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ECS Journal of Solid State Science and Technology, 6 (6) M3113 M3115 (2017) M3113 JSS FOCUS ISSUE ON NANOCARBONS—IN MEMORY OF SIR HARRY KROTO Computational Comparison of the Water Dimer Encapsulations[.]

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ECS Journal of Solid State Science and Technology, 6 (6) M3113-M3115 (2017) M3113

JSS FOCUSISSUE ONNANOCARBONS—INMEMORY OFSIRHARRYKROTO Computational Comparison of the Water-Dimer Encapsulations

into D2(22)-C84and D2d(23)-C84 Zdenˇek Slanina, a,z Filip Uhl´ık, b Shigeru Nagase, c Takeshi Akasaka, a Ludwik Adamowicz, d and Xing Lu a, ∗

a State Key Laboratory of Materials Processing and Die & Mould Technology, School of Material Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074, China

b Department of Physical and Macromolecular Chemistry, Charles University, Faculty of Science, Praha 2, Czech Republic

c Fukui Institute for Fundamental Chemistry, Kyoto University, Kyoto 606-8103, Japan

d Department of Chemistry and Biochemistry, University of Arizona, Tucson, Arizona 85721-0041, USA

The water dimer encapsulations into D2 (22)-C 84and D 2d(23)-C 84 fullerenes are evaluated The encapsulation energy is computed

at the M06-2X/6-31++G** level and it is found that the energy gain upon encapsulation into the D2 (22)-C 84and D 2d(23)-C 84

cages is −17.37 and −15.48 kcal/mol, respectively Encapsulation equilibrium constants are computed using partitions functions

based on the M06-2X/6-31++G** molecular data The yield for (H 2 O) 2@D2 (22)-C 84 is higher than for (H 2 O) 2@D 2d(23)-C 84 ,

however, the yield ratio decreases with increasing temperature and for high temperatures is close to 2:1 The M06-2X/6-31++G**

computed rotational constants are presented for a possible use in detection of the water-dimer endohedrals by rotational spectroscopy

in laboratory or interstellar space.

© The Author(s) 2017 Published by ECS This is an open access article distributed under the terms of the Creative Commons

Attribution Non-Commercial No Derivatives 4.0 License (CC BY-NC-ND, http://creativecommons.org/licenses/by-nc-nd/4.0/ ),

which permits non-commercial reuse, distribution, and reproduction in any medium, provided the original work is not changed in any

way and is properly cited For permission for commercial reuse, please email: oa@electrochem.org [DOI: 10.1149/2.0201706jss ]

All rights reserved.

Manuscript submitted December 12, 2016; revised manuscript received January 31, 2017 Published February 8, 2017.This paper

is part of the JSS Focus Issue on Nanocarbons – In Memory of Sir Harry Kroto.

The very recent production of C70with encapsulated water dimer1

represents a further example of fullerene endohedrals prepared2 via

organic synthesis Moreover, it offers a stabilized, conserved water

dimer (though influenced by the carbon cage) that can be used for

various spectral characterizations of the prototype hydrogen-bonded

aggregate It also represents an interesting observed species for further

computational studies, this experiment-theory symbiosis being always

quite common6 , 7in fullerene science, even in its prehistoric times8 , 9

before the C60breakthrough observation10in 1985

In addition to the water1 , 2 , 5 and hydrogen molecule3 , 4 containing

endohedrals, also encapsulations of other non-metal species inside

the fullerene cages have been studied, for example atomic11 – 15and

molecular16 , 17nitrogen Endohedrals with rare gas atoms, in particular

with He, were produced using18 , 19high temperatures (650oC), high

pressures (3000 atm) and a catalyst Such fullerene encapsulations

of non-metals have been computed,20 – 25too This paper continues in

the research line with calculations on two C84endohedrals containing

encapsulated water dimer

Calculations

C84has twenty four26isolated-pentagon rule (IPR) isomers, two

major isomers of D2 and D 2d symmetries are conventionally

la-beled as 22 and 23, respectively, or D2(22)-C84 and D 2d(23)-C84

They belong to most abundant empty fullerenes besides C60and C70

(some minor C84isomers are also known27) The D2and D 2dspecies

were prepared28in a ratio of 2:1 and can be separated by recycling

chromatography.29The D 2dstructure has the lowest energy30among

the C84IPR isomers, however, owing to entropy effects it is still less

populated For example, at a temperature of 1000 K, the D2(22)-C84

isomer is computed31 , 32as 60.3% while the D 2d(23)-C84 species as

only 34.2% in the IPR isomeric mixture

The water dimer has also been vigorously studied as an H-bond

model and also as a component of Earth’s33and cometary34 , 35

atmo-spheres Interestingly, it has been established through computations

∗Electrochemical Society Member.

