In situ identification and absolute separation of small molecules by single crystal X-ray diffraction in metal–organic frameworks

CrystEngComm ◽  
2016 ◽  
Vol 18 (29) ◽  
pp. 5429-5433 ◽  
Author(s):  
Heng Ya Gao ◽  
Le Zhang ◽  
Chang Sheng Yan ◽  
Li Na Meng ◽  
Jian Qiang Li ◽  
...  
Keyword(s):  
Single Crystal ◽  
Small Molecules ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic

scholarly journals In situ X‐ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)‐based Metal‐Organic Frameworks with UiO‐66 and MIL‐140 architectures

2021 ◽  
Author(s):  
Stephen J. I. Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic

A series of microporous and robust Ln-MOFs showing luminescent properties and catalytic performances towards Knoevenagel reactions

2021 ◽  
Author(s):  
Qing-Xia Yao ◽  
Miaomiao Tian ◽  
Jun Zheng ◽  
Jintang Xue ◽  
Xuze Pan ◽  
...  
Keyword(s):  
Single Crystal ◽  
Metal Organic Frameworks ◽  
Luminescent Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
Catalytic Performances

A series of microporous Ln(III)-based metal-organic frameworks (1-Ln) have been hydrothermally synthesized by using 4,4',4''-nitrilotribenzoic acid (H3NTB). Single crystal X-ray diffraction analyses show 1-Ln are isostructural and have 3D porous...

scholarly journals In situ X-ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)-based Metal-Organic Frameworks with UiO-66 and MIL-140 architectures

2020 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Metal Organic Frameworks ◽  
Building Blocks ◽  
Nucleation And Growth ◽  
X Ray Diffraction ◽  
X Ray ◽  
Rate Determining Step ◽  
Wide Range ◽  
Metal Organic

We report on the results of a thorough <i>in situ</i> synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds <i>in situ</i> in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO<sub>3</sub>) and amount of the coordination modulator acetic acid (AcOH). When only HNO<sub>3</sub> is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO<sub>3</sub>, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO<sub>3</sub> slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO<sub>3</sub> favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO<sub>3</sub>. Based on these <i>in situ</i> results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

scholarly journals Coordination Polymers of Scandium(III) and Thiophenedicarboxylic Acid

2021 ◽  
Vol 47 (9) ◽  
pp. 593-600
Author(s):  
A. A. Lysova ◽  
V. A. Dubskikh ◽  
K. D. Abasheeva ◽  
A. A. Vasileva ◽  
D. G. Samsonenko ◽  
...  
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Coordination Polymers ◽  
Elemental Analysis ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
Phase Purity ◽  
X Ray ◽  
Metal Organic

Abstract Three new metal−organic frameworks based on scandium(III) cations and 2,5-thiophenedicarboxylic acid (H2Tdc) are synthesized: [Sc(Tdc)(OH)]·1.2DMF (I), [Sc(Tdc)(OH)]·2/3DMF (II), and (Me2NH2)[Sc3(Tdc)4(OH)2]·DMF (III) (DMF is N,N-dimethylformamide). The structures of the compounds are determined by single-crystal X-ray structure analysis (CIF file CCDC nos. 2067819 (I), 2067820 (II), and 2067821 (III)). The chemical and phase purity of compound I is proved by elemental analysis, thermogravimetry, X-ray diffraction analysis, and IR spectroscopy.

scholarly journals Remodelling a Shp: Transmetallation in a Rare-Earth Cluster-Based Metal–Organic Framework

2021 ◽  
Author(s):  
Hudson de Aguiar Bicalho ◽  
P. Rafael Donnarumma ◽  
Victor Quezada-Novoa ◽  
Hatem M. Titi ◽  
Ashlee J Howarth
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Surface Area ◽  
De Novo ◽  
Metal Organic Framework ◽  
Metal Organic Frameworks ◽  
Metal Exchange ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic

<div> <p>Post-synthetic modification (PSM) of metal–organic frameworks (MOFs) is an important strategy for accessing MOF analogues that cannot be easily synthesized <i>de novo</i>. In this work, the rare-earth (RE) cluster-based MOF, Y-CU-10, with <b>shp</b> topology was modified through transmetallation using a series of RE ions, including: La(III), Nd(III), Eu(III), Tb(III), Er(III), Tm(III), and Yb(III). In all cases, metal-exchange higher than 70 % was observed, with reproducible results. All transmetallated materials were fully characterized and compared to the parent MOF, Y-CU-10, in regards to crystallinity, surface area, and morphology. Additionally, single-crystal X-ray diffraction (SCXRD) measurements were performed to provide further evidence of transmetallation occurring in the nonanuclear cluster nodes of the MOF. </p> </div>

scholarly journals Two metal–organic frameworks based on Sr2+ and 1,2,4,5-tetrakis(4-carboxyphenyl)benzene linkers

2021 ◽  
Vol 77 (12) ◽  
Author(s):  
Muhammad Usman ◽  
Lydia Ogebule ◽  
Raúl Castañeda ◽  
Evgenii Oskolkov ◽  
Tatiana Timofeeva
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structural Control ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
Solvent Systems ◽  
Semiconductor Properties

Two structurally different metal–organic frameworks based on Sr2+ ions and 1,2,4,5-tetrakis(4-carboxyphenyl)benzene linkers have been synthesized solvothermally in different solvent systems and studied with single-crystal X-ray diffraction technique. These are poly[[μ12-4,4′,4′′,4′′′-(benzene-1,2,4,5-tetrayl)tetrabenzoato](dimethylformamide)distrontium(II)], [Sr2(C34H18O8)(C3H7NO)2] n , and poly[tetraaqua{μ2-4,4′-[4,5-bis(4-carboxyphenyl)benzene-1,2-diyl]dibenzoato}tristrontium(II)], [Sr3(C34H20O8)2(H2O)4]. The differences are noted between the crystal structures and coordination modes of these two MOFs, which are responsible for their semiconductor properties, where structural control over the bandgap is desirable. Hydrogen bonding is present in only one of the compounds, suggesting it has a slightly higher structural stability.

Triazole-directed Fabrication of Polyoxovanadate-based Metal-organic Frameworks as Efficient Multifunctional Heterogeneous Catalysts for Knoevenagel Condensation and Oxidation of Alcohols

2021 ◽  
Author(s):  
Jikun Li ◽  
Chuanping Wei ◽  
Yinfeng Han ◽  
Yu Mei ◽  
Xueli Cheng ◽  
...  
Keyword(s):  
Single Crystal ◽  
Heterogeneous Catalysts ◽  
Knoevenagel Condensation ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxidation Of Alcohols ◽  
Metal Organic

By introducing 4-amino-1,2,4-triazole (4-NH2-trz), three new polyoxovanadate-based metal-organic frameworks (PMOFs) [Ni3(4-NH2-trz)6][V6O18]•3H2O (1), [Co3(4-NH2-trz)6][V6O18]•3H2O (2) and [Cu3OH(4-NH2-trz)3H2O][VO3]5•H2O (3) have been synthesized and thoroughly characterized by single-crystal X-ray diffraction (SXRD), powder X-ray...

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