# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Mr Fernando Gomez-Baquero'
_publ_contact_author_email       aduarter@unal.edu.co

_publ_section_title              
;
Synthesis and structure of
[Na4(DMSO)15][(I3)3(I)]. Self-assembly of
hexacoordinated sodium

;
loop_
_publ_author_name
A.Duarte-Ruiz
N.Nunez-Dallos
L.Garzon-Tovar
K.Wurst
;
E.Avella-Moreno
;
F.Gomez-Baquero

# Attachment '- lac.cif'

data_la
_database_code_depnum_ccdc_archive 'CCDC 820376'
#TrackingRef '- lac.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H90 I10 Na4 O15 S15'
_chemical_formula_weight         2532.88

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P63/m

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

_cell_length_a                   12.0292(4)
_cell_length_b                   12.0292(3)
_cell_length_c                   32.9777(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4132.61(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    34143
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      26.0

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2408
_exptl_absorpt_coefficient_mu    4.193
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      233(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  'Nonius KappaCCD'
_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_%        ?
_diffrn_reflns_number            16891
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2729
_reflns_number_gt                1915
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       ?
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Well ordered chain of anionic (I3)-3 x I- units along the
hexagonal c-axis. I2, I3, I4 and I5 lies on the '6 bar' rotoinversion
axis with multiplicity of 0.3333, whereas I1 and I6 lies in the
inverision centre of this axis with multiplicity of 0.1666.
Disordered clusters of Na(x)DMSO(3x+3) by partial occupation of the
position Na2 and Na3. Na1 and Na2 lies on '6 sub 3' screw axis with
centre of symmetry and a normal multiplicity of 0.3333, whereas Na3 lies
on this centre of symmetry with normal multiplicity of 0.1666. The
occupation disorder leads for an occupation factor of 0.2833 for Na2
and 0.05 for Na3. This means, that the position of Na2 is occopied only
to 85% and of Na3 only to 30%. Therefore we can form a mixture of
monomers, dimers, trimers, tetramers and so on (with the major product of
the tetrameric cluster Na4(DMSO)15) along these columns in direction of the
hexagonal c-axis. This disorder is also shown by the anisotropic refinement
of the general postion O3, which leads to extremly cigar-like ellipsoids.
Therefore this position was splitted into O3, O4 and O5 with 0.70 occupancy
for O3 and 0.15 for O4 and O5 (O3 is connected to Na2 , O4 connects Na2 and
Na3 and at least O5 is connected to Na3).
The DMSO molecules lies on general positions, except C1-S1-O1 whereas S1 and
O1 lies on a mirror plane with occupation of 0.5 for each.
;

