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  • Synthesis  (12)
  • Wiley-Blackwell  (12)
  • Cell Press
  • De Gruyter
  • Oxford University Press
  • 1995-1999  (12)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1493-1495 
    ISSN: 0044-2313
    Keywords: Synthesis ; Crystal structure ; Crown ether ; Lanthanides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [La2I2(OH)2(dibenzo-18-crown-6)2]I(I3), a Cationic Dimeric in-cavity Complex with Iodide and Triiodide as AnionsSingle crystals of [La2I2(OH)2(dibenzo-18-crown-6)2]I(I3) are obtained from the reaction of LaI3 and dibenzo-18-crown-6 in acetonitrile. The crystal structure monoclinic, C2/m, Z = 4, T = 293 [100] K, a = 2179(3) [2162.3(3)], b = 1070.3(3) [1069.6(1)], c = 1118.2(3) [1110.6(1)] pm, β = 93.1(1) [92.83(1)]°, R1 = 0.0601 [0.0411], wR2 = 0.1449 [0.1014] contains hydroxide-bridged cationic dimers and iodide as well as triiodide as anions.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 791-795 
    ISSN: 0044-2313
    Keywords: Lithium Niobium Chloride ; Niobium Cluster ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zweidimensionale Netzwerke in der Struktur von Li2[Nb6Cl16]Li2[Nb6Cl16] wurde aus Nb-Pulver, NbCl5 und LiCl in Quarzglasampullen bei 700°C hergestellt. Die anhand von Einkristall-Röntgendaten verfeinerte Kristallstruktur ist orthorhombisch, Raumgruppe Cmca (Nr. 64), mit Z = 4 und Gitterkonstanten von a = 1274.7(1) pm, b = 1318.5(1) pm, c = 1341.1(2) pm. Die Verfeinerung aller Atompositionen ergab R1 = 0.031 (basierend auf F-Werten) und wR2 = 0.081 (basierend auf F2-Werten). Die Struktur enthält Schichten aus [Nb6Cl12i]2+ mit äußeren Cla-a-Liganden, die vier Ecken jedes oktaedrischen Niobclusters in Schichten verknüpfen, plus zwei terminale Cla-Liganden an jedem Niobcluster, entsprechend [Nb6Cl12iCl4/2a-aCl2a]2-. Das gleiche Verknüpfungsmuster liegt in binären Mo6X12-Halogeniden vor, die jedoch acht innere Halogenliganden besitzen (Mo6Cl8i). Gewinkelte Nb-Cla-a-Nb Brücken (159°) zwischen benachbarten Niobclustern korrespondieren mit Verdrehungen der [Nb6Cl16]2--Einheiten innerhalb der Schichten, wodurch zwei Li+ verzerrt trigonal-bipyramidale Lücken besetzen.
    Notes: Li2[Nb6Cl16] has been synthesized from the reaction of Nb powder, NbCl5 and LiCl in sealed silica tubes at 700°C. The structure, as determined by single-crystal X-ray diffraction, is orthorhombic, space group Cmca (no. 64) with Z = 4 and has lattice parameters a = 1274.7(1) pm, b = 1318.5(1) pm, c = 1341.1(2) pm. The refinement of all atomic positions yielded Rl = 0.031 (based on F values) and wR2 = 0.081 (based on F2 values). The structure contains layers formed by [Nb6Cl2i]2+ with outer Cla-a ligands that bridge four vertices of each octahedral niobium cluster into sheets, plus two terminal Cla ligands of each cluster, to be described as [Nb6Cl12iCl4/2a-aCl2a]2-. The same connectivity pattern is present for binary Mo6X12 halides, containing eight inner halide ligands (Mo6Cl8i). Non-linear Nb-Cla-a-Nb bridges (159°) correspond with intra-layer rotations of [Nb6Cl16]2 units and thereby accommodate two Li+ in distorted trigonal - bipyramidal voids.
