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1.
《Journal of Coordination Chemistry》2012,65(4):397-408
Abstract Two copper(I) complexes, [Cu(H2net)2Cl] · CH2Cl2 (1) and [Cu(H2nmt)2Cl]2 · (CHCl3)2 (2), were synthesized by the reaction of CuCl2 · 2H2O with N-(p-nitrophenyl)-N′-(ethoxycarbonyl)-thiourea (H2net) and N-(p-nitrophenyl)-N′-(methoxycarbonyl)-thiourea(H2nmt), respectively. Both complexes crystallize in the monoclinic space group C2/c. For complex 1, a = 29.52(2), b=13.920(6), c = 14.873(3)Å; β= 101.75(2)°, V = 5984(4) Å3, Z = 8 and R = 0.053; for complex 2, a = 30.68(1), b = 13.369(4), c = 14.226(7) Å, β = 99.52(4)°. V = 5754(4) Å3, Z = 4 and R = 0.063. In complex 1, two H2net molecules are bonded to Cu(I) atom through two S atoms forming a mononuclear complex with trigonal geometry for the Cu(I) ion [Cl(1)-Cu-S(1)=118.54(7), Cl(1)-Cu-S(2)=119.70(7), S(1)-Cu-S(2)=112.17(8)°, Cu-S(1) = 2.251(2), Cu-S(2) = 2.255(2), Cu-Cl(1) = 2.263(2) Å]. Complex 2 is a dimer formed by long Cu-S interactions [Cu-S* = 2.607(3) Å] from adjacent twc H2nmt molecules; the Cu(I) ion has distorted tetrahedral coordination [Cl(1)-Cu-S(1) = 119.8(1), Cl(1)-Cu-S(2)=120.0(1), S(1)-Cu-S(2)=108.85(9)°] with unequal Cu-S [2.268(2), 2.247(2)Å] and Cu-Cl(1) [2.255(2)Å] bonds. 相似文献
2.
HAN Ying TAO Wen-Tian HUANG Yao-Zeng JIN Xiang-Lin SUN JieLaboratory of Organometallic Chemistry Shanghai Institute of Organic Chemistry Chinese Academy of Sciences Shanghai China 《中国化学》1994,12(6):542-548
Tricyclopentylgallium reacted with phenol, naphthol respectively to yield phenox-ide (or naphthoxide) of biscyclopentylgallium which have been characterized by elemental analysis, IR, 1H NMR and mass spectrometry. X-ray diffraction analysis of compound 1 indicated that it belongs to the monoclinic system, space groups P21/c, with cell constants 0=9.602(3), 6=14.365(7), c=11.256(4)A, and β=97.54(3)°, Z=2(dimers), R=0.0706. Compound 2 assigned to the triclinic system, space groups P1 with cell constants a=9.392(4), 6=9.928(7), c=11.263(7) A, a=112.48(5), β=104.74(4), γ=99.95(5)°, and Z=l(dimers), R=0.0526. The molecule of 1 or 2 contains an oxygen-bridged coplanar Ga2O2 four-membered ring respectively. 相似文献
3.
