Pseudo-oxocarbons complexes - complexation of 2,4-bis(dicyanomethylene)-cyclobutane-1,3-dione dianion with copper. X-ray identification and electrochemical properties of the dianion and copper(I) and (II) complexes

2000 ◽  
Vol 78 (2) ◽  
pp. 280-290 ◽  
Author(s):  
Paul-Louis Fabre ◽  
Christophe Pena ◽  
Anne Marie Galibert ◽  
Brigitte Soula ◽  
Gérald Bernardinelli ◽  
...  
Keyword(s):  
Copper Complexes ◽  
Electrochemical Behaviour ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Polymeric Chains ◽  
Complex Copper

The compound (Ph4P)2(trans-cdcb)·2H2O (trans-cdcb2- = 2,4-bis(dicyanomethylene)-cyclobutane-1,3-dione dianion) has been synthesized and characterized by X-ray crystallography. Crystal data: triclinic, space group P1, a = 10.829(2) Å, b = 11.297(2) Å, c = 11.515(2) Å, α = 79.61(1)°, β = 68.54(1)°, γ = 63.49(1)°, V = 1172.9(4) Å3, Z = 1, R = 0.036, Rw = 0.047. With the dianion as a ligand, two complexes have been obtained and characterized by X-ray crystallography, UV-visible spectroscopy, and electrochemistry. The copper(II) complex [Cu(trans-cdcb)(H2O)4·2H2O]n consists of polymeric chains with copper atoms bonded to two of the nitrile groups of the ligand. Crystal data: monoclinic, space group P21/c, a = 9.6366(6) Å, b = 7.1292(3) Å, c = 10.7018(6) Å, β = 99.603(4)°, V = 724.92(7) Å3, Z = 2, R = 0.026, Rw = 0.041. The copper(I) complex[Cu2(trans-cdcb)(CH3CN)4·2CH3CN]n consists of polymeric chains with copper atoms bonded by all the four nitrile groups of the ligand. Crystal data: monoclinic, space group P21/n, a = 10.654(2) Å, b = 8.736(1) Å, c = 14.654(3) Å, β = 109.01(2)°, V = 1291.3(9) Å3, Z = 2, R = 0.037, Rw = 0.041. In CH3CN solution, the copper complexes are dissociated. Moreover, copper(II) is reduced into copper(I) by the dianion. Electrochemistry in the solid state (polymer coated electrode) showed the redox transitions of the different compounds.Key words: pseudo-oxocarbons, X-ray diffraction, copper(II) complex, copper(I) complex, electrochemical behaviour.

Strukturuntersuchungen an Diaryldichalkogeniden: Die Molekülstrukturen von [2,4,6-(CF3)3C6H2S]2,[2,4,6-Me3C6H2Te]2 und [2-Me2N-4,6-(CF3)2C6H2Te]2 / Structural Investigations of Diaryl Dichalcogenides: The Molecular Structures of [2,4,6-(CF3)3C6H2S]2, [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2

1992 ◽  
Vol 47 (3) ◽  
pp. 305-309 ◽  
Author(s):  
Anja Edelmann ◽  
Sally Brooker ◽  
Norbert Bertel ◽  
Mathias Noltemeyer ◽  
Herbert W. Roesky ◽  
...  
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Structural Investigations ◽  
Space Group ◽  
X Ray

Abstract The Molecular Structures of [2,4,6-(CF3)3C6H2S]2 (1) [2,4,6-Me3C6H2Te]2 and [2-Me2N-4,6-(CF3)2C6H2Te]2 (3) have been determined by X-ray diffraction. Crystal data: 1: orthorhombic, space group P212121, Z = 4, a = 822.3(2), b = 1029.2(2), c = 2526.6(5) pm (2343 observed independent reflexions, R = 0.042); 2: orthorhombic, space group Iba 2, Z = 8, a = 1546.5(2), b = 1578.4(2), c = 1483.9(1) pm (2051 observed independent reflexions, R = 0.030); 3: monoclinic, space group P 21/c, Z = 4, a = 1118.7(1), b = 1536.5(2), c = 1492.6(2) pm, β = 98.97(1)° (3033 observed independent reflexions, R = 0.025).

