Poly[[hemi-μ(4)-oxalato-hemi-μ(2)-oxalato-bis-(μ(3)-pyrazine-2-carboxyl-ato)neodymium(III)silver(I)] monohydrate].

In the title coordination polymer, {[AgNd(C(5)H(3)N(2)O(2))(2)(C(2)O(4))]·H(2)O}(n), the Nd(III) atom is coordinated in a distorted monocapped square-anti-prismatic geometry by two O and two N atoms of two N,O-bidentate pyrazine-2-carboxyl-ate (2-pzc) ligands, four O atoms of two bidentate oxalate ligands, and one O atom of a monodentate carboxyl-ate group of a 2-pzc ligand. The Ag(I) ion is coordinated in a distorted tetra-hedral geometry by two N atoms from two monodentate 2-pzc ligands, one O atom from one monodentate oxalate ligand and one O atom of a bridging carboxyl-ate group of a 2-pzc ligand. The oxalate anions link neighbouring neodymium(III) metal centres into Nd-oxalate chains, which are inter-connected by Ag(2-pyz)(2) units, forming a three-dimensional polymeric framework. Inter-molecular O-H⋯O and C-H⋯O hydrogen bonds are observed in the crystal structure.

Related literature

For general background to coordination polymers and open-framework materials, see: Barbour (2006 ▶); Kepert (2006 ▶); Kong et al. (2008 ▶); Zhang et al. (2005 ▶); Gheorghe et al. (2002 ▶). For the synthesis and crystal structure of heterometallic complexes of pyrazine-2-carboxylic acid, see: Ciurtin et al. (2002 ▶); Dong et al. (2000 ▶).

Experimental

Crystal data

[AgNd(C5n class="Species">H3N2O2)2(C2O4)]·H2O

M = 604.33

Monoclinic,

a = 10.112 (2) Å

b = 18.847 (4) Å

c = 8.0359 (16) Å

β = 95.47 (3)°

V = 1524.6 (5) Å3

Z = 4

Mo Kα radiation

μ = 4.72 mm−1

T = 293 K

0.32 × 0.26 × 0.21 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer

Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.241, T max = 0.370

12072 measured reflections

2747 indepen class="Chemical">ndent reflections

1946 reflections with I > 2σ(I)

R int = 0.093

Refinement

R[F 2 > 2σ(F 2)] = 0.038

wR(F 2) = 0.111

S = 1.13

2747 reflections

244 parameters

3 restraints

H-atom parameters constrained

Δρmax = 1.59 e Å−3

Δρmin = −1.77 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPII (Johnson, 1976 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680902128X/rz2330sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680902128X/rz2330Isup2.hkl

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

[AgNd(C5H3N2O2)2(C2O4)]·H2O	F(000) = 1148
Mr = 604.33	Dx = 2.633 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2433 reflections
a = 10.112 (2) Å	θ = 1.4–28.0°
b = 18.847 (4) Å	µ = 4.72 mm−1
c = 8.0359 (16) Å	T = 293 K
β = 95.47 (3)°	Block, colourless
V = 1524.6 (5) Å3	0.32 × 0.26 × 0.21 mm
Z = 4

Rigaku/MSC Mercury CCD diffractometer	2747 independent reflections
Radiation source: fine-focus sealed tube	1946 reflections with I > 2σ(I)
graphite	Rint = 0.093
ω scans	θmax = 25.2°, θmin = 3.3°
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	h = −12→12
Tmin = 0.241, Tmax = 0.370	k = −22→22
12072 measured reflections	l = −9→9