_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^)+(0.0300P)^2^+4.7652P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2729
_refine_ls_number_parameters     121
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0902
_refine_ls_wR_factor_gt          0.0833
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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
I1 I 0.3333 0.6667 0.2500 0.0485(2) Uani 1 6 d S . .
I2 I 0.3333 0.6667 0.140690(13) 0.04424(15) Uani 1 3 d S . .
I3 I 0.3333 0.6667 0.053230(13) 0.04294(15) Uani 1 3 d S . .
I4 I 0.3333 0.6667 -0.040885(14) 0.04928(16) Uani 1 3 d S . .
I5 I 0.3333 0.6667 -0.160467(13) 0.04572(16) Uani 1 3 d S . .
I6 I 0.3333 0.6667 -0.2500 0.04029(18) Uani 1 6 d S . .
Na1 Na 0.0000 1.0000 0.20005(5) 0.0323(6) Uani 1 3 d S . .
Na2 Na 0.0000 1.0000 0.10057(7) 0.0321(7) Uani 0.85 3 d SP . .
Na3 Na 0.0000 1.0000 0.0000 0.045(3) Uani 0.30 6 d SP . .
S1 S 0.27831(12) 1.05806(12) 0.2500 0.0342(3) Uani 1 2 d S . .
S2 S 0.05721(9) 0.78082(9) 0.15030(3) 0.0360(2) Uani 1 1 d . . .
S3 S 0.26987(11) 1.04715(10) 0.05416(3) 0.0473(3) Uani 1 1 d . . .
O1 O 0.1342(3) 0.9677(3) 0.2500 0.0386(8) Uani 1 2 d S . .
O2 O -0.0364(3) 0.8297(3) 0.15311(7) 0.0458(7) Uani 1 1 d . . .
O3 O 0.1327(4) 0.9396(5) 0.06537(14) 0.0469(14) Uiso 0.70 1 d P . .
O4 O 0.1313(18) 0.9626(18) 0.0542(7) 0.024(4) Uiso 0.15 1 d P . .
O5 O 0.133(2) 0.943(2) 0.0371(6) 0.055(6) Uiso 0.15 1 d P . .
C1 C 0.3395(4) 1.0079(4) 0.20938(12) 0.0490(12) Uani 1 1 d . . .
H1A H 0.3141 1.0285 0.1838 0.074 Uiso 1 1 calc . . .
H1B H 0.3053 0.9160 0.2111 0.074 Uiso 1 1 calc . . .
H1C H 0.4324 1.0519 0.2110 0.074 Uiso 1 1 calc . . .
C2 C 0.0222(5) 0.6741(5) 0.19166(13) 0.0533(12) Uani 1 1 d . . .
H2A H 0.0476 0.7225 0.2168 0.080 Uiso 1 1 calc . . .
H2B H 0.0691 0.6284 0.1885 0.080 Uiso 1 1 calc . . .
H2C H -0.0692 0.6131 0.1923 0.080 Uiso 1 1 calc . . .
C3 C 0.0013(4) 0.6655(4) 0.11063(12) 0.0503(11) Uani 1 1 d . . .
H3A H 0.0134 0.7086 0.0848 0.075 Uiso 1 1 calc . . .
H3B H -0.0892 0.6047 0.1146 0.075 Uiso 1 1 calc . . .
H3C H 0.0491 0.6202 0.1108 0.075 Uiso 1 1 calc . . .
C4 C 0.3598(5) 1.0181(5) 0.09043(14) 0.0659(14) Uani 1 1 d . . .
H4A H 0.3424 1.0391 0.1172 0.099 Uiso 1 1 calc . . .
H4B H 0.4505 1.0710 0.0845 0.099 Uiso 1 1 calc . . .
H4C H 0.3360 0.9283 0.0896 0.099 Uiso 1 1 calc . . .
C5 C 0.3233(5) 1.0033(5) 0.01063(13) 0.0662(15) Uani 1 1 d . . .
H5A H 0.2809 1.0123 -0.0131 0.099 Uiso 1 1 calc . . .
H5B H 0.3032 0.9148 0.0131 0.099 Uiso 1 1 calc . . .
H5C H 0.4154 1.0586 0.0079 0.099 Uiso 1 1 calc . . .

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
I1 0.0448(3) 0.0448(3) 0.0559(4) 0.000 0.000 0.02241(14)
I2 0.0419(2) 0.0419(2) 0.0489(3) 0.000 0.000 0.02096(11)
I3 0.0378(2) 0.0378(2) 0.0533(3) 0.000 0.000 0.01888(10)
I4 0.0526(2) 0.0526(2) 0.0427(3) 0.000 0.000 0.02629(11)
I5 0.0476(2) 0.0476(2) 0.0419(3) 0.000 0.000 0.02380(11)
I6 0.0347(2) 0.0347(2) 0.0515(4) 0.000 0.000 0.01733(12)
Na1 0.0325(10) 0.0325(10) 0.0319(11) 0.000 0.000 0.0162(5)
Na2 0.0321(11) 0.0321(11) 0.0322(13) 0.000 0.000 0.0161(6)
Na3 0.044(5) 0.044(5) 0.048(6) 0.000 0.000 0.022(2)
S1 0.0328(8) 0.0313(7) 0.0380(6) 0.000 0.000 0.0157(6)
S2 0.0351(6) 0.0310(6) 0.0416(5) -0.0022(4) -0.0028(4) 0.0162(5)
S3 0.0473(7) 0.0374(6) 0.0610(6) -0.0039(4) -0.0032(5) 0.0240(5)
O1 0.029(2) 0.045(2) 0.0398(18) 0.000 0.000 0.0170(18)
O2 0.0526(19) 0.0413(18) 0.0546(15) -0.0095(12) -0.0068(13) 0.0319(15)
C1 0.037(3) 0.055(3) 0.046(2) -0.0065(19) 0.0065(17) 0.017(2)
C2 0.062(3) 0.068(3) 0.045(2) 0.011(2) 0.006(2) 0.044(3)
C3 0.060(3) 0.060(3) 0.041(2) -0.0127(19) -0.0076(19) 0.038(2)
C4 0.077(4) 0.062(3) 0.046(2) 0.008(2) -0.008(2) 0.025(3)
C5 0.081(4) 0.059(3) 0.042(2) -0.009(2) 0.003(2) 0.023(3)

