Poly[[hexa-aqua-(μ(2)-oxalato-κO,O:O,O)bis-(μ(3)-pyridine-2,4-dicarboxyl-ato-κN,O:O:O)dilanthanum(III)] monohydrate].

In the polymeric title compound, {[La(2)(C(7)H(3)NO(4))(2)(C(2)O(4))(H(2)O)(6)]·H(2)O}(n), the La(3+) cation is nine-coordinated in a distorted LaNO(8) tricapped trigonal-prismatic geometry formed by three pyridinedicarboxylate anions, one oxalate anion and three water mol-ecules. The oxalate anion is located on an inversion center. The oxalate and pyridine-dicarboxyl-ate anions bridge the La(3+) cations, forming a two-dimensional polymeric complex parallel to (010). Inter-molecular O-H⋯O hydrogen bonding and weak C-H⋯O hydrogen bonding is present in the crystal structure and π-π stacking [centroid-centroid distance = 3.571 (3) Å] is observed between parallel pyridine rings of adjacent mol-ecules. The uncoordinated water molecule shows an occupancy of 0.5.

Related literature

For related structures, see: Aghabozorg et al. (2011 ▶); Li et al. (2007 ▶); Wang et al. (2009 ▶).

Experimental

Crystal data

[La2(C7H3NO4)2(C2O4)(H2O)6]·H2O

M = 822.16

Triclinic,

a = 6.4614 (8) Å

b = 6.6844 (8) Å

c = 14.0796 (17) Å

α = 89.735 (2)°

β = 85.266 (2)°

γ = 73.135 (2)°

V = 579.85 (12) Å3

Z = 1

Mo Kα radiation

μ = 3.73 mm−1

T = 295 K

0.30 × 0.10 × 0.10 mm

Data collection

Bruker SMART 1000 CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.686, T max = 0.950

5023 measured reflections

2046 independent reflections

1795 reflections with I > 2σ(I)

R int = 0.035

Refinement

R[F 2 > 2σ(F 2)] = 0.032

wR(F 2) = 0.093

S = 1.09

2046 reflections

175 parameters

H-atom parameters constrained

Δρmax = 2.14 e Å−3

Δρmin = −2.13 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: PLATON.

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S160053681104668X/xu5376sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681104668X/xu5376Isup2.hkl

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

[La2(C7H3NO4)2(C2O4)(H2O)6]·H2O	Z = 1
Mr = 822.16	F(000) = 396
Triclinic, P1	Dx = 2.355 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.4614 (8) Å	Cell parameters from 3390 reflections
b = 6.6844 (8) Å	θ = 2.5–25.0°
c = 14.0796 (17) Å	µ = 3.73 mm−1
α = 89.735 (2)°	T = 295 K
β = 85.266 (2)°	Columnar, brown
γ = 73.135 (2)°	0.30 × 0.10 × 0.10 mm
V = 579.85 (12) Å3

