X-ray structural characterization of an outer-sphere copper(II) dimer, dicyanobis(2,2',2''-triaminotriethylamine)dicopper(II) tetraphenylborate. Hydrogen-bonding between two trigonal-bipyramidal copper cations

1974 ◽  
Vol 13 (8) ◽  
pp. 1911-1916 ◽  
Author(s):  
D. Michael. Duggan ◽  
David N. Hendrickson
1997 ◽  
Vol 53 (3) ◽  
pp. 504-512 ◽  
Author(s):  
A. Martin ◽  
A. A. Pinkerton ◽  
R. D. Gilardi ◽  
J. C. Bottaro

Three biguanidinium salts of the energetic dinitramide anion have been prepared and structurally characterized from room-temperature X-ray diffraction data. Biguanidinium mono-dinitramide, (BIGH)(DN), triclinic, P\overline 1, a = 4.3686 (4), b = 9.404 (2), c = 10.742 (1) Å, \alpha = 83.54 (1), \beta = 80.386 (9), \gamma = 79.93 (1)°, V = 426.8 (1) Å3, Z = 2, D x = 1.62 g cm−3. Biguanidinium bis-dinitramide, (BIGH2)(DN)2, monoclinic, C2/c, a = 11.892 (2), b = 8.131 (1), c = 13.038 (2) Å, \beta = 115.79 (1)°, V = 1135.1 (3) Å3, Z = 4, D x = 1.84 g cm−3. Biguanidinium bis-dinitramide monohydrate, (BIGH2)(DN)2.H2O, orthorhombic, P212121, a = 6.4201 (6), b = 13.408 (1), c = 14.584 (2) Å, V = 1255.4 (4) Å3, Z = 4, D x = 1.76 g cm−3. All three structures are characterized by extensive hydrogen bonding. Both the mono- and diprotontated cations consist of two planar halves twisted with respect to each other. The dinitramide anion has a surprisingly variable and asymmetric structure. The two halves of the anion are twisted with respect to each other; however, the twist varies from 5.1 to 28.9°. In addition, the two ends of the anion have significantly different geometries, e.g. the `equivalent' N—N bond lengths differ by up to 0.045 Å.


1997 ◽  
Vol 50 (6) ◽  
pp. 675 ◽  
Author(s):  
Effendy ◽  
Warren J. Grigsby ◽  
Robert D. Hart ◽  
Colin L. Raston ◽  
Brian W. Skelton ◽  
...  

Room-temperature single-crystal X-ray structural characterizations of two oxidation products of triphenylstibine of the form XPh3SbOSbPh3X are recorded for X = Cl, NO3. ClPh3SbOSbPh3Cl is monoclinic, P 21/c, Z = 4 f.u., a 9·109(4), b 19·809(8), c 19·30(2) Å, β 109·27(5)°, conventional R on F being 0·038 for No 4431 ‘observe’ (I > 3σ(I)) independent reflections. In this complex, Sb-O-Sb is quasi-linear, 173·1(3)°, in contrast to the previously recorded benzene solvate, in which it is 139·0(3)°; in the nitrate, [(O2NO)Ph3SbOSbPh3(ONO2)], triclinic, P-1, Z = 2 f.u., a 15·609(5), b 13·238(4), c 10·140(2) Å, α 87·11(2), β 88·46(7), γ 72·93(2)°, R 0·036 for No 5275, it is also bent (137·0(2)°). The anionic substituent is opposed to the oxo bridge in the trigonal bipyramidal five-coordinate array about the metal in both complexes. A redetermination of the structure of Ph8Sb4O6 is recorded, presenting a non-disordered model in a triclinic P-1 cell, a 19·98(3), b 11·635(2), c 9·739(2) Å, α 92·28(1), β 98·98(1), γ 99·74(1)°, Z = 2 f.u., R 0·046 for No 3578. A new (‘β’) phase of triphenylstibine, crystallized from hexane/toluene is also recorded: monoclinic, P 21/c, a 15·386(8), b 11·304(5), c 19·078(8) Å, β11·64(4)°, Z = 8, R 0·045 for No 3393.


2007 ◽  
Vol 2007 (suppl_26) ◽  
pp. 61-66 ◽  
Author(s):  
B. Peplinski ◽  
B. Adamczyk ◽  
G. Kley ◽  
K. Adam ◽  
F. Emmerling ◽  
...  

Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.


1988 ◽  
Vol 6 (3) ◽  
pp. 1946-1949 ◽  
Author(s):  
B. T. Jonker ◽  
S. B. Qadri ◽  
J. J. Krebs ◽  
G. A. Prinz

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