Mohamad Jaber Al-Jeboori Hasan Ahmad Hasan Worood A. Jaafer Al-Sa’idy 《Transition Metal Chemistry》2009,34(6):593-598
The new multidentate Schiff-base (E)-6,6′-((1E,1′E)-(ethane-1,2-diylbis(azan-1-yl-1-ylidene))bis(methan-1-yl-ylidene))bis(4-methyl-2-((E)(pyridine-2-ylmethylimino)methyl)phenol) H2L and its polymeric binuclear metal complexes with Cr(III), Mn(II), Fe(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II)
are reported. The reaction of 2,6-diformyl-4-methyl-phenol with ethylenediamine in mole ratios of 2:1 gave the precursor 3,3′-(1E,1′E)-(ethane-1,2-diylbis(azan-1-yl-1ylidene))bis(methan-1-yl-1-ylidene)bis(2-hydroxy-5-methylbenzaldehyde) W. Condensation of the precursor with 2-(amino-methyl)pyridine in mole ratios of 1:2 gave
the new N6O2 multidentate Schiff-base ligand H2L. Upon complex formation, the ligand behaves as a dibasic octadentate species with the involvement of the nitrogen atoms
of the pyridine groups in coordination for all complexes. The mode of bonding and overall geometry of the complexes were determined
through physico-chemical and spectroscopic methods. These studies revealed octahedral geometries for Cr(III), Mn(II), Fe(II),
Co(II), Ni(II), Cu(II), Cd(II) and Hg(II) complexes of general formulae [Cr2III(L)Cl2]Cl2, [Ni2II(L)(H2O)2]Cl2 and [M2(L)Cl2] and five co-ordinate Zn(II) complex of general formula [Zn2II(L)]Cl2. 相似文献
4.
Three new neolignans, named 1‐deoxycarinatone ( 1 ), isodihydrocarinatidin ( 2 ), and isolicarin A ( 3 ), together with the known neolignan (+)‐dehydrodiisoeugenol ( 4 ), were isolated from mace (the aril of Myristica fragrans Houtt .). Their structures were elucidated as 2‐[(1S)‐2‐(4‐hydroxy‐3‐methoxyphenyl)‐1‐methylethyl]‐6‐methoxy‐4‐(prop‐2‐enyl)phenol ( 1 ), 4‐[(2R,3R)‐2,3‐dihydro‐7‐methoxy‐3‐methyl‐5‐(prop‐2‐enyl)benzofuran‐2‐yl]‐2‐methoxyphenol ( 2 ), and 4‐{(2S,3R)‐2,3‐dihydro‐7‐methoxy‐3‐methyl‐5‐[(1E)‐prop‐1‐enyl]benzofuran‐2‐yl}‐2‐methoxyphenol ( 3 ) on the basis of spectroscopic data. 相似文献
5.
1-Hydroxy-2-methyl-2-(penta-2,4-dienyl)-1,2-dihydronaphthalene ( 2 ), on treatment with 0,75N H2SO4 in ether at 0°, underwent a [1s, 2s]-sigmatropic rearrangement to give 2-methyl-1-(penta-2,4-dienyl)-naphthalene ( 5 ), cf. scheme 2. 2-Hydroxy-1-methyl-1-(penta-2,4-dienyl)-1,2-dihydronaphthalene ( 4 ) under the same conditions gave 38% of the [1s, 2s]-product 1-methyl-2-(penta-2,4-dienyl)-naphthalene ( 6 ), together with 26% 1-methylnaphthalene, 21% 1-methyl-4-(penta-2,4-dienyl)-naphthalene ( 7 ) and 1% 1-methyl-5-(penta-2,4-dienyl)-naphthalene ( 8 ), cf. scheme 2. Most likely the latter two naphthalene derivatives at least are products of an intermolecular process. 相似文献
6.
E. Hecht T. Gelbrich S. Wernik R. Weimann K.-H. Thiele J. Sieler H. Schumann 《无机化学与普通化学杂志》1998,624(6):1061-1066
Chiral Dimethylgallium Amino Alkoxides Me3Ga reacts with (S)-1-methyl-2-pyrrolidinyl-methanol, (+);(–)-2-piperidyl-methanol, and (S)-α,α,-diphenyl-2-pyrrolidinyl-methanol in molar ratio 1 : 1 with formation of the corresponding dimethylgallium aminoalkoxides 1 – 3 . As a consequence of the Ga–N-interaction new centres of chirality containing asymmetric surrounded N-atoms are formed. Compounds 1 – 3 were characterized by their 1H, 13C nmr and mass spectra. The crystal structures of 1 – 3 were determined by single crystal structure analysis. 1 and 2 are dimeric in solid state, 3 is forming monomeric molecules. 1 and 3 crystallize in the monoclinic space group P21 with Z = 2, a = 7.245(4), b = 11.887(3), c = 11.807(6) Å, β = 93.48(3)° for 1 and Z = 4, a = 11.0871(7); b = 6.539(4), c = 12.6919(8) Å, β = 107.04(1)° for 3 . 2 and 2 a crystallize in the monoclinic space groups C2/m and C2/c with Z = 2, a = 15.891(3), b = 9.526(2), c = 7.345(1) Å, β = 111.89(3)° for 2 and Z = 4, a = 19.374(4), b = 8.430(2), c = 19.961(4) Å, β = 100.09(3)° for 2 a . 相似文献
7.
