TY - CONF A1 - Wilke, Manuel A1 - Fischer, F. A1 - Tröbs, L. A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Verfolgung mechanochemischer Synthesen durch in situ Röntgendiffraktometrie T2 - Zeit- und temperaturaufgelöste Röntgen-Pulver-Diffraktometrie CY - Pfinztal, Germany DA - 2013-11-14 PY - 2013 AN - OPUS4-29853 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Manuel A1 - Fischer, F. A1 - Tröbs, L. A1 - Redemann, K. A1 - Emmerling, Franziska T1 - Verfolgung mechanochemischer Synthesen durch in situ Röntgendiffraktometrie T2 - Adlershofer Foschungsforum CY - Berlin, Germany DA - 2013-11-12 PY - 2013 AN - OPUS4-29854 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Batzdorf, Lisa A1 - Fischer, Franziska A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - Cadmium phenylphosphonates: preparation, characterisation and in situ investigation N2 - The successful mechanochemical syntheses of three cadmium phenylphosphonates indicates that mechanochemistry is ideally suited for synthesizing metal phosphonates. With this powerful synthesis tool it is possible to synthesize rapidly and efficiently both known and novel phosphonates. The Crystal structures of the two new compounds, and, were solved from PXRD data. They contain monodeprotonated phenylphosphonate and neutral phenylphosphonic acid ligands. The synthesis pathways of all three compounds were investigated in situ. A diffusion mechanism is corroborated by our findings. Intermediates could be detected and identified. The kinetically favored product (3) could always be detected during the syntheses. The thermodynamic stability of the compounds and the stoichiometric ratio of the starting materials are the two directing factors for the synthesis of the final products. KW - Mechanochemistry KW - Metal phosphonate KW - In situ KW - MOF KW - XRD PY - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-363322 SN - 2046-2069 VL - 6 IS - 42 SP - 36011 EP - 36019 PB - Royal Soc Chemistry CY - Cambridge, UK AN - OPUS4-36332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - The structure and in situ synthesis investigation of isomorphic mononuclear molecular metal phenylphosphonates N2 - We describe a fast and effective synthesis for molecular metal phosphonates. Isomorphic compounds [M(II)(HO₃PPh)₂(H₂O₃PPh)₂(H₂O)₂] (M = Mn (1), Co (2), Ni (3); Ph = C₆H₅) were obtained by grinding. The complexes are mononuclear compounds containing neutral and monodeprotonated phenylphosphonic acid and water as ligands. The crystal structures were determined using powder X-ray diffraction (PXRD) data and validated by extended X-ray absorption fine structure (EXAFS) data. Combined synchrotron XRD measurements and Raman spectroscopy were conducted for investigating the reactions in situ. Based on these data, the intermediates were characterized and the formation mechanism was derived. KW - Mechanochemistry KW - Metal phosphonate KW - In situ KW - XRD PY - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-363944 SN - 1477-9226 SN - 1477-9234 SN - 1364-5447 VL - 45 IS - 23 SP - 9460 EP - 9467 AN - OPUS4-36394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Manuel A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Crystallization of Transition Metal Phosphonates T2 - Hercules School 2014 CY - Grenoble, France DA - 2014-02-23 PY - 2014 AN - OPUS4-31319 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Wilke, Manuel A1 - Szczerba, Wojciech A1 - Reinholz, Uwe A1 - Emmerling, Franziska T1 - Mechanochemical synthesis and characterisation of two new bismuth metal organic frameworks N2 - Two metal organic structures composed of the ligands benzene-1,4-dicarboxylate and pyridine- 2,5-dicarboxylate and bismuth cations are presented: (H2Im)[Bi(1,4-bdc)2] (1) and [Bi(pydc)(NO3)2(H2O)2]*H2O (2) (bdc = benzenedicarboxylate, H2Im = imidazole cation, pydc = pyridinedicarboxylate). Both compounds were synthesised via grinding and the crystal structure of compound (2) was solved based on its powder diffraction pattern. Compound 1 crystallises isostructurally to the dimethyl ammonium containing compound (dma)[(Bi(1,4- bdc)2]. Raman spectroscopy and Extended X-ray absorption fine structure (EXAFS) measurements provided additional information about the two mechanochemically synthesised metal organic compounds. KW - crystal structure KW - mechanochemically synthesis KW - powder diffraction measurements PY - 2014 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-306296 UR - http://pubs.rsc.org/en/content/articlepdf/2014/ce/c3ce42633e SN - 1466-8033 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. VL - 16 IS - 25 SP - 5560 EP - 5565 CY - London, UK AN - OPUS4-30629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Gorelik, T. E. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Kolb, U. A1 - Rademann, K. A1 - Emmerling, Franziska T1 - The crystallisation of copper(II) phenylphosphonates N2 - The crystal structures and syntheses of four different copper(II) phenylphosphonates, the monophenylphosphonates α-, β-, and γ-Cu(O3PC6H5)·H2O (α-CuPhPmH (1) β-CuPhPmH (2) and γ-CuPhPmH (3)), and the diphosphonate Cu(HO3PC6H5)2·H2O (CuPhP2mH (4)), are presented. The compounds were synthesized from solution at room temperature, at elevated temperature, under hydrothermal conditions, and mechanochemical conditions. The structures of α-CuPhPmH (1) and CuPhP2mH (4) were solved from powder X-ray diffraction data. The structure of β-CuPhPmH (2) was solved by single crystal X-ray analysis. The structures were validated by extended X-ray absorption fine structure (EXAFS) and DTA analyses. Disorder of the crystal structure was elucidated by electron diffraction. The relationship between the compounds and their reaction pathways were investigated by in situ synchrotron measurements. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-384217 SN - 1477-9226 SN - 1477-9234 VL - 45 IS - 43 SP - 17453 EP - 17463 PB - The Royal Society of Chemistry AN - OPUS4-38421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Manuel A1 - Batzdorf, Lisa A1 - Fischer, Franziska A1 - Rademann, K. A1 - Emmerling, Franziska T1 - In situ investigations of the mechanochemical syntheses of cadmium phenylphonates T2 - 29th European Crystallographic Meeting und Electron Crystallography School 2015 CY - Rovinj, Kroatien und Porec, Kroatien DA - 2015-08-23 PY - 2015 AN - OPUS4-34036 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Fischer, Franziska A1 - Wilke, Manuel A1 - Wenzel, Klaus-Jürgen A1 - Emmerling, Franziska T1 - Direct in situ investigation of milling reactions using combined x-ray diffraction and raman spectroscopy N2 - The combination of two analytical methods including time-resolved in situ X-ray diffraction (XRD) and Raman spectroscopy provides a new opportunity for a detailed analysis of the key mechanisms of milling reactions. To prove the general applicability of our setup, we investigated the mechanochemical synthesis of four archetypical model compounds, ranging from 3D frameworks through layered structures to organic molecular compounds. The reaction mechanism for each model compound could be elucidated. The results clearly show the unique advantage of the combination of XRD and Raman spectroscopy because of the different information content and dynamic range of both individual methods. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structures and thus obtaining reliable data for mechanistic studies. PY - 2015 U6 - https://doi.org/10.1002/anie.201409834 SN - 1433-7851 SN - 1521-3773 SN - 0570-0833 VL - 54 IS - 6 SP - 1799 EP - 1802 PB - Wiley-VCH CY - Weinheim AN - OPUS4-34630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Scholz, G. A1 - Batzdorf, Lisa A1 - Wilke, Manuel A1 - Emmerling, Franziska T1 - Synthesis, structure determination, and formation of a theobromine: oxalic acid 2:1 cocrystal N2 - The structure and the formation pathway of a new theobromine : oxalic acid (2 : 1) cocrystal are presented. The cocrystal was synthesised mechanochemically and its structure was solved based on the powder X-ray data. The mechanochemical synthesis of this model compound was studied in situ using synchrotron XRD. Based on the XRD data details of the formation mechanism were obtained. The formation can be described as a self-accelerated ('liquid like') process from a highly activated species. KW - ssNMR spectroscopy KW - Synchrotron measurements KW - API molecule PY - 2015 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-331567 SN - 1466-8033 VL - 17 IS - 4 SP - 824 EP - 829 CY - London, UK AN - OPUS4-33156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Manuel A1 - Fischer, Franziska A1 - Batzdorf, Lisa A1 - Emmerling, Franziska A1 - Rademann, K. T1 - Monitoring