Literature DB >> 21577423

Poly[diaqua-(μ(2)-oxalato-κO,O:O,O)(μ(2)-pyrazine-2-carboxyl-ato-κN,O:O,O')neodymium(III)].

Ke-Chun Chen, Huan-Mian Luo, Qiu-Hui Meng, Yi-Fan Luo, Rong-Hua Zeng.

Abstract

In the title complex, [Nd(C(5)H(3)N(2)O(2))(C(2)O(4))(H(2)O)(2)](n), the Nd(III) atom is ten-coordinated by one N atom and three O atoms from two pyrazine-2-carboxyl-ate ligands, four O atoms from two oxalate ligands and two water mol-ecules in a distorted bicapped square-anti-prismatic geometry. The two crystallographically independent oxalate ligands, each lying on an inversion center, act as bridging ligands, linking Nd atoms into an extended zigzag chain. Neighboring chains are linked by the pyrazine-2-carboxyl-ate ligands into a two-dimensional layerlike network in the (10) plane. The layers are further connected by O-H⋯O and O-H⋯N hydrogen bonds, forming a three-dimensional supra-molecular network.

Entities: CellLine Chemical Disease Species

Year: 2009 PMID： 21577423 PMCID： PMC2969933 DOI： 10.1107/S1600536809031250

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For general background to lanthanide coordination frameworks, see: Han et al. (2009 ▶); Li et al. (2006 ▶); Wang et al. (2006 ▶); Zhou et al. (2006 ▶).

Experimental

Crystal data

[Nd(C5H3N2O2)(C2O4)(H2O)2] M = 391.39 Triclinic, a = 7.948 (3) Å b = 8.6512 (18) Å c = 8.7425 (18) Å α = 115.525 (2)° β = 101.970 (3)° γ = 96.306 (3)° V = 517.0 (2) Å3 Z = 2 Mo Kα radiation μ = 5.06 mm−1 T = 296 K 0.23 × 0.19 × 0.17 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.320, T max = 0.420 2533 measured reflections 1824 independent reflections 1756 reflections with I > 2σ(I) R int = 0.065

Refinement

R[F 2 > 2σ(F 2)] = 0.051 wR(F 2) = 0.132 S = 1.08 1824 reflections 175 parameters 6 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 1.95 e Å−3 Δρmin = −2.98 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809031250/hy2217sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809031250/hy2217Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Nd(C₅H₃N₂O₂)(C₂O₄)(H₂O)₂]	Z = 2
M_r = 391.39	F(000) = 374
Triclinic, P1	D_x = 2.514 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.948 (3) Å	Cell parameters from 2522 reflections
b = 8.6512 (18) Å	θ = 2.7–28.3°
c = 8.7425 (18) Å	µ = 5.06 mm⁻¹
α = 115.525 (2)°	T = 296 K
β = 101.970 (3)°	Block, colorless
γ = 96.306 (3)°	0.23 × 0.19 × 0.17 mm
V = 517.0 (2) Å³

Bruker APEXII CCD diffractometer	1824 independent reflections
Radiation source: fine-focus sealed tube	1756 reflections with I > 2σ(I)
graphite	R_int = 0.065
φ and ω scans	θ_max = 25.2°, θ_min = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→9
T_min = 0.320, T_max = 0.420	k = −8→10
2533 measured reflections	l = −10→10

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)] = 0.051	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.132	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ²(F_o²) + (0.0478P)² + 0.0313P] where P = (F_o² + 2F_c²)/3
1824 reflections	(Δ/σ)_max = 0.002
175 parameters	Δρ_max = 1.95 e Å⁻³
6 restraints	Δρ_min = −2.98 e Å⁻³

