[Et_4N]_2[Zn_2(OPh)_2Cl_4]的合成和晶体结构

ZnCl2, PhONa和Et4NCl稨2O在乙腈溶剂中反应合成了一种二核锌配合物[Et4N]2[Zn2(OPh)2Cl4]。X射线衍射结果表明,晶体属单斜晶系,C2/m空间群,晶胞参数 a = 14.1366(2), b=13.6985(5), c=9.3308(3)牛?107.851(2)o, V=1719.92(9)?,C28H50O2N2Zn2Cl4,Mr=721.24,Z=2,Dx=1.393g/cm3,μ(MoKα)=1.732mm—1,F(000)=756, R=0.0552, wR=0.1534, S=1.027。 配合物是由2个阳离子Et4N+和1个阴离子[Zn2(OPh)2Cl4]2—组成。阴离子[Zn2(OPh)2Cl4]2—包含着1个中心Zn2O2菱形平面。配合物中的2个锌原子通过2个苯酚中的氧原子桥连,每个锌原子还与2个氯原子配位形成变形四面体结构。

Synthesis and Crystal Structure of Pd(ptac-C,N)(acac-O,O)

A stable organometallic Pd (Ⅱ) compound Pd(ptac-C,N)(acac-O,O) (Hacac = acetyl acetone, Hptac = 3-(2-pyridinethioxy)-acac, formula: C15H17NO4SPd, Mr = 413.76) 1 has been synthesized and its crystal structure was determined by X-ray crystallography. The crystal is of monoclinic with space group C2/c, a = 17.9342(3), b = 17.7791(4), c = 13.1800(1) ? b = 128.400(1), V = 3293.5(1) 3, Z = 8, Dc = 1.669 g/cm3, F(000) = 1664, m = 1.269 mm-1, R = 0.0261 and wR = 0.0710 for 2653 observed reflections (I > 2s(I)). There exist two Pd rings in the title compound, C(14)O(4)PdO(3)C(12)C(13) and C(1)NPdC(8)S, with the palladium atom taking a square-planar coordination. Two oxygen atoms from the acetyl acetone ligand (PdO, 1.991(2) and 2.036(2) ), one N atom (PdN 2.019 ? and the g-carbon atom (PdC 2.067(3) ? from the ptac ligand are coordinated to Pd.

A Novel (4,6)-Connected Net Based on Dysprosium Benzenedicarboxylate,[Dy(OAc)(BDC)]_n

A new lanthanide coordination polymer, [Dy（OAc）（BDC）]n 1 （OAc = acetate, BDC = 1,4-benzenediacarboxylate）, has been synthesized under hydrothermal conditions. Single-crystal X-ray diffraction analysis reveals that complex 1 has infinite zigzag Dy-OAc chains, which are further connected by BDC to form a 3D metal-organic framework. According to topology analysis, this framework can be characterized as （4,6）-connected （3.4.54）（32.4.56.66） net that has never been reported before. Crystal structure for 1： space group Pbca, a = 13.314（3）, b = 8.0269（18）, c = 20.275（5）A, V= 2166.8（9）A3, C10H7O6Dy, Mr = 385.66, Z= 8, Dc = 2.364 g/cm^3, μ= 6.910 mm^-1, F（000） = 1448, the final R = 0.0181 and wR = 0.0520.

Synthesis and Crystal Structure of [Cu(phen)_2(SO_4)(H_2O)]·0.5C_4H_4O_4·7H_2O

The title compound, [Cu（phen）2（SO4）（H2O）]·0.5C4H4O4·7H2O （phen = 1,10-phe-nan throline and C4H4O4 = fumaric acid）, has been synthesized and characterized by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1^- with a = 11.4827（2）, b = 11.9086（2）, c = 13.77350（10） A, α = 80.6830（10）, β = 66.6480（10）, γ = 64.048000）°, V = 1554.63（4） A^3, Mr = 722.17, Z = 2, Dc = 1.543 g/cm^3,μ = 0.845 mm^-1, F（000） = 750, R = 0.0349 and wR = 0.0837 for 4754 observed reflections （1 〉 2σ（I））. The compound contains a six-coordinated copper（Ⅱ） center, which is surround by four N atoms of two phen ligands （Cu-N distances in the range of 1.997（2）- 2.225（2） A）, one sulfate O atom （Cu-O = 2.0037（17） A） and one water O atom （Cu-O（Sw） = 2.719（2） A,） in a distorted octahedral geometry. Extensive hydrogen-bonding interactions are involved in water molecules, ligated sulfate anions and fumaric acid molecules. In addition, π-π interactions via aromatic nitrogen-containing ligands are also discussed. The combination of non-covalent interactions leads to the formation of a 3-D network structure.

Synthesis, Structure and Luminescent Property of a New Zinc(Ⅱ) Complex

One new coordination polymer, namely {[Zn（HL）（Hbipy）]2·3H2O}n（bipy = 4,4A-bipyridine, H4 L = 6-（3＇,4＇-dicarboxyl-phenoxy） isophthalic acid）, has been synthesized through a hydrothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectra（IR）, and thermogravimetric（TG） analysis. The crystal structure is of monoclinic, space group P21/n with a = 9.6435（3）, b = 19.8515（7）, c = 12.9731（5） A, β = 103.023（4）o, V = 2419.67（15） A3, C52H38Zn2N4O21, Mr = 1185.6, Z = 2, Dc = 1.619 g/cm^3, F（000） = 1200, μ = 1.083 mm-1, the final R = 0.0443 and w R = 0.1079 for 4269 observed reflections（I 2σ（I）. The compound features a two-dimensional（2D） framework and stabilizes itself by interlayer π···π interactions and innerlayer hydrogen bonds. The 2D layer presents a simple 3-connected 63 topology. Moreover, the thermal dynamic stability and luminescent property of the compound have also been discussed in detail.

