Trigold(I) Phosphine Derivatives of Clusters Containing Octahedral Rh2Ru4B-Boride Cores: The X-Ray Structure of [Rh2Ru4(CO)15Rh2Ru4B{AuPCy3}3] (Cy = cyclohexyl)

1999 ◽  
Vol 64 (6) ◽  
pp. 959-970 ◽  
Author(s):  
Andrew D. Hattersley ◽  
Catherine E. Housecroft ◽  
Arnold L. Rheingold
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Boron Atom ◽  
Variable Temperature ◽  
Mass Spectrometric ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Third ◽  
Phosphine Derivatives ◽  
Derivatives Of

The reaction of [Rh(CO)2Cl]2 with [HRu4(CO)12BH]- followed by treatment with an excess (at least three-fold) of [Cy3PAuCl] (Cy = cyclohexyl) leads to the formation of [Rh2Ru4(CO)16B{AuPCy3}] (previously prepared by another route) and [Rh2Ru4(CO)15B{AuPCy3}3]. The new trigold derivative has been characterized by spectroscopic and mass spectrometric methods, and by single crystal X-ray diffraction. It possesses an octahedral Rh2Ru4 core containing an interstitial boron atom; two of the gold(I) phosphine units cap two adjacent faces and the third bridges an edge of the octahedral cage. There are no close Au···Au contacts. Reactions of [Rh2Ru4(CO)16B]- with [(R3PAu)3O]+ (R = Ph, 2-MeC6H4) resulted in the formation of [Rh2Ru4(CO)15B{AuPR3}3]; for R = Ph, two isomers in respect of the arrangements of the AuPPh3 were isolated. Fluxional processes involving the gold(I) phosphine fragments have been observed using solution variable-temperature 31P NMR spectroscopy.

Conformational analysis and potential anticancer activity of [Pt(phen)(L1-κS)2] studied by single crystal X-ray diffraction and variable temperature 1H and 195Pt NMR spectroscopy

2019 ◽  
Vol 43 (9) ◽  
pp. 3665-3672 ◽  
Author(s):  
Edmore F. Kangara ◽  
Tebogo Peega ◽  
Leonie Harmse ◽  
Juanita L. van Wyk ◽  
Demetrius C. Levendis ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Conformational Analysis ◽  
Single Crystal ◽  
Anticancer Activity ◽  
Variable Temperature ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Π Stacking

Conformers of [Pt(phen)(L1-κS)2] observed in solution as a result of π-stacking interactions between the unusual κS-coordinated N,N-diethyl-N′-1-naphthoylthioureato ligands and 1,10-phenanthroline.

Synthese und Charakterisierung von Halogen-phosphor(III)- Derivaten des 8-Hydroxychinolins. Röntgenstrukturanalyse von 8-[Phenyl(chloro)-phosphito]-chinolin/ Synthesis and Characterization of Halogen-phosphorus(III) Derivatives of 8-Hydroxyquinoline. X -Ray Structure Analysis of 8-[Phenyl(chloro)phosphito]-quinoline

1993 ◽  
Vol 48 (1) ◽  
pp. 85-89 ◽  
Author(s):  
Lin Yang ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Compounds ◽  
Derivatives Of

The reaction of 8 -trimethylsiloxyquinoline, 2 with PCl3, PhPCl2, and PhPF2 has furnished the corresponding 8 -quinolyl halophosphite derivatives, 3-5 . The synthesis of two metal complexes, 8 and 9, of 4 with Au(I) and Pt(II) is described. The new compounds were characterized by elemental analysis and by 1H and 31P NMR spectroscopy. A single crystal X-ray diffraction study of 4 has been conducted; a short intramolecular P ··· N contact (230.9 pm) and a long P-Cl bond (218.7 pm) were observed.

scholarly journals New Spin-Crossover Compounds Containing the [Ni(mnt)] Anion (mnt = Maleonitriledithiolate)

2021 ◽  
Vol 7 (5) ◽  
pp. 72
Author(s):  
Scott S. Turner ◽  
Joanna Daniell ◽  
Hiroki Akutsu ◽  
Peter N. Horton ◽  
Simon J. Coles ◽  
...  
Keyword(s):  
Electrical Conductivity ◽  
Single Crystal ◽  
Spin Crossover ◽  
Variable Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Counter Ions ◽  
Bulk Magnetization ◽  
L1 And L2 ◽  
Derivatives Of

Two novel salts containing the anion [Ni(mnt)2]− (mnt = maleonitriledithiolate) have been synthesized. The counter-ions, [Fe(II)(L1 or L2)2], are cationic complexes where L1 and L2 are methylated derivatives of 2,6-bis(pyazolyl)pyridine or pyrazine, which are similar to ligands found in a series of spin-crossover (SCO) complexes. Both salts are characterized by variable temperature single crystal X-ray diffraction and bulk magnetization measurements. Compound 1, [Fe(II)(L1)2][Ni(mnt)2]2 displays an incomplete and gradual SCO up to 300 K, followed by a more rapid increase in the high-spin fraction between 300 and 350 K. Compound 2, [Fe(II)(L2)2][Ni(mnt)2]2.MeNO2, shows a gradual, but more complete SCO response centered at 250 K. For compound 2, the SCO is confirmed by variable temperature Mössbauer spectroscopy. In both cases, the anionic moieties are isolated from each other and so no electrical conductivity is observed.