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.

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.

scholarly journals Indole alkaloids from Vinca erecta type of sarpagine and ajmaline

2019 ◽  
Vol 10 (4) ◽  
pp. 409-416 ◽  
Author(s):  
Shahobiddin Adizov ◽  
Bakhodir Tashkhodjaev
Keyword(s):  
Conformational Changes ◽  
Absolute Configuration ◽  
Indole Alkaloids ◽  
Diffraction Method ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

The single crystal X-ray diffraction method established the absolute configuration of the Vinca erecta indole alkaloids of the akuammidine sarpagine type (3S, 5S, 15R, 16R) and its o-acyl derivative, as well as the type of ajmaline, quebrachidine (2S, 3S, 5S, 7R, 15S, 16R, 17S) and majoridine (2R, 3S, 5S, 7R, 15R, 16S, 17R). Crystal data for C21H24N2O3 (1): orthorhombic, space group P212121 (no. 19), a = 6.3949(5) Å, b = 13.5009(10) Å, c = 22.461(3) Å, Z = 4, 7694 reflections measured (7.64° ≤ 2Θ ≤ 152.294°), 3813 unique (Rint = 0.0798) which were used in all calculations. The final R1 was 0.0680 (I > 2σ(I)) and wR2 was 0.1650 (all data). Crystal data for C23H26N2O4 (2): orthorhombic, space group P212121 (no. 19), a = 9.9730(13) Å, b = 10.2090(10) Å, c = 20.409(3) Å, Z = 4, 7959 reflections measured (8.666° ≤ 2Θ ≤ 151.998°), 4212 unique (Rint = 0.0386) which were used in all calculations. The final R1 was 0.0477 (I > 2σ(I)) and wR2 was 0.1171 (all data). Crystal data for C42H48N4O6 (3): monoclinic, space group P21 (no. 4), a = 8.9320(10) Å, b = 21.515(5) Å, c = 9.5420(10) Å, β = 97.103(10)°, Z = 2, 16677 reflections measured (9.34° ≤ 2Θ ≤ 151.836°), 7393 unique (Rint = 0.0278) which were used in all calculations. The final R1 was 0.0366 (I > 2σ(I)) and wR2 was 0.1037 (all data). Crystal data for C23H28N2O3 (4): orthorhombic, space group P212121 (no. 19), a = 10.636(2) Å, b = 11.208(12) Å, c = 16.725(13) Å, Z = 4, 1650 reflections measured (9.498° ≤ 2Θ ≤ 119.97°), 1650 unique (Rint = 0.0436) which were used in all calculations. The final R1 was 0.0608 (I > 2σ(I)) and wR2 was 0.1720 (all data). In alkaloids such as sarpagine and ajmaline exo, the substituents of alkaloids do not lead to conformational changes of a stable polycyclic framework. In the series of sarpagine, alkaloids form mono-salts in the tetrahedral nitrogen N4, and in indolines of the ajmaline type, the tetrahedral hybridization of the N1 and N4 atoms favors the formation of disols. In V. erecta alkaloids, the exomethylene fragment (C18-C19=C20-C21) of the polycyclic backbone always takes on the E-state.

Preparation and X-ray crystal structures of the arsenic pentafluoride adducts of benzo-2,1,3-thiadiazole and benzo-1,2,3-thiadiazole

1986 ◽  
Vol 64 (5) ◽  
pp. 849-853 ◽  
Author(s):  
Allen Apblett ◽  
Tristram Chivers ◽  
John F. Richardson
Keyword(s):  
Nitrogen Atom ◽  
Crystal Structures ◽  
Benzene Ring ◽  
Heterocyclic Ring ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

The reaction of arsenic pentafluoride with benzo-2,1,3-thiadiazole, 1, or benzo-1,2,3-thiadiazole, 2, in liquid SO2 gave 1:1 adducts that were characterized spectroscopically (infrared and 13C nmr) and by X-ray crystallography. Crystal data: for 1•AsF5, monoclinic, space group P21/n, a = 6.932(1), b = 9.113(1), c = 15.136(2) Å, β = 98.035(7)°, V = 946.8(2) Å3, Z = 4; for 2•AsF5, monoclinic, space group P21/a, a = 7.573(2), b = 13.101(2), c = 9.514(3) Å, β = 90.95(2)°, V = 943.9(4) Å3, Z = 4. The coordination of AsF5 to one of the nitrogen atoms in 1 introduces asymmetry in the heterocyclic ring, with the longer bond lengths being associated with the coordinated nitrogen atom, d(S—N) = 1.633(5) and 1.577(6) Å, d(C—N) = 1.364(7) and 1.339(8) Å. The quinonoid character of the benzene ring is still apparent in the adduct. In 2•AsF5, the AsF5 molecule is coordinated to the nitrogen atom that is bonded to carbon.

Crystal and Molecular Structures of the Functional Lithium Cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph, Me

2000 ◽  
Vol 55 (11) ◽  
pp. 1005-1010 ◽  
Author(s):  
Ulrich Jürgen Bildmann ◽  
Martin Winkler ◽  
Gerhard Müller Fachbereich
Keyword(s):  
Solid State ◽  
Functional Group ◽  
Molecular Structures ◽  
The Other ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal and molecular structures of the phosphinomethyl-substituted lithium cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph (1), Me (2) (tmeda = N,N,N',N'-tetramethylethylenediamine) were determined as their tmeda adducts on the basis of low temperature single crystal X-ray diffraction. (Crystal data: 1: monoclinic, space group P21/n, a = 8.511(5), b = 11.936(2), c = 24.20(1) Å, β = 90.02(3)°, Z = 4.2: monoclinic, space group P21/n, a = 10.887(2), b = 13.326(2), c = 13.131(2) Å, β= 92.872(6)°, Z = 4). In both compounds lithium has a slightly distorted 17 coordination to the cyclopentadienide (Cp) ring. There are no interactions between lithium and the phosphine donors in the solid state as the phosphinomethyl substituents are oriented to the other side of the Cp ring for steric reasons. The isopropene-substituted lithium cyclopentadienide, which is formed as a by-product in the synthesis of phosphinomethyl cyclopentadienides containing a CMe2 bridge, was also structurally characterized as its tmeda adduct [Li(tmeda)][H2C=CMeC5H4] (3). (Crystal data: monoclinic, P21/c, a = 8.00(2), b = 16.701(2), c = 11.942(6) Å, β= 112.68(7)°, Z = 4). As in 1 and 2, lithium is η5 -coordinated to the Cp ring, and there is no interaction of the functional group (isopropene) with lithium.

A comparison of the molecular structures of Dicyclohexyl(N-phenylthiocarbamoyl)-phosphine and Diphenyl(N-phenylthiocarbamoy1)phosphine as determined by X-ray crystallography

1984 ◽  
Vol 37 (10) ◽  
pp. 1991 ◽  
Author(s):  
SW Cowan ◽  
BF Hoskins ◽  
ERT Tiekink
Keyword(s):  
Three Dimensional ◽  
Unit Cell ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Conformational Effects

The crystal and molecular structures of the title compounds, (C6H11)2PC(S)N(H)C6H5(1) and (C6H5)2PC(S)N(H)C6H5(2) have been determined by single-crystal three-dimensional X-ray diffraction techniques. Crystals of (1) are monoclinic, space group P21/c, with eight molecules in the unit cell of dimensions a 20.541(4), b 17.784(2), c 10.2564(9) � and β 94.54(1)�; (2) crystallizes in the triclinic space group P1 with two molecules in the unit cell which has the dimensions a 9.242(2), b 9.994(3), c 10.373(3) �, α 68.56(2), β 71.21(2) and γ 86.00(2)�. Both structures were refined by a least-squares procedure, applying anisotropic thermal parameters to all non-hydrogen atoms, with the use of 3119 and 2971 statistically significant reflections for (1) and (2) respectively; final R 0.055 for (1) and R 0.061 (Rw 0.062) for (2). The N, C(l), S moieties of both (1) and (2) display features consistent with the delocalization of π-electrons. There are notable differences in some of the bond angles between (I) and (2) which have been attributed to conformational effects arising from variations in steric pressures; this may account for the observed differences in reactivity between the two compounds.

