Crystal Structure of S8 Molecule from Thiourea2020 · <p>Sulfur S<sub>8</sub> was isolated from a reaction solution of thiourea and bismuth nitrate in <i>N,N</i>-dimethylformamide. The crystal structure was determined by the single-crystal X-ray diffraction method at 90 K. It crystallizes in the orthorhombic space group <i>Fddd</i> with <i>a</i> = 10.3310(8)Å, <i>b</i> = 12.6786(10)Å, <i>c</i> = 24.3519(19)Å, <i>V</i> = 3189.7(4)Å<sup>3</sup>, <i>D</i><sub>x</sub> = 2.136 g/cm<sup>3</sup>, and <i>Z</i> = 6. The <i>R</i>1 [<i>I</i> > 2σ(<i>I</i>)] and <i>wR</i>2 (all data) values are 0.0220 and 0.0570, respectively, for all 1864 independent reflections. The S<sub>8</sub> molecule has a crown-shaped ring structure with the α-form.</p>
Synthesis and Characterization of a Di-µ-oxalato Tetracopper(Ⅱ) Complex with Tetranucleating Macrocyclic Ligand2016 · A tetracopper(II) complex containing two oxalate anions in the metal-based host cavity, [Cu<sub>4</sub>(L<sub>py</sub>)(µ-ox)<sub>2</sub>](PF<sub>6</sub>)<sub>2</sub>·2(2-PrOH), where ox<sup>2−</sup>: oxalato (C<sub>2</sub>O<sub>4</sub><sup>2−</sup>), was prepared by reacting <b>H<sub>2</sub>L<sub>py</sub></b>, a phenol-based tetranucleating macrocyclic ligand with four pyridylmethyl pendant arms, Cu(ClO<sub>4</sub>)<sub>2</sub>·6H<sub>2</sub>O, and sodium oxalate (1:4:2 stoichiometry, respectively) in methanol, followed by exchange of the counteranion with excess of NH<sub>4</sub>PF<sub>6</sub>. Single-crystal X-ray diffraction of <b>1</b> revealed that two {Cu(II)Cu(II)} units, bridged by a phenolato group of <b>L<sub>py</sub></b><sup>2−</sup>, were connected by two oxalato anions, to construct a rectangular “{CuCu}(µ-ox)<sub>2</sub>{CuCu}” tetranuclear framework. This rectangular framework was maintained in DMF solution. The magnetic measurement of <b>1</b> in the 2–300 K range revealed antiferromagnetic behavior. The antiferromagnetic interaction in this complex occurs between the Cu(II) centers bridged by an oxalate (<i>J</i> = −140 cm<sup>−1</sup>).
Synthesis and magnetic properties of a dinuclear manganese(II) complex with two manganese(II) ions of C-2-twisted octahedral geometry2016 · A dinuclar manganese(II) complex [Mn-2(sym-hcp)(2)](BPh4)(2).2acetone.2H(2)O (1) was synthesized with a new dinucleating ligand, 4-chloro-2,6-bis1(2-hydroxyethyl)methylaminomethyllphenol [H(sym-hcp)I, for the purpose of studying the magnetic properties. The single-crystal X-ray analysis revealed a bis-mu-phenolato-dimanganese(II) core structure containing two distorted octahedral manganese(II) ions of C-2 symmetry. The order of the coordination bond lengths is Mn-O(phenolato) < Mn-O(hydroxy) < Mn-N. Magnetic susceptibility data for 1 was fitted well with the parameters 2J = -0.93 cm(-1) and g = 2.03, indicating weak antiferromagnetic interaction. (C) 2016 Elsevier Ltd. All rights reserved.
