scholarly journals Komplexe offenkettiger und zyklischer Diazathiaalkane. Die Kristallstrukturen von 1,7-Diaza-4-thiaheptan-tricarbonyl-molybdän(0), 1-Thia-4,7-diazacycIononan-tricarbonyI-molybdän(0) und 1-Thia-4,7-diazacyclononan-tricarbonyl-rhenium(I)-bromid

1987 ◽  
Vol 42 (7) ◽  
pp. 867-873 ◽  
Author(s):  
Peter Hoffmann ◽  
Andreas Steinhoff ◽  
Rainer Mattes
Keyword(s):  
Monoclinic Space Group ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Bond Lengths

Abstract The reactions of Mo(CO)6, W(CO)6 and Re(CO)6Br with the ligand l-thia-4,7-diazacyclononane (C6H14N2S = L) yield crystals of LMo(CO)3 (4a), LW(CO)3 (4b) and LRe(CO)3Br (5). A n improved synthesis of L has been developed, and the structures of 4a and 5 have been determined. Crystal data: 4a, monoclinic, space group P21/n, a = 791.3(4), b - 1332.6(4), c = 1149.2(6) pm, β - 98.96(4)°, Z = 4.1841 reflexions, R = 0.045. 5, orthorhombic, space group Pbca, a = 1413.4(5), b = 1398.0(5), c = 1409.5(5) pm, Z = 8.2619 reflexions, R = 0.038. Both crystals contain pseudooctahedral LM(CO)3 moieties, with facial coordination of the CO molecules. The Re - N bond lengths (average 220.3(4) pm) are rather short. The structure of L 'Mo(CO)3 (3) with the acyclic ligand 1,7-diaza-4-thiaheptane (C4H10N2S = L') was also determined. Crystal data: monoclinic, space group P21/c, a = 682.8(2), b = 1213.0(3), c = 1253.0(3), β = 99.74°, Z = 4.1889 reflexions, R = 0.023.

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).

The Crystal and Molecular Structures of Two Modifications of cis-Dichloro-mer-tris-(dimethylphenylphosphine)hydridoiridium(III)

1988 ◽  
Vol 41 (3) ◽  
pp. 283 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Heavy Atom ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Metal Ligand ◽  
Ligand Bond

The structures of two crystalline modifications of mer -(Pme2Ph)3H-cis-Cl2IrIII, (1), have been determined from single-crystal X-ray diffraction data. Modification (A) is monoclinic, space group P21/c with a 12.635(1), b 30.605(3), c 14.992(2)Ǻ, β 110.01(2)° and Z = 8. Modification (B) is orthorhombic, space group Pbca with a 27.646(3), b 11.366(1), c 17.252(2)Ǻ and Z = 8. The structures were solved by conventional heavy atom techniques and refined by full-matrix least- squares analyses to conventional R values of 0.037 [(A), 8845 independent reflections] and 0.028 [(B), 5291 independent reflections]. Important bond lengths [Ǻ] are Ir -P(trans to Cl ) 2.249(1) av. (A) and 2.234(1) (B), Ir -P(trans to PMe2Ph) 2.339(2) av. (A) and 2.344(1), 2.352(1) (B), Ir-Cl (trans to H) 2.492(2), 2.518(2) (A) and 2.503(1) (B) and Ir-Cl (trans to PMe2Ph)2.452(2) av. (A) and 2.449(1)(B). Differences in chemically equivalent metal- ligand bond lengths emphasize the importance of non-bonded contacts in determining those lengths.

Strukturen der mehrkernigen nickelthiolato-komplexe [(μ-SMe)2(Ni(MeNHCS2))2] und cyclo-[(μ-SMe)2Ni]6 / Structures of Two Polynuclear Nickel-Thiolato-Complexes [(μ-SMe)2(Ni(MeNHCS2))2] and cyclo-[(μ-SMe)2Ni]6

1994 ◽  
Vol 49 (6) ◽  
pp. 770-772 ◽  
Author(s):  
Klaus Schulbert ◽  
Rainer Mattes
Keyword(s):  
Crystal Structures ◽  
Nickel Acetate ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Dithiocarbamic Acid ◽  
Coordination Spheres ◽  
Partial Degradation ◽  
Acid Esters