_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
I2 I3 2.8842(7) . ?
I3 I4 3.1037(6) . ?
I5 I6 2.9526(4) . ?
I6 I5 2.9526(4) 10 ?
Na1 O2 2.427(3) 3_465 ?
Na1 O2 2.427(3) . ?
Na1 O2 2.427(3) 2_675 ?
Na1 O1 2.469(3) 2_675 ?
Na1 O1 2.469(3) . ?
Na1 O1 2.469(3) 3_465 ?
Na1 Na2 3.281(3) . ?
Na1 Na1 3.294(4) 10_556 ?
Na2 O3 2.363(5) 3_465 ?
Na2 O3 2.363(5) 2_675 ?
Na2 O3 2.363(5) . ?
Na2 O4 2.40(2) 3_465 ?
Na2 O4 2.40(2) . ?
Na2 O4 2.40(2) 2_675 ?
Na2 O2 2.549(3) 2_675 ?
Na2 O2 2.549(3) 3_465 ?
Na2 O2 2.549(3) . ?
Na2 O5 2.92(2) 3_465 ?
Na2 O5 2.92(2) . ?
Na2 O5 2.92(2) 2_675 ?
Na3 O5 2.37(2) 2_675 ?
Na3 O5 2.37(2) 3_465 ?
Na3 O5 2.37(2) 8_455 ?
Na3 O5 2.37(2) 7_575 ?
Na3 O5 2.37(2) . ?
Na3 O5 2.37(2) 9_665 ?
Na3 O4 2.57(2) 7_575 ?
Na3 O4 2.57(2) 8_455 ?
Na3 O4 2.57(2) 9_665 ?
Na3 O4 2.57(2) 2_675 ?
Na3 O4 2.57(2) . ?
Na3 O4 2.57(2) 3_465 ?
S1 O1 1.517(4) . ?
S1 C1 1.773(4) . ?
S1 C1 1.773(4) 10_556 ?
S2 O2 1.511(3) . ?
S2 C2 1.774(4) . ?
S2 C3 1.776(4) . ?
S3 O4 1.456(19) . ?
S3 O3 1.549(5) . ?
S3 O5 1.60(2) . ?
S3 C5 1.758(5) . ?
S3 C4 1.761(5) . ?
O1 Na1 2.469(3) 10_556 ?
O3 O5 0.93(2) . ?
O4 O5 0.62(2) . ?

