Interplay between Chemical Composition and Cation Ordering in the Magnetism of Ni/Fe Layered Double Hydroxides

We report the synthesis of a family of ferrimagnetic NiFe layered double hydroxides (LDHs) with a variable Ni(2+)/Fe(3+) in-plane composition of [Ni(1-x)Fe(x)(OH)2](CO3)(x/2)·yH2O (x = 0.20, 0.25, and 0.33) by following a modified homogeneous precipitation. These layered magnets display high crystallinity, homogeneous hexagonal morphologies, and micrometric size that enable their quantitative exfoliation into single layers by sonomechanical treatment of the solids in polar solvents. This was confirmed by dynamic light scattering, UV-vis spectroscopy, high-resolution transmission electron miscroscopy, and atomic force microscopy methodologies to study the resulting steady suspensions. Our ma…

Cubane-Type Mo3FeS44+,5+ Complexes Containing Outer Diphosphane Ligands: Ligand Substitution Reactions, Spectroscopic Studies, and Electronic Structure

A general protocol to access Mo(3)FeS(4)(4+) clusters selectively modified at the Fe coordination site is presented starting from the all-chlorine Mo(3)(FeCl)S(4)(dmpe)(3)Cl(3) (1) [dmpe = 1,2-bis(dimethylphosphane-ethane)] cluster and tetrabutylammonium salts (n-Bu(4)NX) (X = CN(-), N(3)(-), and PhS(-)). Clusters Mo(3)(FeX)S(4)(dmpe)(3)Cl(3) [X = CN(-) (2), N(3)(-) (3), and PhS(-) (4)] are prepared in high yield, and comparison of geometric and redox features upon modification of the coordination environment at the Fe site at parity of ligands at the Mo sites is also presented. The existence of the cubane-type Mo(3)FeS(4)(4+,5+) redox couple is demonstrated by cyclic voltammetry and for co…

Iron(ii) complexes of tris(2-pyridylmethyl)amine (TPMA) and neutral bidentate ligands showing thermal- and photo-induced spin crossover

Three new mononuclear Fe(ii) complexes have been prepared and characterized by the combination of tetradentate tris(2-pyridylmethyl)amine (TPMA) with three neutral bidentate ligands, such as ethylenediamine (en), 1,2-diaminopropane (pn) and 2-picolylamine (2-pic), in compounds [FeII(TPMA)(en)](ClO4)2 (1), [FeII(TPMA)(2-pic)](ClO4)2 (2) and [FeII(TPMA)(pn)](ClO4)2 (3). Structural and magnetic characterization demonstrates that the three compounds present a complete SCO behavior. The absence of strong intermolecular interactions and solvent molecules leads to reversible and gradual spin transitions. The different ligands allow tuning T1/2 from 130 K (2) to 325 K (3). The compound with the low…

Prussian blue@MoS2 layer composites as highly efficient cathodes for sodium- and potassium-ion batteries

Prussian blue (PB) represents a simple, economical, and eco‐friendly system as cathode material for sodium‐ion batteries (SIBs). However, structural problems usually worsen its experimental performance thus motivating the search for alternative synthetic strategies and the formation of composites that compensate these deficiencies. Herein, a straightforward approach for the preparation of PB/MoS2‐based nanocomposites is presented. MoS2 provides a 2D active support for the homogeneous nucleation of porous PB nanocrystals, which feature superior surface areas than those obtained by other methodologies, giving rise to a compact PB shell covering the full flake. The nanocomposite exhibits an ex…

Isoreticular two-dimensional magnetic coordination polymers prepared through pre-synthetic ligand functionalization

Chemical functionalization is a powerful approach to tailor the physical and chemical properties of two-dimensional (2D) materials, increase their processability and stability, tune their functionalities and, even, create new 2D materials. This is typically achieved through post-synthetic functionalization by anchoring molecules on the surface of an exfoliated 2D crystal, but it inevitably alters the long-range structural order of the material. Here we present a pre-synthetic approach that allows the isolation of crystalline, robust and magnetic functionalized monolayers of coordination polymers. A series of five isostructural layered magnetic coordination polymers based on Fe(ii) centres a…

Multifunctional magnetic materials obtained by insertion of spin-crossover Fe(III) complexes into chiral 3D bimetallic oxalate-based ferromagnets.

