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1.
Organoarsino-Substituted Sulphur Diimides: Crystal Structure Analyses of 3, 7-Di-t-butyl-3H, 7H-1λ4, 5λ4, 2, 4, 6, 8, 3, 7-dithiatetrazadiarsocine and Bis (diphenylarsino)sulphur Diimide Reaction of the salt K2SN2 with organoarsenic chlorides leads to sulphur diimides containing organoarsino substituents at both ends. Single crystal X-ray structure analyses were carried out for two typical compounds, i.e. the cyclic eight-membered 3, 7-di-t-butyl-3H, 7H-1λ4, 5λ4, 2, 4, 6, 8, 3, 7-dithiatetrazadiarsocine ( 1a , prepared from K2SN2 and (t-Bu)AsCl2 (1:1)) and the open-chain bis(diphenylarsino)sulphur diimide ( 2a , prepared from K2SN2 and Ph2AsCl (1:2)). In both compounds the sulphur diimide groups are coplanar with their directly bound arsenic atoms. This coplanarity principle leads, in the case of 1a , to about conformation (mm2(C2v) symmetry) of the eight-membered heterocycle; the t-butyl substituents occupy quasi equatorial positions. Small deviations from mm2 symmetry and torsions around the S?N bonds up to 12° can be explained as a consequence of the transnnular repulsion of the lone pairs at the arsenic atoms (As …As distance 3.683(1) Å). In the case of the open-chain S(N? AsPh2)2 ( 2a , 2(C2) symmetry), a cis, cis configuration was found at the S?N double bonds which indicates As…As interaction. The As…As distance (3.379(1) Å) is shorter than in 1a and parallells a reduced interaction of the lone pairs at the As atoms. The S?N bond lenghts (1.517(5) Å in 1 a and 1.521(3) Å in 2a ) are characteristic of sulphur diimides withoug significant π-interaction with the substituents and correspond to SIV?N double bonds. 相似文献
2.
Ya‐Ling Liu Pei Zou Hao Wu Min‐Hao Xie Shi‐Neng Luo 《Acta Crystallographica. Section C, Structural Chemistry》2012,68(9):o338-o340
The title compound, C16H24O10·0.11H2O, is a key intermediate in the synthesis of 2‐deoxy‐2‐[18F]fluoro‐d ‐glucose (18F‐FDG), which is the most widely used molecular‐imaging probe for positron emission tomography (PET). The crystal structure has two independent molecules (A and B) in the asymmetric unit, with closely comparable geometries. The pyranose ring adopts a 4C1 conformation [Cremer–Pople puckering parameters: Q = 0.553 (2) Å, θ = 16.2 (2)° and ϕ = 290.4 (8)° for molecule A, and Q = 0.529 (2) Å, θ =15.3 (3)° and ϕ = 268.2 (9)° for molecule B], and the dioxolane ring adopts an envelope conformation. The chiral centre in the dioxolane ring, introduced during the synthesis of the compound, has an R configuration, with the ethoxy group exo to the mannopyranose ring. The asymmetric unit also contains one water molecule with a refined site‐occupancy factor of 0.222 (8), which bridges between molecules A and B via O—H...O hydrogen bonds. 相似文献
3.
Levent
ztürk Muhammed Iklan Zeynel Kl Tuncer Hkelek 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(2):o80-o83
The title compound, C26H55N11P4, consists of a bicyclic phosphazene ring with five bulky pyrrolidino and one propylamino group, together with a second propylamino group bridging the two P atoms. The asymmetric unit contains two molecules with very similar conformations. The bulky substituents are instrumental in determining the bicyclic P4N5 ring conformation. Each of the fused six‐membered N3P3 rings is in a sofa conformation. The P—N distances in the bridge are non‐equivalent and one of them is the longest P—N bond in the molecule. The hybridization of the bridging N atom is pyramidal. The single and double P—N bonds cannot easily be distinguished, since they retain their phosphazenic character in the phosphazene macro‐rings. 相似文献
4.
