Similarities and peculiarities between the crystal structures of the hydrates of sodium sulfate and selenate

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 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 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.

S1. Experimental

S1.1. Refinement

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

S2. Results and discussion

Computing details

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

(Na2_Se04_75H2O_120k) Sodium selenate heptahemihydrate

Crystal data

H15Na2O11.50Se	F(000) = 1304
Mr = 324.06	Dx = 1.748 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 25.082 (7) Å	Cell parameters from 1703 reflections
b = 7.2222 (13) Å	θ = 3.1–32.2°
c = 14.148 (5) Å	µ = 3.16 mm^−1
β = 106.08 (3)°	T = 120 K
V = 2462.6 (12) Å^3	Monoclinic prism, colourless
Z = 8	0.25 × 0.18 × 0.11 mm

Data collection

STOE IPDS 2T diffractometer	4234 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus	3466 reflections with I > 2σ(I)
Plane graphite monochromator	Rint = 0.107
Detector resolution: 6.67 pixels mm^-1	θmax = 32.0°, θmin = 2.9°
rotation method scans	h = −37→37
Absorption correction: integration Coppens (1970)	k = −10→10
Tmin = 0.292, Tmax = 0.536	l = −20→20
51914 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.026	All H-atom parameters refined
wR(F^2) = 0.079	'w = 1/[σ^2(Fo^2) + (0.0487P)^2 + 2.4105P]' ' where P = (Fo^2 + 2Fc^2)/3'
S = 1.00	(Δ/σ)max = 0.002
4234 reflections	Δρmax = 0.49 e Å^−3
192 parameters	Δρmin = −1.03 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00151 (17)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Se1	0.12538 (2)	0.50581 (2)	0.43856 (2)	0.00804 (6)
Na1	0.25402 (3)	0.48478 (8)	0.25255 (5)	0.01318 (13)
Na2	0.48802 (3)	0.50577 (8)	0.12460 (5)	0.01393 (13)
O1	0.5000	0.7533 (2)	0.2500	0.0169 (3)
O2	0.49834 (5)	0.27554 (19)	0.00232 (9)	0.0163 (2)
O3	0.39327 (6)	0.51391 (17)	0.01325 (10)	0.0168 (2)
O4	0.43838 (5)	0.38294 (17)	0.24329 (9)	0.0168 (2)
O5	0.35257 (5)	0.54197 (19)	0.30729 (10)	0.0176 (2)
O6	0.25084 (6)	0.23441 (17)	0.36455 (9)	0.0152 (2)
O7	0.15405 (5)	0.43353 (18)	0.20215 (9)	0.0173 (2)
O8	0.24653 (5)	0.73830 (17)	0.36305 (9)	0.0148 (2)
O9	0.16577 (5)	0.32150 (15)	0.45515 (8)	0.0139 (2)
O10	0.08697 (5)	0.51212 (14)	0.32289 (8)	0.0135 (2)
O11	0.08559 (5)	0.49515 (14)	0.51372 (9)	0.0132 (2)
O12	0.16395 (5)	0.69410 (15)	0.46262 (8)	0.0131 (2)
H1	0.4729 (11)	0.824 (4)	0.230 (2)	0.037 (7)*
H2A	0.5245 (12)	0.214 (4)	0.008 (2)	0.027 (7)*
H2B	0.4728 (13)	0.204 (4)	−0.007 (2)	0.038 (8)*
H3A	0.3766 (13)	0.430 (4)	0.024 (2)	0.041 (8)*
H3B	0.3744 (12)	0.601 (4)	0.023 (2)	0.043 (8)*
H4A	0.4325 (11)	0.269 (4)	0.2288 (19)	0.035 (7)*
H4B	0.4092 (14)	0.428 (5)	0.255 (2)	0.048 (8)*
H5A	0.3694 (13)	0.519 (3)	0.368 (2)	0.026 (7)*
H5B	0.3521 (11)	0.652 (4)	0.3055 (18)	0.032 (7)*
H6A	0.2217 (12)	0.262 (4)	0.3815 (18)	0.025 (6)*
H6B	0.2746 (12)	0.220 (4)	0.409 (2)	0.029 (7)*
H7A	0.1346 (15)	0.462 (4)	0.150 (3)	0.042 (9)*
H7B	0.1350 (12)	0.464 (4)	0.243 (2)	0.032 (7)*
H8A	0.2181 (12)	0.728 (4)	0.385 (2)	0.033 (7)*
H8B	0.2721 (13)	0.756 (4)	0.406 (2)	0.031 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Se1	0.00788 (8)	0.00783 (8)	0.00858 (8)	−0.00008 (5)	0.00258 (5)	−0.00012 (4)
Na1	0.0141 (3)	0.0126 (3)	0.0134 (3)	−0.0001 (2)	0.0047 (2)	0.0001 (2)
Na2	0.0144 (3)	0.0133 (3)	0.0134 (3)	0.0006 (2)	0.0028 (2)	0.0001 (2)
O1	0.0165 (8)	0.0115 (7)	0.0194 (8)	0.000	−0.0004 (7)	0.000
O2	0.0147 (6)	0.0127 (5)	0.0225 (6)	0.0006 (4)	0.0067 (5)	0.0001 (4)
O3	0.0157 (6)	0.0129 (5)	0.0214 (6)	0.0003 (4)	0.0046 (5)	0.0004 (4)
O4	0.0149 (6)	0.0163 (5)	0.0195 (6)	−0.0034 (4)	0.0053 (4)	−0.0040 (4)
O5	0.0155 (6)	0.0186 (5)	0.0185 (6)	0.0012 (5)	0.0041 (5)	0.0001 (5)
O6	0.0145 (6)	0.0182 (5)	0.0126 (5)	0.0037 (4)	0.0032 (4)	0.0009 (4)
O7	0.0153 (6)	0.0247 (6)	0.0121 (5)	0.0026 (5)	0.0038 (4)	−0.0001 (4)
O8	0.0129 (6)	0.0182 (5)	0.0139 (5)	−0.0030 (4)	0.0044 (4)	−0.0012 (4)
O9	0.0138 (5)	0.0110 (5)	0.0169 (5)	0.0044 (4)	0.0043 (4)	0.0018 (4)
O10	0.0134 (5)	0.0155 (5)	0.0096 (5)	−0.0001 (4)	0.0000 (4)	0.0004 (3)
O11	0.0126 (5)	0.0157 (5)	0.0138 (5)	−0.0013 (4)	0.0079 (4)	−0.0002 (4)
O12	0.0128 (5)	0.0108 (4)	0.0160 (5)	−0.0040 (4)	0.0047 (4)	−0.0018 (4)

Geometric parameters (Å, º)

Se1—O12	1.6489 (11)	Na2—O3	2.4616 (18)
Se1—O11	1.6493 (12)	Na2—O2	2.4642 (15)
Se1—O9	1.6497 (11)	Na2—O1	2.4774 (15)
Se1—O10	1.6538 (13)	Na2—O2^iv	2.4853 (15)
Na1—O5	2.4124 (17)	Na2—O4	2.5129 (16)
Na1—O8^i	2.4147 (15)	Na2—Na2^iii	3.4306 (18)
Na1—O6	2.4201 (15)	Na2—Na2^iv	3.7379 (18)
Na1—O6^ii	2.4286 (15)	O1—Na2^iii	2.4774 (15)
Na1—O7	2.4377 (17)	O2—Na2^iv	2.4853 (15)
Na1—O8	2.4483 (15)	O4—Na2^iii	2.4034 (16)
Na1—Na1^ii	3.6163 (7)	O6—Na1^i	2.4286 (15)
Na1—Na1^i	3.6164 (6)	O8—Na1^ii	2.4147 (15)
Na2—O4^iii	2.4034 (16)
O12—Se1—O11	109.30 (5)	O4^iii—Na2—O3	154.68 (5)
O12—Se1—O9	109.51 (6)	O4^iii—Na2—O2	95.13 (5)
O11—Se1—O9	109.15 (6)	O3—Na2—O2	80.64 (5)
O12—Se1—O10	109.22 (6)	O4^iii—Na2—O1	78.16 (5)
O11—Se1—O10	110.40 (7)	O3—Na2—O1	110.19 (4)
O9—Se1—O10	109.24 (6)	O2—Na2—O1	166.93 (5)
O5—Na1—O8^i	99.02 (5)	O4^iii—Na2—O2^iv	124.52 (5)
O5—Na1—O6	97.72 (6)	O3—Na2—O2^iv	79.87 (5)
O8^i—Na1—O6	84.12 (5)	O2—Na2—O2^iv	81.91 (6)
O5—Na1—O6^ii	86.87 (5)	O1—Na2—O2^iv	92.59 (5)
O8^i—Na1—O6^ii	95.48 (5)	O4^iii—Na2—O4	76.47 (6)
O6—Na1—O6^ii	175.40 (3)	O3—Na2—O4	82.35 (5)
O5—Na1—O7	177.96 (6)	O2—Na2—O4	113.50 (5)
O8^i—Na1—O7	82.96 (5)	O1—Na2—O4	76.14 (4)
O6—Na1—O7	81.97 (5)	O2^iv—Na2—O4	154.16 (5)
O6^ii—Na1—O7	93.43 (5)	Na2^iii—O1—Na2	87.64 (7)
O5—Na1—O8	85.41 (5)	Na2—O2—Na2^iv	98.09 (6)
O8^i—Na1—O8	175.33 (4)	Na2^iii—O4—Na2	88.47 (5)
O6—Na1—O8	96.80 (5)	Na1—O6—Na1^i	96.46 (5)
O6^ii—Na1—O8	83.23 (5)	Na1^ii—O8—Na1	96.08 (5)
O7—Na1—O8	92.62 (5)

Symmetry codes: (i) −x+1/2, y−1/2, −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)

