Zirconium alkyl and borohydride complexes stabilized by a sterically demanding anionic organic amide. The crystal structures of ZrMeL3 (2) and Zr(BH4)L3 (3) (L = (3,5-Me2Ph)N(Ad); Ad = adamantyl)

1997 ◽  
Vol 75 (11) ◽  
pp. 1494-1499 ◽  
Author(s):  
Aparna Kasani ◽  
Sandro Gambarotta ◽  
Corinne Bensimon
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Crystal Data ◽  
Lithium Amide ◽  
X Ray ◽  
X Ray Crystallography ◽  
Sterically Demanding

The lithium amide [3,5-Me2PhN(Ad)]Li•Et2O (L) reacts with ZrCl4(THF)2 to give ZrClL3. Reactions of ZrClL3 with MeLi and NaBH4 produce the corresponding ZrMeL3 (2) and Zr(BH4)L3 (3), respectively. The molecular structures of 2 and 3 were determined by X-ray crystallography. Crystal data are as follows. 2: C55H75N3Zr, FW 869.45, orthorhombic, Pcab; a = 19.2436(3) Å,b = 45.9342(4) Å, c = 21.2935(3) Å, V = 18822.2(4) Å3Z = 8; 3: C54H76BN3Zr, FW 869.25, orthorhombic; Pbc21, a = 11.5399(3) Å,b = 19.4091(4) Å, c = 20.4471(5) Å,V = 4579.72(19) Å3Z = 4. Keywords: zirconium, amide, alkyl, borohydride, structure.

Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXI The Crystal and Molecular Structures of the Unsolvated Forms of Dibromotris(triphenylphosphine)dicopper(I) and 'step' Tetrabromotetrakis(triphenyl-phosphine)tetracopper(I)

1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Lewis Base ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.

Syntheses, Crystal Structures and Electrochemical Properties of Acetylacetonato-Ruthenium Complexes Containing Substituted Pyridine Ligands

2013 ◽  
Vol 68 (9) ◽  
pp. 993-999 ◽  
Author(s):  
Xiuli Wu ◽  
Rufei Ye ◽  
Ai-Quan Jia ◽  
Qun Chen ◽  
Qian-Feng Zhang
Keyword(s):  
Electrochemical Properties ◽  
Crystal Structures ◽  
Zinc Dust ◽  
Ruthenium Complexes ◽  
Reducing Agent ◽  
Molecular Structures ◽  
X Ray ◽  
X Ray Crystallography ◽  
Crystal And Molecular Structures ◽  
Pyridine Ligands

Treatment of Ru(acac)3 with 2-cyano-pyridine and 3,5-dimethyl-pyridine in the presence of zinc dust as reducing agent in refluxing THF afforded the ruthenium(II) complexes cis-[RuII(acac)2(2- CN-py)2] (1) and cis-[RuII(acac)2(3,5-Me2-py)2] (2), respectively. Interaction of Ru(acac)3 with 3- Me-pyridine and 3,5-Me2-pyridine in the presence of Br2 in refluxing THF gave the ruthenium(III) complexes [RuIII(acac)Br2(3-Me-py)2] (3) and [RuIII(acac)Br2(3,5-Me2-py)2] (4), respectively. The four complexes have been spectroscopically and electrochemically characterized, and their crystal and molecular structures have been established by X-ray crystallography

Synthesis, Characterization and Crystal Structures of 1,2-Disubstituted Ferrocenyl Stibines

2012 ◽  
Vol 67 (1) ◽  
pp. 36-40
Author(s):  
Diego Pérez ◽  
Pankaj Sharma ◽  
Ana M. Ortiz ◽  
Armando Cabrera ◽  
Simon Hernández ◽  
...  
Keyword(s):  
Solid State ◽  
Acetic Anhydride ◽  
Nucleophilic Substitution ◽  
Sodium Hydroxide ◽  
Crystal Structures ◽  
Analytical Methods ◽  
Molecular Structures ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pendant Arm

New 1,2-disubstituted ferrocenyl stibines containing a -CH2OR pendant arm were synthesized and characterized by various spectral and analytical methods. Nucleophilic substitution of rac-diphenyl[( 2-trimethylammoniomethylferrocen-1-yl)]stibine iodide by methanol produces compound Fc(CH2OMe)SbPh2 (1). The acetylation of diphenyl(2-dimethylaminomethylferrocen-1-yl)stibine by acetic anhydride affords compound Fc(CH2OCOCH3)SbPh2 (2), which on further reaction with sodium hydroxide affords the alcohol Fc(CH2OH)SbPh2 (3). The molecular structures of the stibines 1, 2 and 3 were determined by X-ray crystallography. None of the heterobimetallic compounds containing a -CH2OR arm shows hypervalent interactions in the solid state. By contrast, hypervalent interactions were found in ferrocenyl stibines with a -CH2NR2 pendant arm.