Bruker SMART 1000 CCD area-detector diffractometer	2046 independent reflections
Radiation source: fine-focus sealed tube	1795 reflections with I > 2σ(I)
graphite	Rint = 0.035
Detector resolution: 9 pixels mm-1	θmax = 25.0°, θmin = 1.5°
φ and ω scans	h = −7→7
Absorption correction: multi-scan (SADABS; Bruker, 2001)	k = −7→7
Tmin = 0.686, Tmax = 0.950	l = −16→16
5023 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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.093	H-atom parameters constrained
S = 1.09	w = 1/[σ2(Fo2) + (0.0639P)2] where P = (Fo2 + 2Fc2)/3
2046 reflections	(Δ/σ)max = 0.001
175 parameters	Δρmax = 2.14 e Å−3
0 restraints	Δρmin = −2.13 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 on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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)
La1	0.36051 (5)	0.32815 (5)	0.80389 (2)	0.0265 (1)
O1	0.7674 (8)	0.3427 (7)	0.2806 (3)	0.0392 (16)
O2	1.0913 (8)	0.2154 (8)	0.3384 (3)	0.0525 (19)
O3	1.0788 (7)	0.2730 (8)	0.6993 (3)	0.0396 (16)
O4	0.7592 (7)	0.3177 (9)	0.7799 (3)	0.0521 (18)
O5	0.5103 (8)	0.2478 (6)	0.9657 (3)	0.0423 (14)
O6	0.5841 (9)	0.3677 (7)	1.1030 (3)	0.0485 (18)
O7	−0.0071 (10)	0.5171 (10)	0.8990 (5)	0.0863 (19)
O8	0.5618 (9)	−0.0608 (7)	0.7835 (4)	0.0542 (19)
O9	0.1731 (10)	0.0871 (10)	0.9025 (5)	0.0863 (19)
N1	0.5725 (7)	0.2598 (7)	0.6261 (3)	0.0249 (14)
C1	0.7769 (9)	0.2729 (9)	0.6137 (4)	0.0257 (17)
C2	0.5722 (10)	0.2408 (9)	0.4559 (4)	0.0294 (17)
C3	0.7801 (9)	0.2612 (8)	0.4439 (4)	0.0260 (17)
C4	0.8843 (9)	0.2739 (9)	0.5250 (4)	0.0285 (17)
C5	0.4771 (9)	0.2395 (9)	0.5474 (4)	0.0291 (17)
C6	0.8914 (10)	0.2739 (9)	0.3464 (4)	0.0301 (17)
C7	0.8804 (10)	0.2893 (10)	0.7040 (4)	0.0341 (19)
C8	0.5274 (10)	0.3885 (9)	1.0197 (4)	0.0288 (17)
O10	−0.1015 (18)	−0.0885 (16)	0.9137 (11)	0.072 (5)	0.500
H2A	0.49810	0.22820	0.40340	0.0350*
H4A	1.02570	0.28300	0.51960	0.0340*
H5A	0.33850	0.22340	0.55470	0.0350*
H7A	−0.08470	0.47740	0.86270	0.0800*
H7B	−0.05250	0.64720	0.89900	0.0800*
H8A	0.67010	−0.11890	0.74700	0.0800*
H8B	0.55880	−0.18960	0.81340	0.0800*
H9A	0.29540	−0.01320	0.89080	0.0800*
H9B	0.07450	0.05280	0.87580	0.0800*
H10A	−0.22390	−0.01980	0.89910	0.0800*	0.500
H10B	−0.11240	−0.06870	0.97360	0.0800*	0.500

	U11	U22	U33	U12	U13	U23
La1	0.0283 (2)	0.0378 (2)	0.0187 (2)	−0.0182 (2)	−0.0020 (1)	0.0042 (1)
O1	0.043 (3)	0.047 (3)	0.025 (2)	−0.009 (2)	−0.004 (2)	0.0078 (19)
O2	0.033 (3)	0.074 (4)	0.039 (3)	−0.001 (2)	0.009 (2)	0.014 (2)
O3	0.028 (2)	0.060 (3)	0.038 (3)	−0.022 (2)	−0.0100 (19)	0.002 (2)
O4	0.037 (3)	0.112 (4)	0.023 (2)	−0.046 (3)	−0.005 (2)	0.007 (2)
O5	0.067 (3)	0.029 (2)	0.032 (2)	−0.013 (2)	−0.015 (2)	0.0013 (19)
O6	0.079 (4)	0.038 (2)	0.036 (3)	−0.022 (2)	−0.030 (3)	0.013 (2)
O7	0.059 (3)	0.072 (3)	0.113 (4)	−0.008 (2)	0.037 (3)	0.026 (3)
O8	0.071 (4)	0.034 (3)	0.053 (3)	−0.016 (2)	0.023 (3)	0.001 (2)
O9	0.059 (3)	0.072 (3)	0.113 (4)	−0.008 (2)	0.037 (3)	0.026 (3)
N1	0.020 (2)	0.029 (2)	0.027 (3)	−0.0093 (19)	−0.0018 (19)	0.002 (2)
C1	0.018 (3)	0.029 (3)	0.031 (3)	−0.008 (2)	−0.003 (2)	0.006 (2)
C2	0.030 (3)	0.037 (3)	0.023 (3)	−0.011 (3)	−0.009 (2)	0.002 (2)
C3	0.025 (3)	0.027 (3)	0.024 (3)	−0.005 (2)	−0.001 (2)	0.004 (2)
C4	0.019 (3)	0.039 (3)	0.027 (3)	−0.008 (2)	−0.002 (2)	0.008 (3)
C5	0.023 (3)	0.036 (3)	0.030 (3)	−0.011 (2)	−0.004 (2)	0.003 (2)
C6	0.033 (3)	0.032 (3)	0.023 (3)	−0.007 (3)	0.001 (2)	0.000 (2)
C7	0.030 (3)	0.046 (4)	0.033 (3)	−0.021 (3)	−0.006 (3)	0.011 (3)
C8	0.032 (3)	0.030 (3)	0.022 (3)	−0.006 (2)	0.000 (2)	0.003 (2)
O10	0.044 (6)	0.044 (6)	0.135 (12)	−0.014 (5)	−0.036 (7)	0.007 (7)

