Preparation and Crystal Structure of Na4TiSe4. A Selenotitanate with Discrete Tetrahedral Anions

2000 ◽  
Vol 55 (1) ◽  
pp. 39-44 ◽  
Author(s):  
Kurt O. Klepp
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Monoclinic Space Group ◽  
Tetrahedral Complex ◽  
Space Group ◽  
Distorted Octahedral ◽  
Intimate Mixture ◽  
New Type ◽  
Complex Anions

Red crystals of Na4TiSe4 were obtained by reacting an intimate mixture of Na2Se, Ti and Se at 750°C. Na4TiSe4 is monoclinic, space group I2/a with a = 24.027(6), b = 7.346(4), c = 21.572(6) Å, (β = 104.52(2)°, Z = 16. Its crystal structure was determined from diffractometer data (AgK α-radiation) and refined to a conventional R of 0.036 for 2673 F0′s and 158 variables. The crystal structure is of a new type, characterized by the presence of discrete tetrahedral complex anions, [TiSe4]4- , which are arranged in slabs parallel to (100). The average Ti-Se bond length is 2.385(1) Å. The Na+ cations are in different chalcogen environments with distorted octahedral, square pyramidal or planar configurations, respectively

Darstellung und Kristallstruktur von Na4Ga2S5. Ein Thiogallat mit -Zweier-Doppelketten / Preparation and Crystal Structure of Na4Ga2S5. A Thiogallate with --zweier-Double Chains

1992 ◽  
Vol 47 (7) ◽  
pp. 937-941 ◽  
Author(s):  
Kurt O. Klepp
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Single Crystals ◽  
Monoclinic Space Group ◽  
Alkali Cations ◽  
Space Group ◽  
Distorted Octahedral ◽  
New Type

Transparent single crystals of Na4Ga2S5 were obtained from a melt of Na2S, Ga and S. Na4Ga2S5 is monoclinic, space group P21/c with a = 7.967(1), b = 6.133(2), c = 19.852(9) Å, β = 91.61(2)°, Ζ = 4. Its crystal structure was refined to a conventional R of 0.033 for 1150 observed reflections.The structure of Na4Ga2S5 is of a new type. It is characterized by infinite ribbon like thiogallate anions, -, which are built up by GaS4-tetrahedra (mean Ga-S bond length 2.28 A) sharing apices and edges. The four crystallographically independent alkali cations are coordinated to six sulphur atoms in distorted octahedral configurations.

Nitrido-und Oxochlorokomplexe des Vanadiums(V); die Kristallstruktur von AsPh4 [V0C14] Nitrido and Oxochloro Complexes of Vanadium(V); the Crystal Structure of AsPh4[VOCl4]

1980 ◽  
Vol 35 (5) ◽  
pp. 522-525 ◽  
Author(s):  
Gisela Beindorf ◽  
Joachim Strähle ◽  
Wolfgang Liebelt ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Bond Length ◽  
Bond Angle ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Linear Arrangement ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

The complexes AsPh4[Cl4V = N-Cl] and AsPh4[VOCl4] are prepared by the reaction of AsPh4Cl with Cl3VNCl and VOCl3, respectively. The IR spectra indicate C4v symmetry for the complex anions with multiple VN and VO bonds and a linear arrangement for the VNCl-group. AsPh4[VOCl4] crystallizes in the tetragonal space group P4/n with two formula units in the unit cell. The crystal structure was solved by X-ray diffraction methods (R = 0,062, 1096 observed, independent reflexions). The structure consists of AsPh4+ cations and [VOCl4]- anions with symmetry C4v. The extremely short VO bond length corresponds with a VO triple; its steric requirements cause the relatively large bond angle OVCl of 103.4°.

scholarly journals Serendipitous formation and characterization of K2[Pd(NO3)4]·2HNO3

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Solvothermal Process ◽  
X Ray Diffraction ◽  
Glass Ampoule ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.

scholarly journals Die Kristallstruktur des Silbertetrachloroaurats(III) AgAuCl4 und seine kristallchemische Verwandtschaft zum Rubidiumtetrachloroaurat(III) RbAuCl4 / The Crystal Structure of Silver Tetrachloroaurate(III) AgAuCl4 and its Crystal Chemical Relationship to the Rubidium Tetrachloroaurate(III) RbAuCl4

