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The COVID-19 pandemic highlighted the inaccessibility of quick and affordable clinical diagnostics. This led to increased interest in creating low-cost portable electrochemical (EC) devices for environmental monitoring and clinical diagnostics. One important perspective is to develop new fabrication methods for functional and low-cost electrode chips. Techniques, such as electron beam and photolithography, allow precise and high-resolution electrode fabrication; however, they are costly and can be time-consuming. More recently, fused deposition modeling three-dimensional (3-D) printing is being used as an alternative fabrication technique due to the low-cost of the printer and rapid prototyping capability. In this study, we explore enhancing the conductivity of 3-D printed working electrodes with EC gold deposition. Two commercial conductive filament brands were used and investigated to fabricate electrode chips. Furthermore, strategies to apply epoxy glue and conductive silver paint were investigated to control the electrode surface area and ensure good electrical connection. This device enables detection at drinking water concentration thresholds. The practical application of the fabricated electrodes is demonstrated by detecting Cu

A phosphaguanidine [Me2NC(PPh2)=N i Pr], the analogous guanidine [Me2NC(NPh2)=N i Pr], and their hydrochloride (HCl) salts were prepared to study the influence of substituting a phosphorus atom for a nitrogen atom on the basicity of the two compounds and the bonding in their conjugate acids. The pK a values of both HCl salts were measured in acetonitrile by NMR titration. Surprisingly, the substitution of P for N has essentially no effect on basicity even though the geometry at that atom is changed. The presence of phenyl substituents in the protonated guanidine reduces the resonance in the CN3 core, whereas poor orbital overlap between P and C reduces the resonance in the N2CP core of the protonated phosphaguanidine. The neutral phosphaguanidine binds to a Cu(I) halide through both the Nimine and the P, which suggested that the basic N atom on the bound ligand may have little utility as a Brønsted base. Fortunately, however, a Cu(I) halide complex of the protonated phosphaguanidine is stable. Thus, the tendency of the basic N to bind to metals does not proscribe it serving as a metal-proximate Brønsted base.

We report the synthesis and solid-state 17O NMR characterization of three 17O-labeled oxiranes: (2S*,3S*)-2,3-bis(4-nitrophenyl)-[17O]oxirane, (2S*,3R*)-2,3-bis(4-nitrophenyl)-[17O]oxirane, and 2,2,3-triphenyl-[17O]oxirane. In addition, we have determined the crystal structure of (2S*,3R*)-2,3-bis(4-nitrophenyl)oxirane by X-ray crystallography. When the experimentally determined 17O NMR tensors for oxiranes (where the C–O–C bond angle is about 60°) are compared with those for dimethyl ether (where the C–O–C bond angle is 113°) and other R–O–R′ functional groups, we found that the highly constrained geometry of oxiranes results in distinct tensor orientations in the molecular frame of reference. The experimental results are complemented by quantum chemical computations. This study represents the first time that 17O chemical shift and quadrupole coupling tensors are simultaneously determined for oxirane compounds.

Pseudo-octahedral complexes built on chelating ligands offer valuable isomeric properties such as the formation of fac vs mer isomers, and Λ vs Δ enantiomers. This article discusses factors guiding the fac vs mer selection of complexes built from the triazolyl-pyridine platform bearing a benzyl substituent, in conjunction with labile metal ions such as zinc(II), iron(II), and nickel(II). Critical parameters that are explored include the geometrical flexibility of the individual metal ion, and the nature of the counteranion. In essence, it was observed that ions which can withstand significant distortions in their first coordination sphere, such as zinc(II), generally prefer forming the mer isomer irrespective of the counteranion, whereas ions with more restricted geometry, such as iron(II), are directed either to a fac arrangement by small, tetrahedral anions such as tetrafluoroborate or perchlorate or to a mer organization by counteranions of lower symmetry, such as triflate. The molecular interactions o...

