Synthesis and X-Ray Structural Characterization of WO(S2)(S2CNEt2)2 and Related Complexes

1987 ◽  
Vol 40 (2) ◽  
pp. 381 ◽  
Author(s):  
JA Broomhead ◽  
JH Enemark ◽  
B Hammer ◽  
RB Ortega ◽  
W Pienkowski
Keyword(s):  
Structural Analysis ◽  
Structural Characterization ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Independent Data ◽  
Dichloromethane Solution ◽  
Space Group ◽  
X Ray

The reaction of SO2 and W(CO)3(S2CNR2)2 in dichloromethane solution under dinitrogen gives the title complex along with WS(S2)(S2CNR2)2 and Syn-W2O2(�-S)2(S2CNR2)2 (R = Me, Et, Pri , C6H5CH2; NR2 = pyrrolidinyl ). X-ray structural analysis of WO(S2)(S2CNEt2)2 reveals a seven-coordinate tungsten complex with a terminal oxo group and a dihapto - disulfido ligand in a mutually triangular arrangement. Crystals are monoclinic space group P21 1 n, with a 9.379(2), b 22.276(7), c 9.408(2), β 106.86(1)�, U 188l.1(7) �33 and Z 4.2758 independent data were refined to a weighted agreement factor 0.036.

Reactions of Transition-Metal Sigma-Acetylides. V. Synthesis and X-Ray Structure of Co2(µ-η2-PhC2Fe(Co)2(η-C5h5))(Co)6

1986 ◽  
Vol 39 (1) ◽  
pp. 159 ◽  
Author(s):  
MI Bruce ◽  
DN Duffy ◽  
MG Humphrey
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Single Crystal ◽  
Diffraction Study ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Independent Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The reaction between Co2(CO)8 and Fe(C2Ph)(CO)2(η-C5H5) gave the title complex in 44% yield. The molecular structure was determined from a single-crystal X-ray diffraction study, and consists of the transition metal acetylide acting as a conventional μ- alkyne ligand to a Co2(CO)6 unit. Crystals are monoclinic, space group P21/n, with a 11.610(8), b 14.657(4), c 12.526(6)Ǻ, β 90.30(5)°, and Z 4; 1683 independent data were refined to R 0.080, Rw 0.087.

Structural Characterization of Cationic 16-Electron Pentamethylcyclopentadienyl Ruthenium(II) Complexes Containing the Binuclear [Cp*Ru(μ-Cl)3RuCp*]– Anion

2008 ◽  
Vol 63 (10) ◽  
pp. 1155-1159 ◽  
Author(s):  
Thomas Glöge ◽  
Dejan Petrovic ◽  
Cristian G. Hrib ◽  
Peter G. Jones ◽  
Matthias Tamm
Keyword(s):  
Crystal Structures ◽  
Structural Characterization ◽  
Complex Salt ◽  
Monoclinic Space Group ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Diimine Ligand ◽  
Half Sandwich

AbstractThe reaction of the diimine ligand 1,2-bis(1,3-diisopropyl-4,5-dimethylimidazolin-2-imino)ethane (BLiPr) with tetrameric [Cp*RuCl]4 in a 1 : 0.75 ratio afforded the complex salt [1][2] containing the 16-electron half-sandwich cation [Cp*Ru(BLiPr)]+ (1) and the dinuclear anion [Cp*Ru(μ- Cl)3RuCp*]− (2). The X-ray crystal structures of [1][2]·31/2THF (monoclinic, space group P21/n, Z = 4) and of [1][2]·THF (monoclinic, space group C2/m, Z = 4) are reported, allowing the structural characterization of the unprecedented anion 2, in which two [(η5-C5Me5)Ru(II)] moieties are bridged by three μ2-chlorine atoms.