1977 ◽  
Vol 32 (7) ◽  
pp. 741-744 ◽  
Author(s):  
Walther Werner ◽  
Joachim Strähle
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Octahedral Coordination ◽  
Monoclinic Space Group ◽  
Crystal Chemical ◽  
Space Group ◽  
Square Planar ◽  
Cl Atoms

AgAuCl4 crystallizes in the monoclinic space group I2/c with Zi = 4. The crystal structure is built up by Ag+ cations and square planar AuCl4⁻ anions with Au-Cl bond length of 228 pm. The Ag+ ions have an octahedral coordination of Cl atoms. AgAuCl4 is topologically related to RbAuCl4.

The crystal structure of Bis[2-(pyridin-2-ylamino)-4-(pyridin-2-yl)thiazole]iron(II) Bis(tetrafluoroborate) trihydrate

1984 ◽  
Vol 37 (2) ◽  
pp. 443 ◽  
Author(s):  
AT Baker ◽  
HA Goodwin ◽  
AD Rae
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Complex Cation ◽  
Monoclinic Space Group ◽  
Octahedral Structure ◽  
Space Group ◽  
X Ray ◽  
Disordered Structure ◽  
Distorted Octahedral ◽  
A Cell

The crystal structure of an iron(II) complex of 2-(pyridin-2-ylamino)-4-(pyridin-2-yl)tliazoe (paptH) has been determined by single-crystal X-ray diffractometry. [Fe(paptH)2] [BF4]2.3H2O is monoclinic, space group P21/c, with Z = 4 in a cell of dimensions a 8.968(6), b 9.038(4), c 41.15(2)�, β 94.81(2)�. The disordered structure was refined to a residual R 0.0826 for 2549 observed reflections. The ligands and anions are orientationally disordered, and the waters of crystallization are positionally disordered. Comprehensive constrained refinement, with 220 parameters for 139 atom positions, produced reliable geometry. The complex cation has a distorted octahedral structure of meridional configuration with both paptH ligands functioning as tridentates.

The preparation and X-ray crystal structure of Te(N3)3SbF6 containing the triazidotellurium(IV) cation, Te(N3)3+

1989 ◽  
Vol 67 (11) ◽  
pp. 1687-1692 ◽  
Author(s):  
James P. Johnson ◽  
Gregory K. MacLean ◽  
Jack Passmore ◽  
Peter S. White
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Angles ◽  
X Ray Crystallography ◽  
Distorted Octahedral ◽  
Average Bond

The crystal structure of Te(N3)3SbF6 containing the first binary tellurium–nitrogen cation, triazidotellurium(IV) (Te(N3)3+), has been determined by X-ray crystallography. Single crystals of Te(N3)3SbF6 are monoclinic, space group P21/c with a = 9.201(6), b = 8.445(4), c = 13.582(7) Å, β = 100.36(5)°, Z = 4, final R1 = 0.036 for 1286 observed reflections. The structure consists of discrete Te(N3)3+ cations and distorted octahedral SbF6− anions, with some cation–anion interactions. The average Te—Nα—Nβ—Nγ bond distances in Te(N3)3+ are Te—Nα, 1.994(7); Nα—Nβ, 1.237(11); and Nβ—Nγ, 1.116(12) Å. The average bond angles about the Te, Nα, and Nβ atoms are 94.1(3)°, 116.5(6)°, and 173.7(9)°. Structural correlations with other TeX3+ species have yielded an estimate of the electronegativity of the N3− group to be 3.1 ± 0.1. Keywords: tetratellurium (2+) cation, triazidotellurium(IV) cation, electronegativity, azide.

The Crystal Structure of (2,2′-Bipyridine)(pyrazine)(2,2′:6′,2″-terpyridine)ruthenium(II) Hexafluorophosphate

1996 ◽  
Vol 49 (4) ◽  
pp. 527 ◽  
Author(s):  
PT Gulyas ◽  
TW Hambley ◽  
PA Lay
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Steric Strain ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Distorted Octahedral ◽  
Back Bonding

The crystal structure of [ Ru ( terpy )( bpy )( pz )] (PF6)2 has been determined by X-ray diffraction methods and refined to a residual of 0.046 for 1855 independent observed reflections. The crystals are monoclinic, space group P 21/a, a 16.836(7), b 10.778(5), c l9.342(5) Ǻ, β 115.11(3)°. The coordination geometry around the ruthenium(II) ion is distorted octahedral, with the various Ru -N bond lengths indicative of considerable interligand steric strain. The Ru -N pyrazine bond is the longest within the structure, consistent with other evidence that n back-bonding to pyrazine is weak in the complex.

