catena-Poly[[[μ-aqua-penta­aqua­dizinc(II)]-μ4-benzene-1,2,4,5-tetra­carboxyl­ato] dihydrate]

Rotondo, A.; Bruno, G.; Nicoló, F.; Cento, A.

doi:10.1107/S160053680902666X

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 8| August 2009| Pages m915-m916

doi:10.1107/S160053680902666X

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catena-Poly[[[μ-aqua-pentaaquadizinc(II)]-μ₄-benzene-1,2,4,5-tetracarboxylato] dihydrate]

Archimede Rotondo,^a ^* Giuseppe Bruno,^a Francesco Nicoló ^a and Angelo Cento ^b

^aDipartimento di Chimica Inorganica, Chimica Analitica e Chimica Fisica, Universitá di Messina, Salita Sperone, 31-98166-Messina, Italy, and ^bITCGC Ferraris, Reggio Calabria, Italy
^*Correspondence e-mail: arotondo@unime.it

(Received 15 June 2009; accepted 8 July 2009; online 11 July 2009)

The asymmetric unit of the title compound, {[Zn₂(C₁₀H₂O₈)(H₂O)₆]·2H₂O}_n, contains two distinct Zn atoms joined by a bridging water molecule and two bridging carboxylate groups belonging to distinct halves of benzene-1,2,4,5-tetracarboxylate (tbec) tetraanionic ligands, both lying on crystallographic inversion centres. The structure of this new isopolymorphic one-dimensional coordination polymer features asymmetric bimetallic octahedral knots. O—H⋯O hydrogen bonds between water molecules and carboxylate O atoms help to consolidate the crystal packing.

Related literature

For background to 1,2,4,5,-benzenetetracarboxylate anions, see: Robl (1987 ); Wei et al. (1991 ). For their use in constructing stable metal-organic frameworks, see: Du et al. (2007 ); Rochon & Massarweh (2000 ); Wang et al. (2007 ); Wen et al. (2007 ); Yang et al. (2003 ). For a description of the Cambridge Structural Database, see: Allen (2002 ).

Experimental

Crystal data

[Zn₂(C₁₀H₂O₈)(H₂O)₆]·2H₂O
M_r = 525.02
Triclinic, $[P \overline 1]$
a = 6.8429 (1) Å
b = 8.0167 (1) Å
c = 16.6700 (2) Å
α = 101.620 (1)°
β = 92.555 (1)°
γ = 93.439 (1)°
V = 892.62 (2) Å³
Z = 2
Mo Kα radiation
μ = 2.77 mm⁻¹
T = 296 K
0.50 × 0.40 × 0.12 mm

Data collection

Bruker APEXII diffractometer
Absorption correction: ψ scan (North et al., 1968 ) T_min = 0.300, T_max = 0.717
17507 measured reflections
3632 independent reflections
3506 reflections with I > 2σ(I)
R_int = 0.051

Refinement

R[F² > 2σ(F²)] = 0.029
wR(F²) = 0.083
S = 1.04
3632 reflections
279 parameters
H-atom parameters constrained
Δρ_max = 0.80 e Å⁻³
Δρ_min = −0.72 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Zn1—O1W	2.0374 (15)
Zn1—O5W	2.0464 (16)
Zn1—O2	2.0484 (14)
Zn1—O2W	2.0550 (16)
Zn1—O6	2.1462 (14)
Zn1—O1B	2.2540 (14)
Zn2—O4W	1.9886 (16)
Zn2—O1	2.0065 (13)
Zn2—O3W	2.0525 (17)
Zn2—O5	2.0868 (13)
Zn2—O1B	2.1693 (14)
Zn2—O6	2.4325 (15)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1B—H1BA⋯O4ⁱ	0.85	1.82	2.667 (2)	178
O1B—H1BB⋯O7ⁱ	0.85	1.79	2.638 (2)	175
O1W—H1WA⋯O8ⁱ	0.85	1.90	2.721 (2)	163
O1W—H1WB⋯O8ⁱⁱ	0.85	1.97	2.770 (2)	156
O2W—H2WA⋯O3ⁱ	0.85	1.85	2.689 (2)	171
O2W—H2WB⋯O5ⁱⁱⁱ	0.85	1.90	2.724 (2)	163
O3W—H3WB⋯O6W^iv	0.85	1.89	2.737 (2)	174
O3W—H3WA⋯O7W	0.85	1.98	2.829 (3)	178
O4W—H4WA⋯O3^v	0.85	1.81	2.661 (2)	176
O4W—H4WB⋯O6W	0.85	1.80	2.649 (2)	175
O5W—H5WA⋯O7Wⁱⁱⁱ	0.85	1.93	2.768 (2)	170
O5W—H5WB⋯O8	0.85	2.01	2.855 (2)	171
O6W—H6WA⋯O1^vi	0.85	1.94	2.774 (2)	167
O6W—H6WB⋯O4ⁱ	0.85	1.91	2.687 (2)	152
O7W—H7WA⋯O3^vii	0.85	2.15	2.995 (3)	171
O7W—H7WB⋯O7	0.85	1.89	2.721 (2)	167
Symmetry codes: (i) x+1, y, z; (ii) -x, -y+1, -z; (iii) x, y-1, z; (iv) x-1, y, z; (v) x+1, y+1, z; (vi) -x+1, -y+2, -z+1; (vii) x, y+1, z.

