1A C6A C7A 1.9(8) . . . . ?
Cu1A N1A C2A C3A 178.2(6) . . . . ?
O1T W1 O19 W9 131.4(6) . . . . ?
O3T W3 O38 W8 -131.8(7) . . . . ?
O2T W2 O23 W3 170.7(4) . . . . ?
O8T W8 O89 W9 -170.3(4) . . . . ?
O7T W7 O78 W8 132.0(7) . . . . ?
O6T W6 O26 W2 132.6(7) . . . . ?
O5T W5 O25 W2 -132.6(7) . . . . ?
O4T W4 O49 W9 -134.0(6) . . . . ?
O9T W9 O89 W8 172.2(4) . . . . ?
O12T W12 O102 W10 -134.2(7) . . . . ?
O11T W11 O112 W12 -131.9(7) . . . . ?
O13 W1 O1T Cu1A 45.1(4) . . . . ?
O13 W1 O19 W9 -127.0(6) . . . . ?
O13 W3 O38 W8 125.2(7) . . . . ?
O23 W3 O38 W8 45.9(11) . . . . ?
O12 W1 O1T Cu1A -44.4(4) . . . . ?
O12 W1 O19 W9 -46.2(10) . . . . ?
O12 W2 O23 W3 68.7(4) . . . . ?
O38 W8 O89 W9 86.9(4) . . . . ?
O37 W3 O38 W8 -31.1(7) . . . . ?
O37 W7 O78 W8 30.2(7) . . . . ?
O26 W2 O23 W3 -86.6(4) . . . . ?
O25 W2 O23 W3 -10.2(8) . . . . ?
O14 W1 O1T Cu1A -134.2(4) . . . . ?
O14 W1 O19 W9 30.7(6) . . . . ?
O14 W4 O49 W9 -31.7(6) . . . . ?
O19 W1 O1T Cu1A 136.6(4) . . . . ?
O19 W9 O89 W8 -86.8(4) . . . . ?
O78 W8 O89 W9 8.8(8) . . . . ?
O67 W7 O78 W8 -46.6(11) . . . . ?
O67 W6 O26 W2 -127.7(7) . . . . ?
O56 W6 O26 W2 30.4(7) . . . . ?
O56 W5 O25 W2 -31.2(7) . . . . ?
O45 W5 O25 W2 126.0(7) . . . . ?
O45 W4 O49 W9 42.4(10) . . . . ?
O49 W9 O89 W8 -7.5(9) . . . . ?
O810 W8 O89 W9 -70.3(4) . . . . ?
O712 W7 O78 W8 -126.7(7) . . . . ?
O712 W12 O102 W10 125.6(7) . . . . ?
O612 W6 O26 W2 -44.5(11) . . . . ?
O612 W12 O102 W10 44.2(11) . . . . ?
O511 W5 O25 W2 41.7(11) . . . . ?
O511 W11 O112 W12 126.9(7) . . . . ?
O411 W4 O49 W9 124.7(6) . . . . ?
O411 W11 O112 W12 47.0(10) . . . . ?
O910 W9 O89 W8 70.7(4) . . . . ?
O112 W12 O102 W10 -31.7(7) . . . . ?
O101 W11 O112 W12 -29.3(6) . . . . ?
O123 W1 O19 W9 -53.5(6) . . . . ?
O123 W3 O38 W8 53.3(7) . . . . ?
O123 W2 O23 W3 -2.7(3) . . . . ?
O123 P1 O890 W8 -58.0(4) . . . . ?
O123 P1 O890 W9 57.2(4) . . . . ?
O123 P1 O890 W10 179.3(3) . . . . ?
O123 P1 O39 W7 61.8(4) . . . . ?
O123 P1 O39 W6 -60.2(4) . . . . ?
O123 P1 O39 W12 179.5(3) . . . . ?
O123 P1 O451 W5 59.6(4) . . . . ?
O123 P1 O451 W4 -60.8(4) . . . . ?
O123 P1 O451 W11 180.0(3) . . . . ?
O890 W8 O89 W9 1.6(3) . . . . ?
O890 W9 O89 W8 -1.6(3) . . . . ?
O890 P1 O123 W1 -60.2(4) . . . . ?
O890 P1 O123 W3 60.5(4) . . . . ?
O890 P1 O123 W2 178.6(3) . . . . ?
O890 P1 O39 W7 -59.2(4) . . . . ?
O890 P1 O39 W6 178.8(3) . . . . ?
O890 P1 O39 W12 58.5(4) . . . . ?
O890 P1 O451 W5 -179.5(3) . . . . ?
O890 P1 O451 W4 60.1(4) . . . . ?
O890 P1 O451 W11 -59.1(4) . . . . ?
O39 W7 O78 W8 -53.7(7) . . . . ?
O39 W6 O26 W2 -54.1(7) . . . . ?
O39 W12 O102 W10 53.0(7) . . . . ?