Darstellung und spektroskopische Charakterisierung von Methylnitro-closo-hexaboraten sowie Kristallstrukturen von cis-(Ph4As)2[B6H4(CH3)(NO2)],fac-(Ph4As)2[B6H3(CH3)(NO2)2] · CH3CN und mer-(Ph4P)2[B6H3(CH3)(NO2)C2] / Synthesis and Spectroscopic Characterization of Methylnitro-closo-hexaborates and Crystal Structures of cis -(Ph4As)2[B6H4(CH3)(NO2)],fac-(Ph4As)2[B6H3(CH3)(NO2)2] · CH3CN and mer-(Ph4P)2[B6H3(CH3)(NO2)C2]

1999 ◽  
Vol 54 (3) ◽  
pp. 349-356 ◽  
Author(s):  
C. Drewes ◽  
W. Preetz
Keyword(s):  
Nmr Spectra ◽  
Spectroscopic Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Dichloromethane Solution ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cis And Trans

By electrochemical oxidation of (n-Bu4N)[B6H6(CH3)] in the presence of nitrite ions and of the base DBU in dichloromethane solution cis- and trans-[B6H4(CH3)(NO2)]2- , fac- [B6H3(CH3)(NO2)2]2- and mer-[B6H3(CH3)(NO2)c2]2- are formed. X-ray diffraction analyses have been performed on single crystals of cis-(Ph4As)2[B6H4(CH3O)(NO2)] (1) (monoclinic, space group P21/a, a = 20.063(2), b = 10.858(1), c =21.384(2) Å, β = 105.818(9)°, Z = 4), fac-(Ph4As)2[B6H3(CH3)(NO2)2] ·CH3CN (2) (triclinic, space group P1̄, a = 10.333(3), b = 10.695(3), c = 22.833(6) Å, α = 93.91(3), β = 96.79(3), γ = 104.56(2)°, Z = 2), and mer-(Ph4P)2[B6H3(CH3)(NO2)c2] (3) (triclinic, space group P1̄, a - 10.100(1), b = 10.402(3), c = 22.923(3) Å, α = 96.328(18), β = 89.928(12), γ = 107.963(16)°, Z = 2). The 11B NMR spectra and the vibrational spectra of the methylnitro compounds are discussed and compared with those of the monomethyl- and mononitro-closo-hexaborates.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LII. Synthesis and Structural Characterization of Mononuclear Chloro- and Bromo-pyridinebis-(triphenylphosphine)silver(I) Complexes

1989 ◽  
Vol 42 (6) ◽  
pp. 907 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Silver Atom ◽  
Lewis Base ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Weak Coordination

The mononuclear adducts chloro - and bromo-pyridinebis (triphenylphosphine)silver have been synthesized and structurally characterized by single-crystal X-ray diffraction methods. The two complexes are isomorphous, monoclinic, space group P21 or P21/m, a ≈ 9.8, b ≈ 20.0, c ≈ 9.1 � , β ≈ 97.5�, Z 2; in space group P21/m, they were refined to residuals of 0.038, 0.036 for 2392, 2157 'observed' reflections respectively. No comparable iodide adduct has been isolated. In both structures the silver atom is four-coordinate; Ag-Cl,Br are 2.511(2), 2.629(1) �; Ag-P, 2.472(1), 2.476(1) �, and Ag-N, 2.585(5), 2.570(5) � respectively, the Ag-N distance being longer than Ag-P, indicating very weak coordination of the pyridine.

Synthesis and Structural Characterization of Copper(I) and Copper(II) Complexes with an Ambivalent Phenanthroline-Type Ligand

1997 ◽  
Vol 50 (10) ◽  
pp. 951 ◽  
Author(s):  
Jean-Paul Collin ◽  
Pablo Gaviña ◽  
Jean-Pierre Sauvage ◽  
André De Cian ◽  
Jean Fischer
Keyword(s):  
Cyclic Voltammetry ◽  
Structural Characterization ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Coordination Modes ◽  
X Ray Crystallography ◽  
Phenanthroline Ligand

