Kristallstrukturen von zwei Modifikationen des Mo(IV)-Komplexsalzes [(Et2PS2)3Mo3S(S2)3]+(Et2PS2)- / Crystal Structures of Two Modifications of the Mo(IV) Complex Salt [(Et2PS2)3Mo3S(S2)3] + (Et2PS2)-

1982 ◽  
Vol 37 (11) ◽  
pp. 1437-1441 ◽  
Author(s):  
Beate Meyer ◽  
Hartmut Wunderlich
Keyword(s):  
Crystal Structures ◽  
Coordination Number ◽  
Local Symmetry ◽  
Complex Salt ◽  
X Ray ◽  
Anions And Cations ◽  
R Factors

Tris(diothyldithiophosphinato)-tris-μ-disulfido-μ3-thiotriangulo-trimolybdenum(IV)-di-ethyldithiophosphinate, [(et2PS2)3Mo3S(S2)3+(et2PS2)-, crystallizes in two orthorhombic modifications with crystallographic parameters of A: a = 20.651(3), b=10.152(2), c = 19.019(2) Å, Pca21, Z = 4 and B: a = 20.128(2), b= 15.655(2), c = 12.608(1) Å, Pinna, Z = 4. Both crystal structures were determined from 2886 (A) and 3414 (B) X-ray data with R factors of 0.058 and 0.045, respectively. The Mo atoms form a trinuclear Mo3S(S2)3 cluster with local symmetry close to C3V in both modifications which differ in the packing of anions and cations and in the conformation of the ethyl groups. The av. distance Mo-Mo is 2.737 Å, the coordination number of the Mo atoms is 7 within the cluster and 9 on inclusion of the S atoms of the dithiophosphinato group.

Hydrogen bonding in the crystal structures of the adducts between 1-phenyl-3,5-dimethylpyrazole with oxalic and perchloric acids

1984 ◽  
Vol 62 (4) ◽  
pp. 725-728 ◽  
Author(s):  
J. Zukerman-Schpector ◽  
E. E. Castellano ◽  
G. Oliva ◽  
A. C. Massabni ◽  
A. Derbli Pinto
Keyword(s):  
Crystal Structures ◽  
Proton Donor ◽  
Proton Acceptor ◽  
Strong Hydrogen Bond ◽  
Full Matrix ◽  
X Ray ◽  
Space Groups ◽  
Cell Dimensions ◽  
R Factors ◽  
Positively Charged

The crystal structures of the title compounds have been determined from diffractometric X-ray data and refined by full-matrix least-squares to final R factors of 0.057 and 0.071 for the oxalic and perchloric adducts respectively.The space groups and cell dimensions are: (oxalic) C2/c, a = 16.516(3), b = 11.685(2), c = 12.587(3) Å, β = 107.11(2)° with Z = 4; (perchloric) Pbca, a = 16.204(3), b = 15.329(6), c = 10.296(3) Å with Z = 8.In both structures the complex is stabilized by a strong hydrogen bond between the N(2) of the 1-phenyl-3,5-dimethylpyrazole (PDMP) group and an oxygen of the acid. In the oxalic adduct the PDMP group is neutral and the N(2) atom acts as a proton acceptor, while in the perchloric complex the PDMP group is positively charged with the N(2) atom acting as a proton donor.

Silberdiammin-disilber-hexacyanometallate(III): Kantenverknüpfte Doppeltetraeder-Einheiten Ag2N6 in den unterschiedlichen Strukturen von Eisen- und Cobaltkomplex / Silverdiammine Disilver Hexacyanometallates(III): Edge-Sharing Tetrahedra Ag2N6 in the Different Structures of Iron and Cobalt Complex

1988 ◽  
Vol 43 (12) ◽  
pp. 1589-1597 ◽  
Author(s):  
B. Ziegler ◽  
K. Seitz ◽  
D. Babel
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Dihedral Angle ◽  
Cobalt Complex ◽  
Iron Complex ◽  
Space Group ◽  
X Ray ◽  
R Factors ◽  
Ray Methods

