# Electronic Supplementary Material (ESI) for RSC Advances
# This journal is © The Royal Society of Chemistry 2013


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#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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data_compound1
_database_code_depnum_ccdc_archive 'CCDC 915551'
#TrackingRef 'Compound 1 .cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H108 Cu7 N18 O96 P2 W22'
_chemical_formula_weight         6664.59
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
_cell_length_a                   17.946(3)
_cell_length_b                   19.663(4)
_cell_length_c                   16.913(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.455(2)
_cell_angle_gamma                90.00
_cell_volume                     5917.7(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5870.0
_exptl_absorpt_coefficient_mu    22.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.031
_exptl_absorpt_correction_T_max  0.042
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18974
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         25.25
_reflns_number_total             5524
_reflns_number_gt                3600
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
During the refinement, the command 'omit-3 50' was used to omit the weak reflection above 50 degree. The commands 'isor' or 'simu' were used to restrain the non-H atoms (N3, C3, N4, C4, N1, C1, C2, O15, C5, C3, O3, O13, N5, O12 and O16) with ADP or NPD problems. The Cu3 and W7 atoms were constrained by EADP and EXYZ command, because of the site-occupancy disorder. These restraint refinement leads to a relatively high restraint value 78. The highest residual peak 5.97 eA-3 is close to the W4 position, which is featureless, and should be due to the "series termination errors". The H atoms on water molecules cannot be found from the residual peaks and directly included into the final molecular formula.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0828P)^2^+374.5343P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5489
_refine_ls_number_parameters     400
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.1787
_refine_ls_wR_factor_gt          0.1545
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.76284(5) 0.58606(4) 0.55962(6) 0.0331(3) Uani 1 1 d . . .
W2 W 0.68531(5) 0.67925(4) 0.71200(7) 0.0330(3) Uani 1 1 d . . .
W3 W 0.54503(6) 0.59357(5) 0.77890(7) 0.0350(3) Uani 1 1 d . . .
W4 W 0.82202(6) 0.58436(5) 0.86316(7) 0.0398(3) Uani 1 1 d . . .
W5 W 0.88858(8) 0.5000 0.69180(11) 0.0428(4) Uani 1 2 d S . .
W6 W 0.67656(10) 0.5000 0.92527(10) 0.0474(4) Uani 1 2 d S . .
W7 W 0.56909(7) 0.59181(6) 0.58696(9) 0.0252(3) Uani 0.50 1 d P . .
Cu3 Cu 0.56909(7) 0.59181(6) 0.58696(9) 0.0252(3) Uani 0.50 1 d P . .
Cu1 Cu 0.3468(2) 0.69033(16) 0.7528(3) 0.0720(13) Uani 1 1 d . . .
P1 P 0.6959(4) 0.5000 0.7202(5) 0.0183(17) Uani 1 2 d S . .
O1 O 0.5496(13) 0.5000 0.5759(14) 0.036(6) Uani 1 2 d S . .
O2 O 0.6137(8) 0.6820(7) 0.6248(10) 0.031(4) Uani 1 1 d . . .
O3 O 0.5080(9) 0.6063(8) 0.6726(10) 0.039(4) Uani 1 1 d U . .
O4 O 0.5000 0.6275(10) 0.5000 0.052(7) Uani 1 2 d S . .
O5 O 0.4734(10) 0.6280(10) 0.8232(11) 0.053(5) Uani 1 1 d . . .
O6 O 0.5205(12) 0.5000 0.7729(12) 0.028(5) Uani 1 2 d S . .
O7 O 0.6071(10) 0.6741(8) 0.7788(10) 0.044(4) Uani 1 1 d . . .
O8 O 0.6146(11) 0.5644(9) 0.8741(12) 0.058(5) Uani 1 1 d . . .
O9 O 0.7102(10) 0.7628(8) 0.7227(12) 0.053(5) Uani 1 1 d . . .
O10 O 0.6530(16) 0.5000 1.0179(17) 0.062(8) Uani 1 2 d S . .
O11 O 0.7572(9) 0.6442(7) 0.8037(9) 0.034(4) Uani 1 1 d . . .
O12 O 0.7435(13) 0.5000 0.8092(14) 0.037(5) Uani 1 2 d SU . .
