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.

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.

scholarly journals Synthesis and characterization of hybrid Anderson hexamolybdoaluminates(III) functionalized with indometacin or cinnamic acid

2018 ◽  
Vol 74 (11) ◽  
pp. 1378-1383 ◽  
Author(s):  
Nadiia I. Gumerova ◽  
Amir Blazevic ◽  
Tania Caldera Fraile ◽  
Alexander Roller ◽  
Gerald Giester ◽  
...  
Keyword(s):  
Cinnamic Acid ◽  
Inhibitory Concentration ◽  
Antibacterial Activities ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
H Nmr ◽  
Single Side

The single-side Al-centred tris-functionalized hybrid organic–inorganic Anderson polyoxomolybdates (C16H36N)3[Al(OH)3Mo6O18(OCH2)3CNH(C10H8O)]·C9H7N·4CH3OH·5H2O (AlMo6-NH-Cin; Cin is cinnamic acid, C10H9O2) and (C16H36N)3[Al(OH)3Mo6O18(OCH2)3CNH(C19H15ClNO3)]·9H2O (AlMo6-NH-Indo; Indo is indometacin, C19H16ClNO4) have been prepared in a mild three-step synthesis and structurally characterized by single-crystal X-ray diffraction, 1H NMR and IR spectroscopies and elemental analysis. Both AlMo6-NH-Cin and AlMo6-NH-Indo crystallize in the orthorhombic space group Pbca. The antibacterial activities of AlMo6-NH-Cin and AlMo6-NH-Indo against the Gram-negative human mucosal pathogen Moraxella catarrhalis were investigated by determination of the minimum inhibitory concentration, which is 32 µg ml−1 for AlMo6-NH-Cin and 256 µg ml−1 for AlMo6-NH-Indo.

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.

scholarly journals Crystallization, optimization and preliminary X-ray characterization of a metal-dependent PI-PLC fromStreptomyces antibioticus

2012 ◽  
Vol 68 (11) ◽  
pp. 1378-1386 ◽  
Author(s):  
Michael R. Jackson ◽  
Thomas L. Selby
Keyword(s):  
X Ray Diffraction ◽  
Hanging Drop ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Streptomyces Antibioticus ◽  
Cell Parameters ◽  
Heavy Atoms ◽  
Hanging Drop Method

A recombinant metal-dependent phosphatidylinositol-specific phospholipase C (PI-PLC) fromStreptomyces antibioticushas been crystallized by the hanging-drop method with and without heavy metals. The native crystals belonged to the orthorhombic space groupP222, with unit-cell parametersa= 41.26,b= 51.86,c = 154.78 Å. The X-ray diffraction results showed significant differences in the crystal quality of samples soaked with heavy atoms. Additionally, drop pinning, which increases the surface area of the drops, was also used to improve crystal growth and quality. The combination of heavy-metal soaks and drop pinning was found to be critical for producing high-quality crystals that diffracted to 1.23 Å resolution.

Determination of the Crystal Structure and Redefinition of Tsugaruite, Pb28As15S50Cl, the First Lead-Arsenic Chloro-Sulfosalt

2020 ◽  
Author(s):  
Cristian Biagioni ◽  
Luca Bindi ◽  
Koichi Momma ◽  
Ritsuro Miyawaki ◽  
Yoshitaka Matsushita ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Atomic Ratio ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Specific Position ◽  
Actual Classification ◽  
Aomori Prefecture

Abstract Tsugaruite was originally defined as a lead-arsenic sulfosalt from the Yunosawa mine, Aomori Prefecture, Japan. Until recently its crystal structure remained unsolved and its actual classification in the sulfosalt realm was unknown. Here the refinement of the crystal structure of tsugaruite using single-crystal X-ray diffraction data is reported. The mineral is orthorhombic, space group P2nn, with unit-cell parameters a = 8.0774(10), b = 15.1772(16), c = 38.129(4) Å, V = 4674.3(9) Å3, in agreement with previous studies. The solution of the crystal structure of this mineral revealed Cl occupying a specific position. Chlorine was thus sought and found using the electron microprobe; the average of six spot analyses gave (in wt.%): Pb 68.04, As 12.83, S 18.29, Cl 0.63, total 99.80. The empirical formula, calculated on the basis of Pb + As = 43 atoms per formula unit, is Pb28.26As14.74S49.08Cl1.52. Tsugaruite is an N = 4 plesiotypic derivative of the homologous series of Pb-Sb chloro-sulfosalts having the general formula Pb(2+2N)(Sb,Pb)(2+2N)S(2+2N)(S,Cl)(4+2N)ClN. It has a Cl/(Cl + S) atomic ratio close to that of other known Pb-Sb chloro-sulfosalts (pillaite, pellouxite) and slightly higher than that of dadsonite.

