Poly[μ3-aqua-μ2-2,4-dinitro­phenolato-rubidium(I)]

Yang, Z.; Hu, M.; Wang, X.

doi:10.1107/S1600536807066792

metal-organic compounds

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Volume 64| Part 1| January 2008| Page m225

https://doi.org/10.1107/S1600536807066792

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Poly[μ₃-aqua-μ₂-2,4-dinitrophenolato-rubidium(I)]

Zhangqin Yang,^a Mancheng Hu ^a ^* and Xiuhang Wang ^a

^aSchool of Chemistry and Materials Science, ShaanXi Normal University, Xi'an 710062, People's Republic of China
^*Correspondence e-mail: hmch@snnu.edu.cn

(Received 16 November 2007; accepted 13 December 2007; online 21 December 2007)

The asymmetric unit of the title compound, [Rb(C₆H₃N₂O₅)(H₂O)]_n, comprises a rubidium cation, a 2,4-dinitrophenoxide anion and a water molecule. The Rb⁺ cation is 11-coordinated by O atoms from 2,4-dinitrophenolate anions and water molecules. The metal centre is firstly coordinated by two μ₃-H₂O to form a one-dimensional ladder-shaped unit, [Rb₂(μ₃-H₂O)₂], which is further linked by 2,4-dinitrophenolate 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_r = 286.59
Monoclinic, P 2₁ /c
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[F² > 2σ(F²)] = 0.037
wR(F²) = 0.101
S = 1.00
1599 reflections
143 parameters
3 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.50 e Å⁻³
Δρ_min = −0.71 e Å⁻³

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) -x, -y+2, -z; (ii) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

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.

Supporting information

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

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536807066792/pk2074Isup2.hkl

checkCIF report

Comment top

Research on nitrogen-rich compounds is the focus of attention for their usage as energetic materials. Much work has concentrated on their alkaline or alkali-earth metal salts (Harrowfield et al., 1995; Cole and Holt, 1986; von Prondzinski et al., 2007), among which some polynitro-substituted phenoxide was found to be environment-friendly (Brill et al., 2000). Our group has already demonstrated the structure of caesium 2,4-dinitrophenolate (Mancheng Hu et al., 2005). Herein, we report its rubidium analogue [Rb(OC₆H₃N₂O₄).H₂O].

The asymmetric unit of the title compound comprises a rubidium cation, a 2,4-dinitrophenoxide anion and a water molecule. The central cation is coordinated to eleven O atoms (Fig. 1) with the Rb—O distances ranging from 2.914 (3) Å to 3.474 (4) Å, which are well within the range reported in the literature (Cametti et al., 2005; Shannon, 1976; Devi and Vidyasagar, 2000).

The metal center is firstly coordinated by two µ₃-H₂O to form a one-dimensional ladder-shape unit, [Rb₂(µ₃-H₂O)₂], which is further linked by 2,4-dinitrophenoxide to give the three-dimensional framework of the title compound. In the structure of [Rb₂(µ₃-H₂O)₂] fragment (Fig.2), each rubidium ion is connected to three oxygen atoms of the water, and each water molecule is connected to three rubidium ions. The Rb—O—Rb angle along the sides of the ladder is 134.09 (13) °. It should be noted that the triply bridging water has been found in several lighter group I metal complexes (Klaui et al., 1987; Abrahams et al., 1998). A similar extended ladder-like structure motif was also found in the structure of [Rb(OC₆H₃Ph₂-2,6)]_x (1) (Weinert et al., 2003), however, each Rb atom in 1 is not connected to three water molecules but three O atoms from phenoxide. The corresponding Rb—O—Rb angle in 1 is about 155.5 (1) °, which is markedly larger than in the title compound.

The [Rb₂(µ₃-H₂O)₂] fragments are connected to each other to form a two-dimensional netlike layer structure by the oxygen atoms from the nitro group and phenolate. Further, the two-dimensional layers are assembled via the 2,4-dinitrophenoxide into a three-dimensional framework in an ABAB fashion.