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
I2 I3 I4 180.0 . . ?
I5 I6 I5 180.0 10 . ?
O2 Na1 O2 83.67(11) 3_465 . ?
O2 Na1 O2 83.67(11) 3_465 2_675 ?
O2 Na1 O2 83.67(11) . 2_675 ?
O2 Na1 O1 97.39(9) 3_465 2_675 ?
O2 Na1 O1 177.62(10) . 2_675 ?
O2 Na1 O1 98.55(9) 2_675 2_675 ?
O2 Na1 O1 177.62(10) 3_465 . ?
O2 Na1 O1 98.55(9) . . ?
O2 Na1 O1 97.39(9) 2_675 . ?
O1 Na1 O1 80.36(9) 2_675 . ?
O2 Na1 O1 98.55(9) 3_465 3_465 ?
O2 Na1 O1 97.39(9) . 3_465 ?
O2 Na1 O1 177.62(10) 2_675 3_465 ?
O1 Na1 O1 80.36(9) 2_675 3_465 ?
O1 Na1 O1 80.36(9) . 3_465 ?
O2 Na1 Na2 50.37(7) 3_465 . ?
O2 Na1 Na2 50.37(7) . . ?
O2 Na1 Na2 50.37(7) 2_675 . ?
O1 Na1 Na2 131.84(6) 2_675 . ?
O1 Na1 Na2 131.84(6) . . ?
O1 Na1 Na2 131.84(6) 3_465 . ?
O2 Na1 Na1 129.63(7) 3_465 10_556 ?
O2 Na1 Na1 129.63(7) . 10_556 ?
O2 Na1 Na1 129.63(7) 2_675 10_556 ?
O1 Na1 Na1 48.16(6) 2_675 10_556 ?
O1 Na1 Na1 48.16(6) . 10_556 ?
O1 Na1 Na1 48.16(6) 3_465 10_556 ?
Na2 Na1 Na1 180.0 . 10_556 ?
O3 Na2 O3 97.93(16) 3_465 2_675 ?
O3 Na2 O3 97.93(16) 3_465 . ?
O3 Na2 O3 97.93(16) 2_675 . ?
O3 Na2 O4 11.2(5) 3_465 3_465 ?
O3 Na2 O4 94.4(5) 2_675 3_465 ?
O3 Na2 O4 87.9(5) . 3_465 ?
O3 Na2 O4 94.4(5) 3_465 . ?
O3 Na2 O4 87.9(5) 2_675 . ?
O3 Na2 O4 11.2(5) . . ?
O4 Na2 O4 83.6(8) 3_465 . ?
O3 Na2 O4 87.9(5) 3_465 2_675 ?
O3 Na2 O4 11.2(5) 2_675 2_675 ?
O3 Na2 O4 94.4(5) . 2_675 ?
O4 Na2 O4 83.6(8) 3_465 2_675 ?
O4 Na2 O4 83.6(8) . 2_675 ?
O3 Na2 O2 165.73(15) 3_465 2_675 ?
O3 Na2 O2 87.56(13) 2_675 2_675 ?
O3 Na2 O2 94.32(13) . 2_675 ?
O4 Na2 O2 176.8(5) 3_465 2_675 ?
O4 Na2 O2 99.0(5) . 2_675 ?
O4 Na2 O2 98.5(5) 2_675 2_675 ?
O3 Na2 O2 87.56(13) 3_465 3_465 ?
O3 Na2 O2 94.32(13) 2_675 3_465 ?
O3 Na2 O2 165.73(15) . 3_465 ?
O4 Na2 O2 98.5(5) 3_465 3_465 ?
O4 Na2 O2 176.8(5) . 3_465 ?
O4 Na2 O2 99.0(5) 2_675 3_465 ?
O2 Na2 O2 78.86(10) 2_675 3_465 ?
O3 Na2 O2 94.32(13) 3_465 . ?
O3 Na2 O2 165.73(15) 2_675 . ?
O3 Na2 O2 87.56(13) . . ?
O4 Na2 O2 99.0(5) 3_465 . ?
O4 Na2 O2 98.5(5) . . ?
O4 Na2 O2 176.8(5) 2_675 . ?
O2 Na2 O2 78.86(10) 2_675 . ?
O2 Na2 O2 78.86(10) 3_465 . ?
O3 Na2 O5 16.5(4) 3_465 3_465 ?