Nabih S. Girgis Howard B. Cottam Roland K. Robins 《Journal of heterocyclic chemistry》1988,25(2):361-366
The 2′-deoxyribofuranose analog of the naturally occurring antibiotics SF-2140 and neosidomycin were prepared by the direct glycosylation of the sodium salts of the appropriate indole derivatives, with 1-chloro-2- deoxy-3,5-di-O-p-toluoyl-α-D-erythropentofuranose ( 5 ). Thus, treatment of the sodium salt of 4-methoxy-1H- indol-3-ylacetonitrile ( 4a ) with 5 provided the blocked nucleoside, 4-methoxy-1-(2-deoxy-3,5-di-O-p-toluoyl-β- D-erythropentofuranosyl)-1H-indol-3-ylacetonitrile ( 6a ), which was treated with sodium methoxide to yield the SF-2140 analog, 4-methoxy-1-(2-deoxy-β-D-erythropentofuranosyl)-1H-indol-3- ylacetonitrile ( 7a ). The neosidomycin analog ( 8 ) was prepared by treatment of the sodium salt of 1H-indol-3-ylacetonitrile ( 4b ) with 5 to obtain the blocked intermediate 1-(2-deoxy-3,5-di-O-p-toluoyl-β-D-erythropentofuranosyl) ?1H-indol-3-ylace-tonitrile ( 6b ) followed by sodium methoxide treatment to give 1-(2-deoxy-β-D-erythropentofuranosyl)-1H- indol-3-ylacetonitrile ( 7b ) and finally conversion of the nitrile function of 7b to provide 1-(2-deoxy-β-D- erythropentofuranosyl)-1H-indol-3-ylacetamide ( 8 ). In a similar manner, indole ( 9a ) and several other substituted indoles including 1H-indole-4-carbonitrile ( 9b ), 4-nitro-1H-indole ( 9c ), 4-chloro-1H-indole-2-carboxamide ( 9d ) and 4-chloro-1H-indole-2-carbonitrile ( 9e ) were each glycosylated and deprotected to provide 1-(2-deoxy-β-D-erythropentofuranosyl)-1H-indole ( 11a ), 1-(2-deoxy-β-D-erythropentofuranosyl)-1H-indole-4- carbonitrile ( 11b ), 4-nitro-1-(2-deoxy-β-D-erythropentofuranosyl)-1H-indole ( 11c ), 4-chloro-1-(2-deoxy-β-D- erythropentofuranosyl)-1H-indole-2-carboxamide ( 11d ) and 4-chloro-1-(2-deoxy-β-D-erythropentofuranosyl)- 1H-indole-2-carbonitrile ( 11e ), respectively. The 2′-deoxyadenosine analog in the indole ring system was prepared for the first time by reduction of the nitro group of 11c using palladium on carbon thus providing 4-amino-1-(2-deoxy-β-D-erythropentofuranosyl)- 1H-indole ( 16 , 1,3,7-trideaza-2′-deoxyadenosine). 相似文献
8.
