
TY  - JOUR
A1  - Dance, IG 
A1  - Guerney, PJ 
A1  - Rae, AD 
A1  - Scudder, ML 
A1  - Baker, AT 
T1  - Metal-Complexes of Thiocholinate, -SCH<sub>2</sub>CH<sub>2</sub>Nme<sub>3</sub><sup>+</sup>. I. Preparation and Crystal-Structure of Pentakis(Thiocholinato)Dilead(II) Hexafluorophosphate
JF  - Australian Journal of Chemistry
JO  - Aust. J. Chem.
Y1  - 1986
VL  - 39
IS  - 3
SP  - 383
EP  - 398
KW  - 
UR  - https://doi.org/10.1071/CH9860383 
N2  - Aqueous solutions containing lead(II) and deprotonated  thiocholine contain water-soluble homoleptic lead thiolates , which crystallize as yellow needles of [Pb2(SCH2CH2NMe3)5] (PF6)4 in the presence of PF6-, but crystallize [ Pb (SCH2CH2NMe3)2](ClO4)2 with 1 : 2 stoichiometry in the presence of ClO4-. Crystalline [Pb2(SCH2CH2NMe3)5](PF6)4 contains almost linear chains composed of end-linked {(SR)2Pb(&#956;-SR) Pb (SR)2} coordination units, within which the primary Pb -S coordination (mean 2.73 &#506;, sample e.s.d . 0.10 &#506;) is orthogonal trigonal (S- Pb -S, mean 88.9&#176;, sample e.s.d .3.7&#176;) at each lead atom. Within the {Pb2(SR)5} unit there is one double bridge with two rimary bonds, and one double bridge involving one secondary Pb --S connection (mean 3.23 &#506;, sample e.s.d . 0.12 &#506;). Three double-bridges involving secondary Pb --S coordination link the ends of the dimetallic units, and consequently bis - and tris -double thiolate bridges alternate along the chain. Overall coordination at each lead atom is pseudo-octahedral, with one non-bonding electron pair and two cis secondary Pb --S bonds. The cationic tails of the ligands radiate from the chains into a matrix of PF6- ions, and the chains are approximately hexagonally close-packed with a separation of 14.4 &#506;. Along the b axis there are homogeneous stacks of the ammonium functions, the anions, and the Pb, S chains, with a pseudo-symmetric repeat of b/3 in each stack, allowing disorder due to stacking faults. This disorder has been adequately modelled in the refinement, which also incorporated back-Fourier-transform techniques to avoid inaccuracies due to spherically disordered PF6- ions. Crystal data: Cc, 25.535(8), b 43.13(1), c 15.123(5)&#506;, &#946; 100.36(9)&#176;, Z 12 (&#215; Pb2S5C25H65N5P4F24), 3585 observed data, R 0.066. 
ER  -