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8B···O12^v	0.76 (3)	2.12 (3)	2.880 (2)	172 (3)
O8—H8A···O12	0.85 (3)	1.99 (3)	2.8273 (18)	168 (3)
O7—H7B···O10	0.87 (3)	1.90 (3)	2.7683 (19)	173 (3)
O7—H7A···O11^vi	0.79 (4)	2.00 (4)	2.790 (2)	174 (3)
O6—H6B···O9^vii	0.74 (3)	2.11 (3)	2.844 (2)	172 (3)
O6—H6A···O9	0.85 (3)	2.01 (3)	2.8473 (18)	166 (2)
O5—H5B···O7^ii	0.79 (3)	2.04 (3)	2.834 (2)	177 (3)
O5—H5A···O3^viii	0.87 (3)	1.99 (3)	2.837 (2)	168 (3)
O4—H4B···O5	0.86 (3)	1.96 (4)	2.8021 (19)	168 (3)
O4—H4A···O10^i	0.85 (3)	2.00 (3)	2.8502 (17)	172 (3)
O3—H3B···O9^ii	0.82 (3)	1.95 (3)	2.7738 (17)	175 (3)
O3—H3A···O12^i	0.78 (3)	2.02 (3)	2.7897 (17)	172 (3)
O2—H2B···O11^i	0.80 (3)	2.09 (3)	2.8842 (18)	172 (3)
O2—H2A···O11^ix	0.78 (3)	2.14 (3)	2.9055 (18)	169 (3)
O1—H1···O10^ii	0.83 (3)	2.01 (3)	2.8409 (17)	174 (3)
O8—H8B···O12^v	0.76 (3)	2.12 (3)	2.880 (2)	172 (3)
O8—H8A···O12	0.85 (3)	1.99 (3)	2.8273 (18)	168 (3)
O7—H7B···O10	0.87 (3)	1.90 (3)	2.7683 (19)	173 (3)
O7—H7A···O11^vi	0.79 (4)	2.00 (4)	2.790 (2)	174 (3)
O6—H6B···O9^vii	0.74 (3)	2.11 (3)	2.844 (2)	172 (3)
O6—H6A···O9	0.85 (3)	2.01 (3)	2.8473 (18)	166 (2)
O5—H5B···O7^ii	0.79 (3)	2.04 (3)	2.834 (2)	177 (3)
O5—H5A···O3^viii	0.87 (3)	1.99 (3)	2.837 (2)	168 (3)
O4—H4B···O5	0.86 (3)	1.96 (4)	2.8021 (19)	168 (3)
O4—H4A···O10^i	0.85 (3)	2.00 (3)	2.8502 (17)	172 (3)
O3—H3B···O9^ii	0.82 (3)	1.95 (3)	2.7738 (17)	175 (3)
O3—H3A···O12^i	0.78 (3)	2.02 (3)	2.7897 (17)	172 (3)
O2—H2B···O11^i	0.80 (3)	2.09 (3)	2.8842 (18)	172 (3)
O2—H2A···O11^ix	0.78 (3)	2.14 (3)	2.9055 (18)	169 (3)
O1—H1···O10^ii	0.83 (3)	2.01 (3)	2.8409 (17)	174 (3)
O1—H1···O10^ii	0.83 (3)	2.01 (3)	2.8409 (17)	174 (3)
O2—H2A···O11^ix	0.78 (3)	2.14 (3)	2.9055 (18)	169 (3)
O2—H2B···O11^i	0.80 (3)	2.09 (3)	2.8842 (18)	172 (3)
O3—H3A···O12^i	0.78 (3)	2.02 (3)	2.7897 (17)	172 (3)
O3—H3B···O9^ii	0.82 (3)	1.95 (3)	2.7738 (17)	175 (3)
O4—H4A···O10^i	0.85 (3)	2.00 (3)	2.8502 (17)	172 (3)
O4—H4B···O5	0.86 (3)	1.96 (4)	2.8021 (19)	168 (3)
O5—H5A···O3^viii	0.87 (3)	1.99 (3)	2.837 (2)	168 (3)
O5—H5B···O7^ii	0.79 (3)	2.04 (3)	2.834 (2)	177 (3)
O6—H6A···O9	0.85 (3)	2.01 (3)	2.8473 (18)	166 (2)
O6—H6B···O9^vii	0.74 (3)	2.11 (3)	2.844 (2)	172 (3)
O7—H7A···O11^vi	0.79 (4)	2.00 (4)	2.790 (2)	174 (3)
O7—H7B···O10	0.87 (3)	1.90 (3)	2.7683 (19)	173 (3)
O8—H8A···O12	0.85 (3)	1.99 (3)	2.8273 (18)	168 (3)
O8—H8B···O12^v	0.76 (3)	2.12 (3)	2.880 (2)	172 (3)

Symmetry codes: (i) −x+1/2, y−1/2, −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, z−1/2; (vii) −x+1/2, −y+1/2, −z+1; (viii) x, −y+1, z+1/2; (ix) x+1/2, −y+1/2, z−1/2.

(Na2_SeO4_10H2O_200k) Sodium selenate decahydrate

Crystal data

H20Na2O14Se	F(000) = 752
Mr = 369.10	Dx = 1.611 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.6498 (13) Å	Cell parameters from 10963 reflections
b = 10.5446 (9) Å	θ = 2.0–29.6°
c = 13.0181 (15) Å	µ = 2.58 mm^−1
β = 107.929 (9)°	T = 200 K
V = 1521.5 (3) Å^3	Monoclinic prism, colourless
Z = 4	0.12 × 0.09 × 0.05 mm

Data collection

STOE IPDS 2T diffractometer	3495 independent reflections
Radiation source: sealed X-ray tube, 12x0.4mm long-fine focus	3060 reflections with I > 2σ(I)
Plane graphite monochromator	Rint = 0.027
Detector resolution: 6.67 pixels mm^-1	θmax = 27.5°, θmin = 2.5°
rotation method scans	h = −15→14
Absorption correction: integration Coppens (1970)	k = −13→13
Tmin = 0.620, Tmax = 0.780	l = 0→16
6800 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.024	All H-atom parameters refined
wR(F^2) = 0.061	'w = 1/[σ^2(Fo^2) + (0.0352P)^2 + 0.2411P]' ' where P = (Fo^2 + 2Fc^2)/3'
S = 1.06	(Δ/σ)max = 0.002
3495 reflections	Δρmax = 0.54 e Å^−3
235 parameters	Δρmin = −0.51 e Å^−3
20 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0106 (5)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Se1	0.74825 (2)	0.63964 (2)	0.75969 (2)	0.01560 (7)
Na1	0.24297 (6)	0.75513 (6)	−0.02119 (5)	0.02274 (15)
Na2	0.25650 (6)	0.88793 (7)	0.23684 (5)	0.02151 (15)
O5	0.14506 (11)	0.71982 (12)	0.11612 (10)	0.0246 (3)
O2	0.35336 (11)	0.78364 (12)	−0.14703 (10)	0.0237 (3)
O6	0.38166 (11)	0.89064 (13)	0.11681 (11)	0.0257 (3)
O1	0.11765 (11)	0.60739 (13)	−0.15178 (11)	0.0259 (3)
O4	0.37015 (12)	0.56985 (14)	0.05278 (11)	0.0293 (3)
O7	0.13353 (12)	1.04175 (12)	0.11740 (11)	0.0270 (3)
O3	0.11521 (12)	0.93934 (14)	−0.08438 (12)	0.0310 (3)
O12	0.63205 (10)	0.69711 (11)	0.66509 (9)	0.0239 (3)
O10	0.76752 (11)	0.71909 (11)	0.87208 (9)	0.0269 (3)
O11	0.72352 (12)	0.49094 (11)	0.78199 (10)	0.0294 (3)
O13	0.86808 (11)	0.65052 (12)	0.71978 (10)	0.0282 (3)
O8	0.37693 (12)	1.04003 (12)	0.36147 (11)	0.0283 (3)
O14	0.90014 (13)	0.65112 (13)	0.08492 (11)	0.0284 (3)
O9	0.59775 (13)	0.85025 (13)	0.94526 (11)	0.0288 (3)
H1A	0.0485 (11)	0.628 (2)	−0.1850 (18)	0.042 (7)*
H1B	0.110 (2)	0.5352 (12)	−0.1324 (18)	0.042 (7)*
H2A	0.334 (2)	0.8521 (13)	−0.1759 (18)	0.035 (7)*
H2B	0.4255 (10)	0.793 (2)	−0.1190 (18)	0.044 (7)*
H3A	0.121 (2)	0.9920 (17)	−0.1279 (15)	0.041 (7)*
H3B	0.128 (4)	0.966 (5)	−0.0224 (17)	0.16 (2)*
H4A	0.341 (2)	0.539 (2)	0.0961 (16)	0.048 (7)*
H4B	0.4423 (12)	0.558 (5)	0.080 (3)	0.143 (17)*
H5A	0.170 (2)	0.6512 (14)	0.1437 (19)	0.039 (7)*
H5B	0.0720 (9)	0.713 (3)	0.100 (2)	0.053 (8)*
H6A	0.388 (2)	0.9635 (12)	0.0972 (18)	0.044 (7)*
H6B	0.4506 (12)	0.864 (2)	0.137 (2)	0.057 (9)*
H7A	0.0611 (11)	1.050 (5)	0.103 (4)	0.157 (19)*
H7B	0.162 (2)	1.1121 (13)	0.121 (2)	0.038 (7)*
H8A	0.362 (2)	1.1151 (11)	0.349 (2)	0.036 (7)*
H8B	0.366 (3)	1.016 (3)	0.4178 (17)	0.104 (13)*
H9A	0.6383 (19)	0.8028 (19)	0.9205 (18)	0.041 (7)*
H9B	0.618 (2)	0.834 (2)	1.0092 (9)	0.046 (7)*
H14A	0.8792 (19)	0.7064 (16)	0.1187 (15)	0.030 (6)*
H14B	0.862 (2)	0.666 (3)	0.0222 (10)	0.048 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Se1	0.01716 (10)	0.01285 (10)	0.01630 (10)	0.00012 (5)	0.00444 (6)	0.00002 (5)
Na1	0.0238 (3)	0.0223 (3)	0.0227 (3)	−0.0006 (3)	0.0079 (3)	−0.0012 (3)
Na2	0.0232 (3)	0.0190 (3)	0.0218 (3)	0.0005 (2)	0.0061 (3)	0.0005 (2)
O5	0.0216 (6)	0.0227 (6)	0.0281 (6)	−0.0002 (5)	0.0059 (5)	0.0016 (5)
O2	0.0215 (6)	0.0214 (6)	0.0263 (6)	−0.0018 (5)	0.0042 (5)	0.0025 (5)
O6	0.0206 (6)	0.0246 (6)	0.0316 (7)	0.0006 (5)	0.0075 (5)	0.0001 (5)
O1	0.0199 (6)	0.0259 (6)	0.0297 (7)	−0.0012 (5)	0.0044 (5)	0.0012 (5)
O4	0.0281 (7)	0.0322 (7)	0.0301 (7)	0.0029 (6)	0.0127 (5)	0.0042 (6)
O7	0.0245 (6)	0.0207 (6)	0.0332 (7)	−0.0020 (5)	0.0051 (5)	0.0016 (5)
O3	0.0310 (7)	0.0300 (7)	0.0346 (7)	0.0025 (6)	0.0142 (6)	0.0082 (6)
O12	0.0195 (6)	0.0247 (6)	0.0236 (6)	0.0021 (5)	0.0011 (5)	0.0027 (5)
O10	0.0337 (7)	0.0247 (6)	0.0219 (6)	−0.0001 (5)	0.0080 (5)	−0.0054 (5)
O11	0.0420 (8)	0.0156 (6)	0.0304 (6)	−0.0021 (5)	0.0107 (6)	0.0012 (5)
O13	0.0225 (6)	0.0336 (7)	0.0297 (7)	0.0009 (5)	0.0099 (5)	0.0034 (5)
O8	0.0312 (7)	0.0209 (6)	0.0299 (7)	0.0000 (5)	0.0049 (5)	0.0015 (5)
O14	0.0295 (7)	0.0289 (7)	0.0257 (7)	0.0034 (5)	0.0071 (6)	−0.0010 (5)
O9	0.0258 (7)	0.0332 (7)	0.0264 (7)	0.0031 (5)	0.0068 (5)	0.0005 (6)