《Journal of Coordination Chemistry》2012,65(4):505-521
Abstract The grinding of a 2: 1 molar ratio mixture of isonitrosoacetylacetone and 1,3-diaminopropan-2-ol led to formation of the tribasic ligand (H3L), (1) with two oxime groups and a flexible alcoholic backbone. The 1:2 molar ratio reaction of (1) with CuX2 produced the planar dinuclear complexes LCu2(X) nH2O; × = acetate (2), phenylacetate (3), formate (4), monochloroacetate (5), dichloroacetate (6), trichloroacetate (7), benzoate (8), and p-hydroxybenzoate (9); n = 1 for (2) and (8); n = 2 for (3)-(7); and n = 4 for (9). The copper(II) ions are bridged by the carbox-ylate and the alcoholic oxygen. The strong antiferromagnetic interactions in (2)-(9) are impeded in (5)-(7) by the chloroacetate bridge withdrawing electron density from the carboxylate. The latter bridge is replaced by picrate in the 1:1 molar ratio reaction of (2) with picric acid (10). The 1:1 molar ratio reaction of (1) with copper(II) acetate produced the tetranuclear [HLCu]2[LCu2(OAc)] 5H2O (11), whereas the 2:1 molar ratio reaction, similar to the reaction which led to (8), produced HLCu (12). The latter complex reacted (1:1 molar ratio) with either copper(ll) acetate or nickel(II) acetate to produce complexes (2) and the heterodinuclear LNi-Cu(OAc) 2H2O (13), respectively. Similar reactions with (11) gave the same complexes (2) and (13). The acid adducts of (9) with p-hydroxybenzoic acid (14) and LCu2(X)-HX (15); × = p-aminobenzoic acid were isolated. The cobalt(II) analogue of the mononuclear (12), HLCo 2H2O (16) was obtained from the 1:1 molar reaction of (1) with cobalt(II) acetate. The supramolecular structure of (11), (12) and (16) took place via intermolecular hydrogen bonding of the alcoholic proton with the oximato oxygen of the adjacent molecule which mediated electron density and allowed for a magnetic exchange interaction. The suggested structures of the ligand and metal complexes are in accordance with analytical, spectral and magnetic moment data. 相似文献
9.
3-Dcazacytosine (4-amino-2-pyridone, 3 ), 3-doazauracil (4-hydroxy-2-pyridone, 5 ), 3-deaza-cytidine (4-amino-1-β-D-ribofuranosyl-2-pyridonc, 9 ), and 3-deazauridine (4-hydroxy-1-β-D-ribo-furanosyl-2-pyridone, 11 ) were prepared in high overall yields from 1-methoxy-1-buten-3-yne ( 1 ). Ethyl 3,5,5-triethoxy-3-pentenoate ( 2 ), obtained from acylatioti of 1 with diethyl carbonate and subsequent in situ conjugate addition of ethoxide, was cyelized with ammonia to provide 3 . Diazotization of 3 and subsequent in situ hydroxydediazotization afforded 5 . Nucleoside 9 was obtained from the stannic chloride-catalyzed condensation of bis-trimethylsilylated 3 and 1-O-acetyl-2,3,5-tri-O-benzoyl-β-D-ribofuranose ( 7 ), followed by ammonolysis of the blocking groups. Diazotization of 9 and subsequent in situ hydroxydediazotization afforded nucleosidc 11 . 相似文献
10.
