# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Mark Weller'
_publ_contact_author_email       MTW@SOTON.AC.UK

_publ_section_title              
;
Hydrothermal Routes to New Sodium Polytungstates
;
_publ_requested_category         FI
loop_
_publ_author_name
'Mark Weller'
'Kate V. Redrup'

# Attachment 'Na2[H10W12O42]-20H2O.cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2009-03-02 at 11:45:47
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : 2006kvb0012

data_2006kvb0012
_database_code_depnum_ccdc_archive 'CCDC 705467'

_audit_creation_date             2009-03-02T11:45:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
?
;
_chemical_formula_sum            'Na O31 W6'
_chemical_formula_weight         1622.09

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

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                   11.9865(4)
_cell_length_b                   14.0300(5)
_cell_length_c                   15.5104(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.588(2)
_cell_angle_gamma                90
_cell_volume                     2512.45(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)

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

_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    4.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2812
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    27.499
_exptl_absorpt_correction_type   multi-scan

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

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_number            31236
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             5765
_reflns_number_gt                4160
_reflns_threshold_expression     >2sigma(I)

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

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

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

_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.
;
_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^)+(0.0490P)^2^+0.0000P] 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_number_reflns         5765
_refine_ls_number_parameters     343
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.078
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.11
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.911
_refine_diff_density_min         -3.137
_refine_diff_density_rms         0.588

#----------------------------------------------------------------------------#
# 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
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.8495(8) 0.4703(6) 0.1411(5) 0.013(2) Uani 1 1 d . . .
O2 O 0.6664(8) 0.3669(6) 0.0251(6) 0.013(2) Uani 1 1 d . . .
O3 O 0.7418(8) 0.4534(5) -0.1115(6) 0.012(2) Uani 1 1 d . . .
O4 O 0.9085(8) 0.5533(5) 0.0204(5) 0.0076(18) Uani 1 1 d U . .
O5 O 0.6965(8) 0.5641(5) 0.0148(6) 0.0096(19) Uani 1 1 d . . .
OW7 O 0.4963(11) 0.2957(8) 0.3825(7) 0.043(3) Uani 1 1 d . . .
O6 O 1.0595(9) 0.8546(6) 0.1346(5) 0.015(2) Uani 1 1 d . . .
O7 O 0.8528(9) 0.6582(6) 0.1402(6) 0.016(2) Uani 1 1 d . . .
OW8 O 1.0068(10) 0.7785(7) 0.2963(7) 0.032(3) Uani 1 1 d . . .
O8 O 0.6801(8) 0.7601(6) 0.0175(6) 0.013(2) Uani 1 1 d . . .
OW9 O 0.1150(10) 0.4576(7) 0.5838(7) 0.031(3) Uani 1 1 d . . .
O9 O 0.9148(8) 0.7455(6) 0.0085(5) 0.0125(19) Uani 1 1 d . . .
OW10 O 0.4636(10) 0.4369(8) -0.1105(6) 0.031(3) Uani 1 1 d . . .
O10 O 0.7584(8) 0.6551(5) -0.1108(6) 0.0094(19) Uani 1 1 d . . .
O11 O 0.5804(8) 0.5691(5) -0.2388(6) 0.0108(19) Uani 1 1 d . . .
O12 O 0.7641(9) 0.6460(6) -0.2859(5) 0.015(2) Uani 1 1 d . . .
O13 O 0.7473(8) 0.4517(6) -0.2699(6) 0.0102(19) Uani 1 1 d . . .
O14 O 1.0792(8) 0.4598(6) 0.1592(6) 0.0117(19) Uani 1 1 d U . .
O15 O 1.4206(8) 0.6710(6) 0.2372(6) 0.015(2) Uani 1 1 d U . .
O16 O 1.2435(8) 0.7379(6) 0.2968(6) 0.016(2) Uani 1 1 d . . .
O17 O 1.2386(8) 0.7495(6) 0.1156(6) 0.0118(19) Uani 1 1 d U . .
O18 O 1.0785(8) 0.6541(6) 0.1497(5) 0.0120(19) Uani 1 1 d U . .
O19 O 1.0940(8) 0.8453(6) -0.0294(5) 0.0115(19) Uani 1 1 d . . .
O20 O 0.8937(8) 0.3515(5) 0.0183(5) 0.0088(18) Uani 1 1 d U . .
O21 O 1.0048(8) 0.5628(6) 0.2850(6) 0.012(2) Uani 1 1 d U . .
OW1 O 0.2923(9) 0.5621(6) -0.2605(7) 0.023(2) Uani 1 1 d . . .
OW2 O 0.2683(9) 0.3380(6) -0.2845(7) 0.025(2) Uani 1 1 d . . .
OW3 O 0.5153(10) 0.3135(8) 0.1269(7) 0.038(3) Uani 1 1 d . . .
OW4 O 0.8103(11) 0.9677(8) 0.0717(7) 0.036(3) Uani 1 1 d . . .
OW5 O 0.6469(11) 1.1320(8) 0.0402(7) 0.043(3) Uani 1 1 d . . .
OW6 O 0.4346(13) 0.4347(8) -0.4153(7) 0.043(3) Uani 1 1 d . . .
Na1 Na 0.4328(5) 0.4487(3) -0.2640(3) 0.0143(11) Uani 1 1 d . . .
W1 W 0.78114(5) 0.43589(3) 0.01459(3) 0.00854(13) Uani 1 1 d . . .
W2 W 0.78560(5) 0.67351(3) 0.01928(3) 0.00992(14) Uani 1 1 d . . .
W3 W 0.73386(5) 0.56930(3) -0.20812(3) 0.00912(13) Uani 1 1 d . . .
W4 W 1.26861(5) 0.66465(3) 0.21481(3) 0.00933(14) Uani 1 1 d . . .
W5 W 1.07569(5) 0.77258(3) 0.05635(3) 0.01001(14) Uani 1 1 d . . .
W6 W 0.98213(5) 0.55243(3) 0.17050(3) 0.00831(13) Uani 1 1 d . . .