Metallorganische Verbindungen für MOCVD-Prozesse: Kristallstruktur des dimeren Addukts [Et3AsXAsCl3]2 / Crystal Structure of the Dimeric Triethylarsine-Arsenictrichloride Adduct, Dimer [Et3AsxAsCl3: Synthesis, Molecular and Crystal Structure

1989 ◽  
Vol 44 (5) ◽  
pp. 560-564 ◽  
Author(s):  
Gerhard Baum ◽  
Arnd Greiling ◽  
Werner Massa ◽  
Benjamin C. Hui ◽  
Jörg Lorberth
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Quantitative Yield ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Arsenic Atom ◽  
Space Group ◽  
X Ray

Reaction of Et3As with AsCl3 in n-pentane yields dimeric [Et3AsxAsCl3]2 in quantitative yield; sublimation in vacuo affords white crystals.X-Ray diffraction data were collected at 133 K (3149 independent observed reflections; R = 0.029. Rw = 0.026). Crystal data: monoclinic space group P21/c, a = 761.9(8). b = 1118.8(4). c = 1406.0(14) pm; β = 100.90(4)°. Ζ = 2 dimers.The dimer contains a planar As2Cl6-unit with terminal and bridging As-Cl bonds; each arsenic atom is bonded to a Et3As molecule via an arsenic-arsenic bond. The dimer thus has pseudo four- and six-coordinate arsenic atoms.

Synthese und Struktur der Basenaddukte von Kupfer(I)-Halogeniden mit Dimethylsulfid und Tetrahydrothiophen / Synthesis and Crystal Structure of Lewis Base Adducts of Copper(I)-Halides with Dimethylsulfide and Tetrahydrothiophene

1992 ◽  
Vol 47 (9) ◽  
pp. 1276-1280 ◽  
Author(s):  
Harald Maelger ◽  
Falk Olbrich ◽  
Jürgen Kopf ◽  
Dirk Abeln ◽  
Erwin Weiss
Keyword(s):  
Copper Complexes ◽  
Layer Structure ◽  
Lewis Base ◽  
Monoclinic Space Group ◽  
Direct Reaction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Polymeric Chains ◽  
Polymeric Layer

Copper complexes of the general formula [(CuX)a(L)b]n with L = tetrahydrothiophene (THT) or dimethylsulfide (DMS) and X = Cl, Br or I are formed by direct reaction of copper(I)halides with the corresponding ligands. All compounds have been characterized by X-ray crystallography. [(CuCl)(dms)]„ (la) crystallizes in the monoclinic space group P 21/c (a = 762.6(1), b = 638.0(2), c = 1154.8(3) pm, β = 108.10(2)° and Ζ = 4), [(Cul)(dms)1.5]n (le) in Ι 2/a (a = 1202.9(2), b = 780.0(2), c = 1714.6(2) pm, β = 97.92(2)° and Ζ = 8), [(CuCl)(tht)1.5]n (2a) in C 2/c (a = 1244.7(2), b = 1610.3(2), c = 988.9(2) pm,β = 111.51(1)° and Z = 8) and [(CuBr)(tht), 5]„ (2b) also in C2/c (a = 1159.6(2), b = 1638.8(3), c = 1015.1(2) pm, β= 109.44(1)° and Z = 8).The crystal structures of [(CuBr)(dms)]„ (lb) and [(CuI)(tht)2]2 (2 c) are already known. In all structures the central copper atom is coordinated to two halide and two sulphur atoms with formation of a distorted tetrahedron. Two copper and two halogen atoms form planar Cu2X2 rings which are linked by the sulphur atoms of the thioethers. The thioether ligands can either function as bridges or they are coordinated “end on”. In la and lb a polymeric layer structure is found, while 1 c, 2a und 2b form polymeric chains. 2c forms dimers. Cu · · · Cu distances are in the range of 268.4 to 298.3 pm and Cu–S bond lengths are between 228.1 and 237.2 pm.

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

Sign in / Sign up

Export Citation Format

Share Document