# 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_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H104 N24 Ni5 O73 P2 W19'
_chemical_formula_weight         5757.96

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   P2(1)3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.4954(13)
_cell_length_b                   21.4954(13)
_cell_length_c                   21.4954(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9932.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5866
_cell_measurement_theta_min      1.34
_cell_measurement_theta_max      25.01

_exptl_crystal_description       block
_exptl_crystal_colour            'dark blue'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10328
_exptl_absorpt_coefficient_mu    22.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0859
_exptl_absorpt_correction_T_max  0.1040
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50204
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5866
_reflns_number_gt                5011
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID AUTO'
_computing_cell_refinement       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
The restraint command 'isor' was employed to restrain several C and O atoms 
c6 c8 c9 o26 so as to avoid the ADP and NPD problems on them. Such refinement
led to the restraint value of 24. That the {P2W18O62} moiety has P1 and P2 
on a threefold axis, that the [WO4{Ni(en)2(H2O)}3] moiety has W7 and O5
on a threefold axis, that the [Ni(en)3] moieties with Ni1 and Ni3 have the Ni 
atoms on threefold axes, that the carbonate moiety has C9 on a threefold axis,
and finally that the water oxygen OW1 also lies on a threefold axis.
;

_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^)+(0.0509P)^2^+90.6199P] 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     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(19)
_refine_ls_number_reflns         5866
_refine_ls_number_parameters     446
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.154
_refine_ls_shift/su_mean         0.003

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 0.55920(4) 0.58512(3) 1.17060(3) 0.03248(18) Uani 1 1 d . . .
W2 W 0.65935(4) 0.48726(4) 1.06660(4) 0.03387(19) Uani 1 1 d . . .
W3 W 0.42609(4) 0.69468(4) 1.17337(4) 0.03459(19) Uani 1 1 d . . .
W4 W 0.53430(4) 0.69261(4) 1.03952(4) 0.03514(19) Uani 1 1 d . . .
W5 W 0.63395(4) 0.59407(4) 0.93582(4) 0.03663(19) Uani 1 1 d . . .
W6 W 0.68981(3) 0.43330(4) 0.90521(4) 0.03302(18) Uani 1 1 d . . .
W7 W 0.99307(4) 0.00693(4) 0.50693(4) 0.0425(4) Uani 1 3 d S . .
P1 P 0.43117(18) 0.56883(18) 1.06883(18) 0.0190(14) Uani 1 3 d S . .
P2 P 0.5382(2) 0.4618(2) 0.9618(2) 0.0220(15) Uani 1 3 d S . .
Ni1 Ni 0.86313(12) 0.36313(12) 1.13687(12) 0.0355(10) Uani 1 3 d S . .
Ni2 Ni 1.10257(13) 0.08682(13) 0.60900(12) 0.0444(7) Uani 1 1 d . . .
Ni3 Ni 0.75659(14) 0.24341(14) 0.74341(14) 0.0449(12) Uani 1 3 d S . .
O1 O 0.7304(6) 0.5000(6) 1.0996(6) 0.044(3) Uani 1 1 d . . .
O2 O 0.6763(6) 0.3458(6) 0.9196(6) 0.036(3) Uani 1 1 d . . .
O3 O 1.0284(8) 0.1331(9) 0.6579(8) 0.075(5) Uani 1 1 d . . .
O4 O 1.0386(10) 0.0285(9) 0.5708(10) 0.097(7) Uani 1 1 d . . .
O5 O 1.0378(13) -0.0378(13) 0.4622(13) 0.142(17) Uani 1 3 d S . .
O6 O 0.4713(6) 0.7155(5) 1.1016(6) 0.034(3) Uani 1 1 d . . .
O7 O 0.5664(6) 0.6398(5) 1.1008(6) 0.033(3) Uani 1 1 d . . .
O8 O 0.4800(5) 0.5383(6) 1.1115(5) 0.031(3) Uani 1 1 d . . .
O9 O 0.3882(5) 0.6118(5) 1.1118(5) 0.024(4) Uani 1 3 d S . .
O10 O 0.6110(5) 0.5281(5) 1.1283(5) 0.029(3) Uani 1 1 d . . .