Geometric parameters (Å, º)

Se1—O11	1.6362 (12)	Na1—Na2	3.5977 (10)
Se1—O13	1.6366 (13)	Na2—O7	2.3936 (15)
Se1—O12	1.6401 (11)	Na2—O8	2.4024 (15)
Se1—O10	1.6404 (11)	Na2—O2^ii	2.4045 (14)
Na1—O2	2.3928 (14)	Na2—O6	2.4436 (14)
Na1—O5	2.4269 (14)	Na2—O5	2.4580 (14)
Na1—O3	2.4313 (15)	Na2—O1^ii	2.4831 (15)
Na1—O1	2.4332 (14)	Na2—Na1^ii	3.5396 (10)
Na1—O4	2.4619 (16)	O2—Na2^i	2.4045 (14)
Na1—O6	2.4683 (15)	O1—Na2^i	2.4829 (15)
Na1—Na2^i	3.5395 (10)
O11—Se1—O13	109.73 (6)	O4—Na1—O6	89.68 (5)
O11—Se1—O12	109.73 (6)	O7—Na2—O8	95.43 (5)
O13—Se1—O12	108.86 (6)	O7—Na2—O2^ii	171.68 (5)
O11—Se1—O10	108.32 (6)	O8—Na2—O2^ii	90.82 (5)
O13—Se1—O10	110.58 (6)	O7—Na2—O6	86.12 (5)
O12—Se1—O10	109.62 (6)	O8—Na2—O6	94.86 (5)
O2—Na1—O5	175.61 (5)	O2^ii—Na2—O6	98.85 (5)
O2—Na1—O3	94.02 (5)	O7—Na2—O5	88.89 (5)
O5—Na1—O3	89.67 (5)	O8—Na2—O5	175.55 (5)
O2—Na1—O1	86.30 (5)	O2^ii—Na2—O5	84.99 (5)
O5—Na1—O1	95.71 (5)	O6—Na2—O5	84.33 (5)
O3—Na1—O1	95.85 (5)	O7—Na2—O1^ii	89.92 (5)
O2—Na1—O4	88.96 (5)	O8—Na2—O1^ii	86.70 (5)
O5—Na1—O4	87.30 (5)	O2^ii—Na2—O1^ii	84.94 (5)
O3—Na1—O4	176.73 (5)	O6—Na2—O1^ii	175.86 (5)
O1—Na1—O4	85.68 (5)	O5—Na2—O1^ii	94.41 (5)
O2—Na1—O6	93.22 (5)	Na1—O5—Na2	94.87 (5)
O5—Na1—O6	84.46 (5)	Na1—O2—Na2^i	95.09 (5)
O3—Na1—O6	88.80 (5)	Na2—O6—Na1	94.18 (5)
O1—Na1—O6	175.34 (5)	Na1—O1—Na2^i	92.10 (5)

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+3/2, z+1/2.

(Na2_SO_4_7H2O_120k) Sodium sulfate heptahydrate

Crystal data

H14Na2O11S	Dx = 1.564 Mg m^−3
Mr = 268.15	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P41212	Cell parameters from 27181 reflections
a = 14.3249 (15) Å	θ = 2.0–29.6°
c = 22.202 (4) Å	µ = 0.40 mm^−1
V = 4556.0 (10) Å^3	T = 120 K
Z = 16	, colourless
F(000) = 2240	0.53 × 0.48 × 0.44 mm

Data collection

STOE IPDS 2 diffractometer	6253 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus	3969 reflections with I > 2σ(I)
Plane graphite monochromator	Rint = 0.064
Detector resolution: 6.67 pixels mm^-1	θmax = 29.4°, θmin = 1.7°
rotation method scans	h = −13→13
Absorption correction: integration Coppens (1970)	k = 0→19
Tmin = 0.529, Tmax = 0.721	l = 0→30
6253 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	Only H-atom coordinates refined
wR(F^2) = 0.110	'w = 1/[σ^2(Fo^2) + (0.0622P)^2 + 0.0819P]' ' where P = (Fo^2 + 2Fc^2)/3'
S = 1.06	(Δ/σ)max = 0.008
6253 reflections	Δρmax = 0.36 e Å^−3
340 parameters	Δρmin = −0.40 e Å^−3
39 restraints	Absolute structure: 'Refined as an inversion twin.'
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.46 (19)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Na1	0.61239 (11)	0.62755 (10)	0.11347 (9)	0.0113 (3)
Na2	0.86243 (11)	0.62747 (10)	0.13653 (9)	0.0110 (3)
Na3	1.11223 (11)	0.62209 (10)	0.11353 (9)	0.0112 (3)
Na4	1.36229 (11)	0.62337 (10)	0.13648 (10)	0.0112 (3)
S1	0.37372 (7)	0.37372 (7)	1.0000	0.0068 (3)
S2	0.87743 (7)	0.87743 (7)	0.0000	0.0052 (3)
S3	0.37736 (6)	0.87374 (7)	−0.00020 (8)	0.00575 (13)
O1	0.9621 (2)	0.87792 (16)	0.03787 (15)	0.0122 (6)
O2	0.7929 (2)	0.87552 (16)	0.03841 (15)	0.0116 (6)
O3	0.7385 (2)	0.7428 (2)	0.12626 (12)	0.0130 (5)
H17	0.749 (2)	0.776 (2)	0.0967 (10)	0.016*
H18	0.738 (3)	0.773 (2)	0.1568 (10)	0.016*
O4	0.9906 (2)	0.73588 (19)	0.12342 (14)	0.0108 (5)
H10	1.015 (2)	0.761 (2)	0.1515 (12)	0.013*
H28	0.976 (2)	0.777 (2)	0.1001 (12)	0.013*
O5	0.84084 (17)	0.62624 (15)	0.02527 (12)	0.0142 (5)
H16	0.868 (2)	0.5822 (17)	0.0107 (19)	0.017*
H15	0.856 (2)	0.6728 (17)	0.0066 (17)	0.017*
O6	0.64416 (18)	0.64416 (18)	0.0000	0.0168 (7)
H23	0.6967 (17)	0.645 (2)	0.0096 (18)	0.020*
O7	0.9846 (2)	0.5125 (2)	0.12435 (16)	0.0141 (6)
H11	0.994 (2)	0.477 (2)	0.1533 (11)	0.017*
H12	0.991 (3)	0.481 (2)	0.0936 (10)	0.017*
O8	0.4886 (2)	0.5129 (2)	0.12318 (14)	0.0142 (5)
H24	0.502 (3)	0.472 (2)	0.1479 (13)	0.017*
H25	0.491 (3)	0.485 (2)	0.0901 (10)	0.017*
O9	0.7382 (2)	0.5172 (2)	0.12578 (11)	0.0095 (5)
H19	0.754 (3)	0.492 (2)	0.0951 (11)	0.011*
H20	0.721 (2)	0.479 (2)	0.1499 (11)	0.011*
O10	0.89422 (16)	0.64399 (16)	0.25008 (14)	0.0149 (5)
H13	0.9453 (17)	0.6291 (18)	0.244 (2)	0.018*
H14	0.8817 (19)	0.6962 (17)	0.2396 (16)	0.018*
O11	0.4861 (2)	0.7361 (2)	0.12468 (14)	0.0113 (5)
H27	0.469 (2)	0.775 (2)	0.1015 (12)	0.014*
H26	0.517 (2)	0.761 (2)	0.1490 (13)	0.014*
O12	1.39358 (19)	0.60642 (19)	0.2500	0.0183 (7)
H3	1.4488 (17)	0.609 (2)	0.2395 (18)	0.022*
O13	1.09071 (16)	0.62254 (16)	0.22498 (11)	0.0140 (5)
H8	1.101 (2)	0.576 (2)	0.2476 (18)	0.017*
H9	1.120 (2)	0.665 (2)	0.248 (2)	0.017*
O14	0.58986 (16)	0.62724 (16)	0.22466 (12)	0.0150 (5)
H21	0.600 (2)	0.5792 (17)	0.2462 (15)	0.018*
H22	0.618 (2)	0.6679 (18)	0.2445 (19)	0.018*
O15	1.2366 (2)	0.7329 (2)	0.12545 (12)	0.0146 (6)
H6	1.233 (3)	0.763 (2)	0.1564 (10)	0.018*
H7	1.244 (2)	0.765 (2)	0.0959 (10)	0.018*
O16	1.34020 (17)	0.62341 (16)	0.02522 (12)	0.0155 (5)
H1	1.354 (2)	0.6708 (17)	0.0060 (17)	0.019*
H2	1.368 (2)	0.5805 (18)	0.009 (2)	0.019*
O17	1.2396 (2)	0.5106 (2)	0.12675 (11)	0.0108 (6)
H5	1.222 (2)	0.471 (2)	0.1501 (11)	0.013*
H4	1.257 (3)	0.487 (2)	0.0974 (11)	0.013*
O18	0.2922 (2)	0.86527 (18)	0.03800 (14)	0.0098 (5)
O19	0.38331 (17)	0.7888 (2)	−0.03822 (14)	0.0096 (6)
O20	0.4615 (2)	0.88116 (17)	0.03838 (15)	0.0112 (6)
O21	0.37158 (17)	0.9581 (2)	−0.03852 (15)	0.0116 (6)
O22	0.37269 (15)	0.2887 (2)	0.96110 (14)	0.0091 (6)
O23	0.4588 (2)	0.37422 (16)	1.03840 (14)	0.0108 (6)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Na1	0.0111 (7)	0.0106 (7)	0.0123 (7)	0.0024 (4)	0.0012 (6)	−0.0001 (5)
Na2	0.0102 (7)	0.0094 (7)	0.0136 (8)	−0.0011 (4)	−0.0008 (6)	−0.0004 (5)
Na3	0.0110 (7)	0.0109 (7)	0.0117 (7)	0.0026 (4)	0.0013 (6)	−0.0002 (5)
Na4	0.0102 (7)	0.0105 (7)	0.0130 (7)	−0.0009 (4)	−0.0005 (6)	−0.0001 (5)
S1	0.0073 (4)	0.0073 (4)	0.0058 (7)	0.0023 (3)	0.0002 (3)	−0.0002 (3)
S2	0.0054 (4)	0.0054 (4)	0.0048 (6)	−0.0003 (3)	0.0000 (3)	0.0000 (3)
S3	0.0029 (4)	0.0091 (5)	0.0053 (2)	0.0009 (3)	0.0000 (3)	0.0002 (3)
O1	0.0102 (13)	0.0145 (14)	0.0118 (15)	−0.0018 (8)	−0.0034 (12)	0.0002 (9)
O2	0.0092 (13)	0.0137 (14)	0.0120 (15)	−0.0013 (8)	0.0052 (13)	−0.0007 (8)
O3	0.0198 (13)	0.0081 (12)	0.0111 (10)	0.0015 (9)	0.0030 (10)	−0.0031 (9)
O4	0.0124 (13)	0.0068 (10)	0.0132 (9)	0.0000 (9)	−0.0049 (10)	−0.0002 (9)
O5	0.0221 (13)	0.0093 (11)	0.0112 (12)	−0.0007 (10)	0.0024 (9)	−0.0016 (8)
O6	0.0184 (9)	0.0184 (9)	0.0137 (15)	−0.0012 (13)	−0.0005 (13)	0.0005 (13)
O7	0.0140 (14)	0.0127 (13)	0.0156 (10)	−0.0005 (8)	−0.0044 (11)	−0.0004 (10)
O8	0.0131 (13)	0.0119 (13)	0.0174 (10)	−0.0022 (9)	−0.0027 (10)	−0.0020 (11)
O9	0.0188 (12)	0.0042 (11)	0.0054 (9)	−0.0003 (9)	0.0059 (10)	0.0000 (8)
O10	0.0155 (10)	0.0125 (10)	0.0166 (11)	0.0023 (6)	0.0013 (12)	0.0001 (12)
O11	0.0121 (13)	0.0068 (10)	0.0148 (9)	0.0010 (8)	−0.0051 (10)	−0.0004 (9)
O12	0.0187 (9)	0.0187 (9)	0.0174 (16)	−0.0021 (13)	−0.0019 (13)	−0.0019 (13)
O13	0.0198 (13)	0.0100 (11)	0.0124 (12)	0.0020 (10)	−0.0027 (9)	−0.0020 (8)
O14	0.0204 (13)	0.0094 (11)	0.0153 (13)	0.0000 (10)	−0.0027 (9)	−0.0019 (8)
O15	0.0183 (12)	0.0145 (13)	0.0111 (11)	−0.0025 (10)	0.0025 (11)	−0.0022 (10)
O16	0.0221 (13)	0.0105 (12)	0.0140 (12)	−0.0015 (10)	0.0041 (9)	−0.0028 (8)
O17	0.0181 (13)	0.0084 (12)	0.0058 (9)	0.0050 (9)	0.0049 (10)	0.0005 (9)
O18	0.0071 (11)	0.0117 (10)	0.0106 (13)	0.0014 (8)	0.0041 (10)	0.0025 (9)
O19	0.0104 (11)	0.0092 (12)	0.0093 (13)	0.0000 (8)	−0.0006 (9)	−0.0050 (10)
O20	0.0098 (12)	0.0120 (12)	0.0118 (14)	−0.0018 (8)	−0.0037 (11)	−0.0019 (9)
O21	0.0150 (14)	0.0100 (13)	0.0096 (14)	−0.0016 (8)	0.0014 (9)	0.0039 (11)
O22	0.0120 (13)	0.0074 (12)	0.0079 (13)	0.0033 (7)	−0.0027 (8)	−0.0048 (12)
O23	0.0097 (13)	0.0132 (13)	0.0096 (14)	−0.0010 (8)	−0.0036 (12)	−0.0032 (8)

