Studies of β-Diketone Complexes of Rhenium. I. Trispentane-2,4-dionatorhenium(III) and Tris(1,1,1,5,5,5-hexafluoropentane-2,4-dionato)rhenium(III)

1972 ◽  
Vol 50 (1) ◽  
pp. 8-17 ◽  
Author(s):  
W. D. Courrier ◽  
W. Forster ◽  
C. J. L. Lock ◽  
G. Turner
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Magnetic Susceptibility ◽  
Infrared Spectroscopy ◽  
Physical Properties ◽  
Ligand Field ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
X Ray ◽  
Monoclinic Cell

Pure samples2 of Re(hfac)3 and Re(acac)3 have been prepared and their physical properties studied by ultraviolet–visible and infrared spectroscopy, mass spectrometry, magnetic susceptibility measurements, and X-ray diffraction. The compounds are monomeric and the physical properties may be explained if the rhenium atom sits in an essentially octahedral ligand field. Re(hfac)3 has a hexagonal unit cell and the acetyl-acetone complex adopts the monoclinic cell of the α-form of the three typical crystal structure types which Astbury (1) observed for trispentane-2,4-dionatometal(III) compounds. The properties observed for trispentane-2,4-dionatorhenium(III) differ from those reported previously (2, 3). The difficulties experienced in obtaining pure Re(C5H7O2)3 were caused by the ease with which the material is oxidized.

Synthesis, crystal structure, and magnetic properties of the complex [(CH3)3NH]2 [Co(NCS)4]

2018 ◽  
Vol 73 (8) ◽  
pp. 571-575
Author(s):  
Yang Jie ◽  
Huang Yuan ◽  
Zhong YouQuan ◽  
Fang Ting ◽  
Hao Fan ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Magnetic Susceptibility ◽  
Infrared Spectroscopy ◽  
Magnetic Measurements ◽  
X Ray Diffraction ◽  
Magnetic Susceptibility Data ◽  
X Ray ◽  
Susceptibility Data ◽  
Ferromagnetic Interactions

AbstractA new complex [(CH3)3NH]2[Co(NCS)4], in which zero-dimensional [Co(NCS)4]n2− anions are balanced by 2n [(CH3)3NH]+ cations, was synthesized. The complex has been characterized by single X-ray diffraction, infrared spectroscopy, elemental analysis, and magnetic measurements. Magnetic susceptibility data indicate ferromagnetic interactions among the CoII ions.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

Synthesis and Crystal Structure of the Flexible Ligand Coordination Polymer [Co3(bpd)5.5(NCS)6(NH3)]n⋅2H2O(bpd= 1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene)

2013 ◽  
Vol 803 ◽  
pp. 80-84
Author(s):  
Yu Qi Liu ◽  
Yong Yang ◽  
Rui Yang ◽  
Xiao Jun Xu
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Coordination Polymer ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Elemental Analyses ◽  
Ligand Coordination ◽  
Point Symbol

A novel metalorganic coordination polymer, namely [Co3(bpd)5.5(NCS)6(NH3)]n2H2O (1) (bpd=1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene), has been synthesized and characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. Compound 1 presents 2D[3,4,-connected 3-nodal net with the point symbol (4268210)(4462)(8210). In addition, four identical 2D single nets is interlocked with each other in parallel, thus directly leading to the formation of a polycatenated layer (2D2D).

Effects of Electron Beam on Structure and Physical Properties of Natural Colorless Topaz

2015 ◽  
Vol 1125 ◽  
pp. 60-63
Author(s):  
Chutharat Paikaew ◽  
Juthamas Inthanont ◽  
Adisak Punyanut ◽  
Ekachai Hoonnivathana ◽  
Pichet Limsuwan ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Electron Beam ◽  
Physical Properties ◽  
Orthorhombic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Spin Resonance ◽  
Function Group ◽  
And Function ◽  
Beam Dose

The purpose of this research was to investigate physical properties, configuration and color of topaz. Topazes were irradiated with electron beam linear accelerator at different dose from 40 to 180 MGy. The color of topaz was analyzed by UV-vis and it was shown that the color of topaz was becoming strong color with increased electron beam dose. Crystal structure and function group of topaz were characterized by X- ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. The results showed that the topaz has orthorhombic structure and no other crystalline. After irradiated, topaz released OH indicating higher crystallinity of topaz and this was confirmed with the results of electron spin resonance (ESR). Electron beam dose response of topaz was investigated. ESR results showed that the Al3+ ion was substituted in Si4+ site and Ti3+ impurity in Al4+ site and this result corresponds to the results of FTIR. The experiment result indicated that electron beam could be making defect on crystal structure and color enhancement of topaz.

