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1.

Abstract  

Erbium (III) coordination compound with the formula [Er(IN)3(H2O)2]n 1 (HIN = isonicotinic acid) was synthesized by mixing Er2O3 with isonicotinic acid under hydrothermal condition. The structure of the title compound was determined by single crystal X-ray diffraction analysis, which reveals that the 1-D chain-like structure is formed by the erbium polyhedra through the carboxyl groups of IN. It crystallizes in the monoclinic system, possesses space group C2/c, with lattice parameters: a = 20.229(10) ?, b = 11.594(6) ?, c = 9.871(5) ?, α = γ=90°, β = 115.509(6)°, V = 2089.3(18) ?3, and D calc = 1.811 mg/cm3 for Z = 4, F(000) = 1108, GOF = 1.109, R1 = 0.0675. Compound 1 has been characterized by IR absorption spectroscopy, ultraviolet excitation and emission spectrum.  相似文献   

2.

Abstract  

Two neodymium thiostannates [Nd(dien)3]2[(Sn2S6)Cl2] (1) and [Nd(dien)3]2[(Sn2S6)(SH)2] (2) (dien = diethylenetriamine) were synthesized by the reaction of tin and sulfur in the presence of NdCl3 and Nd2O3, respectively under solvothermal conditions. Compounds 1 and 2 crystallize in monoclinic space group P21/n. Crystallographic data for 1: a = 11.6722(16), b = 15.119(2), c = 14.1566(19) ?, β = 96.213(3)°, V = 2483.6(6) ?3, Z = 4. For 2: a = 11.7190(14), b = 15.2168(19), c = 14.2209(18) ?, β = 95.775(4)°, V = 2523.1(5) ?3, Z = 4. The nine-coordinate [Nd(trien)3]3+ complex cation formed in situ acts as the counter ion to the [Sn2S6]4− anion. The [Nd(dien)3]3+, [Sn2S6]4− and Cl (or SH) ions form a 3-dimensional network structure through the N–H···S and N–H···Cl hydrogen bonds.  相似文献   

3.
Abstract  The crystal structures for two of the ligands C6H5CH2SOCH2CONHCH2C6H5 (1) and C6H5SOCH2CON(iC3H7)2 (2) have been determined by X-ray diffraction. These compounds crystallize in orthorhombic system with space groups and cell parameters, Pca21(no. 29), a = 8.4600(5) ?, b = 5.3534(5) ?, c = 32.136(2) ?, V = 1455.42(15) ?3 and Pna21(no. 33) a = 17.5563(11) ?, b = 5.7902(4) ?, c = 14.2866(9) ?, V = 1452.30(16) ?3, respectively. These molecules are stabilized in solid state by various intra and intermolecular hydrogen bonding interactions to give polymeric structures. The reported IR spectra of these compounds in solid state could be explained on the basis of the observed intermolecular hydrogen bonding interactions. Index Abstract  The title compounds C6H5CH2SOCH2CONHCH2C6H5 (1) and C6H5SOCH2CON(iC3H7)2 (2) were prepared by the oxidation of corresponding sulfides with H2O2/SeO2 in methanol and their structures were determined. The structures show that the SO and CO groups are having “anti” configuration in 1 and “syn” configuration in 2. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.  相似文献   

4.
To explore the characteristics of potential fluorescent probes that could be used to screen prospective HDS catalysts, new 5-thienyl dipyrromethene derivatives have been prepared. 5-(2-thienyl)- (1a), 5-(3-thienyl)- (1b), and 5-(3-(2,5-dibromothienyl))-dipyrromethane (1c), were oxidized with DDQ (2,3-dichloro-5,6-dicyano-1,4-benzoquinone) separately to give the corresponding dipyrrins 2a2c. These were subsequently treated with F3B·OEt2 to afford the respective N,N′-difluoroboryl-5-(thienyl)dipyrrin compounds, 3a3c; the latter two may serve as polymer precursors. Significant fluorescence signal enhancement is achieved with 3a3c over 2a2c. Orange fluorescence is observed for 3a whereas its isomer 3b gives green fluorescence (365 nm). An X-ray diffraction study of 3a was performed (orthorhombic, P212121, a=10.684(10) ?, b=15.208(13) ?, c=7.256(6) ?, V=1179.0(17) ?3, Z=4, R 1=0.0428, wR 2=0.0686) and its geometry was studied by way of DFT (Gaussian 03; B3LYP/6-31G*) to give a HOMO/LUMO energy level difference of 414 nm, and a 2-thienyl group rotational barrier of 6 kcal/mol, compared to that of ∼12 kcal/mol for the phenyl derivative. Theoretical modeling of 2a demonstrated that the [N–H⋯N] interaction is favored by ca. 10 kcal/mol, whereas [N–H⋯S] bonding is sterically unattainable.  相似文献   

5.

