Papers by Kjell Ove Kongshaug
Dalton Transactions, 2003
ABSTRACT
Solid State Sciences, 2000
ABSTRACT The synthesis and crystal structure of a novel hydrated magnesium diphosphate and its hi... more ABSTRACT The synthesis and crystal structure of a novel hydrated magnesium diphosphate and its high temperature variant are described. Both structures were solved from powder X-ray diffraction data. The room temperature variant with composition Mg2P2O7·3.5H2O crystallises in the monoclinic space group P21/c (No. 14) with a=10.9317(1), b=8.05578(9), c=9.2774(1) Å, β=90.201(1)°, V=816.99(2) Å3 and Z=4. The structure consists of sheets stacked along [100] which are linked through MgO2(H2O)4 pillars into a three-dimensional framework with cavities containing water molecules. Within the sheets there are infinite edge-sharing chains of Mg octahedra along [010] which are cross linked by P2O74− groups. A high temperature variant exists around 200°C. The crystal structure of this compound with composition Mg2P2O7·H2O was solved and refined in the monoclinic space group C2/c (No. 15) with a=18.6596(4), b=7.9769(1), c=8.9757(2) Å, β=107.378(1)°, V=1275.01(4) Å3, Z=8. The transformation to Mg2P2O7·H2O involves removal of the water molecules in the cavities and the water molecules of the Mg octahedral pillars in Mg2P2O7·3.5H2O. The sheets in Mg2P2O7·3.5H2O however remain unchanged during the transformation as the water molecule coordinating Mg here is retained. These sheets are linked through tetrahedral MgO4 pillars into a three-dimensional structure containing infinite 10-membered ring channels along [001]. Both compounds have been further characterised by 31P MAS NMR spectroscopy, thermogravimetric analysis and high temperature powder X-ray diffraction.
Solid State Sciences, 2003
The two coordination polymers [Ni(ndc)(lutidine) 2 (H 2 O) 2 ], CPO-3, and [Ni 3 (ndc) 3 (pyridin... more The two coordination polymers [Ni(ndc)(lutidine) 2 (H 2 O) 2 ], CPO-3, and [Ni 3 (ndc) 3 (pyridine) 4 ], CPO-4, were obtained by hydrothermal reactions between 2,6-naphthalenedicarboxylic acid (ndc), 3,4-lutidine and nickel(II) nitrate (CPO-3) and ndc, pyridine and nickel(II) nitrate (CPO-4), respectively. In CPO-3, the combination of octahedral nickel(II) ions and ndc ligands leads to the formation of infinite chains. CPO-4 is based on linear trinuclear building units of octahedral nickel(II) ions that are crosslinked via the ndc ligands to form a 3Dstructure. The crystal structure of CPO-3 was solved from synchrotron powder X-ray data, while the crystal structure of CPO-4 was solved from conventional single-crystal X-ray data. Crystal data for CPO-3: monoclinic space group Cc (No. 9), a = 14.8583(2), b = 20.3985(3), c = 10.7258(1) Å, β = 129.0067(6) • , V = 2526.14(5) Å 3 and Z = 4. Crystal data for CPO-4: monoclinic space group P 2 1 /c (No. 14), a = 11.491(3), b = 17.917(4), c = 12.781(3) Å, β = 116.142(7) • , V = 2362.2(9) Å 3 and Z = 2. The thermal and magnetic properties of both compounds were investigated.
Journal of Solid State Chemistry, 2001
2 O, has been synthesized hydrothermally and characterized by synchrotron powder X-ray di4raction... more 2 O, has been synthesized hydrothermally and characterized by synchrotron powder X-ray di4raction, thermogravimetric analysis, and magnetic measurements. The compound is structurally closely related to both a magnesium phosphate and an iron phosphate, and crystallizes in the triclinic space group P-1 (No. 2) with a ؍ 12.81926(12) A > , b ؍ 15.87361(20) A > , c ؍ 6.47912(7) A > , ؍ 99.8660(11)3, ؍ 90.3913(10)3, ؍ 103.4265(9)3, V ؍ 1261.928(25) A > 3 , and Z ؍ 2. The structure consists of anionic sheets of manganese phosphate separated by piperazinium cations and water molecules. The basic building unit of the inorganic layers is a hexamer of edge-sharing Mn polyhedra. Magnetic susceptibility measurements and bond valence calculations con5rm the assignment of high-spin Mn 2؉ (d 5 ) in the title compound.