Geometric parameters (Å, º)

Na1—O11	2.399 (3)	Na4—O15	2.401 (4)
Na1—O9	2.414 (3)	Na4—O11^iii	2.413 (3)
Na1—O8	2.426 (4)	Na4—O8^iii	2.421 (3)
Na1—O3	2.463 (3)	Na4—O16	2.490 (3)
Na1—O14	2.490 (3)	Na4—O12	2.571 (2)
Na1—O6	2.571 (2)	Na4—Na1^iii	3.619 (2)
Na1—Na2	3.618 (3)	S1—O23^iv	1.488 (3)
Na1—Na4^i	3.619 (2)	S1—O23	1.488 (3)
Na2—O9	2.391 (3)	S1—O22^iv	1.493 (3)
Na2—O7	2.418 (3)	S1—O22	1.493 (3)
Na2—O4	2.422 (3)	S2—O1^v	1.475 (3)
Na2—O3	2.436 (4)	S2—O1	1.475 (3)
Na2—O5	2.490 (3)	S2—O2^v	1.482 (3)
Na2—O10	2.573 (4)	S2—O2	1.482 (3)
Na2—Na3	3.615 (3)	S3—O21	1.480 (3)
Na3—O4	2.397 (3)	S3—O20	1.482 (3)
Na3—O15	2.401 (3)	S3—O19	1.483 (3)
Na3—O7	2.421 (4)	S3—O18	1.490 (3)
Na3—O17	2.443 (3)	O6—Na1^v	2.571 (2)
Na3—O13	2.494 (3)	O8—Na4^i	2.421 (3)
Na3—O10^ii	2.570 (4)	O10—Na3^vi	2.570 (4)
Na3—Na4	3.618 (3)	O11—Na4^i	2.413 (3)
Na4—O17	2.397 (4)	O12—Na4^vii	2.572 (2)
O11—Na1—O9	167.53 (13)	O17—Na4—O15	83.20 (13)
O11—Na1—O8	83.01 (11)	O17—Na4—O11^iii	168.60 (13)
O9—Na1—O8	95.31 (11)	O15—Na4—O11^iii	95.89 (11)
O11—Na1—O3	96.12 (12)	O17—Na4—O8^iii	95.53 (12)
O9—Na1—O3	83.01 (13)	O15—Na4—O8^iii	167.15 (14)
O8—Na1—O3	168.28 (13)	O11^iii—Na4—O8^iii	82.81 (12)
O11—Na1—O14	78.50 (10)	O17—Na4—O16	79.49 (10)
O9—Na1—O14	89.05 (10)	O15—Na4—O16	78.66 (10)
O8—Na1—O14	79.39 (11)	O11^iii—Na4—O16	89.17 (11)
O3—Na1—O14	88.97 (10)	O8^iii—Na4—O16	88.52 (11)
O11—Na1—O6	100.09 (10)	O17—Na4—O12	98.77 (9)
O9—Na1—O6	92.26 (8)	O15—Na4—O12	107.00 (13)
O8—Na1—O6	106.20 (13)	O11^iii—Na4—O12	92.38 (9)
O3—Na1—O6	85.48 (12)	O8^iii—Na4—O12	85.84 (12)
O14—Na1—O6	174.10 (12)	O16—Na4—O12	173.92 (12)
O9—Na2—O7	94.44 (12)	O23^iv—S1—O23	108.7 (2)
O9—Na2—O4	167.30 (13)	O23^iv—S1—O22^iv	110.09 (13)
O7—Na2—O4	82.80 (12)	O23—S1—O22^iv	109.70 (19)
O9—Na2—O3	84.06 (13)	O23^iv—S1—O22	109.70 (19)
O7—Na2—O3	168.21 (13)	O23—S1—O22	110.09 (13)
O4—Na2—O3	96.10 (11)	O22^iv—S1—O22	108.6 (2)
O9—Na2—O5	78.69 (10)	O1^v—S2—O1	108.5 (2)
O7—Na2—O5	88.52 (11)	O1^v—S2—O2^v	110.1 (2)
O4—Na2—O5	88.82 (11)	O1—S2—O2^v	110.31 (14)
O3—Na2—O5	79.71 (10)	O1^v—S2—O2	110.31 (14)
O9—Na2—O10	106.87 (10)	O1—S2—O2	110.1 (2)
O7—Na2—O10	92.53 (11)	O2^v—S2—O2	107.5 (2)
O4—Na2—O10	85.68 (10)	O21—S3—O20	108.61 (14)
O3—Na2—O10	99.11 (11)	O21—S3—O19	110.2 (2)
O5—Na2—O10	174.23 (9)	O20—S3—O19	109.94 (17)
O4—Na3—O15	94.58 (12)	O21—S3—O18	110.36 (17)
O4—Na3—O7	83.27 (11)	O20—S3—O18	110.0 (2)
O15—Na3—O7	167.93 (14)	O19—S3—O18	107.71 (15)
O4—Na3—O17	167.70 (13)	Na2—O3—Na1	95.22 (13)
O15—Na3—O17	82.23 (13)	Na3—O4—Na2	97.24 (11)
O7—Na3—O17	97.36 (11)	Na1—O6—Na1^v	158.03 (18)
O4—Na3—O13	79.48 (10)	Na2—O7—Na3	96.67 (12)
O15—Na3—O13	88.89 (11)	Na4^i—O8—Na1	96.60 (11)
O7—Na3—O13	79.04 (11)	Na2—O9—Na1	97.70 (12)
O17—Na3—O13	88.56 (10)	Na3^vi—O10—Na2	158.12 (10)
O4—Na3—O10^ii	106.28 (11)	Na1—O11—Na4^i	97.56 (11)
O15—Na3—O10^ii	92.11 (11)	Na4—O12—Na4^vii	158.09 (18)
O7—Na3—O10^ii	99.90 (12)	Na4—O15—Na3	97.80 (13)
O17—Na3—O10^ii	85.76 (9)	Na4—O17—Na3	96.75 (13)
O13—Na3—O10^ii	174.05 (9)

