HPM-16, a Stable Interrupted Zeolite with a Multidimensional Mixed Medium–Large Pore System Containing Supercages

Article abstract of DOI:10.1002/anie.202106734

HPM-16 is a highly porous germanosilicate zeolite with an interrupted framework that contains a three-dimensional system of 12+10×10(12)×12+10-membered ring (MR) pores. The 10(12) MR pore in the b direction is a 10 MR pore with long 12 MR stretches forming 30 ? long tubular supercages. Along one direction the 10 MR pores are fused, meaning that the separation between adjacent pores consists of a single tetrahedron that is, additionally, connected to only three additional tetrahedra (a Q³). These fused pores are thus decorated by T-OH groups along the whole diffusion path, creating a hydrophilic region embedded in an otherwise essentially hydrophobic environment. The structure is built from highly porous 12×12×12 MR uninterrupted layers that are connected to each other through Q³ producing a second system of 10×10×10 MR pores. This zeolite can be extensively degermanated yielding a material with high thermal stability, despite its interrupted nature.

Full text of DOI:10.1002/anie.202106734

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How to cite:
International Edition: doi.org/10.1002/anie.202106734
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Zeolites Hot Paper
HPM-16, a Stable Interrupted Zeolite with a Multidimensional Mixed
Medium–Large Pore System Containing Supercages
Zihao Rei Gao, Salvador R. G. Balestra, Jian Li,* and Miguel A. Camblor*
Abstract: HPM-16 is a highly porous germanosilicate zeolite
with an interrupted framework that contains a three-dimen-
sional system of 12 + 10 ꢀ 10(12) ꢀ 12 + 10-membered ring
sitions and physicochemical properties. For instance, pure
silica zeolites with no SiÀOH groups are strictly hydrophobic,
while the presence of -OH groups increases their hydro-
[
4]
(
MR) pores. The 10(12) MR pore in the b direction is
philicity. The hydrophilic/hydrophobic character of zeolites
may largely influence their performance in catalysis and
a 10 MR pore with long 12 MR stretches forming 30 ꢁ long
tubular supercages. Along one direction the 10 MR pores are
fused, meaning that the separation between adjacent pores
consists of a single tetrahedron that is, additionally, connected
[5]
adsorption processes. On the other hand, zeolites with
a mixed 12 ꢀ 10 MR channel system were once highly sought
after because they could provide special shape selectivity
3
[6]
[7]
to only three additional tetrahedra (a Q ). These fused pores
properties, which was later confirmed. Large cavities in
zeolites, often called supercages, are also attractive as
confined spaces for the ship-in-a-bottle inclusion of species
are thus decorated by T-OH groups along the whole diffusion
path, creating a hydrophilic region embedded in an otherwise
essentially hydrophobic environment. The structure is built
from highly porous 12 ꢀ 12 ꢀ 12 MR uninterrupted layers that
[
8]
active in catalytic or sensing applications. Here we present
an interrupted germanosilicate zeolite framework with a new
highly porous topology containing a mixed 10/12 MR 3D pore
system and mixed hydrophilic/hydrophobic environments.
This is the only zeolite topology that contains a 2D system of
interconnected 12 MR pores plus a 3D system of intercon-
nected 10 MR pores. Straight 10 and 12 MR pores run along
[100] and [001], while in the [010] direction the two systems
are interconnected through large (30 ꢁ long) elongated
supercages constituting an undulated 10 MR pore. After
degermanation, this zeolite displays an outstanding thermal
stability.
3
are connected to each other through Q producing a second
system of 10 ꢀ 10 ꢀ 10 MR pores. This zeolite can be extensively
degermanated yielding a material with high thermal stability,
despite its interrupted nature.
