共查询到20条相似文献,搜索用时 15 毫秒
1.
《Journal of Coordination Chemistry》2012,65(3):155-159
The title complex was prepared by reaction of succinatomanganese(II) with imidazole in water-ethanol. The complex crystallizes in orthorhombic space group Pna 2 1 with a = 7.9990(15), b = 14.8690(15), c = 11.028(2) Å. The metal assumes a distorted octahedral coordination. In the crystal, each succinate dianion bridges three Mn(II) atoms to form a polymer with a layered structure. 相似文献
2.
《Journal of Coordination Chemistry》2012,65(21):3877-3890
In aqueous methanolic solution, reactions of CuCl2, m-hydroxybenzoic acid (HL), and NaOH with 2,2'-bipyridine (bpy) and 1,10-phenanthroline (phen) at room temperature afforded {[Cu(bpy)L](µ2?Cl)(µ2?L)[Cu(bpy)L]}?1.2H2O (1) and {[Cu(phen)Cl](µ2?Cl)(µ2?L)[Cu(phen)L]} (2) with chloro- and carboxylato-bridged dinuclear [Cu(µ2?Cl)(µ2?COO)Cu] cores. The Cu2 dimers in 1 are pairwise aggregated to form H-bonded tetranuclear motifs, which are extended by H2O into 1-D H-bonded chains and further assembled into 2-D supramolecular networks. The Cu2 dimers in 2 are also linked into 1-D H-bonded chains and further assembled into 2-D supramolecular layers. Magnetic measurements indicate that significant antiferromagnetic interactions (J = ?15.9, ?12.2 cm?1) between Cu2+ ions are dominant in these dinuclear [Cu(µ2?Cl)(µ2?COO)Cu] cores. To the best of our knowledge, 2, crystallizing in the acentric polar orthorhombic space group Pna21, represents the first example of metal m-hydroxybenzoato complexes with ferroelectric properties with a remnant polarization (Pr) of ca. 0.04?µC cm?2, coercive field (Ec) of ca. 2.52 kV cm?1, and saturation of the spontaneous polarization (Ps) at ca. 0.195?µC cm?2. 相似文献
3.
A. A. Trifonov D. M. Lyubov E. A. Fedorova G. G. Skvortsov G. K. Fukin Yu. A. Kurskii M. N. Bochkarev 《Russian Chemical Bulletin》2006,55(3):435-441
The insertion of N,N′-dicyclohexylcarbodiimide at one of the Y-N bonds of the [(Me3Si)2N]3Y complex in toluene at 70 °C afforded the monoguanidinate diamide derivative { (Me3Si)2NC(N-cyclo-Hex)2}Y[N(SiMe)3]2 (1) (cyclo-Hex is cyclohexyl) in 72% yield. The reaction of equimolar amounts of sodium N,N′-dicyclohexyl-N″-bis(trimethylsilyl)guanidinate, which was prepared in situ from {(Me3Si)2N}Na and N,N′-dicyclohexylcarbodiimide, and YbI2(THF)2 in THF gave the [{(Me3Si)2NC(N-cyclo-Hex)2}YbI(THF)2]2 complex (2). An attempt to use this procedure for the synthesis of the yttrium compound { (Me3Si)2NC(NSiMe3)2}2YCl containing the sterically more hindered guanidinate ligand unexpectedly led to the formation of the diamide chloride complex [{(Me3Si)2N}2Y(THF)(µ-Cl)]2 (3). The structures of complexes 1–3 were established by X-ray diffraction. Compound 1 is mononuclear. Complexes 2 and 3 are dinuclear and contain two µ2-bridging halide ligands. 相似文献
4.
A. V. Virovets A. L. Gushchin P. A. Abramov N. I. Alferova M. N. Sokolov V. P. Fedin 《Journal of Structural Chemistry》2006,47(2):326-338
Various synthetic approaches are used to obtain new triangular complexes with rare cluster nuclei M3Te7 4+ (M = Mo, W), as well as with partial substitution for chalcogen W3Te3.8Se 3.2 4+ . The crystalline structure has been identified for K5{[Mo3Te7(CN)6]2I}·2.5H2O (I), K3{[Mo3Te7(CN)6]SeCN}·3.25H2O (II), Cs2K{ [W3Te7(CN)6]Br0.8Cl0.2}·2.5H2O (III), Cs3{ [W3Te7(CN)6]Br}·2H2O (IV), Cs1.59K1.41{[W3Te3.8Se3.2× ×(CN)6]Br}·1,5H2O (V), [W3Te7((EtO)2PS2)3]Br (VI). The compounds are characterized by IR methods and electronic spectroscopy, electrospray-mass-spectrometry. The crystalline structure of this class of compounds is analyzed. Specific non-valence interactions in these systems are considered in detail. 相似文献
5.
