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1.
Uzma Habib Amin Badshah Ulrich Flörke Rizwana Aleem Qureshi Bushra Mirza Nazar-ul-Islam Azeem Khan 《Journal of chemical crystallography》2009,39(10):730-734
Abstract The reaction of Cu(OOCCH3)2·H2O with (2,4-diamino-5-(3′,4′,5′-trimethoxybenzyl) pyrimidine (trimethoprim) in ethanolic solution at 80 °C affords the title
complex which has been characterized by elemental, IR, and NMR (1H and 13C).The crystal structure has been determined by single crystal X-ray diffraction. Compound 1 (C36H48Cu2N8O14) is triclinic, space group P-1 with a = 7.2676(4) ?, b = 11.6721(7) ?, c = 12.8279(8) ?, α = 95.839(1)°, β = 93.456(1)°, γ = 105.541(1)°, Z = 1. Two copper atoms are coordinated directly to each other as well as are held together by four bridging aceto groups.
Each copper atom is also bonded opposite the Cu–Cu vector to a trimethoprim molecule through the N(1) atom of the pyrimidine
ring. Trimethoprim acts as a monodentate ligand through the pyrimidine nitrogen N(1) atom. The complex was screened for the
activity against several bacteria, showing more activity against bacteria as compared to trimethoprim.
Graphical Abstract To enhance the activity of trimethoprim, its derivative was prepared and there bacterial activity against several bacteria
was analyzed.
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2.
Audra F. Gushwa Yamina Belabassi Jean-Luc Montchamp Anne F. Richards 《Journal of chemical crystallography》2009,39(5):337-347
Abstract The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities,
differences and 31P chemical shifts compared. A series of seven trityl-substituted phosphorus-containing compounds have been characterized by
single crystal X-ray diffraction. Ph3CPPh2, 1, a bulky P(III) compound crystallizes in the triclinic space group , a = 7.5624(6) ?, b = 9.5470(8) ?, c = 16.9722(14) ?, α = 83.4720(10)°, β = 80.541(2)°, γ = 68.1580(10)°, the borane complex of 1, 2, Ph3CPPh2(BH3) crystallizes as monoclinic colorless crystals, P21/c, a = 10.0972(12) ?, b = 9.6955(12) ?, c = 25.197(3) ?, β = 90.258(2)°. The analogous methyl substituted, 3, Ph3CPMe2(BH3) is monoclinic, C2/c, a = 15.628(3) ?, b = 12.770(3) ?, c = 18.406(4) ?, β = 103.968(3)°. Compounds 4–7 are trityl substituted P(V) compounds: Ph3CP(Ph)(O)(OH), 4, crystallizes in the triclinic space group , a = 8.9847(18) ?, b = 9.7443(19) ?, c = 12.786(3) ?, α = 72.045(3)°, β = 72.031(3)°, γ = 78.769(3)°. Esterification of 4 affords TrCP(O)(Ph)OBn 5, space group, P21/c, a = 7.9196(5) ?, b = 31.701(2) ?, c = 19.8062(13) ?, β = 99.7750(10)°. A phosphonate diester was also characterized, Ph3CP(O)(OEt)2, 6, triclinic, , a = 7.9521(17) ?, b = 9.2205(19) ?, c = 14.471(3) ?, α = 85.906(4)°, β = 83.031(4)°, γ = 68.283(4)°. Treatment of the trityl H-phosphinic acid, Ph3CPO2H2, with elemental selenium yields yellow crystals of 7, [Ph3CP(O)(OH)Se]2, P21/c, a = 9.0603(4) ?, b = 22.3652(11) ?, c = 16.9134(7) ?, β = 107.035(2)°. In our efforts to isolate a nickel-phosphine complex, two Ni(II) complexes were crystallographically analyzed,
[Ni(OP(H)Ph2)6]2BF4
−
8 and 9. Complex 8 with an uncoordinated BF4
− ion crystallizes as yellow orthorhombic crystals, Pbca, a = 18.8247(12) ?, b = 18.5518(12) ?, c = 21.0976(14) ?, while crystals of 9 are trigonal, , a = b = 13.1545(12) ?, c = 68.461(9) ?.
Graphical Abstract The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities,
differences and 31P chemical shifts compared.