Journal of Materials Chemistry, 2000
The crystal structure of a new potassium stannosilicate K 4 Sn 2 Si 6 O 18 (AV-11) has been deter... more The crystal structure of a new potassium stannosilicate K 4 Sn 2 Si 6 O 18 (AV-11) has been determined ab initio from powder X-ray diffraction data. The unit cell is trigonal, space group R3 (no. 146), Z=3 with cell dimensions a = 10.1587, c = 14.8039 Å, γ= 120º, V = 1323 Å 3 . The structure is made up of SnO 6 octahedra and SiO 4 tetrahedra by sharing corners. The SiO 4 tetrahedra form a helix chain, periodically repeating every six tetrahedra. These chains extend along the [001] direction and are linked by isolated Sn-O octahedron giving a mixed framework.
Journal of Solid State Chemistry, 2003
A series of new nickel(II) perchlorate complexes containing an α-diimine(enR) and the anion of a ... more A series of new nickel(II) perchlorate complexes containing an α-diimine(enR) and the anion of a b-dione (1,3ketoenol or 1,3-ketoester, bH) was prepared and characterized. The composition and the overall structure of the new chelates depend on ligand concentration, on steric and electronic effects induced by substituents within the ligands and the ability of the perchlorate group to coordinate. The IR and electronic excitation spectra of [Ni enR) 2 b]ClO 4 and [Ni(enR)b(O 2 ClO 2 )] indicate, in conjunction with other physicochemical measurements, bidentate coordination of the ligands and replacement of the (O,O') perchlorato group by basic solvents. The structure of the new chelates was further supported by an X-ray structure analysis of [Ni(ncup) 2 Etacet]ClO 4 , where ncup denotes neocuproine and Etacet the anion of the ethyl acetoacetate (orthorhombic, space group Pc2 1 n, a = 14.087(5), b = 14.713(5) and c = 15.952(5) A Ê , Z = 4). The coordination sphere of nickel is a distorted octahedron, arised from the chromophore NiN 4 O 2 , in which the base is favored by three neocuproine nitrogens and one Etacet oxygen. The apical sites are occupied by the remaining oxygen and nitrogen atoms, one from Etacet and one from neocuproine respectively. Keywords: Ni II chelates of b-diones and α-diimines; spectra of mixed-ligand nickel(II) chelates; crystal and molecular structure of [Ni(ncup) 2 Etacet]ClO 4 Synthese und Charakterisierung von gemischten Nickel(II)-Chelaten mit b-Dionen und α-Diiminen. Kristall-und Molekularstruktur von [Ni(ncup) 2 Etacet]ClO 4 Inhaltsu È bersicht. Eine Reihe neuer Nickel(II)-perchlorat-Komplexe, die eine stickstoffhaltige Base(enR) und das Anion eines b-dions(bH) enthalten, wurde dargestellt und charakterisiert. Die Zusammensetzung und Struktur der neuen Chelate ist von der Liganden-Konzentration, von sterischen und elektronischen Effekten, welche durch die Substituenten der Liganden erzeugt werden und von der Fa È higkeit des Perchlorat-Anions zu koordinieren, abha È ngig. Die IR-und Elektronenspektren von [Ni(enR) 2 b]ClO 4 und [Ni(enR)b(O 2 ClO 2 )], zeigen zusammen mit anderen physikochemischen Eigenschaften zweiza È hnige Koordination der Liganden und Substitution der (O,O')-Perchlorato-Gruppe durch basische Lo È sungsmittel.