O11 O 0.6418(6) 0.4087(6) 1.1068(6) 0.044(3) Uani 1 1 d . . .
O12 O 0.5236(6) 0.5212(6) 1.2217(5) 0.033(3) Uani 1 1 d . . .
O13 O 0.5829(6) 0.6509(6) 0.9790(5) 0.035(3) Uani 1 1 d . . .
O14 O 0.5808(5) 0.4192(5) 0.9192(5) 0.028(5) Uani 1 3 d S . .
O15 O 0.6502(6) 0.5564(6) 1.0142(6) 0.036(3) Uani 1 1 d . . .
O16 O 0.6119(6) 0.6157(6) 1.2217(6) 0.037(3) Uani 1 1 d . . .
O17 O 0.3708(7) 0.6470(6) 1.2258(5) 0.039(3) Uani 1 1 d . . .
O18 O 0.5644(6) 0.4554(5) 1.0276(5) 0.032(3) Uani 1 1 d . . .
O19 O 0.4900(5) 0.6395(5) 1.1956(6) 0.030(3) Uani 1 1 d . . .
O20 O 0.6890(6) 0.4421(5) 0.9929(6) 0.037(3) Uani 1 1 d . . .
O21 O 0.6972(7) 0.6403(7) 0.9241(7) 0.053(4) Uani 1 1 d . . .
O22 O 0.7677(6) 0.4326(6) 0.8878(6) 0.040(3) Uani 1 1 d . . .
O23 O 0.5797(6) 0.7584(6) 1.0491(7) 0.048(4) Uani 1 1 d . . .
O24 O 0.4399(7) 0.7573(6) 1.2210(6) 0.044(3) Uani 1 1 d . . .
O25 O 0.6717(6) 0.5166(5) 0.9010(6) 0.035(3) Uani 1 1 d . . .
OW1 O 0.8651(14) 0.1349(14) 0.6349(14) 0.141(17) Uani 1 3 d S . .
C1 C 0.8749(12) 0.2272(12) 0.8082(11) 0.064(7) Uani 1 1 d . . .
H1A H 0.9185 0.2372 0.8141 0.077 Uiso 1 1 calc R . .
H1B H 0.8696 0.1829 0.8149 0.077 Uiso 1 1 calc R . .
C2 C 0.9487(10) 0.2676(8) 1.1765(10) 0.046(5) Uani 1 1 d . . .
H2A H 0.9509 0.2821 1.2192 0.055 Uiso 1 1 calc R . .
H2B H 0.9652 0.2256 1.1752 0.055 Uiso 1 1 calc R . .
C3 C 0.8351(15) 0.2636(13) 0.8558(11) 0.078(9) Uani 1 1 d . . .
H3A H 0.8457 0.2509 0.8978 0.093 Uiso 1 1 calc R . .
H3B H 0.8430 0.3079 0.8519 0.093 Uiso 1 1 calc R . .
C4 C 1.1684(13) 0.0901(12) 0.4906(14) 0.081(9) Uani 1 1 d . . .
H4A H 1.1436 0.0661 0.4615 0.097 Uiso 1 1 calc R . .
H4B H 1.2096 0.0945 0.4728 0.097 Uiso 1 1 calc R . .
C5 C 0.9874(9) 0.3083(11) 1.1369(12) 0.060(7) Uani 1 1 d . . .
H5A H 0.9863 0.2943 1.0939 0.072 Uiso 1 1 calc R . .
H5B H 1.0302 0.3081 1.1510 0.072 Uiso 1 1 calc R . .
C6 C 1.167(3) 0.098(2) 0.725(2) 0.161(19) Uani 1 1 d U . .
H6A H 1.2053 0.1074 0.7464 0.194 Uiso 1 1 calc R . .
H6B H 1.1331 0.1135 0.7505 0.194 Uiso 1 1 calc R . .
C7 C 1.1616(13) 0.0367(13) 0.7224(12) 0.073(8) Uani 1 1 d . . .
H7A H 1.1480 0.0214 0.7626 0.088 Uiso 1 1 calc R . .
H7B H 1.2020 0.0187 0.7136 0.088 Uiso 1 1 calc R . .
C8 C 1.1399(16) 0.1538(16) 0.4970(17) 0.103(11) Uani 1 1 d U . .
