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The crystal structures of the two hydrates Na2SeO4·10H2O and Na2SeO4·7.5H2O are studied for the first time. The structures of Na2SO4·10H2O and Na2SO4·7H2O are reinvestigated as a function of temperature with respect to the degree of disorder of the O atoms of {\rm SO}_{4}^{2-} in the decahydrate and the O atom of water in the heptahydrate. For Na2SO4·10H2O, the unit site occupancy factor (SOF) of O atoms of {\rm SO}_{4}^{2-} was determined at 120 K. After the temperature dependence of the lattice parameters was studied from 120 to 260 K, it was shown that SOF decreased from 1.0 at 120 K to 0.247 at room temperature. The interesting fact that two salts with different chemical compositions and different crystal structures (Na2SO4·7H2O, tetragonal, space group P41212 and Na2SeO4·7.5H2O, monoclinic, space group C2/c) can act mutually as a crystal nucleus is accounted for by similarities in certain fragments of their crystal structures. This phenomenon is attributed to similarities between particular elements of their structures.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614007653/bp5062sup1.cif
Contains datablocks Na2_Se04_75H2O_120k, Na2_SeO4_10H2O_200k, Na2_SO_4_7H2O_120k, Na2_SO4_10H2O_120k, Na2_SO4_10H2O_250k

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614007653/bp5062Na2_Se04_75H2O_120ksup2.hkl
Contains datablock test_selenat01

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614007653/bp5062Na2_SeO4_10H2O_200ksup3.hkl
Contains datablock hs_selenate_10h20

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614007653/bp5062Na2_SO_4_7H2O_120ksup4.hkl
Contains datablock a_naso4_7h2o

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614007653/bp5062Na2_SO4_10H2O_120ksup5.hkl
Contains datablock hs_nase_10h2o_new

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614007653/bp5062Na2_SO4_10H2O_250ksup6.hkl
Contains datablock hs_glauberssalt250_0m

CCDC references: 995680; 995681; 995682; 995683; 995684

Experimental top

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Results and discussion top

Computing details top

Data collection: STOE X-AREA for Na2_Se04_75H2O_120k, Na2_SeO4_10H2O_200k, Na2_SO_4_7H2O_120k, Na2_SO4_10H2O_120k; Bruker APEX2 for Na2_SO4_10H2O_250k. Cell refinement: STOE X-AREA for Na2_Se04_75H2O_120k, Na2_SeO4_10H2O_200k, Na2_SO_4_7H2O_120k, Na2_SO4_10H2O_120k; Bruker SAINT for Na2_SO4_10H2O_250k. Data reduction: STOE X-RED for Na2_Se04_75H2O_120k, Na2_SeO4_10H2O_200k, Na2_SO_4_7H2O_120k, Na2_SO4_10H2O_120k; Bruker SAINT for Na2_SO4_10H2O_250k. For all compounds, program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008). Molecular graphics: Diamond for Na2_Se04_75H2O_120k; Diamond3 for Na2_SeO4_10H2O_200k, Na2_SO_4_7H2O_120k, Na2_SO4_10H2O_120k; Bruker SHELXTL for Na2_SO4_10H2O_250k. Software used to prepare material for publication: publCIF for Na2_Se04_75H2O_120k, Na2_SeO4_10H2O_200k, Na2_SO_4_7H2O_120k, Na2_SO4_10H2O_120k; Bruker SHELXTL for Na2_SO4_10H2O_250k.

