Transition metal chemistry of main group hydrazides. 4. Phosphorus hydrazido ferrocences as novel synthons to new iron(II)-palladium(II) heterotrimetallic organometallic compounds. Synthesis and characterization of palladium(II) chloride complexes of ferrocene functionalized phosphorus hydrazides. Single-crystal x-ray structures of C[sub 2]H[sub 5]OP(S)(NCH[sub 3]NCHCp[prime]FeCp)[sub 2] and C[sub 2]H[sub 5]OP(S)(NCH[sub 3]NCHCp[prime]FeCp)[sub 2]-PdCl[sub 2] [Cp[prime] = C[sub 5]H[sub 4], Cp = C[sub 5]H[sub 5]]

Journal Article · Tue Feb 01 00:00:00 EST 1994 · Organometallics; (United States)

DOI:https://doi.org/10.1021/om00014a027· OSTI ID:7235493

Katti, K V; Ge, Y W; Singh, P R; Date, S V; Barnes, C L ^[1]

---

1. Univ. of Missouri, Columbia, MO (United States)

The reactions of aryl-, alkyl-, and alkoxy-substituted phosphorus hydrazides, RP(E)(NMeNH[sub 2])[sub 2] (R = Ph, E = S, I; R = OEt, E = S, 2; R = Ph, E = O, 3; R = Et, E = O, 4; R = Me, E = O, 5) with ferrocenecarboxaldehyde gave metallocene-functionalized phosphorus hydrazides in good yields (approximately 90-95%) as air-stable crystalline solids with the following chemical compositions: RP(E)(NMeNCHCp[prime]FeCp)[sub 2] (R = Ph, E = S, 6; R = OEt, E = S, 7; R = Ph, E = O, 8; R = Et, E = O, 9; R = Me, E = O, 10). These ferrocenyl phosphorus hydrazides 6-10 can be used as versatile synthons to produce new heterometallic organometallic compounds. The chemical constitutions of 6-10 and 11-15 were established by complete NMR ([sup 1]H and [sup 31]P) spectroscopic and C, H, and N analysis. As representative examples, X-ray structures of 7 and 12 have been determined. Crystal data for C[sub 2]H[sub 5]OP(S)(NMeNCHCp[prime]FeCp)[sub 2], 7: orthorhombic, space group P2[sub 1]2[sub 1]2[sub 1], a = 7.5556(11) [angstrom], b = 10.7652(12) [angstrom], c = 33.186(4) [angstrom], V = 2699.3(3) [angstrom][sup 3], Z = 4. The structure was solved by direct methods and was refined to R = 0.038. The structure of 12 comprises the neutral monomeric trimetallic complex C[sub 2]H[sub 5]OP(S)(NMeNCHCp[prime]FeCp)[sub 2][center dot]PdCl[sub 2] with the Pd(II) center in a square planar geometry. The structure of 12 is characterized by a six-membered ring with the Pd(II) bonded to two terminal hydrazine units of 7 in a cis disposition. Crystal data of 12: monoclinic, space group P2[sub 1]/c, a = 15.731(3) [angstrom], l = 18.695(3) [angstrom], c = 11.918(2) [angstrom], [beta] = 98.180(7)[degree], V = 3469.3(10) [angstrom][sup 3], Z = 4. The structure was solved by direct methods and was refined to R = 0.033. 21 refs., 2 figs., 6 tabs.

• OSTI ID: 7235493
• Journal Information: Organometallics; (United States), Vol. 13:2; ISSN 0276-7333
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
IRON COMPLEXES
MOLECULAR STRUCTURE
SYNTHESIS
PALLADIUM COMPLEXES
AROMATICS
COMPILED DATA
CRYSTALLOGRAPHY
HYDRAZIDES
NUCLEAR MAGNETIC RESONANCE
ORGANOMETALLIC COMPOUNDS
PHOSPHORUS COMPOUNDS
COMPLEXES
DATA
INFORMATION
MAGNETIC RESONANCE
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
RESONANCE
TRANSITION ELEMENT COMPLEXES
400201* - Chemical & Physicochemical Properties
400102 - Chemical & Spectral Procedures