Calcium disodium hexa­thio­diphosphate(IV) octa­hydrate

Ehrhardt, C.; Gjikaj, M.

doi:10.1107/S1600536810025304

inorganic compounds

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Volume 66| Part 8| August 2010| Page i54

https://doi.org/10.1107/S1600536810025304

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Calcium disodium hexathiodiphosphate(IV) octahydrate

Claus Ehrhardt ^a and Mimoza Gjikaj ^a ^*

^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 ); Klingen et al. (1973 ). For the synthesis of Na₄(P₂S₆)·6H₂O, see: Fincher et al. (1998 ). For the isotypic structure of SrNa₂(P₂S₆)·8H₂O, see: Gjikaj & Ehrhardt (2010 ).

Experimental

Crystal data

CaNa₂(P₂S₆)·8H₂O
M_r = 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)
R_int = 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
Δρ_max = 0.68 e Å⁻³
Δρ_min = −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	D⋯A	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⋯S1^iv	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⋯S3^v	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 ); cell refinement: X-AREA; data reduction: X-AREA; 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.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810025304/wm2364sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810025304/wm2364Isup2.hkl

checkCIF report

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.

Structure description top

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

	Fig. 1. The crystal structure of CaNa₂(P₂S₆).8H₂O in a projection along [010].
	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.
	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)·8H₂O	F(000) = 992
M_r = 484.49	D_x = 1.852 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 15599 reflections
a = 14.702 (2) Å	θ = 1.0–30.5°
b = 9.3081 (14) Å	µ = 1.34 mm⁻¹
c = 14.052 (2) Å	T = 223 K
β = 115.383 (11)°	Block, colorless
V = 1737.3 (4) Å³	0.29 × 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 tube	R_int = 0.050
Graphite monochromator	θ_max = 30.5°, θ_min = 2.7°
ω–scans	h = −20→20
15223 measured reflections	k = −13→13
2650 independent reflections	l = −20→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.029	All H-atom parameters refined
wR(F²) = 0.065	w = 1/[σ²(F_o²) + (0.0256P)² + 2.2311P] where P = (F_o² + 2F_c²)/3
S = 1.13	(Δ/σ)_max < 0.001
2650 reflections	Δρ_max = 0.68 e Å⁻³
122 parameters	Δρ_min = −0.53 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0046 (3)

Crystal data top

CaNa₂(P₂S₆)·8H₂O	V = 1737.3 (4) Å³
M_r = 484.49	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 14.702 (2) Å	µ = 1.34 mm⁻¹
b = 9.3081 (14) Å	T = 223 K
c = 14.052 (2) Å	0.29 × 0.24 × 0.23 mm
β = 115.383 (11)°

Data collection top

Stoe IPDS 2 diffractometer	2369 reflections with I > 2σ(I)
15223 measured reflections	R_int = 0.050
2650 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	0 restraints
wR(F²) = 0.065	All H-atom parameters refined
S = 1.13	Δρ_max = 0.68 e Å⁻³
2650 reflections	Δρ_min = −0.53 e Å⁻³
122 parameters

