Poly[μ(3)-aqua-μ(2)-2,4-dinitro-phenolato-rubidium(I)].

The asymmetric unit of the title compound, [Rb(C(6)H(3)N(2)O(5))(H(2)O)](n), comprises a rubidium cation, a 2,4-dinitro-phenoxide anion and a water mol-ecule. The Rb(+) cation is 11-coordinated by O atoms from 2,4-dinitro-phenolate anions and water mol-ecules. The metal centre is firstly coordinated by two μ(3)-H(2)O to form a one-dimensional ladder-shaped unit, [Rb(2)(μ(3)-H(2)O)(2)], which is further linked by 2,4-dinitro-phenolate to give the three-dimensional framework of the title compound. The crystal structure involves O-H⋯O hydrogen bonds.

Related literature

For related literature, see: Abrahams et al. (1998 ▶); Brill et al. (2000 ▶); Cametti et al. (2005 ▶); Cole & Holt (1986 ▶); Devi & Vidyasagar (2000 ▶); Harrowfield et al. (1995 ▶); Hu et al. (2005 ▶); Klaui et al. (1987 ▶); Shannon (1976 ▶); von Prondzinski et al. (2007 ▶); Weinert et al. (2003 ▶).

Experimental

Crystal data

[Rb(C6H3N2O5)(H2O)]

M = 286.59

Monoclinic,

a = 5.8519 (18) Å

b = 20.846 (7) Å

c = 7.412 (2) Å

β = 93.148 (5)°

V = 902.8 (5) Å3

Z = 4

Mo Kα radiation

μ = 5.50 mm−1

T = 293 (2) K

0.40 × 0.35 × 0.30 mm

Data collection

Bruker APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.125, T max = 0.202

4449 measured reflections

1599 independent reflections

1214 reflections with I > 2σ(I)

R int = 0.063

Refinement

R[F 2 > 2σ(F 2)] = 0.037

wR(F 2) = 0.101

S = 1.00

1599 reflections

143 parameters

3 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.50 e Å−3

Δρmin = −0.71 e Å−3

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: APEX2; data reduction: SAINT (Bruker, 2005 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a ▶); molecular graphics: SHELXTL (Sheldrick, 1997b ▶) and DIAMOND (Brandenburg & Brendt, 2001 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807066792/pk2074sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807066792/pk2074Isup2.hkl

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

[Rb(C6H3N2O5)(H2O)]	F000 = 560
Mr = 286.59	Dx = 2.109 Mg m−3
Monoclinic, P21/c	Mo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1599 reflections
a = 5.8519 (18) Å	θ = 2.0–25.1º
b = 20.846 (7) Å	µ = 5.50 mm−1
c = 7.412 (2) Å	T = 293 (2) K
β = 93.148 (5)º	Block, yellow
V = 902.8 (5) Å3	0.40 × 0.35 × 0.30 mm
Z = 4

Bruker APEXII CCD area-detector diffractometer	1599 independent reflections
Radiation source: fine-focus sealed tube	1214 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.063
T = 293(2) K	θmax = 25.1º
φ and ω scans	θmin = 2.0º
Absorption correction: multi-scan(SADABS; Sheldrick, 1996)	h = −6→6
Tmin = 0.125, Tmax = 0.202	k = −20→24
4449 measured reflections	l = −7→8

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.101	w = 1/[σ2(Fo2) + (0.0556P)2 + 0.12P] where P = (Fo2 + 2Fc2)/3
S = 1.00	(Δ/σ)max = 0.002
1599 reflections	Δρmax = 0.50 e Å−3
143 parameters	Δρmin = −0.71 e Å−3
3 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997a), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0120 (18)

