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Dr. M. John Plater Amara Darr Catriona Crawford Craig Murray Struan Simpson Prof. William T. A. Harrison Prof. Juan M. Clemente-Juan 《ChemistryOpen》2019,8(9):1204-1208
The synthesis of a Cu4(OH)4 cube which is coordinated by four molecules of the dipyridyl ligand 1,6-[di(pyridin-4-yl)hex-3-ene] is reported. This compound has a trans double bond which restricts the conformational freedom of the ligand and favours coordination within a unique copper cube. The structure was solved by an X-Ray single crystal structure determination and low temperature magnetic susceptibility measurements examined its magnetic properties. The cube classification corresponds to the type I classification of Mergehenn and Haase and the short/long distribution of Cu ⋅⋅⋅ Cu separations in the cube as defined by Ruiz. The magnetic susceptibility measurements show paramagnetic behaviour down to 50 K but below this the copper cube shows weak ferromagnetic exchange interactions. The low temperature magnetic susceptibility characteristics are examined in detail then modelled and compared to other similar Cu4O4 copper cubes. 相似文献
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Bis(tetraphenylphosphonium) hexachloridodiberyllate, (Ph4P)2[Be2Cl6], reacts with excess trimethylsilyl‐iso‐thiocyanate to give a mixture of colourless single crystals of (Ph4P)2[Be(NCS)4] ( 1 ) and (Ph4P)4[{Be2(NCS)4(μ‐NCS)2}{Be2(NCS)6(μ‐H2N2C2S2)}] ( 2 ), which can be separated by selection. Both complexes were characterized by X‐ray diffraction. Compound 1 can be prepared without by‐products by treatment of (Ph4P)2[BeCl4] with excess Me3SiNCS in dichloromethane solution. 1 : Space group I41/a, Z = 4, lattice dimensions at 100(2) K: a = b = 1091.2(1), c = 3937.1(3) pm, R1 = 0.0474. The [Be(NCS)4]2– ion of 1 forms tetragonally distorted tetrahedral anions with Be–N distances of 168.4(2) pm and weak intermolecular S ··· S contacts along [100] and [010]. 2 ·4CH2Cl2: Space group P , Z = 1, lattice dimensions at 100(2) K: a = 919.5(1), b = 1248.3(1), c = 2707.0(2) pm, α = 101.61(1) °, β = 95.08(1) °, γ = 94.52(1) °, R1 = 0.103. Compound 2 contains two different anionic complexes in the ratio 1:1. In {Be2(NCS)4(μ‐NCS)2}2–, the beryllium atoms are connected by (NCS)– bridging groups forming centrosymmetric eight‐membered Be2(NCS)2 rings with distances Be–N of 168(1) pm and Be–S of 235.2(9) pm. The second anion {Be2(NCS)6(μ‐H2N2C2S2)}2– consists of two {Be(NCS)3}– units, which are linked by the nitrogen atoms of the unique dimeric cyclo‐addition product of HNCS with Be–N distances of 179(1) pm. 相似文献
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