THE SYNTHESIS AND CRYSTAL STRUCTURE OF B-(32) MODEL COMPOUND: 1-C_4H_9Co(salen)(Py)

The title complex i-C_4H_9Co(salen)(Py) (Py=pyridine. salen=dianion of disalicylideneethylenediamine) has been first synthesized. Its crystal structure has been determined by X-ray diffraction method. The crystsis are monoclinic with space group P2_1/ C. The unit cell parametes are presented. The structure has been refined to a final R of 0.038.

STUDIES ON SOLID STATE REACTIONS OF COORDINATION COMPOUNDS(LXⅡ)Solid state synthesis and crystal structure of the complex ICu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)CIJ·0.5CS_2

[Cu_(0.84)Au_(0.16)(PPh_3)_2(SC(Ph)NHPh)Cl]·0.5CS_2=,Mr=895.79,monoclinic,space group P2_1/a,a=17.231(3),b=14.611(2),c=18.000(3) ,β=105.56(2)°,V=4365(1) ~3, Z=4,D_c=1.37g/cm^3.,λ(MoK_α)=0.71073 ,μ=12.15cm^(-1),F(000)=1855,R=0.052, R_W=0.045 for 3930 observed reflections with Ⅰ>1.5σ(Ⅰ).The central metal atom has a dis. torted tetrahedral geometry with bond lengths Cu-S=2.384(2) (Au-S=2.389(4)), Cu-Cl=2.481(3)(Au-Cl=2.474(1))and Cu-P=2.269(2)-2.289(2)(Au-P=2.270(4)-2.279(4)) .

Solvothermal Synthesis and Crystal Structure of Zn(en)_3B_5O_7(OH)_3

A new polyborate containing ehiral metal-complex Zn（en）3 B5O7（OH）3, where en = ethylenediamine, was synthesizedunder solvothermal conditions and structurally characterized by means of X-ray diffraction analysis. Crystal data： Zn（en）3 B5O7（OH）3, monoclinic, space group P21/c, a =0.8532（72） nm, b =2.3340（5） nm, c = 0.9526（92） nm, β =107. 04（3）°, Z=4, V=1.8140（6） nm^3, Dc =1.694 g/cm^3, p=1.416 mm^-1, F（000） = 960, GOF = 1. 020, R =0. 0276, Rw =0. 0828. There is a chiral Zn（en）3^2＋ complex cation and an isolated B5O7（OH）3^2- group in a Zn（en）3 B5O7（OH）3 molecule. The enantiomer of the chiral complex cation is separated orderly as ,4 and A configurations in the compound and the borate group consists of two B303 cycles linked through a bridging boron atom.

Hydrothermal Synthesis and Crystal Structure of a Novel Polymolybdate with Two Kinds of Organonitrogen Ligands

A novel inorganic-organic compound （C4N2H12）（C2N2H10）2[Mo5P2O23] （1） has been synthesized by the reaction of （NH4）2MoO4, H3PO4, C2N2H8 （ethylenediaminium）, C4N2H10·6H2O （piperazine hexahydrate） and water in aqueous solution under mild hydrothermal conditions. Single-crystal X-ray analysis reveals that the title compound is crystallized in the triclinic system, space group P1 with a = 9.258（19）, b = 9.382（19）, c = 17.681（4）, α = 76.28（3）, β = 84.48（3）, γ = 70.82（3）o, V = 1408.9（6）3, Mr = 1122.04, Z = 2, Dc = 2.645 g/cm3, μ = 2.384 mm-1, F（000） = 1092.0, the final R = 0.0391, wR = 0.1185 and S = 1.006 for 6169 observed reflections with I 2σ（I）. The crystal packing is stabilized by intra- and intermolecular N–H···O hydrogen bonds to form an infinite 3D network.