H8A H 1.1717 0.1832 0.5097 0.123 Uiso 1 1 calc R . .
H8B H 1.1239 0.1670 0.4569 0.123 Uiso 1 1 calc R . .
N1 N 0.7688(9) 0.2503(9) 0.8432(9) 0.059(5) Uani 1 1 d . . .
H1C H 0.7448 0.2810 0.8585 0.071 Uiso 1 1 calc R . .
H1D H 0.7576 0.2144 0.8616 0.071 Uiso 1 1 calc R . .
N2 N 0.9601(9) 0.3717(9) 1.1426(10) 0.058(5) Uani 1 1 d . . .
H2C H 0.9742 0.3964 1.1118 0.069 Uiso 1 1 calc R . .
H2D H 0.9709 0.3888 1.1792 0.069 Uiso 1 1 calc R . .
N3 N 1.1176(9) 0.0167(9) 0.6750(8) 0.057(5) Uani 1 1 d . . .
H3C H 1.0813 0.0066 0.6931 0.069 Uiso 1 1 calc R . .
H3D H 1.1324 -0.0175 0.6558 0.069 Uiso 1 1 calc R . .
N4 N 0.8823(9) 0.2668(8) 1.1559(9) 0.053(5) Uani 1 1 d . . .
H4C H 0.8573 0.2522 1.1861 0.064 Uiso 1 1 calc R . .
H4D H 0.8774 0.2434 1.1216 0.064 Uiso 1 1 calc R . .
N5 N 1.0918(9) 0.1540(8) 0.5405(8) 0.050(5) Uani 1 1 d . . .
H5C H 1.0554 0.1475 0.5207 0.060 Uiso 1 1 calc R . .
H5D H 1.0899 0.1917 0.5586 0.060 Uiso 1 1 calc R . .
N6 N 1.1735(9) 0.0554(8) 0.5482(9) 0.053(5) Uani 1 1 d . . .
H6C H 1.2111 0.0618 0.5655 0.064 Uiso 1 1 calc R . .
H6D H 1.1691 0.0145 0.5408 0.064 Uiso 1 1 calc R . .
N8 N 1.1666(12) 0.1365(12) 0.6617(11) 0.091(8) Uani 1 1 d . . .
H8C H 1.2044 0.1367 0.6436 0.109 Uiso 1 1 calc R . .
H8D H 1.1540 0.1760 0.6679 0.109 Uiso 1 1 calc R . .
N7 N 0.8563(10) 0.2431(10) 0.7440(11) 0.071(6) Uani 1 1 d . . .
H7C H 0.8710 0.2146 0.7170 0.085 Uiso 1 1 calc R . .
H7D H 0.8711 0.2807 0.7333 0.085 Uiso 1 1 calc R . .
C9 C 1.244(2) 0.256(2) 0.744(2) 0.1219(10) Uani 1 3 d SU . .
O26 O 1.199(4) 0.235(5) 0.799(4) 0.49(3) Uani 1 1 d U . .

