Synthesis and structural systematics of ethane-1,2-dithiolato complexes

Rao, Ch. Pulla; Dorfman, Jay R.; Holm, R. H.

doi:10.1021/ic00224a011

Cited by 121 publications

(55 citation statements)

References 7 publications

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“…From the bond angles and distances in model compounds (30) and proteins with known tetrathiolate Cd(II) binding sites (31), the four sulfur ligands should be ϳ2.5 Å from the Cd(II) and 4.5 Å from each other. Cd K-edge x-ray absorption spectroscopy of the Cd(II)⅐CadC complex showed a distance of 2.53 Å between metal and sulfur atoms.…”

Section: Cross-linking Of Cadc Homodimers With Single and Double Cystmentioning

confidence: 99%

The Soft Metal Ion Binding Sites in theStaphylococcus aureus pI258 CadC Cd(II)/Pb(II)/Zn(II)-responsive Repressor Are Formed between Subunits of the Homodimer

Wong

Lin

Rosen

2002

Journal of Biological Chemistry

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Section: Cross-linking Of Cadc Homodimers With Single and Double Cystmentioning

confidence: 99%

The Soft Metal Ion Binding Sites in theStaphylococcus aureus pI258 CadC Cd(II)/Pb(II)/Zn(II)-responsive Repressor Are Formed between Subunits of the Homodimer

Wong

Lin

Rosen

2002

Journal of Biological Chemistry

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“…[7] Our new nickel-zinc complexes [Ni 2 (bsms) 3 -ZnBr 3 ] and [Ni 3 (xbsms) 2 (ZnBr 3 ) 2 ] are noticeably different from these earlier reported structures, and are also quite different from each other, as a result of dissociation of the didentate bsms ligand from part of the mononuclear complex and re-assembly to form a dinuclear core similar to that of the nickel ethanedithiolate compound [Ni 2 (edt) 3 ]. [30] The binding of the ZnBr 3 -group to one thiolate sulfur atom is similar to the binding observed in the dinuclear complex [Ni(N 2 S 2 )ZnCl 2 (dmf)]. [7] The proposed structure of the pentanuclear complex of general formula [Ni 3 (xbsms) 2 (ZnBr 3 ) 2 ] is based on the assumption of a similar binding of the ZnBr 3 -groups; binding at two sides of the trinuclear core is proposed for reasons of steric bulk and the existence of a symmetrical structure as indicated by NMR spectroscopy.…”

Section: Discussionmentioning

confidence: 99%

Nickel Thiolate Complexes as Ligands for Copper and Zinc: Novel Additions to a Library of Binding Modes

et al. 2006

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The reactivity of the two nickel complexes [Ni(xbsms)] and [Ni(bsms) 2 ] [H 2 xbsms = α,αЈ-bis(4-mercapto-3,3-dimethyl-2-thiabutyl)-o-xylene; Hbsms = 4-mercapto-3,3-dimethyl-1-phenyl-2-thiabutane] towards copper iodide and zinc bromide has been investigated. The reactions yield novel aggregates of higher nuclearity with topologies that are different from previous reports; the nickel complexes in all cases can be considered as didentate S ligands. The X-ray structure of the novel octanuclear cluster [{Ni(bsms) 2 } 3 (CuI) 5 ] shows a unique arrangement in which the cis-NiS 2 SЈ 2 units act as didentate ligands to a trigonal-bipyramidal array of five Cu I ions. The tetranuclear structure of [{Ni(xbsms)CuI} 2 ] shows unprecedented asymmetric bridging of the thiolate sulfur atoms, with one of the thiolate groups binding to one copper

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“…Watson, Rao, Dorfman & Holm, 1985;Rao, Dorfman & Holm, 1986;Snyder, Rao & Holm, 1986;Bianconi et ai., 1987;Vrtis, Rao, Warner & Lippard, 1988;Villacorta, Rao & Lippard, 1988). Selection and mounting of crystals are performed in a glove (dry) box maintained under an inert atmosphere such as nitrogen or argon.…”

Section: Methods Developedmentioning

confidence: 99%

Rationale of a quick adjustment method for crystal orientation in oscillation photography. Erratum

Suh¹,

Suh²,

Ko³

et al. 1989

J Appl Cryst

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We have developed the following methods and successfully applied them in the case of several highly air-sensitive inorganic and organometallic compounds without the use of a cold stream of nitrogen (e.g. Watson, Rao, Dorfman & Holm, 1985;Rao, Dorfman & Holm, 1986;Snyder, Rao & Holm, 1986; Bianconi et ai., 1987;Vrtis, Rao, Warner & Lippard, 1988;Villacorta, Rao & Lippard, 1988). Selection and mounting of crystals are performed in a glove (dry) box maintained under an inert atmosphere such as nitrogen or argon. While working, we found interesting ways of splitting multiple crystals (aggregates), sizing them to the required dimensions and also shaping them to minimize absorption effects, simply by rubbing these crystals gently on the gloves (inside the dry box) and/or rolling them in a small pool of solvent in which the compound is moderately soluble. While rubbing the crystals on the gloves, we were often able to differentiate powdered lumps from single crystals. This method overcomes the use of a microscope in the dry box. Satisfactory crystals are loaded into Lindemann-glass capillaries of appropriate size and wedged into the narrow portion, often with a light touch of apeizon grease that is free from heavy elements. Application of the apeizon grease not only ensures the position of the crystal in the capillary (free from wobbling), but also provides extra protection from deterioration by unidentified means through the formation of a thin film on the crystal. Crystals losing solvent of crystallization and/or becoming opaque outside the mother liquor are coated with a thin film of '5-minute' epoxy resin. Of course, in this case apeizon grease is not required. The open ends of these loaded capillaries, normally cup portions, are plugged with vacuum grease or candle wax before being brought out of the glove box. Immediately after they are brought out, these are sealed in a fine flame. Subsequently, selection of good crystals suitable for X-ray diffraction is done by examining these sealed capillaries under a microscope, preferably in polarized light.This method has worked successfully for a large number of very air-sensitive and thermal-insensitive (at ambient temperatures) compounds and yields good X-ray diffraction data at minimum cost, besides providing convenient and easy handling techniques. No cold stream of liquid nitrogen has been used in this process. These methods are, in fact, applied routinely in our laboratories to handle highly airsensitive compounds and to collect their X-ray diffraction intensities. It is conceivable that this method will provide single crystals of air-sensitive compounds suitable not only for X-ray diffraction studies but also for other physicochemical measurements. AbstractSWATAB is a Fortran IV computer program which helps in obtaining most of the required tables for crystal structure publication from the widely used SHELX76 program output. The strategy, installation, required local modifications, merits and limitations are discussed.

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Synthesis and structural systematics of ethane-1,2-dithiolato complexes

Cited by 121 publications

References 7 publications

The Soft Metal Ion Binding Sites in theStaphylococcus aureus pI258 CadC Cd(II)/Pb(II)/Zn(II)-responsive Repressor Are Formed between Subunits of the Homodimer

The Soft Metal Ion Binding Sites in theStaphylococcus aureus pI258 CadC Cd(II)/Pb(II)/Zn(II)-responsive Repressor Are Formed between Subunits of the Homodimer

Nickel Thiolate Complexes as Ligands for Copper and Zinc: Novel Additions to a Library of Binding Modes

Rationale of a quick adjustment method for crystal orientation in oscillation photography. Erratum

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