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Calcium disodium hexa­thio­diphosphate(IV) octa­hydrate

aInstitute of Inorganic and Analytical Chemistry, Clausthal University of Technology, Paul-Ernst-Strasse 4, 38678 Clausthal-Zellerfeld, Germany
*Correspondence e-mail: mimoza.gjikaj@tu-clausthal.de

(Received 11 June 2010; accepted 28 June 2010; online 3 July 2010)

Single crystals of the title compound, CaNa2(P2S6)·8H2O, were obtained by adding calcium hydroxide to an aqueous solution of Na4(P2S6)·6H2O. The structure is isotypic with that of its strontium analogue and consists of one Ca2+ cation, two Na+ cations, one-half of a centrosymmetric (P2S6)4− anion with staggered confirmation and four water mol­ecules in the asymmetric unit. The crystal structure can be described as being built up from layers of cations and anions extending parallel to (101). Within a layer, each CaO8 polyhedron is connected via edge-sharing to two NaO4S2 octa­hedra and to one NaO2S4 octa­edron. The NaO4S2 octa­hedra are, in turn, linked with two (P2S6)4− anions through common corners. Various O—H⋯S hydrogen-bonding inter­actions lead to cohesion of adjacent layers. The Ca2+ and one Na+ cation are situated on a twofold rotation axis and the second Na+ cation is situated on an inversion centre.

Related literature

For background to thio­diphosphates(IV), including their crystal structures, see: Jörgens et al. (2003[Jörgens, S., Mewis, A., Hoffmann, R.-D., Pöttgen, R. & Mosel, B. D. (2003). Z. Anorg. Allg. Chem. 629, 429-433.]); Klingen et al. (1973[Klingen, W., Ott, R. & Hahn, H. (1973). Z. Anorg. Allg. Chem. 396, 271-278.]). For the synthesis of Na4(P2S6)·6H2O, see: Fincher et al. (1998[Fincher, T., LeBret, G. & Cleary, D. A. (1998). J. Solid State Chem. 141, 274-281.]). For the isotypic structure of SrNa2(P2S6)·8H2O, see: Gjikaj & Ehrhardt (2010[Ehrhardt, C. & Gjikaj, M. (2010). Acta Cryst. E66, i55.]).

Experimental

Crystal data
  • CaNa2(P2S6)·8H2O

  • Mr = 484.49

  • Monoclinic, C 2/c

  • a = 14.702 (2) Å

  • b = 9.3081 (14) Å

  • c = 14.052 (2) Å

  • β = 115.383 (11)°

  • V = 1737.3 (4) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 1.34 mm−1

  • T = 223 K

  • 0.29 × 0.24 × 0.23 mm

Data collection
  • Stoe IPDS 2 diffractometer

  • 15223 measured reflections

  • 2650 independent reflections

  • 2369 reflections with I > 2σ(I)

  • Rint = 0.050

Refinement
  • R[F2 > 2σ(F2)] = 0.029

  • wR(F2) = 0.065

  • S = 1.13

  • 2650 reflections

  • 122 parameters

  • All H-atom parameters refined

  • Δρmax = 0.68 e Å−3

  • Δρmin = −0.53 e Å−3

Table 1
Selected bond lengths (Å)

Ca—O1 2.4244 (14)
Ca—O2 2.4614 (13)
Ca—O3 2.5123 (13)
Ca—O4 2.5249 (13)
Na1—O3 2.3523 (14)
Na1—O4 2.3713 (13)
Na1—S2i 2.9768 (5)
Na2—O2 2.5282 (17)
Na2—S1i 2.9242 (8)
Na2—S3 2.9673 (7)
P—S1 2.0156 (6)
P—S2 2.0241 (6)
P—S3 2.0282 (6)
P—Pi 2.2381 (8)
Symmetry code: (i) [-x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z].

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O1—H1A⋯S3ii 0.78 (5) 2.58 (5) 3.2922 (17) 153 (4)
O1—H1B⋯S2iii 0.79 (4) 2.62 (4) 3.2892 (16) 144 (4)
O2—H2A⋯S2ii 0.79 (3) 2.54 (3) 3.3270 (15) 172 (3)
O2—H2B⋯S2i 0.88 (3) 2.30 (3) 3.1877 (15) 179 (3)
O3—H3A⋯S1iv 0.78 (3) 2.43 (3) 3.1908 (15) 168 (2)
O3—H3B⋯S1ii 0.86 (3) 2.39 (3) 3.2174 (14) 161 (3)
O4—H4A⋯S3v 0.85 (3) 2.41 (3) 3.2468 (14) 171 (3)
O4—H4B⋯S3 0.83 (3) 2.37 (3) 3.1957 (14) 171 (3)
Symmetry codes: (i) [-x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z]; (ii) [x+{\script{1\over 2}}, y-{\script{1\over 2}}, z]; (iii) [-x+1, y-1, -z+{\script{1\over 2}}]; (iv) [-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]; (v) [-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}].

