Synthesis and Characterization of Gold(III) Halide Complexes of Quinaldic Acid (Hqd), Methyl Quinaldate and Ethyl Quinaldate, and X-Ray Structure of [(HQd)2H] [AuBr4].H2O

1994 ◽  
Vol 47 (7) ◽  
pp. 1423 ◽  
Author(s):  
MAS Goher ◽  
AK Hafez ◽  
RJ Wang ◽  
XM Chen ◽  
TCW Mak
Keyword(s):  
Hydrogen Bond ◽  
Far Infrared ◽  
Synthesis And Characterization ◽  
Coordination Environment ◽  
X Ray ◽  
Quinaldic Acid ◽  
Halide Complexes ◽  
Monodentate Ligands ◽  
Far Infrared Spectra

Complexes of the types HAuX4.2HQd, where X = Cl or Br and HQd = quinaldic acid, and AuX3L2, where L is methyl or ethyl quinaldate , have been prepared and characterized. Quinaldic acid as well as methyl and ethyl quinaldates function as monodentate ligands in these complexes, whose stereochemistries are discussed in relation to the number of gold-halogen stretching frequencies observed in their far-infrared spectra. The measured conductivities of these complexes are also discussed. Single-crystal X-ray analysis of monohydrated HAuBr4.2HQd revealed that it should be formulated as [( HQd )2H][AuBr4].H2O, in which a pair of zwitterionic HQd moieties are connected by a strong O...H...O hydrogen bond, and the gold(III) atom is in an elongated octahedral coordination environment with two long Au-O bonds of 3.388(8) and 3.440(8)Ǻ.

Synthesis of ReItricarbonyl complexes with various sulfur- and oxygen-donating ligands: crystal structures of two ReIdinuclear structures bridged by S atoms

2018 ◽  
Vol 74 (10) ◽  
pp. 1116-1122
Author(s):  
Pheello I. Nkoe ◽  
Hendrik G. Visser ◽  
Chantel Swart ◽  
Alice Brink ◽  
Marietjie Schutte-Smith
Keyword(s):  
Hydrogen Bond ◽  
Intermolecular Hydrogen Bond ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Pyridine Ligand ◽  
X Ray ◽  
Hydrogen Bond Interactions ◽  
Mononuclear Complexes

The synthesis and characterization of two dinuclear complexes, namelyfac-hexacarbonyl-1κ3C,2κ3C-(pyridine-1κN)[μ-2,2′-sulfanediyldi(ethanethiolato)-1κ2S1,S3:2κ3S1,S2,S3]dirhenium(I), [Re2(C4H8S3)(C5H5N)(CO)6], (1), and tetraethylammoniumfac-tris(μ-2-methoxybenzenethiolato-κ2S:S)bis[tricarbonylrhenium(I)], (C8H20N)[Re2(C7H7OS)3(CO)6], (2), together with two mononuclear complexes, namely (2,2′-bithiophene-5-carboxylic acid-κ2S,S′)bromidotricarbonylrhenium(I), (3), and bromidotricarbonyl(methyl benzo[b]thiophene-2-carboxylate-κ2O,S)rhenium(I), (4), are reported. Crystals of (1) and (2) were characterized by X-ray diffraction. The crystal structure of (1) revealed two Re—S—Re bridges. The thioether S atom only bonds to one of the ReImetal centres, while the geometry of the second ReImetal centre is completed by a pyridine ligand. The structure of (2) is characterized by three S-atom bridges and an Re...Re nonbonding distance of 3.4879 (5) Å, which is shorter than the distance found for (1) [3.7996 (6)/3.7963 (6) Å], but still clearly a nonbonding distance. Complex (1) is stabilized by six intermolecular hydrogen-bond interactions and an O...O interaction, while (2) is stabilized by two intermolecular hydrogen-bond interactions and two O...π interactions.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXIV Syntheses, Spectroscopy and Structures of Some 1 : 4 Adducts of Copper(I) and Silver(I) Perchlorates with Triphenylarsine and Triphenylstibine