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 0.0332(4) 0.0333(4) 0.0309(4) -0.0016(3) -0.0062(3) -0.0014(3)
W2 0.0305(4) 0.0341(4) 0.0369(4) -0.0019(3) -0.0071(3) 0.0012(3)
W3 0.0373(4) 0.0298(4) 0.0367(4) -0.0036(3) -0.0013(3) 0.0002(3)
W4 0.0347(4) 0.0300(4) 0.0406(5) 0.0036(3) -0.0020(3) -0.0037(3)
W5 0.0309(4) 0.0335(4) 0.0455(5) 0.0038(4) -0.0003(4) -0.0030(3)
W6 0.0285(4) 0.0340(4) 0.0365(4) 0.0009(3) -0.0005(3) -0.0002(3)
W7 0.0425(4) 0.0425(4) 0.0425(4) 0.0032(4) -0.0032(4) -0.0032(4)
P1 0.0190(14) 0.0190(14) 0.0190(14) -0.0004(17) 0.0004(17) 0.0004(17)
P2 0.0220(15) 0.0220(15) 0.0220(15) 0.0021(18) -0.0021(18) -0.0021(18)
Ni1 0.0355(10) 0.0355(10) 0.0355(10) -0.0038(11) -0.0038(11) 0.0038(11)
Ni2 0.0474(16) 0.0492(16) 0.0367(15) 0.0033(12) -0.0024(12) 0.0025(13)
Ni3 0.0449(12) 0.0449(12) 0.0449(12) 0.0064(13) -0.0064(13) -0.0064(13)
O1 0.044(8) 0.045(8) 0.044(8) 0.004(7) -0.011(6) -0.008(7)
O2 0.032(7) 0.033(7) 0.044(8) 0.002(6) -0.011(6) 0.006(6)
O3 0.072(12) 0.087(13) 0.064(11) -0.017(10) 0.025(9) 0.017(10)
O4 0.116(16) 0.077(13) 0.097(15) 0.010(12) -0.025(13) -0.047(12)
O5 0.142(17) 0.142(17) 0.142(17) -0.013(18) 0.013(18) 0.013(18)
O6 0.042(8) 0.028(7) 0.032(7) -0.010(5) 0.013(6) 0.001(6)
O7 0.024(6) 0.027(6) 0.047(8) -0.002(6) -0.003(6) 0.002(5)
O8 0.030(7) 0.036(7) 0.027(6) -0.009(5) 0.003(5) -0.006(5)
O9 0.024(4) 0.024(4) 0.024(4) 0.005(5) -0.005(5) -0.005(5)
O10 0.017(6) 0.036(7) 0.032(7) 0.001(6) -0.003(5) 0.005(5)
O11 0.055(9) 0.048(8) 0.029(7) -0.003(6) 0.002(6) 0.009(7)
O12 0.040(7) 0.036(7) 0.021(6) 0.002(5) -0.006(5) -0.001(6)
O13 0.033(7) 0.043(8) 0.027(7) 0.003(6) 0.006(5) 0.013(6)
O14 0.028(5) 0.028(5) 0.028(5) -0.011(5) 0.011(5) 0.011(5)
O15 0.043(8) 0.033(7) 0.034(7) 0.007(6) 0.002(6) -0.003(6)
O16 0.043(8) 0.033(7) 0.036(7) 0.004(6) -0.005(6) -0.009(6)
O17 0.063(9) 0.038(8) 0.017(6) 0.001(5) 0.001(6) -0.020(7)
O18 0.040(7) 0.028(6) 0.027(7) -0.005(5) -0.001(6) -0.001(5)
O19 0.033(7) 0.022(6) 0.036(7) -0.002(5) -0.007(6) 0.005(5)
O20 0.029(7) 0.025(6) 0.057(8) 0.000(6) -0.012(6) -0.005(5)
O21 0.043(8) 0.049(9) 0.067(10) 0.003(8) 0.009(8) -0.016(7)
O22 0.030(7) 0.037(8) 0.053(9) -0.002(6) 0.000(6) 0.004(6)
O23 0.042(8) 0.042(8) 0.059(10) -0.008(7) 0.009(7) -0.004(6)
O24 0.063(9) 0.035(8) 0.035(7) -0.015(6) 0.000(7) -0.005(7)
O25 0.039(7) 0.022(6) 0.042(8) -0.003(5) 0.000(6) 0.001(6)
OW1 0.141(17) 0.141(17) 0.141(17) 0.00(2) 0.00(2) 0.00(2)
C1 0.063(16) 0.074(17) 0.056(15) -0.009(13) -0.026(13) 0.022(13)
C2 0.061(14) 0.019(9) 0.058(14) -0.010(9) -0.021(11) 0.009(9)
C3 0.14(3) 0.066(17) 0.028(12) -0.005(11) -0.015(15) -0.009(18)
C4 0.071(18) 0.067(17) 0.10(2) 0.015(16) 0.050(17) 0.025(15)
C5 0.023(10) 0.077(17) 0.080(17) -0.020(14) 0.022(11) 0.004(11)
C6 0.16(2) 0.16(2) 0.16(2) 0.000(10) -0.006(10) 0.003(10)
C7 0.073(18) 0.08(2) 0.064(17) 0.025(15) -0.007(14) -0.020(15)
C8 0.105(14) 0.098(13) 0.105(13) 0.009(9) 0.014(9) 0.008(9)
N1 0.061(13) 0.056(12) 0.060(13) 0.021(10) -0.007(10) -0.003(10)
N2 0.056(12) 0.055(12) 0.063(13) -0.013(10) 0.000(10) 0.003(10)
N3 0.059(12) 0.071(13) 0.043(11) 0.009(10) -0.012(9) -0.013(10)
N4 0.064(13) 0.043(11) 0.053(12) -0.022(9) -0.005(10) 0.010(9)
N5 0.063(12) 0.048(11) 0.038(10) 0.019(8) 0.024(9) 0.000(9)
N6 0.059(12) 0.039(10) 0.061(12) 0.001(9) 0.009(10) 0.017(9)
N8 0.094(18) 0.093(18) 0.087(18) -0.046(15) -0.040(15) 0.011(15)
N7 0.064(14) 0.055(13) 0.093(17) 0.012(12) -0.020(12) -0.018(11)
C9 0.1219(10) 0.1219(10) 0.1219(10) 0.0000(6) 0.0000(6) 0.0000(6)
O26 0.49(3) 0.49(3) 0.49(3) 0.0000(10) 0.0000(10) 0.0000(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 O16 1.709(13) . ?
