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1.
Crystals of PbCu3(OH)(NO3)(SeO3)3·1/2H2O [a=7.761(3)Å,b=9.478(4)Å,c=9.514(4)Å, =66.94(2)°, =69.83(2)°, =81.83(2)°, space group P ,Z=2] and Pb2Cu3O2(NO3)2(SeO3)2 [a=5.884(2)Å,b=12.186(3)Å,c=19.371(4)Å, space group Cmc21,Z=4] were synthesized under hydrothermal conditions. Their crystal structures were refined with three-dimensional X-ray data toR w=0.033 resp. 0.055. In PbCu3(OH)(NO3)(SeO3)3·1/2H2O the Cu atoms are [4+1] and [4+2] coordinated and via SeO3 groups a three-dimensional atomic arrangement is built up. In Pb2Cu3O2(NO3)2(SeO3)2 there are sheets, which are connected only via Pb-O bonds ranging from 2.98 Å to 3.16 Å.
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2.
Summary Single crystal X-ray data of the hydrothermally grown new phase Li2Cu3(SeO3)2(SeO4)2 were measured with a four-circle diffractometer up to sin /=0.81 Å–1 [I2/a,Z=4,V=1175.5 Å3,a=16.293(6),b=5.007(2),c=14.448(6) Å, = 94.21(1)°]. The structure was determined by direct and Fourier methods and refined toR=0.034,R w =0.027 for 2 086 independent reflections.Cu(1)[4+1]O5 forms a tetragonal pyramid, Cu(2)[4 + 2]O6 is a strongly elongated octahedron. The Li atom is surrounded by four O atoms forming a distorted tetrahedron. Se(IV)O3 and Se(VI)O4 groups are in accordance to literature, mean Se-O bond lengths are 1.714 and 1.644 Å.
Die Kristallstruktur von Li2Cu3(SeO3)2(SeO4)2
Zusammenfassung Einkristall-Röntgendaten der hydrothermal gezüchteten neuen Phase Li2Cu3(SeO3)2(SeO4)2 wurden mit einem Vierkreisdiffraktometer im Bereich bis zu sin /=0.81 Å–1 gemessen [I2/a,Z=4,V=1175.5 Å3,a=16.293(6),b=5.007(2),c=14.448(6) Å, =94.21(1)°]. Die Kristallstruktur wurde mittels direkter und Fourier-Methoden bestimmt und für 2 086 unabhängige Reflexe zuR=0.034,R w =0.027 verfeinert.Cu(1)[4+1]O5 bildet eine tetragonale Pyramide, Cu(2)[4+2]O6 ist ein stark verlängertes Oktaeder. Das Li-Atom ist von vier O-Atomen in Gestalt eines verzerrten Tetraeders umgeben. Die Se(IV)O3-und Se(VI)O4-Gruppen entsprechen der Literatur, die mittleren Se-O-Abstände betragen 1.714 und 1.644 Å.
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3.
Summary Single crystals of LiFe3+(SeO3)2 were prepared by hydrothermal synthesis. The crystal structure of LiFe3+(SeO3)2 is reported: tetragonal, space group I 2d,a=10.649(2) Å,c=9.959(2) Å,V=1129.4 Å3,Z=8, 1268 unique reflections,R=0.037. The structure contains LiFeO8 groups, built up by FeO6 octahedra edgesharing with strongly distorted LiO4 tetrahedra. These LiFeO8 groups share corners with trigonal pyramidal SeO3 groups to form a three dimensional network. The mean bondlengths are 1.994 Å, 2.006 Å and 1.699 Å for Li-O, Fe-O and Se(IV)-O, respectively.
