Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222

_publ_contact_author             
# Name and address of author for correspondence
;
Dr A. Dolbecq
Institut Lavoisier, IREM, UMR CNRS 8180
Universit\'e de Versailles Saint-Quentin-en-Yvelines
45 Avenue des Etats Unis
78035 Versailles cedex
France
;
_publ_contact_author_phone       '(33) 1 39 25 43 83'
_publ_contact_author_fax         '(33) 1 39 25 43 81'
_publ_contact_author_email       dolbecq@chimie.uvsq.fr

_publ_section_title              
;
Square versus tetrahedral iron clusters
with polyoxometalates ligands
;

# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.

loop_
_publ_author_name
_publ_author_address

C.Pichon
; Institut Lavoisier, IREM, UMR CNRS 8180
Universit\'e de Versailles Saint-Quentin-en-Yvelines
45 Avenue des Etats Unis
78035 Versailles cedex
France
;
A.Dolbecq
; Institut Lavoisier, IREM, UMR CNRS 8637
Universit\'e de Versailles Saint-Quentin-en-Yvelines
45 Avenue des Etats Unis
78035 Versailles cedex
France
;
P.Mialane
; Institut Lavoisier, IREM, UMR CNRS 8637
Universit\'e de Versailles Saint-Quentin-en-Yvelines
45 Avenue des Etats Unis
78035 Versailles cedex
France
;
J.Marrot
; Institut Lavoisier, IREM, UMR CNRS 8637
Universit\'e de Versailles Saint-Quentin-en-Yvelines
45 Avenue des Etats Unis
78035 Versailles cedex
France
;
E.Riviere
; Institut de Chimie Mol\'eculaire et des Mat\'eriaux dOrsay, UMR 8182
Universit\'e Paris-Sud
91405 Orsay
France
;
F.Secheresse
; Institut Lavoisier, IREM, UMR CNRS 8637
Universit\'e de Versailles Saint-Quentin-en-Yvelines
45 Avenue des Etats Unis
78035 Versailles cedex
France
;

#====================================================================

_publ_section_references         
;
Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure
determination. Univ. of G\"ottingen, Federal Republic of Germany.

Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal
structures. Univ. of G\"ottingen, Federal Republic of Germany.
;
_publ_contact_author_name        'Dr A. Dolbecq'

#====================================================================

data_1
_database_code_depnum_ccdc_archive 'CCDC 661377'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H198 Fe13 N22 O202 P8 W36'
_chemical_formula_weight         11596.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
P P 0.1023 0.0942 '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'
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'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   I-43m

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

_cell_length_a                   21.1011(4)
_cell_length_b                   21.1011(4)
_cell_length_c                   21.1011(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     9395.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5520
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      25.97

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.099
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10444
_exptl_absorpt_coefficient_mu    23.110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0906
_exptl_absorpt_correction_T_max  0.3912
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
'Blessing, Acta Cryst. (1995) A51, 33-38'
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36795
_diffrn_reflns_av_R_equivalents  0.1095
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         30.31
_reflns_number_total             2598
_reflns_number_gt                2062
_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.
There is a discrepancy between the formulae determined by elemental analysis
and the formulae deduced from the crystallographic atom list because of the
difficulty in locating all the disordered water molecules and cations,
a common feature among the structure of polyoxotungstates. The data set
was corrected with the program PLATON/SQUEEZE.
;

_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^)+(0.0434P)^2^+305.4734P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         2598
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1046
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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 0.77471(3) 0.64996(4) 0.77471(3) 0.02786(19) Uani 1 2 d S . .
W2 W 0.80965(3) 0.42852(3) 0.68659(3) 0.02708(14) Uani 1 1 d . . .
Fe1 Fe 0.64714(9) 0.46448(12) 0.64714(9) 0.0182(5) Uani 1 2 d S . .
Fe2 Fe 0.5474(5) 0.5474(5) 0.4526(5) 0.023(4) Uani 0.25 6 d SP . .
P1 P 0.8128(2) 0.8128(2) 0.8128(2) 0.0160(12) Uani 1 6 d S . .
O1 O 0.8268(4) 0.8268(4) 0.7420(6) 0.023(3) Uani 1 2 d S . .
O2 O 0.8546(7) 0.8546(7) 0.8546(7) 0.026(5) Uani 1 6 d S . .
O3 O 0.8604(5) 0.4906(5) 0.6928(6) 0.038(3) Uani 1 1 d . . .
O4 O 0.7466(6) 0.5824(7) 0.7466(6) 0.038(4) Uani 1 2 d S . .
O5 O 0.7862(7) 0.6984(4) 0.6984(4) 0.032(3) Uani 1 2 d S . .
O6 O 0.7399(4) 0.4595(5) 0.6484(4) 0.025(2) Uani 1 1 d . . .
O7 O 0.7742(5) 0.6350(5) 0.8624(5) 0.032(2) Uani 1 1 d . . .
O8 O 0.6369(4) 0.5543(6) 0.6369(4) 0.023(3) Uani 1 2 d S . .
O9 O 0.8397(7) 0.3925(4) 0.6075(4) 0.029(3) Uani 1 2 d S . .
O10 O 0.7672(4) 0.4276(7) 0.7672(4) 0.031(3) Uani 1 2 d S . .
O11 O 0.5522(5) 0.5522(5) 0.5522(5) 0.020(5) Uani 1 6 d S . .
O12 O 0.5540(4) 0.4460(4) 0.6462(7) 0.022(3) Uani 1 2 d S . .
P2 P 0.5942(2) 0.5942(2) 0.5942(2) 0.0204(16) Uani 1 6 d S . .
OW1 O 0.5000 0.5000 0.7597(10) 0.039(5) Uani 1 4 d S . .
OW2 O 0.5946(6) 0.5946(6) 0.7667(9) 0.050(5) Uani 1 2 d S . .
OW3 O 0.8869(12) 0.6306(11) 0.6306(11) 0.101(9) Uani 1 2 d S . .

