Poly[[diaqua-μ2-hydroxido-(μ7-2-phos­pho­nato­ethane­sulfonato)­dicopper(II)] trihydrate]

Sonnauer, A.; Lieb, A.; Stock, N.

doi:10.1107/S1600536808033229

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 11| November 2008| Pages m1417-m1418

doi:10.1107/S1600536808033229

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Poly[[diaqua-μ₂-hydroxido-(μ₇-2-phosphonatoethanesulfonato)dicopper(II)] trihydrate]

Andreas Sonnauer,^a Alexandra Lieb ^b and Norbert Stock ^a ^*

^aInstitute of Inorganic Chemistry, Christian-Albrechts-University, Max-Eyth-Strasse 2, D 24118 Kiel, Germany, and ^bSchool of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ, England
^*Correspondence e-mail: stock@ac.uni-kiel.de

(Received 29 September 2008; accepted 13 October 2008; online 18 October 2008)

The crystal structure of the title compound, [Cu₂(C₂H₄O₆PS)(OH)(H₂O)₂]·3H₂O, consists of two Cu²⁺ ions, one (O₃PC₂H₄SO₃)³⁻ ion and one OH⁻ ion, as well as five water molecules, two of which are coordinated to Cu²⁺. The Cu²⁺ ions are coordinated by six O atoms. The CuO₆ polyhedra are connected by μ- and μ₃-O atoms into zigzag chains along the b axis. These chains are further connected by –CH₂CH₂– groups to form layers, in turn building a three-dimensional framework via hydrogen bonding.

Related literature

For related structures, see: Sonnauer et al. (2007 ); Sonnauer & Stock (2008a ,b ); Benedetto et al. (1997 ); Adani et al. (1998 ); Du et al. (2006a ,b ); Du, Li et al. (2007 ); Du, Prosvirin & Mao (2007 ); Du, Xu et al. (2007 ).

Experimental

Crystal data

[Cu₂(C₂H₄O₆PS)(OH)(H₂O)₂]·3H₂O
M_r = 421.25
Monoclinic, P 2₁ /n
a = 10.553 (2) Å
b = 7.1312 (14) Å
c = 15.791 (3) Å
β = 105.07 (3)°
V = 1147.5 (4) Å³
Z = 4
Mo Kα radiation
μ = 4.09 mm⁻¹
T = 120 (2) K
0.16 × 0.05 × 0.02 mm

Data collection

Bruker Nonius APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2007 ) T_min = 0.783, T_max = 0.922
20855 measured reflections
4352 independent reflections
3542 reflections with I > 2σ(I)
R_int = 0.061

Refinement

R[F² > 2σ(F²)] = 0.047
wR(F²) = 0.089
S = 1.11
4352 reflections
163 parameters
H-atom parameters constrained
Δρ_max = 0.75 e Å⁻³
Δρ_min = −0.78 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
OW1—H2O1⋯OW3ⁱ	0.82	1.90	2.709 (3)	168
OW1—H1O1⋯O6ⁱⁱ	0.82	2.10	2.802 (3)	144
OW2—H1O2⋯O6ⁱⁱ	0.82	1.90	2.689 (3)	162
OW2—H2O2⋯OW4ⁱⁱ	0.82	1.85	2.634 (3)	159
OW3—H1O3⋯O1	0.82	1.89	2.692 (3)	166
OW3—H2O3⋯OW5ⁱⁱⁱ	0.82	2.16	2.967 (4)	170
OW4—H2O4⋯O2ⁱⁱⁱ	0.82	1.89	2.707 (3)	174
OW4—H1O4⋯OW5ⁱⁱⁱ	0.82	1.97	2.677 (4)	144
OW5—H1O5⋯OW2^iv	0.82	2.32	2.912 (4)	130
OW5—H2O5⋯OW4^v	0.82	1.93	2.735 (4)	168
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) x+1, y, z; (iii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iv) x-1, y, z; (v) x, y+1, z.