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
O1 0.015(6) 0.013(4) 0.008(4) 0.000(4) -0.002(4) -0.003(4)
O2 0.012(5) 0.015(4) 0.012(4) 0.000(4) 0.001(4) -0.007(4)
O3 0.010(5) 0.011(4) 0.011(4) 0.001(3) -0.006(4) -0.002(4)
O4 0.007(2) 0.008(2) 0.0079(19) -0.0004(10) 0.0021(11) 0.0007(10)
O5 0.014(5) 0.009(4) 0.010(4) 0.000(3) 0.009(4) 0.003(4)
OW7 0.042(9) 0.044(7) 0.038(7) 0.004(6) 0.003(6) 0.017(6)
O6 0.023(6) 0.012(4) 0.007(4) 0.001(3) 0.001(4) -0.006(4)
O7 0.024(6) 0.012(4) 0.016(5) 0.000(4) 0.009(4) 0.001(4)
OW8 0.036(8) 0.027(6) 0.036(6) -0.005(5) 0.016(6) 0.000(5)
O8 0.002(5) 0.015(4) 0.022(5) -0.008(4) 0.002(4) -0.004(4)
OW9 0.034(8) 0.029(6) 0.027(6) -0.008(5) 0.001(5) -0.010(5)
O9 0.017(6) 0.009(4) 0.011(4) -0.002(3) 0.002(4) -0.001(4)
OW10 0.016(7) 0.062(8) 0.015(5) -0.010(5) 0.005(5) 0.011(5)
O10 0.005(5) 0.007(4) 0.017(4) -0.005(3) 0.004(4) -0.001(3)
O11 0.002(5) 0.012(4) 0.018(5) -0.003(4) 0.002(4) -0.001(3)
O12 0.024(6) 0.011(4) 0.009(4) -0.004(4) 0.004(4) 0.002(4)
O13 0.005(5) 0.014(4) 0.011(4) 0.002(3) 0.001(4) -0.003(4)
O14 0.006(4) 0.013(3) 0.015(3) 0.001(3) 0.001(3) -0.007(3)
O15 0.007(5) 0.017(4) 0.019(4) 0.003(4) 0.002(4) -0.001(3)
O16 0.005(5) 0.016(5) 0.023(5) 0.000(4) -0.005(4) -0.003(4)
O17 0.007(4) 0.013(3) 0.016(3) -0.001(3) 0.006(3) -0.004(3)
O18 0.007(4) 0.015(3) 0.012(3) -0.003(3) -0.001(3) -0.001(3)
O19 0.006(5) 0.015(4) 0.013(4) 0.005(4) 0.001(4) 0.000(4)
O20 0.009(4) 0.004(3) 0.011(3) 0.000(3) -0.002(3) -0.002(3)
O21 0.012(2) 0.013(2) 0.012(2) 0.0002(10) 0.0037(11) -0.0002(10)
OW1 0.018(6) 0.023(5) 0.028(6) -0.006(4) 0.004(5) -0.007(4)
OW2 0.019(7) 0.017(5) 0.035(6) 0.003(4) 0.003(5) 0.000(4)
OW3 0.025(8) 0.048(7) 0.041(7) 0.001(6) 0.007(6) 0.006(6)
OW4 0.049(9) 0.042(6) 0.019(5) -0.002(5) 0.015(6) -0.017(6)
OW5 0.039(9) 0.054(8) 0.032(6) 0.008(6) 0.003(6) 0.003(6)
OW6 0.066(11) 0.044(7) 0.024(6) -0.003(5) 0.017(6) -0.002(6)
Na1 0.015(3) 0.010(2) 0.019(3) -0.001(2) 0.006(2) 0.005(2)
W1 0.0069(3) 0.0092(2) 0.0093(2) -0.00059(19) 0.0018(2) -0.00064(19)
W2 0.0078(3) 0.0097(3) 0.0111(3) -0.0005(2) 0.0007(2) 0.0016(2)
W3 0.0073(3) 0.0092(2) 0.0099(2) 0.00040(19) 0.0006(2) 0.0007(2)
W4 0.0079(3) 0.0084(3) 0.0106(3) -0.00015(19) 0.0005(2) -0.0001(2)
W5 0.0102(3) 0.0081(2) 0.0105(2) 0.0005(2) 0.0007(2) 0.0002(2)
W6 0.0071(3) 0.0089(2) 0.0085(2) 0.00013(19) 0.0014(2) 0.00032(19)