A 1-phosphonium-8-borane-decorated naphthalene molecule 2 has been found to react with N,N'-dimethylimidazol-2-ylidene (IMe), a popular member of the N-heterocyclic carbene (NHC) family, which converts it into two vinyl-amine fragments one of which is trapped between the phosphonium and borane unit by the formation of a C-C and a B-N bond. The same reactivity was not observed for larger NHC molecules. Control experiments and mechanistic studies have established the involvement of an ylide-borane molecule and an imidazolium salt in addition to IMe carbene in this new transformation of an NHC.

Transformation of 1-t-Boc-4-methoxyindole-3-glucosinolate under acidic conditions yielded the potent phytoalexin rapalexin A, providing its first biomimetic synthesis via Lossen type rearrangement, while a novel 1-thioimidocarbonyl-β-d-glucopyranose heterocyclic system was obtained under basic conditions via Neber type rearrangement.

Dimeric rhodium N-heterocyclic carbene complexes are demonstrated to be effective catalyst precursors for directed C-H borylation reactions at room temperature. The reactions are highly selective for mono-borylation and can be combined with a one-pot Suzuki-Miyaura coupling to give C-H arylation products with exclusive selectivity for mono-arylation without the requirement for steric blocking groups.

Here we report the structure and optical properties of a new Cu–cysteamine complex (Cu–Cy) with a formula of Cu3Cl(SR)2 (R = CH2CH2NH2). This Cu–Cy has a different structure from a previous Cu–Cy complex, in which both thio and amine groups from cysteamine bond with copper ions. Single-crystal X-ray diffraction and solid-state nuclear magnetic resonance results show that the oxidation state of copper in Cu3Cl(SR)2 is +1 rather than +2. Further, Cu3Cl(SR)2 has been observed to show intense photoluminescence and X-ray excited luminescence. More interesting is that Cu3Cl(SR)2 particles can produce singlet oxygen under irradiation by light or X-ray. This indicates that Cu3Cl(SR)2 is a new photosensitizer that can be used for deep cancer treatment as X-ray can penetrate soft tissues. All these findings mean that Cu3Cl(SR)2 is a new material with potential applications for lighting, radiation detection and cancer treatment.

The synthesis and characterization of ferrocene-based oligomers that contained two different elements (Si and Sn) as alternating bridges is described for the first time. The salt-metathesis reaction of R(2) Si[(C(5) H(4) )Fe(C(5) H(4) Li)](2) (R=Me, Et) with R'(2) SnCl(2) (R'=Me, nBu, tBu) afforded a mixture of oligomers (6(Me) SnMe(2), 6(Et) SnMe(2), 6(Me) SnnBu(2), 6(Et) SnnBu(2), 6(Me) SntBu(2), and 6(Et) SntBu(2)). These oligomers were characterized by (1) H, (13) C, (29) Si, and (119) Sn NMR spectroscopy and by mass spectrometry. MS (MALDI-TOF) studies of 6(Et) SnMe(2) revealed the presence of linear (l) and cyclic (c) species that contained up to 20 ferrocene moieties. The molecular weights of the polymers were determined by gel-permeation chromatography (GPC) and by dynamic-light scattering (DLS). GPC analysis revealed average molecular weights of 2100-6300 Da with respect to polystyrene as a standard. DLS analysis yielded very similar results. Some compounds, c-(6(Me) SnMe(2) )(1), c-(6(Me) SntBu(2))(2), c-(6(Et) SnMe(2))(1), c-(6(Et) SntBu(2))(2), l-(6(Me) SnnBu(2) )(2), and l-(6(Me) SnnBu(2))(3), which contained up to six ferrocene moieties, were isolated in their pure form either by column chromatography or by crystallization. The Si- and Sn-bridged macrocycles that contained four ferrocene units (c-(6(Me) SntBu(2))(2) and c-(6(Et) SntBu(2))(2)) were structurally characterized by single-crystal X-ray analysis.