W1 O10 1.890(12) . ?
W1 O7 1.913(12) . ?
W1 O12 1.918(12) . ?
W1 O19 1.966(12) . ?
W1 O8 2.352(11) . ?
W2 O1 1.706(13) . ?
W2 O15 1.875(12) . ?
W2 O10 1.900(12) . ?
W2 O11 1.935(14) . ?
W2 O20 1.965(13) . ?
W2 O18 2.309(12) . ?
W3 O24 1.718(12) . ?
W3 O6 1.876(12) . ?
W3 O19 1.877(11) . ?
W3 O17 1.931(12) . ?
W3 O17 1.954(12) 10_646 ?
W3 O9 2.365(11) . ?
W4 O23 1.732(14) . ?
W4 O7 1.870(12) . ?
W4 O13 1.894(12) . ?
W4 O12 1.913(12) 10_646 ?
W4 O6 1.965(11) . ?
W4 O8 2.377(12) 10_646 ?
W5 O21 1.702(13) . ?
W5 O13 1.887(12) . ?
W5 O15 1.902(12) . ?
W5 O11 1.922(14) 10_646 ?
W5 O25 1.997(12) . ?
W5 O18 2.394(12) 10_646 ?
W6 O22 1.716(12) . ?
W6 O25 1.835(12) . ?
W6 O20 1.894(13) . ?
W6 O2 1.928(12) . ?
W6 O2 1.935(12) 10_646 ?
W6 O14 2.381(10) . ?
W7 O5 1.67(5) . ?
W7 O4 1.75(2) . ?
W7 O4 1.75(2) 10_646 ?
W7 O4 1.75(2) 7_665 ?
P1 O8 1.540(13) . ?
P1 O8 1.540(13) 10_646 ?
P1 O8 1.540(13) 7_665 ?
P1 O9 1.60(2) . ?
P2 O18 1.530(12) . ?
P2 O18 1.530(12) 10_646 ?
P2 O18 1.530(12) 7_665 ?
P2 O14 1.586(19) . ?
Ni1 N2 2.096(19) . ?
Ni1 N2 2.096(19) 8_746 ?
Ni1 N2 2.096(19) 11_567 ?
Ni1 N4 2.150(17) 8_746 ?
Ni1 N4 2.150(17) . ?
Ni1 N4 2.150(18) 11_567 ?
Ni2 O4 2.034(19) . ?
Ni2 N5 2.075(16) . ?
Ni2 N8 2.08(2) . ?
Ni2 N3 2.096(18) . ?
Ni2 N6 2.119(17) . ?
Ni2 O3 2.154(16) . ?
Ni3 N7 2.14(2) . ?
Ni3 N7 2.14(2) 10_646 ?
Ni3 N7 2.14(2) 7_665 ?
Ni3 N1 2.17(2) 7_665 ?
Ni3 N1 2.17(2) 10_646 ?
Ni3 N1 2.17(2) . ?
O2 W6 1.935(12) 7_665 ?
O8 W4 2.377(12) 7_665 ?