z E-mail: zdeneks@email.arizona.edu

that the dimer mole fraction36 – 38 in saturated water vapor increases with increasing temperature It may be a surprising result but in fact

it can easily be rationalized While the equilibrium constant for the dimer formation decreases with temperature, the saturated pressure increases and actually grows faster.39The water dimer formation is

described by the usual dimerization equilibrium constant K p ,2in terms

of the partial pressures of the components:

In fact, the recent evaluation40of the water dimerization constant (G3&MP2/AUG-cc-pVQZ level) reaches nearly perfect agreement with the available experimental data

The dimeric-water encapsulations into both C84cages (Figure1) are similarly described by the encapsulation equilibrium constants

K p ,enc,i:

(H2O)2(g) + D2(22) − C84(g)



 (H2O)2@D2(22) − C84(g) , K p,enc,D2 [2]

(H2O)2(g) + D 2d(23)− C84(g)   (H2O)2@D 2d(23)− C84(g) ,

The relative yields of both encapsulates (here represented by the

ratio of their partial pressures p - see Eq.4) can actually be estimated using the ratio of equilibrium constants (2) and (3), especially if the starting amount of both empty fullerenes (or more precisely, their amounts in the equilibrium gas phase) would be the same:

p (H2O)2@D2(22)−C84

p (H2O)2@D 2d(23)−C84

= K p ,enc,D2

K p ,enc,D 2d

[4]

as other partial pressures would cancel out in the arrangement The relative yields exhibit a useful feature that they do not depend on water-vapor pressure or on the water-dimer population In fact, the stability measure defined by Eq.4is basically given by ratios of the partition functions for two isomeric pairs and thus, it allows for a convenient cancellation-out of related contributions, especially of at least part of the anharmonic corrections

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M3114 ECS Journal of Solid State Science and Technology, 6 (6) M3113-M3115 (2017)

Figure 1 The M06-2X/6-31++G** optimized structures of (H2 O) 2@D2

(22)-C 84 (top) and (H 2 O) 2@D 2d(23)-C 84 (bottom).

All the molecular parameters needed for the construction of the

equilibrium constants on the base of partition functions are computed

here with the Gaussian program package.41

Results and Discussion

The structural and energy data for the encapsulation equilibrium

constants are calculated using the M06-2X density functional with

the standard 6-31++G** basis set (M06-2X/6-31++G**) The

par-tition functions are of the usual rigid rotor and harmonic oscillator

quality and the vibrational frequencies here are also from the

M06-2X/6-31++G** approach Addition of the diffuse functions for

com-plexes with large distances is desirable, however, it brings rather large

demands on computational resources, especially for the vibrational

calculations Therefore, in the previous computations the

frequen-cies (with an exception of the free water dimer) were only of the

M06-2X/6-31G** quality.25Let us note in addition, that the simpler

M06-2X/6-31G** approach (in contrast to the M06-2X/6-31++G**

level used here) is not able to produce the trans conformation known

for the free water dimer

The M06-2X/6-31++G** encapsulation energiesE enc,iwith

in-clusion of the basis set superposition error (BSSE/CP2) and so-called

steric correction40 , 42 , 43are given in TableI The BSSE/CP2 term

re-duces the energy gain upon encapsulation by 3.96 and 4.02 kcal/mol

for the D2(22)-C84and D 2d(23)-C84cage, respectively

Table I The M06-2X/6-31++G** water-dimer encapsulation energiesE enc ,i into D2 (22)-C 84and D 2d(23)-C 84

a See Figure 1

Table II The K K p ,enc,D2

p ,enc,D2d ratios of the M06-2X/6-31++G**

equilibrium constants for the water-dimer encapsulations into

D2 (22)-C 84and D 2d(23)-C 84at selected temperatures T

p ,enc,D2d

a The critical temperature.