Figures top
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(Na2_Se04_75H2O_120k) Sodium selenate heptahemihydrate top
Crystal data top
H15Na2O11.50SeF(000) = 1304
Mr = 324.06Dx = 1.748 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 25.082 (7) ÅCell parameters from 1703 reflections
b = 7.2222 (13) Åθ = 3.1–32.2°
c = 14.148 (5) ŵ = 3.16 mm1
β = 106.08 (3)°T = 120 K
V = 2462.6 (12) Å3Monoclinic prism, colourless
Z = 80.25 × 0.18 × 0.11 mm
Data collection top
STOE IPDS 2T
diffractometer
4234 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3466 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.107
Detector resolution: 6.67 pixels mm-1θmax = 32.0°, θmin = 2.9°
rotation method scansh = 3737
Absorption correction: integration
Coppens (1970)
k = 1010
Tmin = 0.292, Tmax = 0.536l = 2020
51914 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.026All H-atom parameters refined
wR(F2) = 0.079 'w = 1/[σ2(Fo2) + (0.0487P)2 + 2.4105P]' '
where P = (Fo2 + 2Fc2)/3'
S = 1.00(Δ/σ)max = 0.002
4234 reflectionsΔρmax = 0.49 e Å3
192 parametersΔρmin = 1.03 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00151 (17)
Crystal data top
H15Na2O11.50SeV = 2462.6 (12) Å3
Mr = 324.06Z = 8
Monoclinic, C2/cMo Kα radiation
a = 25.082 (7) ŵ = 3.16 mm1
b = 7.2222 (13) ÅT = 120 K
c = 14.148 (5) Å0.25 × 0.18 × 0.11 mm
β = 106.08 (3)°
Data collection top
STOE IPDS 2T
diffractometer
4234 independent reflections
Absorption correction: integration
Coppens (1970)
3466 reflections with I > 2σ(I)
Tmin = 0.292, Tmax = 0.536Rint = 0.107
51914 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0260 restraints
wR(F2) = 0.079All H-atom parameters refined
S = 1.00Δρmax = 0.49 e Å3
4234 reflectionsΔρmin = 1.03 e Å3
192 parameters
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Se10.12538 (2)0.50581 (2)0.43856 (2)0.00804 (6)
Na10.25402 (3)0.48478 (8)0.25255 (5)0.01318 (13)
Na20.48802 (3)0.50577 (8)0.12460 (5)0.01393 (13)
O10.50000.7533 (2)0.25000.0169 (3)
O20.49834 (5)0.27554 (19)0.00232 (9)0.0163 (2)
O30.39327 (6)0.51391 (17)0.01325 (10)0.0168 (2)
O40.43838 (5)0.38294 (17)0.24329 (9)0.0168 (2)
O50.35257 (5)0.54197 (19)0.30729 (10)0.0176 (2)
O60.25084 (6)0.23441 (17)0.36455 (9)0.0152 (2)
O70.15405 (5)0.43353 (18)0.20215 (9)0.0173 (2)
O80.24653 (5)0.73830 (17)0.36305 (9)0.0148 (2)
O90.16577 (5)0.32150 (15)0.45515 (8)0.0139 (2)
O100.08697 (5)0.51212 (14)0.32289 (8)0.0135 (2)
O110.08559 (5)0.49515 (14)0.51372 (9)0.0132 (2)
O120.16395 (5)0.69410 (15)0.46262 (8)0.0131 (2)
H10.4729 (11)0.824 (4)0.230 (2)0.037 (7)*
H2A0.5245 (12)0.214 (4)0.008 (2)0.027 (7)*
H2B0.4728 (13)0.204 (4)0.007 (2)0.038 (8)*
H3A0.3766 (13)0.430 (4)0.024 (2)0.041 (8)*
H3B0.3744 (12)0.601 (4)0.023 (2)0.043 (8)*
H4A0.4325 (11)0.269 (4)0.2288 (19)0.035 (7)*
H4B0.4092 (14)0.428 (5)0.255 (2)0.048 (8)*
H5A0.3694 (13)0.519 (3)0.368 (2)0.026 (7)*
H5B0.3521 (11)0.652 (4)0.3055 (18)0.032 (7)*
H6A0.2217 (12)0.262 (4)0.3815 (18)0.025 (6)*
H6B0.2746 (12)0.220 (4)0.409 (2)0.029 (7)*
H7A0.1346 (15)0.462 (4)0.150 (3)0.042 (9)*
H7B0.1350 (12)0.464 (4)0.243 (2)0.032 (7)*
H8A0.2181 (12)0.728 (4)0.385 (2)0.033 (7)*
H8B0.2721 (13)0.756 (4)0.406 (2)0.031 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Se10.00788 (8)0.00783 (8)0.00858 (8)0.00008 (5)0.00258 (5)0.00012 (4)
Na10.0141 (3)0.0126 (3)0.0134 (3)0.0001 (2)0.0047 (2)0.0001 (2)
Na20.0144 (3)0.0133 (3)0.0134 (3)0.0006 (2)0.0028 (2)0.0001 (2)
O10.0165 (8)0.0115 (7)0.0194 (8)0.0000.0004 (7)0.000
O20.0147 (6)0.0127 (5)0.0225 (6)0.0006 (4)0.0067 (5)0.0001 (4)
O30.0157 (6)0.0129 (5)0.0214 (6)0.0003 (4)0.0046 (5)0.0004 (4)
O40.0149 (6)0.0163 (5)0.0195 (6)0.0034 (4)0.0053 (4)0.0040 (4)
O50.0155 (6)0.0186 (5)0.0185 (6)0.0012 (5)0.0041 (5)0.0001 (5)
O60.0145 (6)0.0182 (5)0.0126 (5)0.0037 (4)0.0032 (4)0.0009 (4)
O70.0153 (6)0.0247 (6)0.0121 (5)0.0026 (5)0.0038 (4)0.0001 (4)
O80.0129 (6)0.0182 (5)0.0139 (5)0.0030 (4)0.0044 (4)0.0012 (4)
O90.0138 (5)0.0110 (5)0.0169 (5)0.0044 (4)0.0043 (4)0.0018 (4)
O100.0134 (5)0.0155 (5)0.0096 (5)0.0001 (4)0.0000 (4)0.0004 (3)
O110.0126 (5)0.0157 (5)0.0138 (5)0.0013 (4)0.0079 (4)0.0002 (4)
O120.0128 (5)0.0108 (4)0.0160 (5)0.0040 (4)0.0047 (4)0.0018 (4)
Geometric parameters (Å, º) top
Se1—O121.6489 (11)Na2—O32.4616 (18)
Se1—O111.6493 (12)Na2—O22.4642 (15)
Se1—O91.6497 (11)Na2—O12.4774 (15)
Se1—O101.6538 (13)Na2—O2iv2.4853 (15)
Na1—O52.4124 (17)Na2—O42.5129 (16)
Na1—O8i2.4147 (15)Na2—Na2iii3.4306 (18)
Na1—O62.4201 (15)Na2—Na2iv3.7379 (18)
Na1—O6ii2.4286 (15)O1—Na2iii2.4774 (15)
Na1—O72.4377 (17)O2—Na2iv2.4853 (15)
Na1—O82.4483 (15)O4—Na2iii2.4034 (16)
Na1—Na1ii3.6163 (7)O6—Na1i2.4286 (15)
Na1—Na1i3.6164 (6)O8—Na1ii2.4147 (15)
Na2—O4iii2.4034 (16)
O12—Se1—O11109.30 (5)O4iii—Na2—O3154.68 (5)
O12—Se1—O9109.51 (6)O4iii—Na2—O295.13 (5)
O11—Se1—O9109.15 (6)O3—Na2—O280.64 (5)
O12—Se1—O10109.22 (6)O4iii—Na2—O178.16 (5)
O11—Se1—O10110.40 (7)O3—Na2—O1110.19 (4)
O9—Se1—O10109.24 (6)O2—Na2—O1166.93 (5)
O5—Na1—O8i99.02 (5)O4iii—Na2—O2iv124.52 (5)
O5—Na1—O697.72 (6)O3—Na2—O2iv79.87 (5)
O8i—Na1—O684.12 (5)O2—Na2—O2iv81.91 (6)
O5—Na1—O6ii86.87 (5)O1—Na2—O2iv92.59 (5)
O8i—Na1—O6ii95.48 (5)O4iii—Na2—O476.47 (6)
O6—Na1—O6ii175.40 (3)O3—Na2—O482.35 (5)
O5—Na1—O7177.96 (6)O2—Na2—O4113.50 (5)
O8i—Na1—O782.96 (5)O1—Na2—O476.14 (4)
O6—Na1—O781.97 (5)O2iv—Na2—O4154.16 (5)
O6ii—Na1—O793.43 (5)Na2iii—O1—Na287.64 (7)
O5—Na1—O885.41 (5)Na2—O2—Na2iv98.09 (6)
O8i—Na1—O8175.33 (4)Na2iii—O4—Na288.47 (5)
O6—Na1—O896.80 (5)Na1—O6—Na1i96.46 (5)
O6ii—Na1—O883.23 (5)Na1ii—O8—Na196.08 (5)
O7—Na1—O892.62 (5)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1, y, z+1/2; (iv) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H8B···O12v0.76 (3)2.12 (3)2.880 (2)172 (3)
O8—H8A···O120.85 (3)1.99 (3)2.8273 (18)168 (3)
O7—H7B···O100.87 (3)1.90 (3)2.7683 (19)173 (3)
O7—H7A···O11vi0.79 (4)2.00 (4)2.790 (2)174 (3)
O6—H6B···O9vii0.74 (3)2.11 (3)2.844 (2)172 (3)
O6—H6A···O90.85 (3)2.01 (3)2.8473 (18)166 (2)
O5—H5B···O7ii0.79 (3)2.04 (3)2.834 (2)177 (3)
O5—H5A···O3viii0.87 (3)1.99 (3)2.837 (2)168 (3)
O4—H4B···O50.86 (3)1.96 (4)2.8021 (19)168 (3)
O4—H4A···O10i0.85 (3)2.00 (3)2.8502 (17)172 (3)
O3—H3B···O9ii0.82 (3)1.95 (3)2.7738 (17)175 (3)
O3—H3A···O12i0.78 (3)2.02 (3)2.7897 (17)172 (3)
O2—H2B···O11i0.80 (3)2.09 (3)2.8842 (18)172 (3)
O2—H2A···O11ix0.78 (3)2.14 (3)2.9055 (18)169 (3)
O1—H1···O10ii0.83 (3)2.01 (3)2.8409 (17)174 (3)
O8—H8B···O12v0.76 (3)2.12 (3)2.880 (2)172 (3)
O8—H8A···O120.85 (3)1.99 (3)2.8273 (18)168 (3)
O7—H7B···O100.87 (3)1.90 (3)2.7683 (19)173 (3)
O7—H7A···O11vi0.79 (4)2.00 (4)2.790 (2)174 (3)
O6—H6B···O9vii0.74 (3)2.11 (3)2.844 (2)172 (3)
O6—H6A···O90.85 (3)2.01 (3)2.8473 (18)166 (2)
O5—H5B···O7ii0.79 (3)2.04 (3)2.834 (2)177 (3)
O5—H5A···O3viii0.87 (3)1.99 (3)2.837 (2)168 (3)
O4—H4B···O50.86 (3)1.96 (4)2.8021 (19)168 (3)
O4—H4A···O10i0.85 (3)2.00 (3)2.8502 (17)172 (3)
O3—H3B···O9ii0.82 (3)1.95 (3)2.7738 (17)175 (3)
O3—H3A···O12i0.78 (3)2.02 (3)2.7897 (17)172 (3)
O2—H2B···O11i0.80 (3)2.09 (3)2.8842 (18)172 (3)
O2—H2A···O11ix0.78 (3)2.14 (3)2.9055 (18)169 (3)
O1—H1···O10ii0.83 (3)2.01 (3)2.8409 (17)174 (3)
O1—H1···O10ii0.83 (3)2.01 (3)2.8409 (17)174 (3)
O2—H2A···O11ix0.78 (3)2.14 (3)2.9055 (18)169 (3)
O2—H2B···O11i0.80 (3)2.09 (3)2.8842 (18)172 (3)
O3—H3A···O12i0.78 (3)2.02 (3)2.7897 (17)172 (3)
O3—H3B···O9ii0.82 (3)1.95 (3)2.7738 (17)175 (3)
O4—H4A···O10i0.85 (3)2.00 (3)2.8502 (17)172 (3)
O4—H4B···O50.86 (3)1.96 (4)2.8021 (19)168 (3)
O5—H5A···O3viii0.87 (3)1.99 (3)2.837 (2)168 (3)
O5—H5B···O7ii0.79 (3)2.04 (3)2.834 (2)177 (3)
O6—H6A···O90.85 (3)2.01 (3)2.8473 (18)166 (2)
O6—H6B···O9vii0.74 (3)2.11 (3)2.844 (2)172 (3)
O7—H7A···O11vi0.79 (4)2.00 (4)2.790 (2)174 (3)
O7—H7B···O100.87 (3)1.90 (3)2.7683 (19)173 (3)
O8—H8A···O120.85 (3)1.99 (3)2.8273 (18)168 (3)
O8—H8B···O12v0.76 (3)2.12 (3)2.880 (2)172 (3)
