The reactions between[Mo(NO)(tp*)I
2] {tp* =HB(3,5-Me
2C
3HN
2)
3}and HE-EH {HE-EH =1,3-(HSCH
2)
2C
6H
4and 1,4-(HSCH
2)
2C
6H
4}afford the cyclic dimers[Mo(NO)(tp*)(E-E)]
2 and cyclic trimers[Mo(NO)(tp*)(E-E)]
3.These reactions also produce the monometallomacrocycles[Mo(NO)(tp*)(E-E)
x](
x = 2, 3) and, from1,3-(SCH
2)
2C
6H
4,[Mo(NO)(tp*){(3-SCH
2C
6H
4CH
2)
2S}].The reaction between [Mo(NO)(tp*)I
2]and 1,2-(HSCH
2)
2C
6H
4 affords, asits major product, the chelate complex[Mo(NO)(tp*){1,2-(SCH
2)
2C
6H
4}],nometallomacrocycles bein
g found amon
g the reaction products in thiscase. Cyclic voltammo
grams of themacrocyclic complexes contain sin
gle reduction waves in the re
gion-1.374 to -1.486 V (vs ferrocene/ferrocenium), and the binuclear metallomacrocycles show noelectrochemically resolvable metal-metal interactions.The molecular structures of[Mo(NO){HB(3,5-Me
2C
3HN
2)
3}{1,4-(SCH
2)
2C
6H
4}
n](
n = 2, 3) have been determinedcrystallo
graphically:[Mo(NO){HB(3,5-Me
2C
3HN
2)
3}{1,4-(SCH
2)
2C
6H
4}
2],C
31H
38BMoN
7OS
4,orthorhombic,space
group
Pna2
1,
a =16.193(8) &Arin
g;,
b = 12.878(5) &Arin
g;,
c =16.620(5) &Arin
g;,
Z = 4;[Mo(NO){HB(3,5-Me
2C
3HN
2)
3}{1,4-(SCH
2)
2C
6H
4}
3],C
39H
46BMoN
7OS
6,monoclinic space
group
P2
1/
n,
a = 19.140(5) &Arin
g;,
b =10.708(3)&Arin
g;,
c = 22.072(5) &Arin
g;,
![](/ima<font color=)
ges/
gifchars/beta2.
gif" BORDER=0 ALIGN="middle"> = 100.73(2)
![](/ima<font color=)
ges/entities/de
g.
gif">,
Z = 4.