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Dynamic Control of MOF-5 Crystal Positioning Using
a Magnetic Field
Paolo Falcaro,* Francois Normandin, Masahide Takahashi, Paolo Scopece,
Heinz Amenitsch, Stefano Costacurta, Cara M. Doherty, Jamie S. Laird,
Matthew D. H. Lay, Fabio Lisi, Anita J. Hill, and Dario Buso*
Metal organic frameworks (MOF) are very promising ultrap-
orous materials for a variety of applications, including sensing,[1]
detecting,[2] gas storage and separation,[3,4] catalysis,[5] and drug
delivery.[6] The high surface area in the thousands of square
meters per gram, and the controlled pore size and pore size
distribution of MOFs are relevant features for the fabrication of
devices that rely on materials with highly controlled transport
properties. In addition, recent investigations describe MOFs as
adaptive materials[1,7] because they respond to a variety of stimuli
(e.g., molecular and environmental).[8] Despite the interesting
intrinsic properties of these ultraporous materials, different
strategies are currently under investigation to achieve spatial
control of MOF position on a variety of substrates. The different
proposed routes involve controlled crystal sizes for subsequent
growth,[9] surface functionalization,[10] soft lithography,[11] and
seeding approaches through heterogeneous nucleation.[1] This
latter approach has been shown to allow exogenous function-
ality to be coupled with the properties intrinsic to MOFs. In the
Dr. P. Falcaro, C. M. Doherty, M. D. H. Lay, F. Lisi, A. J. Hill, D. Buso
CSIRO, Division of Materials Science and Engineering
Private Bag 33, Clayton South MDC, Victoria 3169, Australia
E-mail: paolo.falcaro@csiro.au; dario.buso@csiro.au
Dr. F. Normandin
Industrial Materials Institute National Research Council of Canada
75 boul. de Mortagne Boucherville, Québec, Canada J4B 6Y4
Dr. M. Takahashi
Graduate School of Engineering Osaka Prefecture University Sakai
Osaka 599-8531, Japan
Dr. P. Scopece, Dr. S. Costacurta
Associazione CIVEN
Via delle Industrie 5, 30175 Venezia, Italy
Dr. H. Amenitsch
Institute of Biophysics and Nanosystems Research
Austrian Academy of Sciences
Schmiedlstraße 6, 8042, Graz, Austria
J. S. Laird
CSIRO, Science and Resource Engineering
School of Physics
University of Melbourne
Parkville 3010, Victoria, Australia
Dr. D. Buso
Centre for Micro-Photonics and CUDOS
Faculty of Engineering and Industrial Sciences
Swinburne University of Technology
PO Box 218, Hawthorn, VIC 3122, Australia
DOI: 10.1002/adma.201101233
Adv. Mater. 2011, 23, 3901–3906 © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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present study we utilize functionality gained through synthesis
of MOF with magnetic nanoparticles to control the location of
MOF crystal growth and to dynamically position 3D MOF forms
for use in reconfigurable engineering devices.
Once one or more exogenous species are embedded in
the MOF crystals, a framework composite (FC) is obtained.[1]
Because of the exciting potential properties, the recent research
trend has focused on the synthesis of the nanospecies into
preformed MOF crystals. A variety of FCs, mainly based on
metallic inclusions, has been reported. Fischer’s group used
chemical vapor deposition to grow a variety of metallic nano-
particles (e.g., Pd, Au, and Cu) inside the MOF lattice.[12,13] AgS-
like compounds and TiO2 particles have been grown inside the
porous framework as well.[14,15] Alternatively, MOFs have been
used as templates for the preparation of silica nanoparticles.[16]
The route involving MOF preparation and the subsequent
growth of nanoparticles in the frameworks is a two-step
approach in which not all kinds of particles can be synthesized
because of the need for chemical vapor deposition precursors.
Furthermore, not all of the precursors can be used because their
chemical compatibility with the MOF network is a prerequisite.