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  • 3
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato-Phosphaneimine Complex of Titanium ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of [TiF3(NPPh3)(HNPPh3)]2 and of HNPPh3The phosphoraneiminato-phosphaneimine complex [TiF3(NPPh3)(HNPPh3)]2 was obtained by the reaction of TiF4 with Me3SiNPPh3 in boiling dichloromethane. It crystallizes from 1,2-dichloroethane as yellow crystals which include four molecules C2H4Cl2 per dimeric formula unit. Space group P21/n, Z = 2, structure solution with 7270 independent reflections, R = 0.060 for reflections with I 〉 2σ(I). Lattice dimensions at -50°C: a = 1417.5, b = 1896.9, c = 1586.6 pm, β = 101.22°. The compound forms centrosymmetric dimeric molecules via μ2-F bridges with TiF distances of 194.6 and 223.3 pm, the longer one being in trans-position to the N atom of the (NPPh3)- ligand. Its TiN bond length of 177.7 pm corresponds with a double bond. The TiN bond length of the HNPPh3 donor molecule of 213.4 pm is typical for a donor acceptor bond.According to the crystal structure determination the phosphaneimine HNPPh3 forms monomeric molecules without intermolecular hydrogen bridges with a PN bond length of 152.4 pm. Space group P21/c, Z = 4, structure solution with 3229 independent reflections, R = 0.062 for reflections with I 〉 2σ(I). Lattice dimensions at -70°C: a = 1460.4, b = 928.9, c = 1096.6 pm, β = 93.35°.
    Notes: Der Phosphaniminato-Phosphanimin-Komplex [TiF3(NPPh3)(HNPPh3)]2 wird aus TiF4 und Me3SiNPPh3 in siedendem Dichlormethan erhalten. Er kristallisiert aus 1,2-Dichlorethan als gelbe Kristalle unter Einschluß von vier Molekülen C2H4Cl2 pro dimere Formeleinheit. Raumgruppe P21/n, Z = 2, Strukturlösung mit 7270 unabhängigen Reflexen, R = 0,060 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -50°C: a = 1417,5; b = 1896,9; c = 1586,6 pm; β = 101,22°. Die Verbindung bildet zentrosymmetrische Dimere, in denen die Titanatome über μ2-F-Brücken mit TiF-Abständen von 194,6 und 223,3 pm verknüpft sind. Die lange Ti—F-Bindung befindet sich in trans-Position zum N-Atom des (NPPh3)--Liganden, dessen TiN-Bindung mit 177,7 pm einer Doppelbindung entspricht. Der vom HNPPh3-Liganden ausgehende Ti—N-Abstand beträgt 213,4 pm.Das Phosphanimin HNPPh3 bildet nach der Kristallstrukturanalyse monomere Moleküle mit einer PN-Bindungslänge von 152,4 pm ohne intermolekulare Wasserstoffbrücken. Raumgruppe P21/c, Z = 4, Strukturlösung mit 3229 unabhängigen Reflexen, R = 0,062 für Reflexe mit I 〉 2σ(I). Gitterkonstanten bei -70°C: a = 1460,4; b = 928,9; c = 1096,6 pm; β = 93,35°.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1466-1470 
    ISSN: 0044-2313
    Keywords: Synthesis ; Crystal structure ; Halides ; Clusters ; Lanthanides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Bromide with Trigonal-Bipyramidal [M5(C2)] Clusters: [Pr5(C2)]Br9The bromide [Pr5(C2)]Br9 is obtained via metallothermic reduction of PrBr3 with rubidium in the presence of praseodymium and carbon in a sealed niobium container at 730°C as dark red single crystals. [Pr5(C2)]Br9 crystallizes in the monoclinic crystal system [P21/n; Z = 4; a = 1 006.9(1); b = 1 886.1(1); c = 1 045.9(1) pm; β = 108.130(1)°; Rint = 0.059; R1 = 0.038; wR2 = 0.077]. One edge in the base of the trigonal bipyramid in [Pr5(C2)]Br9 is usually long (440 pm). It is not brigded by a Bri ligand. In addition to the eight Bri, the cluster is coordinated by 12 terminal ligands (Bra). Except for the known Bra-a-a and Bri-a connections, Bri-a-a brigdes are observed for the first time for trigonal-bipyramidal clusters.
    Notes: Das Bromid [Pr5(C2)]Br9 erhält man durch metallothermische Reduktion von PrBr3 mit Rubidium in Gegenwart von Praseodym und Kohlenstoff in einer verschweißten Niobampulle bei 730°C in Form dunkelroter Kristalle. [Pr5(C2)]Br9 kristallisiert im monoklinen Kristallsystem [P21/n; Z = 4; a = 1 006,9(1); b = 1 886,1(1); c = 1 045,9(1) pm; β = 108,130(1)°; Rint = 0,059; R1 = 0,038; wR2 = 0,077]. Eine Kante in der Basis der trigonalen Bipyramide in [Pr5(C2)]Br9 ist mit 440 pm ungewöhnlich lang und wird nicht von einem Bri-Liganden überbrückt. Zusätzlich zu den acht Bri werden die Cluster von 12 terminalen Liganden koordiniert (Bra). Neben den bekannten Bra-a-a- und Bri-a-Brücken treten hier erstmals bei trigonal-bipyramidalen Clustern Bri-a-a-Brücken auf.