Die Kristallstruktur von LiFe3+(SeO3)2
Zusammenfassung Einkristalle von LiFe3+(SeO3)2 wurden auf hydrothermalem Weg dargestellt und ihre Kristallstruktur bestimmt: tetragonal, Raumgruppe I 2d,a=10.649(2) Å,c=9.959(2) Å,V=1129.4 Å3,Z=8, 1268 unabhängige Reflexe,R=0.037. Kennzeichnend für die Atomanordnung sind LiFeO8 Gruppen, die aus FeO6 Oktaedern und mit ihnen kantenverknüpften, stark verzerrten LiO4 Tetraedern aufgebaut sind. Diese LiFeO8 Baueinheiten bilden, mit trigonal pyramidalen SeO3 Gruppen über Ecken verbunden, ein dreidimensionales Netzwerk. Die Mittelwerte der Li-O, Fe-O and Se(IV)-O Abstände sind 1.994 Å, 2.006 Å und 1.699 Å.
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4.
Summary The new synthetic compound ZnFe 2 3+ (SeO3)4 forms at low-hydrothermal conditions at 220 °C. It belongs to the monoclinic system; the structure was determined by single-crystal X-ray diffraction in the space group Pc. The unit cell data are:a=8.196(4) Å,b=7.997(4) Å,c=8.033(4) Å, =92.27(3)°,V=526.1 Å3;Z=2. The structure of ZnFe 2 3+ (SeO3)4 contains two types of FeO6 octahedra, one distorted ZnO5 trigonal bipyramid, and four selenite groups. Formal clusters consisting of the ZnO5 group, edge-linked with both FeO6 groups and one SeO3 pyramid, are connected by common corners, involving three further selenite groups to a framework structure.
Die Kristallstruktur von ZnFe 2 3+ (SeO3)4
Zusammenfassung Die neue synthetische Verbindung ZnFe 2 3+ (SeO3)4 bildet sich bei niedrighydrothermalen Bedingungen (220°C). Die Kristallstruktur wurde mit Einkristallröntgenmethoden in der monoklinen Raumgruppe Pc gelöst. Die Zellparameter sind:a=8.196(4) Å,b=7.997(4) Å,c=8.033(4) Å, =92.27(3)°,V=526.1 Å3;Z=2. Die Kristallstruktur von ZnFe 2 3+ (SeO3)4 weist zwei Arten von FeO6-Oktaedern, eine verzerrte trigonale ZnO5-Dipyramide sowie vier Selenitgruppen auf. Formal können Cluster, bestehend aus dem ZnO5-Polyeder, kantenverknüpft mit den beiden FeO6-Gruppen sowie einer SeO3-Pyramide, beschrieben werden. Die Verknüpfung über Ecken zu einer Gerüststruktur erfolgt unter Beteiligung von drei weiteren Selenitgruppen.
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5.
Syntheses within the system CuO-SeO2-H2O revealed four copper(II)-oxo-selenites. The crystal structures of these compounds were determined by single crystal X-ray techniques. Chemical formulae, lattice parameters and space groups are: Cu2O(SeO3)-I [a=8.925 (1) Å, P213], Cu2O(SeO3)-II [a=6.987 (5) Å,b=5.953 (4) Å,c=8.429 (6) Å, =92.17 (3)°, P21/n], Cu4O(SeO3)3-I [a=15.990 (8) Å,b=13.518 (8) Å,c=17.745 (12) Å, =90.49 (5)°, P21/a], and Cu4O(SeO3)3-II [a=7.992 (6) Å,b=8.141 (6) Å,c=8.391 (6) Å, =77.34 (3)°, =65.56 (3)°, =81.36 (3)°, ].All the Cu atoms are-with one exception-[4], [4+1], and [4+2] coordinated by O atoms. The four nearest O atoms are more or less distorted square planar arranged. Within the CuO4 squares the Cu-O bond lengths are significantly shorter for the [4] coordinated O atoms as compared with those of the [4+1] and [4+2] coordinated Cu atoms. The exception in the coordination of the Cu atoms is the Cu(1) atom in Cu2O(SeO3)-I with the site symmetry 3, which is trigonal dipyramidal [5] coordinated. A common feature of these four crystal structures is, that O atoms outside the SeO3 groups are tetrahedrally coordinated by four Cu(II) atoms. The Se atoms are as usual [3] coordinated, building up SeO3 pyramids. In all these four compounds the copper-oxygen polyhedra are combined to a three-dimensional network.
