Gold(I) Complexes Bearing P∩N-Ligands: An Unprecedented Twelve-membered Ring Structure Stabilized by Aurophilic Interactions

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1513-1524 ◽  
Author(s):  
Uwe Monkowius ◽  
Manfred Zabel ◽  
Michel Fleck ◽  
Hartmut Yersin
Keyword(s):  
Solid State ◽  
Ring Structure ◽  
Phosphine Ligands ◽  
X Ray Crystallography ◽  
Aggregation Pattern ◽  
Elemental Analyses ◽  
High Yields ◽  
First Time ◽  
Solid State Structures ◽  
Aurophilic Interactions

The P∩N-ligands Ph2Pqn, 1, Ph2 Piqn, 2, Ph2 Ppym, 3, and the As∩N-ligands Ph2Asqn, 4, Ph2Asiqn, 5, (Ph = phenyl, qn = 8-quinoline, iqn = 1-isoquinoline, pym = 2-pyrimidine) have been synthesized, the ligands 2 and 5 for the first time. Their ligand properties were probed by the synthesis of gold(I) complexes. Reaction with (tht)AuCl (tht = tetrahydrothiophene) yielded the chlorogold complexes Ph2RP-Au-Cl (R = qn, 6; iqn, 7; pym, 8) and Ph2RAs-Au-Cl (R = qn, 9; iqn, 10) in high yields. Further treatment of 7 and 8 with one equivalent of AgBF4 provided the complexes [(Ph2Piqn)Au]BF4, 11, [(Ph2Ppym)Au]BF4, 12, and [(Ph2Piqn)Au(tht)]BF4, 14. For comparison, the previously reported complex [(Ph2Ppy)Au]BF4 (py = pyridine), 13, was re-investigated. The compounds were characterized by elemental analyses, mass spectrometry and NMR spectroscopy. In addition, the solid-state structures of 2, 3, 6, 7, 9 - 14 have been determined by X-ray crystallography. The chloro-gold compounds crystallize in the common rod-like structure known from R3EAuCl (R = aryl, E = P, As) complexes without further aggregation via aurophilic interactions. In all cases the phosphine acts as a monodentate ligand. In the solid state compounds 11 - 13 feature an unprecedented cyclic trinuclear aggregation pattern, in which the Au(I) atoms are linearly coordinated by the bridging phosphine ligands forming a cyclic (P-Au-N)3 arrangement. The resulting twelvemembered ring is further stabilized by Au · · · Au interactions. Due to the presence of these Au · · · Au contacts, 11 - 13 are emissive in the solid state but not in solution

scholarly journals Simple Methylcadmium Alkoxides

2007 ◽  
Vol 62 (10) ◽  
pp. 1339-1342 ◽  
Author(s):  
Surajit Jana ◽  
Tania Pape ◽  
Norbert W. Mitzel
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Molecular Formula ◽  
Equimolar Ratio ◽  
X Ray ◽  
X Ray Crystallography ◽  
Elemental Analyses ◽  
Solid State Structures ◽  
Structural Aspects ◽  
C Nmr

The reaction of dimethylcadmium with alcohols R-OH in equimolar ratio leads to the formation of tetrameric methylcadmium alkoxides with molecular formula [(MeCd)4 (OR)4] [R = Me (1), Et (2) and iPr (3)]. These compounds have been characterised by 1H, 13C NMR and IR spectroscopy, by mass spectrometry, elemental analyses and by X-ray crystallography (for 2 and 3). The solid state structures show distorted cubane-type aggregates with Cd4O4 cores. The structural aspects and the spectroscopic characterisations of these compounds are discussed.

