Disodium tetra­aqua­bis(sulfato)iron(II)

Hudák, M.; Díaz, J.G.; Kožíšek, J.

doi:10.1107/S1600536808000214

inorganic compounds

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ISSN: 2056-9890

Volume 64| Part 2| February 2008| Page i10

doi:10.1107/S1600536808000214

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Disodium tetraaquabis(sulfato)iron(II)

Martin Hudák,^a Jesús García Díaz ^b and Jozef Kožíšek ^a ^*

^aInstitute of Physical Chemistry and Chemical Physics, Slovak University of Technology, Radlinského 9, 81237 Bratislava, Slovak Republic, and ^bMaterials Degree, Institute Technologic of Morelia, Michoacán, Mexico
^*Correspondence e-mail: jozef.kozisek@stuba.sk

(Received 30 November 2007; accepted 3 January 2008; online 9 January 2008)

In the title compound, [FeNa₂(SO₄)₂(H₂O)₄], the Fe²⁺ cation is situated on a centre of inversion and is hexacoordinated by four O atoms from water molecules and two O atoms from two sulfate anions in an octahedral geometry. The coordination environment of Na⁺ comprises six O atoms in a more distorted octahedral arrangement, with Na—O distances between 2.368 (1) and 2.612 (1) Å. The structure contains an extensive three-dimensional network of O—H⋯O hydrogen bonds.

Related literature

For related structures, see: Held (2003 ); Barton et al. (2002 ).

Experimental

Crystal data

[FeNa₂(SO₄)₂(H₂O)₄]
M_r = 366.01
Monoclinic, P 2₁ /c
a = 5.551 (1) Å
b = 8.252 (1) Å
c = 11.162 (1) Å
β = 100.20 (1)°
V = 503.1 (1) Å³
Z = 2
Mo Kα radiation
μ = 2.06 mm⁻¹
T = 301 (2) K
0.55 × 0.44 × 0.17 mm

Data collection

Oxford Diffraction Gemini R CCD diffractometer
Absorption correction: analytical [CrysAlis RED (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.]$ ), based on Clark & Reid (1995 )] T_min = 0.398, T_max = 0.720
19525 measured reflections
1343 independent reflections
1288 reflections with I > 2σ(I)
R_int = 0.022

Refinement

R[F² > 2σ(F²)] = 0.018
wR(F²) = 0.047
S = 1.07
1343 reflections
96 parameters
All H-atom parameters refined
Δρ_max = 0.31 e Å⁻³
Δρ_min = −0.40 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O8—H8A⋯O5ⁱ	0.78 (3)	1.97 (3)	2.7513 (15)	172 (2)
O8—H8B⋯O6ⁱⁱ	0.73 (3)	2.00 (3)	2.7116 (15)	165 (2)
O9—H9A⋯O6ⁱⁱⁱ	0.74 (3)	2.16 (3)	2.8741 (14)	162 (2)
O9—H9B⋯O5ⁱ	0.70 (3)	2.32 (3)	2.9379 (15)	150 (3)
Symmetry codes: (i) x-1, y, z; (ii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iii) $[x-1, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ .

Data collection: CrysAlis CCD (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, Oxfordshire, England.]$ ); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1998 ); software used to prepare material for publication: enCIFer (Allen et al., 2004 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808000214/bi2271sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808000214/bi2271Isup2.hkl

checkCIF report

Comment top

In order to find convenient crystals as model compounds for investigation of the electronic structure of Fe^II complexes, the title compound was prepared. The unit cell contains two Fe^II cations situated on centres of inversion, four Na⁺ cations, four SO₄^2- anions and eight water molecules. The structure contains a three-dimensional network of O—H···O hydrogen bonds.

In the title compound (Fig. 1), the Fe1—O8 [2.115 (1) Å] and Fe1—O9 [2.170 (1) Å] bond lengths are in reasonable agreement with a similar compounds in the Cambridge Structural Database (CSD; Version 5.27, 2006 release). For example, in ethylenediammonium tetra-aqua-bis(sulfato-O)-iron(II) (Held, 2003; CSD refcode WABHIR), the Fe—O(water) distances are 2.111 and 2.143 Å, respectively. The Fe1—O2 distance to the sulfate anion [2.095 (1) Å] compares to 2.126 Å in WABHIR. In the crystal structure of pentaaqua-(3-(diphenylphosphino)phenylsulfonato)-iron(II) (diphenyl(3-sulfonatophenyl)phosphine) (Barton et al., 2002; CSD refcode XOHHOR), there are two symmetrically independent units with corresponding distances for Fe—O(water) in the range 2.085 to 2.125 Å and for Fe—O of the sulfonato anion between 2.10 and 2.126 Å.