O13 O 0.7512(11) 0.5721(10) 0.9265(12) 0.060(5) Uani 1 1 d U . .
O14 O 0.8819(11) 0.6418(9) 0.9153(14) 0.066(6) Uani 1 1 d . . .
O15 O 0.8706(14) 0.5000 0.8972(16) 0.049(6) Uani 1 2 d SU . .
O16 O 0.8696(10) 0.5668(9) 0.7693(11) 0.046(4) Uani 1 1 d U . .
O17 O 0.9839(13) 0.5000 0.6995(15) 0.043(6) Uani 1 2 d S . .
O18 O 0.8683(9) 0.5663(9) 0.6106(12) 0.052(5) Uani 1 1 d . . .
O19 O 0.7580(11) 0.5000 0.6529(13) 0.027(5) Uani 1 2 d S . .
O20 O 0.7566(9) 0.6463(8) 0.6470(9) 0.035(4) Uani 1 1 d . . .
O21 O 0.7863(10) 0.6389(9) 0.4867(11) 0.048(5) Uani 1 1 d . . .
O22 O 0.7732(13) 0.5000 0.5036(16) 0.045(6) Uani 1 2 d S . .
O23 O 0.6600(9) 0.5827(7) 0.5368(10) 0.036(4) Uani 1 1 d . . .
O26 O 0.6457(9) 0.5679(7) 0.7084(10) 0.037(4) Uani 1 1 d . . .
C1 C 0.385(2) 0.7286(18) 0.599(2) 0.094(6) Uani 1 1 d U . .
H1A H 0.3433 0.7566 0.5758 0.113 Uiso 1 1 calc R . .
H1B H 0.4121 0.7129 0.5565 0.113 Uiso 1 1 calc R . .
C2 C 0.436(2) 0.7690(18) 0.657(2) 0.094(6) Uani 1 1 d U . .
H2A H 0.4435 0.8136 0.6352 0.113 Uiso 1 1 calc R . .
H2B H 0.4839 0.7465 0.6681 0.113 Uiso 1 1 calc R . .
C3 C 0.309(3) 0.663(2) 0.929(3) 0.113(6) Uani 1 1 d U . .
H3A H 0.3488 0.6381 0.9605 0.136 Uiso 1 1 calc R . .
H3B H 0.2753 0.6844 0.9617 0.136 Uiso 1 1 calc R . .
C4 C 0.274(3) 0.627(2) 0.868(3) 0.113(6) Uani 1 1 d U . .
H4A H 0.2294 0.6544 0.8507 0.136 Uiso 1 1 calc R . .
H4B H 0.2556 0.5875 0.8930 0.136 Uiso 1 1 calc R . .
N1 N 0.3559(18) 0.6689(14) 0.6404(19) 0.094(6) Uani 1 1 d U . .
H1C H 0.3873 0.6335 0.6384 0.113 Uiso 1 1 calc R . .
H1D H 0.3106 0.6569 0.6150 0.113 Uiso 1 1 calc R . .
N2 N 0.4007(12) 0.7764(9) 0.7341(14) 0.048(6) Uani 1 1 d . . .
H2C H 0.3683 0.8116 0.7300 0.058 Uiso 1 1 calc R . .
H2D H 0.4367 0.7845 0.7752 0.058 Uiso 1 1 calc R . .
N3 N 0.334(2) 0.7079(18) 0.865(2) 0.113(6) Uani 1 1 d U . .
H3C H 0.3792 0.7235 0.8870 0.136 Uiso 1 1 calc R . .
H3D H 0.3029 0.7438 0.8629 0.136 Uiso 1 1 calc R . .
N4 N 0.296(2) 0.5991(18) 0.788(2) 0.113(6) Uani 1 1 d U . .
H4C H 0.2555 0.5867 0.7541 0.136 Uiso 1 1 calc R . .
H4D H 0.3285 0.5643 0.7960 0.136 Uiso 1 1 calc R . .
O1W O 0.6257(15) 0.5000 0.3728(17) 0.059(8) Uani 1 2 d S . .
O2W O 0.9103(18) 0.6803(17) 0.427(3) 0.19(2) Uani 1 1 d . . .
O3W O 0.792(5) 0.5000 0.329(5) 0.33(6) Uani 1 2 d S . .
