Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2003

data_global

_publ_contact_author_email       CAESAR@CHE.NSK.SU

_publ_contact_author_name        'Dr Maxim Sokolov'
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_publ_contact_author_address     
;
A.V. Nikolayev Institute of Inorganic Chemistry
Siberian Branch of the
Russian
Prospect Lavrentyeva 3
Novosibirsk
630090
RUSSIAN FEDERATION
;

_publ_section_title              
;
Preparation and structure of [Sn8W18O66]8- a
26-nuclear stannotungstate with a hexagonal belt of six Sn(II) ions with
outward-looking lone pairs
;

_publ_section_references         
;
Bruker (1998a) SAINTPlus Data Reduction and Correction Program v. 6.01, Bruker
AXS, Madison, Wisconsin, USA.

Bruker (1998b) SMART. Bruker Molecular Analysis Research Tool,
v. 5.059. Bruker AXS, Madison, Wisconsin, USA.

Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector
Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA.

Sheldrick G.M. (1998b). SHELXTL v. 5.10, Structure Determination Software
Suite, Bruker AXS, Madison, Wisconsin, USA.
;

_publ_section_exptl_refinement   
;
There is a high positive residual density of 8.73 e\%A^-3^ near the Sn(3)
atom (distance 0.76 %A^) due to considerable absorption effects which could not
be completely corrected
;

loop_
_publ_author_name
'Maxim Sokolov'
'Mikhail Yu Antipin'
'Vladimir P. Fedin'
'Natalya V. Izarova'
'Zoya A. Starikova'
;
A.V.Virovets
;

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 218283'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     
'12(Na +1), W18 Sn8 O66 -8, 4 (H O -1), 46(H2 O)'
_chemical_formula_sum            'H96 Na12 O116 Sn8 W18'
_chemical_formula_weight         6487.47

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'
Sn Sn -0.6537 1.4246 '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           Hexagonal
_symmetry_space_group_name_H-M   'P 63/m m c'

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

_cell_length_a                   14.478(8)
_cell_length_b                   14.478(8)
_cell_length_c                   32.08(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5823,47(60)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    994
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      27.85

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5776
_exptl_absorpt_coefficient_mu    19.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(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 SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            42631
_diffrn_reflns_av_R_equivalents  0.1530
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         28.14
_reflns_number_total             2695
_reflns_number_gt                1718
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'

_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^)+(0.0821P)^2^+473.3398P] 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       0.000080(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2695
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0632
_refine_ls_wR_factor_ref         0.1980
_refine_ls_wR_factor_gt          0.1516
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.137
_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
Na1 Na 0.5031(17) -0.2484(9) 0.5764(6) 0.064(5) Uani 1 2 d S . .
Na2 Na 0.7589(15) 0.0000 0.5000 0.077(6) Uani 1 2 d S . .
O1N O 0.3333 -0.3333 0.5378(15) 0.063(16) Uani 1 6 d S . .
O2N O 0.4056(15) -0.189(3) 0.6229(12) 0.076(11) Uani 1 2 d S . .
O3N O 0.5831(19) -0.0880(17) 0.5392(6) 0.057(6) Uani 1 1 d . . .
O4N O 0.674(5) -0.163(2) 0.6070(11) 0.12(2) Uani 1 2 d S . .
W1 W 0.58232(5) 0.16464(10) 0.57206(3) 0.0191(3) Uani 1 2 d S . .
W2 W 0.65712(7) 0.08972(7) 0.65438(2) 0.0199(3) Uani 1 1 d . . .
Sn1 Sn 0.80945(12) 0.19055(12) 0.7500 0.0206(6) Uani 1 4 d S . .
Sn2 Sn 0.52341(18) 0.0468(4) 0.7500 0.0455(10) Uani 1 4 d S . .
Sn3 Sn 0.6667 0.3333 0.68083(9) 0.0158(7) Uani 1 6 d S . .
O1 O 0.5581(9) 0.1161(19) 0.5224(6) 0.030(5) Uani 1 2 d S . .
O2 O 0.7265(9) 0.2735(9) 0.5655(6) 0.025(5) Uani 1 2 d S . .
O3 O 0.6313(12) 0.0754(11) 0.5947(4) 0.021(3) Uani 1 1 d . . .
O4 O 0.7947(8) 0.2053(8) 0.6434(6) 0.021(4) Uani 1 2 d S . .
O5 O 0.6825(13) -0.0134(13) 0.6587(4) 0.030(4) Uani 1 1 d . . .
O6 O 0.5059(8) 0.0118(16) 0.6619(6) 0.026(5) Uani 1 2 d S . .
O7 O 0.6712(12) 0.1367(12) 0.7093(4) 0.020(3) Uani 1 1 d . . .
O8 O 0.5995(7) 0.1989(14) 0.6397(6) 0.017(4) Uani 1 2 d S . .
O2W O 0.695(2) -0.1526(12) 0.4565(9) 0.060(9) Uani 1 2 d S . .
O3W O 0.827(6) -0.086(3) 0.5463(19) 0.19(3) Uani 1 2 d S . .
O4W O 0.695(9) -0.153(4) 0.7500 0.17(4) Uani 1 4 d S . .
O5W O 0.511(5) -0.244(2) 0.717(2) 0.16(2) Uani 1 2 d S . .
O6W O 0.942(6) 0.058(6) 0.636(8) 0.39(17) Uani 0.50 2 d SP . .