O3 Na2 O5 87.5(4) 2_675 3_465 ?
O3 Na2 O5 86.7(4) . 3_465 ?
O4 Na2 O5 7.2(7) 3_465 3_465 ?
O4 Na2 O5 81.2(6) . 3_465 ?
O4 Na2 O5 76.6(7) 2_675 3_465 ?
O2 Na2 O5 175.1(4) 2_675 3_465 ?
O2 Na2 O5 101.1(4) 3_465 3_465 ?
O2 Na2 O5 106.0(4) . 3_465 ?
O3 Na2 O5 87.5(4) 3_465 . ?
O3 Na2 O5 86.7(4) 2_675 . ?
O3 Na2 O5 16.5(4) . . ?
O4 Na2 O5 76.6(7) 3_465 . ?
O4 Na2 O5 7.2(7) . . ?
O4 Na2 O5 81.2(6) 2_675 . ?
O2 Na2 O5 106.0(4) 2_675 . ?
O2 Na2 O5 175.1(4) 3_465 . ?
O2 Na2 O5 101.1(4) . . ?
O5 Na2 O5 74.1(6) 3_465 . ?
O3 Na2 O5 86.7(4) 3_465 2_675 ?
O3 Na2 O5 16.5(4) 2_675 2_675 ?
O3 Na2 O5 87.5(4) . 2_675 ?
O4 Na2 O5 81.2(6) 3_465 2_675 ?
O4 Na2 O5 76.6(7) . 2_675 ?
O4 Na2 O5 7.2(7) 2_675 2_675 ?
O2 Na2 O5 101.1(4) 2_675 2_675 ?
O2 Na2 O5 106.0(4) 3_465 2_675 ?
O2 Na2 O5 175.1(4) . 2_675 ?
O5 Na2 O5 74.1(6) 3_465 2_675 ?
O5 Na2 O5 74.1(6) . 2_675 ?
O5 Na3 O5 95.8(7) 2_675 3_465 ?
O5 Na3 O5 180.0(9) 2_675 8_455 ?
O5 Na3 O5 84.2(7) 3_465 8_455 ?
O5 Na3 O5 84.2(7) 2_675 7_575 ?
O5 Na3 O5 84.2(7) 3_465 7_575 ?
O5 Na3 O5 95.8(7) 8_455 7_575 ?
O5 Na3 O5 95.8(7) 2_675 . ?
O5 Na3 O5 95.8(7) 3_465 . ?
O5 Na3 O5 84.2(7) 8_455 . ?
O5 Na3 O5 180.0(9) 7_575 . ?
O5 Na3 O5 84.2(7) 2_675 9_665 ?
O5 Na3 O5 180.0(9) 3_465 9_665 ?
O5 Na3 O5 95.8(7) 8_455 9_665 ?
O5 Na3 O5 95.8(7) 7_575 9_665 ?
O5 Na3 O5 84.2(7) . 9_665 ?
O5 Na3 O4 95.6(7) 2_675 7_575 ?
O5 Na3 O4 90.4(8) 3_465 7_575 ?
O5 Na3 O4 84.4(7) 8_455 7_575 ?
O5 Na3 O4 13.5(6) 7_575 7_575 ?
O5 Na3 O4 166.5(6) . 7_575 ?
O5 Na3 O4 89.6(8) 9_665 7_575 ?
O5 Na3 O4 166.5(6) 2_675 8_455 ?
O5 Na3 O4 95.6(7) 3_465 8_455 ?
O5 Na3 O4 13.5(6) 8_455 8_455 ?
O5 Na3 O4 89.6(8) 7_575 8_455 ?
O5 Na3 O4 90.4(8) . 8_455 ?
O5 Na3 O4 84.4(7) 9_665 8_455 ?
O4 Na3 O4 77.0(7) 7_575 8_455 ?
O5 Na3 O4 90.4(8) 2_675 9_665 ?
O5 Na3 O4 166.5(6) 3_465 9_665 ?
O5 Na3 O4 89.6(8) 8_455 9_665 ?
O5 Na3 O4 84.4(7) 7_575 9_665 ?
O5 Na3 O4 95.6(7) . 9_665 ?
O5 Na3 O4 13.5(6) 9_665 9_665 ?
O4 Na3 O4 77.0(7) 7_575 9_665 ?
O4 Na3 O4 77.0(7) 8_455 9_665 ?
O5 Na3 O4 13.5(6) 2_675 2_675 ?
O5 Na3 O4 84.4(7) 3_465 2_675 ?
O5 Na3 O4 166.5(6) 8_455 2_675 ?