Data collection: APEX2 (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP (Bruker, 2007), ORTEP-3 for Windows (Farrugia, 1997 ) and Mercury (Macrae et al., 2006 ); software used to prepare material for publication: WingGX (Farrugia, 1999 ), PARST (Nardelli, 1995 ), enCIFer (Allen et al., 2004 ) and PLATON (Spek, 2009 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680902666X/jh2083sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053680902666X/jh2083Isup2.hkl

checkCIF report

Comment top

There are many crystallogaraphic studies of 1,2,4,5,-benzenetetracarboxylic ions (btec) coordinated to zinc in the Cambridge Structural Database (Allen, 2002). The previous studies (Robl, 1987; Wei et al., 1991) were followed by others aimed at building stable metal-organic frameworks even exploiting hydrothermal conditions (Wen et al. 2007; Wang et al., 2007; Rochon & Massarweh 2000; Yang et al. 2003; Du et al. 2007). The polymorph presented here is obtained from a simple water solution containing the sodium dicarboxylate, zinc nitrate and melamine. The two metal centers of (I) display a skewed octahedral geometry (Figure 1, Table 1) with water molecules supplementing the organic ligands. Beyond the mono-dimensional scaffold running along the long diagonal of the b and c crystallographic axes (Figure 2), a close hydrogen bonding network supports the crystal packing (Table 2). Similar syntheses with different amines demonstrate that the btec coordination modes and packing strongly depend on the nature of the metal and the ancillary amines used (Bruno & Rotondo, to be published)

Related literature top

For background to 1,2,4,5,-benzenetetracarboxylic ions, see: Robl (1987); Wei et al. (1991). For their use in constructing stable metal-organic frameworks, see: Du et al. (2007); Rochon & Massarweh (2000); Wang et al. (2007); Wen et al. (2007); Yang et al. (2003). For a description of the Cambridge Structural Database, see: Allen (2002).

Experimental top

A water solution of 5 ml of Zn(NO₃)₂ 50mM with an equimolar solution of melamine were aded to 10 ml of a 25mM disodium-dihydrogen 1,2,4,5-benzenetetracarboxylate solution. The resulting clear solution with pH= 5.15 was left covered at room temperature Colourless crystals could be separated from the solution after five days.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP (Bruker, 2007), ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae et al., 2006); software used to prepare material for publication: WingGX (Farrugia, 1999), PARST (Nardelli, 1995), enCIFer (Allen et al., 2004) and PLATON (Spek, 2009).

Figures top

	Fig. 1. View of I. Displacement ellipsoids are drawn at the 40% probability level and dashed atoms are obtained by symmetry transformations. Symmetry codes #: -x, -y + 1, -z + 1; *: -x, -y + 2, -z.
	Fig. 2. Monodimensional framework running along the long diagonal of b and c crystallographic axes. Dashed lines indicate intermolecular hydrogen bonds also reported in the tables.

catena-Poly[[[µ-aqua-pentaaquadizinc(II)]- µ₄-benzene-1,2,4,5-tetracarboxylato- 1:2:1':2'κ⁶O¹,O^1':O^1':O⁴:O⁴,O^4'] dihydrate] top

Crystal data top

[Zn₂(C₁₀H₂O₈)(H₂O)₆]·2H₂O	Z = 2
M_r = 525.02	F(000) = 532
Triclinic, P1	D_x = 1.953 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.8429 (1) Å	Cell parameters from 3632 reflections
b = 8.0167 (1) Å	θ = 4.1–26.4°
c = 16.6700 (2) Å	µ = 2.77 mm⁻¹
α = 101.620 (1)°	T = 296 K
β = 92.555 (1)°	Laminar, colourless
γ = 93.439 (1)°	0.5 × 0.4 × 0.12 mm
V = 892.62 (2) Å³

Data collection top

Bruker APEXII diffractometer	3506 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.051
ω scans	θ_max = 26.4°, θ_min = 4.1°
Absorption correction: ψ scan (North et al., 1968)	h = −8→8
T_min = 0.3, T_max = 0.717	k = −10→10
17507 measured reflections	l = −20→20
3632 independent 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)] = 0.029	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.083	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0561P)² + 0.4217P] where P = (F_o² + 2F_c²)/3
3632 reflections	(Δ/σ)_max = 0.001
279 parameters	Δρ_max = 0.80 e Å⁻³
0 restraints	Δρ_min = −0.72 e Å⁻³

