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To examine their luminescence behavior, two air-stable BN addition compounds were synthesized by the reaction of 5-fluoro-2-(2′-pyridyl)indole with 1,4- and 1,3-bis(bromo(methyl)boryl)benzene, respectively. Both BN adducts are luminescent. Their emission maxima (1,3-substituted BN adduct: 495 nm; 1,4-substituted BN adduct: 497 nm) are comparable with the value (490 nm) of the related mono-borylated benzene species, which is composed of a BPh2 fragment and a 5-fluoro-2-(2′-pyridyl) indole unit. The starting materials 1,4- and 1,3-bis(bromo(methyl)boryl)benzene were accessible by treatment of 1,4- or 1,3-bis(dibromoboryl)benzene with two equivalents of SnMe4. In addition, the results of the X-ray structure analyses of the B,B′-bis-5-fluoro-2-(2′-pyridyl)indolyl-complexed meta-bismethylborylbenzene fragment (9, triclinic, P1̅) as well as of 5-chloro-2-(2′-pyridyl)indole (2, monoclinic, P21/c) and 5-fluoro-2-(2′-pyridyl)indole (1, orthorhombic, Pca21) are reported. The pyridylindole derivatives of this approach were synthesized by an optimized two-step procedure from 2-acetylpyridine and 4-fluoro- or 4-chlorophenylhydrazine hydrochloride.
The title complex, [PdCl2(C18H15P)2]·0.5C6H6, has the PdII ion in a square-planar coordination mode (r.m.s. deviation for Pd, P and Cl atoms = 0.024 Å) with the PPh3 and Cl ligands mutually trans. The benzene solvent molecule is located about a crystallographic inversion centre. The title complex is isostructural with trans-dichloridobis(triphenylphosphane)palladium(II) 1,4-dichlorobenzene sesquisolvate [Kitano et al. (1983 [triangle]). Acta Cryst. C39, 1015–1017].
A new polymorph of the title compound, [Pd2(C8H18P)2(C8H19P)2], has been found. It belongs to the triclinic P-1 space group, whereas the known form [Leoni, Sommovigo, Pasquali, Sabatino & Braga (1992 [triangle]), J. Organomet. Chem. 423, 263–270] crystallizes in the monoclinic C2/c space group. The title compound features a dinuclear palladium complex with a planar central Pd2(μ-P)2 core (r.m.s. deviation = 0.003 Å). The Pd—Pd distance of 2.5988 (5) Å is within the range of a PdI—PdI bond. The molecules of both polymorphs are located on a crystallographic centre of inversion. The molecular conformations of the two polymorphs are essentially identical. The crystal packing patterns, on the other hand, are slightly different.
The crystal structure of the title compound, [Fe(C5H5)(CH3CN)(CO)2]BF4, of which only the coordinates of the non-H atoms of the cation have previously been reported [Fadel et al. (1979 [triangle]). Z. Anorg. Allg. Chem. 453, 98–106] has been redetermined. The FeII atom in the complex cation is coordinated by a cyclopentadienyl ring, two carbonyl ligands and an acetonitrile molecule displaying a three-legged piano stool structure. Three of the four F atoms of the BF4 − anion are disordered over two sets of sites, with a site-occupancy factor of 0.709 (10) for the major occupied site.
The crystal structure of the title compound, Na[(C6F5)BH3], is composed of discrete anions and cations. The sodium cations are surrounded by four anions with three short Na...B [2.848 (8), 2.842 (7) and 2.868 (8) Å] and two short Na...F contacts [2.348 (5) and 2.392 (5) Å], forming a three-dimensional network. The anion is the first structural example of a pentafluorophenyl ring carrying a BH3 group.
The bis(trimethyl)silylamido complex Na(THF){Fe[N(SiMe3)2]3} and the disilane tBu3SiSitBu3 were obtained from the reaction of Fe[N(SiMe3)2]3 with the sodium silanide Na(THF)2[SitBu3] in a mixture of benzene and THF. Single crystals of Na(THF){Fe[N(SiMe3)2]3} suitable for X-ray diffraction were grown from the reaction solution at ambient temperature (orthorhombic, C2221, Z = 4). The solid-state structure features a contact-ion pair with two short N-Na contacts. The THF adducts {M(THF)2[N(SiMe3)2]2} reacted with 2,2´-bipyridine to give the corresponding complexes {M(2,2´bipy)[N(SiMe3)2]2} (M= Mn; Fe). Their structures (M= Fe: orthorhombic, Pca21, Z = 8; M = Mn: orthorhombic, Pbca, Z = 8) feature monomeric units. The cyclic voltammogram of Fe[N(SiMe3)2]3 revealed a reversible redox transition with the potential of -0;523 V (E½), which was assigned to the Fe(III)[N(SiMe3)2]3 → Fe(II)[N(SiMe3)2]-3 redox transition, whereas the compounds {Fe(THF)2[N(SiMe3)2]2} (Eox = -0;379 V) and {Fe(2,2´bipy)[N(SiMe3)2]2} (Eox = -0;436 V) featured irreversible oxidation waves. The related manganese bis(trimethylsilyl)amido complexes {Mn(THF)2[N(SiMe3)2]2} (Eox = -0;458 V) and {Mn(2,2´bipy)[N(SiMe3)2]2} (Eox = -0513 V) also underwent irreversibile electron transfer processes.
1-(Bromomercurio)ferrocene
(2013)
The asymmetric unit of the title compound, [Fe(C5H5)(C5H4BrHg)], contains two independent molecules, A and B, in which the Hg-C bond lengths are 2.045 (6) and 2.046 (6) Å, the Hg-Br bond lengths are 2.4511 (9) and 2.4562 (7) Å, and the C-Hg-Br angles are 176.42 (17) and 177.32 (17)°. The two cyclopentadienyl rings of mol-ecule A are eclipsed, while those of mol-ecule B are almost staggered. The HgBr groups are connected by intermolecular Hg⋯Br contacts of 3.3142 (9)-3.4895 (11) Å, forming layers parallel to (001). These layers contain both four-membered (HgBr)2 and eight-membered (HgBr)4 rings. Ferrocene-ferrocene C-H⋯π contacts connect the molecular layers along the c-axis direction.
Di-μ-bromido-bis-[(diethyl ether-κO)(2,4,6-trimethylphenyl)magnesium] : the mesityl Grignard reagent
(2013)
The crystal structure of the title compound, [Mg2Br2(C9H11)2(C4H10O)2], features a centrosymmetric two-centre magnesium complex with half a mol-ecule in the asymmetric unit. The Mg atom is in a considerably distorted Br2CO coordination. Bond lengths and angles are comparable with already published values. The crystal packing is stabilized by C-H⋯π inter-actions linking the complexes into sheets parallel to (0-11).