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1.
Lijie Han Xiaochang Sun Yalin Zhu Wanli Zhou Qi Chen Yan Xu 《Journal of chemical crystallography》2010,40(7):579-582
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 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3.
Xiaoping Wang Shih-Huang Huang Michael G. Richmond 《Journal of chemical crystallography》2010,40(2):173-178
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4.
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
5.
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6.
Feng Liu Weiping Zhang Shuiyang He Liujie Wang Xiangrong Liu 《Journal of chemical crystallography》2008,38(10):755-760
Abstract A novel binuclear Smarium (III) complex with N-(2-propionic acid)-salicyloyl hydrazone (C10H10N2O4, H3L) was prepared and characterized. The crystal structure of [Sm2(H2L)2(HL)2(H2O)4] (1) was determined by X-ray single crystal diffractometry. 1 crystallizes in the monoclinic systerm, space group P2(1)/c,
with a = 0.10229(2), c = 31.549(7), b = 0.70599(15) nm, and Z = 4. In the structure, Sm(III) is nine-coordinated by carboxyl O and acyl O atoms and imido N atoms
of two ligands (H2L and HL forms) and O atoms from two water molecules. H2L and HL act as tridentate ligands which form two stable five-numbered chelating rings sharing one edge in the keto form for
each ligand, and the carboxyl groups of two ligands were coordinated via bidentated bridging form. The coordination polyhedron
around Sm (III) was described as a monocapped square antiprism. The inter- and intramolecular hydrogen bonds resulted in a
three-dimensional network and provided extra stability for the structure. The complex was researched the interaction with
calf thymus DNA by electronic absorption titration and emission titration. The results show that the complex is bound to calf
thymus DNA mainly by intercalation .The complex also shows good fluorescence property.
Index Abstract The title compound, [Sm2(H2L)2(HL)2(H2O)4] was synthesized by the treatment of N-(2-propionic acid)-salicyloyl hydrazone (C10H10N2O4, H3L) and Sm(NO3) · 4H2O and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that Sm (III) is nine-coordinated
by carboxyl O and acyl O atoms and imido N atoms of two ligands (H2L and HL forms) and O atoms from two water molecules. The carboxyl groups of two ligands were coordinated via bidentated bridging
form. The coordination polyhedron around Sm (III) was described as a monocapped square antiprism. The inter- and intramolecular
hydrogen bonds resulted in a three-dimensional network and provided extra stability for the structure.
相似文献
7.
S. Kannan S. Chantrapromma H. K. Fun S. Robinson Jebas 《Journal of chemical crystallography》2009,39(1):9-12
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.
L. B. Serezhkina E. V. Peresypkina A. V. Virovets M. O. Karasev 《Crystallography Reports》2010,55(1):19-23
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
9.
L. B. Serezhkina A. V. Vologzhanina V. V. Klepov V. N. Serezhkin 《Crystallography Reports》2011,56(1):132-135
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 AA′B
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
10.
《Journal of chemical crystallography》1991,27(7):391-395
[Cd(C5H4O4)(OH2)2] (1), crystallizes in the monoclinic system, space groupP21/n, with lattice parametersa=7.323(2),b=16.028(6),c=7.202(2) Å, β=113.11(1)°, andZ=4. The Cd atom coordinates to seven oxygens in a monocapped trigonal antiprism fashion. The antiprisms share one vertex to
form chains which run approximately parallel to thec axis. The itaconate ligands link the chains to form layers which stack along theb axis. 相似文献
11.
Peter C. Kunz Wilhelm Huber Bernhard Spingler 《Journal of chemical crystallography》2011,41(2):105-110
Abstract
The three title compounds show extensive hydrogen bonding networks in the solid state. The structure of diphenyl-2-isopropylimidazol-4(5)yl phosphane oxide (3) is dominated by N–H⋯OP hydrogen bonds, whereas in bis(2-isopropylimidazol-4(5)-yl)phenyl- (2) and tris(2-isopropylimidazol-4(5)yl)phosphane oxide (1) both, N–H⋯N and N–H⋯OP hydrogen bonds determine the solid-state structures. Compound 1 crystallises in the monoclinic space group Cc with cell parameters a = 19.5447(6) ?, b = 10.45764(16) ?, c = 10.8549(3) ? and β = 121.418(4)°; 2 in the orthorhombic space group Pna21, with a = 11.5997(3) ?, b = 9.5836(2) ?, c = 16.1860(4) ? and 3 in the orthorhombic space group Pca21, with a = 10.8430(2) ?, b = 10.9277(2) ? and c = 27.7088(6) ?. 相似文献12.
Abstract
Assembly of orotic acid (2,6-dioxo-1,2,3,6-tetrahydropyrimidine-4-carboxylic acid, H3dtpc) and Cd(OAc)2·2H2O gave rise to two complexes [Cd2(H2dtpc)2(H2O)6] (I) and [Cd(H2dtpc)(bpy)(H2O)]n (II) (bpy = 2,2′-bipyridine). Complex (I) and (II) have been characterized by X-ray single crystal diffraction, IR, PXRD, TGA and fluorescence spectra. Structural analyses reveal that (I) is a binuclear structure, and complex (II) possesses a one-dimensional infinite zig-zag chain architecture and the chains are further assembled into 2D supramolecular network by strong hydrogen bonding interactions. Crystal data for (I): Monoclinic, space group P2(1)/n, a = 9.3221(19) ?, b = 6.6315(13) ?, c = 15.322(3) ?, β = 102.31(3)°, V = 925.4(3) ?3, Z = 4, R1 = 0.0269, and wR2 = 0.0604; for (II): Monoclinic, space group P2(1)/c, a = 9.9880(2) ?, b = 14.5085(2) ?, c = 11.6957(2) ?, β = 107.976(2)°, V = 1612.10(5) ?3, Z = 4, R1 = 0.0234 and wR2 = 0.0554. 相似文献13.
