Synthesis and structure of 4-methylpyridine complexes of cobalt(II) and nickel(II) hexafluorophosphate and hexafluoroarsenate

1978 ◽  
Vol 56 (7) ◽  
pp. 985-991 ◽  
Author(s):  
Raymond M. Morrison ◽  
Robert C. Thompson

The complexes M(4mepy)4A2 and M(H2O)2(4mepy)8A2 (where M is Ni or Co and A is PF6 or AsF6) have been prepared and their electronic spectra and magnetic properties studied. A preliminary report is made of single crystal X-ray diffraction studies on Ni(H2O)2(4mepy)8(PF6)2, Co(H2O)2(4mepy)8(PF6)2, and Co(4mepy)4(PF6)2. All of the complexes have structures involving complex cations and non-coordinated anions, consistent with extremely weak ligating abilities for both PF6− and AsF6−. Cations identified and characterized are the squashed tetrahedral [Co(4mepy)4]2+ ion, the square planar [Ni(4mepy)4]2+ ion, and the tetragonal [Co(4mepy)4((4mepy)2H2O)2]2+and [Ni(4mepy)4((4mepy)2H2O)2]2+ ions. The ligand field strength of 4-methylpyridine is found to be indistinguishable from that of pyridine in these complexes. Infrared spectra are reported and infrared criteria for establishing the presence of non-coordinated anions in PF6− and AsF6− complexes are suggested.

2004 ◽  
Vol 848 ◽  
Author(s):  
Evan Lyle Thomas ◽  
Erin E. Erickson ◽  
Monica Moldovan ◽  
David P. Young ◽  
Julia Y. Chan

AbstractA new member of the LnMIn5 family, ErCoIn5, has been synthesized by a flux-growth method. The structure of ErCoIn5 was determined by single crystal X-ray diffraction. It crystallizes in the tetragonal space group P4/mmm, Z = 1, with lattice parameters a = 4.5400(4) and c = 7.3970(7) Å, and V = 152.46(2) Å3. Electrical resistivity data show metallic behavior. Magnetic susceptibility measurements show this compound to be antiferromagnetic with TN = 5.1 K. We compare these experimental results with those of LaCoIn5 in an effort to better understand the effect of the structural trends observed on the transport and magnetic properties.


IUCrData ◽  
2019 ◽  
Vol 4 (11) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus

Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].


2017 ◽  
Vol 72 (12) ◽  
pp. 937-940 ◽  
Author(s):  
Xiao-Hong Zhu ◽  
Xiao-Chun Cheng ◽  
Yun-Hua Qian

AbstractThe neutral, four-fold protonated pyridine-3,5-dicarbox(3,5-dicarboxylatoanilide) (H4L) reacts with Mn(II) salts under hydrothermal conditions to yield a new complex: [Mn2(L)(H2O)2]·H2O (1), which has been characterized by single crystal X-ray diffraction, infrared spectroscopy, and elemental and thermogravimetric analyses. Complex 1 exhibits a binodal (4,8)-connected 3D framework with flu (412.612.84)(46)2 topology. The magnetic properties of 1 were investigated.


2018 ◽  
Vol 42 (4) ◽  
pp. 198-201 ◽  
Author(s):  
Liping Wang ◽  
Erpeng Zhang ◽  
Xiaoli Zhou ◽  
Yufei Wang ◽  
Yanli Liu ◽  
...  

The coordination polymer [Cu3(tci)2(phen)2] n (H3tci = 1,3,5-tris(2-carboxyethyl)isocyanurate; phen = 1,10-phenanthroline) has been synthesised. Single-crystal X-ray diffraction studies have shown that the polymer displays a 2-D metal–organic framework based on linear trinuclear copper cluster units, and its magnetic properties indicate antiferromagnetic interactions.


2014 ◽  
Vol 1 (3) ◽  
pp. 278-283 ◽  
Author(s):  
Shiliang Huang ◽  
Jie Su ◽  
Kirsten Christensen ◽  
A. Ken Inge ◽  
Jie Liang ◽  
...  

An open-framework germanate SU-79 was synthesized using nickel complex and amine as the templates. The crystal structure was solved by the combination of rotation electron diffraction (RED) and synchrotron single crystal X-ray diffraction.


