Poly[μ(3)-aqua-aqua(μ(3)-3,5-dinitro-benzoato-κO(1):O(3):O(5))caesium].

In the structure of the title complex, [Cs(C(7)H(3)N(2)O(6))(H(2)O)(2)](n), the Cs salt of 3,5-dinitro-benzoic acid, the metal complex centres have have irregular CsO(8) coordination, comprising two water mol-ecules (one triply bridging and the other monodentate) and four O-atom donors from two nitro groups and one bridging carboxyl-ate O-atom donor from the ligand. Intra-unit O-H⋯O hydrogen-bonding inter-actions involving both water mol-ecules are observed in the three-dimensional polymeric complex structure.

Related literature

For exanples of structures of alkali metal complexes with 3,5-dinitro­benzoic acid, see: Yang & Ng (2007 ▶) (Li, Na); Tiekink et al. (1990 ▶); Jones et al. (2005 ▶); Madej et al. (2007 ▶) (Na); Miao & Fan (2011 ▶); Miao et al. (2011 ▶) (Rb). For examples of Cs complexes with nitro­benzoic acids, see: Smith & Wermuth (2011a ▶,b ▶).

Experimental

Crystal data

[Cs(C7H3N2O6)(H2O)2]

M = 380.06

Monoclinic,

a = 15.1249 (5) Å

b = 4.6223 (1) Å

c = 17.1024 (6) Å

β = 107.782 (4)°

V = 1138.54 (7) Å3

Z = 4

Mo Kα radiation

μ = 3.29 mm−1

T = 200 K

0.28 × 0.15 × 0.06 mm

Data collection

Oxford Diffraction Gemini-S CCD-detector diffractometer

Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012 ▶) T min = 0.792, T max = 0.980

7596 measured reflections

2652 independent reflections

2336 reflections with I > 2σ(I)

R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.024

wR(F 2) = 0.048

S = 1.05

2652 reflections

179 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.47 e Å−3

Δρmin = −0.56 e Å−3

Data collection: CrysAlis PRO (Agilent, 2012 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); 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/S1600536812037130/ng5289sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812037130/ng5289Isup2.hkl

Supplementary material file. DOI: 10.1107/S1600536812037130/ng5289Isup3.cml

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

[Cs(C7H3N2O6)(H2O)2]	F(000) = 728
Mr = 380.06	Dx = 2.217 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 3275 reflections
a = 15.1249 (5) Å	θ = 3.2–28.8°
b = 4.6223 (1) Å	µ = 3.29 mm−1
c = 17.1024 (6) Å	T = 200 K
β = 107.782 (4)°	Needle, yellow
V = 1138.54 (7) Å3	0.28 × 0.15 × 0.06 mm
Z = 4

Oxford Diffraction Gemini-S CCD-detector diffractometer	2652 independent reflections
Radiation source: Enhance (Mo) X-ray source	2336 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.030
Detector resolution: 16.077 pixels mm-1	θmax = 28.9°, θmin = 3.2°
ω scans	h = −20→20
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012)	k = −6→5
Tmin = 0.792, Tmax = 0.980	l = −22→22
7596 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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.048	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ2(Fo2) + (0.0172P)2] where P = (Fo2 + 2Fc2)/3
2652 reflections	(Δ/σ)max = 0.001
179 parameters	Δρmax = 0.47 e Å−3
0 restraints	Δρmin = −0.56 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
Cs1	0.63127 (1)	0.11431 (3)	0.94980 (1)	0.0232 (1)
O1W	0.57824 (16)	−0.3598 (5)	1.05448 (13)	0.0315 (7)
O2W	0.69998 (16)	0.0306 (5)	1.14991 (13)	0.0311 (7)
O11	0.37491 (13)	0.6190 (4)	0.75558 (11)	0.0278 (6)
O12	0.52278 (14)	0.6236 (3)	0.83580 (11)	0.0266 (6)
O31	0.74660 (14)	0.3113 (4)	0.68972 (12)	0.0315 (6)
O32	0.71260 (15)	−0.0756 (4)	0.61600 (12)	0.0351 (7)
O51	0.39421 (16)	−0.3890 (4)	0.51426 (12)	0.0351 (7)
O52	0.28880 (15)	−0.1482 (4)	0.54804 (12)	0.0381 (7)
N3	0.69218 (16)	0.1222 (4)	0.65482 (13)	0.0234 (7)
N5	0.36953 (17)	−0.2001 (5)	0.55368 (12)	0.0246 (7)
C1	0.48439 (18)	0.3386 (5)	0.71545 (14)	0.0169 (7)
C2	0.57543 (18)	0.3203 (5)	0.71383 (14)	0.0177 (7)
C3	0.59685 (18)	0.1317 (5)	0.65956 (15)	0.0186 (7)
C4	0.53156 (19)	−0.0458 (5)	0.60715 (14)	0.0191 (7)
C5	0.44224 (19)	−0.0198 (5)	0.60976 (14)	0.0187 (7)
C6	0.41608 (18)	0.1685 (5)	0.66192 (14)	0.0187 (7)
C11	0.45850 (19)	0.5455 (5)	0.77413 (15)	0.0186 (7)
H2	0.62150	0.43370	0.74890	0.0210*
H4	0.54740	−0.17570	0.57210	0.0230*
H6	0.35450	0.18100	0.66120	0.0220*
H11W	0.616 (3)	−0.280 (7)	1.091 (2)	0.038 (10)*
H12W	0.559 (3)	−0.478 (7)	1.081 (2)	0.055 (12)*
H21W	0.677 (3)	0.124 (6)	1.180 (2)	0.052 (12)*
H22W	0.750 (3)	−0.041 (6)	1.1818 (19)	0.037 (9)*