The syntheses, structures, and magnetic properties of compounds of formula [Fe(III)(5-Clsal(2)-trien)][Mn(II)Cr(III)(ox)(3)]·0.5(CH(3)NO(2)) (1), [Fe(III)(5-Brsal(2)-trien)][Mn(II)Cr(III)(ox)(3)] (2), and [In(III)(5-Clsal(2)-trien)][Mn(II)Cr(III)(ox)(3)] (3) are reported. The structure of the three compounds, which crystallize in the orthorhombic P2(1)2(1)2(1) chiral space group, presents a 3D chiral anionic network formed by Mn(II) and Cr(III) ions linked through oxalate ligands with inserted [Fe(III)(5-Clsal(2)-trien)](+), [Fe(III)(5-Brsal(2)-trien)](+), and [In(III)(5-Clsal(2)-trien)](+) cations. The magnetic properties indicate that the three compounds undergo long-range ferromagnetic o…

Cover Feature: Fundamental Insights into the Covalent Silane Functionalization of NiFe Layered Double Hydroxides (Chem. Eur. J. 29/2020)

A highly stable and hierarchical tetrathiafulvalene-based metal organic framework with improved performance as a solid catalyst

[EN] Herein we report the synthesis of a tetrathiafulvalene (TTF)-based MOF, namely MUV-2, which shows a non-interpenetrated hierarchical crystal structure with mesoporous one-dimensional channels of ca. 3 nm and orthogonal microporous channels of ca. 1 nm. This highly stable MOF (aqueous solution with pH values ranging from 2 to 11 and different organic solvents), which possesses the well-known [Fe3(¿3-O)(COO)6] secondary building unit, has proven to be an efficient catalyst for the aerobic oxidation of dibenzothiophenes.

Spontaneous Magnetization in Heterometallic NiFe-MOF-74 Microporous Magnets by Controlled Iron Doping

We report the direct synthesis of mixed-metal NiFe-MOF-74 solids that display combination of porosity with ferrimagnetic ordering. Compared to the undoped Ni phase, controlled doping with Fe enables to modify intra and interchain magnetic interactions for the onset of spontaneous magnetization at temperatures fixed by the doping level. Synthesis of porous magnets remains somewhat elusive due to the difficulties in isolating foreseeable metal-organic architectures that combine small bridging linkers, for strong magnetic coupling, with polyaromatic connectors responsible for porosity. In turn, we demonstrate that metal doping is better fitted to modify the magnetism of Metal-Organic Framework…

Exploiting the Redox Activity of MIL-100(Fe) Carrier Enables Prolonged Carvacrol Antimicrobial Activity

The design of efficient food contact materials that maintain optimal levels of food safety is of paramount relevance to reduce the increasing number of foodborne illnesses. In this work, we develop a smart composite metal-organic framework (MOF)-based material that fosters a unique prolonged antibacterial activity. The composite is obtained by entrapping a natural food preserving molecule, carvacrol, into a mesoporous MIL-100(Fe) material following a direct and biocompatible impregnation method, and obtaining particularly high payloads. By exploiting the intrinsic redox nature of the MIL-100(Fe) material, it is possible to achieve a prolonged activity against Escherichia coli and Listeria i…

Hybrid materials containing organometallic cations and 3-D anionic metal dicyanamide networks of type [Cp*2M][M′(dca)3]

A new series of hybrid materials of type [Cp*2M][M′(dca)3] has been prepared by cation templation and structurally characterised (M = Fe(III), Co(III); M′ = Mn(II), Fe(II), Co(II), Ni(II), Cd(II); dca− = N(CN)2−). The crystallographic analysis of [Cp*2Fe][Cd(dca)3] showed that the [Cd(dca)3]− anionic framework is of a symmetrical 3-D α-polonium type, containing octahedral Cd nodes and μ1,5-dca bridging ligands. The [Cp*2Fe]+ cations occupy the cube-like cavities within the framework. The cationic and anionic-framework sublattices remain magnetically independent and display susceptibilities, over the range 300 to 2 K, of a Curie–Weiss nature obtained by adding a S = 1/2 (Cp*2Fe+) or a S = 0 …