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 0.0307(3) 0.0221(4) 0.0307(3) -0.0060(2) -0.0032(3) -0.0060(2)
W2 0.0223(3) 0.0265(3) 0.0325(3) 0.0022(2) -0.0057(2) -0.0003(2)
Fe1 0.0182(8) 0.0182(13) 0.0182(8) 0.0008(7) -0.0040(10) 0.0008(7)
Fe2 0.023(4) 0.023(4) 0.023(4) 0.000(4) 0.000(4) 0.000(4)
P1 0.0160(12) 0.0160(12) 0.0160(12) -0.0023(16) -0.0023(16) -0.0023(16)
O1 0.022(4) 0.022(4) 0.025(6) -0.003(3) -0.003(3) -0.008(5)
O2 0.026(5) 0.026(5) 0.026(5) 0.011(6) 0.011(6) 0.011(6)
O3 0.028(6) 0.043(6) 0.042(6) 0.007(5) -0.012(5) -0.011(5)
O4 0.046(6) 0.021(8) 0.046(6) -0.004(5) -0.003(7) -0.004(5)
O5 0.042(8) 0.027(4) 0.027(4) -0.013(6) -0.010(4) -0.010(4)
O6 0.019(5) 0.033(5) 0.025(5) 0.004(4) -0.002(4) 0.001(4)
O7 0.023(5) 0.029(5) 0.045(6) 0.005(5) 0.002(4) 0.001(4)
O8 0.027(4) 0.016(6) 0.027(4) -0.001(3) -0.010(5) -0.001(3)
O9 0.031(8) 0.028(5) 0.028(5) 0.007(6) -0.002(4) 0.002(4)
O10 0.030(5) 0.032(8) 0.030(5) 0.000(4) -0.011(6) 0.000(4)
O11 0.020(5) 0.020(5) 0.020(5) -0.006(5) -0.006(5) -0.006(5)
O12 0.019(4) 0.019(4) 0.027(7) -0.003(4) 0.003(4) -0.001(5)
P2 0.0204(16) 0.0204(16) 0.0204(16) 0.0025(18) 0.0025(18) 0.0025(18)
OW1 0.047(9) 0.047(9) 0.023(11) 0.000 0.000 -0.013(11)
OW2 0.046(6) 0.046(6) 0.059(12) -0.026(6) -0.026(6) 0.004(8)
OW3 0.072(18) 0.116(15) 0.116(15) 0.010(18) -0.017(11) -0.017(11)

