Metall-Komplexe mit S4N4 -Liganden: Die Strukturen von zwei Komplexen der Zusammensetzung [TiCl4(S4N4)]2 / Metal Complexes with S4N4 Ligands: The Structures of Two Complexes of Composition [TiCl4(S4N4)]2

1988 ◽  
Vol 43 (4) ◽  
pp. 467-471 ◽  
Author(s):  
Ulf Thewalt ◽  
Konrad Holl
Keyword(s):  
Crystal Structure ◽  
Metal Complexes ◽  
Dinuclear Complexes ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Bridging Ligands ◽  
Space Group ◽  
Slow Reaction ◽  
Orange Yellow ◽  
Monodentate Ligands

AbstractSlow reaction of TiCl4 with S4N4 in CH2Cl2/CCl4 produces a mixture of two crystalline dinuclear complexes of composition [TiCl4(S4N4)]2. Crystal data for the orange-yellow α-isomer: mono­clinic, space group P21/n with a = 11.608(3) Å. b = 8.304(3) Å, c = 10.938(5) Å, β = 101.06(4)° and Z = 2. Crystal data for the red-brown β-isomer: monoclinic, space group P21/c with a = 11.220(2) Å, b = 13.868(2) Å, c = 14.839(4) Å, β = 106.18(2)° and Z = 4. Crystal structure analyses reveal that the S4N4 molecules in the α-form act as 1,3-N,N′-bonded bridging ligands and in the β-form as N-bonded monodentate ligands.

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

Untersuchungen an Polyhalogeniden, XXXVI. Zur Kenntnis des Oktaiodid-Ions I82-: Darstellung und Kristallstruktur des [(Crypt-2.2.2)H2]l8, des [Ni(phen)3]I8 · 2CHCl3 und der Bis(N-alkylurotropinium) oktaiodide (UrR)2I8 mit R = Methyl und Ethyl / Studies on Polyhalides, XXXVI. On the Octaiodide Ion I82-: Preparation and Crystal Structure of [(Crypt-2.2.2)H2]I8, of [Ni(phen)3]I8-2CHCl3 and of the Bis(N-alkylurotropinium)octaiodides (UrR)2I8 with R = methyl and ethyl

1998 ◽  
Vol 53 (7) ◽  
pp. 641-652 ◽  
Author(s):  
Arista Gräfe-Kavoosian ◽  
Shida Nafepour ◽  
Klaus Nagel ◽  
Karl-Friedrich Tebbe
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Iodine Molecule ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group

Abstract The new compound [(Crypt-2.2.2)H2]I8 has been prepared by the reaction of [(Crypt-2.2.2)H2](I3)2 with iodine in methanol. It crystallizes in the orthorhombic space group Pbcn with a = 11.476 (2), b = 13.589 (2), c = 22.888 (2) Å and Z = 4. The crystal structure has been refined to RF = 0.031 for 1618 reflections. It may be described as a layerlike packing of octaiodide anions I82-and diprotonated 2.2.2-Crypt as cations. The non planar octaiodide anion is built up from two triiodide groups and a bridging iodine molecule.Tris(1, 10-phenanthroline)nickel(II) octaiodide bis(chloroform) crystallizes in the monoclinic space group P21/n with a = 11.683 (8), b = 21.717 (8), c = 20.752 (5) Å, β = 95.03 (5)° and Z = 4 formula units. The crystal structure has been refined to RF = 0.058 for 3894 reflections. The structure consists of two chloroform molecules, octahedrally coordinated complex cations [Ni(phen)3]2+ and nonplanar octaiodide anions I82- each composed of two asymmetric triiodide units I3- weakly associated with an elongated bridging iodine molecule I2.The already known structure of bis(N-methylurotropinium) octaiodide, (UrMe)2I8, has been verified and more accurate crystal data have been collected. The crystal structure has been refined to RF = 0.045 for 1908 reflections. The compound crystallizes in the monoclinic space group P21/c with a = 11.302 (2), b = 9.850 (2), c = 14.188 (2) Å , β = 92.59 (1)° and Z = 2. The anion has the shape of a stretched Z.The structure of bis(N-ethylurotropinium) octaiodide (UrEt)2I8 has been determined and a new configuration (I3-, I5-) for octaiodide ions between Z (I3- · I2 ·I3-) and a “broken” configuration (I3-, I5-) has been observed. The compound crystallizes in the triclinic space group P1̄ with a = 9.741 (3), b = 11.815 (3), c = 15.426 (3) Å, α = 91.80 (2), β = 107.14 (2), γ = 90.04 (2)° and Z = 2. The crystal structure has been refined to RF = 0.037 for 3657 reflections.