Heterometallic Titanium-Organic Frameworks as Dual Metal Catalysts for Synergistic Non-Buffered Hydrolysis of Nerve Agent Simulants

Heterometallic metal-organic frameworks (MOFs) can offer important advantages over their homometallic counterparts to enable targeted modification of their adsorption, structural response, electronic structure, or chemical reactivity. However, controlling metal distribution in these solids still remains a challenge. The family of mesoporous titanium-organic frameworks, MUV-101(M), displays heterometallic TiM2 nodes assembled from direct reaction of Ti(IV) and M(II) salts. We use the degradation of nerve agent simulants to demonstrate that only TiFe2 nodes are capable of catalytic degradation in non-buffered conditions. By using an integrative experimental-computational approach, we rational…

Spin-crossover complex encapsulation within a magnetic metal-organic framework.

The solid-state incorporation of a mononuclear iron(III) complex within the pores of a magnetic 3D metal–organic framework (MOF) in a single crystal to single crystal process leads to the formation of a new hybrid material showing both a guest-dependent long-range magnetic ordering and a spin-crossover (SCO) behaviour.

Modeling the magnetic properties and Mössbauer spectra of multifunctional magnetic materials obtained by insertion of a spin-crossover Fe(III) complex into bimetallic oxalate-based ferromagnets.

In this article, we present a theoretical microscopic approach to describe the magnetic and spectroscopic behavior of multifunctional hybrid materials which demonstrate spin crossover and ferromagnetic ordering. The low-spin to high-spin transition is considered as a cooperative phenomenon that is driven by the interaction of the electronic shells of the Fe ions with the full symmetric deformation of the local surrounding that is extended over the crystal lattice via the acoustic phonon field. The proposed model is applied to the analysis of the series [Fe(III)(sal2-trien)] [Mn(II)Cr(III)(ox)3]·solv, in short 1·solv, where solv = CH2Cl2, CH2Br2, and CHBr3.

Hydrogen-bonded networks of [Fe(bpp)2]2+spin crossover complexes and dicarboxylate anions: structural and photomagnetic properties

The paper reports the syntheses, crystal structures, thermal and (photo)magnetic properties of spin crossover salts of formula [Fe(bpp)2](C6H8O4)·4H2O (1·4H2O), [Fe(bpp)2](C8H4O4)·2CH3OH·H2O (2·2MeOH·H2O) and [Fe(bpp)2](C8H4O4)·5H2O (2·5H2O) (bpp = 2,6-bis(pyrazol-3yl)pyridine; C6H8O4 = adipate dianion; C8H4O4 = terephthalate dianion). The salts exhibit an intricate network of hydrogen bonds between low-spin iron(II) complexes and carboxylate dianions, with solvent molecules sitting in the voids. Desolvation is accompanied by a low-spin (LS) to high-spin (HS) transformation in the materials. The dehydrated phase 2 undergoes a two-step transition with a second step showing thermal hysteresis…

Multifunctional magnetic materials obtained by insertion of a spin-crossover Fe(III) complex into bimetallic oxalate-based ferromagnets.

The syntheses, structures and magnetic properties of the compounds of formula [Fe(III)(sal(2)-trien)][Mn(II)Cr(III)(ox)(3)].CH(2)Cl(2) (1; H(2)sal(2)-trien=N,N'-disalicylidenetriethylenetetramine, ox=oxalate), [Fe(III)(sal(2)-trien)][Mn(II)Cr(III)(ox)(3)].CH(3)OH (2), [In(III)(sal(2)-trien)][Mn(II)Cr(III)(ox)(3)].0.25H(2)O.0.25CH(3)OH.0.25CH(3)CN (3), and [In(III)(sal(2)-trien)][Mn(II)Cr(III)(ox)(3)].CH(3)NO(2).0.5H(2)O (4) are reported. The structure of 1 presents a 2D honeycomb anionic layer formed by Mn(II) and Cr(III) ions linked through oxalate ligands and a cationic layer of [Fe(sal(2)-trien)](+) complexes intercalated between the 2D oxalate network. The structures of 2, 3, and 4 pres…

Light-induced decarboxylation in a photo-responsive iron-containing complex based on polyoxometalate and oxalato ligands.