Abstract  

N 6-benzyladeninium nitrate, (1), C12H12N5 + NO3 crystallizes in P2 1/c, with a = 15.0035(13), b = 5.3788(5), c = 16.8954(13) ?, β = 107.331(6)°, Z = 4 and N 6-benzyladeninium 3-hydroxy picolinate, (2), C12H12N5 + C6H4NO3 , crystallizes in P1, with a = 8.3017(4), b = 14.6170(7), c = 14.7909 (8) ?, α = 78.801 (4), β = 81.979 (4),γ = 88.849 (4)°, Z = 4. In both the salts, the cation exists as N(7)H tautomer with protonation at the N3 atom. The dihedral angle of 76.64 (16)° for (1), 67.91(12)° for (cation A) and 68.27 (13)° for (cation B) in (2), between the adenine plane and phenyl ring plane, the distal orientation of the N6 substituent with respect to the imidazole ring and the free N1 position, make these benzyladeninium cations meet all the requirements necessary for cytokinin activity. The crystal structures are stabilized by N–H···N, N–H···O, C–H···O hydrogen bonds and C–H···π stacking interaction between symmetry related benzyladenine molecule.  相似文献   

6.

Abstract  

The title compound is monomeric with a Zn(II) hexacoordinated center. The coordination sphere is formed by four nitrogens from two phenanthroline molecules, one oxygen from a monodentate peroxodisulfate ion, and one oxygen from a water molecule. A non-coordinated water molecule completes the formula with an important role in the stabilization of the structure through the formation of two OHW–H···Opds bridges (acting as a donor) and one OCW–H···OHW bridge where it is an acceptor group (HW: hydration water; pds: peroxodisulfato; CW: coordinated water). The compound is triclinic, space group P-1 with a = 8.763 (3) ?, b = 9.068 (3) ?, c = 17.531 (6) ?, α = 96.48 (2)°, β = 103.94 (3)°, γ = 104.57 (3)°, V = 1286.0 (7) ?3 and Z = 2. The structure was solved by direct methods with a conventional R (on F) = 0.050 for 4534 reflections with Fo > 4σ(Fo). The compound is isomorphous with the Cd analogue (in Harvey et al. Aust J Chem 54:307, 2001). An eventual dependence of conformation and coordination mode of the peroxodisulfate anion on the ancillary organic ligand taking part in the coordination compounds analyzed is discussed.  相似文献   

7.

Abstract  

A pair of copper(II) complexes, [CuL1(ONO2)(OH2)] 1 and [CuBrL2N3] 2, where L1 is 5-methoxy-2-[(2-morpholin-4-ylethylimino)methyl]phenolate, and L2 is (2-morpholin-4-ylethyl)-(1-pyridin-2-ylethylidene)amine, have been synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic space group P21/c, with a = 10.496(2), b = 19.113(3), c = 8.586(2) ?, β = 105.186(10)°. Complex 2 crystallizes in the monoclinic space group C2/c, with a = 16.606(3), b = 7.357(2), c = 26.043(5) ?, β = 94.996(2)°. The Cu atom in each complex is five-coordinate in a square pyramidal geometry.  相似文献   

8.

Abstract  

A cadmium(II) coordination polymer [Cd2(2-mBIM)2Cl2(C4H4O4)(H2O)2(H2O)] n (1) (wherein 2-mBIM = bis(2-methylimidazo-1-yl) methane, C4H4O4 = succinate anion) has been synthesized and characterized by X-ray diffraction. Complex 1 crystallizes in the monoclinic space group C2/c with a = 23.5265(15) ?, b = 7.3558(5) ?, c = 17.4771(11) ?, β = 90.3560(10)°, V = 3024.5(3) ?3, Z = 4. Each Cd(II) atom is octahedrally coordinated and connected with two adjacent Cd(II) atoms by two individual 2-mBIM ligands in a trans-configuration to form one-dimensional (1D) helical structure. Such 1D helical chain structures were connected to each other via the succinate anion ligands and result in the formation of a two-dimensional (2D) framework. Meanwhile, an overall three-dimensional (3D) supramolecular network was formed via the weak hydrogen bond interactions between metal-coordination and free water molecules.  相似文献   

