A one-dimensional ladder-like coordination polymer: poly[[hexa-aqua-bis(μ-5-nitro-benzene-1,3-dicarboxyl-ato-κO,O',O'')(μ-oxalato-κO,O':O'',O''')diyttrium(III)] trihydrate].

In the crystal structure of the title one-dimensional coordination polymer, [Y(2)(C(8)H(3)NO(6))(2)(C(2)O(4))(H(2)O)(6)]·3H(2)O, each Y(III) ion is bridged to its neighbours by two 5-nitro-benzene-1,3-dicarboxyl-ate (nbdc) dianions and one oxalate dianion (located on an inversion centre) to form a ladder-like polymeric structure. The two carboxylate groups of nbdc assume different modes of coordination, one is chelating whereas the other is monodentate. Three water mol-ecules coordinate to the Y(III) ion to complete an eight-coordinate distorted dodecahedral geometry. The ladder-like polymers are assembled together by hydrogen bonding and π-π stacking [centrio-centriod distance = 3.819 (9) Å] in the crystal structure.

Related literature

For general background, see: Biradha (2003 ▶); Braga et al. (2005 ▶); Burrows et al. (2003 ▶); Kongshaug & Fjellvag (2006 ▶); Moulton & Zaworotko (2001 ▶); Ohmori et al. (2004 ▶); Tang et al. (2006 ▶); Janiak (2003 ▶). For related structures, see: Thomas et al. (2002 ▶); Nordell et al. (2003 ▶); Janiak (2000 ▶). For related literature, see: Ren et al. (2006 ▶); Si et al. (2004 ▶).

Experimental

Crystal data

[Y2(C8H3NO6)2(C2O4)(H2O)6]·3H2O

M = 846.21

Triclinic,

a = 7.4270 (15) Å

b = 9.2070 (18) Å

c = 11.522 (2) Å

α = 74.16 (3)°

β = 71.76 (3)°

γ = 80.01 (2)°

V = 716.5 (3) Å3

Z = 1

Mo Kα radiation

μ = 4.14 mm−1

T = 298 (2) K

0.20 × 0.15 × 0.12 mm

Data collection

Enraf–Nonius CAD-4 diffractometer

Absorption correction: ψ scan (XCAD4; Harms & Wocadlo, 1995 ▶) T min = 0.48, T max = 0.60

3018 measured reflections

2785 independent reflections

2260 reflections with I > 2σ(I)

R int = 0.097

3 standard reflections every 200 reflections intensity decay: 1.0%

Refinement

R[F 2 > 2σ(F 2)] = 0.043

wR(F 2) = 0.112

S = 1.05

2785 reflections

220 parameters

H-atom parameters constrained

Δρmax = 0.67 e Å−3

Δρmin = −0.64 e Å−3

Data collection: CAD-4 Software (Enraf–Nonius, 1989 ▶); cell refinement: CAD-4 Software; data reduction: XCAD4 (Harms & Wocadlo, 1995 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL (Sheldrick, 2000 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807064306/xu2377sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807064306/xu2377Isup2.hkl

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

[Y2(C8H3NO6)2(C2O4)(H2O)6]·3H2O	Z = 1
Mr = 846.21	F000 = 424
Triclinic, P1	Dx = 1.961 Mg m−3
Hall symbol: -P 1	Mo Kα radiation λ = 0.71073 Å
a = 7.4270 (15) Å	Cell parameters from 25 reflections
b = 9.2070 (18) Å	θ = 2.3–15.0º
c = 11.522 (2) Å	µ = 4.14 mm−1
α = 74.16 (3)º	T = 298 (2) K
β = 71.76 (3)º	Block, colorless
γ = 80.01 (2)º	0.20 × 0.15 × 0.12 mm
V = 716.5 (3) Å3

Enraf–Nonius CAD-4 diffractometer	Rint = 0.097
Radiation source: fine-focus sealed tube	θmax = 26.0º
Monochromator: graphite	θmin = 1.9º
T = 298(2) K	h = 0→9
ω/2θ scans	k = −11→11
Absorption correction: ψ scan(XCAD4; Harms & Wocadlo, 1995)	l = −13→14
Tmin = 0.48, Tmax = 0.60	3 standard reflections
3018 measured reflections	every 200 reflections
2785 independent reflections	intensity decay: 1.0%
2260 reflections with I > 2σ(I)