A series of nitroimidazoles were subjected to hydroxymethylations under a variety of conditions. Hydroxymethylation of 1-(2-hydroxyethyl), 1-(2-acetoxyethyl), and 1-(2-chloroethyl) substituted 5-nitroimidazoles with paraformaldehyde in dimethyl sulfoxide yielded the respective 2-hydroxymethyl analogs (5–7). However, attempts to hydroxymethylate 1-(2-hydroxyethyl), 1-(2-acetoxyethyl), 1-(2-cyanoethyl) substituted 4-nitroimidazoles and 1-(2-hydroxyethyl)-2-nitroimidazole were unsuccessful. Treatment of 1-(2-acetoxyethyl)-5-nitro-2-imidazolecar-baldehyde(10) with hydroxylamine-O-sulfonic acid afforded a mixture of corresponding 2-carbonitrile (12) and 2-(N-hydroxy)carboximidamide (13). Hydrolysis of 10 with ethanolic hydrochloric acid yielded 8-ethoxy-5,6-dihydro-3-nitro-8H-imidazo[2,1-c] [1,4]oxazine (11) which, on subsequent reaction with hydroxylamine-O-sulfonic acid, afforded 1-(2-hydroxyethyl)-5-nitroimidazole-2-(N-hydroxy)carboximidamide (15). Reaction of 4(5)-nitroimidazole with chloropropionitrile produced a mixture of the isomeric 1-(2-cyanoethyl) substituted 4- and 5-nitroimidazoles. Treatment of 2,4(5)-dinitroímidazole with chloropropionitrile afforded a mixture of 4(5)-chloro-5(4)-nitroimidazole and 1-(2-cyanoethyl)-4-nitro-5-chloroimidazoIe. Reaction of nitroimidazoles with acrylonitrile in the presence of Triton B yielded the corresponding 1-(2-cyanoethyl) substituted derivatives. 相似文献
11.
Hai‐Liang Zhu Xiu‐Ying Liu Xian‐Jiang Wang Feng Yang Anwar Usman Hoong‐Kun Fun 《无机化学与普通化学杂志》2003,629(11):1986-1990
Three polymeric silver(I) complexes with terephthalate anions as counterions or ligands, [Ag(pren)]2(tp)·2H2O ( 1 ), [Ag(en)][Ag(μ2‐tp)]·H2O ( 2 ), and [Ag2(μ4‐tp)(apy)2] ( 3 ) (where pren = 1, 2‐propylenediamine, tp =terephthalate dianion, en = ethylenediamine, and apy = 2‐aminopyridine) were synthesized and characterized by X‐ray single crystal analysis and infrared spectroscopy. 1 crystallizes in the monoclinic space group P211/c with a = 11.3221(5), b = 7.1522(3), c = 14.8128(5)Å, V = 1015.77(7)Å3, β = 122.132(2), and Z = 2. 2 crystallizes in the orthorhombic space group Pnma with a = 9.6144(6), b = 11.3465(7), c = 11.4810(7)Å, V = 1252.5(1)Å3, and Z = 4. 3 crystallizes in the monoclinic space group P21/n with a = 8.2003(5), b = 5.8869(4), c = 18.3769(11)Å, β = 92.593(1), V = 886.2(1)Å3, and Z = 4. Terephthalate dianions are not coordinated to the metal atoms in 1 , but act as a μ2‐bridging ligand in 2 and as a μ4‐bridging ligand in 3 . 相似文献
12.
Xu‐Jun Dong Xiang‐Dong Zhu Yi‐Feng Wang Qiong Wang Peng Ju Shide Luo 《Helvetica chimica acta》2006,89(5):983-987
Three new secoprezizaane sesquiterpene lactones, (1R,2S)‐1,2‐epoxyneomajucin ( 1 ), (2R)‐2‐hydroxyneomajucin ( 2 ), and (2R)‐2‐hydroxymajucin ( 3 ), along with six known compounds ( 4 – 9 ), were isolated from the poisonous shrub Illicium micranthum. Their structures were established by in‐depth analyses of spectroscopic and mass‐spectrometric data. 相似文献
13.