9.
The tetrabutylammonium salt of mononiobotungstate [(n-C4H9)4N]3NbW5O19 (1) and the tetrabutylammonium salt of monovanadotungstate [(n-C4H9)4N]3VW5O19 (2) are isotypes; both crystallize in the monoclinic system, space group C2/c (N° 15) with Z=8. The cell parameters for 1 are a=30.4038(8) ?, b=18.5948(8) ?, c=27.3330(3) ?, β=112.4555(6)°, V=14281.1(7) ?3 and the final reliability factors are R=0.043 and R w=0.047 for 5801 reflections. The cell parameters for 2 are a=30.096(8) ?, b=18.373(3) ?, c= 27.201(6) ?, β=112.402(14)°, V=13906(5) ?3 and the final reliability factors are R=0.048 and R w=0.054 for 6122 reflections. Both anions, [NbW5O19] 3− and [VW5O19] 3− exhibit the Lindqvist structure of the parent hexatungstate anion. The six metal positions are disordered and for each metal site the occupation factor is close to 1/6 M (M=Nb, V) and 5/6 W. Furthermore the two compounds were characterized by IR in the solid state, and 183W solution NMR. The 183W spectrum of [NbW5O19] 3− presents two resonances with relative intensities 4:1 in agreement with the C4v symmetry of the anion.  相似文献   

10.

Abstract  

Treatment of TaCl(NMe2)4 with ZnMe2 in pentane furnishes a mixture of TaCl(Me)(NMe2)3, TaMe(NMe2)4, and Ta(NMe2)5 as the principal reaction products based on 1H NMR spectroscopy. Depending upon the work-up conditions employed, the compounds TaCl(Me)(NMe2)3 and ZnCl2(NHMe2)2 have been isolated and their molecular structures established by X-ray crystallography. TaCl(Me)(NMe2)3 crystallizes in the orthorhombic space group Pna21, a = 13.644(4) ?, b = 12.934(4) ?, c = 6.992(2) ?, V = 1233.9(7) ?3, Z = 4, and d calc = 1.958 Mg/m3; R = 0.0316 and wR 2 = 0.0707 for 2630 reflections with I > 2σ(I). The molecular structure of TaCl(Me)(NMe2)3 consists of a trigonal bipyramidal core and contains axial and equatorial chlorine and methyl groups, respectively. ZnCl2(NHMe2)2 crystallizes in the orthorhombic space group P212121, a = 5.759(1) ?, b = 10.810(2) ?, c = 15.174(3) ?, V = 944.1(3) ?3, Z = 4, d calc = 1.593 Mg/m3; R = 0.0213 and wR 2 = 0.0494 for 1872 reflections with I > 2σ(I). ZnCl2(NHMe2)2 exhibits a tetrahedral motif and represents the first reported four-coordinate zinc(II) compound containing acyclic monodentate secondary amine groups. The reaction between TaCl(NMe2)4 and MeMgCl afforded a mixture of tantalum products, of which TaCl(Me)(NMe2)3 and Ta(NMe2)5 were found as the major products by 1H NMR spectroscopy.  相似文献   

11.
The crystal structure of 5-methyl-acetophenonethiosemicarbazone monohydrate,A, and salicylaldehyde-2-methylthiosemicarbazone monohydrate,B, were determined using single crystal X-ray diffraction.A crystallizes in the monoclinic space groupC2/c, with lattice parametersa=14.161(2),b=15.753(1) ?,c=11.084(1) ?, β=112.59(1)° andZ=4, yielding a calculated density ofD calc=1.352 mg/m3.B crystallizes in the triclinic space groupP1, witha=7.233(2) ?,b=7.371(2) ?,c=11.841(2) ?, α=82.77(2)°, β=78.33(2)°, γ=63.06(2)° andD calc=1.371 mg/m3 forZ=2,. In bothA andB the immine nitrogen and the sulfur atom areanti with respect to N2-C8. WhileA presents the usual intramolecular six membered hydrogen bond ring,B has instead an intermolecular hydrogen bond between the hydroxy moiety of the salicyladehyde and a water molecule. AM1 calculations agree with the experimental conformations observed in both compounds. Contribution No. 1619 of the Instituto de Química, UNAM.  相似文献   

12.
13.