The bulky m-terphenyl phenol Ar*OH 1 (Ar* = C6H3-2,6-Mes2, Mes = 2,4,6-trimethylphenyl) was synthesized via the treatment of Ar*Li with nitrobenzene. The phenol 1 is prepared in modest to good yield using this method. Attempts were also made to prepare 1 through oxidation of the bulky boronic acid Ar*B(OH)2with Oxone®, but this reaction was not suitable for preparative-scale reactions. Side products of the reaction between Ar*Li and nitrobenzene were identified as Ar*[N(O)Ph] and [C6H5N(O)]2and were characterized by X-ray crystallography and EPR spectroscopy. A variety of main-group and transition-metal complexes of Ar*OH were prepared, namely Sn(OAr*)2, Ge(OAr*)2, [N(SiMe3)2]Ge(OAr*), [Me2Al(OAr*)]2, and Ti(NMe2)(OAr*)2. All compounds were characterized spectroscopically and most were studied by single-crystal X-ray diffraction as well.Key words: m-terphenyl, main-group compounds, X-ray crystallography, multinuclear NMR spectroscopy, EPR spectroscopy.

Treatment of Cp*RuCl(kappa2-P,N-2b) (2b = 2-NMe2-3-PiPr2-indene) with TlSO3CF3 produced the cyclometalated complex [4]+SO3CF3- in 94% isolated yield. Exposure of [4]+X- (X = B(C6F5)4 or SO3CF3) to Ph2SiH2 (10 equiv) or PhSiH3 afforded the corresponding [Cp*(mu-P,N-2b)(H)2Ru=SiRPh]+X- complexes, [5]+X- (R = Ph; X = B(C6F5)4, 82%; X = SO3CF3, 39%) and [6]+X- (R = H; X = B(C6F5)4, 94%; X = SO3CF3, 95%). Notably, these transformations represent the first documented examples of Ru-mediated silylene extrusion via double geminal Si-H bond activation of an organosilane-a key step in the recently proposed Glaser-Tilley (G-T) alkene hydrosilylation mechanism. Treatment of [5]+B(C6F5)4- with KN(SiMe3)2 or [6]+SO3CF3- with NaN(SiMe3)2 afforded the corresponding zwitterionic Cp*(mu-2-NMe2-3-PiPr2-indenide)(H)2Ru=SiRPh complex in 69% (R = Ph, 7) or 86% (R = H, 8) isolated yield. Both [6]+X- and 8 proved unreactive toward 1-hexene and styrene and provided negligible catalytic turnover in the attempted metal-mediated hydrosilylation of these substrates with PhSiH3, thereby providing further empirical evidence for the required intermediacy of base-free Ru=Si species in the G-T mechanism. Isomerization of the P,N-indene ligand backbone in [6]+X-, giving rise to [Cp*(mu-1-PiPr2-2-NMe2-indene)(H)2Ru=SiHPh]+X- ([9]+X-), was observed. In the case of [9]+SO3CF3-, net intramolecular addition of the Ru=Si-H group across the styrene-like C=C unit within the ligand backbone to give 10 (96% isolated yield) was observed. Crystallographic characterization data are provided for [4]+X-, [5]+X-, [6]+X-, 8, and 10.

