0000000001299659
AUTHOR
Igor O. Fritsky
Cu(II), Ni(II) and Zn(II) mononuclear building blocks based on new polynucleating azomethine ligand : Synthesis and characterization
Five new mononuclear complexes formed by the polynucleating ligand 2-[1-(3,5-dimethyl)pyrazolyl]-2-hydroxyimino-N′-[1-(2-pyridyl)ethylidene]acetohydrazide (HL): [Ni(L)(HL)]ClO4·2CH3OH (1), [Ni(L)2]·CH3OH (2), [Zn(L)(HL)]ClO4·2CH3OH (3), [Zn(L)2]·CH3OH (4) and [Cu(L)2]·CH3OH (5) were synthesized and characterized by elemental analysis, mass-spectrometry, IR-spectroscopy and X-ray analysis. The complexes reveal distorted octahedral N4O2 coordination arrangement formed by both protonated and deprotonated (1, 3) or two deprotonated ligand molecules (2, 4, 5). The presence of non-coordinated oxime and pyrazole groups resulted in the formation of extensive systems of hydrogen bonds in the crystal…
Coordination Diversity in Mono- and Oligonuclear Copper(II) Complexes of Pyridine-2-Hydroxamic and Pyridine-2,6-Dihydroxamic Acids
Solution and solid state studies on Cu(II) complexes of pyridine-2-hydroxamic acid (HPicHA) and pyridine-2,6-dihydroxamic acid (H2PyDHA) were carried out. The use of methanol/water solvent allowed us to investigate the Cu(II)-HPicHA equilibria under homogeneous conditions between pH 1 and 11. In agreement with ESI-MS indication, the potentiometric data fitted very well with the model usually reported for copper(II) complexes of α-aminohydroxamate complexes ([CuL](+), [Cu5(LH-1)4](2+), [CuL2], [CuL2H-1](-)), however with much higher stability of the 12-MC-4 species. A series of copper(II) complexes has been isolated in the solid state and characterized by a variety of spectroscopic methods, …
Chiral spin crossover nanoparticles and gels with switchable circular dichroism
Spin crossover complexes represent spectacular examples of molecular switchable materials. We describe a new approach towards homochiral coordination nanoparticles of [Fe(NH2trz)3](L-CSA)2 (NH2trz = 4-amino-1,2,4-triazole, L-CSA = L-camphorsulfonate) that display an abrupt switch of chiral properties associated with a cooperative spin transition. This is an original method that generates stable and additive-free colloidal solutions of nanoparticles with a spin transition around room temperature. The introduction of a chiral anion to the coordination framework makes these nanoparticles display specific chiro-optical (circular dichroism) properties that are different in high and low spin stat…
High temperature spin crossover in [Fe(pyrazine){Ag(CN) 2 } 2 ] and its solvate
A high temperature spin crossover (Tup = 367 K) was detected in a metal–organic framework [Fe(pz){Ag(CN)2}2]·MeCN (pz = pyrazine). Upon heating, this solvate released acetonitrile guest molecules, which slightly shifted the transition temperature of the complex (Tup = 370 K and Tdown = 356 K).
Dioxomolybdenum(VI) complexes of hydrazone phenolate ligands - syntheses and activities in catalytic oxidation reactions
Abstract The new cis-dioxomolybdenum (VI) complexes [MoO2(L2)(H2O)] (2) and [MoO2(L3)(H2O)] (3) containing the tridentate hydrazone-based ligands (H2L2 = N'-(3,5-di-tert-butyl-2-hydroxybenzylidene)-4-methylbenzohydrazide and H2L3 = N'-(2-hydroxybenzylidene)-2-(hydroxyimino)propanehydrazide) have been synthesized and characterized via IR, 1H and 13C NMR spectroscopy, mass spectrometry, and single crystal X-ray diffraction analysis. The catalytic activities of complexes 2 and 3, and the analogous known complex [MoO2(L1)(H2O)] (1) (H2L1 = N'-(2-hydroxybenzylidene)-4-methylbenzohydrazide) have been evaluated for various oxidation reactions, viz. oxygen atom transfer from dimethyl sulfoxide to t…
Imparting hysteretic behavior to spin transition in neutral mononuclear complexes
A series of spin transition neutral compounds [FeL(NCS)2] has been synthesized and characterized by means of magnetic susceptibility studies, X-ray diffraction, IR and Mossbauer spectroscopic, and calorimetric measurements (L = N,N-bis((3-alkoxypyridin-2-yl)methylene)-propane-1,3-diamine, number of carbon atoms in chains (n) = 4, 12, 14, 16, 18, 20). The shortest chain compound is crystalline and displays a gradual spin transition above ambient temperature. Growing the aliphatic substituent up to n = 12 and 14 leads to loss of crystalline order and deterioration of magnetic properties. At the critical chain length n = 16 and above, the compounds undergo a phase transition reflected by a spi…