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 > 2σ(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	0.18947 (8)	1.00955 (2)	0.24241 (6)	0.0381 (2)
O1	−0.0671 (5)	0.91314 (15)	0.4428 (4)	0.0404 (8)
O2	0.3775 (6)	0.93503 (16)	0.5483 (5)	0.0580 (11)
O3	0.5150 (5)	0.86504 (16)	0.7365 (4)	0.0456 (9)
O4	0.3512 (6)	0.64498 (16)	0.6287 (5)	0.0537 (10)
O5	0.0559 (6)	0.61696 (16)	0.4603 (5)	0.0562 (10)
O6	0.3268 (7)	1.03788 (18)	−0.1415 (5)	0.0526 (9)
H6A	0.382 (10)	1.0686 (17)	−0.086 (6)	0.079*
H6B	0.281 (10)	1.053 (2)	−0.239 (4)	0.079*
N1	0.3753 (6)	0.88137 (18)	0.6150 (5)	0.0331 (9)
N2	0.1790 (7)	0.65827 (18)	0.5345 (5)	0.0373 (9)
C1	−0.0063 (7)	0.8557 (2)	0.4619 (5)	0.0290 (10)
C2	0.2080 (7)	0.8349 (2)	0.5482 (5)	0.0261 (10)
C3	0.2641 (7)	0.7709 (2)	0.5735 (5)	0.0269 (10)
H3	0.4019	0.7594	0.6333	0.032*
C4	0.1145 (7)	0.7246 (2)	0.5096 (5)	0.0289 (10)
C5	−0.0968 (7)	0.7407 (2)	0.4243 (6)	0.0346 (11)
H5	−0.1973	0.7088	0.3830	0.042*
C6	−0.1537 (7)	0.8033 (2)	0.4023 (6)	0.0357 (11)
H6	−0.2952	0.8131	0.3458	0.043*

	U11	U22	U33	U12	U13	U23
Rb1	0.0429 (3)	0.0320 (4)	0.0387 (3)	−0.0036 (2)	−0.0061 (2)	0.00384 (19)
O1	0.0411 (18)	0.029 (2)	0.050 (2)	0.0061 (15)	−0.0026 (16)	0.0050 (15)
O2	0.069 (2)	0.030 (2)	0.071 (3)	−0.0178 (18)	−0.032 (2)	0.0149 (18)
O3	0.0428 (19)	0.038 (2)	0.054 (2)	−0.0031 (15)	−0.0188 (17)	0.0056 (16)
O4	0.067 (2)	0.031 (2)	0.061 (3)	0.0131 (17)	−0.016 (2)	0.0011 (17)
O5	0.067 (2)	0.028 (2)	0.073 (3)	−0.0102 (18)	−0.003 (2)	−0.0112 (18)
O6	0.054 (2)	0.050 (2)	0.053 (2)	−0.005 (2)	−0.0014 (19)	0.0058 (19)
N1	0.032 (2)	0.031 (2)	0.036 (2)	−0.0009 (17)	−0.0042 (17)	0.0016 (17)
N2	0.049 (2)	0.026 (2)	0.038 (2)	−0.0007 (18)	0.0042 (19)	−0.0026 (17)
C1	0.029 (2)	0.030 (3)	0.028 (3)	0.0015 (19)	0.0013 (19)	0.0044 (19)
C2	0.026 (2)	0.023 (2)	0.029 (2)	−0.0053 (17)	−0.0047 (18)	−0.0001 (17)
C3	0.027 (2)	0.031 (3)	0.022 (2)	0.0001 (19)	−0.0010 (18)	0.0022 (18)
C4	0.036 (2)	0.023 (2)	0.027 (2)	0.000 (2)	0.0044 (18)	−0.0015 (18)
C5	0.035 (2)	0.035 (3)	0.034 (3)	−0.006 (2)	−0.001 (2)	−0.003 (2)
C6	0.027 (2)	0.045 (3)	0.035 (3)	0.001 (2)	−0.0053 (19)	−0.005 (2)

