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1.
One-dimensional Co(dien)2(VO3)3·(H2O) was prepared from the hydrothermal reaction of NH4VO3, Co2O3, diethylenetriamine (dien) and H2O at 130 °C. The compound crystallizes in the monoclinic system, space group P21/c with a=16.1581(6) Å, b=8.7006(3) Å, c=13.9893(4) Å, β=103.1483(11)°, V=1915.13(11) Å3, Z=4, and R1=0.0268 for 3060 observed reflections. Single crystal X-ray diffraction revealed that the structure is composed of infinite one-dimensional chains formed by corner-sharing VO4 tetrahedra with Co(dien)3+ complex cations and crystallization water molecules occupying the interchain positions, which are held together to a three-dimensional network via extensive hydrogen-bonding interactions. The compound, with a new zig-zag conformation of metavanadate chains, is the first example of vanadium oxides incorporating trivalent transition metal coordination groups. Other characterizations by elemental analysis, IR and thermal analysis are also described. 相似文献
2.
Barbara A. Fir Hlne P. A. Mercier Jeremy C. P. Sanders David A. Dixon Gary J. Schrobilgen 《Journal of fluorine chemistry》2001,110(2):89-107
The XeOSeF5+ cation has been synthesized for the first time and characterized in solution by 19F, 77Se and 129Xe NMR spectroscopy and in the solid state by X-ray crystallography and Raman spectroscopy with AsF6− as its counter anion. The X-ray crystal structures of the tellurium analogue and of the Xe(OChF5)2 derivatives have also been determined: [XeOChF5][AsF6] crystallize in tetragonal systems, P4/n, a=6.1356(1) Å, c=13.8232(2) Å, V=520.383(14) Å3, Z=2 and R1=0.0453 at −60°C (Te) and a=6.1195(7) Å, c=13.0315(2) Å, V=488.01(8) Å3, Z=2 and R1=0.0730 at −113°C (Se); Xe(OTeF5)2 crystallizes in a monoclinic system, P21/c, a=10.289(2) Å, b=9.605(2) Å, c=10.478(2) Å, β=106.599(4)°, V=992.3(3) Å3, Z=4 and R1=0.0680 at −127°C; Xe(OSeF5)2 crystallizes in a triclinic system,
, a=8.3859(6) Å, c=12.0355(13) Å, V=732.98(11) Å3, Z=3 and R1=0.0504 at −45°C. The energy minimized geometries and vibrational frequencies of the XeOChF5+ cations and Xe(OChF5)2 were calculated using density functional theory, allowing for definitive assignments of their experimental vibrational spectra. 相似文献
3.
《Journal of Molecular Structure》2003,650(1-3):49-56
Two novel hydrogen maleato (HL) bridged Cu(II) complexes ∞1[Cu(phen)Cl(HL)2/2] 1 and ∞1[Cu(phen)(NO3)(HL)2/2] 2 were obtained from reactions of 1,10-phenanthroline, maleic acid with CuCl2·2H2O and Cu(NO3)2·3H2O, respectively, in CH3OH/H2O (1:1 v/v) at pH=2.0 and the crystal structures were determined by single crystal X-ray diffraction methods. Both complexes crystallize isostructurally in the monoclinic space group P21/n with cell dimensions: 1 a=8.639(2) Å, b=15.614(3) Å, c=11.326(2) Å, β=94.67(3)°, Z=4, Dcalc=1.720 g/cm3 and 2 a=8.544(1) Å, b=15.517(2) Å, c=12.160(1) Å, β=90.84(8)°, Z=4, Dcalc=1.734 g/cm3. In both complexes, the square pyramidally coordinated Cu atoms are bridged by hydrogen maleato ligands into 1D chains with the coordinating phen ligands parallel on one side. Interdigitation of the chelating phen ligands of two neighbouring chains via π–π stacking interactions forms supramolecular double chains, which are then arranged in the crystal structures according to pseudo 1D close packing patterns. Both complexes exhibit similar paramagnetic behavior obeying Curie–Weiss laws χm(T−θ)=0.414 cm3 mol−1 K with the Weiss constants θ=−1.45, −1.0 K for 1 and 2, respectively. 相似文献
4.
