Buy article online - an online subscription or single-article purchase is required to access this article.
The crystal structures of the two hydrates Na
2SeO
4·10H
2O and Na
2SeO
4·7.5H
2O are studied for the first time. The structures of Na
2SO
4·10H
2O and Na
2SO
4·7H
2O 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 Na
2SO
4·10H
2O, 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 (Na
2SO
4·7H
2O, tetragonal, space group
P4
12
12 and Na
2SeO
4·7.5H
2O, 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
CCDC references: 995680; 995681; 995682; 995683; 995684
Crystal data, data collection and structure refinement details are summarized
in Table 1.
S2. Results and discussion
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.
(Na2_Se04_75H2O_120k) Sodium selenate heptahemihydrate
top
Crystal data top
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) Å3 | Monoclinic prism, colourless |
Z = 8 | 0.25 × 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 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 top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.026 | All 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 reflections | Δρmax = 0.49 e Å−3 |
192 parameters | Δρmin = −1.03 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00151 (17) |
Crystal data top
H15Na2O11.50Se | V = 2462.6 (12) Å3 |
Mr = 324.06 | Z = 8 |
Monoclinic, C2/c | Mo Kα radiation |
a = 25.082 (7) Å | µ = 3.16 mm−1 |
b = 7.2222 (13) Å | T = 120 K |
c = 14.148 (5) Å | 0.25 × 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 = 0.536 | Rint = 0.107 |
51914 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.026 | 0 restraints |
wR(F2) = 0.079 | All H-atom parameters refined |
S = 1.00 | Δρmax = 0.49 e Å−3 |
4234 reflections | Δρmin = −1.03 e Å−3 |
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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
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—O2iv | 2.4853 (15) |
Na1—O5 | 2.4124 (17) | Na2—O4 | 2.5129 (16) |
Na1—O8i | 2.4147 (15) | Na2—Na2iii | 3.4306 (18) |
Na1—O6 | 2.4201 (15) | Na2—Na2iv | 3.7379 (18) |
Na1—O6ii | 2.4286 (15) | O1—Na2iii | 2.4774 (15) |
Na1—O7 | 2.4377 (17) | O2—Na2iv | 2.4853 (15) |
Na1—O8 | 2.4483 (15) | O4—Na2iii | 2.4034 (16) |
Na1—Na1ii | 3.6163 (7) | O6—Na1i | 2.4286 (15) |
Na1—Na1i | 3.6164 (6) | O8—Na1ii | 2.4147 (15) |
Na2—O4iii | 2.4034 (16) | | |
| | | |
O12—Se1—O11 | 109.30 (5) | O4iii—Na2—O3 | 154.68 (5) |
O12—Se1—O9 | 109.51 (6) | O4iii—Na2—O2 | 95.13 (5) |
O11—Se1—O9 | 109.15 (6) | O3—Na2—O2 | 80.64 (5) |
O12—Se1—O10 | 109.22 (6) | O4iii—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—O8i | 99.02 (5) | O4iii—Na2—O2iv | 124.52 (5) |
O5—Na1—O6 | 97.72 (6) | O3—Na2—O2iv | 79.87 (5) |
O8i—Na1—O6 | 84.12 (5) | O2—Na2—O2iv | 81.91 (6) |
O5—Na1—O6ii | 86.87 (5) | O1—Na2—O2iv | 92.59 (5) |
O8i—Na1—O6ii | 95.48 (5) | O4iii—Na2—O4 | 76.47 (6) |
O6—Na1—O6ii | 175.40 (3) | O3—Na2—O4 | 82.35 (5) |
O5—Na1—O7 | 177.96 (6) | O2—Na2—O4 | 113.50 (5) |
O8i—Na1—O7 | 82.96 (5) | O1—Na2—O4 | 76.14 (4) |
O6—Na1—O7 | 81.97 (5) | O2iv—Na2—O4 | 154.16 (5) |
O6ii—Na1—O7 | 93.43 (5) | Na2iii—O1—Na2 | 87.64 (7) |
O5—Na1—O8 | 85.41 (5) | Na2—O2—Na2iv | 98.09 (6) |
O8i—Na1—O8 | 175.33 (4) | Na2iii—O4—Na2 | 88.47 (5) |
O6—Na1—O8 | 96.80 (5) | Na1—O6—Na1i | 96.46 (5) |
O6ii—Na1—O8 | 83.23 (5) | Na1ii—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) top
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H8B···O12v | 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···O11vi | 0.79 (4) | 2.00 (4) | 2.790 (2) | 174 (3) |
O6—H6B···O9vii | 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···O7ii | 0.79 (3) | 2.04 (3) | 2.834 (2) | 177 (3) |
O5—H5A···O3viii | 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···O10i | 0.85 (3) | 2.00 (3) | 2.8502 (17) | 172 (3) |
O3—H3B···O9ii | 0.82 (3) | 1.95 (3) | 2.7738 (17) | 175 (3) |
O3—H3A···O12i | 0.78 (3) | 2.02 (3) | 2.7897 (17) | 172 (3) |
O2—H2B···O11i | 0.80 (3) | 2.09 (3) | 2.8842 (18) | 172 (3) |
O2—H2A···O11ix | 0.78 (3) | 2.14 (3) | 2.9055 (18) | 169 (3) |
O1—H1···O10ii | 0.83 (3) | 2.01 (3) | 2.8409 (17) | 174 (3) |
O8—H8B···O12v | 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···O11vi | 0.79 (4) | 2.00 (4) | 2.790 (2) | 174 (3) |
O6—H6B···O9vii | 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···O7ii | 0.79 (3) | 2.04 (3) | 2.834 (2) | 177 (3) |
O5—H5A···O3viii | 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···O10i | 0.85 (3) | 2.00 (3) | 2.8502 (17) | 172 (3) |
O3—H3B···O9ii | 0.82 (3) | 1.95 (3) | 2.7738 (17) | 175 (3) |
O3—H3A···O12i | 0.78 (3) | 2.02 (3) | 2.7897 (17) | 172 (3) |
