Solvothermal Synthesis,Crystal Structure and Characterizations of a Novel 2D Organic Decorated Manganese Thiostannate:MnSnS3(1,2-DACH)

A novel 1,2-diaminocyclohexane（1,2-DACH） decorated manganese thiostannate,namely MnSnS_3（1,2-DACH）（1）,has been solvothermally synthesized by the reaction of Mn（CH_3COO）_2·4H_2O,Sn and S in the stoichiometric ratio in 1,2-DACH,which acted as an efficient structure-directing agent（SDA） and reactive solvent in the formation of the title compound. Single-crystal X-ray diffraction studies revealed that the title compound crystallizes in the monoclinic space group P2_1/c with a = 12.2458（7）,b = 13.8588（7）,c = 7.2292（4） ？,β = 99.460（6）°,V = 1210.20（12） ？~3,Z = 4,Dc = 2.108 g·cm^（-3）,F（000） = 748,μ = 3.584 mm^（-1）,R = 0.0348 and wR = 0.0823（I 〉 2σ（I））. The structure features a neutral two-dimensional（2D） network constructed by the unsaturated [Mn（1,2-DACH）] complexes interconnecting [SnS_3]_n^（2n-） chains via sharing S. Thermal stability and optical property of compound 1 were characterized.

Synthesis and Crystal Structure of a Novel Three-dimensional Manganese(Ⅱ) Coordination Polymer:[Mn(pdc)]_n (pdc=Pyridine-2,4-dicarboxylate)

A novel manganese（H） coordination polymer [Mn（pdc）]n （pdc = pyridine-2,4- dicarboxylate） has been synthesized under hydrothermal conditions. The crystal is of monoclinic, space group P211n with a = 6.506（4）, b = 9.392（6）, c = 11.217（7） A, β = 105.650（12）°, V= 660.0（7）A3, Z = 4, Mr = 220.04, Dc = 2.215 g/cm3,μ = 1.971 mm-1, F（000） = 436, Rint = 0.0345, R = 0.0360 and wR = 0.0778 for 1259 observed reflections with I 〉 2σ（I）. In the structure, the Mn（Ⅱ） atom is coordinated in a distorted octahedral arrangement by one pyridine N and five carboxylate O atoms from five pdc ligands, each of which coordinates to five Mn atoms to propagate a three-dimensional layered framework.

A 2D Layered Thiostannate: Synthesis and Crystal Structure of [tmdpH_2]Sn_3S_7

A new thiostannate,[tmdpH2]Sn3S7 1（tmdp = 4,4＇-trimethylenedipiperidine）,has been synthesized under solvothermal conditions and characterized by elemental analysis,IR spectroscopy,and single-crystal X-ray diffraction analysis.In 1,the Sn3S4 secondary incomplete cubane-like building units are bridged by μ2-S atoms to form Sn12S12 rings which are then joined parallelly to the [001] plane,giving the final 2D（Sn3S7^2-）n layer of（6,3） network.The layers are stacked along the c axis so that 24-membered ring channels are generated,in which the organic cations are accommodated.The compound crystallizes in monoclinic,space group C2/c,with a=23.052（3）,b=13.4039（12）,c=18.412（2）A,β=120.112（4）°,V=4921.3（9）A^3,C13H28N2S7Sn3,Mr=792.86,Z=8,Dc=2.140 g/cm^3,F（000）=3056,μ=3.619 mm^-1,the final R=0.0488 and wR=0.1125 for 4607 observed reflections with I〉2σ（I）.

Two-dimensional Network Crown Ether Complex. Synthesis and Crystal Structure of 18-Crown-6 Complex: [K(18-C-6)]_2[Cd-(mnt)_2]

The novel complex [K(18-C-6)]_2 [Cd(mnt)_2] [18-C-6 = 18-crown-6, mnt =1,2-dicyanoethene-1,2-dithiolate, C_2S_2-(CN)_2^(2-)] was synthesized and characterized by elementalanalysis, IR spectrum and X-ray diffraction analysis. The complex displays two-dimensional networkstructure of [K(18-C-6)] complex segments and [Cd(mnt)_2] complex segment bridged by S-K-S, S-K-Nand N-K-N interactions between adjacent [K(18-C-6)] and [Cd(mnt)_2] units.

