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1.
Christof Kratky Wolfgang Reischl Elisabeth Altmann Erich Zbiral 《Monatshefte für Chemie / Chemical Monthly》1982,113(4):439-448
Oxidation of the α- and β-4-phenyl-1,2,4-triazolin-3,5-dione adducts of vitamin D3 (2 and1) withMCPBA yields two diastereomeric mixtures of the (5,10)-(7,8)-dioxiranes3 a,3 b,3 c and4 a,4 b respectively. The corresponding benzoates5 a,5 b,6 a and6 b were prepared and the X-ray crystal structure of5 b was determined. This analysis proved5 b to be the (5R, 1 OS)-(7R, 8R)-dioxirane of the β-resp. (6S)-4-phenyl-1,2,4-triazolin-3,5-dione adduct1 of vitamin D3. 相似文献
2.
Prof. Dr. G. Zigeuner H. W. Schramm A. Fuchsgruber W. Wendelin 《Monatshefte für Chemie / Chemical Monthly》1975,106(2):407-416
Bromination of 1-benzyl-4-methyl-3.4-dihydro-2(1H)-pyrimidinone (9 a) with 1 mole Br2 in CHCl3 yields 1-benzyl-5-bromo-6-hydroxy-4-methyltetrahydro-2(1H)-pyrimidinone,12 a, or the 6-ethoxypyrimidinone13 a, according to whether H2O orEtOH is used in working up. With 2 moles Br2,9 a analogously affords the 5.5-dibromopyrimidinnes14 a or15 a. Bromination of the 6-hydroxypyrimidinone10 a yields the same products,12 a and13 a, or14 a and15 a respectively, while the 4-phenyl-pyrimidinones9 b and11 b yield the corresponding 5-bromo-and 5.5-dibromopyrimidinones13 b and15 b. The structures of the compounds12 a-15 b are confirmed by their NMR data and chemical properties: the oxopyrimidinylmethylureas16 a and17 a are formed by the action of methylurea on12 a and13 a, or on14 a and15 a respectively; with hexamethylenetetramine,12 a reacts to give the 5.6-dihydroxypyrimidinone18 a, while13 b is transformed to the 4-phenylpyrimidinone19 b. 13 b was also synthesized from α-bromocinnamaldehyde. The mechanism of bromination is discussed. 相似文献
3.
Hassan A. El-Sayed Said A. Said Abd El-Galil E. Amr 《Research on Chemical Intermediates》2014,40(2):833-845
A series of pyridofuro compounds were synthesized from 4-(4-chlorophenyl)-1,2-dihydro-2-oxo-6-(thiophen-2-yl)pyridine-3-carbonitrile (1) as starting material. Alkylation of 1 with ethyl bromoacetate gave the corresponding ester 2, which was condensed with hydrazine hydrate to afford the corresponding acid hydrazide derivative 3. Thrope-Ziegler cyclization of 2 with sodium methoxide gave furo[2,3-b]pyridine derivative 4, which was reacted with thiosemicarbazide, allyl isothiocyanate, formamide or hydrazine hydrate to give furopyridine derivatives 5–8, respectively. The latter compound 8 was cyclized with acetylacetone or formic acid to give the corresponding compounds 9 and 10, respectively. Furthermore, sulfurization of 1 with P2S5 gave the corresponding thioxopyridine 11, which was reacted with glycosyl (or galactosyl) bromide, morpholine or piperidine to give the corresponding thioglycoside 12a,b and Mannich base 14a,b derivatives. The deacetylation of 12a,b gave the corresponding deacetylated thioglycosides 13a,b, respectively. All the newly synthesized compounds were characterized by the elemental analyses and spectroscopic evidences (IR, 1H- and 13C NMR). 相似文献
4.