Synthesis and molecular structures of N,N-dialkyl-4-nitrosoaniline adducts of formally d6 metalloporphyrins of ruthenium and cobalt

2001 ◽  
Vol 05 (09) ◽  
pp. 702-707 ◽  
Author(s):  
LI CHEN ◽  
JESSE B. FOX ◽  
GEUN-BAE YI ◽  
MASOOD A. KHAN ◽  
GEORGE B. RICHTER-ADDO
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Molecular Structures ◽  
Spectroscopic Methods ◽  
X Ray ◽  
X Ray Crystallography ◽  
High Yields ◽  
Solid State Structures

Para-aminosubstituted nitrosoarenes react with Ru ( CO )( OEP ) or [ Co ( TPP )( THF )2] SbF 6 (OEP2- = 2,3,7,8,12,13,17,18-octaethylporphyrinato dianion, TPP2- = 5,10,15,20-tetraphenylporphyrinato dianion) to generate Ru ( OEP )( ONC 6 H 4 NMe 2)2 and [ Co ( TPP )( ONC 6 H 4 NR 2)2] SbF 6 ( R = Me , Et ), respectively, in fair to high yields. These N -bound nitrosoarene complexes have been characterized by spectroscopic methods. The complexes Ru ( OEP )( ONC 6 H 4 NMe 2)2 and [ Co ( TPP )( ONC 6 H 4 NMe 2)2] ClO 4 have also been characterized by single-crystal X-ray crystallography. Their structures represent the first reported solid-state structures of Ru and Co porphyrins containing C-nitroso ligands.

Bis(1-phenyl-1-propyne) complexes of tungsten(II): crystal structures of [WI2(CO)(NCR)(η2-MeC2Ph)2] (R = Me, Et, or Ph)

2001 ◽  
Vol 79 (3) ◽  
pp. 263-271
Author(s):  
Paul K Baker ◽  
Michael GB Drew ◽  
Deborah S Evans
Keyword(s):  
Carbon Monoxide ◽  
Solid State ◽  
Crystal Structures ◽  
Octahedral Geometry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Alkyne Complexes ◽  
First Time

Reaction of [WI2(CO)3(NCMe)2] with two equivalents of 1-phenyl-1-propyne (MeC2Ph) in CH2Cl2, and in the absence of light, gave the bis(1-phenyl-1-propyne) complex [WI2(CO)(NCMe)(η2-MeC2Ph)2] (1) in 77% yield. Treatment of equimolar quantities of 1 and NCR (R = Et, i-Pr, t-Bu, Ph) in CH2Cl2 afforded the nitrile-exchanged products, [WI2(CO)(NCR)(η2-MeC2Ph)2] (2-5) (R = Et (2), i-Pr (3), t-Bu (4), Ph (5)). Complexes 1, 2, and 5 were structurally characterized by X-ray crystallography. All three structures have the same pseudo-octahedral geometry, with the equatorial sites being occupied by cis and parallel alkyne groups, which are trans to the cis-iodo groups. The trans carbon monoxide and acetonitrile ligands occupy the axial sites. In structures 1 and 2, the methyl and phenyl substituents of the 1-phenyl-1-propyne ligands are cis to each other, whereas for the bulkier NCPh complex (5), the methyl and phenyl groups are trans to one another. This is the first time that this arrangement has been observed in the solid state in bis(alkyne) complexes of this type.Key words: bis(1-phenyl-1-propyne), carbonyl, nitrile, diiodo, tungsten(II), crystal structures.

scholarly journals Revisiting the bis(dimethylamido) metallocene complexes of thorium and uranium: improved syntheses, structure, spectroscopy, and redox energetics of (C5Me5)2An(NMe2)2 (An = Th, U)

2017 ◽  
Vol 46 (34) ◽  
pp. 11208-11213 ◽  
Author(s):  
K. A. Erickson ◽  
B. D. Kagan ◽  
B. L. Scott ◽  
D. E. Morris ◽  
J. L. Kiplinger
Keyword(s):  
Solid State ◽  
Uv Visible ◽  
First Time ◽  
Solid State Structures ◽  
Metallocene Complexes

In addition to improved syntheses, the solid-state structures, voltammetric data and UV-visible–NIR spectra of (C5Me5)2An(NMe2)2 (An = Th, U) complexes are presented for the first time.