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3.
Saroj K. S. Hazari Debashish Palit Tapashi G. Roy Sukla Rakshit Julio Zukerman-Schpector Edward R. T. Tiekink 《Journal of chemical crystallography》2009,39(4):261-265
Abstract The title dinuclear complex, [(cis-MoO2L)(μ-O)(cis-MoOL(OH2)], was characterized as a chloroform solvate. In this structure, one Mo atom features a cis-[MoO2]2+ core to which is also bonded a dinegative, tridentate S-benzyl 3-(2-hydroxyphenyl)methylenedithiocarbazate ligand (= L), via sulfur-, oxygen-, and nitrogen-donors, and a water molecule
completes the distorted octahedral coordination geometry. A similar NO4S donor set is found for the other Mo atom but in this case, the water molecule is substituted by a bridging oxo atom derived
from the first Mo species. Two dimers associate via cooperative O–H⋯O hydrogen bonds to form a supramolecular dimer which,
in turn, are linked into supramolecular chains via O–H⋯N hydrogen bonding. The complex crystallizes in the triclinic space
group P-1 with a = 10.4714(12) ?, b = 10.7627(14) ?, c = 16.708(2) ?, α = 87.916(7)°, β = 76.249(6)°, γ = 83.610(7)°, and Z = 2.
Index Abstract Dinuclear [(cis-MoO2L)(μ-O)(cis-MoOL(OH2)], characterized as a chloroform solvate, with octahedral Mo centers, are connected into supramolecular dimers via O–H⋯O
hydrogen bonding which are connected via O–H⋯N hydrogen bonds into chains.
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4.
James E. Johnson Diana C. Canseco Debra D. Dolliver John A. Schetz Frank R. Fronczek 《Journal of chemical crystallography》2009,39(5):329-336
Abstract Three aplysinopsin analogs were synthesized by reacting 5-bromo-5-fluoro- and 6-bromoindole-3-carboxaldehyde with either creatinine
or 2-imino-1,3-dimethyl-imidazolidin-4-one or 2-imino-1-methyl-3-ethylimidazolidin-4-one Single crystal structures on 5-bromo-4′-de-N-methylaplysinopsin DMF solvate [from creatinine, space group P21/n, lattice parameters a = 13.117(3) ?, b = 8.6663(15) ?, c = 14.743(3) ?, β = 99.538(10)° at 173 K], 5-fluoroaplysinopsin DMF
solvate [from 2-imino-1,3-dimethyl-imidazolidin-4-one, space group P21/c, lattice parameters a = 11.114(3) ?, b = 19.118(2) ?, c = 8.503(2) ?, β = 112.290(7)°], and 6-bromoindole-3-carboxaldehyde
(space group P21/n, lattice parameters a = 7.657(2) ?, b = 7.933(2) ?, c = 13.521(3) ?, β = 99.046(13)°) have been determined. Characterizations
include spectrometric identifications employing IR, UV, HRMS, and 1H and 13C NMR. 5-Bromo-4′-de-N-methylaplysinopsin and 5-fluoroaplysinopsin exist in the E configuration.
Index Abstract Single crystal X-ray structural analyses were carried out on 5-bromo-4′-de-N-methylaplysinopsin, 5-fluoroaplysinopsin, and 6-bromoindole-3-carboxaldehyde.
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5.
Ilia A. Guzei Howard E. Zimmerman Sergey Shorunov Lara C. Spencer 《Journal of chemical crystallography》2009,39(6):399-406
Abstract 2,3-Diphenyl-1-naphthol (1) undergoes two unexpected reactions under different conditions. Compound (1) was heated in DMSO-d6 and underwent a Pummerer type thermal reaction to give two isomeric products, 1-(methylthio)methoxy-2,3-diphenyl naphthol-d5 which crystallized in the space group with a = 7.1610(9) ?, b = 11.2795(15) ?, c = 12.8905(17) ?, α = 114.049(2)°, β = 96.589(2)°, and γ = 102.945(2)°, and 2-(methylthio)methyl-2,3-diphenyl 1(2H)-naphthalenone-d5 which crystallized in the space group with a = 8.5981(5) ?, b = 10.4374(6) ?, c = 11.1078(6) ?, α = 78.748(2)°, β = 67.709(2)°, and γ = 83.184(2)°. Photolysis (254 nm) of (1) resulted in 2,2′,3,3′-tetraphenyl-1,1′-bi-2-naphthol which crystallized in the space group P21/c with a = 26.3616(11) ?, b = 10.1707(4) ?, c = 23.3376(9) ?, and β = 99.034(2)°.