Journal of Solid State Chemistry, 2004
The two organically pillared layered zinc hydroxides [Zn 2 (OH) 2 (ndc)], CPO-6, and [Zn 3 (OH) 4... more The two organically pillared layered zinc hydroxides [Zn 2 (OH) 2 (ndc)], CPO-6, and [Zn 3 (OH) 4 (bpdc)], CPO-7, were obtained in hydrothermal reactions between 2,6-naphthalenedicarboxylic acid (ndc) and zinc nitrate (CPO-6) and 4,4 0 biphenyldicarboxylate (bpdc) and zinc nitrate (CPO-7), respectively. In CPO-6, the tetrahedral zinc atoms are connected by two m 2 -OH groups and two carboxylate oxygen atoms, forming infinite layers extending parallel to the bc-plane. These layers are pillared by ndc to form a threedimensional structure. In CPO-7, the zinc hydroxide layers are containing four-, five-and six coordinated zinc atoms, and the layers are built like stairways running along the [001] direction. Each step is composed of three infinite chains running in the [010] direction. Both crystal structures were solved from conventional single crystal data. Crystal data for CPO-6: Monoclinic space group P2 1 =c (No. 14), a ¼ 11:9703ð7Þ; b ¼ 7:8154ð5Þ; c ¼ 6:2428ð4Þ Å , b ¼ 90:816ð2Þ ; V ¼ 583:97ð6Þ Å 3 and Z ¼ 4: Crystal data for CPO-7: Monoclinic space group C2=c (No. 15), a ¼ 35:220ð4Þ; b ¼ 6:2658ð8Þ; c ¼ 14:8888ð17Þ Å , b ¼ 112:580ð4Þ ; V ¼ 3033:8ð6Þ Å 3 and Z ¼ 8: The compounds were further characterized by thermogravimetric-and chemical analysis. r 2004 Published by Elsevier Inc.
Cheminform, 2010
ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was e... more ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
Journal of Materials Chemistry, 2008
ABSTRACT
Solid State Sciences, 2001
ABSTRACT The synthesis and crystal structure of a novel hydrated magnesium phosphate is described... more ABSTRACT The synthesis and crystal structure of a novel hydrated magnesium phosphate is described. The crystal structure was solved from powder X-ray diffraction data. Mg3(PO4)2·4H2O crystallizes in the orthorhombic space group Cmc21 (No. 36) with a=8.41087(9) Å, b=17.3850(2) Å, c=12.8034(1) Å, V=1872.15(4) Å3 and Z=8. The structure consists of sheets stacked along [010], which are linked by edge sharing octahedral Mg2O6(H2O)4 dimers. Within the sheets there are infinite edge-sharing chains of Mg octahedra along [100]. The compound has been further characterized by 31P MAS NMR spectroscopy and thermogravimetric analysis. The crystal structure of two dehydrated variants existing around 200 (Mg3(PO4)2·2.5H2O) and 275°C (Mg3(PO4)2·2H2O) remain unknown.
Chemistry of Materials, 2000
The synthesis and crystal structure of Mg 4 (PO 4 ) 4 ‚2C 2 H 10 N 2 , which is the first example... more The synthesis and crystal structure of Mg 4 (PO 4 ) 4 ‚2C 2 H 10 N 2 , which is the first example of an organically templated open framework magnesium phosphate, is described. UiO-20 is characterized by means of single-crystal and powder X-ray diffraction, solid-state 31 P MAS NMR spectroscopy, and thermogravimetric analysis. Crystal data for UiO-20: space group C2/c (no. 15); a ) 20.9098
Adsorption-journal of The International Adsorption Society, 2008
Three different porous metal organic framework (MOF) materials have been prepared with and withou... more Three different porous metal organic framework (MOF) materials have been prepared with and without uncoordinated amine functionalities inside the pores. The materials have been characterized and tested as adsorbents for carbon dioxide. At 298 K the materials adsorb significant amount of carbon dioxide, the amine functionalised adsorbents having the highest CO2 adsorption capacities, the best adsorbing around 14 wt% CO2 at 1.0 atm CO2 pressure. At 25 atm CO2 pressure, up to 60 wt% CO2 can be adsorbed. At high pressures the CO2 uptake is mostly dependent on the available surface area and pore volume of the material in question. For one of the iso-structural MOF pairs the introduction of amine functionality increases the differential adsorption enthalpy (from isosteric method) from 30 to around 50 kJ/mole at low CO2 pressures, while the adsorption enthalpies reach the same level at increase pressures. The high pressure experimental results indicate that MOF based solid adsorbents can have a potential for use in pressure swing adsorption of carbon dioxide at elevated pressures.