2004 ◽  
Vol 2 (2) ◽  
pp. 323-333
Author(s):  
Adrian Patrut ◽  
Adrian Nicoara ◽  
Dragos Margineanu ◽  
Michael Koop ◽  
Paul Kögerler ◽  
...  

AbstractThe paper presents a new polymeric polyoxomolybdate cluster with infinite octamolybdate chains cross-linked by iron (II) centers. The layer-type substance contains sodium cations sandwiched between the [Fe(H2O)4Mo8O27]∞ layers. The structure was determined by single crystal X-ray diffraction analysis. Magnetic properties, due to the presence of paramagnetic iron (II) centers, are presented and discussed.


IUCrData ◽  
2020 ◽  
Vol 5 (1) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus

Caesium tetrafluoridobromate(III), CsBrF4, was crystallized in form of small blocks by melting and recrystallization. The crystal structure of CsBrF4 was redetermined from single-crystal X-ray diffraction data. In comparison with a previous study based on powder X-ray diffraction data [Ivlev et al. (2013). Z. Anorg. Allg. Chem. 639, 2846–2850], bond lengths and angles were determined with higher precision, and all atoms were refined with anisotropic displacement parameters. It was confirmed that the structure of CsBrF4 contains two square-planar [BrF4]− anions each with point group symmetry mmm, and a caesium cation (site symmetry mm2) that is coordinated by twelve fluorine atoms, forming an anticuboctahedron. CsBrF4 is isotypic with CsAuF4.


2021 ◽  
Vol 3 (1) ◽  
pp. 0210102
Author(s):  
Masahiro Mikuriya ◽  
Atsushi Fujita ◽  
Takanori Kotera ◽  
Daisuke Yoshioka ◽  
Hiroshi Sakiyama ◽  
...  

New trinuclear CoII complexes, [{Co(apaet)2}2Co]X2 (apaet– = 2-[(3-aminopropyl)amino]ethanethiolato; X = SCN (1), ClO4 (2), NO3 (3), Cl (4), Br (5), I (6)) and [{Co(apampt)2}2Co]X2 (apampt– = 1-[(3-aminopropyl)amino]-2-methylpropane-2-thiolato; X = NO3(7), ClO4 (8), Cl (9), Br (10), I (11)), and mononuclear CoIII complexes, [Co(apaet)2]X (X = ClO4 (12), NO3 (13)), were synthesized. Single-crystal X-ray crystallography of 1 and 7 confirmed that the trinuclear complexes have a linear arrangement of octahedral CoIIS2N4-tetrahedral CoIIS4-octahedral CoIIS2N4 chromophores where two thiolate ligands are coordinated to each terminal Co atom in a mer coordination mode and the two thiolato S atoms are further bound to the central Co atom, which is consistent with the electronic spectra and antiferromagnetic properties


1992 ◽  
Vol 47 (4) ◽  
pp. 517-525 ◽  
Author(s):  
Thomas G. Meyer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler

A new synthesis for 2-chloro-1,3,5-trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinane (1) is described. Chlorine-fluorine exchange in 1 by means of sodium fluoride in acetonitrile in the presence of catalytic amounts of a crown ether furnished 2-fluoro-1,3,5-trimethyl-4,6-dioxo-1,3,5,2λ3-triazaphosphinane (2). The synthesis of the bromine and iodine analogues, 3 and 4, by metathesis of 1 with the appropriate trimethylsilyl halides, Me3SiBr and Me3SiI, respectively, is also described. The syntheses of an iron(0)tetracarbonyl complex (5) and of a dichloroplatinum( II) complex (6) are reported. A single crystal X-ray diffraction study was conducted on 6. [P21/c, a = 1161.3(3), b = 1423.2(3), c = 1247.7(3) pm, β = 109.42(2)°, R = 0.028], There are deviations from ideal square planar geometry at platinum. The heterocycles display a flattened boat conformation. A Staudinger reaction of 1 with Me3SiN3 led to the formation of a substituted cyclotriphosphazene.


Sign in / Sign up

Export Citation Format

Share Document