Graphical Abstract When 2,3-diphenyl-1-naphthol was heated in DMSO-d6 two unexpected isomers, 1-(methylthio)methoxy-2,3-diphenyl naphthol-d5 and the racemate 2-(methylthio)methyl-2,3-diphenyl 1(2H)-naphthalenone-d5 were produced. Photolysis in THF at 254 nm led to the unexpected product 2,2′,3,3′-tetraphenyl-1,1′-bi-2-naphthol. All structures
were elucidated by X-ray crystallography.
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6.
Chun-nian Xia Wei-xiao Hu Wei Zhou Guo-hong Wang 《Journal of chemical crystallography》2008,38(8):583-586
Abstract The title compound, C16H22O4, synthesized by modified Knoevenagel condensation of protocatechualdehyde with monoheptyl-malonate and recrystallized from
benzene, was confirmed by single-crystal X-ray diffraction (CCDC 272827). The compound crystallizes in triclinic space group
Pī with cell parameters a = 5.296(3) ?, b = 10.711(13) ?, c = 13.870(4) ?, α = 98.84(7)°, β = 90.97(4)°, γ = 96.77(7)° and
Z = 2. The structure is the E isomer and its packing is stabilized by intermolecular O–H···O and C–H···O hydrogen bonds.
Index Abstract The title compound, C16H22O4, synthesized by modified Knoevenagel condensation, was confirmed by single-crystal X-ray diffraction showing its structure
is in E isomer and its packing is stabilized by hydrogen bonds.
相似文献
7.
Abstract A new complex, [H3teta][Mo(CN)8] · H2O, (teta = 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetra-azacyocloteradeca-4,11-diene), has been synthesized and characterized
by IR spectrum, element analysis and single crystal X-ray diffraction: monoclinic, space group P2(1)/c with a = 10.8553(8) ?, b = 12.4854(8) ?, c = 22.6348(15) ?, α = 90.00°, β = 97.3080(10)°, γ = 90.00°, Mr = 609.63, v = 3042.8(4), Z = 4. There are one [H3teta]3+, one [Mo(CN)8]3− and one water molecule in the asymmetric unit. The complex is interconnected through hydrogen bond and formed into a 3D porous
network.
Graphical Abstract A new complex, [H3teta][Mo(CN)8] · H2O, has been synthesized and characterized by IR spectrum, element analysis and single crystal X-ray diffraction. And it shows
a 3D porous network through hydrogen bonds.
相似文献
8.
Abstract The zinc(II) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Zn(2-(2-hydroxyphenyl)benzimidazolate)2]·C2H5OH (1 · C2H5OH) has been synthesized and characterized by X-ray crystallography and photoluminescent analysis. The complex crystallizes
in monoclinic space group P21/c with cell parameters a = 10.156(1) ?, b = 25.771(3) ?, c = 9.674(1) ?, α = 90°, β = 103.641(2)°, γ = 90°, Z = 4, V = 2460.4(4) ?3. The central Zn(II) is four-coordinate and has a tetrahedral geometry. The steady-state and time-resolved photoluminescent
spectra for the title compound have also been studied. The emission property can be ascribed to ligand-centered charge-transfer
transition (LCCT) with π → π* property.
Index Abstract
A new co-crystal of Zn(II) complex of 2-(2-hydroxylphenyl)benzimidazole with ethanol solvate has been prepared, characterized
by X-ray crystallography and fluorescent studies.
相似文献
9.
