Herein, we report a magnetically retrievable mixed-valent Fe3O4@SiO2/Pd0/PdIINP (5) nanocomposite system for tandem Suzuki coupling/transfer hydrogenation reaction. The nanocomposite 5 was prepared first by making a layer of $$\hbox {SiO}_{2}$$
SiO
2
on $$\hbox {Fe}_{3}\hbox {O}_{4}\hbox {NP}$$
Fe
3
O
4
NP
followed by deposition of $$\hbox {Pd}^{0}$$
Pd
0
and sorption of $$\hbox {Pd}^{\mathrm{II}}$$
Pd
II
ions successively onto the surface of Fe3O4@SiO2NP. The nanocomposite was characterized by powder XRD, electron microscopy (SEM-EDS and TEM-EDS) and XPS spectroscopy techniques. The mixed-valent $$\hbox {Pd}^{0}/\hbox {Pd}^{\mathrm{II}}$$
Pd
0
/
Pd
II
present onto the surface of nanocomposite 5 was confirmed by XPS technique. Interestingly, the mixed-valent nanocomposite Fe3O4@SiO2/Pd0/PdIINP (5) exhibited tandem Suzuki coupling/transfer hydrogenation reaction during the reaction of aryl bromide with aryl boronic acid (90% of C). The nanocomposite 5 displayed much better reactivity as compared to the monovalent Fe3O4@SiO2/Pd0NP (3) (25% of C) and Fe3O4@SiO2/PdIINP (4) (15% of C) nanocomposites. Further, because of the presence of magnetic $$\hbox {Fe}_{3}\hbox {O}_{4}$$
Fe
3
O
4
, the nanocomposite displayed its facile separation from the reaction mixture and reused at least for five catalytic cycles.