#----------------------------------------------------------------------------#
# 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
O1 W6 1.916(9) . ?
O1 W1 1.972(8) . ?
O2 W1 1.726(9) . ?
O3 W1 1.900(8) . ?
O3 W3 2.196(8) . ?
O3 W4 2.284(8) 3_765 ?
O4 W1 2.231(8) . ?
O4 W2 2.236(8) . ?
O4 W6 2.258(8) . ?
O5 W2 1.861(8) . ?
O5 W1 2.065(8) . ?
O6 W5 1.720(8) . ?
O7 W2 1.844(9) . ?
O7 W6 2.105(9) . ?
O8 W2 1.748(9) . ?
O9 W2 1.894(9) . ?
O9 W5 1.909(9) . ?
OW10 Na1 2.315(11) . ?
O10 W3 1.891(8) . ?
O10 W2 1.972(8) . ?
O11 W3 1.772(9) . ?
O11 Na1 2.401(10) . ?
O12 W3 1.727(8) . ?
O13 W4 1.875(8) 3_765 ?
O13 W3 1.936(8) . ?
O14 W6 1.784(9) . ?
O14 W3 2.203(9) 3_765 ?
O15 W4 1.763(9) . ?
O15 Na1 2.385(10) 3_765 ?
O16 W4 1.723(9) . ?
O17 W4 1.902(8) . ?
O17 W5 1.949(9) . ?
O18 W6 1.916(9) . ?
O18 W5 2.199(8) . ?
O18 W4 2.236(9) . ?
O19 W5 1.736(8) . ?
O20 W1 1.784(8) . ?
O20 W5 2.176(8) 3_765 ?
O21 W6 1.730(8) . ?
OW1 Na1 2.328(12) . ?
OW2 Na1 2.462(11) . ?
OW6 Na1 2.361(12) . ?
Na1 O15 2.385(10) 3_765 ?
W3 O14 2.203(9) 3_765 ?
W4 O13 1.875(8) 3_765 ?
W4 O3 2.284(8) 3_765 ?
W5 O20 2.176(8) 3_765 ?

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
W6 O1 W1 118.7(4) . . ?
W1 O3 W3 138.7(4) . . ?
W1 O3 W4 125.5(4) . 3_765 ?
W3 O3 W4 94.2(3) . 3_765 ?
W1 O4 W2 96.6(3) . . ?
W1 O4 W6 96.4(3) . . ?
W2 O4 W6 94.9(3) . . ?
W2 O5 W1 116.2(5) . . ?
W2 O7 W6 113.8(4) . . ?
W2 O9 W5 146.8(5) . . ?
W3 O10 W2 148.0(4) . . ?
W3 O11 Na1 135.3(4) . . ?
W4 O13 W3 119.0(4) 3_765 . ?
W6 O14 W3 136.9(4) . 3_765 ?
W4 O15 Na1 132.3(4) . 3_765 ?
W4 O17 W5 115.7(4) . . ?
W6 O18 W5 140.4(5) . . ?
W6 O18 W4 124.1(4) . . ?
W5 O18 W4 94.6(3) . . ?
W1 O20 W5 138.4(4) . 3_765 ?
OW10 Na1 OW1 86.6(4) . . ?
OW10 Na1 OW6 167.1(5) . . ?
OW1 Na1 OW6 106.3(5) . . ?
OW10 Na1 O15 82.1(4) . 3_765 ?
OW1 Na1 O15 168.7(4) . 3_765 ?
OW6 Na1 O15 84.9(4) . 3_765 ?
OW10 Na1 O11 88.6(4) . . ?
OW1 Na1 O11 91.2(3) . . ?
OW6 Na1 O11 91.0(4) . . ?
O15 Na1 O11 89.5(4) 3_765 . ?
OW10 Na1 OW2 89.3(4) . . ?
OW1 Na1 OW2 82.8(4) . . ?
OW6 Na1 OW2 92.3(4) . . ?
O15 Na1 OW2 96.0(3) 3_765 . ?
O11 Na1 OW2 173.8(4) . . ?
O2 W1 O20 103.9(4) . . ?
O2 W1 O3 100.7(4) . . ?
O20 W1 O3 95.5(4) . . ?
O2 W1 O1 99.9(4) . . ?
O20 W1 O1 91.2(4) . . ?
O3 W1 O1 156.1(3) . . ?
O2 W1 O5 94.8(4) . . ?
O20 W1 O5 160.9(4) . . ?
O3 W1 O5 84.4(3) . . ?
O1 W1 O5 81.9(3) . . ?
O2 W1 O4 164.8(4) . . ?
O20 W1 O4 89.1(3) . . ?
O3 W1 O4 85.6(3) . . ?
O1 W1 O4 71.5(3) . . ?
O5 W1 O4 71.8(3) . . ?
O8 W2 O7 102.4(4) . . ?
O8 W2 O5 99.6(4) . . ?
O7 W2 O5 91.8(4) . . ?
O8 W2 O9 103.5(4) . . ?
O7 W2 O9 90.4(4) . . ?
O5 W2 O9 155.7(4) . . ?
O8 W2 O10 98.9(4) . . ?
O7 W2 O10 158.7(4) . . ?
O5 W2 O10 85.3(3) . . ?
O9 W2 O10 83.9(4) . . ?
O8 W2 O4 175.0(3) . . ?
O7 W2 O4 78.3(3) . . ?
O5 W2 O4 75.4(3) . . ?
O9 W2 O4 81.4(3) . . ?
O10 W2 O4 80.6(3) . . ?
O12 W3 O11 102.2(4) . . ?
O12 W3 O10 98.3(4) . . ?
O11 W3 O10 98.2(4) . . ?
O12 W3 O13 97.2(4) . . ?
O11 W3 O13 94.8(4) . . ?
O10 W3 O13 157.2(4) . . ?
O12 W3 O3 163.7(4) . . ?
O11 W3 O3 91.9(4) . . ?
O10 W3 O3 87.6(3) . . ?
O13 W3 O3 73.3(3) . . ?
O12 W3 O14 88.3(4) . 3_765 ?
O11 W3 O14 168.2(3) . 3_765 ?
O10 W3 O14 85.2(3) . 3_765 ?
O13 W3 O14 78.5(3) . 3_765 ?
O3 W3 O14 76.9(3) . 3_765 ?
O16 W4 O15 101.6(4) . . ?
O16 W4 O13 97.1(4) . 3_765 ?
O15 W4 O13 100.4(4) . 3_765 ?
O16 W4 O17 101.1(4) . . ?
O15 W4 O17 95.1(4) . . ?
O13 W4 O17 153.2(4) 3_765 . ?
O16 W4 O18 90.8(4) . . ?
O15 W4 O18 165.1(3) . . ?
O13 W4 O18 86.1(3) 3_765 . ?
O17 W4 O18 74.2(3) . . ?
O16 W4 O3 164.3(4) . 3_765 ?
O15 W4 O3 91.9(4) . 3_765 ?
O13 W4 O3 72.3(3) 3_765 3_765 ?
O17 W4 O3 85.6(3) . 3_765 ?
O18 W4 O3 77.2(3) . 3_765 ?
O6 W5 O19 102.0(4) . . ?
O6 W5 O9 96.5(4) . . ?
O19 W5 O9 98.1(4) . . ?
O6 W5 O17 93.9(4) . . ?
O19 W5 O17 98.2(4) . . ?
O9 W5 O17 158.4(3) . . ?
O6 W5 O20 167.8(3) . 3_765 ?
O19 W5 O20 89.4(3) . 3_765 ?
O9 W5 O20 86.0(3) . 3_765 ?
O17 W5 O20 80.0(3) . 3_765 ?
O6 W5 O18 91.5(3) . . ?
O19 W5 O18 165.0(4) . . ?
O9 W5 O18 86.6(3) . . ?
O17 W5 O18 74.2(3) . . ?
O20 W5 O18 76.7(3) 3_765 . ?
O21 W6 O14 103.6(4) . . ?
O21 W6 O18 100.1(4) . . ?
O14 W6 O18 95.0(4) . . ?
O21 W6 O1 100.7(4) . . ?
O14 W6 O1 93.4(4) . . ?
O18 W6 O1 155.0(4) . . ?
O21 W6 O7 94.2(4) . . ?
O14 W6 O7 162.1(4) . . ?
O18 W6 O7 83.0(4) . . ?
O1 W6 O7 81.8(4) . . ?
O21 W6 O4 165.7(4) . . ?
O14 W6 O4 89.2(3) . . ?
O18 W6 O4 84.8(3) . . ?
O1 W6 O4 71.9(3) . . ?
O7 W6 O4 72.9(3) . . ?

