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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  

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   

4.

Abstract  

Two new alkali thorium phosphate materials, K3Th2(PO4)3F2 and RbThPO4F2, were isolated by hydrothermal synthesis at 575 °C. These structures were characterized by single crystal X-ray diffraction using a full-matrix least squares method. The K3Th2(PO4)3F2 compound crystallizes in C2/c (No. 15) with a = 15.8179(15) ?, b = 9.8172(8) ?, c = 9.6472(9) ?, β = 121.132(7)°, Z = 4 and R 1 = 0.0329. This structure contains two large open channels possibly suitable for incorporating radioactive cesium isotopes for waste storage. The RbThPO4F2 structure forms in the P2 1 /m (No. 11) space group with a = 6.719(4) ?, b = 6.002(3) ?, c = 7.431(5) ?, β = 113.925(19)°, Z = 2 and R 1 = 0.0359. Unique to this material is a chain of edge sharing thorium with square antiprism coordination environments where fluorine occupies both sites along the edge. Both structures also represent the first occurrences of a fluorinated alkali thorium phosphate material.  相似文献   

5.

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   

6.
Three heteroacidoligand uranyl complexes M 4[(UO2)2C2O4(SO4)2(NCS)2] (M = K+ (I), Rb+ (II)) and K4[(UO2)2C2O4(SeO4)2(NCS)2] (III) have been synthesized and their crystal structure has been determined by X-ray diffraction analysis. The compounds I–III are isostructural and crystallized in the monoclinic system, sp. gr. P21/c, Z = 2, a = 11.5548(3) ?, b = 7.0847(1) ?, c = 13.5172(3) ?, β = 93.130(1)°, V = 1104.90(4), R = 0.015 (I); a = 11.5854(9) ?, b = 7.3841(6) ?, c = 13.9072(9) ?, β = 95.754(3)°, V = 1183.74(15), R = 0.0235 (II); a = 11.6715(3) ?, b = 7.1418(2) ?, c = 13.8546(1) ?, β = 93.539(1)°, V = 1152.66(5), R = 0.0126 (III). Basic structural units of these crystals are [(UO2)2C2O4(XO4)2(NCS)2]4− chains, which belong to the crystallochemical group A 2 K 02 B 22 M 21 (A = UO22+, K 02 = C2O2−4, B 2 = SO42− or SeO42−, M 1 = NCS) of uranyl complexes. Uranium-containing chains are connected into a 3D framework via a system of electrostatic interactions with potassium or rubidium cations from outer spheres. Original Russian Text ? I.V. Medrish, E.V. Peresypkina, A.V. Virovets, L.B. Serezhkina, 2008, published in Kristallografiya, 2008, Vol. 53, No. 3, pp. 495–498.  相似文献   

7.
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   

8.

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   

9.

Abstract  

The synthesis and crystal structure of the title organic charge-transfer salt (TTF)[Pt(mnt)2] (TTF = tetrathiafulvalene; mnt = cis-3,4-dimercapto-2-butenedinitrile) is described. The salt crystallizes in the P-1 space group with a = 7.9174(13) ?, b = 11.1583(18) ?, c = 11.2600(18) ?, α = 107.490(3)°, β = 91.631(3)°, and γ = 94.980(3)°. The stoichiometry between TTF and [Pt(mnt)2] is 1:1. The structure of (TTF)[Pt(mnt)2] consists of alternating stacks of dimerised TTF+ cations and dimerised [Pt(mnt)2] anions, linked together by many kinds of short contacts and hydrogen bonds. Both the dimerised TTF+ cations and dimerised [Pt(mnt)2] anions are arranged in a parallel face-to-face mode.  相似文献   

10.
The absolute configuration at the chiral sulfurs centers of (−)-(S S , 1R, 2S, 5R)-menthyl-p-tolylsulfinate (1) and (S S )-[(p-tolyl)sulfinyl]ferrocene (2) were determined by single crystal X-ray diffraction with anomalous dispersion effects and the corresponding calculation of Flack’s absolute structure parameters. Both compounds crystallize in the monoclinic crystal system in space group P21 (no. 4); chiral sulfinate ester 1: a = 8.2868(6), b = 6.1399(3), c = 16.366(2) ?, β = 91.816(6)°, V = 832.3(2) ?3, Z = 2 and absolute structure parameter −0.03(7); chiral ferrocenyl sulfoxide 2: a = 5.8371(3), b = 15.390(2), c = 16.143(2) ?, β = 97.748(6)°, V = 1436.9(3) ?3, Z = 4 and absolute structure parameter +0.01(1). The trigonal pyramidal geometry at the chiral sulfur atom of 2 is close to expected values while the one of 1 is slightly distorted. With direct determination of the absolute configuration at the chiral sulfur centers an important gap concerning the widely used precursors 1 and 2 for the syntheses of chiral sulfoxides and 1,2-disubstituted planar chiral ferrocenyl ligands is now closed. The latter substance class is playing a key role in enantioselective catalysis.  相似文献   

11.