1997 ◽  
Vol 50 (6) ◽  
pp. 539 ◽  
Author(s):  
Graham A. Bowmaker ◽  
Effendy ◽  
Robert D. Hart ◽  
John D. Kildea ◽  
Brian W. Skelton ◽  
...  
Keyword(s):  
Room Temperature ◽  
Far Infrared ◽  
Lewis Base ◽  
X Ray ◽  
Cation Disorder ◽  
Structure Determinations ◽  
Consistent Picture ◽  
Far Infrared Spectra

Syntheses and room-temperature single crystal X-ray structure determinations are recorded for adducts [M(EPh3)4] (ClO4), M = Cu, E = As (1), Sb (2); M = Ag, E = As (3), Sb (4), enabling comparison with analogous, previously studied MP4 and MN4 environments. The four complexes so characterized all crystallize in the familiar rhombohedral R-3 array (a ≈ 14·4, c ≈ 52 Å, hexagonal setting) with the metal and chlorine atoms located on crystallographic threefold axes. In these arrays Cu–E (axial, off axis) are 2·493(2), 2·533(1) for (1), and 2·572(1), 2·577(1) Å for (2), the disparity in the two independent M-E distances being diminished relative to those of previously studied phosphorus analogues, perhaps in consequence of increasing E size. In (3) and (4), some cation disorder is evident in respect of the ligand pnictide atom (E); for the major components Ag-E are 2·652(3), 2·680(2) in (3); 2·732(2), 2·7295(8) Å in (4). Problems associated in defining the metal atom environment geometries in the latter are, nevertheless, more satisfactorily overcome in two further determinations of nitrate salts: [Ag(SbPh3)4] (NO3) (5) is of the rhombohedral family with no cation core disorder, Ag–E (axial, off axis) being 2·720(4), 2·725(2) Å, while the structural characterization of a 1 : 4 triphenylarsine adduct of silver nitrate is recorded as its tetraethanol solvate, namely [Ag(AsPh3)4] (NO3).~ 4C2H5OH(6), monoclinic, C2/c, a 18·373(4), b 20·786(5), c 21·070(8) Å, β 108·18(3)°, Z = 4 f.u. The silver atom of the [Ag(AsPh3)4]+cation unusually lies on a crystallographic 2 (rather than a 3 ) axis of the incipiently23 (T) array, with Ag-As 2·649(2), 2·650(2) Å and As-Ag-As ranging from 108·22(4) to 111·41(6)°. The structure determination of a chloroform solvate of (2), denoted (2a), of low precision, is noted, together with the structure of an interesting artefact, isomorphous with the rhombohedral oxoanion array, modelled as [Ag(PPh3)4]2 (SiF6).py (7). Bands in the far-infrared spectra of [M(AsPh3)4] (ClO4) are assigned to v(MAs) vibrations at 119 (M = Cu) and 103 cm¯1 (M = Ag); this produces a more consistent picture of the variation in the wavenumbers of the v(ME) modes in [M(EPh3)4]+ compounds than was available previously.

scholarly journals Field-induced single-ion magnet based on a quasi-octahedral Co(II) complex with mixed sulfur-oxygen coordination environment

2021 ◽  
Author(s):  
Denis V. Korchagin ◽  
Yaroslav E. Gureev ◽  
Elena A. Yureva ◽  
Gennady V. Shilov ◽  
Alexander V. Akimov ◽  
...  
Keyword(s):  
Magnetic Properties ◽  
Octahedral Complex ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Oxygen Coordination

Synthesis and characterization of structure and magnetic properties of the quasi-octahedral complex (pipH2)[Co(TDA)2] 2H2O (I), (pipH22+ = piperazine dication, TDA2-= thiodiacetic anion) are described. X-ray diffraction studies reveal the first...

scholarly journals Synthesis and Characterization of Bis(4-methylbenzylammonium) Tetrachloridocadmate(II)

2011 ◽  
Vol 2011 ◽  
pp. 1-7 ◽  
Author(s):  
R. Kefi ◽  
M. Zeller ◽  
F. Lefebvre ◽  
C. Ben Nasr
Keyword(s):  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Hybrid Compound ◽  
Coordination Environment ◽  
X Ray ◽  
Organic Hybrid ◽  
Distorted Octahedral ◽  
Cp Mas Nmr

