This article was published as part of the 2009 Metal–organic frameworks issue Reviewing the latest developments across the interdisciplinary area of metal–organic frameworks from an academic and industrial perspective Guest Editors Jeffrey Long and Omar Yaghi Please take a look at the issue 5 table of contents to access the other reviews. Published on 31 March 2009. Downloaded by California Institute of Technology on 20/05/2013 18:11:26. View Article Online / Journal Homepage / Table of Contents for this issue
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This article was published as part of the
2009 Metal–organic frameworks issueReviewing the latest developments across the interdisciplinary area of
metal–organic frameworks from an academic and industrial perspective Guest Editors Jeffrey Long and Omar Yaghi
Please take a look at the issue 5 table of contents to access the other reviews.
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. View Article Online / Journal Homepage / Table of Contents for this issue
Secondary building units, nets and bonding in the chemistry
of metal–organic frameworksw
David J. Tranchemontagne, Jose L. Mendoza-Cortes, Michael O’Keeffe
and Omar M. Yaghi*
Received 18th February 2009
First published as an Advance Article on the web 31st March 2009
DOI: 10.1039/b817735j
This critical review presents a comprehensive study of transition-metal carboxylate clusters which
may serve as secondary building units (SBUs) towards construction and synthesis of
metal–organic frameworks (MOFs). We describe the geometries of 131 SBUs, their connectivity
and composition. This contribution presents a comprehensive list of the wide variety of
transition-metal carboxylate clusters which may serve as secondary building units (SBUs) in the
construction and synthesis of metal–organic frameworks. The SBUs discussed here were obtained
from a search of molecules and extended structures archived in the Cambridge Structure
Database (CSD, version 5.28, January 2007) which included only crystals containing metal
carboxylate linkages (241 references).
Introduction
The chemistry of stitching molecular building units by strong
bonds into extended structures (reticular chemistry) continues to
develop at an unusually fast pace. This is leading to the
proliferation of new structures in which typically metal ion
‘joints’ are used in connecting organic ‘struts’ to make porous
metal–organic frameworks (MOFs) which we clearly differentiate
from coordination polymers. At present, this chemistry has
matured to the point where researchers from fields beyond
chemistry are involved in the design and study of MOF
structures and their properties. Naturally, as in any other mature
field, a system of organization and nomenclature should be
developed to facilitate the navigation within the field for current
and future researchers. In this context, the concept of secondary
building units (SBUs) has served as an organizing concept for
the classification of the MOF structures into their underlying
topology. SBUs are essential to the design of directionality for
the construction of MOFs and to the achievement of robust
frameworks. In this contribution we (1) provide a comprehensive
list of SBUs that are known as discrete metal carboxylates and
that are potentially useful in the construction of MOFs,
(2) identify and describe their underlying geometry, (3) discuss
the general classification of the nets of MOF structures, and
(4) present a unified view of the bonding within MOFs based on
SBUs and compare it to coordination polymers.
Nets and their symbols
Since the earliest days of crystallography crystal structures
have been described in terms of nets in which atoms are the
Center for Reticular Chemistry, Department of Chemistry andBiochemistry, University of California, Los Angeles, Los Angeles,CA 90095, USA. E-mail: [email protected];Fax: (+001) 310-206-5891; Tel: (+001) 310-206-0398w Part of the metal–organic frameworks themed issue.
David J. Tranchemontagne
David J. Tranchemontagnewas born in Nashua, NH,USA (1981). He received hisBSc (2003) from the Univer-sity of New Hampshire, andhis PhD from the University ofCalifornia in Los Angeles(2007) with Professor OmarM. Yaghi. He is now workingas a Research Scientist withProfessor Omar M. Yaghi.His current research interestsinclude the use of newporous materials for chemicalapplications. Jose L. Mendoza-Cortes
Jose L. Mendoza-Cortes wasborn in Pochutla, Oaxaca,Mexico in 1985. He receivedhis BSc (2008) in Chemistryfrom the Instituto Tecnologicoy de Estudios Superioresde Monterrey (ITESM),Campus Monterrey, Mexico.He spent a year and a half inProf. Omar M. Yaghi’s lab atUCLA creating 3D covalentorganic frameworks andstudying new possible buildingblocks for new porousmaterials. He then did hisBSc Thesis with Prof. Yaghi
and Prof. Goddard in a joint appointment between UCLA andthe California Institute of Technology (Caltech). He iscurrently a PhD student at Caltech.
