Triaqua-bis-[4-(meth-oxy-carbon-yl)benzoato-κO]zinc dihydrate.

In the crystal structure of the title complex, [Zn(C(9)H(7)O(4))(2)(H(2)O)(3)]·2H(2)O, the Zn atom and the apical aqua ligand are located on a crystallographic twofold axis, with the Zn(II) ion in a distorted square-pyramidal coordination geometry composed of five O atoms, two from the monodentate methyl-terephthalato group and three from water mol-ecules. The resulting complex and the two hydrate water mol-ecules are inter-connected by O-H⋯O hydrogen bonds.

Related literature

For related Zn(II) complexes with terephtalato anions as ligands, see: Hawxwell et al. (2006 ▶); Li et al. (1998 ▶); Clausen et al. (2005 ▶); Sun et al. (2006 ▶); Yin et al. (2008 ▶); Carton et al. (2009 ▶). For hydrogen-bond motifs, see: Etter et al. (1990 ▶); Etter (1991 ▶). For a description of the coordination of the metal atom, see: Holmes (1984 ▶).

Experimental

Crystal data

[Zn(C9H7O4)2(H2O)3]·2H2O

M = 513.74

Monoclinic,

a = 13.7157 (15) Å

b = 5.9719 (7) Å

c = 25.874 (3) Å

β = 91.551 (2)°

V = 2118.5 (4) Å3

Z = 4

Mo Kα radiation

μ = 1.23 mm−1

T = 130 K

0.28 × 0.17 × 0.02 mm

Data collection

Bruker SMART APEX CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.725, T max = 0.976

12212 measured reflections

2435 independent reflections

2269 reflections with I > 2σ(I)

R int = 0.045

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.083

S = 1.06

2435 reflections

152 parameters

H-atom parameters constrained

Δρmax = 0.43 e Å−3

Δρmin = −0.30 e Å−3

Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT-Plus (Bruker, 1999 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811010269/nc2223sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811010269/nc2223Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Zn(C9H7O4)2(H2O)3]·2H2O	F(000) = 1064
Mr = 513.74	Dx = 1.611 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 2818 reflections
a = 13.7157 (15) Å	θ = 3.0–30.6°
b = 5.9719 (7) Å	µ = 1.23 mm−1
c = 25.874 (3) Å	T = 130 K
β = 91.551 (2)°	Plate, colorless
V = 2118.5 (4) Å3	0.28 × 0.17 × 0.02 mm
Z = 4

Bruker SMART APEX CCD diffractometer	2435 independent reflections
Radiation source: fine-focus sealed tube	2269 reflections with I > 2σ(I)
graphite	Rint = 0.045
ω scans	θmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −17→17
Tmin = 0.725, Tmax = 0.976	k = −7→7
12212 measured reflections	l = −33→33

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.083	H-atom parameters constrained
S = 1.06	w = 1/[σ2(Fo2) + (0.0415P)2 + 1.9928P] where P = (Fo2 + 2Fc2)/3
2435 reflections	(Δ/σ)max < 0.001
152 parameters	Δρmax = 0.43 e Å−3
0 restraints	Δρmin = −0.30 e Å−3

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.