	U11	U22	U33	U12	U13	U23
Cs1	0.0226 (1)	0.0231 (1)	0.0235 (1)	−0.0002 (1)	0.0063 (1)	0.0030 (1)
O1W	0.0308 (13)	0.0405 (12)	0.0214 (10)	−0.0117 (10)	0.0053 (9)	0.0000 (10)
O2W	0.0259 (12)	0.0355 (11)	0.0284 (11)	0.0046 (10)	0.0032 (10)	−0.0094 (10)
O11	0.0174 (10)	0.0373 (11)	0.0279 (10)	0.0052 (8)	0.0059 (8)	−0.0072 (8)
O12	0.0229 (11)	0.0330 (10)	0.0210 (9)	−0.0005 (8)	0.0023 (8)	−0.0092 (8)
O31	0.0204 (11)	0.0385 (11)	0.0356 (11)	−0.0040 (9)	0.0084 (9)	−0.0042 (9)
O32	0.0310 (12)	0.0442 (12)	0.0324 (11)	0.0130 (9)	0.0130 (10)	−0.0079 (9)
O51	0.0492 (15)	0.0248 (10)	0.0266 (10)	−0.0040 (9)	0.0045 (10)	−0.0093 (8)
O52	0.0252 (12)	0.0548 (13)	0.0342 (11)	−0.0143 (10)	0.0089 (9)	−0.0132 (10)
N3	0.0223 (13)	0.0294 (12)	0.0180 (11)	0.0075 (10)	0.0055 (9)	0.0042 (9)
N5	0.0304 (15)	0.0246 (11)	0.0169 (11)	−0.0075 (10)	0.0044 (10)	−0.0012 (9)
C1	0.0203 (14)	0.0179 (11)	0.0128 (11)	−0.0002 (10)	0.0055 (10)	0.0013 (9)
C2	0.0171 (13)	0.0182 (11)	0.0161 (12)	−0.0004 (10)	0.0024 (10)	0.0025 (10)
C3	0.0188 (14)	0.0198 (12)	0.0178 (12)	0.0039 (10)	0.0067 (10)	0.0057 (10)
C4	0.0278 (15)	0.0153 (11)	0.0141 (12)	0.0013 (10)	0.0063 (10)	−0.0001 (9)
C5	0.0244 (15)	0.0175 (11)	0.0130 (11)	−0.0039 (11)	0.0039 (10)	−0.0005 (10)
C6	0.0197 (14)	0.0207 (12)	0.0152 (11)	−0.0023 (10)	0.0048 (10)	0.0034 (10)
C11	0.0220 (14)	0.0192 (12)	0.0168 (12)	−0.0014 (10)	0.0091 (10)	0.0022 (10)