Mechanochemical Synthese by in situ X-ray Diffraction T2 - BESSY User Meeting 2013 CY - Berlin DA - 2013-12-05 PY - 2013 AN - OPUS4-32501 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Klimakow, Maria A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Fast and efficient synthesis of a host guest system: a mechanochemical approach N2 - An unusually fast and effective synthesis procedure for a host guest system consisting of a metal organic framework (MOF) and a polyoxometalate (POM) is described. The material was synthesised mechanochemically and the evolution of the structure was monitored ex and in situ using synchrotron X-ray diffraction (XRD). KW - Mechanochemistry KW - MOF KW - in situ PY - 2016 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-354910 UR - http://pubs.rsc.org/en/Content/ArticleLanding/2016/CE/C5CE01868D#!divAbstract VL - 18 IS - 7 SP - 1096 EP - 1100 AN - OPUS4-35491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Manuel A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - Crystallisation of transition metal phosphonates - A mechanochemical approach N2 - Mechanochemistry is a convenient way to form metal phosphonates with neutral and/or monodeprotonated phosphonates, controlled by the stoichiometric. In situ investigation of reactions helps understanding mechanisms and formation of intermediates. The knowledge of intermediates helps to find metastable structures.The diffusion mechanism is most probable for the mechanochemical synthesis of metal phosphonates. T2 - Institutskolloquium CY - Heinrich Heine University Düsseldorf (HHU), Düsseldorf, Germany DA - 28.01.2016 KW - metal phosphonates KW - Mechanochemistry KW - mof PY - 2016 AN - OPUS4-35860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Akhmetova, Irina A1 - Beyer, Sebastian A1 - Schutjajew, K. A1 - Tichter, T. A1 - Wilke, Manuel A1 - Prinz, Carsten A1 - B. Martins, Inês C. A1 - Al-Sabbagh, Dominik A1 - Roth, C. A1 - Emmerling, Franziska T1 - Cadmium benzylphosphonates - the close relationship between structure and properties N2 - Cadmium benzylphosphonate Cd(O3PBn)·H2O and its fluorinated derivates Cd(O3PBn-3F)·H2O, Cd(O3PBn-4F)·H2O, and Cd(O3PBn-F5)·H2O were synthesized mechanochemically. The Crystal structures of the compounds were determined based on powder X-ray diffraction (PXRD) data. The influence of the ligand substitution on the crystal structure of the metal phosphonate was determined. The hydrophobicity as a function of degree of fluorination was investigated using dynamic vapor sorption. KW - Mechanochemistry KW - Metal phosphonates KW - PXRD KW - DVS PY - 2019 U6 - https://doi.org/10.1039/c9ce00776h VL - 21 SP - 5958 EP - 5964 PB - RSC Royal Society of Chemistry AN - OPUS4-49930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Wilke, Manuel A1 - Fischer, Franziska A1 - Röllig, Mathias A1 - Maierhofer, Christiane A1 - Emmerling, Franziska T1 - Warming up for mechanosynthesis – temperature development in ball mills during synthesis N2 - We present a first direct measurement of the temperature during milling combined with in situ Raman spectroscopy monitoring. The data reveal a low temperature increase due to the mechanical impact and clear temperature increases as a consequence of the reaction heat. Based on the data, temperature rises as postulated in the magma plasma and hot spot theory can be excluded for soft matter milling syntheses. KW - Thermography KW - Milling KW - Mechanochemistry KW - Soft matter PY - 2017 U6 - https://doi.org/10.1039/c6cc08950j SN - 1364-548X SN - 1359-7345 SN - 0009-241X VL - 53 IS - 10 SP - 1664 EP - 1667 AN - OPUS4-39251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Bach, S. A1 - Gorelik, T. A1 - Kolb, U. A1 - Tremel, W. A1 - Emmerling, Franziska T1 - Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution N2 - Divalent metal phosphonates are promising hybrid materials with a broad field of application. The rich coordination chemistry of the phosphonate linkers enables the formation of structures with different dimensionalities ranging from isolated complexes and layered structures to porous frameworks incorporating various functionalities through the choice of the building blocks. In brief, metal phosphonates offer an interesting opportunity for the design of multifunctional materials. Here, we provide a short review on the class of divalent