Dioxomolybdenum(VI) complexes of hydrazone phenolate ligands -syntheses and activities in catalytic oxidation reactions
The new cis-dioxomolybdenum(VI) complexes [MoO2(L2)(H2O)] (2) and [MoO2(L3) (H2O)] (3) containing the tridentate hydrazone-based ligands (H2L2 = N'-(3,5-di-tert-butyl-2-hydroxybenzylidene)-4-methylbenzohydrazide and H2L3 = N'-(2-hydroxybenzylidene)-2-(hydroxyimino)propanehydrazide) have been synthesised and characterized via IR, 1H and 13C NMR spectroscopy, mass spectrometry, and single crystal X-ray diffraction analysis. The catalytic activities of complexes 2 and 3, and the analogous known complex [MoO2(L1)(H2O)] (1) (H2L1 = N'-(2-hydroxybenzylidene)-4-methylbenzohydrazide) have been evaluated for various oxidation reactions, viz. oxygen atom transfer from dimethyl sulfoxide to triphenylp…
Room temperature hysteretic spin crossover in a new cyanoheterometallic framework.
A new iron(II)-based spin-crossover compound with thermal hysteresis operating under ambient conditions is reported. This complex exhibits a high reproducibility of the spin transition in many successive thermal cycles, stability of both spin states at room temperature and an attractive operational temperature range.
Bis(3,5-dimethyl-1H-pyrazolyl)selenide--a new bidentate bent connector for preparation of 1D and 2D co-ordination polymers.
The synthesis and description of eight polymeric complexes formed by transition metals with the bifurcated ligand bis(3,5-dimethyl-1H-pyrazolyl)selenide are discussed together with X-ray crystal analysis as well as variable temperature magnetic susceptibility and characterization by Mossbauer spectroscopy. Preferable types of binding patterns of the ligand were determined, which include a variation of the bridging modes (cis- and trans-) and of the separation length, where the latter parameter together with bending of the ligand molecule were found to be dependent on the type of co-ordination geometry of the central atom and the nature of the anion. A strategy for increasing the structure d…
Strong Cooperative Spin Crossover in 2D and 3D FeII −MI,II HofmannLike Coordination Polymers Based on 2‑Fluoropyrazine
Self-assembling iron(II), 2-fluoropyrazine (Fpz), and [MII(CN)4] 2− (MII = Ni, Pd, Pt) or [AuI (CN)2] − building blocks have afforded a new series of two- (2D) and threedimensional (3D) Hofmann-like spin crossover (SCO) coordination polymers with strong cooperative magnetic, calorimetric, and optical properties. The iron(II) ions, lying on inversion centers, define elongated octahedrons equatorially surrounded by four equivalent centrosymmetric μ4-[MII(CN)4]2− groups. The axial positions are occupied by two terminal Fpz ligands affording significantly corrugated 2D layers {Fe(Fpz)2([MII(CN)4]}. The Pt and Pd derivatives undergo thermal- and light-induced SCO characterized by T1/2 temperatur…
Iron (II) isothiocyanate complexes with substituted pyrazines: Experimental and theoretical views on their electronic structure
Abstract Synthesis, structural, magnetic, Mossbauer and thermal studies of isothiocyanate iron (II) complexes with substituted pyrazines (iodo-, bromo- and amino-derivatives) are discussed here. Complexes with iodo- and bromo-derivatives were found to have the composition [Fe(Ipz)2(SCN)2(H2O)2]·2Ipz (1) and [Fe(Brpz)2(SCN)2(H2O)2]·2Brpz (2), whereas in the case of amino-functionalized pyrazine the formation of [Fe(NH2pz)4(SCN)2] (3) was observed. 3D organization of the molecular complexes is stabilized within different hydrogen, halogen and lone pair–π interactions. Spin state of iron (II) ions in 1–3 was determined as high spin by Mossbauer and magnetic measurements. DFT calculations for t…
Complex formation of copper(II), nickel(II) and zinc(II) with ethyl phosphonohydroxamic acid : solution speciation, synthesis and structural characterization
The first example of a Cu(II) 12-MC-4 hydroxamic metallacrown containing an ethylphosphonate group as an additional donor function in the β-position with respect to the hydroxamic group is described. The solution equilibrium of ethylphosphonoacetohydroxamic acid (PAHEt) with Cu(II) was investigated in aqueous solution by a combination of potentiometry, mass spectrometry, UV-Vis and EPR spectroscopies, and isothermal titration calorimetry. A model containing mononuclear [CuL], [CuL2]2− and [CuL2H−1]3− and pentanuclear [Cu5(LH−1)4]2− species is proposed. The predominance of the [Cu5(LH−1)4]2− species in solution over the pH range 4–9 was confirmed by the signals present in the ESI-MS spectra,…
