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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 47-53 
    ISSN: 0044-2313
    Keywords: Mercury-N,N′-bis(trimethylsilyl)benzamidinate ; synthesis ; i.r. spectrum ; 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 Mercury(II)-N,N′-bis(trimethylsilyl)benzamidinate, Hg[Ph—C(NSiMe3)2]2The title compound has been synthesized by the reaction of N,N,N′-tris(trimethylsilyl)benzamidine with mercury(I)-acetate in boiling acetonitrile because of redox disproportionation, forming white crystal needles, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P1; Z = 2; 6846 observed unique reflections; R = 0.048. Lattice dimensions at -90 ° C: a = 1091.9, b = 1212.8, c = 1433.5 pm; α = 106.89°, β = 109.25°, γ = 90.62°. The compound forms a nearly centro-symmetric molecule structure with sp-hybridized Hg atom (r Hg—N = 207 pm).
    Notes: Die Titelverbindung entsteht bei der Reaktion von N,N,N′-tris(trimethylsilyl)-benzamidin mit Quecksilber(I)-acetat in siedendem Acetonitril durch Redox-Disproportionierung in Form weißer Kristallnadeln, die durch das IR-Spektrum und durch eine röntgenographische Kristallstrukturanalyse charakterisiert werden. Raumgruppe P1, Z = 2, 6 846 beobachtete unabhängige Reflexe; R = 4, 8%. Gitterabmessungen bei -90 °C: a = 1091,9; b = 1212,8; c = 1433,5 pm; α = 106,89α β = 109,25°; γ = 90,62°. Die Verbindung bildet eine nahezu zentrosymmetrische Molekülstruktur mit sp-hybridisiertem Hg-Atom (r Hg—N = 207 pm).
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 133-138 
    ISSN: 0044-2313
    Keywords: Benzamidinium hexachlorostannate ; synthesis ; crystal structure ; i.r. spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Benzamidinium Hexachlorostannate: Synthesis and Crystal Structure[Ph—C(NH2)2SnCl6] has been prepared by the reaction of hydrogen chloride with the amidinato complex [Ph—C(NSiMe3)2SnCl3] in CH2Cl2 solution, forming colourless crystals. which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P21/c, Z = 4, 3070 observed unique reflexions, R = 0.029. Lattice dimensions at -50°C: a = 892.5, b = 1076.7, c = 1175.6 pm, β = 109.3°. The compound consists of benzamidinium ions C6H5—C(NH2)2+ and anions SnCl62-, which are connected by a network of N—H…Cl hydrogen bridges.
    Notes: [Ph—C(NH2)2]2SnCl6 entsteht in Form farbloser Einkristalle durch Einwirkung von Chlorwasserstoff auf eine Lösung des Amidinatokomplexes [Ph—C(NSiMe3)2SnCl3] in Dichlormethan. Die Verbindung wird durch das IR-Spektrum und durch eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 3070 beobachtete unabhängige Reflexe, R = 2,9%. Gitterabmessungen bei -50°C: a = 892,5; b = 1076,7; c = 1175,6 pm; β = 109,3°. Die Verbindung besteht aus Benzamidinium-Kationen C6H5—C(NH2)2+ und SnCl62--Ionen, in denen ein Netz von N—H…Cl-Wasserstoffbrücken besteht.