Rb1—O2	2.914 (3)	O4—Rb1vii	3.474 (4)
Rb1—O1i	2.956 (3)	O5—N2	1.232 (5)
Rb1—O1	2.957 (3)	O5—Rb1viii	3.016 (3)
Rb1—O5ii	3.016 (3)	O5—Rb1vii	3.429 (4)
Rb1—O6	3.057 (4)	O6—Rb1iv	3.127 (4)
Rb1—O2iii	3.119 (3)	O6—Rb1v	3.228 (4)
Rb1—O6iv	3.127 (4)	O6—H6A	0.818 (10)
Rb1—O3iii	3.134 (3)	O6—H6B	0.820 (10)
Rb1—O6v	3.228 (4)	N1—C2	1.446 (5)
Rb1—O5vi	3.429 (4)	N1—Rb1iii	3.533 (4)
Rb1—O4vi	3.474 (4)	N2—C4	1.443 (5)
Rb1—N1iii	3.533 (4)	C1—C2	1.443 (5)
Rb1—H6A	3.00 (5)	C1—C6	1.446 (6)
O1—C1	1.255 (5)	C2—C3	1.384 (6)
O1—Rb1i	2.956 (3)	C3—C4	1.369 (6)
O2—N1	1.223 (5)	C3—H3	0.9300
O2—Rb1iii	3.119 (3)	C4—C5	1.398 (6)
O3—N1	1.231 (4)	C5—C6	1.353 (6)
O3—Rb1iii	3.134 (3)	C5—H5	0.9300
O4—N2	1.226 (5)	C6—H6	0.9300
O2—Rb1—O1i	76.94 (10)	O6v—Rb1—N1iii	156.48 (9)
O2—Rb1—O1	55.06 (9)	O5vi—Rb1—N1iii	144.49 (9)
O1i—Rb1—O1	79.77 (10)	O4vi—Rb1—N1iii	117.89 (9)
O2—Rb1—O5ii	158.84 (11)	O2—Rb1—H6A	135.0 (11)
O1i—Rb1—O5ii	81.90 (10)	O1i—Rb1—H6A	122.3 (6)
O1—Rb1—O5ii	120.93 (10)	O1—Rb1—H6A	155.4 (2)
O2—Rb1—O6	136.06 (12)	O5ii—Rb1—H6A	58.7 (11)
O1i—Rb1—O6	135.80 (9)	O6—Rb1—H6A	15.5 (2)
O1—Rb1—O6	139.96 (10)	O2iii—Rb1—H6A	85.5 (6)
O5ii—Rb1—O6	62.29 (11)	O6iv—Rb1—H6A	63.4 (11)
O2—Rb1—O2iii	63.18 (11)	O3iii—Rb1—H6A	57.8 (2)
O1i—Rb1—O2iii	68.35 (10)	O6v—Rb1—H6A	109.0 (8)
O1—Rb1—O2iii	115.03 (9)	O5vi—Rb1—H6A	84.5 (3)
O5ii—Rb1—O2iii	108.92 (10)	O4vi—Rb1—H6A	93.7 (8)
O6—Rb1—O2iii	98.24 (10)	N1iii—Rb1—H6A	71.5 (4)
O2—Rb1—O6iv	73.11 (11)	C1—O1—Rb1i	120.7 (3)
O1i—Rb1—O6iv	128.52 (9)	C1—O1—Rb1	123.8 (3)
O1—Rb1—O6iv	113.35 (9)	Rb1i—O1—Rb1	100.23 (10)
O5ii—Rb1—O6iv	121.87 (11)	N1—O2—Rb1	142.2 (3)
O6—Rb1—O6iv	63.31 (11)	N1—O2—Rb1iii	99.5 (2)
O2iii—Rb1—O6iv	60.97 (10)	Rb1—O2—Rb1iii	116.82 (11)
O2—Rb1—O3iii	102.84 (9)	N1—O3—Rb1iii	98.5 (2)
O1i—Rb1—O3iii	70.30 (9)	N2—O4—Rb1vii	97.0 (3)
O1—Rb1—O3iii	146.73 (9)	N2—O5—Rb1viii	172.5 (3)
O5ii—Rb1—O3iii	69.62 (9)	N2—O5—Rb1vii	99.1 (3)
O6—Rb1—O3iii	73.29 (9)	Rb1viii—O5—Rb1vii	79.58 (8)
O2iii—Rb1—O3iii	40.11 (8)	Rb1—O6—Rb1iv	116.69 (11)
O6iv—Rb1—O3iii	76.78 (9)	Rb1—O6—Rb1v	82.29 (9)
O2—Rb1—O6v	109.00 (9)	Rb1iv—O6—Rb1v	134.09 (13)
O1i—Rb1—O6v	94.91 (10)	Rb1—O6—H6A	78 (4)
O1—Rb1—O6v	54.09 (9)	Rb1iv—O6—H6A	92 (4)
