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A new zeolite (named as ITQ-52) having large cavities and small and medium channels has been synthesized. This was achieved by using a new family of amino-phosphonium cations as organic structure directing agents (OSDA). These cations contain P−C and P−N bonds, and therefore they lie between previously reported P-containing OSDA, such as tetraalkylphosphonium and phosphazenes. In this study, it has been found that 1,4- butanediylbis[tris(dimethylamino)]phosphonium dication is a very efficient OSDA for crystallization of several zeolites, and in some particular conditions, the new zeolite ITQ-52 was synthesized as a pure phase. The structure of ITQ-52 has been solved using high-resolution synchrotron X-ray powder diffraction data of the calcined solid. This new zeolite crystallizes in the space group I2/m, with cell parameters a = 17.511 Å, b = 17.907 Å, c = 12.367 Å, and β = 90.22°. The topology of ITQ-52 can be described as a replication of a composite building unit with ring notation [435461] that gives rise to the formation of an interconnected 8R and 10R channel system. ; We thank financial support by the Spanish Government (MAT2012-38567-C02-01, MAT2012-38567-C02-02, Consolider Ingenio 2010-Multicat CSD-2009-00050 and Severo Ochoa SEV-2012-0267). R.S. acknowledges to UPV for a FPI predoctoral fellowship. Authors thank ALBA Light Source for beam allocation at beamline MSPD. We thank G. Sastre and J. A. Vidal for computational calculations and MAS NMR experiments, respectively. ; Simancas Coloma, R.; Jorda Moret, JL.; Rey Garcia, F.; Corma Canós, A.; Cantin Sanz, A.; Peral, I.; Popescu, C. (2014). A new microporous zeolitic silicoborate (ITQ-52) with interconnected small and medium pores. Journal of the American Chemical Society. 136(9):3342-3345. doi:10.1021/ja411915c ; S ; 3342 ; 3345 ; 136 ; 9

[EN] In this work a new ultrafast data collection strategy for electron diffraction tomography is presented that allows reducing data acquisition tithe by one order of Magnitude.,,This Methodology minimizes the radiation damage of, beam-sensitive materials, such as microporous materials. This method, combined with the precession of the electron beam, provides high quality data enabling the determination of very complex structures. Most importantly,, the implementation of this new, electron diffraction methodology is, easily affordable in any modem electron Microscope. As a proof of concept, we have solved a new highly complex zeolitic structure named ITQ-58, with a very low symmetry (triclinic) and a large unit cell volume (1874.61(3)), containing 16 silicon and 32 oxygen atoms in its asymmetric unit, which would be very difficult to solve with the state of the art techniques. ; The authors gratefully acknowledge financial support of European Research Council (ERC-2014-AdG ref 671093 "MATching zeolite SYNthesis with CATalytic activity"), Spanish Government (MAT2015-71842-P (MINECO/FEDER), MAT2012-38567-C02-01 and Severo Ochoa SEV-2012-0267), and Generalitat Valenciana (Project Prometeo). E.M. was also supported by the Italian project FIR2013 Exploring the Nanoworld. Authors thank beamline MSPD at Spanish Synchrotron ALBA for beam time allocation. We acknowledge JEOL Japan, JEOL Europe, and specially Junichi Morimoto from JEOL Europe for the assistance during the specific alignments of the microscope. Finally, authors specially thank the Electron Microscopy Service of the Universitat Politecnica de Valencia and, in particular, Manuel J. Planes and Jose L. Moya for their invaluable support for setting up the EDT data acquisition. Original data (collected EDT frames and integrated intensities) can be requested directly from corresponding authors. ; Simancas-Coloma, J.; Simancas Coloma, R.; Bereciartua-Pérez, PJ.; Jorda Moret, JL.; Rey Garcia, F.; Corma Canós, A.; Nicolopoulos ., S. (2016). Ultrafast Electron ...

