Synthese von Nitrenkomplexen mit N-Trimethylsilylanilin I. Charakterisierung und Kristallstruktur von [Re(NPh)Cl3(Et2PhP)2] und [Re(NPh)Cl3(Ph3P)2] ·1/2 CHCl3 / Synthesis of Nitrene Complexes with N –T rimethylsilylaniline I. Characterisation and Crystal Structure of [Re(NPh)Cl3(Et2PhP)2] and [Re(N Ph)Cl3(Ph3P)2] · 1/2CHCl3

1995 ◽  
Vol 50 (7) ◽  
pp. 997-1003 ◽  
Author(s):  
Ursula Wittern ◽  
Joachim Strähle ◽  
Ulrich Abram
Keyword(s):  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Complex Molecules ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Distorted Octahedral ◽  
In Trans ◽  
Cl Atoms

trans-mer--Trichlorobis(diethylphenylphosphine)phenylnitrene rhenium(V), [Re(NPh)Cl3- (Et2PhP)2], has been synthesized from [ReOCl3 (Et2 PhP)2 ] and N-trimethylsilylaniline, while trans-mer-trichlorophenylnitrenebis (triphenylphosphine) rhenium(V), [Re(NPh)Cl3 (Ph3P)2] has been obtained via a novel route, from (Bu4N)[ReOCl4 ] and N-trimethylsilylanilin. The products were studied by mass spectrometry, IR spectroscopy and X-ray diffraction.trans-mer-[Re(NPh)Cl3(Et2PhP)2 ] crystallizes in the monoclinic space group P21/n with a = 1498.5(3), b = 1068.6(1), c = 1784.0(4) pm and β = 91.28(1)°, Z = 4. The rhenium atom exhibits a distorted octahedral coordination with the phosphine groups in trans positions, and the Cl ligands in a meridional arrangement. The Re ≡N -C moiety is linear with a bond angle o f 169,4(5)°and a Re= N bond length o f 171.8(6) pm.[Re(NPh)Cl3(Ph3P)2 ]· 0.5 CHCI3 crystallizes in the triclinic space group P 1̄ with a = 1232.1 (4), b= 1431.6(5), c = 2236.6(8) pm, a = 89.19(2)°, β = 80.50(2)°and γ = 88.26(2)°, Z = 4. The asymmetric unit contains two symmetry independent complex molecules of approximately the same structure, with Cl atoms meridionally arranged and the phosphine groups in trans positions. The coordination geometry is a distorted octahedron. The almost linear Re≡N -C moieties have Re≡N bond lengths of 170.2(7) and 170.8(7) pm, respectively, and Re≡N -C angles of 173.3(6)°and 175.0(7)°.

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.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.

Structural Systematics of Metal Acetylide Complexes: X-Ray Studies of Some 'Extended-Chain' Gold σ-Acetylide Complexes

1997 ◽  
Vol 50 (10) ◽  
pp. 991 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Ground State ◽  
Structural Data ◽  
Monoclinic Space Group ◽  
Confidence Limits ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Back Bonding ◽  
Ground State Geometry

The structures of Au(4-C≡CC6H4XYC6H4-4′-NO2)(PPh3) (XY = (E )-CH=CH (1), (Z)-CH=CH (2), C≡C (3), N=CH (4)) have been determined by single-crystal X-ray diffraction analyses, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a8·847(1), b 17·870(4), c 19·705(3) Å, α116·25(1), β 93·33(1), γ 92·64(2)˚, Z 4, 6747 unique reflections (703 parameters), converging at R 0·025 and Rw 0·029. For (2), crystals are monoclinic, space group P 21/a, with a 10·718(6), b 19·398(5), c14·469(3) Å, β 108·96(2)˚, Z 4, 3295 unique reflections (352 parameters), converging atR 0·040 and Rw 0·034. For (3), crystals are triclinic, space group P-1, with a 10·671(4), b 17·599(7), c 18·220(8) Å, α 116·31(3), β 105·00(4), γ 95·08(4)˚, Z 4, 4828 unique reflections (703 parameters), converging at R 0·043 and Rw 0·030. For (4), crystals are triclinic, space group P-1, with a 8·8314(6), b 17·834(2), c 20·001(2) Å, α 115·249(7), β 90·930(7), γ 94·082(7)˚, Z 4, 4724 unique reflections (703 parameters), converging at R 0·035 and Rw 0·034. Despite the [ligated metal donor]-bridge-[nitro acceptor] composition of these complexes, Au–C and C≡C distances are normal and consistent with minimal allenylidene contribution to the ground-state geometry. Within the 3σ confidence limits, the structural data do not provide evidence for π*-back-bonding in these complexes

