The crystal and molecular structure of the binuclear complex [(μ-S)-α,α'-{(2-Mercapto-4-methylbenzene-1,3-diyl)di(methylidyne)di(azino)}bis(cyclohexanemethanol)ato(3 - )]-(μ-1-propylimidazolato-C(4),N(3))-dipalladium(II)-ethanol (1/0.75)

1984 ◽  
Vol 37 (7) ◽  
pp. 1395 ◽  
Author(s):  
BF Hoskins ◽  
IAS Mcdonald

The crystal and molecular structure of the 1-propylimidazolate bridged binuclear complex, LPd2(primid) has been determined by single-crystal X-ray diffraction techniques at 20�C; disordered ethanol molecules are also present in the lattice. The quinquedentate ligand L3- is formally the trianion α,α'-{(2-mercapto-4-methylbenzene-1,3-diyl)di(methylidyne)di(azino)bis(cyclohexane-methanol)ato(3 -). Crystals of LPd2 (primid) are triclinic, P1, with a 7.078(2), b l3.615(3), c 17365(3) �, α 78.52(2), β 80.21(2) and γ 83.83(2)�. The structure was solved by conventional Fourier methods and refined by full-matrix least-squares procedures to convergence with R and Rw 0.053 obtained for the 4133 statistically significant structure amplitudes. The ligand sidearms are essentially equivalent with both palladium centres displaying similar distorted square-planar geometries, the separation being 3.605 �. The propylimidazolate bridging group is comfortably accommodated within the binuclear framework and displays a geometry typical of metal complexes of imidazole and its derivatives. Coordination to the palladium centres occurs through C4 and N3, a bridging mode not previously characterized by X-ray crystallography, and one which illustrates the remarkable stability and flexibility of the binuclear LPd2+ core.

2017 ◽  
Vol 73 (8) ◽  
pp. 1148-1150
Author(s):  
Shravan Kumar Ellandula ◽  
Cosmos Opoku Amoako ◽  
Joel T. Mague ◽  
Perumalreddy Chandrasekaran

The unsymmetrical α-diimine ligand N-{2-[2,6-bis(propan-2-yl)phenylimino]pentan-3-ylidene}-2,6-bis(propan-2-yl)aniline, [ArN=C(Me)—(Et)C=NAr] [Ar = 2,6-(iPr)2C6H3], (I), and the corresponding palladium complex, cis-(N-{2-[2,6-bis(propan-2-yl)phenylimino]pentan-3-ylidene}-2,6-bis(propan-2-yl)aniline)dichloridopalladium(II) 1,2-dichloroethane monosolvate, [PdCl2(C29H42N2)]·C2H4Cl2 or cis[PdCl2{I}], (II), have been synthesized and characterized. The crystal and molecular structure of the palladium(II) complex have been established by single-crystal X-ray diffraction. The compound crystallized along with a 1,2-dichloroethane solvent of crystallization. The coordination plane of the PdII atom shows a slight tetrahedral distortion from square-planar, as indicated by the dihedral angle between the PdCl2 and PdN2 planes of 4.19 (8)°. The chelate ring is folded along the N...N vector by 7.1 (1)°.


1986 ◽  
Vol 39 (4) ◽  
pp. 713 ◽  
Author(s):  
D Dakternieks ◽  
BF Hoskins ◽  
CL Rolls ◽  
ERT Tiekink

The crystal and molecular structure of bis ( tricyclohexylphosphine )cadmium(II) nitrate as its dichloromethane solvate, Cd [P(c-C6H11)3]2(NO3)2.CH2Cl2, has been determined by single- crystal, three-dimensional X-ray diffraction methods. The crystals of the cadmium(II) complex are monoclinic with space group C2/c, a 20.880(6), b 12.775(3), c 17.075(5) Ǻ and β 106.38(2)°, Z 4. The structure was solved by normal Fourier methods and refined by a full-matrix least-squares procedure. The refinement used the 2169 statistically independent reflections for which I ≥ 2σ(I) converged with R and Rw of 0.065 and 0.067 respectively. The crystals consist of discrete Cd [P(c-C6H11)3]2(NO3)2 molecules and CH2Cl2 in the ratio 1 : 1. There is a distorted tetrahedral environment around the cadmium atom formed from the coordination of the two phosphines and two nitrates with each nitrate essentially occupying one stereochemical position. The two markedly different Cd -O bond lengths of 2.405(9) and 2.575(8) Ǻ show gross asymmetry in the coordination of the nitrate.


1989 ◽  
Vol 67 (1) ◽  
pp. 48-53 ◽  
Author(s):  
David Eric Berry ◽  
Jane Browning ◽  
Gordon William Bushnell ◽  
Keith Roger Dixon ◽  
Alan Pidcock

Reaction of "cyclamphosphorane" (cyclamPH) with [Pt2Cl4(PEt3)2] yields [PtCl(PEt3)(cyclamPH)]Cl. The complex crystallizes as a dichloromethane solvate in the monoclinic space group P21/n, with a = 13.877(3), b = 23.231(7), c = 8.295(2)Å, β = 91.86(4)°, and an X-ray diffraction study shows square planar platinum coordination in which the labile proton of cyclamPH has transferred from phosphorus to nitrogen and the ligand is attached via simple [Formula: see text] chelation. The phosphorus is trans to chlorine in the platinum coordination plane.The corresponding product, trans-[PtCl2(PEt3)(cyclenPH2)]Cl, derived from reaction of "cyclenphosphorane" (cyclenPH) with [Pt2Cl4(PEt3)2], is shown by NMR studies to have a quite different structure in which the ligand is protonated at two nitrogen sites but not at phosphorus. The phosphorus is pentacoordinate with four attachments to nitrogen atoms and one to platinum. The two chlorine atoms are mutually trans in the platinum coordination plane. Keywords: crystal structure, cyclenphosphorane reaction, cyclamphosphorane reaction, X-ray diffraction.


