Structural studies on catalysts and catalyst precursors. The X-ray structure determination of (3-Allylpentane-2,4 dithionato)chloro(triethylphosphine)nickel(II), Ni(asacsac)(Pet3)Cl

1984 ◽  
Vol 37 (2) ◽  
pp. 273 ◽  
Author(s):  
KJ Cavell ◽  
DG Hay ◽  
AF Masters ◽  
GA Williams
Keyword(s):  
Structure Determination ◽  
Monoclinic Space Group ◽  
Structural Studies ◽  
Donor Atom ◽  
X Ray Diffraction ◽  
X Ray ◽  
Related Compounds ◽  
Atom Bond

The preparation and characterization of Ni(asacsac)(PEt3)Cl by single-crystal X-ray diffraction [refined to R = 0,049, R' = 0,052 with 1888 data having I ≥ 3σ(I)], are reported. The compound crystallizes as discrete molecules in the monoclinic space group P21/c, with a = 10,078(2), b = 8.202(3), c = 22.984(5) �, β = 97.57(2)�, U = 1883.3 �3 and Z = 4. The nickel-donor atom bond distances are Ni-S (trans Cl) 2.083(2), Ni-S (trans P) 2.127(2), Ni-Cl 2.208(2) and Ni-P 2,234(2) �, with the ligands at angles S-Ni-S 96.8(1), S-Ni-C1 86.2(1), S-Ni-P 90.7(1) and Cl-Ni-P 86.9(1)�. The coordination about the nickel(11) centre is approximately planar, but the planes NiSS and NiPCl are inclined at 8.3�. Comparisons are made with the structures of related compounds, in particular, that of Ni(sacsac)PEt3Cl.

Structural Studies on Catalysts and Catalyst Precursors. II. The X-Ray Structure Determination of Chloro(Pentante-2,4-dithionato)(tributylphosphine)nickel(II), Ni(sacsac)(PBu3)Cl

1985 ◽  
Vol 38 (3) ◽  
pp. 369 ◽  
Author(s):  
KJ Cavell ◽  
DG Hay ◽  
AF Masters ◽  
GA Williams
Keyword(s):  
Structural Studies ◽  
Donor Atom ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Apical Position ◽  
X Ray ◽  
Butyl Group ◽  
Atom Bond

The preparation and characterization of Ni( sacsac )(PBu3) Cl by single crystal X-ray diffraction [refined to R 0.052, R? 0.042 with 1325 data having I ≥ 3σ(I)], are reported. The compound crystallizes as discrete molecules in the orthorhombic space group P bca, with a 15.526(4), b 15.774(4), c 18.377(8)Ǻ, U 4500.7 Ǻ3, and Z 8. The nickel-donor atom bond distances are Ni-S (trans Cl ) 2.097(3), Ni-S (trans P) 2.138(3), Ni- Cl 2.216(3) and Ni-P 2.237(3)Ǻ, with the ligands subtending angles S-Ni-S 98.6(1), S-Ni- Cl 85.4(1), S-Ni-P 89.5(1) and Cl -Ni-P 86.8(1). The coordination about the nickel(II) centre is planar; however, one butyl group of the phosphine is oriented so that a hydrogen is directed towards the apical position of the nickel. The structure is correlated with the N.M.R . spectra in both solid and solution phases and compared with the structures of related com- pounds. The Ni-S bonds are shown to be short and the Ni-P bond long relative to such dimensions in comparable compounds.

New Coordination Compounds of Fe(III) with Organic Ligands

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  
Keyword(s):  
Chemical Analysis ◽  
Complex Compounds ◽  
Organic Ligands ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Chemical Analysis ◽  
Structural Formulae ◽  
Paramagnetic Properties

In this paper the synthesis and the study of some complex compounds of Fe(III) with ligands derived from: 2-(4-chloro-phenylsulfanyl)-1-(2-hydroxy-3,5-diiodo-phenyl)-ethanone (HL1), 1-(3,5-dibromo-2-hydroxy-phenyl)-2-phenylsulfanyl-ethanone(HL2), and 2-(4-chloro-phenylsulfanyl)-1-(3,5-dibromo-2-hydroxy-phenyl)-ethanone (HL3) is presented. The characterization of these complexes is based on method as: the elemental chemical analysis, IR and ESR spectroscopy, M�ssbauer, the thermogravimetric analysis and X-ray diffraction. Study of the IR and chemical analysis has evidenced that the precipitates form are a complexes and the combination ratio of M:L is 1:2. The central atoms of Fe(III) presented paramagnetic properties and a octaedric hybridization. Starting from this precipitation reactions, a method for the gravimetric determination of Fe(III) with this organic ligands has been possible. Based on the experimental data on literature indications, the structural formulae of the complex compounds are assigned.