The reactions of CdCl2 or HgCl2 with {Li2[Te(N-t-Bu)3]}2 in n-hexane–THF give rise to two distinctly different types of product. In the former case the complexes [Li(THF)x][(CdCl)3{Te(N-t-Bu)3}2] (7a (x = 4), 7b (x = 3)) are obtained. The tetrasolvated complex 7a is a solvent-separated ion pair. The trisolvated complex 7b is a contact ion pair in which the fourth coordination site at the Li+ centre is occupied by one of the Cl ligands of the anion. The polycyclic anion in 7a and 7b is comprised of two tripodal [Te(N-t-Bu)3]2– dianions that exhibit different coordination modes to the three CdCl+ units. One ligand is N,N′-chelated to all three metal centres, and each nitrogen atom bridges two Cd atoms, whereas the other is bonded in a tris-N-monodentate fashion in 7b. In 7a there is an additional weak Cd-N interaction. The reaction of HgCl2 with {Li2[Te(N-t-Bu)3]}2 produces the adduct [t-BuNTe(µ-N-t-Bu)2TeN-t-Bu]HgCl2 (8), in which the dimeric tellurium diimide ligand in its cis(exo,exo) configuration is N,N′-chelated to mercury. Polymeric strands parallel to the b axis are formed by weak Te•••Cl interactions (3.5248(16) Å, 3.5876(15) Å) involving both Cl atoms, but only one Te atom of the ligand. Key words: imido ligands, cadmium, mercury, tellurium.

The dilithiated boraamidinate complexes {Li2[RB(N-t-Bu)2]}2 (1a, R = Ph; 1b, R = t-Bu), prepared by the reaction of B[N(H)-t-Bu]3 with three equivalents of LiR, are shown by X-ray crystallography to have dimeric structures consisting of a distorted Li4N4 cube capped on two opposite faces by RB units. Reactions of 1a with TeCl4 or PX3 (X = Cl, Br) yielded complexes PhB(μ-N-t-Bu)2TeCl2 (2) and PhB(μ-N-t-Bu)2PX (4a, X = Cl; 4b, X = Br), respectively. The structures of 2 and 4b were determined by X-ray crystallography. In the solid state, complex 2 forms a dimer with weak Te···Cl contacts (3.2411(6) Å). Complex 4b is monomeric with a P—Br bond length of 2.3047(11) Å. The reactions of 2 and 4a with the appropriate amounts of Li[N(H)-t-Bu] produce the monomeric tellurium imide PhB(μ-N-t-Bu)2Te=N-t-Bu and the amido derivative PhB(μ-N-t-Bu)2PN(H)-t-Bu (4c), respectively. The X-ray structure of 4c was determined. Deprotonation of 4c with n-BuLi produces the dimeric monolithium derivative {Li[PhB(μ-N-t-Bu)2PN-t-Bu]}2 (5), which was shown by X-ray crystallography to have a centrosymmetric structure with a central transoid Li2N2 ring.Key words: boraamidinates, lithium, tellurium, phosphorus, X-ray structures.

Whereas a new coordinatively unsaturated Cp*Ru(kappa(2)-P,O) complex (1a) forms adducts with two-electron donors (including sigma-H(2) and mu-N(2) ligands), double Si-H bond activation is observed upon treatment with Ph(2)SiH(2) or PhSiH(3), leading to the clean formation of products corresponding to the net insertion of a Ph(2)Si: or Ph(H)Si: fragment into the Ru-O bond of 1a.

An elaborate coordination polymer is formed using the weak Lewis-base [Au(CN)4]- coupled to a Jahn−Teller distorted CuII ion. Such structural complexity is inaccessible if a stronger structure-directing bonding interaction is present, as in the simpler NiII analog.