The steric correction is applied in order to reflect the cage distor-tion - it includes the difference between the energy of the carbon-cage geometry simply taken from a treated endohedral and the energy of the related fully-optimized empty fullerene cage, and also the respective energy difference for the water dimer The steric correction reduces further the already BSSE/CP2 corrected energy gain upon

encapsu-lation, namely by 2.69 and 3.25 kcal/mol for the D2(22)-C84 and

D 2d(23)-C84species, respectively In fact, the water-dimer distortion represents a larger part of the steric correction

The potential-energy changes upon encapsulationE enc,i are just the first step in the relative yields evaluations Only after evaluations

of the related encapsulation standard enthalpy and entropy changes

one can get the related encapsulation equilibrium constants K p,enc,i Their ratios at selected temperatures are presented in TableII The calculated ratios show that the water-dimer encapsulation into the

D2(22)-C84 cage exhibits a higher yield over the D 2d(23)-C84 case though the difference in the yields is decreasing with the increasing temperature Still, both cages should be a promising target for an application of a high temperature and high pressure technique18 – 20

for the water-dimer encapsulations as already indicated with

evalu-ations for the sole D2(22)-C84species.25 The applied temperatures are likely to go over the critical point (when saturation is not pos-sible and pressures become arbitrary) The high temperatures (and

a catalyst) allow for a temporary window in the cage, yet they cannot be too high in order to prevent a larger cage destruction (and also water dissociation)

Interestingly enough, the cage presence influences the water dimer conformation (Figure1) which is otherwise trans for the free species However, in the D2(22)-C84case the encapsulated trans arrangement

is higher in energy only by 0.08 kcal/mol Other structural parameters

of the water dimer are also influenced by the encapsulation as seen in TableIII The encapsulates in various endohedrals undergo relatively

Table III The M06-2X/6-31++G** structural parameters a in the water-dimer.

(H 2 O) 2 species HOa[Å] OdOa[Å]  OaOdH [◦]

a HOa - hydrogen bond (Oa - acceptor-monomer oxygen); OdOa -distance between oxygen atoms of donor (Od) and acceptor monomer;

 OaOdH - deviation from linearity.

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ECS Journal of Solid State Science and Technology, 6 (6) M3113-M3115 (2017) M3115

Table IV The M06-2X/6-31++G** rotational constants A, B, C

[GHz] for the C 84 endohedrals with the water-dimer.

(H 2 O) 2@D2 (22)-C 84 0.044133 0.042536 0.041200

(H 2 O) 2@D 2d(23)-C 84 0.042925 0.042458 0.042453

a See Figure 1

free motions which is responsible for reconstruction of the cage

sym-metries, as documented by NMR spectroscopy The fully optimized

(H2O)2@C84aggregates exhibit just C1static symmetry However, in

order to reflect the fast internal motions, it is more realistic to describe

the aggregates by the effective dynamic D2or D 2dsymmetry

This type of yield evaluation should be also performed for

(H2O)2@C70 in order to clarify its relative production in

compari-son with encapsulation into the C84 cages Incidentally, the recent

final confirmation44of C60in the interstellar space via electron

spec-troscopy allows to search there for fullerene cages with some

encap-sulates, too (though C60itself is too small45to accommodate the water

dimer) As rotational spectroscopy could also be used for detection

of such endohedrals in the interstellar space, TableIVpresents the

computed rotational constants A, B, C for both C84cages with the

encapsulated water dimer, showing that they are rather different for

the two aggregates (however, in the interstellar space the species can

be in an ionized form)

In conclusion, the calculations show that D2(22)-C84is a better

candidate for high temperature and high pressure water-dimer

en-capsulation as the yield for (H2O)2@D2(22)-C84is higher compared

to (H2O)2@D 2d(23)-C84- the yield ratio decreases with increasing

temperature, however, for high temperatures is yet close to 2:1 The

calculations also suggest that still larger water aggregates46 – 50could

be encapsulated and studied for suitably larger nanocarbons

Acknowledgments

The reported research has been supported by the National

Thou-sand Talents Program of China, the NSFC (numbers 21171061 and

51472095), and the Program for Changjiang Scholars and

Inno-vative Research Team in University (IRT1014); an early phase of

the research line was supported by the Alexander von

Humboldt-Stiftung and the Max-Planck-Institut f¨ur Chemie (Otto-Hahn-Institut)

An access to the MetaCentrum (LM2010005) and CERIT-SC

(CZ.1.05/3.2.00/08.0144) computing facilities is acknowledged, too

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