The crystal structure of catena-poly[[(6-carboxypyridine-2-carboxylato-κ3O,N,O′)lithium(I)]-μ-aqua-κ2O:O], [Li(C7H4NO4)(H2O)]n, contains the Li+ ion coordinated to two O atoms and the N atom of the 6-carboxypyridine-2-carboxylate ligand, and to two water O atoms, forming a pentavalent coordination geometry. The molecule resides on a mirror plane which contains the Li and N atoms, the para-CH unit, and the O atom of the coordinated water molecule. The O atom of the water molecule is coordinated to two Li atoms, forming an infinite polymeric chain.
Supporting information
CCDC reference: 184459
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 2000); program(s) used to solve structure: MITHRIL90 (Gilmore, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.
catena-poly[[(6-carboxypyridine-2-carboxylato-
κ3O,
N,
O')lithium(I)]-µ- aqua-
κ2O:
O]
top
Crystal data top
[Li(C7H4NO4)H2O] | F(000) = 196.0 |
Mr = 191.07 | Dx = 1.689 Mg m−3 |
Monoclinic, P21/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yb | Cell parameters from 25 reflections |
a = 3.513 (2) Å | θ = 13.5–14.8° |
b = 11.802 (2) Å | µ = 0.14 mm−1 |
c = 9.191 (1) Å | T = 296 K |
β = 99.50 (2)° | Plate, colourless |
V = 375.8 (2) Å3 | 0.4 × 0.2 × 0.1 mm |
Z = 2 | |
Data collection top
Rigaku AFC-5R diffractometer | Rint = 0.024 |
ω/2θ scans | θmax = 27.5° |
Absorption correction: ψ-scan (North et al., 1968) | h = 0→4 |
Tmin = 0.966, Tmax = 0.986 | k = 0→15 |
1056 measured reflections | l = −11→11 |
910 independent reflections | 3 standard reflections every 150 reflections |
598 reflections with I > 2σ(I) | intensity decay: <1% |
Refinement top
Refinement on F2 | w = 1/[σ2(Fo2) + (0.1419P)2 + 0.0837P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.068 | (Δ/σ)max < 0.001 |
wR(F2) = 0.235 | Δρmax = 0.60 e Å−3 |
S = 1.15 | Δρmin = −0.58 e Å−3 |
910 reflections | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
71 parameters | Extinction coefficient: 0.068 |
H-atom parameters not refined | |
Special details top
Refinement. Refinement using reflections with F2 > -10.0 σ(F2). The
weighted R-factor (wR) and goodness of fit (S) are based
on F2. R-factor (gt) are based on F. The threshold
expression of F2 > 2.0 σ(F2) is used only for calculating
R-factor (gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
O1 | 0.0873 (7) | 0.0743 (2) | 0.4201 (2) | 0.0298 (7) | |