Metal-selenolate chemistry: stereochemistry of adamantane-type clusters of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd)

1992 ◽  
Vol 70 (3) ◽  
pp. 792-801 ◽  
Author(s):  
Jagadese J. Vittal ◽  
Philip A. W. Dean ◽  
Nicholas C. Payne
Keyword(s):  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Space Groups ◽  
X Ray Crystallography ◽  
Cell Dimensions ◽  
Minimum Number

The structures of three tetramethylammonium salts containing anions of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd) were determined by single crystal X-ray diffraction techniques. The Zn salt crystallizes in different space groups depending upon the solvent combination used in the synthesis. Thus crystals of (Me4N)2[Zn4(SePh)10], 1, grown from a mixture of methanol, acetonitrile, and acetone are triclinic, space group [Formula: see text] with cell dimensions a = 13.214(2), b = 23.859(2), c = 13.072(1) Å, α = 91.134(8), β = 113.350(8), γ = 79.865(9)°, and Z = 2. In the absence of acetone, a solvated crystal (Me4N)2[Zn4(SePh)10]•CH3CN, 2, is formed, which belongs to the monoclinic space group P21/n with a = 14.248(1), b = 39.722(2), c = 13.408(1) Å, β = 97.132(5)°, and Z = 4. The Cd salt (Me4N)2[Cd4(SePh)10], 3, crystallizes in the monoclinic space group P21/c, with a = 20.830(2), b = 14.282(1), c = 25.872(1) Å, β = 99.626(6)°, and Z = 4. These three salts are the first examples of homoleptic, tetranuclear selenolatometal(II) anions with (μ-Se)6M4 cages of adamantane-type stereochemistry. In each case the phenyl substituents of the bridging ligands adopt the configuration [aae, aae, aee, aee], which has the minimum number of two 1,3-axial–axial non-bonding substituent interactions. Keywords: selenolate complexes, synthesis, X-ray crystallography, isomerism, adamantane stereochemistry.

scholarly journals Synthesis, Spectral and Thermal Studies, and Crystal Structure of cis-Bis(4-methylimidazole)bis(picolinato)copper(II) [Cu(pic)2(4-MeIm)2]

2006 ◽  
Vol 61 (10) ◽  
pp. 1217-1221 ◽  
Author(s):  
Zerrin Heren ◽  
Cem Keser ◽  
C. Cüneyt Ersanli ◽  
O. Zafer Yeşilel ◽  
Nazan Ocak
Keyword(s):  
Thermal Studies ◽  
X Ray Diffraction ◽  
Complex Molecules ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Distorted Octahedral ◽  
Ft Ir ◽  
In Cis ◽  
Hydrogen Bondings

The mixed-ligand picolinato (pic) complex of Cu(II) with 4-methylimidazole (4-MeIm), [Cu(pic)2(4-MeIm)2], was synthesized and characterized by elemental analysis, magnetic susceptibility, spectroscopic methods (UV/vis and FT-IR) and X-ray diffraction. In the slightly distorted octahedral cis-bis(4-methylimidazole)bis(picolinato)copper(II) complex, the pic ligands are coordinated to the Cu(II) ion as bidentate N,O-donors forming chelate rings. The 4-MeIm ligands are N-coordinated in cis positions. The complex crystallizes in the triclinic space group p̅1 with unit cell parameters a = 9.204(5), b = 9.498(5), c = 13.095(5) Å , α = 90.395(5), β = 101.687(5), γ = 112.291(5)° and Z = 2. Hydrogen bondings and C-H ··· π interactions occur between picolinato and methylimidazole ligands of neighboring complex molecules. The thermal decomposition of the complex is described.