Symmetry codes: (i) x−1, y, z; (ii) y+1/2, −x+3/2, z−1/4; (iii) x+1, y, z; (iv) y, x, −z+2; (v) y, x, −z; (vi) −y+3/2, x−1/2, z+1/4; (vii) −y+2, −x+2, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O17—H4···O22^viii	0.77 (2)	2.14 (3)	2.863 (4)	156 (3)
O17—H5···O18^ix	0.81 (2)	2.05 (2)	2.850 (4)	167 (3)
O16—H2···O23^viii	0.82 (2)	2.03 (3)	2.791 (4)	154 (3)
O16—H1···O19^iii	0.82 (2)	2.00 (2)	2.825 (4)	178 (4)
O15—H7···O18^iii	0.81 (2)	2.04 (2)	2.829 (4)	163 (3)
O15—H6···O22^x	0.81 (2)	2.01 (3)	2.785 (4)	159 (3)
O14—H22···O18^xi	0.83 (2)	2.04 (2)	2.825 (4)	157 (3)
O14—H21···O1^vi	0.85 (2)	1.94 (2)	2.790 (4)	174 (3)
O13—H9···O22^xii	0.90 (4)	1.99 (3)	2.820 (4)	152 (3)
O13—H8···O21^ix	0.85 (3)	1.95 (3)	2.799 (4)	172 (4)
O12—H3···O14^iii	0.82 (2)	2.06 (2)	2.883 (3)	171 (4)
O11—H26···O21^xi	0.78 (2)	2.13 (3)	2.849 (4)	152 (4)
O11—H27···O20	0.80 (2)	2.07 (2)	2.848 (4)	166 (3)
O10—H14···O16^vi	0.80 (2)	2.21 (3)	2.877 (3)	141 (3)
O10—H13···O13	0.77 (2)	2.13 (2)	2.886 (3)	166 (3)
O9—H20···O2^ix	0.80 (2)	2.03 (2)	2.819 (4)	168 (3)
O9—H19···O19^v	0.80 (2)	2.07 (2)	2.825 (4)	158 (3)
O8—H25···O23^xiii	0.84 (2)	2.01 (3)	2.770 (4)	150 (3)
O8—H24···O1^ix	0.82 (2)	2.03 (2)	2.853 (4)	177 (3)
O7—H12···O21^v	0.82 (2)	2.04 (3)	2.802 (4)	153 (3)
O7—H11···O20^ix	0.83 (2)	2.00 (2)	2.809 (4)	168 (4)
O6—H23···O5	0.78 (2)	2.11 (2)	2.884 (3)	170 (4)
O5—H15···O2^v	0.82 (2)	2.01 (2)	2.818 (4)	172 (3)
O5—H16···O20^v	0.81 (2)	2.05 (3)	2.811 (4)	156 (3)
O4—H28···O1	0.81 (2)	2.01 (2)	2.813 (4)	170 (3)
O4—H10···O23^xii	0.80 (2)	2.13 (3)	2.878 (4)	155 (3)
O3—H18···O19^xi	0.81 (2)	2.03 (2)	2.795 (4)	158 (3)
O3—H17···O2	0.82 (2)	2.03 (2)	2.833 (4)	166 (3)
O17—H4···O22^viii	0.77 (2)	2.14 (3)	2.863 (4)	156 (3)
O17—H5···O18^ix	0.81 (2)	2.05 (2)	2.850 (4)	167 (3)
O16—H2···O23^viii	0.82 (2)	2.03 (3)	2.791 (4)	154 (3)
O16—H1···O19^iii	0.82 (2)	2.00 (2)	2.825 (4)	178 (4)
O15—H7···O18^iii	0.81 (2)	2.04 (2)	2.829 (4)	163 (3)
O15—H6···O22^x	0.81 (2)	2.01 (3)	2.785 (4)	159 (3)
O14—H22···O18^xi	0.83 (2)	2.04 (2)	2.825 (4)	157 (3)
O14—H21···O1^vi	0.85 (2)	1.94 (2)	2.790 (4)	174 (3)
O13—H9···O22^xii	0.90 (4)	1.99 (3)	2.820 (4)	152 (3)
O13—H8···O21^ix	0.85 (3)	1.95 (3)	2.799 (4)	172 (4)
O12—H3···O14^iii	0.82 (2)	2.06 (2)	2.883 (3)	171 (4)
O11—H26···O21^xi	0.78 (2)	2.13 (3)	2.849 (4)	152 (4)
O11—H27···O20	0.80 (2)	2.07 (2)	2.848 (4)	166 (3)
O10—H14···O16^vi	0.80 (2)	2.21 (3)	2.877 (3)	141 (3)
O10—H13···O13	0.77 (2)	2.13 (2)	2.886 (3)	166 (3)
O9—H20···O2^ix	0.80 (2)	2.03 (2)	2.819 (4)	168 (3)
O9—H19···O19^v	0.80 (2)	2.07 (2)	2.825 (4)	158 (3)
O8—H25···O23^xiii	0.84 (2)	2.01 (3)	2.770 (4)	150 (3)
O8—H24···O1^ix	0.82 (2)	2.03 (2)	2.853 (4)	177 (3)
O7—H12···O21^v	0.82 (2)	2.04 (3)	2.802 (4)	153 (3)
O7—H11···O20^ix	0.83 (2)	2.00 (2)	2.809 (4)	168 (4)
O6—H23···O5	0.78 (2)	2.11 (2)	2.884 (3)	170 (4)
O5—H15···O2^v	0.82 (2)	2.01 (2)	2.818 (4)	172 (3)
O5—H16···O20^v	0.81 (2)	2.05 (3)	2.811 (4)	156 (3)
O4—H28···O1	0.81 (2)	2.01 (2)	2.813 (4)	170 (3)
O4—H10···O23^xii	0.80 (2)	2.13 (3)	2.878 (4)	155 (3)
O3—H18···O19^xi	0.81 (2)	2.03 (2)	2.795 (4)	158 (3)
O3—H17···O2	0.82 (2)	2.03 (2)	2.833 (4)	166 (3)
O3—H17···O2	0.82 (2)	2.03 (2)	2.833 (4)	166 (3)
O3—H18···O19^xi	0.81 (2)	2.03 (2)	2.795 (4)	158 (3)
O4—H10···O23^xii	0.80 (2)	2.13 (3)	2.878 (4)	155 (3)
O4—H28···O1	0.81 (2)	2.01 (2)	2.813 (4)	170 (3)
O5—H15···O2^v	0.82 (2)	2.01 (2)	2.818 (4)	172 (3)
O6—H23···O5	0.78 (2)	2.11 (2)	2.884 (3)	170 (4)
O7—H11···O20^ix	0.83 (2)	2.00 (2)	2.809 (4)	168 (4)
O7—H12···O21^v	0.82 (2)	2.04 (3)	2.802 (4)	153 (3)
O8—H24···O1^ix	0.82 (2)	2.03 (2)	2.853 (4)	177 (3)
O8—H25···O23^xiii	0.84 (2)	2.01 (3)	2.770 (4)	150 (3)
O9—H19···O19^v	0.80 (2)	2.07 (2)	2.825 (4)	158 (3)
O9—H20···O2^ix	0.80 (2)	2.03 (2)	2.819 (4)	168 (3)
O10—H13···O13	0.77 (2)	2.13 (2)	2.886 (3)	166 (3)
O10—H14···O16^vi	0.80 (2)	2.21 (3)	2.877 (3)	141 (3)
O11—H27···O20	0.80 (2)	2.07 (2)	2.848 (4)	166 (3)
O11—H26···O21^xi	0.78 (2)	2.13 (3)	2.849 (4)	152 (4)
O12—H3···O14^iii	0.82 (2)	2.06 (2)	2.883 (3)	171 (4)
O13—H8···O21^ix	0.85 (3)	1.95 (3)	2.799 (4)	172 (4)
O13—H9···O22^xii	0.90 (4)	1.99 (3)	2.820 (4)	152 (3)
O14—H21···O1^vi	0.85 (2)	1.94 (2)	2.790 (4)	174 (3)
O14—H22···O18^xi	0.83 (2)	2.04 (2)	2.825 (4)	157 (3)
O15—H6···O22^x	0.81 (2)	2.01 (3)	2.785 (4)	159 (3)
O15—H7···O18^iii	0.81 (2)	2.04 (2)	2.829 (4)	163 (3)
O16—H1···O19^iii	0.82 (2)	2.00 (2)	2.825 (4)	178 (4)
O16—H2···O23^viii	0.82 (2)	2.03 (3)	2.791 (4)	154 (3)
O17—H5···O18^ix	0.81 (2)	2.05 (2)	2.850 (4)	167 (3)
O17—H4···O22^viii	0.77 (2)	2.14 (3)	2.863 (4)	156 (3)
O3—H17···O2	0.82 (2)	2.03 (2)	2.833 (4)	166 (3)
O3—H18···O19^xi	0.81 (2)	2.03 (2)	2.795 (4)	158 (3)
O4—H10···O23^xii	0.80 (2)	2.13 (3)	2.878 (4)	155 (3)
O4—H28···O1	0.81 (2)	2.01 (2)	2.813 (4)	170 (3)
O5—H16···O20^v	0.81 (2)	2.05 (3)	2.811 (4)	156 (3)
O5—H15···O2^v	0.82 (2)	2.01 (2)	2.818 (4)	172 (3)
O6—H23···O5	0.78 (2)	2.11 (2)	2.884 (3)	170 (4)
O7—H11···O20^ix	0.83 (2)	2.00 (2)	2.809 (4)	168 (4)
O7—H12···O21^v	0.82 (2)	2.04 (3)	2.802 (4)	153 (3)
O8—H24···O1^ix	0.82 (2)	2.03 (2)	2.853 (4)	177 (3)
O8—H25···O23^xiii	0.84 (2)	2.01 (3)	2.770 (4)	150 (3)
O9—H19···O19^v	0.80 (2)	2.07 (2)	2.825 (4)	158 (3)
O9—H20···O2^ix	0.80 (2)	2.03 (2)	2.819 (4)	168 (3)
O10—H13···O13	0.77 (2)	2.13 (2)	2.886 (3)	166 (3)
O10—H14···O16^vi	0.80 (2)	2.21 (3)	2.877 (3)	141 (3)
O11—H27···O20	0.80 (2)	2.07 (2)	2.848 (4)	166 (3)
O11—H26···O21^xi	0.78 (2)	2.13 (3)	2.849 (4)	152 (4)
O12—H3···O14^iii	0.82 (2)	2.06 (2)	2.883 (3)	171 (4)
O13—H8···O21^ix	0.85 (3)	1.95 (3)	2.799 (4)	172 (4)
O13—H9···O22^xii	0.90 (4)	1.99 (3)	2.820 (4)	152 (3)
O14—H21···O1^vi	0.85 (2)	1.94 (2)	2.790 (4)	174 (3)
O14—H22···O18^xi	0.83 (2)	2.04 (2)	2.825 (4)	157 (3)
O15—H6···O22^x	0.81 (2)	2.01 (3)	2.785 (4)	159 (3)
O15—H7···O18^iii	0.81 (2)	2.04 (2)	2.829 (4)	163 (3)
O16—H1···O19^iii	0.82 (2)	2.00 (2)	2.825 (4)	178 (4)
O16—H2···O23^viii	0.82 (2)	2.03 (3)	2.791 (4)	154 (3)
O17—H5···O18^ix	0.81 (2)	2.05 (2)	2.850 (4)	167 (3)
O17—H4···O22^viii	0.77 (2)	2.14 (3)	2.863 (4)	156 (3)
O3—H17···O2	0.82 (2)	2.03 (2)	2.833 (4)	166 (3)
O3—H18···O19^xi	0.81 (2)	2.03 (2)	2.795 (4)	158 (3)
O4—H10···O23^xii	0.80 (2)	2.13 (3)	2.878 (4)	155 (3)
O4—H28···O1	0.81 (2)	2.01 (2)	2.813 (4)	170 (3)
O5—H16···O20^v	0.81 (2)	2.05 (3)	2.811 (4)	156 (3)
O5—H15···O2^v	0.82 (2)	2.01 (2)	2.818 (4)	172 (3)
O6—H23···O5	0.78 (2)	2.11 (2)	2.884 (3)	170 (4)
O7—H11···O20^ix	0.83 (2)	2.00 (2)	2.809 (4)	168 (4)
O7—H12···O21^v	0.82 (2)	2.04 (3)	2.802 (4)	153 (3)
O8—H24···O1^ix	0.82 (2)	2.03 (2)	2.853 (4)	177 (3)
O8—H25···O23^xiii	0.84 (2)	2.01 (3)	2.770 (4)	150 (3)
O9—H19···O19^v	0.80 (2)	2.07 (2)	2.825 (4)	158 (3)
O9—H20···O2^ix	0.80 (2)	2.03 (2)	2.819 (4)	168 (3)
O10—H13···O13	0.77 (2)	2.13 (2)	2.886 (3)	166 (3)
O10—H14···O16^vi	0.80 (2)	2.21 (3)	2.877 (3)	141 (3)
O11—H27···O20	0.80 (2)	2.07 (2)	2.848 (4)	166 (3)
O11—H26···O21^xi	0.78 (2)	2.13 (3)	2.849 (4)	152 (4)
O12—H3···O14^iii	0.82 (2)	2.06 (2)	2.883 (3)	171 (4)
O13—H8···O21^ix	0.85 (3)	1.95 (3)	2.799 (4)	172 (4)
O13—H9···O22^xii	0.90 (4)	1.99 (3)	2.820 (4)	152 (3)
O14—H21···O1^vi	0.85 (2)	1.94 (2)	2.790 (4)	174 (3)
O14—H22···O18^xi	0.83 (2)	2.04 (2)	2.825 (4)	157 (3)
O15—H6···O22^x	0.81 (2)	2.01 (3)	2.785 (4)	159 (3)
O15—H7···O18^iii	0.81 (2)	2.04 (2)	2.829 (4)	163 (3)
O16—H1···O19^iii	0.82 (2)	2.00 (2)	2.825 (4)	178 (4)
O16—H2···O23^viii	0.82 (2)	2.03 (3)	2.791 (4)	154 (3)
O17—H5···O18^ix	0.81 (2)	2.05 (2)	2.850 (4)	167 (3)
O17—H4···O22^viii	0.77 (2)	2.14 (3)	2.863 (4)	156 (3)