Crystal data top

[Zn₂(C₁₀H₂O₈)(H₂O)₆]·2H₂O	γ = 93.439 (1)°
M_r = 525.02	V = 892.62 (2) Å³
Triclinic, P1	Z = 2
a = 6.8429 (1) Å	Mo Kα radiation
b = 8.0167 (1) Å	µ = 2.77 mm⁻¹
c = 16.6700 (2) Å	T = 296 K
α = 101.620 (1)°	0.5 × 0.4 × 0.12 mm
β = 92.555 (1)°

Data collection top

Bruker APEXII diffractometer	3632 independent reflections
Absorption correction: ψ scan (North et al., 1968)	3506 reflections with I > 2σ(I)
T_min = 0.3, T_max = 0.717	R_int = 0.051
17507 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.029	0 restraints
wR(F²) = 0.083	H-atom parameters constrained
S = 1.04	Δρ_max = 0.80 e Å⁻³
3632 reflections	Δρ_min = −0.72 e Å⁻³
279 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
Zn1	0.19779 (3)	0.58919 (3)	0.188584 (13)	0.02614 (10)
Zn2	0.26320 (3)	0.96925 (3)	0.309777 (13)	0.02578 (9)
C1	0.0467 (3)	0.5880 (2)	0.43868 (11)	0.0224 (3)
C2	−0.1459 (3)	0.5219 (2)	0.44205 (11)	0.0221 (3)
C3	−0.1898 (3)	0.4336 (2)	0.50353 (11)	0.0236 (3)
H3	−0.3173	0.3884	0.5059	0.028*
C4	0.1070 (3)	0.6707 (2)	0.36925 (11)	0.0235 (3)
C5	−0.3060 (3)	0.5493 (2)	0.38211 (11)	0.0250 (4)
O1	0.1889 (2)	0.82096 (17)	0.38882 (8)	0.0292 (3)
O2	0.0801 (2)	0.58438 (19)	0.29902 (8)	0.0333 (3)
O3	−0.4229 (3)	0.4248 (2)	0.35058 (12)	0.0491 (5)
O4	−0.3135 (2)	0.69436 (19)	0.36674 (10)	0.0365 (4)
C6	0.0639 (3)	0.9763 (2)	0.07689 (11)	0.0238 (3)
C7	−0.1212 (3)	0.9066 (2)	0.04319 (11)	0.0240 (4)
C8	−0.1827 (3)	0.9309 (2)	−0.03354 (12)	0.0260 (4)
H9	−0.3053	0.8844	−0.0565	0.031*
C9	0.1354 (3)	0.9520 (2)	0.15918 (11)	0.0244 (4)
C10	−0.2624 (3)	0.8139 (2)	0.08949 (12)	0.0249 (4)
O5	0.2597 (2)	1.06218 (18)	0.20148 (8)	0.0293 (3)
O6	0.0691 (2)	0.82610 (18)	0.18669 (9)	0.0292 (3)
O7	−0.3423 (2)	0.90212 (19)	0.14747 (9)	0.0330 (3)
O8	−0.2988 (2)	0.65586 (18)	0.06365 (9)	0.0325 (3)
O1B	0.4460 (2)	0.77301 (17)	0.25175 (8)	0.0258 (3)
H1BA	0.5201	0.7459	0.2887	0.039*
H1BB	0.519	0.8101	0.2183	0.039*
O1W	0.3101 (2)	0.5950 (2)	0.07794 (9)	0.0350 (3)
H1WA	0.4347	0.6028	0.0811	0.052*
H1WB	0.2724	0.5135	0.0382	0.052*
O2W	0.3691 (3)	0.39693 (19)	0.20722 (11)	0.0391 (4)
H2WA	0.429	0.4152	0.2543	0.055 (9)*
H2WB	0.3207	0.2942	0.1968	0.062 (10)*
O3W	0.0456 (3)	1.1285 (2)	0.34625 (11)	0.0429 (4)
H3WB	−0.0281	1.0929	0.3799	0.064*
H3WA	−0.0278	1.1538	0.3086	0.064*
O4W	0.4683 (3)	1.1212 (2)	0.38193 (13)	0.0457 (4)
H4WA	0.4971	1.2194	0.3721	0.069*
H4WB	0.5726	1.0857	0.4002	0.069*
