RESUMO
The content of ATP, ADP, AMP, sodium phosphate and sodium pyrophosphate were determined by 31P NMR, the linear range of ATP, ADP and AMP were found to be 0.004-0.080 mol x L(-1), sodium phosphate and sodium pyrophosphate were 0.005-0.100 mol x L(-1). The RSD were 0.40%-1.30%, the recovery were 96.9% - 105.2%. The method has been applied to the determination of ATP injection. The impurities of ATP injection were ADP and sodium phosphate. The content of ATP is in line with the requirement of the pharmacopoeia. The results indicated that the method is of good reproducibility, high accuracy, rapid and simple operation, without pretreatment and interference of other elements, 31P NMR is a new and reliable method of analyzing ATP, ADP, AMP and phosphate.
Assuntos
Difosfato de Adenosina/análise , Monofosfato de Adenosina/análise , Trifosfato de Adenosina/análise , Química Farmacêutica/métodos , Preparações Farmacêuticas/análise , Difosfatos/análise , Espectroscopia de Ressonância Magnética , Perfusão , Fosfatos/análise , Controle de Qualidade , Reprodutibilidade dos TestesRESUMO
In the title compound, C(14)H(10)N(6)O(2)S, the dihedral angle between the pyridine and triazole rings is 3.21â (10)°. The mol-ecule is significantly twisted about the N(t)-N(b) (t = triazole and b = benzyl-idene) bond [C-N(t)-N(b)=C = 151.64â (17)°]. In the crystal, mol-ecules are linked by weak N-Hâ¯N hydrogen bonds, generating C(8) chains propagating in [10[Formula: see text]].
RESUMO
The title compound, [Fe(2)(C(3)H(6)S(2))(C(18)H(15)P)(2)(CO)(4)], which might serve as an active-site model of [FeFe]-hydrogenase, contains two fused Fe/S/C/C/C/S six-membered rings, one of which has a chair conformation and the other a boat conformation. Each Fe atom is coordinated by two carbonyl ligands, a triphenyl-phosphane ligand and a bis-bidentate dithiol-ate ligand, and also forms an Fe-Fe bond [2.5167â (16)â Å]. Together, the six bonded atoms form a very distorted octa-hedral arrangement.
RESUMO
In the title solvated complex, [NiCl(2)(C(31)H(27)NP(2))]·CH(2)Cl(2), the Ni(2+) ion is coordinated by two chloride ions and two P atoms of the chelating N,N-bis-(diphenyl-phosphan-yl)benzyl ligand to generate a strongly distorted cis-NiCl(2)P(2) square-planar geometry for the metal ion. In the crystal, the components are linked by C-Hâ¯Cl inter-actions.
RESUMO
In the title complex, [NiCl(2)(C(27)H(27)NP(2))], the Ni(2+) ion is coordinated by two chloride ions and two P atoms of the bidentate N,N-bis-(diphenyl-phosphan-yl)propyl ligand to generate a strongly distorted cis-NiCl(2)P(2) square-planar geometry for the metal ion. A NiP(2)N rhombus occurs within the chelating ligand.
RESUMO
New C-functionalized propanedithiolate-type model complexes (1-8) have been synthesized by functional transformation reactions of the known complex [(mu-SCH2)2CH(OH)]Fe2(CO)6 (A). Treatment of A with the acylating agents PhC(O)Cl, 4-pyridinecarboxylic acid chloride, 2-furancarbonyl chloride, and 2-thiophenecarbonyl chloride in the presence of Et3N affords the expected C-functionalized complexes [(mu-SCH2)2CHO2CPh]Fe2(CO)6 (1), [(mu-SCH2)2CHO2CC5H4N-4]Fe2(CO)6 (2), [(mu-SCH2)2CHO2CC4H3O-2]Fe2(CO)6 (3), and [(mu-SCH2)2CHO2CC4H3S-2]Fe2(CO)6 (4). However, when A is treated with the phosphatizing agents Ph2PCl, PCl3 and PBr3, both C- and Fe-functionalized complexes [(mu-SCH2) 2CHOPPh2-eta1]Fe2(CO)5 (5), [(mu-SCH2) 2CHOPCl2-eta1]Fe2(CO)5 (6), and [(mu-SCH2) 2CHOPBr2-eta1]Fe2(CO)5 (7) are unexpectedly obtained via intramolecular CO substitution by P atoms of the initially formed phosphite complexes. The simplest C-functionalized model complex [(mu-SCH2) 2CO]Fe2(CO)6 (8) can be produced by oxidation of A with Dess-Martin reagent. While 8 is found to be an electrocatalyst for proton reduction to hydrogen, starting complex A can be prepared by another method involving the reaction of HC(OH)(CH2Br)2 with the in situ generated (mu-LiS) 2Fe2(CO)6. X-ray crystallographic studies reveal that the bridgehead C atom of 8 is double-bonded to an O atom to form a ketone functionality, whereas the bridgehead C atoms of A, 1, 3, and 4 are equatorially-bonded to their functionalities and those of 5-7 axially-bonded to their functionalities due to formation of the corresponding P-Fe bond-containing heterocycles.