Y.-H. Xing , J.-Q. Xu , H.-R. Sun , D.-M. Li , Y. Xing , Y.-H. Lin , H.-Q. Jia
{"title":"含柠檬酸盐配体的新型双核钼(V)硫配合物:K2.5Na2NH4[Mo2O2S2(cit)2].5H2O的合成与表征","authors":"Y.-H. Xing , J.-Q. Xu , H.-R. Sun , D.-M. Li , Y. Xing , Y.-H. Lin , H.-Q. Jia","doi":"10.1016/S0992-4361(99)80014-9","DOIUrl":null,"url":null,"abstract":"<div><p>The complex, K<sub>2.5</sub>Na<sub>2</sub>NH<sub>4</sub>[Mo<sub>2</sub>O<sub>2</sub>S<sub>2</sub>(cit)<sub>2</sub>]·5H<sub>2</sub>O (1), was obtained by crystallization from a solution of (NH<sub>4</sub>)<sub>2</sub>MoS<sub>4</sub>, potassium citrate (K<sub>3</sub>cit) and hydroxyl sodium in methanol and water under an atmosphere of pure nitrogen at ambient temperature. The crystals are triclinic, space group P1¯, a = 7.376 (3)Å, b = 14.620 (2) Å, c = 14.661 (1) Å, α = 71.10 (1)°, β = 81.77 (1)°, γ = 78.27(2)°, R = 0.0584 for 2545 observed (I > 2σ (I)) reflections. Single crystal structure analysis reveals that citrate ligand coordinated to molybdenum atom through two carboxylato oxygens and one deprotonated hydroxyl oxygen together with two bridging sulfur atoms and a terminal oxygen atom completes distorted coordination octahedron around each molybdenum atom. Principal dimensions are Mo = O<sub>1</sub>, 1.707 Å (av); Mo-S<sub>b</sub>, 2.341 Å (av); Mo-O<sub>(hydroxyl)</sub>, 2.021 Å (av); Mo-O<sub>(α-carboxyl)</sub>, 2.1290 Å (av) and Mo-O<sub>(β-carboxyl)</sub>, 2.268(av) Å. IR spectrum is in agreement with the structure.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 10","pages":"Pages 745-756"},"PeriodicalIF":0.0000,"publicationDate":"1998-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(99)80014-9","citationCount":"9","resultStr":"{\"title\":\"A new dinuclear molybdenum(V)-sulfur complex containing citrate ligand: Synthesis and characterization of K2.5Na2NH4[Mo2O2S2(cit)2].5H2O\",\"authors\":\"Y.-H. Xing , J.-Q. Xu , H.-R. Sun , D.-M. Li , Y. Xing , Y.-H. Lin , H.-Q. Jia\",\"doi\":\"10.1016/S0992-4361(99)80014-9\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>The complex, K<sub>2.5</sub>Na<sub>2</sub>NH<sub>4</sub>[Mo<sub>2</sub>O<sub>2</sub>S<sub>2</sub>(cit)<sub>2</sub>]·5H<sub>2</sub>O (1), was obtained by crystallization from a solution of (NH<sub>4</sub>)<sub>2</sub>MoS<sub>4</sub>, potassium citrate (K<sub>3</sub>cit) and hydroxyl sodium in methanol and water under an atmosphere of pure nitrogen at ambient temperature. The crystals are triclinic, space group P1¯, a = 7.376 (3)Å, b = 14.620 (2) Å, c = 14.661 (1) Å, α = 71.10 (1)°, β = 81.77 (1)°, γ = 78.27(2)°, R = 0.0584 for 2545 observed (I > 2σ (I)) reflections. Single crystal structure analysis reveals that citrate ligand coordinated to molybdenum atom through two carboxylato oxygens and one deprotonated hydroxyl oxygen together with two bridging sulfur atoms and a terminal oxygen atom completes distorted coordination octahedron around each molybdenum atom. Principal dimensions are Mo = O<sub>1</sub>, 1.707 Å (av); Mo-S<sub>b</sub>, 2.341 Å (av); Mo-O<sub>(hydroxyl)</sub>, 2.021 Å (av); Mo-O<sub>(α-carboxyl)</sub>, 2.1290 Å (av) and Mo-O<sub>(β-carboxyl)</sub>, 2.268(av) Å. IR spectrum is in agreement with the structure.</p></div>\",\"PeriodicalId\":100507,\"journal\":{\"name\":\"European Journal of Solid State and Inorganic Chemistry\",\"volume\":\"35 10\",\"pages\":\"Pages 745-756\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"1998-11-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://sci-hub-pdf.com/10.1016/S0992-4361(99)80014-9\",\"citationCount\":\"9\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"European Journal of Solid State and Inorganic Chemistry\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0992436199800149\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"European Journal of Solid State and Inorganic Chemistry","FirstCategoryId":"1085","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0992436199800149","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 9
摘要
以(NH4)2MoS4、柠檬酸钾(K3cit)和羟基钠为溶剂，在常温纯氮气氛下，在甲醇和水中结晶，制得配合物K2.5Na2NH4[Mo2O2S2(cit)2]·5H2O(1)。晶体为三斜状，空间群P1¯，a = 7.376 (3)Å， b = 14.620 (2) Å， c = 14.661 (1) Å， α = 71.10(1)°，β = 81.77(1)°，γ = 78.27(2)°，R = 0.0584 (I >2σ (I))反射。单晶结构分析表明，柠檬酸盐配体通过两个羧基氧和一个去质子化羟基与两个桥接的硫原子和一个末端氧原子与钼原子配位，在每个钼原子周围形成畸变配位八面体。主维数为Mo = 1,1.707 Å (av);Mo-Sb, 2.341 Å (av);Mo-O(羟基)，2.021 Å (av);Mo-O(α羧基),2.1290 (av)和Mo-O(β羧基),2.268 (av)。红外光谱与结构一致。
A new dinuclear molybdenum(V)-sulfur complex containing citrate ligand: Synthesis and characterization of K2.5Na2NH4[Mo2O2S2(cit)2].5H2O
The complex, K2.5Na2NH4[Mo2O2S2(cit)2]·5H2O (1), was obtained by crystallization from a solution of (NH4)2MoS4, potassium citrate (K3cit) and hydroxyl sodium in methanol and water under an atmosphere of pure nitrogen at ambient temperature. The crystals are triclinic, space group P1¯, a = 7.376 (3)Å, b = 14.620 (2) Å, c = 14.661 (1) Å, α = 71.10 (1)°, β = 81.77 (1)°, γ = 78.27(2)°, R = 0.0584 for 2545 observed (I > 2σ (I)) reflections. Single crystal structure analysis reveals that citrate ligand coordinated to molybdenum atom through two carboxylato oxygens and one deprotonated hydroxyl oxygen together with two bridging sulfur atoms and a terminal oxygen atom completes distorted coordination octahedron around each molybdenum atom. Principal dimensions are Mo = O1, 1.707 Å (av); Mo-Sb, 2.341 Å (av); Mo-O(hydroxyl), 2.021 Å (av); Mo-O(α-carboxyl), 2.1290 Å (av) and Mo-O(β-carboxyl), 2.268(av) Å. IR spectrum is in agreement with the structure.
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