O2—H2B···O11i | 0.80 (3) | 2.09 (3) | 2.8842 (18) | 172 (3) |
O2—H2A···O11ix | 0.78 (3) | 2.14 (3) | 2.9055 (18) | 169 (3) |
O1—H1···O10ii | 0.83 (3) | 2.01 (3) | 2.8409 (17) | 174 (3) |
O1—H1···O10ii | 0.83 (3) | 2.01 (3) | 2.8409 (17) | 174 (3) |
O2—H2A···O11ix | 0.78 (3) | 2.14 (3) | 2.9055 (18) | 169 (3) |
O2—H2B···O11i | 0.80 (3) | 2.09 (3) | 2.8842 (18) | 172 (3) |
O3—H3A···O12i | 0.78 (3) | 2.02 (3) | 2.7897 (17) | 172 (3) |
O3—H3B···O9ii | 0.82 (3) | 1.95 (3) | 2.7738 (17) | 175 (3) |
O4—H4A···O10i | 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···O3viii | 0.87 (3) | 1.99 (3) | 2.837 (2) | 168 (3) |
O5—H5B···O7ii | 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···O9vii | 0.74 (3) | 2.11 (3) | 2.844 (2) | 172 (3) |
O7—H7A···O11vi | 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···O12v | 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
top
Crystal data top
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) Å3 | Monoclinic prism, colourless |
Z = 4 | 0.12 × 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 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 top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.024 | All 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 reflections | Δρmax = 0.54 e Å−3 |
235 parameters | Δρmin = −0.51 e Å−3 |
20 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0106 (5) |
Crystal data top
H20Na2O14Se | V = 1521.5 (3) Å3 |
Mr = 369.10 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.6498 (13) Å | µ = 2.58 mm−1 |
b = 10.5446 (9) Å | T = 200 K |
c = 13.0181 (15) Å | 0.12 × 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 = 0.780 | Rint = 0.027 |
6800 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.024 | 20 restraints |
wR(F2) = 0.061 | All H-atom parameters refined |
S = 1.06 | Δρmax = 0.54 e Å−3 |
3495 reflections | Δρmin = −0.51 e Å−3 |
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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
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—O2ii | 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—O1ii | 2.4831 (15) |
Na1—O1 | 2.4332 (14) | Na2—Na1ii | 3.5396 (10) |
Na1—O4 | 2.4619 (16) | O2—Na2i | 2.4045 (14) |
Na1—O6 | 2.4683 (15) | O1—Na2i | 2.4829 (15) |
Na1—Na2i | 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—O2ii | 171.68 (5) |
O11—Se1—O10 | 108.32 (6) | O8—Na2—O2ii | 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) | O2ii—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) | O2ii—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—O1ii | 89.92 (5) |
O2—Na1—O4 | 88.96 (5) | O8—Na2—O1ii | 86.70 (5) |
O5—Na1—O4 | 87.30 (5) | O2ii—Na2—O1ii | 84.94 (5) |
O3—Na1—O4 | 176.73 (5) | O6—Na2—O1ii | 175.86 (5) |
O1—Na1—O4 | 85.68 (5) | O5—Na2—O1ii | 94.41 (5) |
O2—Na1—O6 | 93.22 (5) | Na1—O5—Na2 | 94.87 (5) |
O5—Na1—O6 | 84.46 (5) | Na1—O2—Na2i | 95.09 (5) |
O3—Na1—O6 | 88.80 (5) | Na2—O6—Na1 | 94.18 (5) |
O1—Na1—O6 | 175.34 (5) | Na1—O1—Na2i | 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
top
Crystal data top
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) Å3 | T = 120 K |
Z = 16 | , colourless |
F(000) = 2240 | 0.53 × 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 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 top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.028 | Only 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 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) |
Crystal data top
H14Na2O11S | Z = 16 |
Mr = 268.15 | Mo Kα radiation |
Tetragonal, P41212 | µ = 0.40 mm−1 |
a = 14.3249 (15) Å | T = 120 K |
c = 22.202 (4) Å | 0.53 × 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 = 0.721 | Rint = 0.064 |
6253 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.028 | Only H-atom coordinates refined |
wR(F2) = 0.110 | Δρmax = 0.36 e Å−3 |
S = 1.06 | Δρmin = −0.40 e Å−3 |
6253 reflections | Absolute structure: 'Refined as an inversion twin.' |
340 parameters | Absolute 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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
Na1—O11 | 2.399 (3) | Na4—O15 | 2.401 (4) |
Na1—O9 | 2.414 (3) | Na4—O11iii | 2.413 (3) |
Na1—O8 | 2.426 (4) | Na4—O8iii | 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—Na1iii | 3.619 (2) |
Na1—Na2 | 3.618 (3) | S1—O23iv | 1.488 (3) |
Na1—Na4i | 3.619 (2) | S1—O23 | 1.488 (3) |
Na2—O9 | 2.391 (3) | S1—O22iv | 1.493 (3) |
Na2—O7 | 2.418 (3) | S1—O22 | 1.493 (3) |
Na2—O4 | 2.422 (3) | S2—O1v | 1.475 (3) |
Na2—O3 | 2.436 (4) | S2—O1 | 1.475 (3) |
Na2—O5 | 2.490 (3) | S2—O2v | 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—Na1v | 2.571 (2) |