_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 O4 1.654(15) . ?
W1 O7 1.877(11) . ?
W1 O7 1.877(11) 21 ?
W1 O5 1.922(4) 9 ?
W1 O5 1.922(4) . ?
W1 O1 2.488(12) 9 ?
W2 O3 1.696(10) . ?
W2 O6 1.801(9) . ?
W2 O10 1.923(4) . ?
W2 O9 1.941(7) . ?
W2 O7 1.999(11) 34_646 ?
W2 O1 2.424(9) 32_646 ?
Fe1 O8 1.919(13) . ?
Fe1 O6 1.960(9) 21 ?
Fe1 O6 1.960(9) . ?
Fe1 O12 2.003(7) . ?
Fe1 O12 2.003(7) 6_566 ?
Fe1 O2 2.319(15) 27_646 ?
Fe2 O12 2.10(2) 10_656 ?
Fe2 O12 2.10(2) 5 ?
Fe2 O12 2.096(19) 4_566 ?
Fe2 O11 2.105(16) . ?
Fe2 O11 2.105(16) 3_656 ?
Fe2 O11 2.105(16) 4_566 ?
Fe2 Fe2 2.83(3) 3_656 ?
Fe2 Fe2 2.83(3) 4_566 ?
Fe2 Fe2 2.83(3) 2_665 ?
P1 O2 1.53(3) . ?
P1 O1 1.551(13) . ?
P1 O1 1.551(13) 5 ?
P1 O1 1.551(13) 9 ?
O1 W2 2.424(9) 47_656 ?
O1 W2 2.424(9) 35_566 ?
O1 W1 2.488(12) 5 ?
O2 Fe1 2.319(15) 27_656 ?
O2 Fe1 2.319(15) 31_665 ?
O2 Fe1 2.319(15) 35_566 ?
O5 W1 1.922(4) 5 ?
O7 W2 1.999(11) 31_665 ?
O8 P2 1.528(13) . ?
O9 W2 1.941(7) 20_566 ?
O10 W2 1.923(4) 21 ?
O11 P2 1.53(2) . ?
O11 Fe2 2.105(16) 3_656 ?
O11 Fe2 2.105(16) 4_566 ?
O12 Fe1 2.003(7) 12_665 ?
O12 Fe2 2.096(19) 4_566 ?
P2 O8 1.528(13) 9 ?
P2 O8 1.528(13) 5 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 W1 O7 101.9(5) . . ?
O4 W1 O7 101.9(5) . 21 ?
O7 W1 O7 89.1(6) . 21 ?
O4 W1 O5 101.7(5) . 9 ?
O7 W1 O5 87.7(6) . 9 ?
O7 W1 O5 156.3(5) 21 9 ?
O4 W1 O5 101.7(5) . . ?
O7 W1 O5 156.3(5) . . ?
O7 W1 O5 87.7(6) 21 . ?
O5 W1 O5 85.9(9) 9 . ?
O4 W1 O1 171.9(6) . 9 ?
O7 W1 O1 72.5(4) . 9 ?
O7 W1 O1 72.5(4) 21 9 ?
O5 W1 O1 84.2(4) 9 9 ?
O5 W1 O1 84.2(4) . 9 ?
O3 W2 O6 105.7(5) . . ?
O3 W2 O10 103.5(6) . . ?
O6 W2 O10 91.1(5) . . ?
O3 W2 O9 99.3(6) . . ?
O6 W2 O9 91.4(5) . . ?
O10 W2 O9 155.4(6) . . ?
O3 W2 O7 98.0(5) . 34_646 ?
O6 W2 O7 156.4(5) . 34_646 ?
O10 W2 O7 84.2(5) . 34_646 ?
O9 W2 O7 83.8(5) . 34_646 ?
O3 W2 O1 167.5(5) . 32_646 ?
O6 W2 O1 84.3(4) . 32_646 ?
O10 W2 O1 83.4(5) . 32_646 ?
O9 W2 O1 72.5(4) . 32_646 ?
O7 W2 O1 72.1(4) 34_646 32_646 ?
O8 Fe1 O6 99.6(4) . 21 ?
O8 Fe1 O6 99.6(4) . . ?
O6 Fe1 O6 88.3(6) 21 . ?
O8 Fe1 O12 94.7(4) . . ?
O6 Fe1 O12 90.7(5) 21 . ?
O6 Fe1 O12 165.6(4) . . ?
O8 Fe1 O12 94.7(4) . 6_566 ?
O6 Fe1 O12 165.6(4) 21 6_566 ?
O6 Fe1 O12 90.7(5) . 6_566 ?
O12 Fe1 O12 86.8(8) . 6_566 ?
O8 Fe1 O2 169.6(7) . 27_646 ?
O6 Fe1 O2 87.8(5) 21 27_646 ?
O6 Fe1 O2 87.8(5) . 27_646 ?
O12 Fe1 O2 77.8(5) . 27_646 ?
O12 Fe1 O2 77.8(5) 6_566 27_646 ?
O12 Fe2 O12 82.0(8) 10_656 5 ?
O12 Fe2 O12 82.0(8) 10_656 4_566 ?
O12 Fe2 O12 82.0(8) 5 4_566 ?
O12 Fe2 O11 90.9(4) 10_656 . ?
O12 Fe2 O11 90.9(4) 5 . ?
O12 Fe2 O11 170.7(10) 4_566 . ?
O12 Fe2 O11 90.9(4) 10_656 3_656 ?
O12 Fe2 O11 170.7(10) 5 3_656 ?
O12 Fe2 O11 90.9(4) 4_566 3_656 ?
O11 Fe2 O11 95.4(8) . 3_656 ?
O12 Fe2 O11 170.6(10) 10_656 4_566 ?
O12 Fe2 O11 90.9(4) 5 4_566 ?
O12 Fe2 O11 90.9(4) 4_566 4_566 ?
O11 Fe2 O11 95.4(8) . 4_566 ?
O11 Fe2 O11 95.4(8) 3_656 4_566 ?
O12 Fe2 Fe2 95.5(5) 10_656 3_656 ?
O12 Fe2 Fe2 138.7(3) 5 3_656 ?
O12 Fe2 Fe2 138.7(3) 4_566 3_656 ?
O11 Fe2 Fe2 47.8(5) . 3_656 ?
O11 Fe2 Fe2 47.8(5) 3_656 3_656 ?
O11 Fe2 Fe2 93.9(6) 4_566 3_656 ?
O12 Fe2 Fe2 138.7(3) 10_656 4_566 ?
O12 Fe2 Fe2 95.5(5) 5 4_566 ?
O12 Fe2 Fe2 138.7(3) 4_566 4_566 ?
O11 Fe2 Fe2 47.8(5) . 4_566 ?
O11 Fe2 Fe2 93.9(6) 3_656 4_566 ?
O11 Fe2 Fe2 47.8(5) 4_566 4_566 ?
Fe2 Fe2 Fe2 60.0 3_656 4_566 ?
O12 Fe2 Fe2 138.7(3) 10_656 2_665 ?
O12 Fe2 Fe2 138.7(3) 5 2_665 ?
O12 Fe2 Fe2 95.5(5) 4_566 2_665 ?
O11 Fe2 Fe2 93.9(6) . 2_665 ?
O11 Fe2 Fe2 47.8(5) 3_656 2_665 ?
O11 Fe2 Fe2 47.8(5) 4_566 2_665 ?
Fe2 Fe2 Fe2 59.999(1) 3_656 2_665 ?
Fe2 Fe2 Fe2 60.0 4_566 2_665 ?
O2 P1 O1 109.6(5) . . ?
O2 P1 O1 109.6(5) . 5 ?
O1 P1 O1 109.3(5) . 5 ?
O2 P1 O1 109.6(5) . 9 ?
O1 P1 O1 109.3(5) . 9 ?
O1 P1 O1 109.3(5) 5 9 ?
P1 O1 W2 125.4(4) . 47_656 ?
P1 O1 W2 125.4(4) . 35_566 ?
W2 O1 W2 90.2(4) 47_656 35_566 ?
P1 O1 W1 125.7(7) . 5 ?
W2 O1 W1 89.3(4) 47_656 5 ?
W2 O1 W1 89.3(4) 35_566 5 ?
P1 O2 Fe1 124.0(5) . 27_656 ?
P1 O2 Fe1 124.0(5) . 31_665 ?
Fe1 O2 Fe1 91.8(8) 27_656 31_665 ?
P1 O2 Fe1 124.0(5) . 35_566 ?
Fe1 O2 Fe1 91.8(8) 27_656 35_566 ?
Fe1 O2 Fe1 91.8(8) 31_665 35_566 ?
W1 O5 W1 151.1(8) 5 . ?
W2 O6 Fe1 147.3(6) . . ?
W1 O7 W2 126.0(5) . 31_665 ?
P2 O8 Fe1 132.6(9) . . ?
W2 O9 W2 124.5(7) . 20_566 ?
W2 O10 W2 145.5(8) . 21 ?
P2 O11 Fe2 129.2(6) . 3_656 ?
P2 O11 Fe2 129.2(6) . . ?
Fe2 O11 Fe2 84.4(9) 3_656 . ?
P2 O11 Fe2 129.2(6) . 4_566 ?
Fe2 O11 Fe2 84.4(9) 3_656 4_566 ?
Fe2 O11 Fe2 84.4(9) . 4_566 ?
Fe1 O12 Fe1 112.5(6) . 12_665 ?
Fe1 O12 Fe2 93.6(5) . 4_566 ?
Fe1 O12 Fe2 93.6(5) 12_665 4_566 ?
O8 P2 O8 107.5(6) 9 5 ?
O8 P2 O8 107.5(6) 9 . ?
O8 P2 O8 107.5(6) 5 . ?
O8 P2 O11 111.3(6) 9 . ?
O8 P2 O11 111.3(6) 5 . ?
O8 P2 O11 111.3(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.31
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.710
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.286
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.113 -0.070 0.492 1920.7 678.8
_platon_squeeze_details          
;
;

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 661378'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H180 Fe8 K4 N24 O186 P4 W40'
_chemical_formula_weight         11863.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Fe Fe 0.3463 0.8444 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4/m

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

_cell_length_a                   29.0731(7)
_cell_length_b                   29.0731(7)
_cell_length_c                   10.5212(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8893.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5347
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      29.94

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10568
_exptl_absorpt_coefficient_mu    26.643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1425
_exptl_absorpt_correction_T_max  0.4158
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'