Indefinitely stable iron(IV) cage complexes formed in water by air oxidation
In nature, iron, the fourth most abundant element of the Earth's crust, occurs in its stable forms either as the native metal or in its compounds in the +2 or +3 (low-valent) oxidation states. High-valent iron (+4, +5, +6) compounds are not formed spontaneously at ambient conditions, and the ones obtained synthetically appear to be unstable in polar organic solvents, especially aqueous solutions, and this is what limits their studies and use. Here we describe unprecedented iron(IV) hexahydrazide clathrochelate complexes that are assembled in alkaline aqueous media from iron(III) salts, oxalodihydrazide and formaldehyde in the course of a metal-templated reaction accompanied by air oxidation…
Cooperative High-Temperature Spin Crossover Accompanied by a Highly Anisotropic Structural Distortion
Spin transitions are a spectacular example of molecular switching that can provoke extreme electronic and structural reorganizations in coordination compounds. A new 3D cyanoheterometallic framework, [Fe(pz)(Au(CN)2)2], has been synthesized in which a highly cooperative spin crossover has been observed at 367 and 349 K in heating and cooling modes, respectively. Mössbauer spectroscopy revealed a complete transition between the diamagnetic and paramagnetic states of the iron centres. The low-spin-to-high-spin transition induced a drastic structural distortion involving a large one-directional expansion (ca. 10.6%) and contraction (ca. 9.6%) of the lattice. Negative thermal expansion along th…
Enantioselective Guest Effect on the Spin State of a Chiral Coordination Framework
The diversity of spin crossover (SCO) complexes that, on the one hand, display variable temperature, abruptness and hysteresis of the spin transition, and on the other hand, are spin-sensitive to the various guest molecules, makes these materials unique for the detection of different organic and inorganic compounds. We have developed a homochiral SCO coordination polymer with a spin transition sensitive to the inclusion of the guest 2-butanol, and these solvates with (R)- and (S)-alcohols demonstrate different SCO behaviours depending on the chirality of the organic analyte. A stereoselective response to the guest inclusion is detected as a shift in the temperature of the transition both fr…
Magnetism and Molecular Nonlinear Optical Second-Order Response Meet in a Spin Crossover Complex
International audience; The quadratic hyperpolarizability of two inorganic Schiff base metal complexes which differ from each other by the nature of the central metal ion (FeII or ZnII) is estimated using hyper-Rayleigh light-scattering (HRS) measurements. The investigated FeII microcrystals exhibit a thermal spin-crossover (SCO) from a diamagnetic to a paramagnetic state centered at T1/2 = 233 K that can be reproduced by the HRS signal whose modest intensity is mainly due to their centrosymmetric packing structure. Diamagnetic ZnII microcrystals even lead to much weaker (∼400 times) HRS intensities which are in addition temperature-independent. These observations allow us to ascribe the ch…
Spin Crossover in Fe(II)–M(II) Cyanoheterobimetallic Frameworks (M = Ni, Pd, Pt) with 2-Substituted Pyrazines
Discovery of spin-crossover (SCO) behavior in the family of Fe(II)-based Hofmann clathrates has led to a "new rush" in the field of bistable molecular materials. To date this class of SCO complexes is represented by several dozens of individual compounds, and areas of their potential application steadily increase. Starting from Fe(2+), square planar tetracyanometalates M(II)(CN)4(2-) (M(II) = Ni, Pd, Pt) and 2-substituted pyrazines Xpz (X = Cl, Me, I) as coligands we obtained a series of nine new Hofmann clathrate-like coordination frameworks. X-ray diffraction reveals that in these complexes Fe(II) ion has a pseudo-octahedral coordination environment supported by four μ4-tetracyanometallat…
Crystal structure and magnetic properties of (tris{4-[1-(2-methoxyethyl)imidazol-2-yl]-3-azabut-3-enyl}amine)iron(II) bis(hexafluoridophosphate)
The title compound, [Fe(C27H41N10O3)](PF6)2, is an example of an iron(II) spin-crossover compound. In this compound, C⋯F and CH⋯F/O contacts, present between the cations and anions, extend the structure into a three-dimensional supramolecular network.