Prof. Dr. Otto Hromatka Dieter Binder Karl Eichinger 《Monatshefte für Chemie / Chemical Monthly》1975,106(2):555-558
The synthesis of 1-(3-thienyl)-benzimidazol-2-ones (3 a and4), described in an earlier paper1, has been further investigated. The Na-salt of3 a is converted to a benzimidazolone substituted in position 3 (3 b). Dehydrogenation of the thiophene nucleus of3 a with chloranil yields5 a, which undergoes substitution in position 3 with Cl(CH2)2N(CH3)2 to give5 b. Monochlorination of5 a yields5 c, the structure of which is confirmed by1H-NMR-spectroscopy.5 d is obtained by reaction of the Na-salt of5 c with Cl(CH2)2N(CH3)2. 相似文献
5.
G. A. Kostin V. I. Mashukov T. M. Korda V. G. Torgov A. B. Drapailo O. V. Kas’yan V. I. Kal’chenko 《Russian Journal of Inorganic Chemistry》2006,51(10):1682-1687
Thiacalixarenes 1 and 2, thiacalixarene thioether 5, and calixarene thioethers 3a–3c, 4a, and 4b are compared with respect to gold(III) extraction from hydrochloric acid solutions. The gold extractability increases in the following order: 1,2 5 3a–3c, 4a, 4b. The effect of the substituents at the sulfur atom in R2S and in 3a–3c, 4a, and 4b is identical when cooperative effects (CE) appear for calixarene thioethers. On the basis of the extraction stoichiometry and the activities of the components of the aqueous phase, the gold distribution in the form of (AuCl3)nL (n = 1?4) species is quantified for cHCl from 0.5 to 6 mol/L. A correlation is found between the gold distribution constants into various diluents and the Kamlet-Taft parameter π*. 相似文献
6.
The betaines1b–d were prepared4 by systematic variation of the alkyl groups and were reacted with trifluoroacetic acid anhydride (TFA) to give the diacyl-ylides2b,c. The betain1d andTFA afford the trifluoroacetate3d 5. The salts3b,c, which result from hydrolysis of2b,c as well as3d (X=I) can be transformed in 75 to 83% yield into the monoacyl-ylides4b–d with the help of silver oxide. Aqueous solutions of4a–d exhibit alkalinepH, which points to the formation of the corresponding ammonium bases. In the case of4b,c the bases5b,c could be isolated. It can be shown, that4b,c and5b,c, respectively, undergo a reversible addition or elimination of one mole wather with great ease. 相似文献
7.
Haleden Chiririwa Freeman Ntuli Edison Muzenda Alfred Muller 《Transition Metal Chemistry》2013,38(4):393-399
The reactions of N-(2(diphenylphosphino) benzylidene) (phenyl) methanamine, Ph2PPhNHCH2-C5H4N, 1 and N-(2-(diphenylphosphino) (benzylidene) (thiophen-2-yl) methanamine, Ph2PPhNHCH2-C4H3S, 2 with MCl2(cod) and MCl(cod)Me (M = Pd, Pt; cod = 1,5-cyclooctadiene) yield the new complexes [M(Ph2PPhNHCH2-C5H4N)Cl2], M = Pd1a, Pt1b, [M(Ph2PPhNHCH2-C5H4N)ClMe], M = Pd1c, Pt 1d, [M(Ph2PPhNHCH2-C4H3S)Cl2], M = Pd2a, Pt 2b, and [M(Ph2PPhNHCH2-C4H3S)ClMe], M = Pd2c, Pt 2d, respectively. The new compounds were isolated as analytically pure crystalline solids and characterized by 31P-, 1H-NMR, IR spectroscopy, electro spray ionization-mass spectrometry (ESI-MS) and elemental analysis. The representative solid-state molecular structures of the platinum complexes 1b and 2b were determined using single crystal X-ray diffraction analysis and revealed that the complexes exhibit a slightly distorted square-planar geometry. Furthermore, the palladium complexes were tested as potential catalysts in the Heck and Suzuki cross-coupling reactions. 相似文献
8.