In addition it is difficult to achieve spatial control of the nano-
species growth within the MOF crystals.[17] Thus several limi-
tations have been identified related to the post-impregnation
route and the achievable properties of the final FC.
Recently, Amelot and co-workers[18] presented an innovative
two-step route to induce Ag nanoparticle formation directly
within a single MOF-5 crystal. Using a solution containing the
proper precursors, a lithographic protocol was used to spatially
control metallic particle formation inside the MOF. In their
study, the MOF crystal was impregnated with a silver nitrate
solution and then lithographed. This approach opens new
routes for FC engineering and spatial control of active species
within photocatalytic MOFs.
An alternative and emerging strategy for FC fabrication is to
use the nanomaterial already prepared, and then add the nano-
species to the MOF growing medium in order to fabricate FC in
a one-pot approach. This route allows for the practical use of any
presynthesized material compatible with the solvent involved in
the MOF synthesis. For example, silica particles prepared using an
inexpensive soft chemistry method can be embedded in MOF-5,
offering a faster route for MOF preparation due to the seeding
effect in solution or on surfaces.[19] Although the silica particles
employed present just a seeding effect, other ceramic particles
can be used to simultaneously increase the MOF production rate
or, if these particles are deposited on a surface, they can be used
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to induce MOF growth in controlled locations.[1] Using recently
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discovered nanoflaked α-hopeite microparticles (called DRMs),
spatially controlled positioning of MOF-5 within lithographed
substrates was demonstrated. These ceramic seeds can be deco-
rated with a variety of functional materials allowing for the prepa-
ration of a new generation of molecule-selective active devices.[1]
This route represents a new straightforward synthetic approach
that could revolutionize the fabrication of MOF-based devices for
a number of applications such as catalysis, optics, and sensing.
The proper choice of the functional extrinsic material is
critical for the preparation of new efficient MOF-based devices
with tailored properties. For example, the control of the crystal
position using an external stimulus might be of high techno-
logical interest for applications such as dynamic filters where
the MOF is needed in an “on” or “off” position to selectively
gate a channel. An effective route is a one-pot approach where
precursors with magnetic properties are utilized in the MOF
synthesis. Traditionally, the strategy employed for the prepara-
tion of MOF with magnetic properties involves precursors of
elements with magnetic properties (e.g., Mn, V, and Co) assem-
bled with organic linkers in a framework that presents a mag-
netic response;[20–23] however, no evidence for the control of the
crystal position using an external field has been reported.
In the recent work of Lohe et al.[7] the possibility to func-
tionalize aluminum- and copper-based MOFs using extrinsic
superparamagnetic nanoparticles (γ-Fe2O3) is explored. The
procedure involves a two-step synthesis: the MOF precursors
are first grafted on the magnetic particle surface; the particles
are then used to grow the MOFs. Application of an alternating
magnetic field is used to vary the temperature of this magnetic
FC highlighting the application of these FCs for controlled
drug release. However additional unexplored advantages can
be offered by such an interesting class of FC. Position-guided
sensors or gates and new routes for patterning MOF-based
devices can take advantage of controlling MOF positions using
an external field. Therefore, depending on the application, dif-
ferent magnetic properties can be preferred.
Here we present a straightforward one-pot protocol to embed
carbon-coated cobalt nanoparticles within zinc-based metal
organic frameworks. The choice of the magnetic particle is due
to the large-scale production of these nanomagnets with high
air and thermal stabilities.[24] As Grass et al. have reported, the
carbon coating improves the magnetic properties.[23] In addition,
the compatibility of MOF-5 with carbon-based materials has been
already demonstrated.[25–27] Therefore we considered such parti-
cles as ideal candidates for the preparation of ferromagnetic FCs.
