Poly[aqua-(μ(3)-2-hy-droxy-5-nitro-benzoato-κO:O:O)rubidium].

In the structure of title compound, [Rb(C(7)H(4)NO(5))(H(2)O)](n), the centrosymmetric cyclic dimeric repeating unit comprises two irregular RbO(4) complex centres bridged by the carboxyl-ate groups of the 5-nitro-salicylate ligands. The coordination about each Rb atom is completed by a monodentate water mol-ecule and a phenolic O-atom donor which gives a bridging extension [Rb-O range = 3.116 (7)-3.135 (5) Å]. The polymeric structure is stabilized by inter-molecular water O-H⋯O(carboxyl-ate) hydrogen bonds and weak inter-ring π-π inter-actions [minimum ring centroid separation = 3.620 (4) Å]. An intramolecular O-H⋯O hydrogen bond between phenol and carboxylate groups is also present.

Related literature

For the structures of some Rb complexes with aromatic carb­oxy­lic acids, see: Dinnebier et al. (2002 ▶); Wiesbrock & Schmidbaur (2003 ▶); Smith et al. (2007 ▶). For the structure of 5-nitro­asalicylic acid and some Lewis base salts and metal complexes of this acid, see: Kumar et al. (2003 ▶); Smith et al. (2005 ▶); Morgant et al. (2006 ▶).

Experimental

Crystal data

[Rb(C7H4NO5)(H2O)]

M = 285.6

Monoclinic,

a = 11.9738 (5) Å

b = 12.0230 (4) Å

c = 6.9571 (3) Å

β = 105.401 (4)°

V = 965.59 (7) Å3

Z = 4

Mo Kα radiation

μ = 5.14 mm−1

T = 200 K

0.50 × 0.20 × 0.10 mm

Data collection

Oxford Diffraction Gemini-S CCD-detector diffractometer

Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010 ▶) T min = 0.572, T max = 0.980

6051 measured reflections

1893 independent reflections

1651 reflections with I > 2σ(I)

R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.054

wR(F 2) = 0.181

S = 1.17

1893 reflections

136 parameters

H-atom parameters constrained

Δρmax = 0.81 e Å−3

Δρmin = −1.11 e Å−3

Data collection: CrysAlis PRO (Oxford Diffraction, 2010 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SIR92 (Altomare et al., 1994 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶) within WinGX (Farrugia, 1999 ▶); molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: PLATON.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811037561/nk2111sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811037561/nk2111Isup2.hkl

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

[Rb(C7H4NO5)(H2O)]	F(000) = 560
Mr = 285.60	Dx = 1.965 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4363 reflections
a = 11.9738 (5) Å	θ = 3.4–28.8°
b = 12.0230 (4) Å	µ = 5.14 mm−1
c = 6.9571 (3) Å	T = 200 K
β = 105.401 (4)°	Needle, yellow
V = 965.59 (7) Å3	0.50 × 0.20 × 0.10 mm
Z = 4

Oxford Diffraction Gemini-S CCD-detector diffractometer	1893 independent reflections
Radiation source: Enhance (Mo) X-ray source	1651 reflections with I > 2σ(I)
graphite	Rint = 0.027
Detector resolution: 16.077 pixels mm-1	θmax = 26.0°, θmin = 3.4°
ω scans	h = −14→14
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2010)	k = −14→14
Tmin = 0.572, Tmax = 0.980	l = −8→8
6051 measured reflections

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)] = 0.054	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.181	H-atom parameters constrained
S = 1.17	w = 1/[σ2(Fo2) + (0.1295P)2 + 0.7347P] where P = (Fo2 + 2Fc2)/3
1893 reflections	(Δ/σ)max < 0.001
136 parameters	Δρmax = 0.81 e Å−3
0 restraints	Δρmin = −1.11 e Å−3

