Syntheses and Structures of Manganese(II) and Manganese(III) Nitrate Diaminosarcophagine Complexes

1993 ◽  
Vol 46 (4) ◽  
pp. 465 ◽  
Author(s):  
II Creaser ◽  
LM Engelhardt ◽  
JM Harrowfield ◽  
AM Sargeson ◽  
BW Skelton ◽  
...  
Keyword(s):  
Transition Metals ◽  
Single Crystal ◽  
X Ray ◽  
Manganese Ion ◽  
Structure Determinations ◽  
Jahn Teller ◽  
Jahn Teller Effect ◽  
The Mean ◽  
Appreciable Variation ◽  
Amine Ligand

The syntheses of [ Mn ((NH3)2sar)](NO3)4.H2O and [ Mn ((NH3)2sar)](NO3)5.2H2O, manganese(II) and manganese(III) complexes of the cage amine ligand diaminosarcophagine ( di-aminosarcophagine = (NH2)2sar = 1,8-diamino-3,6,10,13,16,19-hexaazabicyclo[6.6.6] icosane ) in its diprotonated form are recorded, together with their single-crystal X-ray structure determinations at c. 295 K. The monoclinic P21 array of the manganese(II) complex (a 12.386(5), b 12.431(4), c 8.598(4) Ǻ, β 93.89(4)°, V 1321(1) Ǻ3,Z 2) is archetypical for similar complexes of a wide variety of transition metals; for the present determination, R was 0.027 for 2013 'observed' (I > 3σ(I)) reflections. The manganese(III) complex is monoclinic C 2/c, a 10.744(2), b 13.294(4), c 20.462(9) Ǻ, β 102.38(3)°, Z 4; R was 0.055 for 1629 'observed' reflections. Both structures show the six secondary nitrogen atoms of the ligand to be bound to the manganese ion in a configuration approximately halfway between a trigonal prism and an octahedron. The ligand is in the lel3 conformation. In the first complex, Mn -N distances, appropriate to high-spin manganese(II), range from 2.228(3) to 2.253(3) Ǻ, mean 2.238 Ǻ; in the second, surprisingly, the distances are even more closely ranged (unlike those of the sarcophagine analogue of the previous paper), 2.115(4)-2.127(4) Ǻ, the mean (2.122 Ǻ) being closely comparable to that recorded for the sar analogue, and show no appreciable variation attributable to the expected Jahn-Teller effect.

Über Oxocuprate, XIV Zur Kristallchemie von Sr2Cu3O4Cl2.

1976 ◽  
Vol 31 (4) ◽  
pp. 405-407 ◽  
Author(s):  
Bernd Grande ◽  
Hanskarl Müller-Buschbaum
Keyword(s):  
Single Crystal ◽  
Teller Effect ◽  
Space Group ◽  
X Ray ◽  
Jahn Teller ◽  
Jahn Teller Effect ◽  
Group D ◽  
Octahedral Distortion

The new compound Sr2Cu3O4Cl3 was prepared in melts of SrCl2. A single crystal X-ray examination (a = 546.2, c =1259.1 pm, space group D174h-I 4/mmm) shows that the octahedral distortion of the [Cu3O4Cl2]4--network cannot be explained only by the JAHN-TELLER effect.

Spektroskopische Untersuchungen zum Jahn-Teller-Effekt des Cu2+-Ions in Verbindungen vom Typ A2 CuL6, I / Spectroscopic Ivestigations with Respect to the Jahn-Teller-Effect of Cu(II) in Compounds of the Type A2CuL6, I

1974 ◽  
Vol 29 (5-6) ◽  
pp. 295-303 ◽  
Author(s):  
Claus Friebel
Keyword(s):  
Esr Spectra ◽  
Ligand Field ◽  
X Ray ◽  
Octahedral Sites ◽  
Structural Differences ◽  
Structure Determinations ◽  
Jahn Teller ◽  
Jahn Teller Effect ◽  
Ligand Field Spectra ◽  
Atomic Parameters

Structural relations between perovskite-related lattices of the type A2CuL6 and the perovskite compounds A2(12) [BCu](6)L6 (1: 1 order in the octahedral sites, elpasolite type) are demonstrated by two examples, the compounds A,Cu(OH)6 [A = Ba, Sr] and Ba2CuF6. From the ESR spectra a coupling of Jahn-Teller-distorted Cu-ligand-octahedra in these compounds corresponding to a “disturbed” type of antiferrodistortive order can be deduced. This result is in agreement with recent X-ray structure determinations. The ligand field spectra of the hydroxocuprates(II) indicate tetragonally elongated CuO6-octahedra with very long axial distances. From the ESR investigations further conclusions can be drawn concerning structural differences between the Ba- and the Sr-compound [Sr2Cu(OH6)], the atomic parameters of which are still unknown.