Synthesis and structural characterization of donor-stabilized disubstituted diphenyldithiophosphates of nickel(II)

2014 ◽  
Vol 70 (4) ◽  
pp. 761-767 ◽  
Author(s):  
Sandeep Kumar ◽  
Ruchi Khajuria ◽  
Amanpreet Kaur Jassal ◽  
Geeta Hundal ◽  
Maninder S. Hundal ◽  
...  
Keyword(s):  
Single Crystal ◽  
Chelate Ring ◽  
Donor Ligands ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Donor-stabilized addition complexes of nickel(II) with disubstituted diphenyldithiophosphates, [{(ArO)2PS2}2NiL2] {Ar = 2,4-(CH3)2C6H3[(1), (5)], 2,5-(CH3)2C6H3[(2), (6)], 3,4-(CH3)2C6H3[(3), (7)] and 3,5-(CH3)2C6H3[(4), (8)];L= C5H5N [(1)–(4)] and C7H9N [(5)–(8)]}, were successfully isolated and characterized by elemental analysis, magnetic moment, IR spectroscopy and single-crystal X-ray analysis. Compound (4) crystallizes in the monoclinic space groupP21/nwhereas compounds (7) and (8) crystallize in the triclinic space group P\bar 1. The single-crystal X-ray diffraction analysis of (4), (7) and (8) reveals a six-coordinated octahedral geometry for the NiS4N2chromophore. Two diphenyldithiophosphate ions act as bidentate ligands with their S atoms coordinated to the Ni centre. Each of them forms a four-membered chelate ring in the equatorial plane. The N atoms from two donor ligands are axially coordinated to the Ni atom.

Monomere und dimere Oxotrihalogenoselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C6H5)4]SeOCl3 und [N(C2H5)4]SeOCl3 / Monomerie and Dimeric Oxotrihalogenoselenates(IV): Preparation, Structure and Properties of [As(C6H5)4]SeOCl3 and [N(C2H5)4]SeOCl3

1983 ◽  
Vol 38 (1) ◽  
pp. 20-29 ◽  
Author(s):  
Bernt Krebs ◽  
Marita Hucke ◽  
Michael Hein ◽  
Andreas Schäffer
Keyword(s):  
Polymer Chains ◽  
Monoclinic Space Group ◽  
Structure And Properties ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers

Abstract The monomeric SeOCl3- ion, which can be prepared as the tetraphenylarsonium salt from SeOCl2 and As(C6H5)4Cl, was structurally characterized by a low-temperature single crystal X-ray diffraction analysis. [As(C6H5)4]SeOCl3 is monoclinic, space group P21/c, with a = 9,332(3), b = 13,761(4), c = 18,985(6) Å, β = 110,97(3)° (at -135 °C), Z = 4; it contains a novel type of ψ-trigonal bipyramidal oxotrichloroselenate(IV) anion which is not associated to dimers or polymer chains as in known structures. The equatorial positions are occupied by doubly bonded oxygen (Se-O 1,601(3) Å) and by one Cl(Se-Cl 2,234(1) Å), the axial Se-Cl bonds (2,430(1) and 2,475(1) Å) being significantly longer. [N(C2H5)4]SeOCl3, which was obtained as crystals by oxidation of trichloroselenate(II), is triclinic, space group P1̄, with a = 10,607(3), b = 8,950(2), c = 8,862(2) Å, α = 119,79(2)°, β = 101,07(2)°, γ = 96,28(2)°, Z = 2. The X-ray structure analysis shows the anions to be present as centrosymmetric dimers Se2O2Cl62- like in the [P(C6H5)4]+ salt, with two tetragonal SeOCl4 pyramids linked through a Cl···Cl edge and the lone pairs trans to the axial Se-O bonds (1,589(4) Å). Se-Cl bond lengths are 2.270(1) and 2,351(2) Å (terminal); 2,698(1) and 2,920(1) Å (bridging). The results show that the nature of the reaction products of the Lewis acid SeOCl2 with halogenides as bases changes very sensitively with small variations in cations and environment. The vibrational spectra are discussed.