New reaction of 1H-pyrazoles with selenium dioxide: one-pot synthesis of bis(1H-pyrazol-4-yl)selenides
Abstract A novel reaction between 3- and 3,5-substituted pyrazoles with selenium dioxide proceeds with formation of bis(3R,5R′-1H-pyrazol-4-yl)selenides in high yield. On this basis, an efficient one-pot synthetic procedure has been developed. In the case of the unsubstituted pyrazole a selenonium compound has been obtained. The identity and structure of the isolated selenium derivatives have been confirmed by spectral methods and their molecular structures investigated by X-ray analysis.
Synthesis, solid state and solution studies of cobalt(II) complexes with 2-hydroxyiminopropanoic acid
Abstract This paper describes the synthesis of the Zn(II) complex with H2L = 2-hydroxyiminopropanoic acid. The final structure incorporated two linear dimeric anions with two Zn2+ atoms, which are linked by a carbonate anion into a tetranuclear unit. In each dinuclear unit, the two Zn(II) ions are coordinated by three molecules of the doubly deprotonated ligand in two different coordination modes. This result is confirmed both by X-ray crystallography and by ESI-MS investigations of the crystals dissolved in water. Equilibrium studies of the zinc(II) complexes formed by H2L in aqueous solution based on independent pH-metric titrations and zinc ion-selective electrode (ISE) titrations indica…
Complex formation of copper( ), nickel( ) and zinc( ) with ethylophosphonoacetohydroxamic acid: solution speciation, synthesis and structural characterization
We present herein the thermodynamic and X-ray characterisation of a novel ethyl phosphonohydroxamic acid-based Cu( ) metallacrown, predominating in solution in a broad pH range.
CCDC 1422402: Experimental Crystal Structure Determination
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CCDC 1422398: Experimental Crystal Structure Determination
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CCDC 1422396: Experimental Crystal Structure Determination
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CCDC 1422397: Experimental Crystal Structure Determination
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CCDC 1480686: Experimental Crystal Structure Determination
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CCDC 1534663: Experimental Crystal Structure Determination
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CCDC 867361: Experimental Crystal Structure Determination
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CCDC 1400635: Experimental Crystal Structure Determination
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CCDC 1480684: Experimental Crystal Structure Determination
Related Article: Olesia I. Kucheriv, Sergii I. Shylin, Vadim Ksenofontov, Sebastian Dechert, Matti Haukka, Igor O. Fritsky, and Il’ya A. Gural’skiy|2016|Inorg.Chem.|55|4906|doi:10.1021/acs.inorgchem.6b00446
CCDC 1422405: Experimental Crystal Structure Determination
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CCDC 1422399: Experimental Crystal Structure Determination
Related Article: Il'ya A. Gural'skiy, Bohdan O. Golub, Sergii I. Shylin, Vadim Ksenofontov, Helena J. Shepherd, Paul R. Raithby, Wolfgang Tremel and Igor O. Fritsky|2016|Eur.J.Inorg.Chem.||3191|doi:10.1002/ejic.201600406
CCDC 1534662: Experimental Crystal Structure Determination
Related Article: Karolina Zdyb, Maxym O. Plutenko, Rostislav D. Lampeka, Matti Haukka, Malgorzata Ostrowska, Igor O. Fritsky, Elzbieta Gumienna-Kontecka|2017|Polyhedron|137|60|doi:10.1016/j.poly.2017.07.009
CCDC 1534661: Experimental Crystal Structure Determination
Related Article: Karolina Zdyb, Maxym O. Plutenko, Rostislav D. Lampeka, Matti Haukka, Malgorzata Ostrowska, Igor O. Fritsky, Elzbieta Gumienna-Kontecka|2017|Polyhedron|137|60|doi:10.1016/j.poly.2017.07.009
CCDC 1480687: Experimental Crystal Structure Determination
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CCDC 1422403: Experimental Crystal Structure Determination
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CCDC 1478973: Experimental Crystal Structure Determination