Synthesis and Structural Characterization of Ca14NbxIn1-xAs11 (x ≈ 0.85)

2016 ◽  
Vol 257 ◽  
pp. 147-151 ◽  
Author(s):  
Yi Wang ◽  
Svilen Bobev
Keyword(s):  
Physical Properties ◽  
Side Reaction ◽  
Structure Type ◽  
Major Product ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ongoing Work ◽  
Set Up

Single-crystals of the new compound Ca14NbxIn1–xAs11 have been obtained from a solid-state reaction in a sealed Nb ampoule. The initial experiment had been set up with the aim to investigate the effect of electron doping (via In) on the crystal structure and physical properties of Ca14MnAs11. Subsequent single-crystal X-ray diffraction and elemental analysis work suggested that instead of Ca14MnxIn1–xAs11, the major product of the reaction is the phase Ca14NbxIn1–xAs11. This supposition was corroborated when the title compound was synthesized from a reaction of Ca, In and As in a sealed Nb ampoule, proving that, 1) Mn metal is not included in the structure, and 2) that the inadvertent side reaction of As with the walls of the Nb container is the source of the niobium. The overall structure is isotypic with the tetragonal Ca14AlSb11 structure type (space group I41/acd), although some marked differences between the two must be noted. Current ongoing work is focused on the synthesis of phase pure polycrystalline samples and determination of the physical properties of this unusual transition metal Zintl phase.

Structural studies of technetium complexes. V. The preparation and crystal structure of Dichlorobis(diethyldithiocarbamato)thionitrosyltechnetium(III)

1984 ◽  
Vol 37 (4) ◽  
pp. 751 ◽  
Author(s):  
J Baldas ◽  
J Bonnyman ◽  
MF Mackay ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Positive Charge ◽  
Mirror Plane ◽  
Structural Studies ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Data Set ◽  
Coordination Environment ◽  
X Ray

Dichlorobis(diethyldithiocarbamato)thionitrosyltechnetium(III), [Tc(S2CNEt2)2Cl2(NS)], has been prepared by the reaction of [Tc(S2CNEt2)2N] with either disulfur dichloride or thionyl chloride. The crystal structure of [TC(S2CNEt2)2Cl2(NS)] has been determined by single-crystal X-ray diffraction methods at 15�C. Crystals are orthorhombic, space group Pcmn, with a 8.936(1), b 15.681(1), c 28.445(7) �, and Z 8. Automatic diffractometry has provided significant Bragg intensities for 2078 independent reflections, and the structure has been refined by full-matrix least-squares methods to R 0.078. The crystal lattice is disordered across a non-crystallographic mirror plane, the degree of disorder being 4.0(2)% for the crystal described above, and 21.9(7)% for another crystal initially used to obtain an intensity data set. There are two independent molecules of [Tc(S2CNEt2)2Cl2(NS)] in the asymmetric unit, and in each the technetium atom is seven-coordinate with a pentagonal-bipyramidal coordination environment. The Tc=N=S bonding is linear with Tc=N c. 1.75 and N=S c. 1.52 �, which indicates that the thionitrosyl group is a three-electron donor with a formal positive charge. This is only the third crystal structure of a complex containing the thionitrosyl group to be determined, and the first for technetium.

