X-ray Crystal Structure Of Bis Research Articles

Organomercury Compounds. XXXI. Preparations and 199Hg N.M.R. Spectra of Organomercury Derivatives of 2-Phenylpyridine, Benzo[h]quinoline, 1-Phenylpyrazole and 3,4,5-Trimethyl-1-phenylpyrazole, and the X-Ray Crystal Structure of Bis[2-(pyridin-2'-yl)phenyl]mercury

2-(Pyridin-2'-yl) phenylmercuric acetate has been prepared by mercuration of 2-phenylpyridine. Symmetrization of the corresponding chloride by alkaline sodium stannite gave bis [2-(pyridin-2'-yl)phenyl]mercury, which was also prepared from 2-(2'-aminophenyl)pyridine by the diazo method and treatment of the initial product with copper powder and aqueous ammonia. Mercuration of benzo [h] quinoline and 3,4,5-trimethyl-1-phenylpyrazole with mercuric acetate followed by treatment with lithium chloride yielded benzo [h]quinolin-10-ylmercuric chloride and 2-(3',4',5'-trimethylpyrazol-1'-yl) phenylmercuric chloride respectively. Treatment of the former product with tribromide ions gave 10-bromobenzo[h] quinoline. The exchange Grignard reaction between 1-phenylpyrazole and ethylmagnesium bromide to give 2-(pyrazol-1'-yl) phenylmagnesium bromide has been monitored by reactions with benzonitrile and D2O to establish optimum conditions for reaction with mercuric bromide giving bis [2-(pyrazol-1'-yl)phenyl]mercury. The 199Hg n.m.r. chemical shifts of the majority of mercurials are shifted substantially downfield relative to the corresponding simple phenylmercurials consistent with weak intramolecular coordination by the heterocyclic nitrogen donor atoms, but a small upfield shift is observed for bis [2-(pyrazol-1'-yl)phenyl]mercury. The X-ray crystal structure of bis [2-(pyridin-2′-yl)phenyl]mercury [monoclinic, space group P21/n, a 12.746(2), b 11.660(2), c 5.698(1) Ǻ, β 92.81(1)′, V 845.8 Ǻ3] shows a centrosymmetric molecule with strong linear two coordination [Hg-C 2.098(8) Ǻ; C-Hg-C 180.0°] and significant but much weaker Hg-N interactions [Hg-N 2.798(7) Ǻ; N-Hg-N 180.0°] giving overall distorted square planar stereochemistry. The phenyl rings are mutually coplanar, whilst the two pyridin-2'-yl rings are parallel and inclined at 10.8° to the phenyl groups.

Phospholyl (phosphacyclopentadienyl) and arsolyl (arsacyclopentadienyl) complexes of ytterbium(II) and samarium(II). Synthetic, structural and multinuclear ( 31P and 171Yb) NMR studies

Bis(η 5-phospholyl) or bis (η 5-arsolyl)M(THF) 2 complexes, where M = Sm or Yb, can be obtained either by reaction of potassium phospholides or arsolides with MI 2(THF) 2 or by cleavage of the PP or AsAs bond of a biphospholyl or biarsolyl by ytterbium or samarium metal powders. The THF molecules that coordinate to the metal are labile when the ligands are 2,3,4,5-tetramethylphospholyl or arsolyl, but not when they are 2,5-diphenylphospholyl. An X-ray crystal structure of bis(η 5-2,5-diphenylphospholyl)Yb (THF) 2 is presnted. 171Yb and 31P NMR studies reveal that exchange of ligands is occurring in bis(η 5-2,3,4,5-tetramethylphospholyl)Yb(THF) 2; this exchange is slow at room temperature and frozen at −20°C. For bis(η 5-2,5-phenyldiphenylphospholyl)Yb(THF) 2 31P NMR data suggest that no exchange is occurring at room temperature.

Structural chemistry of organotin carboxylates: XVIII. Synthesis, characterization and X-ray crystal structure of bis(μ-hydroxo)-bis[di-t-butyltin(IV)acetate]: [ tBu 2Sn(O 2CCH 3)(μ-OH)] 2

Base hydrolysis of [ 1Bu 2Sn(O 2CCH 3) 2] yields [ 1Bu 2Sn(O 2CCH 3)(μ-OH)] 2, which can also be prepared by the reaction of [ 1Bu 2Sno] 3 with acetic acid in 1:1 stoichiometry in benzene. The crystal structure of [ tBu 2Sn(O 2CCH 3)(μ-OH)] 2 shows the presence of asymmetrically bridging hydroxy groups leading to a planar Sn 2O 2 unit, SnO(1) 2.046(2) and SnO(1′) 2.204(2) Å. Each Sn atom is also coordinated by an O atom of a monodentate carboxylate ligand (SnO(2) 2.156 (2) Å) and two C atoms of the 1Bu groups so that the Sn environment is based on a trigonal bipyramid.