Sergei N. Konchenko Nikolai A. Pushkarevsky Manfred Scheer 《Journal of Cluster Science》2003,14(3):299-312
The reaction of [Et4N]2[Fe3(μ 3-Q)(CO)9] (Q=Se ([Et4N]2[1b]), Te ([Et4N]2[1c])) with [Cp*M(CH3CN)3][CF3SO3]2 (M=Rh, Ir) leads to the addition of a Cp*M2+ unit to a Fe2Q face of the initial cluster. In this way four new heteronuclear clusters [MFe3(μ 4-Q)(CO)9Cp*] (M=Rh (2b, c); M=Ir (3b, c)) were obtained possessing a butterfly-shaped cluster core bridged by a μ 4-Q unit. Furthermore, reaction with the Ir starting complex leads to the metal-substituted derivatives [IrFe2(μ 3-Q)(CO)7Cp*] (4b, c) in lower yields, whose structures consist of a triangular metal core capped by a μ 3-Q ligand. The products were comprehensively characterised by spectroscopic methods and the molecular structures of 2b, 3c, and 4c were established by single crystal X-ray diffraction measurements. 相似文献
9.
V. Crocq J. -C. Daran M. Gouygou B. Heim Y. Jeannin R. Speel 《Journal of Cluster Science》1996,7(4):505-529
The diiron ynamine complex [Fe2(CO)7{μ-CR)C(NEt2)}] (1:R=Me,2:R = C3H5.3:R=SiMe3.4:R = Ph) reacts at room temperature with diphenyldiazomethane Ph2CN2, in hexane to yield complexes [Fe2(CO)6{C(R)C(NEt2)N (NCPh2)] (5a:R=Me,6a:R=C3H5.7a R=SiMe3.8a:R=Ph) resulting from the insertion of the terminal nitrogen atom into the Fe=C carbene bond. Insertion the second nitrogen atom and formation of compounds [Fe2(CO)6zμ-C(R)C(NEt2)NN(CPh2)}] (5b:R=Me,6b:R=C3H5,7b:R=SiMe3,8b:R=Ph) is observed when compounds5a-5a are treated in refluxing hexane. Transformation of compoundsa tob is also obtained at room temperature within a few days. All compounds were identified by their1H NMR spectra. Compounds6a, 7a, 8a, and8b were characterized by single crystal X-ray diffraction analyses. Crystal data: for6a: space group = P21/n,a=12.853(1) A,b=24.800(7) A,c=8.947(6) A,β=99.29(3)°,Z=4, 2227 rellectionsR=0,038; for7a: space group=Pl,a=ll.483(4) A,b=14.975(4) A,c = 17.890(8) A,α = 82.80(3)°,β=94.29(7)°,γ=85.42(2),Z = 4, 5888 reflectionR = 0.035: for8a: space group = Pcab.a = 31.023(8) A.b=20.137(1) A.c=9.686(2) A.Z=8. 1651 reflections,R=0.071; for8b: space group=P21/n,a=21.459(4),b=10,100(3) A,c=28,439(8) A,ß=103.86(4)°,Z=8. 2431 reflections.R=0.057. 相似文献
10.
V. V. Sharutin O. K. Sharutina V. S. Senchurin 《Russian Journal of Coordination Chemistry》2014,40(2):109-114
The reaction of triphenylantimony with propiolic acid in the presence of hydrogen peroxide (molar ratios 1 : 2 : 1 and 1 : 1 : 1) in diethyl ether affords triphenylantimony dipropiolate Ph3Sb[OC(O)C≡CH]2 (I) and μ2-oxobis[(propiolato)triphenylantimony] [Ph3SbOC(O)C≡CH]2O (II). Tetraphenylantimony propiolate Ph4SbOC(O)C≡CH (III) is synthesized from pentaphenylantimony and propiolic or acetylenedicarboxylic acid in toluene. According to the X-ray diffraction data, the crystals of compounds I and III include two types of crystallographically independent molecules (a and b). The antimony atoms in molecules Ia, Ib, II, IIIa, and IIIb have the trigonal-bipyramidal coordination mode with different degrees of distortion. The OSbO and OSbC axial angles are 176.8(2)° (Ia, Ib), 170.17(15)°, 178.78(14)° (II), and 173.2(5)°, 174.4(5)° (IIIa, IIIb). The CSbC equatorial angles lie in the ranges 108.2(3)°–143.1(3)° (I), 109.0(2)°–131.0(2)° (II), and 113.1(4)°–125.4(4)° (III). The SbOSb angle in II is 141.55(19)°. The Sb-C bond lengths are 2.103(8)–2.141(5) (I), 2.105(5)–2.119(5) (II), and 2.076(12)–2.166(13) Å (III). The Sb-O distances increase in a series of I, II, and III: 2.139(6)–2.156(7) (Ia, Ib); 2.206(4), 2.218(3) (II); and 2.338(10), 2.340(10) Å (III). 相似文献
11.
