Home The crystal structure of dimethylammonium catena-[di(μ-aqua)-bis(μ9-benzene-1,3,5-tricarboxylato)pentalithium], C20H16Li5NO13
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The crystal structure of dimethylammonium catena-[di(μ-aqua)-bis(μ9-benzene-1,3,5-tricarboxylato)pentalithium], C20H16Li5NO13

  • Ying Li , Yu-Cai Qin and Bao-Kuan Chen ORCID logo EMAIL logo
Published/Copyright: September 9, 2020

Abstract

C20H16Li5NO13, orthorhombic, Pnma (no. 62), a = 9.9218(8) Å, b = 14.6941(11) Å, c = 13.5697(10) Å, V = 1978.4(3) Å3, Z = 4, Rgt(F) = 0.0439, wRref(F2) = 0.0960, T = 173(2) K.

CCDC no.: 1442769

Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Colorless block
Size:0.21 × 0.17 × 0.14 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.14 mm−1
Diffractometer, scan mode:Bruker D8 quest, φ and ω
θmax, completeness:26.4°, >99%
N(hkl)measured, N(hkl)unique, Rint:9719, 2086, 0.085
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1430
N(param)refined:190
Programs:Bruker [1], SHELX [2], Olex2 [3]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
C10.3316(2)0.61540(14)0.98985(15)0.0111(5)
C20.3527(2)0.58610(14)0.89394(15)0.0119(5)
H20.2775250.5758260.8520470.014*
C30.4824(2)0.57152(14)0.85810(15)0.0113(5)
C40.5925(2)0.58884(14)0.91913(15)0.0118(5)
H40.6811950.5775460.8957620.014*
C50.5737(2)0.62253(14)1.01400(15)0.0112(5)
C60.4426(2)0.63586(14)1.04877(16)0.0123(5)
H60.4290380.6591361.1133260.015*
C70.1928(2)0.61438(15)1.03547(15)0.0121(5)
C80.5016(2)0.52939(14)0.75820(15)0.0121(5)
C90.6919(2)0.63341(14)1.08296(15)0.0126(5)
C101.0615(4)0.7500000.8549(3)0.0276(9)
H10A1.1348570.7500000.9032120.041*
H10B1.0681370.8044600.8134820.041*
C110.8155(4)0.7500000.8361(3)0.0290(9)
H11A0.7304140.7500000.8727530.044*
H11B0.8202040.6955400.7945130.044*
Li10.2258(4)0.5644(3)1.2248(3)0.0177(8)
Li20.0494(4)0.4660(3)0.9122(3)0.0190(9)
Li30.1297(6)0.7500001.2191(4)0.0200(12)
N10.9301(3)0.7500000.9062(2)0.0294(8)
H10.925(3)0.7991(14)0.9455(16)0.035*
O10.18033(14)0.64744(10)1.12066(10)0.0152(4)
O20.09736(14)0.57719(10)0.98906(10)0.0160(4)
O30.40498(14)0.53272(10)0.69771(10)0.0153(4)
O40.61176(15)0.49114(10)0.73767(10)0.0167(4)
O50.80962(14)0.62671(11)1.04832(10)0.0175(4)
O60.66678(14)0.64572(10)1.17317(10)0.0156(4)
O7−0.0669(2)0.7500001.20898(17)0.0235(6)
H7−0.101(2)0.7056(14)1.1784(16)0.028*

Source of material

A mixture of 1,3,5-benzenetricarboxylic acid (H3BTC; 0.21 g, 1 mmol), LiOH ⋅ H2O (0.125 g, 3 mmol) and N,N′-dimethylacetamide (10 mL) was sealed in a 25 mL Teflon-lined stainless steel vessel and heated at 120 °C for 4320 mins. Yield: 50% based on Li.

Experimental details

The hydrogen atoms from O and N atoms were positioned based on difference electron peaks and refined freely with O7—H7 = 0.844 Å (Uiso(H) = 1.2Ueq(O)) and N1—H1 = 0.899 Å (Uiso(H) = 1.2Ueq(N)).