Symmetry codes: (iii) x+1, y, z; (v) y, x, −z; (vi) −y+3/2, x−1/2, z+1/4; (viii) y+1, x, −z+1; (ix) −x+3/2, y−1/2, −z+1/4; (x) −y+3/2, x+1/2, z−3/4; (xi) −y+3/2, x+1/2, z+1/4; (xii) −x+3/2, y+1/2, −z+5/4; (xiii) x, y, z−1.

(Na2_SO4_10H2O_120k) Sodium sulfate decahydrate

Crystal data

H20Na2O14S	F(000) = 680
Mr = 322.21	Dx = 1.484 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.470 (2) Å	Cell parameters from 4106 reflections
b = 10.3515 (12) Å	θ = 2.8–29.6°
c = 12.759 (2) Å	µ = 0.34 mm^−1
β = 107.815 (15)°	T = 120 K
V = 1442.2 (4) Å^3	Monoclinic prism, colourless
Z = 4	0.53 × 0.45 × 0.37 mm

Data collection

STOE IPDS 2 diffractometer	3876 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-finefocus	3441 reflections with I > 2σ(I)
Plane graphite monochromator	Rint = 0.119
Detector resolution: 6.67 pixels mm^-1	θmax = 29.2°, θmin = 1.9°
rotation method scans	h = −15→14
Absorption correction: integration Coppens (1970)	k = 0→14
Tmin = 0.441, Tmax = 0.796	l = 0→17
3876 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	All H-atom parameters refined
wR(F^2) = 0.076	'w = 1/[σ^2(Fo^2) + (0.054P)^2 + 0.1271P]' ' where P = (Fo^2 + 2Fc^2)/3'
S = 1.05	(Δ/σ)max = 0.001
3876 reflections	Δρmax = 0.69 e Å^−3
235 parameters	Δρmin = −0.56 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0111 (14)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
S1	0.74847 (2)	0.63907 (2)	0.75853 (2)	0.00790 (7)
Na1	0.24380 (3)	0.75456 (4)	−0.01838 (3)	0.01176 (10)
Na2	0.25537 (3)	0.88729 (4)	0.23846 (3)	0.01132 (10)
O1	0.11388 (7)	0.60787 (7)	−0.15079 (6)	0.01386 (14)
O2	0.35429 (7)	0.78653 (7)	−0.14593 (6)	0.01278 (14)
O3	0.11844 (7)	0.94304 (8)	−0.08351 (7)	0.01664 (15)
O4	0.36884 (7)	0.56458 (7)	0.05541 (6)	0.01573 (15)
O5	0.14374 (6)	0.71693 (7)	0.11880 (6)	0.01315 (14)
O6	0.38493 (7)	0.89065 (7)	0.11985 (6)	0.01378 (14)
O7	0.13273 (7)	1.04630 (7)	0.11977 (6)	0.01487 (15)
O8	0.37653 (7)	1.04462 (7)	0.36125 (6)	0.01537 (15)
O9	0.60148 (7)	0.84796 (8)	0.94609 (6)	0.01558 (15)
O10	0.76428 (7)	0.71185 (7)	0.86187 (5)	0.01399 (14)
O11	0.72859 (7)	0.50165 (7)	0.77807 (6)	0.01537 (15)
O12	0.64134 (6)	0.69033 (7)	0.67169 (5)	0.01296 (14)
O13	0.85903 (6)	0.65299 (7)	0.72295 (6)	0.01451 (15)
O14	0.89589 (7)	0.65373 (7)	0.08166 (6)	0.01542 (15)
H1A	0.0412 (16)	0.6308 (15)	−0.1784 (14)	0.024 (4)*
H1B	0.1113 (14)	0.5288 (17)	−0.1298 (13)	0.025 (4)*
H2A	0.3337 (14)	0.8551 (15)	−0.1742 (13)	0.016 (3)*
H2B	0.4254 (18)	0.7955 (18)	−0.1197 (15)	0.036 (5)*
H3A	0.1311 (18)	0.994 (2)	−0.1234 (18)	0.046 (5)*
H3B	0.128 (3)	0.974 (3)	−0.021 (3)	0.095 (9)*
H4A	0.3394 (18)	0.5304 (19)	0.0953 (17)	0.043 (5)*
H4B	0.436 (3)	0.559 (3)	0.075 (3)	0.108 (11)*
H5A	0.1689 (15)	0.6481 (16)	0.1485 (14)	0.022 (4)*
H5B	0.0704 (17)	0.7056 (16)	0.1020 (14)	0.028 (4)*
H6A	0.3923 (14)	0.9687 (18)	0.1026 (13)	0.028 (4)*
H6B	0.4553 (16)	0.8617 (15)	0.1447 (14)	0.023 (4)*
H7A	0.066 (3)	1.055 (3)	0.112 (3)	0.116 (12)*
H7B	0.1626 (17)	1.1247 (18)	0.1270 (15)	0.033 (4)*
H8A	0.3607 (15)	1.1274 (17)	0.3469 (14)	0.028 (4)*
H8B	0.364 (3)	1.023 (3)	0.418 (3)	0.113 (11)*
H9A	0.6453 (15)	0.7976 (16)	0.9223 (14)	0.025 (4)*
H9B	0.6182 (19)	0.836 (2)	1.0070 (18)	0.048 (6)*
H14A	0.8728 (15)	0.7114 (17)	0.1198 (14)	0.030 (4)*
H14B	0.8565 (16)	0.6694 (17)	0.0194 (16)	0.033 (4)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.00917 (11)	0.00747 (11)	0.00655 (11)	0.00007 (6)	0.00164 (8)	−0.00012 (6)
Na1	0.01328 (18)	0.01242 (19)	0.00947 (18)	−0.00044 (14)	0.00330 (13)	−0.00052 (13)
Na2	0.01297 (19)	0.01106 (19)	0.00955 (18)	0.00027 (13)	0.00288 (14)	0.00005 (13)
O1	0.0116 (3)	0.0147 (3)	0.0139 (3)	−0.0007 (3)	0.0018 (2)	0.0007 (3)
O2	0.0119 (3)	0.0124 (3)	0.0124 (3)	−0.0010 (2)	0.0012 (2)	0.0017 (2)
O3	0.0175 (3)	0.0167 (4)	0.0171 (3)	0.0014 (3)	0.0072 (3)	0.0038 (3)
O4	0.0146 (3)	0.0182 (4)	0.0155 (3)	0.0013 (3)	0.0062 (3)	0.0022 (3)
O5	0.0118 (3)	0.0130 (3)	0.0139 (3)	−0.0004 (2)	0.0028 (2)	0.0012 (2)
O6	0.0119 (3)	0.0141 (3)	0.0148 (3)	0.0003 (2)	0.0033 (3)	0.0002 (3)
O7	0.0137 (3)	0.0133 (3)	0.0162 (3)	−0.0013 (3)	0.0025 (3)	0.0007 (2)
O8	0.0167 (3)	0.0134 (3)	0.0140 (3)	0.0001 (3)	0.0018 (3)	0.0003 (2)
O9	0.0142 (3)	0.0194 (4)	0.0129 (3)	0.0020 (3)	0.0037 (3)	0.0009 (3)
O10	0.0186 (3)	0.0134 (3)	0.0095 (3)	−0.0005 (3)	0.0036 (2)	−0.0032 (2)
O11	0.0223 (3)	0.0084 (3)	0.0152 (3)	−0.0014 (3)	0.0054 (3)	0.0004 (2)
O12	0.0113 (3)	0.0145 (3)	0.0103 (3)	0.0010 (2)	−0.0009 (2)	0.0021 (2)
O13	0.0117 (3)	0.0186 (3)	0.0142 (3)	0.0005 (2)	0.0053 (3)	0.0014 (3)
O14	0.0158 (3)	0.0169 (3)	0.0123 (3)	0.0012 (3)	0.0025 (3)	−0.0002 (3)