Die Kristallstrukturen der isotypen Verbindungen Ba3[MoN4] und Ba3[WN4] / The Crystal Structures of the Isotypic Compounds Ba3[MoN4] and Ba3[WN4]

1991 ◽  
Vol 46 (5) ◽  
pp. 566-572 ◽  
Author(s):  
Axel Gudat ◽  
Peter Höhn ◽  
Rüdiger Kniep ◽  
Albrecht Rabenau
Keyword(s):  
Transition Metals ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ternary Compounds ◽  
The Third

The isotypic ternary compounds Ba3[MoN4] and Ba3[WN4] were prepared by reaction of the transition metals with barium (Ba3N2, resp.) under nitrogen. The crystal structures were determined by single crystal X-ray diffraction: Ba3[MoN4] (Ba3[WN4]): Pbca; Z = 8; a = 1083.9(3) pm (1091.8(3) pm), b = 1030.3(3) pm (1037.5(3) pm), c = 1202.9(3) pm (1209.2(4) pm). The structures contain isolated tetrahedral anions [MN4]6- (M = Mo, W) which are arranged in form of slightly distorted hexagonal layers and which are stacked along [010] with the sequence (···AB···). Two of the three Ba atoms are situated between, the third one is placed within the layers of [MN4]-groups. In this way the structures can be derived from the Na3As structure type.

Comparative Structural Studies on Three-Coordinate Copper(I) Halide Complexes With Tertiary Phosphines. Crystal Structures of [(PPh2Mes)CuX]2 and [(PPhMes2)CuX]2 (Mes = Mesityl X = Cl, Br, I)

1992 ◽  
Vol 45 (7) ◽  
pp. 1155 ◽  
Author(s):  
GA Bowmaker ◽  
D Camp ◽  
RD Hart ◽  
PC Healy ◽  
BW Skelton ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Copper Atom ◽  
Structural Studies ◽  
Coordination Environment ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Structure Determinations ◽  
Halide Complexes ◽  
The Subject

The 1 : 1 complexes of the substituted triphenylphosphine ligands mesityldiphenylphosphine and dimesitylphenylphosphine with copper(1) chloride, bromide and iodide have been the subject of single-crystal X-ray structure determinations at 295 K. All six complexes crystallize as air-stable dimeric molecules, [(PPh2Mes)CuX]2 and [ (PPhMes2)CUX]2 with each copper atom in a distorted trigonal PCuX2. coordination environment. Crystals of [(PPh2Mes)CuCl]2 (1) are monoclinic, P21/n, a 9.961(3), b 18.687(6), c 11.009(7) Ǻ, β 114.63(4)°; R was 0.049 for 2450 'observed' reflections. [(PPh2Mes)CuBrI2 (2) is monoclinic, P21/n, a 9.939(2), b 18.832(6), c 11.238(6) Ǻ, β 115.36(3)°; R was 0.046 for 1803 'observed' reflections. [(PPh2Mes)CuI]2.4/3 C6H6 (3) is rhornbohedral, R3, a 36.877(8), c 9.047(5) A; R was 0.039 for 2537 'observed' reflections. Crystals of [(PPhMes2)CuCl]2.2MeCN (4) are triclinic, Pi, a 15.783(7), b 9.570(4), c 8.914(4) Ǻ, α 72.43(3), β 76.37(3), γ 74.03(3)°; R was 0.045 for 3341 'observed' reflections. [(PPhMes2)CuBr]2.3C6H6 (5) is monoclinic, C2/c, a 9.694(6), b 30.15(2), c 20.66(2) Ǻ, β 98.00(7)°; R was 0.047 for 2117 'observed' reflections. [(PPhMes2)CuI]2.2MeCN (6) is orthorhombic, PP1nb, a 11.694(8), b 14.77(1), c 29.76(3) Ǻ; R was 0.049 for 3447 'observed' reflections. Cu-P bond lengths are: 2.196(2) A (1); 2.198(3) Ǻ (2); 2.222(5) and 2.226(5) Ǻ (3); 2.202(1) Ǻ (4); 2.197(3) A (5); 2.201(4) and 2.264(5) Ǻ (6). The geometries of the LCuX2 and CuX2Cu units are compared with data reported for other monomeric and dimeric compounds for both phosphorus- and nitrogen-based ligands L.