Fiona Brady John F. Gallagher 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(11):1407-1410
The title compound, C17H15NO4, derived from l ‐tyrosine, crystallizes with three independent molecules which differ in the conformation of the asymmetric unit: the N—C—C—Cipso torsion angles are ?71.7 (5), ?63.6 (6) and ?52.5 (5)°, respectively. Deformations in the phenol ring hydroxy O—C—C angles of 116.5 (4)/123.9 (4), 121.7 (5)/118.1 (4) and 122.4 (5)/118.6 (5)°, respectively, result from their respective intermolecular hydrogen‐bonding environments. Intermolecular Oacid—H?O=Cindole, Ophenol—H?O—Hphenol and Ophenol—H?O=Cindole hydrogen bonds, with O?O distances in the range 2.607 (4)–2.809 (4) Å, are present in combination with C—H?O and C—H?πarene interactions. The primary hydrogen‐bonding systems assemble with graph sets R33(8) and R32(22). 相似文献
5.
Zora Popovi Gordana Pavlovi Dubravka Matkovi‐alogovi
eljka Soldin 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(5):m165-m167
The asymmetric unit of the title polymeric complex, [HgBr(C6H4NO2)]n or HgBr(nic), contains mercury coordinated via two Br atoms [Hg—Br = 2.6528 (9) and 2.6468 (9) Å], two carboxylate O atoms, which form a characteristic four‐membered chelate ring [Hg—O = 2.353 (6) and 2.478 (7) Å], and an N atom [Hg—N = 2.265 (5) Å], in the form of a very irregular (3+2)‐coordination polyhedron. The pronounced irregularity of the effective Hg (3+2)‐coordination is a result of the rigid stereochemistry of the nicotinate ligand. According to the covalent and van der Waals radii criteria, the strongest bonds are Hg—Br and Hg—N. These covalent interactions form a two‐dimensional polymer. The puckered planes are connected by van der Waals interactions, and there are only two intermolecular C—H⋯O hydrogen bonds [3.428 (10) and 3.170 (10) Å]. 相似文献
6.
Alexander S. Lyakhov Pavel N. Gaponik Michail M. Degtyarik Ludmila S. Ivashkevich 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(6):m204-m206
In the polymeric title complex, [CuCl2(C3H6N4)2]n, there are two ligands in the asymmetric unit. The Cu atom adopts an elongated octahedral geometry, with two 2‐ethyltetrazole ligands [Cu—N = 2.0037 (16) and 2.0136 (16) Å] and two Cl atoms [Cu—Cl = 2.2595 (6) and 2.2796 (6) Å] in equatorial positions. A Cl atom and a symmetry‐related 2‐ethyltetrazole molecule [Cu—Cl = 2.8845 (8) Å and Cu—N = 2.851 (2) Å] lie in the axial positions of the octahedron. One of the two 2‐ethyltetrazole ligands of the asymmetric unit exhibits bidentate binding to two Cu atoms through two N atoms of the tetrazole ring, whereas the other ligand is coordinated in a monodentate fashion via one tetrazole N atom. The Cu‐atom octahedra form dimer entities by sharing edges with equatorial and axial Cl atoms. The dimers are linked together through the 2‐ethyltetrazole ligands to form one‐dimensional polymeric zigzag chains extending along the b axis. The chains are connected into infinite layers parallel to the (10) plane via the 2‐ethyltetrazole ligands. 相似文献
7.
