30 research outputs found
Tris(1,10-phenanthroline-κ2 N,N′)iron(II) bis[(1,10-phenanthroline-κ2 N,N′)tetrakis(thiocyanato-κN)chromate(III)] acetonitrile trisolvate monohydrate
Single crystals of the title heterometallic compound, [Fe(C12H8N2)3][Cr(NCS)4(C12H8N2)]2·3CH3CN·H2O or [Fe(Cphen)3][Cr(NCS)4(phen)]2·3CH3CN·H2O, were prepared using the one-pot open-air reaction of iron powder, Reineckes salt and 1,10-phenanthroline (phen) in acetonitrile. The asymetric unit consists of an [Fe(phen)3]2+ cation, two [Cr(phen)(NCS)4]− anions, three acetonitrile solvent molecules and a water molecule. The Fe and Cr atoms both show a slightly distorted octahedral FeN6 and CrN6 coordination geometry with adjacent angles in the range 79.67 (12)–95.21 (12)°. No classical hydrogen bonding involving the water molecule is observed
Hexakis(dimethylformamide-κO)manganese(II) (dimethylformamide-κO)pentakis(thiocyanato-κN)chromate(III)
The title compound, [Mn(C3H7NO)6][Cr(NCS)5(C3H7NO)], was obtained unintentionally as a product of an attempted synthesis of heterometallic complexes based on Reineckes anion using manganese powder, Reineckes salt and 1-(2-hydroxyethyl)tetrazole as starting materials. The crystal structure of the complex consists of an [Mn(dmf)6]2+ cation and a [Cr(NCS)5(dmf)]2− anion (dmf = dimethylformamide). The MnII and CrIII atoms show a slightly distorted octahedral MnO6 and CrN5O coordination geometries with adjacent angles in the range 85.29 (13)–95.96 (14)°
Diammine(2,2′-bipyridine)bis(thiocyanato-κN)cobalt(III) diamminetetrakis(thiocyanato-κN)chromate(III) acetonitrile disolvate
The new heterometallic title complex, [Co(NCS)2(C10H8N2)(NH3)2][Cr(NCS)4(NH3)2]·2CH3CN, has been prepared using the open-air reaction of cobalt powder, Reineckes salt and 2,2′-bipyridine (dpy) in acetonitrile. The crystal structure consists of discrete cationic [Co(NCS)2(NH3)2(dpy)]+ and anionic [Cr(NCS)4(NH3)2]− building blocks, both with 2 symmetry, and acetonitrile solvent molecules, which are linked together by N—H⋯N hydrogen bonds, forming extended supramolecular chains. Furthermore, N—H⋯S, C—H⋯S and C—H⋯N hydrogen bonds interlink neighbouring chains into a three-dimensional framework. The Co atom is in an elongated octahedral coordination environment with two N atoms from the dpy ligands and two NCS-groups in the equatorial plane and with two NH3 molecules at the axial positions. The CrIII ion is octahedraly coordinated by two NH3 molecules at the axial positions and four NCS-groups in the equatorial plane. Intensity statistics indicated non-merohedral twinning with the twin matrix [100; 00; 0]. The refined ratio of the twin components is 0.530 (1):0.470 (1)
Bis{μ2-2-[(2-hydroxyethyl)(methyl)amino]ethanolato}bis(μ3-N-methyl-2,2′-azanediyldiethanolato)tetrakis(thiocyanatato-κN)dichromium(III)dimanganese(II) dimethylformamide tetrasolvate
The heterometallic title complex, [Cr2Mn2(C5H11NO2)2(C5H12NO2)2(NCS)4]·4C3H7NO, was prepared using manganese powder, Reineckes salt, ammonium thiocyanate and a non-aqueous solution of N-methyldiethanolamine in air. The centrosymmetric molecular structure of the complex is based on a tetranuclear {Mn2Cr2(μ-O)6} core. The tetranuclear complex molecule and the two uncoordinated dimethylformamide molecules are linked by O—H⋯O hydrogen bonds, while the two other molecules of dimethylformamide do not participate in hydrogen bonding
Triiodide-selective Electrode on the Basis of Ionic Associate of Netral Red Triiodide
Створено пластифікований I3
--селективний сенсор, що містить як електродоактивну речовину іонний
асоціат трийодиду нейтрального червоного. Робочий інтервал рН сенсора − 2–12; інтервал лінійності
електродної функції − 9×10-5 – 1×10-1 моль/л, крутизна − 50–59 мВ/pC. Розроблений сенсор апробовано при
потенціометричному титруванні йодидів у фармацевтичних препаратах. The І3
--selective electrodesensor
with ionic associates of neutral red triiodide as electrode-active substance were developed. The рН working
range is 2–12. The linearity ranges of the electrode function are 9 ×10-5 –1×10-1 mol/l, the electrode function slopes are
50–59 mV/decade. The efficiency of the use of sensor for the iodide determination was shown by potentiometric
titration methods
Order in disorder:solution and solid-state studies of [(M2M5II)-M-III] wheels (M-III = Cr, Al; M-II = Ni, Zn)