Kamil Z. Tilyabaev Samat A. Talipov Bakhtiyar T. Ibragimov Michael K. Dowd Abdurasul M. Yuldashev 《Journal of chemical crystallography》2009,39(9):677-682
Abstract The crystal structures of di-ethylaminogossypol with ethyl acetate (DEAG-EA) and pyridine (DEAG-P) were studied by room-temperature
X-ray diffraction. The host-to-guest molecule ratio in these complexes is 2:1 for DEAG-EA and 2:5 for DEAG-P. The crystal
and cell parameters for DEAG-EA are C34H40N2O6·0.5(C4H8O2), M = 660.78, triclinic, space group P-1, a = 11.316(2) ?, b = 12.082(2) ?, c = 15.085(3) ?, α = 73.34(3)°, β = 73.32(3)°, γ = 73.61(3)°, V = 1,847.3(7) ?3, Z = 2, and d
calc. = 1.188 g/cm3 and for DEAG-P are C34H40N2O6·2.5(C5H5 N), M = 769.91, triclinic, space group P-1, a = 9.6090(19) ?, b = 14.894(3) ?, c = 16.038(3) ?, α = 90.66(3)°, β = 106.25(3)°, γ = 103.17(3)°, V = 2138.7(9) ?3, Z = 2, and d
calc. = 1.195 g/cm3. In both structures, the di-ethylaminogossypol molecules are in the enamine form, which is the same tautomer found for other
reported Schiff base gossypol derivatives. The enantiomeric gossypol molecules of each structure form different centrosymmetric
dimer assemblies. These assemblies pack differently in each solvate.
Index Abstract Crystal structures of the solvates of di-ethylaminogossypol with ethyl acetate and pyridine were determined by X-ray diffraction.
相似文献
10.
Irena Ćaleta Dominik Cinčić Grace Karminski-Zamola Branko Kaitner 《Journal of chemical crystallography》2008,38(10):775-780
Abstract Two novel benzothiazoles 2-chloro-N-(benzothiazol-2-yl)benzamide (1) and 2-chloro-N-(6-cyanobenzothiazol-2-yl)benzamide (2) were obtained in multistep synthesis. They were characterised by means of IR, 1H- and 13C-NMR spectroscopy and also by single-crystal X-ray diffraction. The compound 1 crystallises with triclinic space group P
, a = 9.5923(8) ?, b = 9.8583(8) ?, c = 13.8962(10) ?, α = 89.162(6)°, β = 77.741(7)°, γ = 80.064(7)°, V = 1264.5(2) ?3, Z = 4 and compound 2 crystallises as methanol solvate with monoclinic space group P 21/n, a = 7.5093(9) ?, b = 13.0211(14) ?, c = 16.032(2) ?, β = 92.717(10)°, V = 1565.9(3) ?3, Z = 4. Both crystal structures consist of discrete dimers connected into a three-dimensional network by intermolecular C–H···O
and C–H···X (X = Cl or S) hydrogen bonds and by face-to-face π–π stacking interactions.
Index Abstract The synthesis and structure of two novel N-(benzothiazol-2-yl)benzamides. Irena Ćaleta, Dominik Cinčić, GraceKarminski-Zamola and Branko Kaitner. Hydrogen bonds and
π–π interactions in N-(benzothiazol-2-yl)benzamides N-(benzothiazol-2-yl)benzamides.
相似文献
11.
S. Rajeswari G. Venkatesa Prabhu D. Tamilvendan V. Ramkumar 《Journal of chemical crystallography》2009,39(9):650-654
Abstract A new mannich base 1-[(2,5-dioxopyrrolidin-1-yl)(phenyl)methyl] thiourea formed by the direct condensation of thiourea, succinimide
and benzaldehyde has been synthesized. The structure of this mannich base has been elucidated on the basis of micro elemental
analysis, IR, 1H NMR, 13C NMR, Mass and UV–Visible Techniques. The crystal structure of the title compound C12 H13 N3 O2 S was determined. It crystallizes in the monoclinic system, space group P21/c with a = 10.8234 (7) ?, b = 6.0355 (5) ?, c = 19.3692 (14) ?, β = 100.540(3)°, Z = 4 and V = 1243.94 (16) ?3. The structure was solved by the full-matrix least squares on F
2 and had a refined R value of 0.0465 for 1,964 observed reflections. The crystal structure is stabilized by strong intramolecular C–H···O, C–H···S
interactions and inter molecular N–H···O and S···S interactions.
Graphical Abstract This paper describes the spectroscopic and crystallographic studies of the title compound which is essential in ascertaining
the structure of this new compound.
相似文献
12.