Pentafluorophenyl-bis(pentafluorophenylthio)sulfonium hexafluoroarsenate, [(C6F5S)2SC6F5][AsF6], was prepared by the reaction of (C6F5)2S2 and AsF5 in liquid SO2 at room temperature. The compound has been characterized by single-crystal X-ray and powder diffraction, and IR and FT-Raman spectroscopy. Crystals of [(C6F5S)2SC6F5][AsF6] are orthorhombic, space group P212121 (cell dimensions measured at room temperature in brackets): a = 13.132(3) [13.157(2)] Å, b = 21.477(4) [21.575(3)] Å, c = 8.770(2) [8.775(1)] Å, α = ß = γ = 90.00°; V = 2473.3(9) Å3, Z = 4, temperature = 181 ± 1 K. The structure consists of [AsF6]- anions and [(C6F5S)2SC6F5]+ cations that have a different structure than the related [X2MMMX]+ cations (M = S, Se; X = Cl, Br), which contain a trichalcogen chain with a pronounced chalcogen-chalcogen bond alternation. Ab initio calculations suggest the observed [(C6F5S)2SC6F5]+ geometry is due to steric and solid state effects. Comparison of the Raman spectra of [(C6F5)S2SC6F5][AsF6], [Cl2SSSCl][AsF6], and [(CH3)2ClS3]+ implies that [(CH3)2ClS3]+ has a structure with equal sulfur-sulfur distances, and therefore the structure is likely [(CH3S)2SCl]+ and probably not the previously reported [(CH3)2SSSCl]+.Key words: [R3X3]+ cations, X-ray crystal structure, FT-Raman spectroscopy, [(C6F5S)2SC6F5]+, pentafluorophenyl-bis(pentafluorophenylthio)sulfonium cation, hexafluoroarsenate.

The title compound, C24H56N6O2Te42+·2I−·C2H3N or H[(tBuNH)Te(μ-NtBu)2Te(μ-O)]2(I)2·MeCN, provides the first example of the cis form of an imidotelluroxane dication. The basket-shaped structure is bis­pirocyclic, with a `backbone' Te⋯Te⋯Te⋯Te pseudo-torsion angle of −31.51 (3)°. The structure exhibits two ionic Te⋯I inter­actions [3.4103 (8) and 3.445 (1) A] and two Te⋯I close contacts [3.863 (1) and 3.924 (1) A] within the mol­ecule, and two Te⋯I close contacts [3.651 (1) and 3.703 (2) A] between ions. The inter­molecular close contacts connect the cations into pairs which are linked by a weak Te⋯I contact [4.090 (1) A] to form an infinite chain.

The enantiomerically pure dibromoferrocene 3 [(Sp,Sp )-1,1'-dibromo-2,2'-di(isopropyl)ferrocene], equipped with two iPr groups in α positions, was prepared using known "Ugi amine" chemistry. Species 3 was targeted in order to gain access to new [1]ferrocenophanes ([1]FCPs) to be used as monomers for ring-opening polymerization. The iPr groups on the sandwich unit were introduced to stabilize bridging moieties, as well as to increase solubilities of targeted metallopolymers. The planar chiral dibromide 3 can quantitatively be lithiated at 0°C [2 equiv nBuLi, hexanes/thf (9:1), 30 min]. Salt-metathesis reactions with respective element dichloride species gave chiral [1]FCPs with a variety of bridging moieties [ERx =Ga[2-(Me2NCH2)C6H4] (4 a), SiMe2 (4 b), SntBu2 (4 c), BNiPr2 (4 d)]. The new [1]FCPs were fully characterized including single-crystal X-ray analysis. The stabilizing iPr groups on the Cp rings increase the thermal stabilities of 4 b-d compared to known [1]FCPs, equipped with the same bridging moieties. All three compounds 4 b-d are volatile and could be isolated by vacuum sublimation. Our new approach to [1]FCPs has the potential to overcome many of the existing difficulties in ferrocenophane chemistry, such as limited stability of starting monomers and low solubilities of resulting polyferrocenes.

Alternative and, in some cases, improved syntheses of the salts MX3(As/Sb)F6 (M = S, Se) and SCl3(SbCl6/AlCl4) are described. In addition, the synthesis of SeCl3SbF6 is reported. The compounds were characterized by FT–Raman spectroscopy and the X-ray crystal structures of SeCl3AsF6 (also 77Se NMR) and a new phase of SBr3SbF6 were determined. Crystals of SeCl3AsF6 and SBr3SbF6 are monoclinic, space group P21/c with [values for SBr3SbF6 in brackets] a = 7.678(1) [8.137(1)] Å, b = 9.380(3) [9.583(2)] Å, c = 11.920(3) [12.447(2)] Å, β = 98.19(2)° [97.36(1)]°, V = 849.72(3) [962.6(3)] Å3,z = 4, Dx = 2.925 [3.502] Mg m−3, R = 0.0525 [0.055], and Rw = 0.0554 [0.060] for 1151 [1472] observed reflections. Key words: MX3+ salts, FT–Raman spectroscopy, X-ray crystal structures of SeCl3AsF6, SBr3SbF6, and preparation of SeCl3SbF6.