1983 ◽  
Vol 36 (4) ◽  
pp. 683 ◽  
Author(s):  
BF Hoskins ◽  
RJ Steen

The crystal structure of the complex Mn2(CO)8(dam) (dam = Ph2AsCH2AsPh2) has been determined by three-dimensional X-ray diffraction methods. The crystals are triclinic, space group P1, with a 11.191(1), b 16.498(5), c 9.455(1) �, a 93.64(2), β 109.08(2), γ 89.36(2)� and contain two discrete, binuclear molecules of Mn2(CO)8(dam) per unit cell. The structure, solved by direct and Fourier methods, was refined by a least-squares procedure to R and Rw of 0.065 and 0.082 respectively for 1907 independent, statistically significant reflections collected by counter methods. The feature of particular interest in this compound is the accommodation of the bridging bidentate dam ligand [As.. .As separation 3.242(2) �] across a shorter Mn�-Mn� bond [2.962(3) �] which constrains the molecule so that a much less staggered configuration of the two manganese coordination octahedra is observed relative to the parent compound Mn2(CO)10, the rotation of the two equatorial planes in the former being 30�.


1974 ◽  
Vol 52 (17) ◽  
pp. 3125-3133 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Masood A. Khan

The crystal and molecular structure of diazido-2,2′-bipyridinecopper(II), C10H8N2(N3)2Cu, is determined by single crystal X-ray diffraction, and refined to an R value of 0.067. The cell dimensions are a = 664.9(2), b = 843.3(1), c = 1082.0(2) pm, α = 86.99(2)°, β = 87.77(3)°, γ = 78.59(2)°. The space group is [Formula: see text] (No. 2) with 2 molecules per unit cell and the measured density is 1.71(2) g cm−3. The copper coordination is square planar with two additional longer bonds. The coordinate bond lengths in pm to the bipyridine ligand are: Cu—N(1), 201.6(6); Cu—N(2), 201.9(6). The coordinate bonds to the azido ligands are: Cu—N(3), 194.9(6); Cu—N(6), 196.6(6). The longer bonds are: Cu—N(3)″, 268.0(8), Cu—N(6)′ 268.2(8). The N—N bond lengths within each azido ligand are unequal: N(3)—N(4), 118.2(10); N(4)—N(5), 115.4(11); N(6)—N(7), 119.2(9); N(7)—N(8), 114.8(9). The angles at N(3) and N(6) are both 130° and at N(4) and N(7) the angles are both 175(1)°. Each azide takes part in asymmetric bridging through a single nitrogen atom. The results are compared with other structural studies on azido complexes and to a nitrate complex of Ag(II) which is structurally similar.


2007 ◽  
Vol 72 (5-6) ◽  
pp. 609-617 ◽  
Author(s):  
Andrzej Kozioł ◽  
Stanisław Pasynkiewicz ◽  
Antoni Pietrzykowski ◽  
Lucjan B. Jerzykiewicz

trans-Bis[1,3-bis(2,4,6-trimethylphenyl)imidazolidin-2-ylidene]dichloronickel(II), [NiCl2(SIMes)2], was synthesized in a one-pot reaction of fluorenyllithium with nickel(II) bromide followed by the addition of 1,3-bis(2,4,6-trimethylphenyl)imidazolidinium chloride. Labile difluorenyl- nickel, formed in the course of the reaction, behaves differently than nickelocene and indenocene in analogous reactions. It exchanges both fluorenyl ligands giving the title compound. The crystal and molecular structure of this compound have been determined by single-crystal X-ray diffraction. The compound crystallizes in the monoclinic crystal system with square-planar geometry around the central nickel atom.


Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.


2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.


2018 ◽  
Vol 73 (12) ◽  
pp. 1029-1032
Author(s):  
Peter Mayer ◽  
Hans-Christian Böttcher

AbstractTreatment of THF solutions containing the rhodium(II) complex trans-[RhCl2(PtBu2Ph)2] (1) with [Fe2(CO)9] in the same solvent resulted in the formation of the Vaska-type complex trans-[RhCl(CO)(PtBu2Ph)2] (2) in high yield. The title complex 2 was obtained as pale yellow crystals, characterized by NMR and IR spectroscopy, as well as by microanalyses. Additionally, the molecular structure of 2 has been established by X-ray crystallography. As often reported for similar constituted compounds, the chlorido and carbonyl ligands in crystals of 2 are strongly disordered.


1983 ◽  
Vol 36 (2) ◽  
pp. 253 ◽  
Author(s):  
AC McDonell ◽  
TW Hambley ◽  
MR Snow ◽  
AG Wedd

The salts Ph4As [ReO(SPh)4].MeCN and Ph4As [ReO(SePh)4] have been synthesized and characterized. The crystal and molecular structure of the thiolate compound has been determined by X-ray crystallography which reveals a square-pyramidal arrangement of ligand atoms around the central rhenium atom of the [ReO(SPh)4]- anion. Crystal data: a 9.756(4), b 18.171(3), c 25.684(4) �, space group P212121, Z 4.


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