Abstract The crystal structures of the monoclinic compounds Ag(NH3)2Ag2Fe(CN)6 (a = 948.2, b = 1235.5, c = 1246.8 pm, β = 94.98°. Z = 4. space group Cc) and Ag(NH3)2Ag2Co(CN)6 (a = 772.1, b = 1347.9, c = 1405.2 pm, β = 101.25°, Z = 4, C2/c) have been determined by x-ray methods from single crystals. Using 1947 and 2739 reflections, resp.. R factors of about 5% were reached. Both compounds are similar in containing approximately linear Ag(NH3)2+ dumb-bells (Ag-N = 216 pm) and dimeric Ag2N6 units. The latter consist of distorted edge-sharing tetrahedra (average Ag-N = 229 and 231 pm, resp.), the cavities of which are provided by the nitrogen ends of six surrounding M(CN)63- octahedra (Fe -C =195 pm, Co -C = 189 pm, C - N = 115 and 114 pm, resp.). In the iron complex, which is elpasolite-related, the central Ag2N2 ring is planar (Ag-Ag = 327.0 pm). By contrast the unit is folded (Ag-Ag = 307.8 pm, dihedral angle 126° between AgN2 triangles) in the cobalt complex, which has a different structure as discussed in detail

Structural Characterization of Cationic 16-Electron Pentamethylcyclopentadienyl Ruthenium(II) Complexes Containing the Binuclear [Cp*Ru(μ-Cl)3RuCp*]– Anion

2008 ◽  
Vol 63 (10) ◽  
pp. 1155-1159 ◽  
Author(s):  
Thomas Glöge ◽  
Dejan Petrovic ◽  
Cristian G. Hrib ◽  
Peter G. Jones ◽  
Matthias Tamm
Keyword(s):  
Crystal Structures ◽  
Structural Characterization ◽  
Complex Salt ◽  
Monoclinic Space Group ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Diimine Ligand ◽  
Half Sandwich

AbstractThe reaction of the diimine ligand 1,2-bis(1,3-diisopropyl-4,5-dimethylimidazolin-2-imino)ethane (BLiPr) with tetrameric [Cp*RuCl]4 in a 1 : 0.75 ratio afforded the complex salt [1][2] containing the 16-electron half-sandwich cation [Cp*Ru(BLiPr)]+ (1) and the dinuclear anion [Cp*Ru(μ- Cl)3RuCp*]− (2). The X-ray crystal structures of [1][2]·31/2THF (monoclinic, space group P21/n, Z = 4) and of [1][2]·THF (monoclinic, space group C2/m, Z = 4) are reported, allowing the structural characterization of the unprecedented anion 2, in which two [(η5-C5Me5)Ru(II)] moieties are bridged by three μ2-chlorine atoms.

Neutron and X-ray Diffraction Study on the Structure of Ultraphosphate Glasses

1997 ◽  
Vol 52 (3) ◽  
pp. 259-269 ◽  
Author(s):  
Uwe Hoppe ◽  
Günter Walter ◽  
Dörte Stachel ◽  
Andrea Barz ◽  
Alex C. Hannon
Keyword(s):  
Crystal Structures ◽  
Coordination Number ◽  
Real Space ◽  
The Other ◽  
Oxide Content ◽  
X Ray Diffraction ◽  
X Ray ◽  
Space Resolution ◽  
Epithermal Neutrons ◽  
The Mean

Abstract The high real-space resolution of neutron diffraction experiments which is provided by use of the epithermal neutrons from spallation sources was exploited in order to differentiate the unlike P-O bonds existing in the PO4 units of phosphate glass networks. The 2 P-O distance peaks, separated by about 12 pm, which were found in the zinc and the calcium ultraphosphate glasses studied are assigned to oxygen sites on bridging (OB) and terminal (OT) positions. The mean P-O distances are nearly invariable versus the growing metal oxide content which results from an elongation of the P-OB and P-OT bonds. The bond lengths which are known from the related crystal structures and from ab initio calculations show almost the same behaviour. The discussion of further details of the crystal structures leads to the conclusion that P-OB rather than P-OT distances should show more details in case of diffraction measurements of even higher real-space resolution. The change of the Zn-O coordination number from 6 to 4 versus increasing ZnO content, which was obtained in previous X-ray diffraction experiments, is confirmed by the recent combination of neutron and X-ray diffraction data. On the other hand, the Ca-O coordination number of about 6 is almost invariable.