O5ii—Rb1—O6v	72.43 (10)	Rb1v—O6—H6A	134 (4)
O6—Rb1—O6v	97.71 (9)	Rb1—O6—H6B	144 (4)
O2iii—Rb1—O6v	162.41 (11)	Rb1iv—O6—H6B	100 (4)
O6iv—Rb1—O6v	134.09 (13)	Rb1v—O6—H6B	70 (4)
O3iii—Rb1—O6v	140.73 (9)	H6A—O6—H6B	104.1 (17)
O2—Rb1—O5vi	97.36 (9)	O2—N1—O3	121.8 (4)
O1i—Rb1—O5vi	147.52 (9)	O2—N1—C2	119.8 (3)
O1—Rb1—O5vi	71.24 (9)	O3—N1—C2	118.4 (4)
O5ii—Rb1—O5vi	100.42 (8)	O2—N1—Rb1iii	60.6 (2)
O6—Rb1—O5vi	69.13 (9)	O3—N1—Rb1iii	61.3 (2)
O2iii—Rb1—O5vi	137.72 (10)	C2—N1—Rb1iii	176.1 (3)
O6iv—Rb1—O5vi	77.88 (10)	O4—N2—O5	122.6 (4)
O3iii—Rb1—O5vi	141.14 (9)	O4—N2—C4	119.4 (4)
O6v—Rb1—O5vi	56.22 (10)	O5—N2—C4	118.1 (4)
O2—Rb1—O4vi	66.31 (9)	O1—C1—C2	124.8 (4)
O1i—Rb1—O4vi	141.08 (9)	O1—C1—C6	121.7 (4)
O1—Rb1—O4vi	69.16 (9)	C2—C1—C6	113.4 (4)
O5ii—Rb1—O4vi	134.11 (9)	C3—C2—C1	123.0 (4)
O6—Rb1—O4vi	82.20 (10)	C3—C2—N1	116.7 (3)
O2iii—Rb1—O4vi	103.85 (9)	C1—C2—N1	120.4 (4)
O6iv—Rb1—O4vi	52.17 (9)	C4—C3—C2	119.3 (4)
O3iii—Rb1—O4vi	128.95 (9)	C4—C3—H3	120.3
O6v—Rb1—O4vi	85.63 (9)	C2—C3—H3	120.3
O5vi—Rb1—O4vi	36.39 (8)	C3—C4—C5	121.3 (4)
O2—Rb1—N1iii	82.82 (9)	C3—C4—N2	118.2 (4)
O1i—Rb1—N1iii	67.35 (9)	C5—C4—N2	120.5 (4)
O1—Rb1—N1iii	131.67 (9)	C6—C5—C4	119.5 (4)
O5ii—Rb1—N1iii	89.25 (10)	C6—C5—H5	120.3
O6—Rb1—N1iii	86.10 (9)	C4—C5—H5	120.3
O2iii—Rb1—N1iii	19.97 (8)	C5—C6—C1	123.5 (4)
O6iv—Rb1—N1iii	68.15 (9)	C5—C6—H6	118.2
O3iii—Rb1—N1iii	20.16 (8)	C1—C6—H6	118.2
O2—Rb1—O1—C1	−57.1 (3)	O6v—Rb1—O6—Rb1iv	−135.87 (16)
O1i—Rb1—O1—C1	−138.2 (4)	O5vi—Rb1—O6—Rb1iv	−86.57 (13)
O5ii—Rb1—O1—C1	147.8 (3)	O4vi—Rb1—O6—Rb1iv	−51.39 (12)
O6—Rb1—O1—C1	65.2 (4)	N1iii—Rb1—O6—Rb1iv	67.47 (12)
O2iii—Rb1—O1—C1	−78.1 (3)	O2—Rb1—O6—Rb1v	127.89 (11)
O6iv—Rb1—O1—C1	−10.5 (3)	O1i—Rb1—O6—Rb1v	−105.25 (12)
O3iii—Rb1—O1—C1	−112.3 (3)	O1—Rb1—O6—Rb1v	40.64 (17)
O6v—Rb1—O1—C1	118.0 (4)	O5ii—Rb1—O6—Rb1v	−65.46 (10)
O5vi—Rb1—O1—C1	56.7 (3)	O2iii—Rb1—O6—Rb1v	−172.56 (9)
O4vi—Rb1—O1—C1	18.0 (3)	O6iv—Rb1—O6—Rb1v	135.87 (16)
N1iii—Rb1—O1—C1	−91.4 (3)	O3iii—Rb1—O6—Rb1v	−140.81 (10)
O2—Rb1—O1—Rb1i	81.14 (12)	O6v—Rb1—O6—Rb1v	0.0
O1i—Rb1—O1—Rb1i	0.0	O5vi—Rb1—O6—Rb1v	49.30 (8)
O5ii—Rb1—O1—Rb1i	−74.03 (13)	O4vi—Rb1—O6—Rb1v	84.48 (8)
O6—Rb1—O1—Rb1i	−156.60 (12)	N1iii—Rb1—O6—Rb1v	−156.66 (9)