Data collection: X-AREA (Stoe & Cie, 2008[Stoe & Cie (2008). X-AREA. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2004[Brandenburg, K. (2004). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

Alkaline earth hypothiodiphosphates were first reported by Klingen et al. (1973). The structure of the title compound is isotypic with that of the strontium analogue, SrNa2(P2S6).8H2O (Ehrhardt & Gjikaj, 2010). The asymmetric unit of CaNa2(P2S6).8H2O contains one Ca2+ cation, two Na+ cations, one half of a (P2S6)4- anion in staggered conformation and four water molecules (Fig. 1).

Na(1) is octahedrally coordinated by four H2O molecules and two sulfur atoms of two (P2S6)4- anions (Fig 2). Na(2) is also octahedrally coordinated by two H2O molecules and four sulfur atoms of two (P2S6)4- anions (Fig. 3). The calcium cation is eightfold coordinated by water O atoms. The [CaO8] coordination polyhedron can be described as a bicapped trigonal prism. The crystal structure is built up from layers extending parallel to (101). These layers consists of edge-sharing CaO8 and Na(1)O4S2 polyedra, CaO8 and Na(2)O2S4 polyhadra, as well as corner-sharing Na(1)O4S2 and (P2S6)4- polyhedra.

The staggered (P2S6)4- anion is located on a centre of inversion, with a P—P distance of 2.2381 (8) Å. The P—P central bond links two PS3 groups with P—S distances ranging from 2.0156 (6) to 2.0282 (6) Å. These values agree well with those reported previously for another hypothiodiphosphate structure (Jörgens et al., 2003).

Neighbouring layers are held together by various O—H···S hydrogen bonding interactions. The donor—acceptor distances between O atoms of water molecules and S atoms of (P2S6)4- units range from 3.188 to 3.327 Å (Table 2).

Related literature top

For background to thiodiphosphates(IV), including their crystal structures, see: Jörgens et al. (2003); Klingen et al. (1973). For the synthesis of Na4P2S6.6H2O, see: Fincher et al. (1998). For the isotypic structure of SrNa2(P2S6).8H2O, see: Ehrhardt & Gjikaj (2010).

Experimental top

Na4(P2S6).6H2O has been prepared according to Fincher et al. (1998). The new ternary calcium disodium hexathiodiphosphate octahydrate was obtained by adding calcium hydroxide (2 mmol, 0.148 g) to a solution of Na4(P2S6).6H2O (2 mmol, 0.910 g) in 40 ml distilled water at 333 K. Slow cooling to room temperature yielded colorless crystals of the title compound within some days.

Refinement top

Hydrogen atoms were found from the difference Fourier map and were refined independently from their respective oxygen atoms with individual isotropic displacement parameters.

Structure description top

Alkaline earth hypothiodiphosphates were first reported by Klingen et al. (1973). The structure of the title compound is isotypic with that of the strontium analogue, SrNa2(P2S6).8H2O (Ehrhardt & Gjikaj, 2010). The asymmetric unit of CaNa2(P2S6).8H2O contains one Ca2+ cation, two Na+ cations, one half of a (P2S6)4- anion in staggered conformation and four water molecules (Fig. 1).

Na(1) is octahedrally coordinated by four H2O molecules and two sulfur atoms of two (P2S6)4- anions (Fig 2). Na(2) is also octahedrally coordinated by two H2O molecules and four sulfur atoms of two (P2S6)4- anions (Fig. 3). The calcium cation is eightfold coordinated by water O atoms. The [CaO8] coordination polyhedron can be described as a bicapped trigonal prism. The crystal structure is built up from layers extending parallel to (101). These layers consists of edge-sharing CaO8 and Na(1)O4S2 polyedra, CaO8 and Na(2)O2S4 polyhadra, as well as corner-sharing Na(1)O4S2 and (P2S6)4- polyhedra.

The staggered (P2S6)4- anion is located on a centre of inversion, with a P—P distance of 2.2381 (8) Å. The P—P central bond links two PS3 groups with P—S distances ranging from 2.0156 (6) to 2.0282 (6) Å. These values agree well with those reported previously for another hypothiodiphosphate structure (Jörgens et al., 2003).