Thiocarbonyl Complexes of Rhenium. Part I.

1993 ◽  
Vol 48 (6) ◽  
pp. 771-777 ◽  
Author(s):  
Ulrich Abram ◽  
Bernd Lorenz
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
Monomeric Complex ◽  
Structure Solution ◽  
R Value

Novel rhenium complexes with terminal thiocarbonyl groups have been synthesized from ReCl3(Me2PhP)3 and sodium diethyldithiocarbamate. mer-(Diethyldithiocarbamato)tris-(dimethylphenylphosphine)(thiocarbonyl)rhenium(I), mer-[Re(CS)(Me2PhP)3(Et2dtc)], and tris(diethyldithiocarbamato)(thiocarbonyl)rhenium(III), [Re(CS)(Et2dtc)3] have been studied by infrared and NMR spectroscopy, mass spectrometry and X-ray diffraction.mer-[Re(CS)(Me2PhP)3(Et2dtc)] crystallizes orthorhombic in the space group Pna21 with a = 1516.1(2), b = 2189.8(2) and c = 1035.6(1) pm. Structure solution and refinement converged at R = 0.042. The coordination geometry is a distorted octahedron. The Re—C bond length is found to be 184(2) pm.[Re(CS)(Et2dtc)3] crystallizes monoclinic in the space group P21/c with a = 962.2(6), b = 1744.0(2), c = 1537.4(6) pm and β = 96.21(1)°. The final R value is 0.028. In the monomeric complex the rhenium atom is seven-coordinate with an approximate pentagonal-bipyramidal coordination sphere and a rhenium-carbon distance of 181(1) pm.

The hydrocerussite-related phase, NaPb5(CO3)4(OH)3, from the ancient slags of Lavrion, Greece

2018 ◽  
Vol 82 (4) ◽  
pp. 809-819 ◽  
Author(s):  
Oleg I. Siidra ◽  
Diana O. Nekrasova ◽  
Nikita V. Chukanov ◽  
Igor V. Pekov ◽  
Vasiliy O. Yapaskurt ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Sea Water ◽  
Mining District ◽  
X Ray Diffraction ◽  
Electron Pairs ◽  
X Ray ◽  
Lead Hydroxide ◽  
Lamellar Crystals ◽  
Related Phase

ABSTRACTThe hydrocerussite-related phase, NaPb5(CO3)4(OH)3, has been found as colourless lamellar crystals in cavities within a pebble of the ancient marine slag collected in the Pacha Limani area of the Lavrion mining district, Attiki, Greece. This phase of anthropogenic origin was characterized by electron microprobe, infrared spectroscopy, powder and single-crystal X-ray diffraction. The unique crystal structure (P63/mmc,a= 5.2533(11),c= 29.425(6) Å,V= 703.3(3) Å3andR1= 0.047) is based upon structurally and chemically different electroneutral blocks. Each of the blocks can be split into separate sheets. The outer sheets in each block are topologically identical and have the composition [PbCO3]0. The [Pb(OH)2]0lead hydroxide sheet is sandwiched between the two [PbCO3]0sheets resulting in the formation of the first block [Pb3(OH)2(CO3)2]0structurally and compositionally identical to that one in hydrocerussite Pb3(OH)2(CO3)2. Similarly the [Na(OH)]0sheet is sandwiched between another two [PbCO3]0sheets thus forming the [NaPb2(OH)(CO3)2]0block described previously in the structure of abellaite NaPb2(OH)(CO3)2. Stereochemically active lone electron pairs on Pb2+cations are located between the blocks. There are two blocks of each type per unit cell, which corresponds to the following formula: [Pb3(OH)2(CO3)2][NaPb2(OH)(CO3)2] or NaPb5(CO3)4(OH)3in the simplified representation. The formation of NaPb5(CO3)4(OH)3in Lavrion slags is by the contact of lead-rich slags with the sea water over the last two thousand years.