Related literature top

For related structures, see: Held (2003); Barton et al. (2002).

Experimental top

A solution of 1.0 mmol of Fe(SO₄)₂ in 2 ml water with one drop of diluted H₂SO₄(aq) and a piece of Fe metal was mixed with a solution of 2.0 mmol NaNO₂NCN in 10 ml water and a solution of 2.0 mmol of imidazole in 10 ml me thanol. From this system, pale yellow crystals were isolated after a few days standing.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell refinement: CrysAlis RED (Oxford Diffraction, 2007); data reduction: CrysAlis RED (Oxford Diffraction, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: enCIFer (Allen et al., 2004).

Figures top

	Fig. 1. The asymmetric unit of the title compound with displacement ellipsoids shown at the 30% probability level for non-H atoms.
	Fig. 2. Packing diagram viewed along the a axis. Hydrogen-bond interactions are indicated by dashed lines.

Disodium tetraaquabis(sulfonato)iron(II) top

Crystal data top

[FeNa₂(SO₄)₂(H₂O)₄]	F(000) = 368
M_r = 366.01	D_x = 2.416 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 17533 reflections
a = 5.551 (1) Å	θ = 3.0–31.4°
b = 8.252 (1) Å	µ = 2.06 mm⁻¹
c = 11.162 (1) Å	T = 301 K
β = 100.20 (1)°	Block, pale yellow
V = 503.1 (1) Å³	0.55 × 0.44 × 0.17 mm
Z = 2

Data collection top

Oxford Diffraction Gemini R CCD diffractometer	1343 independent reflections
Radiation source: fine-focus sealed tube	1288 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.022
ω and ϕ scans	θ_max = 29.5°, θ_min = 6.6°
Absorption correction: analytical [CrysAlis RED (Oxford Diffraction, 2007), based on Clark & Reid (1995)]	h = −7→7
T_min = 0.398, T_max = 0.720	k = −11→11
19525 measured reflections	l = −15→15

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)] = 0.018	All H-atom parameters refined
wR(F²) = 0.047	w = 1/[σ²(F_o²) + (0.0245P)² + 0.3061P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max = 0.001
1343 reflections	Δρ_max = 0.31 e Å⁻³
96 parameters	Δρ_min = −0.40 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.062 (3)

Crystal data top

[FeNa₂(SO₄)₂(H₂O)₄]	V = 503.1 (1) Å³
M_r = 366.01	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 5.551 (1) Å	µ = 2.06 mm⁻¹
b = 8.252 (1) Å	T = 301 K
c = 11.162 (1) Å	0.55 × 0.44 × 0.17 mm
β = 100.20 (1)°