液相色谱柱后衍生法同时测定Pb~(2+)Cu~(2+)Cd~(2+)Co~(2+)Zn~(2+)和Ni~(2+) 总被引:3,自引:0,他引:3
采用液相色谱流动相为0.05mol·L~(-1)草酸和0.095mol·L~(-1)氢氧化锂,流速为1.0ml·min~(-1);柱后衍生试剂为0.001mol·L~(-1)PAR+0.3mol·L~(-1)氨水+0.1mol·L~(-1)乙酸,流速为1.0ml·min~(-1),进样体积为20μl,检测波长为500nm,同时对Pb~(2+)、Cu~(2+)、Cd~(2+)、Co~(2+)、Zn~(2+)和Ni~(2+)检测。方法可用于水样检测。 相似文献
6.
本文以定量分析水中微量Cu、Zn、Pb、Cd、Mn、Fe、Ni为目的,对401型树脂与原子吸收分光光度法并用的基本条件进行了研究。本方法适用于清洁地面水水质的分析,其定量条件为:氢型树脂2.5克(干重),pH5.5~6,水样交换流速及洗脱液流速分别为2.5~5.0ml/min、3ml/min,以25ml容量瓶定容,试液置于原子吸收分光光度计上测定。用于浑河源头水质背景调查中,水样加标回收率为Cu:101~105%、Pb:110~116%、Zn:98~114%、Cd:94~96%、Mn:95~101%、Fe:97~100%、Ni:96~7%范围内。方法的检测下限为Cu:0.5ng/ml、Pb:1.1ng/ml、Cd:0.1ng/ml、Zn:0.25nmg/ml、Mn:0.7ng/ml、Fe:0.7ng/ml、Ni:0.7ng/ml。 相似文献
7.
Two new dibenzyltin bisditiocarbamates(PhCH2)2 Sn(S2CNEt2)2(1) and (PhCH2)2 Sn(S2CNC4H8)2(2) were synthesized by the reaction of dibenzyltin dichloride with dithiocarbamates and characterized by elemental analysis ,IR,^1H NMR and MS spectra.The crystal structures were determined by X-ray single crystal diffraction analysis.In both complexes,the tin atom is six-coordinated in a distorted octahedral configuration.In the crystals of 1,the molecular packing in unit cell reveals that the two adjacent molecules are symmetrically linked to each other in dimers by two Sn S interactions of 0.3816nm.In the crystals of 2,the molecules are packed in the unit cell in one-dimensional chain structure linked by weaker intermolecular S S conmtacts. 相似文献
8.
9.
高温固相法合成了KNaCa2(PO4)2:Eu2+,Mn2+荧光粉,并探讨其发光性质和Eu2+-Mn2+间的能量传递。Eu2+的470 nm发射峰源于Eu2+的5d-4 f跃迁,最佳掺杂浓度为0.01 mol,Eu2+的激发峰位于400 nm,与UV-LED管芯的发射光谱(350~410 nm)匹配。Mn2+的565和618 nm的发射来自Mn2+的4T1(4G)-6A1(6S)跃迁。KNaCa2(PO4)2:0.01Eu2+,nMn2+系列样品中,随着Mn2+浓度的增加,Eu2+的发射峰逐渐降低,Mn2+的发射峰逐渐增强,Eu2+对Mn2+的发光有明显的敏化作用。根据D exter电多极相互作用能量传递公式,可得出Eu2+与Mn2+之间的能量传递归因于电偶极-电四极相互作用引起的共振能量传递。 相似文献
10.
Peter Švančárek Peter Schwendt Jozef Tatiersky Ivana Smatanová Jaromír Marek 《Monatshefte für Chemie / Chemical Monthly》2000,131(2):145-154
Summary. Oxo peroxo glycolato complexes of vanadium(V) (M
2[V2O2(O2)2(C2H2O3)2]ċnH2O (n=0, 1; M=NBu4
+ (1), K+ (2), NH4
+ (3), Cs+ (4), NPr4
+ (5)) as well as (NBu4)2[V2O4(C2H2O3)2]ċ H2O (6) have been prepared and characterized by spectroscopic methods. X-Ray structure analysis of 1 revealed the presence of dinuclear [V2O2(O2)2(C2H2O3)2]2− anions with a (chemical structure) bridging core and six coordinated vanadium(V) atoms in a distorted pentagonal pyramidal
array.
