Literature DB >> 22058888

Poly[[(μ-3-amino-pyrazine-2-carboxyl-ato-κN,O:O')diaqua-(μ-oxalato-κO,O:O,O)lanthanum(III)] monohydrate].

Abstract

The water-coordinated La(III) atom in the title compound, {[La(C(5)H(4)N(3)O(2))(C(2)O(4))(H(2)O)(2)]·H(2)O}(n), is N,O-chelated by a 3-amino-pyrazine-2-carboxyl-ate ion; this ion links adjacent metal atoms to form a chain parallel to [010]. The oxalate ion serves as a bis-bidentate chelate that links adjacent metal atoms to form a chain parallel to [001]. The two bridging ions give rise to a layer motif parallel to (100) in which the La(III) atom exists in a distorted tricapped trigonal prismatic geometry. Extensive hydrogen bonding between the constituents stabilizes the structure.

Entities: Chemical Disease Species

Year: 2011 PMID： 22058888 PMCID： PMC3200678 DOI： 10.1107/S1600536811034404

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

Related literature

For a related structure, see: Leciejewicz et al. (2004 ▶). For pyrazinecarboxylic acid decomposition with subsequent oxalate formation, which has been documented in other lanthanum systems, see: Li et al. (2006 ▶).

Experimental

Crystal data

[La(C5H4N3O2)(C2O4)(H2O)2]·H2O M = 419.09 Monoclinic, a = 18.2193 (5) Å b = 10.5507 (3) Å c = 13.1307 (5) Å β = 105.292 (1)° V = 2434.70 (13) Å3 Z = 8 Mo Kα radiation μ = 3.56 mm−1 T = 293 K 0.14 × 0.12 × 0.08 mm

Data collection

Rigaku RAXIS-RAPID IP diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.636, T max = 0.764 11571 measured reflections 2780 independent reflections 2408 reflections with I > 2σ(I) R int = 0.038

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.064 S = 1.03 2780 reflections 213 parameters 11 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 1.19 e Å−3 Δρmin = −0.90 e Å−3 Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalClear (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811034404/qk2018sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811034404/qk2018Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[La(C₅H₄N₃O₂)(C₂O₄)(H₂O)₂]·H₂O	F(000) = 1616
M_r = 419.09	D_x = 2.287 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 8439 reflections
a = 18.2193 (5) Å	θ = 3.2–27.4°
b = 10.5507 (3) Å	µ = 3.56 mm⁻¹
c = 13.1307 (5) Å	T = 293 K
β = 105.292 (1)°	Prism, colourless
V = 2434.70 (13) Å³	0.14 × 0.12 × 0.08 mm
Z = 8

Rigaku RAXIS-RAPID IP diffractometer	2780 independent reflections
Radiation source: fine-focus sealed tube	2408 reflections with I > 2σ(I)
graphite	R_int = 0.038
ω scans	θ_max = 27.4°, θ_min = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −22→23
T_min = 0.636, T_max = 0.764	k = −13→11
11571 measured reflections	l = −17→17

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.064	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ²(F_o²) + (0.0366P)² + 0.9654P] where P = (F_o² + 2F_c²)/3
2780 reflections	(Δ/σ)_max = 0.001
213 parameters	Δρ_max = 1.19 e Å⁻³
11 restraints	Δρ_min = −0.90 e Å⁻³