This journal is �c The Royal Society of Chemistry 2009 Chem. Soc. Rev., 2009, 38, 1257–1283 | 1257
CRITICAL REVIEW www.rsc.org/csr | Chemical Society Reviews
vertices and the bonds are the links (edges) between them. The
structure of diamond should be a familiar example. These nets
are special kinds of periodic graph.1 In structures such as those
of zeolites,2 tetrahedrally-coordinated atoms T (typically Si,
Al, P etc.) are joined by –O– links to form a four-coordinated
net of T vertices with the –O– links now acting as edges.
Much of the early interest in nets developed particularly
with the study of coordination polymers beginning some
75 years ago. In coordination polymers typically a transition-
metal (M) ion is linked by a polytopic coordinating ligand
such as bipyridine (BPY) to form salts with charged
continuous periodic frameworks M(BPY)2. The underlying
topology of the structure is again described by a periodic net
in which atoms are the vertices, but now the edges correspond
to the linkers joining the two edges (BPY in this example).
References to some early examples of these materials have
been given elsewhere.3z
The last decade has seen an explosive increase in synthesis
and characterization of crystalline materials with frameworks
in which building blocks are joined by covalent bonds. Most
notable are MOFs in which typically polyatomic inorganic
metal-containing clusters are linked by polytopic chelating
linkers. In the archetypical and iconic MOF, MOF-5, OZn4cationic SBUs are linked by the benzenedicarboxylate (BDC)
anion to form a continuous cubic neutral framework of
composition Zn4O(BDC)3.4 The zinc carboxylate unit has
formula Zn4O(CO2)6, and the six carboxylate carbons
(the points of extension) are at the vertices of a regular
octahedron. The underlying topology of a MOF framework
is also that of a net. In this example the cationic cluster is
represented by an octahedral six-coordinated vertex and the
edges represent the –(C6H4)– linker. Often a polytopic unit can
link metal clusters,3 thus in MOF-1775 in which the same
OZn4 clusters are linked with 1,3,5-benzenetricaboxylic acid
the resulting net is mixed (6,3)-coordination.5
We have developed a system of nomenclature for common
nets and some of their properties are conveniently accessed
through a web-based database known at the Reticular
Chemistry Structure Resource (RCSR). This system has
recently been described in detail elsewhere;6 here we are
content to note that net topologies are assigned a three-letter
symbol in bold lower-case; thus the MOF-5 and MOF-177
topologies have symbols pcu and qom, respectively. Some
derived nets have symbols with extensions, a good example
is the so-called augmented net in which the vertices of the
original net are replaced by a cluster of vertices corresponding
to the vertex figure of the original net. Thus in pcu-a the
original six-coordinated vertices are replaced by an octa-
hedron of vertices. More detail can be found at the cited
reference.
Terminology and bonding: MOFs, ZIFs and coordination
polymers
We propose that a clear distinction be made between MOFs
on the one hand and coordination polymers on the other. We
can make the distinction in a very elementary way in terms of
Michael O’Keeffe
Michael O’Keeffe was born inBury St Edmunds, England(1934). He received his BSc(1954), PhD (1958), andDSc (1976) from the Univer-sity of Bristol. He is Regents’Professor of Chemistry atArizona State University,where he has been since 1963.His current research is parti-cularly focused on studying thebeautiful patterns found inchemistry and elsewhere.