Polyhedron, 2007
Two novel 3D coordination polymers {[Mn(aip)(DMF)]}n, CPO-9, and {[Mn3(Hatp)2(atp)2](H2O)2(DEF)4}... more Two novel 3D coordination polymers {[Mn(aip)(DMF)]}n, CPO-9, and {[Mn3(Hatp)2(atp)2](H2O)2(DEF)4}n CPO-10 (aip=5-aminoisophthalate, atp=2-aminoterephthalate, DMF=dimethylformamide, DEF=diethylformamide) have been synthesized by solvothermal methods. Their properties have been studied by single-crystal X-ray diffraction, thermogravimetric analysis, high-temperature powder X-ray diffraction and magnetic susceptibility measurements. The crystal structure of CPO-9 is based on infinite chains of carboxylato-bridged five-coordinated Mn(II) ions that are crosslinked via the aip ligands to form a 3D structure. CPO-10 is based on linear trinuclear building units of carboxylato-bridged octahedral Mn(II) ions that are crosslinked by the atp ligands into a 3D structure. Both compounds have 1D channels that contain solvent molecules. The solvent accessible void volume for CPO-10 is 51.9% of the unit cell volume. For both compounds, however, the solvent molecules cannot be removed without the collapse of the structures into amorphous phases at 250°C. The magnetic susceptibility measurements indicate antiferromagnetic couplings between the Mn(II) ions in both compounds. The magnetic data have been fitted using theoretical approaches.
Microporous and Mesoporous Materials, 2000
Supramolecular inclusion complexes, polyrotaxanes, of b-cyclodextrin with modified polydimethylsi... more Supramolecular inclusion complexes, polyrotaxanes, of b-cyclodextrin with modified polydimethylsiloxane were prepared. The structure and thermal properties of these complexes were studied as influenced by the preparation conditions, component ratio, and molecular weight of the polymer.
Microporous and Mesoporous Materials, 2000
... Full-size table (<1K). View Within Article. 3. Characterization and crystal structure dete... more ... Full-size table (<1K). View Within Article. 3. Characterization and crystal structure determination. 3.1. Crystal structure determination of UiO-18-as. ... View Within Article. 4. Crystal structures and phase transformations. 4.1. Crystal structure of UiO-18-as. ...