O2 | 0.2198 (8) | −0.0463 (2) | 0.2461 (3) | 0.0350 (8) | |
O3 | −0.312 (1) | 0.2500 | 0.6018 (3) | 0.0277 (9) | |
N1 | 0.195 (1) | 0.2500 | 0.2711 (4) | 0.0190 (9) | |
C1 | 0.2265 (9) | 0.1522 (2) | 0.2009 (3) | 0.0210 (7) | |
C2 | 0.2884 (10) | 0.1484 (3) | 0.0563 (4) | 0.0255 (8) | |
C3 | 0.322 (2) | 0.2500 | −0.0158 (5) | 0.028 (1) | |
C4 | 0.1783 (10) | 0.0491 (3) | 0.2936 (3) | 0.0234 (8) | |
Li1 | 0.127 (3) | 0.2500 | 0.4837 (9) | 0.033 (2) | |
H1 | 0.3052 | 0.0812 | 0.0095 | 0.0232* | |
H2 | 0.3393 | 0.2500 | −0.1124 | 0.0482* | |
H3 | −0.1908 | 0.0697 | 0.4100 | 0.0482* | 0.50 |
H4 | −0.2709 | 0.1999 | 0.6650 | 0.0482* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
O1 | 0.050 (2) | 0.013 (1) | 0.029 (1) | −0.003 (1) | 0.015 (1) | 0.0006 (9) |
O2 | 0.062 (2) | 0.009 (1) | 0.035 (1) | 0.002 (1) | 0.012 (1) | −0.0029 (9) |
O3 | 0.042 (2) | 0.014 (2) | 0.028 (2) | 0.0000 | 0.008 (1) | 0.0000 |
N1 | 0.030 (2) | 0.009 (2) | 0.019 (2) | 0.0000 | 0.006 (1) | 0.0000 |
C1 | 0.022 (1) | 0.012 (1) | 0.028 (2) | 0.001 (1) | 0.004 (1) | −0.001 (1) |
C2 | 0.030 (2) | 0.019 (2) | 0.028 (2) | 0.003 (1) | 0.007 (1) | −0.003 (1) |
C3 | 0.034 (3) | 0.027 (3) | 0.023 (2) | 0.0000 | 0.006 (2) | 0.0000 |
C4 | 0.032 (2) | 0.013 (2) | 0.025 (1) | 0.000 (1) | 0.005 (1) | 0.000 (1) |
Li1 | 0.045 (5) | 0.025 (4) | 0.031 (4) | 0.0000 | 0.011 (4) | 0.0000 |
Geometric parameters (Å, º) top
O1—C4 | 1.290 (4) | N1—C1 | 1.336 (4) |
O1—Li1 | 2.152 (3) | N1—C1ii | 1.336 (4) |
O1—H3 | 0.967 | N1—Li1 | 2.007 (10) |
O2—C4 | 1.225 (4) | C1—C2 | 1.382 (5) |
O3—Li1 | 2.03 (1) | C1—C4 | 1.511 (4) |
O3—Li1i | 2.085 (10) | C2—C3 | 1.385 (4) |
O3—H4 | 0.825 | C2—H1 | 0.908 |
O3—H4ii | 0.825 | C3—H2 | 0.900 |
| | | |
O1···O3iii | 3.220 (3) | O3···O3iii | 3.513 (5) |
O1···C4iv | 3.275 (4) | N1···N1iii | 3.513 (5) |
O1···O2iv | 3.432 (4) | N1···Li1iii | 3.526 (10) |
O1···O1v | 3.498 (5) | N1···C1ix | 3.549 (5) |
O1···O1iii | 3.513 (2) | C1···C1iii | 3.513 (5) |
O2···O3vi | 2.773 (3) | C1···C4iii | 3.528 (5) |
O2···C2vii | 3.275 (4) | C2···C2iii | 3.513 (5) |
O2···C4iii | 3.509 (5) | C3···C3iii | 3.513 (10) |
O2···O2iii | 3.513 (2) | C4···C4iii | 3.513 (5) |
O2···C3viii | 3.542 (4) | Li1···Li1iii | 3.513 (15) |
| | | |
C4—O1—Li1 | 116.9 (3) | C3—C2—H1 | 120.7 |
C4—O1—H3 | 107.3 | C2—C3—C2ii | 120.0 (4) |
Li1—O1—H3 | 95.7 | C2—C3—H2 | 119.8 |
Li1—O3—Li1i | 117.3 (4) | C2ii—C3—H2 | 119.8 |