# Attachment 'Na5[H7W12O420]-20H2O.cif'

data_2007kvb0028mtw
_database_code_depnum_ccdc_archive 'CCDC 705468'

_chemical_compound_source        ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H40 Na5 O62 W12'
_chemical_formula_weight         3353.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
Na Na 0.0362 0.0249 '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           Triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8677(4)
_cell_length_b                   12.4370(4)
_cell_length_c                   12.5313(4)
_cell_angle_alpha                72.260(2)
_cell_angle_beta                 76.107(2)
_cell_angle_gamma                87.059(2)
_cell_volume                     1565.58(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6948
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Block
_exptl_crystal_colour            White
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1479
_exptl_absorpt_coefficient_mu    22.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2061
_exptl_absorpt_correction_T_max  0.6664
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 18726 reflections reduced R(int) from 0.1477 to 0.0872
Ratio of minimum to maximum apparent transmission: 0.478284
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28074
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5498
_reflns_number_gt                4392
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_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.

As with many hydrothermally synthesised compounds difficulties were
encountered during the structure refinement. Even though many crystals
were tried, all contained a secondary fragment that has affected the
intensities; this is in combination with a high absorption coefficient
makes correction difficult. Looking at the ellipsoids it is clear that the
portion of the structure around Na2 exhibits some disorder most likely due
to a growth defect. The structure is a layered one and diffuse electron
density was present between these layers in the form of partial lattice
waters; these were treated using the squeeze algorithm (SQUEEZE - Sluis,
P. v.d. & Spek, A. L. (1990) Acta Cryst. A46, 194-201.) as refinement of
these positions proved problematical. Due to the number of water molecules
there is an extensive hydrogen bonded network resulting in many close
contacts. The hydrogen atoms were not included in the refinement.
;