Synthesis, crystal structure and magnetic properties of novel copper compound Cu(phen)(m-CBA)_2

A novel compound Cu（phen）（m-CBA）2 was synthesized with m-chlorobenzoic acid（m-CBA）, 1,10-phenanthroline（phen） and Cu（OAc）2·H2O. It was characterized by IR, UV, elemental analyses and X-ray crystallography. It crystallizes in the monoclinic crystal system with C2/c space group, a=2.9699（4） nm, b=1.15452（2） nm, c=1.5335（2） nm, β=111.118（2）°, V=4.905 1（1） nm3, Z=8, F（000）=2 328, R1=0.072 8, wR2=0.223 4 [I2σ（I）]. Structure analysis shows that the copper center coordinates with two nitrogen atoms from one 1,10-phenanthroline molecule, two oxygen atoms from two m-chlorobenzoic acid molecules, giving a distorted squared planar coordination geometry. This novel compound shows paramagnetic interactions between copper centers.

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]^(2+)·[SbCl_5]^(2-)}_2

A new supramolecular compound, { [2-（2-pyridyl）benzimidazoleH2]2＋.[SBC15]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylie acid and SbCl3 in 1：1 HC1 solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetfic analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P211c, with a = 16.0397（13）, b = 14.3189（12）, c = 15.6370（13） A, β = 105.8980（10）°, V = 3454.0（5） A3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3,/z = 2.366 mm-1, S = 1.010, F（000） = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3＋ ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb...Cl. Moreover, the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-（2-pyridyl）benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Novel Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]_2·[BiCl_6]·Cl}

A novel supramolecular compound,{[2-（2-pyridyl）benzimidazoleH2]2·[BiCl6]·Cl},was synthesized by the hydrothermal reaction of o-phenylenediamine and α-pyridinecarboxylic acid with BiCl3 in 6.0 mol·L-1 HCl solution,and characterized by elemental analysis,IR,X-ray single-crystal diffraction and photoluminescence spectroscopy.The crystal （C24H22N6Cl7Bi,Mr= 851.61） belongs to the triclinic system,space group P1 with a =7.2887（18）,b =9.548（2）,c= 12.469（3）,α=85.306（4）,β=82.814（4）,γ=71.349（4）°,Z=1,V=814.9（3）3,Dc=1.735 g/cm3,μ（MoKα）=6.007 mm-1,F（000）=410,R=0.0307 and wR=0.0787.The bismuth ion and six chlorine ions construct a distorted octahedral configuration.The three-dimensional supramolecular network is built from electrostatic attractions,hydrogen bonds and π-π interaction between the BiCl6 anion,Cl anion and [2-（2-pyridyl）benzimidazoleH2] cation.The photoluminescence spectroscopy study shows that the title compound has a blue fluorescent emission at 450 nm in the solid state.

Synthesis, Crystal Structure and Quantum Chemical Study of the Ladder Organotin Compound {[(C_6H_5CH_2)2Sn]_2(O)(Cl_2)}_2

The title compound {[（C6H5CH2）2Sn]2（O）（Cl2）}2 has been synthesized by the reaction of bisbenzyltin dichloride with NaOH dilute solution, and its structure was determined by X-ray diffraction. The crystal belongs to monoclinic, space group C2/c, with a = 2.5081（17）, b = 1.0089（7）, c = 2.0909（14） nm, β = 94.267（8）°, V= 5.276（6） nm^3, Z = 4, De= 1.734 g/cm^3,μ（MoKa） = 21.55 cm^-1, F（000） = 2704, R = 0.0398 and Rw = 0.1024. According to structural analysis, the tin atom adopts a distorted five-coordinate trigonal bipyramidal geometry, and the ladder-like structure is shaped by one planar four-membered Sn2O2 ring together with two planar four-membered Sn2OCl rings.

Studies on Functionally Substituted n5-Cyclopentadienyl Transition-Metal Compounds --Synthesis and Crystal Structure of η5-CH3COC5H4W(CO)3CH2C5H5

Reaction of benzyl chloride with η5-CH3COC5H4W(CO)2Na formed in situ from η6-CH3CO C6H4Na and W(CO)2 gives η6-CH3COC6H4W(CO)3CH2C5H5.The single crystal structure of the product was determined by X-ray diffraction method. It crystallizes in the triclinlc space group P1 with unit cell parameters a= 10.199(5),b=12.116(7), c=14.207(6)A;a=69.47(5),β=72. 38(3),γ= 85.89(4);V= 1569. 9A3, Dc= 1.98 g/cm2; Z=4. Least-square refinement led to final R value of 0. 0539 and Rw value of 0. 0553, based on 3548 independent observed reflections.