O9 W3 2.365(11) 10_646 ?
O9 W3 2.365(11) 7_665 ?
O11 W5 1.922(14) 7_665 ?
O12 W4 1.913(12) 7_665 ?
O14 W6 2.381(10) 7_665 ?
O14 W6 2.381(10) 10_646 ?
O17 W3 1.954(12) 7_665 ?
O18 W5 2.394(12) 7_665 ?
C1 N7 1.48(3) . ?
C1 C3 1.55(3) . ?
C2 C5 1.48(3) . ?
C2 N4 1.49(3) . ?
C3 N1 1.48(3) . ?
C4 N6 1.45(3) . ?
C4 C8 1.51(4) . ?
C5 N2 1.49(3) . ?
C6 C7 1.32(5) . ?
C6 N8 1.59(5) . ?
C7 N3 1.45(3) . ?
C8 N5 1.40(3) . ?
C9 O26 1.61(8) 6_566 ?
C9 O26 1.60(8) . ?
C9 O26 1.60(8) 12_664 ?

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
O16 W1 O10 99.7(6) . . ?
O16 W1 O7 102.3(5) . . ?
O10 W1 O7 88.5(5) . . ?
O16 W1 O12 99.9(5) . . ?
O10 W1 O12 92.6(5) . . ?
O7 W1 O12 157.2(5) . . ?
O16 W1 O19 95.6(6) . . ?
O10 W1 O19 164.4(5) . . ?
O7 W1 O19 84.8(5) . . ?
O12 W1 O19 88.2(5) . . ?
O16 W1 O8 172.7(5) . . ?
O10 W1 O8 83.6(4) . . ?
O7 W1 O8 84.1(5) . . ?
O12 W1 O8 73.4(4) . . ?
O19 W1 O8 81.6(5) . . ?
O1 W2 O15 102.5(6) . . ?
O1 W2 O10 97.2(6) . . ?
O15 W2 O10 89.8(5) . . ?
O1 W2 O11 97.4(6) . . ?
O15 W2 O11 160.0(6) . . ?
O10 W2 O11 89.1(5) . . ?
O1 W2 O20 97.1(6) . . ?
O15 W2 O20 86.6(5) . . ?
O10 W2 O20 165.7(5) . . ?
O11 W2 O20 89.5(5) . . ?
O1 W2 O18 171.6(5) . . ?
O15 W2 O18 85.7(5) . . ?
O10 W2 O18 84.6(4) . . ?
O11 W2 O18 74.4(5) . . ?
O20 W2 O18 81.3(4) . . ?
O24 W3 O6 102.3(6) . . ?
O24 W3 O19 102.5(6) . . ?
O6 W3 O19 88.9(5) . . ?
O24 W3 O17 100.0(6) . . ?
O6 W3 O17 157.5(5) . . ?
O19 W3 O17 88.1(6) . . ?
O24 W3 O17 99.3(6) . 10_646 ?
O6 W3 O17 86.3(6) . 10_646 ?
O19 W3 O17 158.2(5) . 10_646 ?
O17 W3 O17 88.3(8) . 10_646 ?
O24 W3 O9 169.8(6) . . ?
O6 W3 O9 84.1(5) . . ?
O19 W3 O9 85.3(5) . . ?
O17 W3 O9 73.4(5) . . ?
O17 W3 O9 73.1(5) 10_646 . ?
O23 W4 O7 101.7(6) . . ?
O23 W4 O13 99.1(6) . . ?
O7 W4 O13 89.6(5) . . ?
O23 W4 O12 99.7(6) . 10_646 ?
O7 W4 O12 158.2(5) . 10_646 ?
O13 W4 O12 90.6(5) . 10_646 ?
O23 W4 O6 95.9(6) . . ?
O7 W4 O6 85.9(5) . . ?
O13 W4 O6 164.9(5) . . ?
O12 W4 O6 88.3(5) 10_646 . ?
O23 W4 O8 172.1(6) . 10_646 ?
O7 W4 O8 85.5(4) . 10_646 ?
O13 W4 O8 83.9(5) . 10_646 ?
O12 W4 O8 72.9(4) 10_646 10_646 ?
O6 W4 O8 81.4(5) . 10_646 ?