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
Na1 0.099(16) 0.059(7) 0.047(10) -0.007(5) -0.014(10) 0.050(8)
Na2 0.071(10) 0.057(12) 0.097(16) -0.014(11) -0.007(6) 0.028(6)
O1N 0.08(3) 0.08(3) 0.03(2) 0.000 0.000 0.041(13)
O2N 0.056(14) 0.09(3) 0.09(3) -0.05(2) -0.026(11) 0.044(13)
O3N 0.088(17) 0.061(14) 0.033(10) -0.024(10) -0.002(11) 0.047(13)
O4N 0.27(6) 0.095(18) 0.045(19) -0.021(15) -0.04(3) 0.14(3)
W1 0.0267(5) 0.0249(6) 0.0051(5) -0.0013(4) -0.0006(2) 0.0125(3)
W2 0.0320(5) 0.0243(5) 0.0069(4) -0.0022(3) -0.0021(3) 0.0167(4)
Sn1 0.0280(11) 0.0280(11) 0.0085(12) 0.000 0.000 0.0161(13)
Sn2 0.0549(18) 0.051(2) 0.0290(18) 0.000 0.000 0.0257(12)
Sn3 0.0224(10) 0.0224(10) 0.0025(13) 0.000 0.000 0.0112(5)
O1 0.041(11) 0.028(12) 0.016(10) -0.001(9) -0.001(5) 0.014(6)
O2 0.031(9) 0.031(9) 0.007(9) -0.004(4) 0.004(4) 0.012(10)
O3 0.028(8) 0.023(7) 0.009(6) -0.004(6) 0.002(6) 0.010(6)
O4 0.027(8) 0.027(8) 0.010(9) -0.001(4) 0.001(4) 0.014(9)
O5 0.042(10) 0.027(8) 0.021(7) -0.004(7) 0.002(7) 0.017(8)
O6 0.049(11) 0.015(10) 0.004(8) -0.001(7) -0.001(4) 0.007(5)
O7 0.023(7) 0.026(8) 0.013(6) -0.008(6) -0.003(6) 0.014(6)
O8 0.026(8) 0.003(8) 0.013(9) -0.002(7) -0.001(4) 0.002(4)
O2W 0.05(2) 0.075(17) 0.044(17) -0.016(8) -0.032(15) 0.027(10)
O3W 0.31(9) 0.15(3) 0.16(6) -0.07(3) -0.14(6) 0.15(5)
O4W 0.37(14) 0.15(4) 0.05(3) 0.000 0.000 0.19(7)
O5W 0.15(5) 0.12(3) 0.22(7) 0.01(2) 0.02(5) 0.08(3)
O6W 0.12(6) 0.12(6) 0.8(5) -0.18(12) 0.18(12) 0.00(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
Na1 O1N 2.46(3) . ?
Na1 O2N 2.49(3) . ?
Na1 O2N 2.49(3) 4_655 ?
Na1 O3N 2.34(3) 20_545 ?
Na1 O3N 2.34(3) . ?
Na1 O4N 2.36(5) . ?
Na2 O3N 2.54(3) 7_556 ?
Na2 O3N 2.54(3) . ?
Na2 O2W 2.375(17) 15_666 ?
Na2 O2W 2.375(17) . ?
Na2 O3W 2.45(4) . ?
Na2 O3W 2.45(4) 15_666 ?
O1N Na1 2.46(3) 3_545 ?
O1N Na1 2.46(3) 4_655 ?
O2N Na1 2.49(3) 3_545 ?
W1 O1 1.70(2) . ?
W1 O2 1.896(6) . ?
W1 O2 1.896(6) 4_665 ?
W1 O3 1.902(15) 19_655 ?
W1 O3 1.902(15) . ?
W1 O8 2.213(18) . ?
W2 O3 1.942(13) . ?
W2 O4 1.887(5) . ?
W2 O5 1.713(16) . ?
W2 O6 1.912(11) . ?
W2 O7 1.863(13) . ?
W2 O8 2.177(12) . ?
Sn1 O7 2.181(14) 10_666 ?
Sn1 O7 2.181(14) . ?
Sn1 O7 2.181(14) 14_557 ?
Sn1 O7 2.181(14) 21_665 ?
Sn2 O7 2.278(15) 14_557 ?
Sn2 O7 2.278(15) . ?
Sn2 O7 2.278(15) 12_656 ?
Sn2 O7 2.278(15) 19_655 ?
Sn3 O8 2.139(18) . ?
Sn3 O8 2.139(18) 3_655 ?
Sn3 O8 2.139(18) 4_665 ?
O2 W1 1.896(6) 3_655 ?
O4 W2 1.887(5) 21_665 ?
O6 W2 1.912(11) 19_655 ?
O8 W2 2.177(12) 19_655 ?
O2W Na2 2.375(17) 16_546 ?
O3W Na2 2.45(4) 16_546 ?

