Isoselenocyanatoborate -Kristallstrukturen von (n-Bu4N)[BH(NCSe)3] und (Ph4P)[B3H7(NCSe)] / Isoselenocyanatoborates -Crystal Structures of (n-Bu4N)[BH(NCSe)3] and (Ph4P)[B3H7(NCSe)]

1998 ◽  
Vol 53 (3) ◽  
pp. 271-274 ◽  
Author(s):  
B. Steuer ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Elemental Selenium ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Structure Determinations ◽  
Average Bond

Abstract The treatment of [B6H6]2- with an excess of (SCN)2 in dichloromethane in the presence of solid KOH gives the hexaisoselenocyanatodiborate anion [B2(NCSe)6]2- as an intermediate (δ(11B) = -10.3 ppm), from which [BH(NCSe)3]- and elemental selenium are formed. The X-ray structure determinations on single crystals of (n-Bu4N)2[BH(NCSe)3] (1) (triclinic, space group Pi with a = 8.512(2), b = 10.885(3), c = 14.895(4) Å, α = 79.52(2), β = 74.86(2), γ = 86.768(2)°, Z = 2) and (Ph4P)[B3H7(NCSe)] (2) (monoclinic, space group C2, a = 7.686(5), b = 10.366(3), c = 17.533(3) A, β = 108.89°, Z = 4) show that the selenocyanate groups are coordinated exclusively via the N atoms with average bond lengths of B-N = 1.52, C-N = 1.15, C-Se = 1.75 A and angles N-C-Se = 179°, B-N-C = 168.7 - 176.8°. The N-B-N angles of 1 range from 107.5 to 109.5°.

Kristallstrukturen der iodierten closo-Hexaborate trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P)2[B6H2I4] · 2 CH3CN und (CH2Py2)[B6HI5]/Crystal Structures of the Iodized closo-Hexaborates trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P )2[B6H2I4] · 2 CH3CN and (CH2Py2)[B6HI5]

1998 ◽  
Vol 53 (2) ◽  
pp. 206-210 ◽  
Author(s):  
D. Sonnak ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

Abstract X-ray structure determinations have been performed on single crystals of trans-(Ph4P)2-[B6H4I2] (1) (triclinic, space group P1̄, a = 9.9680(12), b = 10.9690(11), c = 11.0470(14) Å,α = 88.167(9), β = 80.466(12), γ = 68.839(11)°, Z = 1), mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2 (2)(triclinic, space group P1̄, a = 11.8694(11), b = 15.1699(13), c = 17.051(2) Å, α = 75.118(9), β = 71.953(10), γ = 69.331(8)°, Z = 2), trans-(Ph4P )2[B6H2I4] · 2 CH3CN (3) (monoclinic, space group P21/n, a = 14.9665(10), b = 7.6783(10), c = 23.385(3) Å, β = 95.78(9)°, Z = 2), and (CH2Py2)[B6HI5] (4) (orthorhombic, space group Pnma, a = 13.660(2), b = 11.8711(13), c = 13.839(2) Å, Z = 4). The B6 octahedra are compressed in the direction of the B-I bonds, resulting in shortened diagonal B ··· B distances with average values of the groups I-B ··· B-I = 2.37 and I-B ··· B-H = 2.43 Å as compared with H-B ··· B-H = 2.49 Å.

Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX42- (X = Cl, Br, I)/Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX42- Ions (X = Cl, Br, I)

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

Abstract The compounds [(C6H5)4As]2 TeCl4 (1), [(C2H5)4 N]2 TeBr4 · CH3CN (2), and [(C2H5)4N]2TeI4 (3) were prepared by the reaction of Te, X2 , and excess (C2H5)4NX (X = Br, I) in acetonitrile solution or by heating of [(C6H5)4 As]2TeCl6 , Te, and (C6H5)4 ASCl for several hours in the same solvent.The structures of 1-3 were determined from single crystal X-ray data.1 crystallizes in the monoclinic space group P21/n with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, β = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, I4/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te -CI, Te -Br, and Te-I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively.