_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^)+(0.0727P)^2^+20.7159P] 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         5498
_refine_ls_number_parameters     358
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1278
_refine_ls_wR_factor_gt          0.1193
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_restrained_S_all      0.945
_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 1.03146(6) 0.26243(5) 1.06262(5) 0.01358(17) Uani 1 1 d . . .
W2 W 0.76133(6) 0.31771(5) 1.22835(5) 0.01483(17) Uani 1 1 d . . .
W3 W 0.73786(6) 0.32936(5) 0.93575(5) 0.01431(17) Uani 1 1 d . . .
W4 W 0.99835(6) 0.27036(5) 0.76916(5) 0.01455(17) Uani 1 1 d . . .
W5 W 1.26227(6) 0.38405(5) 0.77565(5) 0.01480(17) Uani 1 1 d . . .
W6 W 0.96684(6) 0.57007(5) 0.77083(5) 0.01337(17) Uani 1 1 d . . .
Na1 Na 0.7667(6) 0.6194(5) 0.5256(5) 0.0241(14) Uani 1 1 d . . .
Na2 Na 0.7575(11) 0.0189(9) 0.9283(10) 0.081(3) Uani 1 1 d . . .
Na3 Na 1.0000 0.0000 1.5000 0.046(3) Uani 1 2 d S . .
O1 O 1.0809(9) 0.2883(9) 1.1930(8) 0.019(2) Uani 1 1 d U . .
O2 O 1.0947(9) 0.1283(8) 1.0762(8) 0.016(2) Uani 1 1 d U . .
O3 O 0.9282(9) 0.2729(8) 0.9575(9) 0.017(2) Uani 1 1 d U . .
O4 O 0.9283(9) 0.4155(8) 1.0984(8) 0.011(2) Uani 1 1 d U . .
O5 O 0.8652(9) 0.2042(8) 1.1870(8) 0.015(2) Uani 1 1 d U . .
O6 O 0.6861(10) 0.5911(9) 0.3724(9) 0.022(2) Uani 1 1 d U . .
O7 O 0.8640(9) 0.3374(8) 1.3211(8) 0.016(2) Uani 1 1 d U . .
O8 O 0.6318(11) 0.2412(9) 1.3267(10) 0.026(3) Uani 1 1 d U . .
O9 O 0.7044(10) 0.4708(9) 1.2154(9) 0.022(2) Uani 1 1 d U . .
O10 O 0.7051(10) 0.3445(9) 1.0835(9) 0.020(2) Uani 1 1 d U . .
O11 O 0.6814(10) 0.1911(9) 0.9690(9) 0.022(2) Uani 1 1 d U . .
O12 O 0.6122(10) 0.4135(9) 0.8903(9) 0.021(2) Uani 1 1 d U . .
O13 O 0.8358(9) 0.3359(8) 0.7810(8) 0.014(2) Uani 1 1 d U . .
O14 O 0.8450(9) 0.4895(9) 0.8891(9) 0.017(2) Uani 1 1 d U . .
O15 O 0.9539(10) 0.1277(9) 0.8154(9) 0.019(2) Uani 1 1 d U . .
O16 O 1.0397(10) 0.3034(9) 0.6193(9) 0.022(2) Uani 1 1 d U . .
O17 O 1.1593(10) 0.2477(8) 0.8044(8) 0.017(2) Uani 1 1 d U . .
O18 O 1.0694(9) 0.4420(9) 0.7600(8) 0.016(2) Uani 1 1 d U . .
O19 O 1.3888(9) 0.3135(8) 0.8259(8) 0.015(2) Uani 1 1 d U . .
O20 O 1.1559(10) 0.3565(9) 0.9581(9) 0.020(2) Uani 1 1 d U . .
O21 O 0.9007(9) 0.5992(8) 0.6519(9) 0.015(2) Uani 1 1 d U . .
O1W O 0.8384(11) 0.4346(10) 0.5242(10) 0.028(3) Uani 1 1 d U . .
O2W O 0.5852(11) 0.5439(11) 0.6718(10) 0.032(3) Uani 1 1 d U . .
O3W O 0.719(2) 0.8180(18) 0.5000(19) 0.095(6) Uani 1 1 d U . .
O4W O 0.5713(19) -0.1069(17) 1.0255(18) 0.088(6) Uani 1 1 d U . .
O5W O 0.8738(17) 0.0217(15) 0.7330(15) 0.075(5) Uani 1 1 d U . .
O6W O 0.6752(18) 0.0439(16) 0.7644(16) 0.079(5) Uani 1 1 d U . .
O7W O 0.8263(18) 0.0021(15) 1.0926(16) 0.072(5) Uani 1 1 d U . .
O8W O 0.9108(11) -0.0008(10) 1.3425(10) 0.029(3) Uani 1 1 d U . .
O9W O 1.0929(12) -0.1711(10) 1.4734(11) 0.036(3) Uani 1 1 d U . .
O10W O 1.1687(13) 0.1091(10) 1.3516(11) 0.036(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 0.0163(3) 0.0187(3) 0.0078(3) -0.0069(3) -0.0033(2) 0.0014(2)
W2 0.0168(3) 0.0216(3) 0.0072(3) -0.0068(3) -0.0015(2) -0.0014(3)
