Bis(μ-5-nitro-2-oxidobenzoato)bis-[triaqua-zinc(II)].

The title complex mol-ecule, [Zn(2)(C(7)H(3)NO(5))(2)(H(2)O)(6)], is a centrosymmetric dimer containing two zinc(II) cations with distorted octa-hedral geometries provided by the O atoms of three water mol-ecules and the two bridging bidentate 5-nitro-salicylate ligands. The separation between the metal centres in the dimer is 3.1790 (11) Å. The crystal structure is stabilized by O-H⋯O hydrogen bonds, one of which intra-dimeric, linking the dimers into a three-dimensional network.

Related literature

For examples of bonding modes exhibited by salicylate anions, see: Klug et al. (1958 ▶); Risannen et al. (1987 ▶); Charles et al. (1983 ▶); Jagner et al. (1976 ▶); Fu et al. (2005 ▶). For the crystal structures of 5-nitro­salicylate zinc(II) complexes, see: Tahir et al. (1997 ▶); Morgant et al. (2006 ▶); Erxleben (2001 ▶).

Experimental

Crystal data

[Zn2(C7H3NO5)2(H2O)6]

M = 601.04

Monoclinic,

a = 10.858 (3) Å

b = 13.645 (3) Å

c = 6.6367 (17) Å

β = 91.887 (4)°

V = 982.7 (4) Å3

Z = 2

Mo Kα radiation

μ = 2.53 mm−1

T = 294 K

0.26 × 0.10 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2000 ▶) T min = 0.752, T max = 0.821

5435 measured reflections

2009 independent reflections

1418 reflections with I > 2σ(I)

R int = 0.041

Refinement

R[F 2 > 2σ(F 2)] = 0.036

wR(F 2) = 0.088

S = 1.03

2009 reflections

154 parameters

H-atom parameters constrained

Δρmax = 0.45 e Å−3

Δρmin = −0.55 e Å−3

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809045607/rz2375sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809045607/rz2375Isup2.hkl

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

[Zn2(C7H3NO5)2(H2O)6]	F(000) = 608
Mr = 601.04	Dx = 2.031 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1942 reflections
a = 10.858 (3) Å	θ = 2.4–25.8°
b = 13.645 (3) Å	µ = 2.53 mm−1
c = 6.6367 (17) Å	T = 294 K
β = 91.887 (4)°	Block, yellow-green
V = 982.7 (4) Å3	0.26 × 0.10 × 0.08 mm
Z = 2

Bruker SMART CCD area-detector diffractometer	2009 independent reflections
Radiation source: fine-focus sealed tube	1418 reflections with I > 2σ(I)
graphite	Rint = 0.041
φ and ω scans	θmax = 26.4°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 2000)	h = −13→13
Tmin = 0.752, Tmax = 0.821	k = −17→12
5435 measured reflections	l = −8→8

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)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.088	H-atom parameters constrained
S = 1.02	w = 1/[σ2(Fo2) + (0.0314P)2 + 1.0942P] where P = (Fo2 + 2Fc2)/3
2009 reflections	(Δ/σ)max = 0.001
154 parameters	Δρmax = 0.45 e Å−3
0 restraints	Δρmin = −0.55 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	0.52129 (4)	0.61159 (3)	0.44189 (8)	0.03665 (16)
O1	0.7644 (3)	0.37686 (19)	0.3938 (5)	0.0555 (9)
O2	0.6145 (2)	0.48166 (16)	0.4439 (4)	0.0310 (6)
O3	0.6603 (2)	0.67583 (17)	0.3118 (4)	0.0364 (6)
O4	1.2058 (2)	0.6122 (2)	0.1104 (5)	0.0506 (8)
O5	1.1653 (2)	0.4656 (2)	0.2105 (4)	0.0393 (7)
O6	0.4498 (3)	0.5753 (2)	0.1270 (5)	0.0564 (8)
H6A	0.4933	0.5848	0.0249	0.068*
H6B	0.3721	0.5766	0.1097	0.068*
O7	0.4029 (3)	0.72837 (19)	0.4384 (5)	0.0507 (8)
H7B	0.3400	0.7042	0.4931	0.061*
H7A	0.3907	0.7724	0.3504	0.061*
O8	0.5896 (3)	0.64083 (19)	0.7437 (4)	0.0493 (8)
H8A	0.6412	0.5961	0.7716	0.059*
H8B	0.6131	0.6997	0.7546	0.059*
N1	1.1340 (3)	0.5505 (2)	0.1763 (5)	0.0333 (7)
C1	0.7233 (3)	0.4611 (2)	0.3858 (5)	0.0271 (8)
C2	0.8053 (3)	0.5409 (2)	0.3128 (5)	0.0242 (7)
C3	0.9258 (3)	0.5143 (3)	0.2764 (5)	0.0273 (8)
H3	0.9503	0.4496	0.2969	0.033*
C4	1.0097 (3)	0.5813 (3)	0.2108 (5)	0.0281 (8)
C5	0.9774 (3)	0.6787 (3)	0.1786 (6)	0.0333 (9)
H5A	1.0350	0.7236	0.1346	0.040*
C6	0.8604 (3)	0.7068 (3)	0.2126 (6)	0.0336 (9)
H6	0.8387	0.7719	0.1905	0.040*
C7	0.7692 (3)	0.6412 (2)	0.2803 (5)	0.0268 (8)