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6.
Summary Crystals of monoclinic Fe2(SeO4)3 were synthesized under hydrothermal conditions. The structure was determined by single crystal X-ray methods and refined in space group P21/n with 2 646 independent reflections (sin /<0.7 Å–1) toR=0.033,R w=0.037:a=8.530 (2) Å,b=8.888 (2) Å,c=11.952 (2) Å, =91.13 (1)°,V=906.0 Å3,Z=4. The crystal structure is isotypic with the monoclinic modification of Fe2(SO4)3, containing two different Fe(III) and three Se(VI) atomic positions. The FeO6 and SeO4 polyhedra are only slightly distorted, the mean Fe-O bond lengths are 1.986 Å and 2.004 Å, the average distances within the SeO4 tetrahedra are each 1.628 Å. The isolated FeO6 octahedra only share corners with SeO4 tetrahedra to build a framework structure.
Synthese und Kristallstruktur von monoklinem Fe2(SeO4)3
Zusammenfassung Kristalle von monoklinem Fe2(SeO4)3 wurden unter Hydrothermalbedingungen gezüchtet. Die Struktur wurde mit Einkristall-Röntgenmethoden bestimmt und in der Raumgruppe P21/n mit 2 646 unabhängigen Reflexen (sin /<0.7Å–1) aufR=0.033,R w=0.037 verfeinert:a=8.530(2) Å,b=8.888(2) Å,c=11.952(2) Å, =91.13(1)°,V=906.0 Å3,Z=4. Die Kristallstruktur ist isotyp mit der monoklinen Modifikation von Fe2(SO4)3, sie enthält zwei unterschiedliche Fe(III) und drei Se(VI) Atompositionen. Die FeO6-Polyeder sind nur gering verzerrt, die mittleren Fe-O Bindungslängen sind 1.986 Å und 2.004 Å, die mittleren Abstände in den SeO4-Tetraedern sind jeweils 1.628 Å. Die isolierten FeO6-Oktaeder sind nur über gemeinsame Ecken mit SeO4-Tetraedern verbunden, wobei eine Gerüststruktur entsteht.
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7.
The crystal structure of the new phase Cu7(OH)6(TeO3)2(SO4)2 [a=7.389 (1),b=7.638 (1),c=7.662 (2) Å, =75.17 (1), =75.90 (1), =84.19 (1)°;Z=1] was determined by direct methods andFourier summations from X-ray intensities, and was refined in space group P -C i 1 toR=0.039. As usual, the Cu(II) atoms are coordinated to four O atoms forming approximately a square with average Cu-O=1.96 (3) Å; one or two more distant O neighbours complete the coordination. The shape of the TeO3 group is a rather clear-cut trigonal pyramid. A disorder was found for the SO4 tetrahedra. The compound was synthesized under hydrothermal conditions [500 (10) K, saturation vapour pressure].
Herrn Prof. Dr.K. Komarek zum 60. Geburtstag gewidmet.  相似文献   

8.
Synthesis, Crystal Structure, and Vibrational Spectra of (n-Bu4N)2[(Mo6I)(NCS)] By treatment of [(Mo6I)I]2– with (SCN)2 in dichloromethane at –20 °C the hexaisothiocyanato cluster anion [(Mo6I)(NCS)]2– is formed. The X-ray structure determination of (n-Bu4N)2[(Mo6I)(NCS)] · 2 Me2CO (monoclinic, space group P21/c, a = 13.168(5), b = 11.964(5), c = 24.636(5) Å, β = 104.960(5)°, Z = 2) shows, that the thiocyanate groups are coordinated exclusively via N atoms with Mo–N bond lengths of 2.141–2.150 Å, Mo–N–C angles of 166–178° and N–C–S-angles of 174–180°. The vibrational spectra exhibit characteristic innerligand vibrations at 2073–2054 (νCN), 846–844 (νCS) and 480–462 cm–1NCS).  相似文献   

9.
