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The design, synthesis, and applications of new boranes are eternal topics in boron chemistry. A new bis(borane)alkanethiolate salt, K[BH 3 S(CH 3 )BH 3 ], was synthesized in high yield by the reaction of K with (CH 3 ) 2 S·BH 3 at room temperature. The formation mechanism was elucidated based on experimental and theoretical studies. The single-crystal structure of the K[BH 3 S(CH 3 )BH 3 ]·18-crown-6 adduct was determined in which the B-S-B bonding information of K[BH 3 S(CH 3 )BH 3 ] was illustrated for the first time. Using K[BH 3 S(CH 3 )BH 3 ] as a starting material, KB 3 H 8 was successfully synthesized.

Improved methods for the synthesis of KB 3 H 8 , NH 3 B 3 H 7 , and N -alkyl analogues of NH 3 B 3 H 7 have been developed based on previous works. KB 3 H 8 was synthesized by the reaction of metallic potassium (K) with borane dimethyl sulfide ((CH 3 ) 2 S·BH 3 ) with high yield and atom-economy. In the preparation of NH 3 B 3 H 7 and its N -alkyl analogues, KB 3 H 8 served as a starting material and was converted to THF·B 3 H 7 first through reactions with HCl diethyl ether solution or oxidation agent CoCl 2 . Then, the formed THF·B 3 H 7 in situ reacted with the corresponding ammonia or amines to form the amine borane final products. This work paves an alternative way for preparing organic-inorganic hybrid materials containing B, N, and C atoms.

The reactions of sodium amidoborane (NaNH 2 BH 3 ) with NiBr 2 have been investigated, and the results showed that black precipitate 1 including the NiBNH x composites could be obtained. From the aqueous solution of the precipitate 1 , the hydrolysis product Ni-B ( 2 ) was isolated and characterized. Both the in situ formed precipitate 1 and the hydrolysis product 2 can catalyze the formation of Na[BH 3 (NH 2 BH 2 ) 2 H]. CoCl 2 showed comparable performance with NiBr 2 . Based on these results, a facile method for the synthesis of Na[BH 3 (NH 2 BH 2 ) 2 H] has been developed. This work provides insights into studying experimental methods for the synthesis of long B/N chain complexes and developing boron and nitrogen chemistry.