Photolysis of N-benzyl-N-phenylearbamoylazide (IVc) afforded 1-benzy 1-2-benzimidazolinone (Ic), 2-benzimidazolinone (IIe), 4-benzy 1-2-benzimidazolinone (IIe), and 5-benzy1-2-benzimidazo-linone (IIf)- The same reaction of N-benzyl-N-(4-chlorophenyl) carbamoyl azide (IVd) gave 3-benzyl-1-(phenylhydrazocarbonyl)-2-benzimidazolinone (VIb) besides the above four products. In the case of N-benzyl-4-(4-butoxyphenyl)carbamoyl azide (IVe), 1-benzy1-5-butoxy-2-benz-imidazolinone (1e), 5-butoxy-2-benzimidazolinone (IId), 5-benzy1-2-benzimidazolinone (IIf), and 4-benzy1-6-butoxy-2-benzimidazolinone (IIg). 相似文献
14.
Keikichi Uno Mutsuko Ohara Harold G. Cassidy 《Journal of polymer science. Part A, Polymer chemistry》1968,6(10):2729-2740
Ten vinylhydroquinone and one vinyl resorcinol derivatives are compared, particularly with respect to NMR spectra and copolymerizability with styrene. They are vinylhydroquinone dimethyl ether (I), vinyl-O,O′-bis(1-ethoxyethyl)hydroquinone (II), vinylhydroquinone di(2-pentyl)ether (III), 4-vinyl resorcinol bismethoxymethyl ether (IV), 2-vinyl-5-methylhydroquinone dimethyl ether (V), 2-vinyl-5-methyl-O,O′-bis(1-ethoxyethyl)hydroquinone (VI), 2-vinyl-6-methylhydroquinone dimethyl ether (VII), 2-vinyl-5-tert-butylhydroquinone dimethyl ether (VIII), 2-vinyl-5-chlorohydroquinone dimethyl ether (IX), 2-vinyl-3,6-dimethylhydroquinone dimethyl ether (X), and 2-vinyl-3,5,6-trimethylhydroquinone dimethyl ether (XI). All the vinyl protons have almost the same coupling constants. Though subtle distinctions are found among all the spectra, they can in general be put into two groups on the basis of the chemical shifts. Let the hydrogen on carbon-1 of the vinyl group be A, the hydrogen cis to A be B the hydrogen trans to A be C, then in the first group, (I) through (IX), the chemical shifts (τ) are (A) 3.02 ± 0.08, (C) 4.41 ± 0.05, and (B) 4.87 ± 0.07, and in the second group, (X) and (XI), they are (A) 3.30 ± 0.03, (C) 4.49 ± 0.01, and (B) 4.59 ± 0.03. It is supposed that in (X) and (XI) the vinyl group is out of the plane of the ring, because of the two ortho substituents, and this conformation is reflected in the NMR data. Ultraviolet spectra are consonant with this interpretation, since the λmax of (X) and (XI) correspond closely with those of nonvinyl reference compounds, while those of (II), (V), and (VIII) are shifted to longer wavelengths. When these compounds are copolymerized separately with styrene, the behaviors are classifiable into the following three groups, where r1 and r2 are monomer reactivity ratios with styrene as the first monomer: (i) r1 < 1 and r2 < 1 for compounds (II) and (III) and the reference compound O,O′-dibenzoylvinylhydroquinone, (ii) r1 < 1 and r2 > 1 for compounds (I), (V), (VII), (VIII), (IX), and (iii) r1 > 1 and r2 = 0 for compounds (X) and (XI). These behaviors are correlated with the effect of electronegativity of groups on the stability of the radical at the growing end of the chain and with the simultaneous effects of steric hindrance. 相似文献
15.
