Bis(ethanamidinium) (1,10-phen-an-thro-line-2,9-dicarboxyl-ato)manganate(II) hepta-hydrate.

In the title complex, (C2H7N2)2[Mn(C14H6N2O4)2]·7H2O, the Mn(II) atom is coordinated by four N atoms and four O atoms from two 1,10-phenanthroline-2,9-dicarboxyl-ate ligands in a distorted dodeca-hedral geometry. The double negative charge is balanced by two ethanamidinium cations. A three-dimensional supra-molecular structure is formed through N-H⋯O and O-H⋯O hydrogen bonds and π-π stacking inter-actions [centroid-centroid distance = 3.553 (2) Å].

[Emulsion liquid membrane extraction with D2EHPA mobile carrier Hirudinaria manillensis hirudin in experimental study].

OBJECTIVE: To study the extraction system of hirudin emulsion liquid membrane with the Poecilobdella manillensis as raw material, di-(2-ethylhexyl) phosphate (D2EHPA) as carrier, Span 80 as emulsifier, octane and D2EHPA mixed to constitute membrane solution, diluted HCl solutions as internal aqueous phase. METHOD: Using the orthogonal experiment to optimize the extraction conditions of hirudin reference substance such as membrane phase, internal aqueous phase volume ratio (MIPVR), external aqueous phase pH, internal aqueous phase pH, mobile carrier concentration and so on, and then using hirudin crude extracts to do purifying experiment, and gaining experimental samples. RESULT: The optimal conditions of hirudin extraction were as follows: MIPVR 10: 3, internal aqueous phase pH 2.6, external aqueous phase pH 3.4, the mass fraction of carrier D2EHPA 2%. In the optimal extraction conditions, when the initial concentration of hirudin was one anti-thrombin activity units (ATU) x mL(-1), ATU recovery rate of the reference substance was 83.06%. In the purifying experiment of crude extracts, ATU recovery rate was 82.99%, and the specific activity of sample was 3 289.48 the ATU x mg(-1). Discontinuous polyacrylamide gel electrophoresis and spectral scanning, the results showed that the purity and reference substance were considerable. CONCLUSION: The method of preparation hirudin was relatively simple, the purity of the experimental samples and ATU recovery were both high.

Two novel Dy8 and Dy11 clusters with cubane [Dy4(µ3-OH)4]8+ units exhibiting slow magnetic relaxation behaviour.

Two unique octa- and hendeca-nuclear dysprosium(III) clusters incorporating [Dy(4)(µ(3)-OH)(4)](8+) cubane units have been synthesized with the 1,10-phenanthroline-2,9-dicarbaldehyde dioxime (H(2)phendox) ligand and DyCl(3)·6H(2)O or Dy(OAc)(3)·4H(2)O. They are [Dy(8)(OH)(8)(phendox)(6)(H(2)O)(8)]Cl(2)(OH)(2)·18H(2)O·18MeOH (1) and [Dy(11)(OH)(11)(phendox)(6)(phenda)(3)(OAc)(3)](OH)·40H(2)O·7MeOH (2). Adjacent Dy(8) in 1 or Dy(11) in 2 motifs are packed by off-set π-π interactions of the aromatic rings on phendox(2-) to generate a 3D supramolecular architecture in the honeycomb topology and with 1D or 3D channels along the c-axis. Adsorption research shows that complex 1 has selective adsorption ability for H(2)O over small gas molecules (H(2), N(2), CO(2)). Complex 2 is stable upon the removal of guest molecules and the desolvated compound absorbed a considerable amount of CO(2). Furthermore, the oximes underwent hydrolysis to carboxylic acid and the resulting 1,10-phenanthroline-2,9-dicarboxylate link the dysprosium atoms to form a hendecanuclear cluster of 2. Magnetic studies reveal that both clusters exhibit slow magnetic relaxation behavior, expanding upon the recent reports of the pure 4f type single-molecule magnets (SMMs).

Synthesis, structures, adsorption behaviour and magnetic properties of a new family of polynuclear iron clusters.

Solvothermal reactions of 1,10-phenanthroline-2,9-dicarbaldehyde dioxime (H(2)phendox) with FeCl(3)·6H(2)O or FeBr(3) under solvothermal conditions yielded two trinuclear iron(III) clusters [Fe(III)(3)(mu(3)-O)(phendox)(3)]X·14H(2)O (X = Cl 1·14H(2)O, Br 2·14H(2)O) and three hexanuclear iron(III) and iron(II) clusters, [Fe(III)(6)(mu(4)-O)(2)(MeO)(6)X(4)(phendox)(2)]·MeOH (X = Cl , Br 4) and (H(3)O)[Fe(II)(6)(mu(6)-Cl)(phenda)(6)]·6H(2)O (5·6H(2)O). The phendox(2-) ligand is very useful in constructing magnetically active and stable high-nuclearity metal clusters in that the phenanthroline rings and the oxime nitrogen atoms grasp the metal ions tightly while the two oxygen atoms on the oximates can link other metal centres in the shortest pairwise magnetic exchange pathway. Adjacent Fe(3)(mu(3)-O)(phendox)(3)(+) motifs in 1 and 2 are packed by off-set pi-pi interactions of the aromatic rings on phendox(2-) to generate a 3D supramolecular architecture in the honeycomb topology and with 1D hexagonal channels in the dimension of 13 x 13 Å along the c-axis. 2 is stable upon the removal of guest molecules and the desolvated compound absorbed considerable amount of N(2), CO(2) and H(2). 3 and 4 are isostructural. Two mu(4)-O(2-) and two phendox(2-) units link four metal atoms into a coplanar butterfly-shaped unit with the mu(4)-O(2-) slightly above and below the plane (+/-0.264 Å). The other two Fe(III) ions are capped on the alternate planes via the three bridging mu(2)-methoxides and accordingly form an unprecedented hexanuclear Fe(III) cluster. Furthermore, the oximes underwent hydrolysis to yield carboxylate groups and the resulted 1,10-phenanthroline-2,9-dicarboxylate link the iron atoms to form a hexanuclear cluster of 5. Magnetic studies show that the antiferromagnetic interactions are present in the Fe(3)O core of 2 and in the (mu(6)-Cl)Fe(6)(mu-O)(12) core of 5.

Aqua-chlorido(4-methyl-benzoato-κO)(1,10-phenanthroline-κN,N')copper(II).

In the title mononuclear complex, [Cu(C(8)H(7)O(2))Cl(C(12)H(8)N(2))(H(2)O)], the Cu(II) atom is coordinated by one carboxylate O atom from a monodentate 4-methyl-benzoate ligand, two N atoms from the 1,10-phenanthroline ligand, one chloride ion and one water mol-ecule in a square-pyramidal geometry. The crystal structure exhibits inter- and intra-molecular C-H⋯Cl, C-H⋯O, O-H⋯Cl and O-H⋯O hydrogen bonds, as well as C-H⋯π inter-actions of phenanthroline and methyl H atoms towards the π-systems of neighboring 4-methyl-benzoate units and the pyridine rings of the phenanthroline system [centroid-centroid distances are 2.706 (2) and 2.992 (1) Å, respectively].