	x	y	z	U_iso*/U_eq
C1	1.1008 (9)	0.3421 (10)	0.7510 (9)	0.0146 (15)
C2	1.2220 (10)	0.2213 (10)	0.7476 (10)	0.0175 (15)
C3	1.2449 (13)	0.0959 (12)	0.5928 (12)	0.0246 (19)
H3	1.1882	0.0920	0.4865	0.030*
C4	1.4345 (11)	0.0053 (11)	0.7489 (11)	0.0227 (17)
H4	1.5126	−0.0660	0.7543	0.027*
C5	1.4166 (11)	0.1312 (11)	0.9049 (11)	0.0235 (17)
H5	1.4818	0.1415	1.0116	0.028*
C6	0.9283 (8)	1.0062 (9)	0.9289 (9)	0.0114 (14)
C7	0.4413 (9)	0.5252 (9)	0.5645 (9)	0.0156 (15)
H1W	1.058 (11)	0.745 (10)	0.649 (9)	0.023*
H2W	1.143 (10)	0.630 (10)	0.676 (10)	0.023*
H3W	0.599 (5)	0.229 (10)	0.680 (9)	0.023*
H4W	0.731 (9)	0.226 (9)	0.802 (10)	0.023*
N1	1.3077 (9)	0.2389 (9)	0.9065 (8)	0.0175 (13)
N2	1.3439 (9)	−0.0191 (9)	0.5892 (9)	0.0240 (15)
Nd1	0.83941 (4)	0.58653 (4)	0.82456 (4)	0.0124 (2)
O1	1.0011 (8)	0.3228 (8)	0.6106 (7)	0.0244 (13)
O2	1.1050 (7)	0.4616 (7)	0.9021 (7)	0.0182 (11)
O3	0.8094 (7)	0.8693 (7)	0.8272 (7)	0.0185 (11)
O4	0.9419 (7)	1.1485 (7)	0.9251 (7)	0.0192 (11)
O5	0.5149 (7)	0.5678 (8)	0.7214 (7)	0.0230 (12)
O6	0.2843 (7)	0.5193 (8)	0.4984 (6)	0.0210 (11)
O1W	1.0754 (9)	0.6971 (9)	0.7148 (8)	0.0240 (13)
O2W	0.7008 (7)	0.2834 (7)	0.7480 (7)	0.0204 (11)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.019 (4)	0.013 (4)	0.016 (4)	0.002 (3)	0.009 (3)	0.009 (3)
C2	0.024 (4)	0.013 (4)	0.016 (4)	0.001 (3)	0.005 (3)	0.007 (3)
C3	0.034 (5)	0.016 (5)	0.020 (4)	0.005 (4)	0.007 (4)	0.006 (4)
C4	0.028 (4)	0.016 (4)	0.028 (4)	0.010 (3)	0.016 (4)	0.010 (4)
C5	0.025 (4)	0.024 (4)	0.030 (4)	0.011 (3)	0.009 (3)	0.018 (4)
C6	0.008 (3)	0.006 (3)	0.014 (3)	−0.001 (2)	−0.001 (3)	0.001 (3)
C7	0.018 (4)	0.006 (4)	0.016 (4)	0.000 (3)	0.007 (3)	−0.001 (3)
N1	0.023 (3)	0.015 (3)	0.018 (3)	0.008 (3)	0.007 (3)	0.009 (3)
N2	0.029 (4)	0.013 (3)	0.027 (4)	0.003 (3)	0.014 (3)	0.004 (3)
Nd1	0.0159 (3)	0.0065 (3)	0.0146 (3)	0.00016 (19)	0.0035 (2)	0.0058 (2)
O1	0.032 (3)	0.027 (3)	0.021 (3)	0.010 (3)	0.009 (2)	0.016 (3)
O2	0.022 (3)	0.014 (3)	0.024 (3)	0.006 (2)	0.011 (2)	0.012 (2)
O3	0.016 (3)	0.013 (3)	0.024 (3)	0.000 (2)	0.000 (2)	0.010 (2)
O4	0.025 (3)	0.010 (3)	0.024 (3)	0.002 (2)	0.003 (2)	0.011 (2)
O5	0.022 (3)	0.033 (3)	0.019 (3)	0.009 (2)	0.008 (2)	0.014 (3)
O6	0.019 (3)	0.024 (3)	0.015 (3)	0.004 (2)	0.003 (2)	0.006 (2)
O1W	0.033 (3)	0.022 (3)	0.022 (3)	0.008 (3)	0.013 (3)	0.012 (3)
O2W	0.029 (3)	0.007 (3)	0.022 (3)	−0.003 (2)	0.006 (2)	0.006 (2)