Journal of Materials Chemistry, 1999
ABSTRACT The synthesis and crystal structure of a novel layered aluminophosphate and its two high... more ABSTRACT The synthesis and crystal structure of a novel layered aluminophosphate and its two high temperature variants are described. All three structures were solved from powder X-ray diffraction data. The as-synthesized material (UiO-15-as), with composition [NH 3 (CH 2 ) 2 NH 3 ] 2+ [Al 2 (OH) 2 (PO 4 ) 2 (H 2 O)] 2– ·H 2 O, crystallizes in the space group P1 with a=10.37490(13), b=6.60775(8), c=9.90937(11) Å, α=90.762(1), β=115.265(1) and γ=90.162(1)°. In the aluminophosphate layers the five- and six-coordinated aluminium polyhedra form infinite chains along [010] that are crosslinked by phosphate groups. These layers are held together by a complex hydrogen bonding scheme involving the terminal oxygen atoms of the phosphate groups and the nitrogens of the ethylenediammonium ions. A high temperature variant exists around 125°C (UiO-15-125). This compound, with composition [NH 3 (CH 2 ) 2 NH 3 ] 2+ [Al 2 (OH) 2 (PO 4 ) 2 ] 2– , crystallizes in the monoclinic space group P2 1 /c with a=10.28899(23), b=6.75080(13), c=9.62527(20) Å and β=116.124(1)°. The transformation to UiO-15-125 involves removal of an interlamellar water molecule and another water molecule which is coordinated to aluminium. The infinite chains of aluminium polyhedra along [010] and the hydrogen bonding scheme of UiO-15-as is maintained in UiO-15-125. Another high temperature variant exists around 225°C (UiO-15-225). This compound, with composition [NH 3 (CH 2 ) 2 NH 3 ] 2+ [Al 2 O(PO 4 ) 2 ] 2– , crystallizes in the monoclinic space group P2 1 /c with a=9.42781(37), b=6.91370(19), c=9.40823(27) Å and β=113.002(1)°. The transformation to UiO-15-225 involves the release of a water molecule from UiO-15-125 and the formation of tetrahedral Al-O-Al bonding. UiO-15-225 is therefore the first compound among the aluminophosphates violating Loewensteins rule.
Dalton Transactions, 2008
The heterobimetallic metal-organic framework {[(BPDC)PtCl(2)](3)(Gd(H(2)O)(3))(2)}.5H(2)O (BPDC =... more The heterobimetallic metal-organic framework {[(BPDC)PtCl(2)](3)(Gd(H(2)O)(3))(2)}.5H(2)O (BPDC = 2,2&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;-bipyridine-5,5&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;-dicarboxylate) has been designed and synthesized by hydrothermal methods. The new coordination polymer contains subunits of (BPDC)PtCl(2) (1) where both N atoms of the BPDC ligand are attached to a square-planar Pt(II) center. The two remaining cis coordination sites at Pt(II) are occupied by chloride ions. The final structure (2) of the polymeric network is obtained when Gd(III) ions link together the (BPDC)PtCl(2) units, which are organized in sheets, into larger blocks. These blocks are stacked along the crystallographic [010] direction and are held together by a hydrogen bonding scheme that involves carboxylate oxygen atoms and water molecules in the coordination sphere of Gd. The coordination polymer 2 can be obtained in a single-step reaction or in a two-step synthesis where the corresponding Pt complex (1) was first synthesized followed by reacting 1 with Gd(NO(3))(3).6H(2)O. In situ high temperature powder X-ray diffraction shows that the crystalline coordination polymer transforms into an anhydrous modification at 100 degrees C. This modification is stable to 350 degrees C, at which temperature the structure starts to decompose. The coordination sphere around platinum in the polymer closely resembles organometallic Pt complexes that have been previously found to catalytically or stoichiometrically activate and functionalize hydrocarbon C-H bonds in homogeneous systems.
Microporous and Mesoporous Materials, 2000
Two novel ferrocenyl substituted N-acetyl-2pyrazolines, N-acetyl-3-(2-furyl)-5-ferrocenyl-2-pyraz... more Two novel ferrocenyl substituted N-acetyl-2pyrazolines, N-acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline (3) and N-acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline (4), have been synthesized and characterized by FTIR, 1 H-NMR, 13 C-NMR techniques, elemental analysis and X-ray structure analysis. Thermal properties of these compounds have been determined by TGA, DTA and DSC analysis. Compound 3 (C 19 H 18 N 2 O 2 Fe) crystallizes in the monoclinic space group P21/c and Z = 4, with a = 8.6970(4) Å , b = 18.4725(9) Å , c = 11.0041(5) Å , b = 110.942(3)°.