	x	y	z	U_iso*/U_eq
La1	0.753537 (8)	0.505715 (13)	0.708865 (11)	0.01578 (8)
O1	0.70771 (10)	0.72700 (18)	0.73633 (16)	0.0229 (4)
O3	0.82152 (11)	0.4381 (2)	0.56948 (15)	0.0265 (5)
O4	0.70436 (11)	0.60558 (18)	0.52529 (15)	0.0232 (4)
O5	0.70189 (11)	0.59526 (17)	0.35400 (15)	0.0215 (4)
O6	0.81026 (11)	0.41769 (18)	0.39750 (15)	0.0237 (4)
O1W	0.67446 (12)	0.33869 (19)	0.59002 (18)	0.0301 (5)
H11	0.6840 (18)	0.2609 (12)	0.590 (3)	0.046 (11)*
H12	0.6393 (18)	0.356 (3)	0.536 (2)	0.064 (13)*
O2W	0.86289 (12)	0.66714 (19)	0.70250 (17)	0.0273 (5)
H21	0.8424 (19)	0.7373 (19)	0.682 (3)	0.053 (12)*
H22	0.8870 (19)	0.643 (3)	0.660 (2)	0.052 (12)*
O2	0.62477 (11)	0.88451 (18)	0.70103 (17)	0.0283 (5)
O3W	0.99478 (18)	0.6325 (3)	0.6200 (3)	0.0556 (7)
H31	1.0385 (11)	0.644 (4)	0.661 (2)	0.075 (17)*
H32	0.999 (2)	0.628 (4)	0.5577 (12)	0.073 (16)*
N1	0.59859 (12)	0.5541 (2)	0.67230 (18)	0.0188 (5)
N2	0.44670 (13)	0.6197 (2)	0.5937 (2)	0.0241 (5)
N3	0.47703 (15)	0.8320 (3)	0.6050 (3)	0.0338 (7)
H1	0.5096 (15)	0.893 (2)	0.630 (3)	0.033 (10)*
H2	0.4284 (8)	0.851 (3)	0.593 (3)	0.043 (10)*
C1	0.54410 (17)	0.4653 (3)	0.6480 (2)	0.0233 (6)
H1A	0.5572	0.3801	0.6577	0.028*
C2	0.4688 (2)	0.4990 (2)	0.6088 (3)	0.0256 (7)
H2A	0.4321	0.4355	0.5924	0.031*
C3	0.50011 (15)	0.7099 (3)	0.6213 (2)	0.0204 (6)
C4	0.57805 (15)	0.6755 (2)	0.6627 (2)	0.0176 (5)
C5	0.64079 (15)	0.7689 (3)	0.7022 (2)	0.0196 (6)
C6	0.72721 (15)	0.5654 (2)	0.4499 (2)	0.0177 (5)
C7	0.79244 (16)	0.4649 (3)	0.4748 (2)	0.0180 (5)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
La1	0.01427 (11)	0.02279 (11)	0.00982 (11)	0.00134 (6)	0.00236 (7)	0.00027 (5)
O1	0.0147 (10)	0.0293 (10)	0.0226 (11)	−0.0015 (9)	0.0012 (8)	−0.0039 (8)
O3	0.0269 (11)	0.0386 (12)	0.0137 (10)	0.0120 (10)	0.0048 (8)	0.0028 (9)
O4	0.0259 (10)	0.0301 (10)	0.0150 (10)	0.0091 (9)	0.0081 (8)	0.0023 (8)
O5	0.0249 (10)	0.0275 (10)	0.0117 (10)	0.0057 (8)	0.0038 (8)	0.0036 (8)
O6	0.0312 (11)	0.0256 (10)	0.0149 (10)	0.0068 (9)	0.0072 (8)	0.0002 (8)
O1W	0.0312 (12)	0.0211 (10)	0.0297 (13)	0.0042 (10)	−0.0066 (10)	−0.0027 (9)
O2W	0.0276 (11)	0.0256 (11)	0.0309 (13)	0.0028 (10)	0.0117 (10)	0.0026 (9)
O2	0.0225 (10)	0.0244 (10)	0.0337 (13)	−0.0033 (9)	−0.0001 (9)	−0.0059 (9)
O3W	0.0518 (18)	0.071 (2)	0.0455 (19)	0.0010 (17)	0.0152 (15)	−0.0004 (16)
N1	0.0172 (11)	0.0232 (12)	0.0160 (12)	0.0003 (10)	0.0045 (9)	0.0008 (9)
N2	0.0165 (11)	0.0327 (13)	0.0223 (13)	−0.0017 (11)	0.0038 (10)	−0.0022 (10)
N3	0.0189 (14)	0.0286 (14)	0.0486 (19)	0.0028 (12)	−0.0005 (13)	−0.0035 (13)
C1	0.0224 (15)	0.0234 (13)	0.0242 (16)	−0.0008 (13)	0.0064 (12)	0.0004 (12)
C2	0.0213 (16)	0.0301 (17)	0.0256 (18)	−0.0086 (12)	0.0067 (13)	−0.0006 (11)
C3	0.0184 (13)	0.0275 (14)	0.0150 (14)	0.0026 (12)	0.0038 (11)	−0.0032 (11)
C4	0.0163 (13)	0.0233 (13)	0.0129 (13)	−0.0031 (11)	0.0032 (10)	−0.0025 (10)
C5	0.0195 (14)	0.0264 (14)	0.0133 (14)	0.0007 (12)	0.0049 (11)	−0.0008 (11)
C6	0.0180 (13)	0.0189 (13)	0.0163 (14)	−0.0004 (12)	0.0044 (10)	0.0012 (10)
C7	0.0163 (14)	0.0225 (12)	0.0144 (14)	0.0003 (12)	0.0029 (11)	0.0002 (11)