Related literature top

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 top

To a solution of 10 mmol 2,4-dinitrophenol in 60 ml bidistilled water, a solution of an equimolar amount of rubidium hydroxide in 40 ml bidistilled water was added dropwise at room temperature. After vigorous stirring for 4 h, the resulting solution was then evaporated to a volume of about 20 ml in vacuum and filtered hot. The filtrate was then set aside for crystallization at room temperature. Three weeks later, yellow crystals of the title compound suitable for X-ray determination were isolated.

Structure description top

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).

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: APEX2 (Bruker, 2006); 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 (Sheldrick, 1997b).

Figures top

	Fig. 1. Coordination sphere of Rb in [Rb(OC₆H₃N₂O₄).H₂O]. Atoms marked with an A, B, C, D, E and F are at the symmetry positions (-x, 2 - y, 1 - z), (1 - x, 2 - y, 1 - z), (x, 3/2 - y, -1/2 + z), (-x, 1/2 + y, 1/2 - z), (-x,2 - y,-z), (1 - x, 2 - y, -z), respectively.
	Fig. 2. The two-dimensional layer structure containing ladder-shape unit, [Rb₂(µ₃-H₂O)₂]. All C atoms and N atoms were omitted for clarity.

Poly[µ₃-aqua-µ₂-2,4-dinitrophenolato-rubidium(I)] top

Crystal data top

[Rb(C₆H₃N₂O₅)(H₂O)]	F(000) = 560
M_r = 286.59	D_x = 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 = 2.0–25.1°
b = 20.846 (7) Å	µ = 5.50 mm⁻¹
c = 7.412 (2) Å	T = 293 K
β = 93.148 (5)°	Block, yellow
V = 902.8 (5) Å³	0.40 × 0.35 × 0.30 mm
Z = 4

Data collection top

Bruker APEXII CCD area-detector diffractometer	1599 independent reflections
Radiation source: fine-focus sealed tube	1214 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.063
φ and ω scans	θ_max = 25.1°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −6→6
T_min = 0.125, T_max = 0.202	k = −20→24
4449 measured reflections	l = −7→8

Refinement top

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(F_o²) + (0.0556P)² + 0.12P] where P = (F_o² + 2F_c²)/3
S = 1.00	(Δ/σ)_max = 0.002
1599 reflections	Δρ_max = 0.50 e Å⁻³
143 parameters	Δρ_min = −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)

Crystal data top

[Rb(C₆H₃N₂O₅)(H₂O)]	V = 902.8 (5) Å³
M_r = 286.59	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 5.8519 (18) Å	µ = 5.50 mm⁻¹
b = 20.846 (7) Å	T = 293 K
c = 7.412 (2) Å	0.40 × 0.35 × 0.30 mm
β = 93.148 (5)°

Data collection top

Bruker APEXII CCD area-detector diffractometer	1599 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1214 reflections with I > 2σ(I)
T_min = 0.125, T_max = 0.202	R_int = 0.063
4449 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	3 restraints
wR(F²) = 0.101	H atoms treated by a mixture of independent and constrained refinement
S = 1.00	Δρ_max = 0.50 e Å⁻³
1599 reflections	Δρ_min = −0.71 e Å⁻³
143 parameters

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
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*

Atomic displacement parameters (Å²) top

	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)