O5 Na3 O4 90.4(8) 7_575 2_675 ?
O5 Na3 O4 89.6(8) . 2_675 ?
O5 Na3 O4 95.6(7) 9_665 2_675 ?
O4 Na3 O4 103.0(7) 7_575 2_675 ?
O4 Na3 O4 180.0(7) 8_455 2_675 ?
O4 Na3 O4 103.0(7) 9_665 2_675 ?
O5 Na3 O4 84.4(7) 2_675 . ?
O5 Na3 O4 89.6(8) 3_465 . ?
O5 Na3 O4 95.6(7) 8_455 . ?
O5 Na3 O4 166.5(6) 7_575 . ?
O5 Na3 O4 13.5(6) . . ?
O5 Na3 O4 90.4(8) 9_665 . ?
O4 Na3 O4 180.0(7) 7_575 . ?
O4 Na3 O4 103.0(7) 8_455 . ?
O4 Na3 O4 103.0(7) 9_665 . ?
O4 Na3 O4 77.0(7) 2_675 . ?
O5 Na3 O4 89.6(8) 2_675 3_465 ?
O5 Na3 O4 13.5(6) 3_465 3_465 ?
O5 Na3 O4 90.4(8) 8_455 3_465 ?
O5 Na3 O4 95.6(7) 7_575 3_465 ?
O5 Na3 O4 84.4(7) . 3_465 ?
O5 Na3 O4 166.5(6) 9_665 3_465 ?
O4 Na3 O4 103.0(7) 7_575 3_465 ?
O4 Na3 O4 103.0(7) 8_455 3_465 ?
O4 Na3 O4 180.000(2) 9_665 3_465 ?
O4 Na3 O4 77.0(7) 2_675 3_465 ?
O4 Na3 O4 77.0(7) . 3_465 ?
O1 S1 C1 106.02(17) . . ?
O1 S1 C1 106.02(17) . 10_556 ?
C1 S1 C1 98.2(3) . 10_556 ?
O2 S2 C2 106.32(19) . . ?
O2 S2 C3 106.49(17) . . ?
C2 S2 C3 98.1(2) . . ?
O4 S3 O3 17.5(8) . . ?
O4 S3 O5 22.7(9) . . ?
O3 S3 O5 34.5(8) . . ?
O4 S3 C5 104.7(8) . . ?
O3 S3 C5 109.9(2) . . ?
O5 S3 C5 82.3(8) . . ?
O4 S3 C4 117.6(9) . . ?
O3 S3 C4 100.1(2) . . ?
O5 S3 C4 125.5(8) . . ?
C5 S3 C4 98.2(3) . . ?
O4 S3 Na2 38.0(8) . . ?
O3 S3 Na2 38.44(18) . . ?
O5 S3 Na2 59.8(8) . . ?
C5 S3 Na2 141.83(17) . . ?
C4 S3 Na2 107.07(18) . . ?
S1 O1 Na1 119.34(14) . . ?
S1 O1 Na1 119.34(14) . 10_556 ?
Na1 O1 Na1 83.68(12) . 10_556 ?
S2 O2 Na1 120.84(15) . . ?
S2 O2 Na2 114.15(15) . . ?
Na1 O2 Na2 82.46(9) . . ?
O5 O3 S3 75.4(13) . . ?
O5 O3 Na2 117.6(14) . . ?
S3 O3 Na2 117.5(3) . . ?
O5 O3 Na3 41.9(13) . . ?
S3 O3 Na3 95.8(2) . . ?
Na2 O3 Na3 75.76(14) . . ?
O5 O4 S3 92(3) . . ?
O5 O4 Na2 144(3) . . ?
S3 O4 Na2 120.0(11) . . ?
O5 O4 Na3 64(3) . . ?
S3 O4 Na3 117.9(11) . . ?
Na2 O4 Na3 83.7(6) . . ?
O4 O5 O3 26(2) . . ?
O4 O5 S3 66(3) . . ?
O3 O5 S3 70.0(12) . . ?
O4 O5 Na3 102(3) . . ?
O3 O5 Na3 122.9(17) . . ?
S3 O5 Na3 122.5(12) . . ?
O4 O5 Na2 29(3) . . ?
O3 O5 Na2 45.9(11) . . ?
S3 O5 Na2 91.9(9) . . ?
Na3 O5 Na2 77.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.087