Synthesis, characterization and crystal structures of two polymorphs of the iodo-bridged ruthenium salt, μ-iodido-bis{η5-cyclopentadienyl-dicarbonyl-ruthenium(II)} tetrafluoroborate

被引：5

作者：

Nyawade, Eunice A. ^{[1
]}

Friedrich, Holger B. ^{[1
]}

M'thiruaine, Cyprian M. ^{[1
]}

Omondi, Bernard ^{[1
]}

机构：

[1] Univ KwaZulu Natal, Sch Chem & Phys, ZA-4000 Durban, South Africa

来源：

JOURNAL OF MOLECULAR STRUCTURE | 2013年 / 1048卷

关键词：

Cyclopentadienylruthenium carbonyl; Iodo-bridged; Cationic complex; Diruthenium complex salt; Polymorphs; Crystal structure; HALIDE ABSTRACTION; COMPLEXES; DERIVATIVES; CHEMISTRY; HALOGENS; CATION;

D O I：

10.1016/j.molstruc.2013.05.050

中图分类号：

O64 [物理化学（理论化学）、化学物理学];

学科分类号：

070304 ; 081704 ;

摘要：

The reaction of RpI (Rp = (eta(5)-C5H5)Ru(CO)(2)) and AgBF4 in two different solvents, tetrahydrofuran and dichloromethane afforded two polymorphs of the iodo-bridged cationic complex [Rp(2)I]BF4. Polymorph I precipitates out of solution as yellow broad-shaped blocks while polymorph II crystallises out as thin-shaped blocks. While I crystallizes in the monoclinic P2/c space group with a = 12.0982(5) angstrom, b = 9.7923(4) angstrom, c = 15.5321(6) angstrom, beta = 102.9880(10)degrees, polymorph (II) crystallizes in the monoclinic P2(1)/c with a = 7.00560(10) angstrom, b = 14.1446(3) angstrom, c = 18.2226(3) angstrom, beta = 96.2390(10)degrees. The IR spectra of the compound showed the presence of terminal carbonyl groups but the absence of bridging carbonyl groups. Thermal studies of the two polymorphs reveal very close melting points, 432.2 and 435.2 K for I and II respectively. The enthalpies associated with their melting points are +15.1 kJ mol(-1) and +21.9 kJ mol(-1) for polymorphs I and II, respectively. ESI-mass spectroscopy showed the presence of a number of statistically possible combinations of the cationic species. The two polymorphs have also been characterized using DSC, IR and NMR. (c) 2013 Elsevier B.V. All rights reserved.