Omar M. Yaghi
Omar M. Yaghi was born inAmman, Jordan (1965). Hereceived his PhD from theUniversity of Illinois-Urbana(1990) with Professor WalterG. Klemperer. He was anNSF Postdoctoral Fellow atHarvard University withProfessor Richard H. Holm(1990–1992). He is currentlyChristopher S. Foote Profes-sor in the Department ofChemistry and Biochemistryat UCLA. He directs theCenter for Reticular Chemistry.He has established several
research programs dealing with the reticular synthesis of discretepolyhedra and extended frameworks from organic and inorganicbuilding blocks.
z At the suggestion of a referee we elaborate on the remarks of theprevious paragraph. First the bond energy for four Zn–O bonds inZnO is determined from the heat of reaction for ZnO(c) - Zn(g) +O(g) calculated to be 725.3 kJ mol�1 for four Zn–O bonds of bondvalence 1/2 (here, as usual, c and g refer to crystalline and gas states).This in turn is determined from the standard heats of formation inkJ mol�1 of ZnO(c) (�348.3), Zn(g) (130.2), and O(g) (246.8).
239 Wenote that a study of bond energies in solid oxides showed that, per molof O, bond energies to a given metal were closely constant for a varietyof ternary, quaternary, etc. compounds and did not depend oncoordination number (thus for one Mg forming four or six or eightbonds to oxygen to total bond energy is the same; i.e. bond energyscales with bond valence).240 Thus first: we expect the Zn–O bondenergy in ZnO to be very similar to that in zinc acetate or in MOF-5 sothat for the two Zn–O links to each acetate group to be about360 kJ mol�1. Second we expect for a coordination link with formalbond valence equal to zero to be rather weaker. To estimate theseenergies we use the enthalpies of reactions such as ZnCl2�4NH3 -ZnCl2 + 4NH3, found to be 609.6 kJ mol�1 from the heats offormation of ZnCl2 (�415.0), NH3 (38.9) and ZnCl2�4NH3 (�869.0).Other thermochemical data lead to similar results. Mass spectroscopicdata reported by Rogers and Armentrout for M(NH3)4
+ - M+ +4NH3 yield 399–472 kJ mol�1 for M = 3d transition elements(see their Table 5).241 We include in our table a comparison betweenMOF-5 and the coordination polymer Zn(L)2(ClO4)2 (L = N,N0-bis(4-pyridyl)urea) to illustrate out point.3 In both cases, tetrahedrallycoordinated Zn are connected by ditopic links to form 3D networks.
1258 | Chem. Soc. Rev., 2009, 38, 1257–1283 This journal is �c The Royal Society of Chemistry 2009
y In this review we generally use names for polyhedra that refer totopology rather than symmetry. Thus an ‘‘octahedron’’ may have lessthan full octahedral (Oh) symmetry but will be a topological octa-hedron with four triangular faces meeting at each vertex.
This journal is �c The Royal Society of Chemistry 2009 Chem. Soc. Rev., 2009, 38, 1257–1283 | 1259
sharing edges and corners via O atoms, is capped by eighteen
carboxylates (Fig. 129).237
Twenty-two points of extension
This SBU consists to two semicircles, each of four octahedral
Cr atoms and one square-pyramidal Cu atom, corner-shared
via Cl atoms; these semicircles are joined at each end by an
octahedral Cr atom with similar corner sharing (Fig. 130).229
Each Cu atom is located at one end of its respective semicircle.
The two Cr atoms joining the semicircles are bridged to a Cu
atom by one carboxylate and to another Cr by two carboxylates.
All other metal atoms are bridged to their neighbors by two
carboxylates.
Sixty-six points of extension
Eighty-four Mn atoms form a ring of edge sharing and corner
sharing octahedra with 72 O atoms, and capped by 66
carboxylates, all bridging adjacent Mn atoms (Fig. 131).238
Twelve carboxylates point into the ring, while the remaining
carboxylates point out of or above the ring; no carboxylates
point below the ring.
Concluding remarks
We exhibited the variety within the almost forgotten arsenal of
discrete metal carboxylates could be employed in the design
and construction of metal–organic frameworks. We expect
that each one of these SBUs will endow the corresponding
MOF with yet unpredictable stability and physical properties.
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