一维链状μ-氯(氧)-三苄基锡的合成和结构研究

合成了两种具有新型结构的苄基锡化合物：一维链状μ-氯-三苄基锡(1)和一维链状μ-氧-三苄基锡(2)，经X-射线方法测定了化合物的晶体结构。晶体结构(1)属正交晶系，空间群为P2₁2₁2₁，晶体学参数：a=0.855 3(3) nm，b=1.081 4(4) nm，c=1.968 1(7) nm，V=1.820 4(11) nm³，Z=4，D_c=1.560 g·cm^-3，μ(Mo Kα)=15.47 cm^-1，F(000)=856，R₁=0.059 7，wR₂=0.141 5。晶体结构(2)属正交晶 系，空间群为P2₁2₁2₁，晶体学参数：a=1.982 3(4) nm，b=1.089 1(2) nm，c=0.861 1(17) nm，V=1.859 0(6) nm³，Z=4，D_c=1.458 g·cm^-3， μ(Mo Kα)=13.76 cm^-1，F(000)=820，R₁=0.032 7，wR₂=0.064 8。配合物中锡原子均呈五配位畸变三角双锥构型。     

梯形结构有机锡配合物{[(p-MeC6H4CH2)2Sn]2(O)(Cl)OC2H5}2的合成和晶体结构

The title compound {[(p-MeC₆H₄CH₂)₂Sn]₂(O)(Cl)OC₂H₅}₂ was synthesized by the reaction of bis(p-met-hylbenzyl)tin dichloride with KOH in ethanol. The crystal structure of the complex has been determined by X- ray diffraction. The crystal belongs to monoclinic, space group P2₁/c with a=1.114 0(19) nm, b=2.423 1(3) nm, c=2.521 1(3) nm, β=99.398(3)°, V=6.714(16) nm³, Z=4, D_c=1.493 g·cm^-3, μ(Mo Kα)=15.94 cm^-1, F(000)=3 024, R₁=0.049 9, wR=0.101 7. The crystal structure shows that the coordination geometry of tin is a distorted trigonal bipyramid, and the ladder-like structure is shaped by three Sn₂O₂ planar four-membered rings. CCDC: 639682.     

配合物[Mn(2,2′-bipy)(H2O)4]·(m-phth)的水热合成和晶体结构

A mononuclear manganese complex [Mn(2,2′-bipy)(H₂O)₄]·(m-phth) (2,2′-bipy=2,2′-bipyridine, m-phth=isophthalate) has been synthesized by hydrothermal methods. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group Pnna with a=0.766 8(8) nm, b=2.050 2(2) nm, c=1.247 0(13) nm, V=1.960 4(4) nm³, Z=4, M_r=447.30, D_c=1.376 g·cm^-3, μ=0.722 mm^-1, F(000)=924, R_int=0.027 0, R=0.028 0 and wR=0.075 5. In the crystal the manganese atom is six-coordinated by two nitrogen atoms from 2,2′-bipyradine and four oxygen atoms from water molecules, completing an octahedral coordination geometry. The isophthalate molecules are included in the lattice and connected to Mn(2,2′-bipy)(H₂O)₄ by hydrogen bonding interactions to form a three-dimensional supramolecular structure. CCDC:286965.     

配合物[Mn(2,2''-bipy)(H2O)4]·(m-phth)的水热合成和晶体结构

A mononuclear manganese complex [Mn(2,2'-bipy)(H2O)4]·(m-phth) (2,2'-bipy=2,2'-bipyridine, m-phth=isophthalate) has been synthesized by hydrothermal methods. The crystal structure was determined by singlecrystal X-ray diffraction. The crystal is of orthorhombic, space group Pnna with a=0.766 8(8) nm, b =2.050 2(2)0.027 0, R=0.028 0 and wR=0.075 5. In the crystal the manganese atom is six-coordinated by two nitrogen atoms from 2,2'-bipyradine and four oxygen atoms from water molecules, completing an octahedral coordination geometry. The isophthalate molecules are included in the lattice and connected to Mn(2,2'-bipy)(H2O)4 by hydrogen bonding interactions to form a three-dimensional supramolecular structure. CCDC:286965.     

配位聚合物[Mn(2，4，6-TMBA)2(H2O)3]n·2nH2O的水热合成和晶体结构

The title compound, [Mn(2,4,6-TMBA)₂(H₂O)₃]_n·2nH₂O(1), where 2,4,6-TMBA=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic, space group C2/c with a=2.929 9(6) nm, b=1.036 4(2) nm, c=8.222 04(17) nm, V=2.494 7(9) nm³, Z=4, M=471.40, D_c=1.255 g·cm^-3, μ=0.571 mm^-1, F(000)=996, R_int=0.029 4, R=0.037 6 and wR=0.094 9. The Mn atoms are octahedrally coordinated by two O atoms of two ligands and four O atoms of water. The carboxyl group coordinates to Mn(Ⅱ) in the mode of monodentate, while the O atoms of water molecules coordinates in bridging mode. The complex shows a one-dimensional chain structure bridged by water molecules. CCDC: 297750.     