K2TiS3, ein neues Thiotitanat(IV) mit fünffach koordiniertem Titan / K2TiS3, A New Thiotitanate(IV) with Pentacoordinate Titanium

1992 ◽  
Vol 47 (2) ◽  
pp. 201-204 ◽  
Author(s):  
Kurt O. Klepp
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Compound K ◽  
Space Group ◽  
One Dimensional ◽  
Atomic Arrangement ◽  
New Type

Fibrous red crystals of the new compound K2TiS3 were obtained by reacting K2S, Ti and S at 1070 K. K2TiS3 is monoclinic, space group C 2/c with a = 11.667(6) Å, b = 8.325(4) Å, c = 6.494(4) Å, β = 9 i.81(4)°, Z = 4. The crystal structure was refined to a conventional residual of 0.070. The atomic arrangement is characterized by pseudo-one-dimensional -∞-[TiS3]2− chains formed by distorted TiS5 square pyramids sharing opposite edges of their basal planes. The structure - though closely related to that of Cs2TiS3 - is of a new type.

Kristallstruktur von Triphenylmethyliodsulfan (C6H5)3CSI [1] / Crystal Structure of Triphenylmethyliodosulfane (C6H5)3 CSI [1]

1988 ◽  
Vol 43 (4) ◽  
pp. 399-402 ◽  
Author(s):  
Rolf Minkwitz ◽  
Hans Preut ◽  
Jürgen Sawatzki
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Space Group

Abstract The crystal structure of (C6H5)3CSI is reported. It is the first structure determination of an iodine sulfane. (C6H5)3CSI crystallizes in the monoclinic space group P21/c with a - 1226.4(7) pm, b = 1398.8(18) pm, c = 941.6(8) pm, β = 96.38(8)° and Z = 4. The sulfur-iodine bond length is 240.6(4) pm corresponding to the sum of the covalent radii with 237 pm. The molecules are linked via short I···S contacts of 321.0(4) pm such that a zig-zag chain is formed.

Komplexe Chalkogenide der IVa Metalle mit niedrigdimensionalen anionischen Partialstrukturen. Darstellung und Kristallstruktur von K2ZrTe3 und Rb2ZrTe3 / Complex Chalcogenides of the IVa Metals with Low Dimensional Anionic Partial Structures. Preparation and Crystal Structures of K2ZrTe3 and Rb2ZrTe3

1999 ◽  
Vol 54 (4) ◽  
pp. 441-446 ◽  
Author(s):  
Kurt O. Klepp ◽  
Andreas Kolb
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Alkali Cations ◽  
Space Group ◽  
Bond Lengths ◽  
Partial Structures ◽  
Distorted Octahedral ◽  
New Type ◽  
The Mean ◽  
Low Dimensional

The isostructural compounds K2ZrTe3 and Rb2ZrTe3 were obtained at 1000°C by reacting K2Te and Rb2Te with stoichiometric amounts of Zr and Te. The compounds are monoclinic, mP24, space group P21/c, Z = 4 with a = 9.089(3), b = 14.148(4), c = 6.986(3) Å, β = 105.90( 1)° and a = 9.735(4), b = 14.300(7), c = 6.952(8) Å, β = 108.61(2)°, respectively. The crystal structure was determined from diffractometer data and refined to R = 0.030 for 1452 Fo's for K2ZrTe3 and R = 0.038 for 1131 Fo's for Rb2ZrTe3. The crystal structure is of a new type, characterized by infinite anionic chains, 1∞-[ZrTe3]2- built up by octahedra sharing opposite faces which run along [001]. The mean Zr-Te bond lengths are 2.921 and 2.920 Å, respectively. The alkali cations separating the chains are characterized by two different - distorted octahedral and pentagonal bipyramidal - chalcogen environments.

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