The salts X2MMMX(AF6)(A = As or Sb, M = S or Se, X = Cl or Br) were prepared quantitatively by the reaction of stoichiometric amounts of MX3AF6 and M or from stoichiometric amounts of M, X2 and AsF5(M = S or Se; X = Br) in liquid SO2. They have been characterised by elemental analysis, single-crystal X-ray diffraction, Fourier-transform (FT)-Raman and 77Se FT-NMR spectroscopy. The crystal structures of X2MMMX(AsF6) consist of (X2MMMX)+ cations and AsF6– anions. The structure of the (X2MMMX)+ cation is dominated by an intracationic halogen–chalcogen contact and M–M bond alternation giving rise to a short M–M bond distance indicative of thermodynamically stable npπ–npπ(n= 3 or 4) bonds. Since the structure of these cations is different from those of (YM)2MY+(Y = Me or C6F5), theoretical calculations were performed to understand these differences and the bonding in these cations. In the X2SSSX(AsF6) salts (X = Cl or Br) the structures of the cations are disordered and therefore exact bond distances could be not obtained. However, bond distances were estimated from their FT-Raman spectra and supported by molecular orbital calculations. The FT-Raman spectrum of Se2Br5AsF6 is reported.

[1.1]Ferrocenophanes with gallium and silicon in bridging positions have been prepared in yields of 29 and 41%, respectively. From the same reactions, polymer-containing fractions were isolated (31% in each case) and shown to be comprised of linear and cyclic species with up to 16 ferrocene units (MALDI-TOF analysis).

The title compound, C56H83N9O9S·3CH3OH, is a methanol trisolvate of the cyclolinopeptide cyclo(Met1—Leu2—Ile3—Pro4—Pro5—Phe6—Phe7—Val8—Ile9) (henceforth referred to as CLP-B), which was isolated from flaxseed oil. All the amino acid residues are in an l-configuration based on the CORN rule. The cyclic nonapeptide exhibits eight trans peptide bonds and one cis peptide bond observed between the two proline residues. The conformation is stabilized by an α-turn and two consecutive β-turns each containing a N—H...O hydrogen bond between the carbonyl group O atom of the first residue and the amide group H atom of the fourth (α-turn) or the third residue (β-turns), repectively. In the crystal, the components of the structure are linked by N—H...O and O—H...O hydrogen bonds into chains parallel to the a axis.

The results of 19F, 14N and 15N NMR measurements for all 14N/15N isotopomers of N3F in CD2Cl2 solution are reported. Substantial deshielding for the N-α and N-γ atoms, relative to other covalent azides XN3 (X Cl, H, CF3, etc.), is observed. The coupling constants also indicate unusual bonding in N3F. 1J(15N-α, F) and 3J(15N-γ, F) are similar (58.2 and 58.6 Hz, respectively), very small for a 1J(15NF) but very large for a 3J(15NF) value. The observed value of 26.5 Hz for 1J(15N-α 15N-β) is the largest, and 2J(15N-α 15N-γ) (5.3 Hz) is the first reported coupling constant for an azide. The unusual N3F NMR data are discussed in terms of calculated atomic charges and the influence of the paramagnetic term which dominates the chemical shifts. This term expresses the deshielding due to the circulation of electrons in the magnetic field between the HOMOs and the LUMOs.