Helen Stoeckli-Evans Lotte Brehm Philippe Pousaz Klaus Bernauer Hans-Beat Bürgi 《Helvetica chimica acta》1985,68(1):185-191
Synthesis of the pentadentate ligand 2,6-bis(3-carboxy-1,2-dimethyl-2-azapropyl)pyridine yields a mixture of the racemic and meso-isomers which it was difficult to separate by column chromatography. When the cationic Co(III)-complex of this ligand was crystallized with hexafluorophosphate as anion, two distinct crystalline forms were produced. The complex of the racemic ligand, 1 , has C2 symmetry and is a dihydrate; a = 8.999(8), b = 12.047(6), c = 20.65(1) Å, orthorhombic, space group Peen,Z = 4, R = 0.074 for 1439 observed reflections. The complex of the meso-ligand, 2 , shows two independent molecules ( 2A and 2B ) per asymmetric unit, both monohydrates with a resolved disordered H2O molecule in 2A ; a = 10.109(4), b = 12.835(2), c = 16.651(3) Å, α = 89.5(1)°, β = 84.7(3)°, γ = 88.6(3)°, triclinic, space group P1 , Z = 4, Rs = 0.054 for 4198 observed reflections. The coordination around the Co-atom is distorted octahedral in both complexes, with the coordinated H2O molecule trans to the pyridine N-atom. In the racemic form of the complex, 1 , the pyridine ring is twisted about the Co-N(1) bond with respect to the plane defined by atoms Co, N(1), O(W1), N(2) and N(2P) by 17.2(2)°. In the meso-form of the complex, 2 , the CH3 substituent C(8P) on atom C(4P), is now axial with respect to the 5-membered chelate ring. As a result of steric hinderance between atom O(1) and CH3(8P), the pyridine ring has been displaced from the best mean-plane formed by atoms Co, O(W1), N(2) and N(2P). The principal axis of the pyridine ring C(3)…N(1), makes an angle of 14.1(1)° (mean) with this plane. At the same time the pyridine ring is twisted about axis C(3)…N(1) with respect to this plane by 19.7(1)° (mean). 相似文献
16.
Pariya Bazyari Masoumeh Tabatabaee Navid Nasirizadeh Michal Dušek Václav Eigner 《无机化学与普通化学杂志》2020,646(17):1444-1448
Reaction of 4-amino-5-methyl-1,2,4-triazol-3(2H)-thione (AMTT) and 4-amino-6-methyl-3-thio-3,4-dihydro-1,2,4-triazin-5(2H)-one (AMTTO) with 2-hydroxybenzaldehyde led to the synthesis of corresponding Schiff base ligands [(Z)-4-((2-hydroxybenzylidene)amino)-3-methyl-1H-1,2,4-triazole-5(4H)-thione ( L1 ) and (Z)-4-((2-hydroxybenzylidene)amino)-6-methyl-3-thioxo-3,4-dihydro-1,2,4-triazin-5(2H)-one ( L2 )]. Treatment of synthesized Schiff base ligands with CuCl provided the complexes [Cu(L1)3Cl] ( 1 ) and [Cu(L2)2Cl] ( 2 ). Synthesized complexes were characterized by elemental analyses, IR spectroscopy and X-ray diffraction studies. Complex 1 consists of a metal ion coordinated with one chloride ion and three Schiff base ligands via sulfur atoms in a distorted tetrahedral environment, whereas 2 consists of a metal ion coordinated with one chloride ion and two sulfur atoms from two different Schiff base ligands in a trigonal planar arrangement. Crystal data for 1 at –153 °C revealed an orthorhombic space group Fdd2, a = 34.8088(7), b = 33.8156(8), c = 11.6142(2) Å, Z = 16, R1 = 0.0357; for 2 at –178 °C the symmetry was triclinic, space group P1 , a = 7.27520(10), b = 15.4620(2), c = 23.7985(4) Å, α = 72.1964(13), β = 86.5208(12), γ = 89.8597(11)°, Z = 4, R1 = 0.0359. 相似文献
17.