A new iron-oxalato polyoxometalate exhibits a remarkable photocoloration effect in the solid state based entirely on an intramolecular process.

Oxalate-Based Soluble 2D Magnets: The Series [K(18-crown-6)]3[MII3(H2O)4{MIII(ox)3}3] (MIII = Cr, Fe; MII = Mn, Fe, Ni, Co, Cu; ox = C2O42−; 18-crown-6 = C12H24O6)

The synthesis and magnetic properties of the oxalate-based molecular soluble magnets with general formula [K(18-crown-6)] 3[M (II) 3(H 2O) 4{M (III)(ox) 3} 3] (M (III) = Cr, Fe; M (II) = Mn, Fe, Ni, Co, Cu; ox = C 2O 4 (2-)) are here described. All the reported compounds are isostructural and built up by 2D bimetallic networks formed by alternating M (III) and M (II) ions connected through oxalate anions. Whereas the Cr (III)M (II) derivatives behave as ferromagnets with critical temperatures up to 8 K, the Fe (III)M (II) present ferri- or weak ferromagnetic ordering up to 26 K.

Oxalate‐Based 3D Chiral Magnets: The Series [Z II (bpy) 3 ][ClO 4 ][M II Fe III (ox) 3 ] (Z II = Fe, Ru; M II = Mn, Fe; bpy = 2,2'‐Bipyridine; ox = Oxalate Dianion)

The synthesis, structure, and physical properties of the oxalate-based molecular magnets with the formula [ZII(bpy)3][ClO4][MIIFeIII(ox)3] (ZII = Fe, Ru; MII = Mn, Fe; bpy = 2,2'-bipyridine; ox = oxalate dianion) are presented here. All compounds are isostructural and crystallize in the chiral cubic space group P4132, and contain three-dimensional dimetallic networks formed by alternating MII and MIII ions that are connected by oxalate anions. These compounds exhibit strong antiferromagnetic interactions that give rise to magnetic ordering as ferrimagnets or weak ferromagnets, with critical temperatures of up to 20 K, which is twice as high as those found for the isostructural magnets based…

Temperature dependence of desolvation effects in hydrogen-bonded spin crossover complexes

The synthesis, crystal structure and (photo)magnetic properties of the anhydrous spin crossover salt of formula [Fe(bpp)2](C6H8O4) (1) (bpp = 2,6-bis(pyrazol-3-yl)pyridine; C6H8O4 = adipate dianion), obtained by desolvation at 400 K of the original tetrahydrate in a single-crystal-to-single-crystal (SC–SC) transformation, are reported. This work offers a comparison between this compound and the previously reported hydrated material ([Fe(bpp)2](C6H8O4)·4H2O, 1·4H2O), highlighting the significance of the thermal conditions used in the dehydration-rehydration processes. In both compounds, a hydrogen-bonded network between iron(II) complexes and adipate anions is observed. The original tetrahyd…

Fundamental Insights into the Covalent Silane Functionalization of NiFe Layered Double Hydroxides

Layered double hydroxides (LDHs) are a class of 2D anionic materials exhibiting wide chemical versatility and promising applications in different fields, ranging from catalysis to energy storage and conversion. However, the covalent chemistry of this kind of 2D materials is still barely explored. Herein, the covalent functionalization with silanes of a magnetic NiFe-LDH is reported. The synthetic route consists of a topochemical approach followed by anion exchange reaction with surfactant molecules prior to covalent functionalization with the (3-aminopropyl)triethoxysilane (APTES) molecules. The functionalized NiFe-APTES was fully characterized by X-ray diffraction, infrared spectroscopy, e…

Hybrid magnetic superconductors formed by TaS2 layers and spin crossover complexes.