Abstract A novel aromatic polycarboxylate polymer, [Zn2(bipy)2(btec)(H2O)2]n (1), has been synthesized and structurally characterized by the single crystal X-ray diffraction. Compound 1 belongs to the triclinic crystal system, space group P-1; a = 7.7449(6) ?, b = 8.9286(8) ?, c = 10.7422(8) ?, α = 80.95(1)°, β = 70.21(1)°, γ = 78.14(1)°, V = 680.93(10) ?3, Z = 2. The coordination geometry of Zn(II) atom is distorted trigonal bipyramidal with two nitrogen atoms of one 2,2′-bipy
group, two oxygen atoms from two different btec ligands, and one water. The 16-membered rings are alternately arranged forming
an infinite 1-D double-chain structure. A 3-D network was constructed by interlayer C···H–O, O···H–O hydrogen bonds and π–π
stacking interactions. Compound 1 exhibits fluorescence at room temperature in the solid state.
Graphical Abstract A 1-D double-chain aromatic polycarboxylate polymer, [Zn2(bipy)2(btec)(H2O)2]n (1), has been synthesized and structurally characterized by the single crystal X-ray diffraction. A 3-D network was constructed
by intermolecular C···H–O, O···H–O hydrogen bonds and π–π stacking interactions. Compound 1 exhibits fluorescence at room temperature in the solid state.
相似文献
13.
Qian Yang Bing-Yu Zhang Wei-Dong Ye Jian-Yong Yuan Duan-Jun Xu Jing-Jing Nie 《Journal of chemical crystallography》2008,38(9):659-661
Abstract The title compound (common name eplerenone), C24H30O6, is an aldosterone receptor antagonist. From the isopropyl acetate solution the compound crystallizes in monoclinic space
group P 21 with a = 8.811(1) ?, b = 11.250(1) ?, c = 11.079(1) ?, β = 93.822(12)°, Z = 2. The molecule contains three six membered rings, two five membered rings and one three membered ring. Both five membered
rings display envelope conformation, whereas three six membered rings show different conformation: chair, half-chair and envelope.
In the crystal the eplerenone molecules link to one another via intermolecular weak C–H···O hydrogen bonding to form the smaller
cavity of 12.0(1) ?3 between eplerenone molecules, no solvent molecule filled in this cavity.
Index Abstract In the title molecule three six-membered rings show different conformation. Weak C–H···O hydrogen bonding links adjacent molecules
to form the small cavity 12.0(1) ?3, no solvent molecule filled in the cavity.
相似文献
14.
Uzma Habib Amin Badshah Ulrich Flörke Rizwana Aleem Qureshi Bushra Mirza Nazar-ul-Islam Azeem Khan 《Journal of chemical crystallography》2009,39(8):607-611
Abstract The title copper (II) complex with Trimethoprim was prepared at 20–25 °C and its crystal structure was determined by single
crystal X-ray diffraction. Compound (C36H50Cu3N8O16) is triclinic, space group P-1 with a = 6.4642(5) ?, b = 12.5495(9) ?, c = 13.4911(10) ?, α = 77.518(1)°, β = 85.326(1)°, γ = 84.413(2)°, Z = 1. In this compound, three copper atoms are bonded to each other, two terminal coppers are bonded to three oxygen atoms
and N1 of pyrimidine ring of Trimethoprim and central copper is bonded to four oxygen atoms. The amino nitrogen atoms are not involved
in the coordination to the metal.
Graphical Abstract To enhance the activity of trimethoprim, its derivative was prepared and there bacterial activity against several bacteria
was analyzed.
相似文献
15.
Robert T. Stibrany 《Journal of chemical crystallography》2009,39(10):719-722
Abstract Two structures containing pseudo-tetrahedral Cu(II)N2Cl2 coordination complexes are reported. The first molecular structure (A) of the compound, 1,1′bis(1-ethylbenzimidazol-2-yl)propane
copper(II) dichloride (triEtBBIM)Cu(II)Cl2, 1, is reported. The complex crystallized in the triclinic space group P-1 with a = 8.616(3) ?, b = 9.302(3) ?, c = 14.314(4) ?, α = 85.613(6)°, β = 85.170(6)°, γ = 66.117(6)° and V = 1044.1(5) ?3 with Z = 2. The second structure (B) contains 1 and (3,3′bis(1-ethylbenzimidazol-2-yl)pentane) copper(II) dichloride (tetEtBBIM)Cu(II)Cl2, 2, both of which, cocrystallize in an equal molar ratio with a nitromethane solvate molecule. The complex crystallized in the
monoclinic space group P21/c with a = 18.876(4) ?, b = 14.975(3) ?, c = 18.344(4) ?, β = 116.75(3)°, and V = 4630.3(16) ?3 with Z = 4. The cocrystallization of such discrete complexes has been coined a chemical Janus.