Received July 12, 1999. Accepted (revised) October 28, 1999 相似文献
11.
《Journal of organometallic chemistry》1987,336(3):377-383
The complexes [WI2(CO)(NCMe)(η2)-RC2R)2] (R = Me and Ph) react in CH2Cl2 with an excess of carbon monoxide to give initially the acetonitrile substituted products [WI2(CO)2(η2-RC2R) 2]. For R= Me, the complex [WI2(CO)2(η2- MeC2Me)2] (1) was isolated and its structure determined by X-ray crystallography. However, for R = Ph, dimerisation occurs to give the iodide-bridged compound [W(μ-I)I(CO)(η2-PhC2Ph)2]2 (2) with loss of carbon monoxide. These reactions are reversible as 1 and 2 react with acetonitrile to give [WI2(CO)(NCMe)(η2-RC2R)2]. The 13C NMR spectra of I and 2 indicate that the two alkyne ligands donate a total of six electrons to the tungsten in these complexes. 相似文献
12.
《Journal of Coordination Chemistry》2012,65(4):533-550
Abstract [trans-Co(en)2(NO2)2]ClO4 (I) crystallizes, at 22°C, from a deionized water solution, as a racemate, in space group P$1 (No. 2), with lattice constants: a = 6.581(2)Å, b = 8.274(1) Å, c = 12.660(3)Å, α = 77.28(2)Å, β = 76.58(2)°, γ = 75.20(2)° V = 638.71;Å3 and d(calc; MW = 370.59,z = 2) = 1.927gcm?3. A total of 2233 data were collected over the range of 4° ≤ 2θ ≤ 50° of these, 1961 (independent and with I ≤ 3σ(I)) were used in the structural analysis. Data were corrected for absorption (μ = 15.989 cm?1) and the relative transmission coefficients ranged from 0.6792 to 0.9874. The final R(F) and R≤(F) residuals were, respectively, 0.0738 and 0.0763. Two half cations are located at inversion centers; the anions are in general positions. meso-[Co-trans-Me-(N-Me-ethylenediamine)2-trans(NO2)2]ClO4 (II) [(N-Meen) = N-methyl-ethylenediamine] crystallizes at 22°C, from a deionized water solution in space group Pbca (No. 61) with lattice constants: a = 16.882(5) Å, b = 11.990(3) Å, c = 15.017(5) Å; V = 3039.72 Å3 and d (calc;MW = 398.64, z = 8) = 1.742g cm?3. A total of 5281 data were collected over the range of 4° ≤ 2θ ≤ 50° of these, 1779 (independent and with I ≤ 2.5σ(I) were used in the structural analysis. Data were corrected for absorption (μ = 13.501 cm?1 and the transmission coefficients ranged from 0.7956 to 0.9947. The final refinement of the structure (anisotropic thermal parameters for the heavy atoms; idealized hydrogens for the cation) are R(F) = 0.045 and Rw (F) = 0.052). The -NO2 ligands are trans to one another in the axial direction while the N-methyl groups are trans to one another across the basal plane. The cations are located in general positions and the torsional angles of the en rings are δ(N1-C1-C2-N2 = 52.0°) and δ(N3-C3-C4-C4 = 51.0°), in contrast with those of (I) which are of opposite helical chirality. This compound is one of two trans-Co(III)X2 cations of which we are aware that, while sitting at a general position of the space group, has two ethytenediamine rings of the same helical chirality. K[trans-Co(β-alaninato)2(NO2)2] (III) obtained after several batches of crystals of (TV) had separated from the mother liquor (see Syntheses). (III) crystallizes at 22°C, in space group Cc (No. 9) with lattice constants: a = 12.385(6)Å, b=13.109(5)Å, c = 8.290(5)Å, β=115.19° V = 1217.97 Å3 and d(calc; MW = 366.22, z = 4) = 1.997 g cm?3. A total of 1238 data were collected over the range of 4° ≤ 2θ 50° of these, 1016 (independent and