The Crystal Structure of cis-Dichloro(2,2′-oxydi-3-butene)platinum(II), PtCl2((CH2=CH—CH(CH3))2O)

1973 ◽  
Vol 51 (4) ◽  
pp. 604-608 ◽  
Author(s):  
J. Hubert ◽  
A. L. Beauchamp ◽  
T. Theophanides

The reaction of K2PtCl4 with CH3—CH=CH—CH2—OH yields the complex cis-[PtCl2((CH2=CH—CH(CH3))2O)]. The crystals are triclinic, space group [Formula: see text], a = 9.420(2) Å, b = 8.359(4) Å, c = 7.837(4) Å, α = 91.10(4)°, β = 62.13(4)°, γ = 80.80(5)°, and Z = 2. The structure, solved by standard methods, has been refined anisotropically by full matrix least-squares methods to a R factor of 0.052 by use of 2441 independent observed reflections. The complex is a monomer, where both double bonds of the diolefin ether are coordinated to the platinum atom as in Zeise's salt. The usual square planar coordination of platinum(II) is completed by two chlorine atoms. The (=CH2) groups of both double bonds are found on the same side of the coordination plane. Various possible conformations of the coordinated ligand in the complex are discussed.

1979 ◽  
Vol 57 (1) ◽  
pp. 57-61 ◽  
Author(s):  
R. Melanson ◽  
F. D. Rochon

The crystal structure of [Pt(diethylenetriamine)(guanosine)](ClO4)2 has been determined by X-ray diffraction. The crystals are orthorhombic, space group P212121, with a = 12.486(6), b = 13.444(7), c = 14.678(11) Å, and Z = 4. The structure was refined by block-diagonal least-squares analysis to a conventional R factor of 0.050 and a weighted Rw = 0.045.The coordination around the platinum atom is square planar. Guanosine is bonded to platinum through N(7). The purine planar ring makes an angle of 62.7° with the platinum coordination plane. The structure is stabilized by hydrogen bonding.


1980 ◽  
Vol 58 (7) ◽  
pp. 664-668 ◽  
Author(s):  
Rosemary C. E. Durley ◽  
William L. Waltz ◽  
Beverly E. Robertson

Crystals of [Pt(Et4dien)I]I, where Et4dien = (C2H5)2NC2H4NHC2H4N(C2H5)2, have been prepared. A three dimensional crystal structure analysis has been carried out in a monoclinic unit cell having a = 12.565(8), b = 7.576(6), c = 21.040(15) Å, β = 91.12(2)° and space group P21/c, Z = 4. Full-matrix least-squares using 1982 independent, observed reflections converged at R = 0.067. The platinum atom has square-planar co-ordination. The orientation of the four ethyl groups with respect to the plane of the ligand is similar to that observed in related molecules, in spite of a lack of similarity of the molecular packing. The iodide ion appears to be hydrogen bonded to the ligand.


1980 ◽  
Vol 58 (2) ◽  
pp. 97-101 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
R. Melanson

The crystal structure of trans-[Pt(DMF)(2,6-lutidine)Cl2] has been determined by X-ray diffraction. The crystals are orthorhombic, space group Pbca, with a = 11.612(13), b = 26.504(33), c = 9.271(9) Å, and Z = 8. The structure was refined by full matrix least-squares analysis to a conventional R factor of 0.051 and a weighted Rw = 0.044. The coordination around the platinum atom is square planar. The 2,6-lutidine ring is perpendicular to the platinum plane. DMF is bonded to platinum through the oxygen atom. It is planar and makes an angle of 71 ° with the platinum plane. The cis–trans configuration of the [Pt(DMF)(L)Cl2] (L = pyridine derivative) complexes in DMF solution is discussed.


1976 ◽  
Vol 54 (6) ◽  
pp. 1002-1006 ◽  
Author(s):  
R. Melanson ◽  
F. D. Rochon

The molecular and crystal structure of potassium trichloro(2,6-lutidine)platinum(II) has been determined by X-ray diffraction. The complex salt forms monoclinic crystals, a = 6.941, b = 24.301, c = 11.168 Å, β = 141.58°, Z = 4, and space group P21/c. Positional and anisotropic thermal parameters were refined by full matrix least squares calculations to R = 0.038 and Rw = 0.034.The coordination around the platinum atom is planar. The Pt—Cl bond lengths are 2.301, 2.299, and 2.302 Å and the Pt—N bond length is 2.011 Å. The 2,6-lutidine ring lies almost perpendicular to the coordination plane of the platinum atom (81.6°). The PtCl3 moieties are packed around the potassium ions, which are surrounded by four chlorine atoms at distances smaller than 3.15 Å forming a distorted tetrahedron.


1975 ◽  
Vol 53 (8) ◽  
pp. 1139-1143 ◽  
Author(s):  
Robert Melanson ◽  
Joseph Hubert ◽  
F. D. Rochon

The molecular and crystal structure of the [Pt(dien)Br]Br complex (dien = diethylenetriamine) has been studied by X-ray diffraction. The compound belongs to the orthorhombic Pca21 space group and the cell parameters are: a = 14.211, b = 4.940, c = 13.450 Å, and Z = 4. The refinement of the positional and anisotropic thermal parameters, carried out by full matrix least squares calculations, converged to R = 0.039 and Rw = 0.036.The coordination around the platinum atom is planar. The crystal consists of alternate layers of [Pt(dien)Br]+ cations and Br− ions parallel to the ac plane.