Yun Gong Changwen Hu Hui Li Wanlong Pan Xueli Niu Zhifa Pu 《Journal of Molecular Structure》2005,740(1-3):153-158
Two nickel (imidazole) complexes, Ni(im)6Cl2·4H2O (1) and Ni(im)6(NO3)2 (2) (im=imidazole) have been synthesized and characterized by elemental analysis, IR, UV, TG and single crystal X-ray diffraction. 1 crystallizes in the triclinic space group P-1 with a=8.800(6) Å, b=9.081(6) Å, c=10.565(7) Å, =75.058(9)°, β=83.143(8)°, γ=61.722(8)°, V=718.3(8) Å3, Z=1 and R1 (wR2)=0.0469 (0.1497). 2 crystallizes in the trigonal space group R-3 with a=12.370(6) Å, b=12.370(6) Å, c=14.782(14) Å, =90.00°, β=90.00°, γ=120.00°, V=1959(2) Å3, Z=3 and R1 (wR2)=0.0358 (0.0955). 1 and 2 exhibit different supramolecular network due to their different counter anions and different hydrogen bonding connection. In compound 1, [Ni(im)6]2+ cation and counter anions Cl− alternatively array in an ABAB fashion via N–HCl hydrogen bonding. In compound 2, the plane of each NO32− is almost parallel and each NO32− connect three different [Ni(im)6]2+ cations via N–HO hydrogen bonding. 相似文献
5.
A new complex [Cu (C4H7N3) H2O (4,4′-Hbpy)]·SO4·NO3 was synthesized and X-ray characterized. Elemental analysis, X-ray diffraction and infrared spectroscopy of the complex were performed. The crystal system is orthorhombic. Crystal data: Fw=498.98, spacegroup: P212121. Z=4, a=14.952(3), b=20.491(4), c=6.713 Å. V=2056.7(9) Å. λ(Mo-K)=0.71070 Å. μ=12.18 cm−1, Dcalc=1.66 g/cm3, F000=1032.00, R=0.062, Rw=0.087. X-ray analysis illustrated that 4,4′-bpy is mono-protonated and that there are two kinds of anions in one molecule, which give rise to the hydrogen interaction between the molecules in the crystal. Then an extended three-dimensional network is formed along the hydrogen bonds and π–π bonds between the pyridine rings. 相似文献
6.
Yong Li Jing Lu Jiqing Xu Xiaobing Cui Yinghua Sun Qingxin Yang Lingyun Pan 《Journal of Molecular Structure》2004,690(1-3):131-135
Nest-shaped cluster [MoOICu3S3(2,2′-bipy)2] (1) was synthesized by the treatment of (NH4)2MoS4, CuI, (n-Bu)4NI, and 2,2′-bipyridine (2,2′-bipy) through a solid-state reaction. It crystallizes in monoclinic space group P21/n, a=9.591(2) Å, b=14.820(3) Å, c=17.951(4) Å, β=91.98(2)°, V=2549.9(10) Å3, and Z=4. The nest-shaped cluster was obtained for the first time with a neutral skeleton containing 2,2′-bipy ligand. The non-linear optical (NLO) property of [MoOICu3S3(2,2′-bipy)2] in DMF solution was measured by using a Z-scan technique with 15 ns and 532 nm laser pulses. The cluster has large third-order NLO absorption and the third-order NLO refraction, its 2 and n2 values were calculated as 6.2×10−10 and −3.8×10−17 m2 W−1 in a 3.7×10−4 M DMF solution. 相似文献
7.