O4W O 0.5000 0.587(6) 0.0000 0.34(6) Uani 1 2 d S . .
O5W O 0.5000 0.734(4) 0.0000 0.26(4) Uani 1 2 d S . .
O6W O 0.546(2) 0.785(2) 0.853(3) 0.23(3) Uani 1 1 d . . .
O7W O 1.0000 0.572(5) 0.5000 0.27(4) Uani 1 2 d S . .
Cu2 Cu 1.0000 0.5000 1.0000 0.070(2) Uani 1 4 d S . .
N5 N 1.052(2) 0.432(2) 0.938(3) 0.039(10) Uani 0.50 1 d PU . .
H5C H 1.0818 0.4056 0.9712 0.046 Uiso 0.50 1 calc PR . .
H5D H 1.0174 0.4059 0.9089 0.046 Uiso 0.50 1 calc PR . .
C5 C 1.086(4) 0.461(3) 0.897(5) 0.086(19) Uani 0.50 1 d PU . .
H5B H 1.0690 0.4464 0.8429 0.103 Uiso 0.50 1 calc PR . .
H5A H 1.1377 0.4464 0.9096 0.103 Uiso 0.50 1 calc PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.0250(5) 0.0277(5) 0.0458(7) 0.0077(4) 0.0017(5) -0.0023(4)
W2 0.0252(5) 0.0182(4) 0.0533(7) -0.0029(4) -0.0037(5) 0.0001(4)
W3 0.0283(6) 0.0320(5) 0.0435(7) -0.0069(4) 0.0002(5) 0.0078(4)
W4 0.0322(6) 0.0339(5) 0.0484(7) -0.0061(5) -0.0131(5) -0.0026(4)
W5 0.0191(7) 0.0327(7) 0.0729(13) 0.000 -0.0083(7) 0.000
W6 0.0577(11) 0.0459(9) 0.0362(10) 0.000 -0.0035(8) 0.000
W7 0.0197(7) 0.0181(6) 0.0357(9) 0.0012(5) -0.0037(6) -0.0001(5)
Cu3 0.0197(7) 0.0181(6) 0.0357(9) 0.0012(5) -0.0037(6) -0.0001(5)
Cu1 0.045(2) 0.0297(17) 0.140(4) 0.007(2) 0.005(2) -0.0008(15)
P1 0.010(4) 0.019(3) 0.025(5) 0.000 0.000(3) 0.000
O1 0.036(14) 0.035(12) 0.034(15) 0.000 -0.010(11) 0.000
O2 0.020(8) 0.028(8) 0.042(11) -0.001(7) -0.011(7) -0.001(6)
O3 0.039(4) 0.039(4) 0.039(4) 0.0000(10) 0.0052(11) -0.0003(10)
O4 0.08(2) 0.016(11) 0.07(2) 0.000 0.025(16) 0.000
O5 0.055(12) 0.065(12) 0.039(12) -0.018(9) 0.010(10) 0.001(10)
O6 0.026(12) 0.038(12) 0.021(13) 0.000 0.003(10) 0.000
O7 0.045(11) 0.045(10) 0.038(11) -0.005(8) -0.009(9) -0.002(8)
O8 0.072(14) 0.047(11) 0.053(14) 0.002(9) -0.005(11) 0.012(10)
O9 0.046(11) 0.021(8) 0.086(16) -0.010(9) -0.016(11) -0.013(8)
O10 0.07(2) 0.075(19) 0.044(18) 0.000 0.023(16) 0.000
O11 0.036(9) 0.023(7) 0.039(11) -0.011(7) -0.008(8) -0.002(7)
O12 0.037(6) 0.037(6) 0.037(6) 0.000 0.0045(12) 0.000
O13 0.060(5) 0.060(5) 0.061(5) -0.0007(10) 0.0082(12) 0.0000(10)
O14 0.052(12) 0.037(10) 0.098(17) 0.004(10) -0.031(12) 0.007(9)
O15 0.049(7) 0.049(7) 0.049(7) 0.000 0.0060(13) 0.000
O16 0.046(5) 0.046(5) 0.047(5) 0.0004(10) 0.0060(12) -0.0001(10)
O17 0.025(13) 0.049(14) 0.055(18) 0.000 0.001(12) 0.000