One-dimensional ribbons of solvated Ag sulfonates

1999 ◽  
Vol 77 (3) ◽  
pp. 313-318 ◽  
Author(s):  
George KH Shimizu ◽  
Gary D Enright ◽  
Gabriela S Rego ◽  
John A Ripmeester
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
The Other ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Structure Determinations

Single crystal X-ray structure determinations of two solvated silver sulfonates have been obtained and these compounds have been shown to adopt infinite one-dimensional motifs. {AgOTs(MeCN)}[Formula: see text] (OTs = p-toluenesulfonate) crystallizes in the monoclinic space group, P21, a = 8.4278(5) Å, b = 5.7413(3) Å, c = 12.1057(7) Å, β = 109.24(1)°. {Ag(NDSA)(MeCN)2(H3O)(H2O)2}[Formula: see text] (NDSA = 1,5-naphthalenedisulfonate) crystallizes in the triclinic space group, P[Formula: see text], a = 8.3407(4) Å, b = 10.4374(5) Å, c = 12.3399(6) Å, α = 101.941(8)°, β = 109.24(1)°, γ = 102.190(8)°. Despite one compound containing a monosulfonate and the other a disulfonate, both complexes form infinite one-dimensional arrays.Key words: silver, sulfonates, coordination polymer.

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.

Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalysen von trans-[PtX2(acac)2], X = CI, Br, I, SCN / Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of trans-[PtX2(acac)2], X = Cl, Br, I, SCN

1996 ◽  
Vol 51 (10) ◽  
pp. 1400-1406 ◽  
Author(s):  
D. Rickert ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Normal Modes ◽  
Force Constants ◽  
Monoclinic Space Group ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Valence Force ◽  
Space Group ◽  
X Ray ◽  
Modes Of Vibration

The crystal structures of trans-[PtCl2(acac)2](monoclinic, space group P21/c, a - 7.616(5), b = 12.759(5), c = 7.892(5) Å, β = 118.459(5)°, Z = 2), trans-[PtBr2(acac)2] (triclinic, space group P1̅, a = 7.502(5), b = 7.665(5), c = 8.155(5) Å, α = 114~508(5), β = 94.537(5), γ = 117.669(5)°. Z = 1) and trans-[Pt(SCN)2(acac)2] (triclinic, space group P1̅ , a = 7.9095(10), b = 7.9393( 10), c = 7.9631 Å, a = 114.051 (10), β = 100.955(10), γ = 100.573(10)°, Z = 1) have been determined by single crystal X-ray diffraction analysis. The crystal structure of trans- [Ptl2(acac)2] is known from the literature. To enhance the spectroscopic resolution, the IR and Raman spectra of the four complexes have been measured at low temperature (10 K). Using the X-ray data, normal coordinate analyses based on a modified valence force field have been performed and the normal modes of vibration for the octahedral skeleton [PtX2O4] have been assigned. With a set of 19 or 23 force constants taking into account the inner-ligand vibrations a good agreement between observed and calculated frequencies has been achieved. The valence force constants are e.g.fd (PtCl) = 2.16, fd (PtBr) = 1.45, fd (PtI) = 1.01, fd (PtS) = 1.80 mdyn/Å, and fd (PtO) ranges from 1.89 to 1.91 mdyn/Å.

Die Kristallstrukturen von Ph3AsCI2 und β-Ph3AsBr2 / Crystal Structures of Ph3AsCI2 and β-Ph3AsBr2

1999 ◽  
Vol 54 (12) ◽  
pp. 1611-1614 ◽  
Author(s):  
Bernhard Neumüller ◽  
Soheila Chitsaz ◽  
Kurt Dehnicke
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Arsenic Atom ◽  
Space Group ◽  
X Ray ◽  
Halogen Atoms ◽  
Structure Determinations ◽  
Acetonitrile Solutions

Colourless single crystals of Ph3AsCl2 as well as of β-Ph3AsBr2 were obtained from acetonitrile solutions and were suitable for X-ray structure determinations. Ph3AsCl2: Space group P212121, Z = 4, lattice dimensions at -90 °C: a = 1247.9(2), b = 1267.5(1), c = 1033.4(1) pm, R x = 0.0484.β-Ph3AsBr2: Space group P1̄ , Z = 4, lattice dimensions at -80 °C: a = 949.1(1), b = 1189.7(1), c = 1693.7(2) pm, a = 98.32(1)°, ß = 103.64(1)°, γ = 109.44(1)°, R x - 0.0628. The structures consist of Ph3AsX2 molecules (X = Cl, Br) with trigonalbipyramidal coordination of the arsenic atom with the halogen atoms in the axial positions.

