The Crystal Structure of cis-Chlorobis(triethylphosphine)-1,10-phenanthrolineplatinum(II) fluoroborate, (PtCl(PEt3)2(phen))BF4, a Complex Containing Monodentate 1,10-Phenanthroline

1974 ◽  
Vol 52 (8) ◽  
pp. 1367-1376 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Keith R. Dixon ◽  
Masood A. Khan

The crystal structure of cis-chlorobis(triethylphosphine)-1,10-phenanthrolineplatinum(II) fluoroborate has been determined and refined to an R-value of 0.051. The space group is P21/c and the cell dimensions are a = 0.9215(2), b = 1.1991(3), c = 2.6832(6) nm, β = 99.38(3)°, with 4 molecules per unit cell. The interatomic distances to Pt are: Pt—N(1), 213.7(19); Pt—N(2), 284.3(20); Pt—P(1), 223.9(7); Pt—P(2), 224.1(6); Pt—Cl, 236.1(6) pm.The coordination number and geometry is discussed in terms of 5-coordinate tetragonal pyramidal and 4-coordinate square planar models, the latter being regarded as the more acceptable.Monodentate o-phenanthroline is thus observed for the first time in the solid state. The structure of the complex in solution is discussed with the aid of conductance and nuclear magnetic resonance results which suggest the possibility of a novel fluxional system.

1978 ◽  
Vol 56 (4) ◽  
pp. 450-455 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Keith R. Dixon ◽  
Masood A. Khan

The crystal structure of cis-chlorobis(triethylphosphine)-1,8-naphthyridineplatinum(II) tetrafluoroborate has been determined by single crystal X-ray diffraction and refined to an R-value of 0.063. The cell dimensions are a = 1.4246, b = 1.2676, c = 1.6530 nm, β = 115.66°. The space group is P21/c with 4 molecules per unit cell, and the measured density is 1.665 g cm−3. The structure is essentially a 4-coordinate square planar platinum(II) complex containing monodentate 1,8-naphthyridine. Interatomic distances to platinum are: Pt—Cl, 236.6(4); Pt—P(1), 225.4(4); Pt—P(2), 225.2(4); Pt—N(1), 208.3(11); and Pt—N(2), 304.5(14) pm. The structure is discussed in relation to variable temperature nmr studies of solutions, which indicate fluxional behaviour of the heterocyclic ligand.


1990 ◽  
Vol 68 (12) ◽  
pp. 2192-2197
Author(s):  
Jean-Pierre Reboul ◽  
Pierre Brouant ◽  
Jacques Barbe ◽  
Claude Caranoni ◽  
Catherine Soula ◽  
...  

The solid state configuration of 1-isopropyl-2-phenyl-1,3-diaza-6-one-bicyclo[3.3.0]oct-2-ene was determined from X-ray diffraction data (a = 10.039(3) Å; b = 8.683(3) Å; c = 15.505(6) Å; β = 90.72(9)°; P21/c;R = 0.047). This structure is compared to those of three other related (Δ-2)-imidazolines. Molecular structure in solution was investigated by 1H nuclear magnetic resonance spectroscopy. Results clearly indicate that the title compound has the same structure in the solid state as in solution. On the contrary, this configuration differs appreciably from those of other (Δ-2)-imidazolines considered in this report. Keywords: (Δ-2)-imidazolines, crystal structure, NMR, conformations.


1978 ◽  
Vol 56 (6) ◽  
pp. 878-883 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Keith R. Dixon

The crystal structure of cis-chlorobis(triethylphosphine)phthalazineplatinum(II) tetrafluoroborate has been determinee by single crystal X-ray diffraction and refined to an R-value of 0.076 for 1935 reflections. The cell dimensions are a = 1315.7(2), b = 2462.7(4), c = 899.6(3) pm, β = 104.99(2)°. The space group is P21/c with 4 molecules per unit cell, ρo = 1.593, ρc = 1.613 g cm−3. The structure is a square planar 4-coordinate platinum(II) complex with an angle of 80.0° between the plane of the phthalazine molecule and that of the coordination. Interatomic distances to platinum are Pt—Cl, 235.4(9); Pt—P(1), 225.2(8); Pt—P(2), 226.9(8); Pt—N(1), 208(3); and Pt—N(2), 297(3) pm, the phthalazine ligand being monodentate. The structure is compared to previous results and discussed in relation to variable temperature nmr studies of solutions, which show that the heterocyclic ligand exchanges its point of attachment to and fro between N(1) and N(2) by a dissociative mechanism at elevated temperatures.


1978 ◽  
Vol 56 (13) ◽  
pp. 1773-1778 ◽  
Author(s):  
G. W. Bushnell

The crystal structure of di-(μ-hydroxo)tetrakis(triethylphosphine)diplatinum(II)fluoroborate has been determined and refined to an R value of 0.032. The space group is P21/c and the cell dimensions are a = 1.604(1), b = 1.847(1), c = 1.336(1) nm, β = 101.6 °, with 4 molecules per unit cell. The dimeric cation consists of two square planar Pt(II) centres bridged by a pair of hydroxo ligands. The angle between the mean plane normals is 36.4°. One of the BF4− groups, situated close to the dihydroxo bridge on the more open side, and having lower thermal parameters than the second fluoroborate anion, is hydrogen bonded to the oxygen atoms. The hydrogen atoms were not located. The interatomic distances (pm) are Pt—P = 223.5 (mean), Pt—O = 213.3 (mean), Pt(1)—Pt(2) = 312.1(1), O(1)—O(2) = 272(2), O(1)—F(1) = 288(2), O(2)—F(2) = 282(3). The mean bond angles (deg) are O—Pt—O = 79.4, P—Pt—P = 97.7, P—Pt—O = 91.5, and Pt—O—Pt = 94. One of the triethylphosphine groups is disordered or in thermal motion and was refined by constrained least squares using two superimposed partial structures. The results are discussed in relation to other known hydroxo bridged platinum species relevant to the field of platinum containing, cancer chemotherapeutic drugs.


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