Graphical Abstract The title complexes contain pseudo-tetrahedral Cu(II)N2Cl2 coordination. One of the structures is the result of an unusual cocrystallization, in which two different discrete Cu(II)
molecules cocrystallize in an equimolar ratio with a nitromethane solvate molecule.
相似文献
16.
Gino Bentivoglio Alexander Schwärzler Klaus Wurst Volker Kahlenberg Gerhard Nauer Günther Bonn Herwig Schottenberger Gerhard Laus 《Journal of chemical crystallography》2009,39(9):662-668
Abstract The synthesis and crystal structures of 1,3-diamino-2-methylimidazolium bis(trifluoromethylsulfonyl)imide (1), 1,3-dihydroxy-2-methylimidazolium bis(trifluoromethylsulfonyl)imide (2) and 1-(2-(diethylammonio)ethyl)-3-methylimidazolium bis(bis(trifluoromethylsulfonyl)imide) (4) are reported. The salts 1, 2 and 4 have melting points below 100 °C, the intermediate 1-(2-(diethylamino)ethyl)-3-methylimidazolium bis(trifluoromethylsulfonyl)imide
(3) is liquid at room temperature. Compound 1 is monoclinic, space group P21/n with a = 8.4979(4) ?, b = 12.2803(6) ?, c = 13.9400(7) ?, β = 93.086(4)°, and Z = 4. Compound 2 is monoclinic, space group P21/c with a = 7.6165(2) ?, b = 20.5323(8) ?, c = 9.7654(3) ?, β = 111.046(2)°, and Z = 4. Compound 4 is triclinic, space group with a = 8.5313(4) ?, b = 9.2157(4) ?, c = 20.5812(8) ?, α = 84.668(2)°, β = 83.738(2)°, γ = 63.096(2)°, and Z = 2. The ions in 1 build a network of N–H···O hydrogen bonds, in 2 they are linked to chains by O–H···N and bifurcated O–H···O hydrogen bonds, whereas in 4 they form pairs by N–H···O contacts. The triflimide anions adopt transoid conformations.
Index Abstract Short interionic contacts, conformational flexibility, and disorder phenomena were identified in the crystal structures of
three new, low-melting, protic imidazolium triflimides.
相似文献
17.
Wesley H. Monillas Glenn P. A. Yap Klaus H. Theopold 《Journal of chemical crystallography》2009,39(7):535-538
Abstract Addition LiNHPh to a [(NacNac)Cr(μ-I)]2 [NacNac = 2,4 pentane-N-N′-bis(2,6-diisopropylphenyl) ketiminato] in THF yields a dimeric anilido complex, 1, that crystallizes in P21/n with unit cell parameters a = 13.390(2) ?, b = 26.298(5) ?, c = 21.326(4) ?, β = 93.905(4)°, V = 7492(2) ?3 and Z = 4. The same reaction in the presence of aniline yields a monomeric anilido complex, 2, with a coordinated aniline molecule. Complex 2 crystallizes in P2
1
/c with unit cell parameters a = 28.530(5) ?, b = 10.8116(18) ?, c = 26.492(5) ?, β = 115.685(3)°, V = 7364(2) ?3 and Z = 8. Addition of aniline to isolated 1 yields 2. Addition of LiNPh2 to [(NacNac)Cr(μ-I)]2 in THF yields a monomeric complex that crystallizes in P21/n with the unit cell parameters a = 11.152(6) ?, b = 23.820(12) ?, c = 17.915(9) ?, β = 106.223(9)°, V = 4569(4) ?3 and Z = 4. All complexes have been spectroscopically and structurally characterized.