Da-Ming Du Wen-Ting Hua Ling-Ping Zhou Jian-Wu Wang Xiang-Lin Jin 《Journal of Molecular Structure》2001,560(1-3):23-28
The new host 1,4,11,14-tetramethoxy-dibenzo[b,n]tetraphenylene forms a 1:1 inclusion compound with pyridine, in which a pair of centrosymmetrically-related guest species are enclosed in the cage surrounded by six host molecules. C36H28O4·C5H5N, FW=603.68, triclinic, space group P-1, a=11.796(2), b=16.075(3), c=9.004(2) Å; =98.39(3)°, β=90.01(3)°, γ=108.19(3)°, V=1602.8(5) Å3, Z=2, F(000)=636, Dc=1.251 g/cm3, μ=0.080 mm−1. The final R indices [I>2σ(I)] R1=0.0759, wR2=0.1970 for 5623 MoK observed data. 相似文献
8.
B. Sieklucka W.
asocha L. M. Proniewicz R. Podgajny H. Schenk 《Journal of Molecular Structure》2000,520(1-3):155-163
The bimetallic [Pt(NH3)4]2[W(CN)8][NO3]·2H2O is characterised by single-crystal X-ray diffraction [S.G.P21/m(11), a=8.0418(7), b=19.122(2), c=9.0812(6) Å, Z=2]. All platinum centres have the square-plane D4h geometry with average dimensions Pt(1)–N 2.042(2) and Pt(2)–N 2.037(10) Å. The octacyanotungstate anion has the square-antiprismatic D4d configuration with average dimensions W(1)–C 2.164(13), C–N 1.140(12), W(1)–N 3.303(5) Å. The structure exhibits two different mutual orientations of Pt versus W units resulting in Pt(2)–W(1), W(1)* separations of 4.77(2), 4.55(2)* and Pt(1)–W(1) of 6.331(8) Å. A centrosymmetric structure reveals groups of two distinct columns: the first is formed by intercalated NO3− between parallel [Pt(1)(NH3)4]2+ planes and the second consists of [W(CN)8]3− interlayered by, parallel to square faces of W-antiprisms, [Pt(2)(NH3)4]2+. The structure is stabilised through a three-dimensional hydrogen bond network via nitrogen atoms of cyanide ligands, hydrogen atoms of NH3 ligands, water molecules and oxygen atoms of NO3− counteranions. The vibrational pattern and the range of ν(CN) frequencies attributable to the electronic environment of W(V) and W(IV) are consistent with the ground state Pt(II)↔W(V) charge transfer. 相似文献
9.
Yunlan Su Limin Yang Xianglin Jin Shifu Weng Jinguang Wu 《Journal of Molecular Structure》2002,616(1-3):221-230
The crystal structure of LaCl3·galactitol·6H2O has been determined. It is monoclinic. The space group is P21/n with unit cell dimensions a=10.5091(7), b=12.5366(7), c=14.4420(10) Å, β=90.974(2)°, V=1902.4(2) Å3 and Z=4. Each La3+ ion in the unit cell is coordinated to 10 oxygen atoms, three from O1, O2 and O3 of one alditol, three from O4, O5 and O6 of another alditol and four from water molecules, with La–O distances from 2.5099 to 2.6916 Å. The other two water molecules are hydrogen-bonded. FT-IR spectrum of LaCl3·galactitol·6H2O is apparently different from that of other lanthanide–galactitol complexes. It is consistent with the differences between their crystal structures. Both the IR result and the crystal structure of LaCl3·galactitol·6H2O complex show that it has the different coordination mode compared with other lanthanide complexes. 相似文献
10.