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  • 3
    ISSN: 0044-2313
    Keywords: Multinuclear phosphido-bridged Ag-, Zn- and Cd-Complexes ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Phosphido-bridged Multinuclear Complexes of Ag, Cd and Zn. The Crystal Structures of [Ag4(PPh2)4(PMe3)4], [Ag6(PPh2)6(PtBu3)2] and [M4Cl4(PPh2)4(PnPr3)2] (M = Zn, Cd)AgCl reacts with Ph2PSiMe3 in the presence of a tertiary Phosphine PMe3 or PtBu3 to form the multinuclear complexes [Ag4(PPh2)4(PMe3)4] (1) and [Ag6(PPh2)6(PtBu3)2] (2). In analogy to that MCl2 reacts with Ph2PSiMe3 in the presence of PnPr3 to form the two multinuclear complexes [M4Cl4(PPh2)4(PnPr3)2] (M = Zn (3), Cd (4)). The structures were characterized by X-ray single crystal structure analysis (1: space group Pna21 (Nr. 33), Z = 4, a = 1 313.8(11) pm, b = 1 511.1(6) pm, c = 4 126.0(18) pm, 2: space group P-1 (Nr. 2), Z = 2, a = 1 559.0(4) pm, b = 1 885.9(7) pm, c = 2 112.4(8) pm, α = 104.93(3)°, β = 94.48(3)°, γ = 104.41(3)°; 3: space group C2/c (Nr. 15), Z = 4, a = 2 228.6(6) pm, b = 1 847.6(6) pm, c = 1 827.3(6) pm, β = 110.86(2); 4: space group C2/c (Nr. 15), Z = 4, a = 1 894.2(9) pm, b = 1 867.9(7) pm, c = 2 264.8(6) pm, β = 111.77(3)°). 3 and 4 may be considered as intermediates on the route towards polymeric [M(PPh2)2]n (M = Zn, Cd).
    Notes: AgCl reagiert mit Ph2PSiMe3 in Gegenwart der tertiären Phosphane PMe3 und PtBu3 unter Bildung der mehrkernigen Komplexe [Ag4(PPh2)4(PMe3)4] (1) und [Ag6(PPh2)6(PtBu3)2] (2). Analog dazu reagiert MCl2 mit Ph2PSiMe3 und PnPr3 zu den mehrkernigen Komplexen [M4Cl4(PPh2)4(PnPr3)2] (M = Zn 3), Cd (4)). Die Struktur der Komplexe konnte durch Kristallstrukturanalysen aufgeklärt werden (1: Raumgruppe Pna21 (Nr. 33), Z = 4, a = 1 313,8(11) pm, b = 1 511,1(6) pm, c = 4 126,0(18) pm, 2: Raumgruppe P1 (Nr. 2), Z = 2, a = 1 559,0(4) pm, b = 1 885,9(7) pm, c = 2 112,4(8) pm, α = 104,93(3)°, β = 94,48(3)°, γ = 104,41(3)°; 3: Raumgruppe C2/c (Nr. 15), Z = 4, a = 2 228,6(6) pm, b = 1 847,6(6) pm, c = 1 827,3(6) pm, β = 110,86(2); 4: Raumgruppe C2/c (Nr. 15), Z = 4, a = 1 894,2(9) pm, b = 1 867,9(7) pm, c = 2 264,8(6) pm, β = 111,77(3) 3 und 4 können als Vorstufen auf dem Weg zur Bildung von polymerem [M(PPh2)2]n (M = Zn, Cd) angesehen werden.
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  • 4
    ISSN: 0044-2313
    Keywords: Polytellurido complexes of copper and silver ; synthesis ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Polytellurido Complexes (PPh4)4[M2Te12] of Copper(I) and Silver(I)The title compounds have been prepared as black crystal needles by reactions of Na2Te3 with CuCl and AgNO3, respectively, in dimethylformamide in the presence of PPh4Br. With regard to the large cell dimensions the crystal structure determinations were done by an imaging plate instrument.(PPh4)4[Cu2Te12]: Space group P21/n, Z = 6, 51 338 detected reflections, structure determination with 14 177 unique reflections with I 〉 4σ(I), R = 0.081. Lattice dimensions at - 50°C: a = 1 704.5, b = 1 694.5, c = 5 044 pm, β = 94.20°.(PPh4)4[Ag2Te12]: Space group P21/n, Z = 6, 80 811 detected reflections, structure determination with 16 092 unique reflections with I 〉 3σ(I), R = 0.052. Lattice dimensions at - 50°C: a = 1 703.8, b = 1 722.9, c = 5 123 pm, β = 94.65°.The structures of the isotypic compounds consist of six symmetry independent PPh4+ ions and two symmetry independent anions [M2Te12]4-, in which the metal atoms of two (MTe4)--fivering fragments are linked by a Te42- chain.