引用

页码：426 / 433

页数：8

共 17 条

[11] SYNTHESIS AND REACTIVITY OF BINUCLEAR PYRAZOLATE-BRIDGED RUTHENIUM(I) COMPLEXES - CRYSTAL-STRUCTURES OF BIS[MU-(3,5-DIMETHYLPYRAZOLATO-NN')-TRICARBONYLRUTHENIUM(I)] (RU-RU) AND BIS[MU-(3,5-DIMETHYLPYRAZOLATO-NN')]-MU-IODO-BIS[TRICARBONYLRUTHENIUM(II)] TRI-IODIDE
CABEZA, JA
LANDAZURI, C
ORO, LA
BELLETTI, D
TIRIPICCHIO, A
CAMELLINI, MT
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1989, (06): : 1093 - 1100
[12] SYNTHESIS, STRUCTURE, AND MAGNETIC-PROPERTIES OF FLUORIDE-BRIDGED COPPER(II) DIMERS - CRYSTAL AND MOLECULAR-STRUCTURES OF BIS(MU-FLUORO)BIS[TRIS(3,4,5-TRIMETHYLPYRAZOLE-N-2)COPPER(II)] BIS(TETRAFLUOROBORATE) AND BIS(MU-FLUORO)BIS[(5-METHYLPYRAZOLE-N-2)BIS(3,5-DIMETHYLPYRAZOLE-N-2)COPPER(II)] BIS(TETRAFLUOROBORATE
RIETMEIJER, FJ
DEGRAAFF, RAG
REEDIJK, J
INORGANIC CHEMISTRY, 1984, 23 (02) : 151 - 156
[13] BIS(CYCLOPENTADIENYL) CLUSTERS OF RUTHENIUM - THE SYNTHESIS, CHARACTERIZATION AND MOLECULAR-STRUCTURES OF [RU5C(CO)10(ETA(5)-C5H5)2] AND [RU6C(CO)12(ETA(5)-C5H5)2]
BLAKE, AJ
DYSON, PJ
GASH, RC
JOHNSON, BFG
TRICKEY, P
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1994, (07): : 1105 - 1108
[14] THE CHEMISTRY OF CYCLOPENTADIENYL-RUTHENIUM AND CYCLOPENTADIENYL-OSMIUM COMPLEXES .5. THE SYSTEMATIC SYNTHESIS OF NOVEL BRIDGED DIRUTHENIUM CATIONS CONTAINING CYCLOPENTADIENYL AND BIDENTATE AMINE LIGANDS - THE CRYSTAL AND MOLECULAR-STRUCTURE OF [((ETA-5-C5H5)RU(1,10-PHEN))2(MU-DPPM)](PF6)2.CH2CL2 [DPPM=BIS(DIPHENYLPHOSPHINO)METHANE - PHEN=PHENANTHROLINE]T
ALBERS, MO
LILES, DC
ROBINSON, DJ
SINGLETON, E
ORGANOMETALLICS, 1987, 6 (10) : 2179 - 2189
[15] PHOSPHINOALKYLSILYL COMPLEXES .7. SYNTHESIS AND REACTIVITY OF OCTAHEDRAL, BIS(CHELATE)DICARBONYL COMPLEXES OF RUTHENIUM(II) AND OSMIUM(II) - CONFORMATIONAL PROPERTIES OF THE BIS(CHELATE) FRAMEWORK AND X-RAY CRYSTAL-STRUCTURES OF [RU(PPH2CH2CH2SIME2)2(CO)2] OR [OS(PPH2CH2CH2SIME2)2
HOLMESSMITH, RD
STOBART, SR
VEFGHI, R
ZAWOROTKO, MJ
JOCHEM, K
CAMERON, TS
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1987, (05): : 969 - 974
[16] STRUCTURAL CHARACTERIZATION OF POLY(1-PYRAZOLYL)BORATE-METAL AND POLY(1-PYRAZOLYL)METHANE-METAL COMPLEXES CONTAINING CARBOCYCLIC PI-ACCEPTOR LIGANDS - SYNTHESIS AND CRYSTAL AND MOLECULAR-STRUCTURES OF [TETRAKIS(1-PYRAZOLYL)BORATO](ETA6-BENZENE)RUTHENIUM(II) HEXAFLUOROPHOSPHATE AND [HYDROTRIS(1-PYRAZOLYL)BORATO](ETA5-PENTAMETHYLCYCLOPENTADIENYL)RHODIUM(II) HEXAFLUOROPHOSPHATEA
RESTIVO, RJ
FERGUSON, G
OSULLIVAN, DJ
LALOR, F
INORGANIC CHEMISTRY, 1975, 14 (12) : 3046 - 3052
[17] Lanthanocene chemistry with [CpR]-, [Cpt]-, [Cptt]-, and [CpR′2SiMe2]2- ligands:: Synthesis and characterization of bis(cyclopentadienyl)lanthanide(III) halides and bis(cyclopentadienyl)lanthanide(II) complexes and crystal structures of [{NdCpR2(μ-Cl)}2], [{TmCptt2(μ-I)}2], and [Yb(CpR′2SiMe2)(THF)2] (CpR = η5-C5H4{CH(SiMe3)2}, Cpt = η5-C5H4(SiMe2But), Cptt = η5-C5H3(SiMe2But)2-1,3, and CpR′ = η5-C5H3{CH(SiMe3)2}-3)
Hitchcock, PB
Lappert, MF
Tian, S
ORGANOMETALLICS, 2000, 19 (17) : 3420 - 3428

← 1 2 →