	x	y	z	Uiso*/Ueq
Zn1	0.5000	0.22322 (5)	0.2500	0.01550 (11)
O1	0.43857 (11)	−0.1990 (2)	0.16962 (5)	0.0234 (3)
O2	0.50650 (10)	0.1406 (2)	0.17621 (5)	0.0206 (3)
O3	0.30981 (11)	0.0349 (3)	−0.08830 (5)	0.0282 (3)
O4	0.36264 (11)	0.3853 (2)	−0.07513 (5)	0.0256 (3)
O5	0.5000	0.5587 (3)	0.2500	0.0363 (6)
H50	0.4839	0.6475	0.2239	0.053 (9)*
O6	0.65137 (10)	0.1991 (3)	0.25858 (6)	0.0263 (3)
H60	0.6780	0.3069	0.2724	0.041 (8)*
H61	0.6851	0.1665	0.2313	0.048 (8)*
C1	0.45986 (13)	−0.0115 (3)	0.15193 (7)	0.0166 (4)
C2	0.42900 (12)	0.0408 (3)	0.09683 (6)	0.0153 (4)
C3	0.38816 (15)	−0.1255 (3)	0.06540 (7)	0.0207 (4)
H3	0.3786	−0.2715	0.0789	0.025*
C4	0.36134 (14)	−0.0791 (3)	0.01444 (7)	0.0207 (4)
H4	0.3347	−0.1940	−0.0071	0.025*
C5	0.44032 (15)	0.2554 (3)	0.07716 (8)	0.0209 (4)
H5	0.4676	0.3701	0.0985	0.025*
C6	0.41201 (15)	0.3030 (3)	0.02661 (8)	0.0218 (4)
H6	0.4189	0.4506	0.0135	0.026*
C7	0.37346 (13)	0.1352 (3)	−0.00510 (7)	0.0158 (4)
C8	0.34468 (13)	0.1775 (3)	−0.06031 (7)	0.0178 (4)
O10	0.77354 (10)	0.0523 (3)	0.18399 (5)	0.0229 (3)
H100	0.8165	0.1421	0.1773	0.060 (10)*
H101	0.7457	0.0254	0.1559	0.051 (8)*
C10	0.33801 (16)	0.4409 (4)	−0.12870 (8)	0.0288 (5)
H10A	0.3762	0.3468	−0.1517	0.043*
H10B	0.3529	0.5989	−0.1350	0.043*
H10C	0.2683	0.4142	−0.1355	0.043*

	U11	U22	U33	U12	U13	U23
Zn1	0.02039 (17)	0.01448 (17)	0.01142 (16)	0.000	−0.00319 (11)	0.000
O1	0.0324 (8)	0.0186 (7)	0.0188 (7)	−0.0025 (6)	−0.0073 (6)	0.0041 (5)
O2	0.0232 (7)	0.0263 (8)	0.0120 (6)	−0.0072 (6)	−0.0019 (5)	−0.0022 (5)
O3	0.0412 (8)	0.0253 (8)	0.0174 (7)	−0.0040 (7)	−0.0100 (6)	0.0009 (6)
O4	0.0369 (8)	0.0218 (8)	0.0176 (7)	−0.0032 (6)	−0.0065 (6)	0.0071 (6)
O5	0.0728 (17)	0.0133 (10)	0.0215 (10)	0.000	−0.0236 (10)	0.000
O6	0.0220 (7)	0.0342 (9)	0.0229 (7)	−0.0058 (6)	−0.0002 (6)	−0.0088 (6)
C1	0.0153 (8)	0.0200 (10)	0.0143 (8)	0.0017 (7)	−0.0015 (6)	−0.0008 (7)
C2	0.0147 (8)	0.0173 (9)	0.0137 (8)	0.0012 (7)	−0.0006 (6)	−0.0015 (7)
C3	0.0302 (10)	0.0141 (9)	0.0175 (9)	−0.0036 (8)	−0.0039 (7)	0.0021 (7)
C4	0.0266 (10)	0.0177 (10)	0.0174 (9)	−0.0041 (8)	−0.0055 (7)	−0.0015 (7)
C5	0.0297 (10)	0.0160 (9)	0.0169 (9)	−0.0050 (8)	−0.0041 (8)	−0.0024 (7)
C6	0.0326 (11)	0.0133 (9)	0.0194 (9)	−0.0033 (8)	−0.0029 (8)	0.0025 (7)
C7	0.0152 (8)	0.0181 (9)	0.0139 (8)	0.0004 (7)	−0.0008 (6)	0.0005 (7)
C8	0.0161 (9)	0.0215 (10)	0.0158 (9)	0.0026 (7)	0.0002 (7)	0.0010 (7)
O10	0.0238 (7)	0.0285 (8)	0.0160 (6)	−0.0015 (6)	−0.0046 (5)	0.0008 (6)
C10	0.0326 (11)	0.0325 (12)	0.0209 (10)	0.0001 (9)	−0.0053 (8)	0.0103 (9)