Antimicrobial Properties of Mono- and Di-fac-rhenium Tricarbonyl 2-Pyridyl-1,2,3-triazole Complexes

2016 ◽  
Vol 69 (5) ◽  
pp. 489 ◽  
Author(s):  
Sreedhar V. Kumar ◽  
Warrick K. C. Lo ◽  
Heather J. L. Brooks ◽  
Lyall R. Hanton ◽  
James D. Crowley
Keyword(s):  
Staphylococcus Aureus ◽  
Antimicrobial Properties ◽  
13C Nmr Spectroscopy ◽  
1H And 13C Nmr ◽  
X Ray Crystallography ◽  
The Family ◽  
Elemental Analyses ◽  
Solid State Structures ◽  
Rhenium Tricarbonyl

A family of mono- and di-fac-rhenium tricarbonyl 2-pyridyl-1,2,3-triazole complexes with different aliphatic and aromatic substituents was synthesized in good-to-excellent yields (46–99 %). The complexes were characterized by 1H and 13C NMR spectroscopy, infrared spectroscopy, electronic (UV-visible) spectroscopy, high-resolution electrospray mass spectrometry, and elemental analyses. In four examples, the solid-state structures of the rhenium(i) complexes were confirmed by X-ray crystallography. The family of the mono- and di-rhenium(i) complexes and the corresponding 2-pyridyl-1,2,3-triazole was tested for antimicrobial activity in vitro against both Gram-positive (Staphylococcus aureus) and Gram-negative (Escherichia coli) microorganisms. Agar-based disk diffusion assays indicated that most of the rhenium(i) complexes were active against Staphylococcus aureus and that the cationic rhenium(i) complexes were more active than the related neutral systems. However, in all cases, the minimum inhibitory concentrations for all the complexes were modest (i.e. 16–1024 µg mL–1).

scholarly journals Exploring the Self-Assembled Tacticity in Aurophilic Polymeric Arrangements of Diphosphanegold(I) Fluorothiolates

Molecules ◽  
2019 ◽  
Vol 24 (23) ◽  
pp. 4422 ◽  
Author(s):  
Moreno-Alcántar ◽  
Salazar ◽  
Romo-Islas ◽  
Flores-Álamo ◽  
Torrens
Keyword(s):  
Solid State ◽  
Self Assembly ◽  
Structural Diversity ◽  
Supramolecular Structures ◽  
X Ray Diffraction ◽  
Ligand Effects ◽  
Rational Control ◽  
Solid State Structures ◽  
Further Development ◽  
Aurophilic Interactions

Despite the recurrence of aurophilic interactions in the solid-state structures of gold(I) compounds, its rational control, modulation, and application in the generation of functional supramolecular structures is an area that requires further development. The ligand effects over the aurophilic-based supramolecular structures need to be better understood. This paper presents the supramolecular structural diversity of a series of new 1,3-bis(diphenylphosphane)propane (dppp) gold(I) fluorinated thiolates with the general formula [Au2(SRF)2(μ-dppp)] (SRF = SC6F5 (1); SC6HF4-4 (2); SC6H3(CF3)2-3,5 (3); SC6H4CF3-2 (4); SC6H4CF3-4 (5); SC6H3F2-3,4 (6); SC6H3F2-3,5 (7); SC6H4F-2 (8); SC6H4F-3 (9); SC6H4F-4 (10)). These compounds were synthesized and characterized, and six of their solid-state crystalline structures were determined using single-crystal X-ray diffraction. In the crystalline arrangement, they form aurophilic-bridged polymers. In these systems, the changes in the fluorination patterns of the thiolate ligands tune the aurophilic-induced self-assembly of the compounds causing tacticity and chiral differentiation of the monomers. This is an example of the use of ligand effects on the tune of the supramolecular association of gold complexes.