Cs1—O1W	3.087 (2)	O1W—H11W	0.80 (4)
Cs1—O2W	3.282 (2)	O2W—H21W	0.83 (4)
Cs1—O12	3.1751 (16)	O2W—H22W	0.85 (4)
Cs1—O12i	3.1120 (17)	N3—C3	1.469 (4)
Cs1—O1Wii	3.261 (2)	N5—C5	1.476 (3)
Cs1—O32iii	3.244 (2)	C1—C2	1.388 (4)
Cs1—O1Wiv	3.346 (2)	C1—C6	1.395 (3)
Cs1—O52v	3.271 (2)	C1—C11	1.522 (3)
O11—C11	1.253 (4)	C2—C3	1.382 (3)
O12—C11	1.250 (3)	C3—C4	1.382 (4)
O31—N3	1.224 (3)	C4—C5	1.371 (4)
O32—N3	1.224 (3)	C5—C6	1.388 (3)
O51—N5	1.229 (3)	C2—H2	0.9300
O52—N5	1.219 (4)	C4—H4	0.9300
O1W—H12W	0.82 (4)	C6—H6	0.9300
O1W—Cs1—O2W	50.74 (6)	H11W—O1W—H12W	100 (4)
O1W—Cs1—O12	134.87 (6)	Cs1i—O1W—H11W	123 (3)
O1W—Cs1—O12i	70.44 (5)	Cs1iv—O1W—H11W	108 (3)
O1W—Cs1—O1Wii	93.43 (6)	Cs1i—O1W—H12W	90 (3)
O1W—Cs1—O32iii	149.39 (6)	Cs1iv—O1W—H12W	75 (3)
O1W—Cs1—O1Wiv	80.87 (6)	Cs1—O1W—H11W	83 (2)
O1W—Cs1—O52v	60.79 (6)	H21W—O2W—H22W	105 (3)
O2W—Cs1—O12	131.87 (5)	Cs1—O2W—H22W	131 (2)
O2W—Cs1—O12i	120.39 (5)	Cs1—O2W—H21W	122 (2)
O1Wii—Cs1—O2W	64.41 (6)	O32—N3—C3	117.8 (2)
O2W—Cs1—O32iii	112.44 (6)	O31—N3—C3	118.5 (2)
O1Wiv—Cs1—O2W	93.38 (6)	O31—N3—O32	123.7 (3)
O2W—Cs1—O52v	55.78 (6)	O51—N5—O52	124.1 (2)
O12—Cs1—O12i	94.64 (4)	O51—N5—C5	117.8 (2)
O1Wii—Cs1—O12	67.47 (5)	O52—N5—C5	118.0 (2)
O12—Cs1—O32iii	75.75 (5)	C6—C1—C11	119.9 (2)
O1Wiv—Cs1—O12	55.02 (5)	C2—C1—C6	119.5 (2)
O12—Cs1—O52v	164.29 (6)	C2—C1—C11	120.5 (2)
O1Wii—Cs1—O12i	135.75 (6)	C1—C2—C3	119.3 (2)
O12i—Cs1—O32iii	113.90 (5)	C2—C3—C4	122.8 (3)
O1Wiv—Cs1—O12i	85.35 (5)	N3—C3—C2	119.4 (2)
O12i—Cs1—O52v	90.21 (5)	N3—C3—C4	117.7 (2)
O1Wii—Cs1—O32iii	100.85 (5)	C3—C4—C5	116.3 (2)
O1Wii—Cs1—O1Wiv	50.88 (6)	C4—C5—C6	123.6 (2)
O1Wii—Cs1—O52v	118.15 (5)	N5—C5—C6	118.0 (3)
O1Wiv—Cs1—O32iii	128.87 (5)	N5—C5—C4	118.4 (2)
O32iii—Cs1—O52v	88.62 (5)	C1—C6—C5	118.4 (3)
O1Wiv—Cs1—O52v	140.47 (5)	O11—C11—O12	126.9 (2)
Cs1—O1W—Cs1i	93.43 (6)	O11—C11—C1	116.5 (2)
Cs1—O1W—Cs1iv	99.13 (6)	O12—C11—C1	116.6 (2)
Cs1i—O1W—Cs1iv	129.12 (7)	C1—C2—H2	120.00
Cs1—O12—C11	115.28 (13)	C3—C2—H2	120.00
Cs1—O12—Cs1ii	94.64 (5)	C3—C4—H4	122.00
Cs1ii—O12—C11	149.86 (14)	C5—C4—H4	122.00
Cs1vi—O32—N3	148.16 (18)	C1—C6—H6	121.00
Cs1vii—O52—N5	117.78 (15)	C5—C6—H6	121.00
Cs1—O1W—H12W	174 (3)
O2W—Cs1—O1W—Cs1i	−127.44 (9)	O1W—Cs1—O1Wiv—Cs1iv	0.00 (6)
O2W—Cs1—O1W—Cs1iv	102.04 (8)	O2W—Cs1—O1Wiv—Cs1iv	−49.33 (6)
O12—Cs1—O1W—Cs1i	118.81 (6)	O12—Cs1—O1Wiv—Cs1iv	169.89 (8)
O12—Cs1—O1W—Cs1iv	−11.71 (9)	O1W—Cs1—O52v—N5v	−167.08 (18)
O12i—Cs1—O1W—Cs1i	42.25 (5)	O2W—Cs1—O52v—N5v	−106.86 (18)
O12i—Cs1—O1W—Cs1iv	−88.27 (6)	Cs1—O12—C11—O11	122.9 (2)
