Poly[(μ-2-hy-droxy-3,5-dinitro-benzoato)rubidium].

The asymmetric unit of the title compound, [Rb(C(7)H(3)N(2)O(7))](n), comprises an Rb(+) cation and a 3,5-dinitro-salicylate ligand. The Rb(+) cation is 10-coordinated by O atoms from eight 3,5-dinitro-salicylate anions and is linked by three μ(2)-O atoms, forming a zigzag chain along the b-axis direction, which is further linked by the phenyl groups, giving the three-dimensional framework. The crystal structure involves intra-anionic O-H⋯O hydrogen bonds and strong π-π stacking inter-actions [centroid-centroid distance = 3.6755 (7) Å].

Related literature

For 3,5-dinitro­salicylate complexes, see: Hu et al. (2005 ▶); Song et al. (2007 ▶, 2008 ▶). For Rb–O bond lengths, see: Cametti et al. (2005 ▶).

Experimental

Crystal data

[Rb(C7H3N2O7)]

M = 312.58

Monoclinic,

a = 7.5957 (15) Å

b = 7.2971 (15) Å

c = 17.036 (3) Å

β = 95.10 (3)°

V = 940.5 (3) Å3

Z = 4

Mo Kα radiation

μ = 5.30 mm−1

T = 293 K

0.64 × 0.60 × 0.20 mm

Data collection

Bruker SMART CCD diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.219, T max = 0.548

8781 measured reflections

1715 independent reflections

1548 reflections with I > 2σ(I)

R int = 0.065

Refinement

R[F 2 > 2σ(F 2)] = 0.044

wR(F 2) = 0.107

S = 1.07

1715 reflections

154 parameters

H-atom parameters constrained

Δρmax = 0.59 e Å−3

Δρmin = −1.28 e Å−3

Data collection: SMART (Bruker, 2002 ▶); cell refinement: SAINT (Bruker, 2002 ▶); 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/S1600536811008476/om2407sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811008476/om2407Isup2.hkl

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

[Rb(C7H3N2O7)]	F(000) = 608
Mr = 312.58	Dx = 2.208 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 3447 reflections
a = 7.5957 (15) Å	θ = 3.0–25.4°
b = 7.2971 (15) Å	µ = 5.30 mm−1
c = 17.036 (3) Å	T = 293 K
β = 95.10 (3)°	Block, yellow
V = 940.5 (3) Å3	0.64 × 0.60 × 0.20 mm
Z = 4

Bruker SMART CCD diffractometer	1715 independent reflections
Radiation source: fine-focus sealed tube	1548 reflections with I > 2σ(I)
graphite	Rint = 0.065
φ and ω scans	θmax = 25.4°, θmin = 3.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→9
Tmin = 0.219, Tmax = 0.548	k = −7→8
8781 measured reflections	l = −18→20

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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107	H-atom parameters constrained
S = 1.07	w = 1/[σ2(Fo2) + (0.0621P)2] where P = (Fo2 + 2Fc2)/3
1715 reflections	(Δ/σ)max = 0.001
154 parameters	Δρmax = 0.59 e Å−3
0 restraints	Δρmin = −1.28 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
Rb1	1.61252 (5)	1.14921 (5)	0.20167 (2)	0.0369 (2)
C1	1.2759 (5)	0.8926 (5)	0.1057 (2)	0.0273 (8)
C2	1.1105 (5)	0.8137 (5)	0.0645 (2)	0.0242 (8)
C3	1.0990 (5)	0.7877 (5)	−0.0199 (2)	0.0241 (8)
C4	0.9370 (5)	0.7063 (5)	−0.0527 (2)	0.0247 (8)
C5	0.8025 (5)	0.6593 (4)	−0.0081 (2)	0.0251 (8)
H5	0.6998	0.6056	−0.0314	0.030*
C6	0.8215 (5)	0.6929 (5)	0.0721 (2)	0.0248 (8)
C7	0.9735 (5)	0.7708 (5)	0.1085 (2)	0.0240 (8)
H7	0.9826	0.7939	0.1624	0.029*
N1	0.9095 (5)	0.6663 (4)	−0.13724 (19)	0.0310 (8)
N2	0.6787 (5)	0.6448 (4)	0.1190 (2)	0.0335 (8)
O1	1.2938 (4)	0.9117 (4)	0.17699 (15)	0.0361 (7)
O2	1.3980 (3)	0.9418 (4)	0.06105 (15)	0.0377 (7)
O3	1.0271 (5)	0.6878 (6)	−0.17888 (19)	0.0680 (11)
O4	0.7641 (5)	0.6080 (5)	−0.16227 (18)	0.0562 (9)
O5	0.5666 (4)	0.5376 (5)	0.09310 (19)	0.0554 (9)
O6	0.6775 (4)	0.7154 (5)	0.18481 (17)	0.0500 (8)
O7	1.2245 (4)	0.8369 (4)	−0.05933 (16)	0.0356 (7)
H7A	1.3073	0.8813	−0.0282	0.053*