    Notes: Die Titelverbindungen entstehen als schwarze Kristallnadeln aus Na2Te3 und CuCl bzw. AgNO3 in Dimethylformamid in Gegenwart von PPh4Br. Wegen der großen Zellabmessungen wurden die Kristallstrukturen mit Hilfe des Flächendetektors der Firma Stoe vermessen.(PPh4)4[Cu2Te12]: Raumgruppe P21/n, Z = 6, 51 338 gemessene Reflexe, Strukturlösung mit 14 177 unabhängigen Reflexen mit I 〉 4σ(I), R = 0,081. Gitterabmessungen bei - 50°C: a = 1 704,5; b = 1 694,5; c = 5 044 pm; β = 94,20°.(PPh4)4[Ag2Te12]: Raumgruppe P21/n, Z = 6, 80 811 gemessene Reflexe, Strukturlösung mit 16 092 unabhängigen Reflexen, mit I 〉 3σ(I), R = 0,052. Gitterabmessungen bei - 50°C: a = 1 703,8; b = 1 722,9; c = 5 123 pm; β = 94,65°.Die beiden miteinander isotypen Strukturen enthalten sechs symmetrieunabhängige PPh4+-Ionen und zwei symmetrieunabhängige Anionen [M2Te12]4-. In diesen sind die Metallatome zweier (MTe4)--Fünfringfragmente über eine Te42--Kette miteinander verknüpft.
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  • 5
    ISSN: 0044-2313
    Keywords: Cyclotriphosphanes ; multinuclear phosphorus-bridged complexes of Re, Mn, Co, Ir and Ni ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Phosphorus-bridged Transition Metal Carbonyl Complexes. The Crystal Structures of [Re2(CO)7(PtBu)3], [Co4(CO)10(PtBu)2], [Ir4(CO)6(PtBu)6], and [Ni4(CO)10(PiPr)6],(PtBu)3 reacts with [Mn2(CO)10], [Re2(CO)10], [Co2(CO)8] and [Ir4(CO)12] to form the multinuclear complexes [M2(CO)7(PtBu)3] (M = Re (1), Mn (5)), [Co4(CO)10(PtBu)2] (2) and [Ir4(CO)6(PtBu)6] (3). The reaction of (PiPr)3 with [Ni(CO)4] leads to the tetranuclear cluster [Ni4(CO)10(PiPr)6] (4). The complex structures were obtained by X-ray single crystal structure analysis: (1: space group P1 (Nr. 2), Z = 2, a = 917.8(3) pm, b = 926.4(3) pm, c = 1 705.6(7) pm, α = 79.75(3)°, β = 85.21(3)°, γ = 66.33(2)°; 2: space group C2/c (Nr. 15), Z = 4, a = 1 347.7(6) pm, b = 1 032.0(3) pm, c = 1 935.6(8) pm, β = 105.67(2)°; 3: space group P1 (Nr. 2), Z = 4, a = 1 096.7(4)pm, b = 1 889.8(10)pm, c = 2 485.1(12) pm, α = 75.79(3)°, β = 84.29(3)°, γ = 74.96(3)°; 4: space group P21/c (Nr. 14), Z = 4, a = 2 002.8(5) pm, b = 1 137.2(8) pm, c = 1 872.5(5) pm, β = 95.52(2)°).
