Synthesis and structural characterization of a tetramolybdate, (Mo sub 4 O sub 12 (C sub 8 H sub 6 N sub 4 )) sup 2 minus , containing a bridging phthalazine-1-hydrazido(2-) ligand. Comparison to the structure of (Mo sub 4 O sub 10 (OMe) sub 2 (NNMePh) sub 2 ) sup 2 minus , a tetramolybdate species exhibiting ligation to a terminal monodentate hydrazido(2-) group
- State Univ. of New York, Albany (USA)
The reaction of (n-Bu{sub 4}N){sub 2}(Mo{sub 2}O{sub 7}) with 1-methyl-1-phenylhydrazine in CH{sub 2}Cl{sub 2}-methanol yields the tetranuclear poly oxomolybdate (n-Bu{sub 4}N){sub 2}(Mo{sub 4}O{sub 10}(OCH{sub 3}){sub 2}(NNMePh){sub 2}) (I). Complex I displays the methoxy-bridged binuclear core (MoO(NNMePh)({mu}-OCH{sub 3}){sub 2}MoO(NNMePh)){sup 2+}, bridged by two double-bridging bidentate (MoO{sub 4}){sup 2{minus}} units. Complex I is structurally related to the class of tetranuclear poly oxomolybdates coordinated to small organic molecules, (Mo{sub 4}O{sub 6-10}L{sub 1}L{sub 2}){sup n-}. The reaction of (n-Bu{sub 4}N){sub 2}(Mo{sub 2}O{sub 7}) with the potentially chelating and bridging hydrazino ligand hydrazinophthalazine, H{sub 2}NNH(C{sub 8}H{sub 5}N{sub 2}) (H{sub 2}-NNH-pht), yields the analogous tetranuclear species (n-Bu{sub 4}N){sub 2}(Mo{sub 4}O{sub 12}(HNN-pht))(II). Although structurally related to I, II reveals a number of distinctive features. The binuclear core (Mo{sub 2}O{sub 4}HNN-pht){sup 2+} displays a bridging oxo group and a bidentate bridging phthalazine moiety, in contrast to the two bridging methoxy groups of I. The Mo centers of this core are nonequivalent, one exhibiting MoO{sub 4}N{sub 2} coordination and the other (MoO{sub 5}N). The bridging (MoO{sub 4}){sup 2{minus}} moieties display unexceptional geometry. The {sup 17}O NMR spectra of I, II, and the related 1,4-dihydrazinophthalazine derivative (Mo{sub 4}O{sub 11}(C{sub 8}H{sub 6}N{sub 6})){sup 2{minus}} are consistent with the solid-state structures, exhibiting resonances in the regions assigned to doubly bridging Mo{sub 2}O groups (350-450 ppm) and to terminal MoO groups (750-950 ppm). Crystal data for the complexes are reported. 28 references, 3 figures, 7 tables.
- OSTI ID:
- 5208176
- Journal Information:
- Inorganic Chemistry; (USA), Vol. 27:11; ISSN 0020-1669
- Country of Publication:
- United States
- Language:
- English
Similar Records
Reactions of oxomolybdenum(VI) hydroxamate and thiohydroxamate complexes with hydrazines. Syntheses and structures of a diazenido-hydrazido(1-) complex containing an end-on-bonded hydrazido(1-) ligand and of a diazene-diazenido(1-) derivative
Alkoxy and aryloxy derivatives of (pentamethylcyclopentadienyl)ruthenium. X-ray crystal structures of ((. eta. sup 5 -C sub 5 Me sub 5 )Ru(. mu. -OMe)) sub 2 , ((. eta. sup 5 -C sub 5 Me sub 5 )(CO)Ru(. mu. -OEt)) sub 2 , and (. eta. sup 5 -C sub 5 Me sub 5 )Ru(. eta. sup 5 -2,6- sup t Bu sub 2 C sub 6 H sub 3 O) and molecular orbital analysis of ((. eta. sup 5 -C sub 5 H sub 5 )Ru(. mu. -OMe)) sub 2
Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ALKANES
CRYSTAL STRUCTURE
MOLECULAR STRUCTURE
SYNTHESIS
AROMATICS
MOLYBDENUM COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
EXPERIMENTAL DATA
NMR SPECTRA
OXYGEN 17
DATA
EVEN-ODD NUCLEI
HYDROCARBONS
INFORMATION
ISOTOPES
LIGHT NUCLEI
NUCLEI
NUMERICAL DATA
ORGANIC COMPOUNDS
OXYGEN ISOTOPES
REFRACTORY METAL COMPOUNDS
SPECTRA
STABLE ISOTOPES
TRANSITION ELEMENT COMPOUNDS
400201* - Chemical & Physicochemical Properties
400202 - Isotope Effects
Isotope Exchange
& Isotope Separation