O5W	−0.0407 (2)	0.4428 (2)	0.12882 (10)	0.0361 (3)
H5WA	−0.1	0.3807	0.1571	0.054*
H5WB	−0.1224	0.5086	0.1144	0.054*
O6W	0.7863 (3)	1.0157 (2)	0.44733 (9)	0.0365 (3)
H6WA	0.793	1.0501	0.4991	0.055*
H6WB	0.7683	0.9075	0.4373	0.055*
O7W	−0.1929 (3)	1.2210 (2)	0.22149 (12)	0.0436 (4)
H7WA	−0.268	1.2784	0.254	0.065*
H7WB	−0.2568	1.1285	0.1981	0.065*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Zn1	0.03275 (15)	0.02292 (14)	0.02313 (14)	−0.00024 (10)	0.00215 (10)	0.00610 (9)
Zn2	0.03256 (15)	0.02316 (14)	0.02257 (14)	−0.00172 (10)	0.00053 (10)	0.00829 (9)
C1	0.0280 (9)	0.0191 (8)	0.0207 (8)	−0.0007 (7)	0.0026 (7)	0.0060 (6)
C2	0.0258 (8)	0.0203 (8)	0.0199 (8)	0.0002 (6)	−0.0015 (6)	0.0044 (6)
C3	0.0240 (8)	0.0239 (8)	0.0232 (8)	−0.0020 (7)	0.0009 (7)	0.0068 (7)
C4	0.0243 (8)	0.0237 (8)	0.0243 (9)	0.0005 (7)	−0.0001 (7)	0.0096 (7)
C5	0.0268 (9)	0.0267 (9)	0.0225 (8)	0.0007 (7)	−0.0013 (7)	0.0084 (7)
O1	0.0401 (8)	0.0230 (6)	0.0250 (6)	−0.0055 (5)	0.0033 (6)	0.0081 (5)
O2	0.0456 (8)	0.0312 (7)	0.0224 (7)	−0.0100 (6)	0.0034 (6)	0.0070 (5)
O3	0.0503 (10)	0.0357 (8)	0.0617 (11)	−0.0184 (7)	−0.0307 (9)	0.0244 (8)
O4	0.0439 (9)	0.0244 (7)	0.0411 (8)	0.0001 (6)	−0.0145 (7)	0.0105 (6)
C6	0.0278 (9)	0.0233 (8)	0.0211 (8)	0.0005 (7)	0.0009 (7)	0.0068 (6)
C7	0.0263 (9)	0.0222 (8)	0.0246 (9)	−0.0003 (7)	0.0036 (7)	0.0070 (7)
C8	0.0257 (9)	0.0272 (9)	0.0251 (9)	−0.0033 (7)	0.0004 (7)	0.0072 (7)
C9	0.0262 (9)	0.0251 (8)	0.0242 (9)	0.0049 (7)	0.0035 (7)	0.0086 (7)
C10	0.0256 (9)	0.0275 (9)	0.0230 (9)	−0.0017 (7)	0.0004 (7)	0.0096 (7)
O5	0.0349 (7)	0.0284 (7)	0.0246 (6)	−0.0025 (6)	−0.0049 (6)	0.0083 (5)
O6	0.0315 (7)	0.0286 (7)	0.0313 (7)	0.0028 (5)	0.0038 (6)	0.0149 (6)
O7	0.0371 (8)	0.0303 (7)	0.0322 (7)	−0.0014 (6)	0.0125 (6)	0.0069 (6)
O8	0.0361 (8)	0.0274 (7)	0.0326 (7)	−0.0079 (6)	0.0045 (6)	0.0052 (6)
O1B	0.0254 (6)	0.0278 (7)	0.0264 (7)	0.0008 (5)	0.0028 (5)	0.0106 (5)
O1W	0.0358 (8)	0.0386 (8)	0.0274 (7)	−0.0063 (6)	0.0053 (6)	0.0013 (6)
O2W	0.0450 (9)	0.0261 (7)	0.0447 (9)	0.0010 (6)	−0.0083 (7)	0.0071 (6)
O3W	0.0494 (10)	0.0450 (9)	0.0390 (9)	0.0158 (8)	0.0111 (7)	0.0144 (7)
O4W	0.0499 (10)	0.0279 (8)	0.0581 (11)	−0.0095 (7)	−0.0232 (8)	0.0149 (7)
O5W	0.0387 (8)	0.0319 (8)	0.0370 (8)	−0.0044 (6)	−0.0034 (7)	0.0091 (6)
O6W	0.0466 (9)	0.0305 (7)	0.0312 (7)	0.0025 (7)	−0.0010 (7)	0.0045 (6)
O7W	0.0473 (10)	0.0316 (8)	0.0506 (10)	−0.0004 (7)	0.0074 (8)	0.0055 (7)