    Notes: Das Cyclotriphosphan (PtBu)3 reagiert mit [Mn2(CO)10], [Re2(CO)10], [Co2(CO)8] und [Ir4(CO)12] unter Bildung der Mehrkernkomplexe [M2(CO)7(PtBu)3] (M = Re (1), Mn (5)), [Co4(CO)10(PtBu)2] (2) und [Ir4(CO)6(PtBu)6] (3). Die Umsetzung von (PiPr)3 mit [Ni(CO)4] führt zu dem vierkernigen Cluster [Ni4(CO)10(PiPr)6] (4). Die Strukturen der Komplexe konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden (1: Raumgruppe P1 (Nr.2), Z = 2, a = 917,8(3)pm, b = 926,4(3)pm, c = 1 705,6(7)pm, α = 79,75(3)°, β = 85,21(3)°, γ = 66,33(2)°; 2: Raumgruppe C2/c (Nr. 15), Z = 4, a = 1 347,7(6) pm, b = 1 032,0(3) pm, c = 1 935,6(8) pm, β = 105,67(2)°; 3: Raumgruppe P1 (Nr. 2), Z = 4, a = 1 096,7(4) pm, b = 1 889,8(10) pm, c = 2 485,1(12) pm, α = 75,79(3)°, β = 84,29(3)°, γ = 74,96(3)°; 4: Raumgruppe P21/c (Nr. 14), Z = 4, a = 2 002,8(5) pm, b = 1 137,2(8) pm, c = 1 872,5(5) pm, β = 95,52(2)°).
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  • 6
    ISSN: 0044-2313
    Keywords: Cyclotriphosphanes ; transition metal carbonyl complexes of Fe, Co, Ir, and Ni ; phosphorus-bridged ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of the Phosphorus-bridged Transition Metal Complexes [Fe2(CO)6(PR)6] (R = tBu, iPr), [Fe2(CO)4(PiPr)6], [Fe2(CO)3Cl2(PtBu)5], [Co4(CO)10(PiPr)3], [Ni5(CO)10(PiPr)6], and [Ir4(C8H12)4Cl2(PPh)4](PtBu)3 and (PiPr)3 react with [Fe2(CO)9] to form the dinuclear complexes [Fe2(CO)6(PR)6] (R = tBu: 1; iPr: 2). 2 is also formed besides [Fe2(CO)4(PiPr)6] (3) in the reaction of [Fe(CO)5] with (PiPr)3. When PiPr(PtBu)2 and PiPrCl2 are allowed to react with [Fe2(CO)9] it is possible to isolate [Fe2(CO)3Cl2(PtBu)5] (4). The reactions of (PiPr)3 with [Co2(CO)8] and [Ni(CO)4] lead to the tetra- and pentanuclear clusters [Co4(CO)10(PiPr)3] (5), [Ni4(CO)10(PiPr)6] [2] and [Ni5(CO)10(PiPr)6] (6). Finally the reaction of [Ir(C8H12)Cl]2 with K2(PPh)4 leads to the complex [Ir4(C8H12)4Cl2(PPh)4] (7). The structures of 1-7 were obtained by X-ray single crystal structure analysis (1: space group P21/c (Nr. 14), Z = 8, a = 1 758.8(16) pm, b = 3 625.6(18) pm, c = 1 202.7(7) pm, β = 90.07(3)°; 2: space group P1 (Nr. 2), Z = 1, a = 880.0(2) pm, b = 932.3(3) pm, c = 1 073.7(2) pm, α = 79.07(2)°, β = 86.93(2)°, γ = 72.23(2)°; 3: space group Pbca (Nr. 61), Z = 8, a = 952.6(8) pm, b = 1 787.6(12) pm, c = 3 697.2(30) pm; 4: space group P21/n (Nr. 14), Z = 4, a = 968.0(4) pm, b = 3 362.5(15) pm, c = 1 051.6(3) pm, β = 109.71(2)°; 5: space group P21/n (Nr. 14), Z = 4, a = 1 040.7(5) pm, b = 1 686.0(5) pm, c = 1 567.7(9) pm, β = 93.88(4)°; 6: space group Pbca (Nr. 61), Z = 8, a = 1 904.1(8) pm, b = 1 959.9(8) pm, c = 2 309.7(9) pm. 7: space group P1 (Nr. 2), Z = 2, a = 1 374.4(7) pm, b = 1 476.0(8) pm, c = 1 653.2(9) pm, α = 83.87(4)°, β = 88.76(4)°, γ = 88.28(4)°).