La1—O1W	2.536 (2)	O2W—H22	0.838 (10)
La1—O1	2.5371 (19)	O2—C5	1.254 (3)
La1—O6ⁱ	2.5507 (19)	O2—La1^iv	2.5627 (19)
La1—O2ⁱⁱ	2.5627 (19)	O3W—H31	0.844 (10)
La1—O4	2.5659 (19)	O3W—H32	0.843 (10)
La1—O3	2.5668 (19)	N1—C4	1.331 (3)
La1—O5ⁱ	2.5687 (18)	N1—C1	1.341 (4)
La1—O2W	2.639 (2)	N2—C2	1.334 (3)
La1—N1	2.783 (2)	N2—C3	1.341 (4)
O1—C5	1.263 (3)	N3—C3	1.355 (4)
O3—C7	1.248 (3)	N3—H1	0.880 (10)
O4—C6	1.246 (3)	N3—H2	0.880 (10)
O5—C6	1.261 (3)	C1—C2	1.379 (5)
O5—La1ⁱⁱⁱ	2.5687 (18)	C1—H1A	0.9300
O6—C7	1.248 (3)	C2—H2A	0.9300
O6—La1ⁱⁱⁱ	2.5507 (19)	C3—C4	1.427 (4)
O1W—H11	0.838 (10)	C4—C5	1.495 (4)
O1W—H12	0.841 (10)	C6—C7	1.561 (4)
O2W—H21	0.842 (10)

O1W—La1—O1	124.90 (6)	C6—O5—La1ⁱⁱⁱ	121.85 (17)
O1W—La1—O6ⁱ	146.79 (7)	C7—O6—La1ⁱⁱⁱ	122.53 (17)
O1—La1—O6ⁱ	68.57 (6)	La1—O1W—H11	126 (2)
O1W—La1—O2ⁱⁱ	102.67 (6)	La1—O1W—H12	123 (2)
O1—La1—O2ⁱⁱ	132.12 (6)	H11—O1W—H12	109.1 (17)
O6ⁱ—La1—O2ⁱⁱ	68.29 (7)	La1—O2W—H21	108 (2)
O1W—La1—O4	72.92 (7)	La1—O2W—H22	111 (3)
O1—La1—O4	73.09 (6)	H21—O2W—H22	108.7 (17)
O6ⁱ—La1—O4	137.21 (6)	C5—O2—La1^iv	108.04 (16)
O2ⁱⁱ—La1—O4	133.14 (6)	H31—O3W—H32	108.1 (17)
O1W—La1—O3	70.77 (7)	C4—N1—C1	118.5 (2)
O1—La1—O3	126.58 (7)	C4—N1—La1	116.11 (17)
O6ⁱ—La1—O3	129.22 (6)	C1—N1—La1	124.51 (19)
O2ⁱⁱ—La1—O3	70.67 (7)	C2—N2—C3	117.9 (2)
O4—La1—O3	63.83 (6)	C3—N3—H1	119 (2)
O1W—La1—O5ⁱ	84.75 (7)	C3—N3—H2	120 (2)
O1—La1—O5ⁱ	94.45 (6)	H1—N3—H2	117 (3)
O6ⁱ—La1—O5ⁱ	62.92 (6)	N1—C1—C2	120.7 (3)
O2ⁱⁱ—La1—O5ⁱ	83.81 (6)	N1—C1—H1A	119.7
O4—La1—O5ⁱ	139.62 (6)	C2—C1—H1A	119.7
O3—La1—O5ⁱ	138.92 (6)	N2—C2—C1	122.2 (3)
O1W—La1—O2W	137.74 (7)	N2—C2—H2A	118.9
O1—La1—O2W	71.95 (6)	C1—C2—H2A	118.9
O6ⁱ—La1—O2W	73.16 (6)	N2—C3—N3	117.4 (2)
O2ⁱⁱ—La1—O2W	76.60 (6)	N2—C3—C4	120.1 (2)
O4—La1—O2W	77.57 (7)	N3—C3—C4	122.6 (3)
O3—La1—O2W	69.30 (7)	N1—C4—C3	120.5 (2)
O5ⁱ—La1—O2W	135.93 (6)	N1—C4—C5	115.5 (2)
O1W—La1—N1	68.62 (7)	C3—C4—C5	123.9 (2)
O1—La1—N1	59.92 (6)	O2—C5—O1	123.0 (2)
O6ⁱ—La1—N1	104.01 (6)	O2—C5—C4	118.9 (2)
O2ⁱⁱ—La1—N1	152.36 (7)	O1—C5—C4	118.1 (2)
O4—La1—N1	71.07 (6)	O4—C6—O5	126.7 (3)
O3—La1—N1	125.89 (6)	O4—C6—C7	117.4 (2)
O5ⁱ—La1—N1	69.55 (6)	O5—C6—C7	115.9 (2)
O2W—La1—N1	128.03 (7)	O3—C7—O6	125.9 (3)
C5—O1—La1	126.49 (17)	O3—C7—C6	117.6 (2)
C7—O3—La1	119.28 (17)	O6—C7—C6	116.5 (2)
C6—O4—La1	120.00 (17)

