Organoamido- and Aryloxo-Lanthanoids. XI. Syntheses and Crystal Structures of Nd(Odpp)3, Nd(Odpp)3(thf) and [Nd(Odpp)3(thf)2].2(thf) (Odpp-=2,6-Diphenylphenolate): Variations in Intramolecular π-Ph-Nd Interactions

1995 ◽  
Vol 48 (4) ◽  
pp. 741 ◽  
Author(s):  
GB Deacon ◽  
TC Feng ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Phenyl Group ◽  
Triangular Array ◽  
The Other ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The X-ray crystal structure of Nd (Odpp)3 ( Odpp- = 2,6-diphenylphenolate), obtained by sublimation of Nd ( Odpp )3( thf )2 ( thf = tetrahydrofuran ) [triclinic, Pī , a 15.835(5), b 13.499(10), c 10.955(11) Ǻ, α 116.25(7), β 92.87(7), γ 101.66(6)°, V 2031 Ǻ3, Z2, No 5726 'observed' data (I > 3σ(I)) refined to conventional R 0.047 shows a near triangular array of oxygens surrounding neodymium { Nd -O} 2.169 Ǻ, ∑ O- Nd -O 353.2° with additional, intramolecular Nd-η6-Ph chelate interactions { Nd -C} 3.046 Ǻ and Nd-η1-Ph ( Nd -C 2.964(7)Ǻ). There is a pseudotrigonal bipyramidal arrangement of the oxygens, the centroid of the η6-Ph, and the η1-carbon. The complex Nd ( Odpp )3( thf ), obtained by crystallization of Nd ( Odpp )3( thf )2 from toluene (monoclinic, P21/c, a 12.213(4), b 21.447(4), c 17.744Ǻ, β 104.25(2)°, V 4505 Ǻ3, Z 4, R 0.042 for No 8014) also has pseudotrigonal bipyramidal stereochemistry, with a triangular equatorial array of aryl oxide oxygens { Nd -O} 2.193 Ǻ; ∑ O- Nd -O 358.7°, an apical thf oxygen (Nd -O 2.446(3)Ǻ), and an apical intramolecular chelating phenyl group. As the last has three Nd -C contacts (3.094(5), 3.144(5), 3.010(5)Ǻ) significantly shorter than the other three (3.300(5), 3.427(5), 3.377(5)Ǻ), an η3-Ph-Nd interaction seems likely. For [ Nd ( Odpp )3( thf )2].2( thf ), obtained by crystallization from tetrahydrofuran without drying of the crystals, the X-ray structure (monoclinic, P21, a 10.230(2), b 21.919(5), c 13.411(4) Ǻ, β 101.15(2)°, V 2950 A3, Z2, R 0.058 for No 3237) reveals a distorted trigonal bipyramidal arrangement of three aryl oxide oxygens (two equatorial 2.208(9), 2.16(1) Ǻ; one axial 2.203(9) Ǻ) and two thf oxygens (one equatorial 2.44(1) Ǻ; one axial (significantly distant) 2.62(1) Ǻ). The X-ray structure of [La( Odpp )3( thf )2].2( thf ) shows it to be isostructural with the neodymium analogue.

Neue Oxopnictate AI3MVO4: Darstellung und Kristallstruktur von A3AsO4 (A = K, Rb, Cs) und K3BiO4 / New Oxopnictates AI3MVO4: Synthesis and Crystal Structure of A3AsO4 (A = K, Rb, Cs) and K3BiO4

2002 ◽  
Vol 57 (6) ◽  
pp. 599-604 ◽  
Author(s):  
Franziska Emmerling ◽  
Mamdouh Idilbi ◽  
Caroline Röhr
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Close Packing ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Trigonal Bipyramidal Geometry ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds have been synthesized via oxidation of the elemental pnicogenes (M = As, Bi) with the hyperoxides AO2 (A = K, Rb, Cs) and their crystal structures were determined on the basis of single crystal X-ray data. In K3AsO4 (orthorhombic, Cccm, a = 1060:1(1), b = 1135:2(1), c = 1694:0(2) pm, Z = 16) and Cs3AsO4(orthorhombic, Pnma, a = 1254:3(2), b = 902:9(2), c = 658:5(3) pm, Z = 4) isolated tetrahedra [AsO4]3- with distances As-O between 167.0 and 170.5 pm are present, which are arranged in a nearly cubic close packing. The structure of K3BiO4 (triclinic, P1̄, a = 643:18(6), b = 657:27(6), c = 762:41(7) pm, α = 101:724(2)°, β = 96:472(2)°, γ = 105:465(2)°, Z = 2) contains centrosymmetric dimers [O3BiO2BiO3]6-, in which the Bi(V) atoms are surrounded by five O atoms in a distorted trigonal bipyramidal geometry with distances Bi-O in the range of 199.5 to 233.1 pm.