Summary The compound RbFe(SeO4)2 was prepared hydrothermally by reaction of Rb2CO3 and FeC2O4·2H2O with H2O and H2SeO4 at 490 K. Single crystal X-ray methods revealed isotypy with KAl(SO4)2. RbFe(SeO4)2 crystallizes in space group P321;Z=1;a=5.005(1)Å,c=8.548(2) Å,V=185.4 Å3; 781 unique data up to 80 °2;R,R w =0.045, 0.042. The structure is best described as sheets of [Fe(SeO4)2] parallel (001), interconnected by Rb+. FeO6 trigonal prims and SeO4 tetrahedra have bond lengths of 1.99 Å and 1.63 Å, respectively. The Rb atom is [6 + 6] coordinated with Rb-O distances of 3.04 Å and 3.48 Å.
Die Kristallstruktur des wasserfreien Alauns RbFe3+(SeO4)2
Zusammenfassung Die Verbindung RbFe(SeO4)2 wurde hydrothermal dargestellt durch Reaktion von Rb2CO3 und FeC2O4·2H2O mit H2O und H2SeO4 bei 490K. Einkristallröntgenmethoden belegten die Isotypie mit KAl(SO4)2 RbFe(SeO4)2 kristallisiert in der Raumgruppe P321;Z=1;a=5.005(1) Å,c=8.548(2) Å,V=185.4 Å3; 781 unabhängige Daten bis 80 °2;R,R w =0.045, 0.042. Die Struktur läßt sich am besten als Schichten von [Fe(SeO4)2] parallel (001) beschreiben, die durch Rb+ verbunden sind. FeO6 trigonale Prismen und SeO4 Tetraeder weisen Bindungslängen von 1.99 Å bzw. 1.63 Å auf. Das Rb-Atom ist [6+6] koordiniert mit Rb-O Abständen von 3.04 Å und 3.48 Å.
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10.
Crystals of K2Co3(OH)2(SO4)3·2H2O were synthesized under hydrothermal conditions. The crystal structure [a=17.945 (4) Å,b=7.557 (2) Å,c=9.760 (3) Å, space group Cmc21,Z=4] was determined by direct methods and refined with single crystal X-ray data. The H atoms were located byFourier syntheses. Their structural parameters were refined, too. The finalR-values areR=0.025 andR w =0.028 (w=1/) for 612 reflections withF 0>3 (F 0). Both Co(II) atoms are octahedral six coordinated and form zigzag chains running parallel [001]. These chains are connected via sulfate groups to built up sheets parallel (100). The KO9 polyhedron and one of the four hydrogen bonds link these sheets.
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11.
Summary The crystal structure of synthetic Cu3SeO4(OH)4 was determined by single crystal X-ray methods:a=8.382 (2) Å,b=6.087 (1) Å,c=12.285 (2) Å,V=626.8 Å3,Z=4, space group Pnma,R=0.026,R w =0.021 for 1255 independent reflections (sin / 0.8 Å–1). The crystal structure is isotypic to that of the mineral antlerite, Cu3SO4(OH)4. The copper atoms are Jahn-Teller distorted with Cu[4+2]O6 polyhedra forming triple chains along [010]. These chains are linked via SeO4 tetrahedra and weak hydrogen bonds to a framework structure.
Die Kristallstruktur von synthetischem Cu3SeO4(OH)4
Zusammenfassung Die Kristallstruktur von synthetischem Cu3SeO4(OH)4 wurde mittels Einkristall-Röntgenmethoden ermittelt:a=8.382 (2) Å,b=6.087 (1) Å,c=12.285 (2) Å,V=626.8 Å3,Z=4, Raumgruppe Pnma,R=0.026,R w =0.021 für 1255 unabhängige Reflexe (sin / 0.8 Å–1). Die Kristallstruktur ist isotyp mit der des Minerals Antlerit, Cu3SO4(OH)4. Die Kupferatome sind Jahn-Teller-verzerrt, die Cu[4+2]O6 Polyeder bilden Dreierketten entlang [010]. Diese Ketten sind über SeO4-Tetraeder und schwache Wasserstoffbrücken zu einer Gerüststruktur verbunden.