Geometric parameters (Å, º) top

Zn1—O1W	2.0374 (15)	C6—C9	1.489 (2)
Zn1—O5W	2.0464 (16)	C7—C8	1.383 (3)
Zn1—O2	2.0484 (14)	C7—C10	1.514 (2)
Zn1—O2W	2.0550 (16)	C8—C6ⁱⁱ	1.390 (3)
Zn1—O6	2.1462 (14)	C8—H9	0.93
Zn1—O1B	2.2540 (14)	C9—O6	1.259 (2)
Zn2—O4W	1.9886 (16)	C9—O5	1.268 (2)
Zn2—O1	2.0065 (13)	C10—O7	1.245 (3)
Zn2—O3W	2.0525 (17)	C10—O8	1.259 (2)
Zn2—O5	2.0868 (13)	O1B—H1BA	0.85
Zn2—O1B	2.1693 (14)	O1B—H1BB	0.8499
Zn2—O6	2.4325 (15)	O1W—H1WA	0.85
Zn2—C9	2.5955 (19)	O1W—H1WB	0.8499
C1—C3ⁱ	1.386 (3)	O2W—H2WA	0.85
C1—C2	1.398 (3)	O2W—H2WB	0.8499
C1—C4	1.506 (2)	O3W—H3WB	0.85
C2—C3	1.391 (3)	O3W—H3WA	0.8499
C2—C5	1.506 (2)	O4W—H4WA	0.85
C3—C1ⁱ	1.386 (3)	O4W—H4WB	0.8499
C3—H3	0.93	O5W—H5WA	0.85
C4—O2	1.234 (2)	O5W—H5WB	0.8499
C4—O1	1.271 (2)	O6W—H6WA	0.85
C5—O4	1.243 (2)	O6W—H6WB	0.8499
C5—O3	1.252 (2)	O7W—H7WA	0.85
C6—C8ⁱⁱ	1.390 (3)	O7W—H7WB	0.8499
C6—C7	1.399 (3)

O1W—Zn1—O5W	89.16 (6)	O4—C5—C2	117.88 (17)
O1W—Zn1—O2	178.96 (7)	O3—C5—C2	118.09 (17)
O5W—Zn1—O2	90.13 (6)	C4—O1—Zn2	125.40 (12)
O1W—Zn1—O2W	92.28 (7)	C4—O2—Zn1	135.19 (13)
O5W—Zn1—O2W	98.80 (6)	C8ⁱⁱ—C6—C7	120.02 (17)
O2—Zn1—O2W	88.58 (7)	C8ⁱⁱ—C6—C9	119.49 (17)
O1W—Zn1—O6	89.74 (6)	C7—C6—C9	120.50 (16)
O5W—Zn1—O6	93.96 (6)	C8—C7—C6	119.02 (17)
O2—Zn1—O6	89.55 (6)	C8—C7—C10	118.37 (17)
O2W—Zn1—O6	167.10 (6)	C6—C7—C10	122.52 (17)
O1W—Zn1—O1B	90.00 (5)	C7—C8—C6ⁱⁱ	120.96 (17)
O5W—Zn1—O1B	174.33 (6)	C7—C8—H9	119.5
O2—Zn1—O1B	90.63 (5)	C6ⁱⁱ—C8—H9	119.5
O2W—Zn1—O1B	86.83 (6)	O6—C9—O5	120.91 (17)
O6—Zn1—O1B	80.43 (5)	O6—C9—C6	120.18 (17)
O4W—Zn2—O1	97.62 (7)	O5—C9—C6	118.89 (16)
O4W—Zn2—O3W	93.08 (8)	O6—C9—Zn2	68.41 (10)
O1—Zn2—O3W	91.65 (7)	O5—C9—Zn2	52.68 (9)
O4W—Zn2—O5	103.69 (7)	C6—C9—Zn2	169.69 (13)
O1—Zn2—O5	158.69 (6)	O7—C10—O8	124.97 (18)
O3W—Zn2—O5	87.18 (6)	O7—C10—C7	117.16 (17)
O4W—Zn2—O1B	98.94 (7)	O8—C10—C7	117.73 (17)
O1—Zn2—O1B	88.79 (6)	C9—O5—Zn2	98.43 (11)
O3W—Zn2—O1B	167.80 (7)	C9—O6—Zn1	128.94 (12)
O5—Zn2—O1B	87.99 (5)	C9—O6—Zn2	82.82 (11)
O4W—Zn2—O6	160.35 (7)	Zn1—O6—Zn2	91.75 (5)
O1—Zn2—O6	101.22 (5)	Zn2—O1B—Zn1	96.19 (5)
O3W—Zn2—O6	91.92 (6)	Zn2—O1B—H1BA	108.5
O5—Zn2—O6	57.60 (5)	Zn1—O1B—H1BA	120
O1B—Zn2—O6	76.05 (5)	Zn2—O1B—H1BB	110.8
O4W—Zn2—C9	132.49 (7)	Zn1—O1B—H1BB	112.9
O1—Zn2—C9	129.83 (6)	H1BA—O1B—H1BB	107.7
O3W—Zn2—C9	88.13 (6)	Zn1—O1W—H1WA	112
O5—Zn2—C9	28.89 (6)	Zn1—O1W—H1WB	117.1
O1B—Zn2—C9	82.25 (5)	H1WA—O1W—H1WB	107.7
O6—Zn2—C9	28.77 (5)	Zn1—O2W—H2WA	114.1
C3ⁱ—C1—C2	119.98 (17)	Zn1—O2W—H2WB	119.7
C3ⁱ—C1—C4	118.49 (16)	H2WA—O2W—H2WB	107.7
C2—C1—C4	121.35 (17)	Zn2—O3W—H3WB	113
C3—C2—C1	118.96 (17)	Zn2—O3W—H3WA	116.9
C3—C2—C5	119.88 (17)	H3WB—O3W—H3WA	107.7
C1—C2—C5	121.13 (16)	Zn2—O4W—H4WA	118.5
C1ⁱ—C3—C2	121.06 (17)	Zn2—O4W—H4WB	123.4
C1ⁱ—C3—H3	119.5	H4WA—O4W—H4WB	107.7
C2—C3—H3	119.5	Zn1—O5W—H5WA	114.7
O2—C4—O1	125.95 (17)	Zn1—O5W—H5WB	108.5
O2—C4—C1	117.27 (16)	H5WA—O5W—H5WB	107.7
O1—C4—C1	116.71 (16)	H6WA—O6W—H6WB	107.7
O4—C5—O3	124.03 (18)	H7WA—O7W—H7WB	107.7