With this approach we demonstrate some advantages pro-
vided by the use of an external field to control the position of
MOF-5 crystals embedding a small amount of magnetic nano-
particles in the framework. The presented recipe involves the
addition of carbon-coated cobalt nanoparticles and a surfactant
(Pluronic F127) in the MOF-5 growing medium, followed
by classical solvothermal synthesis. The clouds of surfactant
embed the magnetic nanoparticles, avoiding premature sedi-
mentation of the functional nanospheres. After 24 h of thermal
treatment, dark crystals are obtained. Cubic shape of the syn-
thesized crystals is detected, similar to the shape of the MOF-5
control sample. An optical microscopy image of the magnetic
FC shows cobalt clusters evenly distributed inside and outside
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the crystals (see Figure S1, Supporting Information). Solvent
exchange was performed, removing the original precursor solu-
tion with fresh dichloromethane (this process was repeated
5 times). With this procedure unembedded Co particles were effi-
ciently removed and the original solvent was substituted. Dried
Co FC crystals appear dark blue in color while regular MOF-5
crystals are white (see Figure S2, Supporting Information). This
color is a clear indication that cobalt species are embedded in
the porous framework. By inductively coupled plasma optical
emission spectroscopy (ICP-OES) analysis performed on Co
FC crystals, 197 mg g−1 of Zn and 4.4 mg g−1 of Co have been
measured. This corresponds to a volume concentration of
0.052% of Co nanoparticles within each MOF-5 crystal, calcu-
lated using the size and the density of the Co particles, as well
as of MOF-5. From the optical microscopy investigation, clus-
ters of metal nanoparticles are detected. An elemental mapping
using particle induced X-ray emission (PIXE) confirms an inho-
mogeneous distribution of the magnetic material inside MOF
crystals detecting micrometer-sized domains of cobalt clusters
(Figure S3, Supporting Information).
Using scanning electron microscopy (SEM) we investigated
the morphology of the Co FC crystals. The cubic crystal faces
(Figure 1a) are decorated with clusters of micrometer and sub-
micrometer size (Figure 1b). Performing an energy dispersive
a d
b e
Counts Counts
Zn
c 1500
f
1000 Zn
O
Co
1000 C
O
C
500
Co
500
Co
Zn
Ir
Ir Zn Co Zn
Co Co Zn
0 0
0 2 4 6 8
Energy (keV)
2 4 6 8
Energy (keV)
Figure 1. SEM characterization of the carbon-coated cobalt nanoparticle
doped MOF-5 framework composite (Co FC). a) SEM image of a Co FC
crystal. Similar to MOF-5 the Co FC crystals have a cubic shape. X-ray dif-
fraction confirms the typical pattern of MOF-5 for both control and Co FC
samples (see Supporting Information, Figure S4). b) SEM image of the
Co FC surface which highlights the presence of clusters. c) EDX analysis
of the cluster inside the dashed square presented in (b). A strong signal
of Co (Lα, Kα, Kβ) is detected in the EDX spectra. d) SEM image of the
same Co FC crystal presented in (a) after focusing a 30 keV electron beam
on a 2 μm × 2 μm area for 6 min. The crack induced by the electrons is
highlighted in the dotted square. e) Close-up of the crack presenting the
area in which an EDX measurement has been performed (continuous line
contoured square). f) EDX spectra related to the previous figure. Cobalt
signal is detected inside the crack.
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X-ray (EDX) analysis, these clusters present an intense signal
of cobalt (Figure 1c). Cobalt Lα, Kα, and Kβ emissions are
detected at 0.776, 6.929, and 7.648 keV, respectively. The signals
of the elements constituting MOF-5 are detected: carbon (Kα,
0. 277 keV), oxygen (Kα, 0.523 keV) and zinc (Lα, 1.012 keV; Kα,
8.637 keV; Kβ, 9.53 keV). An iridium signal (Mα, 1.978 keV)
is also detected because an iridium target was used to deposit
a conductive thin metal coating on top of the sample in order
to collect the SEM images. We used a 30 keV electron beam
for 6 min in order to generate a crack on the top surface of
the Co FC crystal (Figure 1d) with a crack width of 1.65 μm
(Figure 1e). This crack dimension was large enough for an EDX
measurement inside the crystal framework. The collected spec-
trum is presented in Figure 1f. Although the cobalt signal is
less intense than the one recorded on the surface, it proves that
the cobalt nanoparticles were also embedded within the MOFs.