scholarly journals Crystal structure refinement of magnesium zinc divanadate, MgZnV2O7, from powder X-ray diffraction data

2021 ◽  
Vol 77 (6) ◽  
pp. 588-591
Author(s):  
Stephanie J. Hong ◽  
Jun Li ◽  
Mas A. Subramanian
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Structure Refinement ◽  
Atomic Ratio ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Wyckoff Position ◽  
Distorted Trigonal Bipyramidal

The crystal structure of magnesium zinc divanadate, MgZnV2O7, was determined and refined from laboratory X-ray powder diffraction data. The title compound was synthesized by a solid-state reaction at 1023 K in air. The crystal structure is isotypic with Mn0.6Zn1.4V2O7 (C2/m; Z = 6) and is related to the crystal structure of thortveitite. The asymmetric unit contains two metal sites with statistically distributed magnesium and zinc atoms with the atomic ratio close to 1:1. One (Mg/Zn) metal site (M1) is located on Wyckoff position 8j and the other (M2) on 4h. Three V sites (all on 4i), and eight O (three 8j, four 4i, and one 2b) sites complete the asymmetric unit. The structure is an alternate stacking of V2O7 layers and (Mg/Zn) atom layers along [20\overline{1}]. It is distinct from other related structures in that each V2O7 layer consists of two groups: a V2O7 dimer and a V4O14 tetramer. Mixed-occupied M1 and M2 are coordinated by oxygen atoms in distorted trigonal bipyramidal and octahedral sites, respectively.

scholarly journals Darstellung und Kristallstruktur von K2Sn2S5 und K2Sn2Se5 / Preparation and Crystal Structure of K2Sn2S5 and K2Sn2Se5

1992 ◽  
Vol 47 (2) ◽  
pp. 197-200 ◽  
Author(s):  
Kurt O. Klepp
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structure Type ◽  
Slow Cooling ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Equatorial Bond ◽  
Binary Compounds ◽  
R Factors ◽  
Distorted Trigonal Bipyramidal

K2Sn2S5 and K2Sn2Se5 were prepared by reacting stoichiometric powdered mixtures of the binary compounds K2S or K2Se with Sn and the corresponding chalcogen at 1070 K, followed by slow cooling of the melt. The two compounds are isostructural and crystallize with the Tl2Sn2S5 structure type, s.g. C 2/c, Z = 4 with a = 11.072(5) Å, b = 7.806(3)Å, c = 11.517(5)Å, β = 108.43(2)° for K2Sn2S5 and a = 11.613(5)Å, b = 8.189(3) Å, c = 11,897(6) Å, β = 108.28(2)° for K2Sn2Se5. The crystal structures were refined to conventional R-factors of 0.032 and 0.031, respectively. Sn-atoms are in a distorted trigonal-bipyramidal chalcogen coordination. The average equatorial bond lengths are Sn -S: 2.427 Å and Sn -Se: 2.552 Å , the axial ones are Sn -S: 2.600 Å and Sn -Se: 2.774 Å.

Organoamido- and Aryloxo-lanthanoids. X. Tris(η2-3,5-di-t-butylpyrazolato)lanthanoid(III) Complexes and the X-Ray Crystal Structure of Er(η2-But2pz)3(thf)2

1994 ◽  
Vol 47 (7) ◽  
pp. 1223 ◽  
Author(s):  
JE Cosgriff ◽  
GB Deacon ◽  
BM Gatehouse ◽  
H Hemling ◽  
H Schumann
Keyword(s):  
Crystal Structure ◽  
Triphenylphosphine Oxide ◽  
The Other ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Oxygen Atoms