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  • 5
    ISSN: 0044-2313
    Keywords: Synthesis ; Crystal Structure ; Rare Earths ; Ternary Lithium Nitrate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Lithium Rare Earth Nitrates with Lonesome Nitrate Ions: Li3[M(NO3)5](NO3) (M = Gd—Lu, Y). The Crystal Structure of Li3Er(NO3)6Single crystals of the ternary nitrate Li3Er(NO3)6 are obtained from a solution of “Er(NO3)3” in the melt of LiNO3. In Li3Er(NO3)6 (monoclinic, P21/n, Z = 4; a = 776.0(1); b = 748.86(8); c = 2 396(1) pm; β = 90.76(3)°; R1 = 0.0490; wR2 = 0.0792), Er3+ is surrounded by five bidentate nitrate ligands yielding the anionic units [Er(NO3)5]2-. These are arranged in the direction of the 21 screw axis. Two lonesome NO3- ions are in the middle of such a “helix” and are connected by Li+ with the anions [Er(NO3)5]2-. The helices are moved against each other by about half of the lattice constant a and are connected by further Li+ ions.
    Notes: Einkristalle des ternären Nitrates Li3Er(NO3)6 erhält man durch Lösen von „Er(NO3)3“ in einer Schmelze von LiNO3. In Li3Er(NO3)6 (monoklin, P21/n, Z = 4; a = 776,0(1); b = 748,86(8); c = 2 396(1) pm; β = 90,76(3)°; R1 = 0,0490; wR2 = 0,0792) ist Er3+ von fünf Nitratliganden jeweils zweizähnig in Form der anionischen Einheit [Er(NO3)5]2- umgeben. Diese Einheiten sind längs der 21-Schraubenachse angeordnet. In der Mitte dieser „Spirale“ befinden sich zwei einsame NO3--Ionen, die über Li+-Ionen mit den Anionen [Er(NO3)5]2- verbunden sind. Die „Spiralen“ sind um die halbe Gitterkonstante a gegeneinander verschoben und über weitere Li+-Ionen verknüpft.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1646-1650 
    ISSN: 0044-2313
    Keywords: Synthesis ; crystal structures ; complex fluorides ; silicon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of NH4[Si(NH3)F5] and [Si(NH3)2F4]Single crystals of NH4[Si(NH3)F5] and [Si(NH3)2F4] are obtained by reaction of silicon powder with NH4HF2 in sealed Monel ampoules at 400°C. NH4[Si(NH3)F5] crystallizes with the tetragonal space group P4/n (no. 85) with a = 614.91(7) pm, c = 721.01(8) pm, Z = 2. Characteristic for the structure is the anionic octahedron [Si(NH3)F5]-. Si(NH3)2F4 crystallizes with the monoclinic space group P21/c (no. 14) with a = 506.9(1) pm, b = 728.0(1) pm, c = 675.9(1), β = 93,21(2)°, Z = 2. Trans-[Si(NH3)2F4] molecules are characteristic for this structure.