The magnetic characterization presented in Figure 2a has
been performed on undoped MOF-5 and shows a diamagnetic
response in the scanned field range. On the other hand, a
strong ferromagnetic response (150 emu g−1 at saturation) has
been measured on a pure Co nanoparticle sample (Figure 2b).
Finally, the Co FCs present a magnetic response, which is the
overlap of the paramagnetic behavior of the porous framework
and the magnetization properties of the metallic nanoparticles.
A saturation value of 0.8 emu g−1 is measured for the Co FCs
(Figure 2c).
The magnetic response is strong enough to allow control of
the Co FCs position using a magnetic field. A 4 mL vial con-
taining washed dark blue Co FC crystals in dichloromethane has
been vigorously stirred and a magnet has been put in contact
with the vial. The cobalt-doped MOFs accumulate at the glass
surface where the magnetic field is most dense (close to the
magnet tip) as shown in Figure 3a. Figures 3b,c show the quick
removal of the magnet. Because of the removal of the mag-
netic field, the crystals slide along the glass surface (Figure 3d)
falling down onto the bottom of the glass (Figure 3e) and then
lying in the lower part of the sealed vessel (Figure 3f). The
sequence of frames represents the experimental evidence of the
Co FC response to the magnetic field. Using the magnetic field
as an external stimulus, the position of the FC can be statically
or dynamically controlled opening new prospects in the field
of MOF based devices. Despite the fact that the carbon coated
magnetic particles are bigger than the MOF-5 pore diameter,
the Brunauer–Emmett–Teller (BET) surface area is 2282 m2 g−1
(see Figure S5, Supporting Information). The control sample,
prepared in similar conditions without adding cobalt nanopar-
ticles and surfactant, presents a surface area of 2376 m2 g−1.
These results indicate that the introduction of the Co nanopar-
ticles provokes a surface area loss of 4%. The magnetic MOFs
presented in this work have the highest surface area reported Figure 2. Magnetization curves of a) MOF-5, b) cobalt nanoparticles,
thus far. and c) carbon-coated cobalt-nanoparticle-doped MOF-5 framework
A possibility offered by controlling the position of such ultrap- composite (Co FC).
orous crystals is presented in Figure 4. Here, two magnetic bars
have been inserted in a 1 mm glass capillary (Figure 4a). This growth due to the seeding effect of the original Co FC crystals
custom-made magnetic finger was used to collect washed Co was interrupted. Crystals were then immersed in a solution
FCs. The crystals preferentially accumulate close to the extremi- with tetrahydrofuran (THF) containing a dye (fluorescein iso-
ties of the two magnets. The finger with the magnetic MOFs thiocyanate, FITC). After 3 h the color of the crystals turned to
was subsequently introduced into a new MOF growing medium orange (Figure 4b). The original contour of the dark crystals can
to promote further crystal growth. After 48 h, the subsequent be appreciated and the subsequent growth can be observed as

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Figure 3. Effect of a magnet on the carbon-coated cobalt-nanoparticle-doped MOF-5 framework composite (Co FC). After stirring the solution containing
Co FCs a significant proportion of crystals are collected by the magnet. Removing the magnet, the crystals slide down to the bottom of the vial.

well. The magnetic-dye-doped crystals under UV irradiation are
luminescent, and the typical cubic MOF-5 shape can be detected
(Figure 4c). In Figure 4d a SEM image taken of the same sample
is presented. The image shows interpenetrated crystals with
dimensions up to 20 times the original magnetic seed crystal
sizes. The crystals attached to the magnetic finger were dried
under vacuum and detached from the substrate. The ring of
Co FC crystals could then be moved along the glass capillary by
moving the magnetic field (Figure 4e,f).