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)] = 0.043	H-atom parameters constrained
wR(F2) = 0.112	w = 1/[σ2(Fo2) + (0.0432P)2 + 2.6078P] where P = (Fo2 + 2Fc2)/3
S = 1.05	(Δ/σ)max < 0.001
2785 reflections	Δρmax = 0.67 e Å−3
220 parameters	Δρmin = −0.64 e Å−3
Primary atom site location: structure-invariant direct methods	Extinction correction: none

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	Occ. (<1)
C1	0.3395 (7)	0.2400 (6)	0.1373 (5)	0.0176 (10)
C2	0.2913 (7)	0.3978 (6)	0.0685 (5)	0.0182 (10)
C3	0.2644 (7)	0.4243 (6)	−0.0506 (5)	0.0200 (11)
H3	0.2853	0.3461	−0.0909	0.024*
C4	0.2095 (7)	0.5698 (6)	−0.1067 (5)	0.0188 (10)
C5	0.1769 (7)	0.6925 (6)	−0.0509 (5)	0.0187 (10)
H5	0.1321	0.7878	−0.0904	0.022*
C6	0.2101 (7)	0.6653 (6)	0.0648 (5)	0.0181 (10)
C7	0.2687 (7)	0.5187 (6)	0.1238 (5)	0.0201 (11)
H7	0.2862	0.4994	0.2030	0.024*
C8	0.1873 (7)	0.7916 (6)	0.1298 (5)	0.0187 (10)
C9	0.6051 (7)	−0.0058 (6)	0.4632 (5)	0.0177 (10)
N1	0.1769 (7)	0.5962 (5)	−0.2319 (4)	0.0265 (10)
O1	0.3821 (6)	0.2183 (4)	0.2395 (3)	0.0261 (9)
O2	0.3332 (5)	0.1288 (4)	0.0962 (3)	0.0228 (8)
O3	0.3182 (5)	0.7902 (4)	0.1793 (3)	0.0223 (8)
O4	0.0460 (5)	0.8849 (4)	0.1325 (4)	0.0251 (8)
O5	0.1269 (9)	0.7245 (5)	−0.2819 (5)	0.0564 (15)
O6	0.1979 (8)	0.4894 (5)	−0.2778 (4)	0.0461 (12)
O7	0.7221 (5)	0.0136 (4)	0.5150 (3)	0.0214 (8)
O8	0.6444 (5)	−0.0325 (4)	0.3571 (3)	0.0232 (8)
O9	0.6774 (5)	−0.0796 (4)	0.1250 (3)	0.0244 (8)
H9A	0.6641	−0.0316	0.0534	0.029*
H9B	0.7642	−0.0428	0.1386	0.029*
O10	0.4350 (6)	−0.3006 (4)	0.3988 (4)	0.0326 (10)
H10A	0.5526	−0.3322	0.3807	0.039*
H10B	0.3968	−0.3009	0.4765	0.039*
O11	0.0652 (5)	−0.0383 (5)	0.3376 (4)	0.0318 (10)
H11B	0.0191	0.0193	0.3884	0.038*
H11A	0.0252	−0.0036	0.2728	0.038*
O12	0.3768 (8)	0.3842 (5)	0.4156 (5)	0.0492 (13)
H12B	0.3942	0.4764	0.3793	0.059*
H12A	0.4299	0.3285	0.3639	0.059*
O13	0.0067 (15)	0.3583 (14)	0.5020 (11)	0.068 (3)	0.50
H13A	0.0037	0.2670	0.5003	0.081*	0.50
H13B	−0.1035	0.3933	0.5392	0.081*	0.50
Y	0.39399 (7)	−0.05405 (6)	0.27921 (5)	0.01386 (15)