Interhalogen-Kationen: Darstellung und Kristallstrukturen (143 K) von I3Cl2SbCl6, I3Cl2AlCl4 und I3Br2SbCl6 / Interhalogen Cations: Preparation and Crystal Structures (143 K) of I3Cl2SbCl6, I3Cl2AlCl4 and I3Br2SbCl6

1981 ◽  
Vol 36 (3) ◽  
pp. 283-288 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak
Keyword(s):  
Low Temperature ◽  
Single Crystal ◽  
Crystal Structures ◽  
The Novel ◽  
Covalent Bonds ◽  
X Ray ◽  
Anions And Cations

Abstract The title compounds were prepared and their crystal structures determined from low temperature single crystal X-ray data. The structures contain the anions SbCl6- and AlCL4-and the novel interhalogen cations I3Cl2+ and I3Br2+ . Anions and cations are linked to infinite chains by weak covalent bonds.

Strukturen zweier isomerer Gadolinium(III)-Polyaminopolycarboxylate -Argumente für signifikante Unterschiede ihrer 1H-NMR-Relaxation/Structures of Two Isomeric Gadolinium(III) Polyamino Polycarboxylates -Relation to their Significant Differences in 1H NMR Relaxation

1997 ◽  
Vol 52 (7) ◽  
pp. 805-809 ◽  
Author(s):  
Robert Ruloff ◽  
Thomas Gelbrich ◽  
Joachim Sieler ◽  
Eberhard Hoyer ◽  
Lothar Beyer
Keyword(s):  
Aqueous Solution ◽  
Crystal Structures ◽  
Coordination Number ◽  
1H Nmr ◽  
Nmr Relaxation ◽  
Acetate Group ◽  
Water Molecules ◽  
X Ray ◽  
H Nmr ◽  
Low Efficiency

Abstract We present preparation and X-ray crystal structures of gadolinium(III) complexes with two isomeric ligands; triethylenetetraminehexaacetic acid, H6ttha, and tris(2-aminoethyl)amine-hexaacetic acid, H6ttaha, respectively. In case of [C(NH2)3]2[Gd(Httha)] · 5 H2O (1) the inner coordination sphere is made up of 9 donor atoms of the ligand and reflects the low efficiency in accelerating 1H NMR relaxation of an aqueous solution. In case of [C(NH2)3]3[Gd(ttaha)] · 3 H2O (2) the coordination number of 9 is realized via 7 donor atoms of the ligand and 2 oxygen atoms of a pending acetate group of the adjacent complex. Luminescence studies in aqueous solution confirm replacement of this acetate group by 2 water molecules. The relaxivity of [Gd(Httaha)]2- is 7.3 ± 0.1 mM -1 s -1 as determined at pH = 7.2, 20 MHz and 40°C.

Gesteuerte Kristallisation des Gadolinium(III)-Komplexes von Diethylentriaminpentaacetat: Monomere und dimere Struktur / Controlled Crystallization of the Gadolinium(III) Complex of Diethylenetriamine-Pentaacetate: Monomeric and Dimeric Structure

1998 ◽  
Vol 53 (9) ◽  
pp. 955-959 ◽  
Author(s):  
Robert Ruloff ◽  
Thomas Gelbrich ◽  
Eberhard Hoyer ◽  
Joachim Sieler ◽  
Lothar Beyer
Keyword(s):  
Water Molecule ◽  
Crystal Structures ◽  
Coordination Number ◽  
X Ray ◽  
Dimeric Structure ◽  
Carboxylate Oxygen ◽  
Metal Atoms ◽  
Controlled Crystallization ◽  
Coordinated Water ◽  
Oxygen Atoms

We present the preparation and X-ray crystal structures of two gadolinium(III) complexes of the ligand diethylenetriamine pentaacetic acid (H5dtpa). With two equivalents of guanidinium (gu+) per equivalent of complex we obtained the dimer (gu)4[Gd2(dtpa)2]·(gu)HCO3 , and with one equivalent of aminoguanidinium (agu+) the monomer (agu)[Gd(Hdtpa)(H2O)]·2H2O , both with the metal atoms in a coordination number of 9. The dimer contains no coordinated water molecule. The monomer is present as two crystallographically independent complexes hydrogen-bridged via carboxylate oxygen atoms (O···O 2.48 Å; O-H···O 172°) and with Gd-Ocoord. water distances of 2.418(4) and 2.423(4) Å, respectively.