Na3—O13 | 2.494 (3) | O8—Na4i | 2.421 (3) |
Na3—O10ii | 2.570 (4) | O10—Na3vi | 2.570 (4) |
Na3—Na4 | 3.618 (3) | O11—Na4i | 2.413 (3) |
Na4—O17 | 2.397 (4) | O12—Na4vii | 2.572 (2) |
| | | |
O11—Na1—O9 | 167.53 (13) | O17—Na4—O15 | 83.20 (13) |
O11—Na1—O8 | 83.01 (11) | O17—Na4—O11iii | 168.60 (13) |
O9—Na1—O8 | 95.31 (11) | O15—Na4—O11iii | 95.89 (11) |
O11—Na1—O3 | 96.12 (12) | O17—Na4—O8iii | 95.53 (12) |
O9—Na1—O3 | 83.01 (13) | O15—Na4—O8iii | 167.15 (14) |
O8—Na1—O3 | 168.28 (13) | O11iii—Na4—O8iii | 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) | O11iii—Na4—O16 | 89.17 (11) |
O3—Na1—O14 | 88.97 (10) | O8iii—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) | O11iii—Na4—O12 | 92.38 (9) |
O3—Na1—O6 | 85.48 (12) | O8iii—Na4—O12 | 85.84 (12) |
O14—Na1—O6 | 174.10 (12) | O16—Na4—O12 | 173.92 (12) |
O9—Na2—O7 | 94.44 (12) | O23iv—S1—O23 | 108.7 (2) |
O9—Na2—O4 | 167.30 (13) | O23iv—S1—O22iv | 110.09 (13) |
O7—Na2—O4 | 82.80 (12) | O23—S1—O22iv | 109.70 (19) |
O9—Na2—O3 | 84.06 (13) | O23iv—S1—O22 | 109.70 (19) |
O7—Na2—O3 | 168.21 (13) | O23—S1—O22 | 110.09 (13) |
O4—Na2—O3 | 96.10 (11) | O22iv—S1—O22 | 108.6 (2) |
O9—Na2—O5 | 78.69 (10) | O1v—S2—O1 | 108.5 (2) |
O7—Na2—O5 | 88.52 (11) | O1v—S2—O2v | 110.1 (2) |
O4—Na2—O5 | 88.82 (11) | O1—S2—O2v | 110.31 (14) |
O3—Na2—O5 | 79.71 (10) | O1v—S2—O2 | 110.31 (14) |
O9—Na2—O10 | 106.87 (10) | O1—S2—O2 | 110.1 (2) |
O7—Na2—O10 | 92.53 (11) | O2v—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—Na1v | 158.03 (18) |
O4—Na3—O13 | 79.48 (10) | Na2—O7—Na3 | 96.67 (12) |
O15—Na3—O13 | 88.89 (11) | Na4i—O8—Na1 | 96.60 (11) |
O7—Na3—O13 | 79.04 (11) | Na2—O9—Na1 | 97.70 (12) |
O17—Na3—O13 | 88.56 (10) | Na3vi—O10—Na2 | 158.12 (10) |
O4—Na3—O10ii | 106.28 (11) | Na1—O11—Na4i | 97.56 (11) |
O15—Na3—O10ii | 92.11 (11) | Na4—O12—Na4vii | 158.09 (18) |
O7—Na3—O10ii | 99.90 (12) | Na4—O15—Na3 | 97.80 (13) |
O17—Na3—O10ii | 85.76 (9) | Na4—O17—Na3 | 96.75 (13) |
O13—Na3—O10ii | 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) top
D—H···A | D—H | H···A | D···A | D—H···A |
O17—H4···O22viii | 0.77 (2) | 2.14 (3) | 2.863 (4) | 156 (3) |
O17—H5···O18ix | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O16—H2···O23viii | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O15—H6···O22x | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O14—H22···O18xi | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O13—H9···O22xii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O13—H8···O21ix | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O11—H26···O21xi | 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···O16vi | 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···O2ix | 0.80 (2) | 2.03 (2) | 2.819 (4) | 168 (3) |
O9—H19···O19v | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O8—H25···O23xiii | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O8—H24···O1ix | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O7—H12···O21v | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O7—H11···O20ix | 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···O2v | 0.82 (2) | 2.01 (2) | 2.818 (4) | 172 (3) |
O5—H16···O20v | 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···O23xii | 0.80 (2) | 2.13 (3) | 2.878 (4) | 155 (3) |
O3—H18···O19xi | 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···O22viii | 0.77 (2) | 2.14 (3) | 2.863 (4) | 156 (3) |
O17—H5···O18ix | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O16—H2···O23viii | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O15—H6···O22x | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O14—H22···O18xi | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O13—H9···O22xii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O13—H8···O21ix | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O11—H26···O21xi | 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···O16vi | 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···O2ix | 0.80 (2) | 2.03 (2) | 2.819 (4) | 168 (3) |
O9—H19···O19v | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O8—H25···O23xiii | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O8—H24···O1ix | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O7—H12···O21v | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O7—H11···O20ix | 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···O2v | 0.82 (2) | 2.01 (2) | 2.818 (4) | 172 (3) |
O5—H16···O20v | 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···O23xii | 0.80 (2) | 2.13 (3) | 2.878 (4) | 155 (3) |
O3—H18···O19xi | 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···O19xi | 0.81 (2) | 2.03 (2) | 2.795 (4) | 158 (3) |