Data collection: COLLECT (Nonius, 1998 ); cell refinement: DENZO (Otwinowski & Minor, 1997 ) and COLLECT; data reduction: DENZO and COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 1999 ); software used to prepare material for publication: publCIF (Westrip, 2008 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808033229/bt2803sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808033229/bt2803Isup2.hkl

checkCIF report

Comment top

Inorganic–organic hybrid materials based on metal carboxylates, sulfonates and phosphonates are intensively investigated due to their potential application in the field of gas separation, storage, as well as catalysis, or as sensor materials. We are interested in the use of organic ligands containing two or more different functional groups for the synthesis of functionalized hybrid compounds. Although a large number of metal phosphonates and metal sulfonates have been reported in the literature, compounds based on ligands containing simultaneously a phosphonic as well as a sulfonic acid group have only recently been investigated. These few studies are limited to the use of linker molecules based on rigid phosphonoarylsulfonic acids. Our group has started a systematic investigation using the flexible linker 2-phosphonoethansulfonic acid, which has been reported in the literature (Sonnauer et al., 2007; Sonnauer & Stock, 2008a,b). Here we report the crystal structure of the new copper phosphonatosulfonate Cu₂[(O₃PC₂H₄SO₃)(OH)(H₂O)₂](H₂O)₃, which was obtained from a hydrothermal reaction in a glass tube.

The title compound consists of two crystallographic independent copper(II) ions, one fully deprotonated (O₃PC₂H₄SO₃)^3- anion, one hydroxide ion, as well as five water molecules (two coordinated to the copper ions)(Fig. 1). The copper ions are coordinated by six oxygen atoms and form CuO₆ polyhedra. These polyhedra are connected by µ-O and µ₃-O atoms. Thus, Cu—O—Cu zigzag chains of edge-sharing polyhedra are observed (Fig. 2), which are connected by the organic group –C₂H₄– to form layers. These layers are connected via hydrogen bonds into a three-dimensional framework (Fig. 3).

Related literature top

For related structures, see: Sonnauer et al. (2007); Sonnauer & Stock (2008a,b); Benedetto et al. (1997); Adani et al. (1998); Du et al. (2006a,b); Du, Li et al. (2007); Du, Prosvirin & Mao (2007); Du, Xu et al. (2007).

Experimental top

H₂O₃PC₂H₄SO₃H was synthesized as previously reported (Sonnauer & Stock, 2008b). All other reagents were of analytical grade (Aldrich and Fluka) and were used without further purification. The synthesis was performed in a glass reactor (DURAN culture tubes 12 × 100 mm D50 GL 14 M.KAP, SCHOTT 261351155). 263 µl of 2.0 M H₃L (0.53 mmol), 536 µl of 2.0 M Cu(NO₃)₂ (1.06 mmol), and 789 µl of 2.0 M NaOH (1.59 mmol) were mixed and H₂O was added to give the final volume of 2900 µl. The mixture was heated at 90 °C for 24 h. After filtration single-crystals were isolated from the filtrate.

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998); data reduction: DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 1999); software used to prepare material for publication: publCIF (Westrip, 2008).

Figures top

	Fig. 1. Asymmetric unit of the title compound. Displacement ellipsoids are drawn at the 50% probability level.
	Fig. 2. Chains of edge-sharing CuO₆ polyhedra along the b-axis. Polyhedra are shaded in grey.
	Fig. 3. The framework consists of layers, which are connected via hydrogen bonds (dotted line).