Z
eolites are classically defined as crystalline microporous
[1]
tectosilicates. This implies that their ordered structures are
built by silicon (aluminum) oxide tetrahedra that share all
their oxygen atoms once and only once with neighboring
tetrahedra. The Structure Commission of the International
Zeolite Association (IZA) assigns a three-letter code to each
HPM-16 was synthesized as a germanosilicate using 1-
methyl-2-ethyl-3-n-propylimidazolium (1M2E3nPrIM) and
fluoride as structure-directing agents (Section S1 in Support-
[
2]
accepted zeolite topology. However, zeolite-like topologies
in which not all the tetrahedra are 4-connected, the so-called
zeolite interrupted frameworks, are also assigned IZA codes
preceded by a hyphen and are also collected in the database
of Zeolite Structures. The wide applicability of zeolites
relies on their large diversity of structures, chemical compo-
[
3]
ing Information, SI). The Ge fraction, Ge = Ge/(Si + Ge), in
f
the crystals was determined by Energy-Dispersive X-ray
Spectroscopy (EDS) to be 0.30, which is coincident with the
[
2]
Ge value in the synthesis gel (Table S1). Typically, HPM-16 is
f
composed of individual and twinned tablet-shaped crystals
3
with an approximate crystal size around 2 ꢀ 1 ꢀ 0.1 mm (Fig-
[
*] Z. R. Gao, Dr. S. R. G. Balestra, Prof. Dr. M. A. Camblor
Instituto de Ciencia de Materiales de Madrid
Consejo Superior de Investigaciones Cientꢀficas (ICMM-CSIC)
c/ Sor Juana Inꢁs de la Cruz, 3, 28049 Madrid (Spain)
E-mail: macamblor@icmm.csic.es
ure S1b), while some samples synthesized in different con-
ditions consisted of larger crystallites in the form of highly
twinned gear-like crystals (Figure S1a). The structure of
HPM-16 was solved using 3D electron diffraction (3D ED)
and Rietveld refined against synchrotron powder X-ray
diffraction (PXRD) data (Figure 1), and details can be
found in SI (Section S2.1–S2.2, Table S2–S8, and Figure S2–
S4).
Dr. J. Li
Berzelii Center EXSELENT on Porous Materials
Department of Materials and Environmental Chemistry
Stockholm University
1
0691 Stockholm (Sweden)
The micropore system of HPM-16 can be described as
a 3D 12 + 10 ꢀ 10(12) ꢀ 12 + 10 MR intersecting pore system.
The 12 MR pores are 2D, straight, intersect each other and
run along [001] and [100] (Figure 2A,B) with a crystallo-
graphic size of 7.8 ꢀ 6.8 ꢁ and 9.0 ꢀ 5.7 ꢁ (Figure S5), respec-
tively. Along [010] (Figure 2C) the 10(12) description refers
to the existence of long stretches of 12 MR pores that are
connected only through 10 MR (size 5.7 ꢀ 4.9 ꢁ and 6.0 ꢀ
E-mail: jxpxlijian@pku.edu.cn
Supporting information and the ORCID identification number(s) for
the author(s) of this article can be found under:
https://doi.org/10.1002/anie.202106734.
ꢂ 2021 The Authors. Angewandte Chemie International Edition
published by Wiley-VCH GmbH. This is an open access article under
the terms of the Creative Commons Attribution Non-Commercial
NoDerivs License, which permits use and distribution in any
medium, provided the original work is properly cited, the use is non-
commercial and no modifications or adaptations are made.
1
0
8
8
4
5
.2 ꢁ, Figure S5), yielding an elongated [4 6 10 12 ] super-
cage 30 ꢁ long, with access through 10 and 12 MR windows
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Figure 3. The supercages in HPM-16 and MWW: a) the disordered
OSDAs in the supercage of HPM-16, showing the OSDA locations at
two distinct 10 MR and 12 MR channel intersections, b) 30.0 ꢃ length
1
0
8
8
4
12 14
6
[
4 6 10 12 ] supercage in HPM-16 and c) 18.8 ꢃ length [5 6 10 ]
supercage in MWW.
Figure 1. Rietveld refinement plot (l=0.618668 ꢃ) for as-made HPM-
6 (containing a small, <3%, STW impurity, see SI). Red: experimen-
tal, black: calculated, blue: difference. Vertical bars are allowed
reflections for HPM-16 (green) and STW (purple). CCDC NO. 2097880
and 2097878 for as-made and calcined HPM-16, respectively.
