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.

Organoamido- and Aryloxo-lanthanoids. IX. Preparations and Structures of Tris(η2-3,5-diphenyl-pyrazolato)lanthanoid(III) Complexes With Triphenylphosphine Oxide and Tetrahydrofuran

1993 ◽  
Vol 46 (12) ◽  
pp. 1881 ◽  
Author(s):  
JE Cosgriff ◽  
GB Deacon ◽  
BM Gatehouse
Keyword(s):  
Crystal Structure ◽  
Triphenylphosphine Oxide ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Oxygen Donor ◽  
Neodymium Complex ◽  
Cell Data

From reaction of lanthanoid metals with bis ( pentafluorophenyl )mercury and 3,5-diphenylpyrazole (HPh2pz) in 1,2-dimethoxyethane ( dme ) and treatment of the products with triphenylphosphine oxide, the complexes [ Ln (η2-Ph2pz)3(OPPh3)2].( dme )n ( Ln = Er or Nd , n = 1; Ln = La, n = 0.6) have been isolated. An X-ray crystal structure shows that the erbium complex [monoclinic, space group C2, a 22.08(3), b 14.30(1), c 13.37(1) Ǻ, β 124.09(7)°, Z 2 2730 'observed' data refined to R 0.046] is monomeric , with eight coordination of the metal. There is a trigonal bipyramidal arrangement of the centre ( Cen ) of the N-N bonds of three η2-3,5-diphenylpyrazolate groups ( ΣCen-Er-Cen 360°; ( Er -N) 2.344 Ǻ) and the oxygens of two equivalent trans triphenylphosphine oxide ligands [O- Er -O 176(1)°; Er -O 2.207(9)Ǻ]. Unit cell data indicate that the neodymium analogue [monoclinic, space group C2, a 23.01(3), b 14.94(2), c 13.82(2) Ǻ, β 123.65(8)°] is isostructural with the erbium complex. An analogous reaction of lanthanum or neodymium metal, Hg(C6F5)2, and HPh2pz in tetrahydrofuran ( thf ) gives [ Ln (η2-Ph2pz)3( thf )3]. thf ( Ln = La or Nd ). The X-ray crystal structure of the neodymium complex [orthorhombic, space group P212121, a 14.009(9), b 16.280(8), c 22.640(16)Ǻ, Z 4, 2967 'observed' data refined to R 0.046 reveals a nine-coordinate monomer with three η2-Ph2pz ligands [ Nd -N 2.420(10)-2.524(8)Ǻ] and three thf ligands [ Nd -O 2.497(8)-2.587(8)Ǻ]. There is a trigonal prismatic arrangement of the centres of the N-N bonds and the oxygen donor atoms.

Oxotetrafluoro-vanadate(V): Die Kristallstruktur von [enH2] [VOF4(H2O)]2.

1976 ◽  
Vol 31 (5) ◽  
pp. 541-543 ◽  
Author(s):  
Helmut Rieskamp ◽  
Rainer Mattes
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Space Group ◽  
X Ray ◽  
In Trans ◽  
Oxygen Atoms

The crystal structure of [enH2][VOF4(H2O)]2 has been determined from X-ray diffractometer data. Crystals are monoclinic, space group C2/c with Z = 4 in a unit cell of dimensions a = 16.576(13), b = 7.781(4), c = 10.338(8) Å, β = 120.0(1)°.The structure was refined by least-squares methods to R 0.053 for 1436 reflections. The structure contains monomeric [VOF4(H2O)]⁻-ions with the oxygen atoms in trans position. The bond distances are 1.577 Å (terminal oxygen) and 2.333 Å (H2O molecule), resp. The V–F distances vary between 1.769(2) and 1.858(2) Å for fluorine atoms involved in strong hydrogen bonds.