Poly[[diaqua-µ₂-hydroxido-(µ₇-2-phosphonatoethanesulfonato)dicopper(II)] trihydrate] top

Crystal data top

[Cu₂(C₂H₄O₆PS)(OH)(H₂O)₂]·3H₂O	F(000) = 848
M_r = 421.25	D_x = 2.438 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 30417 reflections
a = 10.553 (2) Å	θ = 2.9–33.1°
b = 7.1312 (14) Å	µ = 4.09 mm⁻¹
c = 15.791 (3) Å	T = 120 K
β = 105.07 (3)°	Plate, colourless
V = 1147.5 (4) Å³	0.16 × 0.05 × 0.02 mm
Z = 4

Data collection top

Bruker Nonius APEXII CCD diffractometer	4352 independent reflections
Radiation source: Bruker Nonius FR591 rotating-anode	3542 reflections with I > 2σ(I)
10cm confocal mirrors monochromator	R_int = 0.061
Detector resolution: 4096 pixels mm^-1	θ_max = 33.1°, θ_min = 3.2°
ϕ and ω scans	h = −15→16
Absorption correction: multi-scan (SADABS; Sheldrick, 2007)	k = −10→10
T_min = 0.783, T_max = 0.922	l = −24→24
20855 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.089	H-atom parameters constrained
S = 1.11	w = 1/[σ²(F_o²) + 7.2829P] where P = (F_o² + 2F_c²)/3
4352 reflections	(Δ/σ)_max < 0.001
163 parameters	Δρ_max = 0.75 e Å⁻³
0 restraints	Δρ_min = −0.78 e Å⁻³
0 constraints

Crystal data top

[Cu₂(C₂H₄O₆PS)(OH)(H₂O)₂]·3H₂O	V = 1147.5 (4) Å³
M_r = 421.25	Z = 4
Monoclinic, P2₁/n	Mo Kα radiation
a = 10.553 (2) Å	µ = 4.09 mm⁻¹
b = 7.1312 (14) Å	T = 120 K
c = 15.791 (3) Å	0.16 × 0.05 × 0.02 mm
β = 105.07 (3)°