Abstract  

The structures of two hydrated proton-transfer compounds of 4-piperidinecarboxamide (isonipecotamide) with the isomeric heteroaromatic carboxylic acids indole-2-carboxylic acid and indole-3-carboxylic acid, namely 4-carbamoylpiperidinium indole-2-carboxylate dihydrate (1) and 4-carbamoylpiperidinium indole-3-carboxylate hemihydrate (2) have been determined at 200 K. Crystals of both 1 and 2 are monoclinic, space groups P21/c and P2/c, respectively with Z = 4 in cells having dimensions a = 10.6811(4), b = 12.2017(4), c = 12.5456(5) ?, β = 96.000(4)° (1) and a = 15.5140(4), b = 10.2908(3), c = 9.7047(3) ?, β = 97.060(3)° (2). Hydrogen-bonding in 1 involves a primary cyclic interaction involving complementary cation amide N–H···O(carboxyl) anion and anion hetero N–H···O(amide) cation hydrogen bonds [graph set R22(9)]. Secondary associations involving also the water molecules of solvation give a two-dimensional network structure which includes weak water O–H···π interactions. In the three-dimensional hydrogen-bonded structure of 2, there are classic centrosymmetric cyclic head-to-head hydrogen-bonded amide–amide interactions [graph set R22(8)] as well as lateral cyclic amide-O linked amide–amide extensions [graph set R42(8)]. The anions and the water molecule, which lies on a twofold rotation axis, are involved in secondary extensions.  相似文献   

14.

Abstract  

N-methyl-N-(1-phenylvinyl)benzamide (I) has empirical formula C16H15NO, crystallizes in the monoclinic space group, P21/n, with unit cell parameters a = 8.9101(2) ?, b = 15.1416(4) ?, c = 9.7737(2) ?, α = 90°, β = 109.3320(10)°, γ = 90°, Z = 4. Interestingly, the Compound (I) undergoes photocyclization upon irradiation of light to give two cyclic lactams (A and B) below 3100 ?. Compound (I) can be cyclized at either of two equivalent ortho positions. The mechanism for formation of lactam A may involve electrocyclic ring closure reaction upon irradiation of light to give six-membered cyclic zwitterionic intermediate. The ring proton rearranges via [1, 5]-H shift to give isomerized product A. The minor photoproduct B is supposed to be formed via photocyclization process followed by a loss of proton and the tautomerized product undergoes oxidation for the revival of aromaticity.  相似文献   

15.

Abstract  

One salt and two Cu(II) complexes (H2hsm)(ox), 1, [Cu(hsm)(ox)], 2, and [Cu(hsm)(ox)H2O], 3, have been synthesized and X-ray characterized (hsm is histamine and ox2− is the oxalate dianion). Starting from the prochiral tetracoordinated complex 2, pentacoordinated complex 3 crystallizes as a racemic mixture of the enantiomeric Δ and Λ isomers, in space group P21/c. In all cases, the side chain of the hsm group is gauche, allowing the formation of strong hydrogen bonds in the salt 1, and to chelate the metal center in complexes 2 and 3. The combination hsm/ox seems to favor the formation of 2D supramolecular structures (planes or wavy planes), through efficient networks of N–H···O hydrogen bonds. Cell parameters: 1, P21/c, a = 6.260 (2) ?, b = 11.500 (4) ?, c = 12.525 (4) ?, β = 104.047 (17)o; 2, C2/c, a = 10.7966 (13) ?, b = 15.5622 (16) ?, c = 11.3996 (15) ?, β = 106.261 (11)o; 3, P21/c, a = 7.0627 (6) ?, b = 7.1323 (6) ?, c = 20.0296 (19) ?, β = 91.529 (7)o.  相似文献   

16.

Abstract  

The reaction of [Ni(L)]Cl2·2H2O (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane) with pyrazine-2-carboxylic acid (H-pyc) yields mononuclear nickel(II) complex, [Ni(L)(pyc)2]·2H2O (1). This complex has been characterized by X-ray crystallography, electronic absorption and cyclic voltammetry. The crystal structure of 1 exhibits a distorted octahedral geometry with four nitrogen atoms of the macrocycle and two pyrazine-2-carboxylate ligands. It crystallizes in the triclinic system P-1 with a = 9.6643(17), b = 10.116(3), c = 16.99(4) ?, V = 1633(3) ?3, Z = 2. Electronic spectrum of 1 also reveals a high-spin octahedral environment. Cyclic voltammetry of 1 undergoes two waves of a one-electron transfer corresponding to NiII/NiIII and NiII/NiI processes.  相似文献   

17.