Triazadienyl fluoride, N3F, forms stable adducts with BF3 and AsF5 at low temperatures, as demonstrated by infrared measurements. The Lewis acids are bonded to the Nα-atom of N3F, as deduced from the data for 15N-isotopically enriched N3F. The basicity of N3F is comparable to that of ethine and ethene, according to the HF stretching frequency of the N3F/HF complex isolated in an argon matrix. Despite the low NF bond energy (< 150 kJ/mol), abstraction of the fluoride ion and formation of an N3 + salt was not possible. The different behavior of N3F and ClN3 towards Lewis acids is discussed.

The different coordination behavior of the ligand tBuN=Te(µ-NtBu)(2)Te=NtBu (L) towards Cu(+) and Ag(+) results from a cis-->trans isomerization. The two Cu(+) ions in [Cu(2)L(3)](2+) (shown schematically) bridge trans and cis isomers of the ligand, whereas the Ag(+) ions in [Ag(2)L(2)](2+) link two trans ligands and exhibit a weak Ag small middle dot small middle dot small middle dotAg interaction.

The versatile new ligand precursor 1/3-P(i)Pr(2)-2-S(t)Bu-indene has been employed in the preparation of neutral and cationic (kappa(2)-P,S)Pt(benzyl) complexes, as well as structurally related zwitterions in which the formally cationic metal fragment is counterbalanced by an uncoordinated indenide or borate fragment that is contained within the ancillary ligand backbone.

An 18-electron Cp*Ru(κ3-P,C,C‘) complex provides access to a 16-electron Cp*Ru(κ2-P,C) zwitterion by way of an unprecedented Ru−C(sp3) bond cleavage process that is both facile and reversible. Notably, this reactive zwitterion has proven capable of facilitating the Ru-mediated double geminal Si−H bond activation of Ph2SiH2.

The title compound, C56H83N9O11S·2C4H10O·H2O, is a butanol–water solvate of the cyclolinopeptide cyclo(Metsulfone1-Leu2–Ile3–Pro4–Pro5–Phe6–Phe7–Val8–Ile9) (henceforth referred to as CLP-K) which was isolated from flax oil. All the amino acid residues are in an l configuration based on the CORN rule. The cyclic nonapeptide exhibits eight trans peptide bonds and one cis peptide bond observed between the two proline residues. The conformation is stabilized by an α- and a β-turn, each containing an N—H...O hydrogen bond between the carbonyl group O atom of the first residue and the amide group H atom of the fourth (α-turn) and the third residue (β-turn), repectively. In the crystal, the components of the structure are linked by intermolecular N—H...O and O—H...O hydrogen bonds into a two-dimensional network parallel to (001). The –C(H2)OH group of one of the butanol solvent molecules is disordered over two sets of sites with refined occupancies of 0.863 (4) and 0.137 (4).

The asymmetric unit of the title compound, [K(C(3)H(7)O(3))](n) or K[H(2)gl](n), common name potassium glycerolate, contains half the K(+) cation and half of the glycerolate anion. The other half of the anion is generated through a mirror plane passing through the K atom, and a C, an H and an O atom of the glycerolate ligand. The K(+) ion is coordinated by the O atoms of the OH groups, leading to a six-membered chelate ring that adopts a very distorted boat conformation. The negatively charged O atom of the glycerolate anion, [H(2)gl(-)], is found in the flagpole position and forms an ionic bond with the K(+) ion. The O atoms of the hydroxo groups are coordinated to two K(+) ions, whereas the negatively charged O atom is bonded to one K(+) ion. The K(+) ion is coordinated by three other symmetry-related monodentate H(2)gl(-) ligands, so that each H(2)gl(-) ligand is bonded to two K(+) ions, and the potassium has a seven-coordinate environment. The H(2)gl(-) ligands are connected via a strong O-H⋯O hydrogen bond and, together with the K⋯O inter-connections, form polymeric sheets which propagate in the directions of the a and b axes.