_exptl_special_details           
;
'Blessing, Acta Cryst. (1995) A51, 33-38'
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 512x512
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53716
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         0.99
_diffrn_reflns_theta_max         30.06
_reflns_number_total             6836
_reflns_number_gt                3709
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker APEX2'
_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.
There is a discrepancy between the formulae determined by elemental analysis
and the formulae deduced from the crystallographic atom list because of the
difficulty in locating all the disordered water molecules and cations,
a common feature among the structure of polyoxotungstates. The data set
was corrected with the program PLATON/SQUEEZE
;

_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^)+(0.1053P)^2^+216.1228P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6836
_refine_ls_number_parameters     285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.2243
_refine_ls_wR_factor_gt          0.2023
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.09142(3) 0.33338(2) 0.25976(6) 0.0443(2) Uani 1 1 d . . .
W2 W -0.01611(2) 0.27119(3) 0.26322(6) 0.0410(2) Uani 1 1 d . . .
W3 W 0.00891(4) 0.35697(3) 0.5000 0.0490(3) Uani 1 2 d S . .
W4 W 0.17421(3) 0.31097(4) 0.5000 0.0514(3) Uani 1 2 d S . .
W5 W 0.15195(2) 0.22513(3) 0.26331(6) 0.0458(2) Uani 1 1 d . . .
W6 W 0.04492(3) 0.16431(2) 0.26763(6) 0.0451(2) Uani 1 1 d . . .
Fe1 Fe -0.03818(8) 0.18972(9) 0.5000 0.0240(5) Uani 1 2 d S . .
Fe2 Fe 0.12955(9) 0.14424(9) 0.5000 0.0266(6) Uani 1 2 d S . .
P1 P 0.06838(12) 0.24912(12) 0.5000 0.0103(6) Uani 1 2 d S . .
O1 O 0.1038(5) 0.3733(5) 0.1462(13) 0.075(4) Uani 1 1 d . . .
O2 O 0.1225(6) 0.2818(5) 0.2014(16) 0.091(6) Uani 1 1 d . . .
O3 O 0.0374(5) 0.3067(6) 0.1994(16) 0.083(5) Uani 1 1 d . . .
O4 O 0.1407(6) 0.3443(5) 0.3780(15) 0.092(6) Uani 1 1 d . . .
O5 O 0.0550(5) 0.3688(6) 0.3778(14) 0.097(6) Uani 1 1 d . . .
O6 O 0.0470(7) 0.2866(7) 0.4125(17) 0.034(4) Uani 0.50 1 d P . .
O7 O 0.1072(6) 0.2712(7) 0.4159(18) 0.035(4) Uani 0.50 1 d P . .
O8 O -0.0547(5) 0.2852(6) 0.1475(13) 0.074(4) Uani 1 1 d . . .
O9 O -0.0499(6) 0.2378(5) 0.3723(15) 0.092(6) Uani 1 1 d . . .
O10 O 0.0160(6) 0.2210(5) 0.2000(16) 0.089(6) Uani 1 1 d . . .
O11 O -0.0232(5) 0.3224(6) 0.3763(15) 0.100(5) Uani 1 1 d . . .
O12 O 0.0302(6) 0.2282(6) 0.4159(17) 0.029(4) Uani 0.50 1 d P . .
O13 O -0.0197(7) 0.4105(7) 0.5000 0.095(9) Uani 1 2 d S . .
O14 O 0.2251(7) 0.3406(7) 0.5000 0.084(7) Uani 1 2 d S . .
O15 O 0.1849(6) 0.2658(6) 0.3755(16) 0.102(6) Uani 1 1 d . . .
O16 O 0.1908(4) 0.2166(6) 0.1456(12) 0.077(5) Uani 1 1 d . . .
O17 O 0.1658(6) 0.1790(6) 0.3685(14) 0.096(6) Uani 1 1 d . . .
O18 O 0.1003(5) 0.1968(6) 0.1951(14) 0.095(6) Uani 1 1 d . . .
O19 O 0.0890(7) 0.2121(7) 0.4100(16) 0.038(5) Uani 0.50 1 d P . .
O20 O 0.0341(6) 0.1269(5) 0.1458(12) 0.077(5) Uani 1 1 d . . .
O21 O 0.0846(6) 0.1308(6) 0.3662(15) 0.098(6) Uani 1 1 d . . .
O22 O -0.0060(6) 0.1568(5) 0.3668(15) 0.092(6) Uani 1 1 d . . .
O23 O -0.0909(6) 0.1600(8) 0.5000 0.101(10) Uani 1 2 d S . .
K1 K 0.06785(16) 0.24885(17) 0.0000 0.0389(10) Uani 1 2 d S . .
O1W O 0.2550(6) 0.2119(7) 0.5000 0.071(6) Uani 1 2 d S . .
O2W O -0.1140(7) 0.3066(10) 0.5000 0.109(9) Uani 1 2 d S . .
O3W O -0.0705(8) 0.3729(8) 0.0000 0.100(5) Uani 1 2 d S . .