The crystal structure of the new inorganic-organic hybrid compound [4-CH3C6H4CH2NH3]2[CdCl4] has been determined by single crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group Pnma with lattice parameters a=10.721(2), b=33.986(6), c=5.326(1) Å, β=97.222(1)°, V=1940.8(7) Å3, and Z=4. The framework of the title compound is built upon layers parallel to (010) made up from corner-sharing CdCl6 octahedra. 4-Methylbenzylammonium cations are situated between the layers and connect them via an N–H⋯Cl hydrogen bonding network. The Cd atom is located on an inversion centre, and the coordination environment is described as distorted octahedral. Solid state 13C CP-MAS NMR spectroscopy is in agreement with the X-ray structure. DFT calculations allow the attribution of the carbon peaks to the independent crystallographic sites. Thermal analysis and infrared spectroscopy were also used to characterize the complex.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXXI Synthesis, Spectroscopy and Structural Systematics of Some 1 : 2 Binuclear Adducts of Silver(I) Compounds with Triphenylarsine, [(Ph3As)2Ag(µ-X)2Ag(AsPh3)2], X = Cl, Br, I, SCN

1997 ◽  
Vol 50 (6) ◽  
pp. 627 ◽  
Author(s):  
Graham A. Bowmaker ◽  
Effendy ◽  
John D. Kildea ◽  
Eban N. de Silva ◽  
Allan H. White
Keyword(s):  
Infrared Spectra ◽  
Structural Characterization ◽  
Room Temperature ◽  
Far Infrared ◽  
Lewis Base ◽  
X Ray ◽  
C 23 ◽  
Pseudo Halides ◽  
Far Infrared Spectra

The syntheses and room-temperature single-crystal X-ray structural characterization of binuclear 1 : 2 adducts formed between silver(I) (pseudo-)halides, AgX, and triphenylarsine, AsPh3, for X = Cl, Br, I, SCN (1)–(4), are described. The chloride (1), obtained from 2-methylpyridine, is triclinic, P-1, a 10·410(2), b 12·716(2), c 14·196(6) Å, α 113·38(2), β 109·41(2), γ 75·08(1)°, Z = 1 (dimer); conventional R on F was 0·037 for No 3979 independent ‘observed’ (I > 3σ(I)) reflections. The bromide (2a), obtained from 2,6-dimethylpyridine, and iodide (3), obtained from a mixture of AgI/saturated KI in MeOH solutions, are isomorphous, monoclinic, P 21/c a≈ 24·2, b ≈ 13·9, c ≈ 20·2 Å, β ≈ 109·5°, Z = 4 dimers; R was 0·046 and 0·044 for No 5670 and 6039 respectively. The thiocyanate (4) has a similar cell, a 24·12(1), b 12·558(8), c 23·244(4) Å, β 110·11(3)°, Z = 4 dimers, R being 0·044 for No 7956; one of the thiocyanate ligands (which bridge in Ag-SCN-Ag mode) is disordered. A second polymorph of the bromide (2b) (from a mixture of AgBr/saturated KBr in H2O) is also monoclinic, P 21/c, a 14·121(8), b 25·577(3), c 21·968(2) Å, β 125·54(3)°, Z = 4 dimers (R was 0·047 for No 5715). Ag–As range between 2·568(1) and 2·633(1) Å throughout the series; in the isomorphous bromide and iodide, values increase slightly: 2·578(1)–2·611(1), cf. 2·601(2)-2·633(1) Å respectively. Ag–X are 2·568(2)-2·670(2) (Cl); 2·688(2)–2·715(2) (Br); 2·828(2)–2·856(1) Å (I); Ag-S, N for the ordered SCN group are 2·646(3), 2·255(6) Å. A redetermination of improved precision (R 0·035, No 6030) is reported for the triphenylphosphine/thiocyanate analogue. The far-infrared spectra of [(Ph3As)2Ag(µ-X)2Ag (AsPh3)2] show v(AgX) bands at 185, 145 (X = Cl), 145, 130, 106 (X = Br) and 121 cm-1 (X = I). The splittings and band widths reflect a decrease in the degree of distortion of the Ag(µ-X)2Ag units from a symmetrically bridged structure from X = Cl to I.