Xin-hua Lu Jing-jing Liang Jing Zhao Yong Zhang Ding-xian Jia 《Journal of chemical crystallography》2011,41(4):557-562
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14.
Brian Emerich Matthew Smith Matthias Zeller Curtis M. Zaleski 《Journal of chemical crystallography》2010,40(9):769-777
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15.
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16.
Miguel A. Harvey María E. Díaz de Vivar Ricardo Baggio Sergio Baggio 《Journal of chemical crystallography》2011,41(11):1717-1721
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17.
The crystal structures of three Pd(II) compounds with diamine tetracarboxylates in different protonation states are determined,
namely, [Pd(H2
Cdta)] · H2O (I), [Pd(H3
EdtpCl] · 2H2O (II), and (H6
Edtp)[PdCl4] · 4H2O (III) (R
1 = 0.0230, 0.0313, and 0.0277 for 3040, 3377, and 3809 reflections with I > 2σ(I) for I–III, respectively). Crystals I and II are built of neutral complexes [Pd(H2
Cdta)] and [Pd(H3
Edtp)Cl], respectively, and crystallization water molecules. Crystal III consists of [PdCl4]2− anionic complexes, H6
Edtp
2+ cations, and water molecules. In I, one of the protonated acetate groups of the H2
Cdta
2− ligand forms a very weak additional Pd-O bond [2.968(2) Å] over the 2N + 2O coordination square. In II and III, the protonated propionate groups of the H3
Edtp
− ligand and the H6
Edtp
2+ cation are not involved in Pd coordination and the coordination squares consist of the 2N + O + Cl and 4Cl atoms, respectively.
__________
Translated from Kristallografiya, Vol. 48, No. 2, 2003, pp. 278–282.
Original Russian Text Copyright ? 2003 by Polyakova, Poznyak, Sergienko. 相似文献
18.
A new basic Nd3+ nitrate, [Nd6O(OH)8(H2O)14(NO3)6](NO3)2 · 2H2O (I), is isolated in the crystal form and studied. Compound I differs from the basic Ln nitrates containing [Ln
6O(OH)8] clusters in that it involves a larger number of water molecules. The incorporation of additional water molecules is accompanied
by changes in the coordination environment of one of the three crystallographically independent Nd3+ cations. Two cations have coordination polyhedra in the form of a monocapped tetragonal antiprism with a coordination number
of 9, and the third cation has a polyhedron in the form of a bicapped tetragonal antiprism with a coordination number of 10.
Original Russian Text ? I.A. Charushnikova, C. Den Auwer, 2007, published in Kristallografiya, 2007, Vol. 52, No. 2, pp. 248–251. 相似文献
19.
Wei Xiong Yan Su Zhong Zhang Zilu Chen Fupei Liang Lixia Wang 《Journal of chemical crystallography》2011,41(10):1510-1514
Abstract
The reactions of a new compound of N-Carboxyphenylenesulfonyl-S-Carboxymethyl-l-Cysteine (Cs-cmc) with Zn(II) or Co(II) salts in the presence of 4,4′-bipyridine (4,4′-bipy) led to the decomposition of Cs-cmc and produced [Zn(4,4′-bipy)(H2O)4]X2 (X = p-sulfamoylbenzoate) 1 and [Co(4,4′-bipy)(H2O)4]Y·H2O (Y = p-sulfonatobenzoate) 2, in which the decomposition products of Cs-cmc exist as free counter-anions. The single crystal X-ray diffraction analyses revealed that compound 1 crystallizes in monoclinic C2/c space group with a = 18.748(4) ?, b = 11.520(2) ?, c = 12.751(3) ?, β = 90.290(4)°, V = 2753.9(10) ?, Z = 4 and compound 2 crystallizes in orthorhombic Pca21 space group with a = 12.114(3) ?, b = 11.369(2) ?, c = 14.770(3) ?, V = 2034.1(7) ?, Z = 4. It was revealed that 1D chains were constructed from metal ions and 4,4′-bipy in both compounds. The 1D chains interact with the counter-anions by hydrogen bonds, forming 3D supramolecular structures. 相似文献20.
The crystal structure of a new synthetic aluminophosphate {[Rb1.94(H2O,OH)3.84](H2O)0.1}{Al4(OH)4[PO4]3} synthesized under mild hydrothermal conditions (T = 280°C, P = 100 atm) in the Rb2O-Al2O3-P2O5-H2O system is determined using X-ray diffraction (Stoe IPDS diffractometer, λMoK
α, graphite monochromator, 2θmax = 64.33°, R = 0.032 for 312 reflections). The main crystal data are as follows: a = 7.4931(6) ?, space group P
3m, Z = 1, and ρcalcd = 2.76 g/cm3. It is shown that the synthesized compound belongs to the pharmacosiderite structure type with a characteristic mixed open
microporous framework composed of octahedra and tetrahedra. A comparative crystal chemical analysis of related phases is performed,
and the chemical compositions of promising absorbents, i.e., hypothetical compounds potentially possible in the structure
type under consideration, are proposed. It is established that pharmacosiderite and rhodizite are homeotypic to each other.
Original Russian Text ? O.V. Yakubovich, W. Massa, O.V. Dimitrova, 2008, published in Kristallografiya, 2008, Vol. 53, No.
3, pp. 442–449. 相似文献