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 0.0582(4) 0.0434(4) 0.0313(3) 0.0065(2) 0.0028(3) -0.0078(3)
W2 0.0375(4) 0.0597(4) 0.0259(3) 0.0053(3) -0.0036(2) 0.0053(3)
W3 0.0517(6) 0.0437(6) 0.0517(6) 0.000 0.000 0.0095(4)
W4 0.0376(5) 0.0678(7) 0.0488(6) 0.000 0.000 -0.0130(5)
W5 0.0387(4) 0.0710(5) 0.0276(3) 0.0027(3) 0.0063(2) 0.0087(3)
W6 0.0644(5) 0.0459(4) 0.0250(3) -0.0022(3) 0.0001(3) -0.0041(3)
Fe1 0.0221(13) 0.0296(13) 0.0203(12) 0.000 0.000 -0.0107(10)
Fe2 0.0341(14) 0.0241(13) 0.0216(13) 0.000 0.000 0.0106(10)
P1 0.0145(19) 0.0110(18) 0.0054(15) 0.000 0.000 0.0011(16)
O1 0.117(12) 0.064(8) 0.045(8) 0.018(6) -0.001(8) -0.026(8)
O2 0.123(13) 0.068(9) 0.081(10) -0.028(8) -0.067(10) 0.056(9)
O3 0.061(9) 0.106(12) 0.083(11) -0.047(9) 0.039(8) -0.028(8)
O4 0.120(14) 0.077(10) 0.078(11) -0.029(8) -0.045(10) 0.022(9)
O5 0.081(10) 0.140(15) 0.070(10) -0.070(10) 0.033(8) -0.059(10)
O6 0.043(11) 0.038(11) 0.021(9) 0.004(8) 0.002(8) -0.006(9)
O7 0.026(9) 0.044(11) 0.036(10) -0.011(9) -0.001(8) -0.016(8)
O8 0.060(8) 0.120(13) 0.041(7) 0.001(8) -0.007(6) 0.033(8)
O9 0.114(13) 0.079(10) 0.083(11) 0.030(8) 0.066(10) 0.035(9)
O10 0.110(12) 0.069(9) 0.087(11) 0.036(8) 0.073(10) 0.038(8)
O11 0.083(9) 0.122(11) 0.095(10) -0.079(10) 0.029(8) -0.066(8)
O12 0.032(10) 0.031(9) 0.024(9) -0.001(7) -0.014(7) -0.008(8)
O13 0.061(13) 0.049(12) 0.18(3) 0.000 0.000 0.012(10)
O14 0.053(12) 0.060(12) 0.14(2) 0.000 0.000 -0.010(9)
O15 0.113(13) 0.110(13) 0.084(12) -0.033(10) -0.061(10) 0.058(11)
O16 0.050(8) 0.141(14) 0.040(7) 0.000(8) 0.011(6) 0.024(8)
O17 0.094(11) 0.127(14) 0.067(10) 0.062(10) -0.036(9) -0.039(10)
O18 0.087(11) 0.139(15) 0.059(9) 0.062(10) -0.030(8) -0.042(10)
O19 0.051(12) 0.049(12) 0.013(8) 0.005(8) 0.004(8) -0.009(10)
O20 0.133(14) 0.069(9) 0.030(7) -0.013(6) -0.006(7) -0.017(9)
O21 0.092(11) 0.129(14) 0.073(10) 0.062(10) -0.037(9) -0.031(10)
O22 0.126(14) 0.069(9) 0.083(11) 0.034(8) 0.059(10) 0.036(9)
O23 0.043(11) 0.085(17) 0.17(3) 0.000 0.000 -0.025(11)
K1 0.042(3) 0.054(3) 0.0201(19) 0.000 0.000 0.000(2)
O1W 0.059(12) 0.071(13) 0.085(15) 0.000 0.000 0.017(10)
O2W 0.047(13) 0.15(2) 0.13(2) 0.000 0.000 -0.043(14)
O3W 0.083(9) 0.122(11) 0.095(10) -0.079(10) 0.029(8) -0.066(8)