Structure and Spectroscopic Studies of Cd(II) Complexes of Tris(2-pyridyl)amine: 1D and 2D Supramolecular Assemblies

2003 ◽  
Vol 68 (11) ◽  
pp. 2139-2149 ◽  
Author(s):  
Yong-Shu Xie ◽  
Xue-Ting Liu ◽  
Jia-Xiang Yang ◽  
Hui Jiang ◽  
Qing-Liang Liu ◽  
...  
Keyword(s):  
Spectroscopic Data ◽  
Far Infrared ◽  
Spectroscopic Studies ◽  
X Ray Diffraction ◽  
Absorption Bands ◽  
X Ray ◽  
Halide Complexes ◽  
2D Network ◽  
Far Infrared Spectra ◽  
Dinuclear Structure

Cd(II) halide complexes [Cd2X4(tpa)2] (1: X = Cl, 2: X = Br, 3: X = I; tpa = tris(2-pyridyl)amine) have been synthesized. X-Ray diffraction analyses of 2 and 3 reveal their asymmetrical dinuclear structures: one Cd(II) atom is octahedrally coordinated to four N atoms of two tpa ligands and two bridging halides; the other Cd(II) is tetrahedrally coordinated to two terminal (X(t)) and two bridging (X(b)) halides. By multiple intra- and intermolecular π-π interactions between the tpa pyridine rings, the ligands of 2 and 3 are linked to form a 2D network and 1D linear structures, respectively. In the Raman and far-infrared spectra, the absorption bands due to Cd-X(b) stretching modes lie at lower wavenumbers compared to the Cd-X(t) stretches. It can be inferred from the spectroscopic data that 1 has a dinuclear structure similar to those of 2 and 3.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXXIII Synthesis, Spectroscopy and Structural Systematics of New 1 : 1 'Cubane' Tetramers of Copper(I) and Silver(I) Halides with Triphenylarsine

1997 ◽  
Vol 50 (6) ◽  
pp. 653 ◽  
Author(s):  
Graham A. Bowmaker ◽  
Effendy ◽  
Robert D. Hart ◽  
John D. Kildea ◽  
Allan H. White
Keyword(s):  
Room Temperature ◽  
Far Infrared ◽  
Lewis Base ◽  
Potassium Iodide Solution ◽  
X Ray ◽  
Iodide Solution ◽  
Benzene Solvate ◽  
The Common ◽  
Far Infrared Spectra