	U11	U22	U33	U12	U13	U23
C1	0.018 (2)	0.018 (3)	0.017 (2)	−0.0018 (19)	−0.005 (2)	−0.004 (2)
C2	0.019 (3)	0.017 (3)	0.019 (3)	−0.002 (2)	−0.005 (2)	−0.005 (2)
C3	0.020 (3)	0.020 (3)	0.022 (3)	−0.002 (2)	−0.007 (2)	−0.008 (2)
C4	0.020 (3)	0.024 (3)	0.015 (2)	−0.004 (2)	−0.004 (2)	−0.007 (2)
C5	0.024 (3)	0.012 (2)	0.022 (3)	−0.002 (2)	−0.011 (2)	−0.002 (2)
C6	0.021 (3)	0.018 (3)	0.020 (3)	−0.004 (2)	−0.009 (2)	−0.006 (2)
C7	0.022 (3)	0.021 (3)	0.020 (3)	−0.002 (2)	−0.009 (2)	−0.005 (2)
C8	0.017 (2)	0.020 (3)	0.018 (2)	−0.004 (2)	−0.002 (2)	−0.006 (2)
C9	0.018 (3)	0.016 (3)	0.019 (3)	−0.0011 (19)	−0.006 (2)	−0.003 (2)
N1	0.034 (3)	0.027 (3)	0.021 (2)	−0.004 (2)	−0.013 (2)	−0.004 (2)
O1	0.044 (2)	0.0195 (19)	0.0213 (19)	−0.0005 (17)	−0.0204 (17)	−0.0047 (15)
O2	0.037 (2)	0.0142 (18)	0.0217 (19)	−0.0004 (15)	−0.0135 (16)	−0.0062 (15)
O3	0.0254 (19)	0.0190 (19)	0.033 (2)	0.0032 (15)	−0.0188 (17)	−0.0132 (16)
O4	0.0216 (19)	0.025 (2)	0.036 (2)	0.0056 (15)	−0.0149 (17)	−0.0160 (17)
O5	0.113 (5)	0.028 (3)	0.036 (3)	0.007 (3)	−0.046 (3)	0.000 (2)
O6	0.078 (4)	0.038 (3)	0.034 (2)	0.007 (2)	−0.029 (2)	−0.020 (2)
O7	0.0161 (17)	0.036 (2)	0.0171 (18)	−0.0056 (15)	−0.0082 (14)	−0.0089 (16)
O8	0.0213 (19)	0.037 (2)	0.0159 (18)	−0.0030 (16)	−0.0066 (15)	−0.0118 (16)
O9	0.0205 (19)	0.039 (2)	0.0171 (18)	−0.0029 (16)	−0.0058 (15)	−0.0124 (16)
O10	0.046 (3)	0.028 (2)	0.028 (2)	0.0010 (19)	−0.0182 (19)	−0.0061 (17)
O11	0.0196 (19)	0.057 (3)	0.028 (2)	0.0038 (18)	−0.0103 (16)	−0.027 (2)
O12	0.079 (4)	0.036 (3)	0.044 (3)	−0.008 (2)	−0.033 (3)	−0.008 (2)
O13	0.045 (6)	0.075 (8)	0.074 (8)	−0.031 (6)	−0.011 (6)	0.006 (6)
Y	0.0155 (2)	0.0154 (2)	0.0136 (2)	−0.00013 (16)	−0.00695 (17)	−0.00552 (17)