C3ⁱ—C1—C2—C3	−0.5 (3)	O3W—Zn2—C9—C6	50.3 (7)
C4—C1—C2—C3	174.41 (16)	O5—Zn2—C9—C6	−37.3 (7)
C3ⁱ—C1—C2—C5	177.60 (17)	O1B—Zn2—C9—C6	−137.2 (7)
C4—C1—C2—C5	−7.5 (3)	O6—Zn2—C9—C6	147.7 (8)
C1—C2—C3—C1ⁱ	0.5 (3)	C8—C7—C10—O7	−104.6 (2)
C5—C2—C3—C1ⁱ	−177.61 (17)	C6—C7—C10—O7	71.8 (2)
C3ⁱ—C1—C4—O2	117.8 (2)	C8—C7—C10—O8	71.4 (2)
C2—C1—C4—O2	−57.2 (3)	C6—C7—C10—O8	−112.2 (2)
C3ⁱ—C1—C4—O1	−59.3 (2)	O6—C9—O5—Zn2	−5.4 (2)
C2—C1—C4—O1	125.70 (19)	C6—C9—O5—Zn2	172.89 (14)
C3—C2—C5—O4	134.3 (2)	O4W—Zn2—O5—C9	176.27 (12)
C1—C2—C5—O4	−43.8 (3)	O1—Zn2—O5—C9	−3.9 (2)
C3—C2—C5—O3	−46.0 (3)	O3W—Zn2—O5—C9	−91.24 (13)
C1—C2—C5—O3	135.9 (2)	O1B—Zn2—O5—C9	77.56 (12)
O2—C4—O1—Zn2	8.8 (3)	O6—Zn2—O5—C9	2.83 (10)
C1—C4—O1—Zn2	−174.40 (12)	O5—C9—O6—Zn1	−81.8 (2)
O4W—Zn2—O1—C4	−157.51 (16)	C6—C9—O6—Zn1	99.93 (19)
O3W—Zn2—O1—C4	109.16 (16)	Zn2—C9—O6—Zn1	−86.43 (13)
O5—Zn2—O1—C4	22.7 (3)	O5—C9—O6—Zn2	4.61 (17)
O1B—Zn2—O1—C4	−58.65 (16)	C6—C9—O6—Zn2	−173.65 (16)
O6—Zn2—O1—C4	16.87 (16)	O1W—Zn1—O6—C9	−35.77 (16)
C9—Zn2—O1—C4	20.22 (19)	O5W—Zn1—O6—C9	−124.92 (16)
O1—C4—O2—Zn1	19.5 (3)	O2—Zn1—O6—C9	144.99 (16)
C1—C4—O2—Zn1	−157.33 (15)	O2W—Zn1—O6—C9	63.3 (3)
O5W—Zn1—O2—C4	−161.3 (2)	O1B—Zn1—O6—C9	54.27 (16)
O2W—Zn1—O2—C4	99.9 (2)	O1W—Zn1—O6—Zn2	−117.95 (5)
O6—Zn1—O2—C4	−67.4 (2)	O5W—Zn1—O6—Zn2	152.91 (6)
O1B—Zn1—O2—C4	13.1 (2)	O2—Zn1—O6—Zn2	62.81 (5)
C8ⁱⁱ—C6—C7—C8	0.4 (3)	O2W—Zn1—O6—Zn2	−18.8 (3)
C9—C6—C7—C8	−179.71 (17)	O1B—Zn1—O6—Zn2	−27.91 (4)
C8ⁱⁱ—C6—C7—C10	−176.03 (18)	O4W—Zn2—O6—C9	−22.1 (2)
C9—C6—C7—C10	3.9 (3)	O1—Zn2—O6—C9	174.66 (11)
C6—C7—C8—C6ⁱⁱ	−0.4 (3)	O3W—Zn2—O6—C9	82.59 (11)
C10—C7—C8—C6ⁱⁱ	176.18 (18)	O5—Zn2—O6—C9	−2.84 (10)