O1W—La1—O1—C5	7.2 (2)	O3—La1—N1—C1	69.9 (2)
O6ⁱ—La1—O1—C5	−138.1 (2)	O5ⁱ—La1—N1—C1	−66.4 (2)
O2ⁱⁱ—La1—O1—C5	−165.2 (2)	O2W—La1—N1—C1	160.6 (2)
O4—La1—O1—C5	61.3 (2)	C4—N1—C1—C2	3.3 (4)
O3—La1—O1—C5	98.2 (2)	La1—N1—C1—C2	−165.7 (2)
O5ⁱ—La1—O1—C5	−79.5 (2)	C3—N2—C2—C1	−2.2 (5)
O2W—La1—O1—C5	143.4 (2)	N1—C1—C2—N2	−0.3 (5)
N1—La1—O1—C5	−16.2 (2)	C2—N2—C3—N3	179.7 (3)
O1W—La1—O3—C7	67.4 (2)	C2—N2—C3—C4	1.6 (4)
O1—La1—O3—C7	−52.4 (2)	C1—N1—C4—C3	−3.8 (4)
O6ⁱ—La1—O3—C7	−143.4 (2)	La1—N1—C4—C3	166.12 (19)
O2ⁱⁱ—La1—O3—C7	179.0 (2)	C1—N1—C4—C5	173.5 (2)
O4—La1—O3—C7	−12.6 (2)	La1—N1—C4—C5	−16.5 (3)
O5ⁱ—La1—O3—C7	124.2 (2)	N2—C3—C4—N1	1.4 (4)
O2W—La1—O3—C7	−98.5 (2)	N3—C3—C4—N1	−176.6 (3)
N1—La1—O3—C7	24.1 (2)	N2—C3—C4—C5	−175.7 (3)
O1W—La1—O4—C6	−66.9 (2)	N3—C3—C4—C5	6.3 (4)
O1—La1—O4—C6	157.1 (2)	La1^iv—O2—C5—O1	−4.6 (3)
O6ⁱ—La1—O4—C6	130.02 (19)	La1^iv—O2—C5—C4	174.72 (19)
O2ⁱⁱ—La1—O4—C6	24.6 (2)	La1—O1—C5—O2	−166.0 (2)
O3—La1—O4—C6	9.60 (19)	La1—O1—C5—C4	14.7 (3)
O5ⁱ—La1—O4—C6	−126.34 (19)	N1—C4—C5—O2	−176.0 (2)
O2W—La1—O4—C6	82.4 (2)	C3—C4—C5—O2	1.2 (4)
N1—La1—O4—C6	−139.6 (2)	N1—C4—C5—O1	3.3 (4)
O1W—La1—N1—C4	−143.34 (19)	C3—C4—C5—O1	−179.4 (3)
O1—La1—N1—C4	16.16 (17)	La1—O4—C6—O5	171.5 (2)
O6ⁱ—La1—N1—C4	70.73 (18)	La1—O4—C6—C7	−6.8 (3)
O2ⁱⁱ—La1—N1—C4	140.54 (18)	La1ⁱⁱⁱ—O5—C6—O4	−177.5 (2)
O4—La1—N1—C4	−64.83 (18)	La1ⁱⁱⁱ—O5—C6—C7	0.8 (3)
O3—La1—N1—C4	−99.37 (19)	La1—O3—C7—O6	−164.8 (2)
O5ⁱ—La1—N1—C4	124.31 (19)	La1—O3—C7—C6	14.4 (3)
O2W—La1—N1—C4	−8.7 (2)	La1ⁱⁱⁱ—O6—C7—O3	−174.9 (2)
O1W—La1—N1—C1	25.9 (2)	La1ⁱⁱⁱ—O6—C7—C6	5.8 (3)
O1—La1—N1—C1	−174.6 (2)	O4—C6—C7—O3	−5.2 (4)