Microdifferential thermal analysis (μ-DTA), X-ray diffraction (XRD) and infrared (IR) spectroscopy were used for the first time to investigate the liquidus and solidus relations in the KPO3–Y(PO3)3 system. The only compound observed within the system was KY(PO3)4 melting incongruently at 1033 K. An eutectic appears at 13.5 mol% Y(PO3)3 at 935 K, the peritectic occurs at 1033 K and the phase transition for potassium polyphosphate KPO3 was observed at 725 K. Three monoclinic allotropic phases of the single crystals were obtained. KY(PO3)4 polyphosphate has the P21 space group with lattice parameters: a=7.183(4) Å, b=8.351(6) Å, c=7.983(3) Å, β=91.75(3)° and Z=2 is isostructural with KNd(PO3)4. The second allotropic form of KY(PO3)4 belongs to the P21/n space group with lattice parameters: a=10.835(3) Å, b=9.003(2) Å, c=10.314(1) Å, β=106.09(7)° and Z=4 and is isostructural with TlNd(PO3)4. The IR absorption spectra of the two forms show a chain polyphosphates structure. The last modification of KYP4O12 crystallizes in the C2/c space group with lattice parameters: a=7.825(3) Å, b=12.537(4) Å, c=10.584(2) Å, β=110.22(7)° and Z=4 is isostructural with RbNdP4O12 and contains cyclic anions. The methods of chemical preparations, the determination of crystallographic data and IR spectra for these compounds are reported. 相似文献
11.
Li-Yun Feng Yong-Hui Wang Chang-Wen Hu Yang-Guang Li En-Bo Wang 《Journal of Molecular Structure》2003,650(1-3):115-122
A novel three-dimensional (3D) mixed-valence iron coordination polymer [Fe2IIIFeIIO2(IN)2(ox)] (IN=isonicotinate, OX=oxalate) (1) has been hydrothermally synthesized by using two different anionic ligands and characterized by elemental analysis, IR spectrum, electron spin resonance (ESR), X-ray photoelectron spectrum (XPS), thermogravimetric analysis (TGA) and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic, space group P2(1)/c with a=5.8774(7) Å, b=18.528(2) Å, c=7.7117(9) Å,
V=817.69(17) Å3, Z=2, and R1=0.0321 (wR2=0.0777). The Fe(II) and Fe(III) centers in 1 both exhibit a distorted octahedral coordination geometry and are bridged by the IN and oxalate groups into a covalently bonded 3D metal–organic network. TGA showed that the 3D network possesses a good stability up to 291 °C. 相似文献
12.
Polarized absorption spectra of Ba(MnO4)2·3H2O/Ba(ClO4)2·3H2O mixed single crystals are reported at 4.2°K. Previous 1T2 → 1A1 assignments for the 5200 Å and 3000 Å absorption bands of MnO4− are substantiated; further support is provided for the 1T1 → 1A1 assignment of the 3600 Å absorption band of MnO4−. The site-splitting of the 5200 Å 1T2 state is E(1E)−E(1A) ≈ −150 cm−1; that of the 3000 Å 1T2 state is E(1E)−E(1A) ≈ 300 cm−1. A significant e vibronic intensity component is observed in the 5200 Å 1T2 state. 相似文献
13.
Two polymeric mercury(II) halide adducts of an olefinic double betaine, cis-(p-Me2NC5H4N+)2C2(COO−)2 (L), have been prepared and characterized by X-ray crystallography. [{Hg2L2Cl4·6HgCl2}n] (1) crystallizes in the monoclinic space group C2/c with Z = 4, and [{Hg2L2Br4·HgBr2}n] (2) in the triclinic space group P
with Z = 1. Complexes 1 and 2 are structurally similar, being composed of centrosymmetric fourteen-membered rings and nearly linear HgX2 (X = Cl, Br) moieties that are further inter-linked by weak HgX [HgCl = 2.930–3.136(9) Å, HgBr = 3.057–3.310(6) Å] and HgO [2.64, 2.75(3) Å] bonds to generate a two-dimensional polymeric network. 相似文献
14.
