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Download Author Version (PDF) Chemical Science Accepted Manuscript This is an Accepted Manuscript, which has been through the Royal Society of Chemistry peer review process and has been accepted for publication. Accepted Manuscripts are published online shortly after acceptance, before technical editing, formatting and proof reading. Using this free service, authors can make their results available to the community, in citable form, before we publish the edited article. We will replace this Accepted Manuscript with the edited and formatted Advance Article as soon as it is available. You can find more information about Accepted Manuscripts in the Information for Authors. Please note that technical editing may introduce minor changes to the text and/or graphics, which may alter content. The journal’s standard Terms & Conditions and the Ethical guidelines still apply. In no event shall the Royal Society of Chemistry be held responsible for any errors or omissions in this Accepted Manuscript or any consequences arising from the use of any information it contains. www.rsc.org/chemicalscience Page 1 of 5 Chemical Science Chemical Science RSC Publishing ARTICLE Addition of pnictogen atoms to chromium(II): synthesis, structure and magnetic properties of a Cite this: DOI: 10.1039/x0xx00000x chromium(IV) phosphide and a chromium(III) arsenide Received 00th January 2012, Accepted 00th January 2012 Sabine Reisinger, a Michael Bodensteiner, a Eufemio Moreno Pineda, b,c Joseph J. b a, b, DOI: 10.1039/x0xx00000x W. McDouall, Manfred Scheer * and Richard A. Layfield * www.rsc.org/ Chromium(II) chloride reacts with lithium pentamethylcyclopentadienide (LiCp*, Cp* = 5 C5Me 5) and LiE(SiMe 3)2 (E = P or As) to give the heterocubane chromium phosphide [( η - 5 Cp*Cr)( µ3-P)] 4 (1) or the chromium arsenide cage [( η -Cp*Cr) 3(µ3-As) 2] ( 2), respectively. The crystal and molecular structures of both compounds have been determined by X-ray crystallography. The reactions represent unusual oxidative additions of pnictogen atoms to Manuscript chromium(II), which in the case of 1 results in the formation of the unusual chromium(IV) formal oxidation state, and in the case of 2 provides access to chromium(III). Compound 1 is also a rare example of a transition metal µ3-phosphide-ligated cubane. Magnetic susceptibility and magnetization measurements, with support from DFT calculations, indicate S = 2 and S = 9/2 ground states for 1 and 2, respectively, which can be rationalized by considering the electronic structure in terms of chromium-chromium bonding. Introduction spin S = 2 ions was found to be strong and also pnictogen- dependent, with exchange coupling constants of J = –166 cm –1 –1 Cluster compounds containing unsubstituted group 15 element for E = P and J = –77.5 cm for E = As (2 J formalism). The Accepted antiferromagnetic exchange in the manganese(II) analogues is ligands of the type [E ] (E = P or As, n ≥ 1), or so-called n more than an order of magnitude weaker, but these compounds ‘naked’ pnictogen ligands, continue to attract considerable are more noteworthy because of their S = 5/2 to S = 3/2 spin interest due to their remarkable structural diversity, and also crossover properties. In the case of the arsenide-bridged because of the opportunities for using the clusters themselves as 1 manganese(II) dimer, the spin crossover is a two-step process novel ligands and in supramolecular chemistry. Synthetic that shows hysteresis at 96-105 K in the temperature routes to [E ]-containing coordination compounds are well n dependence of the magnetic susceptibility. developed, particularly in the case of phosphorus, with The spin configurations of first-row transition metal Cp activation reactions of white phosphorus, P , proving to be a 4 complexes can be very sensitive to the ligand substituents, particularly successful source of [P n] complexes, including 8 2 particularly in the case of manganese(II) and, to a lesser extent, Science complexes of P itself. Although somewhat less extensive 4 chromium(II). 9 Chromocene itself has a low-spin, S = 1 owing to greater technical challenges, analogous chemistry with 10 – – configuration, but substituting a [Cp] ligand by [(Me 3Si) 2E] yellow arsenic, As 4, leading to complexes of [As n] ligands, has µ also been reported. 