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The hetero-metal clusters [■~5-C_5H_4C(O)CH_2CH_2C(O)OCH_3]FeCoM(■_3-S)(CO)_8 (M = Mo 1, M = W 2) were prepared by thermal reactions of FeCo2(CO)9((3-S) with metal exchange reagent [■~5-C_5H_4C(O)CH_2CH_2C(O)OCH_3]M(CO)3Na (M = Mo or W) in THF. Cluster 1 reacted with 2,4-dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative ((3-S)CoFeMo(CO)8[(5-C5H4C(NR)Me] [R = NHC6H_3-2,4-(NO2)2] 3. All the compounds were characterized by elemental analyses, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P, a = 8.148(2), b = 10.685(3), c = 13.410(4) ?, ( = 100.077(5), ( = 102.452(5), ( = 91.108(6)(, V = 1120.4(5) ?3, Z = 2, Dc = 1.915 g/cm3, F(000) = 636, ( = 2.071 mm(1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I > 2((I)).
The hetero-metal clusters [■ ~ 5-C_5H_4C (O) CH_2CH_2C (O) OCH_3] FeCoM (■ _3-S) (CO) _8 (M = Mo 1, M = W 2) were prepared by thermal reactions of FeCo 2 (M = Mo or W) in THF. Cluster 1 reacted with 2,4 (CO) 9 (3-S) with metal exchange reagent [5-5C_5H_4C (O) CH_2CH_2C (O) OCH_3] M -dinitrophenylhydrazine at room temperature to yield the cluster hydrazone derivative (3-S) CoFeMo (CO) 8 [(5-C5H4C (NR) Me] [R = NHC6H_3-2,4- (NO2) 2] compounds were characterized by elemental analyzes, IR and NMR spectra. Cluster 1 was determined by single crystal X-ray diffraction. Crystal data: C18H11O11SCoFeMo, Mr = 646.05, triclinic, space group P, a = 8.148 (2), b = 10.685 3 = 1, Z = 2, Dc = 1.915 g, V = 1120.4 (5) ?, c = 13.410 ?,? = 100.077 ?,? = 102.452? / cm3, F (000) = 636, (= 2.071 mm (1, the final R = 0.0378 and wR = 0.0968 for 5074 observations with (I> 2 (I)).