C8ⁱⁱ—C6—C9—O6	−155.20 (18)	O1B—Zn2—O6—C9	−99.44 (11)
C7—C6—C9—O6	24.9 (3)	O4W—Zn2—O6—Zn1	106.93 (19)
C8ⁱⁱ—C6—C9—O5	26.5 (3)	O1—Zn2—O6—Zn1	−56.30 (6)
C7—C6—C9—O5	−153.42 (18)	O3W—Zn2—O6—Zn1	−148.36 (6)
C8ⁱⁱ—C6—C9—Zn2	59.9 (8)	O5—Zn2—O6—Zn1	126.20 (7)
C7—C6—C9—Zn2	−120.0 (7)	O1B—Zn2—O6—Zn1	29.61 (5)
O4W—Zn2—C9—O6	170.11 (11)	C9—Zn2—O6—Zn1	129.05 (12)
O1—Zn2—C9—O6	−6.83 (14)	O4W—Zn2—O1B—Zn1	171.17 (6)
O3W—Zn2—C9—O6	−97.42 (11)	O1—Zn2—O1B—Zn1	73.64 (6)
O5—Zn2—C9—O6	175.03 (18)	O3W—Zn2—O1B—Zn1	−18.6 (3)
O1B—Zn2—C9—O6	75.05 (11)	O5—Zn2—O1B—Zn1	−85.29 (5)
O4W—Zn2—C9—O5	−4.91 (16)	O6—Zn2—O1B—Zn1	−28.23 (4)
O1—Zn2—C9—O5	178.14 (11)	C9—Zn2—O1B—Zn1	−56.86 (5)
O3W—Zn2—C9—O5	87.55 (13)	O1W—Zn1—O1B—Zn2	121.58 (6)
O1B—Zn2—C9—O5	−99.97 (12)	O2—Zn1—O1B—Zn2	−57.59 (6)
O6—Zn2—C9—O5	−175.03 (18)	O2W—Zn1—O1B—Zn2	−146.14 (7)
O4W—Zn2—C9—C6	−42.2 (8)	O6—Zn1—O1B—Zn2	31.84 (5)
O1—Zn2—C9—C6	140.9 (7)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1B—H1BA···O4ⁱⁱⁱ	0.85	1.82	2.667 (2)	178
O1B—H1BB···O7ⁱⁱⁱ	0.85	1.79	2.638 (2)	175
O1W—H1WA···O8ⁱⁱⁱ	0.85	1.90	2.721 (2)	163
O1W—H1WB···O8^iv	0.85	1.97	2.770 (2)	156
O2W—H2WA···O3ⁱⁱⁱ	0.85	1.85	2.689 (2)	171
O2W—H2WB···O5^v	0.85	1.90	2.724 (2)	163
O3W—H3WB···O6W^vi	0.85	1.89	2.737 (2)	174
O3W—H3WA···O7W	0.85	1.98	2.829 (3)	178
O4W—H4WA···O3^vii	0.85	1.81	2.661 (2)	176
O4W—H4WB···O6W	0.85	1.80	2.649 (2)	175
O5W—H5WA···O7W^v	0.85	1.93	2.768 (2)	170
O5W—H5WB···O8	0.85	2.01	2.855 (2)	171
O6W—H6WA···O1^viii	0.85	1.94	2.774 (2)	167
O6W—H6WB···O4ⁱⁱⁱ	0.85	1.91	2.687 (2)	152
O7W—H7WA···O3^ix	0.85	2.15	2.995 (3)	171
O7W—H7WB···O7	0.85	1.89	2.721 (2)	167