Synthesis and Crystal Structure of a New Zn(Ⅱ) Coordination Polymer Constructed by 1,2,4,5-Benzenetetracarboxylate

A new Zn（Ⅱ） coordination polymer [Zn3（btec）（OH）2（H2O）2]n （1, btec = 1,2,4,5- benzenetetracarboxylate） has been synthesized by hydrothermal reaction and its structure was determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in mono- clinic, space group C2/c, with a = 19.580（3）, b = 5.0137（8）, c = 15.975（3）, β = 121.629（2）°, V = 1335.3（4）3, C10H8O12Zn3, Mr = 516.27, Z = 4, Dc = 2.568g/cm3, μ = 5.419 mm-1, F（000） = 1016, R = 0.0590 and Rw = 0.1279 for 1110 observed reflections （I 2σ（I））. X-ray analysis shows that the asymmetric unit of the title compound contains two crystallographically unique Zn（Ⅱ） atoms which are connected through the bridging carboxylate oxygen atoms of the btec ligands and μ2-bridging oxygen atoms of water molecules to generate an infinite one-dimensional chain. The adjacent chains are linked together through the benzene rings of the btec ligands to form a two-dimensional polymeric network. The adjacent two-dimensional layers are further connected together by the benzene rings of btec ligands to give the final three-dimensional structure. The benzene rings act as pillars between two layers.

Synthesis and Crystal Structure of a Salicylaldehyde Ethylene Diamine Schiff Base Manganese (Ⅲ) Complex

The title compound, [Mn(salen)(salicyl)]?.5H2O ( H2salen = N, N?ethylenebis- (salicylideneaminato), Hsalicyl = salicylaldehyde), has been obtained from the reaction system containing (o-HOC6H4CH=NCH2)2, o-HOC6H4CHO and Mn(ClO4)2?H2O in EtOH solvent and structurally characterized. It crystallizes in the monoclinic, space group P21/c with a = 13.0548(4), b = 13.9254(4), c = 11.6630(1) ? b = 105.199(2)? V = 2046.09(9) ?, Z = 4, C23H22MnN2O5.5, Mr = 469.37, Dc = 1.524 g/cm3, F(000) = 972, m = 0.687mm-1 . R = 0.0630 and wR = 0.1142 for 1901 observed reflections with I >2(I). The Mn(Ⅲ) is coordinated by N(1), N(2), O(1) and O(2) of the Schiff base ligand and phenolate O atom of salicylaldehyde with O(3)Mn distance of 2.050(4) , forming a relatively rare five-coordinate square-pyramidal structure.

Synthesis and Crystal Structure of the Perchlorate Salt of Diprotonated 2,3-Di-2-pyridyl-5-nitroquinoxaline

The diprotonated perchlorate salt of 2,3-di-2-pyridyl-5-nitroquinoxaline [C18H13N5O2](ClO4)2·(CH3OH)·(C2H5OH) has been synthesized and characterized by elemental analysis, IR and NMR spectra. X-ray diffraction analysis at room temperature indicates that the title compound (C21H23N5O12Cl2, Mr = 608.34) crystallizes in triclinic, space group P 1 with a = 7.992(8), b = 12.82(1), c = 13.42(1) A, α = 104.77(2),β = 97.84(2), r= 95.48(2)°, V= 1305(2) A3, Z = 2,DC= 1.549 g/cm3, F(000) = 628 and μ(MoKα) = 0.317 mm-1. The final R and wR factors are 0.0566 and 0.1016, respectively with 4325 independent reflections. The quinoxaline ring makes the dihedral angles of 44.2(2) and 33.9(5)° with two protonated pyridine rings whose dihedral angle is 48.1(6)°. The favored orientation of two protonated pyridine rings is that thek N atoms are opposite to each other. There exist intra- and inter-molecular N-H…O hydrogen bonds and π…π interactions which stabilize the structure further.