Abstract  

Two copper coordination polymers [CuI(bipy)1/2Cl] n (1) and {[(CuII)4(phen)4(SSA)2Cl2] (H2O)2(DMF)2} n (2)(bipy = 4,4′-bipyridine, phen = 1,10-phenanthroline, H3SSA = 5-sulfosalicylic acid, DMF = N,N-dimethylformamide) have been prepared and characterized by X-ray diffraction, elemental analysis, IR spectrum and 2 was also studied by cyclic voltammetric method. X-ray analysis indicates that both of them have Cu2Cl2 bridging subunit. Complex 1 is a two dimensional network structure. While 2 shows a one dimensional zigzag chain. Electrochemistry studies reveal that complex 2 undergo a quasi reversible one-electron metal-centered redox process at E 1/2 = +0.062 V.  相似文献   

12.

Abstract  

The metallacrown complex MnII(OAc)2[15-MCMnIII (N)shi-5](Im)3(EtOH)3 has been synthesized and characterized by single-crystal X-ray diffraction and infrared spectroscopy. The compound crystallizes in the monoclinic space group P21/c with a = 24.3326(15) ?, b = 24.0354(15) ?, c = 27.0531(17) ?, α = 90.00°, β = 100.3883(11)°, γ = 90.00°, V = 15562.5(17) ?3, Z = 4, and Z′ = 2. Four of the five manganese(III) ions of the metallacrown ring adopt a distorted octahedral coordination geometry, and the fifth manganese(III) ion is five coordinate and exhibits a distorted square pyramidal environment. The configuration of the manganese(III) ions about the ring follows a pattern of ΔΛΔPP, with P representing planar. In addition, the imidazole units are bound to three separate ring manganese(III) ions, and the imidazole units are directed to the outside of the molecule. A manganese(II) ion is encapsulated in the central core of the molecule, and the central ion is seven coordinate with a face-capped trigonal prismatic geometry.  相似文献   

13.
Single crystals of the compound (NH4)3[UO2(CH3COO)3]2[UO2(CH3COO)(NCS)2(H2O)] (I) are synthesized, and their structure is investigated using X-ray diffraction. Compound I crystallizes in the monoclinic system with the unit cell parameters a = 18.3414(6) ?, b = 16.3858(7) ?, c = 12.4183(5) ?, β = 92.992(1)°, space group C2/c, Z = 4, V = 3727.1(3) ?3, and R = 0.0253. The uranium-containing structural units of crystals I are mononuclear complexes of two types with an island structure, i.e., the [UO2(CH3COO)3] anionic complexes belonging to the crystal-chemical group (AB 301 = UO22+, B 01 = CH3COO) of the uranyl complexes and the [UO2(CH3COO)(NCS)2(H2O)] anionic complexes belonging to the crystal-chemical group AB 01M31 (A = UO22+, B 01 = CH3COO, M 1 = NCS or H2O).  相似文献   

14.

Abstract  

A new acetyl phosphorylamidate P(O)[NHC(O)C6H4(4-NO2)][N(CH(CH3)2)(CH2C6H5)]2 has been synthesized and characterized by elemental analysis, 1H, 13C and 31P NMR, IR and single crystal X-ray diffraction. Single crystal X-ray analysis shows that it belongs to triclinic system, space group P[`1] P\bar{1} , with a = 10.5868(16) Å, b = 11.8058(18) Å, c = 12.4364(19) Å, α = 65.410(3)°, β = 67.492(4)°, γ = 85.879(3)°, V = 1,298.6(3) Å3, and Z = 2. The intermolecular PO···HN hydrogen bond makes H-bonded dimer of molecule with Ci symmetry. In the crystal network, the dimers are aggregated in the chain arrays through π-stacking between p-NO2–C6H4–C(O)–NH– moieties. Moreover, weak C–H···O and C–H···π interactions exist in the crystal network.  相似文献   

15.
The synthesis and X-ray diffraction analysis of K2(H5O2)[UO2(C2O4)2(HSeO3)] single crystals have been performed. This compound crystallizes in the triclinic system with the unit-cell parameters a = 6.7665(4) ?, b = 8.8850(4) ?, c = 12.3147(7) ?, α = 94.73°, β = 90.16°, γ = 92.11°, sp. gr. P[`1]P\bar 1, Z = 2, and R = 0.019. The basic structural units are island [UO2(C2O4)2(HSeO3)]3− groups, which belong to the AB 201 M 1 crystallochemical group of uranyl complexes (A = UO22+, B 01 = C2O42−, and M 1 = HSeO3). Uraniumcontaining complexes are linked through K+ and H5O2+ ions and via a system of hydrogen bonds with the participation of oxonium hydrogen atoms in this structure.  相似文献   

16.