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)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.111	H-atom parameters constrained
S = 1.13	w = 1/[σ2(Fo2) + (0.0182P)2 + 17.3537P] where P = (Fo2 + 2Fc2)/3
2747 reflections	(Δ/σ)max = 0.028
244 parameters	Δρmax = 1.59 e Å−3
3 restraints	Δρmin = −1.77 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
Ag1	1.15900 (9)	0.92327 (6)	0.60684 (11)	0.0369 (3)
C1	0.9481 (10)	0.9114 (6)	0.0822 (13)	0.026 (3)
N1	0.8209 (8)	0.9101 (5)	0.0274 (10)	0.027 (2)
Nd1	0.64656 (5)	0.89514 (3)	0.26047 (7)	0.02128 (18)
O1	0.8807 (6)	0.9057 (5)	0.3541 (8)	0.0298 (19)
O1W	0.9655 (10)	0.7408 (7)	0.0126 (18)	0.099 (5)
H1W	0.9199	0.7431	0.0945	0.149*
H2W	0.9262	0.7594	−0.0734	0.149*
C2	1.0449 (10)	0.9146 (6)	−0.0258 (13)	0.029 (3)
H2	1.1337	0.9136	0.0168	0.035*
N2	1.0149 (9)	0.9190 (5)	−0.1900 (11)	0.030 (2)
O2	1.0988 (7)	0.9106 (5)	0.3253 (8)	0.035 (2)
C3	0.8869 (11)	0.9176 (7)	−0.2454 (13)	0.037 (3)
H3	0.8622	0.9195	−0.3598	0.045*
O3	1.6618 (7)	0.8233 (4)	0.5173 (9)	0.034 (2)
C4	0.7896 (11)	0.9134 (7)	−0.1356 (12)	0.034 (3)
H4	0.7006	0.9130	−0.1775	0.041*
O4	1.7098 (7)	0.7193 (4)	0.6421 (10)	0.0317 (18)
C5	0.9806 (10)	0.9093 (6)	0.2720 (13)	0.027 (3)
O5	0.5044 (7)	0.9079 (4)	−0.0030 (9)	0.0309 (18)
O6	0.3693 (7)	0.9833 (4)	−0.1510 (9)	0.0304 (19)
O7	0.5658 (7)	1.0571 (4)	0.6552 (9)	0.0274 (18)
O8	0.6685 (7)	0.9827 (4)	0.4928 (8)	0.0270 (18)
N10	1.2894 (9)	0.8232 (6)	0.6898 (12)	0.039 (3)
C11	0.4622 (10)	0.9689 (6)	−0.0439 (13)	0.026 (3)
N11	1.4588 (8)	0.7064 (5)	0.7235 (10)	0.024 (2)
C12	0.5689 (10)	1.0120 (6)	0.5441 (11)	0.022 (2)
C6	1.4972 (10)	0.7674 (6)	0.6640 (13)	0.027 (3)
C7	1.4155 (11)	0.8253 (6)	0.6552 (14)	0.031 (3)
H7	1.4498	0.8685	0.6234	0.037*
C8	1.2491 (11)	0.7609 (6)	0.7402 (15)	0.034 (3)
H8	1.1617	0.7560	0.7654	0.041*
C9	1.3340 (11)	0.7018 (7)	0.7569 (14)	0.033 (3)
H9	1.3016	0.6587	0.7922	0.040*
C10	1.6348 (11)	0.7698 (7)	0.6033 (13)	0.030 (3)

	U11	U22	U33	U12	U13	U23
Ag1	0.0338 (5)	0.0520 (7)	0.0262 (4)	0.0081 (4)	0.0096 (4)	0.0043 (4)
C1	0.028 (6)	0.024 (7)	0.026 (6)	−0.007 (5)	0.006 (5)	−0.004 (5)
N1	0.028 (5)	0.035 (6)	0.018 (4)	−0.008 (4)	0.002 (4)	0.001 (4)
Nd1	0.0222 (3)	0.0239 (3)	0.0182 (3)	0.0008 (3)	0.0041 (2)	−0.0008 (3)
O1	0.009 (3)	0.063 (6)	0.017 (3)	−0.001 (4)	0.001 (3)	0.002 (4)
O1W	0.052 (7)	0.092 (11)	0.155 (12)	0.000 (6)	0.020 (7)	−0.042 (9)
C2	0.019 (5)	0.040 (8)	0.028 (6)	0.009 (5)	0.003 (4)	0.009 (5)
N2	0.032 (5)	0.037 (6)	0.022 (5)	−0.001 (4)	0.008 (4)	0.004 (4)
O2	0.021 (4)	0.066 (7)	0.017 (4)	0.004 (4)	−0.004 (3)	−0.006 (4)
C3	0.033 (7)	0.064 (10)	0.014 (5)	0.016 (6)	−0.003 (5)	−0.007 (5)
O3	0.036 (5)	0.040 (6)	0.027 (4)	−0.009 (4)	0.005 (3)	0.015 (4)
C4	0.036 (7)	0.055 (9)	0.012 (5)	−0.002 (6)	0.007 (5)	−0.007 (5)
O4	0.034 (4)	0.015 (4)	0.048 (5)	−0.001 (3)	0.013 (4)	0.008 (4)
C5	0.027 (6)	0.029 (7)	0.025 (5)	−0.008 (5)	0.010 (5)	0.006 (5)
O5	0.039 (5)	0.029 (5)	0.025 (4)	−0.004 (4)	0.000 (3)	0.003 (4)
O6	0.022 (4)	0.033 (5)	0.035 (4)	0.005 (3)	−0.007 (3)	0.002 (4)
O7	0.024 (4)	0.033 (5)	0.024 (4)	−0.001 (3)	0.000 (3)	−0.008 (4)
O8	0.026 (4)	0.034 (5)	0.021 (4)	0.007 (3)	0.006 (3)	−0.007 (3)
N10	0.029 (5)	0.043 (7)	0.043 (6)	0.004 (5)	−0.001 (5)	0.004 (5)
C11	0.024 (6)	0.028 (7)	0.027 (6)	0.002 (5)	0.003 (5)	0.008 (5)
N11	0.018 (4)	0.027 (6)	0.029 (5)	0.000 (4)	0.010 (4)	0.001 (4)
C12	0.034 (6)	0.020 (6)	0.012 (5)	0.000 (5)	0.003 (4)	−0.012 (4)
C6	0.026 (6)	0.032 (7)	0.023 (5)	0.000 (5)	0.002 (4)	0.013 (5)
C7	0.034 (7)	0.016 (7)	0.043 (7)	−0.001 (5)	0.003 (5)	0.002 (5)
C8	0.033 (6)	0.022 (7)	0.050 (7)	−0.004 (5)	0.019 (6)	0.011 (6)
C9	0.038 (7)	0.029 (7)	0.032 (6)	−0.004 (5)	0.006 (5)	0.011 (5)
C10	0.044 (7)	0.029 (8)	0.019 (5)	−0.007 (6)	0.010 (5)	−0.004 (5)