Synthesis and characterization of [MII(bqb)] (M = Co, Ni, Cu), [N(n-Bu)4][CoIII(bqb)(CN)2], and [N(n-Bu)4][CoIII(bqb)(N3)2] containing deprotonated N,N'-bis(2-quinolinecarboxamide)-1,2-benzene (bqb) – X-ray crystal structures of [NiII(bqb)] and [N(n-Bu)4][CoIII(bqb)(N3)2]

2006 ◽  
Vol 84 (7) ◽  
pp. 971-978 ◽  
Author(s):  
Soria Meghdadi ◽  
Mehdi Amirnasr ◽  
Vratislav Langer ◽  
Alison Zamanpoor
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Square Planar ◽  
Distorted Octahedral ◽  
Elemental Analyses

Cobalt(II), nickel(II), copper(II), and two cobalt(III) complexes of a new dianionic ligand, bqb, [H2bqb = N,N'-bis(2-quinolinecarboxamide)-1,2-benzene] have been synthesized and characterized by elemental analyses, IR, and 1H NMR spectroscopy. The crystal and molecular structures of the [Ni(bqb)] (2) and [N(n-Bu)4][CoIII(bqb)(N3)2] (5) complexes were determined by X-ray crystallography. Complex 2 crystallizes in the monoclinic space group C2/c with a distorted square-planar structure including two short Ni–N (1.848 Å) and two long Ni–N (1.958 Å) bonds. The structure consists of sheets formed in the plane parallel to the b axis and diagonal to vectors a and c by intermolecular hydrogen bonds. Complex 5 crystallizes in the monoclinic space group C2 with a distorted octahedral structure. The [N(n-Bu)4]+ ion is disordered at the C3A and C4A atoms of one Bu. The IR and 1H NMR spectra of the complexes are also discussed.Key words: N4-dianionic amido ligand (bqb), (bqb) complexes of Co(II), Ni(II), Cu(II), and Co(III), azide, cyanide, X-ray crystal structures.

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.

gem-Dibromovinyl boron dipyrrins: synthesis, spectral properties and crystal structures

2019 ◽  
Vol 48 (30) ◽  
pp. 11492-11507
Author(s):  
Hasrat Ali ◽  
Brigitte Guérin ◽  
Johan E. van Lier
Keyword(s):  
Crystal Structures ◽  
Surface Analysis ◽  
Spectral Properties ◽  
Hirshfeld Surface ◽  
Molecular Structures ◽  
Hirshfeld Surface Analysis ◽  
X Ray ◽  
X Ray Crystallography

New asymmetric/symmetric BODIPY derivatives, bearing gem-dibromovinyl substituents were synthesized and studied for their absorption, fluorescence, solvatochromism, X-ray crystallography and Hirshfeld surface analysis to determine molecular structures.

Crystal structures of dihydroquercetin 3-acetate and dihydroquercetin 3,3'4',7-tetraacetate: hydrogen bonding in 5-hydroxyflavanones

1999 ◽  
Vol 77 (8) ◽  
pp. 1436-1443 ◽  
Author(s):  
Eberhard Kiehlmann ◽  
Kumar Biradha ◽  
Konstantin V Domasevitch ◽  
Michael J Zaworotko
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Crystal Structures ◽  
Crystal Packing ◽  
Heterocyclic Ring ◽  
Molecular Structures ◽  
Crystal Data ◽  
Aromatic Rings ◽  
X Ray

The molecular structures of dihydroquercetin 3-acetate 3 and dihydroquercetin 3,3',4',7-tetraacetate 4 were determined by single crystal X-ray analysis. Comparison of their crystal data with those of 16 known 5-hydroxyflavanones shows intramolecular O(5)-H···O(4)=C hydrogen bonding, preference for nearly perpendicular orientation of the two aromatic rings and preferred sofa conformation of the heterocyclic ring. The major stabilizing force in the crystal packing pattern of 3 is intermolecular hydrogen bonding.Key words: crystal structure, dihydroquercetin, flavanones, hydrogen bonding.