O4—H10···O23xii | 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···O2v | 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···O20ix | 0.83 (2) | 2.00 (2) | 2.809 (4) | 168 (4) |
O7—H12···O21v | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O8—H24···O1ix | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O8—H25···O23xiii | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O9—H19···O19v | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O9—H20···O2ix | 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···O16vi | 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···O21xi | 0.78 (2) | 2.13 (3) | 2.849 (4) | 152 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O13—H8···O21ix | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O13—H9···O22xii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O14—H22···O18xi | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O15—H6···O22x | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O16—H2···O23viii | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O17—H5···O18ix | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O17—H4···O22viii | 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···O19xi | 0.81 (2) | 2.03 (2) | 2.795 (4) | 158 (3) |
O4—H10···O23xii | 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···O20v | 0.81 (2) | 2.05 (3) | 2.811 (4) | 156 (3) |
O5—H15···O2v | 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···O20ix | 0.83 (2) | 2.00 (2) | 2.809 (4) | 168 (4) |
O7—H12···O21v | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O8—H24···O1ix | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O8—H25···O23xiii | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O9—H19···O19v | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O9—H20···O2ix | 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···O16vi | 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···O21xi | 0.78 (2) | 2.13 (3) | 2.849 (4) | 152 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O13—H8···O21ix | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O13—H9···O22xii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O14—H22···O18xi | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O15—H6···O22x | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O16—H2···O23viii | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O17—H5···O18ix | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O17—H4···O22viii | 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···O19xi | 0.81 (2) | 2.03 (2) | 2.795 (4) | 158 (3) |
O4—H10···O23xii | 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···O20v | 0.81 (2) | 2.05 (3) | 2.811 (4) | 156 (3) |
O5—H15···O2v | 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···O20ix | 0.83 (2) | 2.00 (2) | 2.809 (4) | 168 (4) |
O7—H12···O21v | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O8—H24···O1ix | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O8—H25···O23xiii | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O9—H19···O19v | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O9—H20···O2ix | 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···O16vi | 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···O21xi | 0.78 (2) | 2.13 (3) | 2.849 (4) | 152 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O13—H8···O21ix | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O13—H9···O22xii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O14—H22···O18xi | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O15—H6···O22x | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O16—H2···O23viii | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O17—H5···O18ix | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O17—H4···O22viii | 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
top
Crystal data top
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) Å3 | Monoclinic prism, colourless |
Z = 4 | 0.53 × 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-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 top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.028 | All 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 reflections | Δρmax = 0.69 e Å−3 |
235 parameters | Δρmin = −0.56 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0111 (14) |
Crystal data top
H20Na2O14S | V = 1442.2 (4) Å3 |
Mr = 322.21 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.470 (2) Å | µ = 0.34 mm−1 |
b = 10.3515 (12) Å | T = 120 K |
c = 12.759 (2) Å | 0.53 × 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 = 0.796 | Rint = 0.119 |