Geometric parameters (Å, º)

S1—O11	1.4740 (7)	Na1—Na2	3.5182 (7)
S1—O12	1.4785 (7)	Na2—O2^ii	2.3826 (8)
S1—O13	1.4790 (7)	Na2—O7	2.3828 (9)
S1—O10	1.4806 (7)	Na2—O8	2.3886 (9)
Na1—O2	2.3719 (9)	Na2—O6	2.4240 (9)
Na1—O5	2.4002 (9)	Na2—O5	2.4258 (9)
Na1—O3	2.4153 (9)	Na2—O1^ii	2.4568 (9)
Na1—O1	2.4166 (9)	Na2—Na1^ii	3.4714 (7)
Na1—O6	2.4431 (9)	O1—Na2^i	2.4569 (9)
Na1—O4	2.4464 (9)	O2—Na2^i	2.3826 (8)
Na1—Na2^i	3.4714 (7)
O11—S1—O12	109.69 (4)	O6—Na1—O4	90.27 (3)
O11—S1—O13	109.72 (4)	O2^ii—Na2—O7	172.68 (3)
O12—S1—O13	109.22 (4)	O2^ii—Na2—O8	92.15 (3)
O11—S1—O10	108.88 (4)	O7—Na2—O8	93.31 (3)
O12—S1—O10	109.39 (4)	O2^ii—Na2—O6	97.50 (3)
O13—S1—O10	109.93 (4)	O7—Na2—O6	87.07 (3)
O2—Na1—O5	176.35 (3)	O8—Na2—O6	93.15 (3)
O2—Na1—O3	92.18 (3)	O2^ii—Na2—O5	84.28 (3)
O5—Na1—O3	90.85 (3)	O7—Na2—O5	90.39 (3)
O2—Na1—O1	87.29 (3)	O8—Na2—O5	176.04 (3)
O5—Na1—O1	94.45 (3)	O6—Na2—O5	85.63 (3)
O3—Na1—O1	95.29 (3)	O2^ii—Na2—O1^ii	86.13 (3)
O2—Na1—O6	92.27 (3)	O7—Na2—O1^ii	89.20 (3)
O5—Na1—O6	85.77 (3)	O8—Na2—O1^ii	87.88 (3)
O3—Na1—O6	88.61 (3)	O6—Na2—O1^ii	176.18 (3)
O1—Na1—O6	176.08 (3)	O5—Na2—O1^ii	93.58 (3)
O2—Na1—O4	90.16 (3)	Na1—O1—Na2^i	90.84 (3)
O5—Na1—O4	86.78 (3)	Na1—O2—Na2^i	93.80 (3)
O3—Na1—O4	177.45 (3)	Na1—O5—Na2	93.60 (3)
O1—Na1—O4	85.84 (3)	Na2—O6—Na1	92.58 (3)

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+3/2, z+1/2.

(Na2_SO4_10H2O_250k) Sodium sulfate-water (1/10)

Crystal data

H20Na2O14S	F(000) = 680
Mr = 322.20	Dx = 1.481 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 11.467 (2) Å	Cell parameters from 2802 reflections
b = 10.3455 (12) Å	θ = 3.3–27.3°
c = 12.795 (2) Å	µ = 0.34 mm^−1
β = 107.805 (15)°	T = 250 K
V = 1445.2 (4) Å^3	Monoclinic prism, colourless
Z = 4	0.4 × 0.3 × 0.2 mm

Data collection

Bruker APEX-II CCD diffractometer	3331 independent reflections
Radiation source: sealed tube	2694 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.031
ϕ and ω scans	θmax = 27.6°, θmin = 1.9°
Absorption correction: integration Coppens (1970)	h = −14→14
Tmin = 0.884, Tmax = 0.934	k = −11→13
25202 measured reflections	l = −16→16

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.024	All H-atom parameters refined
wR(F^2) = 0.061	'w = 1/[σ^2(Fo^2) + (0.0245P)^2 + 0.3224P]' ' where P = (Fo^2 + 2Fc^2)/3'
S = 1.03	(Δ/σ)max = 0.001
3331 reflections	Δρmax = 0.23 e Å^−3
270 parameters	Δρmin = −0.31 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0161 (7)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Na1	0.24416 (4)	0.75357 (4)	−0.01647 (4)	0.02840 (13)
Na2	0.25493 (4)	0.88689 (4)	0.23914 (4)	0.02661 (12)
S1	0.25056 (2)	0.14019 (2)	0.74135 (2)	0.02026 (9)
O1	0.11249 (9)	0.60955 (10)	−0.15066 (8)	0.0318 (2)
O2	0.35382 (9)	0.78731 (9)	−0.14485 (8)	0.0293 (2)
O3	0.36785 (11)	0.56190 (10)	0.05530 (9)	0.0370 (2)
O4	0.11939 (11)	0.94226 (11)	−0.08276 (9)	0.0385 (2)
O5	0.14467 (9)	0.71575 (9)	0.12011 (8)	0.0296 (2)
O6	0.38589 (9)	0.88979 (10)	0.12104 (8)	0.0316 (2)
O7	0.13296 (11)	1.04628 (10)	0.11975 (8)	0.0340 (2)
O8	0.37671 (12)	1.04447 (10)	0.36061 (9)	0.0348 (2)
O9	0.60116 (9)	0.84812 (10)	0.94565 (10)	0.0353 (2)
O10	0.89687 (10)	0.65267 (10)	0.08112 (10)	0.0356 (2)
O11	0.35703 (8)	0.19000 (8)	0.82784 (7)	0.0324 (2)
O12A	0.27034 (12)	0.00311 (11)	0.72349 (10)	0.0370 (3)	0.85
O12B	0.2221 (5)	0.0024 (5)	0.7558 (5)	0.0208 (12)	0.15
O13A	0.14162 (11)	0.15529 (14)	0.77600 (11)	0.0364 (3)	0.85
O13B	0.1380 (6)	0.2190 (6)	0.7448 (6)	0.0258 (14)	0.15
O14A	0.23706 (14)	0.21065 (13)	0.63879 (12)	0.0325 (3)	0.85
O14B	0.2674 (8)	0.1601 (7)	0.6324 (7)	0.0280 (16)	0.15
H1A	0.1077 (13)	0.5351 (17)	−0.1297 (13)	0.044 (5)*
H1B	0.0409 (16)	0.6332 (14)	−0.1826 (13)	0.044 (5)*
H2A	0.3336 (15)	0.8570 (16)	−0.1715 (14)	0.046 (5)*
H2B	0.4228 (17)	0.7964 (16)	−0.1180 (14)	0.050 (5)*
H3A	0.3427 (16)	0.5278 (18)	0.0916 (15)	0.052 (6)*
H3B	0.435 (3)	0.560 (3)	0.077 (2)	0.145 (13)*
H4A	0.1340 (17)	0.9907 (19)	−0.1228 (16)	0.065 (6)*
H4B	0.058 (3)	0.936 (3)	−0.100 (2)	0.129 (12)*
H5A	0.1701 (15)	0.6442 (17)	0.1482 (15)	0.050 (5)*
H5B	0.0741 (17)	0.7072 (16)	0.1038 (14)	0.050 (5)*
H6B	0.4529 (16)	0.8645 (15)	0.1419 (13)	0.043 (5)*
H6A	0.3913 (14)	0.9659 (18)	0.0983 (13)	0.053 (5)*
H7A	0.1539 (16)	1.1176 (18)	0.1298 (14)	0.051 (5)*
H7B	0.073 (3)	1.057 (3)	0.118 (2)	0.022 (8)*	0.5
H7C	0.133 (3)	1.008 (4)	0.024 (3)	0.077 (11)*	0.5
H8A	0.436 (3)	1.050 (3)	0.372 (3)	0.033 (11)*	0.5
H8B	0.3614 (14)	1.1233 (17)	0.3500 (13)	0.044 (5)*
H8C	0.356 (3)	1.018 (3)	0.436 (3)	0.068 (11)*	0.5
H9A	0.6413 (16)	0.7959 (17)	0.9194 (14)	0.055 (5)*
H9B	0.6129 (16)	0.8376 (17)	1.0014 (15)	0.049 (6)*
H10A	0.8743 (15)	0.7103 (18)	0.1193 (15)	0.058 (5)*
H10B	0.8617 (16)	0.6647 (17)	0.0288 (16)	0.047 (6)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Na1	0.0301 (3)	0.0298 (3)	0.0268 (3)	−0.00172 (19)	0.0109 (2)	−0.0022 (2)
Na2	0.0291 (3)	0.0253 (2)	0.0254 (3)	0.00016 (19)	0.0082 (2)	0.00041 (18)
S1	0.02278 (15)	0.01809 (14)	0.01982 (16)	−0.00057 (11)	0.00638 (11)	−0.00014 (10)
O1	0.0260 (5)	0.0331 (5)	0.0343 (5)	−0.0023 (4)	0.0060 (4)	0.0015 (4)
O2	0.0264 (5)	0.0290 (5)	0.0301 (5)	−0.0020 (4)	0.0051 (4)	0.0030 (4)
O3	0.0340 (6)	0.0412 (6)	0.0385 (6)	0.0035 (4)	0.0152 (5)	0.0071 (5)
O4	0.0342 (6)	0.0417 (6)	0.0426 (6)	0.0031 (5)	0.0164 (5)	0.0103 (5)
O5	0.0254 (5)	0.0304 (5)	0.0326 (5)	−0.0015 (4)	0.0083 (4)	0.0020 (4)
O6	0.0255 (5)	0.0329 (5)	0.0366 (6)	0.0002 (4)	0.0098 (4)	0.0006 (4)
O7	0.0301 (6)	0.0289 (5)	0.0403 (6)	−0.0019 (4)	0.0067 (4)	0.0004 (4)
O8	0.0338 (6)	0.0283 (6)	0.0384 (6)	−0.0003 (4)	0.0049 (5)	0.0003 (4)
O9	0.0322 (5)	0.0428 (6)	0.0311 (6)	0.0042 (4)	0.0100 (5)	0.0020 (5)
O10	0.0332 (5)	0.0403 (6)	0.0313 (6)	0.0030 (4)	0.0068 (5)	−0.0001 (5)
O11	0.0286 (4)	0.0347 (5)	0.0293 (5)	−0.0023 (4)	0.0019 (4)	−0.0041 (4)
O12A	0.0513 (8)	0.0202 (5)	0.0384 (7)	0.0018 (5)	0.0123 (6)	−0.0006 (5)
O12B	0.034 (3)	0.015 (3)	0.021 (3)	−0.005 (2)	0.020 (3)	−0.002 (2)
O13A	0.0284 (6)	0.0465 (8)	0.0369 (8)	−0.0010 (6)	0.0139 (5)	−0.0040 (6)
O13B	0.023 (3)	0.020 (3)	0.036 (4)	0.010 (3)	0.010 (3)	0.004 (3)
O14A	0.0407 (8)	0.0314 (8)	0.0254 (7)	0.0001 (6)	0.0102 (6)	0.0060 (6)
O14B	0.037 (4)	0.027 (4)	0.023 (3)	0.003 (3)	0.013 (3)	−0.001 (3)