_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 O1 1.704(12) . ?
W1 O2 1.855(13) . ?
W1 O3 1.863(14) . ?
W1 O4 1.925(15) . ?
W1 O5 1.929(14) . ?
W1 O6 2.470(18) . ?
W1 O7 2.48(2) . ?
W1 K1 3.739(3) . ?
W2 O8 1.705(12) . ?
W2 O9 1.796(13) . ?
W2 O10 1.855(13) . ?
W2 O11 1.916(13) . ?
W2 O3 1.984(13) . ?
W2 O12 2.440(17) . ?
W2 O6 2.456(19) . ?
W2 K1 3.748(3) . ?
W3 O13 1.765(19) . ?
W3 O5 1.889(14) . ?
W3 O5 1.889(14) 10_556 ?
W3 O11 1.891(12) . ?
W3 O11 1.891(12) 10_556 ?
W3 O6 2.50(2) . ?
W3 O6 2.50(2) 10_556 ?
W4 O14 1.714(19) . ?
W4 O4 1.880(15) 10_556 ?
W4 O4 1.880(15) . ?
W4 O15 1.882(15) . ?
W4 O15 1.882(15) 10_556 ?
W4 O7 2.431(17) . ?
W4 O7 2.431(17) 10_556 ?
W5 O16 1.694(12) . ?
W5 O17 1.784(14) . ?
W5 O18 1.856(15) . ?
W5 O15 1.925(16) . ?
W5 O2 1.968(12) . ?
W5 O19 2.424(18) . ?
W5 O7 2.463(19) . ?
W5 K1 3.759(3) . ?
W6 O20 1.711(12) . ?
W6 O22 1.824(14) . ?
W6 O21 1.831(14) . ?
W6 O10 1.983(14) . ?
W6 O18 2.017(14) . ?
W6 O19 2.413(19) . ?
W6 O12 2.464(18) . ?
W6 K1 3.797(3) . ?
Fe1 O23 1.759(18) . ?
Fe1 O22 1.938(14) . ?
Fe1 O22 1.938(14) 10_556 ?
Fe1 O9 1.968(15) 10_556 ?
Fe1 O9 1.968(15) . ?
Fe2 O23 1.786(18) 11_556 ?
Fe2 O21 1.961(15) 10_556 ?
Fe2 O21 1.961(15) . ?
Fe2 O17 2.012(14) 10_556 ?
Fe2 O17 2.012(14) . ?
P1 O12 1.544(16) 10_556 ?
P1 O12 1.544(16) . ?
P1 O19 1.55(2) . ?
P1 O19 1.55(2) 10_556 ?
P1 O6 1.557(19) 10_556 ?
P1 O6 1.557(19) . ?
P1 O7 1.572(19) 10_556 ?
P1 O7 1.572(19) . ?
O2 K1 2.817(14) . ?
O3 K1 2.830(13) . ?
O6 O12 1.77(3) . ?
O6 O7 1.81(3) . ?
O7 O7 1.77(4) 10_556 ?
O7 O19 1.80(3) . ?
O10 K1 2.712(12) . ?
O12 O12 1.77(3) 10_556 ?
O12 O19 1.77(3) . ?
O18 K1 2.720(13) . ?
O23 Fe2 1.786(18) 3 ?
K1 O10 2.712(12) 10 ?
K1 O18 2.720(13) 10 ?
K1 O2 2.817(14) 10 ?
K1 O3 2.830(13) 10 ?
K1 W1 3.739(3) 10 ?
K1 W2 3.748(3) 10 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 O2 102.4(8) . . ?
O1 W1 O3 102.8(7) . . ?
O2 W1 O3 87.8(7) . . ?
O1 W1 O4 100.6(8) . . ?
O2 W1 O4 89.1(6) . . ?
O3 W1 O4 156.5(8) . . ?
O1 W1 O5 101.8(8) . . ?
O2 W1 O5 155.7(8) . . ?
O3 W1 O5 88.8(6) . . ?
O4 W1 O5 84.5(7) . . ?
O1 W1 O6 160.3(7) . . ?
O2 W1 O6 91.5(8) . . ?
O3 W1 O6 63.4(7) . . ?
O4 W1 O6 93.4(7) . . ?
O5 W1 O6 65.7(7) . . ?
O1 W1 O7 156.9(7) . . ?
O2 W1 O7 62.7(7) . . ?
O3 W1 O7 94.5(7) . . ?
O4 W1 O7 63.6(6) . . ?
O5 W1 O7 93.7(8) . . ?
O6 W1 O7 42.8(6) . . ?
O1 W1 K1 88.5(5) . . ?
O2 W1 K1 46.9(4) . . ?
O3 W1 K1 47.3(4) . . ?
O4 W1 K1 135.8(5) . . ?
O5 W1 K1 136.1(4) . . ?
O6 W1 K1 91.0(4) . . ?
O7 W1 K1 92.3(4) . . ?
O8 W2 O9 103.1(8) . . ?
O8 W2 O10 105.2(8) . . ?
O9 W2 O10 94.5(6) . . ?
O8 W2 O11 100.8(8) . . ?
O9 W2 O11 88.0(7) . . ?
O10 W2 O11 152.5(8) . . ?
O8 W2 O3 98.6(8) . . ?
O9 W2 O3 157.9(8) . . ?
O10 W2 O3 83.9(7) . . ?
O11 W2 O3 83.7(6) . . ?
O8 W2 O12 162.9(7) . . ?
O9 W2 O12 66.7(7) . . ?
O10 W2 O12 63.7(7) . . ?
O11 W2 O12 92.7(7) . . ?
O3 W2 O12 93.2(7) . . ?
O8 W2 O6 154.7(7) . . ?
O9 W2 O6 95.7(8) . . ?
O10 W2 O6 89.9(8) . . ?
O11 W2 O6 62.7(7) . . ?
O3 W2 O6 62.4(6) . . ?
O12 W2 O6 42.3(6) . . ?
O8 W2 K1 86.7(5) . . ?
O9 W2 K1 137.3(5) . . ?
O10 W2 K1 43.2(4) . . ?
O11 W2 K1 131.5(4) . . ?
O3 W2 K1 47.9(4) . . ?
O12 W2 K1 92.2(5) . . ?
O6 W2 K1 91.0(4) . . ?
O13 W3 O5 100.0(8) . . ?
O13 W3 O5 100.0(8) . 10_556 ?
O5 W3 O5 85.8(9) . 10_556 ?
O13 W3 O11 103.7(8) . . ?
O5 W3 O11 88.7(6) . . ?
O5 W3 O11 156.2(9) 10_556 . ?
O13 W3 O11 103.7(8) . 10_556 ?
O5 W3 O11 156.2(9) . 10_556 ?
O5 W3 O11 88.7(6) 10_556 10_556 ?
O11 W3 O11 87.0(10) . 10_556 ?
O13 W3 O6 158.4(4) . . ?
O5 W3 O6 65.4(7) . . ?
O5 W3 O6 94.9(8) 10_556 . ?
O11 W3 O6 62.0(7) . . ?
O11 W3 O6 92.1(8) 10_556 . ?
O13 W3 O6 158.4(4) . 10_556 ?
O5 W3 O6 94.9(8) . 10_556 ?
O5 W3 O6 65.4(7) 10_556 10_556 ?
O11 W3 O6 92.1(8) . 10_556 ?
O11 W3 O6 62.0(7) 10_556 10_556 ?
O6 W3 O6 43.2(8) . 10_556 ?
O14 W4 O4 100.8(8) . 10_556 ?