3 Recently, Cummins et al . have also to give [CpCr{ -E(SiMe 3)2}] 2 (E = P or As) evidently weakens the ligand field sufficiently to give high-spin S = 2 developed a series of transition metal complexes based on the 6 naked mixed-pnictogen starting material P As. 4 chromium(II). In an attempt to induce thermal spin crossover 3 µ One branch of coordination chemistry in which the potential in [CpCr{ -E(SiMe 3)2}] 2 by forcing the ground state of the metal to switch from S = 2 to S = 1 with the aid of a stronger of [E n] ligands has been underexploited is molecular magnetism. Indeed, there is a general paucity of studies ligand field, we have targeted the analogous pentamethyl- µ addressing the magnetic properties of compounds containing P- cyclopentadienyl (Cp*) dimers [(Cp*)Cr{ -E(SiMe 3)2}] 2. y– and As -donor ligands of the type [R xE] , where x = 2 and y = 1, 5 x = 1 and y = 2, or x = 0 and y = 3. We recently reported Chemical studies of the P- and As -mediated exchange coupling in the Results and discussion phosphide- and arsenide-bridged dimers [( η5-Cp)M{ µ- 6 7 µ E(SiMe 3)2}] 2, with M = Cr(II) or Mn(II), and determined the The method used to synthesize [CpCr{ -E(SiMe 3)2}] 2, in which exchange coupling constants via phenomenological spin Cp 2Cr is transmetallated by [(Me 3Si) 2ELi] with concomitant Hamiltonians. In the case of the chromium(II) dimers, the elimination of LiCp, was initially used to target [Cp*Cr{ µ- antiferromagnetic super-exchange coupling between the high- E(SiMe 3)2}] 2, but only starting materials were recovered. An This journal is © The Royal Society of Chemistry 2013 J. Name ., 2013, 00 , 1-3 | 1 Chemical Science Page 2 of 5 ARTICLE Journal Name alternative, two-step approach was then attempted, in which chromium(II) chloride and lithium pentamethylcyclopentadienide (LiCp*) were combined as solids in a 1:1 stoichiometry, cooled to – 78 °C, and then thf was added. The reaction mixtures were slowly warmed to room temperature, which resulted in the formation of a blue solution. The solution was cooled to –78 °C, and [(Me 3Si) 2PLi] or [(Me 3Si) 2AsLi] (1 stoichiometric equivalent) in thf was added. Once again, the reactions were warmed to room temperature and stirred overnight. In the case of the phosphorus-containing reaction, the thf was evaporated and replaced with toluene, and the resulting solution was filtered, concentrated and stored at –30 °C for several days, which resulted in the formation of dark brown crystals of the 5 heterocubane chromium phosphide [( η -Cp*Cr)( µ3-P)] 4 (1), which was isolated in a yield of 33% based on the chromium starting material. For the arsenic-containing reaction, the same procedure led to the formation of large, brown crystals of the arsenide-bridged Fig. 1. Ball-and-stick representation of the molecular structure of 1. Cr = green; P 5 = purple; C = grey (hydrogen atoms not shown). trimetallic cage [( η -Cp*Cr) 3(µ3-As) 2] ( 2) in 42% yield based on the chromium starting material (Scheme 1). The moderate yields of 1 and 2 are a consequence of their high solubility, even in hydrocarbon undergoing ring whizzing) is reflected in the Cr(1)–Cr(2), solvents, at the temperature used for the recrystallizations. Although Cr(1)–Cr(3) and Cr(2)–Cr(3) distances of 2.7658(5), 2.7869(4) both 1 and 2 are very air-sensitive, both compounds can be heated to and 2.7677(4) Å, respectively, and the Cr(3)-Cr(1)-Cr(2), reflux in toluene for brief periods with obvious signs of Cr(1)-Cr(2)-Cr(3) and Cr(2)-Cr(3)-Cr(1) angles of 59.79(1), ° η5 decomposition, and they appear to be stable indefinitely at room 60.48(1) and 59.73(1) . Within each {( -Cp*)Cr} unit, the Cr– temperature under an inert atmosphere of nitrogen or argon. C distances are in the range 2.227(2)-2.238(2) Å for Cr(1), 2.224(2)-2.238(2) Å for Cr(2), and 2.226(2)-2.240(2) Å for Cr(3). The D3h symmetry of molecules of 2 is underscored by Manuscript the similarity of the lengths of the Cr–As bonds, which are 2.4304(4)-2.4381(4) Å to As(1) and 2.4258(4)-2.4316(4) Å to As(2). The As(1)-Cr(1)-As(2), As(1)-Cr(2)-As(2) and As(1)- Cr(3)-As(2) angles are 97.85(1), 97.59(1) and 97.48(1) °, respectively. In contrast to 1, the chromium centres in 2 are present formally as Cr(III). Several examples of five-vertex coordination cages containing {M 3E2} cores are known for M = Fe with E = P or As, 11 and for M = Co with E = P, including the closely related t 12 [(Cp ′′Co) 3(µ3-P) 2] (Cp ′′ = C 5H3 Bu 2). However, compound 2 is the first example of such a cluster to contain chromium. The formation of 1 is even more remarkable, for four reasons. Accepted Firstly, whereas clusters containing the {M S } (E = O, S) unit 4 4 are extremely well known, 13 only two molecular compounds Scheme 1. containing {M 4P4} heterocubane units have been structurally characterized, both of which have M = Co and were formed either in low yield 14 or as part of a mixture resulting from the Compound 1 (Figure 1) crystallizes in the tetragonal space thermolysis of [Cp RCo(CO) ] with [Cp*Fe(P )].
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