The reactions of N-substituted dithiocarbamic acid esters and nickel acetate yield, by partial degradation of the esters, the polynuclear nickel thiolato complexes cyclo-[(μ-SMe)2Ni]6, 1 and [(μ-SMe)2(Ni(MeNHCS2))2, 2. Their crystal structures have been determined. The Ni coordination spheres are comprised of four sulfur atoms in a planar arrangement. 1 is a second, highly symmetrical modification of the already known cyclic hexamer Ni6(SMe)12. In 2 two Ni(PhNHCS2) moieties are bridged to dimers by thiolato groups. Two of these dimers are connected to a tetramer by weak axial Ni-S interactions. Crystal data for 1: monoclinic, space group P21/n, a = 986.1(2), b = 1308.1(3), c = 1228.6(2) pm, β = 96.07(3)°, Z = 2, R = 0.072, Rw = 0.062, 3797 reflections. 2: orthorhombic, space group Pnma, a = 1790.0(4), b = 1806.7(4), c = 934.4(2) pm. Z = 4, R = 0.061, Rw = 0.051, 2079 reflections

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.

Steric Modification of Metal-Phosphorus Bond Lengths: the Preparation, Characterization and CrystalStructures of mer-trans-(PPri3)2(Pme2Ph)-Cl-cis-H2IrIII(1) and mer-trans-(PPri3)2(PMe2Ph)H3IrIII

1995 ◽  
Vol 48 (6) ◽  
pp. 1183 ◽  
Author(s):  
EJ Ditzel ◽  
GB Robertson
Keyword(s):  
Chloride Content ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Steric Crowding ◽  
Unit Increase

The syntheses and subsequent characterization of the complexes mer -trans-(PPri3)2(Pme2Ph)-Cl-cis-H2IrIII(1) and mer-trans-(PPri3)2(PMe2Ph)H3IrIII (2) by n.m.r. and by low temperature (153�5 K) X-ray diffraction analyses are reported. Crystals of (1) are monoclinic, space group P21/c with a 19.277(2), b 9.020(1), c 17.657(2) Ǻ, β 101.40(1)° and Z 4. Crystals of (2) are orthorhombic, space group P212121, with a 19.373(3), b 18.724(2), c 8.113(1) Ǻ and Z 4. Full-matrix least-squares analyses converged with R = 0.027 and wR = 0.031 for (1) (3243 reflections), and R = 0.030 and wR = 0.038 for (2) (2892 reflections). Consistent with previous observation, the unit increase in chloride content (in place of hydride) in (1) is accompanied by a global lengthening of 0.036 Ǻ (av.) in the Ir -P bond lengths cf. those in (2). Also, because of increased steric crowding (two PPri3 ligands in place of two Pme2Ph), the Ir-PMe2Ph bond in (1) is 0.019(2) Ǻ longer than the chemically equivalent bond in mer-(PMe2Ph)3Cl-cis-H2IrIII. In previously reported complexes in this series metrically similar increases in Ir-PMe2Ph distances result from the replacement of just one Pme2Ph ligand by PPri3.

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 structure of 2-chloro-1,3-dimethyldiaza-2-arsenane, 1,3-dimethyldiaza-2-arsenanium tetrachlorogallate, and butadiene cycloadducts of diazarsenium cations

1996 ◽  
Vol 74 (11) ◽  
pp. 2209-2216 ◽  
Author(s):  
Neil Burford ◽  
Charles L.B. Macdonald ◽  
Trenton M. Parks ◽  
Gang Wu ◽  
Borzena Borecka ◽  
...  
Keyword(s):  
Solid State ◽  
Chloride Ion ◽  
2D Nmr ◽  
Diels Alder ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
State Structure ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

1,3-Dimethyldiaza-2-arsenanium tetrachlorogallate (crystal data: C5H12AsCl4GaN2, M = 386.61, orthorhombic, space group Pca21, a = 14.432(3) Å, b = 6.7580(14) Å, c = 13.905(3) Å, V = 1356.2(5) Å3) is synthesized by the routine chloride ion abstraction procedure from 2-chloro-1,3-dimethyldiaza-2-arsenane (crystal data: C5H12AsClN2, M = 210.54, monoclinic, space group P21/n, a = 7.206(1) Å, b = 9.650(1) Å, c = 13.021(2) Å, β = 99.61(2)°, V = 892.8(2) Å3). X-ray crystallographic studies of both compounds are described together with that for 2-chloro-1,3-dimethyldiaza-2-arsolidine (crystal data: C4H10AsClN2, M = 196.51, monoclinic, space group P21/n, a = 6.959(7) Å, b = 9.23(2) Å, c = 12.14(2) Å, β = 95.4(1)°, V = 777(4) Å3) providing useful structural comparisons. In contrast to the closely related arsolidinium salts, the diazarsenanium gallate exhibits a monomeric solid state structure. Rapid and quantitative cycloaddition reactions of the diazarsolidinium and diazarsenanium cations with 2,4-dimethylbutadiene give similar cycloadducts. The Diels–Alder type arsolidinium adduct is structurally characterized (crystal data: C10H20AsCl4GaN2, M = 454.73, orthorhombic, space group Pca21, a = 18.471(2) Å, b = 7.000(2) Å, c = 13.738(1) Å, V = 1776.2(8) Å3), and the related structure of the arsenanium cycloadduct is confirmed by 2D NMR. Key words: arsenium, cycloadditions, arsenanium, Diels–Alder, cyclochloroarsines.

