III Dihydrate

RESOLUTION OF POTASSIUM (ETHYLENEDUMINETETRA-ACETATO)COBALTATE(III) DIHYDRATE, K[Co(edta)] HjO 

Only one absorption band appears in the visible region (egig = 151), since the second d-d band is covered by a more intense charge-transfer band. 

Inorganic Syntheses, Volume XVIII Edited by Bodie E. Douglas Copyright 1978 by Jolni Wiley Sons, Inc. Ethylene(iiamine-N,N -Di acetic Acid Complexes ofCobalt(III) 103 

Submitted by LEON J. HALLORAN, ARLENE L. GILLIE, and J. IVAN LEGG Checked by PATRICK J. GARNETT, and DONALD W. WATTS  

Presented here are the synthesis and resolution of asym-cis- and sym-cis-[Co(edda)(en)], as well as the synthesis of Na[Co(edda)(C03)] (primarily the asym-cis-isomer) employed for the synthesis of ax w-c/x-[Co(edda)(en)]Cl. For the preparation of asym-cis complexes there is no advantage in obtaining pure asym-cis- [Co(edda)(C03)] , since some isomerization occurs during the displacement of the carbonate, necessitating subsequent separation of isomers. However, the two isomers of [Co(edda)(C03)] can be obtained readily by fractional crystallization. These synthetic, separation, and resolution procedures are generally useful for charged complexes, such as those of amino acids. 

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Sodium bis(L-cysteinato)chromate(III) dihydrate has been prepared by refluxing L-cysteine with chromium(III) nitrate and neutralizing the solution.1185. The product is a dark blue solid in which cysteine is coordinated with the sulfur atoms trans (see 252-254). A number of chloro and other complexes of cysteine and related amino acids have been studied.1186 A related complex L-histidinato-D-penicillaminatochromium(III) has been prepared11 7 and its crystal structure reported. 

F.A. Cotton et al., The crystal and molecular structure of dipotassium octachlorodirhenate(III) dihydrate, K2[Re2Cl8]2H20. Inorg. Chem. 4, 330-333 (1965)... 

POTASSIUM cw-[DIAQUABIS(OXALATO)CHROMATE(III)] DIHYDRATE AND POTASSIUM trans-[DIAQUABIS(OXAL ATO)-CHROMATE(III)] TRIHYDRATE... 

Gold(III) chloride (0 33m for gold). Dissolve 13 3 g sodium tetrachloro-aurate(III) dihydrate, NaAuCl4.2H20, in water and dilute to 100 ml. Alternatively, dissolve 6 57 g gold metal in 50 ml aqua regia, evaporate the solution to dryness, and dissolve the residue in 100 ml water. 

Figure 3.6 Structures of (a) [DyL3(H20)3] and (b) [TbL lHiOja] (HL = pivalic acid and HE = 2, 6-dihydoxybenzoic acid) [RE, black O, grey C, white H, omitted]. (Redrawn from the CIF files of M.L. Huang et al, Study on the synthesis and the structures of rare earth complexes with 4-aminobenzoic acid, Huaxue Yanjiu Yu Yingyong (Chinese) (Chemical Research Applications), 18, 245-251, 2006 [30] and T. Glowiak et al., Crystal structure of the isomorphous complexes tetraaquabis(2,6-dihydroxy-benzoato-0)(2,6-dihydroxy-benzoato-0, O)terbium(III) and hohnium(III)dihydrate, Journal of Coordination Chemistry, 48 (4), 477-486, 1999 [43].)...

Glowiak, T., Brzyska, W., Kula, A., and Rzaczynska, Z. (1999) Crystal structure of the isomorphous complexes tetraaquabis(2,6-dihydroxy-benzoato-0)(2,6-dihydroxy-benzoato-0,0)terbium(III) and holmium(III) dihydrate. Journal of Coordination Chemistry, 48 (4), 477 86. 