The interaction between Mo2(O2CCH3)4, Me3SiI and I2 in THF resulted in oxygen abstraction from the solvent and formation of [Mo2(μ-O)(μ-I)(μ-O2CCH3) I2(THF)4]+[MoOI4(THF)]− and I---(CH2)4---I. The molybdenum complex has been characterized by X-ray diffractometry. Crystal data: triclinic, space group P
, a = 13.827(3) Å; b = 15.803(7) Å; c = 9.950(3) Å; = 93.34(4)°; β = 102.40(2)°; γ = 90.09(2)°; V = 2120(2) Å3; Z = 2; dcalc = 2.559 g cm−3; R = 0.0476 (Rw = 0.0613) for 370 parameters and 3938 data with F02> 3σ(F02). The metal-metal distance in the cation is 2.527(2) Å and indicates a strong interaction. The magnetic behavior is consistent with the assignment of one unpaired electron to the Mo27+ core of the cation and one to the d1 Mo(V) center of the anion. The interaction between Mo(CO)6 and I2 in THF also results in the formation of 1,4-diiodobutane. 相似文献
15.
Y. Zhang J. Li H. Xu H. Hou M. Nishiura T. Imamoto 《Journal of Molecular Structure》1999,510(1-3):191-196
Synthesis, structure, spectroscopy and thermal properties of complex [Co(NCS)2(hmt)2(H2O)2][Co(NCS)2(H2O)4] (H2O) (I), assembled by hexamethylenetetramine and octahedral Co(II) metal ions, are reported. Crystal data for I: Fw 387.34, a=9.020(8), b=12.887(9), c=7.95(1) Å, =96.73(4), β=115.36(5), γ=94.16(4)°, V=820(1) Å3, Z=2, space group=P−1, T=173 K, λ(Mo-K)=0.71070 Å, ρcalc=1.718567 g cm−3, μ=17.44 cm−1, R=0.088, Rw=0.148. An interesting two-dimensional network is assembled via hydrogen bonds through coordinated and free water molecules. The d–d transition energy levels of Co(II) ion are determined by UV–vis spectroscopy and calculated by ligand field theory. The calculated results agree well with experiment ones. 相似文献
16.
Ganglin Xue Bin Liu Huaiming Hu Jianhui Yang Jiwu Wang Feng Fu 《Journal of Molecular Structure》2004,690(1-3):95-103
A new family of heteropolytungstate complexes (NH4)21[Ln(H2O)5{Ni(H2O)}2As4W40O140]·xH2O(Ln=Y, Ce, Pr, Nd, Sm, Eu, Gd) were prepared by the reaction of Na27[NaAs4W40O140]·60H2O with NiCl2·6H2O and Ln(NO3)3·xH2O at pH≈4.5. The crystal structures of (NH4)21[Gd(H2O)5{Ni(H2O)}2As4W40O140]·51H2O was determined by X-ray diffraction analysis and element analysis. The compound crystallizes in the monoclinic space group P21/n with a=19.754(3), b=24.298(4), c=39.350(6) Å, β=100.612(3)°, V=18564(5) Å3, Z=2, R1(wR2)=0.0544(0.0691). The central site S1 and two opposite sites S2 of the big cyclic ligand [As4W40O140]28− are occupied by one Ln3+and two Ni2+, respectively, each site supply four Od coordinating to metal ion, another one water molecule and other five water molecules coordinate, respectively, to Ni2+and Ln3+. Polyanion [Ln(H2O)5{Ni(H2O)}2As4W40O140]21− has C2v symmetry. IR and UV–vis spectra of [NaAs4W40O140]27− of the title compounds are discussed. 相似文献
17.
Xiao-Bing Cui Ji-Qing Xu Lan Ding Hong Ding Ling Ye Guo-Yu Yang 《Journal of Molecular Structure》2003,660(1-3):131-137
The compound [Zn(H2O)4]2[H2As6V15O42(H2O)]·2H2O (1) has been synthesized and characterized by elemental analysis, IR, ESR, magnetic measurement, third-order nonlinear property study and single crystal X-ray diffraction analysis. The compound 1 crystallizes in trigonal space group R3, a=b=12.0601(17) Å, c=33.970(7) Å, γ=120°, V=4278.8(12) Å3, Z=3 and R1(wR2)=0.0512 (0.1171). The crystal structure is constructed from [H2As6V15O42(H2O)]4− anions and [Zn(H2O)4]2+ cations linked through hydrogen bonds into a network. The [H2As6V15O42(H2O)]6− cluster consists of 15 VO5 square pyramids linked by three As2O5 handle-like units. 相似文献
18.