scholarly journals Einkristallzüchtung und Röntgenstrukturanalyse polymerer 1:1-Komplexe von CuBr2 und CuCl2 mit Pyrazin aus Gelen / Crystal Growth in Gels and X-Ray Characterization of Polymeric 1:1-Complexes of CuBr2 and CuCl2 with Pyrazine

1989 ◽  
Vol 44 (5) ◽  
pp. 553-556 ◽  
Author(s):  
Th. Fetzer ◽  
A. Lentz ◽  
T. Debaerdemaeker
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Crystal Growth ◽  
Chloro Complex ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Linear Chains

Single crystals of Cu(pz)Br2 and Cu(pz)Cl2 were grown by using gel methods with tetramethoxysilane as the gel-forming reagent. Thermal decomposition is interpreted. Crystal data for the bromo complex: monoclinic, space group C2/m with a = 1239.2(3) pm, b = 685.9(2) pm, c = 390.7(3) pm, β = 96,23(5)°. Crystal data for the chloro-complex: monoclinic, space group C2/m with a = 1197.1(3) pm, b = 684.9(3) pm, c = 370.1(3) pm, β = 95.96(5)°. Crystal structure analyses reveal that CuHal2 molecules are bonded by pyrazine to form linear chains. These chains are cross-linked by bridging halogen atoms.

Synthese von zweikernigen Triazenido- und Pentaazadienidokomplexen des einwertigen Silbers. Kristallstruktur von [Ag(MeOC6H4N3C6H4OM e)]2· 2/3 Py, [Ag(MeOC6H4N5C6H4OMe)]2 und [Ag(EtOC6H4N5C6H4OEt)]2 · Py / Dimeric Triazenido and Pentaazadienido Complexes of Monovalent Silver. Synthesis and Structure of [Ag(MeOC6H4N3C6H4OM e)]2· 2/3 Pyridine, [Ag(MeOC6H4N5C6H4OMe)]2 und [Ag(EtOC6H4N5C6H4OEt)]2 · Pyridine

1989 ◽  
Vol 44 (7) ◽  
pp. 778-785 ◽  
Author(s):  
Edmund Hartmann ◽  
Raimund Schmid ◽  
Joachim Strähle
Keyword(s):  
Unit Cell ◽  
Dinuclear Complexes ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Bridging Ligand ◽  
Orange Yellow ◽  
Ag Contact ◽  
Saturated Solutions

[Ag(MeOC6H4N3C6H4OMe)]2 (1) is formed in THF from AgNO3 , and the triazenide anion, as obtained from the corresponding triazene and Na. 1 crystallizes from pyridine in the form of orange-yellow , air stable crystals with the com position 1·2/3 C5H5N: space group P 1̅ with a = 1468.0(5), b = 1514.1(6), c - 1316.1(3) pm, a = 113.45(3)°, β = 1 1 4 .8 1 (2 )°, γ = 66.78(3)°, Z - 3. The triazenide ion functions as a bridging ligand forming planar (AgN3)2 heterocycles. The unit cell contains two symmetry-independent dinuclear complexes, one of which is centrosymmetrical. The short Ag -Ag distances of 268.0 and 269.8 pm suggest Ag -Ag bonding. The pentaazadienido complexes Ag(RN5R) with R = p -MeO - C6H4 (2), p -EtO - C6H4 (3), p-Cl -C6H4 (4), p -F -C6H4 (5), are obtained from saturated solutions of the pentaazadiene in conc. NH3 and AgNO3 , as explosive, red precipitates which are stable in air. Crystals of 2 and 3 · C5H5N are obtained from pyridine. 2 crystallizes in the monoclinic space group P21/c: a - 583.7(6), b = 1705.1(9), c = 1489.6(9) pm. β = 96.2(1)°, Z = 2; 3 · C5H5N is triclinic (space group P 1̅) with a = 1160.4(4). b = 1671.0(6), c = 509.0(1) pm. a = 97.51(2)°, β = 97.36(2)°, γ = 81.51(3)°, Z = 1. The complexes 2 and 3 are dinuclear with the pentaazadienide ion as a (N1)-η1,(N5)-η1 bridging ligand in 2 and a (N1)-η1, (N3)-η1 bridging ligand in 3. The bridging mode in 3 results in a short Ag -Ag contact of 283.44 pm. The Ag -N distances range from 210.8 to 215.7 pm in 1 and from 215.0 to 220 pm in (2) and (3).

