Trigonal bi- and monopyramidal cobalt(II) complexes of a novel guanidine-based tripodal ligand

Inorganic Chemistry

Volumn 49, Issue 24, 2010, Pages 11261-11263

  Searls, Cassandra E ^a   Kleespies, Scott T ^a   Eppright, Matthew L ^a   Schwartz, Sarina C ^a   Yap, Glenn P A ^b   Scarrow, Robert C ^a  

^a HAVERFORD COLLEGE   (United States)

^b UNIVERSITY OF DELAWARE   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 78650383187     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic101612f     Document Type: Article

References (23)

1. 3tren, tris[(N ′, N ′, N ″, N ″-tetramethylguanidinyl)- N -ethylene]amine; tren, tris(2-aminoethyl)amine.
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10. 1H NMR septet below 100 °C. This could be due to slow rotation around the C-N bonds or could indicate a slow tautomeric equilibrium involving the guanidine protons.
11. Allen, F. H. Acta Crystallogr. 2002, B58, 380-388
12. The CSD (11) (update May 2010) contains 67 instances of -NH(i Pr) moeities within guanidine or guanidinium groups. The |θ| [NCNC(i Pr)] dihedral angles are 14 ± 11 and 167 ± 10° (mean ± e.s.d), with no |θ| between 40 and 140°. The deviations from planarity are larger in an additional 12 examples with -NH(i Pr) as part of the guanidine groups coordinated to metal ions (|θ| = 26 ± 16 and 154 ± 16°), but still there are no |θ| between 50 and 130°.
13. Details of syntheses and crystallography are given in the Supporting Information; see the note at end of paper.
14. The desired 1+ ion mass peak at 525 amu accounts for about 70% of the total ions; the major impurity at 399 amu presumably results from the reaction of only two of the primary amines of tren with DIC. Using an excess of DIC results in the formation of higher mass species (651 and 777 amu), presumed to include biguanidine groups.
15. I) = 0.0708. CCDC 786126. The atomic coordinates for these structure have been deposited with the Cambridge Crystallographic Data Centre. The coordinates can be obtained, upon request, from the Director, Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, U.K.
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