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

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
Rb1	0.11224 (4)	−0.11709 (4)	0.23072 (7)	0.0208 (2)
O1W	0.0713 (6)	−0.1033 (5)	−0.2300 (10)	0.068 (2)
O2	0.1661 (5)	0.3786 (4)	0.5968 (10)	0.056 (2)
O11	0.2015 (5)	0.0401 (5)	0.5983 (9)	0.063 (2)
O12	0.0880 (4)	0.1881 (5)	0.5829 (8)	0.0583 (19)
O51	0.6650 (5)	0.2709 (6)	0.5398 (9)	0.070 (2)
O52	0.6074 (6)	0.1054 (5)	0.5877 (13)	0.068 (3)
N5	0.5896 (5)	0.2061 (6)	0.5701 (9)	0.049 (2)
C1	0.2840 (6)	0.2186 (6)	0.5897 (9)	0.041 (2)
C2	0.2690 (6)	0.3339 (6)	0.5920 (10)	0.043 (2)
C3	0.3609 (7)	0.4063 (7)	0.5906 (11)	0.049 (3)
C4	0.4652 (7)	0.3660 (6)	0.5873 (12)	0.046 (2)
C5	0.4801 (6)	0.2488 (6)	0.5818 (9)	0.043 (2)
C6	0.3918 (6)	0.1769 (6)	0.5851 (10)	0.042 (2)
C11	0.1863 (7)	0.1422 (6)	0.5922 (11)	0.043 (2)
H2	0.10940	0.32000	0.58910	0.0670*
H3	0.34960	0.48270	0.59180	0.0580*
H4	0.52640	0.41390	0.58870	0.0560*
H6	0.40380	0.10050	0.58420	0.0500*
H11W	0.11310	−0.05780	−0.28540	0.0810*
H12W	0.02110	−0.12980	−0.34140	0.0810*

	U11	U22	U33	U12	U13	U23
Rb1	0.0199 (4)	0.0188 (4)	0.0234 (4)	−0.0022 (2)	0.0050 (2)	0.0002 (2)
O1W	0.069 (4)	0.071 (4)	0.058 (4)	−0.022 (3)	0.009 (3)	0.002 (3)
O2	0.045 (3)	0.058 (4)	0.065 (4)	0.005 (2)	0.014 (3)	−0.003 (2)
O11	0.072 (4)	0.048 (4)	0.074 (4)	−0.007 (3)	0.027 (3)	−0.008 (3)
O12	0.045 (3)	0.071 (4)	0.059 (3)	−0.002 (3)	0.014 (2)	−0.005 (3)
O51	0.053 (3)	0.071 (4)	0.090 (4)	−0.007 (3)	0.026 (3)	0.003 (4)
O52	0.057 (4)	0.050 (4)	0.099 (5)	0.012 (3)	0.024 (4)	0.007 (3)
N5	0.043 (3)	0.047 (4)	0.056 (4)	−0.002 (3)	0.012 (3)	0.004 (3)
C1	0.045 (4)	0.042 (4)	0.035 (3)	0.000 (3)	0.010 (3)	−0.005 (3)
C2	0.043 (4)	0.046 (4)	0.040 (4)	0.005 (3)	0.013 (3)	0.003 (3)
C3	0.058 (5)	0.042 (4)	0.047 (4)	0.005 (3)	0.015 (4)	0.002 (3)
C4	0.050 (4)	0.044 (4)	0.047 (4)	−0.009 (3)	0.016 (3)	0.002 (3)
C5	0.044 (4)	0.044 (4)	0.039 (3)	0.004 (3)	0.009 (3)	0.000 (3)
C6	0.048 (4)	0.039 (4)	0.038 (3)	0.000 (3)	0.011 (3)	0.002 (3)
C11	0.046 (4)	0.044 (4)	0.039 (4)	−0.003 (3)	0.010 (3)	−0.009 (3)