Comment

Metal-organic frameworks (MOFs) are porous materials composed of metal ions/clusters and organic units, which have the characteristics of porosity, high specific surface area and are easy to modify. MOFs and CPs are widely used in gas storage and separation [4], fluorescent responses [5], proton conductivity [6], membrane separation [7], [8], environmental pollution control [9], [10] and energy conversion [11], [12]. However, most of the MOFs are constructed from the transition metals or rare earth, and the alkali-metal-based MOFs are rare examples, particularly the lithium-based MOFs [13], [14]. Compared to other metals, the lithium-based MOFs can enhance gravimetric energy storage capacity more effectively, so we are interested in embarking on the synthesis of the lightest lithium-based MOFs.

Single crystal X-ray analysis reveals that the title compound crystallizes orthorhombically in the space group Pnma and contains three crystallographically independent Li ions (two in general positions one on a mirror plane). The Li1 center adopts four-coordinated geometry with four O atoms from different BTC ligands (Li1–O:1.887–1.920 Å). The Li2 center is five-coordinated with the square pyramidal geometry and the Li–O bond lengths are in the range of Li2–O: 1.996–2.289 Å. Although the Li3 center also adopts five-coordinated geometry, one coordinated O atom is from one water (Li3–O:1.954–2.149 Å). Note, the oxygen atoms offered by BTC anions connect different Li ions to form a complex 3D framework, which is completely different from other reported skeleton structures based on lithium and BTC [15], [16], [17].

Acknowledgements

This work was supported by the Natural Science Foundation of Liaoning Shihua University (2019XJJL-019).

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Received: 2020-06-02
Accepted: 2020-06-22
Published Online: 2020-09-09
Published in Print: 2020-10-27

©2020 Ying Li et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  72. Crystal structure of 4-[(3-methoxyphenyl)carbamoyl]butanoic acid, C12H15NO4
  73. Crystal structure of dichlorido-bis(tri-4-tolylphosphane oxide-κO)-di(4-chlorophenyl-κC)tin(IV), C54H50Cl4O2P2Sn
  74. Crystal structure of dichloridodimethylbis(tri-4-tolylphosphane oxide-κO)-tin(IV), C44H48Cl2O2P2Sn
  75. Crystal structure of chlorido(2-methylquinolin-8-olato-κ2N,O)-bis(4-tolyl-κC)tin(IV), C24H22ClNOSn
  76. Crystal structure of (E)-dichloro(1-chloro-3-methoxyprop-1-en-2-yl)(4-methoxyphenyl)-λ4-tellane, C11H13Cl3O2Te
  77. Crystal structure of bis{N-methyl-N′-[3-(4-methoxyphenyl)-1-methylpropane-1-ylidene]carbamohydrazonothioato}zinc(II), C26H36N6O2S2Zn
  78. Crystal structure of (2-carboxy-4-(3-carboxy-5-carboxylatophenoxy)benzoato-κ2O,O′)bis(1,10-phenantroline-κ2N,N′)cobalt(II), C40H24N4O9Co
  79. The crystal structure of (3S,8R,10R,14R)-17-((2S,5S)-5-(2-hydroxypropan-2-yl)-2-methyltetrahydrofuran-2-yl)-4,4,8,10,14-pentamethyl-12-oxohexadecahydro-1H-cyclopenta[a]phenanthren-3-yl acetate, C32H52O5
  80. Crystal structure of (μ2-1,1′-bis(diphenylphosphino)ferrocene-κ2P,P′)-bis[(Z)N-(3-fluorophenyl)-O-methylthiocarbamato-S]digold(I) chloroform solvate, C50H42Au2F2FeN2O2P2S2, CHCl3
  81. Crystal structure of poly[bis(μ2-1,4-di(1H-imidazol-1-yl)benzene-κ2N:N′)-(μ2-tetraoxidomolybdato(VI)-κ2O:O′)cobalt(II)], C24H20N8O4MoCo
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