Graphical Abstract Addition of LiNHPh or LiNPh2 to [(NacNac)Cr(μ-I)]2 yields a dimeric or a monomeric complex whereas addition of LiNHPh in the presence of aniline yields the monomeric anilido
complex.
相似文献
18.
Dalibor Mili? Vi?nja Vrdoljak Dubravka Matkovi?-?alogovi? Marina Cindri? 《Journal of chemical crystallography》2009,39(8):553-557
Abstract Red crystals of cis-dioxo(3-methoxysalicylaldehyde 4-methylthiosemicarbazonato-N,O,S)(γ-picoline-N)molybdenum(VI), [MoO2L(γ-pic)], [L2−=CH3OC6H4(O)CH=NN=C(S)NHCH3, 3-methoxysalicylaldehyde 4-methylthiosemicarbazonato] were prepared by the reaction of [MoO2L]
n
with γ-picoline in dry methanol. The title compound crystallized in the monoclinic space group P21/n, a = 6.7984(7) ?, b = 15.9760(12) ?, c = 17.1466(14) ?, β = 93.613(8)°, V = 1858.6(3) ?3, Z = 4. The coordination geometry around the molybdenum center is distorted octahedral with the tridentate thiosemicarbazonato
ligand (L2−) bonded meridionally to the [MoO2]2+ core. The sixth coordination site is occupied by a weakly bound γ-picoline molecule. The adjacent molecules are joined by
the N–H···O hydrogen bonds between their amino and methoxy groups thus forming infinite molecular chains. The three-dimensional
solid-state structure is achieved by the additional C–H···O, C–H···π and van der Waals interactions.
Graphical Abstract In the title compound, [MoO2L(γ-pic)], the tridentate thiosemicarbazonato ligand (L2−) is meridionally bound to the [MoO2]2+ core, while a molecule of γ-picoline completes the distorted octahedral coordination around the metal atom.
相似文献
19.
Wesley H. Monillas Glenn P. A. Yap Klaus H. Theopold 《Journal of chemical crystallography》2009,39(1):73-77
Abstract A series of complexes of the form [bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato](iodo)(solvent) chromium were synthesized and structurally characterized (solvent = tetrahydrofuran,
acetonitrile, α-picoline). The tetrahydrofuran adduct crystallized in the P21/n space group with the crystal cell parameters a = 17.628(6) ?, b = 10.218(3) ?, c = 20.646(7) ?, β = 109.209(4)°, V = 3512(2) ?3 and Z = 4. The acetonitrile adduct crystallized in the P21/c space group with the crystal cell parameters a = 16.104(7) ?, b = 11.965(5) ?, c = 18.201(8) ?, β = 116.091(6)°, V = 3150(2) ?3 and Z = 4. The α-picoline adduct crystallized in the C2/c space group with the crystal cell parameters a = 39.982(9) ?, b = 11.637(2) ?, c = 16.560(4) ?, β = 108.085(4)°, V = 7325(3) ?3 and Z = 8. For each compound, the coordination around each chromium center is square planar with varying degrees of distortion.
Graphical Abstract A series of Cr(II) complexes of the form LCrI(S) (where L = nacnac = β-diketiminate; S = solvent) were synthesized and structurally characterized.
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20.
Brahim Bennani Abdelali Kerbal Brahim El-Bali Michael Bolte 《Journal of chemical crystallography》2009,39(6):466-468
Abstract The crystal structure of the title compound, C11H11NOS, was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/c with cell parameters a = 10.533(2) ?, b = 12.7826(19) ?, c = 7.6491(17) ?, β = 107.997(17)°, V = 979.5(3) ?3 and Z = 4. The S containing heterocycle adopts a sofa conformation, whereas the 5-membered ring adopts an envelope conformation.
The crystal packing is characterized by weak C–H···N contacts and π-stacking interactions.
Graphical Abstract The title compound, 3-methyl-3a,4-dihydro-3H-thiochromeno[4,3-c]isoxazol was synthesized by an 1,3 dipolar cycloaddition reaction
and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the aromatic 6-membered ring
is planar, whereas the ring containing the S atom adopts a sofa conformation and the 5-membered ring an envelope conformation.
The methyl group is in an equatorial position.
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