二茂铁甲酸(三邻氯苄基)锡配合物的合成、结构和量子化学研究

The novel complex tri(o-chlorobenzyl)tin ferrocenecarboxylate have been synthesized.The crystal structure of the complex has been determined by X-ray diffraction.The crystal belong to orthorhombic with space group Pbca with a=0.1242(5), b=1.7242(7), c=3.0583(13)nm, V=5.928(4)nm³,Z=8, D_c=1.623g·cm^-3,μ(MoKα)= 0.1631cm^-1,F(000)=2896,R₁=0.0461,wR₂=0.0931. The bond lengths of Sn-C is 0.2148(4), 0.2152(6) and 0.2176(5)nm, respectively. The Sn-O is 0.2073(4)nm. The tin atom has a distorted tetrahedral geometry. The study on title complex has been performed,with quantum chemistry calculation by means of G98W package and taking Lanl2dz basis set. The stability of the complex, some frontier molecular orbital energies, the populations of the atomic net charges in complex and composition characteristics of some frontier molecular orbitals have been investigated. CCDC: 184267.     

Cd（Ⅱ）—SAF—DDMBA显色反应的研究及应用

研究了Cd(Ⅱ)与水杨基荧光酮(SAF)-溴化十二烷基二甲基苄铵(DDMBA)显色反应的条件,在表面活性剂DDMBA存在下,pH 10的硼砂-氢氧化钠缓冲介质中,Cd(Ⅱ)与SAF形成1:4紫红色配合物,配合物于570nm有最大吸收,表观摩尔吸光系数9.26×10~4,镉含量在0～6μg/25ml符合比耳定律,方法简便、灵敏,精密度高,准确度好,应用于铅渣中镉的测定,结果满意。     

多元混配合物[Ni(NPA)2(Phen)(Ac)(H2O)]·H2O的合成、晶体结构

A Nickle(Ⅱ) complex [Ni(NPA)₂(Phen)(Ac)(H₂O)]·H₂O has been synthesized (NPA=N-phenylanthranilic acid， Phen=1，10-phenanthroline and Ac=acetate) and characterized by IR， elemental analysis and X-ray crystal structure determination. It crystallizes in triclinic system， space group P1 with a=0.891 25(2) nm， b=1.451 85(3) nm， c=1.485 54(3) nm， α=67.384(1)°， β=82.932(1)°， γ=85.168(1)°， V=1.759 50(6) nm³， Z=2， D_c=1.405 g·cm^-3， F(000)=778， R₁=0.032 3， wR=0.084 7. The crystal structure shows that the Nikcle(Ⅱ) ion is coordinated with two oxygen atoms from two N-phenylanthranilic acid，two nitrogen atoms from one 1，10-phenanthroline， two oxygen atoms from one acetate and one water respectively， forming a distorted octahedral coordination geometry. CCDC: 657265.     

α-取代苯并噻吩钌乙炔及钌乙烯配合物的合成、表征、电化学及光谱电化学性质

以α-取代苯并噻吩乙炔及乙烯基为配体,与不同辅助配体键合的金属钌为氧化还原活性端基,分别合成并表征了α-取代苯并噻吩钌乙炔及钌乙烯配合物1和2,两个配合物均经X射线单晶衍射的确证。电化学性质表明配合物1具有较好的氧化还原可逆性,金属氧化态相对于2比较稳定。红外光谱电化学研究表明配合物1和2分别形成1~+和2~+后,与金属相连的ν(C≡C)和ν(C≡O)伸缩振动吸收均发生变化,其中ν(C≡C)变化较大,可能由于形成了Ru=C=C结构;紫外可见近红外光谱电化学研究发现电解后,中性分子1和2在紫外区域的强吸收峰均逐渐降低,1~+分别在可见及近红外580 nm,698 nm及874 nm处出现较弱的3个吸收峰,3个吸收峰可能归属于LMCT吸收。2~+在296 nm处出现1个很弱的吸收峰,这不同于配合物1~+,可能源于2~+的稳定性。     

一维链状锰配合物[Mn3(L)6(CH3OH)2]n·0.5nH2O的水热合成和晶体结构

The title compound, [Mn3(L)6(CH3OH)2]n·0.5nH2O (1), where HL=3,5-dirnethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction structure analysis. The crystal is of triclinic,space group P1 with α=1.275 1(13) nm, b=1.354 6(14) nm, c=1.882 3(19) nm, α=110.826(1)°,β=94.358(2)°,γ=108.038(1)°, V=2.825 4(5) nm3, Z=1, Mr=2 265.77, Dc=1.332 g·cm-3,μ=0.723 mm-1, F(000)=1180, Rint=0.037, R=0.056 4, wR=0.128 5. In the crystal the manganese atom is six-coordinated by six oxygen atoms, completing an octahedral geometry. The molecules are connected by 3,5-dimethylbenzoic acid to form a 1D chain structure bridged. CCDC: 694097.