Coordination compounds of substituted 1,10-phenanthrolines and related bipyridyls. XI. Physicochemical study of complexes of copper(II) and 2-Methyl-1,10-phenanthroline

1970 ◽  
Vol 23 (4) ◽  
pp. 691 ◽  
Author(s):  
EW Ainscough ◽  
RA Plowman
Keyword(s):  
Organic Solvents ◽  
Infrared Spectra ◽  
Coordination Compounds ◽  
Water Solution ◽  
Sodium Perchlorate ◽  
Copper Nitrate ◽  
Visible Absorption ◽  
Magnetic Susceptibilities ◽  
Excess Copper ◽  
Donor Nitrogen

Solutions of 2-methyl-1,10-phenanthroline (rnep) with excess copper(II) salts in organic solvents yielded complexes of the formula Cu(mep)X2 (X = NO3, Cl, Br, I). These were non-electrolytes in nitrobenzene. When excess rnep was present bis- complexes of the type Cu(mep)2Cl2,6H2O, Cu(mep)2/sub>(NO3)2,H2O, and hydrated forms of the type Cu(mep)2XClO4 (X = Cl, NO3) were obtained. These were 1 : 1 electrolytes in nitrobenzene and the copper(II) ion was at least five-coordinated with the donor nitrogen atoms taking up a flattened tetrahedral arrangement. Hydrated copper(II) perchlorate with rnep in a 1 : 2 or 1 : 1 ratio yielded Cu(mep)2(ClO4)2,2H2O which is a 2 : 1 electrolyte in nitrobenzene. From a water solution of copper nitrate and rnep in the ratio 1 : 3.5, a complex Cu(mep)3(ClO>sub>4)2 precipitated upon the addition of a sodium perchlorate solution. I t was thought previously that this compound did not exist. The magnetic susceptibilities, the conductivities, and the visible, absorption, and infrared spectra of some rnep complexes have been obtained and structures are proposed from this information.

Coordination Compounds of Substituted 1,lO-Phenanthrolines and Related Dipyridyls. IV. Physicochemical Study of Complexes of Copper and 2,9-Dimethyl-1,10-phenanthroline

1963 ◽  
Vol 16 (1) ◽  
pp. 34 ◽  
Author(s):  
JR Hall ◽  
NK Marchant ◽  
RA Plowman
Keyword(s):  
Organic Solvents ◽  
Infrared Spectra ◽  
Copper Atom ◽  
Coordination Compounds ◽  
Magnetic Moments ◽  
Physicochemical Study ◽  
Magnetic Susceptibilities ◽  
Donor Nitrogen ◽  
Substituted 1

The magnetic susceptibilities, conductivities, and infrared spectra of some complexes of copper and 2,9-dimethyl-1,10-phenanthroline (dmp) have been obtained. The magnetic moments of the copper(II) compounds lie in the range 1.9 to 2.0 B.M. Complexes of formula CudmpX2, where X = NO3, Cl, and Br, are nonelectrolytes in nitrobenzene. The substances Cu(dmp)2X2H2O and hydrated forms of the compounds Cu(dmp)2XClO4, where X = NO3, Cl, and Br behave as 1 : 1 electrolytes. The copper(II) ion in the bis complexes is at least five-coordinate and it is proposed that the donor nitrogen atoms take up a flattened tetrahedral arrangement. The complexes of formula Cu(dmp)2X, where X = NO3, ClO4, Cl, Br. I, and I3 are diamagnetic solids, 1 : 1 electrolytes in nitrobenzene, and are expected to have a tetrahedral arrangement of the four donor nitrogen atoms about the copper atom. The mono complexes CudmpX, where X = Cl, Br, and I are diamagnetic, practically insoluble in organic solvents, and probably dimeric with a tetrahedral arrangement of the ligand donor atoms.

Coordination compounds of substituted 1,10-Phenanthrolines and related dipyridyls. VIII. Complexes of silver and 2,9-Dimethyl-1,10-phenanthroline

1965 ◽  
Vol 18 (9) ◽  
pp. 1345 ◽  
Author(s):  
JR Hall ◽  
RA Plowman ◽  
HS Preston
Keyword(s):  
Aqueous Solutions ◽  
Organic Solvents ◽  
Infrared Spectra ◽  
Coordination Compounds ◽  
Molecular Weights ◽  
Low Solubility ◽  
Covalently Bound

Addition of 2,9-dimethyl-1,10-phenanthroline (dmp) in organic solvents to aqueous solutions of silver(1) salts yielded mono complexes represented by AgXdmp, where X = NO3, Cl, Br, I; 2X = SO4, and bis complexes Ag(dmp),Y, where Y = NO3, Cl04. Water of crystallization was present only in the sulphate. The mono complexes were empirically three-coordinate. Low solubility prevented the determination of molecular weights. Infrared spectra indicated that the polyatomic anions were covalently bound. The 1 : 1 electrolyte [Ag(dmp)(py)]ClO4 subsequently prepared seemed to be an example of three-coordination. The bis complexes were 1 : 1 electrolytes in nitrobenzene and were most likely tetrahedral.

