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.

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

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.

Distorted chiolite crystal structures of α-Na5M3F14 (M=Cr,Fe,Ga) studied by X-ray powder diffraction

2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Refinements ◽  
Space Group ◽  
X Ray ◽  
Precise Characterization

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.

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 The preparation and characterization of SeCl3SbF6, improved syntheses of MCl3(As/Sb)F6 (M = S, Se), and the X-ray crystal structure determination of SeCl3AsF6 and a new phase of SBr3SbF6

1996 ◽  
Vol 74 (9) ◽  
pp. 1671-1681 ◽  
Author(s):  
Jack Passmore ◽  
Paul D. Boyle ◽  
Gabriele Schatte ◽  
Todd Way ◽  
T. Stanley Cameron
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Ft Raman Spectroscopy ◽  
New Phase ◽  
Ft Raman

Alternative and, in some cases, improved syntheses of the salts MX3(As/Sb)F6 (M = S, Se) and SCl3(SbCl6/AlCl4) are described. In addition, the synthesis of SeCl3SbF6 is reported. The compounds were characterized by FT–Raman spectroscopy and the X-ray crystal structures of SeCl3AsF6 (also 77Se NMR) and a new phase of SBr3SbF6 were determined. Crystals of SeCl3AsF6 and SBr3SbF6 are monoclinic, space group P21/c with [values for SBr3SbF6 in brackets] a = 7.678(1) [8.137(1)] Å, b = 9.380(3) [9.583(2)] Å, c = 11.920(3) [12.447(2)] Å, β = 98.19(2)° [97.36(1)]°, V = 849.72(3) [962.6(3)] Å3,z = 4, Dx = 2.925 [3.502] Mg m−3, R = 0.0525 [0.055], and Rw = 0.0554 [0.060] for 1151 [1472] observed reflections. Key words: MX3+ salts, FT–Raman spectroscopy, X-ray crystal structures of SeCl3AsF6, SBr3SbF6, and preparation of SeCl3SbF6.

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.

The Constituents of Marine Sponges. IX New Norditerpenoids from Aplysilla pallida

1997 ◽  
Vol 50 (9) ◽  
pp. 903 ◽  
Author(s):  
Trevor W. Hambley ◽  
Walter C. Taylor ◽  
Stephen Toth
Keyword(s):  
Crystal Structures ◽  
Spectroscopic Studies ◽  
Marine Sponges ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

Four novel norditerpenoids were isolated from a new encrusting sponge, conveniently labelled Aplysilla pallida. The structures of aplypallidenone (1), aplypallidoxone (2), aplypallidione (3) and aplypallidioxone (4) were elucidated by spectroscopic studies and the crystal structures of aplypallidenone and aplypallidoxone have been determined by X-ray diffraction methods. The structure of (1) was refined to a residual of 0·040 for 1665 independent observed reflections and the structure of (2) was refined to a residual of 0·031 for 1699 independent observed reflections. The crystals of (1) are orthorhombic, space group P212121, a 7·728(2), b 10·838(4), c 24·880(5) Å, Z 4. Those of (2) are monoclinic, space group C 2, a 23·927(7), b 6·674(2), c 14·033(3) Å, Z 4.

Organoamido- and Aryloxo-lanthanoids. XII. The Coordination Chemistry of Bis(2-phenylindol-1-yl)ytterbium(II), and the X-Ray Crystal Structures of Yb(pin)2(diglyme)(thf) and [Yb(pin)2(dme)]2 (pin = 2-Phenylindol-1-yl, diglyme = Bis(2-methoxyethyl) Ether, thf Equals Tetrahydrofuran, dme = 1,2-Dimethoxyethane)

1995 ◽  
Vol 48 (12) ◽  
pp. 1933 ◽  
Author(s):  
CT Abrahams ◽  
GB Deacon ◽  
CM Forsyth ◽  
WC Patalinghug ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Coordination Chemistry ◽  
Crystal Structures ◽  
Coordination Polyhedron ◽  
Basal Plane ◽  
Monoclinic Space Group ◽  
Coordinate Structure ◽  
Space Group ◽  
X Ray ◽  
Nitrogen Donor

With the facile displacement being utilized of thf from Yb(pin)2(thf)4 (pin = 2-phenylindol-1-yl, thf = tetrahydrofuran) in toluene solution, the complexes Yb(pin)2(dme)2 (dme = 1,2- dimethoxyethane), Yb(pin)2 (tmen)(tmen = N,N,N′,N′-tetramethylethane-1,2-diamine) and Yb(pin)2(diglyme)(thf) (diglyme = bis(2-methoxyethyl) ether) have been prepared from the respective ligands and Yb(pin)2(thf)4. Yb(pin)2 (diglyme) (thf) [monoclinic, space group P 21 /c, a 15.35(1), b 16.179(5), c 14.45(2) Ǻ, β 107.51(8)°, Z 4, R 0.044 for 2956 (I > 3σ(I)) 'observed' reflections] has a monomeric six-coordinate structure with transoid nitrogen donor atoms, N-Yb-N 143.6(4)° and an irregular coordination polyhedron described as either a distorted trigonal prism or a monocapped square pyramid. Attempted crystallization of Yb(pin)2 (thf) by partial desolvation of Yb(pin)2(thf)4 in hot toluene, containing a trace of dme, gave a mixture of red Yb(pin)2(thf) and orange [Yb(pin)2(dme)]2. The latter was independently synthesized by partial desolvation of Yb(pin)2(dme)2 in toluene. An X-ray crystal structure showed [Yb(pin)2(dme)]2 [monoclinic, space group P 21/c, a 11 .614(2), b 15.945(7), c 15.327(4) Ǻ, β 110.19(2)°, Z 2 dimers, R 0.070 for 2314 (I ≥ 3σ(I)) 'observed' reflections] to be a dimer with two bridging pin ligands, coordinated through nitrogen only. There is an approximately square pyramidal five-coordinate ytterbium environment with an apical dme oxygen, and with two bridging nitrogens, a terminal nitrogen, and a dme oxygen in the basal plane.

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