The restacking of charged TaS2 nanosheets with molecular counterparts has so far allowed for the combination of superconductivity with a manifold of other molecule-intrinsic properties. Yet, a hybrid compound that blends superconductivity with spin crossover switching has still not been reported. Here we continue to exploit the solid-state/molecule-based hybrid approach for the synthesis of a layered TaS2-based material that hosts Fe(2+) complexes with a spin switching behavior. The chemical design and synthetic aspects of the exfoliation/restacking approach are discussed, highlighting how the material can be conveniently obtained in the form of highly oriented easy-to-handle flakes. Finall…

Ultramicroporous iron-isonicotinate MOFs combining size-exclusion kinetics and thermodynamics for efficient CO2/N2 gas separation

Two ultramicroporous 2D and 3D iron-based Metal-Organic Frameworks (MOFs) have been obtained by solvothermal synthesis using different ratios and concentrations of precursors. Their reduced pore space decorated with pendant pyridine from tangling isonicotinic ligands enables the combination of size-exclusion kinetic gas separation, due to their small pores, with thermodynamic separation, resulting from the interaction of the linker with CO2 molecules. This combined separation results in efficient materials for dynamic breakthrough gas separation with virtually infinite CO2/N2 selectivity in a wide operando range and with complete renewability at room temperature and ambient pressure.

Layered Molecule-Based Magnets Formed by Decamethylmetallocenium Cations and Two-Dimensional Bimetallic Complexes [MIIRuIII(ox)3]−(MII=;Mn, Fe, Co, Cu and Zn; ox=oxalate)

Abstract A new series of hybrid organometallic-inorganic layered magnets with formula [Z III Cp * 2 ] [M II Ru III (ox) 3 ] ( Z III =Co and Fe; M II =Mn, Fe, Co, Cu, and Zn; ox=oxalate: Cp * =pentamethylcyclopentadienyl) has been prepared. All of these compounds are isostructural to the previously reported [ Z III Cp * 2 ] [ M II M III (ox) 3 ] ( M III =Cr, Fe) series and crystallize in the monoclinic space group C 2/ m , as found by powder X-ray diffraction analysis. They are novel examples of magnetic materials formed by bimetallic oxalate-based extended layers separated by layers of organometallic cations. The magnetic properties of all these compounds have been investigated (ac and dc m…

Exploiting redox activity of MIL-100(Fe) carrier enables carvacrol prolonged antimicrobial activity

The design of efficient food contact materials that maintain optimal levels of food safety is of paramount relevance to reduce the increasing foodborne illnesses. In this work, we develop a smart composite MOF-based material that fosters a unique prolonged antibacterial activity. The composite is obtained by entrapping a natural preserving food molecule, carvacrol, into the mesoporous MIL-100(Fe) material following a direct and biocompatible impregnation method and obtaining particularly high payloads. By exploiting the intrinsic redox nature of MIL-100(Fe) material it is possible to achieve a prolonged activity against E. coli bacteria due to a triggered two-step carvacrol release of films…

Defect-Free Chemical Functionalization of Magnetic Monolayers Based on Coordination Polymers

<p>Chemical functionalization has demonstrated to be a powerful approach to tailor the physical and chemical properties of two-dimensional (2D) materials, to increase their processability and</p> <p>stability, to add new functionalities and, even, to create new 2D materials. However, this post synthetic method – which involves the anchoring of molecules on the surface of an exfoliated 2D crystal – inevitably leads to defective materials, which lack long-range structural order. If defect-free functionalized monolayers are required, a radically new approach needs to be developed. Here we present a pre-synthetic method based on coordination chemistry that affords the isolatio…

( n -Bu 4 N) 2 [Fe(dcbdt) 2 ] 2 . Synthesis, crystal structure and magnetic characterisation

Abstract The ( n -Bu 4 N) 2 [Fe(dcbdt) 2 ] 2 complex, where 4,5-dicyanobenzene-1,2-dithiolate (dcbdt), was prepared and characterised by X-ray diffraction, Mossbauer spectroscopy and magnetisation measurements. The crystal structure as determined by single crystal X-ray diffraction is triclinic, space group P 1 with cell parameters a =9.5660(1) A, b =13.0200(2) A, c =16.0850(2) A, α =67.554°(1), β =86.797°(1), γ =70.523°(1), V =1738.77(4) A 3 and it consists in strongly dimerised [Fe(dcbdt) 2 ] − units, which are stacked side by side as chains along a . The magnetic susceptibility shows that the [Fe(dcbdt) 2 ] − units have a low spin S =1/2 configuration and, besides a strong intradimer ant…