COORDINATION COMPOUNDS OF HYDRAZINE: PART III. THE INTERACTION OF SILICON TETRAFLUORIDE WITH HYDRAZINE

1963 ◽  
Vol 41 (4) ◽  
pp. 876-882 ◽  
Author(s):  
R. C. Aggarwal ◽  
M. Onyszchuk
Keyword(s):  
Hydrogen Chloride ◽  
Organic Solvents ◽  
Infrared Spectra ◽  
Hydrofluoric Acid ◽  
Coordination Compounds ◽  
Boron Trifluoride ◽  
Silicon Tetrafluoride ◽  
Volatile Solid ◽  
Octahedral Structure

Silicon tetrafluoride and hydrazine react in a vacuum to produce a white, non-volatile, solid, 1:2 complex, SiF4.2N2H4. This compound sublimes with decomposition above 200° and is insoluble in common organic solvents. It reacts with (a) 55% hydrofluoric acid, (b) anhydrous hydrogen chloride, (c) ethylenediamine, (d) ammonia, and (e) boron trifluoride, producing: (a) (N2H5+)2SiF62−, (b) N2H5+Cl−, (c) SiF4.NH2(CH2)2NH2, (d) SiF4.2NH3, and (e) BF3.N2H4. A comparison of the infrared spectra of SiF4.2NH3, SiF4.2N2H4, and SiF4.NH2(CH2)2NH2 suggests that all three complexes have cis octahedral structure.

Coordination compounds of substituted 1,10-Phenanthrolines and related dipyridyls. V. Complexes of cobalt and 2,9-Dimethyl-1,10-phenanthroline

1965 ◽  
Vol 18 (5) ◽  
pp. 691 ◽  
Author(s):  
DB Fox ◽  
JR Hall ◽  
RA Plowman
Keyword(s):  
Absorption Spectra ◽  
Infrared Spectra ◽  
Coordination Compounds ◽  
Magnetic Moments ◽  
Visible Absorption

A series of complexes of cobalt(II) and 2,9-dimethyl-1,10-phenanthroline (dmp) has been prepared. Complexes of formula CoX2dmp (X = Cl, Br, I, KCS) are monomeric in acetone and camphor and non-electrolytes in nitrobenzene and nitromethane. The magnetic moments and visible absorption spectra favour the assignment of tetrahedral stereochemistry about the Co atom. Complexes containing 2 moles dmp per Co appear to have octahedral arrangements of ligands about the Co atom. These are of the type [CoNO3(H2O)dmp2]X, (X = NO3, ClO4, BPh4) and Co(NCS)2dmp2. The magnetic moments, visible and infrared spectra, and conductances in nitrobenzene and nitromethane support this conclusion. With other mono-dmp complexes (CoX2dmp, X = NO3, �SO4) and bis-dmp complexes {CoXdmp,ClO4,H2O (X = Cl, Br) ; Codmp2(ClO4)2}, stereochemical assignments could not be made.

Impurities in Commercial Saccharin. I. Impurities Soluble in Organic Solvents

1976 ◽  
Vol 59 (5) ◽  
pp. 1051-1058 ◽  
Author(s):  
Bozidar Stavrić ◽  
Raymond Klassen ◽  
W Arnold
Keyword(s):  
Organic Solvents ◽  
Water Solution ◽  
Water Soluble ◽  
Chromatographic Column ◽  
Gas Liquid Chromatography ◽  
Sodium Saccharin ◽  
Chemical Purity ◽  
Liquid Chromatographic ◽  
Chloroform Methanol ◽  
Sodium Form

Abstract Thirteen saccharin samples used for carcinogenicity tests in animals in various laboratories were analyzed for their chemical purity. Although most of the impurities were water-soluble, some were mainly soluble in organic solvents. These impurities were extracted with chloroform-methanol from a water solution of sodium saccharin. Samples obtained as acid-saccharin were converted to the sodium form before extraction. The major impurity in commercial saccharin, o-toluenesulfonamide, was also soluble in this system. Impurities were separated by gas-liquid chromatography of the underivatized, concentrated extract. Eleven major, well separated peaks were collected from the gas chromatographic column and identified by mass spectroscopy. Some of the peaks were compared with known standards. Qualitative and quantitative differences in impurities were observed among different saccharin samples. The identified impurities (in order of appearance from the gas-liquid chromatographic column) were as follows: o-toluenesulfonamide; p-toluenesufonamide; 1,2-benzisothiazole 1,1-dioxide; 1,2-benzisothiazoline 1,1-dioxide; diphenylsulfone; o,o′-ditolylsulfone; o,m′-ditolylsulfone, o,p′-ditolylsulfone; m,p′-ditolylsulfone; p,p′-ditolylsulfone, and tetracosane.

Coordination compounds of substituted 1,10-Phenanthrolines and related dipyridyls. VII. Complexes of copper(I) and 4,6,4',6'-Tetramethyl-2,2'-bipyridine

1965 ◽  
Vol 18 (9) ◽  
pp. 1339 ◽  
Author(s):  
JR Hall ◽  
MR Litzow ◽  
RA Plowman
Keyword(s):  
Solid State ◽  
Physical Properties ◽  
Copper Atom ◽  
Coordination Compounds ◽  
Donor Nitrogen ◽  
Partial Dissociation

A number of diamagnetic complexes of copper(I) and 4,6,4',6'-tetramethyl-2,2'-bipyridine (tmb) have been prepared and some physical properties measured. The complexes of formula Cu(tmb)2X where X = NO3, ClO4, Br, and I behave as 1 : 1 electrolytes in nitrobenzene and nitromethane, while the complex Cu(tmb)2Cl,H2O apparently undergoes partial dissociation in these solvents. All are expected to have a tetrahedral arrangement of the four donor nitrogen atoms about the copper atom. The mono complexes CuXtmb, where X = Cl, Br, and I, appear to be dimeric in the solid state with halogen bridging, but in solution the chloro and bromo complexes rearrange to varying degrees depending on the solvent, forming the salt-type compounds [Cu(tmb)2][CuX2]. CuItmb is insoluble in all common solvents.

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