The Na(+) cation in the title compound, [Na(C(3)H(7)O(3))](n) or Na[H(2)gl], is coordinated by five O atoms leading to a distorted trigonal-bipyramidal geometry. The negatively charged O atom of the glycerolate anion is in an equatorial position, and the O atom of the hydroxo group, attached to the secondary C atom, occupies an axial position completing a five-membered non-planar chelate ring; this defines the asymmetric unit. The Na(+) cation is coordinated by three other symmetry-related monodentate H(2)gl(-) ligands, so that each H(2)gl(-) ligand is bonded to four Na(+) ions. The H(2)gl(-) ligands are connected via strong O-H⋯O hydrogen bonds and these, together with the Na⋯O inter-connections, are responsible for the formation of polymeric sheets which propagate in the directions of the b and c axes.

The treatment of Me3SiN=P(NHBut)3 with three equivalents of LiBun in toluene produces (Li3(P(NBut)3(NSiMe3)))2 comprised of a Li6N6 cyclic ladder capped on the two hexagonal faces by mu 3-PNSiMe3 groups; the corresponding reaction of O=P(NHBut)3 yields the face-sharing double-cubane (Li2(THF)P(O)(NBut)2(NHBut))2 with a central Li2O2 ring.

Treatment of [Li2Te(NBut)3]2 with Sn(O3SCF3)2 or SnCl2 in diethyl ether generates the stannanetellurone [ButNSn(mu-NBut)2 TeNBut](mu3-SnTe) involving four-coordinate tin with d(Sn=Te) = 2.589(1) A; the two Sn and two Te atoms are in different oxidation states (+II/+IV and +IV/-II, respectively).

Lithiation of SP[N(H)R]3 with LiBun produces the dimers [(THF)LiSP(NR)(NHR)2]2 (R = Pri) or ([LiSP(NR)-(NHR)2][(THF)LiSP(NR)2(NHR)])2 (R = But) with central Li2N2 or Li2S2 rings, respectively; further lithiation yields the dianion [SP(NR)2(NHR)]2- (R = Pri) or leads to sulfur extrusion when R = But.

The title compound, CH3O–C(O)–Fc–C(O)–OBt or [Fe(C7H7O2)(C12H8N3O2)] (Bt is benzotriazole), shows a cis configuration of the Bt group relative to the ferrocene core, with the benzene ring in close proximity to the methyl ester group.

Stable dark red (M = Al) or dark green (M = Ga) neutral radicals {[PhB(mu-NtBu)2]2M} are obtained by the oxidation of their corresponding anions with iodine, and EPR spectra supported by DFT calculations show that the spin density is equally delocalized over all four nitrogen atoms in these spiroconjugated systems.

An improved synthesis of SF5(CN), by direct fluorination of SF3(CN), has been achieved. This product forms a stable adduct at low temperature with AsF5, and addition of MeCN to this adduct led to very pure SF5(CN). The SF5(CN)·AsF5 adduct has been characterized by vibrational and 19F Fourier-transform NMR spectroscopy and by its dissociation vapour-pressure curve. The salt SNSAsF6 and an excess of SF5(CN) reacted in sulfur dioxide solution to give the stable salt F5S[graphic omitted]AsF6 which has been characterized by vibrational, 19F NMR and mass spectroscopy and X-ray crystallography. The structure consists of discrete F5S[graphic omitted]+ cations and AsF6– anions. The mass spectrum of F5S[graphic omitted]AsF6 was consistent with loss of AsF5 and fluoride ion transfer to give F5S[graphic omitted] which dissociated to SF4 and F2[graphic omitted]. Reduction of a dilute solution of the salt in SO2 led to identification (ESR spectroscopy) of the radical F5S[graphic omitted]˙.

The reaction of ButNTe(μ-NBut)2TeNBut with ButNCO in a 1∶4 molar ratio in thf produces N,N′-bis(tert-butyl)ureato telluroxide dimers [OC(μ-NBut)2TeO]2, which form an extended helical network via weak CO⋯Te interactions.