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12.
Preparation and Crystal Structure of Diammin Magnesium Diazide Mg(NH3)2(N3)2 Diammin magnesium diazide was synthesized from Mg3N2 and NH4N3 in liquid ammonia and crystallized at 150 °C under autogenous atmosphere of HN3 and NH3 using sealed ampoules. Mg(NH3)2(N3)2 is a colorless, microcrystalline powder which can detonate above 180 °C. Caution, preparation and manipulation of Mg(NH3)2(N3)2 is very dangerous! The crystal structure was solved from powder data using the Patterson method and a Rietveld refinement was performed (Mg(NH3)2(N3)2, I 4/m, no. 87; a = 6.3519(1), c = 7.9176(2) Å; Z = 2, R(F2)= 0.1162). The crystal structure of Mg(NH3)2(N3)2 is related to that of SnF4. It consists of planes built up from corner sharing Mg(NH3)2(N3)4 octahedra connected equatorially over their four azide bridges with the ammonia ligands being in trans position. IR data were collected and interpreted in accordance with the structural data.  相似文献   

13.
Synthesis and Crystal Structure of the Selenyl-Phosphoraneiminato Complex SeO(NPPh3)2 SeO(NPPh3)2 has been prepared from SeO2 and Me3SiNPPh3 in a SeO2 suspension in acetonitrile, forming colourless crystals. The compound is characterized by IR spectroscopy and by a crystal structure determination. Space group P1 , Z = 2, structure solution with 5 344 observed unique reflections, R = 0.064. Lattice dimensions at ?40°C: a = 931.6, b = 947.6, c = 1 762 pm, α = 77.50°, β = 81.78°, γ = 79.23°. The compound forms monomeric molecules in which the selenium atom is φ-tetrahedrally surrounded with bond lengths SeO = 161.7 pm and SeN = 179.9 and 181.6 pm.  相似文献   

14.
The monoclinic compound PbCuAs2O7 [a=5.553 (1),b=8.404 (1),c=13.011 (2) Å, =91.61 (2)° space group P21/n-C 2h 5 ;Z=4] was synthesized under hydrothermal conditions. The structure was solved by direct methods and was refined to anR value of 3.6%. The Pb atom is irregularly eight coordinated by O atoms, and the Cu atom tetragonal pyramidal [4+1] coordinated by O atoms. Each two AsO4 tetrahedra share a common O atom corner building up As2O7 groups. These groups are connected with the CuO4 polyhedra to sheets parallel (101). These sheets are combined by the PbO8 polyhedra to a framework.
Herrn Prof. Dr.K. Komarek zum 60. Geburtstag gewidmet.  相似文献   

15.
Anhydrous Selenites of Lanthanum: Syntheses and Crystal Structures of La2(SeO3)3 and LaFSeO3 Colorless single crystals of La2(SeO3)3 were obtained via the decomposition of La2(SeO4)3 in the presence of NaCl in sealed gold ampoules. The compound crystallizes in the orthorhombic system (Pnma, Z = 4, a = 846.7(1), b = 1428.6(1), c = 710.3(2) pm, Rall = 0.0223) and contains La3+ in tenfold coordination of oxygen atoms which belong to seven SeO32– groups. Hence, three of the latter act as bidentate ligands. The reaction of LiF with La2(SeO4)3 in sealed gold ampoules yielded colorless single crystals of LaFSeO3 (monoclinic, P21/c, Z = 12, a = 1819.8(3), b = 715.75(8), c = 846.4(1) pm, β = 96.89(2)°, Rall = 0.0352). The crystal structure contains three crystallographically different La3+ ions. La1 is surrounded by six oxygen atoms from five SeO32– groups and four fluoride ions, La2 is coordinated by two bidentate SeO32– ions and seven fluoride ligands. La3 is surrounded by oxygen atoms only with the coordination number and polyhedron being almost the same as found for La3+ in La2(SeO3)3. Furthermore, the crystal structures of both compounds are strongly influenced by the lone pairs of the SeO32– groups.  相似文献   

16.