Li1—O3—H4 | 108.3 | O1—C4—O2 | 126.5 (3) |
Li1—O3—H4ii | 108.3 | O1—C4—C1 | 113.0 (3) |
Li1i—O3—H4 | 114.1 | O2—C4—C1 | 120.5 (3) |
Li1i—O3—H4ii | 114.1 | O1—Li1—O1ii | 148.8 (4) |
H4—O3—H4ii | 91.6 | O1—Li1—O3 | 97.1 (3) |
C1—N1—C1ii | 119.5 (4) | O1—Li1—O3iii | 98.9 (3) |
C1—N1—Li1 | 120.2 (2) | O1—Li1—N1 | 75.4 (2) |
C1ii—N1—Li1 | 120.2 (2) | O1ii—Li1—O3 | 97.1 (3) |
N1—C1—C2 | 122.1 (3) | O1ii—Li1—O3iii | 98.9 (3) |
N1—C1—C4 | 113.4 (3) | O1ii—Li1—N1 | 75.4 (2) |
C2—C1—C4 | 124.5 (3) | O3—Li1—O3iii | 117.3 (4) |
C1—C2—C3 | 118.1 (3) | O3—Li1—N1 | 138.0 (5) |
C1—C2—H1 | 121.1 | O3iii—Li1—N1 | 104.7 (5) |
| | | |
O1—C4—C1—N1 | 4.8 (4) | N1—C1—C2—H1 | −178.9 |
O1—C4—C1—C2 | −173.8 (3) | N1—C1ii—C2ii—C3 | −0.6 (5) |
O1—Li1—O1ii—C4ii | −31 (1) | N1—C1ii—C2ii—H1ii | 178.9 |
O1—Li1—O1ii—H3ii | 81.4 | N1—Li1—O1—C4 | 10.0 (4) |
O1—Li1—O3—Li1i | −76.1 (2) | N1—Li1—O1—H3 | −102.7 |
O1—Li1—O3—H4 | 54.8 | N1—Li1—O1ii—C4ii | −10.0 (4) |
O1—Li1—O3—H4ii | 152.9 | N1—Li1—O1ii—H3ii | 102.7 |
O1—Li1—N1—C1 | −7.1 (5) | N1—Li1—O3—Li1i | 0.0000 (2) |
O1—Li1—N1—C1ii | 176.0 (3) | N1—Li1—O3—H4 | 130.9 |
O2—C4—O1—Li1 | 170.4 (4) | N1—Li1—O3—H4ii | −130.9 |
O2—C4—O1—H3 | −83.7 | C1—N1—C1ii—C2ii | 0.5 (6) |
O2—C4—C1—N1 | −176.2 (3) | C1—N1—C1ii—C4ii | 179.1 (3) |
O2—C4—C1—C2 | 5.2 (5) | C1—C2—C3—C2ii | −0.7 (7) |
O3—Li1—O1—C4 | 147.9 (3) | C1—C2—C3—H2 | −174.2 |
O3—Li1—O1—H3 | 35.2 | C1—C4—O1—Li1 | −10.7 (4) |
O3—Li1—O1ii—C4ii | −147.9 (3) | C1—C4—O1—H3 | 95.3 |
O3—Li1—O1ii—H3ii | −35.2 | C2—C1—N1—Li1 | −177.4 (4) |
O3—Li1—N1—C1 | −91.6 (3) | C2—C3—C2ii—H1ii | −178.8 |
O3—Li1—N1—C1ii | 91.6 (3) | C3—C2—C1—C4 | 179.1 (3) |
O3—Li1i—O1i—C4i | −93.0 (4) | C3—C2ii—C1ii—C4ii | −179.1 (3) |
O3—Li1i—O1i—H3i | 154.3 | C4—C1—N1—Li1 | 4.0 (5) |
O3—Li1i—O1ix—C4ix | 93.0 (4) | C4—C1—C2—H1 | −0.5 |
O3—Li1i—O1ix—H3ix | −154.3 | Li1—O3—Li1i—O3i | 180.0000 (1) |
O3—Li1i—O3i—H4i | −49.1 | H1—C2—C3—H2 | 5.4 |
O3—Li1i—O3i—H4ix | 49.1 | H1—C2—C3—H2 | 5.4 |
N1—C1—C2—C3 | 0.6 (5) | | |
Symmetry codes: (i) x−1, y, z; (ii) x, −y+1/2, z; (iii) x+1, y, z; (iv) −x, −y, −z+1; (v) −x+1, −y, −z+1; (vi) −x, y−1/2, −z+1; (vii) −x, −y, −z; (viii) −x, y−1/2, −z; (ix) x−1, −y+1/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H3···O1i | 0.97 | 2.55 | 3.513 (2) | 171 |
O3—H4···O2iv | 0.83 | 1.98 | 2.775 (3) | 160 |
Symmetry codes: (i) x−1, y, z; (iv) −x, −y, −z+1. |