Steric Modification of Metal-Phosphorus Bond Lengths: the Preparation, Characterization and CrystalStructures of mer-trans-(PPri3)2(Pme2Ph)-Cl-cis-H2IrIII(1) and mer-trans-(PPri3)2(PMe2Ph)H3IrIII

1995 ◽  
Vol 48 (6) ◽  
pp. 1183 ◽  
Author(s):  
EJ Ditzel ◽  
GB Robertson
Keyword(s):  
Chloride Content ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Steric Crowding ◽  
Unit Increase

The syntheses and subsequent characterization of the complexes mer -trans-(PPri3)2(Pme2Ph)-Cl-cis-H2IrIII(1) and mer-trans-(PPri3)2(PMe2Ph)H3IrIII (2) by n.m.r. and by low temperature (153�5 K) X-ray diffraction analyses are reported. Crystals of (1) are monoclinic, space group P21/c with a 19.277(2), b 9.020(1), c 17.657(2) Ǻ, β 101.40(1)° and Z 4. Crystals of (2) are orthorhombic, space group P212121, with a 19.373(3), b 18.724(2), c 8.113(1) Ǻ and Z 4. Full-matrix least-squares analyses converged with R = 0.027 and wR = 0.031 for (1) (3243 reflections), and R = 0.030 and wR = 0.038 for (2) (2892 reflections). Consistent with previous observation, the unit increase in chloride content (in place of hydride) in (1) is accompanied by a global lengthening of 0.036 Ǻ (av.) in the Ir -P bond lengths cf. those in (2). Also, because of increased steric crowding (two PPri3 ligands in place of two Pme2Ph), the Ir-PMe2Ph bond in (1) is 0.019(2) Ǻ longer than the chemically equivalent bond in mer-(PMe2Ph)3Cl-cis-H2IrIII. In previously reported complexes in this series metrically similar increases in Ir-PMe2Ph distances result from the replacement of just one Pme2Ph ligand by PPri3.

Ab initiostructure determination of the Γ form ofD-sorbitol (D-glucitol) by powder synchrotron X-ray diffraction

2004 ◽  
Vol 37 (5) ◽  
pp. 766-772 ◽  
Author(s):  
Mwaffak Rukiah ◽  
Jacques Lefebvre ◽  
Olivier Hernandez ◽  
Wouter van Beek ◽  
Michel Serpelloni
Keyword(s):  
Monte Carlo ◽  
Simulated Annealing ◽  
Interatomic Bond ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Rietveld Refinements ◽  
X Ray ◽  
Monte Carlo Simulated Annealing ◽  
Starting Model

A high-resolution powder synchrotron X-ray diffraction pattern of the Γ form of D-sorbitol has been recorded at 293 K on the BM1B beamline at the ESRF (Grenoble). The starting model of the structure was found by Monte Carlo simulated annealing. The final structure was obtained through Rietveld refinements performed with soft restraints on interatomic bond lengths and angles. The symmetry is orthorhombic, space groupP21212, with 12 molecules within the cell [a= 24.3012 (2),b= 20.5726 (2),c= 4.8672 (1) Å,V= 2433.30 (3) Å3,Z′ = 3, 36 non-H independent atoms]. Crystalline cohesion between neighbouring molecules is achieved by three networks of O—H...O hydrogen bonds. The width of the Bragg peaks is interpreted through a microstructural approach in terms of anisotropic strain effects.

An expert system for the structural characterization of kaolinites

Clay Minerals ◽  
1990 ◽  
Vol 25 (3) ◽  
pp. 249-260 ◽  
Author(s):  
A. Plançon ◽  
C. Zacharie
Keyword(s):  
Expert System ◽  
Defect Structure ◽  
Defect Structures ◽  
X Ray Diffraction ◽  
Diffraction Profile ◽  
X Ray ◽  
Diffraction Patterns ◽  
Xrd Patterns

AbstractUntil recently, the determination of the defect structures (previously referred to incorrectly as “crystallinity”) of kaolinites has been obtained in one of two ways: (1) measurement of the Hinckley index, or (2) by comparing calculated X-ray diffraction patterns based on a model of the defect structure (including types of defects and abundances) with experimental diffraction profiles. The Hinckley method is simple and easy to perform but contains no real information about the defect structure. Calculated XRD patterns are based on real defects but these calculations are time consuming and require some skill in application. Another approach is proposed: an expert system which will accurately describe the defect structure of kaolinites based on a few measurements taken from a normal powder diffraction profile. This system has been verified for nine kaolinite samples for which the defect structure was previously determined by comparison of calculated and observed diffraction profiles. The expert system reproduced the correct defect structure for each of the samples.

Sign in / Sign up

Export Citation Format

Share Document