Ramaswamy Murugavel Natesan Thirupathi Setharampattu S. Krishnamurthy Munirathinam Nethaji 《Heteroatom Chemistry》1995,6(1):63-70
Oxidation of the cis isomer of the λ3-cyclotriphosphazane [EtNP(OCH2CF3)]3 with trimethylamine-N-oxide (TMNO) gives the cis isomer of trioxo-λ5-cyclotriphosphazane [EtNP(O)(OCH2CF3)]3; the trans isomer of [EtNP(O)(OCH2CF3)]3 is obtained by the treatment of a cis and trans mixture of [EtNP(OCH2CF3)]3 with aqueous H2O2. The two trioxocyclotriphosphazanes have been characterized by elemental analysis, IR, and NMR (1H, 13C, 19F, and 31P) spectroscopy. The solid state structures of both the isomers have been determined by single crystal X-ray diffraction. The six-membered P3N3 ring in both the isomers exhibits a twist-boat conformation; in the cis isomer, the trifluoroethoxy substituents lie on the same side of the ring, whereas, in the trans isomer, two trifluoroethoxy groups are on one side of the ring and the third on the other side of the ring. Crystal data for cis-[EtNP(O)(OCH2CF3)]3: monoclinic, P 21/ n , a = 13.593(3), b = 9.721(2), c = 17.539(3) Å, β = 99.49(2)°, V = 2286(1) Å3, Z = 4, and Final R = 0.047. Crystal data for trans-[EtNP(O)(OCH2CF3)]3: monoclinic, P 21/ n , a = 11.685(4), b = 15.115(5), c = 13.233(5) Å, - = 102.21(3)°, V = 2284(1) Å3, Z = 4, and Final R = 0.078. 相似文献
8.
Sabahat
zcan Engin Kendi Meral Tunbilek Hakan Gker 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(4):459-460
The title compound, C21H23ClN4O2·0.5H2O, contains two independent molecules in the asymmetric unit. In each molecule the piperazine ring adopts a chair conformation; the deviations of the piperazine N atoms from the best plane through the remaining four C atoms are ?0.678 (3) and 0.662 (3) Å in molecule A, and 0.687 (3) and ?0.700 (3) Å in molecule B. The molecules are linked by two hydrogen bonds of the O—H?N type involving the O atom of the water molecule of crystallization. 相似文献
9.
Experimental and Theoretical Studies of 4‐(1‐benzyl‐5‐methyl‐1H‐1,2,3‐triazol‐4‐yl)‐6‐(2,4‐dichlorophenyl)pyrimidin‐2‐amine: A Potential Antibacterial Agent 下载免费PDF全文
S. Murugavel R. Madhanraj D. K. Andrew Prasanna Kumar Sangaraiah Nagarajan Alagusundaram Ponnuswamy 《中国化学会会志》2015,62(11):974-983
The title compound ( 1 ), 4‐(1‐benzyl‐5‐methyl‐1H‐1,2,3‐triazol‐4‐yl)‐6‐(2,4‐dichlorophenyl)pyrimidin‐2‐amine (C20H16Cl2N6), was synthesized and structurally characterized by elemental analysis, 1H NMR and 13C NMR and single crystal X‐ray diffraction. The compound crystallizes as a colourless needle shaped in the triclinic system, space group P‐1 with cell constants: a = 10.7557(11) Å, b = 12.7078(17) Å, c = 15.511(2) Å, α = 68.029(4)0, β = 86.637(5)0, γ = 87.869(4)0; V = 1962.4 (4) Å3, Z = 4. There are two structurally similar but crystallographically independent molecules (A and B) in the asymmetric unit of the title compound, which is linked via N‐H…Cl hydrogen bond. An intramolecular C‐H…N hydrogen also occurs in each molecule. In the crystal, each of independent molecules forms a centrosymmetric dimer with an R22(8) ring motifs through a pair of N‐H…N hydrogen bonds. These dimers are further connected by intermolecular N‐H…Cl and C‐H…Cl hydrogen bonds, forming an infinite two dimensional supramolecular network lying parallel to the [010] plane. The molecular geometry was also optimized using density functional theory (DFT/B3LYP) method with the 6‐311G (d, p) basis set and compared with the experimental data. Mulliken population analyses on atomic charges, HOMO‐LUMO energy levels, Molecular electrostatic potential and chemical reactivity of the title compound were investigated by theoretical calculations. The thermo dynamical properties of the title compound at different temperature have been calculated and corresponding relations between the properties and temperature have also been obtained. The in vitro antibacterial activity has been screened against Gram‐positive (Bacillus cerus and Staphylococcus epidermidis) and Gram‐Negative (Escherichia coli, Acinetobacter baumannii and Proteus vulgaris). The results revealed that the compound exhibited good to moderate antibacterial activity. 相似文献
10.