Symmetry codes: (i) x+1/2, y1/2, z+1/2; (ii) x+1/2, y+1/2, z+1/2; (v) x+1/2, y+3/2, z+1; (vi) x, y+1, z1/2; (vii) x+1/2, y+1/2, z+1; (viii) x, y+1, z+1/2; (ix) x+1/2, y+1/2, z1/2.
(Na2_SeO4_10H2O_200k) Sodium selenate decahydrate top
Crystal data top
H20Na2O14SeF(000) = 752
Mr = 369.10Dx = 1.611 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 11.6498 (13) ÅCell parameters from 10963 reflections
b = 10.5446 (9) Åθ = 2.0–29.6°
c = 13.0181 (15) ŵ = 2.58 mm1
β = 107.929 (9)°T = 200 K
V = 1521.5 (3) Å3Monoclinic prism, colourless
Z = 40.12 × 0.09 × 0.05 mm
Data collection top
STOE IPDS 2T
diffractometer
3495 independent reflections
Radiation source: sealed X-ray tube, 12x0.4mm long-fine focus3060 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.027
Detector resolution: 6.67 pixels mm-1θmax = 27.5°, θmin = 2.5°
rotation method scansh = 1514
Absorption correction: integration
Coppens (1970)
k = 1313
Tmin = 0.620, Tmax = 0.780l = 016
6800 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024All H-atom parameters refined
wR(F2) = 0.061 'w = 1/[σ2(Fo2) + (0.0352P)2 + 0.2411P]' '
where P = (Fo2 + 2Fc2)/3'
S = 1.06(Δ/σ)max = 0.002
3495 reflectionsΔρmax = 0.54 e Å3
235 parametersΔρmin = 0.51 e Å3
20 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0106 (5)
Crystal data top
H20Na2O14SeV = 1521.5 (3) Å3
Mr = 369.10Z = 4
Monoclinic, P21/cMo Kα radiation
a = 11.6498 (13) ŵ = 2.58 mm1
b = 10.5446 (9) ÅT = 200 K
c = 13.0181 (15) Å0.12 × 0.09 × 0.05 mm
β = 107.929 (9)°
Data collection top
STOE IPDS 2T
diffractometer
3495 independent reflections
Absorption correction: integration
Coppens (1970)
3060 reflections with I > 2σ(I)
Tmin = 0.620, Tmax = 0.780Rint = 0.027
6800 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02420 restraints
wR(F2) = 0.061All H-atom parameters refined
S = 1.06Δρmax = 0.54 e Å3
3495 reflectionsΔρmin = 0.51 e Å3
235 parameters
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Se10.74825 (2)0.63964 (2)0.75969 (2)0.01560 (7)
Na10.24297 (6)0.75513 (6)0.02119 (5)0.02274 (15)
Na20.25650 (6)0.88793 (7)0.23684 (5)0.02151 (15)
O50.14506 (11)0.71982 (12)0.11612 (10)0.0246 (3)
O20.35336 (11)0.78364 (12)0.14703 (10)0.0237 (3)
O60.38166 (11)0.89064 (13)0.11681 (11)0.0257 (3)
O10.11765 (11)0.60739 (13)0.15178 (11)0.0259 (3)
O40.37015 (12)0.56985 (14)0.05278 (11)0.0293 (3)
O70.13353 (12)1.04175 (12)0.11740 (11)0.0270 (3)
O30.11521 (12)0.93934 (14)0.08438 (12)0.0310 (3)
O120.63205 (10)0.69711 (11)0.66509 (9)0.0239 (3)
O100.76752 (11)0.71909 (11)0.87208 (9)0.0269 (3)
O110.72352 (12)0.49094 (11)0.78199 (10)0.0294 (3)
O130.86808 (11)0.65052 (12)0.71978 (10)0.0282 (3)
O80.37693 (12)1.04003 (12)0.36147 (11)0.0283 (3)
O140.90014 (13)0.65112 (13)0.08492 (11)0.0284 (3)
O90.59775 (13)0.85025 (13)0.94526 (11)0.0288 (3)
H1A0.0485 (11)0.628 (2)0.1850 (18)0.042 (7)*
H1B0.110 (2)0.5352 (12)0.1324 (18)0.042 (7)*
H2A0.334 (2)0.8521 (13)0.1759 (18)0.035 (7)*
H2B0.4255 (10)0.793 (2)0.1190 (18)0.044 (7)*
H3A0.121 (2)0.9920 (17)0.1279 (15)0.041 (7)*
H3B0.128 (4)0.966 (5)0.0224 (17)0.16 (2)*
H4A0.341 (2)0.539 (2)0.0961 (16)0.048 (7)*
H4B0.4423 (12)0.558 (5)0.080 (3)0.143 (17)*
H5A0.170 (2)0.6512 (14)0.1437 (19)0.039 (7)*
H5B0.0720 (9)0.713 (3)0.100 (2)0.053 (8)*
H6A0.388 (2)0.9635 (12)0.0972 (18)0.044 (7)*
H6B0.4506 (12)0.864 (2)0.137 (2)0.057 (9)*
H7A0.0611 (11)1.050 (5)0.103 (4)0.157 (19)*
H7B0.162 (2)1.1121 (13)0.121 (2)0.038 (7)*
H8A0.362 (2)1.1151 (11)0.349 (2)0.036 (7)*
H8B0.366 (3)1.016 (3)0.4178 (17)0.104 (13)*
H9A0.6383 (19)0.8028 (19)0.9205 (18)0.041 (7)*
H9B0.618 (2)0.834 (2)1.0092 (9)0.046 (7)*
H14A0.8792 (19)0.7064 (16)0.1187 (15)0.030 (6)*
H14B0.862 (2)0.666 (3)0.0222 (10)0.048 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Se10.01716 (10)0.01285 (10)0.01630 (10)0.00012 (5)0.00444 (6)0.00002 (5)
Na10.0238 (3)0.0223 (3)0.0227 (3)0.0006 (3)0.0079 (3)0.0012 (3)
Na20.0232 (3)0.0190 (3)0.0218 (3)0.0005 (2)0.0061 (3)0.0005 (2)
O50.0216 (6)0.0227 (6)0.0281 (6)0.0002 (5)0.0059 (5)0.0016 (5)
O20.0215 (6)0.0214 (6)0.0263 (6)0.0018 (5)0.0042 (5)0.0025 (5)
O60.0206 (6)0.0246 (6)0.0316 (7)0.0006 (5)0.0075 (5)0.0001 (5)
O10.0199 (6)0.0259 (6)0.0297 (7)0.0012 (5)0.0044 (5)0.0012 (5)
O40.0281 (7)0.0322 (7)0.0301 (7)0.0029 (6)0.0127 (5)0.0042 (6)
O70.0245 (6)0.0207 (6)0.0332 (7)0.0020 (5)0.0051 (5)0.0016 (5)
O30.0310 (7)0.0300 (7)0.0346 (7)0.0025 (6)0.0142 (6)0.0082 (6)
O120.0195 (6)0.0247 (6)0.0236 (6)0.0021 (5)0.0011 (5)0.0027 (5)
O100.0337 (7)0.0247 (6)0.0219 (6)0.0001 (5)0.0080 (5)0.0054 (5)
O110.0420 (8)0.0156 (6)0.0304 (6)0.0021 (5)0.0107 (6)0.0012 (5)
O130.0225 (6)0.0336 (7)0.0297 (7)0.0009 (5)0.0099 (5)0.0034 (5)
O80.0312 (7)0.0209 (6)0.0299 (7)0.0000 (5)0.0049 (5)0.0015 (5)
O140.0295 (7)0.0289 (7)0.0257 (7)0.0034 (5)0.0071 (6)0.0010 (5)
O90.0258 (7)0.0332 (7)0.0264 (7)0.0031 (5)0.0068 (5)0.0005 (6)
Geometric parameters (Å, º) top
Se1—O111.6362 (12)Na1—Na23.5977 (10)
Se1—O131.6366 (13)Na2—O72.3936 (15)
Se1—O121.6401 (11)Na2—O82.4024 (15)
Se1—O101.6404 (11)Na2—O2ii2.4045 (14)
Na1—O22.3928 (14)Na2—O62.4436 (14)
Na1—O52.4269 (14)Na2—O52.4580 (14)
Na1—O32.4313 (15)Na2—O1ii2.4831 (15)
Na1—O12.4332 (14)Na2—Na1ii3.5396 (10)
Na1—O42.4619 (16)O2—Na2i2.4045 (14)
Na1—O62.4683 (15)O1—Na2i2.4829 (15)
Na1—Na2i3.5395 (10)
O11—Se1—O13109.73 (6)O4—Na1—O689.68 (5)
O11—Se1—O12109.73 (6)O7—Na2—O895.43 (5)
O13—Se1—O12108.86 (6)O7—Na2—O2ii171.68 (5)
O11—Se1—O10108.32 (6)O8—Na2—O2ii90.82 (5)
O13—Se1—O10110.58 (6)O7—Na2—O686.12 (5)
O12—Se1—O10109.62 (6)O8—Na2—O694.86 (5)
O2—Na1—O5175.61 (5)O2ii—Na2—O698.85 (5)
O2—Na1—O394.02 (5)O7—Na2—O588.89 (5)
O5—Na1—O389.67 (5)O8—Na2—O5175.55 (5)
O2—Na1—O186.30 (5)O2ii—Na2—O584.99 (5)
O5—Na1—O195.71 (5)O6—Na2—O584.33 (5)
O3—Na1—O195.85 (5)O7—Na2—O1ii89.92 (5)
O2—Na1—O488.96 (5)O8—Na2—O1ii86.70 (5)
O5—Na1—O487.30 (5)O2ii—Na2—O1ii84.94 (5)
O3—Na1—O4176.73 (5)O6—Na2—O1ii175.86 (5)
O1—Na1—O485.68 (5)O5—Na2—O1ii94.41 (5)
O2—Na1—O693.22 (5)Na1—O5—Na294.87 (5)
O5—Na1—O684.46 (5)Na1—O2—Na2i95.09 (5)
O3—Na1—O688.80 (5)Na2—O6—Na194.18 (5)
O1—Na1—O6175.34 (5)Na1—O1—Na2i92.10 (5)
Symmetry codes: (i) x, y+3/2, z1/2; (ii) x, y+3/2, z+1/2.
(Na2_SO_4_7H2O_120k) Sodium sulfate heptahydrate top
Crystal data top
H14Na2O11SDx = 1.564 Mg m3
Mr = 268.15Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P41212Cell parameters from 27181 reflections
a = 14.3249 (15) Åθ = 2.0–29.6°
c = 22.202 (4) ŵ = 0.40 mm1
V = 4556.0 (10) Å3T = 120 K
Z = 16, colourless
F(000) = 22400.53 × 0.48 × 0.44 mm
Data collection top
STOE IPDS 2
diffractometer
6253 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3969 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.064
Detector resolution: 6.67 pixels mm-1θmax = 29.4°, θmin = 1.7°
rotation method scansh = 1313
Absorption correction: integration
Coppens (1970)
k = 019
Tmin = 0.529, Tmax = 0.721l = 030
6253 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Only H-atom coordinates refined
wR(F2) = 0.110 'w = 1/[σ2(Fo2) + (0.0622P)2 + 0.0819P]' '
where P = (Fo2 + 2Fc2)/3'
S = 1.06(Δ/σ)max = 0.008
6253 reflectionsΔρmax = 0.36 e Å3
340 parametersΔρmin = 0.40 e Å3
39 restraintsAbsolute structure: 'Refined as an inversion twin.'
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.46 (19)
Crystal data top
H14Na2O11SZ = 16
Mr = 268.15Mo Kα radiation
Tetragonal, P41212µ = 0.40 mm1
a = 14.3249 (15) ÅT = 120 K
c = 22.202 (4) Å0.53 × 0.48 × 0.44 mm
V = 4556.0 (10) Å3
Data collection top
STOE IPDS 2
diffractometer
6253 independent reflections
Absorption correction: integration
Coppens (1970)
3969 reflections with I > 2σ(I)
Tmin = 0.529, Tmax = 0.721Rint = 0.064
6253 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.028Only H-atom coordinates refined
wR(F2) = 0.110Δρmax = 0.36 e Å3
S = 1.06Δρmin = 0.40 e Å3
6253 reflectionsAbsolute structure: 'Refined as an inversion twin.'
340 parametersAbsolute structure parameter: 0.46 (19)
39 restraints
Special details top

