Novel methadone salt containing a discrete, square-planar CuCl4 2? anion: X-ray crystal and molecular structure of bis(1-methyl-4-oxo-3,3-diphenylhexyldimethylammonium) tetrachlorocuprate(II)

Author(s):  
Harold C. Nelson ◽  
Stanley H. Simonsen ◽  
George W. Watt
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)°.


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.


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.


1978 ◽  
Vol 56 (12) ◽  
pp. 1602-1609 ◽  
Author(s):  
Robert F. Stepaniak ◽  
Nicholas C. Payne

The crystal and molecular structure of trans-chloro(3-hydroxypropyl-N,N-dimethylaminocarbene)bis(dimethylphenylphosphine)platinum(II) hexafluorophosphate has been determined from three-dimensional X-ray data collected on an automated four circle diffractometer using CuKα radiation. The compound crystallizes in the orthorhombic space group Pna21, with Z = 4, and cell dimensions a = 14.403(2), b = 12.631(2), and c = 16.151(2) Å. Full matrix least-squares refinement on F gave a final conventional R factor of 0.047 for 3442 observations with I > 3σ(I). The cation coordination geometry is square planar, with the carbene ligand lying approximately perpendicular to the plane. The Pt—Cl bond length is 2.356(4) Å and the Pt—C(carbene) distance is 1.978(12) Å. The C(carbene)—N bond length is 1.293(16) Å. These dimensions are discussed in terms of the trans influences of the carbene and chloride ligands and the bonding in the carbene species.


1979 ◽  
Vol 57 (11) ◽  
pp. 1368-1371 ◽  
Author(s):  
Richard G. Ball ◽  
James Trotter

The molecular structure of cis-dichloro(2,2′-o-phenylenebisbenzothiazole)copper(II) has been determined by single crystal X-ray diffractometry. The crystal is monoclinic, P21/n, a = 8.408(1), b = 15.819(1), c = 14.229(2) Å, β = 93.19(1)°, and Z = 4. The structure has been refined by full-matrix least-squares techniques on F, using 3316 unique reflections for which F2 > 3σ(F2), to a final agreement factor of 0.028. The complex adopts an approximately square planar coordination geometry with the Cu bound to two cis Cl atoms and the N atoms of the chelating benzothiazole ligand. The mean Cu—N and Cu—Cl distances are 2.016(6) and 2.217(6) Å, respectively.


1981 ◽  
Vol 59 (16) ◽  
pp. 2429-2434 ◽  
Author(s):  
Norman L. Paddock ◽  
T. N. Ranganathan ◽  
Steven J. Rettig ◽  
Rajendra D. Sharma ◽  
James Trotter

Dodecamethylcyclohexaphosphazene N6P6Me12, 1, forms 1:1 complexes with palladium(II) chloride, 2, and platinum(II) chloride, 3. Their 31P, 1H, and 13C nmr spectra show them to be rigid molecules in solution, with an approximate plane of symmetry. Crystals of 2 are orthorhombic, a = 17.4030(3), b = 15.4897(5), c = 10.7417(2) Å, Z = 4, space group P21212. The structure was determined from diffractometer X-ray data and refined by full-matrix least-squares methods to R = 0.031 for 3545 reflections with I ≥ 3σ(I). The metal atom has square planar coordination, and forms 6- and 10-membered chelate rings with the phosphazene ligand. The mean P—N bond length is 1.609 Å; the variation of bond lengths within the ring is consistent with model calculations of changes in bond order arising from the localization of bonding electrons.


1980 ◽  
Vol 33 (6) ◽  
pp. 1373 ◽  
Author(s):  
GB Robertson ◽  
PO Whimp

The crystal and molecular structure of a platinum(0) complex of cyclooctyne, [(coct)Pt(PPh3)2], has been determined from three- dimensional X-ray data collected by counter methods. The complex crystallizes in the space group P21/n [a non-standard setting of space group P21/c (C2h5, No. 14)], with a 20.660(9), b 12.299(5), c 15.470(7) Ǻ, β 110.26(2)°, Z 4. The structure was solved by conventional Patterson and Fourier methods and was refined by block-diagonal least-squares techniques to weighted and unweighted R-factors of 0.048 and 0.047 respectively, for the 4733 unique reflections with I/σ(I) ≥ 3.0. The molecule is essentially square planar about the 'central' platinum atom, with the triphenylphosphine groups occupying cis coordination sites. The Pt-C distances are equal within experimental error [2.034(9) and 2.037(9) Ǻ] and compare favourably with the corresponding distances in the platinum(0)-cyclohexyne and -cycloheptyne analogues. The acetylenic C=C distance is 1.279(13) Ǻ and shows the normal bond lengthening consequent upon coordination.


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.


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.


1981 ◽  
Vol 46 (1) ◽  
pp. 6-19 ◽  
Author(s):  
Viktor Kettman ◽  
Ján Garaj ◽  
Jaroslav Majer

The crystal and molecular structure of [Cr(S2CN(CH2)5)3].2 CHCl3 was found by the X-ray structural analysis method. The value R 0.090 was found for 1 131 observed independent reflections. The substance crystallizes in a space group of symmetry P212121 with the following unit cell dimensions: a = 0.8675 (6), b = 1.815(2), c = 2.155(3) nm. The experimentally observed crustal density was 1.48 Mgm-3 and the value calculated for Z = 4 was 1.51 Mgm-3. The CrS6 coordination polyhedron has the shape of a trigonally distorted octahedron, where the D3 symmetry is a approximately retained. The degree of trigonal distortion expressed as the projection of the chelate S-Cr-S angle onto the plane perpendicular to the C3 pseudo axis is Φ = 41.7° (Φ = 60° for an octahedron). The skeleton of the structure formed by the complex molecules contains channels filled with chloroform molecules. The specific type of complex-chloroform interaction consists of the formation of hydrogen bonds of the chloroform protons with the fully occupied pπ-orbitals of the sulphur atoms in the coordination polyhedra. The low stability and crystal decomposition can be explained by loss of chloroform from the channels.


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