Viktor A. Tafeenko Rene Peschar Olga V. Kaukova Henk Schenk Leonid A. Aslanov 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(1):o62-o64
In the title compound, C8H12N+·C8HN4O2−, the anion and cation lie on a crystallographic mirror plane and form planar ribbons via N—H⋯O [N⋯O = 2.933 (4) Å, H⋯O = 2.01 Å and N—H⋯O = 170°] and N—H⋯N [N⋯N = 3.016 (5) Å, H⋯N = 2.15 Å and N—H⋯N = 169°] hydrogen bonds. The ribbons are further linked via weak C—H⋯O and C—H⋯N hydrogen bonds. In adjacent planes, anions lie opposite cations; π–π interactions (separation a/2 = 3.520 Å) exist between the anions and the cations, and stacks are formed, running along the a axis. The cations are disordered over two interpenetrating sites, with occupancies of 0.833 (5) and 0.167 (5). 相似文献
11.
Xiao‐Yan Chen Wei‐Zheng Shen Peng Cheng Shi‐Ping Yan Dai‐Zheng Liao Zong‐Hui Jiang 《无机化学与普通化学杂志》2003,629(4):697-702
Three 3, 5‐dimethylpyrazole (pz*) copper(II) complexes, [Cu(pz*)4(H2O)](ClO4)2 ( 1 ), [Cu(pz*)2(NCS)2]·H2O ( 2 ), and [Cu(pz*)2(OOCCH=CHCOO)(H2O)]·1.5H2O ( 3 ), have been synthesized and characterized with single crystal X‐ray structure analysis. 1 crystallizes in the tetragonal space group, 14/m, with a = 14.027 (3) Å, c = 16.301 (5) Å, and Z = 4. 2 crystallizes in the monoclinic space group, P21/c, with a = 8.008 (3) Å, b = 27.139 (9) Å, c = 8.934 (3) Å, β = 106.345 (6)°, and Z = 4. 3 crystallizes in the triclinic space group, P1¯, with a = 7.291 (9) Å, b = 10.891 (13) Å, c = 11.822 (14) Å, α = 80.90 (2)°, β = 79.73(2)°, γ = 70.60(2)°, and Z = 2. In 1 , one water molecule and four pz* ligands are coordinated to CuII. Two [Cu(pz*)4(H2O)]2+ units are connected to ClO4— via hydrogen bonds. One lattice water molecule is found in the unit cell of 2 , which forms an one‐dimensional chain via intermolecular hydrogen bonds with the N‐H atom of pz*. In 3 , the oxygen atom of the coordinated water molecule is connected with two C=O groups of two neighbouring maleic acid molecules to form a linear parallelogram structure. Another C=O group of maleic acid forms a hydrogen bond with the N‐H atom of pz* to create a two‐dimensional structure. The spectroscopic and bond properties are also discussed. 相似文献
12.
Robert E. Dinnebier Matthias Wagner Frank Peters Kenneth Shankland William I. F. David 《无机化学与普通化学杂志》2000,626(6):1400-1405
The crystal structure of [(C5H4BMe2)2Fe]‐4,4′‐bipyridine [ 2 · bipy]n has been determined by the method of simulated annealing from high resolution X‐ray powder diffraction at room temperature. The compound is of interest, because it proves that highly ordered organometallic macromolecules can be formed in the solid state via the self‐assembly of N–B‐donor‐acceptor bonds. [ 2 · bipy]n crystallizes in the triclinic space group, P 1, Z = 2, with unit cell parameters of a = 8.3366(2) Å, b = 11.4378(3) Å, c = 12.6740(5) Å, α = 112.065(2)°, β = 108.979(1)°, γ = 90.551(2)°, and V = 1047.06(6) Å3. For the structure solution of [ 2 · bipy]n 11 degrees of freedom (3 translational, 3 orientational, 5 torsion angles) were determined within several hours, demonstrating that the crystal packing and the molecular conformation of medium sized (< 50 non‐hydrogen atoms) coordination compounds can nowadays be solved routinely from high resolution powder diffraction data. 相似文献
13.