Structure determination of ultrathin NbSe2 films by Grazing incidence x-ray diffraction

1994 ◽  
Vol 89 (7) ◽  
pp. 583-586 ◽  
Author(s):  
Toshihiro Shimada ◽  
Yukito Furukawa ◽  
Etsuo Arakawa ◽  
Kunikazu Takeshita ◽  
Tadashi Matsushita ◽  
...  
Keyword(s):  
Structure Determination ◽  
Grazing Incidence ◽  
X Ray Diffraction ◽  
X Ray

Structure determination of modulated structures by powder X-ray diffraction and electron diffraction

2016 ◽  
Vol 3 (11) ◽  
pp. 1351-1362 ◽  
Author(s):  
Zhengyang Zhou ◽  
Lukáš Palatinus ◽  
Junliang Sun
Keyword(s):  
Electron Diffraction ◽  
Structure Determination ◽  
X Ray Diffraction ◽  
X Ray ◽  
Modulated Structures ◽  
Conventional Methods

The combination of PXRD and ED is applied to determine modulated structures which resist solution by more conventional methods.

Interrupted silicogermanate with 10-ring channels: synthesis and structure determination by combining rotation electron diffraction and powder X-ray diffraction

2017 ◽  
Vol 4 (10) ◽  
pp. 1654-1659 ◽  
Author(s):  
Yilin Wang ◽  
Yunchen Wang ◽  
Jie Su ◽  
Xiaowei Song ◽  
Wei Wan ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Structure Determination ◽  
X Ray Diffraction ◽  
X Ray

Structure determination of silicogermanate with sti layers pillared by D4R/Ge7 units by rotation electron diffraction and powder X-ray diffraction.

Structure determination of fatty acid ester biofuels via in situ cryocrystallisation and single crystal X-ray diffraction

CrystEngComm ◽  
2019 ◽  
Vol 21 (1) ◽  
pp. 41-52 ◽  
Author(s):  
Siriyara Jagannatha Prathapa ◽  
Cara Slabbert ◽  
Manuel A. Fernandes ◽  
Andreas Lemmerer
Keyword(s):  
Crystal Structure ◽  
Fatty Acid ◽  
Fatty Acid Ester ◽  
Structure Determination ◽  
Homologous Series ◽  
Methyl Esters ◽  
X Ray Diffraction ◽  
X Ray

In situ cryocrystallisation enabled the crystal structure determination of a homologous series of low-melting n-alkyl methyl esters Cn−1H2n+1CO2CH3.

scholarly journals Serendipitous formation and characterization of K2[Pd(NO3)4]·2HNO3

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Solvothermal Process ◽  
X Ray Diffraction ◽  
Glass Ampoule ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.

Structure determination of a partially ordered layered silicate material with an NMR crystallography approach

2017 ◽  
Vol 73 (3) ◽  
pp. 184-190 ◽  
Author(s):  
Darren Henry Brouwer ◽  
Sylvian Cadars ◽  
Kathryn Hotke ◽  
Jared Van Huizen ◽  
Nicholas Van Huizen
Keyword(s):  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Three Dimensional ◽  
Layered Silicate ◽  
Silicate Layer ◽  
Silicate Material ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Crystallography

Structure determination of layered materials can present challenges for conventional diffraction methods due to the fact that such materials often lack full three-dimensional periodicity since adjacent layers may not stack in an orderly and regular fashion. In such cases, NMR crystallography strategies involving a combination of solid-state NMR spectroscopy, powder X-ray diffraction, and computational chemistry methods can often reveal structural details that cannot be acquired from diffraction alone. We present here the structure determination of a surfactant-templated layered silicate material that lacks full three-dimensional crystallinity using such an NMR crystallography approach. Through a combination of powder X-ray diffraction and advanced 29Si solid-state NMR spectroscopy, it is revealed that the structure of the silicate layer of this layered silicate material templated with cetyltrimethylammonium surfactant cations is isostructural with the silicate layer of a previously reported material referred to as ilerite, octosilicate, or RUB-18. High-field 1H NMR spectroscopy reveals differences between the materials in terms of the ordering of silanol groups on the surfaces of the layers, as well as the contents of the inter-layer space.

Ab initio structure determination of anhydrous sodium alendronate from laboratory powder X-ray diffraction data

2009 ◽  
Vol 98 (6) ◽  
pp. 2113-2121 ◽  
Author(s):  
Minakshi Asnani ◽  
K. Vyas ◽  
Apurba Bhattacharya ◽  
Surya Devarakonda ◽  
Santu Chakraborty ◽  
...  
Keyword(s):  
Ab Initio ◽  
Diffraction Data ◽  
Structure Determination ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ab Initio Structure
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