The new phenanthroline ligand 2-(p-methoxyphenyl)-9-(5′-methylpyridin-2′-yl)-1,10-phenanthroline L has been synthesized and shown to form four-coordinate CuI(L)2 (1) and six-coordinate CuII(L)2 (2) complexes. Their structures have been determined by X-ray crystallography: (1) C50H38CuN6O2.BF4, triclinic, space group P -1, a12·924(3), b 14·567(4), c 12·649(3) Å , α 105·57(2), β 107·68(2), γ 104·00(2)°; (2) C50H38CuN6O2.2PF6, monoclinic, space group P 21/c, a 17·701(5), b 19·285(5), c 14·93(4) Å, β 98·20(2)°. In solution, cyclic voltammetry measurements indicate for the copper(I) and copper(II) complexes a very fast rearrangement of the pyridine substituent with the change of the oxidation state. Surprisingly, the X-ray data show two different coordination modes for the ligand around the copper(I) ion, the 1,10-phenanthroline nucleus being either mono- or bi-dentate. In solution, since the 1H n.m.r. spectra obtained even at several temperatures display only one set of signals, it is proposed that a fast equilibrium takes place between two coordination modes of the phenanthroline

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.

Crystallographic characterization of three cathinone hydrochlorides new on the NPS market: 1-(4-methylphenyl)-2-(pyrrolidin-1-yl)hexan-1-one (4-MPHP), 4-methyl-1-phenyl-2-(pyrrolidin-1-yl)pentan-1-one (α-PiHP) and 2-(methylamino)-1-(4-methylphenyl)pentan-1-one (4-MPD)

2022 ◽  
Vol 78 (1) ◽  
Author(s):  
Marcin Rojkiewicz ◽  
Piotr Kuś ◽  
Maria Książek ◽  
Joachim Kusz
Keyword(s):  
Chemical Structure ◽  
Crystallographic Data ◽  
New Psychoactive Substances ◽  
Monoclinic Space Group ◽  
Psychoactive Substances ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Analytical Laboratories

Cathinones belong to a group of compounds of great interest in the new psychoactive substances (NPS) market. Constant changes to the chemical structure made by the producers of these compounds require a quick reaction from analytical laboratories in ascertaining their characteristics. In this article, three cathinone derivatives were characterized by X-ray crystallography. The investigated compounds were confirmed as: 1-[1-(4-methylphenyl)-1-oxohexan-2-yl]pyrrolidin-1-ium chloride (1, C17H26NO+·Cl−, the hydrochloride of 4-MPHP), 1-(4-methyl-1-oxo-1-phenylpentan-2-yl)pyrrolidin-1-ium chloride (2; C16H24NO+·Cl−, the hydrochloride of α-PiHP) and methyl[1-(4-methylphenyl)-1-oxopentan-2-yl]azanium chloride (3; C13H20NO+·Cl−, the hydrochloride of 4-MPD). All the salts crystallize in a monoclinic space group: 1 and 2 in P21/c, and 3 in P21/n. To the best of our knowledge, this study provides the first detailed and comprehensive crystallographic data on salts 1–3.

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 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.

Benzo-18-krone-6 -Acetonitril (1/2): Kristallisation und Tieftemperatur- Röntgenstrukturanalyse / Benzo-18 -crown-6 -Acetonitrile (1/2): Crystallization and Low-Temperature X-Ray Analysis

1998 ◽  
Vol 53 (12) ◽  
pp. 1528-1530 ◽  
Author(s):  
Karna Wijaya ◽  
Oliver Moers ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Data Collection ◽  
Single Crystals ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Mecn Solution

Abstract Benzo-18 -crown-6 -Acetonitrile (1/2), Crystal Structure Single crystals of the title complex resulted fortuitously during an attempt to co-crystallise MeN(SO2Me)2 with benzo-18-crown-6 from an MeCN solution at -30 °C. The crystal structure has been determined via data collection at -100 °C (monoclinic, space group P21/n, Z = 4). The nitrile molecules are located with their me­ thyl groups above and below the plane of the 18-membered crown ring, the Me hydrogen atoms being rotationally disordered about the MeCN axes; C(methyl)···O(crown) distances range from 309.4(3) to 384.9(3) pm.

Sign in / Sign up

Export Citation Format

Share Document