C1—O1	1.246 (9)	Nd1—O2W	2.467 (5)
C1—O2	1.270 (9)	Nd1—O3	2.474 (5)
C1—C2	1.492 (10)	Nd1—O6ⁱⁱ	2.490 (5)
C2—N1	1.350 (10)	Nd1—O4ⁱ	2.508 (5)
C2—C3	1.386 (11)	Nd1—O5	2.512 (5)
C3—N2	1.328 (11)	Nd1—O1W	2.549 (6)
C3—H3	0.9300	Nd1—O2ⁱⁱⁱ	2.557 (5)
C4—N2	1.345 (11)	Nd1—O2	2.573 (5)
C4—C5	1.379 (11)	Nd1—N1ⁱⁱⁱ	2.765 (6)
C4—H4	0.9300	Nd1—O1	2.885 (6)
C5—N1	1.337 (10)	O2—Nd1ⁱⁱⁱ	2.557 (5)
C5—H5	0.9300	O4—Nd1ⁱ	2.508 (5)
C6—O4	1.239 (9)	O6—Nd1ⁱⁱ	2.490 (5)
C6—O3	1.259 (9)	O1W—H1W	0.84 (9)
C6—C6ⁱ	1.553 (13)	O1W—H2W	0.85 (8)
C7—O5	1.243 (9)	O2W—H3W	0.84 (5)
C7—O6	1.247 (9)	O2W—H4W	0.84 (8)
C7—C7ⁱⁱ	1.560 (13)

O1—C1—O2	123.1 (7)	O6ⁱⁱ—Nd1—O2ⁱⁱⁱ	151.94 (19)
O1—C1—C2	120.3 (6)	O4ⁱ—Nd1—O2ⁱⁱⁱ	72.00 (17)
O2—C1—C2	116.6 (6)	O5—Nd1—O2ⁱⁱⁱ	107.89 (16)
N1—C2—C3	121.0 (7)	O1W—Nd1—O2ⁱⁱⁱ	125.89 (18)
N1—C2—C1	115.7 (6)	O2W—Nd1—O2	76.93 (18)
C3—C2—C1	123.3 (7)	O3—Nd1—O2	133.80 (17)
N2—C3—C2	123.2 (8)	O6ⁱⁱ—Nd1—O2	113.72 (16)
N2—C3—H3	118.4	O4ⁱ—Nd1—O2	76.60 (17)
C2—C3—H3	118.4	O5—Nd1—O2	153.11 (18)
N2—C4—C5	122.9 (7)	O1W—Nd1—O2	74.92 (18)
N2—C4—H4	118.6	O2ⁱⁱⁱ—Nd1—O2	60.11 (19)
C5—C4—H4	118.6	O2W—Nd1—N1ⁱⁱⁱ	97.86 (19)
N1—C5—C4	121.6 (7)	O3—Nd1—N1ⁱⁱⁱ	72.90 (18)
N1—C5—H5	119.2	O6ⁱⁱ—Nd1—N1ⁱⁱⁱ	128.29 (18)
C4—C5—H5	119.2	O4ⁱ—Nd1—N1ⁱⁱⁱ	68.70 (19)
O4—C6—O3	126.2 (6)	O5—Nd1—N1ⁱⁱⁱ	65.79 (18)
O4—C6—C6ⁱ	117.3 (8)	O1W—Nd1—N1ⁱⁱⁱ	131.7 (2)
O3—C6—C6ⁱ	116.4 (8)	O2ⁱⁱⁱ—Nd1—N1ⁱⁱⁱ	59.62 (17)
O5—C7—O6	127.3 (6)	O2—Nd1—N1ⁱⁱⁱ	116.80 (17)
O5—C7—C7ⁱⁱ	116.5 (8)	O2W—Nd1—O1	66.01 (18)
O6—C7—C7ⁱⁱ	116.2 (8)	O3—Nd1—O1	128.48 (16)
C5—N1—C2	116.2 (7)	O6ⁱⁱ—Nd1—O1	66.65 (16)
C5—N1—Nd1ⁱⁱⁱ	126.3 (5)	O4ⁱ—Nd1—O1	113.54 (17)
C2—N1—Nd1ⁱⁱⁱ	114.6 (5)	O5—Nd1—O1	120.34 (17)
C3—N2—C4	114.9 (7)	O1W—Nd1—O1	64.46 (19)
O2W—Nd1—O3	149.08 (18)	O2ⁱⁱⁱ—Nd1—O1	99.62 (15)
O2W—Nd1—O6ⁱⁱ	83.06 (18)	O2—Nd1—O1	47.38 (16)
O3—Nd1—O6ⁱⁱ	80.47 (18)	N1ⁱⁱⁱ—Nd1—O1	158.20 (17)
O2W—Nd1—O4ⁱ	139.97 (17)	C1—O1—Nd1	87.4 (4)
O3—Nd1—O4ⁱ	65.15 (16)	C1—O2—Nd1ⁱⁱⁱ	122.1 (4)
O6ⁱⁱ—Nd1—O4ⁱ	135.42 (18)	C1—O2—Nd1	101.6 (4)
O2W—Nd1—O5	76.22 (19)	Nd1ⁱⁱⁱ—O2—Nd1	119.89 (19)
O3—Nd1—O5	73.09 (18)	C6—O3—Nd1	120.1 (4)
O6ⁱⁱ—Nd1—O5	64.36 (16)	C6—O4—Nd1ⁱ	119.1 (4)
O4ⁱ—Nd1—O5	124.93 (17)	C7—O5—Nd1	121.0 (4)
O2W—Nd1—O1W	130.01 (19)	C7—O6—Nd1ⁱⁱ	121.8 (4)
O3—Nd1—O1W	68.27 (19)	Nd1—O1W—H1W	125 (5)
O6ⁱⁱ—Nd1—O1W	71.92 (19)	Nd1—O1W—H2W	117 (6)
O4ⁱ—Nd1—O1W	69.52 (19)	H1W—O1W—H2W	105 (8)
O5—Nd1—O1W	125.09 (18)	Nd1—O2W—H3W	124 (5)
O2W—Nd1—O2ⁱⁱⁱ	68.90 (17)	Nd1—O2W—H4W	128 (5)
O3—Nd1—O2ⁱⁱⁱ	124.64 (16)	H3W—O2W—H4W	106 (8)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W···O1^iv	0.84 (9)	2.02 (6)	2.707 (8)	139 (7)
O1W—H2W···O6^v	0.85 (8)	2.07 (4)	2.838 (8)	152 (6)
O2W—H3W···N2^vi	0.84 (5)	2.50 (5)	3.229 (9)	145 (6)
O2W—H4W···O4^vii	0.84 (8)	2.13 (4)	2.872 (8)	147 (7)