Complexes of structural analogues of terpyridyl with iron and zinc; the x-ray crystal structure of bis[2,6-bis(benzimidazol2-yl)pyridine]iron(II) trifluoromethylsulphonate bis-ethanol solvate

Complexes of iron(II) and zinc(II) with a series of tridentate ligands of the type [2,6-bis(benz-X-azol-2-yl)pyridine] (X = imid, thi, ox) have been prepared. The crystal structure of [Fe(2,6-bis(benzimidazol-2-yl)pyridine) 2](CF 3SO 3) 2·2C 2H 5OH shows the iron(II) to be low spin with a meridional octahedral coordination by two tridentate ligands. 57Fe Mössbauer spectra of the complexes [FeL 2] 2+ show strong dependence of ligand strength on the non-coordinated heteroatom, X, of the ligand: benzimidazole ligands give low spin complexes, benzoxazoles give high spin complexes and benzthiazoles show spin-crossover properties. Derivatization of the imidazole nitrogen has only a small effect on the ligand strength. The complexes [FeLX 2] (X = anion) are all high spin. Partial dissociation is observed in solvents with a strong affinity for iron(II); the iron(II) complexes show metal-to-ligand charge transfer transitions whose intensity depends strongly on the spin state of the iron.

Complexes of copper(II) and nickel(II) with the new ligand N-[2-(3-ethyl-indole)]pyridoxaldimine. X-ray crystal structure of bis{N-[2-(3-ethyl-indole)]pyridoxaldiminate}nickel(II)

The monoanionic bidentate ligand N-[2-(3-ethyl-indole)]pyridoxaldimine prepared by 1:1 Schiff-base condensation of 3-(2-amino-ethyl)indole (tryptamine, TPA) with [3-hydroxy-5-(hydroxy-methyl)-2-methyl-4-pyridinecarboxaldehyde] (pyridoxal, pyrdox) and three different copper complexes are reported. The nickel(II) compound with the same ligand is also studied. All complexes were characterized by IR, UVvis and 1H NMR spectra, magnetic measurements and thermoanalytical data. A single-crystal of the nickel complex was subjected to X-ray diffraction analysis. The coordination of the nickel(II) complex is trans planar (NiN 2O 2) with NiO and NiN bond lengths of 1.841(l) and 1.926(2) Å, respectively. The spectroscopic data for the copper(II) complexes suggest the same chromophore group (CuN 2O 2) with a trans configuration in the solid phase for all. Finally, the dehydration reaction Cu(pyrdoxTPA) 2· yH 2O(s) → Cu(pyrdoxTPA) 2(s) + yH 2O(g) for the two copper complexes is studied.

(2-Methylthio-3-Pyridinecarboxylato)-diethyltin and -di-n-butyltin compounds: synthesis, spectroscopic characterization and in vitro antitumour activity. X-ray crystal structure of bis[diethyl(2-methylthio-3-Pyridinecarboxylato)tin] oxide and of diethyltin bis(2-methylthio-3-pyridinecarboxylate)

The X-ray crystal structures of [diethyl(2-methylthio-3-pyridinecarboxylato)tin] oxide (1a) and diethyltin bis(2-methylthio-3-pyridinecarboxylate) (1b) were determined. Compound 1a is a centrosymmetric dimer with two distinct types of carboxylate moieties and tin atoms with trigonal bipyramidal geometries. Compound 1b is monomeric with a six-coordinate tin atom and two equivalent carboxylate groups chelating the tin atom. Compounds 2a and 2b, the di-n-butyl analogues of 1a and 1b, have also been synthesized and characterized spectroscopically. The in vitro activity of compounds 2b and 2a against the human tumour cell line WiDr, a colon carcinoma, is better than that of cis-platin and doxorubicin. They are much less active than doxorubicin against MCF-7, a mammary tumour cell line. Compound 1b is inactive.