La1—N1	2.726 (4)	O8—H8B	0.9600
La1—O1i	2.454 (4)	O9—H9B	0.8500
La1—O3ii	2.541 (5)	O9—H9A	0.8800
La1—O4	2.551 (5)	O10—H10A	0.8300
La1—O5	2.543 (4)	O10—H10B	0.8500
La1—O6iii	2.550 (5)	N1—C5	1.338 (7)
La1—O7	2.604 (7)	N1—C1	1.346 (8)
La1—O8	2.553 (5)	C1—C4	1.379 (8)
La1—O9	2.612 (7)	C1—C7	1.503 (8)
O1—C6	1.271 (8)	C2—C3	1.386 (9)
O2—C6	1.232 (9)	C2—C5	1.382 (8)
O3—C7	1.251 (8)	C3—C6	1.510 (8)
O4—C7	1.253 (7)	C3—C4	1.388 (8)
O5—C8	1.247 (7)	C8—C8iii	1.541 (8)
O6—C8	1.253 (7)	C2—H2A	0.9300
O7—H7B	0.8300	C4—H4A	0.9300
O7—H7A	0.8400	C5—H5A	0.9300
O8—H8A	0.8300
O4—La1—O5	73.91 (15)	La1—O5—C8	121.8 (4)
O4—La1—O7	143.20 (19)	La1iii—O6—C8	121.6 (4)
O4—La1—O8	76.08 (19)	La1—O7—H7B	119.00
O4—La1—O9	130.46 (19)	H7A—O7—H7B	105.00
O4—La1—N1	60.09 (14)	La1—O7—H7A	96.00
O3ii—La1—O4	136.05 (14)	La1—O8—H8A	129.00
O1i—La1—O4	94.15 (17)	H8A—O8—H8B	93.00
O4—La1—O6iii	71.03 (17)	La1—O8—H8B	138.00
O5—La1—O7	85.94 (19)	La1—O9—H9A	87.00
O5—La1—O8	78.78 (15)	H9A—O9—H9B	108.00
O5—La1—O9	68.31 (19)	La1—O9—H9B	116.00
O5—La1—N1	129.55 (15)	H10A—O10—H10B	102.00
O3ii—La1—O5	143.58 (15)	La1—N1—C5	123.7 (4)
O1i—La1—O5	131.93 (14)	La1—N1—C1	118.9 (3)
O5—La1—O6iii	62.98 (13)	C1—N1—C5	116.8 (5)
O7—La1—O8	130.39 (19)	N1—C1—C4	122.9 (5)
O7—La1—O9	64.2 (2)	N1—C1—C7	115.1 (5)
O7—La1—N1	143.97 (18)	C4—C1—C7	121.9 (6)
O3ii—La1—O7	76.45 (18)	C3—C2—C5	118.7 (5)
O1i—La1—O7	76.62 (19)	C2—C3—C6	122.0 (5)
O6iii—La1—O7	72.42 (19)	C4—C3—C6	120.1 (5)
O8—La1—O9	66.27 (19)	C2—C3—C4	117.9 (5)
O8—La1—N1	71.47 (16)	C1—C4—C3	119.6 (6)
O3ii—La1—O8	88.67 (17)	N1—C5—C2	123.9 (6)
O1i—La1—O8	144.45 (16)	O1—C6—O2	126.8 (6)
O6iii—La1—O8	134.78 (18)	O2—C6—C3	117.2 (5)
O9—La1—N1	128.72 (18)	O1—C6—C3	116.1 (6)
O3ii—La1—O9	75.33 (18)	O4—C7—C1	116.7 (6)
O1i—La1—O9	135.03 (19)	O3—C7—C1	119.0 (5)
O6iii—La1—O9	115.40 (18)	O3—C7—O4	124.3 (6)
O3ii—La1—N1	76.02 (14)	O5—C8—O6	126.8 (5)
O1i—La1—N1	74.06 (14)	O5—C8—C8iii	116.9 (5)
O6iii—La1—N1	114.76 (15)	O6—C8—C8iii	116.4 (5)
O1i—La1—O3ii	74.77 (16)	C5—C2—H2A	121.00
O3ii—La1—O6iii	136.50 (17)	C3—C2—H2A	121.00
O1i—La1—O6iii	69.06 (15)	C1—C4—H4A	120.00
La1i—O1—C6	137.1 (4)	C3—C4—H4A	120.00