Stereospecific reactions of aryltellurium(IV) trichlorides with 3-cyclohexene-1-methanol and 3-cyclohexene-1,1-dimethanol: the X-ray crystal structure of 2′,4′-dimethoxyphenyl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichloride

1995 ◽  
Vol 73 (2) ◽  
pp. 255-263 ◽  
Author(s):  
Bozena Borecka ◽  
T. Stanley Cameron ◽  
M. Azad Malik ◽  
Barry C. Smith
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Lone Pair ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Compound C ◽  
Stereospecific Reactions

Aryltellurium(IV) trichlorides react with 3-cyclohexene-1-methanol and 3-cyclohexene-1,1-dimethanol to give aryl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichlorides and aryl(cis-1-hydroxymethyl-trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichlorides. The structure of 2′,4′-dimethoxyphenyl(trans-6-oxabicyclo[3.2.1]oct-4-yl)tellurium(IV) dichloride has been determined by single crystal X-ray analysis. The compound C15H20Cl2O3Te, Mr = 446.8, crystallizes in the monoclinic space group P21/c with a = 9.626(2) Å, b = 15.768(5) Å, c = 11.176(3) Å, β = 92.08(1)°, V = 1695.2(5) Å3 and D(calc) = 1.751 for Z = 4. Tellurium is bonded axially to two chlorines and equatorially to aryl carbon and carbon from the cyclohexyl portion of oxabicyclo[3.2.1]oct-4-yl in a pseudo-trigonal-bipyramidal arrangement having an equatorial lone pair of electrons. Bond lengths are Te—Cl(1) = 2.492(3) Å, Te—Cl(2) = 2.539(3) Å, Te—C(4) = 2.175(10) Å, and Te—C(9) = 2.090(10) Å. Keywords: organotellurium(IV), 3-cyclohexene-1-methanol, 3-cyclohexene-1, 1-dimethanol.

Darstellung und Kristallstruktur von Zinkazid · 4-Methylpyridin / Preparation and Crystal Structure of Zinc Azide · 4-Methylpyridine

1988 ◽  
Vol 43 (3) ◽  
pp. 253-256 ◽  
Author(s):  
Franz A. Mautner ◽  
Harald Krischner ◽  
Christoph Kratky
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Single Crystal ◽  
Zinc Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

Zinc azide · 4-methylpyridine (1) is formed by the reaction of zinc azide with the corresponding pyridine in aqueous solution. The crystal structure was determined by single crystal X-ray diffraction methods. The crystals of 1 are monoclinic, space group C2/c, Z = 4, a = 1085.5(2), b = 1692.7(11), c = 619.7(6) pm, β = 113.47(5)°. Each zinc atom is surrounded by five nitrogen atoms (four from azide groups and one from the pyridine adduct) in a distorted trigonal bipyramidal fashion. The ZnN5-polyhedra share common edges to form chains along the crystallographic c-axis.

Die Kristallstruktur von Te6O11Cl2 / The Crystal Structure of Te6O11Cl2

1981 ◽  
Vol 36 (4) ◽  
pp. 405-409 ◽  
Author(s):  
Walter Abriel
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Trigonal Bipyramidal Coordination ◽  
Trigonal Bipyramidal ◽  
Oxygen Atoms

Abstract Crystals of the title compound are monoclinic (space group P21/m) with a = 6.844(4) Å, 6 = 6.800(4) Å, c= 15.227(9) Å, y= 120.19° and Z = 2. The structure contains infinite cationic [(Te12O22) 4+]∞ -chains with three different sites for tellurium. There are three oxygen atoms in a y-tetrahedral arrangement around Te 1, and four oxygen atoms in a ψ-trigonal-bipyramidal coordination around Te 2 and Te 3.

Synthese und Kristallstruktur von (Cu,Zn)3,75Mo3O12 / Synthesis and Crystal Structure of (Cu,Zn)3,75Mo3O12

1995 ◽  
Vol 50 (2) ◽  
pp. 247-251 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Single Crystals ◽  
The Other ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Occupancy Factor ◽  
X Ray ◽  
Group D ◽  
Oxygen Atoms