TlFeSe2 is monoclinic, space groupC2/mC 2h 3 ,a=11.973 Å,b=5.490 Å,c=7.110 Å, =118.2°,Z=4.TlFeS2 is isotypic witha=11.636 Å,b=5.304 Å,c=6.799 Å, =116.7°.The crystal structure of TlFeSe2 has been determined from single crystal diffractometer data. Isotypy of the sulfide has been confirmed from powder diffraction data. The crystal structure containing infinite linear chains of edgesharing FeX 4-tetrahedra, and its relationship to the thio- and selenoferrates of the alkali metals are discussed. The mineral raguinite is very probably isotypic to synthetic TlFeS2.
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17.
The crystal structure of Ca9(Ca x Mg1–x )(AsO4)6(AsO3OH) withx 0.5 (a=10.73,c=37.74 Å; space group R3c-C 3v 6 ;Z=6) was solved from 985 independent X-ray intensities collected on a 4-circle diffractometer, and refined toR=5.7% for all data. This compound is isotypic to Ca9Mg(PO4)6(PO3OH), a structure of the whitlockite-type.
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18.
The crystal structure of Cr2H2(As2O7)(As4O12) has been determined by X-ray methods using single crystal diffractometer data (1,152 reflections,R=0.054, orthorhombic,Pmmn,a=1317.7 (7),b=1124.9 (6),c=494.3 (4) pm,Z=2). The crystal structure contains both diarsenate(V) and the hitherto unknown cyclo-tetraarsenate(V)-anions. The magnetic susceptibility follows theCurie-Weiss law (=3.86±0.01 B/Cr3+, =–31 K).
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19.
Two oxoborates, (Pb3O)2(BO3)2MO4 (M=Cr, Mo), have been prepared by solid-state reactions below 700 °C. Single-crystal XRD analyses showed that the Cr compound crystallizes in the orthorhombic group Pnma with a=6.4160(13) Å, b=11.635(2) Å, c=18.164(4) Å, Z=4 and the Mo analog in the group Cmcm with a=18.446(4) Å, b=6.3557(13) Å, c=11.657(2) Å, Z=4. Both compounds are characterized by one-dimensional chains formed by corner-sharing OPb4 tetrahedra. BO3 and CrO4 (MoO4) groups are located around the chains to hold them together via Pb–O bonds. The IR spectra further confirmed the presence of BO3 groups in both structures and UV–vis diffuse reflectance spectra showed band gaps of about 1.8 and 2.9 eV for the Cr and Mo compounds, respectively. Band structure calculations indicated that (Pb3O)2(BO3)2MoO4 is a direct semiconductor with the calculated energy gap of about 2.4 eV.  相似文献   

20.
KAg(NO3)2 crystallizes in space group P21/a-C 2h 5 ,a=13.953,b=4.955,c=8.220 Å, =97.76°,Z=4. X-ray intensities were collected with a two-circle diffractometer. The structure was solved by means of direct methods andFourier syntheses and was refined by the least squares method toR=0.034 with 1346 observed reflexions. 1 {Ag2(NO3)4}2–-chains run parallel toy and are linked by potassium ions. Ag shows a distorted tetrahedral coordination with four relatively close O. K is irregularily surrounded by ten O. The isotypic compounds NH4Ag(NO3)2 and RbAg(NO3)2 were refined toR=0.032 and 0.035, respectively. The coordination figures are compareable with those in KAg(NO3)2.
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