3876 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.028 | 0 restraints |
wR(F2) = 0.076 | All H-atom parameters refined |
S = 1.05 | Δρmax = 0.69 e Å−3 |
3876 reflections | Δρmin = −0.56 e Å−3 |
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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
S1—O11 | 1.4740 (7) | Na1—Na2 | 3.5182 (7) |
S1—O12 | 1.4785 (7) | Na2—O2ii | 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—O1ii | 2.4568 (9) |
Na1—O1 | 2.4166 (9) | Na2—Na1ii | 3.4714 (7) |
Na1—O6 | 2.4431 (9) | O1—Na2i | 2.4569 (9) |
Na1—O4 | 2.4464 (9) | O2—Na2i | 2.3826 (8) |
Na1—Na2i | 3.4714 (7) | | |
| | | |
O11—S1—O12 | 109.69 (4) | O6—Na1—O4 | 90.27 (3) |
O11—S1—O13 | 109.72 (4) | O2ii—Na2—O7 | 172.68 (3) |
O12—S1—O13 | 109.22 (4) | O2ii—Na2—O8 | 92.15 (3) |
O11—S1—O10 | 108.88 (4) | O7—Na2—O8 | 93.31 (3) |
O12—S1—O10 | 109.39 (4) | O2ii—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) | O2ii—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) | O2ii—Na2—O1ii | 86.13 (3) |
O2—Na1—O6 | 92.27 (3) | O7—Na2—O1ii | 89.20 (3) |
O5—Na1—O6 | 85.77 (3) | O8—Na2—O1ii | 87.88 (3) |
O3—Na1—O6 | 88.61 (3) | O6—Na2—O1ii | 176.18 (3) |
O1—Na1—O6 | 176.08 (3) | O5—Na2—O1ii | 93.58 (3) |
O2—Na1—O4 | 90.16 (3) | Na1—O1—Na2i | 90.84 (3) |
O5—Na1—O4 | 86.78 (3) | Na1—O2—Na2i | 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)
top
Crystal data top
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) Å3 | Monoclinic prism, colourless |
Z = 4 | 0.4 × 0.3 × 0.2 mm |
Data collection top
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 top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.024 | All 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 reflections | Δρmax = 0.23 e Å−3 |
270 parameters | Δρmin = −0.31 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0161 (7) |
Crystal data top
H20Na2O14S | V = 1445.2 (4) Å3 |
Mr = 322.20 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 11.467 (2) Å | µ = 0.34 mm−1 |
b = 10.3455 (12) Å | T = 250 K |
c = 12.795 (2) Å | 0.4 × 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 = 0.934 | Rint = 0.031 |
25202 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.061 | All H-atom parameters refined |
S = 1.03 | Δρmax = 0.23 e Å−3 |
3331 reflections | Δρmin = −0.31 e Å−3 |
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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
Na1—O2 | 2.3800 (11) | Na2—Na1ii | 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—Na2i | 3.4843 (8) | S1—O12B | 1.487 (5) |
Na1—Na2 | 3.5167 (8) | S1—O13B | 1.539 (6) |
Na2—O8 | 2.3867 (12) | O1—Na2i | 2.4629 (11) |
Na2—O7 | 2.3880 (11) | O2—Na2i | 2.3891 (10) |
Na2—O2ii | 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—O1ii | 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—O2ii | 92.21 (4) | O14A—S1—O13B | 84.4 (3) |
O7—Na2—O2ii | 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) |
O2ii—Na2—O5 | 84.07 (4) | Na1—O1—Na2i | 91.02 (4) |
O8—Na2—O6 | 92.67 (4) | Na1—O2—Na2i | 93.87 (4) |
O7—Na2—O6 | 86.92 (4) | Na1—O5—Na2 | 93.78 (4) |
O2ii—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—O1ii | 88.59 (4) | O12A—O12B—S1 | 73.0 (4) |
O7—Na2—O1ii | 89.69 (4) | O13B—O13A—S1 | 81.3 (5) |
O2ii—Na2—O1ii | 85.84 (4) | O13A—O13B—S1 | 69.3 (4) |
O5—Na2—O1ii | 93.49 (4) | O14B—O14A—S1 | 78.3 (8) |
O6—Na2—O1ii | 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) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O10iii | 0.823 (17) | 2.045 (18) | 2.8672 (15) | 176.9 (15) |
O1—H1B···O13Aiv | 0.834 (17) | 2.081 (17) | 2.9033 (17) | 168.5 (15) |
O1—H1B···O13Biv | 0.834 (17) | 2.152 (18) | 2.978 (6) | 170.5 (15) |
O2—H2A···O12Av | 0.801 (17) | 2.005 (18) | 2.7842 (15) | 164.2 (17) |
O2—H2A···O12Bv | 0.801 (17) | 2.008 (19) | 2.770 (6) | 158.7 (16) |
O2—H2B···O9vi | 0.765 (18) | 2.028 (19) | 2.7878 (15) | 171.5 (18) |
O3—H3A···O12Avii | 0.710 (19) | 2.121 (19) | 2.7938 (18) | 158.5 (19) |
O3—H3A···O14Bvii | 0.710 (19) | 2.25 (2) | 2.875 (7) | 147.3 (19) |
O3—H3B···O8viii | 0.74 (3) | 2.07 (3) | 2.8004 (17) | 177 (3) |
O4—H4A···O12Bv | 0.77 (2) | 2.10 (2) | 2.743 (5) | 141.3 (18) |
O4—H4A···O13Av | 0.77 (2) | 2.16 (2) | 2.9102 (18) | 165.7 (19) |
O4—H4B···O7ix | 0.68 (3) | 2.13 (3) | 2.7881 (17) | 165 (3) |
O5—H5A···O12Avii | 0.835 (18) | 1.974 (18) | 2.7906 (15) | 165.7 (16) |
O5—H5A···O12Bvii | 0.835 (18) | 2.013 (19) | 2.820 (6) | 162.4 (16) |
O5—H5B···O10x | 0.777 (18) | 2.042 (19) | 2.8075 (15) | 168.4 (17) |
O6—H6B···O11xi | 0.778 (17) | 2.168 (17) | 2.9360 (14) | 169.3 (16) |
O6—H6A···O9xii | 0.849 (18) | 2.013 (19) | 2.8601 (15) | 175.3 (16) |
O7—H7A···O13Bi | 0.774 (18) | 2.285 (19) | 2.899 (7) | 136.9 (16) |