    Notes: Einkristalle von NH4[Si(NH3)F5] und Si(NH3)2F4 erhält man durch Umsetzung von pulverförmigem Silicium mit NH4HF2 in verschlossenen Monelampullen bei 400°C. NH4[Si(NH3)F5] kristallisiert tetragonal in der Raumgruppe P4/n (Nr. 85) mit a = 614,91(7) pm, c = 721,01(8) pm; Z = 2. Charakteristische Baueinheit ist der anionische Oktaeder [Si(NH3)F5]-. Si(NH3)2F4 kristallisiert monoklin in der Raumgruppe P21/c (Nr. 14) mit a = 506,9(1) pm, b = 728,0(1) pm, c = 675,9(1), β = 93,21(2)°, Z = 2. Es liegt eine Molekülstruktur mit trans-[Si(NH3)2F4]-Oktaedern vor.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1723-1728 
    ISSN: 0044-2313
    Keywords: Lithium Niobium Chloride ; Niobium Cluster ; Synthesis ; Crystal Structure ; Lithium mobility ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Struktur und Eigenschaften von LiNb6Cl15Schwarze Einkristalle von LiNb6Cl15 wurden aus Reaktionen von Nb-Pulver, NbCl5 und LiCl in verschweißten Niobrohren bei 850°C hergestellt. Die Schweratomstruktur von LiNb6Cl15 (Ia3d (Nr. 230), Z = 16, a = 2055.5(2) pm at 100 K, R(F) = 0.028, R(F2) = 0.053) ist mit der Struktur von Ta6Cl15 isotyp. Die [Nb6Cl12]2+-Cluster sind in der Struktur dreidimensional über drei zusätzliche Cla-a verbrückt. Diese verbrücken alle Ecken der Niobcluster, entsprechend der Schreibweise [Nb6Cl12iCl6/2a-a]- (die Nb—Cla-a—Nb-Bindungswinkel betragen 140°). Bei tiefen Temperaturen sind die Lithiumionen über ein Drittel von Lagen (48 f) fehlgeordnet und besetzen Hohlräume in verzerrten Chlorid-Tetraedern, die eine gemeinsame Kante teilen. Diese Positionen der Lithiumionen repräsentieren die engsten Stellen der unendlichen Kanäle in der Struktur, die von Chlorid gebildet werden. 7Li-NMR-Messungen zeigen oberhalb von 170 K eine deutliche Zunahme der Lithiumionenbeweglichkeit.
    Notes: Black single crystals of LiNb6Cl15 were obtained from reactions of Nb powder, NbCl5 and LiCl in sealed niobium tubes at 850°C. The heavy atom structure of LiNb6Cl15 (Ia3d (no. 230), Z = 16, a = 2055.5(2) pm at 100 K, R(F) = 0.028, R(F2) = 0.053) is isotypic with the structure of Ta6Cl15. The [Nb6Cl12]2+ clusters in the structure are three-dimensionally interconnected via three additional Cla-a. These bridge all vertices of niobium clusters, consistent with [Nb6Cl12iCl6/2a-a]- (the Nb—Cla-a—Nb angles are 140°). At low temperatures the lithium ions are disordered over one-third of sites (48 f), occupying cavities inside of two distorted corner-sharing tetrahedra of chloride. These positions for lithium represent the narrowest sections of infinite channels in the structure built up by chloride. An increased lithium ion mobility is obtained above 170 K by 7Li-NMR measurements.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1299-1303 
    ISSN: 0044-2313
    Keywords: Synthesis ; Crystal Structure ; Halides ; Clusters ; Lanthanides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Chlorides with Trigonal-Bipyramidal Clusters: [M5(C2)]Cl9 (M = La—Pr)The chlorides [M5(C2)]Cl9 (M = La—Pr) are obtained by metallothermic reduction of the respective trichlorides MCl3 with caesium in the presence of the lanthanide metal and carbon in sealed niobium ampoules at 800°C. They contain trigonal-bipyramidal clusters [M5(C2)] crystallizing with the triclinic crystal system. Only seven of the nine edges of the trigonal bipyramids are brigded by chloride (Cli). Each cluster is surrounded by twelve terminal ligands (Cla) so that units of the composition [M5(C2)Cl7i]Cl12a have to be considered. These are connected not only via Cli-a and Cla-a-a bridges. Rather, Cla-a (one linear and one bent) and Cli-i bridges are also observed.
    Notes: Die Chloride [M5(C2)]Cl9 (M = La—Pr) erhält man durch metallothermische Reduktion der entsprechenden Trichloride MCl3 mit Caesium in Gegenwart des jeweiligen Metalls M und Kohlenstoff in verschweißten Niobampullen bei 800°C. Sie enthalten trigonal-bipyramidale [M5(C2)]-Cluster und kristallisieren im triklinen Kristallsystem. Von den neun Kanten der trigonalen Bipyramiden werden nur sieben von Cli-Liganden überbrückt. Zusätzlich werden die [M5(C2)]-Cluster von zwölf terminalen Liganden koordiniert, so daß man zu Einheiten [M5(C2)Cl7i]Cl12a gelangt. Die trigonal-bipyramidalen Cluster werden über Cli-a- und Cla-a-a-Brücken, auch über Cla-a-Brücken (eine gewinkelte und eine lineare) sowie Cli-i-Brücken miteinander vernetzt.