Table 1

Selected bond lengths (Å)

Nd1—O2W	2.467 (5)
Nd1—O3	2.474 (5)
Nd1—O6ⁱ	2.490 (5)
Nd1—O4ⁱⁱ	2.508 (5)
Nd1—O5	2.512 (5)
Nd1—O1W	2.549 (6)
Nd1—O2ⁱⁱⁱ	2.557 (5)
Nd1—O2	2.573 (5)
Nd1—N1ⁱⁱⁱ	2.765 (6)
Nd1—O1	2.885 (6)

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

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1W⋯O1^iv	0.84 (9)	2.02 (6)	2.707 (8)	139 (7)
O1W—H2W⋯O6^v	0.85 (8)	2.07 (4)	2.838 (8)	152 (6)
O2W—H3W⋯N2^vi	0.84 (5)	2.50 (5)	3.229 (9)	145 (6)
O2W—H4W⋯O4^vii	0.84 (8)	2.13 (4)	2.872 (8)	147 (7)

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

4 in total

Review 1. Lanthanide-transition metal coordination polymers based on multiple N- and O-donor ligands.

Authors: Youfu Zhou; Maochun Hong; Xintao Wu
Journal: Chem Commun (Camb) Date: 2005-11-22 Impact factor: 6.222

2. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

3. [Ln2(C2O4)2(pyzc)2(H2O)2]n[Ln = Pr (1), Er (2)]: novel two-dimensional lanthanide coordination polymers with 2-pyrazinecarboxylate and oxalate.

Authors: Bing Li; Wen Gu; Li-Zhi Zhang; Jie Qu; Zhen-Ping Ma; Xin Liu; Dai-Zheng Liao
Journal: Inorg Chem Date: 2006-12-25 Impact factor: 5.165

4. A sodalite-like framework based on octacyanomolybdate and neodymium with guest methanol molecules and neodymium octahydrate ions.

Authors: Zhao-Xi Wang; Xiao-Fei Shen; Jun Wang; Peng Zhang; Yi-Zhi Li; Emmanuel N Nfor; You Song; Shin-ichi Ohkoshi; Kazuhito Hashimoto; Xiao-Zeng You
Journal: Angew Chem Int Ed Engl Date: 2006-05-12 Impact factor: 15.336

4 in total