Reaction of 1,1′-diacetylferrocene with hydrazine hydrate: Synthesis and X-ray crystal structures of bis(hydrazine)bis(hydrazinecarboxylato-N′,O)iron(II), [Fe(N 2H 4) 2(O 2CNHNH 2) 2], and the cyclic biferrocene diazine, [N(Me)CC 5H 4FeC 5H 4C(Me)N] 2

1,1′-Diacetylferrocene reacts with neat hydrate over a period of 72 h at 20°C to give the dihydrazone [H 2NN(Me)CC 5H 4FeC 5H 4C(Me)NNH 2] ( 6) in almost quantitative yield. Either prolonging the reaction time or reacting 6 with fresh hydrazine causes the iron to be stripped from the metallocene and bis(hydrazine)bis(hydrazinecarboxylato-N′,O) iron(II), [Fe(N 2H 4) 2(OOCNHNH 2) 2] ( 11), crystallizes. In the presence of Ba 2+ or Mo 2+ ions two molecules of complex 6 react to give the cyclic diazine [N(Me)CC 5H 4FeC 5H 4C (Me)N] 2 ( 7) in high yield. Hydrazine is liberated in this reaction. Complexes 6 and 11 have been characterized crystallographically. The cyclic voltammograms of complexes 6 and 7 contain essentially non-reversible oxidation peaks.

Synthesis and photolysis of mixed copper(I) complexes with thiones and tri- p-tolylphosphine or triphenylphosphine; X-ray crystal structure of bis[copper(I)(1,3-thiazolidine-2-thione) (tri- p-tolylphosphine)chloride

Reaction of [Cu(PR 3)Cl] 4 [where PR 3 = tri- p-tolylphosphine (tptp), or triphenylphosphine (tpp)] with several heterocyclic thiones (L) yields binuclear complexes of the general formula [Cu(PR 3)(L)Cl] 2 [L = 1,3-thiazolidine-2-thione (tzdtH), benz-1,3- thiazoline-2-thione (bztztH), dithiouracil (dtu), purine-6-thione (pur6SH) and thiourea (tu)]. Irradition of the complexes, in chloroform, methanol and acetonitrile solutions, caused phosphine evolution while the Cu 2S 2 core remained intact. The crystal structure of [Cu(tptp)(tzdtH)Cl] 2 has been established by single-crystal X-ray diffraction methods. In the Cu 2S 2 core the CuS bond lengths are 2.386(1) and 2.470(1) Å. The CuP and CuCl distances are 2.222(1) and 2.283(1) Å, respectively.

Cumulenes as ligands: IV. Rhodium and platinum complexes of tetraphenylhexapentaene. X-ray crystal structure of bis(triphenylphosphine)chloro(tetraphenylhexapentaene)rhodium

The interaction of tetraphenylhexapentaene with chlorotris(triphenylphosphine) rhodium produces a red complex in which rhodium is bound to the second CC bond of the cumulene. In contrast, reaction of the same cumulene with (PPh 3) 2Pt 0 generated by reducing (PPh 3) 2PtCl 2 with hydrazine in ethanol results in the formation of a yellow symmetrical complex as the kinetic product. This complex isomerizes to a red unsymmetrical complex. An X-ray crystal structure of bis(triphenylphosphine)chloro(tetraphenylhexapentaene)rhodium is reported.

X-ray crystal structure of bis(4-benzoyl-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-onato) dibutyl tin(IV), C 42H 44N 4O 4Sn, with trans RR Sn configuration

A dialkyl tin complex of composition Bu 2SnL 2 ( I) (L is a monofunctional bidentate ligand) has been made by reaction of ClBu 2SnOSnBu 2Cl with the substituted pyrazolone, PhCO C:C(OH)N(Ph)N:C CH 3, in dry benzene. Crystals of I ( M= 787.5) are monoclinic, space group P2 1/ C, a= 9.714(6), b=19.621(6), c=22.68(1) Å, β=114.00(4)°, V=3949.2 Å 3, Z=4, D calc=1.3240 cm −3, λ(Mo Kα)=0.71069 Å, μ=6.960 cm −1, T=295 K, F(000)=1624, R=0.0628 for 2187 unique reflections. The molecule has a distorted octahedral geometry with Bu groups trans to each other. Four oxygen atoms of the pyrazolone moieties and the central Sn atom lie in the same plane.