Abstract  

The title compound (C5Me5)2U(OtBu)(SePh) (1) was synthesized and characterized by NMR spectroscopy, elemental analysis, and X-ray crystallography. This system represents a unique example of an actinide complex with two different group 16 elements coordinated to the metal center and the first mixed-ligand actinide alkoxide-selenide complex. The complex crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 17.830(7) ?, b = 14.973(6) ?, c = 21.254(8) ?, V = 5674(4) ?3, Z = 8, D calc = 1.727 Mg/m3. The uranium(IV) mixed-ligand alkoxide-selenide complex adopts a pseudo-tetrahedral geometry, with the tert-butoxide and phenylselenide ligands occupying the plane bisecting the metallocene unit. Structural comparisons of the complex (C5Me5)2U(OtBu)(SePh) (1) are made with related selenide and alkoxide uranium(IV) complexes.  相似文献   

18.
Abstract  The cation in the solid state structure of [Fe{HC(3,5-Me2pz)3}2][Fe2OCl6] (pz = pyrazolyl ring) contains an octahedral iron(II) center with an average Fe–N bond distance of 2.17 Å, indicating that the iron(II) is in the high-spin form. While M–N bond distances of this length with κ3-[HC(3,5-Me2pz)3] ligands generally cause tilting of pz to open up the “bite” angle, in this structure the average tilting angle is only 3.1°, a much lower value than observed in earlier structures of this same cation paired with different anions. The crystals are monoclinic, space group P21/n, with a = 11.1671(12) Å, b = 10.8091(11) Å, c = 17.4385(17) Å, α = γ = 90°, β = 95.685(2)°, and Z = 2. Graphical Abstract  The cation in the solid state structure of [Fe{HC(3,5-Me2pz)3}2][Fe2OCl6] (pz = pyrazolyl ring) contains an octahedral iron(II) center in the high-spin form with unusual orientations of the pyrazolyl rings.   相似文献   

19.
Two imidazolidin ruthenium complexes, [RuCl2{[N-(2,4,6-trimethyl-benzyl)-N-(n-butyl)]-imidazolidin-2-ylidene}], 1, and [RuCl2{[N-(2,4,6-trimethyl-benzyl)-N-(2-methoxyethyl)]-imidazolidin-2-ylidene}], 2, have been synthesised and their crystal structures have been determined from single crystal X-ray diffraction data. Compound 1 is monoclinic, of space group C2/c with a = 18.466(4) Å, b = 14.816(3) Å, c = 15.413(3) Å, β = 118.067(2), and V = 3720.9(12) Å3 with Z = 8 for dcalc = 1.536 g/cm3. Compound 2 is monoclinic, of space group P21/c with a = 8.1800(5) Å, b = 14.344(8) Å, c = 14.809(9), β = 91.604(10), and V = 1736.7(18) Å3 with Z = 4 for dcalc = 1.653 g/cm3. In each complex the ligand functions as an arene and carbene, occupying four coordination sites. The two chlorines in each compound complete a distorted octahedron.  相似文献   

20.

Abstract  

Two novel complexes constructed from the sulfonamide Schiff base ligand H 2 L, N-[2-(5-bromo-2-hydroxybenzylideneamino)ethyl]-4-methylbenzene-sulfonamide, [Cu(HL)2] (1) and [CuL(H2O)] (2) are synthesized and characterized via X-ray single-crystal diffraction, elemental analysis, FT-IR and UV–Vis. 1 and 2 both form 1-D supramolecular architectures by π–π stacking interactions. 1 and 2 both crystallize in monoclinic, with space group C2/c and P2/c for 1 and 2, with unit cell parameters a = 27.640(18) ?, b = 7.907(5) ?, c = 17.945(14) ?, β = 118.27(2)°, V = 3454(4) ?3, Z = 4 for 1, and a = 16.758(5) ?, b = 7.272(2) ?, c = 15.080(4) ?, β = 106.334(5)°, V = 1763.6(9) ?3, Z = 4 for 2.  相似文献   

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