1984 ◽  
Vol 62 (12) ◽  
pp. 2657-2660 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
R. Melanson

Three types of complexes, trans-[Pt(LH)2Cl2], [Pt(L)2], and [Pt(LH)2(SR)2] where LH = NH2—C(CH3)2(CH2OH) and NH2—C(CH2OH)3 and L are the deprotonated ligands, have been synthesized.The crystal structure of trans-[Pt(NH2—C(CH3)2CH2OH)2Cl2] has been determined by X-ray diffraction methods. The crystals are monoclinic, space group P21/c, with a = 6,282(3), b = 20,901(13), c = 10,769(10) Å, β = 92,64(6)°, and Z = 4. The structure was refined by full-matrix least-squares analysis to a conventional R factor of 0.049 and Rw = 0.042. The coordination around the platinum atom is square planar. The Pt—Cl distances are 2.306(2) and 2.309(3) Å and the Pt—N bonds are 2.060(8) and 2.071 (7) Å. The hydroxyl oxygen atoms are disordered; the disorder is different for each organic ligand. The structure is stabilized by an extensive hydrogen bonding system.


1980 ◽  
Vol 58 (4) ◽  
pp. 381-386 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
B. Coulombe ◽  
R. Melanson

The interactions between [Pd(dien)Cl]Cl and some nucleosides and nucleotides were studied by nmr. The binding site of guanosine, guanosinemonophosphoric acid, xanthosine, and inosine is N(7). Cytidine is coordinated to palladium through N(3). Adenosinemonophosphate acts as a bidentate, binding two different palladium atoms at N(1) and N(7).The crystal structure of [Pd(dien)(guanosine)](ClO4)2 has been determined by X-ray diffraction. The crystals are orthorhombic, space group P212121, with a = 13.422, b = 14.587, c = 12.432, and Z = 4. The structure was refined by block-diagonal least-squares analysis to a conventional R factor of 0.047 and a weighted Rw = 0.043. The coordination around the palladium atom is square planar. Guanosine is bonded to palladium through N(7). The planar purine ring makes an angle of 63.4° with the palladium coordination plane. The structure is stabilized by hydrogen bonding.


1979 ◽  
Vol 44 (11) ◽  
pp. 3350-3356 ◽  
Author(s):  
Bohumil Kratochvíl ◽  
Jana Podlahová ◽  
Jindřich Hašek

The crystal structure of Co2SiO4 (olivine structure type) was solved by Patterson and Fourier synthesis and refined by the full matrix least squares method. A final value of the R factor of 0.057 was obtained from 911 independent reflection intensities. The structure symmetry corresponds to space group Pnma with lattice parameters a = 1032.8(3), b = 601.9(2) and c = 478.2(1) pm. The unit cell contains four formula units. The Si-O distance in isolated SiO4 tetrahedra varies from 162.1(3) to 165.9(3) pm. Both cobalt atoms are octahedrally surrounded by oxygen atoms with Co-O distances of 208.0(3)-223.1(2) pm.


1983 ◽  
Vol 61 (8) ◽  
pp. 1823-1826 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
R. Melanson

mer-[Rh(DMSO)2(DMF)Cl3] was prepared by dissolving [Rh(DMSO)3Cl3] in dimethylformamide (DMF). It forms monoclinic crystals, a = 11.530(3), b = 8.971(2), c = 15.912(3) Å, β = 107.88(2)°, Z = 4, and space group P21/c. The structure was refined by full-matrix least-squares analysis to a conventional R factor of 0.038 (3495 observed reflections).The coordination around the Rh atom is octahedral. The compound is the peripheral or the 1,2,6-isomer. The DMF molecule is in trans position to a DMSO ligand and bonded to rhodium through the oxygen atom. The two molecules of DMSO are bonded to rhodium through sulfur. The Rh—Cl(1) bond (2.366(1) Å) trans to a DMSO molecule seems slightly longer than the two Rh—Cl bonds trans to each other (2.329(1) and 2.343(1) Å).


1971 ◽  
Vol 49 (2) ◽  
pp. 167-172 ◽  
Author(s):  
F. Leung ◽  
S. C. Nyburg

The crystal structure of a thiathiophthen nitrogen isostere (7) has been solved by X-ray analysis. The crystal belongs to the triclinic system with unit cell dimensions: a = 11.275(11), b = 9.558(10), c = 10.797(10) Å, α = 92.50(10), β = 116.98(10), γ = 92.61(10)°. There are two molecules per unit cell, space group [Formula: see text]. The data were collected by diffractometer with CuKα radiation. The structure was solved by symbolic addition procedures, and fully refined anisotropically using full-matrix least squares to an R factor of 6.3%.The S—S and S—N bond lengths were found to be 2.364 and 1.887 Å, respectively. This reveals the partial bonding character between S … S … N atoms.


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