Data collection top

Bruker Nonius APEXII CCD diffractometer	4352 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 2007)	3542 reflections with I > 2σ(I)
T_min = 0.783, T_max = 0.922	R_int = 0.061
20855 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.047	0 restraints
wR(F²) = 0.089	H-atom parameters constrained
S = 1.11	Δρ_max = 0.75 e Å⁻³
4352 reflections	Δρ_min = −0.78 e Å⁻³
163 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
Cu1	0.82890 (4)	0.68693 (6)	0.59499 (2)	0.00711 (8)
Cu2	0.75171 (4)	0.93431 (6)	0.75238 (3)	0.00646 (8)
P1	0.55820 (7)	0.69233 (12)	0.62006 (5)	0.00591 (13)
O1	0.5805 (2)	0.5079 (3)	0.67215 (15)	0.0087 (4)
O2	0.5796 (2)	0.8648 (3)	0.68088 (14)	0.0082 (4)
O3	0.6414 (2)	0.7048 (3)	0.55453 (14)	0.0080 (4)
S1	0.18276 (7)	0.82114 (11)	0.43204 (5)	0.00632 (12)
O4	0.1526 (2)	0.9848 (3)	0.37393 (15)	0.0099 (4)
O5	0.1833 (2)	0.6481 (3)	0.38242 (15)	0.0097 (4)
O6	0.0958 (2)	0.8096 (4)	0.49057 (15)	0.0123 (4)
C1	0.3885 (3)	0.6862 (5)	0.56008 (19)	0.0083 (5)
H1A	0.3725	0.5717	0.5258	0.010*
H1B	0.3350	0.6820	0.6015	0.010*
C2	0.3448 (3)	0.8532 (4)	0.4986 (2)	0.0096 (5)
H2A	0.4044	0.8679	0.4615	0.012*
H2B	0.3486	0.9667	0.5330	0.012*
O7	0.8254 (2)	0.6840 (3)	0.72394 (13)	0.0067 (4)
H7	0.9031	0.6654	0.7482	0.010*
OW1	0.8352 (2)	0.6968 (4)	0.47036 (15)	0.0138 (5)
H1O1	0.8932	0.7573	0.4569	0.021*
H1O2	1.0598	0.7033	0.5919	0.021*
OW2	1.0209 (2)	0.6627 (3)	0.62678 (14)	0.0106 (4)
H2O1	0.7633	0.7017	0.4347	0.016*
H2O2	1.0403	0.5590	0.6487	0.016*
OW3	0.3840 (2)	0.2617 (4)	0.66291 (16)	0.0153 (5)
H1O3	0.4395	0.3368	0.6564	0.023*
H2O3	0.3752	0.3195	0.7059	0.023*
OW4	0.1112 (2)	0.3811 (4)	0.73327 (16)	0.0147 (5)
H1O4	0.1639	0.4569	0.7617	0.022*
H2O4	0.0512	0.3840	0.7574	0.022*
OW5	0.1476 (3)	1.0144 (4)	0.6947 (2)	0.0227 (6)
H1O5	0.0800	0.9714	0.6626	0.034*
H2O5	0.1251	1.1196	0.7059	0.034*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cu1	0.00682 (16)	0.00862 (17)	0.00601 (15)	−0.00029 (14)	0.00186 (12)	0.00002 (13)
Cu2	0.00614 (15)	0.00526 (15)	0.00695 (15)	−0.00005 (12)	−0.00012 (11)	−0.00153 (12)
P1	0.0060 (3)	0.0054 (3)	0.0054 (3)	−0.0002 (3)	−0.0003 (2)	−0.0005 (3)
O1	0.0066 (10)	0.0079 (10)	0.0096 (10)	−0.0010 (8)	−0.0014 (8)	0.0024 (8)
O2	0.0094 (10)	0.0059 (9)	0.0083 (9)	−0.0011 (8)	0.0001 (8)	−0.0021 (7)
O3	0.0061 (9)	0.0104 (10)	0.0069 (9)	0.0002 (8)	0.0008 (7)	−0.0003 (8)
S1	0.0069 (3)	0.0057 (3)	0.0059 (3)	0.0002 (2)	0.0007 (2)	0.0003 (2)
O4	0.0107 (10)	0.0070 (10)	0.0106 (10)	0.0008 (8)	0.0003 (8)	0.0016 (8)
O5	0.0124 (10)	0.0064 (10)	0.0093 (9)	0.0006 (8)	0.0008 (8)	−0.0013 (8)
O6	0.0105 (10)	0.0144 (11)	0.0122 (10)	0.0006 (9)	0.0036 (8)	0.0017 (9)
C1	0.0067 (12)	0.0080 (12)	0.0090 (11)	−0.0011 (11)	−0.0002 (9)	0.0005 (11)
C2	0.0095 (13)	0.0085 (13)	0.0099 (12)	−0.0014 (10)	0.0007 (10)	0.0008 (10)
O7	0.0069 (9)	0.0050 (9)	0.0077 (8)	0.0004 (8)	0.0010 (7)	0.0000 (8)
OW1	0.0091 (10)	0.0230 (13)	0.0085 (9)	−0.0046 (10)	0.0010 (8)	0.0012 (9)
OW2	0.0121 (10)	0.0114 (11)	0.0102 (9)	0.0001 (8)	0.0061 (8)	0.0016 (8)
OW3	0.0141 (11)	0.0161 (12)	0.0146 (11)	−0.0034 (9)	0.0019 (9)	0.0018 (9)
OW4	0.0126 (11)	0.0165 (12)	0.0164 (11)	0.0000 (9)	0.0063 (9)	0.0016 (9)
OW5	0.0161 (13)	0.0183 (13)	0.0310 (15)	−0.0033 (11)	0.0010 (11)	−0.0078 (12)