	U11	U22	U33	U12	U13	U23
Rb1	0.0346 (3)	0.0485 (3)	0.0288 (3)	−0.01148 (17)	0.0097 (2)	−0.00679 (15)
C1	0.022 (2)	0.0290 (18)	0.031 (2)	−0.0011 (16)	0.0012 (16)	0.0035 (15)
C2	0.023 (2)	0.0228 (17)	0.027 (2)	−0.0013 (15)	0.0019 (16)	0.0008 (14)
C3	0.025 (2)	0.0243 (17)	0.0238 (18)	0.0021 (16)	0.0059 (15)	0.0050 (15)
C4	0.031 (2)	0.0272 (18)	0.0160 (17)	0.0016 (16)	0.0020 (15)	0.0024 (14)
C5	0.020 (2)	0.0239 (18)	0.031 (2)	−0.0034 (14)	−0.0018 (16)	0.0013 (14)
C6	0.021 (2)	0.0265 (17)	0.028 (2)	−0.0020 (15)	0.0036 (15)	0.0017 (15)
C7	0.027 (2)	0.0227 (17)	0.0233 (17)	−0.0006 (15)	0.0049 (15)	0.0017 (14)
N1	0.032 (2)	0.0367 (19)	0.0237 (17)	−0.0022 (14)	0.0004 (16)	0.0025 (13)
N2	0.026 (2)	0.042 (2)	0.033 (2)	−0.0057 (15)	0.0073 (16)	0.0027 (14)
O1	0.0316 (16)	0.0488 (17)	0.0275 (15)	−0.0104 (14)	0.0005 (12)	−0.0017 (12)
O2	0.0226 (14)	0.0557 (18)	0.0351 (15)	−0.0144 (14)	0.0048 (11)	0.0052 (13)
O3	0.042 (2)	0.136 (4)	0.0265 (17)	−0.015 (2)	0.0110 (16)	−0.0129 (18)
O4	0.054 (2)	0.086 (2)	0.0274 (16)	−0.0344 (19)	−0.0043 (15)	−0.0013 (15)
O5	0.0378 (18)	0.070 (2)	0.060 (2)	−0.0309 (17)	0.0149 (15)	−0.0087 (17)
O6	0.0384 (19)	0.086 (2)	0.0284 (16)	−0.0061 (17)	0.0174 (13)	−0.0040 (16)
O7	0.0283 (17)	0.0526 (18)	0.0267 (15)	−0.0122 (12)	0.0067 (12)	0.0018 (11)