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ca	0.5000	0.24842 (5)	0.2500	0.01531 (10)
Na1	0.2500	0.2500	0.0000	0.0240 (2)
Na2	0.5000	0.67523 (13)	0.2500	0.0318 (2)
P	0.20227 (3)	0.76310 (4)	0.04363 (3)	0.01394 (9)
S1	0.06893 (3)	0.67248 (4)	−0.04913 (3)	0.02064 (10)
S2	0.18887 (3)	0.97575 (4)	0.06497 (3)	0.01807 (9)
S3	0.27954 (3)	0.66563 (4)	0.18473 (3)	0.02051 (10)
O1	0.59411 (11)	0.04315 (16)	0.23418 (13)	0.0268 (3)
O2	0.50720 (10)	0.45732 (14)	0.14604 (10)	0.0217 (2)
O3	0.41702 (10)	0.16862 (14)	0.06107 (10)	0.0216 (2)
O4	0.31872 (9)	0.32895 (14)	0.17753 (10)	0.0199 (2)
H1A	0.629 (4)	0.053 (5)	0.205 (4)	0.096 (15)*
H1B	0.627 (3)	0.002 (4)	0.287 (3)	0.068 (12)*
H2A	0.554 (3)	0.462 (3)	0.133 (3)	0.048 (9)*
H2B	0.453 (2)	0.477 (3)	0.088 (3)	0.045 (8)*
H3A	0.4123 (19)	0.085 (3)	0.059 (2)	0.029 (6)*
H3B	0.454 (2)	0.192 (3)	0.030 (2)	0.042 (8)*
H4A	0.288 (2)	0.294 (3)	0.212 (3)	0.049 (8)*
H4B	0.306 (2)	0.416 (3)	0.172 (2)	0.040 (7)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ca	0.0144 (2)	0.01655 (19)	0.01458 (19)	0.000	0.00584 (15)	0.000
Na1	0.0192 (5)	0.0302 (5)	0.0196 (5)	−0.0001 (4)	0.0053 (4)	−0.0011 (4)
Na2	0.0283 (6)	0.0396 (6)	0.0249 (5)	0.000	0.0089 (4)	0.000
P	0.01509 (18)	0.01411 (17)	0.01436 (17)	0.00019 (13)	0.00797 (14)	0.00016 (12)
S1	0.01688 (19)	0.02004 (18)	0.0257 (2)	−0.00401 (14)	0.00981 (15)	−0.00281 (14)
S2	0.01954 (19)	0.01504 (17)	0.01967 (18)	0.00092 (13)	0.00844 (14)	−0.00104 (13)
S3	0.0250 (2)	0.02236 (19)	0.01657 (17)	0.00676 (15)	0.01122 (15)	0.00515 (14)
O1	0.0201 (6)	0.0272 (6)	0.0298 (7)	0.0039 (5)	0.0075 (5)	−0.0023 (5)
O2	0.0197 (6)	0.0261 (6)	0.0187 (5)	−0.0009 (5)	0.0076 (5)	0.0038 (5)
O3	0.0241 (6)	0.0203 (6)	0.0227 (6)	0.0002 (5)	0.0124 (5)	−0.0026 (5)
O4	0.0210 (6)	0.0195 (5)	0.0214 (6)	0.0014 (4)	0.0112 (5)	−0.0002 (4)

Geometric parameters (Å, º) top

Ca—O1	2.4244 (14)	Na2—S1^iv	2.9242 (8)
Ca—O1ⁱ	2.4244 (15)	Na2—S3	2.9673 (7)
Ca—O2	2.4614 (13)	Na2—S3ⁱ	2.9674 (7)
Ca—O2ⁱ	2.4615 (13)	P—S1	2.0156 (6)
Ca—O3ⁱ	2.5122 (13)	P—S2	2.0241 (6)
Ca—O3	2.5123 (13)	P—S3	2.0282 (6)
Ca—O4	2.5249 (13)	P—P^iv	2.2381 (8)
Ca—O4ⁱ	2.5249 (13)	S1—Na2^iv	2.9242 (8)
Na1—O3	2.3523 (14)	S2—Na1^vi	2.9768 (5)
Na1—O3ⁱⁱ	2.3523 (14)	O1—H1A	0.78 (5)
Na1—O4	2.3713 (13)	O1—H1B	0.79 (4)
Na1—O4ⁱⁱ	2.3713 (13)	O2—H2A	0.79 (3)
Na1—S2ⁱⁱⁱ	2.9767 (5)	O2—H2B	0.88 (3)
Na1—S2^iv	2.9768 (5)	O3—H3A	0.78 (3)
Na2—O2	2.5282 (17)	O3—H3B	0.86 (3)
Na2—O2ⁱ	2.5283 (17)	O4—H4A	0.85 (3)
Na2—S1^v	2.9242 (8)	O4—H4B	0.83 (3)