Synthesis and Crystal Structure of {Cu_2(pdc)_2(4,4'-bipy)(H_2O)·3H_2O}_2

The title compound {Cu2(pdc)2(4,4?-bipy)(H2O)3H2O}2 1 (H2pdc = pyridine-2,6- dicarboxylic acid, also known as dipicolinic acid; 4,4?-bipy = 4,4?-bipyridine) has been synthesized by the hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pi with a = 7.2278(3), b = 10.6259(4), c = 17.7614(6) ? a = 79.5990(10), = 83.6300(10), ? = 71.8280(10)o, V = 1272.60(8) ?, C48H44Cu4N8O24, Mr = 1371.07, Z = 1, Dc = 1.789 g/cm3, = 1.747 mm-1, F(000) = 696, R = 0.0397 and wR = 0.1137 for 3938 observed reflections (I > 2s(I)). There are two kinds of Cu coordination environments, and each central copper(II) atom is five-coordinated in a distorted square-based pyramidal coordination geo- metry. Four copper(II) atoms are linked by four pdc and two 4,4?-bipy ligands to form an annular rectangle structure. Extensive hydrogen-bonding interactions involving carboxylate O atoms as well as coordinated and free water molecules lead to the formation of a three-dimensional network struc- ture.

A Porous 3D Supramolecular Architecture of Cd(II) Complex with Water Clusters as Pillars

A supramolecular complex of Cd（II） with 1D water tapes as pillars[Cd2（dpa）2（phen）2（H2O）2]·6H2O 1 （H2dpa = diphenic acid, phen = phenanthroline）, has been synthesized and characterized by elemental analysis, IR spectroscopy, and single-crystal X-ray diffraction analysis. The crystal is of triclinic, space group P1^- with a = 9.7029（4）, b = 11.9601（5）, c = 12.1788（4） A, α = 71.6990（10）, β = 71.8740（10）, γ = 74.4680（10）°, V = 1252.39（8） A^3, C52H48Cd2N4O16, Mr = 1209.76, Z= 1, Dc = 1.604 g/cm^3,μ = 0.925 mm^-1, F（000） = 612, R = 0.0679 and wR = 0.2514 for 3870 observed reflections （I 〉 2σ（I））. Two intramolecular Cd（II） centers of this complex are encircled by two dpa^2- ligands forming an 18-membered ring, which is further assembled into a pillared three-dimensional （3D） supramolecular architecture through the synergetic effect of intermolecular face-to-face π…π stacking and weak O-H…O hydrogen-bonding interactions. Moreover, this complex exhibits photoluminescence with the main emission bands located at about 456 nm upon excitation at 355 nm in the solid state at room temperature.

Synthesis and Crystal Structure of a Mo-S Cluster Compound Coordinated by Isonicotinate

A cluster compound, Mo3S4（DTP）3（IN）（Py）·EtOH I （DTP = diethyl dithiophosphate, IN = isonicotinate） has been rationally synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 13.6345（2）, b = 13.7805（2）, c = 14.5400（1）A, α = 107.078（1）, β = 113.380（1）, γ = 96.310（1）°, C25H45Mo3- N2O9P3S10, Mr = 1218.96, V = 2315.75（5） A^3, Z = 2, Dc = 1.748 g/cm^3, μ = 1.399, F（000） = 1224, R = 0.0425 and wR = 0.1144 for 6335 observed reflections （I 〉 2σ（I））. 31^P NMR spectrum has been measured with the resonance 110.050 and 108.783 （2：1）.

A Three-dimensional Supramolecular Complex {[Co(H_2btec)(2,2'-bipy)(H_2O)_3]·H_2O}_n Assembled via Hydrogen Bonding and π-π Stacking Interactions

A new cobalt compound,{[Co（H2btec）（2,2＇-bipy）（H2O）3]·H2O}n （1,H4btec=1,2,4,5-benzenetetracarboxylic acid,2,2＇-bipy=2,2＇-bipyridine）,has been synthesized and charac-terized by single-crystal X-ray diffraction,elemental analysis,IR and X-ray powder diffraction.The crystal belongs to the triclinic system,space group P1,with a=7.230（3）,b=11.626（5）,c=14.001（6）,α=108.12（0）°,β=95.85（0）°,V=1095.33（157）3,C20H20CoN2O12,Mr=539.31,Z= 2,Dc=1.635 g/cm3,μ=0.855 mm-1,F（000）=554,R=0.0427 and wR=0.1042 for 3883 observed reflections （I 〉 2σ（I））.The title compound features a discrete molecular structure,which is connected with each other through extensive O-H…O hydrogen bonds into an intricate 3D supramolecular network.Additionally,two different patterns of π-π stacking interactions further consolidate the framework.