Approaches to the Synthesis of Lincosamine, a Derived Portion of the Antibiotic Lincomycin

1990 ◽  
Vol 43 (10) ◽  
pp. 1657 ◽  
Author(s):  
LM Engelhardt ◽  
BW Skelton ◽  
RV Stick ◽  
DMG Tilbrook ◽  
AH White
Keyword(s):  
Nitrogen Atom ◽  
Single Crystal ◽  
Structure Elucidation ◽  
X Ray ◽  
Structure Determinations

A variety of approaches towards the synthesis of lincosamine, a derived portion of the antibiotic lincomycin , are reported. Initial approaches involved the intramolecular delivery of a nitrogen atom ( trichloroacetimidate , trichloroacetylcarbamate , carbamate, 2-amino-2- phenylacetate ) attached to O4 onto C6 of a 6,7-anhydrooctoside. Later approaches, albeit more direct but again largely unsuccessful, involved the Sharpless titanium(IV)-mediated nucleophilic opening of a suitable 6,7-anhydrooctose, and the Sharpless oxyamination and the aziridination of suitable octenoses . As an aid to the structure elucidation of several compounds encountered in this work, single-crystal X-ray structure determinations are reported for methyl 6,7-anhydro-2,3-di-O-benzyl-8-deoxy-α-D-threo-D-galacto-octopyranoside , methyl 6,7-anhydro-2,3-di-O-benzyl-8-deoxy-α-D-threo-D-gluco-octopyranoside and 7-azido-7-deoxy-1,2:3,4-di-O-isopropylidene-β-L-erythro-Dgalacto-octose.

Notizen: Einkristall-Strukturdaten einiger Fluoride und Cyanide A2IBIMIIIX6 der Elpasolithfamilie / Single Crystal Structural Data of Some Fluorides and Cyanides A2IBIMIIIX6 of the Elpasolite Family

1975 ◽  
Vol 30 (5-6) ◽  
pp. 462-464 ◽  
Author(s):  
R. Haegele ◽  
W. Verscharen ◽  
D. Babel
Keyword(s):  
Single Crystal ◽  
Structural Data ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Structure Determinations ◽  
Crystal Structural Data ◽  
Crystal Structural

The parameters of complete X-ray structure determinations are given for the fluoridesRb2NaFeF6 and Rb2KFeF6 (cubic), Cs2NaCrF6 and Cs2NaFeF6 (hexagonal-rhom-bohedral) and Cs2LiGaF6 (hexagonal). Space group and lattice constants of the monoclinic cyanides Cs2BFe(CN)6 (B = Na, K, Rb) are reported as well.

On the Reaction of ortho-Diphenoquinone Valence Isomers with Primary and Secondary Amines. X-Ray Structure Analysis of a 2,3-Dihydro-1H-azepinone and its Photochemical and Oxidative Conversion Products

1979 ◽  
Vol 32 (9) ◽  
pp. 1931 ◽  
Author(s):  
H Becker ◽  
K Gustafsson ◽  
CL Raston ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Secondary Amines ◽  
Reaction Products ◽  
Oxidative Conversion ◽  
X Ray Diffraction ◽  
X Ray ◽  
Primary And Secondary Amines ◽  
Diffraction Structure ◽  
Structure Determinations ◽  
Photochemical Isomerization

Single-crystal X-ray diffraction structure determinations are reported for three reaction products and photoisomers formed from reactions between an o-diphenoquinone valence isomer and primary and secondary amines, namely: 3,5-di-t-butyl-7-(3,5-di-t-butyl-2-hydroxyphenyl)-1-methyl-2,3-dihydro-1H-azepin-2-one (8; R1 = R2 = But, R3 = Me), its photochemical isomerization product 4,6-di-t-butyl-1-(3,5-di-t-butyl-2-hydroxyphenyl)-2-methyl-2-azabicyclo[3,2,0]hept-6-en-3-one (9; R1 = R2 = But, R3 = Me) and 4',5,7-tri-t-butyl-3'-(2,2-dimethylpropionyl)-1'-methylspiro[benzofuran-3(2H)-2'- pyrrolidinel-2,5'-dione (12; R1 = R2 = But, R3 = Me).

Sign in / Sign up

Export Citation Format

Share Document