O18 0.036(10) 0.048(10) 0.062(14) -0.011(9) -0.031(10) 0.007(8)
O19 0.018(11) 0.036(11) 0.028(14) 0.000 -0.001(10) 0.000
O20 0.036(9) 0.037(9) 0.029(10) 0.001(7) -0.005(8) -0.001(7)
O21 0.049(11) 0.048(10) 0.046(12) 0.013(9) 0.006(10) -0.011(9)
O22 0.030(14) 0.043(13) 0.056(18) 0.000 -0.011(13) 0.000
O23 0.035(10) 0.029(8) 0.042(11) -0.006(7) 0.005(8) -0.014(7)
O26 0.051(11) 0.023(7) 0.029(10) -0.003(6) -0.025(8) -0.002(7)
C1 0.103(13) 0.074(11) 0.101(14) -0.023(10) -0.007(11) 0.056(11)
C2 0.103(14) 0.074(11) 0.101(14) -0.023(10) -0.007(12) 0.056(11)
C3 0.113(6) 0.113(6) 0.113(6) 0.0002(10) 0.0148(12) 0.0001(10)
C4 0.113(6) 0.113(6) 0.113(6) 0.0001(14) 0.0148(16) 0.0000(14)
N1 0.103(14) 0.074(11) 0.101(14) -0.023(10) -0.007(12) 0.056(11)
N2 0.045(13) 0.026(10) 0.069(17) 0.005(10) -0.008(12) 0.015(9)
N3 0.113(6) 0.113(6) 0.113(6) 0.0003(15) 0.0150(16) 0.0001(15)
N4 0.113(6) 0.113(6) 0.114(6) 0.0000(18) 0.0148(19) 0.0000(18)
O1W 0.052(17) 0.065(18) 0.052(19) 0.000 -0.026(15) 0.000
O2W 0.09(2) 0.12(3) 0.35(6) 0.11(3) 0.05(3) 0.02(2)
O3W 0.37(12) 0.49(15) 0.19(7) 0.000 0.22(8) 0.000
O4W 0.22(8) 0.62(18) 0.20(8) 0.000 0.15(7) 0.000
O5W 0.32(9) 0.24(8) 0.17(6) 0.000 -0.11(6) 0.000
O6W 0.11(3) 0.25(5) 0.33(6) -0.21(5) 0.02(3) -0.01(3)
O7W 0.22(7) 0.52(13) 0.09(4) 0.000 0.07(5) 0.000
Cu2 0.068(5) 0.068(5) 0.068(6) 0.000 -0.009(5) 0.000
N5 0.039(10) 0.039(10) 0.039(10) -0.0001(10) 0.0050(16) 0.0000(10)
C5 0.086(19) 0.086(19) 0.086(19) 0.0000(10) 0.011(3) 0.0001(10)
_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 O21 1.707(16) . ?
W1 O23 1.837(16) . ?
W1 O20 1.908(16) . ?
W1 O22 1.960(14) . ?
W1 O18 2.013(16) . ?
W1 O19 2.323(15) . ?
W2 O9 1.706(14) . ?
W2 O2 1.828(15) . ?
W2 O20 1.906(16) . ?
W2 O7 1.914(18) . ?
W2 O11 2.006(16) . ?
W2 O26 2.300(14) . ?
W3 O5 1.709(17) . ?
W3 O3 1.851(17) . ?
W3 O6 1.891(5) . ?
W3 O7 1.937(17) . ?
W3 O8 1.989(19) . ?
W3 O26 2.344(18) . ?
W4 O14 1.721(18) . ?
W4 O13 1.78(2) . ?
W4 O11 1.857(15) . ?
W4 O16 1.929(18) . ?
W4 O15 1.927(13) . ?
W4 O12 2.289(16) . ?
W5 O17 1.70(2) . ?
W5 O18 1.894(19) 6_565 ?
W5 O18 1.894(19) . ?
W5 O16 1.917(17) . ?
W5 O16 1.917(17) 6_565 ?
W5 O19 2.35(2) . ?
W6 O10 1.68(3) . ?
W6 O8 1.828(18) 6_565 ?
W6 O8 1.828(18) . ?
W6 O13 1.95(2) 6_565 ?
W6 O13 1.95(2) . ?
W6 O12 2.43(2) . ?
W7 O1 1.844(5) . ?