Winfried Wendelin Karl Schermanz Johannes Kerbl 《Monatshefte für Chemie / Chemical Monthly》1983,114(6-7):717-737
Guanidine reacts with chalkone1 a, 4-methylchalkone1 b and 4′-methylchalkone1 c resp. to yield mixtures of pyrimidinamines2 a,3 b and3 c (=3 b) resp. with (2:1)-condensatesA,B andC resp. The structures of the compoundsA-C (whicha priori could be dihydropyrimidopyrimidines4 a-c or5 a-c or6 a-c) are elucidated. NMR-investigations show that the saltsA-C · HCl must be symmetrically substituted pyrimidopyrimidinyliumchlorides4 a-c · HCl or5 a-c · HCl (and not6 a-c · HCl). Furthermore, it is proved by chemical methods that the condensatesB · HCl andC · HCl are pyrimidopyrimidinyliumchlorides4 b andc · HCl (and not5 b andc · HCl): The structure ofB · HCl (=4 b · HCl) was established by total synthesis of dimethylpyrimidopyrimidinyliumpicrate9 b-Pi from10 c (via13 c · HI-18 · HCl) and transformation ofB · HCl into an identical salt9 b-Pi via hexahydropyrimidopyrimidine8 b · HCl. The structure ofC · HCl (=4 c · HCl) was determined by comparison of its hydrogenation product (=8c · HCl) with8 b · HCl. The structure of condensateA · HCl (=4 a · HCl) results from conclusion by analogy. The spatial structure of4 a-c · HCl and8 a-c · HCl is discussed; it was established by NMR that the salts are racemic mixtures of stereoisomers4 a-c K · HCl and8 a-c K · HCl resp. and their antipodes (with C2 symmetry). 相似文献
12.
The first order rate constants for the tautomerization of the hydrio(alkynyl) clusters Ru3Pt(μ-H){μ4-ν2-C ≡ C1Bu}(CO)9(L2);1a: L2 = dppe,1b; L2 = dppet,1c; L2 = dppp and1d; L2 =S,S-dppb to the corresponding vinylidene clusters Ru3Pt{μ4-ν2-C = C(H)tBu}(CO)9(L2)2 have been measured, and they follow the orser1d <1a <1b ~1c. The reactions involving1a and1d exhibit an inverse kinetic deuterium isotope effect. The structures of1b, 2b, 2c, and2d were determined by X-ray crystallography, and are compared with those of1a and2a which have been previously reported. Crystal data for1b, space groupPbca,a = 13.338(4) Å,b = 17.771(6) Å,c = 36.092(8) Å,Z = 8,R(R w) = 0.059(0.058) for 2342 absorption corrected, observed data; for2b, space group P21/n,a = 10.566(2) Å,b = 20.234(5) Å,c = 20.270(3) Å,β = 96.11(1)°,Z = 4,R(R w) = 0.043(0.053) for 5865 absorption corrected, observed data; for2c, space group P21/n,a = 14.211(5) Å,b = 19.534(2) Å,c = 15.870(2) Å,β = 100.81(2)°,Z = 4,R(R w) = 0.055(0.031) for 6566 absorption corrected, observed data: for2d, space group P212121,a = 12.309(4) Å,b = 19.047(6) Å,c = 19.206(4) Å,Z = 4,R(R w) = 0.055(0.053) fpr 2151 absorption corrected, observed data. The fluxional behavior of1d and1e (which consists of two interconverting isomers) has been examined by variable temperature13C NMR spectroscopy and by31P EXSY. 相似文献
13.