C1—O2	1.253 (6)	N1—O6	1.204 (6)
C1—O1	1.269 (6)	N1—O5	1.215 (6)
C1—C2	1.495 (7)	O1—Y	2.414 (4)
C1—Y	2.790 (5)	O2—Y	2.424 (4)
C2—C7	1.388 (7)	O3—Yii	2.299 (3)
C2—C3	1.398 (7)	O7—Yi	2.365 (3)
C3—C4	1.372 (7)	O8—Y	2.361 (3)
C3—H3	0.9264	O9—Y	2.314 (4)
C4—C5	1.397 (7)	O9—H9A	0.8500
C4—N1	1.484 (7)	O9—H9B	0.8501
C5—C6	1.380 (7)	O10—Y	2.336 (4)
C5—H5	0.9288	O10—H10A	0.8500
C6—C7	1.398 (7)	O10—H10B	0.8501
C6—C8	1.507 (7)	O11—Y	2.311 (4)
C7—H7	0.9274	O11—H11B	0.8500
C8—O4	1.233 (6)	O11—H11A	0.8498
C8—O3	1.268 (6)	O12—H12B	0.8499
C9—O8	1.247 (6)	O12—H12A	0.8500
C9—O7	1.258 (6)	O13—H13A	0.8500
C9—C9i	1.527 (9)	O13—H13B	0.8500
O2—C1—O1	119.8 (5)	H10A—O10—H10B	108.3
O2—C1—C2	120.3 (4)	Y—O11—H11B	110.1
O1—C1—C2	119.9 (4)	Y—O11—H11A	109.8
O2—C1—Y	60.2 (3)	H11B—O11—H11A	109.8
O1—C1—Y	59.8 (3)	H12B—O12—H12A	109.7
C2—C1—Y	174.6 (3)	H13A—O13—H13B	109.5
C7—C2—C3	119.5 (5)	O3iii—Y—O11	74.28 (13)
C7—C2—C1	120.2 (4)	O3iii—Y—O9	78.95 (13)
C3—C2—C1	120.3 (4)	O11—Y—O9	147.86 (13)
C4—C3—C2	118.1 (5)	O3iii—Y—O10	74.18 (13)
C4—C3—H3	121.0	O11—Y—O10	95.62 (16)
C2—C3—H3	120.8	O9—Y—O10	93.86 (15)
C3—C4—C5	123.7 (5)	O3iii—Y—O8	138.88 (13)
C3—C4—N1	117.7 (4)	O11—Y—O8	139.85 (13)
C5—C4—N1	118.6 (4)	O9—Y—O8	72.16 (12)
C6—C5—C4	117.4 (5)	O10—Y—O8	79.18 (14)
C6—C5—H5	122.0	O3iii—Y—O7i	133.63 (13)
C4—C5—H5	120.5	O11—Y—O7i	71.41 (12)
C5—C6—C7	120.3 (5)	O9—Y—O7i	140.67 (12)
C5—C6—C8	121.3 (5)	O10—Y—O7i	79.12 (14)
C7—C6—C8	118.4 (4)	O8—Y—O7i	68.51 (12)
C2—C7—C6	120.9 (5)	O3iii—Y—O1	132.35 (12)
C2—C7—H7	118.6	O11—Y—O1	90.19 (15)
C6—C7—H7	120.4	O9—Y—O1	94.96 (14)
O4—C8—O3	125.6 (5)	O10—Y—O1	153.26 (13)
O4—C8—C6	119.0 (4)	O8—Y—O1	79.61 (13)
O3—C8—C6	115.4 (4)	O7i—Y—O1	78.08 (13)
O8—C9—O7	126.2 (4)	O3iii—Y—O2	79.18 (12)
O8—C9—C9i	117.0 (5)	O11—Y—O2	80.27 (14)
O7—C9—C9i	116.8 (5)	O9—Y—O2	77.50 (13)
O6—N1—O5	123.2 (5)	O10—Y—O2	153.13 (13)
O6—N1—C4	118.6 (5)	O8—Y—O2	120.73 (13)
O5—N1—C4	118.2 (5)	O7i—Y—O2	123.38 (13)
C1—O1—Y	93.2 (3)	O1—Y—O2	53.60 (12)
C1—O2—Y	93.2 (3)	O3iii—Y—C1	105.48 (14)
C8—O3—Yii	136.0 (3)	O11—Y—C1	83.57 (15)
C9—O7—Yi	118.6 (3)	O9—Y—C1	86.78 (14)
C9—O8—Y	119.0 (3)	O10—Y—C1	179.19 (14)
Y—O9—H9A	109.9	O8—Y—C1	101.50 (14)
Y—O9—H9B	109.8	O7i—Y—C1	100.69 (14)
H9A—O9—H9B	108.4	O1—Y—C1	27.01 (13)
Y—O10—H10A	109.3	O2—Y—C1	26.64 (13)
Y—O10—H10B	109.8
O2—C1—C2—C7	169.7 (5)	C9—O8—Y—O3iii	−134.9 (4)
O1—C1—C2—C7	−8.3 (7)	C9—O8—Y—O11	1.1 (5)
O2—C1—C2—C3	−8.9 (7)	C9—O8—Y—O9	177.5 (4)
O1—C1—C2—C3	173.0 (5)	C9—O8—Y—O10	−84.8 (4)
C7—C2—C3—C4	−2.3 (7)	C9—O8—Y—O7i	−2.3 (4)
C1—C2—C3—C4	176.3 (4)	C9—O8—Y—O1	78.8 (4)
C2—C3—C4—C5	−0.8 (8)	C9—O8—Y—O2	114.6 (4)
C2—C3—C4—N1	−178.6 (4)	C9—O8—Y—C1	94.7 (4)
C3—C4—C5—C6	2.9 (8)	C1—O1—Y—O3iii	−6.7 (4)
N1—C4—C5—C6	−179.3 (4)	C1—O1—Y—O11	−75.3 (3)
C4—C5—C6—C7	−1.8 (7)	C1—O1—Y—O9	72.9 (3)
C4—C5—C6—C8	177.3 (4)	C1—O1—Y—O10	−178.3 (3)
C3—C2—C7—C6	3.3 (8)	C1—O1—Y—O8	143.7 (3)
C1—C2—C7—C6	−175.3 (4)	C1—O1—Y—O7i	−146.3 (3)
C5—C6—C7—C2	−1.2 (8)	C1—O1—Y—O2	2.4 (3)
C8—C6—C7—C2	179.7 (4)	C1—O2—Y—O3iii	170.8 (3)
C5—C6—C8—O4	44.6 (7)	C1—O2—Y—O11	95.1 (3)
C7—C6—C8—O4	−136.2 (5)	C1—O2—Y—O9	−108.3 (3)
C5—C6—C8—O3	−136.3 (5)	C1—O2—Y—O10	178.3 (3)
C7—C6—C8—O3	42.8 (7)	C1—O2—Y—O8	−48.1 (3)
C3—C4—N1—O6	0.8 (7)	C1—O2—Y—O7i	35.1 (3)
C5—C4—N1—O6	−177.1 (5)	C1—O2—Y—O1	−2.4 (3)
C3—C4—N1—O5	179.5 (5)	O2—C1—Y—O3iii	−9.4 (3)
C5—C4—N1—O5	1.5 (8)	O1—C1—Y—O3iii	174.9 (3)
O2—C1—O1—Y	−4.3 (5)	O2—C1—Y—O11	−81.1 (3)
C2—C1—O1—Y	173.8 (4)	O1—C1—Y—O11	103.2 (3)
O1—C1—O2—Y	4.3 (5)	O2—C1—Y—O9	68.2 (3)
C2—C1—O2—Y	−173.8 (4)	O1—C1—Y—O9	−107.5 (3)
O4—C8—O3—Yii	−6.0 (8)	O2—C1—Y—O8	139.3 (3)
C6—C8—O3—Yii	175.0 (3)	O1—C1—Y—O8	−36.4 (3)
O8—C9—O7—Yi	−177.9 (4)	O2—C1—Y—O7i	−150.8 (3)
C9i—C9—O7—Yi	2.7 (7)	O1—C1—Y—O7i	33.5 (3)
O7—C9—O8—Y	−177.5 (4)	O2—C1—Y—O1	175.7 (5)
C9i—C9—O8—Y	1.9 (7)	O1—C1—Y—O2	−175.7 (5)