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

Refinement. 'Refined as a 2-component inversion twin.' 'Inversion twinning was indicated by' 'SHELXL, because of a large Flack parameter.' 'A structure solution in a corresponding centrosymmetric' 'space-group was not successful.'

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Na10.61239 (11)0.62755 (10)0.11347 (9)0.0113 (3)
Na20.86243 (11)0.62747 (10)0.13653 (9)0.0110 (3)
Na31.11223 (11)0.62209 (10)0.11353 (9)0.0112 (3)
Na41.36229 (11)0.62337 (10)0.13648 (10)0.0112 (3)
S10.37372 (7)0.37372 (7)1.00000.0068 (3)
S20.87743 (7)0.87743 (7)0.00000.0052 (3)
S30.37736 (6)0.87374 (7)0.00020 (8)0.00575 (13)
O10.9621 (2)0.87792 (16)0.03787 (15)0.0122 (6)
O20.7929 (2)0.87552 (16)0.03841 (15)0.0116 (6)
O30.7385 (2)0.7428 (2)0.12626 (12)0.0130 (5)
H170.749 (2)0.776 (2)0.0967 (10)0.016*
H180.738 (3)0.773 (2)0.1568 (10)0.016*
O40.9906 (2)0.73588 (19)0.12342 (14)0.0108 (5)
H101.015 (2)0.761 (2)0.1515 (12)0.013*
H280.976 (2)0.777 (2)0.1001 (12)0.013*
O50.84084 (17)0.62624 (15)0.02527 (12)0.0142 (5)
H160.868 (2)0.5822 (17)0.0107 (19)0.017*
H150.856 (2)0.6728 (17)0.0066 (17)0.017*
O60.64416 (18)0.64416 (18)0.00000.0168 (7)
H230.6967 (17)0.645 (2)0.0096 (18)0.020*
O70.9846 (2)0.5125 (2)0.12435 (16)0.0141 (6)
H110.994 (2)0.477 (2)0.1533 (11)0.017*
H120.991 (3)0.481 (2)0.0936 (10)0.017*
O80.4886 (2)0.5129 (2)0.12318 (14)0.0142 (5)
H240.502 (3)0.472 (2)0.1479 (13)0.017*
H250.491 (3)0.485 (2)0.0901 (10)0.017*
O90.7382 (2)0.5172 (2)0.12578 (11)0.0095 (5)
H190.754 (3)0.492 (2)0.0951 (11)0.011*
H200.721 (2)0.479 (2)0.1499 (11)0.011*
O100.89422 (16)0.64399 (16)0.25008 (14)0.0149 (5)
H130.9453 (17)0.6291 (18)0.244 (2)0.018*
H140.8817 (19)0.6962 (17)0.2396 (16)0.018*
O110.4861 (2)0.7361 (2)0.12468 (14)0.0113 (5)
H270.469 (2)0.775 (2)0.1015 (12)0.014*
H260.517 (2)0.761 (2)0.1490 (13)0.014*
O121.39358 (19)0.60642 (19)0.25000.0183 (7)
H31.4488 (17)0.609 (2)0.2395 (18)0.022*
O131.09071 (16)0.62254 (16)0.22498 (11)0.0140 (5)
H81.101 (2)0.576 (2)0.2476 (18)0.017*
H91.120 (2)0.665 (2)0.248 (2)0.017*
O140.58986 (16)0.62724 (16)0.22466 (12)0.0150 (5)
H210.600 (2)0.5792 (17)0.2462 (15)0.018*
H220.618 (2)0.6679 (18)0.2445 (19)0.018*
O151.2366 (2)0.7329 (2)0.12545 (12)0.0146 (6)
H61.233 (3)0.763 (2)0.1564 (10)0.018*
H71.244 (2)0.765 (2)0.0959 (10)0.018*
O161.34020 (17)0.62341 (16)0.02522 (12)0.0155 (5)
H11.354 (2)0.6708 (17)0.0060 (17)0.019*
H21.368 (2)0.5805 (18)0.009 (2)0.019*
O171.2396 (2)0.5106 (2)0.12675 (11)0.0108 (6)
H51.222 (2)0.471 (2)0.1501 (11)0.013*
H41.257 (3)0.487 (2)0.0974 (11)0.013*
O180.2922 (2)0.86527 (18)0.03800 (14)0.0098 (5)
O190.38331 (17)0.7888 (2)0.03822 (14)0.0096 (6)
O200.4615 (2)0.88116 (17)0.03838 (15)0.0112 (6)
O210.37158 (17)0.9581 (2)0.03852 (15)0.0116 (6)
O220.37269 (15)0.2887 (2)0.96110 (14)0.0091 (6)
O230.4588 (2)0.37422 (16)1.03840 (14)0.0108 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0111 (7)0.0106 (7)0.0123 (7)0.0024 (4)0.0012 (6)0.0001 (5)
Na20.0102 (7)0.0094 (7)0.0136 (8)0.0011 (4)0.0008 (6)0.0004 (5)
Na30.0110 (7)0.0109 (7)0.0117 (7)0.0026 (4)0.0013 (6)0.0002 (5)
Na40.0102 (7)0.0105 (7)0.0130 (7)0.0009 (4)0.0005 (6)0.0001 (5)
S10.0073 (4)0.0073 (4)0.0058 (7)0.0023 (3)0.0002 (3)0.0002 (3)
S20.0054 (4)0.0054 (4)0.0048 (6)0.0003 (3)0.0000 (3)0.0000 (3)
S30.0029 (4)0.0091 (5)0.0053 (2)0.0009 (3)0.0000 (3)0.0002 (3)
O10.0102 (13)0.0145 (14)0.0118 (15)0.0018 (8)0.0034 (12)0.0002 (9)
O20.0092 (13)0.0137 (14)0.0120 (15)0.0013 (8)0.0052 (13)0.0007 (8)
O30.0198 (13)0.0081 (12)0.0111 (10)0.0015 (9)0.0030 (10)0.0031 (9)
O40.0124 (13)0.0068 (10)0.0132 (9)0.0000 (9)0.0049 (10)0.0002 (9)
O50.0221 (13)0.0093 (11)0.0112 (12)0.0007 (10)0.0024 (9)0.0016 (8)
O60.0184 (9)0.0184 (9)0.0137 (15)0.0012 (13)0.0005 (13)0.0005 (13)
O70.0140 (14)0.0127 (13)0.0156 (10)0.0005 (8)0.0044 (11)0.0004 (10)
O80.0131 (13)0.0119 (13)0.0174 (10)0.0022 (9)0.0027 (10)0.0020 (11)
O90.0188 (12)0.0042 (11)0.0054 (9)0.0003 (9)0.0059 (10)0.0000 (8)
O100.0155 (10)0.0125 (10)0.0166 (11)0.0023 (6)0.0013 (12)0.0001 (12)
O110.0121 (13)0.0068 (10)0.0148 (9)0.0010 (8)0.0051 (10)0.0004 (9)
O120.0187 (9)0.0187 (9)0.0174 (16)0.0021 (13)0.0019 (13)0.0019 (13)
O130.0198 (13)0.0100 (11)0.0124 (12)0.0020 (10)0.0027 (9)0.0020 (8)
O140.0204 (13)0.0094 (11)0.0153 (13)0.0000 (10)0.0027 (9)0.0019 (8)
O150.0183 (12)0.0145 (13)0.0111 (11)0.0025 (10)0.0025 (11)0.0022 (10)
O160.0221 (13)0.0105 (12)0.0140 (12)0.0015 (10)0.0041 (9)0.0028 (8)
O170.0181 (13)0.0084 (12)0.0058 (9)0.0050 (9)0.0049 (10)0.0005 (9)
O180.0071 (11)0.0117 (10)0.0106 (13)0.0014 (8)0.0041 (10)0.0025 (9)
O190.0104 (11)0.0092 (12)0.0093 (13)0.0000 (8)0.0006 (9)0.0050 (10)
O200.0098 (12)0.0120 (12)0.0118 (14)0.0018 (8)0.0037 (11)0.0019 (9)
O210.0150 (14)0.0100 (13)0.0096 (14)0.0016 (8)0.0014 (9)0.0039 (11)
O220.0120 (13)0.0074 (12)0.0079 (13)0.0033 (7)0.0027 (8)0.0048 (12)
O230.0097 (13)0.0132 (13)0.0096 (14)0.0010 (8)0.0036 (12)0.0032 (8)
Geometric parameters (Å, º) top
Na1—O112.399 (3)Na4—O152.401 (4)
Na1—O92.414 (3)Na4—O11iii2.413 (3)
Na1—O82.426 (4)Na4—O8iii2.421 (3)
Na1—O32.463 (3)Na4—O162.490 (3)
Na1—O142.490 (3)Na4—O122.571 (2)
Na1—O62.571 (2)Na4—Na1iii3.619 (2)
Na1—Na23.618 (3)S1—O23iv1.488 (3)
Na1—Na4i3.619 (2)S1—O231.488 (3)
Na2—O92.391 (3)S1—O22iv1.493 (3)
Na2—O72.418 (3)S1—O221.493 (3)
Na2—O42.422 (3)S2—O1v1.475 (3)
Na2—O32.436 (4)S2—O11.475 (3)
Na2—O52.490 (3)S2—O2v1.482 (3)
Na2—O102.573 (4)S2—O21.482 (3)
Na2—Na33.615 (3)S3—O211.480 (3)
Na3—O42.397 (3)S3—O201.482 (3)
Na3—O152.401 (3)S3—O191.483 (3)
Na3—O72.421 (4)S3—O181.490 (3)
Na3—O172.443 (3)O6—Na1v2.571 (2)
Na3—O132.494 (3)O8—Na4i2.421 (3)
Na3—O10ii2.570 (4)O10—Na3vi2.570 (4)
Na3—Na43.618 (3)O11—Na4i2.413 (3)
Na4—O172.397 (4)O12—Na4vii2.572 (2)
O11—Na1—O9167.53 (13)O17—Na4—O1583.20 (13)
O11—Na1—O883.01 (11)O17—Na4—O11iii168.60 (13)
O9—Na1—O895.31 (11)O15—Na4—O11iii95.89 (11)
O11—Na1—O396.12 (12)O17—Na4—O8iii95.53 (12)
O9—Na1—O383.01 (13)O15—Na4—O8iii167.15 (14)
O8—Na1—O3168.28 (13)O11iii—Na4—O8iii82.81 (12)
O11—Na1—O1478.50 (10)O17—Na4—O1679.49 (10)
O9—Na1—O1489.05 (10)O15—Na4—O1678.66 (10)
O8—Na1—O1479.39 (11)O11iii—Na4—O1689.17 (11)
O3—Na1—O1488.97 (10)O8iii—Na4—O1688.52 (11)
O11—Na1—O6100.09 (10)O17—Na4—O1298.77 (9)
O9—Na1—O692.26 (8)O15—Na4—O12107.00 (13)
O8—Na1—O6106.20 (13)O11iii—Na4—O1292.38 (9)
O3—Na1—O685.48 (12)O8iii—Na4—O1285.84 (12)
O14—Na1—O6174.10 (12)O16—Na4—O12173.92 (12)
O9—Na2—O794.44 (12)O23iv—S1—O23108.7 (2)
O9—Na2—O4167.30 (13)O23iv—S1—O22iv110.09 (13)
O7—Na2—O482.80 (12)O23—S1—O22iv109.70 (19)
O9—Na2—O384.06 (13)O23iv—S1—O22109.70 (19)
O7—Na2—O3168.21 (13)O23—S1—O22110.09 (13)
O4—Na2—O396.10 (11)O22iv—S1—O22108.6 (2)
O9—Na2—O578.69 (10)O1v—S2—O1108.5 (2)
O7—Na2—O588.52 (11)O1v—S2—O2v110.1 (2)
O4—Na2—O588.82 (11)O1—S2—O2v110.31 (14)
O3—Na2—O579.71 (10)O1v—S2—O2110.31 (14)
O9—Na2—O10106.87 (10)O1—S2—O2110.1 (2)
O7—Na2—O1092.53 (11)O2v—S2—O2107.5 (2)
O4—Na2—O1085.68 (10)O21—S3—O20108.61 (14)
O3—Na2—O1099.11 (11)O21—S3—O19110.2 (2)
O5—Na2—O10174.23 (9)O20—S3—O19109.94 (17)
O4—Na3—O1594.58 (12)O21—S3—O18110.36 (17)
O4—Na3—O783.27 (11)O20—S3—O18110.0 (2)
O15—Na3—O7167.93 (14)O19—S3—O18107.71 (15)
O4—Na3—O17167.70 (13)Na2—O3—Na195.22 (13)
O15—Na3—O1782.23 (13)Na3—O4—Na297.24 (11)
O7—Na3—O1797.36 (11)Na1—O6—Na1v158.03 (18)
O4—Na3—O1379.48 (10)Na2—O7—Na396.67 (12)
O15—Na3—O1388.89 (11)Na4i—O8—Na196.60 (11)
O7—Na3—O1379.04 (11)Na2—O9—Na197.70 (12)
O17—Na3—O1388.56 (10)Na3vi—O10—Na2158.12 (10)
O4—Na3—O10ii106.28 (11)Na1—O11—Na4i97.56 (11)
O15—Na3—O10ii92.11 (11)Na4—O12—Na4vii158.09 (18)
O7—Na3—O10ii99.90 (12)Na4—O15—Na397.80 (13)
O17—Na3—O10ii85.76 (9)Na4—O17—Na396.75 (13)
O13—Na3—O10ii174.05 (9)
Symmetry codes: (i) x1, y, z; (ii) y+1/2, x+3/2, z1/4; (iii) x+1, y, z; (iv) y, x, z+2; (v) y, x, z; (vi) y+3/2, x1/2, z+1/4; (vii) y+2, x+2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O17—H4···O22viii0.77 (2)2.14 (3)2.863 (4)156 (3)
O17—H5···O18ix0.81 (2)2.05 (2)2.850 (4)167 (3)
O16—H2···O23viii0.82 (2)2.03 (3)2.791 (4)154 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O15—H6···O22x0.81 (2)2.01 (3)2.785 (4)159 (3)
O14—H22···O18xi0.83 (2)2.04 (2)2.825 (4)157 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O13—H9···O22xii0.90 (4)1.99 (3)2.820 (4)152 (3)
O13—H8···O21ix0.85 (3)1.95 (3)2.799 (4)172 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O11—H26···O21xi0.78 (2)2.13 (3)2.849 (4)152 (4)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O9—H20···O2ix0.80 (2)2.03 (2)2.819 (4)168 (3)
O9—H19···O19v0.80 (2)2.07 (2)2.825 (4)158 (3)
O8—H25···O23xiii0.84 (2)2.01 (3)2.770 (4)150 (3)
O8—H24···O1ix0.82 (2)2.03 (2)2.853 (4)177 (3)
O7—H12···O21v0.82 (2)2.04 (3)2.802 (4)153 (3)
O7—H11···O20ix0.83 (2)2.00 (2)2.809 (4)168 (4)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O5—H15···O2v0.82 (2)2.01 (2)2.818 (4)172 (3)
O5—H16···O20v0.81 (2)2.05 (3)2.811 (4)156 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O4—H10···O23xii0.80 (2)2.13 (3)2.878 (4)155 (3)
O3—H18···O19xi0.81 (2)2.03 (2)2.795 (4)158 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O17—H4···O22viii0.77 (2)2.14 (3)2.863 (4)156 (3)
O17—H5···O18ix0.81 (2)2.05 (2)2.850 (4)167 (3)
O16—H2···O23viii0.82 (2)2.03 (3)2.791 (4)154 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O15—H6···O22x0.81 (2)2.01 (3)2.785 (4)159 (3)
O14—H22···O18xi0.83 (2)2.04 (2)2.825 (4)157 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O13—H9···O22xii0.90 (4)1.99 (3)2.820 (4)152 (3)
O13—H8···O21ix0.85 (3)1.95 (3)2.799 (4)172 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O11—H26···O21xi0.78 (2)2.13 (3)2.849 (4)152 (4)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O9—H20···O2ix0.80 (2)2.03 (2)2.819 (4)168 (3)