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  • 9
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes ; Copper(II) ; Synthesis ; Magnetic Behaviour ; EPR Spectrum ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Cu4(NPMe3)3(O2C—CH3)5] - a Tetrameric Phosphorane Iminato Complex of Copper(II). Synthesis, Crystal Structure, Magnetic Behaviour, and EPR SpectrumThe title compound and the corresponding benzoate complex [Cu4(NPMe3)3(O2C—C6H5)5] have been prepared by reactions of copper(II)acetate and copper(II)benzoate, respectively, with Me3SiNPMe3 in dichloromethane. Both complexes are characterized by IR spectroscopy. The acetate complex is additionally characterized by the measurement of the magnetic susceptibility, by its EPR spectrum, and by a crystal structure determination.[Cu4(NPMe3)3(O2C—CH3)5] · CH2Cl2: Space group I41/a, Z = 16, structure solution with 7 960 independent reflections, R = 0.044. Lattice dimensions at -70°C: a = b = 3 670.6; c = 1 091.9 pm. The structure consists of four Cu atoms which are arranged at the corners of a distorted tetrahedron with Cu…Cu distances between 290 and 318 pm. Three of the faces of the tetrahedron are linked by μ3-N atoms of the phosphorane iminato groups. Three of the acetate ligands form chelates, the other two are monofunctionally coordinated. Three of the copper atoms have a planar surrounding, the forth Cu atom has a (4 + 1) coordination.
    Notes: Die Titelverbindung sowie der entsprechende Benzoat-Komplex [Cu4(NPMe3)3(O2C—C6H5)5] wurden durch Reaktion von Kupfer(II)acetat bzw. von Kupfer(II)benzoat mit Me3SiNPMe3 in Dichlormethan hergestellt und durch ihre IR-Spektren charakterisiert. Der Acetatkomplex wurde zusätzlich durch die Messung der magnetischen Suszeptibilität, des EPR-Spektrums und durch eine Kristallstrukturanalyse charakterisiert.[Cu4(NPMe3)3(O2C—CH3)5] · CH2Cl2: Raumgruppe I41/a, Z = 16, Strukturlösung mit 7 960 unabhängigen Reflexen, R = 0,044. Gitterkonstanten bei -70°C: a = b = 3 670,6; c = 1 091,9 pm. Die Struktur besteht aus vier Cu-Atomen, die ein verzerrtes Tetraeder bilden mit Cu…Cu-Abständen zwischen 290 und 318 pm. Drei der Tetraederflächen sind durch μ3-N-Atome dreier NPMe3--Gruppen überbrückt, drei der Acetatliganden sind chelatartig gebunden, während zwei Acetatgruppen monofunktionell koordinieren. Drei der Cu-Atome haben planare Umgebung, das vierte hat eine (4 + 1)-Koordination.
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  • 10
    ISSN: 0044-2313
    Keywords: Rare Earths ; Bromides ; Copper ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of (NH4)3Cu4Ho2Br13. Further Bromides of the (NH4)3Cu4M2Br13 Type (M = Dy—Lu, Y) and on Rb3Cu4Ho2Br13Single crystals of (NH4)3Cu4Ho2Br13 were obtained for the first time from the reaction of CuBr with HoBr3 which was contaminated with NH4Br: cubic, space group Pn3, Z = 2, a = 1101.71(5) pm. The crystal structure may be considered as a variant of the fluorite type according to [(HoBr6)4][(NH4)6(Cu4Br)2] ≡ Ca4F8. Pure products can be prepared from the binary halides in glass ampoules at 350°C. The bromides (NH4)3Cu4M2Br13 (M = Dy—Lu, Y) and Rb3Cu4Ho2Br13 are isotypic with (NH4)3Cu4Ho2Br13.
    Notes: Einkristalle von (NH4)3Cu4Ho2Br13 wurden erstmals bei der Reaktion von CuBr mit HoBr3, das mit NH4Br „verunreinigt“ war, erhalten: kubisch, Raumgruppe Pn3, Z = 2, a = 1101,71(5) pm. Die Kristallstruktur ist gemäß [(HoBr6)4][(NH4)6(Cu4Br)2] ≡ Ca4F8 als eine Variante des Flußspat-Typs aufzufassen. Reine Produkte können aus den binären Halogeniden bei 350°C in Glasampullen dargestellt werden. Die Bromide (NH4)3Cu4M2Br13 (M = Dy—Lu, Y) und Rb3Cu4Ho2Br13 sind mit (NH4)3Cu4Ho2Br13 isotyp.
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