Substitutionsreaktionen an der N-Chlornitrenogruppe des [WCl4(NCl)]2. Die Kristallstrukturen von [CH3CN—WCl4(NSMe)] und [WNCl3 · NC—CH3]4 / Substitution Reactions at the N-Chloronitreno Group of [WCl4(NCl)]2. The Crystal Structures of [CH3CN—WCl4(NSMe)] and [WNCl3 · NC—CH3]4

1989 ◽  
Vol 44 (8) ◽  
pp. 903-910 ◽  
Author(s):  
Astrid Görge ◽  
Ute Patt-Siebel ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Crystal Data ◽  
Substitution Reactions ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

[WCl4(NCl)]2 reacts in acetonitrile with the trimethylsilyl compounds Me3SiSR (R = Me, Ph), and Me3SiESiMe3 (E = S, Se), with substitution of the chlorine atom of the N-chloronitreno group W=N–Cl and formation of CH3CN–WCl4(NSR) and CH3CN–WCl4(NEN)WCl4–NCCH3, respectively. Excess Me3SiBr reacts with CH3CN–WCl4(NSMe) to afford CH3CN–WBr4(NSMe). [CH3CN–WNCl3]4 was obtained from CH3CN–WCl4(NCl) and N(SiMe3)3. The products were characterized by their IR spectra. Two X-ray crystal structure determinations were also carried out. CH3CN—WCl4(NSMe) forms twinned crystals, and only non-overlapping reflexions of one of the twin individuals were used for the structure determination (846 unique values, R = 0.055). Crystal data: a = 592.4(2), b = 758.8(2), c = 1203.7(8) pm, β = 95.06(4)°, monoclinic, space group P21/m, Z = 2. The compound is a monomer in which the acetonitrile ligand is situated in the trans position to the W≡N–S̱̅–Me group. The bond lengths (W≡N 174(2), N–S 161(2) pm) and bond angles (WNS 176(1), NSC 102.1(9)°) are in agreement with the proposed formula. Crystal data for [CH3CN–WNCl3]4: a = 1009.5(2), b = 1274.5(2), c = 1287.9(2) pm, β = 108.17(1)°, monoclinic, space group P21/c, Z = 2 (2113 unique reflexions, R = 0.057). The compound forms tetrameric units, in which the W atoms form a square and are linked with one another via N atoms at alternating distances (W=N 171(2), W–N 207(2), W–NCMe 238(2) pm).

Schwermetall-π-Komplexe II [1] Arenkomplexe des Quecksilbers(I)

1987 ◽  
Vol 42 (7) ◽  
pp. 828-834 ◽  
Author(s):  
W. Frank ◽  
B. Dincher
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Aluminium Trichloride

Abstract The crystalline compounds [(CH3C6H5)2Hg,][AlCl4]2 (1), [(1,2-(CH3)2C6H4)2Hg2][AlCl4]2(2), [(1,3,5-(CH3)3C6H3)2Hg2][AlCl4]2 (3), [1,2,4,5-(CH3)4C6H2Hg2][AlCl4]2 (4) and [((CH3)6C6)2Hg2][AlCl4]2-CH3C6H5 (5) have been prepared from mercury(I)chloride, aluminium trichloride and the corresponding arenes and characterized by elem ental analysis. The crystal structure of 5 has been determ ined from single crystal X-ray diffraction data and refined to R - 0.093 for 3269 unique reflections. Crystal data: monoclinic, space group P21/c, a = 2116(1), b = 1095.1(7), c = 1880(1) pm, β - 104,9(1)°, Z = 4. Each atom of a central Hg2 unit (Hg -Hg distance 251.5 pm) is asymmetrically complexed by hexamethylbenzene, the Hg - Carene distances being in the range from 241 to 340 pm. Two distorted AlCl4 tetrahedra complete a “molecular” [arene2Hg2][AlCl4]2 unit. The shortest Hg-Cl distances are 310 and 312 pm, respectively.

Bildung eines Kupfer-Nitratokomplexes aus einem Azidokomplex und Ozon. Die Kristallstruktur von (PPh4)2[CuCl(NO3)3] · CH2Cl2/ Formation of a Copper Nitrato Complex from an Azido Complex. Crystal Structure of (PPh4)2[CuCl(NO3)3] · CH2Cl2

1992 ◽  
Vol 47 (1) ◽  
pp. 31-34 ◽  
Author(s):  
Karin Ruhlandt-Senge ◽  
Alfred D. Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Coordination Number ◽  
The Other ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Complex Crystal Structure ◽  
Monodentate Ligands ◽  
Complex Crystal

(PPh4)2[CuCl(NO3)3] · CH2Cl2 is formed when ozone reacts with (PPh4)2[Cu2(N3)6] in dichloromethane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1113(1), b = 1156(1), c = 1965(2) pm , α = 101.02(1), β = 93.74(1), γ = 104.05(2)° at 130 K, space group P1̄, Z = 2, R = 0.057 for 3951 observed reflexions. The structure contains CH2Cl2 molecules and PPh4+ and [CuCl(NO3)3]2- ions, with copper having coordination number 5. One nitrate ligand acts as a bidentate chelating unit, and the other two as monodentate ligands.