O9—H19···O19v0.80 (2)2.07 (2)2.825 (4)158 (3)
O8—H25···O23xiii0.84 (2)2.01 (3)2.770 (4)150 (3)
O8—H24···O1ix0.82 (2)2.03 (2)2.853 (4)177 (3)
O7—H12···O21v0.82 (2)2.04 (3)2.802 (4)153 (3)
O7—H11···O20ix0.83 (2)2.00 (2)2.809 (4)168 (4)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O5—H15···O2v0.82 (2)2.01 (2)2.818 (4)172 (3)
O5—H16···O20v0.81 (2)2.05 (3)2.811 (4)156 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O4—H10···O23xii0.80 (2)2.13 (3)2.878 (4)155 (3)
O3—H18···O19xi0.81 (2)2.03 (2)2.795 (4)158 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O3—H18···O19xi0.81 (2)2.03 (2)2.795 (4)158 (3)
O4—H10···O23xii0.80 (2)2.13 (3)2.878 (4)155 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O5—H15···O2v0.82 (2)2.01 (2)2.818 (4)172 (3)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O7—H11···O20ix0.83 (2)2.00 (2)2.809 (4)168 (4)
O7—H12···O21v0.82 (2)2.04 (3)2.802 (4)153 (3)
O8—H24···O1ix0.82 (2)2.03 (2)2.853 (4)177 (3)
O8—H25···O23xiii0.84 (2)2.01 (3)2.770 (4)150 (3)
O9—H19···O19v0.80 (2)2.07 (2)2.825 (4)158 (3)
O9—H20···O2ix0.80 (2)2.03 (2)2.819 (4)168 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O11—H26···O21xi0.78 (2)2.13 (3)2.849 (4)152 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O13—H8···O21ix0.85 (3)1.95 (3)2.799 (4)172 (4)
O13—H9···O22xii0.90 (4)1.99 (3)2.820 (4)152 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O14—H22···O18xi0.83 (2)2.04 (2)2.825 (4)157 (3)
O15—H6···O22x0.81 (2)2.01 (3)2.785 (4)159 (3)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O16—H2···O23viii0.82 (2)2.03 (3)2.791 (4)154 (3)
O17—H5···O18ix0.81 (2)2.05 (2)2.850 (4)167 (3)
O17—H4···O22viii0.77 (2)2.14 (3)2.863 (4)156 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O3—H18···O19xi0.81 (2)2.03 (2)2.795 (4)158 (3)
O4—H10···O23xii0.80 (2)2.13 (3)2.878 (4)155 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O5—H16···O20v0.81 (2)2.05 (3)2.811 (4)156 (3)
O5—H15···O2v0.82 (2)2.01 (2)2.818 (4)172 (3)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O7—H11···O20ix0.83 (2)2.00 (2)2.809 (4)168 (4)
O7—H12···O21v0.82 (2)2.04 (3)2.802 (4)153 (3)
O8—H24···O1ix0.82 (2)2.03 (2)2.853 (4)177 (3)
O8—H25···O23xiii0.84 (2)2.01 (3)2.770 (4)150 (3)
O9—H19···O19v0.80 (2)2.07 (2)2.825 (4)158 (3)
O9—H20···O2ix0.80 (2)2.03 (2)2.819 (4)168 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O11—H26···O21xi0.78 (2)2.13 (3)2.849 (4)152 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O13—H8···O21ix0.85 (3)1.95 (3)2.799 (4)172 (4)
O13—H9···O22xii0.90 (4)1.99 (3)2.820 (4)152 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O14—H22···O18xi0.83 (2)2.04 (2)2.825 (4)157 (3)
O15—H6···O22x0.81 (2)2.01 (3)2.785 (4)159 (3)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O16—H2···O23viii0.82 (2)2.03 (3)2.791 (4)154 (3)
O17—H5···O18ix0.81 (2)2.05 (2)2.850 (4)167 (3)
O17—H4···O22viii0.77 (2)2.14 (3)2.863 (4)156 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O3—H18···O19xi0.81 (2)2.03 (2)2.795 (4)158 (3)
O4—H10···O23xii0.80 (2)2.13 (3)2.878 (4)155 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O5—H16···O20v0.81 (2)2.05 (3)2.811 (4)156 (3)
O5—H15···O2v0.82 (2)2.01 (2)2.818 (4)172 (3)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O7—H11···O20ix0.83 (2)2.00 (2)2.809 (4)168 (4)
O7—H12···O21v0.82 (2)2.04 (3)2.802 (4)153 (3)
O8—H24···O1ix0.82 (2)2.03 (2)2.853 (4)177 (3)
O8—H25···O23xiii0.84 (2)2.01 (3)2.770 (4)150 (3)
O9—H19···O19v0.80 (2)2.07 (2)2.825 (4)158 (3)
O9—H20···O2ix0.80 (2)2.03 (2)2.819 (4)168 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O11—H26···O21xi0.78 (2)2.13 (3)2.849 (4)152 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O13—H8···O21ix0.85 (3)1.95 (3)2.799 (4)172 (4)
O13—H9···O22xii0.90 (4)1.99 (3)2.820 (4)152 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O14—H22···O18xi0.83 (2)2.04 (2)2.825 (4)157 (3)
O15—H6···O22x0.81 (2)2.01 (3)2.785 (4)159 (3)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O16—H2···O23viii0.82 (2)2.03 (3)2.791 (4)154 (3)
O17—H5···O18ix0.81 (2)2.05 (2)2.850 (4)167 (3)
O17—H4···O22viii0.77 (2)2.14 (3)2.863 (4)156 (3)
Symmetry codes: (iii) x+1, y, z; (v) y, x, z; (vi) y+3/2, x1/2, z+1/4; (viii) y+1, x, z+1; (ix) x+3/2, y1/2, z+1/4; (x) y+3/2, x+1/2, z3/4; (xi) y+3/2, x+1/2, z+1/4; (xii) x+3/2, y+1/2, z+5/4; (xiii) x, y, z1.
(Na2_SO4_10H2O_120k) Sodium sulfate decahydrate top
Crystal data top
H20Na2O14SF(000) = 680
Mr = 322.21Dx = 1.484 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 11.470 (2) ÅCell parameters from 4106 reflections
b = 10.3515 (12) Åθ = 2.8–29.6°
c = 12.759 (2) ŵ = 0.34 mm1
β = 107.815 (15)°T = 120 K
V = 1442.2 (4) Å3Monoclinic prism, colourless
Z = 40.53 × 0.45 × 0.37 mm
Data collection top
STOE IPDS 2
diffractometer
3876 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-finefocus3441 reflections with I > 2σ(I)
Plane graphite monochromatorRint = 0.119
Detector resolution: 6.67 pixels mm-1θmax = 29.2°, θmin = 1.9°
rotation method scansh = 1514
Absorption correction: integration
Coppens (1970)
k = 014
Tmin = 0.441, Tmax = 0.796l = 017
3876 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028All H-atom parameters refined
wR(F2) = 0.076 'w = 1/[σ2(Fo2) + (0.054P)2 + 0.1271P]' '
where P = (Fo2 + 2Fc2)/3'
S = 1.05(Δ/σ)max = 0.001
3876 reflectionsΔρmax = 0.69 e Å3
235 parametersΔρmin = 0.56 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0111 (14)
Crystal data top
H20Na2O14SV = 1442.2 (4) Å3
Mr = 322.21Z = 4
Monoclinic, P21/cMo Kα radiation
a = 11.470 (2) ŵ = 0.34 mm1
b = 10.3515 (12) ÅT = 120 K
c = 12.759 (2) Å0.53 × 0.45 × 0.37 mm
β = 107.815 (15)°
Data collection top
STOE IPDS 2
diffractometer
3876 independent reflections
Absorption correction: integration
Coppens (1970)
3441 reflections with I > 2σ(I)
Tmin = 0.441, Tmax = 0.796Rint = 0.119
3876 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.076All H-atom parameters refined
S = 1.05Δρmax = 0.69 e Å3
3876 reflectionsΔρmin = 0.56 e Å3
235 parameters
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
S10.74847 (2)0.63907 (2)0.75853 (2)0.00790 (7)
Na10.24380 (3)0.75456 (4)0.01838 (3)0.01176 (10)
Na20.25537 (3)0.88729 (4)0.23846 (3)0.01132 (10)
O10.11388 (7)0.60787 (7)0.15079 (6)0.01386 (14)
O20.35429 (7)0.78653 (7)0.14593 (6)0.01278 (14)
O30.11844 (7)0.94304 (8)0.08351 (7)0.01664 (15)
O40.36884 (7)0.56458 (7)0.05541 (6)0.01573 (15)
O50.14374 (6)0.71693 (7)0.11880 (6)0.01315 (14)
O60.38493 (7)0.89065 (7)0.11985 (6)0.01378 (14)
O70.13273 (7)1.04630 (7)0.11977 (6)0.01487 (15)
O80.37653 (7)1.04462 (7)0.36125 (6)0.01537 (15)
O90.60148 (7)0.84796 (8)0.94609 (6)0.01558 (15)
O100.76428 (7)0.71185 (7)0.86187 (5)0.01399 (14)
O110.72859 (7)0.50165 (7)0.77807 (6)0.01537 (15)
O120.64134 (6)0.69033 (7)0.67169 (5)0.01296 (14)
O130.85903 (6)0.65299 (7)0.72295 (6)0.01451 (15)
O140.89589 (7)0.65373 (7)0.08166 (6)0.01542 (15)
H1A0.0412 (16)0.6308 (15)0.1784 (14)0.024 (4)*
H1B0.1113 (14)0.5288 (17)0.1298 (13)0.025 (4)*
H2A0.3337 (14)0.8551 (15)0.1742 (13)0.016 (3)*
H2B0.4254 (18)0.7955 (18)0.1197 (15)0.036 (5)*
H3A0.1311 (18)0.994 (2)0.1234 (18)0.046 (5)*
H3B0.128 (3)0.974 (3)0.021 (3)0.095 (9)*
H4A0.3394 (18)0.5304 (19)0.0953 (17)0.043 (5)*
H4B0.436 (3)0.559 (3)0.075 (3)0.108 (11)*
H5A0.1689 (15)0.6481 (16)0.1485 (14)0.022 (4)*
H5B0.0704 (17)0.7056 (16)0.1020 (14)0.028 (4)*
H6A0.3923 (14)0.9687 (18)0.1026 (13)0.028 (4)*
H6B0.4553 (16)0.8617 (15)0.1447 (14)0.023 (4)*
H7A0.066 (3)1.055 (3)0.112 (3)0.116 (12)*
H7B0.1626 (17)1.1247 (18)0.1270 (15)0.033 (4)*
H8A0.3607 (15)1.1274 (17)0.3469 (14)0.028 (4)*
H8B0.364 (3)1.023 (3)0.418 (3)0.113 (11)*
H9A0.6453 (15)0.7976 (16)0.9223 (14)0.025 (4)*
H9B0.6182 (19)0.836 (2)1.0070 (18)0.048 (6)*
H14A0.8728 (15)0.7114 (17)0.1198 (14)0.030 (4)*
H14B0.8565 (16)0.6694 (17)0.0194 (16)0.033 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.00917 (11)0.00747 (11)0.00655 (11)0.00007 (6)0.00164 (8)0.00012 (6)
Na10.01328 (18)0.01242 (19)0.00947 (18)0.00044 (14)0.00330 (13)0.00052 (13)
Na20.01297 (19)0.01106 (19)0.00955 (18)0.00027 (13)0.00288 (14)0.00005 (13)
O10.0116 (3)0.0147 (3)0.0139 (3)0.0007 (3)0.0018 (2)0.0007 (3)
O20.0119 (3)0.0124 (3)0.0124 (3)0.0010 (2)0.0012 (2)0.0017 (2)
O30.0175 (3)0.0167 (4)0.0171 (3)0.0014 (3)0.0072 (3)0.0038 (3)
O40.0146 (3)0.0182 (4)0.0155 (3)0.0013 (3)0.0062 (3)0.0022 (3)
O50.0118 (3)0.0130 (3)0.0139 (3)0.0004 (2)0.0028 (2)0.0012 (2)
O60.0119 (3)0.0141 (3)0.0148 (3)0.0003 (2)0.0033 (3)0.0002 (3)
O70.0137 (3)0.0133 (3)0.0162 (3)0.0013 (3)0.0025 (3)0.0007 (2)
O80.0167 (3)0.0134 (3)0.0140 (3)0.0001 (3)0.0018 (3)0.0003 (2)
O90.0142 (3)0.0194 (4)0.0129 (3)0.0020 (3)0.0037 (3)0.0009 (3)
O100.0186 (3)0.0134 (3)0.0095 (3)0.0005 (3)0.0036 (2)0.0032 (2)
O110.0223 (3)0.0084 (3)0.0152 (3)0.0014 (3)0.0054 (3)0.0004 (2)
O120.0113 (3)0.0145 (3)0.0103 (3)0.0010 (2)0.0009 (2)0.0021 (2)
O130.0117 (3)0.0186 (3)0.0142 (3)0.0005 (2)0.0053 (3)0.0014 (3)
O140.0158 (3)0.0169 (3)0.0123 (3)0.0012 (3)0.0025 (3)0.0002 (3)
Geometric parameters (Å, º) top
S1—O111.4740 (7)Na1—Na23.5182 (7)
S1—O121.4785 (7)Na2—O2ii2.3826 (8)
S1—O131.4790 (7)Na2—O72.3828 (9)
S1—O101.4806 (7)Na2—O82.3886 (9)
Na1—O22.3719 (9)Na2—O62.4240 (9)
Na1—O52.4002 (9)Na2—O52.4258 (9)
Na1—O32.4153 (9)Na2—O1ii2.4568 (9)
Na1—O12.4166 (9)Na2—Na1ii3.4714 (7)
Na1—O62.4431 (9)O1—Na2i2.4569 (9)
Na1—O42.4464 (9)O2—Na2i2.3826 (8)
Na1—Na2i3.4714 (7)
O11—S1—O12109.69 (4)O6—Na1—O490.27 (3)
O11—S1—O13109.72 (4)O2ii—Na2—O7172.68 (3)
O12—S1—O13109.22 (4)O2ii—Na2—O892.15 (3)
O11—S1—O10108.88 (4)O7—Na2—O893.31 (3)
O12—S1—O10109.39 (4)O2ii—Na2—O697.50 (3)