Geometric parameters (Å, º) top

Rb1—O2	2.914 (3)	O4—Rb1^vii	3.474 (4)
Rb1—O1ⁱ	2.956 (3)	O5—N2	1.232 (5)
Rb1—O1	2.957 (3)	O5—Rb1^viii	3.016 (3)
Rb1—O5ⁱⁱ	3.016 (3)	O5—Rb1^vii	3.429 (4)
Rb1—O6	3.057 (4)	O6—Rb1^iv	3.127 (4)
Rb1—O2ⁱⁱⁱ	3.119 (3)	O6—Rb1^v	3.228 (4)
Rb1—O6^iv	3.127 (4)	O6—H6A	0.818 (10)
Rb1—O3ⁱⁱⁱ	3.134 (3)	O6—H6B	0.820 (10)
Rb1—O6^v	3.228 (4)	N1—C2	1.446 (5)
Rb1—O5^vi	3.429 (4)	N1—Rb1ⁱⁱⁱ	3.533 (4)
Rb1—O4^vi	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)	O6^v—Rb1—N1ⁱⁱⁱ	156.48 (9)
O2—Rb1—O1	55.06 (9)	O5^vi—Rb1—N1ⁱⁱⁱ	144.49 (9)
O1ⁱ—Rb1—O1	79.77 (10)	O4^vi—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)	O6^iv—Rb1—H6A	63.4 (11)
O2—Rb1—O2ⁱⁱⁱ	63.18 (11)	O3ⁱⁱⁱ—Rb1—H6A	57.8 (2)
O1ⁱ—Rb1—O2ⁱⁱⁱ	68.35 (10)	O6^v—Rb1—H6A	109.0 (8)
O1—Rb1—O2ⁱⁱⁱ	115.03 (9)	O5^vi—Rb1—H6A	84.5 (3)
O5ⁱⁱ—Rb1—O2ⁱⁱⁱ	108.92 (10)	O4^vi—Rb1—H6A	93.7 (8)
O6—Rb1—O2ⁱⁱⁱ	98.24 (10)	N1ⁱⁱⁱ—Rb1—H6A	71.5 (4)
O2—Rb1—O6^iv	73.11 (11)	C1—O1—Rb1ⁱ	120.7 (3)
O1ⁱ—Rb1—O6^iv	128.52 (9)	C1—O1—Rb1	123.8 (3)
O1—Rb1—O6^iv	113.35 (9)	Rb1ⁱ—O1—Rb1	100.23 (10)
O5ⁱⁱ—Rb1—O6^iv	121.87 (11)	N1—O2—Rb1	142.2 (3)
O6—Rb1—O6^iv	63.31 (11)	N1—O2—Rb1ⁱⁱⁱ	99.5 (2)
O2ⁱⁱⁱ—Rb1—O6^iv	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—Rb1^vii	97.0 (3)
O1—Rb1—O3ⁱⁱⁱ	146.73 (9)	N2—O5—Rb1^viii	172.5 (3)
O5ⁱⁱ—Rb1—O3ⁱⁱⁱ	69.62 (9)	N2—O5—Rb1^vii	99.1 (3)
O6—Rb1—O3ⁱⁱⁱ	73.29 (9)	Rb1^viii—O5—Rb1^vii	79.58 (8)
O2ⁱⁱⁱ—Rb1—O3ⁱⁱⁱ	40.11 (8)	Rb1—O6—Rb1^iv	116.69 (11)
O6^iv—Rb1—O3ⁱⁱⁱ	76.78 (9)	Rb1—O6—Rb1^v	82.29 (9)
O2—Rb1—O6^v	109.00 (9)	Rb1^iv—O6—Rb1^v	134.09 (13)
O1ⁱ—Rb1—O6^v	94.91 (10)	Rb1—O6—H6A	78 (4)
O1—Rb1—O6^v	54.09 (9)	Rb1^iv—O6—H6A	92 (4)
O5ⁱⁱ—Rb1—O6^v	72.43 (10)	Rb1^v—O6—H6A	134 (4)
O6—Rb1—O6^v	97.71 (9)	Rb1—O6—H6B	144 (4)
O2ⁱⁱⁱ—Rb1—O6^v	162.41 (11)	Rb1^iv—O6—H6B	100 (4)
O6^iv—Rb1—O6^v	134.09 (13)	Rb1^v—O6—H6B	70 (4)
O3ⁱⁱⁱ—Rb1—O6^v	140.73 (9)	H6A—O6—H6B	104.1 (17)
O2—Rb1—O5^vi	97.36 (9)	O2—N1—O3	121.8 (4)
O1ⁱ—Rb1—O5^vi	147.52 (9)	O2—N1—C2	119.8 (3)
O1—Rb1—O5^vi	71.24 (9)	O3—N1—C2	118.4 (4)
O5ⁱⁱ—Rb1—O5^vi	100.42 (8)	O2—N1—Rb1ⁱⁱⁱ	60.6 (2)
O6—Rb1—O5^vi	69.13 (9)	O3—N1—Rb1ⁱⁱⁱ	61.3 (2)
O2ⁱⁱⁱ—Rb1—O5^vi	137.72 (10)	C2—N1—Rb1ⁱⁱⁱ	176.1 (3)
O6^iv—Rb1—O5^vi	77.88 (10)	O4—N2—O5	122.6 (4)
O3ⁱⁱⁱ—Rb1—O5^vi	141.14 (9)	O4—N2—C4	119.4 (4)
O6^v—Rb1—O5^vi	56.22 (10)	O5—N2—C4	118.1 (4)
O2—Rb1—O4^vi	66.31 (9)	O1—C1—C2	124.8 (4)
O1ⁱ—Rb1—O4^vi	141.08 (9)	O1—C1—C6	121.7 (4)
O1—Rb1—O4^vi	69.16 (9)	C2—C1—C6	113.4 (4)
O5ⁱⁱ—Rb1—O4^vi	134.11 (9)	C3—C2—C1	123.0 (4)
O6—Rb1—O4^vi	82.20 (10)	C3—C2—N1	116.7 (3)