Benzothiarsolium cations: evidence for pπ-bonding between arsenic and sulfur in the first structurally characterized arsenium system

1992 ◽  
Vol 70 (3) ◽  
pp. 703-709 ◽  
Author(s):  
Neil Burford ◽  
Trenton M. Parks ◽  
Bruce W. Royan ◽  
John F. Richardson ◽  
Peter S. White
Keyword(s):  
Crystal Structure ◽  
Significant Degree ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Keywords Arsenic

Tetrachloroaluminate salts of the benzothiazarsolium and toluodithiarsolium heteronaphthalenic cations have been prepared from the corresponding chloroarsoles by a routine halide ion abstraction procedure. Characterization data are presented, including the X-ray crystal structure of the thiaza derivative. (Crystal data for C6H5AlAsCl4NS: monoclinic, space group P21/c, a = 6.4259(5) Å, b = 23.654(3) Å, c = 8.5859(7) Å, β = 98.203(6)°, V = 1291.7(2) Å3, Z = 4, R = 0.054.) A planar bicyclic cationic unit is observed, typical of other heteronaphthalenic systems. The crystal structure of 2-chlorobenzo-1,3,2-thiazarsole has been obtained for direct comparison, and also has a close to planar heterobicyclic moiety. (Crystal data for C6H5AsClNS: monoclinic, space group P21/c, a = 8.370(3) Å, b = 10.829(3) Å, c = 8.756(2) Å, β = 95.99(2)°, V = 789.2(3) Å3, Z = 4, R = 0.025.) The planarity and short heterocyclic bond lengths observed in the two compounds imply a significant degree of pπ bonding, which is unique between sulfur and arsenic. In addition, the cation is a rare example of a structurally characterized cationic dicoordinate arsenic, or arsenium, system. Keywords: arsenic, arsolium, arsenium, pπ-bonding, sulfur, heteronaphthalenic.

Darstellung und Struktur von (CH3NH3)3PrCl6 · 2 H2O / Synthesis and Structure of (CH3NH3)3PrCl6 · 2 H2O

1990 ◽  
Vol 45 (5) ◽  
pp. 603-606 ◽  
Author(s):  
Petra Runge ◽  
Mathias Schulze ◽  
Werner Urland
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Magnetic Behaviour ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Chlorine Atoms ◽  
Space Group ◽  
Lattice Constants ◽  
Group I ◽  
Light Green

(CH3NH3)3PrCl6 · 2 H2O has been prepared as light green, air sensitive crystals by the reaction of PrCl3·xH2O with [CH3NH3]Cl in ethanol. The compound was characterized by crystal structure determination. Crystal data: monoclinic space group I 2/a, Z = 8. Lattice constants: a = 1963.3(4), b = 925.9(3), c = 1954.3(4) pm, β = 90.56(1)°. The compound forms [PrCl4(H2O)2]--chains where two Pr3+-ions are connected via two chlorine atoms. The magnetic behaviour of (CH3NH3)3PrCl6· 2H2O has been studied.

The Synthesis and Crystal Structures of Two Cobalt(III) Complexes Containing the Ligand 1,4,8,11-Tetraazacyclotetradecane

2002 ◽  
Vol 55 (8) ◽  
pp. 535 ◽  
Author(s):  
A. M. Funston ◽  
W. D. McFadyen ◽  
P. A. Tregloan
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Triclinic Space Group ◽  
Space Group ◽  
Octahedral Environment ◽  
Related Complex

The new cobalt(III) complex [Co(cyclam)(NO3)2]NO3�HNO3 (2) has been synthesized. The crystal structure of this complex and the related complex [Co(cyclam)(NH3)2]Cl2BF4�2H2O (1) have been determined. Crystal data for (1): M 451.04, monoclinic, space group P21/c (No. 14), a 7.3927(10), b 13.3082(7), c 19.524(2) Å, β 97.625(14)�, V 1903.9(3) Å3, F(000) 936, Z 4, Dc 1.574 g cm–3, μ 1.225 cm–1, Mo Kα (graphite monochromatized) λ 0.71073 Å, T 293(1) K. Crystal data for (2): M 571.33, triclinic, space group P1–(No. 2),a 7.3988(14), b 8.5682(16), c�9.209(3) Å, α 89.02(2), β 76.64(3), γ 82.340(16)�, V 562.9(2) Å3, F(000) 296, Z 1, Dc 1.685 g cm–3, μ 0.854 cm–1, Mo Kα (graphite monochromatized) λ 0.71073 Å, T 293(1) K. In both complexes the complex crystallizes in the trans-III form with the cobalt in the usual octahedral environment.

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