2122 2125 54 17 ; S Ch. Baerlocher , A.Hepp and W. M.Meier , DLS-76. Distance least squares refinement program , ETH Zurich Institut fur Kristallographie , Zurich, Switzerland , 1977 ; Sun, J., Bonneau, C., Cantín, Á., Corma, A., Díaz-Cabañas, M. J., Moliner, M., … Zou, X. (2009). The ITQ-37 mesoporous chiral zeolite. Nature, 458(7242), 1154-1157. doi:10.1038/nature07957 ; [EN] Here, we present the synthesis and structure determination of the new zeolite ITQ-62. Its structure was determined via ultra-fast electron diffraction tomography and refined using powder XRD data of the calcined material. This new zeolite contains a tridirectional channel system of highly distorted 8-rings, as well as a monodirectional 12-ring channel system. The authors gratefully acknowledge financial support from the Spanish Government (MAT2015-71842-P and MAT2015-71261-R MINECO/FEDER and Severo Ochoa SEV-2016-0683). The authors thank ALBA Light Source for beam allocation at the beamline MSPD, and specially thank the Electron Microscopy Service of the Universitat Politecnica de Valencia. Finally, the authors thank Dr Alejandro Vidal and Dr Teresa Blasco for helping in the NMR data discussion. Bieseki, L.; Simancas Coloma, R.; Jorda Moret, JL.; Bereciartua-Pérez, PJ.; Cantin Sanz, A.; Simancas-Coloma, J.; Pergher, SB. (2018). Synthesis and structure determination via ultra-fast electron diffraction of the new microporous zeolitic germanosilicate ITQ-62. Chemical Communications. 54(17):2122-2125. https://doi.org/10.1039/c7cc09240g Barrer, R. M., & Denny, P. J. (1961). 201. Hydrothermal chemistry of the silicates. Part IX. Nitrogenous aluminosilicates. Journal of the Chemical Society (Resumed), 971. doi:10.1039/jr9610000971 Kerr, G. T. (1966). Chemistry of Crystalline Aluminosilicates. II. The Synthesis and Properties of Zeolite ZK-4. Inorganic Chemistry, 5(9), 1537-1539. doi:10.1021/ic50043a015 Burton, A. W., & Zones, S. I. (2007). Organic Molecules in Zeolite Synthesis: Their Preparation and Structure-Directing Effects. ...

[EN] Here, we present the synthesis and structure determination of the new zeolite ITQ-62. Its structure was determined via ultra-fast electron diffraction tomography and refined using powder XRD data of the calcined material. This new zeolite contains a tridirectional channel system of highly distorted 8-rings, as well as a monodirectional 12-ring channel system. ; The authors gratefully acknowledge financial support from the Spanish Government (MAT2015-71842-P and MAT2015-71261-R MINECO/FEDER and Severo Ochoa SEV-2016-0683). The authors thank ALBA Light Source for beam allocation at the beamline MSPD, and specially thank the Electron Microscopy Service of the Universitat Politecnica de Valencia. Finally, the authors thank Dr Alejandro Vidal and Dr Teresa Blasco for helping in the NMR data discussion. ; Bieseki, L.; Simancas Coloma, R.; Jorda Moret, JL.; Bereciartua-Pérez, PJ.; Cantin Sanz, A.; Simancas-Coloma, J.; Pergher, SB. (2018). Synthesis and structure determination via ultra-fast electron diffraction of the new microporous zeolitic germanosilicate ITQ-62. Chemical Communications. 54(17):2122-2125. https://doi.org/10.1039/c7cc09240g ; S ; 2122 ; 2125 ; 54 ; 17 ; Barrer, R. M., & Denny, P. J. (1961). 201. Hydrothermal chemistry of the silicates. Part IX. Nitrogenous aluminosilicates. Journal of the Chemical Society (Resumed), 971. doi:10.1039/jr9610000971 ; Kerr, G. T. (1966). Chemistry of Crystalline Aluminosilicates. II. The Synthesis and Properties of Zeolite ZK-4. Inorganic Chemistry, 5(9), 1537-1539. doi:10.1021/ic50043a015 ; Burton, A. W., & Zones, S. I. (2007). Organic Molecules in Zeolite Synthesis: Their Preparation and Structure-Directing Effects. Introduction to Zeolite Science and Practice, 137-179. doi:10.1016/s0167-2991(07)80793-2 ; Zones, S. I., Nakagawa, Y., Lee, G. S., Chen, C. Y., & Yuen, L. T. (1998). Searching for new high silica zeolites through a synergy of organic templates and novel inorganic conditions. Microporous and Mesoporous Materials, 21(4-6), 199-211. ...