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CCDC 1400636: Experimental Crystal Structure Determination
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CCDC 1455020: Experimental Crystal Structure Determination
Related Article: Maksym Seredyuk, Kateryna Znovjyak, M. Carmen Muñoz, Yurii Galyametdinov, Igor O. Fritsky, Jose A. Real|2016|RSC Advances|6|39627|doi:10.1039/C6RA05342D
CCDC 1455021: Experimental Crystal Structure Determination
Related Article: Maksym Seredyuk, Kateryna Znovjyak, M. Carmen Muñoz, Yurii Galyametdinov, Igor O. Fritsky, Jose A. Real|2016|RSC Advances|6|39627|doi:10.1039/C6RA05342D
CCDC 1878182: Experimental Crystal Structure Determination
Related Article: Volodymyr M. Hiiuk, Sergiu Shova, Aurelian Rotaru, Vadim Ksenofontov, Igor O. Fritsky, Il'ya A. Gural'skiy|2019|Chem.Commun.|55|3359|doi:10.1039/C8CC10260K
CCDC 867362: Experimental Crystal Structure Determination
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CCDC 1534660: Experimental Crystal Structure Determination
Related Article: Karolina Zdyb, Maxym O. Plutenko, Rostislav D. Lampeka, Matti Haukka, Malgorzata Ostrowska, Igor O. Fritsky, Elzbieta Gumienna-Kontecka|2017|Polyhedron|137|60|doi:10.1016/j.poly.2017.07.009
CCDC 1422404: Experimental Crystal Structure Determination
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CCDC 2045994: Experimental Crystal Structure Determination
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CCDC 875578: Experimental Crystal Structure Determination
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CCDC 2045993: Experimental Crystal Structure Determination
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CCDC 1534664: Experimental Crystal Structure Determination
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CCDC 1458636: Experimental Crystal Structure Determination
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CCDC 1480685: Experimental Crystal Structure Determination
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CCDC 1422400: Experimental Crystal Structure Determination
Related Article: Il'ya A. Gural'skiy, Bohdan O. Golub, Sergii I. Shylin, Vadim Ksenofontov, Helena J. Shepherd, Paul R. Raithby, Wolfgang Tremel and Igor O. Fritsky|2016|Eur.J.Inorg.Chem.||3191|doi:10.1002/ejic.201600406
CCDC 1480683: Experimental Crystal Structure Determination
Related Article: Olesia I. Kucheriv, Sergii I. Shylin, Vadim Ksenofontov, Sebastian Dechert, Matti Haukka, Igor O. Fritsky, and Il’ya A. Gural’skiy|2016|Inorg.Chem.|55|4906|doi:10.1021/acs.inorgchem.6b00446
CCDC 1878181: Experimental Crystal Structure Determination
Related Article: Volodymyr M. Hiiuk, Sergiu Shova, Aurelian Rotaru, Vadim Ksenofontov, Igor O. Fritsky, Il'ya A. Gural'skiy|2019|Chem.Commun.|55|3359|doi:10.1039/C8CC10260K
CCDC 867363: Experimental Crystal Structure Determination
Related Article: Elzbieta Gumienna-Kontecka, Irina A. Golenya, Agnieszka Szebesczyk, Matti Haukka, Roland Krämer, and Igor O. Fritsky|2013|Inorg.Chem.|52|7633|doi:10.1021/ic4007229
CCDC 1534659: Experimental Crystal Structure Determination
Related Article: Karolina Zdyb, Maxym O. Plutenko, Rostislav D. Lampeka, Matti Haukka, Malgorzata Ostrowska, Igor O. Fritsky, Elzbieta Gumienna-Kontecka|2017|Polyhedron|137|60|doi:10.1016/j.poly.2017.07.009
CCDC 1480682: Experimental Crystal Structure Determination
Related Article: Olesia I. Kucheriv, Sergii I. Shylin, Vadim Ksenofontov, Sebastian Dechert, Matti Haukka, Igor O. Fritsky, and Il’ya A. Gural’skiy|2016|Inorg.Chem.|55|4906|doi:10.1021/acs.inorgchem.6b00446
CCDC 875577: Experimental Crystal Structure Determination
Related Article: Aleksander Kufelnicki, Stefania V. Tomyn, Victoria Vitske, Jolanta Jaciubek-Rosińska, Matti Haukka, Igor O. Fritsky|2013|Polyhedron|56|144|doi:10.1016/j.poly.2013.03.053
CCDC 1422401: Experimental Crystal Structure Determination
Related Article: Il'ya A. Gural'skiy, Bohdan O. Golub, Sergii I. Shylin, Vadim Ksenofontov, Helena J. Shepherd, Paul R. Raithby, Wolfgang Tremel and Igor O. Fritsky|2016|Eur.J.Inorg.Chem.||3191|doi:10.1002/ejic.201600406