O2ⁱⁱⁱ—Rb1—O4^vi	103.85 (9)	C1—C2—N1	120.4 (4)
O6^iv—Rb1—O4^vi	52.17 (9)	C4—C3—C2	119.3 (4)
O3ⁱⁱⁱ—Rb1—O4^vi	128.95 (9)	C4—C3—H3	120.3
O6^v—Rb1—O4^vi	85.63 (9)	C2—C3—H3	120.3
O5^vi—Rb1—O4^vi	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)
O6^iv—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)	O6^v—Rb1—O6—Rb1^iv	−135.87 (16)
O1ⁱ—Rb1—O1—C1	−138.2 (4)	O5^vi—Rb1—O6—Rb1^iv	−86.57 (13)
O5ⁱⁱ—Rb1—O1—C1	147.8 (3)	O4^vi—Rb1—O6—Rb1^iv	−51.39 (12)
O6—Rb1—O1—C1	65.2 (4)	N1ⁱⁱⁱ—Rb1—O6—Rb1^iv	67.47 (12)
O2ⁱⁱⁱ—Rb1—O1—C1	−78.1 (3)	O2—Rb1—O6—Rb1^v	127.89 (11)
O6^iv—Rb1—O1—C1	−10.5 (3)	O1ⁱ—Rb1—O6—Rb1^v	−105.25 (12)
O3ⁱⁱⁱ—Rb1—O1—C1	−112.3 (3)	O1—Rb1—O6—Rb1^v	40.64 (17)
O6^v—Rb1—O1—C1	118.0 (4)	O5ⁱⁱ—Rb1—O6—Rb1^v	−65.46 (10)
O5^vi—Rb1—O1—C1	56.7 (3)	O2ⁱⁱⁱ—Rb1—O6—Rb1^v	−172.56 (9)
O4^vi—Rb1—O1—C1	18.0 (3)	O6^iv—Rb1—O6—Rb1^v	135.87 (16)
N1ⁱⁱⁱ—Rb1—O1—C1	−91.4 (3)	O3ⁱⁱⁱ—Rb1—O6—Rb1^v	−140.81 (10)
O2—Rb1—O1—Rb1ⁱ	81.14 (12)	O6^v—Rb1—O6—Rb1^v	0.0
O1ⁱ—Rb1—O1—Rb1ⁱ	0.0	O5^vi—Rb1—O6—Rb1^v	49.30 (8)
O5ⁱⁱ—Rb1—O1—Rb1ⁱ	−74.03 (13)	O4^vi—Rb1—O6—Rb1^v	84.48 (8)
O6—Rb1—O1—Rb1ⁱ	−156.60 (12)	N1ⁱⁱⁱ—Rb1—O6—Rb1^v	−156.66 (9)
O2ⁱⁱⁱ—Rb1—O1—Rb1ⁱ	60.13 (12)	Rb1—O2—N1—O3	167.0 (4)
O6^iv—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)
O6^v—Rb1—O1—Rb1ⁱ	−103.77 (13)	Rb1ⁱⁱⁱ—O2—N1—C2	−175.5 (3)
O5^vi—Rb1—O1—Rb1ⁱ	−165.14 (11)	Rb1—O2—N1—Rb1ⁱⁱⁱ	163.8 (6)
O4^vi—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)	Rb1^vii—O4—N2—O5	−23.8 (5)
O1—Rb1—O2—N1	39.3 (5)	Rb1^vii—O4—N2—C4	155.5 (3)
O5ⁱⁱ—Rb1—O2—N1	125.4 (5)	Rb1^vii—O5—N2—O4	24.3 (5)
O6—Rb1—O2—N1	−89.1 (5)	Rb1^vii—O5—N2—C4	−155.1 (3)
O2ⁱⁱⁱ—Rb1—O2—N1	−162.0 (6)	Rb1ⁱ—O1—C1—C2	−70.6 (5)
O6^iv—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)
O6^v—Rb1—O2—N1	35.1 (5)	Rb1—O1—C1—C6	−122.3 (4)
O5^vi—Rb1—O2—N1	−21.6 (5)	O1—C1—C2—C3	177.1 (4)
O4^vi—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)
O6^iv—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)
O6^v—Rb1—O2—Rb1ⁱⁱⁱ	−162.86 (13)	C2—C3—C4—C5	−2.0 (6)
O5^vi—Rb1—O2—Rb1ⁱⁱⁱ	140.40 (14)	C2—C3—C4—N2	178.8 (4)
O4^vi—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—Rb1^iv	−8.0 (2)	O4—N2—C4—C5	−171.0 (4)
O1ⁱ—Rb1—O6—Rb1^iv	118.88 (14)	O5—N2—C4—C5	8.3 (7)
O1—Rb1—O6—Rb1^iv	−95.23 (16)	C3—C4—C5—C6	0.8 (7)
O5ⁱⁱ—Rb1—O6—Rb1^iv	158.67 (17)	N2—C4—C5—C6	−180.0 (4)
O2ⁱⁱⁱ—Rb1—O6—Rb1^iv	51.57 (14)	C4—C5—C6—C1	0.3 (7)
O6^iv—Rb1—O6—Rb1^iv	0.0	O1—C1—C6—C5	−178.4 (4)
O3ⁱⁱⁱ—Rb1—O6—Rb1^iv	83.33 (12)	C2—C1—C6—C5	−0.2 (6)