Geometric parameters (Å, º) top

Cu1—O3	1.919 (2)	O4—Cu1ⁱ	2.389 (2)
Cu1—OW2	1.965 (2)	O5—Cu2^vi	2.420 (2)
Cu1—OW1	1.988 (2)	O5—Cu1ⁱⁱ	2.424 (2)
Cu1—O7	2.046 (2)	C1—C2	1.530 (4)
Cu1—O4ⁱ	2.389 (2)	C1—H1A	0.9700
Cu1—O5ⁱⁱ	2.424 (2)	C1—H1B	0.9700
Cu2—O1ⁱⁱⁱ	1.932 (2)	C2—H2A	0.9700
Cu2—O2	1.937 (2)	C2—H2B	0.9700
Cu2—O7ⁱⁱⁱ	2.033 (2)	O7—Cu2^v	2.033 (2)
Cu2—O7	2.043 (2)	O7—H7	0.8200
Cu2—O5^iv	2.420 (2)	OW1—H1O1	0.8199
P1—O3	1.524 (2)	OW1—H2O1	0.8200
P1—O1	1.537 (2)	OW2—H1O2	0.8199
P1—O1	1.537 (2)	OW2—H2O2	0.8200
P1—O2	1.541 (2)	OW3—H1O3	0.8200
P1—C1	1.795 (3)	OW3—H2O3	0.8200
O1—Cu2^v	1.932 (2)	OW4—H1O4	0.8200
S1—O5	1.463 (2)	OW4—H2O4	0.8200
S1—O6	1.465 (2)	OW5—H1O5	0.8199
S1—O4	1.468 (2)	OW5—H2O5	0.8200
S1—C2	1.774 (3)

O3—Cu1—OW2	175.39 (9)	O5—S1—O6	112.38 (15)
O3—Cu1—OW1	88.01 (10)	O5—S1—O4	111.51 (13)
OW2—Cu1—OW1	87.60 (10)	O6—S1—O4	111.70 (14)
O3—Cu1—O7	92.77 (9)	O5—S1—C2	106.77 (15)
OW2—Cu1—O7	91.66 (9)	O6—S1—C2	107.42 (14)
OW1—Cu1—O7	178.32 (10)	O4—S1—C2	106.68 (14)
O3—Cu1—O4ⁱ	91.45 (9)	S1—O4—Cu1ⁱ	131.14 (14)
OW2—Cu1—O4ⁱ	90.56 (9)	S1—O5—Cu2^vi	134.67 (14)
OW1—Cu1—O4ⁱ	98.45 (10)	S1—O5—Cu1ⁱⁱ	138.17 (14)
O7—Cu1—O4ⁱ	80.05 (9)	Cu2^vi—O5—Cu1ⁱⁱ	85.68 (7)
O3—Cu1—O5ⁱⁱ	91.43 (9)	C2—C1—P1	114.3 (2)
OW2—Cu1—O5ⁱⁱ	88.08 (9)	C2—C1—H1A	108.7
OW1—Cu1—O5ⁱⁱ	101.37 (10)	P1—C1—H1A	108.7
O7—Cu1—O5ⁱⁱ	80.11 (8)	C2—C1—H1B	108.7
O4ⁱ—Cu1—O5ⁱⁱ	160.06 (8)	P1—C1—H1B	108.7
O1ⁱⁱⁱ—Cu2—O2	177.30 (10)	H1A—C1—H1B	107.6
O1ⁱⁱⁱ—Cu2—O7ⁱⁱⁱ	89.73 (9)	C1—C2—S1	111.2 (2)
O2—Cu2—O7ⁱⁱⁱ	88.38 (9)	C1—C2—H2A	109.4
O1ⁱⁱⁱ—Cu2—O7	91.86 (9)	S1—C2—H2A	109.4
O2—Cu2—O7	90.07 (9)	C1—C2—H2B	109.4
O7ⁱⁱⁱ—Cu2—O7	177.92 (2)	S1—C2—H2B	109.4
O1ⁱⁱⁱ—Cu2—O5^iv	88.29 (9)	H2A—C2—H2B	108.0
O2—Cu2—O5^iv	89.48 (9)	Cu2^v—O7—Cu2	122.09 (10)
O7ⁱⁱⁱ—Cu2—O5^iv	80.47 (8)	Cu2^v—O7—Cu1	107.67 (10)
O7—Cu2—O5^iv	100.90 (8)	Cu2—O7—Cu1	108.43 (10)
O3—P1—O1	112.24 (13)	Cu2^v—O7—H7	99.9
O3—P1—O1	112.24 (13)	Cu2—O7—H7	115.5
O3—P1—O2	111.09 (13)	Cu1—O7—H7	101.1
O1—P1—O2	111.86 (12)	Cu1—OW1—H1O1	119.6
O1—P1—O2	111.86 (12)	Cu1—OW1—H2O1	114.7
O3—P1—C1	108.35 (13)	H1O1—OW1—H2O1	114.8
O1—P1—C1	104.75 (14)	Cu1—OW2—H1O2	117.4
O1—P1—C1	104.75 (14)	Cu1—OW2—H2O2	108.3
O2—P1—C1	108.21 (14)	H1O2—OW2—H2O2	119.3
P1—O1—Cu2^v	123.42 (14)	H1O3—OW3—H2O3	90.8
P1—O2—Cu2	122.06 (14)	H1O4—OW4—H2O4	103.0
P1—O3—Cu1	119.75 (13)	H1O5—OW5—H2O5	102.8