These experiments demonstrate that by the preparation of this
active FC it is possible to control the position of isolated crystals
or to induce the formation of interpenetrated MOF forms in
specific locations using an external stimulus. Both of these sys-
tems might be useful for a variety of applications and the one we
propose here is an amine sensor. Using a magnetic finger, the
Co FCs were positioned to fabricate a sensor device comprised
of a localized cluster of functionalized MOF crystals. The mag-
netically positioned FITC impregnated Co FCs were used for
rapid detection of primary amines (e.g., phenyl-diamine). The
dimension of this molecule ensures that it can diffuse inside
the framework and react with the isothiocyanate group of the
dye. In Figure 5a a real-time photoluminescence measurement
is presented. The initial luminescence of the dye-doped Co FCs
dramatically drops after the injection of the diamine. A small

Figure 4. Scheme showing the magnetic finger used to position Co FCs and the results obtained with further growth of MOF-5 crystals. a) Two magnetic
bars have been inserted in a 1 mm capillary. The magnetic finger was then used to collect Co FCs. The magnetic composite crystals are preferentially
positioned to where the magnetic field lines are most dense. b) Picture under visible light of the positioned Co FCs that act as seeds for the further
growth of the Co FC performed in a MOF-5 growing medium for 48 h. The crystal clusters are then doped with fluorescein isothiocyanate. The impreg-
nation process turns the crystals to orange. c) Picture under UV light (365 nm) of the dye-doped crystal clusters. This picture highlights the contour
of the cubic crystals. d) SEM image of the crystal clusters (scale bar 200 μm). This image shows interpenetrated crystals due to the growing process
when leaving the Co FC crystals in the MOF-5 precursor solution at 95 °C for 48 h. e) After drying the crystals from the solvent the position of ring of
MOF located between the magnetic bars was reconfigurable using the magnetic bars, as presented in the sequence (e–h).

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b
400
Intensity at 550 nm / Counts
350
300
250
200
150
100
50
0 4 mm) were removed from their plastic capsules and introduced into a
0 20 40 60 80 100
time / min
Figure 5. Real-time luminescence response of a bifunctional framework
composite to a primary amine. a) Luminescence spectra of dye-doped Co
FCs collected every 2 min in the 450–750 nm region after the addition of a
dilute 1,4-diaminobenzene solution. b) Intensity of luminescence of dye-
doped Co FCs at 550 nm with time. The combination of multiple stimuli
(magnetic, optical) allows for positioning control and molecular detec-
tion, thereby opening new frontiers for adaptive MOF-based devices.
shift to lower wavenumbers is detected as well. In Figure 5b the
trend of the intensity at 550 nm is reported. Within 4 min a 50%
intensity decrease is detected, and in 12 min the intensity loss is
75%. An overall loss of about 88% is detected after 60 min and
no further significant decrease was detected. For the first time
magnetic and optical properties have been combined in a MOF
for the fabrication of a sensor for primary amine detection. The
application of position-controlled bi-functional FC can hold
great potential for lab-on-chip devices, which enable fast detec-
tion with only small reaction volumes. In such smart platforms,
MOF nanoreactors can be precisely driven across the microflu-
idic chip using an external magnetic field.
Using the presented Co FC, spatially controlled growth of
MOF-5 crystals using a magnetic field is now possible. Further-
more the surface area is not significantly affected by the metal
nanoparticles embedded in the framework. The combination
of the magnetic features with luminescent properties allows
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for the fabrication of a new generation of multistimuli multi-
response MOF-based materials. A new straightforward syn-
thesis in now available for the fabrication of a new generation
of adaptive dynamically reconfigurable MOF-based devices.