Rb1—O7i	2.821 (3)	C5—C6	1.383 (5)
Rb1—O1ii	2.861 (3)	C5—H5	0.9300
Rb1—O1	2.977 (3)	C6—C7	1.383 (5)
Rb1—O3i	3.041 (4)	C6—N2	1.447 (5)
Rb1—O6iii	3.096 (3)	C7—H7	0.9300
Rb1—O4iv	3.122 (3)	N1—O3	1.199 (5)
Rb1—O2	3.161 (3)	N1—O4	1.224 (4)
Rb1—O6v	3.221 (4)	N2—O5	1.210 (4)
Rb1—O4vi	3.381 (4)	N2—O6	1.234 (4)
Rb1—O5vii	3.385 (4)	O1—Rb1viii	2.861 (3)
C1—O1	1.218 (4)	O3—Rb1i	3.041 (4)
C1—O2	1.301 (5)	O4—Rb1ix	3.122 (3)
C1—C2	1.498 (5)	O4—Rb1vi	3.381 (4)
C2—C7	1.371 (5)	O5—Rb1x	3.385 (4)
C2—C3	1.446 (5)	O6—Rb1xi	3.096 (3)
C3—O7	1.266 (5)	O6—Rb1xii	3.221 (4)
C3—C4	1.434 (5)	O7—Rb1i	2.821 (3)
C4—C5	1.370 (5)	O7—H7A	0.8500
C4—N1	1.465 (5)
O7i—Rb1—O1ii	119.80 (8)	O4vi—Rb1—O5vii	53.74 (8)
O7i—Rb1—O1	108.25 (8)	O1—C1—O2	122.0 (3)
O1ii—Rb1—O1	129.70 (4)	O1—C1—C2	121.7 (3)
O7i—Rb1—O3i	53.65 (9)	O2—C1—C2	116.4 (3)
O1ii—Rb1—O3i	70.22 (9)	C7—C2—C3	122.1 (3)
O1—Rb1—O3i	160.00 (9)	C7—C2—C1	118.5 (3)
O7i—Rb1—O6iii	157.29 (9)	C3—C2—C1	119.4 (3)
O1ii—Rb1—O6iii	65.76 (9)	O7—C3—C4	124.8 (3)
O1—Rb1—O6iii	64.16 (8)	O7—C3—C2	120.6 (3)
O3i—Rb1—O6iii	135.84 (10)	C4—C3—C2	114.6 (3)
O7i—Rb1—O4iv	119.92 (9)	C5—C4—C3	122.9 (3)
O1ii—Rb1—O4iv	79.29 (9)	C5—C4—N1	116.5 (3)
O1—Rb1—O4iv	89.80 (9)	C3—C4—N1	120.6 (3)
O3i—Rb1—O4iv	93.04 (11)	C4—C5—C6	119.1 (3)
O6iii—Rb1—O4iv	82.29 (9)	C4—C5—H5	120.4
O7i—Rb1—O2	66.53 (7)	C6—C5—H5	120.4
O1ii—Rb1—O2	161.17 (8)	C5—C6—C7	121.7 (4)
O1—Rb1—O2	41.94 (7)	C5—C6—N2	119.0 (3)
O3i—Rb1—O2	119.98 (8)	C7—C6—N2	119.2 (3)
O6iii—Rb1—O2	101.58 (8)	C2—C7—C6	119.5 (3)
O4iv—Rb1—O2	113.97 (9)	C2—C7—H7	120.3
O7i—Rb1—O6v	82.90 (7)	C6—C7—H7	120.3
O1ii—Rb1—O6v	133.80 (8)	O3—N1—O4	122.4 (3)
O1—Rb1—O6v	62.88 (8)	O3—N1—C4	120.4 (3)
O3i—Rb1—O6v	103.08 (10)	O4—N1—C4	117.2 (3)
O6iii—Rb1—O6v	109.40 (9)	O5—N2—O6	122.6 (3)
O4iv—Rb1—O6v	54.97 (8)	O5—N2—C6	119.5 (3)
O2—Rb1—O6v	62.26 (8)	O6—N2—C6	117.9 (3)
O7i—Rb1—O4vi	103.81 (8)	C1—O1—Rb1viii	130.0 (3)
O1ii—Rb1—O4vi	86.82 (8)	C1—O1—Rb1	103.0 (2)
O1—Rb1—O4vi	67.29 (9)	Rb1viii—O1—Rb1	98.09 (8)
O3i—Rb1—O4vi	121.68 (10)	C1—O2—Rb1	92.0 (2)
O6iii—Rb1—O4vi	53.55 (8)	N1—O3—Rb1i	148.5 (3)
O4iv—Rb1—O4vi	135.41 (5)	N1—O4—Rb1ix	136.8 (3)
O2—Rb1—O4vi	74.36 (8)	N1—O4—Rb1vi	127.5 (3)
O6v—Rb1—O4vi	129.12 (8)	Rb1ix—O4—Rb1vi	85.29 (8)
O7i—Rb1—O5vii	62.09 (8)	N2—O5—Rb1x	107.8 (3)
O1ii—Rb1—O5vii	80.87 (8)	N2—O6—Rb1xi	124.4 (2)
O1—Rb1—O5vii	111.55 (8)	N2—O6—Rb1xii	120.3 (2)
O3i—Rb1—O5vii	69.70 (10)	Rb1xi—O6—Rb1xii	88.53 (8)
O6iii—Rb1—O5vii	99.57 (8)	C3—O7—Rb1i	151.1 (2)
O4iv—Rb1—O5vii	157.25 (9)	C3—O7—H7A	109.0
O2—Rb1—O5vii	88.03 (8)	Rb1i—O7—H7A	99.6
O6v—Rb1—O5vii	141.57 (7)

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O2	0.85	1.67	2.459 (4)	153

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O2	0.85	1.67	2.459 (4)	153