O2iii—Rb1—O1—Rb1i	60.13 (12)	Rb1—O2—N1—O3	167.0 (4)
O6iv—Rb1—O1—Rb1i	127.69 (9)	Rb1iii—O2—N1—O3	3.2 (5)
O3iii—Rb1—O1—Rb1i	25.93 (19)	Rb1—O2—N1—C2	−11.7 (7)
O6v—Rb1—O1—Rb1i	−103.77 (13)	Rb1iii—O2—N1—C2	−175.5 (3)
O5vi—Rb1—O1—Rb1i	−165.14 (11)	Rb1—O2—N1—Rb1iii	163.8 (6)
O4vi—Rb1—O1—Rb1i	156.16 (11)	Rb1iii—O3—N1—O2	−3.2 (5)
N1iii—Rb1—O1—Rb1i	46.81 (14)	Rb1iii—O3—N1—C2	175.5 (3)
O1i—Rb1—O2—N1	125.8 (5)	Rb1vii—O4—N2—O5	−23.8 (5)
O1—Rb1—O2—N1	39.3 (5)	Rb1vii—O4—N2—C4	155.5 (3)
O5ii—Rb1—O2—N1	125.4 (5)	Rb1vii—O5—N2—O4	24.3 (5)
O6—Rb1—O2—N1	−89.1 (5)	Rb1vii—O5—N2—C4	−155.1 (3)
O2iii—Rb1—O2—N1	−162.0 (6)	Rb1i—O1—C1—C2	−70.6 (5)
O6iv—Rb1—O2—N1	−96.5 (5)	Rb1—O1—C1—C2	59.7 (5)
O3iii—Rb1—O2—N1	−168.2 (5)	Rb1i—O1—C1—C6	107.4 (4)
O6v—Rb1—O2—N1	35.1 (5)	Rb1—O1—C1—C6	−122.3 (4)
O5vi—Rb1—O2—N1	−21.6 (5)	O1—C1—C2—C3	177.1 (4)
O4vi—Rb1—O2—N1	−41.1 (5)	C6—C1—C2—C3	−1.0 (6)
N1iii—Rb1—O2—N1	−165.8 (5)	O1—C1—C2—N1	−2.2 (7)
O1i—Rb1—O2—Rb1iii	−72.12 (14)	C6—C1—C2—N1	179.7 (4)
O1—Rb1—O2—Rb1iii	−158.66 (19)	O2—N1—C2—C3	155.4 (4)
O5ii—Rb1—O2—Rb1iii	−72.6 (3)	O3—N1—C2—C3	−23.3 (6)
O6—Rb1—O2—Rb1iii	72.95 (19)	O2—N1—C2—C1	−25.2 (6)
O2iii—Rb1—O2—Rb1iii	0.0	O3—N1—C2—C1	156.0 (4)
O6iv—Rb1—O2—Rb1iii	65.50 (14)	C1—C2—C3—C4	2.1 (7)
O3iii—Rb1—O2—Rb1iii	−6.18 (17)	N1—C2—C3—C4	−178.6 (4)
O6v—Rb1—O2—Rb1iii	−162.86 (13)	C2—C3—C4—C5	−2.0 (6)
O5vi—Rb1—O2—Rb1iii	140.40 (14)	C2—C3—C4—N2	178.8 (4)
O4vi—Rb1—O2—Rb1iii	120.98 (17)	O4—N2—C4—C3	8.2 (6)
N1iii—Rb1—O2—Rb1iii	−3.78 (13)	O5—N2—C4—C3	−172.4 (4)
O2—Rb1—O6—Rb1iv	−8.0 (2)	O4—N2—C4—C5	−171.0 (4)
O1i—Rb1—O6—Rb1iv	118.88 (14)	O5—N2—C4—C5	8.3 (7)
O1—Rb1—O6—Rb1iv	−95.23 (16)	C3—C4—C5—C6	0.8 (7)
O5ii—Rb1—O6—Rb1iv	158.67 (17)	N2—C4—C5—C6	−180.0 (4)
O2iii—Rb1—O6—Rb1iv	51.57 (14)	C4—C5—C6—C1	0.3 (7)
O6iv—Rb1—O6—Rb1iv	0.0	O1—C1—C6—C5	−178.4 (4)
O3iii—Rb1—O6—Rb1iv	83.33 (12)	C2—C1—C6—C5	−0.2 (6)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6B···O1v	0.820 (10)	2.03 (2)	2.822 (5)	161 (6)
O6—H6A···O4ix	0.818 (10)	2.27 (4)	2.919 (5)	137 (5)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H6B⋯O1i	0.820 (10)	2.03 (2)	2.822 (5)	161 (6)
O6—H6A⋯O4ii	0.818 (10)	2.27 (4)	2.919 (5)	137 (5)

Symmetry codes: (i) ; (ii) .