Rb1—O1W	3.116 (7)	N5—C5	1.430 (10)
Rb1—O11	3.131 (6)	C1—C11	1.491 (11)
Rb1—O12i	3.132 (5)	C1—C2	1.399 (10)
Rb1—O2ii	3.135 (5)	C1—C6	1.393 (10)
O2—C2	1.353 (10)	C2—C3	1.405 (11)
O11—C11	1.240 (9)	C3—C4	1.345 (12)
O12—C11	1.286 (10)	C4—C5	1.422 (10)
O51—N5	1.252 (9)	C5—C6	1.371 (10)
O52—N5	1.230 (9)	C3—H3	0.9300
O1W—H11W	0.8900	C4—H4	0.9300
O1W—H12W	0.9000	C6—H6	0.9300
O2—H2	0.9700
O1W—Rb1—O11	137.27 (16)	C6—C1—C11	120.9 (7)
O1W—Rb1—O12i	120.79 (17)	C1—C2—C3	120.7 (7)
O1W—Rb1—O2ii	68.54 (16)	O2—C2—C3	118.3 (7)
O11—Rb1—O12i	87.66 (15)	O2—C2—C1	121.0 (6)
O2ii—Rb1—O11	68.78 (16)	C2—C3—C4	120.6 (7)
O2ii—Rb1—O12i	127.80 (16)	C3—C4—C5	118.8 (7)
Rb1—O2ii—C2ii	129.2 (4)	N5—C5—C6	119.8 (7)
Rb1—O11—C11	123.7 (5)	C4—C5—C6	121.4 (7)
Rb1i—O12—C11	130.8 (5)	N5—C5—C4	118.7 (7)
Rb1—O1W—H11W	121.00	C1—C6—C5	119.8 (7)
Rb1—O1W—H12W	139.00	O11—C11—C1	120.1 (7)
H11W—O1W—H12W	100.00	O12—C11—C1	116.5 (6)
Rb1iii—O2—H2	119.00	O11—C11—O12	123.4 (8)
C2—O2—H2	110.00	C2—C3—H3	120.00
O51—N5—C5	119.9 (7)	C4—C3—H3	120.00
O52—N5—C5	119.0 (7)	C3—C4—H4	121.00
O51—N5—O52	121.1 (7)	C5—C4—H4	121.00
C2—C1—C6	118.7 (7)	C1—C6—H6	120.00
C2—C1—C11	120.5 (7)	C5—C6—H6	120.00
O1W—Rb1—O11—C11	32.4 (7)	C2—C1—C6—C5	−0.4 (9)
O12i—Rb1—O11—C11	−102.9 (6)	C11—C1—C6—C5	179.7 (6)
O2ii—Rb1—O11—C11	29.5 (6)	C2—C1—C11—O11	−177.1 (7)
O1W—Rb1—O12i—C11i	−62.5 (6)	C2—C1—C11—O12	4.5 (10)
O11—Rb1—O12i—C11i	83.8 (6)	C6—C1—C11—O11	2.9 (10)
O1W—Rb1—O2ii—C2ii	−96.4 (6)	C6—C1—C11—O12	−175.5 (6)
O11—Rb1—O2ii—C2ii	81.5 (6)	C11—C1—C2—O2	0.1 (10)
Rb1—O2ii—C2ii—C1ii	−159.4 (5)	C11—C1—C2—C3	179.7 (6)
Rb1—O2ii—C2ii—C3ii	20.2 (9)	C6—C1—C2—O2	−179.9 (6)
Rb1—O11—C11—O12	73.6 (9)	C6—C1—C2—C3	−0.3 (10)
Rb1—O11—C11—C1	−104.7 (7)	O2—C2—C3—C4	179.5 (7)
Rb1i—O12—C11—O11	34.3 (11)	C1—C2—C3—C4	−0.1 (11)
Rb1i—O12—C11—C1	−147.4 (5)	C2—C3—C4—C5	1.1 (11)
O51—N5—C5—C4	−8.9 (9)	C3—C4—C5—N5	177.5 (7)
O52—N5—C5—C4	172.0 (7)	C3—C4—C5—C6	−1.7 (11)
O51—N5—C5—C6	170.3 (6)	N5—C5—C6—C1	−177.8 (6)
O52—N5—C5—C6	−8.8 (10)	C4—C5—C6—C1	1.4 (10)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O12	0.97	1.61	2.468 (8)	145
O1W—H11W···O11iv	0.89	1.90	2.794 (9)	179
O1W—H12W···O12v	0.90	1.96	2.861 (9)	180

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2⋯O12	0.97	1.61	2.468 (8)	145
O1W—H11W⋯O11i	0.89	1.90	2.794 (9)	179
O1W—H12W⋯O12ii	0.90	1.96	2.861 (9)	180

Symmetry codes: (i) ; (ii) .