Experimental Section
Carbon-coated cobalt nanoparticles, Zn(NO3)2, 1,4-benzenecarboxylic
acid (BCA), N-diethyl formamide (DEF), Pluronic F-127, fluorescein
isothiocyanate (FITC), and 1,4-diaminobenzene were purchased from
Aldrich and used as-received.
MOF-5 growing medium was synthesized by dissolving 0.15 g of
Zn(NO3)2 and 0.0127 g of BCA in 4 mL of DEF. The 4 mL sealed vial
was sonicated for 15 min. 0.2 g of Pluronic F127 and 0.016 g of Co
nanoparticles were added and sonicated for another 10 min. 20 vials
(4 mL each) were prepared to obtain Co FC and 20 vials were filled with
MOF-5 growing medium solution to prepare an equivalent number of
control samples. The Co FC crystals and control sample (regular MOF-5)
were collected after 24 h of growth at 95 °C. The samples were stored,
prepared and measured using dry inert gases.
Magnetic Co FCs crystals were washed 5 times with dichloromethane
(DCM) to remove the original DEF used in the zinc-based framework
crystal preparation. THF was then used to wash the crystals twice. The
vessels containing the crystals in THF were introduced into a vacuum
chamber for 5 min to ensure the extraction of DCM from the framework.
The procedure was conducted in a dry air atmosphere, and the samples
were kept under nitrogen.
The magnetic measurements have been performed using a Physical
Properties Measurement System (PPMS) Model 6000, Quantum Design
(qdusa.com). The instrument is equipped with a 9 T superconducting
magnet. For the measurements of the hysteresis an ACMS probe
(magnetometer) was employed. The “DC Extraction method” was used
to perform the measurements.
The magnets of two Teflon-coated magnetic stirrers (Spinbar, 7 mm ×
120 1 mm glass capillary (Capillary Tube Suppliers Ltd). The magnetic finger
was used to collect and position the Co FC crystals and then introduced
into a fresh MOF-5 growing medium.
For the preparation of dye-doped Co FC, fluorescein isothiocyanate
(FITC) powder (15 mg) was dissolved in 4 mL of THF. The Co FC
crystals were added to the dye–THF solution. After 3 h the crystals
turned orange and were subsequently washed 3 times using fresh THF.
Under UV irradiation the dye-doped Co FCs presented strong yellow-
green emissions.
Time-resolved luminescence emission tests were performed
recording the evolution of the emission intensity at 550 nm. The
values were recorded continuously before and after the injection of the
amino molecules over a 2 min time lapse. 1 min after the continuous
acquisition was started, 20 μL of a diluted diaminobenzene solution
(20 μL of diaminobenzene 98% in 1.5 mL THF) was added to the FITC-
doped Co FC immersed in 3 mL of THF; the measurement was then
continued for about 2 h. The reaction between the amino group and the
FITC is illustrated in previous works.[28]
Supporting Information
Supporting Information is available from the Wiley Online Library or
from the author.
Acknowledgements
Dr. Kristina Konstas is acknowledged for the help with BET sample
preparation and Dr. Matthew Hill for helpful discussions on the BET
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analysis. Dr. Laura Villanova is acknowledged for data elaboration
and graphics using R software. Dr. John Ward and Dr. Mark Greaves
are thanked for their expert assistance with the SEM. Dr. Benedetta
Marmiroli and Dr. Fernando Cacho-Nerin are acknowledged for helpful
discussions. D.B., P.F., C.M.D., and A.J.H. acknowledge the CSIRO OCE
Science Leader Scheme for support. D.B. acknowledges the Australian
Research Council for support through the APD grant DP0988106. The
authors thank the director of the CSIRO Computational and Simulation
Sciences Transformational Capability Platform for financial support. The
powder diffraction characterization was performed at the SAXS beamline
of Elettra Synchrotron, Trieste, Italy.
Received: April 3, 2011
Revised: June 13, 2011
Published online: July 20, 2011
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