Structural Systematics of Metal Acetylide Complexes. II. X-Ray Studies of Some Nickel σ-Acetylide Complexes

1998 ◽  
Vol 51 (3) ◽  
pp. 219 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Trans Influence

The structures of Ni(C≡CR)(PPh3)(η-C5H5) (R = Ph (1), C6H4-4-NO2 (2), 4-C6H4C6H4-4′-NO2 (3), (E)-4-C6H4CH=CHC6H4-4′-NO2 (4), 4-C6H4C≡CC6H4-4′-NO2 (5), 4-C6H4N=CHC6H4-4′-NO2 (6)) have been determined by single-crystal X-ray diffraction studies, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a 10·094(2), b13·429(3), c 18·835(5) Å,α 103·24(2), β 91·50(2), γ 90·10(2)°, Z 4, 5844 unique reflections (595 parameters), converging at R 0·033 and Rw 0·024. For (2), crystals are orthorhombic, space group Pna21, with a 16·799(2), b 8·681(2), c 17·485(2) Å, Z 4, 1774 unique reflections (325 parameters), converging at R 0·031 and Rw 0·029. For (3), crystals are monoclinic, space group P 21/c, with a 11·140(3), b 18·282(4), c 15·296(2) Å, β 105·18(2)°, Z 4, 3132 unique reflections (397 parameters), converging at R 0·039 and Rw 0·024. For (4), crystals are monoclinic, space group P 21/n, with a 12·929(7), b 16·953(8), c 15·601(7) Å, β 112·55(3), Z 4, 3023 unique reflections (397 parameters), converging at R 0·039 and Rw 0·025. For (5), crystals are monoclinic, space group P 21/n, with a 12·710(5), b 16·882(3), c 15·693(4) Å, β 111·37(3)°, Z 4, 3216 unique reflections (397 parameters), converging at R 0·035 and Rw 0·030. For (6), crystals are monoclinic, space group P 21/n, with a 12·594(1), b 16·936(2), c 15·611(1) Å, β 112·476(5)°, Z 4, 3564 unique reflections (397 parameters), converging at R 0·038 and Rw 0·041. For structurally characterized 18-electron (cyclopentadienyl)nickel(II) acetylide complexes, statistically insignificant decreases in the average Ni-C(1) distance and trans influence and an increase in the average C(1)-C(2) parameter are observed on introduction of an acceptor substituent at the alkynyl ligand.

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.

One-dimensionally Hydrogen-bonded Silver(I) Saccharinate Complexes with N-(2-Aminoethyl)piperidine and N-(2-Hydroxyethyl)piperidine: Synthesis, Crystal Structures, FTIR and Thermal Studies

2008 ◽  
Vol 63 (2) ◽  
pp. 139-142 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
Orhan Büyükgüngör
Keyword(s):  
Thermal Studies ◽  
Chair Conformation ◽  
Metallic Silver ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
The Individual

Two new complexes [Ag(sac)(aepip)] (1) and [Ag(sac)(hepip)] (2) have been obtained by the reaction of AgNO3 with Na(sac)・2H2O (sac = saccharinate) in the presence of N-(2-aminoethyl)piperidine (aepip) and N-(2-hydroxyethyl)piperidine (hepip), and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group C2 and triclinic space group P1, respectively. In both complexes, silver( I) is tricoordinated. The sac ligand is N-coordinated, while aepip and hepip behave as N-N and N-O bidentate chelating ligands, respectively. The pip rings of both aepip amd hepip ligands adopt typical ‘chair’ conformation. The individual molecules are linked into one-dimensional chains by two N-H···O hydrogen bonds in 1, and one O-H···O hydrogen bond in 2. TG-DTG curves illustrated that the endothermic elimination of aepip and hepip ligands takes place in the early stages of thermal decomposition, while that of the sac moiety occurs exothermically at higher temperatures to give metallic silver

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