W7 O4 1.929(8) . ?
W7 O23 1.942(16) . ?
W7 O3 1.948(17) . ?
W7 O2 2.016(14) . ?
W7 O26 2.366(15) . ?
Cu1 N3 1.97(4) . ?
Cu1 N1 1.97(3) . ?
Cu1 N2 2.00(2) . ?
Cu1 N4 2.14(3) . ?
P1 O26 1.609(15) 6_565 ?
P1 O26 1.609(15) . ?
P1 O12 1.63(2) . ?
P1 O19 1.69(2) . ?
O1 Cu3 1.844(5) 6_565 ?
O1 W7 1.844(5) 6_565 ?
O4 Cu3 1.929(8) 2_656 ?
O4 W7 1.929(8) 2_656 ?
O6 W3 1.891(5) 6_565 ?
O12 W4 2.289(16) 6_565 ?
O15 W4 1.927(13) 6_565 ?
O19 W1 2.323(15) 6_565 ?
O22 W1 1.960(14) 6_565 ?
C1 N1 1.49(5) . ?
C1 C2 1.48(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.52(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.33(5) . ?
C3 N3 1.51(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.55(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
Cu2 N5 2.00(4) 2_757 ?
Cu2 N5 2.00(4) . ?
Cu2 N5 2.00(4) 6_565 ?
Cu2 N5 2.00(4) 5_767 ?
N5 C5 1.14(7) . ?
N5 H5C 0.9000 . ?
N5 H5D 0.9000 . ?
C5 C5 1.53(13) 6_565 ?
C5 H5B 0.9700 . ?
C5 H5A 0.9700 . ?
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
O21 W1 O23 101.8(8) . . ?
O21 W1 O20 103.1(8) . . ?
O23 W1 O20 91.5(7) . . ?
O21 W1 O22 97.4(9) . . ?
O23 W1 O22 91.3(8) . . ?
O20 W1 O22 158.3(8) . . ?
O21 W1 O18 96.9(9) . . ?
O23 W1 O18 161.1(8) . . ?
O20 W1 O18 86.2(7) . . ?
O22 W1 O18 84.1(8) . . ?
O21 W1 O19 165.6(8) . . ?
O23 W1 O19 89.5(7) . . ?
O20 W1 O19 85.1(6) . . ?
O22 W1 O19 73.4(8) . . ?
O18 W1 O19 71.6(8) . . ?
O9 W2 O2 101.8(8) . . ?
O9 W2 O20 101.7(8) . . ?
O2 W2 O20 90.0(7) . . ?
O9 W2 O7 101.0(8) . . ?
O2 W2 O7 89.1(7) . . ?
O20 W2 O7 157.0(7) . . ?
O9 W2 O11 96.6(7) . . ?
O2 W2 O11 161.6(6) . . ?
O20 W2 O11 85.2(6) . . ?
O7 W2 O11 88.4(7) . . ?
O9 W2 O26 174.3(8) . . ?
O2 W2 O26 79.9(6) . . ?
O20 W2 O26 83.7(6) . . ?
O7 W2 O26 73.6(7) . . ?
O11 W2 O26 81.9(5) . . ?
O5 W3 O3 100.2(8) . . ?
O5 W3 O6 103.0(9) . . ?
O3 W3 O6 91.6(8) . . ?
O5 W3 O7 98.2(8) . . ?
O3 W3 O7 91.3(7) . . ?
O6 W3 O7 157.7(8) . . ?
O5 W3 O8 100.8(9) . . ?
O3 W3 O8 159.0(8) . . ?
O6 W3 O8 83.1(8) . . ?
O7 W3 O8 86.3(8) . . ?
O5 W3 O26 168.8(7) . . ?
O3 W3 O26 74.8(6) . . ?
O6 W3 O26 87.3(7) . . ?
O7 W3 O26 72.2(6) . . ?
O8 W3 O26 84.6(7) . . ?
O14 W4 O13 103.1(10) . . ?
O14 W4 O11 99.6(7) . . ?
O13 W4 O11 88.0(8) . . ?
O14 W4 O16 103.0(10) . . ?
O13 W4 O16 153.8(8) . . ?
O11 W4 O16 89.0(7) . . ?
O14 W4 O15 100.6(9) . . ?