with I ≤ 2.5σ(I) were used in the structural analysis. Data were corrected for absorption (μ 17.90cm?1) and the transmission coefficients ranged from 0.5322 to 0.6627. The final R(F) and Rw (F) residuals were, respectively 0.020 and 0.022. Solution of the structure, using the first batch of crystals, proved that the compound isolated was the (H5O2)+ derivative (see below and Discussion). A later batch of crystals contained (III). We have previously observed the precipitation of hydronium salts, trapped by amine carboxylato salts of cobalt (see Discussion). The anions consist of two six-membered rings formed by the metal and two (O,N)-bound β-alaninato ligands; and, both have chair conformations. (H5O2) [trans-Co(β-alaninato)2(NO2)2] (IV) is the substance that first crystalized from an aqueous solution of (III) (see Experimental). It crystallizes, at 22°C, in space group Cc (No. 9) or C2/c (No. 15) with lattice constants: a=12.389(39)Å, b=13.120(11)Å, c=8.299(9) Å, β=115.09(19)° V=1221.72 Å3 and d(calc; MW=364.15, z=4) = 1.980 g cm?3. An incomplete data set of 1592 reflections was collected over the range 4° ≤ 2θ ≤ 50° because the crystal decomposes in air due to rapid loss of water of crystallization, as shown by differential scanning calorimetry. 956 data were independent with I ≤ 2.5°(I) and were used in the structural analysis. Data were not corrected for absorption because of decomposition of the crystal. The final R(F) and Rw (F) residuals were, respectively, 0.14 and 0.16. To the precision of such a data set, the anions are identical with those found in (III); however the cation, which sits at an inversion center, consists of a proton sandwiched between the oxygens of two waters thus forming (H5O2)+ cations similar to those we have described in the past (see Refs. [15–18]). 相似文献
13.
[Pb2(TNR)2(CHZ)2(H2O)2]4H2O的结构及热分解机理 总被引:1,自引:0,他引:1
The coordination compound of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O was prepared by using the aqueous solution of carbohydrazide, lead nitrate and sodium styphnate. The molecular structure of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O(C 7H 13 N 7O 12 Pb, Mr=594.43) was determined by using a single crystal diffraction analysis .The thermal decomposition mechanism of the title compound was studied by TGDTG, DSC and IR techniques. The crystal belongs to monoclinic with space group P2 1/n.The unit cell parameters are as follows: a=0.64700(10)nm, b=1.6074(3)nm, c=1.4883(3)nm,β=97.42(2)°,V=1.5349(5)nm3, Z=2, DC=2.572g•cm -3 ,μ(Mo, Kα)=11.080cm -1 , F(000)=1128. R=0.0422, Rw=0.0735. The binuclear lead coordination compound is bridged by two carbohydrazide molecules. The molecule has a symmetrical center. TNR 2- ,CHZ and H 2O coordinate with the central ions simultaneously. 相似文献
14.
[Mn2(TNR)2(CHZ)2(H2O)4]·2H2O的合成和晶体结构 总被引:3,自引:0,他引:3
将MnCO3与2,4,6-三硝基间苯二酚(斯蒂芬酸、TNR)分散于蒸馏水中,加热搅拌制备出斯蒂酚酸锰溶液,再与碳酰肼(CHZ)水溶液反应制备〖Mn2(TNR)2(CHZ)2(H2O)4〗·2H2O(C14H26Mn2N14O24,Mr=884.36),并对其进行了元素分析和红外表征,利用单晶分析测定了晶体结构。该化合物为双核配合物,属三斜晶系,空间群为^-P1,晶体学数据如下:a=7.280(1) 相似文献
15.
16.
《结构化学》1985,(1)
<正> Mr=996.91, triclinic, P1, a=8.773(2), b=9.712(3), c=13.652(1) A; α=69.24(0), β=70.43(3), γ=66.87(l)°; Z=l, Dx=1.699 g/cm 3. Final R=0.053 for 3186 reflections with I≥3a(I). There is an interesting trans influence of μ-s bridge in this binuclear cluster. Mo-Mo distance is 2.752(1) A. 相似文献
17.