O7—H7A···O14Ai | 0.774 (18) | 2.003 (19) | 2.7623 (17) | 166.6 (18) |
O7—H7A···O14Bi | 0.774 (18) | 2.64 (2) | 3.388 (7) | 163.7 (17) |
O7—H7B···O4ix | 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···O3xiii | 0.65 (4) | 2.16 (4) | 2.8004 (17) | 168 (4) |
O8—H8B···O11i | 0.836 (17) | 1.951 (18) | 2.7776 (14) | 169.6 (15) |
O8—H8C···O3ii | 1.09 (4) | 1.70 (4) | 2.7534 (16) | 159 (3) |
O9—H9A···O14Axiv | 0.843 (19) | 1.979 (19) | 2.8031 (19) | 165.7 (16) |
O9—H9A···O14Bxiv | 0.843 (19) | 1.98 (2) | 2.824 (8) | 174.4 (17) |
O9—H9B···O11xv | 0.693 (18) | 2.124 (19) | 2.8170 (16) | 178 (2) |
O10—H10A···O13Axi | 0.859 (19) | 1.98 (2) | 2.8244 (17) | 168.3 (16) |
O10—H10A···O13Bxi | 0.859 (19) | 1.93 (2) | 2.725 (7) | 153.2 (17) |
O10—H10B···O14Axiii | 0.679 (18) | 2.150 (19) | 2.827 (2) | 175 (2) |
O10—H10B···O14Bxiii | 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. |
Experimental details
| (Na2_Se04_75H2O_120k) | (Na2_SO_4_7H2O_120k) |
Crystal data |
Chemical formula | H15Na2O11.50Se | H14Na2O11S |
Mr | 324.06 | 268.15 |
Crystal system, space group | Monoclinic, C2/c | Tetragonal, P41212 |
Temperature (K) | 120 | 120 |
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), 90 | 90, 90, 90 |
V (Å3) | 2462.6 (12) | 4556.0 (10) |
Z | 8 | 16 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 3.16 | 0.40 |
Crystal size (mm) | 0.25 × 0.18 × 0.11 | 0.53 × 0.48 × 0.44 |
|
Data collection |
Diffractometer | STOE IPDS 2T diffractometer | STOE IPDS 2 diffractometer |
Absorption correction | Integration Coppens (1970) | Integration Coppens (1970) |
Tmin, Tmax | 0.292, 0.536 | 0.529, 0.721 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 51914, 4234, 3466 | 6253, 6253, 3969 |
Rint | 0.107 | 0.064 |
(sin θ/λ)max (Å−1) | 0.745 | 0.690 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.079, 1.00 | 0.028, 0.110, 1.06 |
No. of reflections | 4234 | 6253 |
No. of parameters | 192 | 340 |
No. of restraints | 0 | 39 |
H-atom treatment | All H-atom parameters refined | Only H-atom coordinates refined |
Δρmax, Δρmin (e Å−3) | 0.49, −1.03 | 0.36, −0.40 |
Absolute structure | ? | 'Refined as an inversion twin.' |
Absolute structure parameter | ? | 0.46 (19) |
Hydrogen-bond geometry (Å, º) for (Na2_Se04_75H2O_120k) top
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H8B···O12i | 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···O11ii | 0.79 (4) | 2.00 (4) | 2.790 (2) | 174 (3) |
O6—H6B···O9iii | 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···O7iv | 0.79 (3) | 2.04 (3) | 2.834 (2) | 177 (3) |
O5—H5A···O3v | 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···O10vi | 0.85 (3) | 2.00 (3) | 2.8502 (17) | 172 (3) |
O3—H3B···O9iv | 0.82 (3) | 1.95 (3) | 2.7738 (17) | 175 (3) |
O3—H3A···O12vi | 0.78 (3) | 2.02 (3) | 2.7897 (17) | 172 (3) |
O2—H2B···O11vi | 0.80 (3) | 2.09 (3) | 2.8842 (18) | 172 (3) |
O2—H2A···O11vii | 0.78 (3) | 2.14 (3) | 2.9055 (18) | 169 (3) |
O1—H1···O10iv | 0.83 (3) | 2.01 (3) | 2.8409 (17) | 174 (3) |
O8—H8B···O12i | 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···O11ii | 0.79 (4) | 2.00 (4) | 2.790 (2) | 174 (3) |
O6—H6B···O9iii | 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···O7iv | 0.79 (3) | 2.04 (3) | 2.834 (2) | 177 (3) |
O5—H5A···O3v | 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···O10vi | 0.85 (3) | 2.00 (3) | 2.8502 (17) | 172 (3) |
O3—H3B···O9iv | 0.82 (3) | 1.95 (3) | 2.7738 (17) | 175 (3) |
O3—H3A···O12vi | 0.78 (3) | 2.02 (3) | 2.7897 (17) | 172 (3) |
O2—H2B···O11vi | 0.80 (3) | 2.09 (3) | 2.8842 (18) | 172 (3) |
O2—H2A···O11vii | 0.78 (3) | 2.14 (3) | 2.9055 (18) | 169 (3) |
O1—H1···O10iv | 0.83 (3) | 2.01 (3) | 2.8409 (17) | 174 (3) |
O1—H1···O10iv | 0.83 (3) | 2.01 (3) | 2.8409 (17) | 174 (3) |
O2—H2A···O11vii | 0.78 (3) | 2.14 (3) | 2.9055 (18) | 169 (3) |
O2—H2B···O11vi | 0.80 (3) | 2.09 (3) | 2.8842 (18) | 172 (3) |
O3—H3A···O12vi | 0.78 (3) | 2.02 (3) | 2.7897 (17) | 172 (3) |
O3—H3B···O9iv | 0.82 (3) | 1.95 (3) | 2.7738 (17) | 175 (3) |
O4—H4A···O10vi | 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···O3v | 0.87 (3) | 1.99 (3) | 2.837 (2) | 168 (3) |
O5—H5B···O7iv | 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···O9iii | 0.74 (3) | 2.11 (3) | 2.844 (2) | 172 (3) |
O7—H7A···O11ii | 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···O12i | 0.76 (3) | 2.12 (3) | 2.880 (2) | 172 (3) |
Symmetry codes: (i) −x+1/2, −y+3/2, −z+1; (ii) x, −y+1, z−1/2; (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, y−1/2, −z+1/2; (vii) x+1/2, −y+1/2, z−1/2. |
Hydrogen-bond geometry (Å, º) for (Na2_SO_4_7H2O_120k) top
D—H···A | D—H | H···A | D···A | D—H···A |