Structural studies on the dichlorocarbene adducts with (−)-R-carvone. I. The crystal structures of [1R, 4R, 6R, 9R]-7,7-dichloro-1-methyl-4-[2′,2′-dichloro-1′-methyl- cyclopropyl]-bicyclo[4.1.0]-heptan-2-one and [1R, 4R, 6R, 9S]-7,7-dichloro-1-methyl-4-[2′,2′-dichloro-1′-methylcyclopropyl]-bicyclo[4.1.0]-heptan-2-one

1984 ◽  
Vol 62 (3) ◽  
pp. 570-573 ◽  
Author(s):  
J. Zukerman-Schpector ◽  
E. E. Castellano ◽  
G. Oliva ◽  
Timothy John Brocksom ◽  
Elisabete Terezinha Canevarolo
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Dihedral Angle ◽  
Chemical Reaction ◽  
Unit Cell ◽  
Structural Studies ◽  
Full Matrix ◽  
X Ray ◽  
Cell Dimensions ◽  
R Factors

The crystal structures of the title compounds have been determined from diffractometric X-ray data and refined by full-matrix least-squares to final R factors of 0.047 and 0.060 from 830 and 620 independent reflections above background, respectively. The space group and the number of molecules per unit cell are the same in both cases: P212121 and Z = 4. Cell dimensions are: a = 7.982(2), b = 9.538(3), c = 18.785(3) Å for the S form and a = 10.339(3), b = 11.510(3), and c = 11.886(6) Å for the R form. The molecules, produced simultaneously in the same chemical reaction, have essentially identical configuration except for the location of the chlorine atoms at C-11 (in the S case) and at C-10 (in the R case). This difference gives rise to a completely different molecular packing of the structures. In each compound the two cyclopropane rings present a cis relationship to one another, with an identical dihedral angle of 77.0°.

scholarly journals Kristallstrukturen komplexer Metalate mit dem sterisch anspruchsvollen 1,3,5-Tri(tert-butyl)tropylium-Kation / X-Ray Crystal Structures of Complex Metallates Containing the Sterically Demanding 1,3,5-Tri(tert-butyl)tropylium Cation

2006 ◽  
Vol 61 (10) ◽  
pp. 1189-1197 ◽  
Author(s):  
Matthias Tamm ◽  
Thomas Bannenberg ◽  
Victoria Urban ◽  
Tania Pape ◽  
Olga Kataeva
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Transition Metal Complexes ◽  
Crystal Packing ◽  
Proton Donor ◽  
Close Inspection ◽  
X Ray ◽  
Tert Butyl ◽  
Sterically Demanding ◽  
Anions And Cations

The X-ray crystal structures of anionic transition metal complexes containing the sterically demanding 1,3,5-tri-tert-butyltropylium cation, [1,3,5-C7H4tBu3]+, as the compensating ion are presented. Bis(1,3,5-tri-tert-butyltropylium) hexachlorodiferrate(II), [1,3,5-C7H4tBu3]2[Fe2Cl6] (4), was obtained from the reaction of the 1,3,5-tri-tert-butyltropylium hydrogendichloride, [1,3,5- C7H4tBu3][HCl2] (3), with FeCl2, whereas the 1,3,5-tri-tert-butyltropylium tetrabromooxomolybdate( V) [1,3,5-C7H4tBu3][trans-Mo(O)Br4(CH3CN)] (7) was isolated from the reaction of the cycloheptatrienyl complex [(η7-1,3,5-C7H4tBu3)Mo(CO)2Br] (6) with elemental bromine. The crystal structures of 3, 4, 7 and 7 · CH3CN show in each case well separated anions and cations and the absence of any covalent anion-cation interactions. However, close inspection of the crystal packing reveals that the 1,3,5-tri-tert-butyltropylium cation can act as a CH-proton donor towards the counterion leading to the formation of weak C-H· · ·Cl-M and C-H· · ·O=M hydrogen bonds in 4 and in 7 and 7 ·CH3CN, respectively.

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