Microporous and Mesoporous Materials, 2000
ABSTRACT Two open-framework zinc phosphate materials denoted by UiO-21 and UiO-22 have been prepa... more ABSTRACT Two open-framework zinc phosphate materials denoted by UiO-21 and UiO-22 have been prepared by hydrothermal methods and characterised by single crystal X-ray diffraction. UiO-21, Zn7(PO4)6N6C12H34, crystallises in the trigonal space group R-3 (No. 148) with a=13.7249(2) Å, c=15.3316(1) Å, V=2501.13(5) Å3 and Z=3. The structure has the zeolite topology CHA with double six-ring units stacked in an AABBCC stacking sequence. At the centre of each double six-ring unit there is a zinc atom octahedrally coordinated to six out of the 12 oxygen atoms in the unit. Each cage of the structure contains two 1-(2-aminoethyl)piperazine molecules, each of which being disordered over three positions around the trigonal axis. Each molecule is doubly protonated to compensate for the negative charge of the zinc phosphate framework. There are no hydrogen bonding interactions between the organic templates and the inorganic framework. UiO-22, Zn4(PO4)3(OH)N3C6H17, crystallises in the triclinic space group P-1 with a=5.2697(1) Å, b=12.1400(2) Å, c=13.9161(3) Å, α=115.439(1)°, β=98.392(1)°, γ=91.157(1)°, V=791.91(3) Å3 and Z=2. The structure consists of vertex sharing PO4 and ZnO4 tetrahedra and is of the interrupted type by having terminal Zn–OH bonds and trigonally coordinated oxygen atoms. The structure can be viewed as built from columns of edge-sharing three and four rings running along [1 0 0] which interconnects into a framework exhibiting a two-dimensional eight and 12-ring channel system. Terminal OH groups are located in the staggered eight-ring channel running along [0 0 1]. In the 12-ring channel running along [1 0 0] there are highly disordered organic templates, probably 1-(2-aminoethyl)piperazine molecules that are doubly protonated in order to compensate for the negative charge of the zinc phosphate framework. The disordered nature of the organic templates in UiO-21 and UiO-22 indicates that the organic molecules play the role as space fillers in the crystallisation of these phases.
Journal of Solid State Chemistry, 2002
The two structurally related coordination polymers [Cu(ndc) (pyridine)], and [Zn(ndc)(3,4-lutidin... more The two structurally related coordination polymers [Cu(ndc) (pyridine)], and [Zn(ndc)(3,4-lutidine)], CPO-2-Zn, were obtained by hydrothermal reactions between 2,6-naphthalenedicarboxylic acid (ndc), pyridine and copper(II) nitrate (CPO-2-Cu) and ndc, 3,4-lutidine and zinc(II) nitrate (CPO-2-Zn), respectively. The compounds are based on the binuclear paddle-wheel building unit. In both compounds these building units are connected into 2D sheets by naphthalene rings. In the third dimension there are weaker interactions involving the axial ligands pyridine and 3,4-lutidine. The sheets are stacked so that large 1D channels are formed into which the axial ligands protrude. The crystal structure of CPO-2-Cu was solved from synchrotron powder X-ray data, while the crystal structure of CPO-2-Zn was solved from conventional single-crystal X-ray data. Crystal data for CPO-2-Cu: Monoclinic space group C2=m (No. 12), a ¼ 10:2252ð2Þ; b ¼ 19:0915ð4Þ; c ¼ 8:0521ð2Þ ( A, b ¼ 98:824ð1Þ1; V ¼ 1553:30ð7Þ ( A 3 and Z ¼ 4: Crystal data for CPO-2-Zn: Triclinic space group P À 1 (No. 2), a ¼ 7:540ð1Þ; b ¼ 10:711ð1Þ; c ¼ 11:196ð2Þ ( A, a ¼ 66:490ð5Þ1; b ¼ 87:265ð6Þ1; v ¼ 88:470ð6Þ1; V ¼ 828:2ð2Þ ( A 3 and Z ¼ 2: The thermal properties of both compounds were investigated as well as the magnetic properties of CPO-2-Cu. # 2002 Elsevier Science (USA)
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Papers by Kjell Ove Kongshaug