W3 0.0150(3) 0.0213(3) 0.0093(3) -0.0082(3) -0.0032(2) 0.0005(3)
W4 0.0176(3) 0.0206(3) 0.0085(3) -0.0086(3) -0.0034(3) 0.0012(3)
W5 0.0152(3) 0.0226(3) 0.0096(3) -0.0092(3) -0.0030(2) 0.0020(3)
W6 0.0157(3) 0.0195(3) 0.0073(3) -0.0066(2) -0.0038(2) 0.0008(2)
Na1 0.030(4) 0.032(4) 0.016(3) -0.012(3) -0.010(3) 0.000(3)
Na2 0.101(9) 0.067(7) 0.070(7) -0.025(6) -0.005(6) 0.000(6)
Na3 0.079(9) 0.030(6) 0.046(7) -0.015(5) -0.042(6) -0.006(5)
O1 0.017(5) 0.028(5) 0.007(5) -0.004(4) 0.003(4) 0.008(4)
O2 0.017(5) 0.017(5) 0.012(5) -0.001(4) -0.008(4) 0.000(4)
O3 0.019(5) 0.020(5) 0.014(5) -0.010(4) -0.004(4) -0.001(4)
O4 0.014(4) 0.016(4) 0.010(4) -0.009(3) -0.007(3) 0.002(3)
O5 0.016(5) 0.022(5) 0.004(5) -0.004(4) 0.005(4) -0.007(4)
O6 0.023(5) 0.030(5) 0.016(5) -0.008(4) -0.008(4) 0.003(4)
O7 0.017(5) 0.022(5) 0.005(5) -0.002(4) 0.001(4) 0.001(4)
O8 0.028(5) 0.027(5) 0.023(6) -0.011(4) -0.001(4) -0.002(4)
O9 0.021(5) 0.022(5) 0.023(5) -0.011(4) -0.001(4) 0.001(4)
O10 0.020(5) 0.028(5) 0.013(5) -0.007(4) -0.007(4) -0.001(4)
O11 0.024(5) 0.030(5) 0.015(5) -0.010(4) -0.003(4) -0.002(4)
O12 0.027(5) 0.025(5) 0.016(5) -0.007(4) -0.015(4) 0.006(4)
O13 0.012(5) 0.014(4) 0.014(5) -0.005(4) -0.001(4) 0.000(4)
O14 0.015(5) 0.024(5) 0.013(5) -0.008(4) -0.001(4) 0.003(4)
O15 0.023(5) 0.022(5) 0.015(5) -0.008(4) -0.007(4) 0.000(4)
O16 0.025(5) 0.025(5) 0.018(5) -0.011(4) -0.005(4) -0.001(4)
O17 0.023(5) 0.021(5) 0.009(5) -0.006(4) -0.006(4) 0.004(4)
O18 0.016(5) 0.025(5) 0.009(5) -0.006(4) -0.008(4) 0.006(4)
O19 0.018(5) 0.024(5) 0.009(5) -0.011(4) -0.007(4) 0.002(4)
O20 0.021(5) 0.023(5) 0.017(5) -0.005(4) -0.008(4) -0.004(4)
O21 0.013(5) 0.018(5) 0.013(5) -0.002(4) -0.005(4) 0.001(4)
O1W 0.040(6) 0.033(6) 0.017(5) -0.015(5) -0.008(5) 0.014(5)
O2W 0.021(5) 0.049(6) 0.027(6) -0.013(5) -0.004(5) 0.004(5)
O3W 0.106(10) 0.097(10) 0.099(10) -0.041(8) -0.047(8) 0.022(8)
O4W 0.084(9) 0.078(9) 0.095(10) -0.018(7) -0.020(8) 0.008(7)
O5W 0.082(9) 0.078(9) 0.070(9) -0.029(7) -0.017(7) 0.003(7)
O6W 0.088(9) 0.074(9) 0.075(9) -0.021(7) -0.024(7) 0.003(7)
O7W 0.088(9) 0.070(8) 0.076(9) -0.029(7) -0.044(7) 0.023(7)
O8W 0.032(6) 0.028(5) 0.028(6) -0.005(5) -0.013(5) -0.004(5)
O9W 0.047(7) 0.033(6) 0.030(6) -0.015(5) -0.005(5) -0.003(5)
O10W 0.050(7) 0.036(6) 0.025(6) -0.012(5) -0.010(5) -0.007(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O2 1.747(10) . ?
W1 O20 1.814(10) . ?
W1 O3 1.897(10) . ?
W1 O1 1.955(10) . ?
W1 O5 2.077(9) . ?
W1 O4 2.268(9) . ?
W2 O8 1.731(11) . ?
W2 O7 1.865(10) . ?
W2 O5 1.880(10) . ?
W2 O9 1.942(10) . ?
W2 O10 1.980(10) . ?
W2 O4 2.242(10) . ?
W3 O11 1.748(11) . ?
W3 O12 1.774(10) . ?
W3 O10 1.866(10) . ?
W3 O13 1.955(10) . ?
W3 O3 2.203(10) . ?
W3 O14 2.206(10) . ?
W4 O16 1.744(11) . ?
W4 O15 1.745(10) . ?
W4 O17 1.892(10) . ?
W4 O13 1.900(10) . ?
W4 O18 2.268(10) . ?
W4 O3 2.309(10) . ?
W5 O19 1.736(10) . ?
W5 O6 1.738(11) 2_766 ?
W5 O9 1.901(10) 2_767 ?
W5 O17 1.971(10) . ?
W5 O18 2.215(10) . ?
W5 O20 2.230(11) . ?
W6 O21 1.740(10) . ?
W6 O14 1.801(10) . ?
W6 O18 1.917(10) . ?
W6 O1 1.964(10) 2_767 ?
W6 O7 2.103(10) 2_767 ?
W6 O4 2.261(9) 2_767 ?