Data collection top

Oxford Diffraction Gemini R CCD diffractometer	1343 independent reflections
Absorption correction: analytical [CrysAlis RED (Oxford Diffraction, 2007), based on Clark & Reid (1995)]	1288 reflections with I > 2σ(I)
T_min = 0.398, T_max = 0.720	R_int = 0.022
19525 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.018	0 restraints
wR(F²) = 0.047	All H-atom parameters refined
S = 1.08	Δρ_max = 0.31 e Å⁻³
1343 reflections	Δρ_min = −0.40 e Å⁻³
96 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.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq
O2	0.81620 (17)	0.63212 (12)	0.56957 (10)	0.0228 (2)
O4	0.70650 (19)	0.91424 (13)	0.57758 (9)	0.0234 (2)
O5	1.12799 (17)	0.82849 (12)	0.63063 (10)	0.0234 (2)
O6	0.84525 (19)	0.76778 (12)	0.76330 (9)	0.0224 (2)
O8	0.37101 (18)	0.53699 (14)	0.66515 (9)	0.01827 (19)
H8A	0.294 (4)	0.617 (3)	0.660 (2)	0.039 (6)*
H8B	0.290 (4)	0.472 (3)	0.679 (2)	0.031 (6)*
O9	0.31917 (19)	0.71528 (13)	0.41612 (10)	0.0201 (2)
H9A	0.211 (5)	0.707 (3)	0.368 (2)	0.039 (6)*
H9B	0.272 (5)	0.771 (3)	0.453 (2)	0.040 (7)*
S3	0.86989 (5)	0.78740 (3)	0.63455 (3)	0.01276 (9)
Na7	0.62761 (10)	0.56900 (7)	0.86236 (5)	0.02189 (13)
Fe1	0.5000	0.5000	0.5000	0.01297 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O2	0.0175 (4)	0.0203 (5)	0.0302 (5)	−0.0039 (3)	0.0031 (4)	−0.0113 (4)
O4	0.0263 (5)	0.0248 (5)	0.0183 (4)	0.0113 (4)	0.0017 (4)	0.0034 (4)
O5	0.0148 (4)	0.0218 (5)	0.0342 (5)	−0.0049 (4)	0.0058 (4)	−0.0040 (4)
O6	0.0292 (5)	0.0243 (5)	0.0142 (4)	0.0024 (4)	0.0054 (4)	0.0024 (4)
O8	0.0190 (4)	0.0188 (5)	0.0182 (4)	0.0011 (4)	0.0068 (3)	0.0005 (4)
O9	0.0203 (5)	0.0178 (5)	0.0198 (5)	0.0025 (4)	−0.0030 (4)	−0.0015 (4)
S3	0.01181 (14)	0.01334 (15)	0.01272 (15)	0.00036 (9)	0.00107 (10)	−0.00092 (10)
Na7	0.0242 (3)	0.0222 (3)	0.0185 (3)	−0.0010 (2)	0.0018 (2)	0.0011 (2)
Fe1	0.01386 (13)	0.01298 (13)	0.01206 (13)	−0.00055 (8)	0.00225 (8)	−0.00057 (8)

Geometric parameters (Å, º) top

O2—S3	1.4765 (10)	O9—Na7ⁱ	2.6122 (12)
O2—Fe1	2.0951 (9)	O9—H9A	0.74 (3)
O4—S3	1.4553 (10)	O9—H9B	0.70 (3)
O4—Na7ⁱ	2.3683 (11)	S3—Na7ⁱ	3.3160 (6)
O4—Na7ⁱⁱ	2.4413 (11)	Na7—O4^iv	2.3684 (11)
O5—S3	1.4805 (9)	Na7—O5^v	2.3974 (11)
O5—Na7ⁱⁱⁱ	2.3975 (11)	Na7—O4^vi	2.4413 (11)
O6—S3	1.4764 (10)	Na7—O9^iv	2.6123 (12)
O6—Na7	2.4178 (11)	Na7—S3^iv	3.3160 (6)
O8—Fe1	2.1146 (9)	Na7—Na7^vii	3.7798 (11)
O8—Na7	2.4153 (11)	Na7—H8B	2.64 (2)
O8—H8A	0.78 (3)	Fe1—O2^viii	2.0951 (9)
O8—H8B	0.73 (3)	Fe1—O8^viii	2.1146 (9)
O9—Fe1	2.1695 (10)	Fe1—O9^viii	2.1695 (10)