O13 W4 O15 92.0(10) . . ?
O11 W4 O15 159.3(8) . . ?
O16 W4 O15 82.0(9) . . ?
O14 W4 O12 172.5(9) . . ?
O13 W4 O12 72.1(9) . . ?
O11 W4 O12 86.2(6) . . ?
O16 W4 O12 81.8(8) . . ?
O15 W4 O12 74.2(8) . . ?
O17 W5 O18 98.8(8) . 6_565 ?
O17 W5 O18 98.8(8) . . ?
O18 W5 O18 86.9(10) 6_565 . ?
O17 W5 O16 102.3(8) . . ?
O18 W5 O16 158.9(8) 6_565 . ?
O18 W5 O16 89.5(8) . . ?
O17 W5 O16 102.3(8) . 6_565 ?
O18 W5 O16 89.5(8) 6_565 6_565 ?
O18 W5 O16 158.9(8) . 6_565 ?
O16 W5 O16 86.5(10) . 6_565 ?
O17 W5 O19 168.2(10) . . ?
O18 W5 O19 72.9(6) 6_565 . ?
O18 W5 O19 72.9(6) . . ?
O16 W5 O19 86.1(7) . . ?
O16 W5 O19 86.1(7) 6_565 . ?
O10 W6 O8 103.3(10) . 6_565 ?
O10 W6 O8 103.3(10) . . ?
O8 W6 O8 87.7(12) 6_565 . ?
O10 W6 O13 104.3(9) . 6_565 ?
O8 W6 O13 82.9(9) 6_565 6_565 ?
O8 W6 O13 152.2(9) . 6_565 ?
O10 W6 O13 104.3(9) . . ?
O8 W6 O13 152.2(9) 6_565 . ?
O8 W6 O13 82.9(9) . . ?
O13 W6 O13 93.4(12) 6_565 . ?
O10 W6 O12 165.2(12) . . ?
O8 W6 O12 87.2(7) 6_565 . ?
O8 W6 O12 87.2(8) . . ?
O13 W6 O12 66.3(7) 6_565 . ?
O13 W6 O12 66.3(7) . . ?
O1 W7 O4 100.6(9) . . ?
O1 W7 O23 91.4(8) . . ?
O4 W7 O23 101.2(5) . . ?
O1 W7 O3 95.8(9) . . ?
O4 W7 O3 98.4(5) . . ?
O23 W7 O3 157.5(7) . . ?
O1 W7 O2 163.0(8) . . ?
O4 W7 O2 96.4(7) . . ?
O23 W7 O2 84.2(6) . . ?
O3 W7 O2 82.7(7) . . ?
O1 W7 O26 88.5(8) . . ?
O4 W7 O26 168.0(6) . . ?
O23 W7 O26 86.3(7) . . ?
O3 W7 O26 72.7(7) . . ?
O2 W7 O26 74.8(5) . . ?
N3 Cu1 N1 177.1(15) . . ?
N3 Cu1 N2 97.1(13) . . ?
N1 Cu1 N2 85.7(12) . . ?
N3 Cu1 N4 76.6(14) . . ?
N1 Cu1 N4 100.7(14) . . ?
N2 Cu1 N4 172.6(12) . . ?
O26 P1 O26 112.2(12) 6_565 . ?
O26 P1 O12 109.4(7) 6_565 . ?
O26 P1 O12 109.4(7) . . ?
O26 P1 O19 108.9(8) 6_565 . ?
O26 P1 O19 108.9(8) . . ?
O12 P1 O19 108.0(11) . . ?
Cu3 O1 W7 0.00(9) 6_565 6_565 ?
Cu3 O1 W7 156.6(13) 6_565 . ?
W7 O1 W7 156.6(13) 6_565 . ?
W2 O2 W7 116.0(7) . . ?
W3 O3 W7 122.5(9) . . ?
Cu3 O4 W7 0.00(9) 2_656 2_656 ?
Cu3 O4 W7 137.3(11) 2_656 . ?
W7 O4 W7 137.3(11) 2_656 . ?
W3 O6 W3 153.2(12) 6_565 . ?
W2 O7 W3 120.7(9) . . ?
W6 O8 W3 149.6(11) . . ?
W4 O11 W2 158.6(8) . . ?