O39 P1 O123 W1 179.5(3) . . . . ?
O39 P1 O123 W3 -59.8(4) . . . . ?
O39 P1 O123 W2 58.4(4) . . . . ?
O39 P1 O890 W8 62.2(4) . . . . ?
O39 P1 O890 W9 177.4(3) . . . . ?
O39 P1 O890 W10 -60.4(4) . . . . ?
O39 P1 O451 W5 -60.0(4) . . . . ?
O39 P1 O451 W4 179.6(3) . . . . ?
O39 P1 O451 W11 60.4(4) . . . . ?
O451 W5 O25 W2 53.1(7) . . . . ?
O451 W4 O49 W9 51.8(6) . . . . ?
O451 W11 O112 W12 54.4(6) . . . . ?
O451 P1 O123 W1 59.8(4) . . . . ?
O451 P1 O123 W3 -179.5(3) . . . . ?
O451 P1 O123 W2 -61.3(4) . . . . ?
O451 P1 O890 W8 -178.1(3) . . . . ?
O451 P1 O890 W9 -62.9(4) . . . . ?
O451 P1 O890 W10 59.2(4) . . . . ?
O451 P1 O39 W7 -178.6(3) . . . . ?
O451 P1 O39 W6 59.4(4) . . . . ?
O451 P1 O39 W12 -60.9(4) . . . . ?
N1A C6A C5A C4A -1.7(12) . . . . ?
N1A C6A C7A O8A -0.2(10) . . . . ?
N1A C6A C7A O9A 177.0(8) . . . . ?
C6A N1A C2A C3A -0.3(12) . . . . ?
C6A C5A C4A C3A 2.6(13) . . . . ?
C5A C6A C7A O8A -179.9(8) . . . . ?
C5A C6A C7A O9A -2.8(13) . . . . ?
C5A C4A C3A C2A -2.5(13) . . . . ?
C4A C3A C2A N1A 1.4(13) . . . . ?
C2A N1A C6A C5A 0.5(12) . . . . ?
C2A N1A C6A C7A -179.3(7) . . . . ?
C7A C6A C5A C4A 178.1(8) . . . . ?
N16G N17G N19G C6G -4(4) . . . . ?
N16G N17G C6G N16G 180.00(5) . . . 3_566 ?
N16G N17G C6G N19G -4(3) . . . 3_566 ?
N16G N17G C6G N19G 176(3) . . . . ?
N17G N16G C6G N17G 180.00(3) . . . 3_566 ?
N17G N16G C6G N19G 176(4) . . . 3_566 ?
N17G N16G C6G N19G -4(4) . . . . ?
N17G N19G C6G N16G -178.3(16) . . . 3_566 ?
N17G N19G C6G N16G 1.7(16) . . . . ?
N17G N19G C6G N17G 180.000(13) . . . 3_566 ?
N19G N16G N17G N19G 7(7) 3_566 . . . ?
N19G N16G N17G C6G 4(4) 3_566 . . . ?
N19G N16G C6G N17G -176(4) 3_566 . . . ?
N19G N16G C6G N17G 4(4) 3_566 . . 3_566 ?
N19G N16G C6G N19G 179.997(13) 3_566 . . . ?
N19G N17G C6G N16G -176(3) . . . . ?
N19G N17G C6G N16G 4(3) . . . 3_566 ?
N19G N17G C6G N19G 180.003(17) . . . 3_566 ?
C6G N16G N17G N19G 4(3) . . . . ?
N20G N18G C6G N20G 180.002(19) 3_566 . . . ?

# start Validation Reply Form
_vrf_PLAT975_b20240088_p2agudumo_auto 
;
PROBLEM: Check Calcd Resid. Dens. 0.77Ang From O5W . 2.17 eA-3 
RESPONSE: The O5W is a water molecule located in a region where
hydration water molecules present a certain degree of disorder
in their positions and therefore, they display partial occupancies.
This structural disorder cannot be further modelled. This is a
common fact found in polyoxometalate salts due to the presence of
a large amount of disordered hydration water molecules and heavy
atoms such as W.
;
_vrf_PLAT306_b20240088_p2agudumo_auto 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W Check 
RESPONSE: No hydrogen atom was added to water molecules and therefore,
isolated O atoms can be found in the structure. This is a common fact
found in the refinement of polyoxotungstate structures due to the presence
of a large amount of heavy atoms such as W. Furthermore, hydration water
molecules are disordered over several positions showing partial occupancies.
;
_vrf_PLAT430_b20240088_p2agudumo_auto 
;
PROBLEM: Short Inter D...A Contact O1W ..O8T . 2.79 Ang. 
RESPONSE: These two atoms belong to molecules involved in the
formation of a hydrogen bond. Distances below 2.8 Ang. imply that
the two atoms are not coexisting in the structure; that is, the
sum of their partial occupancies is less than 1.
;
# end Validation Reply Form
# The following lines are used to test the character set of files sent by
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# END of CIF