O17—H4···O22i | 0.77 (2) | 2.14 (3) | 2.863 (4) | 156 (3) |
O17—H5···O18ii | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O16—H2···O23i | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O15—H6···O22iv | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O14—H22···O18v | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O13—H9···O22vii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O13—H8···O21ii | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O11—H26···O21v | 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···O16vi | 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···O2ii | 0.80 (2) | 2.03 (2) | 2.819 (4) | 168 (3) |
O9—H19···O19viii | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O8—H25···O23ix | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O8—H24···O1ii | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O7—H12···O21viii | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O7—H11···O20ii | 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···O2viii | 0.82 (2) | 2.01 (2) | 2.818 (4) | 172 (3) |
O5—H16···O20viii | 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···O23vii | 0.80 (2) | 2.13 (3) | 2.878 (4) | 155 (3) |
O3—H18···O19v | 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···O22i | 0.77 (2) | 2.14 (3) | 2.863 (4) | 156 (3) |
O17—H5···O18ii | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O16—H2···O23i | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O15—H6···O22iv | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O14—H22···O18v | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O13—H9···O22vii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O13—H8···O21ii | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O11—H26···O21v | 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···O16vi | 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···O2ii | 0.80 (2) | 2.03 (2) | 2.819 (4) | 168 (3) |
O9—H19···O19viii | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O8—H25···O23ix | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O8—H24···O1ii | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O7—H12···O21viii | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O7—H11···O20ii | 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···O2viii | 0.82 (2) | 2.01 (2) | 2.818 (4) | 172 (3) |
O5—H16···O20viii | 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···O23vii | 0.80 (2) | 2.13 (3) | 2.878 (4) | 155 (3) |
O3—H18···O19v | 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···O19v | 0.81 (2) | 2.03 (2) | 2.795 (4) | 158 (3) |
O4—H10···O23vii | 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···O2viii | 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···O20ii | 0.83 (2) | 2.00 (2) | 2.809 (4) | 168 (4) |
O7—H12···O21viii | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O8—H24···O1ii | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O8—H25···O23ix | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O9—H19···O19viii | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O9—H20···O2ii | 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···O16vi | 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···O21v | 0.78 (2) | 2.13 (3) | 2.849 (4) | 152 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O13—H8···O21ii | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O13—H9···O22vii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O14—H22···O18v | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O15—H6···O22iv | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O16—H2···O23i | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O17—H5···O18ii | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O17—H4···O22i | 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···O19v | 0.81 (2) | 2.03 (2) | 2.795 (4) | 158 (3) |
O4—H10···O23vii | 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···O20viii | 0.81 (2) | 2.05 (3) | 2.811 (4) | 156 (3) |
O5—H15···O2viii | 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···O20ii | 0.83 (2) | 2.00 (2) | 2.809 (4) | 168 (4) |
O7—H12···O21viii | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O8—H24···O1ii | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O8—H25···O23ix | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O9—H19···O19viii | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O9—H20···O2ii | 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···O16vi | 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···O21v | 0.78 (2) | 2.13 (3) | 2.849 (4) | 152 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O13—H8···O21ii | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O13—H9···O22vii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O14—H22···O18v | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O15—H6···O22iv | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O16—H2···O23i | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O17—H5···O18ii | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O17—H4···O22i | 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···O19v | 0.81 (2) | 2.03 (2) | 2.795 (4) | 158 (3) |