3
1
the c-axis due to the presence of Q atoms close to y = 0.25
3
and 0.75 along this direction (Figure 2A); the Q atoms show
disorder; along the a-axis, the 10 MR are separated by two
bonded Q atoms (Figure 2B). The pore system of HPM-16
3
was characterized using the PoreBlazer 4.0, RASPA, and
[
10]
(
Figure 3b). The 10 MR pores also constitute a 3D system of
iRASPA codes (Figure S6 and Section S3.4), resulting in
reasonable agreement with the experimental porosity of
a freshly calcined zeolite tested by Ar adsorption/desorption
(Figure S7), which allowed to determine a pore size distribu-
tion with maxima at 6.7, 7.9, and 9.0 ꢁ (Figure S8). From N2
adsorption/desorption experiments (Figure S9) a BET sur-
straight pores that intersect each other and run along [001]
and [100] plus an undulating pore running along [010]. The
supercage, in which OSDA cations are found disordered
1
2
14
6
(
Figure 3a), is much larger than the elongated [5 6 10 ]
supercage found in MWW (18.8 ꢁ, Figure 3c), open through
[
9]
2
À1
1
0 MR windows. The straight 10 MR pores in HPM-16 are
face area of 535 m g and a t-plot micropore volume of
3
À1
rather peculiar: two rows of fused 10 MR channels exist along
0.20 cm g were determined.
Figure 2. Structure of HPM-16: along A) [001], B) [100], and C) [010]; D) the 23 ꢃ thick HPM-16-layer, E,F) the 32 T half-open unit (3 mel+2 lau)
in HPM-16, G) the 36 T closed unit (4 mel+2 lau) in NUD-3. Only T–T connections and T-OH (red) are shown. A–C) T atoms in green and blue
correspond to the layer with or without a lateral shift (0.5a, 0.25b, 0c), respectively, F,G) T atoms in yellow show the difference of the units in
HPM-16 and NUD-3. Small unconnected balls in (A–D) show the fluoride sites in the as-made material.
2
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The framework of this new zeolite can be built using 23 ꢁ
thick, highly porous (3D 12 MR), mirror-symmetric layers
HPM-16 is stable upon calcination at 5508C but its
crystallinity decreases after exposure to ambient air at room
temperature (Figure S15). After removal of the OSDA by
ozone treatment, HPM-16 was subjected to several runs of
degermanation in an alcoholic acidic solution (Section S1.5),
and the results were followed by EDS and PXRD. The Gef
values within the crystals, together with the unit cell
parameters and volumes, decrease gradually (Table S9) and
show a good linear relationship. The calculation of the
3
(
Figure 2D) connected to each other along b through Q TO
4
tetrahedra, thus bearing some resemblance to the so-called
Interlayered Expanded Zeolites (IEZ) in which a post-
synthetic reaction of a layered material with an appropriate
2
[11]
silane introduces a Q site that joins the layers. Within the
HPM-16 layer, there is a half-open unit built by 32 T-atoms
2
4
(
[
Figure 2E), constructed of 3 mel, i.e. [45 6 ], and 2 lau, i.e.
2
4
4 6 ] units (Figure 2F), that is similar to the 36-T-atom closed
averaged cell volume of the zeolite with Ge = 0 yields a cell
f
unit in the recently reported NUD-3 (Figure 2G), which is
volume that is in good agreement with the value predicted by
the linear fitting of the experimental results (Figure S16).
[12]
composed of 4 mel and 2 lau units. The 32 T-atom half-open
unit in HPM-16 could be regarded as the 36 T-atoms unit in
NUD-3 lacking one of the single 4 rings (s4r). The half-open
units are connected through d4r along the [100] and [001]
directions, forming a 2D infinite layer. Then, the neighboring
Finally, the Ge in degermanated HPM-16 dropped to 0.09
f
and this material showed a very good thermal stability upon
calcination at 8008C (Figure 4), although treatment at 2008C
in water for 24 hours produced a limited decrease in
2
9
layers are connected after a lateral shift of 0.5a along the [010]
crystallinity. The Si MAS NMR spectrum of the degerma-
nated sample (Figure S10b) shows resonances at À119.5 and
À110 ppm. Under cross polarization (CP) conditions (Fig-
3
direction via Q TO tetrahedra, thus forming an interrupted
4
3
D zeolite framework. Rietveld refinement shows that all
3
3
these Q T atoms are disordered, which is simulated by these
atoms having two orientations at y = 0.25 and 0.75. As a result
of the large thickness of the layers involved, the value of the
b-axis in HPM-16 is very long.
ure S10c) the intensity of a Q resonance at À101.4 ppm is
largely increased relative to the ones at À110 or À119.5 ppm.