Synthesis and solid-state structures of gold(i) complexes of diphosphines

2016 ◽  
Vol 40 (7) ◽  
pp. 6467-6474 ◽  
Author(s):  
Sebastian Molitor ◽  
Christoph Mahler ◽  
Viktoria H. Gessner
Keyword(s):  
Solid State ◽  
Structure Formation ◽  
Gold Complexes ◽  
Solid State Structures ◽  
Aurophilic Interactions

A series of diphosphine bis(gold) complexes were synthesised and the importance of aurophilic interactions for their structure formation was studied.

Bismuth(III) Thiobenzoates and their Activity against Helicobacter pylori

2012 ◽  
Vol 65 (7) ◽  
pp. 883 ◽  
Author(s):  
Philip C. Andrews ◽  
Richard L. Ferrero ◽  
Peter C. Junk ◽  
Jonathan G. Maclellan ◽  
Roshani M. Peiris
Keyword(s):  
Helicobacter Pylori ◽  
Solid State ◽  
Minimum Inhibitory Concentration ◽  
Bactericidal Activity ◽  
Inhibitory Concentration ◽  
X Ray ◽  
X Ray Crystallography ◽  
Thiobenzoic Acid ◽  
High Level ◽  
Solid State Structures

Two new substituted thiobenzoic acids, m-nitrothiobenzoic and m-sulfothiobenzoic acid, and six (four new) homo- and heteroleptic bismuth(iii) compounds derived from thiobenzoic acid and substituted thiobenzoic acid have been synthesised and fully characterised using both solvent free and solvent mediated methods; Bi(SC(=O)C6H5)3 (3), PhBi(SC(=O)C6H5)2 (4), Ph2Bi(SC(=O)C6H5) (5), Bi(SC(=O)C6H4-m-NO2)3 (6), PhBi(SC(=O)C6H4-m-NO2)2 (7), and PhBi(SC(=O)C6H4-m-SO3) (8). The solid-state structures of the previously reported Bi(SC(=O)C6H5)3 (3) and PhBi(SC(=O)]C6H5)2 (4) complexes have now been confirmed by X-ray crystallography. In the solid-state complex 3 forms a column-like polymeric structure resembling stacked bowls through pyramidal intermolecular Bi–S3 bonds of distance 3.359 Å, providing a Bi(iii) centre with a nine coordinate environment. Complex 4 forms discrete tetrameric units cemented by long intermolecular Bi–S (3.774 Å), Bi–O(= C) (3.030, 3.071 Å) and Bi–C bonds (3.627 Å). The complexes were assessed for their activity against three strains of Helicobacter pylori and all show a minimum inhibitory concentration of 6.25 µg mL–1, indicating that the high level of bactericidal activity is insensitive to the degree of substitution at the Bi(iii) centre.

Atom Assignment in Solid-State Structures on the Basis of X-ray Crystallography and DFT Calculations – A Case Study on a Molecular Cu–Sb Alloy

2006 ◽  
Vol 2006 (6) ◽  
pp. 1127-1129 ◽  
Author(s):  
Reinhart Ahlrichs ◽  
Dieter Fenske ◽  
Alexander Rothenberger ◽  
Claudia Schrodt ◽  
Stephan Wieber
Keyword(s):  
Solid State ◽  
Dft Calculations ◽  
X Ray ◽  
X Ray Crystallography ◽  
Solid State Structures

Solid-State Structures oftrans-[RuCl2{Cl2PN(Me)N(Me)PCl2}2] andcis-[MCl2{Cl2PN(Me)N(Me)PCl2}] (M = PtIIand PdII) Studied by X-ray Crystallography and13C CPMAS NMR Spectroscopy

2007 ◽  
Vol 80 (9) ◽  
pp. 1776-1779 ◽  
Author(s):  
Satoshi Takara ◽  
Andrei S. Batsanov ◽  
Douglas J. Schaffer ◽  
Michael Takase ◽  
Janice A. Kunishige ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
X Ray ◽  
X Ray Crystallography ◽  
Solid State Structures
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