O4—H10···O23vii | 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···O20viii | 0.81 (2) | 2.05 (3) | 2.811 (4) | 156 (3) |
O5—H15···O2viii | 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···O20ii | 0.83 (2) | 2.00 (2) | 2.809 (4) | 168 (4) |
O7—H12···O21viii | 0.82 (2) | 2.04 (3) | 2.802 (4) | 153 (3) |
O8—H24···O1ii | 0.82 (2) | 2.03 (2) | 2.853 (4) | 177 (3) |
O8—H25···O23ix | 0.84 (2) | 2.01 (3) | 2.770 (4) | 150 (3) |
O9—H19···O19viii | 0.80 (2) | 2.07 (2) | 2.825 (4) | 158 (3) |
O9—H20···O2ii | 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···O16vi | 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···O21v | 0.78 (2) | 2.13 (3) | 2.849 (4) | 152 (4) |
O12—H3···O14iii | 0.82 (2) | 2.06 (2) | 2.883 (3) | 171 (4) |
O13—H8···O21ii | 0.85 (3) | 1.95 (3) | 2.799 (4) | 172 (4) |
O13—H9···O22vii | 0.90 (4) | 1.99 (3) | 2.820 (4) | 152 (3) |
O14—H21···O1vi | 0.85 (2) | 1.94 (2) | 2.790 (4) | 174 (3) |
O14—H22···O18v | 0.83 (2) | 2.04 (2) | 2.825 (4) | 157 (3) |
O15—H6···O22iv | 0.81 (2) | 2.01 (3) | 2.785 (4) | 159 (3) |
O15—H7···O18iii | 0.81 (2) | 2.04 (2) | 2.829 (4) | 163 (3) |
O16—H1···O19iii | 0.82 (2) | 2.00 (2) | 2.825 (4) | 178 (4) |
O16—H2···O23i | 0.82 (2) | 2.03 (3) | 2.791 (4) | 154 (3) |
O17—H5···O18ii | 0.81 (2) | 2.05 (2) | 2.850 (4) | 167 (3) |
O17—H4···O22i | 0.77 (2) | 2.14 (3) | 2.863 (4) | 156 (3) |
Symmetry codes: (i) y+1, x, −z+1; (ii) −x+3/2, y−1/2, −z+1/4; (iii) x+1, y, z; (iv) −y+3/2, x+1/2, z−3/4; (v) −y+3/2, x+1/2, z+1/4; (vi) −y+3/2, x−1/2, z+1/4; (vii) −x+3/2, y+1/2, −z+5/4; (viii) y, x, −z; (ix) x, y, z−1. |
Hydrogen-bond geometry (Å, º) for (Na2_SO4_10H2O_250k) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O10i | 0.823 (17) | 2.045 (18) | 2.8672 (15) | 176.9 (15) |
O1—H1B···O13Aii | 0.834 (17) | 2.081 (17) | 2.9033 (17) | 168.5 (15) |
O1—H1B···O13Bii | 0.834 (17) | 2.152 (18) | 2.978 (6) | 170.5 (15) |
O2—H2A···O12Aiii | 0.801 (17) | 2.005 (18) | 2.7842 (15) | 164.2 (17) |
O2—H2A···O12Biii | 0.801 (17) | 2.008 (19) | 2.770 (6) | 158.7 (16) |
O2—H2B···O9iv | 0.765 (18) | 2.028 (19) | 2.7878 (15) | 171.5 (18) |
O3—H3A···O12Av | 0.710 (19) | 2.121 (19) | 2.7938 (18) | 158.5 (19) |
O3—H3A···O14Bv | 0.710 (19) | 2.25 (2) | 2.875 (7) | 147.3 (19) |
O3—H3B···O8vi | 0.74 (3) | 2.07 (3) | 2.8004 (17) | 177 (3) |
O4—H4A···O12Biii | 0.77 (2) | 2.10 (2) | 2.743 (5) | 141.3 (18) |
O4—H4A···O13Aiii | 0.77 (2) | 2.16 (2) | 2.9102 (18) | 165.7 (19) |
O4—H4B···O7vii | 0.68 (3) | 2.13 (3) | 2.7881 (17) | 165 (3) |
O5—H5A···O12Av | 0.835 (18) | 1.974 (18) | 2.7906 (15) | 165.7 (16) |
O5—H5A···O12Bv | 0.835 (18) | 2.013 (19) | 2.820 (6) | 162.4 (16) |
O5—H5B···O10viii | 0.777 (18) | 2.042 (19) | 2.8075 (15) | 168.4 (17) |
O6—H6B···O11ix | 0.778 (17) | 2.168 (17) | 2.9360 (14) | 169.3 (16) |
O6—H6A···O9x | 0.849 (18) | 2.013 (19) | 2.8601 (15) | 175.3 (16) |
O7—H7A···O13Bxi | 0.774 (18) | 2.285 (19) | 2.899 (7) | 136.9 (16) |
O7—H7A···O14Axi | 0.774 (18) | 2.003 (19) | 2.7623 (17) | 166.6 (18) |
O7—H7A···O14Bxi | 0.774 (18) | 2.64 (2) | 3.388 (7) | 163.7 (17) |
O7—H7B···O4vii | 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···O3xii | 0.65 (4) | 2.16 (4) | 2.8004 (17) | 168 (4) |
O8—H8B···O11xi | 0.836 (17) | 1.951 (18) | 2.7776 (14) | 169.6 (15) |
O8—H8C···O3xiii | 1.09 (4) | 1.70 (4) | 2.7534 (16) | 159 (3) |
O9—H9A···O14Axiv | 0.843 (19) | 1.979 (19) | 2.8031 (19) | 165.7 (16) |
O9—H9A···O14Bxiv | 0.843 (19) | 1.98 (2) | 2.824 (8) | 174.4 (17) |
O9—H9B···O11xv | 0.693 (18) | 2.124 (19) | 2.8170 (16) | 178 (2) |
O10—H10A···O13Aix | 0.859 (19) | 1.98 (2) | 2.8244 (17) | 168.3 (16) |
O10—H10A···O13Bix | 0.859 (19) | 1.93 (2) | 2.725 (7) | 153.2 (17) |
O10—H10B···O14Axii | 0.679 (18) | 2.150 (19) | 2.827 (2) | 175 (2) |
O10—H10B···O14Bxii | 0.679 (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, z−1; (iv) x, y, z−1; (v) x, −y+1/2, z−1/2; (vi) −x+1, y−1/2, −z+1/2; (vii) −x, −y+2, −z; (viii) x−1, y, z; (ix) −x+1, −y+1, −z+1; (x) −x+1, −y+2, −z+1; (xi) x, −y+3/2, z−1/2; (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. |
Subscribe to Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.