Darstellung, Schwingungsspektren und Normalkoordinatenanalyse von bindungsisomeren Halogenoselenocyanatorhenaten(IV) sowie Kristallstrukturen von mer-(Ph4P)2[ReCl3(NCSe)2cis (SeCN)] und mer-(n-Bu4N)2[ReCl3I(NCSe)2cis] / Synthesis, Vibrational Spectra and Normal Coordinate Analysis of Linkage Isomeric Halogenoselenocyanatorhenates(IV) and Crystal Structures of mer-(Ph4P)2[ReCl3(NCSe)2cis (SeCN)] and mer-(n-Bu4N)2[ReCl3I(NCSe)2cis]

1999 ◽  
Vol 54 (10) ◽  
pp. 1222-1228 ◽  
Author(s):  
S. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Exchange Chromatography ◽  
Normal Coordinate Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Diethylaminoethyl Cellulose

By treatment of fac-[ReCl3I3]2- with (SeCN)2 indichloromethane fac-[ReCl3(NCSe)3]2- (1), mer-[ReCl3(NCSe)2cis (SeCN)]2- (2) and mer-[ReCl3I(NCSe)2cis]2- (3) are formed which have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of mer-(Ph-P)2[ReCl3(NCSe)2cis(SeCN)] (triclinic, space group Pl̅, a = 16.099(1), b = 16.729(3), c =21.026(2) Å, α = 70.194(10), ß = 73.958(10), γ = 83.929(10)°, Z = 4) and mer-(n-Bu4N)2[ReCl3|(NCSe)2cis] (monoclinic, space group P21/c, a = 11.838(1), b = 12.796(2), c = 30.767(2) Å, ß = 97.419(6)°, Z = 4) have been determined by single crystal X-ray diffraction analysis. Based on the molecular parameters of the X-ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts have been assigned by normal coordinate analysis. The valence force constants are fd(ReN) = 1.79 (1), 1.71 (2), 1.71 (3) and fd(ReSe) = 1.15 (2) mdyn/Å.

scholarly journals Kristallstrukturen der Tetrachloroniccolate (PPh4)2[NiCl4] und [Na-15-Krone-5]2[NiCl4] / Crystal Structures of the Tetrachloroniccolates (PPh4)2[NiCl4] and [Na- 15-Crown-5]2[NiCl4]

1990 ◽  
Vol 45 (7) ◽  
pp. 995-999 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Ulrich Müller
Keyword(s):  
Crown Ether ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Sodium Ions ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Cl Atoms

The title compounds were obtained from NiS + PPh4Cl + HCl in dichloromethane, from NiCl2 and PPh4Cl and from NiCl2 + Na2S + 15-crown-5 in acetonitrile or CH2Cl2, respectively. Their crystal structures were determined by X-ray diffraction. (PPh4)2[NiCl4]: monoclinic, space group C 2/c, Z = 4, a = 1094.9(3), b = 1946.1(4), c = 2033.5(5) pm, β = 91.48(3)°; R = 0.07 for 2895 unique observed reflexions. [Na-15-crown-5]2[NiCl4]: triclinic, space group P1̄, Z = 2, a = 987.6(1), b = 998.0(1), c = 1779.9(2) pm, α = 104.17(1), β = 95.43(1), γ = 109.95(1)°; R = 0.090 for 4155 unique observed reflexions. In both cases, the [NiCl4]2- ions have distorted tetrahedral structures. With PPh4+ as the cation the distortion corresponds to a twisted tetrahedron which fulfils the point symmetry D2, the deviation from a flattened D2d-tetrahedron being small. In (PPh4)2[NiCl4] cations and anions alternate in layers parallel to (001). In [Na-15-crown-5]2[NiCl4] two of the Cl atoms of the anion are coordinated to sodium ions; one of the crown ether molecules shows positional disorder.