Yan Li Hui-ling Liu Yan-bo Sun Zhuo Li Xu-ri Huang Chia-chung Sun 《Theoretical chemistry accounts》2009,124(1-2):123-137
The complex triplet potential energy surface for the reaction of HCNO with NH is investigated at the G3B3 level using the B3LYP/6-311++G(d,p), and QCISD/6-311++G(d,p) geometries. Various possible isomerization and dissociation pathways are probed. The initial association between HCNO and NH is found to be carbon to nitrogen attack leading to HNCHNO 2a, which can convert to 2b, 2c, and 2d. Subsequently, 1,4-H-shift of 2a to form NCHNOH 3a followed by dissociation to P 2 (1HCN + 3HON) is the most feasible pathway. Much less competitively, 2d undergoes successive 1,3-H-shift and C-N cleavage to form HNCNOH 8b, and then to product P 3 (1HNC + 3HON), the second feasible pathway. 8b can alternatively isomerize to 8c followed by N–O bond rupture to generate P 6 (2OH + 2HNCN), the lesser followed feasible pathway. In addition, 2b takes continuously 1,3- and 1,2-H-shift to form NC(H)NHO 6a, then to ONHCNH 7a which can convert to 7b. Eventually, 7b may take C-N bond fission to produce P 5 (1HNC + 3HNO), the least feasible pathway. The present paper may be helpful for future experimental identification of the product distributions for the title reaction, and may be helpful to deeply understand the mechanism of the title reaction. 相似文献
14.
Li Yang Vladimir N. Nesterov Xiaoping Wang Michael G. Richmond 《Journal of Cluster Science》2012,23(3):685-702
The reaction of the cluster HOs3(CO)10(??-SC6H4Me-4) (1) with the diphosphine 4,5-bis(diphenylphosphino)-4-cyclopentadiene-1,3-dione (bpcd) has been investigated. 1 reacts with bpcd at room temperature in the presence of Me3NO to give the isomeric clusters 1,2-HOs3(CO)8(bpcd)(??-SC6H4Me-4) (2a) and 1,1-HOs3(CO)8(bpcd)(??-SC6H4Me-4) (2b). Clusters 2a and 2b have been isolated, and the molecular structure of each compound has been established by X-ray crystallography. The X-ray structure of 2a confirms the coordination of one of the non-hydride-bridged Os?COs vectors by the bpcd ligand, while the structure of 2b exhibits a chelating bpcd ligand that is bound to one of the osmium centers ligated by the thiolate and hydrido ligands. 2a and 2b are stable in refluxing toluene and show no evidence for bridge-to-chelate isomerization of the ancillary bpcd ligand. DFT calculations on 2a and 2b indicate that the former cluster is the thermodynamically more stable isomer. Near-UV irradiation of 2b leads to CO loss and ortho metalation of the thiolate moiety, yielding the dihydride cluster H2Os3(CO)7(bpcd)(??,??-SC6H3Me-4) (3). The conversion of 2b to 3 and free CO is computed to be endothermic by 14.1?kcal/mol and the reaction is driven by the entropic release of CO. The photochemically promoted ortho-metalation reaction is isomer dependent since cluster 2a is inert under identical conditions. 相似文献
15.