Synthesis and Crystal Structure of 2,2'-Dihydroxy-[1,1']binaphthalenyl-3,3'-bis-hydroxamic Acids

The first synthesis and structural characterization by X-ray crystallography of racemic 2,2＇-dihydroxy-[1,1＇]binaphthalenyl-3,3＇-bis-hydroxamic acids were reported.The com-pound（C28H30N4O8,Mr = 550.56） crystallizes in orthorhombic system,Fdd2 space group with a = 13.055（3）,b = 34.871（7）,c = 12.570（3） ,V = 5722（2） 3,Z = 8,Dc = 1.278 g/cm3,λ = 0.71073 ,μ（MoKα） = 0.095 mm-1,F（000） = 2320,S = 1.021,R = 0.0349 and wR = 0.0802 for 1757 observed reflections with I 〉 2σ（I）.The N-H and O atom are involved in two-dimensional intermolecular hydrogen bond nets,which further stabilize the structure.

Hydrothermal Synthesis and Structure Analysis of a Chromium Complex [Cr(aea)]_2(OH)_2(aea =N-(2-Aminoethyl)aspartate)

A dimeric chromium compound has been synthesized by hydrothermal method and characterized by IR, EPR spectra and TG-DTA technique. The title compound [Cr（aea）]2（OH）2 （aea = N-（2-aminoethyl）aspartate） crystallizes in monoclinic, space group P21/c with a = 8.9393（10）, b = 6.7198（7）, c = 14.6791（16） A, β = 91.0580（10）°, V= 881.63（17） A3, Z= 2, Mr = 486.34, De= 1.832 g/cm3, F（000） = 500,μ = 1.296 mm-1, R = 0.0271 and wR = 0.0756. Single-crystal X-ray structural analysis indicates that the title compound consists of two Cr（aea） units linked by two bridging hydroxyl groups. The geometry around each chromium center is approximately octahedral and completed by two hydroxyls and a quadridentate ligand which is formed when ethylenediamine reacts with maleic acid.

Synthesis and Crystal Structure of[(CH_3)_4N]_4,H_2[ZnW_(11)SnO_(39)]·9H_2O

The complex [(CH_3)_4N]_4,H_2[ZnW_(11)SnO_(39)]·9H_2O Crystallizes in themonoclinic space group P21/m with cell dimensions: a=13. 164(3) A, b=21. 502(4)A, c=13. 234(3) A, a=90, β=91. 70(3), r=90, V=3744. 3(13) A3, Z=4,Mr= 3307. 15, Dc= 2. 933 g/cm3, A (MoKa ) = 0. 71073 A, u=175. 45 cm-1,F(000) = 2956, T= 293K, R=0. 0801 for 8401 observed reflections. The anion in thetitle compound is of a-typekeggin structure.

Synthesis and Crystal Structure of[Fe_2V (μ_3-O) (μ-O_2CCH_3)_6 (THF)_3]Cl· 3H_2O

The compound [Fe2V(μ3-O) (μ-O2CCH3), (THF)3]Cl. 3H2O (THF=tetrahydrofuran) crystallizes in monoclinic system, space group C2, with cell di-mensions a= l2. 847(2), b= l5. 875 (6), c= lO. 211 (3) A, β= 109- 34 (3)', V=1965. 1(4) A3, Z= 2, D,c= 1. 73 g/cm'3 Mr= 838. 5 . F(000) = 1040, λ(MoKa) =14. 0 cm-1. The final R=0. 094, Rw= 0. O95 for 13O4 observed reflections with I≥3. 0σ (I). The result of structure analysis indicates that the framework of this com-pound is a typical trimeric oxo ccntered carboxylato compound.

Syntheses and Crystal Structures of Two Novel Spiro Compounds Containing 1,5-Dioxaspiro[5.5]undecane-2,4-dione

Two novel spiro compounds,3-benzylidene-1,5-dioxaspiro[5.5]undecane-2,4-dione 1 and 3-（2-fluorobenzylidene）-1,5-dioxaspiro[5.5]undecane-2,4-dione 2,have been synthesized and characterized by X-ray single-crystal diffraction,IR and elemental analysis.Compound 1 belongs to the monoclinic system,space group P21/n with a=12.326（3）,b=5.6420（11）,c=20.089（4）,β= 101.79（3）o,C16H16O4,Mr= 272.29,V=1367.7（5）3,Z=4,Dc=1.322g/cm3,F（000）=576,μ（MoKa）=0.095 mm-1,the final R=0.0420 and wR=0.1159.Compound 2 is of monoclinic system,space group P21/n with a=12.283（3）,b=5.6367（11）,c=20.055（4）,β=102.00（3）o,C16H15FO4,Mr=290.28,V=1358.2（5）3,Z=4,Dc=1.420 g/cm3,F（000）=608,μ（MoKa）=0.110 mm-1,the final R=0.0353 and wR=0.0860.