O21 W5 O13 99.1(6) . . ?
O21 W5 O15 103.5(7) . . ?
O13 W5 O15 87.0(5) . . ?
O21 W5 O11 99.7(7) . 10_646 ?
O13 W5 O11 93.3(5) . 10_646 ?
O15 W5 O11 156.5(5) . 10_646 ?
O21 W5 O25 96.2(6) . . ?
O13 W5 O25 163.8(5) . . ?
O15 W5 O25 84.4(5) . . ?
O11 W5 O25 89.3(5) 10_646 . ?
O21 W5 O18 171.4(6) . 10_646 ?
O13 W5 O18 85.4(5) . 10_646 ?
O15 W5 O18 84.0(5) . 10_646 ?
O11 W5 O18 72.6(5) 10_646 10_646 ?
O25 W5 O18 80.1(4) . 10_646 ?
O22 W6 O25 101.8(6) . . ?
O22 W6 O20 103.1(6) . . ?
O25 W6 O20 87.1(5) . . ?
O22 W6 O2 100.0(6) . . ?
O25 W6 O2 158.1(5) . . ?
O20 W6 O2 86.4(5) . . ?
O22 W6 O2 100.8(6) . 10_646 ?
O25 W6 O2 91.2(6) . 10_646 ?
O20 W6 O2 155.9(5) . 10_646 ?
O2 W6 O2 86.4(7) . 10_646 ?
O22 W6 O14 170.6(6) . . ?
O25 W6 O14 85.5(5) . . ?
O20 W6 O14 83.0(4) . . ?
O2 W6 O14 73.0(4) . . ?
O2 W6 O14 72.9(4) 10_646 . ?
O5 W7 O4 106.4(8) . . ?
O5 W7 O4 106.4(8) . 10_646 ?
O4 W7 O4 112.3(7) . 10_646 ?
O5 W7 O4 106.4(8) . 7_665 ?
O4 W7 O4 112.3(7) . 7_665 ?
O4 W7 O4 112.3(7) 10_646 7_665 ?
O8 P1 O8 111.6(5) . 10_646 ?
O8 P1 O8 111.6(4) . 7_665 ?
O8 P1 O8 111.6(4) 10_646 7_665 ?
O8 P1 O9 107.2(5) . . ?
O8 P1 O9 107.2(5) 10_646 . ?
O8 P1 O9 107.2(5) 7_665 . ?
O18 P2 O18 113.0(4) . 10_646 ?
O18 P2 O18 113.0(4) . 7_665 ?
O18 P2 O18 113.0(4) 10_646 7_665 ?
O18 P2 O14 105.7(5) . . ?
O18 P2 O14 105.7(5) 10_646 . ?
O18 P2 O14 105.7(5) 7_665 . ?
N2 Ni1 N2 88.6(9) . 8_746 ?
N2 Ni1 N2 88.6(9) . 11_567 ?
N2 Ni1 N2 88.6(9) 8_746 11_567 ?
N2 Ni1 N4 96.7(7) . 8_746 ?
N2 Ni1 N4 83.3(7) 8_746 8_746 ?
N2 Ni1 N4 170.2(7) 11_567 8_746 ?
N2 Ni1 N4 83.3(7) . . ?
N2 Ni1 N4 170.2(7) 8_746 . ?
N2 Ni1 N4 96.7(7) 11_567 . ?
N4 Ni1 N4 92.2(7) 8_746 . ?
N2 Ni1 N4 170.2(7) . 11_567 ?
N2 Ni1 N4 96.7(7) 8_746 11_567 ?
N2 Ni1 N4 83.3(7) 11_567 11_567 ?
N4 Ni1 N4 92.2(7) 8_746 11_567 ?
N4 Ni1 N4 92.2(7) . 11_567 ?
O4 Ni2 N5 93.8(8) . . ?
O4 Ni2 N8 170.0(10) . . ?
N5 Ni2 N8 95.9(10) . . ?
O4 Ni2 N3 86.2(8) . . ?
N5 Ni2 N3 176.7(8) . . ?
N8 Ni2 N3 84.2(9) . . ?
O4 Ni2 N6 92.4(9) . . ?
N5 Ni2 N6 82.2(7) . . ?
N8 Ni2 N6 91.3(9) . . ?