Ag1—N2i	2.291 (9)	C3—H3	0.9300
Ag1—O2	2.299 (7)	O3—C10	1.267 (13)
Ag1—N10	2.360 (10)	O3—Nd1vii	2.461 (7)
C1—N1	1.320 (13)	C4—H4	0.9300
C1—C2	1.370 (14)	O4—C10	1.240 (14)
C1—C5	1.530 (14)	O4—Nd1viii	2.465 (7)
N1—C4	1.319 (13)	O5—C11	1.259 (13)
N1—Nd1	2.707 (8)	O6—C11	1.242 (12)
Nd1—O1	2.423 (6)	O6—Nd1ii	2.455 (8)
Nd1—O6ii	2.455 (8)	O7—C12	1.235 (11)
Nd1—O5	2.456 (7)	O7—Nd1v	2.482 (7)
Nd1—O3iii	2.461 (7)	O8—C12	1.252 (12)
Nd1—O4iv	2.465 (8)	N10—C8	1.319 (15)
Nd1—O7v	2.482 (7)	N10—C7	1.332 (14)
Nd1—O8	2.486 (7)	C11—C11ii	1.53 (2)
Nd1—N11iv	2.692 (9)	N11—C9	1.317 (13)
O1—C5	1.260 (12)	N11—C6	1.318 (14)
O1W—H1W	0.8400	N11—Nd1viii	2.692 (9)
O1W—H2W	0.8405	C12—C12v	1.57 (2)
C2—N2	1.328 (13)	C6—C7	1.367 (15)
C2—H2	0.9300	C6—C10	1.517 (15)
N2—C3	1.329 (13)	C7—H7	0.9300
N2—Ag1vi	2.291 (9)	C8—C9	1.406 (16)
O2—C5	1.231 (12)	C8—H8	0.9300
C3—C4	1.385 (15)	C9—H9	0.9300
N2i—Ag1—O2	124.8 (3)	N2—C2—H2	119.2
N2i—Ag1—N10	98.4 (3)	C1—C2—H2	119.2
O2—Ag1—N10	106.5 (3)	C2—N2—C3	117.0 (9)
N1—C1—C2	121.5 (10)	C2—N2—Ag1vi	127.6 (7)
N1—C1—C5	116.3 (9)	C3—N2—Ag1vi	115.3 (7)
C2—C1—C5	122.3 (9)	C5—O2—Ag1	120.1 (7)
C1—N1—C4	117.7 (9)	N2—C3—C4	121.1 (10)
C1—N1—Nd1	116.7 (6)	N2—C3—H3	119.5
C4—N1—Nd1	125.5 (7)	C4—C3—H3	119.5
O1—Nd1—O6ii	93.6 (3)	C10—O3—Nd1vii	153.6 (7)
O1—Nd1—O5	137.2 (2)	N1—C4—C3	121.1 (10)
O6ii—Nd1—O5	65.6 (2)	N1—C4—H4	119.4
O1—Nd1—O3iii	78.7 (2)	C3—C4—H4	119.4
O6ii—Nd1—O3iii	144.2 (3)	C10—O4—Nd1viii	126.5 (7)
O5—Nd1—O3iii	139.7 (3)	O2—C5—O1	128.3 (10)
O1—Nd1—O4iv	84.8 (3)	O2—C5—C1	117.1 (9)
O6ii—Nd1—O4iv	133.5 (3)	O1—C5—C1	114.6 (9)
O5—Nd1—O4iv	84.6 (3)	C11—O5—Nd1	118.1 (7)
O3iii—Nd1—O4iv	81.1 (3)	C11—O6—Nd1ii	118.1 (7)
O1—Nd1—O7v	136.9 (2)	C12—O7—Nd1v	122.0 (6)
O6ii—Nd1—O7v	74.4 (2)	C12—O8—Nd1	121.6 (6)