Alexander V. Pestov Eugenia V. Peresypkina Alexander V. Virovets Nina V. Podberezskaya Yury G. Yatluk Yury A. Skorik 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(12):m510-m512
The CuII ion in the title complex, [Cu(C5H10NO3)2] or [Cu(He‐ala)2] [He‐ala = N‐(2‐hydroxyethyl)‐β‐alaninate], resides at the inversion centre of a square bipyramid comprised of two facially arranged tridentate He‐ala ligands. Each He‐ala ligand binds to a CuII ion by forming one six‐membered β‐alaninate chelate ring in a twist conformation and one five‐membered ethanolamine ring in an envelope conformation, with Cu—N = 2.017 (2) Å, Cu—OCOO = 1.968 (1) Å and Cu—OOH = 2.473 (2) Å. The [Cu(He‐ala)2] molecules are involved in a network of O—H⋯O and N—H⋯O hydrogen bonds, forming layers parallel to the (10) plane. The layers are connected into a three‐dimensional structure by van der Waals interactions, so that the molecular centres form pseudo‐face‐centered close packing. 相似文献
14.
Acyl- and Alkylidenephosphines. XXV. Molecular and Crystal Structure of 1,2-Di(tert-butyl)-3-dimethylamino-1-thio-4-trimethylsilylsulfano-1λ5, 2λ3-diphosphet-3-ene The title compound 1 formed in a nearly quantitative yield by decomposition of tert-butyl(N,N-dimethylthiocarbamoyl)trimethylsilylphosphine, crystallizes in the orthorhombic space group P212121 with {a = 1067.3(1); b = 1077.1(1); c = 1924.6(5) pm; Z = 4} at +20°C. An X-ray structure determination (RG = 0.038) shows two tert-butyl groups at a four- (P1) and a three-coordinate phosphorus atom (P2) to be placed on different sides of the four membered ring. Characteristic bond lengths as well as the angles at the atoms P1, P2, C3, and C4 inside the ring have already been given above. 相似文献
15.
Yvar Van Den Winkel Jeroen Van Der Laarse Frans J. J. De Kanter Thomas Van Der Does Friedrich Bickelhaupt Wilberth J. J. Smeets Anthony L. Spek 《Heteroatom Chemistry》1991,2(1):17-28
The synthesis of 2,2′-bis(bis(dimethylamino)-phosphino)-3,3′5,5′-tetra-tert-butylbiphennyl ( 5 ) is described. It was extensively studied by 1H, 13C, and 31P NMR spectroscopy. Furthermore, the X-ray analysis of 5 is reported. Crystals of 5 are tetragonal, space group P¯421c, a = b = 24.770 (3) Å, c = 12.658 (4) Å, Z = 8. The surprising reaction of 5 with proton acids leading to the formation of various phosphorus containing five- and six-membered ring compounds is discussed. On reaction of one of the six-membered ring compounds ( 9 ) with magnesium in THF, a λ3, λ5-diphosphaphenanthrene ( 19 ) was obtained. 相似文献
16.
《Journal of Coordination Chemistry》2012,65(2):266-276
N-(R-carbamothioyl)cyclohexanecarboxamides (R: diethyl, di-n-propyl, di-n-butyl, diphenyl and morpholine-4) and their Ni(II) and Cu(II) complexes have been synthesized and characterized by elemental analyses, FT-IR and NMR methods. N-(diethylcarbamothioyl)cyclohexanecarboxamide, HL1, C12H22N2OS, crystallizes in the orthorhombic space group P212121, with Z = 4, and unit cell parameters, a = 6.6925(13) Å, b = 9.0457(18) Å, c = 22.728(5) Å. The conformation of the HL1 molecule with respect to the thiocarbonyl and carbonyl moieties is twisted, as reflected by the torsion angles O1–C6–N2–C5, C6–N2–C5–N1 and S1–C5–N2–C6 of 1.68°, ?67.47° and 115.50°, respectively. The structure of HL1 also shows a delocalization of the π electrons of the thiocarbonyl group over the C–N bonds. The ring puckering analysis shows that the cyclohexane ring has a chair conformation. The bis(N-(morpholine-4-carbonothioyl)cyclohexane carboxamido)nickel(II) complex, Ni(L5)2, C24H38N4NiO4S2, crystallizes in the monoclinic space group P21/c, with Z = 4, and unit cell parameters, a = 16.919(3) Å, b = 8.3659(17) Å, c = 19.654(4) Å, β = 107.43(3)°. Ni(L5)2 is a cis-complex with a slightly distorted square-planar coordination of the central nickel by two oxygen and two sulfur atoms. 相似文献
17.