O14 W4 O4 100.8(8) . . ?
O4 W4 O4 86.1(10) 10_556 . ?
O14 W4 O15 102.1(8) . . ?
O4 W4 O15 157.1(9) 10_556 . ?
O4 W4 O15 88.3(6) . . ?
O14 W4 O15 102.1(8) . 10_556 ?
O4 W4 O15 88.3(6) 10_556 10_556 ?
O4 W4 O15 157.1(9) . 10_556 ?
O15 W4 O15 88.2(11) . 10_556 ?
O14 W4 O7 158.7(5) . . ?
O4 W4 O7 94.5(8) 10_556 . ?
O4 W4 O7 65.3(7) . . ?
O15 W4 O7 63.1(7) . . ?
O15 W4 O7 93.1(8) 10_556 . ?
O14 W4 O7 158.7(5) . 10_556 ?
O4 W4 O7 65.3(7) 10_556 10_556 ?
O4 W4 O7 94.5(8) . 10_556 ?
O15 W4 O7 93.1(8) . 10_556 ?
O15 W4 O7 63.1(7) 10_556 10_556 ?
O7 W4 O7 42.7(9) . 10_556 ?
O16 W5 O17 101.1(8) . . ?
O16 W5 O18 101.0(8) . . ?
O17 W5 O18 95.1(7) . . ?
O16 W5 O15 101.9(8) . . ?
O17 W5 O15 88.2(7) . . ?
O18 W5 O15 155.7(8) . . ?
O16 W5 O2 99.8(8) . . ?
O17 W5 O2 158.9(8) . . ?
O18 W5 O2 83.8(8) . . ?
O15 W5 O2 84.6(6) . . ?
O16 W5 O19 161.0(7) . . ?
O17 W5 O19 70.0(8) . . ?
O18 W5 O19 64.3(7) . . ?
O15 W5 O19 94.6(8) . . ?
O2 W5 O19 90.8(8) . . ?
O16 W5 O7 155.3(7) . . ?
O17 W5 O7 97.1(8) . . ?
O18 W5 O7 93.8(7) . . ?
O15 W5 O7 61.9(6) . . ?
O2 W5 O7 62.0(7) . . ?
O19 W5 O7 43.2(7) . . ?
O16 W5 K1 85.5(5) . . ?
O17 W5 K1 137.9(5) . . ?
O18 W5 K1 43.2(4) . . ?
O15 W5 K1 131.5(5) . . ?
O2 W5 K1 47.1(4) . . ?
O19 W5 K1 90.4(5) . . ?
O7 W5 K1 92.1(4) . . ?
O20 W6 O22 101.7(8) . . ?
O20 W6 O21 101.6(8) . . ?
O22 W6 O21 97.1(7) . . ?
O20 W6 O10 100.5(8) . . ?
O22 W6 O10 87.8(6) . . ?
O21 W6 O10 155.9(8) . . ?
O20 W6 O18 99.3(8) . . ?
O22 W6 O18 157.0(8) . . ?
O21 W6 O18 87.7(6) . . ?
O10 W6 O18 79.3(7) . . ?
O20 W6 O19 158.4(8) . . ?
O22 W6 O19 98.4(8) . . ?
O21 W6 O19 67.7(7) . . ?
O10 W6 O19 88.2(8) . . ?
O18 W6 O19 62.7(6) . . ?
O20 W6 O12 157.3(7) . . ?
O22 W6 O12 65.6(7) . . ?
O21 W6 O12 98.7(7) . . ?
O10 W6 O12 61.8(6) . . ?
O18 W6 O12 91.4(7) . . ?
O19 W6 O12 42.6(6) . . ?
O20 W6 K1 83.6(5) . . ?
O22 W6 K1 130.1(5) . . ?
O21 W6 K1 130.8(5) . . ?
O10 W6 K1 43.1(4) . . ?
O18 W6 K1 43.6(4) . . ?
O19 W6 K1 89.7(4) . . ?
O12 W6 K1 90.7(4) . . ?
O23 Fe1 O22 100.3(8) . . ?
O23 Fe1 O22 100.2(8) . 10_556 ?
O22 Fe1 O22 92.6(10) . 10_556 ?
O23 Fe1 O9 101.4(8) . 10_556 ?
O22 Fe1 O9 158.1(8) . 10_556 ?
O22 Fe1 O9 86.6(6) 10_556 10_556 ?
O23 Fe1 O9 101.4(8) . . ?
O22 Fe1 O9 86.6(6) . . ?
O22 Fe1 O9 158.1(8) 10_556 . ?
O9 Fe1 O9 86.1(9) 10_556 . ?
O23 Fe2 O21 99.1(8) 11_556 10_556 ?
O23 Fe2 O21 99.1(8) 11_556 . ?
O21 Fe2 O21 91.8(10) 10_556 . ?
O23 Fe2 O17 100.2(8) 11_556 10_556 ?
O21 Fe2 O17 87.5(6) 10_556 10_556 ?
O21 Fe2 O17 160.6(8) . 10_556 ?
O23 Fe2 O17 100.2(8) 11_556 . ?
O21 Fe2 O17 160.6(8) 10_556 . ?
O21 Fe2 O17 87.5(6) . . ?
O17 Fe2 O17 86.9(9) 10_556 . ?
O12 P1 O12 69.9(14) 10_556 . ?
O12 P1 O19 110.7(10) 10_556 . ?
O12 P1 O19 69.9(10) . . ?
O12 P1 O19 69.9(10) 10_556 10_556 ?
O12 P1 O19 110.7(10) . 10_556 ?
O19 P1 O19 75.1(14) . 10_556 ?
O12 P1 O6 69.5(9) 10_556 10_556 ?
O12 P1 O6 109.1(10) . 10_556 ?
O19 P1 O6 178.6(10) . 10_556 ?
O19 P1 O6 106.2(10) 10_556 10_556 ?
O12 P1 O6 109.1(10) 10_556 . ?
O12 P1 O6 69.5(9) . . ?
O19 P1 O6 106.2(10) . . ?
O19 P1 O6 178.6(10) 10_556 . ?
O6 P1 O6 72.5(14) 10_556 . ?
O12 P1 O7 110.8(10) 10_556 10_556 ?
O12 P1 O7 178.9(10) . 10_556 ?
O19 P1 O7 110.4(11) . 10_556 ?
O19 P1 O7 70.3(10) 10_556 10_556 ?
O6 P1 O7 70.6(10) 10_556 10_556 ?
O6 P1 O7 109.5(10) . 10_556 ?
O12 P1 O7 178.9(10) 10_556 . ?
O12 P1 O7 110.8(10) . . ?
O19 P1 O7 70.3(10) . . ?
O19 P1 O7 110.4(11) 10_556 . ?
O6 P1 O7 109.5(10) 10_556 . ?
O6 P1 O7 70.6(10) . . ?
O7 P1 O7 68.5(13) 10_556 . ?
W1 O2 W5 141.2(10) . . ?
W1 O2 K1 104.4(5) . . ?
W5 O2 K1 102.1(5) . . ?
W1 O3 W2 139.6(10) . . ?
W1 O3 K1 103.7(5) . . ?
W2 O3 K1 100.8(5) . . ?
W4 O4 W1 137.9(9) . . ?
W3 O5 W1 136.9(10) . . ?
P1 O6 O12 54.9(8) . . ?
P1 O6 O7 55.1(9) . . ?
O12 O6 O7 91.7(12) . . ?
P1 O6 W2 123.3(10) . . ?
O12 O6 W2 68.4(8) . . ?
O7 O6 W2 133.7(11) . . ?
P1 O6 W1 124.1(10) . . ?