N3 Ni2 N6 94.4(7) . . ?
O4 Ni2 O3 88.9(9) . . ?
N5 Ni2 O3 86.6(7) . . ?
N8 Ni2 O3 89.3(9) . . ?
N3 Ni2 O3 96.7(8) . . ?
N6 Ni2 O3 168.9(7) . . ?
N7 Ni3 N7 90.2(9) . 10_646 ?
N7 Ni3 N7 90.2(9) . 7_665 ?
N7 Ni3 N7 90.2(9) 10_646 7_665 ?
N7 Ni3 N1 171.7(8) . 7_665 ?
N7 Ni3 N1 94.2(7) 10_646 7_665 ?
N7 Ni3 N1 82.7(8) 7_665 7_665 ?
N7 Ni3 N1 94.2(7) . 10_646 ?
N7 Ni3 N1 82.7(8) 10_646 10_646 ?
N7 Ni3 N1 171.7(8) 7_665 10_646 ?
N1 Ni3 N1 93.5(8) 7_665 10_646 ?
N7 Ni3 N1 82.7(8) . . ?
N7 Ni3 N1 171.7(8) 10_646 . ?
N7 Ni3 N1 94.2(7) 7_665 . ?
N1 Ni3 N1 93.5(8) 7_665 . ?
N1 Ni3 N1 93.5(8) 10_646 . ?
W6 O2 W6 123.1(6) . 7_665 ?
W7 O4 Ni2 149.2(12) . . ?
W3 O6 W4 148.8(7) . . ?
W4 O7 W1 153.5(7) . . ?
P1 O8 W1 129.2(7) . . ?
P1 O8 W4 126.6(6) . 7_665 ?
W1 O8 W4 90.7(4) . 7_665 ?
P1 O9 W3 124.0(4) . . ?
P1 O9 W3 124.0(4) . 10_646 ?
W3 O9 W3 91.7(6) . 10_646 ?
P1 O9 W3 124.0(4) . 7_665 ?
W3 O9 W3 91.7(6) . 7_665 ?
W3 O9 W3 91.7(6) 10_646 7_665 ?
W1 O10 W2 163.3(7) . . ?
W5 O11 W2 121.5(7) 7_665 . ?
W4 O12 W1 122.8(6) 7_665 . ?
W5 O13 W4 164.8(7) . . ?
P2 O14 W6 124.5(3) . . ?
P2 O14 W6 124.5(3) . 7_665 ?
W6 O14 W6 91.0(5) . 7_665 ?
P2 O14 W6 124.5(3) . 10_646 ?
W6 O14 W6 91.0(5) . 10_646 ?
W6 O14 W6 91.0(5) 7_665 10_646 ?
W2 O15 W5 152.7(7) . . ?
W3 O17 W3 121.7(6) . 7_665 ?
P2 O18 W2 129.4(7) . . ?
P2 O18 W5 128.5(6) . 7_665 ?
W2 O18 W5 91.3(4) . 7_665 ?
W3 O19 W1 149.3(7) . . ?
W6 O20 W2 148.8(7) . . ?
W6 O25 W5 151.8(7) . . ?
N7 C1 C3 110.6(19) . . ?
C5 C2 N4 111.9(18) . . ?
N1 C3 C1 108(2) . . ?
N6 C4 C8 115(2) . . ?
C2 C5 N2 105.8(16) . . ?
C7 C6 N8 119(4) . . ?
C6 C7 N3 112(3) . . ?
N5 C8 C4 111(3) . . ?
C3 N1 Ni3 108.1(15) . . ?
C5 N2 Ni1 107.8(13) . . ?
C7 N3 Ni2 111.2(15) . . ?
C2 N4 Ni1 103.2(12) . . ?
C8 N5 Ni2 113.0(18) . . ?
C4 N6 Ni2 108.0(13) . . ?
C6 N8 Ni2 102(2) . . ?
C1 N7 Ni3 106.1(16) . . ?
O26 C9 O26 114(4) 6_566 . ?
O26 C9 O26 114(4) 6_566 12_664 ?
O26 C9 O26 114(4) . 12_664 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         3.298
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.246
_database_code_depnum_ccdc_archive 'CCDC 912033'