O13—S1—O10109.93 (4)O7—Na2—O687.07 (3)
O2—Na1—O5176.35 (3)O8—Na2—O693.15 (3)
O2—Na1—O392.18 (3)O2ii—Na2—O584.28 (3)
O5—Na1—O390.85 (3)O7—Na2—O590.39 (3)
O2—Na1—O187.29 (3)O8—Na2—O5176.04 (3)
O5—Na1—O194.45 (3)O6—Na2—O585.63 (3)
O3—Na1—O195.29 (3)O2ii—Na2—O1ii86.13 (3)
O2—Na1—O692.27 (3)O7—Na2—O1ii89.20 (3)
O5—Na1—O685.77 (3)O8—Na2—O1ii87.88 (3)
O3—Na1—O688.61 (3)O6—Na2—O1ii176.18 (3)
O1—Na1—O6176.08 (3)O5—Na2—O1ii93.58 (3)
O2—Na1—O490.16 (3)Na1—O1—Na2i90.84 (3)
O5—Na1—O486.78 (3)Na1—O2—Na2i93.80 (3)
O3—Na1—O4177.45 (3)Na1—O5—Na293.60 (3)
O1—Na1—O485.84 (3)Na2—O6—Na192.58 (3)
Symmetry codes: (i) x, y+3/2, z1/2; (ii) x, y+3/2, z+1/2.
(Na2_SO4_10H2O_250k) Sodium sulfate-water (1/10) top
Crystal data top
H20Na2O14SF(000) = 680
Mr = 322.20Dx = 1.481 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 11.467 (2) ÅCell parameters from 2802 reflections
b = 10.3455 (12) Åθ = 3.3–27.3°
c = 12.795 (2) ŵ = 0.34 mm1
β = 107.805 (15)°T = 250 K
V = 1445.2 (4) Å3Monoclinic prism, colourless
Z = 40.4 × 0.3 × 0.2 mm
Data collection top
Bruker APEX-II CCD
diffractometer
3331 independent reflections
Radiation source: sealed tube2694 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
ϕ and ω scansθmax = 27.6°, θmin = 1.9°
Absorption correction: integration
Coppens (1970)
h = 1414
Tmin = 0.884, Tmax = 0.934k = 1113
25202 measured reflectionsl = 1616
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024All H-atom parameters refined
wR(F2) = 0.061 'w = 1/[σ2(Fo2) + (0.0245P)2 + 0.3224P]' '
where P = (Fo2 + 2Fc2)/3'
S = 1.03(Δ/σ)max = 0.001
3331 reflectionsΔρmax = 0.23 e Å3
270 parametersΔρmin = 0.31 e Å3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0161 (7)
Crystal data top
H20Na2O14SV = 1445.2 (4) Å3
Mr = 322.20Z = 4
Monoclinic, P21/cMo Kα radiation
a = 11.467 (2) ŵ = 0.34 mm1
b = 10.3455 (12) ÅT = 250 K
c = 12.795 (2) Å0.4 × 0.3 × 0.2 mm
β = 107.805 (15)°
Data collection top
Bruker APEX-II CCD
diffractometer
3331 independent reflections
Absorption correction: integration
Coppens (1970)
2694 reflections with I > 2σ(I)
Tmin = 0.884, Tmax = 0.934Rint = 0.031
25202 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.061All H-atom parameters refined
S = 1.03Δρmax = 0.23 e Å3
3331 reflectionsΔρmin = 0.31 e Å3
270 parameters
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Na10.24416 (4)0.75357 (4)0.01647 (4)0.02840 (13)
Na20.25493 (4)0.88689 (4)0.23914 (4)0.02661 (12)
S10.25056 (2)0.14019 (2)0.74135 (2)0.02026 (9)
O10.11249 (9)0.60955 (10)0.15066 (8)0.0318 (2)
O20.35382 (9)0.78731 (9)0.14485 (8)0.0293 (2)
O30.36785 (11)0.56190 (10)0.05530 (9)0.0370 (2)
O40.11939 (11)0.94226 (11)0.08276 (9)0.0385 (2)
O50.14467 (9)0.71575 (9)0.12011 (8)0.0296 (2)
O60.38589 (9)0.88979 (10)0.12104 (8)0.0316 (2)
O70.13296 (11)1.04628 (10)0.11975 (8)0.0340 (2)
O80.37671 (12)1.04447 (10)0.36061 (9)0.0348 (2)
O90.60116 (9)0.84812 (10)0.94565 (10)0.0353 (2)
O100.89687 (10)0.65267 (10)0.08112 (10)0.0356 (2)
O110.35703 (8)0.19000 (8)0.82784 (7)0.0324 (2)
O12A0.27034 (12)0.00311 (11)0.72349 (10)0.0370 (3)0.85
O12B0.2221 (5)0.0024 (5)0.7558 (5)0.0208 (12)0.15
O13A0.14162 (11)0.15529 (14)0.77600 (11)0.0364 (3)0.85
O13B0.1380 (6)0.2190 (6)0.7448 (6)0.0258 (14)0.15
O14A0.23706 (14)0.21065 (13)0.63879 (12)0.0325 (3)0.85
O14B0.2674 (8)0.1601 (7)0.6324 (7)0.0280 (16)0.15
H1A0.1077 (13)0.5351 (17)0.1297 (13)0.044 (5)*
H1B0.0409 (16)0.6332 (14)0.1826 (13)0.044 (5)*
H2A0.3336 (15)0.8570 (16)0.1715 (14)0.046 (5)*
H2B0.4228 (17)0.7964 (16)0.1180 (14)0.050 (5)*
H3A0.3427 (16)0.5278 (18)0.0916 (15)0.052 (6)*
H3B0.435 (3)0.560 (3)0.077 (2)0.145 (13)*
H4A0.1340 (17)0.9907 (19)0.1228 (16)0.065 (6)*
H4B0.058 (3)0.936 (3)0.100 (2)0.129 (12)*
H5A0.1701 (15)0.6442 (17)0.1482 (15)0.050 (5)*
H5B0.0741 (17)0.7072 (16)0.1038 (14)0.050 (5)*
H6B0.4529 (16)0.8645 (15)0.1419 (13)0.043 (5)*
H6A0.3913 (14)0.9659 (18)0.0983 (13)0.053 (5)*
H7A0.1539 (16)1.1176 (18)0.1298 (14)0.051 (5)*
H7B0.073 (3)1.057 (3)0.118 (2)0.022 (8)*0.5
H7C0.133 (3)1.008 (4)0.024 (3)0.077 (11)*0.5
H8A0.436 (3)1.050 (3)0.372 (3)0.033 (11)*0.5
H8B0.3614 (14)1.1233 (17)0.3500 (13)0.044 (5)*
H8C0.356 (3)1.018 (3)0.436 (3)0.068 (11)*0.5
H9A0.6413 (16)0.7959 (17)0.9194 (14)0.055 (5)*
H9B0.6129 (16)0.8376 (17)1.0014 (15)0.049 (6)*
H10A0.8743 (15)0.7103 (18)0.1193 (15)0.058 (5)*
H10B0.8617 (16)0.6647 (17)0.0288 (16)0.047 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.0301 (3)0.0298 (3)0.0268 (3)0.00172 (19)0.0109 (2)0.0022 (2)
Na20.0291 (3)0.0253 (2)0.0254 (3)0.00016 (19)0.0082 (2)0.00041 (18)
S10.02278 (15)0.01809 (14)0.01982 (16)0.00057 (11)0.00638 (11)0.00014 (10)
O10.0260 (5)0.0331 (5)0.0343 (5)0.0023 (4)0.0060 (4)0.0015 (4)
O20.0264 (5)0.0290 (5)0.0301 (5)0.0020 (4)0.0051 (4)0.0030 (4)
O30.0340 (6)0.0412 (6)0.0385 (6)0.0035 (4)0.0152 (5)0.0071 (5)
O40.0342 (6)0.0417 (6)0.0426 (6)0.0031 (5)0.0164 (5)0.0103 (5)
O50.0254 (5)0.0304 (5)0.0326 (5)0.0015 (4)0.0083 (4)0.0020 (4)
O60.0255 (5)0.0329 (5)0.0366 (6)0.0002 (4)0.0098 (4)0.0006 (4)
O70.0301 (6)0.0289 (5)0.0403 (6)0.0019 (4)0.0067 (4)0.0004 (4)
O80.0338 (6)0.0283 (6)0.0384 (6)0.0003 (4)0.0049 (5)0.0003 (4)
O90.0322 (5)0.0428 (6)0.0311 (6)0.0042 (4)0.0100 (5)0.0020 (5)
O100.0332 (5)0.0403 (6)0.0313 (6)0.0030 (4)0.0068 (5)0.0001 (5)
O110.0286 (4)0.0347 (5)0.0293 (5)0.0023 (4)0.0019 (4)0.0041 (4)
O12A0.0513 (8)0.0202 (5)0.0384 (7)0.0018 (5)0.0123 (6)0.0006 (5)
O12B0.034 (3)0.015 (3)0.021 (3)0.005 (2)0.020 (3)0.002 (2)
O13A0.0284 (6)0.0465 (8)0.0369 (8)0.0010 (6)0.0139 (5)0.0040 (6)
O13B0.023 (3)0.020 (3)0.036 (4)0.010 (3)0.010 (3)0.004 (3)
O14A0.0407 (8)0.0314 (8)0.0254 (7)0.0001 (6)0.0102 (6)0.0060 (6)
O14B0.037 (4)0.027 (4)0.023 (3)0.003 (3)0.013 (3)0.001 (3)
Geometric parameters (Å, º) top
Na1—O22.3800 (11)Na2—Na1ii3.4843 (8)
Na1—O52.3934 (11)S1—O13A1.4561 (12)
Na1—O42.4156 (12)S1—O12A1.4651 (11)
Na1—O12.4211 (11)S1—O14A1.4673 (15)
Na1—O62.4443 (11)S1—O111.4678 (9)
Na1—O32.4475 (12)S1—O14B1.479 (8)
Na1—Na2i3.4843 (8)S1—O12B1.487 (5)
Na1—Na23.5167 (8)S1—O13B1.539 (6)
Na2—O82.3867 (12)O1—Na2i2.4629 (11)
Na2—O72.3880 (11)O2—Na2i2.3891 (10)
Na2—O2ii2.3891 (10)O12A—O12B0.786 (5)
Na2—O52.4239 (10)O13A—O13B0.765 (6)
Na2—O62.4346 (11)O14A—O14B0.647 (6)
Na2—O1ii2.4629 (11)
O2—Na1—O5176.71 (4)O13A—S1—O14A110.69 (8)
O2—Na1—O491.17 (4)O12A—S1—O14A108.69 (7)
O5—Na1—O491.44 (4)O13A—S1—O11109.03 (6)
O2—Na1—O186.98 (4)O12A—S1—O11108.95 (6)
O5—Na1—O194.82 (4)O14A—S1—O11109.62 (7)
O4—Na1—O194.27 (4)O13A—S1—O14B130.1 (3)
O2—Na1—O692.11 (4)O12A—S1—O14B85.2 (3)
O5—Na1—O685.94 (4)O14A—S1—O14B25.4 (2)
O4—Na1—O688.79 (4)O11—S1—O14B110.1 (3)
O1—Na1—O6176.83 (4)O13A—S1—O12B79.8 (2)
O2—Na1—O390.57 (4)O12A—S1—O12B30.88 (19)
O5—Na1—O386.82 (4)O14A—S1—O12B128.4 (2)
O4—Na1—O3178.25 (4)O11—S1—O12B114.0 (2)
O1—Na1—O386.08 (4)O14B—S1—O12B110.4 (4)
O6—Na1—O390.89 (4)O13A—S1—O13B29.4 (2)
O8—Na2—O793.24 (4)O12A—S1—O13B133.5 (2)
O8—Na2—O2ii92.21 (4)O14A—S1—O13B84.4 (3)
O7—Na2—O2ii172.86 (4)O11—S1—O13B107.7 (3)
O8—Na2—O5175.60 (4)O14B—S1—O13B107.8 (4)
O7—Na2—O590.66 (4)O12B—S1—O13B106.6 (3)
O2ii—Na2—O584.07 (4)Na1—O1—Na2i91.02 (4)
O8—Na2—O692.67 (4)Na1—O2—Na2i93.87 (4)
O7—Na2—O686.92 (4)Na1—O5—Na293.78 (4)
O2ii—Na2—O697.43 (4)Na2—O6—Na192.24 (4)
O5—Na2—O685.48 (4)O12B—O12A—S176.1 (4)
O8—Na2—O1ii88.59 (4)O12A—O12B—S173.0 (4)
O7—Na2—O1ii89.69 (4)O13B—O13A—S181.3 (5)
O2ii—Na2—O1ii85.84 (4)O13A—O13B—S169.3 (4)
O5—Na2—O1ii93.49 (4)O14B—O14A—S178.3 (8)
O6—Na2—O1ii176.45 (4)O14A—O14B—S176.3 (8)
O13A—S1—O12A109.84 (8)
Symmetry codes: (i) x, y+3/2, z1/2; (ii) x, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O10iii0.823 (17)2.045 (18)2.8672 (15)176.9 (15)
O1—H1B···O13Aiv0.834 (17)2.081 (17)2.9033 (17)168.5 (15)
O1—H1B···O13Biv0.834 (17)2.152 (18)2.978 (6)170.5 (15)
O2—H2A···O12Av0.801 (17)2.005 (18)2.7842 (15)164.2 (17)
O2—H2A···O12Bv0.801 (17)2.008 (19)2.770 (6)158.7 (16)
O2—H2B···O9vi0.765 (18)2.028 (19)2.7878 (15)171.5 (18)
O3—H3A···O12Avii0.710 (19)2.121 (19)2.7938 (18)158.5 (19)
O3—H3A···O14Bvii0.710 (19)2.25 (2)2.875 (7)147.3 (19)
O3—H3B···O8viii0.74 (3)2.07 (3)2.8004 (17)177 (3)
O4—H4A···O12Bv0.77 (2)2.10 (2)2.743 (5)141.3 (18)
O4—H4A···O13Av0.77 (2)2.16 (2)2.9102 (18)165.7 (19)
O4—H4B···O7ix0.68 (3)2.13 (3)2.7881 (17)165 (3)
O5—H5A···O12Avii0.835 (18)1.974 (18)2.7906 (15)165.7 (16)
O5—H5A···O12Bvii0.835 (18)2.013 (19)2.820 (6)162.4 (16)
O5—H5B···O10x0.777 (18)2.042 (19)2.8075 (15)168.4 (17)
O6—H6B···O11xi0.778 (17)2.168 (17)2.9360 (14)169.3 (16)
O6—H6A···O9xii0.849 (18)2.013 (19)2.8601 (15)175.3 (16)
O7—H7A···O13Bi0.774 (18)2.285 (19)2.899 (7)136.9 (16)
O7—H7A···O14Ai0.774 (18)2.003 (19)2.7623 (17)166.6 (18)
O7—H7A···O14Bi0.774 (18)2.64 (2)3.388 (7)163.7 (17)
O7—H7B···O4ix0.69 (3)2.11 (3)2.7881 (17)166 (3)
O7—H7C···O41.28 (4)1.50 (4)2.7657 (16)169 (3)
O8—H8A···O3xiii0.65 (4)2.16 (4)2.8004 (17)168 (4)
O8—H8B···O11i0.836 (17)1.951 (18)2.7776 (14)169.6 (15)
O8—H8C···O3ii1.09 (4)1.70 (4)2.7534 (16)159 (3)
O9—H9A···O14Axiv0.843 (19)1.979 (19)2.8031 (19)165.7 (16)
O9—H9A···O14Bxiv0.843 (19)1.98 (2)2.824 (8)174.4 (17)
O9—H9B···O11xv0.693 (18)2.124 (19)2.8170 (16)178 (2)
O10—H10A···O13Axi0.859 (19)1.98 (2)2.8244 (17)168.3 (16)
O10—H10A···O13Bxi0.859 (19)1.93 (2)2.725 (7)153.2 (17)
O10—H10B···O14Axiii0.679 (18)2.150 (19)2.827 (2)175 (2)
O10—H10B···O14Bxiii0.679 (18)2.14 (2)2.806 (9)167 (2)
Symmetry codes: (i) x, y+3/2, z1/2; (ii) x, y+3/2, z+1/2; (iii) x+1, y+1, z; (iv) x, y+1/2, z+1/2; (v) x, y+1, z1; (vi) x, y, z1; (vii) x, y+1/2, z1/2; (viii) x+1, y1/2, z+1/2; (ix) x, y+2, z; (x) x1, y, z; (xi) x+1, y+1, z+1; (xii) x+1, y+2, z+1; (xiii) x+1, y+1/2, z+1/2; (xiv) x+1, y+1/2, z+3/2; (xv) x+1, y+1, z+2.