Synthesis and Crystal Structure of Two-dimensional Network Supramolecular Complex [Cu(dafo)_2(H_2O)_2](ClO_4)_2

In an attempt to synthesize supra-molecular complex of copper(II) with mixed ligands in a solution reaction of Cu(ClO 4) 2·6H 2O with 4,5-diazafluorene-9-one (dafo) and o-phthalic acid, the bright blue column-like crystal [Cu(dafo) 2(H 2O) 2]-(ClO 4) 2 was obtained. Its structure was determined by single-crystal X-ray diffraction study. The crystal belongs to monoclinic system, space group P2(1)/n with cell dimensions: a=0.7947(3) nm, b=1.2021(5) nm, c=1.3190(5) nm, α=90.000(5)°, β=90.000(5)°, γ= 90.000(5)°, V=1.2600(9) nm 3, Z=2, F(000)=670, M r=662.83, D c=1.747 g/cm 3, μ (Mo Kα)=1.154 mm -1, R 1=0.0455, wR 2=0.1041. The analysis of the crystal structure indicates that the complex has a two-dimensional network structure which is formed by hydrogen bonds.

Synthesis, Structure and Characterization of Two-dimensional Network Copper Complex [Cu_3(nta)_2(azpy)_2(H_2O)_2]·6H_2O

The copper(Ⅱ) complex [Cu_3(nta)_2(azpy)_2(H_2O)_2]·6H_2O (nta =nitrilotriacetate, azpy = 4,4′-azobispyridine) has been synthesized and characterized. The X-rayanalysis reveals that there are two kinds of copper(Ⅱ) coordination environments. Cu(1) has adistorted square plane symmetry and Cu(2) has a distorted octahedral symmetry. Cu(1) is linked toCu(2) through nta and bound to Cu(1C) by azpy, and Cu(2) is linked to Cu(2A) through azpy, whichextends to two-dimensional network with large rhombus 1.2 nm x 1.7 nm.

Bismuth(Ⅲ) Complexes with N,N-Di(2-hydroxylethyl)amino-dithiocarboxylate: Synthesis and Crystal Structure of {Bi[S_2CN(C_2H_4OH)_2]_2[1,10-Phen]_2(NO_3)}·3H_2O and {Bi[S_2CN(C_2H_4OH)_2]_3}_2

Two novel one- and two-dimensional network structure bismuth(III) complexes with N,N-di(2-hydroxylethyl)- aminodithiocarboxylate, {Bi[S2CN(C2H4OH)2]2[1,10-Phen]2(NO3)}3H2O (1) and {Bi[S2CN(C2H4OH)2]3}2 (2) were synthesized. Their crystal and molecular structures were determined by X-ray single crystal diffraction analysis. The crystal 1 belongs to monoclinic system with space group C2/c, a=1.6431(7) nm, b=2.4323(10) nm, c=1.2646(5) nm, =126.237(5)o, Z=4, V=4.076(3) nm3, Dc=1.757 Mg/m3, =4.598 mm-1, F(000)=2156, R=0.0211, wR=0.0369. The structure shows a distorted square antiprism configuration with eight-coordination for the central Bi atom. The one-dimensional chain structure was formed by H-bonding interaction between hydroxyl group of N,N-di(2-hydroxylethyl)aminodithiocarboxylate ligands and crystal water. The crystal 2 belongs to monoclinic system with space group P2(1)/c, a=1.1149(4) nm, b=2.1274(8) nm, c=2.2107(8) nm, =98.325(8), Z=4, V=5.188(3) nm3, Dc=1.920 Mg/m3, =7.315 mm-1, F(000)=2944, R=0.0565, wR=0.0772. The structure shows a distorted square antiprism configuration with eight-coordination for the central Bi atoms. The two-dimensional network structure was formed by H-bonding interaction between adjacent molecules.