P1 O12 W4 126.1(7) . . ?
P1 O12 W4 126.1(7) . 6_565 ?
W4 O12 W4 92.9(8) . 6_565 ?
P1 O12 W6 119.4(12) . . ?
W4 O12 W6 91.2(7) . . ?
W4 O12 W6 91.2(7) 6_565 . ?
W4 O13 W6 129.4(11) . . ?
W4 O15 W4 118.8(13) 6_565 . ?
W4 O16 W5 145.3(10) . . ?
W5 O18 W1 121.6(10) . . ?
P1 O19 W1 122.8(6) . 6_565 ?
P1 O19 W1 122.8(6) . . ?
W1 O19 W1 93.5(8) 6_565 . ?
P1 O19 W5 122.1(11) . . ?
W1 O19 W5 93.8(6) 6_565 . ?
W1 O19 W5 93.8(6) . . ?
W2 O20 W1 140.3(9) . . ?
W1 O22 W1 119.4(14) 6_565 . ?
W1 O23 W7 141.5(9) . . ?
P1 O26 W2 128.3(9) . . ?
P1 O26 W3 124.9(9) . . ?
W2 O26 W3 92.2(5) . . ?
P1 O26 W7 121.7(8) . . ?
W2 O26 W7 88.6(5) . . ?
W3 O26 W7 90.0(5) . . ?
N1 C1 C2 109(3) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
C1 C2 N2 109(3) . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
N2 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 N3 85(4) . . ?
C4 C3 H3A 114.5 . . ?
N3 C3 H3A 114.5 . . ?
C4 C3 H3B 114.5 . . ?
N3 C3 H3B 114.5 . . ?
H3A C3 H3B 111.6 . . ?
C3 C4 N4 135(4) . . ?
C3 C4 H4A 103.3 . . ?
N4 C4 H4A 103.3 . . ?
C3 C4 H4B 103.3 . . ?
N4 C4 H4B 103.3 . . ?
H4A C4 H4B 105.2 . . ?
C1 N1 Cu1 111(2) . . ?
C1 N1 H1C 109.4 . . ?
Cu1 N1 H1C 109.4 . . ?
C1 N1 H1D 109.4 . . ?
Cu1 N1 H1D 109.4 . . ?
H1C N1 H1D 108.0 . . ?
C2 N2 Cu1 108.4(19) . . ?
C2 N2 H2C 110.0 . . ?
Cu1 N2 H2C 110.0 . . ?
C2 N2 H2D 110.0 . . ?
Cu1 N2 H2D 110.0 . . ?
H2C N2 H2D 108.4 . . ?
C3 N3 Cu1 132(3) . . ?
C3 N3 H3C 104.3 . . ?
Cu1 N3 H3C 104.3 . . ?
C3 N3 H3D 104.3 . . ?
Cu1 N3 H3D 104.3 . . ?
H3C N3 H3D 105.6 . . ?
C4 N4 Cu1 96(3) . . ?
C4 N4 H4C 112.5 . . ?
Cu1 N4 H4C 112.5 . . ?
C4 N4 H4D 112.5 . . ?
Cu1 N4 H4D 112.5 . . ?
H4C N4 H4D 110.0 . . ?
N5 Cu2 N5 96(2) 2_757 . ?
N5 Cu2 N5 180.000(7) 2_757 6_565 ?
N5 Cu2 N5 84(2) . 6_565 ?
N5 Cu2 N5 84(2) 2_757 5_767 ?
N5 Cu2 N5 180.000(11) . 5_767 ?
N5 Cu2 N5 96(2) 6_565 5_767 ?
C5 N5 Cu2 108(4) . . ?
C5 N5 H5C 110.0 . . ?
Cu2 N5 H5C 110.0 . . ?
C5 N5 H5D 110.0 . . ?
Cu2 N5 H5D 110.0 . . ?
H5C N5 H5D 108.4 . . ?
N5 C5 C5 120(4) . 6_565 ?
N5 C5 H5B 107.3 . . ?
C5 C5 H5B 107.3 6_565 . ?
N5 C5 H5A 107.3 . . ?
C5 C5 H5A 107.3 6_565 . ?
H5B C5 H5A 106.9 . . ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         5.793
_refine_diff_density_min         -2.594
_refine_diff_density_rms         0.431