Single crystals of (Cu,Zn)3,75Mo3O12 have been prepared by crystallization from melts and investigated by X-ray diffractometer techniques. (Cu,Zn)3,75Mo3O12 crystallizes orthorhombically, space group D24-P212121, Z = 4, a = 17.947(9), b = 5.092(3), c = 10.685(5) Å. It is isotypic to Cu3,85Mo3O12. All molybdenum atoms are tetrahedrally coordinated by oxygen atoms. There are layers of CuO6 and ZnO6 octahedra, while other metal sites are occupied by copper in a deformed prismatic coordination with one oxygen atom at a remarkably greater distance from copper than the other five. Some of the zinc atoms occupy positions in chains of face-sharing octahedra with an occupancy factor of 0.75. The crystal structure is discussed with respect to the isotypic compound Cu3,85Mo3O12 and compounds of the type CuLnMo2O8.

Complexes of 1,2,4-Triazoles, Part XVII The Crystal Structure of Tris-μ-(4-ethyl-1,2,4-triazole-N1,N2)- (4-ethyl-1,2,4-triazole-N1)-aquo-bis [bis(thiocyanato-N)- nickel(II)]hydrate, Ni2(C4N3H7)4(H2O)(NCS)4 ·H2O(x ≃ 2.5)

1981 ◽  
Vol 36 (7) ◽  
pp. 809-813 ◽  
Author(s):  
Ger Vos ◽  
Anthonie J. de Kok ◽  
Gerrit C. Verschoor
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
The Other ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Coordinated Water

Abstract The crystal structure of Ni2(C4N3H7)4(H2O)(NCS)4 · 2.5 H2O has been determined by X-ray diffraction techniques. The compound crystallizes in the monoclinic space group P21/n with a = 15.121(4), b= 13.237(2), c= 18.069(3), β = 94.71(2)° and Z = 4; R = 0.040 (Rm = 0.051). The compound consists of dimeric units in which two Ni ions are bridged by three ethyltriazole (Ettrz) groups. For one Ni, two N donating NCS- groups and an Ettrz coordinating by only one N atom complete the NiNe octahedron. The other Ni atom, which is also octahedrally coordinated, has a coordinated water molecule instead of a monodentate Ettrz.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

Structure of 3α,4α:5β,6β-Diepoxyandrostan-17-one

1983 ◽  
Vol 36 (11) ◽  
pp. 2333 ◽  
Author(s):  
B Kamenar ◽  
RA Pauptit ◽  
JM Waters
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray

The X-ray crystal structure of 3α,4α:5β,6β-diepoxyandrostan-17-one has been determined. Crystals of the title compound (C19H26O3)are monoclinic, space group P21, with a 9.208(2), b 9.620(4), c 9.312(3) �, β 99.14(2)�, V 814.5 Ǻ3 and Z 2. The structure was solved by direct methods and refined to R 0.039 for 887 observed reflexions. The 3α,4α:5β,6β configuration of the epoxide rings confirms the assignment based on proton n.m.r. studies.

Darstellung von Mononitropentahydrohexaborat(2-) und Kristallstruktur von M2[B6H5(NO2)], M = K, Cs / Preparation of Mononitropentahydrohexaborate(2—) and Crystal Structure of M2[B6H5(NO2)], M = K, Cs

1993 ◽  
Vol 48 (12) ◽  
pp. 1727-1731 ◽  
Author(s):  
A. Franken ◽  
W. Preetz ◽  
M. Rath ◽  
K.-F. Hesse
Keyword(s):  
Crystal Structure ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By electrochemical oxidation of [B6H6]2- in the presence of nitrite ions and the base DBU in dichloromethane solution mononitropentahydrohexaborate [B6H5(NO2)]2- ions are formed and can be isolated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of the K and Cs salt were determined from single crystal X-ray diffraction analyses. K2[B6H5(NO2)] is monoclinic, space group P21/m with a = 5.953(1), b = 8.059(4), c = 8.906(1) Å, β = 109.553(9)°; Cs2[B6H5(NO2)] is monoclinic, space group P21/a with a = 9.438(6), b = 9.644(7), c = 11.138(9) Å, β = 101.44(9)°. The B6 octahedron is compressed in the direction of the B—NO2 bond by about 5%, with bond lengths between 1.67 and 1.77 A.

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