Abstract  

The structures of four spirobisnaphthalenes based monomers 1, 2, 3a and 3b are reported. Each compound represents a methoxylated precursor which after deprotection led to the formation of a monomer successfully used for the synthesis of Polymers of intrinsic microporosity. The spiro-centre represents the site of contortion that, since its rigidity, leads to inefficient packing in the solid state inducing microporosity in the final polymer. Compound 1 crystallized in the monoclinic P2/c space group with unit cell parameters a = 8.1659(19) ?, b = 7.5298(18) ?, c = 19.130(5) ?, β = 97.935(4)°, V = 1165.0(5) ?3, Z = 2, D = 1.210 Mg m−3. Compound 2 crystallized in the monoclinic P21/n space group with unit cell parameters a = 12.6940(9) ?, b = 7.7267(6) ?, c = 19.9754(15) ?, β = 97.220(1)°, V = 1943.7(3) ?3, Z = 4, D = 1.355 Mg m−3. Compound 3a crystallized in the monoclinic P21/c space group with unit cell parameters a = 16.8137(14) ?, b = 10.5577(9) ?, c = 31.344(3) ?, β = 103.618(1)°, V = 5407.5(8) ?3, Z = 8, D = 1.308 Mg m−3. Compound 3b crystallized in the monoclinic Pc space group with unit cell parameters a = 15.594 ?, b = 12.564 ?, c = 18.339 ?, β = 90.224(1)°, V = 3593.0 ?3, Z = 4, D = 1.236 Mg m−3.  相似文献   

17.

Abstract  

Two new glycoluril derivatives, namely 6-phenyl-1,4-dioxo-2,2a,3,4,6,7-hexahydro-1H,5H-2,3,4a,6,7a-pentaazacyclopenta[cd]indene-2a,7b-dicarboxylate (1), and diethyl 6-(2,4-dichorophenyl)-1,4-dioxo-2,2a,3,4,6,7-hexahydro-1H,5H-2,3,4a,6,7a-pentaazacyclopenta[cd]indene-2a,7b-dicarboxylate (2) have been synthesized and structurally determined by X-ray diffraction analysis. Compound 1 is, monoclinic, space group C2/c, with a = 20.0784(7), b = 9.0316(3), c = 23.0980(8) ?, β = 98.3930(10), V = 4143.7(2) ?3, with Z = 8 for d calc = 1.338 Mg/m3. The analog 2 is, Triclinic, space group P-1, with a = 8.9353(18), b = 10.466(2), c = 14.679(3) ?, β = 73.60(3), V = 1268.1(4) ?3, with Z = 2 for d calc = 1.533 Mg/m3. X-ray analysis reveals that both glycoluril derivatives bearing two free syn-urea NH groups and two ureidyl C=O, assemble the same one-dimensional chains in the solid-state running parallel to the [110], [110] and [010] directions via N–H···O hydrogen bonds.  相似文献   

18.

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   

19.
Single crystals of PbUO2(CH3COO)4(H2O)3 have been investigated by X-ray diffraction (R = 0.029 for 3175 reflections). The structure of this compound is formed by [Pb(CH3COO)(H2O)3]+ chains, which are oriented along the [100] axis and limited by one-core complexes [UO2(CH3COO)3]. The coordination numbers of the Pb(II) and U(VI) atoms are 8, and the coordination polyhedron of uranium is a hexagonal bipyramid whose vertices contain oxygen atoms of three bidentate cyclic acetate groups and the uranyl group. Taking into account the different crystallographic roles of acetate ions, the crystal-chemical formula of [PbUO2(CH3COO)4(H2O)3] chains can be written as AAB 21 B 11(B 01)2 M 31, where A = Pb; A′ = UO22+; M 1 = H2O; and B 21, B 11, and B 01 are CH3COO groups.  相似文献   

20.

Abstract  

One new complex, 2,4-Diiodo-6-[(2-morpholin-4-yl-ethylimino)- methyl]- phenolato-zinc(II) has been designed and synthesized. The structure was determined by UV, IR and single X-ray crystallography study. The title complex C26H30O4N4I4Zn crystallizes in the triclinic space group P − 1 with the cell parameters a = 9.938(2) ?, b = 11.937(2) ?, c = 14.527(3) ?, α = 87.14(3)°, β = 79.03(3)°, γ = 76.20(3)°, V = 1565.1(5) ?3 and Z = 2. The central zinc(II) is four coordinate and bonds to two nitrogen atoms and two oxygen atoms from two 3,5-diiodosalicylaldehyde-2- morpholinoethylamine Schiff bases. The complex is linked into a column by weak intermolecular interactions.  相似文献   

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