	U11	U22	U33	U12	U13	U23
Zn1	0.0288 (2)	0.0205 (2)	0.0615 (3)	−0.00197 (18)	0.01434 (19)	−0.0010 (2)
O1	0.0525 (18)	0.0247 (16)	0.092 (2)	0.0100 (12)	0.0359 (17)	0.0158 (15)
O2	0.0268 (13)	0.0184 (12)	0.0483 (17)	−0.0017 (10)	0.0091 (11)	−0.0007 (11)
O3	0.0268 (14)	0.0236 (13)	0.0593 (19)	0.0032 (10)	0.0096 (12)	0.0079 (12)
O4	0.0274 (14)	0.0560 (19)	0.069 (2)	−0.0043 (14)	0.0138 (13)	0.0088 (16)
O5	0.0314 (14)	0.0428 (17)	0.0436 (17)	0.0106 (12)	0.0012 (12)	0.0017 (13)
O6	0.0329 (16)	0.076 (2)	0.060 (2)	−0.0017 (15)	0.0045 (14)	−0.0002 (17)
O7	0.0429 (17)	0.0279 (16)	0.082 (2)	0.0012 (12)	0.0102 (16)	0.0103 (14)
O8	0.064 (2)	0.0238 (14)	0.061 (2)	−0.0075 (13)	0.0134 (15)	−0.0095 (13)
N1	0.0264 (16)	0.044 (2)	0.0293 (18)	−0.0002 (14)	0.0000 (13)	−0.0024 (14)
C1	0.0311 (19)	0.0213 (18)	0.029 (2)	0.0013 (14)	0.0042 (15)	−0.0004 (14)
C2	0.0243 (17)	0.0244 (18)	0.0240 (19)	−0.0004 (13)	0.0021 (14)	0.0008 (14)
C3	0.032 (2)	0.0263 (19)	0.023 (2)	0.0022 (14)	0.0015 (15)	0.0017 (15)
C4	0.0221 (17)	0.039 (2)	0.023 (2)	0.0008 (14)	0.0012 (14)	0.0003 (15)
C5	0.0287 (19)	0.034 (2)	0.037 (2)	−0.0037 (15)	0.0050 (16)	0.0027 (17)
C6	0.035 (2)	0.0226 (19)	0.044 (2)	0.0003 (15)	0.0051 (17)	0.0069 (16)
C7	0.0271 (18)	0.0243 (18)	0.029 (2)	0.0021 (14)	0.0036 (14)	0.0015 (14)