Symmetry codes: (i) −x, −y+2, −z+1; (ii) −x, y+1/2, −z+1/2; (iii) −x+1, −y+2, −z+1; (iv) −x+1, −y+2, −z; (v) −x, −y+2, −z; (vi) x, −y+3/2, z−1/2; (vii) x, −y+3/2, z+1/2; (viii) −x, y−1/2, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6B···O1^v	0.82 (1)	2.03 (2)	2.822 (5)	161 (6)
O6—H6A···O4^ix	0.82 (1)	2.27 (4)	2.919 (5)	137 (5)

Symmetry codes: (v) −x, −y+2, −z; (ix) −x+1, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula	[Rb(C₆H₃N₂O₅)(H₂O)]
M_r	286.59
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	5.8519 (18), 20.846 (7), 7.412 (2)
β (°)	93.148 (5)
V (Å³)	902.8 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.50
Crystal size (mm)	0.40 × 0.35 × 0.30

Data collection
Diffractometer	Bruker APEXII CCD area-detector
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.125, 0.202
No. of measured, independent and observed [I > 2σ(I)] reflections	4449, 1599, 1214
R_int	0.063
(sin θ/λ)_max (Å⁻¹)	0.597

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.101, 1.00
No. of reflections	1599
No. of parameters	143
No. of restraints	3
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.50, −0.71

Computer programs: APEX2 (Bruker, 2006), SAINT (Bruker, 2005), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b) and DIAMOND (Brandenburg & Brendt, 2001), SHELXTL (Sheldrick, 1997b).

Hydrogen-bond geometry (Å, º) top

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) −x, −y+2, −z; (ii) −x+1, y+1/2, −z+1/2.

Acknowledgements

Financial support from the National Natural Science Foundation of China (grant No. 20471035) is gratefully acknowledged.

References

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