A. G. Shipov S. V. Grüner A. A. Korlyukov E. P. Kramarova T. P. Murasheva S. Yu. Bylikin Vad. V. Negrebetskii F. A. Ivashchenko D. V. Airapetyan G. Ya. Zueva M. Yu. Antipin Yu. I. Baukov 《Russian Chemical Bulletin》2010,59(4):761-770
Reactions of GeBr4 with N,N-dimethyl-2-trimethylsiloxypropionamide (2a), (S)-2-trime-thylsiloxypropionpyrrolidide ((S)-2b), and N,N-dimethyl-O-(trimethylsilyl)mandelamide (2c) afforded pentacoordinated neutral (O,O)-monochelates, viz., N,N-dimethyl-2-tribromoger-myloxypropionamide (3a), (S)-2-tribromogermyloxypropionpyrrolidide ((S)-3b), and N,N-dimethyl-O-(tribromogermyl)mandelamide (3c), respectively. X-ray diffraction study was performed for tribromides 3a, (S)-3b, and 3c, as well as for the N,N-dimethylmandelamide (1c) described earlier. According to the X-ray diffraction data, the Ge atom in tribromides 3a, (S)-3b, and 3c is pentacoordinated and has trigonal bipyramidal configuration with two halogen atoms and oxygen atom of the ether group in the equatorial positions and the halogen atom and the amide oxygen atom in the axial fragment, the bonds in which are somewhat longer as compared to the analogous bonds in tetracoordinated Ge compounds. 相似文献
16.
Eman M. H. Abbas Kamelia M. Amin Wageeh S. El-Hamouly Dina H. Dawood Mohamed M. Abdalla 《Research on Chemical Intermediates》2014,40(2):847-869
A series of new compounds bearing a 1,3-benzothiazol-2-one nucleus have been synthesized using 5,6-dimethyl-3-(2-oxo-propyl)-1,3-benzothiazol-2-one (1) as a key starting compound. The reaction of 1 with some nucleophilic compounds led to the formation of compounds 2, 3, 4, 5a, b, 6 and 7a, b. The thiosemicarbazone derivatives 7a, b were treated with a number of halo ketones to produce the new heterocyclic compounds 9–13, while their reaction with acid anhydrides led to the formation of the derivatives 14 and 15. Also, compound 1 was condensed with different aromatic aldehydes to afford the corresponding chalcones 18–22. The structures of all the novel compounds have been determined by analytical and spectral data. Some of the compounds were selected to be evaluated as anti-inflammatory and analgesic agents. 相似文献
17.
Mukesh Kumar Atal Veena Dhayal Meena Nagar Rakesh Bohra Kuldeep S. Rathore Narendra S. Saxena 《Journal of Sol-Gel Science and Technology》2010,53(1):67-78
Reaction of [VO(OPr i )3] (1) with [O(CH2CH2OH)2] in 1:1 molar ratio in anhydrous benzene yield glycol-modified precursor, [VO{OCH2CH2OCH2CH2O}{OPr i }] (2). Further reactions of (2) with internally functionalized oximes in anhydrous benzene yield heteroleptic complexes of the type [VO{OCH2CH2OCH2CH2O}{ON=C(R)(Ar)}] (3–8) {where R=CH3, Ar=C4H3O-2 (3), C4H3S-2 (4), C5H4N-2 (5); and when R=H, Ar=C4H3O-2 (6), C4H3S-2 (7), C5H4N-2 (8)}. All these derivatives have been characterized by elemental analyses, molecular weight measurements and spectroscopic techniques. The crysoscopic molecular weight measurement as well as FAB mass study suggests dimeric nature of (2). However, FAB mass spectrum of (4), and the crysoscopic molecular weight measurements of (3), (4), (5) and (6) indicate the monomeric behavior of the oximato derivatives (3–8). Hexa-coordination around vanadium(V) has been proposed for both monomeric and dimeric derivatives. Sol–gel transformations of (1), (2) or (4) to vanadia [(a), (b) or (c), respectively] have been carried out at low sintering temperature (600 °C). The XRD patterns of (a), (b) or (c) indicate formation of a single orthorhombic phase in all the three cases. The SEM images suggest grain like [for (a) and (b)] and rod like [for (c)] morphology of the crystallites. IR, Raman spectra as well as EDX analyses indicate formation of pure vanadia. Absorption spectra of the vanadia (b) and (c) suggest energy band gaps of 2.53 and 2.65 eV, respectively. 相似文献
18.