Zn1—O3	1.969 (2)	O7—H7A	0.8457
Zn1—O2	2.041 (2)	O8—H8A	0.8452
Zn1—O7	2.047 (3)	O8—H8B	0.8448
Zn1—O2i	2.107 (2)	N1—C4	1.440 (4)
Zn1—O8	2.150 (3)	C1—C2	1.497 (5)
Zn1—O6	2.260 (3)	C2—C3	1.386 (5)
O1—C1	1.234 (4)	C2—C7	1.439 (5)
O2—C1	1.285 (4)	C3—C4	1.372 (5)
O3—C7	1.297 (4)	C3—H3	0.9300
O4—N1	1.237 (4)	C4—C5	1.389 (5)
O5—N1	1.226 (4)	C5—C6	1.353 (5)
O6—H6A	0.8486	C5—H5A	0.9300
O6—H6B	0.8486	C6—C7	1.418 (5)
O7—H7B	0.8511	C6—H6	0.9300
O3—Zn1—O2	90.14 (10)	Zn1—O8—H8B	110.5
O3—Zn1—O7	97.96 (11)	H8A—O8—H8B	118.1
O2—Zn1—O7	170.84 (10)	O5—N1—O4	122.3 (3)
O3—Zn1—O2i	169.08 (10)	O5—N1—C4	120.1 (3)
O2—Zn1—O2i	79.97 (10)	O4—N1—C4	117.5 (3)
O7—Zn1—O2i	91.59 (11)	O1—C1—O2	121.7 (3)
O3—Zn1—O8	94.59 (11)	O1—C1—C2	118.2 (3)
O2—Zn1—O8	89.95 (11)	O2—C1—C2	120.1 (3)
O7—Zn1—O8	93.63 (12)	C3—C2—C7	118.5 (3)
O2i—Zn1—O8	90.07 (10)	C3—C2—C1	116.2 (3)
O3—Zn1—O6	86.38 (11)	C7—C2—C1	125.4 (3)
O2—Zn1—O6	88.33 (11)	C4—C3—C2	121.4 (3)
O7—Zn1—O6	87.93 (12)	C4—C3—H3	119.3
O2i—Zn1—O6	88.69 (11)	C2—C3—H3	119.3
O8—Zn1—O6	178.03 (11)	C3—C4—C5	121.3 (3)
C1—O2—Zn1	130.4 (2)	C3—C4—N1	119.4 (3)
C1—O2—Zn1i	129.6 (2)	C5—C4—N1	119.2 (3)
Zn1—O2—Zn1i	100.03 (10)	C6—C5—C4	118.6 (3)
C7—O3—Zn1	128.7 (2)	C6—C5—H5A	120.7
Zn1—O6—H6A	121.5	C4—C5—H5A	120.7
Zn1—O6—H6B	115.5	C5—C6—C7	122.9 (3)
H6A—O6—H6B	117.7	C5—C6—H6	118.5
Zn1—O7—H7B	101.9	C7—C6—H6	118.5
Zn1—O7—H7A	130.2	O3—C7—C6	118.1 (3)
H7B—O7—H7A	117.4	O3—C7—C2	124.6 (3)
Zn1—O8—H8A	106.0	C6—C7—C2	117.3 (3)
O3—Zn1—O2—C1	2.4 (3)	O2—C1—C2—C7	−6.9 (5)
O2i—Zn1—O2—C1	177.8 (4)	C7—C2—C3—C4	0.0 (5)
O8—Zn1—O2—C1	−92.1 (3)	C1—C2—C3—C4	−179.4 (3)
O6—Zn1—O2—C1	88.8 (3)	C2—C3—C4—C5	0.1 (6)
O3—Zn1—O2—Zn1i	−175.34 (12)	C2—C3—C4—N1	179.6 (3)
O2i—Zn1—O2—Zn1i	0.0	O5—N1—C4—C3	−2.0 (5)
O8—Zn1—O2—Zn1i	90.08 (11)	O4—N1—C4—C3	177.5 (3)
O6—Zn1—O2—Zn1i	−88.96 (12)	O5—N1—C4—C5	177.5 (3)
O2—Zn1—O3—C7	−8.9 (3)	O4—N1—C4—C5	−3.0 (5)
O7—Zn1—O3—C7	175.4 (3)	C3—C4—C5—C6	−0.2 (6)
O2i—Zn1—O3—C7	−33.9 (7)	N1—C4—C5—C6	−179.7 (3)
O8—Zn1—O3—C7	81.0 (3)	C4—C5—C6—C7	0.2 (6)
O6—Zn1—O3—C7	−97.2 (3)	Zn1—O3—C7—C6	−170.1 (3)
Zn1—O2—C1—O1	−178.2 (3)	Zn1—O3—C7—C2	8.7 (5)
Zn1i—O2—C1—O1	−1.1 (5)	C5—C6—C7—O3	178.8 (4)
Zn1—O2—C1—C2	3.9 (5)	C5—C6—C7—C2	−0.1 (6)
Zn1i—O2—C1—C2	−178.9 (2)	C3—C2—C7—O3	−178.8 (3)
O1—C1—C2—C3	−5.5 (5)	C1—C2—C7—O3	0.5 (6)
O2—C1—C2—C3	172.4 (3)	C3—C2—C7—C6	0.0 (5)
O1—C1—C2—C7	175.2 (4)	C1—C2—C7—C6	179.3 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8B···O3ii	0.84	1.81	2.651 (3)	173
O8—H8A···O5iii	0.85	2.26	3.038 (4)	153
O7—H7A···O8iv	0.85	2.58	3.023 (4)	114
O7—H7B···O1i	0.85	1.77	2.596 (4)	163
O6—H6B···O4v	0.85	1.87	2.696 (4)	164
O6—H6A···O8vi	0.85	2.30	3.135 (5)	168

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O8—H8B⋯O3i	0.84	1.81	2.651 (3)	173
O8—H8A⋯O5ii	0.85	2.26	3.038 (4)	153
O7—H7A⋯O8iii	0.85	2.58	3.023 (4)	114
O7—H7B⋯O1iv	0.85	1.77	2.596 (4)	163
O6—H6B⋯O4v	0.85	1.87	2.696 (4)	164
O6—H6A⋯O8vi	0.85	2.30	3.135 (5)	168

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