The reactions of bis[bis(trimethylsilyl)methyl]-germylene ( 1 ) and the corresponding stannylene ( 2 ) with di-tert-butyldiazidosilane gave N-(azidosilyl)germanimine ( 4 ) and the stannanimine ( 5 ) in quantitative yields. The structures have been confirmed by single-crystal X-ray diffraction. Crystal data for 4 : space group P1 , Z = 2, a = 9.236 (1), b = 12.066 (1), c = 17.068 (1) Å, α = 98.45 (1), β = 90.43, γ = 110.27 (1)°. V = 1761.3 Å3, R = 0.051, and Rw = 0.069 based on 4218 reflections with |Fo2| ⩾ 3σ|Fo2|. For 5 : space group P1 , Z = 2, a = 9.183 (1), b = 12.193 (1), c = 17.292 (1) Å, α = 98.74 (1), β = 90.21, γ = 109.96 (1)°, V = 1795.5 Å3, R = 0.040, and Rw = 0.051 based on 4795 reflections. The similar reactions of 1 and 2 with 1,3-diazidohexamethyltrisilane ( 16 ) provided azatrisilacyclobutanes quantitatively. 相似文献
18.
Kurt Klepp 《Monatshefte für Chemie / Chemical Monthly》1980,111(6):1433-1436
TlAgS, TlAgSe and TlAgTe crystallize with the orderedanti-PbCl2-structure type, space group Pnma,Z=4. The lattice constants are: TlAgS:a=722.8(3).b=446.6(1),c=833.1(2)pm. TlAgSe:a=747.56(3),b=463.75(2),c=869.0(1) pm. TlAgTe:a=775.9(1),b=486.8(1),c=877.3(2) pm. The crystal structure of TlAgSe was refined from single crystal diffractometer data to a conventionalR-factor of 0.045. The relationship with the BaCu2S2-structure type is discussed.On leave from Institute of Inorganic Chemistry, University of Vienna A-1090, Wien, Austria 相似文献
19.
NiCl2 · 6 H2O readily reacts with PPh2NHPh in the presence of zinc dust to yield the homoleptic nickel(0) tetrakis‐phosphine complex [Ni(PPh2NHPh)4] ( 1 ). 1 crystallises triclinic P1 (no. 2), with a = 14.656(1), b = 17.124(2), c = 17.424(1) Å, α = 95.998(1), β = 111.845(1), γ = 111.402(1)°, V = 3630.04(5) Å3, Z = 2, R values [I > 2σ(I)]: R1 = 0.0554, all data: wR2 = 0.1720. The nickel atom is coordinated in a distorted tetrahedral fashion by four phosphorus atoms, resembling a compressed tetrahedron along one of the non‐crystallographic S4 axes. 相似文献
20.
Crystal and molecular structures of the planar neutral ligand, C26H16N8, and the four isomorphous five-coordinated metal complexes, [M(C26H16N8)(H2O)], M = Mn(II), Co(II), Cu(II), Zn(II), have been determined from three-dimensional X-ray diffraction data. The free ligand hpH2, C26H16N8, belongs to the P 21/c space group with Z=2, a=4.142(3), b=23.736(6), c=10.338(3) Ä, β=94.66(6)°. The metal complexes monohydrate Mhp-H2O all belong to the orthorhombic Pcab space group with Z=8. The dimensions are roughly 8.8×19.3×23.7 Å3. In each structure, the macrocyclic ligand has an almost planar conformation which differs from the saddle shaped ligand hydrate (hpH2·H2O) and the nickel complex [Nihp]5. The distances from the center of the macrocyclic ring to the nitrogen atom of the free ligand are 1.907(6) and 2.245(6)Å. The coordination geometry in these four complexes is square pyramidal with a water molecule as an axial ligand. The bond distances of M(II)-O(H2O), M(II)-N1 (imine), M(II)-N3 (pyridine) are: 2.19(1), 2.00(2), 2.27(2)Å respectively for the manganese complex; 2.08(1), 1.97(1), 2.23(1)Å for the cobalt complex; 2.33(1), 1.92(3), 2.18(1)Å for the copper complex; 2.110(5), 1.964(6), 2.252(6)Å for the zinc complex. The variation of metal-ligand distances can be correlated to the metal d orbital occupancy. A comparison with similar ligands will be presented. 相似文献