Experimental details

(Na2_Se04_75H2O_120k)(Na2_SO_4_7H2O_120k)
Crystal data
Chemical formulaH15Na2O11.50SeH14Na2O11S
Mr324.06268.15
Crystal system, space groupMonoclinic, C2/cTetragonal, P41212
Temperature (K)120120
a, b, c (Å)25.082 (7), 7.2222 (13), 14.148 (5)14.3249 (15), 14.3249 (15), 22.202 (4)
α, β, γ (°)90, 106.08 (3), 9090, 90, 90
V3)2462.6 (12)4556.0 (10)
Z816
Radiation typeMo KαMo Kα
µ (mm1)3.160.40
Crystal size (mm)0.25 × 0.18 × 0.110.53 × 0.48 × 0.44
Data collection
DiffractometerSTOE IPDS 2T
diffractometer
STOE IPDS 2
diffractometer
Absorption correctionIntegration
Coppens (1970)
Integration
Coppens (1970)
Tmin, Tmax0.292, 0.5360.529, 0.721
No. of measured, independent and
observed [I > 2σ(I)] reflections
51914, 4234, 3466 6253, 6253, 3969
Rint0.1070.064
(sin θ/λ)max1)0.7450.690
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.079, 1.00 0.028, 0.110, 1.06
No. of reflections42346253
No. of parameters192340
No. of restraints039
H-atom treatmentAll H-atom parameters refinedOnly H-atom coordinates refined
Δρmax, Δρmin (e Å3)0.49, 1.030.36, 0.40
Absolute structure?'Refined as an inversion twin.'
Absolute structure parameter?0.46 (19)

Computer programs: STOE X-AREA, STOE X-RED, SHELXS2013 (Sheldrick, 2008), SHELXL2013 (Sheldrick, 2008), Diamond3, publCIF.