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9A···O2iv	0.85	2.14	2.735 (5)	127
O9—H9B···O4v	0.85	2.07	2.726 (5)	134
O10—H10A···O6iv	0.85	2.36	3.115 (7)	148
O10—H10B···O12i	0.85	2.30	2.778 (6)	116
O10—H10B···O12i	0.85	2.30	2.778 (6)	116
O11—H11A···O4iii	0.85	2.09	2.694 (5)	127
O11—H11B···O5vi	0.85	2.57	2.987 (6)	111
O11—H11B···O7vii	0.85	2.23	2.784 (5)	123
O12—H12A···O1	0.85	2.11	2.841 (6)	144
O12—H12B···O10ii	0.85	2.21	2.953 (6)	147
C3—H3···O9iv	0.93	2.54	3.432 (6)	161

Table 1

Selected bond lengths (Å)

O1—Y	2.414 (4)
O2—Y	2.424 (4)
O3—Yi	2.299 (3)
O7—Yii	2.365 (3)
O8—Y	2.361 (3)
O9—Y	2.314 (4)
O10—Y	2.336 (4)
O11—Y	2.311 (4)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O9—H9A⋯O2iii	0.85	2.14	2.735 (5)	127
O9—H9B⋯O4iv	0.85	2.07	2.726 (5)	134
O10—H10A⋯O6iii	0.85	2.36	3.115 (7)	148
O10—H10B⋯O12ii	0.85	2.30	2.778 (6)	116
O10—H10B⋯O12ii	0.85	2.30	2.778 (6)	116
O11—H11A⋯O4v	0.85	2.09	2.694 (5)	127
O11—H11B⋯O5vi	0.85	2.57	2.987 (6)	111
O11—H11B⋯O7vii	0.85	2.23	2.784 (5)	123
O12—H12A⋯O1	0.85	2.11	2.841 (6)	144
O12—H12B⋯O10i	0.85	2.21	2.953 (6)	147

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