2D氢键网络镉配合物Cd(pyridine-2-sulfonato)2(H2O)2和锌配合物Zn(pyridine-2-sulfonato)2(H2O)2的合成和晶体结构 总被引:6,自引:0,他引:6
合成了镉的吡啶-2-磺酸配合物Cd(C5H4NSO3)2(H2O)2 1和锌的吡啶-2-磺酸配合物Zn(C5H4NSO3)2(H2O)2 2。 研究表明, 2个化合物属异质同晶, 均属单斜晶系, 空间群为C2/c. 化合物1晶胞参数为:a = 13.7671(5), b = 7.2778(3), c = 16.1559(9) ? b = 106.656(3)? V = 1550.8(1) 3, Z = 4, Dc = 1.990 g/cm3, m =1.719 mm-1, F(000) = 920, R = 0.0225, wR = 0.0584, 共收集到1759个独立衍射点, 其中I≥2(I)的可观测点为1681个;化合物2晶胞参数为:a = 13.711(1), b = 7.1451(9), c = 15.972(1) , b =107.079(5)? V = 1495.7(3) 3, Z = 4, Dc = 1.855 g/cm3, m = 1.964 mm-1, F(000) = 848, R = 0.0310, wR = 0.0831, 共收集到1707个独立衍射点, 其中I≥2(I)的可观测点为1592个。在2个标题配合物中, Cd2+离子(或Zn2+离子)由2个吡啶-2-磺酸中的2个氮和2个氧以及2个水分子中的2个氧配位形成畸变的N2O4八面体配位构型。每个配合物分子具有晶体学2次旋转轴对称性。配合物分子之间通过许多OH(配位水分子)LO(未配位磺酸根)氢键联结成二维结构网络。 相似文献
18.
《结构化学》1986,(2)
<正> (Ph2Ppy)2(μ-Cl)2Cu2Cl2 (C34H28Cl4Cu2N2P2): Mr=795.5, triclinic, Pl, a=13.891(2), b= 13.196(3), c= 20.158(4) A, d= 90.28(1)°, β=110.05(2)°, r= 90.13(1)°, Z=4, V= 3471.04A3, Dx=1.53 gcm-3, R=0.066, Rw= 0.076 for 5486 observed unique reflections. The complex was prepared by the reaction of (Ph2Ppy)2NiCl2 with CuC≡CPh in CH2Cl2 solution. 相似文献
19.
用碳酰肼 (CHZ ,NH2 NHCONHNH2 )、硝酸铅和三硝基间苯二酚 (TNR ,斯蒂酚酸 )的水溶液制备 [Pb2 (TNR) 2 (CHZ) 2 (H2 O) 2 ]·4H2 O .采用单晶分析的方法测定它的分子结构 ,并用TG DTG、DSC和 IR相结合的技术研究它的热分解机理 .所得晶体属单斜晶系 ,P2 1/n空间群 .晶体学参数为 :a=0 .6470 0 ( 10 )nm ,b =1.60 74 ( 3)nm ,c=1.4 883( 3)nm ,β =97.4 2 ( 2 )° ,V =1.534 9( 5)n ,Z =2 ,DC=2 .572 g·cm- 3,μ(Mo ,Kα) =11.0 80cm- 1,F( 0 0 0 ) =112 8.最终偏离因子R =0 .0 4 2 2 ,Rw=0 .0 735.该配合物分子呈中心对称 ,两个羰基O原子形成两个氧桥 ,TNR2 - ,CHZ和H2 O同时参与了与中心离子的配位 相似文献
20.
Vladimir L. Kolesnichenko Victor B. Rybakov Leonid A. Aslanov Sergei V. Volkov 《Journal of Cluster Science》1997,8(1):27-45
Thioselenohalide complexes Mo2(μ-S2)2Cl6(SeCl2)2 (I), Mo2(μ-S2)2Br6(SeBr2)2 (II), and W2(μ-S2)2Br6(SeBr2)2 (III) were synthesized by the reactions of corresponding metal halides or carbonyls or molybdenum metal with excesses of S2 X 2+Se2 X 2 mixtures. The complex W2(μ-S2)2Cl6(SeCl2)2 (IV) was obtained by an exchange reaction between (III) and excess of Se2Cl2. Coordination of the neutral SeX 2 ligands to thiohalidesM 2(μ-S2)2 X 6 results in higher thermal stability, and suggests the possibility to synthesize SeX 2 complexes of the unstable parent tungsten thiohalides. An unusual oxidative addition reaction of (I) was detected: {fx27-1} Both (I) and (IV) were characterized by X-ray crystal structure analysis. They are isostructural and form discrete molecules. Bridging S 2 2? ligands are coordinated perpendicularly to the metal-metal bond;d(M?M)=2.8066 Å and 2.793 Å for I and IV, respectively. Nonequivalence of chlorine atoms which are bound to the metal atom, relate to nonequivalence of halogen atoms in the complexesM 2(μ?S2)2 X 8 2? . Chlorine atomstrans to SeCl2 ligands form short bonds with the metal; the corresponding35Cl NQR frequency is increased. The selenium dichloride ligand is ambidentate. The selenium atom binds as a donor to the metal and as an acceptor to two chlorine atoms which are also bound covalently to the same metal atom. 相似文献