Syntheses and room-temperature single-crystal X-ray structural characterization of a number of 1 : 1 ‘cube tetramer’ adducts of copper(I) and silver(I) halides, MX, with triphenylarsine, AsPh3, are recorded, being [XM(AsPh3)]4. The CuBr adduct, obtained unsolvated from toluene, orthorhombic Pbcn, a 17·844(5), b 20·778(8), c 18·430(4) Å, Z = 4 tetramers, conventional R on |F| 0·058 for No 1309 independent ‘observed’ reflctions (I > 3σ(I)), is isomorphous with previously recorded [ClAg(PPh3)]4, the tetramer having crystallographically imposed 2 symmetry. The CuI adduct, previously recorded as a monobenzene solvate, has been isolated unsolvated from toluene, monoclinic, P 21/n, a 19·70(5), b 27·110(7), c 13·59(2) Å, β 98·84(9)°, Z = 4 tetramers, R 0·087 for No 4359, isomorphous with previously recorded [ICu(PPh3)]4, as a 6½ benzene solvate, triclinic, P-1 a 26·688(2), b 15·180(7), c 13·090(1) Å, α 85·41(2), β 87·580(7), γ 77·63(2)°, Z = 2 tetramers, R 0·049 for No 11485, and as a chloroform disolvate, triclinic, P-1 a 22·584(9), b 13·979(2), c 13·892(2) Å, α 68 ·99(2), β 77·31(3), γ 75·65(3)°, Z = 2, R 0·041 for No 8701. An unsolvated AgI complex, monoclinic, P 21/c, a 25·26(1), b 12·506(5), c 25·228(9) Å, β 113·54(4)°, Z = 4 tetramers, R 0·054 for No 5520, isomorphous with previously recorded [IAg(PPh3)]4 (denoted ‘α’), was obtained from methanol/saturated potassium iodide solution, while a second ‘β’-form obtained from 2,4,6-trimethylpyridine, rhombohedral R3c, a 17·048(7) Å, α 61·15(5)°, Z = 2 tetramers, R 0·037 for No 1622, is isomorphous with previously recorded [BrAg(PPh3)]4, for which a redetermination is described (R 0·039 for No 1289); the latter has also been obtained in the common orthorhombic Pbcnarray: a 18·10(1), b 2·08(1), c 18·39(1) Å, Z = 4, R 0·041 for No 2877. A new ‘step’ form of [IAg(PPh3)]4, monoclinic, C 2/c, a 26·14(2), b 16·340(9), c 18·64(2) Å, β 114·04(8)°, R 0·058 for No 2107, obtained from acetonitrile and isomorphous with [BrCu(PPh3)]4 (step), is also recorded. In the far-infrared spectra of [(Ph3As)4Cu4X4] bands which have been assigned to vibrations of the Cu4X4 core are: 166, 150, 135, 114 (X = Br); 136, 85 cm-1 (X = I; 2CHCl3 solvate). The 166, 150, 135 cm-1 bands in the bromide are only partially resolved. These, and the 136 cm-1 band in the iodide are assigned to the T2 v(CuX) mode of the Cu4X4 core; the bands at 114 and 85 cm-1 are assigned to the next highest frequency T2 mode of the cluster. The splitting of the highest frequency T2 band for the bromide is consistent with the greater degree of distortion of the Cu4X4core from ideal Td symmetry in this complex relative to the iodide.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LXXII Synthesis, Spectroscopy and Structural Systematics of Some 1 : 2 Binuclear Complexes of Silver(I) Halides with Triphenylstibine, [(Ph3Sb)2Ag(μ-X)2Ag(SbPh3)2], X = Cl, Br, I

1997 ◽  
Vol 50 (6) ◽  
pp. 641 ◽  
Author(s):  
Graham A. Bowmaker ◽  
Effendy ◽  
Eban N. de Silva ◽  
Allan H. White
Keyword(s):  
Infrared Spectra ◽  
Structural Characterization ◽  
Room Temperature ◽  
Far Infrared ◽  
Lewis Base ◽  
Binuclear Complexes ◽  
X Ray ◽  
Centrosymmetric Dimers ◽  
Far Infrared Spectra

Syntheses and room-temperature single-crystal X-ray structural characterization of binuclear 1 : 2 adducts formed between silver(I) halides, AgX (X = Cl, Br, I), and triphenylstibine, SbPh3, are described. The three complexes are isomorphous, being triclinic, P-1, a ≈ 18·5, b ≈ 14·6, c ≈ 14·5 Å, α ≈ 62·5, β ≈ 74, γ ≈ 77°, Z = 2 centrosymmetric dimers. Conventional R on F were 0·043, 0·038 and 0·046 for 4984, 8479 and 4166 independent, ‘observed’ (I > 3σ(I)) reflections respectively. In [(Ph3b)2Ag(µ-X)2Ag(SbPh3)2], Ag–Sb range between 2·702(1) and 2·744(2) Å, lengthening slightly from chloride to iodide; Ag–X are 2·567(5)–2·628(4) (Cl), 2·684(1)–2·737(1) (Br) and 2·826(3)–2·869(3) Å (I). The far-infrared spectra of [(Ph3Sb)2Ag(µ-X)2Ag(SbPh3)2] show v(AgX) bands at 178, 158 (X = Cl), 121 (X = Br) and 110 cm-1 (X = I). The splittings and band widths reflect a decrease in the degree of distortion of the Ag(µ-X)2Ag units from a symmetrically bridged structure from X = Cl to I.

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