The Synthesis, Reaction and Crystal Structures of Ethyltetramethylcyclopentadienylruthenium Compounds

Pentamethylcyclopentadienyl-trimethylphosphine-metal compounds play an important role in the activation studies of saturated hydrocarbons. A method to synthesize ethyltetramethylruthenium compounds was established, which started from the reaction of RuCl_3. H_2O with ethyltetramethylcyclopentadiene to give a dimer compound of 2. When 2 was reacted with different amounts of trimethylphosphine, compounds 3 [C_5Me_4EtRu(PMe_3)Cl_2] and 4 [(C_5Me_4Et)Ru(PMe_3)_2Cl] were obtained. Compound 3 is a 17-electron species which is in formula similar to Bergman's Ir compound used in hydrocarbon activation reaction, but might be more reactive because of its unsaturated electron structure. The crystal structure analysis of compounds 2, 3 and 4, showed that the ruthenium atom was coordinated in a 'threeleg-piano-stool' geometry in all the three compounds. The Ru—Cl bond in 3 and 4 was lengthened, making it labile to other substitution reactions.

Syntheses and Crystal Structures of Two New Macrocyclic Compounds

Two new macrocyclic compounds, [Cu2（L）2]（ClO4）4·2CH3OH （1） and [Cu（L）]（ClO4）2·2H2O （2） （L = 1,3,10,12,15,18-hexaazatetracyclodocosane） were synthesized by condensation reactions involving amines and formaldehyde in the presence of copper anion. Compound 1 crystallizes in triclinic, space group Pí with a = 10.442（2）, b = 14.197（3）, c = 17.388（4）, α = 91.218（4）, β = 90.69（3）, γ = 93.756（4）o, V = 2520.4（9）3, Z = 2, F（000） = 1260, Dc = 1.589 Mg/m3, Mr = 1205.92, μ = 1.137 mm-1, λ = 0.71073, the final R = 0.0668 and wR = 0.1573 for 9703 observed reflections with I 2σ（I）. Compound 2 crystallizes in monoclinic, space group C2/c with a = 16.911（2）, b = 11.4172（15）, c = 27.059（4）, β = 107.787（2）o, V = 4974.7（12）3, Z = 8, F（000） = 2504, Dc = 1.610 Mg/m3, Mr = 602.92, μ = 1.155 mm-1, λ = 0.71073, the final R = 0.0419 and wR = 0.1131 for 4374 observed reflections with I 2σ（I）.

Studies on Selena-Macrocyclic Amides Synthesis and Structural Characterization of 7-Phenyl-5, 9-dioxo-1-selena-4, 7, 10-triazacyclododecane and 6-(4-Nitrobenzyl )-5, 9-dioxo-1, 4, 7, 10-selenatriazacyclododecane

7-Phenyl-5, 9-dioxo-1-selena-4, 7, 10-triazacyclododecane (1) and 6-(4-Nitrobenzyl)-5, 9-dioxo-1, 4, 7, 10-selenatriazacycloedecane (2) were synthesizedby condensation of bis (2-aminoethyl) selenide and corresponding diethyl esters. Theircrystal structures were determined. Crystal data: C14H19N3O2Se (1), Mr= 340. 28,space group P212121, a=5. 328(5), b= 14. 043(5), c= 18. 569(5) A, V= 1403(1)A3, Z= 4, Dc = 1. 610 g/cm3, μ= 3. 676 mm-1, F(000) = 696, T= 296K, R=0. 0269 for 1577 observed data. C15 H20 N4O4Se (2), Mr = 399. 31, space groupP212121, a=13. 849(5), b=4. 936(5), c=24. 942(5) A, V= 1705(1) A s, Z=4,Dc= 1. 566g/cm3, μ= 3. 230 mm-1 F(000) =816, T= 296K, R=0. 0856 for 3442observed data.