scholarly journals Die Kristall- und Molekülstrukturen der Verbindungen [Cl4–xSn{Co(CO)4}x] mit x = 1,2 und 3 / The Crystal and Molecular Structures of the Compounds [Cl4-xSn{Co(CO)4}x] with x = 1,2 and 3

1991 ◽  
Vol 46 (2) ◽  
pp. 187-191 ◽  
Author(s):  
Peter Klüfers
Keyword(s):  
Crystal Structures ◽  
Molecular Structures ◽  
Trigonal Bipyramid ◽  
X Ray ◽  
X Ray Crystallography ◽  
Crystal And Molecular Structures ◽  
Distorted Trigonal Bipyramid

The crystal structures of the compounds [Cl3SnCo(CO)4] 1, [Cl2Sn{Co(CO)4}2]2, and [ClSn{Co(CO)4}3]3, have been determined by X-ray crystallography. Sn is co-ordinated tetrahedrally by Cl- and Co-substituents, the co-ordination polyhedron of Co is a distorted trigonal bipyramid. The Sn -Cl- and the Sn-Co-distances both increase from 1 to 3 (Sn -Co: 247.7 in 1, 253.2 in 2, and 260.6 pm in 3).

Synthesis, structural characterization and catalytic activity of chlororuthenium(II) complexes with substituted Schiff base/phosphine ancillary ligands

2020 ◽  
Vol 75 (9-10) ◽  
pp. 851-857
Author(s):  
Chong Chen ◽  
Fule Wu ◽  
Jiao Ji ◽  
Ai-Quan Jia ◽  
Qian-Feng Zhang
Keyword(s):  
Schiff Base ◽  
Catalytic Activity ◽  
Structural Characterization ◽  
Room Temperature ◽  
Molecular Structures ◽  
Cationic Complex ◽  
Neutral Complex ◽  
Ancillary Ligands ◽  
X Ray ◽  
X Ray Crystallography

AbstractTreatment of [(η6-p-cymene)RuCl2]2 with one equivalent of chlorodiphenylphosphine in tetrahydrofuran at reflux afforded a neutral complex [(η6-p-cymene)RuCl2(κ1-P-PPh2OH)] (1). Similarly, the reaction of [Ru(bpy)2Cl2·2H2O] (bpy = 2,2′-bipyridine) and chlorodiphenylphosphine in methanol gave a cationic complex [Ru(bpy)2Cl(κ1-P-PPh2OCH3)](PF6) (2), while treatment of [RuCl2(PPh3)3] with [2-(C5H4N)CH=N(CH2)2N(CH3)2] (L1) in tetrahydrofuran at room temperature afforded a ruthenium(II) complex [Ru(PPh3)Cl2(κ3-N,N,N-L1)] (3). Interaction of the chloro-bridged complex [Ru(CO)2Cl2]n with one equivalent of [Ph2P(o-C6H4)CH=N(CH2)2N(CH3)2] (L2) led to the isolation of [Ru(CO)Cl2(κ3-P,N,N-L2)] (4). The molecular structures of the ruthenium(II) complexes 1–4 have been determined by single-crystal X-ray crystallography. The properties of the ruthenium(II) complex 4 as a hydrogenation catalyst for acetophenone were also tested.

scholarly journals A mixed chirality α-helix in a stapled bicyclic and a linear antimicrobial peptide revealed by X-ray crystallography

2021 ◽  
Author(s):  
Stéphane Baeriswyl ◽  
Hippolyte Personne ◽  
Ivan Di Bonaventura ◽  
Thilo Köhler ◽  
Christian van Delden ◽  
...  
Keyword(s):  
Antimicrobial Peptides ◽  
Antimicrobial Peptide ◽  
Crystal Structures ◽  
X Ray ◽  
X Ray Crystallography ◽  
Α Helix

We report the first X-ray crystal structures of mixed chirality α-helices comprising only natural residues as the example of bicyclic and linear membrane disruptive amphiphilic antimicrobial peptides containing seven l- and four d-residues.

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