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
OW1—H2O1···OW3ⁱⁱ	0.82	1.90	2.709 (3)	168
OW1—H1O1···O6^vii	0.82	2.10	2.802 (3)	144
OW2—H1O2···O6^vii	0.82	1.90	2.689 (3)	162
OW2—H2O2···OW4^vii	0.82	1.85	2.634 (3)	159
OW3—H1O3···O1	0.82	1.89	2.692 (3)	166
OW3—H2O3···OW5^viii	0.82	2.16	2.967 (4)	170
OW4—H2O4···O2^viii	0.82	1.89	2.707 (3)	174
OW4—H1O4···OW5^viii	0.82	1.97	2.677 (4)	144
OW5—H1O5···OW2^ix	0.82	2.32	2.912 (4)	130
OW5—H2O5···OW4^x	0.82	1.93	2.735 (4)	168

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

Experimental details

Crystal data
Chemical formula	[Cu₂(C₂H₄O₆PS)(OH)(H₂O)₂]·3H₂O
M_r	421.25
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	120
a, b, c (Å)	10.553 (2), 7.1312 (14), 15.791 (3)
β (°)	105.07 (3)
V (Å³)	1147.5 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	4.09
Crystal size (mm)	0.16 × 0.05 × 0.02

Data collection
Diffractometer	Bruker Nonius APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 2007)
T_min, T_max	0.783, 0.922
No. of measured, independent and observed [I > 2σ(I)] reflections	20855, 4352, 3542
R_int	0.061
(sin θ/λ)_max (Å⁻¹)	0.769

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.047, 0.089, 1.11
No. of reflections	4352
No. of parameters	163
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.75, −0.78

Computer programs: , DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 1999), publCIF (Westrip, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
OW1—H2O1···OW3ⁱ	0.82	1.90	2.709 (3)	168.1
OW1—H1O1···O6ⁱⁱ	0.82	2.10	2.802 (3)	143.8
OW2—H1O2···O6ⁱⁱ	0.82	1.90	2.689 (3)	162.3
OW2—H2O2···OW4ⁱⁱ	0.82	1.85	2.634 (3)	158.8
OW3—H1O3···O1	0.82	1.89	2.692 (3)	165.7
OW3—H2O3···OW5ⁱⁱⁱ	0.82	2.16	2.967 (4)	170.0
OW4—H2O4···O2ⁱⁱⁱ	0.82	1.89	2.707 (3)	173.5
OW4—H1O4···OW5ⁱⁱⁱ	0.82	1.97	2.677 (4)	143.8
OW5—H1O5···OW2^iv	0.82	2.32	2.912 (4)	129.9
OW5—H2O5···OW4^v	0.82	1.93	2.735 (4)	167.5

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

Acknowledgements

This work was supported by the Deutsche Forschungsgemeinschaft (DFG) (Project No. STO 643/2-2).

References

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