Cai, W.-X. (2007) Crystal structure of bis((pentaaqua)(4-nitrobenzoato-t0)bis(4-nitrobenzoato-/ 0,0/b)tris(m-4-nitrobenzoato-tO,0/c)-diyttrium(III)) dihydrate, Y4(H20)io(CvH4N04)i2- 2H2O. Zeitschrift filr Kristallo-graphie - New Crystal Structures, 222 (3), 219—221. 

The (-1-),(- -) diastereomer (—4.2 g) is suspended in 15 mL of water contained in a 30-mL beaker, and 4 mL of saturated potassium iodide solution is added gradually with constant stirring. The precipitated resolving agent ([0] = + 720°) is recovered (in yields as high as 3.5-4.0 g or 70-80%) by filtration and is washed with a few milliliters of potassium iodide solution. Potassium (-t-)-tris(oxalato)chromate(III) dihydrate is immediately precipitated as bluish-mauve crystals from the combined filtrate and washings by slow addition of ice-cold ethanol until precipitation appears almost complete (10-20 mL). The product is collected by filtration on a 5-cm Buchner funnel, washed successively with 5-mL portions of ice-cold 80% aqueous ethanol, 95% ethanol, acetone, and is then air dried. 

D. TRIS( 1,2-ETHANEDIAMINE)COBALT(III) cis-DICARBONATO-DICYANOCOBALTATE(III) DIHYDRATE... 

To a solution of 13.2 g (0.05 mole) of sodium cis,c/s-diamminecarbonato-dicyanocobaltate(III) dihydrate in 100 mL of water is added 25 mL of 30% perchloric acid dropwise in an ice-bath until the evolution of carbon dioxide ceases. To the resulting solution is added 18 g (0.10 mole) of potassium oxalate dihydrate, and the mixture is then stirred at 40° for four hours. The solution is filtered after neutralization with a 6 mole/L potassium hydroxide solution, and the filtrate is charged on an ion-exchange column containing Dowex 1-X8 resin in the Cr form (100-200 mesh, 4 cm x 30 cm). After the column has been washed with water, the elution is started with a 0.1 mole/L sodium chloride solution. Only one yellow band descends. The effluent is collected and concentrated to 10 mL, and then filtered to remove the deposited sodium chloride. After keeping the filtrate in a refrigerator, yellow crystals deposit. The crude product is recrystallized from the minimum amount of warm water ( 50°). The crystals are collected on a filter, washed with cold water, ethanol, and diethyl ether, and finally dried under vacuum. The yield is about 3 g. Anal. Calcd. for Na[Co(CN)2(ox)(NH3)2]-2H20 C, 16.45 H, 3.45 N, 19.18. Found C, 16.61 H, 3.37 N, 19.13. 

CoNOijPjRujCmHjo, Ruthenate(l -), trideca-carbonylcobalttri-, p.-nitrido-bis-(triphcnylphosphoms)(l +), 21 61 CoNAQ, Cobaltatc(III), bis(caibonato)-dicy-ano-, cis-, tris(l,2-ethanediamine)-cobalt(III), dihydrate, 23 66 CoNAQH, Cobaltate(lll), (1,2-... 

Potassium heptacyanotechnctate(III)-dihydrate, K4[Tc(CN)7j 2H2O, was synthesized by reaction of (Ml4)2[TcTf,] with KCN in refluxing aqueous methanol under exclusion... 

Sodium nitroferricyanide Sodium nitrosylpentacyanoferrate (III) dihydrate B.P., U.S.P. Nipride (Hofiinann-La Roche) Nitropress (Abbott). 

Spectroscopic measurements were used to support these assignments. Related studies of [Pg.2750]

The structure of blue crystals of sodium bis(L-cysteinate)chromium(III) dihydrate, 1, which formed from a neutral aqueous solution of chromium(III) nitrate and L-cysteine, was found to be a slightly distorted octahedron with the Cr bound to two carboxylate oxygens and two amino nitrogens (mutually cis) and to two sulfur atoms (trans). This complex was found to be subject to acid hydrolysis which caused rapid cleavage of the chromium-sulfur bond and resulted in formation of the red-violet complex, Cr(H20)2(L-cysteinate-0,N)2,... 

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