    Notes: Die Cyclotriphosphane (PtBu)3 und (PiPr)3 reagieren mit [Fe2(CO)9] unter Bildung der Zweikernkomplexe [Fe2(CO)6(PR)6] (R = tBu: 1; iPr: 2). 2 entsteht auch bei der Reaktion von [Fe(CO)5] mit (PiPr)3 neben dem Komplex [Fe2(CO)4(PiPr)6] (3). Aus der Reaktion von PiPr(PtBu)2 und PiPrCl2 mit [Fe2(CO)9] kann weiterhin [Fe2(CO)3Cl2(PtBu)5] (4) isoliert werden. Die Umsetzungen von (PiPr)3 mit [Co2(CO)8] und [Ni(CO)4] führen zu den vier- und fünfkernigen Clustern [Co4(CO)10(PiPr)3] (5), [Ni4(CO)10(PiPr)6] [2] und [Ni5(CO)10(PiPr)6] (6). Weiterhin kann aus der Reaktion von [Ir(C8H12)Cl]2 mit K2(PPh)4 der Komplex [Ir4(C8H12)4Cl2(PPh)4] (7) erhalten werden. Die Strukturen von 1-7 konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden (1: Raumgruppe P21/c (Nr. 14), Z = 8, a = 1 758,8(16) pm, b = 3 625,6(18) pm, c = 1 202,7(7) pm, β = 90,07(3)°; 2: Raumgruppe P1 (Nr. 2), Z = 1, a = 880,0(2) pm, b = 932,3(3) pm, c = 1 073,7(2) pm, α = 79,07(2)°, β = 86,93(2)°, γ = 72,23(2)°; 3: Raumgruppe Pbca (Nr. 61), Z = 8, a = 952,6(8) pm, b = 1 787,6(12) pm, c = 3 697,2(30) pm; 4: Raumgruppe P21/n (Nr. 14), Z = 4, a = 968,0(4) pm, b = 3 362,5(15) pm, c = 1 051,6(3) pm, β = 109,71(2)°; 5: Raumgruppe P21/n (Nr. 14), Z = 4, a = 1 040,7(5) pm, b = 1 686,0(5) pm, c = 1 567,7(9) pm, β = 93,88(4)°; 6: Raumgruppe Pbca (Nr. 61), Z = 8, a = 1 904,1(8) pm, b = 1 959,9(8) pm, c = 2 309,7(9) pm. 7: Raumgruppe P1 (Nr. 2), Z = 2, a = 1 374,4(7) pm, b = 1 476,0(8) pm, c = 1 653,2(9) pm, α = 83,87(4)°, β = 88,76(4)°, γ = 88,28(4)°).