Neighbouring layers are held together by various O—H···S hydrogen bonding interactions. The donor—acceptor distances between O atoms of water molecules and S atoms of (P2S6)4- units range from 3.188 to 3.327 Å (Table 2).

For background to thiodiphosphates(IV), including their crystal structures, see: Jörgens et al. (2003); Klingen et al. (1973). For the synthesis of Na4P2S6.6H2O, see: Fincher et al. (1998). For the isotypic structure of SrNa2(P2S6).8H2O, see: Ehrhardt & Gjikaj (2010).

Computing details top

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2004); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The crystal structure of CaNa2(P2S6).8H2O in a projection along [010].
[Figure 2] Fig. 2. Coordination of Na1 with the atom labelling scheme. The displacement ellipsoids are drawn at the 50% probability level. Symmetry codes as in Table 1. H atoms are represented as spheres of arbirtary radius.
[Figure 3] Fig. 3. View of the edge-shared CaO8 and Na(2)O2S4 polyhedra with the atom labelling scheme. The displacement ellipsoids are drawn at the 50% probability level. Symmetry codes as in Table 1. H atoms are represented as spheres of arbirtary radius.
Calcium disodium hexathiodiphosphate(IV) octahydrate top
Crystal data top
CaNa2(P2S6)·8H2OF(000) = 992
Mr = 484.49Dx = 1.852 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 15599 reflections
a = 14.702 (2) Åθ = 1.0–30.5°
b = 9.3081 (14) ŵ = 1.34 mm1
c = 14.052 (2) ÅT = 223 K
β = 115.383 (11)°Block, colorless
V = 1737.3 (4) Å30.29 × 0.24 × 0.23 mm
Z = 4
Data collection top
Stoe IPDS 2
diffractometer
2369 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.050
Graphite monochromatorθmax = 30.5°, θmin = 2.7°
ω–scansh = 2020
15223 measured reflectionsk = 1313
2650 independent reflectionsl = 2017
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.029All H-atom parameters refined
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0256P)2 + 2.2311P]
where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max < 0.001
2650 reflectionsΔρmax = 0.68 e Å3
122 parametersΔρmin = 0.53 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0046 (3)
Crystal data top
CaNa2(P2S6)·8H2OV = 1737.3 (4) Å3
Mr = 484.49Z = 4
Monoclinic, C2/cMo Kα radiation
a = 14.702 (2) ŵ = 1.34 mm1
b = 9.3081 (14) ÅT = 223 K
c = 14.052 (2) Å0.29 × 0.24 × 0.23 mm
β = 115.383 (11)°
Data collection top
Stoe IPDS 2
diffractometer
2369 reflections with I > 2σ(I)
15223 measured reflectionsRint = 0.050
2650 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0290 restraints
wR(F2) = 0.065All H-atom parameters refined
S = 1.13Δρmax = 0.68 e Å3
2650 reflectionsΔρmin = 0.53 e Å3
122 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca0.50000.24842 (5)0.25000.01531 (10)
Na10.25000.25000.00000.0240 (2)
Na20.50000.67523 (13)0.25000.0318 (2)
P0.20227 (3)0.76310 (4)0.04363 (3)0.01394 (9)
S10.06893 (3)0.67248 (4)0.04913 (3)0.02064 (10)
S20.18887 (3)0.97575 (4)0.06497 (3)0.01807 (9)
S30.27954 (3)0.66563 (4)0.18473 (3)0.02051 (10)
O10.59411 (11)0.04315 (16)0.23418 (13)0.0268 (3)
O20.50720 (10)0.45732 (14)0.14604 (10)0.0217 (2)
O30.41702 (10)0.16862 (14)0.06107 (10)0.0216 (2)
O40.31872 (9)0.32895 (14)0.17753 (10)0.0199 (2)
H1A0.629 (4)0.053 (5)0.205 (4)0.096 (15)*
H1B0.627 (3)0.002 (4)0.287 (3)0.068 (12)*
H2A0.554 (3)0.462 (3)0.133 (3)0.048 (9)*
H2B0.453 (2)0.477 (3)0.088 (3)0.045 (8)*
H3A0.4123 (19)0.085 (3)0.059 (2)0.029 (6)*
H3B0.454 (2)0.192 (3)0.030 (2)0.042 (8)*
H4A0.288 (2)0.294 (3)0.212 (3)0.049 (8)*