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
O1N Na1 O2N 82.9(11) . . ?
O1N Na1 O2N 82.9(11) . 4_655 ?
O2N Na1 O2N 78(2) . 4_655 ?
O3N Na1 O1N 96.6(10) 20_545 . ?
O3N Na1 O1N 96.6(10) . . ?
O3N Na1 O2N 170.9(13) 20_545 . ?
O3N Na1 O2N 92.6(11) . . ?
O3N Na1 O2N 92.6(11) 20_545 4_655 ?
O3N Na1 O2N 170.9(13) . 4_655 ?
O3N Na1 O3N 96.5(12) 20_545 . ?
O3N Na1 O4N 79.7(11) 20_545 . ?
O3N Na1 O4N 79.7(11) . . ?
O4N Na1 O1N 174.4(17) . . ?
O4N Na1 O2N 101.4(11) . . ?
O4N Na1 O2N 101.4(11) . 4_655 ?
O3N Na2 O3N 82.5(12) 7_556 . ?
O2W Na2 O3N 89.8(10) 15_666 7_556 ?
O2W Na2 O3N 96.6(7) . 7_556 ?
O2W Na2 O3N 96.6(7) 15_666 . ?
O2W Na2 O3N 89.8(10) . . ?
O2W Na2 O2W 171.5(17) 15_666 . ?
O2W Na2 O3W 87.2(12) 15_666 . ?
O2W Na2 O3W 87.2(10) . . ?
O2W Na2 O3W 87.2(10) 15_666 15_666 ?
O2W Na2 O3W 87.2(12) . 15_666 ?
O3W Na2 O3N 172(2) . 7_556 ?
O3W Na2 O3N 90(2) 15_666 7_556 ?
O3W Na2 O3N 90(2) . . ?
O3W Na2 O3N 172(2) 15_666 . ?
O3W Na2 O3W 97(4) . 15_666 ?
Na1 O1N Na1 96.9(14) 3_545 . ?
Na1 O1N Na1 96.9(14) 3_545 4_655 ?
Na1 O1N Na1 96.9(14) . 4_655 ?
Na1 O2N Na1 95.7(15) 3_545 . ?
Na1 O3N Na2 128.7(10) . . ?
O1 W1 O2 98.9(8) . . ?
O1 W1 O2 98.9(8) . 4_665 ?
O1 W1 O3 98.4(7) . 19_655 ?
O1 W1 O3 98.4(7) . . ?
O1 W1 O8 170.3(9) . . ?
O2 W1 O2 86.5(14) . 4_665 ?
O2 W1 O3 162.6(7) . 19_655 ?
O2 W1 O3 88.7(8) 4_665 19_655 ?
O2 W1 O3 88.7(8) . . ?
O2 W1 O3 162.6(7) 4_665 . ?
O2 W1 O8 88.2(6) . . ?
O2 W1 O8 88.2(6) 4_665 . ?
O3 W1 O3 90.9(9) 19_655 . ?
O3 W1 O8 74.9(5) 19_655 . ?