4
The latter are both attributed to Q in different crystallo-
graphic sites with acute or obtuse Si-O-Si angles, respec-
2
9
[13]
The Si magic-angle-spinning (MAS) NMR spectrum
tively.
According to the Rietveld refinement of the
(
Figure S10a) shows three resonances at À96.6, À103.7, and
degermanated sample (Figure S17 and Table S10–S12;
CCDC NO. 2097879) sites Si7 and Si9, with average angles
of 165.38 and 162.78, respectively, may be responsible for the
high-field signal (predicted chemical shifts À121.2 and
À119.7 ppm, respectively). All other T sites have more
acute angles (144–1528). Degermanated HPM-16 has strong
OH vibrations after dehydration (Figure S18).
À121.6 ppm. The resonance at À96.6 ppm could be assigned
2
3
to Q Si atoms, that is, Si(OSi) (OH) , or Q Si atoms with
2
2
a neighboring Ge atom, that is, Si(OSi) (OGe)(OH). Consid-
ering the structure model from cRED structure solution and
2
Rietveld refinement, the resonance at À96.6 ppm is assigned
3
to Si(OSi) (OGe)(OH) Q Si atoms. The resonances at À103.7
2
4
3
and À121.6 ppm are assigned to Q sites with acute and
The existence in HPM-16 of pairs of Q sites at fractional
[
13]
29
obtuse, respectively, average T-O-T angles. These Si MAS
NMR spectra proved that the framework of HPM-16 contains
y values close to 0.25 and 0.75 that are not very far apart
(around 5.9 ꢁ) raised the question of whether it could be
possible to condense them by direct synthesis in other
conditions or by post-synthetic treatments of HPM-16. Such
3
4
both Q and Q Si and deconvolution of the spectrum showed
that the Q /Q Si ratio is around 5.0%, which matched well
with the structure solution (5.9%). The F solid state NMR
3
4
1
9
3
condensation of Q pairs that would yield s4r can be discarded
spectrum of HPM-16 presents two resonances at À20.6 and
À
À9.4 ppm (Figure S11), assigned to F anions in d4r units of
type II and III, respectively, that is, d4r with isolated Ge or
with Ge pairs not involved in larger clusters (with no Ge
[
14]
having three Ge neighbors), respectively.
The Rietveld
refinement results show in fact that the d4r are enriched in Ge
(
0
Ge = 0.40–0.54), while the other sites are Ge-poor (Ge = 0–
f f
.18; see cif files in SI). The C solid state NMR spectrum of
1
3
an as-made HPM-16 sample (Figure S12a) matched well with
1
3
the C liquid NMR spectrum of the bromide form of the
+
OSDA in D O (1M2E3nPrIM bromide, Figure S12b). This
2
indicates that the OSDA is essentially intact in the as-made
zeolite, which is also proved by the C,H,N elemental analysis
(
Table S1) giving a C/N ratio of 4.55, very close to the value in
the OSDA (4.5). The experimental value of the H/N ratio
10.31) is significantly higher than the calculated one (8.5),
(
which could be explained by the existence of some water (in
agreement with a low-temperature weight loss step in the TG,
Figure S13) and the aforementioned T-OH groups. The
existence in as-made HPM-16 of both water and T-OH
groups is also strongly supported by infrared spectra of a self-
supported wafer before and after dehydration (Figure S14).
Figure 4. Powder X-ray diffraction patterns of HPM-16: a) as-made,
b) after ozone treatment, c) after final run of degermanation, and
d) calcined at 8008C after final run of degermanation. * marks a trace
impurity of STW in the as-made and ozone treated samples (a,b). This
disappears during the degermanation treatment (c,d).
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in the actual HPM-16 mainly based on Rietveld refinement
results, although the existence of disorder (represented by
two T positions with partial occupancies) might introduce
some uncertainty. To study the issue, we generated a set of ten
derived polymorphs (Figure S19), which for completeness
(MMK) in Stockholm University with the support of Knut
and Alice Wallenberg (KAW) foundation-financed project
3DEM-NATUR.
also included the conversion of the generated s4r into d4r, and Conflict of Interest
calculated their formation energies (see SI). As SiO poly-
2
morphs, they all were much less stable than typical high silica
The authors declare no conflict of interest.
À1
or pure silica zeolites (over 18 kJmol relative to quartz
À1
compared to at most 15 kJmol reported by Navrotsky et al.