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.

Conformational studies on cyclohexa-1,4-diene derivatives. The crystal and molecular structures of 1,2,4,5-tetraphenyl-3,6-dicarbomethoxycyclohexa-1,4-diene and 1,2-dicarbomethoxy-4,5-dimethylcyclohexa-1,4-diene

1978 ◽  
Vol 56 (10) ◽  
pp. 1358-1363 ◽  
Author(s):  
M. J. Bennett ◽  
J. T. Purdham
Keyword(s):  
Direct Methods ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
Orthorhombic Space Group ◽  
Small Deviations ◽  
Conformational Studies ◽  
Space Group ◽  
Bond Lengths ◽  
Least Squares Techniques

1,2,4,5-Tetraphenyl-3,6-dicarbomethoxycyclohexa-1,4-diene crystallizes in the monoclinic space group I2/a (a non-standard setting of C2/c) with a = 20.052(2), b = 5.756(1), c = 22.782(2) Å, β = 95.73(1)°, and Z = 4. 1,2-Dicarbomethoxy-4,5-dimethylcyclohexa-1,4-diene crystallizes in the orthorhombic space group Pbca with a = 25.627(2), b = 11.240(1), c = 8.342(1) Å, and Z = 8. Both structures were solved by direct methods and refined by full matrix least-squares techniques to R = 0.040 and R = 0.036, respectively. Carbon–carbon double bond lengths are similar in the two compounds (1.326 and 1.333 Å, respectively), but the single bond lengths are significantly longer in l,2,4,5-tetraphenyl-3,6-dicarbomethoxycyclohexa-1,4-diene (1.518 Å) compared with the 1.493 Å average found in 1,2-dicarbomethoxy-4,5-dimethyl- cyclohexa-1,4-diene. This and the fact that there are also small deviations from planarity in the former compound are thought to be due to the presence of substituents on the methylenic carbon atoms.

The Crystal Structures of [N,N’-Bis(3-methoxysalicylidene)-1,3- diaminopropane]nickel(II) and -copper(II)

2004 ◽  
Vol 59 (2) ◽  
pp. 228-232 ◽  
Author(s):  
Ayhan Elmali ◽  
Celal T Zeyrek ◽  
Yalcin Elerman
Keyword(s):  
Crystal Structures ◽  
Mirror Symmetry ◽  
Distorted Octahedral Geometry ◽  
Planar Geometry ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Distorted Octahedral

[N,N′’-Bis(3-methoxysalicylidene)-1,3-diaminopropane]nickel(II) dihydrate [Ni(C19H20N2O4)· 2(H2O)] 1 and [N,N′-bis(3-methoxysalicylidene)-1,4-diaminobutane]copper(II) [Cu(C20H22N2O4)] 2 have been synthesized and their crystal structures determined. Crystals of compound 1 are orthorhombic, space group Pnma, a = 7.509(3), b = 22.070(7), c = 11.532(4) Å, V = 1611.1(12) Å3, Z = 4 and Dc = 1.498 g·cm−3. The molecule 1 has mirror symmetry, but the ligand is not planar. The two parts of the Schiff base moieties are folded so as to form an angle of 21.6(1)°. The Ni atom is in a distorted octahedral geometry and coordinated by the donor atoms of the ligand in the horizontal plane and of two water molecules. Crystals of compound 2 are monoclinic, space group P21/c, a = 9.488(1), b = 21.918(3), c = 8.413(1) Å, β = 91.45(1)°, V = 1749.0(4) Å3, Z = 4 and Dc = 1.587 g·cm−3. The Cu atom is coordinated by an N2O2 donor set from the imine-phenol ligand in a distorted planar geometry, with the two phenolate O atoms deprotonated. The Cu-O bond lengths are 1.854(3) and 1.868(3)Å . The Cu-N bond lengths are 1.931(3) and 1.950(3) Å, the dihedral angle between the two 3-methoxysalicylidene groups is 43.4(1)°.

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