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

Experimental details

Crystal data
Chemical formula	[Zn₂(C₁₀H₂O₈)(H₂O)₆]·2H₂O
M_r	525.02
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	6.8429 (1), 8.0167 (1), 16.6700 (2)
α, β, γ (°)	101.620 (1), 92.555 (1), 93.439 (1)
V (Å³)	892.62 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.77
Crystal size (mm)	0.5 × 0.4 × 0.12

Data collection
Diffractometer	Bruker APEXII diffractometer
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.3, 0.717
No. of measured, independent and observed [I > 2σ(I)] reflections	17507, 3632, 3506
R_int	0.051
(sin θ/λ)_max (Å⁻¹)	0.625

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.083, 1.04
No. of reflections	3632
No. of parameters	279
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.80, −0.72

Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP (Bruker, 2007), ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae et al., 2006), WingGX (Farrugia, 1999), PARST (Nardelli, 1995), enCIFer (Allen et al., 2004) and PLATON (Spek, 2009).

Selected geometric parameters (Å, º) top

Zn1—O1W	2.0374 (15)	Zn2—O4W	1.9886 (16)
Zn1—O5W	2.0464 (16)	Zn2—O1	2.0065 (13)
Zn1—O2	2.0484 (14)	Zn2—O3W	2.0525 (17)
Zn1—O2W	2.0550 (16)	Zn2—O5	2.0868 (13)
Zn1—O6	2.1462 (14)	Zn2—O1B	2.1693 (14)
Zn1—O1B	2.2540 (14)	Zn2—O6	2.4325 (15)

O1W—Zn1—O5W	89.16 (6)	O4W—Zn2—O1	97.62 (7)
O1W—Zn1—O2	178.96 (7)	O4W—Zn2—O3W	93.08 (8)
O5W—Zn1—O2	90.13 (6)	O1—Zn2—O3W	91.65 (7)
O1W—Zn1—O2W	92.28 (7)	O4W—Zn2—O5	103.69 (7)
O5W—Zn1—O2W	98.80 (6)	O1—Zn2—O5	158.69 (6)
O2—Zn1—O2W	88.58 (7)	O3W—Zn2—O5	87.18 (6)
O1W—Zn1—O6	89.74 (6)	O4W—Zn2—O1B	98.94 (7)
O5W—Zn1—O6	93.96 (6)	O1—Zn2—O1B	88.79 (6)
O2—Zn1—O6	89.55 (6)	O3W—Zn2—O1B	167.80 (7)
O2W—Zn1—O6	167.10 (6)	O5—Zn2—O1B	87.99 (5)
O1W—Zn1—O1B	90.00 (5)	O4W—Zn2—O6	160.35 (7)
O5W—Zn1—O1B	174.33 (6)	O1—Zn2—O6	101.22 (5)
O2—Zn1—O1B	90.63 (5)	O3W—Zn2—O6	91.92 (6)
O2W—Zn1—O1B	86.83 (6)	O5—Zn2—O6	57.60 (5)
O6—Zn1—O1B	80.43 (5)	O1B—Zn2—O6	76.05 (5)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1B—H1BA···O4ⁱ	0.85	1.82	2.667 (2)	178
O1B—H1BB···O7ⁱ	0.85	1.79	2.638 (2)	175
O1W—H1WA···O8ⁱ	0.85	1.90	2.721 (2)	163
O1W—H1WB···O8ⁱⁱ	0.85	1.97	2.770 (2)	156
O2W—H2WA···O3ⁱ	0.85	1.85	2.689 (2)	171
O2W—H2WB···O5ⁱⁱⁱ	0.85	1.90	2.724 (2)	163
O3W—H3WB···O6W^iv	0.85	1.89	2.737 (2)	174
O3W—H3WA···O7W	0.85	1.98	2.829 (3)	178
O4W—H4WA···O3^v	0.85	1.81	2.661 (2)	176
O4W—H4WB···O6W	0.85	1.80	2.649 (2)	175
O5W—H5WA···O7Wⁱⁱⁱ	0.85	1.93	2.768 (2)	170
O5W—H5WB···O8	0.85	2.01	2.855 (2)	171
O6W—H6WA···O1^vi	0.85	1.94	2.774 (2)	167
O6W—H6WB···O4ⁱ	0.85	1.91	2.687 (2)	152
O7W—H7WA···O3^vii	0.85	2.15	2.995 (3)	171
O7W—H7WB···O7	0.85	1.89	2.721 (2)	167

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

Acknowledgements

We are grateful to the Centro Interdipartimentale della Diffrazione dei Raggi X.

References

Allen, F. H. (2002). Acta Cryst. B58, 380–388. Web of Science CrossRef CAS IUCr Journals Google Scholar
Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335–338. Web of Science CrossRef CAS IUCr Journals Google Scholar
Bruker (2007). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Du, Z.-X., Li, J.-X., Zhang, G.-Y. & Hou, H.-W. (2007). Z. Kristallogr. 222, 107–108. CAS Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838. CrossRef CAS IUCr Journals Google Scholar
Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453–457. Web of Science CrossRef CAS IUCr Journals Google Scholar
Nardelli, M. (1995). J. Appl. Cryst. 28, 659. CrossRef IUCr Journals Google Scholar
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351–359. CrossRef IUCr Journals Web of Science Google Scholar
Robl, C. (1987). Z. Anorg. Allg. Chem. 554, 79–86. CSD CrossRef CAS Web of Science Google Scholar
Rochon, F. D. & Massarweh, G. (2000). Inorg. Chim. Acta, 304, 190–198. Web of Science CSD CrossRef CAS Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wang, J., Lu, L., Yang, B., Zhao, B.-Z. & Ng, S. W. (2007). Acta Cryst. E63, m2986. Web of Science CSD CrossRef IUCr Journals Google Scholar
Wei, G.-C., Jin, Z.-S., Duan, Z.-B., Yang, K.-Y. & Ni, J.-Z. (1991). Chin. J. Struct. Chem. 10, 106–109. CAS Google Scholar
Wen, Y.-H., Zhang, Q.-W., He, Y.-H. & Feng, Y.-L. (2007). Inorg. Chem. Commun. 10, 543–546. Web of Science CSD CrossRef CAS Google Scholar
Yang, S.-Y., Long, L.-S., Huang, R.-B., Zheng, L.-S. & Ng, S. W. (2003). Acta Cryst. E59, m921–m923. Web of Science CSD CrossRef IUCr Journals Google Scholar

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