Olanzapinium benzoate, 1-methyl-4-(2-methyl-10H-thieno[2,3-b][1,5]benzodiazepin-4-yl)-piperazin-1-ium benzoate, (C17H21N4S)+(C7H5O2)? (I), crystallizes in triclinic space group P-1 with unit cell dimensions a = 9.2957(6) Å, b = 11.2416(7) Å, c = 12.0003(8) Å; α = 64.585(1)°, β = 87.568(1)°, γ = 83.248(1)°; V = 1124.8(1) Å3. The asymmetric part of the structure comprises a singly charged olanzapinium cation and a singly charged benzoate anion. The central 1,5-diazepine ring adopts the expected boat conformation, while the piperazine ring favors the chair conformation. The olanzapinium and benzoate ions are linked by intermolecular N-H...O hydrogen bonds forming infinite chains running along the c-axis of the crystal. 相似文献
18.
Ivanka Matijai Gordana Pavlovi Rudolf Trojko Jr 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(4):o184-o186
The X‐ray crystal structure analysis of the title compound, C17H30O8, revealed a 4C1 conformation of the pyranosyl ring [Cremer–Pople puckering parameters of Q = 0.568 (2) Å, θ = 5.1 (2) and ϕ = 218 (3)°]. The structure shows no deviations from the geometric parameters of pyranoside carbohydrates. The hydroxyl groups participate in O—H⃛O hydrogen bonds, forming a two‐dimensional pattern [O⃛O = 2.811 (3) and 2.995 (3) Å]. 相似文献
19.
Antonio Quesada Antonio Marchal John N. Low Christopher Glidewell 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(3):o102-o104
In the title compound, C14H23N6O2+·HSO4−·H2O, the pyrimidinium ring of the cation adopts a twist‐boat conformation, induced by steric clashes between adjacent ring substituents; the anions and the water molecules are linked by three O—H⃛O hydrogen bonds [H⃛O = 1.70–1.78 Å, O⃛O = 2.548 (2)–2.761 (2) Å and O—H⃛O = 161–168°] into chains of edge‐fused R(12) rings, which are linked into sheets by the cations, via three N—H⃛O hydrogen bonds [H⃛O = 1.96–2.17 Å, N⃛O = 2.820 (2)–2.935 (2) Å and N—H⃛O = 145–173°]. 相似文献
20.
Gunji Koyama 《Helvetica chimica acta》1974,57(2):370-375
The crystal and molecular structure of 3-oxo-17β-acetoxy-Δ4-14α-methyl-8α, 9β, 10α, 13α-estrene, C21H30O3, has been determined by X-ray diffraction analysis. The crystals belong to the orthorhombic space group P212121, with the cell dimensions a = 12.093 Å, b = 19.667 Å, c = 7.746 Å; Z = 4. Intensity data were collected at room temperature with an automatic four-circle diffractometer. The structure was solved by direct methods and the parameters were refined by least-squares analysis. All the hydrogen atoms were included in the refinement. The final R value was 0.038 for 1413 observed reflections. The conformation of ring A is intermediate between a half-chair and a 1, 2-diplanar form. The hydrogens at C(9) and C(10) are anti, the B/C ring junction is trans, and rings B and C adopt chair conformations. Ring D is cis fused and is halfway between C2 and Cs forms. 相似文献