La1iv—O3—C7	139.6 (4)	N1—C5—H5A	118.00
La1—O4—C7	128.4 (4)	C2—C5—H5A	118.00
O5—La1—O4—C7	158.8 (6)	N1—La1—O1i—C6i	73.1 (6)
O7—La1—O4—C7	−141.7 (5)	O4—La1—O6iii—C8iii	−86.9 (5)
O8—La1—O4—C7	76.7 (6)	O5—La1—O6iii—C8iii	−5.7 (5)
O9—La1—O4—C7	117.6 (6)	O7—La1—O6iii—C8iii	88.8 (5)
N1—La1—O4—C7	0.3 (5)	O8—La1—O6iii—C8iii	−41.2 (6)
O3ii—La1—O4—C7	3.7 (7)	O9—La1—O6iii—C8iii	39.8 (6)
O1i—La1—O4—C7	−68.6 (6)	N1—La1—O6iii—C8iii	−129.2 (5)
O6iii—La1—O4—C7	−134.8 (6)	La1i—O1—C6—C3	102.3 (6)
O4—La1—O5—C8	82.1 (5)	La1i—O1—C6—O2	−78.5 (8)
O7—La1—O5—C8	−66.7 (5)	La1iv—O3—C7—O4	−11.4 (11)
O8—La1—O5—C8	160.7 (5)	La1iv—O3—C7—C1	169.0 (4)
O9—La1—O5—C8	−130.5 (5)	La1—O4—C7—C1	4.4 (9)
N1—La1—O5—C8	106.5 (5)	La1—O4—C7—O3	−175.2 (5)
O3ii—La1—O5—C8	−127.3 (5)	La1—O5—C8—O6	174.5 (5)
O1i—La1—O5—C8	1.2 (6)	La1—O5—C8—C8iii	−5.3 (8)
O6iii—La1—O5—C8	5.6 (5)	La1iii—O6—C8—O5	174.7 (5)
O4—La1—N1—C1	−5.7 (4)	La1iii—O6—C8—C8iii	−5.5 (8)
O4—La1—N1—C5	−177.0 (5)	C5—N1—C1—C4	2.4 (8)
O5—La1—N1—C1	−32.9 (5)	La1—N1—C1—C7	9.8 (6)
O5—La1—N1—C5	155.9 (4)	C1—N1—C5—C2	−3.0 (8)
O7—La1—N1—C1	135.5 (4)	C5—N1—C1—C7	−178.3 (5)
O7—La1—N1—C5	−35.7 (6)	La1—N1—C5—C2	168.4 (4)
O8—La1—N1—C1	−90.0 (4)	La1—N1—C1—C4	−169.4 (4)
O8—La1—N1—C5	98.8 (4)	N1—C1—C7—O3	170.2 (6)
O9—La1—N1—C1	−125.6 (4)	N1—C1—C7—O4	−9.4 (8)
O9—La1—N1—C5	63.2 (5)	C4—C1—C7—O3	−10.5 (9)
O3ii—La1—N1—C1	176.7 (4)	C4—C1—C7—O4	169.9 (6)
O3ii—La1—N1—C5	5.4 (4)	N1—C1—C4—C3	0.1 (9)
O1i—La1—N1—C1	98.8 (4)	C7—C1—C4—C3	−179.1 (5)
O1i—La1—N1—C5	−72.4 (4)	C5—C2—C3—C4	1.6 (8)
O6iii—La1—N1—C1	41.6 (4)	C3—C2—C5—N1	1.0 (9)
O6iii—La1—N1—C5	−129.7 (4)	C5—C2—C3—C6	−177.2 (5)
O4—La1—O3ii—C7ii	−173.4 (6)	C2—C3—C6—O1	25.5 (8)
O5—La1—O3ii—C7ii	49.4 (8)	C6—C3—C4—C1	176.7 (5)
O7—La1—O3ii—C7ii	−13.9 (7)	C4—C3—C6—O2	27.4 (8)
O8—La1—O3ii—C7ii	118.3 (7)	C2—C3—C6—O2	−153.9 (6)
O9—La1—O3ii—C7ii	52.5 (7)	C4—C3—C6—O1	−153.3 (5)
N1—La1—O3ii—C7ii	−170.5 (7)	C2—C3—C4—C1	−2.1 (8)
O4—La1—O1i—C6i	130.4 (6)	O5—C8—C8iii—O5iii	−180.0 (6)
O5—La1—O1i—C6i	−157.6 (6)	O5—C8—C8iii—O6iii	−0.2 (9)
O7—La1—O1i—C6i	−85.8 (6)	O6—C8—C8iii—O5iii	0.2 (9)
O8—La1—O1i—C6i	58.6 (7)	O6—C8—C8iii—O6iii	180.0 (6)
O9—La1—O1i—C6i	−56.3 (7)