O1Wii—Cs1—O1W—Cs1i	179.98 (9)	Cs1—O12—C11—C1	−57.0 (3)
O1Wii—Cs1—O1W—Cs1iv	49.48 (6)	Cs1ii—O12—C11—O11	−49.7 (5)
O32iii—Cs1—O1W—Cs1i	−61.86 (12)	Cs1ii—O12—C11—C1	130.5 (3)
O32iii—Cs1—O1W—Cs1iv	167.61 (7)	Cs1vi—O32—N3—O31	−0.6 (4)
O1Wiv—Cs1—O1W—Cs1i	130.53 (6)	Cs1vi—O32—N3—C3	179.48 (19)
O1Wiv—Cs1—O1W—Cs1iv	−0.02 (12)	Cs1vii—O52—N5—O51	12.2 (3)
O52v—Cs1—O1W—Cs1i	−59.47 (6)	Cs1vii—O52—N5—C5	−169.48 (15)
O52v—Cs1—O1W—Cs1iv	170.01 (8)	O31—N3—C3—C2	−11.0 (3)
O1W—Cs1—O12—C11	−63.1 (2)	O31—N3—C3—C4	167.3 (2)
O1W—Cs1—O12—Cs1ii	113.15 (7)	O32—N3—C3—C2	169.0 (2)
O2W—Cs1—O12—C11	−135.23 (18)	O32—N3—C3—C4	−12.7 (3)
O2W—Cs1—O12—Cs1ii	41.03 (9)	O51—N5—C5—C4	8.4 (3)
O12i—Cs1—O12—C11	3.7 (2)	O51—N5—C5—C6	−172.0 (2)
O12i—Cs1—O12—Cs1ii	−180.00 (7)	O52—N5—C5—C4	−170.0 (2)
O1Wii—Cs1—O12—C11	−134.4 (2)	O52—N5—C5—C6	9.6 (3)
O1Wii—Cs1—O12—Cs1ii	41.90 (6)	C6—C1—C2—C3	−0.5 (3)
O32iii—Cs1—O12—C11	117.2 (2)	C11—C1—C2—C3	−179.6 (2)
O32iii—Cs1—O12—Cs1ii	−66.50 (5)	C2—C1—C6—C5	1.5 (3)
O1Wiv—Cs1—O12—C11	−77.3 (2)	C11—C1—C6—C5	−179.4 (2)
O1Wiv—Cs1—O12—Cs1ii	98.99 (7)	C2—C1—C11—O11	158.1 (2)
O1W—Cs1—O12i—Cs1i	−43.76 (6)	C2—C1—C11—O12	−22.1 (3)
O1W—Cs1—O12i—C11i	129.5 (4)	C6—C1—C11—O11	−21.0 (3)
O2W—Cs1—O12i—Cs1i	−34.52 (8)	C6—C1—C11—O12	158.9 (2)
O2W—Cs1—O12i—C11i	138.7 (4)	C1—C2—C3—N3	177.0 (2)
O12—Cs1—O12i—Cs1i	180.00 (7)	C1—C2—C3—C4	−1.2 (4)
O12—Cs1—O12i—C11i	−6.8 (4)	N3—C3—C4—C5	−176.4 (2)
O1W—Cs1—O1Wii—Cs1ii	179.98 (9)	C2—C3—C4—C5	1.9 (4)
O2W—Cs1—O1Wii—Cs1ii	137.03 (8)	C3—C4—C5—N5	178.7 (2)
O12—Cs1—O1Wii—Cs1ii	−42.25 (5)	C3—C4—C5—C6	−0.9 (4)
O1W—Cs1—O32iii—N3iii	−174.4 (3)	N5—C5—C6—C1	179.7 (2)
O2W—Cs1—O32iii—N3iii	−124.7 (3)	C4—C5—C6—C1	−0.8 (4)
O12—Cs1—O32iii—N3iii	5.1 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11W···O2W	0.80 (4)	1.98 (4)	2.734 (3)	159 (3)
O1W—H12W···O12iv	0.83 (4)	2.25 (4)	3.016 (3)	155 (4)
O2W—H21W···O11viii	0.83 (4)	1.94 (4)	2.764 (3)	174 (3)
O2W—H22W···O11ix	0.85 (4)	1.96 (4)	2.797 (3)	168 (3)

Table 1

Selected bond lengths (Å)

Cs1—O1W	3.087 (2)
Cs1—O2W	3.282 (2)
Cs1—O12	3.1751 (16)
Cs1—O12i	3.1120 (17)
Cs1—O1W ii	3.261 (2)
Cs1—O32iii	3.244 (2)
Cs1—O1W iv	3.346 (2)
Cs1—O52v	3.271 (2)

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

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H11W⋯O2W	0.80 (4)	1.98 (4)	2.734 (3)	159 (3)
O1W—H12W⋯O12iv	0.83 (4)	2.25 (4)	3.016 (3)	155 (4)
O2W—H21W⋯O11vi	0.83 (4)	1.94 (4)	2.764 (3)	174 (3)
O2W—H22W⋯O11vii	0.85 (4)	1.96 (4)	2.797 (3)	168 (3)

Symmetry codes: (iv) ; (vi) ; (vii) .