S3—O2—Fe1	135.77 (6)	O8—Na7—O9^iv	88.81 (4)
S3—O4—Na7ⁱ	118.30 (6)	O6—Na7—O9^iv	92.51 (4)
S3—O4—Na7ⁱⁱ	134.52 (6)	O4^vi—Na7—O9^iv	74.50 (4)
Na7ⁱ—O4—Na7ⁱⁱ	103.59 (4)	O4^iv—Na7—S3^iv	22.73 (2)
S3—O5—Na7ⁱⁱⁱ	137.19 (6)	O5^v—Na7—S3^iv	97.50 (3)
S3—O6—Na7	131.26 (6)	O8—Na7—S3^iv	162.20 (3)
Fe1—O8—Na7	125.04 (5)	O6—Na7—S3^iv	91.27 (3)
Fe1—O8—H8A	108.5 (17)	O4^vi—Na7—S3^iv	98.04 (3)
Na7—O8—H8A	102.0 (17)	O9^iv—Na7—S3^iv	73.86 (3)
Fe1—O8—H8B	113.3 (17)	O4^iv—Na7—Na7^vii	38.89 (3)
Na7—O8—H8B	99.8 (17)	O5^v—Na7—Na7^vii	90.89 (3)
H8A—O8—H8B	106 (2)	O8—Na7—Na7^vii	117.55 (3)
Fe1—O9—Na7ⁱ	112.65 (4)	O6—Na7—Na7^vii	149.97 (4)
Fe1—O9—H9A	120.0 (19)	O4^vi—Na7—Na7^vii	37.52 (2)
Na7ⁱ—O9—H9A	111.8 (19)	O9^iv—Na7—Na7^vii	70.32 (3)
Fe1—O9—H9B	118 (2)	S3^iv—Na7—Na7^vii	60.819 (15)
Na7ⁱ—O9—H9B	91 (2)	O4^iv—Na7—H8B	141.4 (5)
H9A—O9—H9B	99 (3)	O5^v—Na7—H8B	95.4 (5)
O4—S3—O6	110.26 (6)	O8—Na7—H8B	15.9 (5)
O4—S3—O2	110.70 (6)	O6—Na7—H8B	101.2 (5)
O6—S3—O2	109.73 (6)	O4^vi—Na7—H8B	65.5 (5)
O4—S3—O5	110.72 (6)	O9^iv—Na7—H8B	88.8 (5)
O6—S3—O5	108.11 (6)	S3^iv—Na7—H8B	159.2 (5)
O2—S3—O5	107.24 (6)	Na7^vii—Na7—H8B	102.8 (5)
O6—S3—Na7ⁱ	146.99 (4)	O2^viii—Fe1—O2	180.0
O2—S3—Na7ⁱ	81.15 (5)	O2^viii—Fe1—O8	90.43 (4)
O5—S3—Na7ⁱ	97.39 (5)	O2—Fe1—O8	89.57 (4)
O4^iv—Na7—O5^v	90.76 (4)	O2^viii—Fe1—O8^viii	89.57 (4)
O4^iv—Na7—O8	154.70 (4)	O2—Fe1—O8^viii	90.43 (4)
O5^v—Na7—O8	100.26 (4)	O8—Fe1—O8^viii	180.0
O4^iv—Na7—O6	114.00 (4)	O2^viii—Fe1—O9^viii	91.55 (4)
O5^v—Na7—O6	104.53 (4)	O2—Fe1—O9^viii	88.45 (4)
O8—Na7—O6	85.36 (4)	O8—Fe1—O9^viii	86.80 (4)
O4^iv—Na7—O4^vi	76.41 (4)	O8^viii—Fe1—O9^viii	93.20 (4)
O5^v—Na7—O4^vi	90.63 (4)	O2^viii—Fe1—O9	88.45 (4)
O8—Na7—O4^vi	80.73 (4)	O2—Fe1—O9	91.55 (4)
O6—Na7—O4^vi	161.06 (4)	O8—Fe1—O9	93.20 (4)
O4^iv—Na7—O9^iv	74.82 (4)	O8^viii—Fe1—O9	86.80 (4)
O5^v—Na7—O9^iv	161.21 (4)	O9^viii—Fe1—O9	179.999 (1)