Hydrothermal Synthesis and Crystal Structure of a Meso-Helical Chain Based on Lindqvist Polyoxometalates

2013 ◽  
Vol 68 (4) ◽  
pp. 345-350 ◽  
Author(s):  
Chun-Jing Zhang ◽  
Rui Fang ◽  
Yan Yu ◽  
Hai-Jun Pang ◽  
Hui-Yuan Ma ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Hydrothermal Synthesis ◽  
Chain Structure ◽  
Helical Chain ◽  
X Ray Diffraction ◽  
Hybrid Compound ◽  
Monoclinic System ◽  
Synthesis And Crystal Structure ◽  
X Ray

A new Lindqvist polyoxometalate-based hybrid compound with a helical chain structure, [Cu(bipy)2][W6O19] (1), (bipy = 2;20`-bipyridine), has been hydrothermally synthesized and characterized by elemental analysis, infrared spectroscopy, thermogravimetry, and single-crystal X-ray diffraction. The compound crystallizes in the space group C2/c of the monoclinic system. In 1, the [W6O19]2- anions are connected alternately with [Cu(bipy)2]2+ subunits to form a meso-helical chain. To our knowledge, this structure represents the first example of a helical chain structure consisting of the hexatungstate anion [W6O19]2-. The electrochemical properties of the title compound have been studied.

Article

1998 ◽  
Vol 76 (3) ◽  
pp. 307-312
Author(s):  
A Wallace Cordes ◽  
Robert C Haddon ◽  
Robin G Hicks ◽  
Richard T Oakley ◽  
Kristen E Vajda
Keyword(s):  
Crystal Structure ◽  
Phase Transition ◽  
Magnetic Susceptibility ◽  
Electronic Structure ◽  
Charge Transfer ◽  
Electronic Structures ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Diamagnetic State

Electroreduction of the 2,5-thiophene-bridged bis(1,2,3,5-diselenadiazolylium) salt [T-2,5-Se][SbF6]2 in acetonitrile, at a Pt wire and in the presence of iodine, affords a highly conductive ( sigma = 102 S cm-1 at 293 K) 1:1 charge-transfer (CT) salt [T-2,5-Se][I], the crystal structure of which has been determined by single-crystal X-ray diffraction. The crystals belong to the orthorhombic space group Fm2m, a = 3.544(2), b = 10.9808(16), c = 31.464(5) Å , V = 1224.5(7) Å 3. The structure consists of perfectly superimposed pi -stacks of molecular units bridged by columns of disordered iodines. This packing motif is similar to that of the related 1,3-benzene-bridged derivative [1,3-Se][I], but the lateral intermolecular Se···Se interactions linking adjacent pi -stacks are considerably shorter, indicative of a more isotropic electronic structure for [T-2,5-Se][I]. Magnetic susceptibility measurements on [T-2,5-Se][I] nonetheless indicate a phase transition to a diamagnetic state near 200 K, behaviour similar to that observed for [1,3-Se][I]. The electronic structures and transport properties of the two compounds are discussed in the light of extended Hückel band-structure calculations.Key words: diselenadiazolyl, diradical, charge-transfer salt, magnetic susceptibility, crystal structure.

Boron Carbide-Based Ceramics Via Polymer Route Synthesis

1991 ◽  
Vol 249 ◽  
Author(s):  
Haixing Zheng ◽  
Kevin Thorne ◽  
J.D. Mackenzie ◽  
Xiaoguang Yang ◽  
M.F. Hawthome
Keyword(s):  
Thermal Analysis ◽  
Infrared Spectroscopy ◽  
High Temperature ◽  
Nmr Spectroscopy ◽  
Physical Properties ◽  
Boron Carbide ◽  
X Ray Diffraction ◽  
Polymeric Precursors ◽  
X Ray ◽  
Crystalline Boron

ABSTRACTBoron carbide is a ceramic material with excellent high temperature physical properties. As compared to conventional techniques, the preparation of boron carbide from polymeric precursors is attractive as this technique offers a number of unique advantages. In this paper, the screening of polymeric precursors to boron carbide will be discussed. Two promising boron carbide, carborane containing polymeric precursors have resulted in 60-70 wt.% ceramic yields. The chemistry of polymer synthesis and the transformations from the polymer to amorphous and crystalline boron carbide were investigated with infrared spectroscopy, NMR spectroscopy, thermal analysis, and x ray diffraction.

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