Hydrogen-bond geometry (Å, º) for (Na2_Se04_75H2O_120k) top
D—H···AD—HH···AD···AD—H···A
O8—H8B···O12i0.76 (3)2.12 (3)2.880 (2)172 (3)
O8—H8A···O120.85 (3)1.99 (3)2.8273 (18)168 (3)
O7—H7B···O100.87 (3)1.90 (3)2.7683 (19)173 (3)
O7—H7A···O11ii0.79 (4)2.00 (4)2.790 (2)174 (3)
O6—H6B···O9iii0.74 (3)2.11 (3)2.844 (2)172 (3)
O6—H6A···O90.85 (3)2.01 (3)2.8473 (18)166 (2)
O5—H5B···O7iv0.79 (3)2.04 (3)2.834 (2)177 (3)
O5—H5A···O3v0.87 (3)1.99 (3)2.837 (2)168 (3)
O4—H4B···O50.86 (3)1.96 (4)2.8021 (19)168 (3)
O4—H4A···O10vi0.85 (3)2.00 (3)2.8502 (17)172 (3)
O3—H3B···O9iv0.82 (3)1.95 (3)2.7738 (17)175 (3)
O3—H3A···O12vi0.78 (3)2.02 (3)2.7897 (17)172 (3)
O2—H2B···O11vi0.80 (3)2.09 (3)2.8842 (18)172 (3)
O2—H2A···O11vii0.78 (3)2.14 (3)2.9055 (18)169 (3)
O1—H1···O10iv0.83 (3)2.01 (3)2.8409 (17)174 (3)
O8—H8B···O12i0.76 (3)2.12 (3)2.880 (2)172 (3)
O8—H8A···O120.85 (3)1.99 (3)2.8273 (18)168 (3)
O7—H7B···O100.87 (3)1.90 (3)2.7683 (19)173 (3)
O7—H7A···O11ii0.79 (4)2.00 (4)2.790 (2)174 (3)
O6—H6B···O9iii0.74 (3)2.11 (3)2.844 (2)172 (3)
O6—H6A···O90.85 (3)2.01 (3)2.8473 (18)166 (2)
O5—H5B···O7iv0.79 (3)2.04 (3)2.834 (2)177 (3)
O5—H5A···O3v0.87 (3)1.99 (3)2.837 (2)168 (3)
O4—H4B···O50.86 (3)1.96 (4)2.8021 (19)168 (3)
O4—H4A···O10vi0.85 (3)2.00 (3)2.8502 (17)172 (3)
O3—H3B···O9iv0.82 (3)1.95 (3)2.7738 (17)175 (3)
O3—H3A···O12vi0.78 (3)2.02 (3)2.7897 (17)172 (3)
O2—H2B···O11vi0.80 (3)2.09 (3)2.8842 (18)172 (3)
O2—H2A···O11vii0.78 (3)2.14 (3)2.9055 (18)169 (3)
O1—H1···O10iv0.83 (3)2.01 (3)2.8409 (17)174 (3)
O1—H1···O10iv0.83 (3)2.01 (3)2.8409 (17)174 (3)
O2—H2A···O11vii0.78 (3)2.14 (3)2.9055 (18)169 (3)
O2—H2B···O11vi0.80 (3)2.09 (3)2.8842 (18)172 (3)
O3—H3A···O12vi0.78 (3)2.02 (3)2.7897 (17)172 (3)
O3—H3B···O9iv0.82 (3)1.95 (3)2.7738 (17)175 (3)
O4—H4A···O10vi0.85 (3)2.00 (3)2.8502 (17)172 (3)
O4—H4B···O50.86 (3)1.96 (4)2.8021 (19)168 (3)
O5—H5A···O3v0.87 (3)1.99 (3)2.837 (2)168 (3)
O5—H5B···O7iv0.79 (3)2.04 (3)2.834 (2)177 (3)
O6—H6A···O90.85 (3)2.01 (3)2.8473 (18)166 (2)
O6—H6B···O9iii0.74 (3)2.11 (3)2.844 (2)172 (3)
O7—H7A···O11ii0.79 (4)2.00 (4)2.790 (2)174 (3)
O7—H7B···O100.87 (3)1.90 (3)2.7683 (19)173 (3)
O8—H8A···O120.85 (3)1.99 (3)2.8273 (18)168 (3)
O8—H8B···O12i0.76 (3)2.12 (3)2.880 (2)172 (3)
Symmetry codes: (i) x+1/2, y+3/2, z+1; (ii) x, y+1, z1/2; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y+1/2, z+1/2; (v) x, y+1, z+1/2; (vi) x+1/2, y1/2, z+1/2; (vii) x+1/2, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) for (Na2_SO_4_7H2O_120k) top
D—H···AD—HH···AD···AD—H···A
O17—H4···O22i0.77 (2)2.14 (3)2.863 (4)156 (3)
O17—H5···O18ii0.81 (2)2.05 (2)2.850 (4)167 (3)
O16—H2···O23i0.82 (2)2.03 (3)2.791 (4)154 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O15—H6···O22iv0.81 (2)2.01 (3)2.785 (4)159 (3)
O14—H22···O18v0.83 (2)2.04 (2)2.825 (4)157 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O13—H9···O22vii0.90 (4)1.99 (3)2.820 (4)152 (3)
O13—H8···O21ii0.85 (3)1.95 (3)2.799 (4)172 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O11—H26···O21v0.78 (2)2.13 (3)2.849 (4)152 (4)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O9—H20···O2ii0.80 (2)2.03 (2)2.819 (4)168 (3)
O9—H19···O19viii0.80 (2)2.07 (2)2.825 (4)158 (3)
O8—H25···O23ix0.84 (2)2.01 (3)2.770 (4)150 (3)
O8—H24···O1ii0.82 (2)2.03 (2)2.853 (4)177 (3)
O7—H12···O21viii0.82 (2)2.04 (3)2.802 (4)153 (3)
O7—H11···O20ii0.83 (2)2.00 (2)2.809 (4)168 (4)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O5—H15···O2viii0.82 (2)2.01 (2)2.818 (4)172 (3)
O5—H16···O20viii0.81 (2)2.05 (3)2.811 (4)156 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O4—H10···O23vii0.80 (2)2.13 (3)2.878 (4)155 (3)
O3—H18···O19v0.81 (2)2.03 (2)2.795 (4)158 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O17—H4···O22i0.77 (2)2.14 (3)2.863 (4)156 (3)
O17—H5···O18ii0.81 (2)2.05 (2)2.850 (4)167 (3)
O16—H2···O23i0.82 (2)2.03 (3)2.791 (4)154 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O15—H6···O22iv0.81 (2)2.01 (3)2.785 (4)159 (3)
O14—H22···O18v0.83 (2)2.04 (2)2.825 (4)157 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O13—H9···O22vii0.90 (4)1.99 (3)2.820 (4)152 (3)
O13—H8···O21ii0.85 (3)1.95 (3)2.799 (4)172 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O11—H26···O21v0.78 (2)2.13 (3)2.849 (4)152 (4)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O9—H20···O2ii0.80 (2)2.03 (2)2.819 (4)168 (3)
O9—H19···O19viii0.80 (2)2.07 (2)2.825 (4)158 (3)
O8—H25···O23ix0.84 (2)2.01 (3)2.770 (4)150 (3)
O8—H24···O1ii0.82 (2)2.03 (2)2.853 (4)177 (3)
O7—H12···O21viii0.82 (2)2.04 (3)2.802 (4)153 (3)
O7—H11···O20ii0.83 (2)2.00 (2)2.809 (4)168 (4)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O5—H15···O2viii0.82 (2)2.01 (2)2.818 (4)172 (3)
O5—H16···O20viii0.81 (2)2.05 (3)2.811 (4)156 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O4—H10···O23vii0.80 (2)2.13 (3)2.878 (4)155 (3)
O3—H18···O19v0.81 (2)2.03 (2)2.795 (4)158 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O3—H18···O19v0.81 (2)2.03 (2)2.795 (4)158 (3)
O4—H10···O23vii0.80 (2)2.13 (3)2.878 (4)155 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O5—H15···O2viii0.82 (2)2.01 (2)2.818 (4)172 (3)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O7—H11···O20ii0.83 (2)2.00 (2)2.809 (4)168 (4)
O7—H12···O21viii0.82 (2)2.04 (3)2.802 (4)153 (3)
O8—H24···O1ii0.82 (2)2.03 (2)2.853 (4)177 (3)
O8—H25···O23ix0.84 (2)2.01 (3)2.770 (4)150 (3)
O9—H19···O19viii0.80 (2)2.07 (2)2.825 (4)158 (3)
O9—H20···O2ii0.80 (2)2.03 (2)2.819 (4)168 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O11—H26···O21v0.78 (2)2.13 (3)2.849 (4)152 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O13—H8···O21ii0.85 (3)1.95 (3)2.799 (4)172 (4)
O13—H9···O22vii0.90 (4)1.99 (3)2.820 (4)152 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O14—H22···O18v0.83 (2)2.04 (2)2.825 (4)157 (3)
O15—H6···O22iv0.81 (2)2.01 (3)2.785 (4)159 (3)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O16—H2···O23i0.82 (2)2.03 (3)2.791 (4)154 (3)
O17—H5···O18ii0.81 (2)2.05 (2)2.850 (4)167 (3)
O17—H4···O22i0.77 (2)2.14 (3)2.863 (4)156 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O3—H18···O19v0.81 (2)2.03 (2)2.795 (4)158 (3)
O4—H10···O23vii0.80 (2)2.13 (3)2.878 (4)155 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O5—H16···O20viii0.81 (2)2.05 (3)2.811 (4)156 (3)
O5—H15···O2viii0.82 (2)2.01 (2)2.818 (4)172 (3)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O7—H11···O20ii0.83 (2)2.00 (2)2.809 (4)168 (4)
O7—H12···O21viii0.82 (2)2.04 (3)2.802 (4)153 (3)
O8—H24···O1ii0.82 (2)2.03 (2)2.853 (4)177 (3)
O8—H25···O23ix0.84 (2)2.01 (3)2.770 (4)150 (3)
O9—H19···O19viii0.80 (2)2.07 (2)2.825 (4)158 (3)
O9—H20···O2ii0.80 (2)2.03 (2)2.819 (4)168 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O11—H26···O21v0.78 (2)2.13 (3)2.849 (4)152 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O13—H8···O21ii0.85 (3)1.95 (3)2.799 (4)172 (4)
O13—H9···O22vii0.90 (4)1.99 (3)2.820 (4)152 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O14—H22···O18v0.83 (2)2.04 (2)2.825 (4)157 (3)
O15—H6···O22iv0.81 (2)2.01 (3)2.785 (4)159 (3)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O16—H2···O23i0.82 (2)2.03 (3)2.791 (4)154 (3)
O17—H5···O18ii0.81 (2)2.05 (2)2.850 (4)167 (3)
O17—H4···O22i0.77 (2)2.14 (3)2.863 (4)156 (3)
O3—H17···O20.82 (2)2.03 (2)2.833 (4)166 (3)
O3—H18···O19v0.81 (2)2.03 (2)2.795 (4)158 (3)
O4—H10···O23vii0.80 (2)2.13 (3)2.878 (4)155 (3)
O4—H28···O10.81 (2)2.01 (2)2.813 (4)170 (3)
O5—H16···O20viii0.81 (2)2.05 (3)2.811 (4)156 (3)
O5—H15···O2viii0.82 (2)2.01 (2)2.818 (4)172 (3)
O6—H23···O50.78 (2)2.11 (2)2.884 (3)170 (4)
O7—H11···O20ii0.83 (2)2.00 (2)2.809 (4)168 (4)
O7—H12···O21viii0.82 (2)2.04 (3)2.802 (4)153 (3)
O8—H24···O1ii0.82 (2)2.03 (2)2.853 (4)177 (3)
O8—H25···O23ix0.84 (2)2.01 (3)2.770 (4)150 (3)
O9—H19···O19viii0.80 (2)2.07 (2)2.825 (4)158 (3)
O9—H20···O2ii0.80 (2)2.03 (2)2.819 (4)168 (3)
O10—H13···O130.77 (2)2.13 (2)2.886 (3)166 (3)
O10—H14···O16vi0.80 (2)2.21 (3)2.877 (3)141 (3)
O11—H27···O200.80 (2)2.07 (2)2.848 (4)166 (3)
O11—H26···O21v0.78 (2)2.13 (3)2.849 (4)152 (4)
O12—H3···O14iii0.82 (2)2.06 (2)2.883 (3)171 (4)
O13—H8···O21ii0.85 (3)1.95 (3)2.799 (4)172 (4)
O13—H9···O22vii0.90 (4)1.99 (3)2.820 (4)152 (3)
O14—H21···O1vi0.85 (2)1.94 (2)2.790 (4)174 (3)
O14—H22···O18v0.83 (2)2.04 (2)2.825 (4)157 (3)
O15—H6···O22iv0.81 (2)2.01 (3)2.785 (4)159 (3)
O15—H7···O18iii0.81 (2)2.04 (2)2.829 (4)163 (3)
O16—H1···O19iii0.82 (2)2.00 (2)2.825 (4)178 (4)
O16—H2···O23i0.82 (2)2.03 (3)2.791 (4)154 (3)
O17—H5···O18ii0.81 (2)2.05 (2)2.850 (4)167 (3)
O17—H4···O22i0.77 (2)2.14 (3)2.863 (4)156 (3)
Symmetry codes: (i) y+1, x, z+1; (ii) x+3/2, y1/2, z+1/4; (iii) x+1, y, z; (iv) y+3/2, x+1/2, z3/4; (v) y+3/2, x+1/2, z+1/4; (vi) y+3/2, x1/2, z+1/4; (vii) x+3/2, y+1/2, z+5/4; (viii) y, x, z; (ix) x, y, z1.
Hydrogen-bond geometry (Å, º) for (Na2_SO4_10H2O_250k) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O10i0.823 (17)2.045 (18)2.8672 (15)176.9 (15)
O1—H1B···O13Aii0.834 (17)2.081 (17)2.9033 (17)168.5 (15)
O1—H1B···O13Bii0.834 (17)2.152 (18)2.978 (6)170.5 (15)
O2—H2A···O12Aiii0.801 (17)2.005 (18)2.7842 (15)164.2 (17)
O2—H2A···O12Biii0.801 (17)2.008 (19)2.770 (6)158.7 (16)
O2—H2B···O9iv0.765 (18)2.028 (19)2.7878 (15)171.5 (18)
O3—H3A···O12Av0.710 (19)2.121 (19)2.7938 (18)158.5 (19)
O3—H3A···O14Bv0.710 (19)2.25 (2)2.875 (7)147.3 (19)
O3—H3B···O8vi0.74 (3)2.07 (3)2.8004 (17)177 (3)
O4—H4A···O12Biii0.77 (2)2.10 (2)2.743 (5)141.3 (18)
O4—H4A···O13Aiii0.77 (2)2.16 (2)2.9102 (18)165.7 (19)
O4—H4B···O7vii0.68 (3)2.13 (3)2.7881 (17)165 (3)
O5—H5A···O12Av0.835 (18)1.974 (18)2.7906 (15)165.7 (16)
O5—H5A···O12Bv0.835 (18)2.013 (19)2.820 (6)162.4 (16)
O5—H5B···O10viii0.777 (18)2.042 (19)2.8075 (15)168.4 (17)
O6—H6B···O11ix0.778 (17)2.168 (17)2.9360 (14)169.3 (16)
O6—H6A···O9x0.849 (18)2.013 (19)2.8601 (15)175.3 (16)
O7—H7A···O13Bxi0.774 (18)2.285 (19)2.899 (7)136.9 (16)
O7—H7A···O14Axi0.774 (18)2.003 (19)2.7623 (17)166.6 (18)
O7—H7A···O14Bxi0.774 (18)2.64 (2)3.388 (7)163.7 (17)
O7—H7B···O4vii0.69 (3)2.11 (3)2.7881 (17)166 (3)
O7—H7C···O41.28 (4)1.50 (4)2.7657 (16)169 (3)
O8—H8A···O3xii0.65 (4)2.16 (4)2.8004 (17)168 (4)
O8—H8B···O11xi0.836 (17)1.951 (18)2.7776 (14)169.6 (15)
O8—H8C···O3xiii1.09 (4)1.70 (4)2.7534 (16)159 (3)
O9—H9A···O14Axiv0.843 (19)1.979 (19)2.8031 (19)165.7 (16)
O9—H9A···O14Bxiv0.843 (19)1.98 (2)2.824 (8)174.4 (17)
O9—H9B···O11xv0.693 (18)2.124 (19)2.8170 (16)178 (2)
O10—H10A···O13Aix0.859 (19)1.98 (2)2.8244 (17)168.3 (16)
O10—H10A···O13Bix0.859 (19)1.93 (2)2.725 (7)153.2 (17)
O10—H10B···O14Axii0.679 (18)2.150 (19)2.827 (2)175 (2)
O10—H10B···O14Bxii0.679 (18)2.14 (2)2.806 (9)167 (2)
Symmetry codes: (i) x+1, y+1, z; (ii) x, y+1/2, z+1/2; (iii) x, y+1, z1; (iv) x, y, z1; (v) x, y+1/2, z1/2; (vi) x+1, y1/2, z+1/2; (vii) x, y+2, z; (viii) x1, y, z; (ix) x+1, y+1, z+1; (x) x+1, y+2, z+1; (xi) x, y+3/2, z1/2; (xii) x+1, y+1/2, z+1/2; (xiii) x, y+3/2, z+1/2; (xiv) x+1, y+1/2, z+3/2; (xv) x+1, y+1, z+2.
 

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