Na7ⁱ—O4—S3—O6	−164.83 (6)	Fe1—O8—Na7—O9^iv	142.28 (6)
Na7ⁱⁱ—O4—S3—O6	−10.15 (11)	Fe1—O8—Na7—S3^iv	129.32 (9)
Na7ⁱ—O4—S3—O2	−43.22 (8)	Fe1—O8—Na7—Na7^vii	−150.72 (5)
Na7ⁱⁱ—O4—S3—O2	111.45 (9)	S3—O6—Na7—O4^iv	172.17 (7)
Na7ⁱ—O4—S3—O5	75.58 (8)	S3—O6—Na7—O5^v	74.68 (8)
Na7ⁱⁱ—O4—S3—O5	−129.75 (9)	S3—O6—Na7—O8	−24.74 (8)
Na7ⁱⁱ—O4—S3—Na7ⁱ	154.67 (13)	S3—O6—Na7—O4^vi	−67.51 (16)
Na7—O6—S3—O4	101.13 (8)	S3—O6—Na7—O9^iv	−113.34 (8)
Na7—O6—S3—O2	−21.05 (9)	S3—O6—Na7—S3^iv	172.76 (7)
Na7—O6—S3—O5	−137.70 (7)	S3—O6—Na7—Na7^vii	−166.63 (6)
Na7—O6—S3—Na7ⁱ	83.55 (10)	S3—O2—Fe1—O8	−46.73 (10)
Fe1—O2—S3—O4	−45.49 (11)	S3—O2—Fe1—O8^viii	133.27 (10)
Fe1—O2—S3—O6	76.42 (10)	S3—O2—Fe1—O9^viii	−133.54 (10)
Fe1—O2—S3—O5	−166.38 (9)	S3—O2—Fe1—O9	46.46 (10)
Fe1—O2—S3—Na7ⁱ	−71.33 (9)	Na7—O8—Fe1—O2^viii	150.22 (6)
Na7ⁱⁱⁱ—O5—S3—O4	32.62 (11)	Na7—O8—Fe1—O2	−29.78 (6)
Na7ⁱⁱⁱ—O5—S3—O6	−88.26 (10)	Na7—O8—Fe1—O9^viii	58.69 (6)
Na7ⁱⁱⁱ—O5—S3—O2	153.49 (9)	Na7—O8—Fe1—O9	−121.31 (6)
Na7ⁱⁱⁱ—O5—S3—Na7ⁱ	70.50 (9)	Na7ⁱ—O9—Fe1—O2^viii	−152.73 (5)
Fe1—O8—Na7—O4^iv	−168.78 (8)	Na7ⁱ—O9—Fe1—O2	27.27 (5)
Fe1—O8—Na7—O5^v	−54.28 (7)	Na7ⁱ—O9—Fe1—O8	116.93 (5)
Fe1—O8—Na7—O6	49.67 (6)	Na7ⁱ—O9—Fe1—O8^viii	−63.07 (5)
Fe1—O8—Na7—O4^vi	−143.24 (7)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8A···O5^ix	0.78 (3)	1.97 (3)	2.7513 (15)	172 (2)
O8—H8B···O6^vi	0.73 (3)	2.00 (3)	2.7116 (15)	165 (2)
O9—H9A···O6^x	0.74 (3)	2.16 (3)	2.8741 (14)	162 (2)
O9—H9B···O5^ix	0.70 (3)	2.32 (3)	2.9379 (15)	150 (3)

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

Experimental details

Crystal data
Chemical formula	[FeNa₂(SO₄)₂(H₂O)₄]
M_r	366.01
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	301
a, b, c (Å)	5.551 (1), 8.252 (1), 11.162 (1)
β (°)	100.20 (1)
V (Å³)	503.1 (1)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.06
Crystal size (mm)	0.55 × 0.44 × 0.17

Data collection
Diffractometer	Oxford Diffraction Gemini R CCD diffractometer
Absorption correction	Analytical [CrysAlis RED (Oxford Diffraction, 2007), based on Clark & Reid (1995)]
T_min, T_max	0.398, 0.720
No. of measured, independent and observed [I > 2σ(I)] reflections	19525, 1343, 1288
R_int	0.022
(sin θ/λ)_max (Å⁻¹)	0.692

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.018, 0.047, 1.08
No. of reflections	1343
No. of parameters	96
H-atom treatment	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	0.31, −0.40

Computer programs: CrysAlis CCD (Oxford Diffraction, 2007), CrysAlis RED (Oxford Diffraction, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1998), enCIFer (Allen et al., 2004).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8A···O5ⁱ	0.78 (3)	1.97 (3)	2.7513 (15)	172 (2)
O8—H8B···O6ⁱⁱ	0.73 (3)	2.00 (3)	2.7116 (15)	165 (2)
O9—H9A···O6ⁱⁱⁱ	0.74 (3)	2.16 (3)	2.8741 (14)	162 (2)
O9—H9B···O5ⁱ	0.70 (3)	2.32 (3)	2.9379 (15)	150 (3)

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

Acknowledgements

The authors thank the Grant Agency of the Slovak Republic (grant Nos. VEGA 1/2449/05 and COSNET 545.03-P) and Structural Funds, Interreg IIIA, for financial support in purchasing the diffractometer.

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