The complexes Ln (But2pz)3( thf )2 ( Ln = Y, La, Pr, Nd , Sm, Gd, Dy , Er , Yb, Lu; But2pz- = 3,5-di-t-butylpyrazolate; thf = tetrahydrofuran ), and [ Ln (But2pz)3(OPPh3)2].( dme )n ( Ln = La, n = ⅔ ; Ln = Er , n = 1; dme = 1,2-dimethoxyethane) have been prepared by reaction of the lanthanoid metal with bis ( pentafluorophenyl )mercury and the corresponding pyrazole in either thf , or in dme in the presence of triphenylphosphine oxide. The X-ray crystal structure of Er (η2-But2pz)3( thf )2 [monoclinic, space group P21 (No. 4), a 9.738(4), b 19.602(4), c 11.636(4) Ǻ, β 99.42(3)°, R 0.0374 for 3667 observed reflections] shows the complex to be an eight-coordinate monomer with three chelating But2pz ligands . The arrangement of centres ( Cen ) of the N-N bonds of the But2pz ligands [< Er -N> 2.336 Ǻ; Cen-Er-Cen 140.1(4)°, 110.3(4)° and 109.6(4)°] and the thf oxygen atoms [< Er -O> 2.351 Ǻ; O- Er -O 140.1(4)°] is intermediate between trigonal bipyramidal and square pyramidal. The other Ln (But2pz)3( thf )2 complexes and Ln (But2pz)3(OPPh3)2 are considered to have similar structures.

Tris [(trimethylsilyl)oxy] antimony

1994 ◽  
Vol 49 (7) ◽  
pp. 855-858 ◽  
Author(s):  
Michael Baier ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Gas Phase ◽  
Structure Determination ◽  
Spectroscopic Data ◽  
Mass Spectrometric ◽  
Unit Cell ◽  
The Other ◽  
X Ray ◽  
Trigonal Bipyramidal

Abstract Tris[(trimethylsilyl)oxy]antimony (Sb(OSiMe3)3, 1) has been prepared from SbCl3 and 3 equiv. of LiOSiMe3 in diethylether. According to mass spectrometric and NMR spectroscopic data, 1 appears to be a monomer in solution and in the gas phase. Dimerisation occurs, however, in the solid state as verified by an X-ray crystal structure determination. The unit cell contains three crystallographically independent monomers, two of which form one type of dimer, while the other is part of a centrosymmetrical dimer. In both types of dimers two Sb atoms are connected via two OSiMe3 groups to form distorted Sb2O2-squares. Together with the remaining 4 OSiMe3 groups and the two stereochemically active lone pairs, each Sb exhibits a trigonal bipyramidal coordination.

scholarly journals Azo-linked corner porphyrin systems: synthesis, crystal structures and spectroscopic investigation

2010 ◽  
Vol 14 (06) ◽  
pp. 481-493 ◽  
Author(s):  
Bruno Bašić ◽  
John C. McMurtrie ◽  
Dennis P. Arnold
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Spectroscopic Investigation ◽  
The Other ◽  
X Ray ◽  
Tert Butyl ◽  
Dinitro Derivative

1,2-bis[10,15-di(3,5-di-tert-butyl)phenylporphyrinatonickel(II)-5-yl]diazene was synthesised via copper-catalyzed coupling of aminated nickel(II) 5,10-diarylporphyrin ("corner porphyrin") and its X-ray crystal structure was determined. Two different crystals yielded different structures, one with the free meso-positions in a trans-like orientation, and the other with a cis-like disposition. The free meso-positions of the obtained dimer have been further functionalized while the synthesis of a zinc analog has so far been unsuccessful. The X-ray crystal structure of the dinitro derivative of the dinickel(II) azoporphyrin was determined, and the structure showed a cis-like disposition of the nitro groups.

scholarly journals Sodium selenite pentahydrate, Na2SeO3·5H2O

2013 ◽  
Vol 69 (11) ◽  
pp. i77-i78 ◽  
Author(s):  
Kurt Mereiter
Keyword(s):  
Crystal Structure ◽  
Sodium Selenite ◽  
Crystal Packing ◽  
Rotation Axis ◽  
The Other ◽  
Octahedral Coordination ◽  
Mirror Plane ◽  
Water Molecules ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

In the crystal structure of Na2SeO3·5H2O [disodium selenate(IV) pentahydrate], two Se, two selenite O atoms and one water O atom are located on a mirror plane, and one water O atom is located on a twofold rotation axis. The coordination of one Na+cation is distorted trigonal bipyramidal, formed by three equatorial H2O ligands and two axial selenite O atoms. The other Na+cation has an octahedral coordination by six water molecules. The two independent SeO3groups form almost undistorted trigonal pyramids, with Se—O bond lengths in the range 1.6856 (7)–1.7202 (10) Å and O—Se—O angles in the range 101.98 (3)–103.11 (5)°, and both are μ2-O:O-bonded to a pair of Na+cations. Hydrogen bonds involving all water molecules and selenite O atoms consolidate the crystal packing. Although anhydrous Na2SeO3and Na2TeO3are isotypic, the title compound is surprisingly not isotypic with Na2TeO3·5H2O. In the tellurite hydrate, all Na+cations have an octahedral coordination and the TeO3groups are bonded to Na+onlyviaone of their three O atoms.