H4B0.306 (2)0.416 (3)0.172 (2)0.040 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca0.0144 (2)0.01655 (19)0.01458 (19)0.0000.00584 (15)0.000
Na10.0192 (5)0.0302 (5)0.0196 (5)0.0001 (4)0.0053 (4)0.0011 (4)
Na20.0283 (6)0.0396 (6)0.0249 (5)0.0000.0089 (4)0.000
P0.01509 (18)0.01411 (17)0.01436 (17)0.00019 (13)0.00797 (14)0.00016 (12)
S10.01688 (19)0.02004 (18)0.0257 (2)0.00401 (14)0.00981 (15)0.00281 (14)
S20.01954 (19)0.01504 (17)0.01967 (18)0.00092 (13)0.00844 (14)0.00104 (13)
S30.0250 (2)0.02236 (19)0.01657 (17)0.00676 (15)0.01122 (15)0.00515 (14)
O10.0201 (6)0.0272 (6)0.0298 (7)0.0039 (5)0.0075 (5)0.0023 (5)
O20.0197 (6)0.0261 (6)0.0187 (5)0.0009 (5)0.0076 (5)0.0038 (5)
O30.0241 (6)0.0203 (6)0.0227 (6)0.0002 (5)0.0124 (5)0.0026 (5)
O40.0210 (6)0.0195 (5)0.0214 (6)0.0014 (4)0.0112 (5)0.0002 (4)
Geometric parameters (Å, º) top
Ca—O12.4244 (14)Na2—S1iv2.9242 (8)
Ca—O1i2.4244 (15)Na2—S32.9673 (7)
Ca—O22.4614 (13)Na2—S3i2.9674 (7)
Ca—O2i2.4615 (13)P—S12.0156 (6)
Ca—O3i2.5122 (13)P—S22.0241 (6)
Ca—O32.5123 (13)P—S32.0282 (6)
Ca—O42.5249 (13)P—Piv2.2381 (8)
Ca—O4i2.5249 (13)S1—Na2iv2.9242 (8)
Na1—O32.3523 (14)S2—Na1vi2.9768 (5)
Na1—O3ii2.3523 (14)O1—H1A0.78 (5)
Na1—O42.3713 (13)O1—H1B0.79 (4)
Na1—O4ii2.3713 (13)O2—H2A0.79 (3)
Na1—S2iii2.9767 (5)O2—H2B0.88 (3)
Na1—S2iv2.9768 (5)O3—H3A0.78 (3)
Na2—O22.5282 (17)O3—H3B0.86 (3)
Na2—O2i2.5283 (17)O4—H4A0.85 (3)
Na2—S1v2.9242 (8)O4—H4B0.83 (3)
O1—Ca—O1i75.99 (8)O4ii—Na1—S2iii90.48 (3)
O1—Ca—O2113.37 (5)O3—Na1—S2iv89.02 (4)
O1i—Ca—O2148.04 (5)O3ii—Na1—S2iv90.98 (4)
O1—Ca—O2i148.04 (5)O4—Na1—S2iv90.48 (3)
O1i—Ca—O2i113.37 (5)O4ii—Na1—S2iv89.52 (3)
O2—Ca—O2i75.64 (6)S2iii—Na1—S2iv180.0
O1—Ca—O3i79.99 (5)O2—Na2—O2i73.30 (7)
O1i—Ca—O3i73.01 (5)O2—Na2—S1v149.72 (4)
O2—Ca—O3i137.37 (4)O2i—Na2—S1v85.08 (3)
O2i—Ca—O3i74.41 (4)O2—Na2—S1iv85.08 (3)
O1—Ca—O373.01 (5)O2i—Na2—S1iv149.72 (4)
O1i—Ca—O379.99 (5)S1v—Na2—S1iv122.01 (5)
O2—Ca—O374.42 (4)O2—Na2—S396.20 (4)
O2i—Ca—O3137.37 (4)O2i—Na2—S381.01 (4)
O3i—Ca—O3145.61 (6)S1v—Na2—S3101.16 (2)
O1—Ca—O4137.92 (5)S1iv—Na2—S380.537 (18)
O1i—Ca—O474.08 (5)O2—Na2—S3i81.01 (4)
O2—Ca—O480.36 (5)O2i—Na2—S3i96.20 (4)
O2i—Ca—O472.44 (4)S1v—Na2—S3i80.537 (17)
O3i—Ca—O4117.68 (4)S1iv—Na2—S3i101.16 (2)
O3—Ca—O473.21 (4)S3—Na2—S3i176.55 (5)
O1—Ca—O4i74.08 (5)S1—P—S2112.06 (3)
O1i—Ca—O4i137.92 (5)S1—P—S3115.28 (3)
O2—Ca—O4i72.44 (4)S2—P—S3109.99 (3)
O2i—Ca—O4i80.36 (5)S1—P—Piv105.34 (3)
O3i—Ca—O4i73.21 (4)S2—P—Piv108.14 (3)
O3—Ca—O4i117.68 (4)S3—P—Piv105.48 (3)
O4—Ca—O4i145.46 (6)P—S1—Na2iv105.07 (3)
O3—Na1—O3ii180.0P—S2—Na1vi137.04 (2)
O3—Na1—O478.97 (4)P—S3—Na2111.63 (3)
O3ii—Na1—O4101.03 (4)H1A—O1—H1B105 (4)
O3—Na1—O4ii101.03 (4)Ca—O2—Na2105.53 (5)
O3ii—Na1—O4ii78.97 (4)H2A—O2—H2B108 (3)
O4—Na1—O4ii179.999 (2)Na1—O3—Ca104.38 (5)
O3—Na1—S2iii90.98 (4)Na1—O4—Ca103.44 (5)
O3ii—Na1—S2iii89.02 (4)H4A—O4—H4B106 (3)
O4—Na1—S2iii89.52 (3)
Symmetry codes: (i) x+1, y, z+1/2; (ii) x+1/2, y+1/2, z; (iii) x, y1, z; (iv) x+1/2, y+3/2, z; (v) x+1/2, y+3/2, z+1/2; (vi) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···S3vii0.78 (5)2.58 (5)3.2922 (17)153 (4)
O1—H1B···S2viii0.79 (4)2.62 (4)3.2892 (16)144 (4)
O2—H2A···S2vii0.79 (3)2.54 (3)3.3270 (15)172 (3)
O2—H2B···S2iv0.88 (3)2.30 (3)3.1877 (15)179 (3)
O3—H3A···S1ii0.78 (3)2.43 (3)3.1908 (15)168 (2)
O3—H3B···S1vii0.86 (3)2.39 (3)3.2174 (14)161 (3)
O4—H4A···S3ix0.85 (3)2.41 (3)3.2468 (14)171 (3)
O4—H4B···S30.83 (3)2.37 (3)3.1957 (14)171 (3)
Symmetry codes: (ii) x+1/2, y+1/2, z; (iv) x+1/2, y+3/2, z; (vii) x+1/2, y1/2, z; (viii) x+1, y1, z+1/2; (ix) x+1/2, y1/2, z+1/2.