O1—Ca—O1ⁱ	75.99 (8)	O4ⁱⁱ—Na1—S2ⁱⁱⁱ	90.48 (3)
O1—Ca—O2	113.37 (5)	O3—Na1—S2^iv	89.02 (4)
O1ⁱ—Ca—O2	148.04 (5)	O3ⁱⁱ—Na1—S2^iv	90.98 (4)
O1—Ca—O2ⁱ	148.04 (5)	O4—Na1—S2^iv	90.48 (3)
O1ⁱ—Ca—O2ⁱ	113.37 (5)	O4ⁱⁱ—Na1—S2^iv	89.52 (3)
O2—Ca—O2ⁱ	75.64 (6)	S2ⁱⁱⁱ—Na1—S2^iv	180.0
O1—Ca—O3ⁱ	79.99 (5)	O2—Na2—O2ⁱ	73.30 (7)
O1ⁱ—Ca—O3ⁱ	73.01 (5)	O2—Na2—S1^v	149.72 (4)
O2—Ca—O3ⁱ	137.37 (4)	O2ⁱ—Na2—S1^v	85.08 (3)
O2ⁱ—Ca—O3ⁱ	74.41 (4)	O2—Na2—S1^iv	85.08 (3)
O1—Ca—O3	73.01 (5)	O2ⁱ—Na2—S1^iv	149.72 (4)
O1ⁱ—Ca—O3	79.99 (5)	S1^v—Na2—S1^iv	122.01 (5)
O2—Ca—O3	74.42 (4)	O2—Na2—S3	96.20 (4)
O2ⁱ—Ca—O3	137.37 (4)	O2ⁱ—Na2—S3	81.01 (4)
O3ⁱ—Ca—O3	145.61 (6)	S1^v—Na2—S3	101.16 (2)
O1—Ca—O4	137.92 (5)	S1^iv—Na2—S3	80.537 (18)
O1ⁱ—Ca—O4	74.08 (5)	O2—Na2—S3ⁱ	81.01 (4)
O2—Ca—O4	80.36 (5)	O2ⁱ—Na2—S3ⁱ	96.20 (4)
O2ⁱ—Ca—O4	72.44 (4)	S1^v—Na2—S3ⁱ	80.537 (17)
O3ⁱ—Ca—O4	117.68 (4)	S1^iv—Na2—S3ⁱ	101.16 (2)
O3—Ca—O4	73.21 (4)	S3—Na2—S3ⁱ	176.55 (5)
O1—Ca—O4ⁱ	74.08 (5)	S1—P—S2	112.06 (3)
O1ⁱ—Ca—O4ⁱ	137.92 (5)	S1—P—S3	115.28 (3)
O2—Ca—O4ⁱ	72.44 (4)	S2—P—S3	109.99 (3)
O2ⁱ—Ca—O4ⁱ	80.36 (5)	S1—P—P^iv	105.34 (3)
O3ⁱ—Ca—O4ⁱ	73.21 (4)	S2—P—P^iv	108.14 (3)
O3—Ca—O4ⁱ	117.68 (4)	S3—P—P^iv	105.48 (3)
O4—Ca—O4ⁱ	145.46 (6)	P—S1—Na2^iv	105.07 (3)
O3—Na1—O3ⁱⁱ	180.0	P—S2—Na1^vi	137.04 (2)
O3—Na1—O4	78.97 (4)	P—S3—Na2	111.63 (3)
O3ⁱⁱ—Na1—O4	101.03 (4)	H1A—O1—H1B	105 (4)
O3—Na1—O4ⁱⁱ	101.03 (4)	Ca—O2—Na2	105.53 (5)
O3ⁱⁱ—Na1—O4ⁱⁱ	78.97 (4)	H2A—O2—H2B	108 (3)
O4—Na1—O4ⁱⁱ	179.999 (2)	Na1—O3—Ca	104.38 (5)
O3—Na1—S2ⁱⁱⁱ	90.98 (4)	Na1—O4—Ca	103.44 (5)
O3ⁱⁱ—Na1—S2ⁱⁱⁱ	89.02 (4)	H4A—O4—H4B	106 (3)
O4—Na1—S2ⁱⁱⁱ	89.52 (3)

Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+1/2, −y+1/2, −z; (iii) x, y−1, 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···A	D—H	H···A	D···A	D—H···A
O1—H1A···S3^vii	0.78 (5)	2.58 (5)	3.2922 (17)	153 (4)
O1—H1B···S2^viii	0.79 (4)	2.62 (4)	3.2892 (16)	144 (4)
O2—H2A···S2^vii	0.79 (3)	2.54 (3)	3.3270 (15)	172 (3)
O2—H2B···S2^iv	0.88 (3)	2.30 (3)	3.1877 (15)	179 (3)
O3—H3A···S1ⁱⁱ	0.78 (3)	2.43 (3)	3.1908 (15)	168 (2)
O3—H3B···S1^vii	0.86 (3)	2.39 (3)	3.2174 (14)	161 (3)
O4—H4A···S3^ix	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: (ii) −x+1/2, −y+1/2, −z; (iv) −x+1/2, −y+3/2, −z; (vii) x+1/2, y−1/2, z; (viii) −x+1, y−1, −z+1/2; (ix) −x+1/2, y−1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	CaNa₂(P₂S₆)·8H₂O
M_r	484.49
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	223
a, b, c (Å)	14.702 (2), 9.3081 (14), 14.052 (2)
β (°)	115.383 (11)
V (Å³)	1737.3 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.34
Crystal size (mm)	0.29 × 0.24 × 0.23

Data collection
Diffractometer	Stoe IPDS 2
Absorption correction	–
No. of measured, independent and observed [I > 2σ(I)] reflections	15223, 2650, 2369
R_int	0.050
(sin θ/λ)_max (Å⁻¹)	0.715

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.065, 1.13
No. of reflections	2650
No. of parameters	122
H-atom treatment	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	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—O1	2.4244 (14)	Na2—O2	2.5282 (17)
Ca—O2	2.4614 (13)	Na2—S1ⁱ	2.9242 (8)
Ca—O3	2.5123 (13)	Na2—S3	2.9673 (7)
Ca—O4	2.5249 (13)	P—S1	2.0156 (6)
Na1—O3	2.3523 (14)	P—S2	2.0241 (6)
Na1—O4	2.3713 (13)	P—S3	2.0282 (6)
Na1—S2ⁱ	2.9768 (5)	P—Pⁱ	2.2381 (8)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	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···S1^iv	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···S3^v	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+1/2, −y+3/2, −z; (ii) x+1/2, y−1/2, z; (iii) −x+1, y−1, −z+1/2; (iv) −x+1/2, −y+1/2, −z; (v) −x+1/2, y−1/2, −z+1/2.

References

Brandenburg, K. (2004). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Fincher, T., LeBret, G. & Cleary, D. A. (1998). J. Solid State Chem. 141, 274–281. Web of Science CrossRef CAS Google Scholar
Ehrhardt, C. & Gjikaj, M. (2010). Acta Cryst. E66, i55. Web of Science CrossRef IUCr Journals Google Scholar
Jörgens, S., Mewis, A., Hoffmann, R.-D., Pöttgen, R. & Mosel, B. D. (2003). Z. Anorg. Allg. Chem. 629, 429–433. Google Scholar
Klingen, W., Ott, R. & Hahn, H. (1973). Z. Anorg. Allg. Chem. 396, 271–278. CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (2008). X-AREA. Stoe & Cie, Darmstadt, Germany. Google Scholar

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