O12 O6 W1 133.4(11) . . ?
O7 O6 W1 69.0(9) . . ?
W2 O6 W1 94.3(6) . . ?
P1 O6 W3 122.1(10) . . ?
O12 O6 W3 131.0(11) . . ?
O7 O6 W3 128.6(11) . . ?
W2 O6 W3 93.1(7) . . ?
W1 O6 W3 91.2(6) . . ?
P1 O7 O7 55.8(6) . 10_556 ?
P1 O7 O19 54.4(8) . . ?
O7 O7 O19 92.0(8) 10_556 . ?
P1 O7 O6 54.3(8) . . ?
O7 O7 O6 91.1(8) 10_556 . ?
O19 O7 O6 87.2(11) . . ?
P1 O7 W4 124.4(10) . . ?
O7 O7 W4 68.7(5) 10_556 . ?
O19 O7 W4 134.6(12) . . ?
O6 O7 W4 131.8(11) . . ?
P1 O7 W5 121.6(10) . . ?
O7 O7 W5 130.7(5) 10_556 . ?
O19 O7 W5 67.2(9) . . ?
O6 O7 W5 129.3(10) . . ?
W4 O7 W5 94.2(6) . . ?
P1 O7 W1 122.5(10) . . ?
O7 O7 W1 131.4(4) 10_556 . ?
O19 O7 W1 128.1(10) . . ?
O6 O7 W1 68.2(8) . . ?
W4 O7 W1 92.5(6) . . ?
W5 O7 W1 93.6(7) . . ?
W2 O9 Fe1 136.5(9) . . ?
W2 O10 W6 137.6(9) . . ?
W2 O10 K1 108.9(6) . . ?
W6 O10 K1 106.9(5) . . ?
W3 O11 W2 142.0(10) . . ?
P1 O12 O6 55.6(8) . . ?
P1 O12 O12 55.0(7) . 10_556 ?
O6 O12 O12 91.2(8) . 10_556 ?
P1 O12 O19 55.3(8) . . ?
O6 O12 O19 89.2(12) . . ?
O12 O12 O19 92.0(8) 10_556 . ?
P1 O12 W2 124.9(9) . . ?
O6 O12 W2 69.3(8) . . ?
O12 O12 W2 131.2(4) 10_556 . ?
O19 O12 W2 130.1(10) . . ?
P1 O12 W6 122.3(10) . . ?
O6 O12 W6 131.6(11) . . ?
O12 O12 W6 129.3(4) 10_556 . ?
O19 O12 W6 67.1(9) . . ?
W2 O12 W6 93.7(6) . . ?
W4 O15 W5 140.6(10) . . ?
W5 O17 Fe2 133.3(10) . . ?
W5 O18 W6 135.0(8) . . ?
W5 O18 K1 109.0(6) . . ?
W6 O18 K1 105.6(6) . . ?
P1 O19 O12 54.8(8) . . ?
P1 O19 O7 55.3(9) . . ?
O12 O19 O7 91.8(12) . . ?
P1 O19 W6 124.9(11) . . ?
O12 O19 W6 70.2(9) . . ?
O7 O19 W6 136.7(11) . . ?
P1 O19 W5 124.9(11) . . ?
O12 O19 W5 135.1(11) . . ?
O7 O19 W5 69.6(9) . . ?
W6 O19 W5 95.5(6) . . ?
W6 O21 Fe2 136.1(11) . . ?
W6 O22 Fe1 138.2(10) . . ?
Fe1 O23 Fe2 179.6(15) . 3 ?
O10 K1 O10 101.7(9) 10 . ?
O10 K1 O18 127.8(5) 10 . ?
O10 K1 O18 56.1(5) . . ?
O10 K1 O18 56.1(5) 10 10 ?
O10 K1 O18 127.8(5) . 10 ?
O18 K1 O18 98.0(9) . 10 ?
O10 K1 O2 80.3(7) 10 10 ?
O10 K1 O2 177.2(5) . 10 ?
O18 K1 O2 124.1(5) . 10 ?
O18 K1 O2 54.9(5) 10 10 ?
O10 K1 O2 177.2(5) 10 . ?
O10 K1 O2 80.3(7) . . ?
O18 K1 O2 54.9(5) . . ?
O18 K1 O2 124.1(5) 10 . ?
O2 K1 O2 97.5(9) 10 . ?
O10 K1 O3 55.1(5) 10 10 ?
O10 K1 O3 125.3(5) . 10 ?
O18 K1 O3 177.0(5) . 10 ?
O18 K1 O3 83.1(6) 10 10 ?
O2 K1 O3 54.3(5) 10 10 ?
O2 K1 O3 122.1(5) . 10 ?
O10 K1 O3 125.3(5) 10 . ?
O10 K1 O3 55.1(5) . . ?
O18 K1 O3 83.1(6) . . ?
O18 K1 O3 177.0(5) 10 . ?
O2 K1 O3 122.1(5) 10 . ?
O2 K1 O3 54.3(5) . . ?
O3 K1 O3 95.7(8) 10 . ?
O10 K1 W1 74.4(4) 10 10 ?
O10 K1 W1 149.9(3) . 10 ?
O18 K1 W1 148.6(3) . 10 ?
O18 K1 W1 75.5(4) 10 10 ?
O2 K1 W1 28.7(3) 10 10 ?
O2 K1 W1 102.9(4) . 10 ?
O3 K1 W1 29.0(3) 10 10 ?
O3 K1 W1 102.0(4) . 10 ?
O10 K1 W1 149.9(3) 10 . ?
O10 K1 W1 74.4(4) . . ?
O18 K1 W1 75.5(4) . . ?
O18 K1 W1 148.6(3) 10 . ?
O2 K1 W1 102.9(4) 10 . ?
O2 K1 W1 28.7(3) . . ?
O3 K1 W1 102.0(4) 10 . ?
O3 K1 W1 29.0(3) . . ?
W1 K1 W1 93.94(11) 10 . ?
O10 K1 W2 27.9(3) 10 10 ?
O10 K1 W2 105.2(4) . 10 ?
O18 K1 W2 151.7(4) . 10 ?
O18 K1 W2 76.4(4) 10 10 ?
O2 K1 W2 75.7(4) 10 10 ?
O2 K1 W2 149.8(3) . 10 ?
O3 K1 W2 31.3(3) 10 10 ?
O3 K1 W2 104.0(4) . 10 ?
W1 K1 W2 57.68(4) 10 10 ?
W1 K1 W2 123.06(13) . 10 ?
O10 K1 W2 105.2(4) 10 . ?
O10 K1 W2 27.9(3) . . ?
O18 K1 W2 76.4(4) . . ?
O18 K1 W2 151.7(4) 10 . ?
O2 K1 W2 149.8(3) 10 . ?
O2 K1 W2 75.7(4) . . ?
O3 K1 W2 103.9(4) 10 . ?
O3 K1 W2 31.3(3) . . ?
W1 K1 W2 123.06(13) 10 . ?
W1 K1 W2 57.68(4) . . ?
W2 K1 W2 95.27(10) 10 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.06
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.542
_refine_diff_density_min         -4.541
_refine_diff_density_rms         0.496

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 -0.006 843.0 686.4
2 0.000 0.500 0.120 333.2 415.1
3 0.500 0.500 0.446 843.1 686.4
4 0.500 0.000 0.112 333.2 415.1
_platon_squeeze_details          
;
;

#===END