Synthesis And Structural Studies Of Organic-Inorganic Compounds Containing Multichloroantimonate, And The Application Of SbCl₃ In Separation

The use of trichloroantimony is abroad. As a kind of Lewis solidacid, trichloroantimony can catalyze some organic reaction. Because offormation of colour complex when trichloroantimony react with someorganic compound it is used to be analyze reagent in analytical chemistry.Due to the anticancer activity, trichloroantimony is a good medicament toleucocythemia and malignant lymphoma. With the relatively low priceand extensive use, researches of new compound containing or synthesizeby trichloroantimony will make a great sense.New organic-inorganic heterocompounds containingmultichloroantimonate mentioned in the paper are synthesized bytrichloroantimony reacts with some common organic compound or somemedical compound in condition of existence of hydrochloric acid. Andcrystals gained in the reactions are characterized by X-ray diffraction andIR, etc. The crystal data of the compounds is helpful to collect more basicdata for developing new medicine of trichloroantimony. In these crystals, multichloroantimonates form dimmer or connect to from chain bysecondary bonds．The crystallographical results of the compounds arelisted as follows:The complex of Bis(N-methylpiperazinium) bis [pentachloroantimonate(â…¢)]dihydrate crystallizes in the monoclinic space group P-1with a=7．8952(2)(?),b=9．5289(3)(?),c=19．3386(5)(?),β=90．0040(10)°,V=1425．85(7)(?),Z=3．In the compound,the N atoms ofpiperazin cycles are protonated．The N-methylpiperaziniums are linked toSbCl₅²- and H₂O by hydrogen bonds．The complex of Bis(2-amino-6-methylpyridinium)di-μ-chloro-oxo-μ-bis[dichloroantimonate(â…¢)]dihydrate crystallizes in the monoclinicspace group P2₁ with a=10．0746(10)(?),b=15．1972(16)(?),c=15．4631(14)(?),β=101．597(6)°,V=2319．2(4)(?),Z=4.In thecompound,the N atoms of 2-amino-6-methylpyridines are protonated．The 2-amino-6-methylpyridiniums are linked to Sb₂Cl₆O^2- by hydrogenbonds．The complex of Bis(2,6-dimethylpyridinium)-μ-chloro-heptachlorodiantimonate(â…¢)crystallizes in the truclinic space group P-1with a=7．605(2)(?),b=9．445(2)(?),c=17．526(4)(?),β=87．248(11)°,V=2058．7(4)(?),Z=2．In the compound,the N atoms of2,6-dimethylpyridines are protonated．One 2,6-dimethylpyridinium islinked to Sb₂Cl₈^2- by one hydrogen bond． The complex of Bis(dimethylammonium)pentachloroantimonace(â…¢)crystallizes in the monoclinic space group P2(1)／n with a=10．810(4)(?),b=10．3294(8)(?),c=13．522(5)(?),β=108．489°,V=1431．9(9)(?),Z=13．In the compound,the N atoms of dimethylamines are protonated．The complex of 2-methylpiperazinium pentachloroantimonate(â…¢)monohydrate crystallizes in the monoclinic space group P 2(1)／n with a=9．600(4)(?),b=7．934(2)(?),c=19．499(7)(?),β=101．36(11)°,V=1456．19(9)(?),Z=4．In the compound,the N atoms of piperazin cycleare protonated．H₂O is linked to SbCl₅^2- and the 2-methylpiperazinium byhydrogen bonds．The complex of Bis(Amprolium) tetrachloroantimonate(â…¢) -μ-dichloro-bis(trichloroterbiunl)4-methylbenzene sulfonate crystallizes inthe triclinic space group (?)2(1)／m with a=12．9316(11)(?),b=16．0071(15)(?),c=13．4783(12)(?),β=104．36(2)°,V=2702．8(4)(?),Z=19．In the compound,the N atoms of amprolium,the crystallographicalstructrue of which is determined for the first time,are protonated．And4-methylbenzene sulfonic acid exits in anion way．The complex of Doxofylline tetrachloroantimonate(â…¢)monohydratecrystallizes in the triclinic space group P-1 with a=8．9783(5)(?),b=10．4727(5)(?),c=11．0357(4)(?),β=82．671(2)°,V=959．10(8)(?),Z=2．In the compound,the N atoms of doxofylline are protonated．H₂O islinked to SbCl₄^- and the protonated doxofylline by hydrogen bonds． The complex of Bis(4-methylpyridinium)pentachloroantimonate(â…¢)crystallizes in the truclinic space group P-1 with a=8．9815(13)(?),b=10．4501(16)(?),c=10．7488(16)(?),β=110．180(3)°,V=918．9(2)(?),Z=2.In the compound, the N atoms of 4-methylpyridines are protonated.The 4-methylpyridinium is linked to SbCl₅^- by hydrogen bonds.Crystallization separation, which is popular in organic compoundseparation now because of high effectiveness and low energy, is a processof separation or purification to get a pure compound by solidification.The study of separation of 4-methylpyridine from mixed methylpyridineby crystallization with trichloroantimony is an attempt to separate organiccompound, which are difficult to be separated by distillation orrectification. It is the study of cocrystallization separation of organiccompound and metal salt. And the data of the experiment prove that theproduct purity and yield are over 90%. In addition, as a kind of Lewisacid, trichloroantimony catalyzes 2-methylpiperazine to split up fromlomefloxacin and separates 2-methylpiperazine by cocrystallization incertain conditions. This discovery will be helpful to the sduty ofintegrated reaction-separation process.