Unusual Rearrangement of Naphthalene in the Synthesis of a Novel B8-B8-Bridged Derivative in the [(1,2-C2B9H11)2-3-Co]- Series. X-Ray Structure and 11B NMR Spectra of [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- (CH3)4N+

1997 ◽  
Vol 62 (5) ◽  
pp. 746-751 ◽  
Author(s):  
Andreas Franken ◽  
Jaromír Plešek ◽  
Christiane Nachtigal
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Nucleophilic Substitution ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Unusual Rearrangement ◽  
Multinuclear Nmr Spectroscopy ◽  
11B Nmr ◽  
Isolated Compound

On treatment of the [(1,2-C2B9H11)2Co]- ion with naphthalene in presence of AlCl3 a remarkably bridged [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- ion is obtained as a single isolated compound. The triatomic -CH2-C9H6- bridge is derived from the rearranged naphthalene nucleus. The mechanism of this reaction is obscure but it does resemble the "Electrophile-Induced Nucleophilic Substitution" reported earlier. The structure of the compound was established by multinuclear NMR spectroscopy and by single crystal X-ray diffraction.

Die Kristallstrukturen der isotypen Verbindungen Ba3[MoN4] und Ba3[WN4] / The Crystal Structures of the Isotypic Compounds Ba3[MoN4] and Ba3[WN4]

1991 ◽  
Vol 46 (5) ◽  
pp. 566-572 ◽  
Author(s):  
Axel Gudat ◽  
Peter Höhn ◽  
Rüdiger Kniep ◽  
Albrecht Rabenau
Keyword(s):  
Transition Metals ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ternary Compounds ◽  
The Third

The isotypic ternary compounds Ba3[MoN4] and Ba3[WN4] were prepared by reaction of the transition metals with barium (Ba3N2, resp.) under nitrogen. The crystal structures were determined by single crystal X-ray diffraction: Ba3[MoN4] (Ba3[WN4]): Pbca; Z = 8; a = 1083.9(3) pm (1091.8(3) pm), b = 1030.3(3) pm (1037.5(3) pm), c = 1202.9(3) pm (1209.2(4) pm). The structures contain isolated tetrahedral anions [MN4]6- (M = Mo, W) which are arranged in form of slightly distorted hexagonal layers and which are stacked along [010] with the sequence (···AB···). Two of the three Ba atoms are situated between, the third one is placed within the layers of [MN4]-groups. In this way the structures can be derived from the Na3As structure type.

An Intramolecular Boron Nitrogen Lewis Acid Base Pair on a Rigid Naphthyl Backbone

2012 ◽  
Vol 67 (6) ◽  
pp. 589-593 ◽  
Author(s):  
Daniel Winkelhaus ◽  
Beate Neumann ◽  
Norbert W. Mitzel
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Lewis Acid ◽  
Elemental Analysis ◽  
Base Pair ◽  
Ring System ◽  
X Ray Diffraction ◽  
Acid Base ◽  
X Ray ◽  
Boron Nitrogen

The reaction of (C6F5)2BCl with 8-lithio-N,N-dimethyl-1-naphthylamine (1) afforded the fivemembered ring system 8-bis(pentafluorophenyl)boryl-N,N-dimethyl-1-naphthylamine (2) with an intramolecular dative B-N bond. The compound was characterised by elemental analysis, NMR spectroscopy and single-crystal X-ray diffraction.

Molecular motions of a tetraphenylethylene-derived AIEgen directly monitored through in situ variable temperature single crystal X-ray diffraction

CrystEngComm ◽  
2021 ◽  
Author(s):  
Wei Meng ◽  
Lin Du ◽  
Lin Sun ◽  
Lian Zhou ◽  
Xiaopeng Xuan ◽  
...  
Keyword(s):  
Single Crystal ◽  
Phenyl Ring ◽  
Functional Group ◽  
Variable Temperature ◽  
Molecular Motions ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
X Ray ◽  
Conformation Changes

One organic functional group was introduced to distinguish the four phenyl ring of tetraphenylethylene, and the In situ temperature-dependent crystal structures were determined to exhibit the conformation changes of tert-butyl...

The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2]

2019 ◽  
Vol 75 (6) ◽  
pp. 1144-1151
Author(s):  
Tamara J. Bednarchuk ◽  
Wolfgang Hornfeck ◽  
Vasyl Kinzhybalo ◽  
Zhengyang Zhou ◽  
Michal Dušek ◽  
...  
Keyword(s):  
Phase Transitions ◽  
Single Crystal ◽  
Room Temperature ◽  
Variable Temperature ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Hybrid Compound ◽  
Space Group ◽  
X Ray

The organic–inorganic hybrid compound 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2] (4apFeS), was obtained by slow evaporation of the solvent at room temperature and characterized by single-crystal X-ray diffraction in the temperature range from 290 to 80 K. Differential scanning calorimetry revealed that the title compound undergoes a sequence of three reversible phase transitions, which has been verified by variable-temperature X-ray diffraction analysis during cooling–heating cycles over the temperature ranges 290–100–290 K. In the room-temperature phase (I), space group C2/c, oxygen atoms from the closest Fe-atom environment (octahedral) were disordered over two equivalent positions around a twofold axis. Two intermediate phases (II), (III) were solved and refined as incommensurately modulated structures, employing the superspace formalism applied to single-crystal X-ray diffraction data. Both structures can be described in the (3+1)-dimensional monoclinic X2/c(α,0,γ)0s superspace group (where X is ½, ½, 0, ½) with modulation wavevectors q = (0.2943, 0, 0.5640) and q = (0.3366, 0, 0.5544) for phases (II) and (III), respectively. The completely ordered low-temperature phase (IV) was refined with the twinning model in the triclinic P{\overline 1} space group, revealing the existence of two domains. The dynamics of the disordered anionic substructure in the 4apFeS crystal seems to play an essential role in the phase transition mechanisms. The discrete organic moieties were found to be fully ordered even at room temperature.

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