Eyup Akgün Thomas Kämpchen Ulf Pindur 《Monatshefte für Chemie / Chemical Monthly》1983,114(2):219-225
The 4-pyrazoline-3-one1 reacts with 4-dimethylaminobenzaldehyde to yield the stable asymmetric cyanine dye2b which reacts with1 to give the colorless (aryl) (dipyrazolyl) methane3b. Using aldehydes with less cationstabilizing groups the polymethines2 are not isolated but only the methanes3. The structures of2b and3 are discussed by1 H,13C and Hetero NMR spectra. 相似文献
19.
The reactions of pentaphenylantimony with succinic, malic, and tartaric acids (mole ratio 2: 1) in toluene afford bis(tetraphenylantimony) succinate (I), malate (II), and tartrate (III) in yields of 98, 92, and 94%, respectively. According to the X_ray diffraction analysis results, molecules I and II are centrosymmetric. In compound II, the hydroxy group in the acid residue is disordered over two positions. Crystal III includes two types of crystallographically independent molecules (a and b). The antimony atoms in compounds I, II, IIIa, and IIIb have distorted trigonal bipyramidal coordination modes. The axial angles CaxSbOax are 166.80(8)° (I); 174.8(2)° (II); 176.4(4)°, 177.4(3)° (IIIa); and 173.3(4)°, 172.7(4)° (IIIb). The equatorial angles CeqSbCeq vary in the ranges 99.3(1)°–154.5(1)° (I); 115.2(2)°–123.3(2)° (II); 115.7(4)°–123.3(4)° 115.2(5)°–125.6(5)° (IIIa); and 107.9(4)°-129.1(4)°, 113.7(4)°-124.8(5)° (IIIb). The Sb-C and Sb-O bonds are 2.138(3)-2.176(3), 2.319(2) Å (I); 2.111(6)–2.163(5), 2.243(4) Å (II); 2.072(13)–2.169(11), 2.252(7), 2.284(7) Å (IIIa); and 2.047(11)–2.190(11), 2.224(7), 2.256(7) Å (IIIb). The intramolecular distances Sb…O=C are 2.528(3) (I); 3.267(7) (II); 3.381(7), 3.436(7) (IIIa); and 3.351(7), 3.162(7) Å (IIIb). For structures I, II, and III, the CIF files are CCDC 929151, 941542, and 941543, respectively. 相似文献
20.
V. N. Serezhkin E. V. Peresypkina S. A. Novikov A. V. Virovets L. B. Serezhkina 《Russian Journal of Inorganic Chemistry》2014,59(8):788-797
Four new fluorochromatouranylates, namely, K[UO2(CrO4)F] · 1.5H2O (I), Rb[UO2(CrO4)F] · 1.5H2O (II), Rb[UO2(CrO4)F] · 0.5H2O (III), and Cs[UO2(CrO4)F] · 0.5H2O (IV), have been synthesized, and their crystallographic characteristics have been determined. All the compounds crystallize in monoclinic system, space group P21/c, with the unit cell parameters a = 13.1744(5) Å, b = 9.4598(3) Å, c = 13.0710(4) Å, β = 103.746(1)°, Z = 4, R = 0.0235 (I); a = 13.5902(7) Å, b = 9.5022(4) Å, c = 13.2271(6) Å, β = 102.914(2)°, Z = 4, R = 0.0247 (II); a = 24.7724(8) Å, b = 12.6671(4) Å, c = 9.4464(3) Å, β = 97.661(1)°, Z = 8, R = 0.0448 (III); a = 25.725(1) Å, b = 12.8261(5) Å, c = 9.4929(4) β = 97.208(1)°, Z = 8 (IV). The pairs of compounds I and II and compounds III and IV are isostructural. Crystals of compounds I–III have been subjected to complete X-ray diffraction study. It has been established that the structures of compounds I–III are built of [UO2(CrO4)F] n n? layers, which are parallel to the (100) plane and linked into a framework by alkali-metal cations located between layers, together with water molecules. The effect of topological and geometric isomerism on the structural features of 34 known uranyl compounds of the AT3M2 crystallochemical group, to which the studied compounds I–III also belong, is discussed. 相似文献