metal phosphonates discussing their syntheses, structures, and applications. We present the advantages of the recently introduced mechanochemical pathway for the Synthesis of divalent phosphonates as a possibility to generate new, in certain cases metastable compounds. The benefits of in situ investigation of synthesis mechanisms as well as the implementation of sophisticated methods for the structure analysis of the resulting compounds are discussed. KW - Metal phosphonate KW - Mechanochemistry PY - 2017 U6 - https://doi.org/10.1515/zkri-2016-1971 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 209 EP - 222 PB - De Gruyter AN - OPUS4-40003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Akhemtova, Irina A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Mechanochemical synthesis of cerium(IV)-phosphonates N2 - The syntheses and crystal structures of two cerium(IV) phosphonates are presented. Cerium(IV) bis(phenylphosphonate) Ce(O3PC6H5)2 1 can be formed from precipitation and mechanochemical reaction, whereas cerium(IV) bis(carboxymethylphosphonate) monohydrate Ce(O3PCH2COOH)2 H2O 2 is only accessible via ball milling. All reactions proceed very fast and are completed within a short time span. In situ measurements for the syntheses of 1 show that the product occurs within seconds or a few minutes, respectively. The structures were solved from powder X-ray diffraction data. KW - In situ studies KW - Mechanochemistry KW - XRD PY - 2018 U6 - https://doi.org/10.1007/s10853-018-2507-x SN - 0022-2461 SN - 1573-4803 VL - 53 IS - 19 SP - 13733 EP - 13741 PB - Springer Science + Business Media B.V. AN - OPUS4-45672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Zimathies, Annett A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Crystal structure and in situ investigation of a mechanochemical synthesized 3D zinc N-(phosphonomethyl)glycinate N2 - The mechanochemical synthesis of the zinc N-(phosphonomethyl)glycinate Zn(O₃PCH₂NH₂CH₂CO₂) H₂O is presented. The structure was solved from powder X-ray diffraction (PXRD) data. In the three-dimensional pillared structure, the Zn atoms are coordinated tetrahedrally. In situ investigations of the reaction process with synchrotron PXRD and Raman spectroscopy reveal a two-step process including the formation of an intermediate. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2017 U6 - https://doi.org/10.1007/s10853-017-1121-7 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 20 SP - 12013 EP - 12020 PB - Springer CY - New York AN - OPUS4-41490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matoga, D. A1 - Roztocki, K. A1 - Wilke, Manuel A1 - Emmerling, Franziska A1 - Oszajca, M. A1 - Fitta, M. A1 - Bałanda, M. T1 - Crystalline bilayers unzipped and rezipped: solid-state reaction cycle of a metal–organic framework with triple rearrangement of intralayer bonds N2 - We present a series of remarkable structural transformations for a family of layered metal–organic frameworks (MOFs) in a three-step solid-state reaction cycle. The cycle represents new dynamic behavior of 2D coordination polymers and involves the sequence of reactions: {[Mn2(ina)4(H2O)2]·2EtOH}n (JUK-1) → {(NH4)2[Mn(ina)2(NCS)2]}n·xH2O (JUK-2) → {[Mn2(ina)2(Hina)2(NCS)2]}n (JUK-3) → JUK-1 (Hina = isonicotinic acid), each accompanied by rearrangement of intralayer coordination bonds and each induced by a different external stimulus. In situ investigation of the first step of the cycle by combined synchrotron X-ray diffraction and Raman spectroscopy reveals direct mechanochemical unzipping of JUK-1 bilayers to respective JUK-2 layers with reaction rates dependent on the milling conditions. In contrast, the reverse zipping of JUK-2 layers involves two steps and proceeds through a new MOF (JUK-3) whose structure was elucidated by powder X-ray diffraction. Magnetic measurements confirm conversions of manganese nodes in the reaction cycle. The findings indicate the possibility of developing coordination-based assemblies with large structural responses for use in smart stimuli-responsive systems and sensor technologies. KW - Mechanochemistry KW - In situ KW - XRD KW - MOF PY - 2017 UR - http://pubs.rsc.org/is/content/articlehtml/2017/ce/c7ce00655a U6 - https://doi.org/10.1039/C7CE00655A VL - 19 SP - 2987 EP - 2995 AN - OPUS4-41517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -