532-31-0Relevant articles and documents
Palladium nitrosyl carboxylate complexes X-ray structures of Pd 4(μ-NO)2(μ-OCOCMe3)6
Stromnova, Tatiana A.,Paschenko, Denis V.,Boganova, Lyubov' I.,Daineko, Mikhail V.,Katser, Sergei B.,Churakov, Andrei V.,Kuz'mina, Lyudmila G.,Howard, Judith A.K.
, p. 283 - 288 (2003)
Two types of palladium nitrosyl carboxylate complexes were synthesized and their structures were characterized by several methods including an X-ray diffraction analysis. The tetranuclear complexes Pd4(μ-NO) 2(OCOR)6 (R=CMe3, Me, Ph, CHMe2, CH2Cl, IIa-e, respectively) were synthesized by the reaction of Pd(NO)Cl with silver carboxylates Ag(OCOR). The structure of IIa was determined by a single crystal X-ray diffractometry. Crystals of IIa are monoclinic, space group P21/n, a=12.104(7), b=23.970(8), c=15.495(4) A?, β=90.30(4)°, V=4496(4) A?3. The least-square structure refinement on F2 was converged to R=0.0714 for 6228 reflections [I>2σ(I)]. In IIa the palladium atoms form near regular rectangle Pd4, with the edges bridged by the ligands. Two bridging NO groups occupying the opposite sides of the rectangle are in the cis-positions with respect to the Pd4 plane. These groups are symmetric, with the Pd-N-O angles ranging from 120.4(5) to 121.8(5)°. The coordination polyhedrons of the Pd atoms are close to square planar ones. The reaction of the Pd4(CO)4(OCOCF3)4 clusters with nitrogen monoxide leads to a substitution of the carbonyl groups and formation of the low stable complex Pd4(NO)4(OCOCF3) 4 (III) that was characterized by the spectroscopic and analytical data. The transformation of III during slow recrystallization from toluene gives Pd3(NO)2(OCOCF3) 4·2C6H5Me (IV) and palladium black. The structure of IV was determined by an X-ray diffraction analysis. Crystals of IV are monoclinic, space group P21/n, a=9.2340(2), b=9.2859(2), c=18.0460(4) A?, β=92.339(1)°, V=1546.08(6) A?3. The least-square refinement on F2 was converged to R=0.0205 for 3209 reflections [I>2σ(I)]. In the linear tri-nuclear molecule of IV, any adjacent metal atoms are linked with a couple of the CF3CO 2 ligands and are separated by 3.0755(2) A?. Additionally, the terminal Pd atoms bear the NO and the η2-toluene ligands. The configuration of the N atoms corresponds to the ideal sp2- hybridization. The Pd-N-O angle is 117.2(2)°. The N atoms form short contacts with the aromatic rings. The distance between the center of the ring and the nitrogen atom is 2.70 A?. Complex IV is the first example of the Pd complex with the terminal nitrosyl ligand. The scheme of transformation of complex III to complex IV was proposed.
Synthesis, structures and antimicrobial activity of novel NHC?- and Ph3P-Ag(I)-Benzoate derivatives
O'Beirne, Cillian,Alhamad, Nada F.,Ma, Qinxi,Müller-Bunz, Helge,Kavanagh, Kevin,Butler, Geraldine,Zhu, Xiangming,Tacke, Matthias
, p. 294 - 303 (2019)
The rising threat of Antimicrobial Resistance (AMR) requires a novel approach to the treatment of infectious diseases. Covalently bonded silver, which has known antibacterial and antifungal properties and multiple mechanisms of action, may provide a treatment strategy when used alone or in combination with already known antimicrobial compounds. Here we describe the synthesis of eight novel silver(I) complexes, which were screened for in vitro activity against two pathogenic bacterial strains, Methicillin-resistant Staphylococcus aureus (MRSA) and Escherichia coli (E. coli), and against two pathogenic fungal strains, Candida albicans and Candida parapsilosis. Complexes 5–8 were synthesized by reacting triphenylphosphine in relative equivalents with the relevant silver benzoates (1, 2 & 4), whilst complexes 9–12 were synthesized by generation of a free carbene NHC? (1,3-dibenzyl-4,5-diphenyl-imidazol-2-ylidene) and reacting this with the silver benzoates 1–4, under Schlenk conditions. Complexes 9–12 showed the strongest antimicrobial activity, resulting in 50% inhibition of growth against MRSA and C. parapsilosis at concentrations of 12.5 and 3.25 μg/mL, respectively.
Nucleophilic Opening of the Oxirane Ring with Tetraalkylammonium Salt Anions in the Presence of Proton Donors
Bakhtin, S. G.,Bespalko, Yu. N.,Shved, E. N.,Sinelnikova, M. A.
, p. 524 - 531 (2021/06/02)
Abstract: The behavior of tetraethylammonium salts in nucleophilic opening of the oxirane ring of epichlorohydrin (ECH) in the system ECH–proton donor–Et4N+ X–, where proton donor is benzoic acid or 4-nitrophenol and X = PhCOO or NO3, was studied by the kinetic and spectrophotometric methods. The order of the reaction in tetraethylammonium salt, benzoic acid, and 4-nitrophenol was estimated as first, zero, and less than zero, respectively. The mechanism of nucleophilic opening of the oxirane ring of ECH was elucidated on the basis of monitoring of the accumulation of 4-nitrophenoxide ion in the system ECH–4-nitrophenol–Et4NX upon variation of the initial concentrations of both tetraethylammonium salt and proton donor (4-nitrophenol) itself. The anion X of the initial tetraethylammonium salt was found to be irreversibly consumed as a result of its attack on the oxirane ring with participation of the proton donor, which led to generation of tetraethylammo-nium 4-nitrophenoxide, and the latter catalyzed the subsequent formation of the final product. An increase in the concentration of 4-nitrophenol was accompanied by reduction of both the rate of formation of 4-nitrophenoxide ion and the overall reaction rate, which corresponds to a mechanism involving nucleophilic attack of the anion X on the oxirane ring that is not activated by the proton donor.
Synthesis, Structure and Catalytic Activity of NHC–AgICarboxylate Complexes
Wong, Valerie H. L.,Vummaleti, Sai V. C.,Cavallo, Luigi,White, Andrew J. P.,Nolan, Steven P.,Hii, King Kuok Mimi
supporting information, p. 13320 - 13327 (2016/09/09)
A general synthetic route was used to prepare 15 new N-heterocyclic carbene (NHC)–AgIcomplexes bearing anionic carboxylate ligands [Ag(NHC)(O2CR)], including a homologous series of complexes of sterically flexible ITent ligands, which permit a systematic spectroscopic and theoretical study of the structural and electronic features of these compounds. The complexes displayed a significant ligand-accelerated effect in the intramolecular cyclisation of propargylic amides to oxazolidines. The substrate scope is highly complementary to that previously achieved by NHC–Au and pyridyl–AgIcomplexes.
SALT AND PHOTORESIST COMPOSITION CONTAINING THE SAME
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, (2011/02/18)
A salt represented by the formula (I—Pb): wherein Xpb represents a single bond or —O—, Rpb represents a single bond etc., Ypb represents a polymerizable group, Zpb represents an organic group, Xpc represents a single bond or a C1-C4 alkylene group, and Rpc represents a C1-C10 aliphatic hydrocarbon group which can have one or more substituents etc.
Synthesis, crystal structure and characterization of two polymeric silver(I) complexes containing imidazolate anions
Liu, Xiu-Ying,Zhu, Hai-Liang
, p. 155 - 159 (2008/10/09)
Two new imidazolate-containing complexes, [Ag5(Im) 5]n (1) and [Ag(2-MeIm)]n (2), were prepared and characterized by X-ray single crystal structure determination. (1) consists of 1-D chains running along three different directions, namely [2 1 1], [2 1 1] and [2 1 1]. This type of packing of chains is unusual. The chains are linked to form a three-dimensional structure through weak Ag...Ag interactions. The silver(I) atom in each chain is linearly coordinated by two nitrogen atoms from different imidazolates and the 1-D chain is somewhat helical due to the geometrical constraints imposed by the 1,3-arrangement of the nitrogen atoms in the imidazolate bridges. (2) is a linear chain in which each silver(I) atom is two-coordinated with the different bridged methylimidazolate nitrogen atoms. The two structures were refined to R1 = 0.0315 for (1) and R1 = 0.0495 for (2). Complexes (1) and (2) are sparingly soluble and very stable in CH3CN containing 0.1 mol·L-1 of n-Bu 4NBF4 in the range 2.0 to -2.0 V at room temperature and do not undergo any redox process. When being boiled in a solution of 30% sodium hydroxide for two hours, the large colorless prismatic crystals of (1) and (2) remain unchanged. TG/DTG analyses shows that the two complexes begin to decompose at 382°C for (1) and 357°C for (2). Copyright
Aminopeptidase inhibitors
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, (2008/06/13)
Aminopeptidase inhibitory activity is exhibited by compounds having the formula STR1 wherein R1 is hydrogen, alkyl, carboxyalkyl, halo-substituted alkyl, hydroxyalkyl, aminoalkyl, mercaptoalkyl, alkylthioalkyl, (cycloalkyl)alkyl, (heteroaryl)alkyl, arylalkyl, carbamoylalkyl, guanidinylalkyl or heteroaryl; and R2 and R3 are each independently hydrogen, alkyl, cycloalkyl, hydroxyalkyl, aminoalkyl, aryl, arylalkyl, heteroaryl or heteroarylalkyl.
Preparation and substitution reactions of (diphosphine)platinum(II) carboxylate complexes
Anderson, Gordon K.,Lumetta, Gregg J.
, p. 1291 - 1295 (2008/10/08)
[Pt(OCOPh)2(dppe)] (dppe = 1,2-bis(diphenylphosphino)ethane), [Pt(mal)(dppe)] (mal = malonate), and [Pt(mal)(dppm)] (dppm = bis(diphenylphosphino)methane) are prepared by treatment of [PtCl2(dppe)] or [PtCl2(dppm)] with AgOCOPh or Ag2(mal). [Pt(OCOPh)2(dppe)] reacts with P-W-Bu3 to yield [Pt(OCOPh)(P-n-Bu3)(dppe)]+, which subsequently reacts with chlorinated solvents to produce [PtCl(P-n-Bu3)(dppe)]+. Analogously, [Pt(mal)(dppe)] gives [PtCl(L)(dppe)]+ when treated with P-n-Bu3, PEt3, or PMePh2. In the case of L = P-n-Bu3 the intermediate [Pt+(OCOCH2COO-)(P-n-Bu3)(dppe)] is observed spectroscopically at low temperature and may be protonated with HClO4. The ease of substitution of dicarboxylate or diphosphine ligands is investigated by allowing [Pt(O O)(P P)] (O O = C2O4, mal; P P = dppe, dppm) to react with P-n-Bu3. [Pt(mal)(dppm)] reacts with 2 molar equiv of P-n-Bu3 or PMePh2 to give ion-paired species of the form [Pt(L)2(dppm)][mal].
AMINOPEPTIDASE INHIBITORS
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, (2008/06/13)
Aminopeptidase inhibitory activity is exhibited by compounds having the formula STR1 and pharmaceutically acceptable salts thereof, wherein R. sub.1 and R 2 are each independently hydrogen, alkyl, carboxyalkyl, halo-substituted alkyl, hydroxyalkyl, aminoalkyl, mercaptoalkyl, alkylthioalkyl, (cycloalkyl)alkyl, (heteroaryl)alkyl, arylalkyl, carbamoylalkyl, guanidinylalkyl or heteroaryl;R 3 is hydrogen, alkyl, cycloalkyl, aryl, heteroaryl, arylalkyl, (heteroaryl) alkyl, STR2 R 4 and R 5 are each independently hydrogen, alkyl, cycloalkyl, aryl, heteroaryl, arylalkyl, or (heteroaryl) alkyl;A is glycyl, alanyl, leucyl, phenylalanyl, arginyl, sarcosyl, seryl, asparagyl, lysyl, glutamyl, histidyl, tryptophyl, cysteinyl, methionyl, threonyl, tyrosyl, valyl, aspartyl, prolyl, norleucyl, or norvalyl; andn is an integer of 1 to 6.