X-ray crystal structure of bis(4-nitropyrazol-1-yl)methane, and some empirical rules concerning the bond angles in pyrazoles

The crystal structure of bis(4-nitropyrazol-1-yl)methane has been determined by X-ray diffraction. The nitro groups form angles of 16.45(6) and 11.83(7)°, respectively, with the pyrazole ring to which they are attached. The internal and external angles of the pyrazole rings follow a set of empirical rules: (1) N(1)-N(2)-C(3) is smaller than N(2)-N(1)-C(5); (2) N(2)-C(3)-C(4) is larger than N(1)-N(2)-C(3) and at least one chosen between C(3)-C(4)-C(5) and C(4)-C(5)-N(1); (3) C3-C4-C5 is not the largest internal angle; (4) R1-N1-N2 is smaller than R1-N1-C5; (5) N2-C3-R3 is smaller than R3-C3-C4, or R5-C5-N1 is smaller than C4-C5-R5; (6) C3-C4-R4 and R4-C4-C5 are nearly the same. Provided that the angle considered is not part of another ring, the first five rules are valid for all the pyrazoles investigated up to now, while violation of the last rule is good evidence for steric hindrance or marked asymmetry of the 3- and 5-substituents.

Spectroscopic studies and crystal structure of bis(N-2-pyridinylcarbonyl-2-pyridinecarboximidato) manganese(II) monohydrate: Zero-field splitting param

The X-ray crystal structure of bis(N-2-pyridinylcarbonyl-2-pyridinecarboximidato)manganese(II) monohydrate, Mn(BPCA) 2·H 2O, has been determine

EPR Investigations on bis(dithiophosphinato)copper(II) complexes magnetically diluted in the corresponding nickel(II) single crystals and X-ray crystal structure of bis(di-n-propyldithiophosphinato)nickel(II)

Bis(diethyldithiophosphinato)nickel(II), [(C 2H 5) 2PS 2] 2Ni and bis(di-n-propyl dithiophosphinato)nickel(II), [(n-C 3H 7) 2PS 2] 2Ni, single crystals doped with the corresponding copper(II) complexes have been prepared and studied by EPR spectroscopy. The components of the g-tensor, 63Cu hyperfine coupling tensor and 63Cu nuclear quadrupole coupling tensor have been determined. An X-ray crystal structure determination of bis(di-n-propyldithiophosphinato)nickel(II) shows the nickel atom to lie at a centre of symmetry, coordinated by four sulphur atoms at 2.220(4) and 2.230(3) Å.

Synthesis and characterization of technetium(V) complexes with N-(thiocarbamoyl)benzamidines. X-ray crystal structure of bis[N-(N,N-diethylthiocarbamoyl)benzamidinato]oxotechnetium(V) chloride, [TcO(et2tcb)2]Cl

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTSynthesis and characterization of technetium(V) complexes with N-(thiocarbamoyl)benzamidines. X-ray crystal structure of bis[N-(N,N-diethylthiocarbamoyl)benzamidinato]oxotechnetium(V) chloride, [TcO(et2tcb)2]ClU. Abram, R. Muenze, J. Hartung, L. Beyer, R. Kirmse, K. Koehler, J. Stach, H. Behm, and P. T. BeurskensCite this: Inorg. Chem. 1989, 28, 5, 834–839Publication Date (Print):March 1, 1989Publication History Published online1 May 2002Published inissue 1 March 1989https://doi.org/10.1021/ic00304a008RIGHTS & PERMISSIONSArticle Views81Altmetric-Citations44LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (771 KB) Get e-AlertsSupporting Info (1)»Supporting Information Supporting Information Get e-Alerts

Preparation and X-ray crystal structure of bis(1,8-naphthyridine-N-monoxide)copper(II) nitrate

Abstract The title compound Cu(napyo) 2 (NO 3 ) 2 was formed by the reaction of copper(II) nitrate with 1,8-naphthyridine-N-monoxide (napyo) in methanol. The complex crystallizes in the monoclinic space group P 2 1 / n with Z = 2, a = 7.768(2), b = 13.976(2), c = 9.045(3) A, β = 113.12(3)°. The structure was determined from 1579 observed reflections and refined to R = 0.035. The copper atoms show a tetragonally distorted octahedral configuration, being bonded to two oxygen atoms (CuO, 1.951 A) and two nitrogen atoms (CuN, 1.963 A) of the two napyo ligands and to two oxygen atoms (CuO, 2.410 A) of two nitrate groups.