Geometric parameters (Å, º)

Na1—O2	2.3800 (11)	Na2—Na1^ii	3.4843 (8)
Na1—O5	2.3934 (11)	S1—O13A	1.4561 (12)
Na1—O4	2.4156 (12)	S1—O12A	1.4651 (11)
Na1—O1	2.4211 (11)	S1—O14A	1.4673 (15)
Na1—O6	2.4443 (11)	S1—O11	1.4678 (9)
Na1—O3	2.4475 (12)	S1—O14B	1.479 (8)
Na1—Na2^i	3.4843 (8)	S1—O12B	1.487 (5)
Na1—Na2	3.5167 (8)	S1—O13B	1.539 (6)
Na2—O8	2.3867 (12)	O1—Na2^i	2.4629 (11)
Na2—O7	2.3880 (11)	O2—Na2^i	2.3891 (10)
Na2—O2^ii	2.3891 (10)	O12A—O12B	0.786 (5)
Na2—O5	2.4239 (10)	O13A—O13B	0.765 (6)
Na2—O6	2.4346 (11)	O14A—O14B	0.647 (6)
Na2—O1^ii	2.4629 (11)
O2—Na1—O5	176.71 (4)	O13A—S1—O14A	110.69 (8)
O2—Na1—O4	91.17 (4)	O12A—S1—O14A	108.69 (7)
O5—Na1—O4	91.44 (4)	O13A—S1—O11	109.03 (6)
O2—Na1—O1	86.98 (4)	O12A—S1—O11	108.95 (6)
O5—Na1—O1	94.82 (4)	O14A—S1—O11	109.62 (7)
O4—Na1—O1	94.27 (4)	O13A—S1—O14B	130.1 (3)
O2—Na1—O6	92.11 (4)	O12A—S1—O14B	85.2 (3)
O5—Na1—O6	85.94 (4)	O14A—S1—O14B	25.4 (2)
O4—Na1—O6	88.79 (4)	O11—S1—O14B	110.1 (3)
O1—Na1—O6	176.83 (4)	O13A—S1—O12B	79.8 (2)
O2—Na1—O3	90.57 (4)	O12A—S1—O12B	30.88 (19)
O5—Na1—O3	86.82 (4)	O14A—S1—O12B	128.4 (2)
O4—Na1—O3	178.25 (4)	O11—S1—O12B	114.0 (2)
O1—Na1—O3	86.08 (4)	O14B—S1—O12B	110.4 (4)
O6—Na1—O3	90.89 (4)	O13A—S1—O13B	29.4 (2)
O8—Na2—O7	93.24 (4)	O12A—S1—O13B	133.5 (2)
O8—Na2—O2^ii	92.21 (4)	O14A—S1—O13B	84.4 (3)
O7—Na2—O2^ii	172.86 (4)	O11—S1—O13B	107.7 (3)
O8—Na2—O5	175.60 (4)	O14B—S1—O13B	107.8 (4)
O7—Na2—O5	90.66 (4)	O12B—S1—O13B	106.6 (3)
O2^ii—Na2—O5	84.07 (4)	Na1—O1—Na2^i	91.02 (4)
O8—Na2—O6	92.67 (4)	Na1—O2—Na2^i	93.87 (4)
O7—Na2—O6	86.92 (4)	Na1—O5—Na2	93.78 (4)
O2^ii—Na2—O6	97.43 (4)	Na2—O6—Na1	92.24 (4)
O5—Na2—O6	85.48 (4)	O12B—O12A—S1	76.1 (4)
O8—Na2—O1^ii	88.59 (4)	O12A—O12B—S1	73.0 (4)
O7—Na2—O1^ii	89.69 (4)	O13B—O13A—S1	81.3 (5)
O2^ii—Na2—O1^ii	85.84 (4)	O13A—O13B—S1	69.3 (4)
O5—Na2—O1^ii	93.49 (4)	O14B—O14A—S1	78.3 (8)
O6—Na2—O1^ii	176.45 (4)	O14A—O14B—S1	76.3 (8)
O13A—S1—O12A	109.84 (8)

Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+3/2, z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O10^iii	0.823 (17)	2.045 (18)	2.8672 (15)	176.9 (15)
O1—H1B···O13A^iv	0.834 (17)	2.081 (17)	2.9033 (17)	168.5 (15)
O1—H1B···O13B^iv	0.834 (17)	2.152 (18)	2.978 (6)	170.5 (15)
O2—H2A···O12A^v	0.801 (17)	2.005 (18)	2.7842 (15)	164.2 (17)
O2—H2A···O12B^v	0.801 (17)	2.008 (19)	2.770 (6)	158.7 (16)
O2—H2B···O9^vi	0.765 (18)	2.028 (19)	2.7878 (15)	171.5 (18)
O3—H3A···O12A^vii	0.710 (19)	2.121 (19)	2.7938 (18)	158.5 (19)
O3—H3A···O14B^vii	0.710 (19)	2.25 (2)	2.875 (7)	147.3 (19)
O3—H3B···O8^viii	0.74 (3)	2.07 (3)	2.8004 (17)	177 (3)
O4—H4A···O12B^v	0.77 (2)	2.10 (2)	2.743 (5)	141.3 (18)
O4—H4A···O13A^v	0.77 (2)	2.16 (2)	2.9102 (18)	165.7 (19)
O4—H4B···O7^ix	0.68 (3)	2.13 (3)	2.7881 (17)	165 (3)
O5—H5A···O12A^vii	0.835 (18)	1.974 (18)	2.7906 (15)	165.7 (16)
O5—H5A···O12B^vii	0.835 (18)	2.013 (19)	2.820 (6)	162.4 (16)
O5—H5B···O10^x	0.777 (18)	2.042 (19)	2.8075 (15)	168.4 (17)
O6—H6B···O11^xi	0.778 (17)	2.168 (17)	2.9360 (14)	169.3 (16)
O6—H6A···O9^xii	0.849 (18)	2.013 (19)	2.8601 (15)	175.3 (16)
O7—H7A···O13B^i	0.774 (18)	2.285 (19)	2.899 (7)	136.9 (16)
O7—H7A···O14A^i	0.774 (18)	2.003 (19)	2.7623 (17)	166.6 (18)
O7—H7A···O14B^i	0.774 (18)	2.64 (2)	3.388 (7)	163.7 (17)
O7—H7B···O4^ix	0.69 (3)	2.11 (3)	2.7881 (17)	166 (3)
O7—H7C···O4	1.28 (4)	1.50 (4)	2.7657 (16)	169 (3)
O8—H8A···O3^xiii	0.65 (4)	2.16 (4)	2.8004 (17)	168 (4)
O8—H8B···O11^i	0.836 (17)	1.951 (18)	2.7776 (14)	169.6 (15)
O8—H8C···O3^ii	1.09 (4)	1.70 (4)	2.7534 (16)	159 (3)
O9—H9A···O14A^xiv	0.843 (19)	1.979 (19)	2.8031 (19)	165.7 (16)
O9—H9A···O14B^xiv	0.843 (19)	1.98 (2)	2.824 (8)	174.4 (17)
O9—H9B···O11^xv	0.693 (18)	2.124 (19)	2.8170 (16)	178 (2)
O10—H10A···O13A^xi	0.859 (19)	1.98 (2)	2.8244 (17)	168.3 (16)
O10—H10A···O13B^xi	0.859 (19)	1.93 (2)	2.725 (7)	153.2 (17)
O10—H10B···O14A^xiii	0.679 (18)	2.150 (19)	2.827 (2)	175 (2)
O10—H10B···O14B^xiii	0.679 (18)	2.14 (2)	2.806 (9)	167 (2)

Symmetry codes: (i) x, −y+3/2, z−1/2; (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, z−1; (vi) x, y, z−1; (vii) x, −y+1/2, z−1/2; (viii) −x+1, y−1/2, −z+1/2; (ix) −x, −y+2, −z; (x) x−1, 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.