O3 W1 O8 74.9(5) . . ?
O3 W2 O8 75.0(6) . . ?
O4 W2 O3 88.4(7) . . ?
O4 W2 O6 159.5(8) . . ?
O4 W2 O8 86.2(7) . . ?
O5 W2 O3 95.7(6) . . ?
O5 W2 O4 101.3(8) . . ?
O5 W2 O6 99.0(8) . . ?
O5 W2 O7 102.1(6) . . ?
O5 W2 O8 168.1(7) . . ?
O6 W2 O3 87.6(7) . . ?
O6 W2 O8 73.4(6) . . ?
O7 W2 O3 162.1(6) . . ?
O7 W2 O4 88.8(7) . . ?
O7 W2 O6 88.9(7) . . ?
O7 W2 O8 87.2(7) . . ?
O7 Sn1 O7 121.9(7) 10_666 . ?
O7 Sn1 O7 79.2(8) 10_666 14_557 ?
O7 Sn1 O7 73.5(7) . 14_557 ?
O7 Sn1 O7 73.5(7) 10_666 21_665 ?
O7 Sn1 O7 79.2(8) . 21_665 ?
O7 Sn1 O7 121.9(7) 14_557 21_665 ?
O7 Sn2 O7 69.9(7) 14_557 . ?
O7 Sn2 O7 81.6(7) 14_557 12_656 ?
O7 Sn2 O7 120.7(7) . 12_656 ?
O7 Sn2 O7 120.7(7) 14_557 19_655 ?
O7 Sn2 O7 81.6(7) . 19_655 ?
O7 Sn2 O7 69.9(7) 12_656 19_655 ?
O8 Sn3 O8 86.0(7) . 3_655 ?
O8 Sn3 O8 86.0(7) . 4_665 ?
O8 Sn3 O8 86.0(7) 3_655 4_665 ?
W1 O2 W1 150.1(13) . 3_655 ?
W1 O3 W2 114.9(7) . . ?
W2 O4 W2 152.5(11) . 21_665 ?
W2 O6 W2 116.5(10) 19_655 . ?
W2 O7 Sn1 127.6(7) . . ?
W2 O7 Sn2 115.7(7) . . ?
Sn1 O7 Sn2 107.1(5) . . ?
W2 O8 W1 95.1(6) . . ?
W2 O8 W1 95.1(6) 19_655 . ?
W2 O8 W2 96.6(7) . 19_655 ?
Sn3 O8 W1 139.2(9) . . ?
Sn3 O8 W2 111.3(6) . . ?
Sn3 O8 W2 111.3(6) . 19_655 ?
Na2 O2W Na2 94.6(11) . 16_546 ?
Na2 O3W Na2 91.0(17) . 16_546 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.14
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         8.733
_refine_diff_density_min         -5.891
_refine_diff_density_rms         0.635

#= END of CIF file submission