O5—Nd1—O7v	75.5 (2)	C8—N10—C7	114.8 (10)
O3iii—Nd1—O7v	87.6 (3)	C8—N10—Ag1	128.1 (8)
O4iv—Nd1—O7v	133.3 (2)	C7—N10—Ag1	116.0 (8)
O1—Nd1—O8	72.4 (2)	O6—C11—O5	126.5 (10)
O6ii—Nd1—O8	69.4 (2)	O6—C11—C11ii	117.6 (13)
O5—Nd1—O8	125.8 (3)	O5—C11—C11ii	115.8 (11)
O3iii—Nd1—O8	75.0 (3)	C9—N11—C6	116.9 (9)
O4iv—Nd1—O8	149.6 (2)	C9—N11—Nd1viii	127.6 (7)
O7v—Nd1—O8	64.6 (2)	C6—N11—Nd1viii	115.5 (6)
O1—Nd1—N11iv	138.7 (3)	O7—C12—O8	128.2 (10)
O6ii—Nd1—N11iv	127.1 (2)	O7—C12—C12v	116.3 (11)
O5—Nd1—N11iv	68.0 (3)	O8—C12—C12v	115.5 (10)
O3iii—Nd1—N11iv	71.9 (3)	N11—C6—C7	121.2 (10)
O4iv—Nd1—N11iv	62.7 (3)	N11—C6—C10	117.0 (10)
O7v—Nd1—N11iv	70.6 (3)	C7—C6—C10	121.9 (10)
O8—Nd1—N11iv	124.5 (2)	N10—C7—C6	123.6 (11)
O1—Nd1—N1	61.6 (2)	N10—C7—H7	118.2
O6ii—Nd1—N1	71.3 (3)	C6—C7—H7	118.2
O5—Nd1—N1	76.1 (2)	N10—C8—C9	122.1 (11)
O3iii—Nd1—N1	130.2 (3)	N10—C8—H8	118.9
O4iv—Nd1—N1	67.3 (3)	C9—C8—H8	118.9
O7v—Nd1—N1	142.1 (3)	N11—C9—C8	121.1 (11)
O8—Nd1—N1	115.7 (3)	N11—C9—H9	119.5
N11iv—Nd1—N1	119.8 (3)	C8—C9—H9	119.5
C5—O1—Nd1	130.6 (6)	O4—C10—O3	126.2 (11)
H1W—O1W—H2W	111.8	O4—C10—C6	117.0 (10)
N2—C2—C1	121.5 (10)	O3—C10—C6	116.8 (10)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O4iv	0.84	2.31	2.975 (13)	137
C3—H3···O1vi	0.93	2.34	3.221 (12)	158
C3—H3···O8vi	0.93	2.49	3.150 (13)	128
C4—H4···O5	0.93	2.54	3.170 (13)	125
C9—H9···O2ix	0.93	2.47	3.270 (15)	145
C9—H9···O7x	0.93	2.35	2.971 (15)	124

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯O4i	0.84	2.31	2.975 (13)	137
C3—H3⋯O1ii	0.93	2.34	3.221 (12)	158
C3—H3⋯O8ii	0.93	2.49	3.150 (13)	128
C4—H4⋯O5	0.93	2.54	3.170 (13)	125
C9—H9⋯O2iii	0.93	2.47	3.270 (15)	145
C9—H9⋯O7iv	0.93	2.35	2.971 (15)	124

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