Kristallstrukturen, Schwingungsspektren und Normalkoordinaten- analysen von cis- und trans-[OsX2(acac)2], X = Cl, Br, I / Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of cis- and trans-[OsX2(acac)2], X = Cl, Br, I

1997 ◽  
Vol 52 (8) ◽  
pp. 965-974 ◽  
Author(s):  
K Dallmann ◽  
W Preetz
Keyword(s):  
Crystal Structures ◽  
Normal Modes ◽  
Force Constants ◽  
Monoclinic Space Group ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Valence Force ◽  
Space Group ◽  
X Ray ◽  
Modes Of Vibration

The crystal structures of trans-[OsCl2(acac)2] (triclinic, space group P1̄, a = 7.4114(5), b = 7.6419(9), c = 7.9944(6) Å, α = 62.692(7), β = 87.687(6), γ = 60.667(6)°, Z = 1), trans-[OsBr2(acac)2] (triclinic, space group P1̄, a = 7.467(3), b = 7.621(3), c = 8.260(3) Å, α = 115.03(3), β = 92.78(3), γ = 117.91(3)°, Z = 1), cis-[OsCl2(acac)2] (monoclinic, space group C2/c, a = 13.8532(13), b = 7.7990(8), c = 13.6202(12) Å, β = 108.375(10)°, Z = 4) and cis-[OsBr2(acac)2] (monoclinic, space group C2/c, a = 13.944(2), b = 8.0347(13), c = 13.743(2) Å, β = 106.757(12)°, Z = 4) have been determined by single crystal X-ray diffraction analysis. To enhance the spectroscopic resolution, the IR and Raman spectra of the six complexes have been measured at low temperature (10 K). Using the molecular parameters of the X-ray determinations normal coordinate analyses based on a modified valence force field have been performed for trans-[OsCl2(acac)2], trans-[OsBr2(acac)2] and cis-[OsCl2(acac)2], and the normal modes of vibration assigned. With sets of 31 or 32 force constants, taking into account the innerligand vibrations, a good agreement between observed and calculated frequencies has been achieved. The valence force constants for the X-Os-X axes are fd(OsCl) = 1.81, fd(OsBr) =1.61 mdyn/Å, and for the Cl′-Os-O* axis are fd(OsCl’) = 1.94, fd(OsO*) = 2.81 mdyn/Å and fd(OsO) ranges from 3.27 to 3.31 mdyn/Å.

Kristallstrukturen, Schwingungsspektren und Normalkoordinaten- analysen von trans-[OsO2(ox)2]2– und trans-[OsO2(mal)2]2–/ Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of trans-[OsO2(ox)2]2– and trans -[OsO2(mal)2]2–

1998 ◽  
Vol 53 (8) ◽  
pp. 823-828 ◽  
Author(s):  
A. Strueß ◽  
W. Preetz
Keyword(s):  
Crystal Structures ◽  
Vibrational Spectra ◽  
Room Temperature ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Ir And Raman

Abstract The crystal structures of trans-(Ph4P)2[OsO2(ox)2] (monoclinic, space group P21/n, a = 12.281(2), b = 14.5440(13), c = 13.9810(12) Å, β = 100.000(8)°, Z = 2) and trans- (n-Bu4N)2[OsO2(mal)2] (triclinic, space group P1̄, a = 10.365(4),b = 10.707(3), c - 11.473(5) A, a = 73.00(2), β = 64.44(3), 7 = 82.55(3)°, Z = 1) have been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra of these complexes were measured at room temperature. Based on the molecular parameters of the X-ray determinations normal coordinate analyses have been performed and the vibrations assigned. The valence force constants of [OsO2(ox)2]2- are fd(Os=O) = 6.7, fd(Os-O) = 2.9, fd(C-O) = 5.05, fd(C=O) = 11.2 and fd(C-C) = 4.7 mdyn/Å and of [OsO2(mal)2]2- fd(Os=O) = 6.7, fd(Os-O) = 2.9, fd(C-O) = 4.86, fd(C=O) =11.1 and fd(C-C) = 4.07 mdyn/Å.

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