Limin Yang Dongliang Tao Ying Sun Xianglin Jin Ying Zhao Zhanlan Yang Shifu Weng Jinguang Wu Guangxian Xu 《Journal of Molecular Structure》2001,560(1-3):105-113
The crystal structure of NdCl3·C6H12O6·9H2O has been determined. It crystallizes in the monoclinic system, p2(1)/n space group with cell dimensions: a=15.824(3) Å, b=8.633(2) Å, c=16.219(3) Å, β=107.24°, V=2116.1(7) Å3 and Z=4. Each Nd ion is coordinated to nine oxygen atoms, two from inositol and seven from water molecules, with an Nd–O distance of 2.449–2.683 Å, the other two water molecules are hydrogen bonded. No direct contacts exist between Nd and Cl. There is an extensive network of hydrogen bonds in hydroxyl groups, water molecules and chloride ions in the crystal structure of the lanthanide complex. The Raman spectra of Pr–, Nd– and Sm–inositol are similar, which show that the three metal ions have the same coordination mode. The Raman spectra are consistent with their structures. 相似文献
19.
The complex Fe(η6-C5H5CMe3)2 crystallizes in the centrosymmetric triclinic space group P
(Ci1; No. 2) with unit cell dimensions of a 8.770(1) Å, b 8.878(1) Å, c 11.991(1) Å, 107.56(1)°, β 90.85(1)°, γ 90.13(1)°, V 890.0(2) Å3 and Z = 2. A full sphere of data was collected on a four-circle diffractometer. The structure was solved and refined to R 7.93% for all 3155 independent reflections and R 4.98% for those 2002 data with | F0 | > 6σ. | F0 |. The molecules lie on crystallographic inversion centers at 0, 0, 0 and 1/2, 0, 1/2; the crystallographic asymmetric unit therefore consists of two independent half molecules. The molecule centered at 0, 0, 0 (molecule “A”) is ordered and well-defined; that centered on 1/2, 0, 1/2 (molecule “B”)is probably disordered, as indicated by larger “thermal parameters” and a greater range of apparent interatomic distances. Discussion em phasizes the geometry of molecule A, which has precise Ci symmetry with Fe(1A)-B(1A) 2.297(4) Å and Fe(1A)-C(ring) distances ranging from 2.057(6) Å to 2.138(4) Å. 相似文献
20.
Darryl P. Klein N. Quir s M ndez Jeffery W. Seyler Atta M. Arif J. A. Gladysz 《Journal of organometallic chemistry》1993,450(1-2):157-164
The crystal structures of propionaldehyde complex (RS,SR)-(η5-C5H5)Re(NO)(PPh3)(η2-O=CHCH2CH3)]+ PF6− (1b+ PF6s−; monoclinic, P21/c (No. 14), a = 10.166 (1) Å, b = 18.316(1) Å, c = 14.872(2) Å, β = 100.51(1)°, Z = 4) and butyraldehyde complex (RS,SR)-[(η5-C5H5)Re(NO)(PPh3)(η2-O=CHCH2CH2CH3)]+ PF6− (1c+PF6−; monoclinic, P21/a (No. 14), a = 14.851(1) Å, b = 18.623(3) Å, c = 10.026(2) Å, β = 102.95(1)°, Z = 4) have been determined at 22°C and −125°C, respectively. These exhibit C
O bond lengths (1.35(1), 1.338(5) Å) that are intermediate between those of propionaldehyde (1.209(4) Å) and 1-propanol (1.41 Å). Other geometric features are analyzed. Reaction of [(η5-C5H5)Re(NO)(PPh3)(ClCH2Cl)]+ BF4− and pivalaldehyde gives [(η5-C5H5)Re(NO)(PPh3)(η2-O=CHC(CH3)3)]+BF4− (81%), the spectroscopic properties of which establish a π C
O binding mode. 相似文献