Na1 O21 2.349(11) . ?
Na1 O2W 2.353(13) . ?
Na1 O1W 2.392(13) . ?
Na1 O6 2.414(12) . ?
Na1 O3W 2.44(2) . ?
Na1 O16 2.441(12) 2_766 ?
Na2 O7W 2.30(2) . ?
Na2 O6W 2.36(2) . ?
Na2 O2 2.377(15) 2_757 ?
Na2 O11 2.410(15) . ?
Na2 O4W 2.45(2) . ?
Na2 O5W 2.46(2) . ?
Na2 O15 2.463(15) . ?
Na3 O9W 2.390(12) . ?
Na3 O9W 2.390(12) 2_758 ?
Na3 O10W 2.396(13) 2_758 ?
Na3 O10W 2.396(13) . ?
Na3 O8W 2.401(11) 2_758 ?
Na3 O8W 2.401(11) . ?
Na3 O5W 3.000(18) 1_556 ?
Na3 O5W 3.000(18) 2_757 ?
O1 W6 1.964(10) 2_767 ?
O2 Na2 2.377(15) 2_757 ?
O4 W6 2.261(9) 2_767 ?
O6 W5 1.738(11) 2_766 ?
O7 W6 2.103(10) 2_767 ?
O9 W5 1.901(10) 2_767 ?
O16 Na1 2.441(12) 2_766 ?
O5W Na3 3.000(18) 1_554 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 W1 O20 103.8(5) . . ?
O2 W1 O3 102.2(4) . . ?
O20 W1 O3 94.9(5) . . ?
O2 W1 O1 97.5(4) . . ?
O20 W1 O1 92.7(4) . . ?
O3 W1 O1 156.5(4) . . ?
O2 W1 O5 94.5(4) . . ?
O20 W1 O5 161.5(4) . . ?
O3 W1 O5 84.0(4) . . ?
O1 W1 O5 81.8(4) . . ?
O2 W1 O4 164.1(4) . . ?
O20 W1 O4 88.8(4) . . ?
O3 W1 O4 86.2(4) . . ?
O1 W1 O4 71.8(4) . . ?
O5 W1 O4 72.7(4) . . ?
O8 W2 O7 103.5(5) . . ?
O8 W2 O5 102.6(5) . . ?
O7 W2 O5 91.9(4) . . ?
O8 W2 O9 100.5(5) . . ?
O7 W2 O9 87.9(5) . . ?
O5 W2 O9 156.3(4) . . ?
O8 W2 O10 100.2(5) . . ?
O7 W2 O10 155.9(4) . . ?
O5 W2 O10 87.6(4) . . ?
O9 W2 O10 83.1(4) . . ?
O8 W2 O4 178.9(4) . . ?
O7 W2 O4 77.5(4) . . ?
O5 W2 O4 76.9(4) . . ?
O9 W2 O4 79.9(4) . . ?
O10 W2 O4 78.9(4) . . ?
O11 W3 O12 103.7(5) . . ?
O11 W3 O10 100.0(5) . . ?
O12 W3 O10 97.0(5) . . ?
O11 W3 O13 94.7(4) . . ?
O12 W3 O13 95.8(4) . . ?
O10 W3 O13 157.6(4) . . ?
O11 W3 O3 92.6(4) . . ?
O12 W3 O3 162.1(4) . . ?
O10 W3 O3 87.4(4) . . ?
O13 W3 O3 75.0(4) . . ?
O11 W3 O14 169.1(4) . . ?
O12 W3 O14 86.3(4) . . ?
O10 W3 O14 82.8(4) . . ?
O13 W3 O14 79.8(4) . . ?
O3 W3 O14 76.9(4) . . ?
O16 W4 O15 103.7(5) . . ?
O16 W4 O17 101.4(5) . . ?
O15 W4 O17 95.9(5) . . ?
O16 W4 O13 96.8(5) . . ?
O15 W4 O13 99.8(4) . . ?
O17 W4 O13 152.4(4) . . ?
O16 W4 O18 91.3(4) . . ?
O15 W4 O18 163.3(4) . . ?
O17 W4 O18 73.6(4) . . ?
O13 W4 O18 85.4(4) . . ?
O16 W4 O3 165.7(4) . . ?
O15 W4 O3 88.6(4) . . ?
O17 W4 O3 84.4(4) . . ?
O13 W4 O3 73.5(4) . . ?
O18 W4 O3 77.6(3) . . ?
O19 W5 O6 102.3(5) . 2_766 ?
O19 W5 O9 98.7(5) . 2_767 ?
O6 W5 O9 99.5(5) 2_766 2_767 ?
O19 W5 O17 96.1(4) . . ?
O6 W5 O17 95.8(5) 2_766 . ?
O9 W5 O17 155.9(4) 2_767 . ?
O19 W5 O18 163.4(4) . . ?
O6 W5 O18 91.8(4) 2_766 . ?
O9 W5 O18 87.5(4) 2_767 . ?
O17 W5 O18 73.4(4) . . ?
O19 W5 O20 88.8(4) . . ?
O6 W5 O20 168.0(4) 2_766 . ?
O9 W5 O20 82.9(4) 2_767 . ?
O17 W5 O20 78.4(4) . . ?
O18 W5 O20 76.6(4) . . ?
O21 W6 O14 104.3(5) . . ?
O21 W6 O18 103.2(4) . . ?
O14 W6 O18 94.4(4) . . ?
O21 W6 O1 96.4(5) . 2_767 ?
O14 W6 O1 92.8(4) . 2_767 ?
O18 W6 O1 156.7(4) . 2_767 ?
O21 W6 O7 94.8(4) . 2_767 ?
O14 W6 O7 160.7(4) . 2_767 ?
O18 W6 O7 83.9(4) . 2_767 ?
O1 W6 O7 82.0(4) 2_767 2_767 ?
O21 W6 O4 163.5(4) . 2_767 ?
O14 W6 O4 88.1(4) . 2_767 ?
O18 W6 O4 86.3(4) . 2_767 ?
O1 W6 O4 71.8(4) 2_767 2_767 ?
O7 W6 O4 72.7(4) 2_767 2_767 ?
O21 Na1 O2W 95.0(4) . . ?
O21 Na1 O1W 83.0(4) . . ?
O2W Na1 O1W 91.5(5) . . ?
O21 Na1 O6 158.3(5) . . ?