Experimental details

Crystal data
Chemical formulaCaNa2(P2S6)·8H2O
Mr484.49
Crystal system, space groupMonoclinic, C2/c
Temperature (K)223
a, b, c (Å)14.702 (2), 9.3081 (14), 14.052 (2)
β (°) 115.383 (11)
V3)1737.3 (4)
Z4
Radiation typeMo Kα
µ (mm1)1.34
Crystal size (mm)0.29 × 0.24 × 0.23
Data collection
DiffractometerStoe IPDS 2
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
15223, 2650, 2369
Rint0.050
(sin θ/λ)max1)0.715
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.065, 1.13
No. of reflections2650
No. of parameters122
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.68, 0.53

Computer programs: X-AREA (Stoe & Cie, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2004).

Selected bond lengths (Å) top
Ca—O12.4244 (14)Na2—O22.5282 (17)
Ca—O22.4614 (13)Na2—S1i2.9242 (8)
Ca—O32.5123 (13)Na2—S32.9673 (7)
Ca—O42.5249 (13)P—S12.0156 (6)
Na1—O32.3523 (14)P—S22.0241 (6)
Na1—O42.3713 (13)P—S32.0282 (6)
Na1—S2i2.9768 (5)P—Pi2.2381 (8)
Symmetry code: (i) x+1/2, y+3/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···S3ii0.78 (5)2.58 (5)3.2922 (17)153 (4)
O1—H1B···S2iii0.79 (4)2.62 (4)3.2892 (16)144 (4)
O2—H2A···S2ii0.79 (3)2.54 (3)3.3270 (15)172 (3)
O2—H2B···S2i0.88 (3)2.30 (3)3.1877 (15)179 (3)
O3—H3A···S1iv0.78 (3)2.43 (3)3.1908 (15)168 (2)
O3—H3B···S1ii0.86 (3)2.39 (3)3.2174 (14)161 (3)
O4—H4A···S3v0.85 (3)2.41 (3)3.2468 (14)171 (3)
O4—H4B···S30.83 (3)2.37 (3)3.1957 (14)171 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x+1/2, y1/2, z; (iii) x+1, y1, z+1/2; (iv) x+1/2, y+1/2, z; (v) x+1/2, y1/2, z+1/2.
 

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