Synthesis, Chirality, and Magnetic Properties of Bimetallic Cyanide-Bridged Two-Dimensional Ferromagnets

The assembly of hexacyanoferrate(III) anions and nickel(II) bis-diamino complexes of the chiral ligand trans-cyclohexane-1,2-diamine (trans-chxn) yields cyanide-bridged two-dimensional ferromagnets of the general formula [Ni(trans-chxn)2]3[Fe(CN)6]2‚2H2O. Their crystal structure is built from cyanide-bridged bimetallic planes separated by the bulky chxn ligands, giving rise to a large interlayer distance ( d ) 11.7 A). These materials order ferromagnetically at the Curie temperature TC ) 14 K. AC susceptibility measurements evidence an unusual magnetic behavior below TC, with a marked frequency dependence. A thorough magnetic analysis demonstrates that this complex behavior is due to the pi…

Spin crossover FeII complexes as templates for bimetallic oxalate-based 3D magnets

Abstract We present the synthesis and structural characterization of the salt [Fe(bpp)2][MnCr(ox)3]2 · bpp · CH3OH. It crystallizes in the monoclinic space group. This material contains an anionic [MnCr(ox)3]− 3D 10-gon ferromagnetic network, that orders below 3.0 K. The channels created by this architecture are filled by the spin crossover cations [Fe(bpp)2]2+ (bpp = 2,6(bispyrazol-3-yl)pyridine), free ligand and solvent molecules. No spin transition has been observed at ambient pressure.

Stimuli responsive hybrid magnets : tuning the photoinduced spin-crossover in Fe(III) complexes inserted into layered magnets

The insertion of a [Fe(sal_2 trien)]^+ complex cation into a 2D oxalate network in the presence of different solvents results in a family of hybrid magnets with coexistence of magnetic ordering and photoinduced spin crossover (LIESST effect) in compounds [Fe^{III}(sal_2 trien)][Mn^{II}Cr^{III}(ox)_3]·CHCl_3 (1·CHCl_{3}) [Fe^{III}(sal_{2} trien)][Mn^{II}Cr^{III}(ox)_{3}]·CHBr_{3} (1·CHBr_{3}) and [Fe^{III}(sal_{2} trien)][Mn^{II}Cr^{III}(ox)_{3}]·CH_{2}Br_{2} (1·CH_{2}Br_{2}). The three compounds crystallize in a 2D honeycomb anionic layer formed by Mn^{II} and Cr^{III} ions linked through oxalate ligands and a layer of [Fe(sal_{2} trien)]^{+} complexes and solvent molecules (CHCl_{3} CHBr_{…

CCDC 1491308: Experimental Crystal Structure Determination

Related Article: Verónica Jornet-Mollá, Yan Duan, Carlos Giménez-Saiz, João C. Waerenborgh, Francisco M. Romero|2016|Dalton Trans.|45|17918|doi:10.1039/C6DT02934E

CCDC 1491307: Experimental Crystal Structure Determination

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CSD 1790045: Experimental Crystal Structure Determination

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CCDC 929206: Experimental Crystal Structure Determination

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CCDC 929201: Experimental Crystal Structure Determination

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CCDC 1579606: Experimental Crystal Structure Determination

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CCDC 1828115: Experimental Crystal Structure Determination

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CCDC 1828114: Experimental Crystal Structure Determination

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CCDC 1828117: Experimental Crystal Structure Determination

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CCDC 1828116: Experimental Crystal Structure Determination

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CCDC 929203: Experimental Crystal Structure Determination

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CCDC 2217201: Experimental Crystal Structure Determination

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CCDC 929204: Experimental Crystal Structure Determination

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CCDC 1507864: Experimental Crystal Structure Determination

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CCDC 929205: Experimental Crystal Structure Determination

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CCDC 1828113: Experimental Crystal Structure Determination

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CCDC 1491309: Experimental Crystal Structure Determination

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CCDC 2217199: Experimental Crystal Structure Determination

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CCDC 1819792: Experimental Crystal Structure Determination

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CCDC 2217200: Experimental Crystal Structure Determination

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CCDC 929202: Experimental Crystal Structure Determination

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CCDC 929207: Experimental Crystal Structure Determination

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