Zn1—O2	1.9763 (12)	C2—C3	1.392 (3)
Zn1—O2i	1.9765 (12)	C3—C4	1.387 (2)
Zn1—O5	2.003 (2)	C3—H3	0.95
Zn1—O6	2.0869 (14)	C4—C7	1.388 (3)
Zn1—O6i	2.0870 (14)	C4—H4	0.95
O1—C1	1.247 (2)	C5—C6	1.384 (3)
O2—C1	1.268 (2)	C5—H5	0.95
O3—C8	1.208 (2)	C6—C7	1.390 (3)
O4—C8	1.324 (2)	C6—H6	0.95
O4—C10	1.456 (2)	C7—C8	1.493 (2)
O5—H50	0.88	O10—H100	0.82
O6—H60	0.82	O10—H101	0.83
O6—H61	0.88	C10—H10A	0.98
C1—C2	1.509 (2)	C10—H10B	0.98
C2—C5	1.389 (3)	C10—H10C	0.98
O2—Zn1—O2i	151.08 (9)	C2—C3—H3	119.8
O2—Zn1—O5	104.46 (4)	C3—C4—C7	119.94 (17)
O2i—Zn1—O5	104.46 (4)	C3—C4—H4	120.0
O2—Zn1—O6	90.85 (5)	C7—C4—H4	120.0
O2i—Zn1—O6	87.18 (6)	C6—C5—C2	120.29 (17)
O5—Zn1—O6	93.97 (4)	C6—C5—H5	119.9
O2—Zn1—O6i	87.17 (6)	C2—C5—H5	119.9
O2i—Zn1—O6i	90.85 (5)	C5—C6—C7	120.15 (18)
O5—Zn1—O6i	93.97 (4)	C5—C6—H6	119.9
O6—Zn1—O6i	172.07 (9)	C7—C6—H6	119.9
C1—O2—Zn1	128.49 (12)	C4—C7—C6	119.81 (17)
C8—O4—C10	116.67 (16)	C4—C7—C8	118.24 (17)
Zn1—O5—H50	127.0	C6—C7—C8	121.95 (17)
Zn1—O6—H60	115.1	O3—C8—O4	124.12 (17)
Zn1—O6—H61	118.4	O3—C8—C7	122.99 (18)
H60—O6—H61	106.7	O4—C8—C7	112.89 (16)
O1—C1—O2	125.53 (16)	H100—O10—H101	105.0
O1—C1—C2	118.06 (16)	O4—C10—H10A	109.5
O2—C1—C2	116.41 (16)	O4—C10—H10B	109.5
C5—C2—C3	119.45 (16)	H10A—C10—H10B	109.5
C5—C2—C1	120.40 (16)	O4—C10—H10C	109.5
C3—C2—C1	120.15 (17)	H10A—C10—H10C	109.5
C4—C3—C2	120.33 (18)	H10B—C10—H10C	109.5
C4—C3—H3	119.8

D—H···A	D—H	H···A	D···A	D—H···A
O5—H50···O1ii	0.88	1.78	2.6522 (16)	172
O6—H60···O10iii	0.82	1.96	2.763 (2)	170
O6—H61···O10	0.88	1.87	2.734 (2)	166
O10—H100···O1iv	0.82	1.94	2.741 (2)	166
O10—H101···O3v	0.83	1.92	2.7486 (19)	176

Table 1

Selected bond lengths (Å)

Zn1—O2	1.9763 (12)
Zn1—O2i	1.9765 (12)
Zn1—O5	2.003 (2)
Zn1—O6	2.0869 (14)
Zn1—O6i	2.0870 (14)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H50⋯O1ii	0.88	1.78	2.6522 (16)	172
O6—H60⋯O10iii	0.82	1.96	2.763 (2)	170
O6—H61⋯O10	0.88	1.87	2.734 (2)	166
O10—H100⋯O1iv	0.82	1.94	2.741 (2)	166
O10—H101⋯O3v	0.83	1.92	2.7486 (19)	176

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) .