O2W Na1 O6 95.1(4) . . ?
O1W Na1 O6 77.6(4) . . ?
O21 Na1 O3W 97.9(6) . . ?
O2W Na1 O3W 97.1(7) . . ?
O1W Na1 O3W 171.3(7) . . ?
O6 Na1 O3W 99.8(6) . . ?
O21 Na1 O16 82.4(4) . 2_766 ?
O2W Na1 O16 177.4(5) . 2_766 ?
O1W Na1 O16 88.3(4) . 2_766 ?
O6 Na1 O16 87.4(4) . 2_766 ?
O3W Na1 O16 83.2(6) . 2_766 ?
O7W Na2 O6W 176.0(8) . . ?
O7W Na2 O2 79.3(6) . 2_757 ?
O6W Na2 O2 104.6(7) . 2_757 ?
O7W Na2 O11 78.9(6) . . ?
O6W Na2 O11 97.5(7) . . ?
O2 Na2 O11 153.7(7) 2_757 . ?
O7W Na2 O4W 95.7(8) . . ?
O6W Na2 O4W 83.1(8) . . ?
O2 Na2 O4W 95.4(6) 2_757 . ?
O11 Na2 O4W 101.2(7) . . ?
O7W Na2 O5W 131.4(8) . . ?
O6W Na2 O5W 52.0(7) . . ?
O2 Na2 O5W 65.8(6) 2_757 . ?
O11 Na2 O5W 120.8(7) . . ?
O4W Na2 O5W 119.4(8) . . ?
O7W Na2 O15 88.3(7) . . ?
O6W Na2 O15 93.3(6) . . ?
O2 Na2 O15 78.8(5) 2_757 . ?
O11 Na2 O15 86.0(5) . . ?
O4W Na2 O15 172.3(7) . . ?
O5W Na2 O15 53.7(5) . . ?
O9W Na3 O9W 180.000(3) . 2_758 ?
O9W Na3 O10W 89.2(4) . 2_758 ?
O9W Na3 O10W 90.8(4) 2_758 2_758 ?
O9W Na3 O10W 90.8(4) . . ?
O9W Na3 O10W 89.2(4) 2_758 . ?
O10W Na3 O10W 180.000(1) 2_758 . ?
O9W Na3 O8W 96.9(4) . 2_758 ?
O9W Na3 O8W 83.1(4) 2_758 2_758 ?
O10W Na3 O8W 84.4(4) 2_758 2_758 ?
O10W Na3 O8W 95.6(4) . 2_758 ?
O9W Na3 O8W 83.1(4) . . ?
O9W Na3 O8W 96.9(4) 2_758 . ?
O10W Na3 O8W 95.6(4) 2_758 . ?
O10W Na3 O8W 84.4(4) . . ?
O8W Na3 O8W 180.000(2) 2_758 . ?
O9W Na3 O5W 122.7(5) . 1_556 ?
O9W Na3 O5W 57.3(5) 2_758 1_556 ?
O10W Na3 O5W 49.2(4) 2_758 1_556 ?
O10W Na3 O5W 130.8(4) . 1_556 ?
O8W Na3 O5W 49.8(5) 2_758 1_556 ?
O8W Na3 O5W 130.2(5) . 1_556 ?
O9W Na3 O5W 57.3(5) . 2_757 ?
O9W Na3 O5W 122.7(5) 2_758 2_757 ?
O10W Na3 O5W 130.8(4) 2_758 2_757 ?
O10W Na3 O5W 49.2(4) . 2_757 ?
O8W Na3 O5W 130.2(5) 2_758 2_757 ?
O8W Na3 O5W 49.8(5) . 2_757 ?
O5W Na3 O5W 180.000(2) 1_556 2_757 ?
W1 O1 W6 118.7(5) . 2_767 ?
W1 O2 Na2 161.4(6) . 2_757 ?
W1 O3 W3 139.0(5) . . ?
W1 O3 W4 125.9(5) . . ?
W3 O3 W4 93.4(4) . . ?
W2 O4 W6 95.6(4) . 2_767 ?
W2 O4 W1 95.5(3) . . ?
W6 O4 W1 96.2(4) 2_767 . ?
W2 O5 W1 114.9(5) . . ?
W5 O6 Na1 137.4(6) 2_766 . ?
W2 O7 W6 114.2(5) . 2_767 ?
W5 O9 W2 147.6(6) 2_767 . ?
W3 O10 W2 147.8(6) . . ?
W3 O11 Na2 137.6(6) . . ?
W4 O13 W3 116.9(5) . . ?
W6 O14 W3 137.3(5) . . ?
W4 O15 Na2 134.5(6) . . ?
W4 O16 Na1 132.9(6) . 2_766 ?
W4 O17 W5 116.8(5) . . ?
W6 O18 W5 138.2(5) . . ?
W6 O18 W4 126.0(5) . . ?
W5 O18 W4 94.5(4) . . ?
W1 O20 W5 137.7(5) . . ?
W6 O21 Na1 166.0(6) . . ?
Na2 O5W Na3 173.4(8) . 1_554 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.962
_refine_diff_density_min         -3.270
_refine_diff_density_rms         0.448

# start Validation Reply Form

_vrf_PLAT306_2007kvb0028mtw      
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W
RESPONSE: It was not possible to locate the hydrogen atoms of the water
molecules
;
_vrf_PLAT430_2007kvb0028mtw      
;
PROBLEM: Short Inter D...A Contact O5W .. O6W .. 2.12 Ang.
RESPONSE: Due to hydrogen bonding interactions
;
_vrf_PLAT601_2007kvb0028mtw      
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 325.00 A**3
RESPONSE: Disordered water molecules were treated using SQUEEZE
;

# end Validation Reply Form