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  • 7
    ISSN: 0044-2313
    Keywords: Mulinuclear phosphido-bridged Ag- and Zn-complexes ; Ag—P-rings ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Phosphido-bridged Multinuclear Complexes of Ag and Zn. The Crystal Structures of [Ag3(PPh2)3(PnBu2tBu)3], [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2, PnPr3), [Ag4(PPh2)4(PEt3)4]n, [Zn4(PPh2)4Cl4(PRR′2)2] (PRR′2 = PMenPr2, PnBu3, PEt2Ph), [Zn4(PhPSiMe3)4Cl4(C4H8O)2] and [Zn4(PtBu2)4Cl4]AgCl reacts with Ph2PSiMe3 in the presence of tertiary Phosphines (PnBu2tBu, PMenPr2, PnPr3 and PEt3) to form the multinuclear complexes [Ag3(PPh2)3(PnBu2tBu)3] 1, [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2 2, PnPr3 3) and [Ag4(PPh2)4(PEt3)4]n 4. In analogy to that ZnCl2 reacts with Ph2PSiMe3 and PRR′2 to form the multinuclear complexes [Zn4(PPh2)4Cl4(PRR′2)2] (PRR′2 = PMenPr2 5, PnBu3 6, PEt2Ph 7). Further it was possible to obtain the compounds [Zn4(PhPSiMe3)4Cl4(C4H8O)2] 8 and [Zn4(PtBu2)4Cl4] 9 by reaction of ZnCl2 with PhP(SiMe3)2 and tBu2PSiMe3, respectively. The structures were characterized by X-ray single crystal structure analysis. Crystallographic data see “Inhaltsübersicht”.
    Notes: AgCl reagiert mit Ph2PSiMe3 in Gegenwart der tertiären Phosphane PnBu2tBu, PMenPr2, PnPr3 und PEt3 unter Bildung mehrkerniger Komplexe. Abhängig vom tertiären Phosphan erhält man dabei folgende Verbindungen: [Ag3(PPh2)3(PnBu2tBu)3] 1, [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2 2, PnPr3 3) und [Ag4(PPh2)4(PEt3)4]n 4. Analog hierzu reagiert ZnCl2 mit Ph2PSiMe3 und PRR′2 zu den Mehrkernkomplexen [Zn4(PPh2)4Cl4(PRR′2)2] (PRR′2 = PMenPr2 5, PnBu3 6, PEt2Ph 7). Ferner konnten durch Umsetzung von ZnCl2 mit PhP(SiMe3)2 bzw. tBu2PSiMe3 die Verbindungen [Zn4(PhPSiMe3)4Cl4(C4H8O)2] 8 und [Zn4(PtBu2)4Cl4] 9 erhalten werden. Die Strukturen von 1-9 konnten durch Kristallstrukturanalysen aufgeklärt werden.(1: Raumgruppe P1 (Nr. 2), a = 1 245,8(6) pm, b = 1 662,0(8) pm, c = 2 159,2(12) pm, α = 77,01(3)°, β = 81,59(3)°, γ = 69,07(3)°, 2: Raumgruppe P21/n (Nr. 14), a = 1 283,7(8) pm, b = 2 102,8(13) pm, c = 1 481,7(9) pm, β = 104,31(5)°, 3: Raumgruppe C2/c (Nr. 15), a = 2 925,4(12) pm, b = 1 297,0(6) pm, c = 2 426,5(9) pm, β = 100,00(3)°, 4: Raumgruppe P1 (Nr. 2), a = 1 046,0(5) pm, b = 1 086,1(7) pm, c = 1 733,0(12) pm, α = 71,76(5)°, β = 88,57(5)°, γ = 87,22(5)°, 5: Raumgruppe I2/a (Nr. 15), a = 2 435,2(9) pm, b = 1 908,3(8) pm, c = 3 534,3(16) pm, β = 97,04(3)°, 6: Raumgruppe C2/c (Nr. 15), a = 2 261,6(15) pm, b = 1 888,9(10) pm, c = 1 810,2(13) pm, β = 108,79(4)°, 7: Raumgruppe P1 (Nr. 2), a = 1 495,9(3) pm, b = 2 005,0(3) pm, c = 2 921,5(9) pm, α = 107,80(2)°, β = 92,36(2)°, γ = 103,99(1)°, 8: Raumgruppe P21/n (Nr. 14), a = 910,2(3) pm, b = 2 568,2(6) pm, c = 1 293,5(6) pm, β = 98,42(3)°, 9: Raumgruppe P21/n (Nr. 14), a = 1 227,3(6) pm, b = 1 205,3(9) pm, c = 1 584,5(7) pm, β = 109,32(3)°).
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