O6ⁱ—La1—N1—C1	−120.0 (2)	O5—C6—C7—O3	176.4 (2)
O2ⁱⁱ—La1—N1—C1	−50.2 (3)	O4—C6—C7—O6	174.1 (2)
O4—La1—N1—C1	104.4 (2)	O5—C6—C7—O6	−4.3 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11···O6^v	0.84 (1)	1.89 (1)	2.720 (3)	169 (3)
O1W—H12···N2^vi	0.84 (1)	2.00 (1)	2.842 (3)	175 (3)
O2W—H21···O5^vii	0.84 (1)	1.95 (1)	2.787 (3)	175 (4)
O2W—H22···O3W	0.84 (1)	2.16 (2)	2.908 (4)	148 (4)
O3W—H31···O2W^viii	0.84 (1)	2.19 (1)	3.017 (4)	165 (4)
O3W—H32···N3^vii	0.84 (1)	2.33 (2)	3.152 (5)	165 (4)
N3—H1···O2	0.88 (1)	2.06 (3)	2.711 (3)	130 (3)
N3—H2···O3^ix	0.88 (1)	2.10 (1)	2.967 (3)	167 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H11⋯O6ⁱ	0.84 (1)	1.89 (1)	2.720 (3)	169 (3)
O1W—H12⋯N2ⁱⁱ	0.84 (1)	2.00 (1)	2.842 (3)	175 (3)
O2W—H21⋯O5ⁱⁱⁱ	0.84 (1)	1.95 (1)	2.787 (3)	175 (4)
O2W—H22⋯O3W	0.84 (1)	2.16 (2)	2.908 (4)	148 (4)
O3W—H31⋯O2W^iv	0.84 (1)	2.19 (1)	3.017 (4)	165 (4)
O3W—H32⋯N3ⁱⁱⁱ	0.84 (1)	2.33 (2)	3.152 (5)	165 (4)
N3—H1⋯O2	0.88 (1)	2.06 (3)	2.711 (3)	130 (3)
N3—H2⋯O3^v	0.88 (1)	2.10 (1)	2.967 (3)	167 (3)

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

2 in total

1. A short history of SHELX.

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

2. [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

2 in total

1 in total

1. catena-Poly[[[bis-(3-amino-pyrazine-2-carboxyl-ato)triaqua-praseodymium(III)]-μ-3-amino-pyrazine-2-carboxyl-ato-[(3-amino-pyrazine-2-carboxyl-ato)diaqua-formatopraseodymium(III)]-μ-3-amino-pyrazine-2-carboxyl-ato] hexa-hydrate].

Authors: Shan Gao; Seik Weng Ng
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2011-08-11

1 in total