Die Kristallstrukturen von Tetraphenylphosphonium- octahalogenodiarsenat( III) und -diantimonat(III) mit Acetonitril, (PPh4)2[E2X8] · CH3CN (E = As, Sb; X = CI, Br)/The Crystal Structures of Tetraphenylphosphonium Octahalogenodiarsenate (III) and Diantimonate (III) with Acetonitrile, (PPh4)2[E2X8]·CH3CN(E=As, Sb; X=Cl, Br)

1999 ◽  
Vol 54 (2) ◽  
pp. 288-290 ◽  
Author(s):  
Wolfgang Czado ◽  
Susanne Rabe ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
The Other ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
Cl Atoms

(PPh4)2[As2Cl8] · CH3CN was obtained from PPh4Cl and S2Cl2 with As or As4S4 or AsCl3 in acetonitrile. PPh4Cl, S2Cl2 and Sb2S3 yielded (PPh4)[Sb2Cl8] CH3CN. PPh4Br and AsBr3 gave (PPh4)2[Sb2Br8]-CH3CN. AsCl2OPh (from AsCl3 and NaOPh) reacted with Ph4Br in acetonitrile in the presence of Na2Se, selenium, and HCl, affording (PPh4)2[As2Br4,2Cl3,8] · CH3CN. According to their X-ray crystal structure determinations, all products are isotypic (space group C2/c, Z=4). The centrosymmetric anions consist of two ψ octahedra sharing an edge. In the [As2Br4,2Cl3,8]2- ion the bridging positions are taken solely by bromine atoms, whereas Br and Cl atoms occupy the other halogen positions randomly.

Cyclometallated Compounds. IX. Reactions of 2-Benzoylpyridine With Rhodium(III) Trichloride

1995 ◽  
Vol 48 (9) ◽  
pp. 1573 ◽  
Author(s):  
DJ Degeest ◽  
PJ Steel
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
The Other ◽  
Reaction Conditions ◽  
Initial Product ◽  
X Ray ◽  
X Ray Crystallography

X-Ray crystallography and n.m.r. spectroscopy have been used to study the products of reactions between rhodium(III) trichloride and 2-benzoylpyridine under various reaction conditions. X-Ray crystal structures have shown that the initial product of reaction in refluxing ethanol is a centrosymmetric isomer, as previously proposed, but that this undergoes aqueous hydrolysis to a C2-symmetric isomer, rather than the previously proposed C2v isomer. Reaction in refluxing 2-methoxyethanol produces an unusual complex with one C-N cyclometallated ligand and one N-O coordinated ligand. In Me2SO, the non-cyclometallated ligand of this latter compound undergoes solvolysis to produce a complex containing two Me2SO molecules, one coordinated through oxygen and the other through sulfur. The X-ray crystal structure of this compound is also reported.

Synthesis, Spectroscopic Studies, and Crystal Structure of Diethylchlorotin Dimethylphosphinate Et2ClSnO2PMe2

1998 ◽  
Vol 53 (7) ◽  
pp. 699-703 ◽  
Author(s):  
Abdel-Fattah Shihada ◽  
Frank Weller
Keyword(s):  
Crystal Structure ◽  
Spectroscopic Studies ◽  
Chain Structure ◽  
Polymeric Chain ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Axis Of Symmetry ◽  
Ir Bands ◽  
Distorted Trigonal Bipyramidal

Abstract Diethylchlorotin dimethylphosphinate has been synthesized by treating (Et2ClSn)2O with HO2PMe2 in toluene. Single crystal X-ray analysis shows that O2PMe2 groups behave as bidentate bridge ligands between Et2ClSn units leading to a polymeric chain structure in which the tin atoms exhibit a distorted trigonal bipyramidal geometry with the oxygen atoms in the axial positions. The Sn-Cl bond lies on a C2 axis of symmetry in the (C2v) OCClSnCO unit. Et2ClSnO2PMe2 crystallizes in the monoclinic space group C2/c (a = 877.9 (2), b = 1907.8 (4), c = 695.5 (1) pm, β= 106.72 (2)°, Z = 4 and R = 0.043). The characteristic IR bands of Et2ClSnO2PMe2 are assigned and the mass spectrum is reported and discussed.

Sign in / Sign up

Export Citation Format

Share Document