Additions and Corrections - Synthesis and X-ray Crystal Structure of Bis-(pentamethylcyclopentadienyl) Complexes of Samarium and Europium: (C5Me5)2Sm and (C5Me5)2Eu.

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTAdditions and Corrections - Synthesis and X-ray Crystal Structure of Bis-(pentamethylcyclopentadienyl) Complexes of Samarium and Europium: (C5Me5)2Sm and (C5Me5)2Eu.William J. Evans, Laura A. Hughes, and Timothy P. HanusaCite this: Organometallics 1988, 7, 2, 575Publication Date (Print):February 1, 1988Publication History Published online8 January 2004Published inissue 1 February 1988https://doi.org/10.1021/om00092a601RIGHTS & PERMISSIONSArticle Views39Altmetric-Citations-LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (131 KB) Get e-Alerts Get e-Alerts

Oxidation and reduction chemistry of bis(η-arene)niobium compounds; the X-ray crystal structure of bis(η-toluene)(trimethylphosphine)niobium tetrafluoroborate

Cyclic voltammetry shows that [Nb(η-C6H5Me)2] undergoes both one-electron reversible reduction and oxidation; chemical oxidation with AgBF4 in the presence of PR3(R = Me, R3= Me2Ph) yields [Nb(η-C6H5Me)2(PR3)]BF4. The X-ray crystal structure of [Nb(η-C6H5Me)2(PMe3)]BF4 has been determined and shows the molecule to have the bent bis(η-arene) structure. Reduction of [Nb(η-C6H3Me3-2,4,6)2] with potassium and treatment with carbon monoxide yields [Nb(CO)6]–; reduction in the presence of 18-crown-6 (1,4,7,10,13,16-hexaoxacyclo-octadecane,L) gives [KL][Nb(η-C6H3Me3-2,4,6)2].

The X-ray crystal structure of bis(pentafluorophenyl)tellurium difluoride

Bis(pentafluorophenyl)tellurium difluoride crystallizes, in the space group Cc, as a molecular solid in which pairs of crystallographically independent molecules are linked by two weak secondary [Formula: see text] interactions. (C12F12Te; a = 11.088(6), b = 20.040(10), c = 13.208(5); β = 109.07(4); U = 2774; Z = 8; fw = 499.7). The structural model was refined by full-matrix least-squares methods to a final residual of R1 = 0.035 for 1621 observed reflections. The stereochemistry of the primary bonding about Te is ψ-trigonal bipyramidal as for other R2TeX2 species and is compared with that of diphenyltellurium difluoride. Differences in the stereochemistry of the primary bonding about tellurium can be attributed to the influence of the more electron-withdrawing C6F5 group, and relates to the different secondary bonding and the crystal packing. 125Te nmr coupling constants, [Formula: see text], are reported for this and two related compounds. Previous 125Te Mössbauer data is discussed in the light of the structure.

X-ray crystal structures of bis(dichlorophenyltelluro)methane and bis(trichlorotelluro)methane

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTX-ray crystal structures of bis(dichlorophenyltelluro)methane and bis(trichlorotelluro)methaneR. J. Batchelor, F. W. B. Einstein, C. H. W. Jones, and R. D. SharmaCite this: Organometallics 1987, 6, 10, 2164–2168Publication Date (Print):October 1, 1987Publication History Published online1 May 2002Published inissue 1 October 1987https://doi.org/10.1021/om00153a023RIGHTS & PERMISSIONSArticle Views43Altmetric-Citations10LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (700 KB) Get e-AlertsSupporting Info (1)»Supporting Information Supporting Information Get e-Alerts

Small-ring cyclic cumulenes: synthesis and x-ray crystal structure of bis(triphenylphosphine)chloro(.eta.2-1,2,3-cyclononatriene)rhodium

ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTSmall-ring cyclic cumulenes: synthesis and x-ray crystal structure of bis(triphenylphosphine)chloro(.eta.2-1,2,3-cyclononatriene)rhodiumRichard O. Angus, Musiri N. Janakiraman, Robert A. Jacobson, and Richard P. JohnsonCite this: Organometallics 1987, 6, 9, 1909–1912Publication Date (Print):September 1, 1987Publication History Published online1 May 2002Published inissue 1 September 1987https://doi.org/10.1021/om00152a013RIGHTS & PERMISSIONSArticle Views40Altmetric-Citations8LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (513 KB) Get e-AlertsSupporting Info (1)»Supporting Information Supporting Information Get e-Alerts