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O4ii	0.84	2.08	2.911 (8)	168
O7—H7B···O10v	0.83	1.71	2.533 (12)	168
O8—H8A···O2vi	0.83	1.83	2.660 (7)	173
O8—H8B···O6vii	0.96	2.03	2.914 (7)	153
O9—H9A···O6vii	0.88	2.27	2.987 (8)	138
O9—H9B···O10	0.85	1.73	2.390 (14)	133
O10—H10A···O5ii	0.83	2.24	2.885 (12)	135
O10—H10A···O8ii	0.83	2.29	2.924 (15)	133
O10—H10B···O9viii	0.85	1.77	2.591 (17)	163
C5—H5A···O3ii	0.93	2.49	3.164 (7)	130

Table 1

Selected bond lengths (Å)

La1—N1	2.726 (4)
La1—O1i	2.454 (4)
La1—O3ii	2.541 (5)
La1—O4	2.551 (5)
La1—O5	2.543 (4)
La1—O6iii	2.550 (5)
La1—O7	2.604 (7)
La1—O8	2.553 (5)
La1—O9	2.612 (7)

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

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O4ii	0.84	2.08	2.911 (8)	168
O7—H7B⋯O10iv	0.83	1.71	2.533 (12)	168
O8—H8A⋯O2v	0.83	1.83	2.660 (7)	173
O8—H8B⋯O6vi	0.96	2.03	2.914 (7)	153
O9—H9A⋯O6vi	0.88	2.27	2.987 (8)	138
O9—H9B⋯O10	0.85	1.73	2.390 (14)	133
O10—H10A⋯O5ii	0.83	2.24	2.885 (12)	135
O10—H10A⋯O8ii	0.83	2.29	2.924 (15)	133
O10—H10B⋯O9vii	0.85	1.77	2.591 (17)	163
C5—H5A⋯O3ii	0.93	2.49	3.164 (7)	130

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