Keywords: degermanation · interrupted framework ·
structure solution · three-dimensional electron diffraction ·
zeolites
[
15]
and Piccione et al.; Table S13). However, the same calcu-
lation for STW gave an energy similar to those of the derived
polymorphs, which is interesting: this zeolite has been argued
to be possible as a pure SiO zeolite only because of the
2
[
1] M. A. Camblor, S. B. Hong in Porous Materials, (Eds.: D. W.
Bruce, D. OꢆHare, R. I. Walton), Wiley, Chichester, 2011,
pp. 265 – 325.
facilitating polarizing effect of fluoride, which makes the
[
16]
zeolite more flexible and allows its crystallization.
That
means the polymorphs under consideration may be difficult
to realize but still possible. In this respect, we may consider
the case of one of the derived polymorphs, which is
isostructural to the recently reported NUD-3. This is the
polymorph with the lowest energy among those considered,
but still too high to be taken as feasible under this kind of
considerations. However, NUD-3 has already been prepared,
although so far only as a germanosilicate. When the energies
[2] C. Baerlocher, L. B. McCusker, Database of Zeolite Structures:
http://www.iza-structure.org/databases/, accessed on Feb. 26th,
2
021.
[3] L. B. McCusker, F. Liebau, G. Engelhardt, Pure Appl. Chem.
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[
12]
2
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4] T. Blasco, M. A. Camblor, A. Corma, P. Esteve, J. M. Guil, A.
Martꢇnez, J. A. Perdigꢂn-Melꢂn, S. Valencia, J. Phys. Chem. B
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[7] R. Simancas, D. Dari, N. Velamazꢄn, M. T. Navarro, A. Cantꢇn,
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[
much smaller (lower energies compared to quartz-type GeO )
2
À1
and in that case well below the 15 kJmol feasibility limit
J. L. Jordꢄ, G. Sastre, A. Corma, F. Rey, Science 2010, 330, 1219 –
(
Table S14). Given that what is actually synthesized is always
1222.
an organic–inorganic hybrid compound where host–guest
interactions may significantly alter the stability (as in the
STW case commented above) and since NUD-3 has a real
existence, the future preparation of some of the polymorphs
considered here cannot be discarded.
In summary, the new HPM-16 zeolite has been synthe-
sized as a germanosilicate using 1-methyl-2-ethyl-3-n-propy-
limidazolium and fluoride and its structure has been solved
using electron diffraction and refined against synchrotron
diffraction data. It presents a new interrupted topology
containing a 2D system of large 12 MR pores and a 3D system
of medium 10 MR pores. HPM-16 may be extensively
degermanated, yielding a highly stable zeolite.
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Acknowledgements
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The authors are grateful for financial support to the Spanish
Ministry of Science Innovation and Universities (MICIU)
(
PID2019-105479RB-I00 project, AEI, Spain and FEDER,
EU). SRGB also thanks MICIU for a Juan de la Cierva-
Formaciꢂn Research Contract (FJC2018-035697-I code refer-
ence). Synchrotron experiments were performed at beamline
BL04 (MSPD) at the Spanish ALBA Synchrotron with the
collaboration of ALBA staff, and special thanks are due to A.
Manjꢂn and A. Missiul. Centro Tꢃcnico Informꢄtico-CSIC,
Trueno cluster facility of SGAI-CSIC is acknowledged for
running the calculations. We also deeply thank C. Mꢄrquez-
ꢅlvarez for his kind help in characterization. The cRED data
were collected at the Electron Microscopy Center (EMC),
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3
Manuscript received: May 19, 2021
Revised manuscript received: July 20, 2021
Accepted manuscript online: July 26, 2021
Version of record online: && &&, &&&&
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Communications
Zeolites
HPM-16 is a new interrupted zeolite with
D intersecting 12+10ꢄ10(12)ꢄ12+
3
Z. R. Gao, S. R. G. Balestra, J. Li,*
10 MR channels containing 30 ꢃ long
supercages. The structure, with a very
long b-axis (>50 ꢃ), was solved by state-
of-the-art 3D electron diffraction. Deger-
manated HPM-16 is stable up to 8008C.
Several derived structures were studied,
including one recently reported.
M. A. Camblor*
&&&& — &&&&
HPM-16, a Stable Interrupted Zeolite with
a Multidimensional Mixed Medium–
Large Pore System Containing
Supercages
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