A family of heterometallic Anderson-type ‘wheels’ of general formula [MIII2MII5(hmp)12](ClO4)4 (where MIII = Cr or Al and MII = Ni or Zn giving [Cr2Ni5] (1), [Cr2Zn5] (2), [Al2Ni5] (3) and [Al2Zn5] (4); hmpH = 2-pyridinemethanol) have been synthesised solvothermally. The metallic skeleton common to all structures describes a centred hexagon with the MIII sites disordered around the outer wheel. The structural disorder has been characterised via single crystal X-ray crystallography, 1–3D 1H and 13C solution-state NMR spectroscopy of the diamagnetic analogue (4), and solid-state 27Al MAS NMR spectroscopy of compounds (3) and (4). Alongside ESI mass spectrometry, these techniques show that structure is retained in solution, and that the disorder is present in both the solution and solid-state. Solid-state dc susceptibility and magnetisation measurements on (2) and (3) reveal the Cr–Cr and Ni–Ni exchange interactions to be JCr–Cr = −1 cm−1 and JNi–Ni,r = −5 cm−1, JNi–Ni,c = 10 cm−1. Fixing these values allows us to extract JCr–Ni,r = −1.2 cm−1, JCr–Ni,c = 2.6 cm−1 for (1), the exchange between adjacent Ni and Cr ions on the ring is antiferromagnetic and between Cr ions on the ring and the central Ni ion is ferromagnetic.EKB thanks the EPSRC for funding (EP/N01331X/1, EP/P025986/1). UGN acknowledges funding
from the Villum Young Investigator (VKR022364) and the Danish Council for Independent Research – Natural Sciences (DFF – 7014-00198). ME thanks MINECO for funding (MAT2015-68204-R)Peer reviewe
[CrIII8MII6]12+ Coordination Cubes (MII=Cu, Co)
Four [CrIII8MII6]n+ (MII = Cu, Co) coordination cubes of formulae [Cr8Co6L24Cl12] (1), [Cr8Co6L24(SCN)12] (2), [Cr8Cu6L24(H2O)12](SO4)6 (3), and [Cr8Cu6L24Cl12] (4) (where HL is 1-(4-pyridyl)butane-1,3-dione), were synthesised using the [CrIIIL3] metalloligand in combination with a variety of MII salts. The metallic skeleton of each cage describes a cube in which the [CrIIIL3] moieties occupy the eight vertices and the MII ions lie at the centre of the six faces. The axial coordination sites of the MII cations are occupied by either H2O molecules or Cl?/SCN? anions originating from the MII salt used in the synthesis, resulting in neutral 1, 2 and 4 and the cage in 3 being a 12+ cation; the charge-balancing SO42? anions accommodated both inside and outside the cube. Magnetic susceptibility and magnetisation measurements reveal weak exchange between nearest neighbour metal ions, mediated via the L? ligands. The modular assembly of the cubes suggests that any combination of [MIIIL3] metalloligand and MII salt will work, potentially resulting in an enormous family of supramolecular assemblies. The charge of the cubes is controlled by the nature of the ligand occupying the axial sites on the MII ions, suggesting trivial ligand exchange may offer control over, amongst others, solubility, reactivity, post-synthetic modification and substrate specificity. The large internal cavities of the cubes also suggest host–guest chemistry may be a fruiful route to encapsulating magnetic and/or redox active guests which could be employed to control magnetic behaviour, and the construction of multifunctional materials
Crystal structure of tetrakis[μ2-2-(dimethylamino)ethanolato-κ3N,O:O]di-μ3-hydroxido-dithiocyanato-κ2N-dichromium(III)dilead(II) dithiocyanate acetonitrile monosolvate
The tetranuclear complex cation of the title compound, [Cr2Pb2(NCS)2(OH)2(C4H10NO)4](SCN)2·CH3CN, lies on an inversion centre. The main structural feature of the cation is a distorted seco-norcubane Pb2Cr2O6 cage with a central four-membered Cr2O2 ring. The CrIII ion is coordinated in a distorted octahedron, which involves two N atoms of one bidentate ligand and one thiocyanate anion, two μ2-O atoms of 2-(dimethylamino)ethanolate ligands and two μ3-O atoms of hydroxide ions. The coordination geometry of the PbII ion is a distorted disphenoid, which involves one N atom, two μ2-O atoms and one μ3-O atom. In addition, weak Pb...S interactions involving the coordinating and non-coordinating thiocyanate anions are observed. In the crystal, the complex cations are linked through the thiocyanate anions via the Pb...S interactions and O—H...N hydrogen bonds into chains along the c axis. The chains are further linked together via S...S contacts. The contribution of the disordered solvent acetonitrile molecule was removed with the SQUEEZE [Spek (2015). Acta Cryst. C71, 9–18] procedure in PLATON. The solvent is included in the reported molecular formula, weight and density
trans-Chloridobis(ethane-1,2-diamine-κ2N,N′)(thiocyanato-κN)cobalt(III) diamminetetrakis(thiocyanato-κN)cromate(III)
The title ionic complex [CoCl(NCS)(C2H8N2)2][Cr(NCS)4(NH3)2], which crystallizes as a non-merohedral twin, is build up of a complex cation [CoCl(NCS)(en)2]+ (en is ethane-1,2-diamine) and the Reinecke's salt anion [Cr(NCS)4(NH3)2]− as complex counter-ion. A network of N—H...S and N—H...Cl hydrogen bonds, as well as short S...S contacts [3.538 (2) and 3.489 (3) Å], between the NCS groups of the complex anions link the molecules into a three-dimentional supramolecular network. Intensity statistic indicated twinning by non-merohedry with refined weighs of twin components are 0.5662:0.4338