THE CRYSTAL STRUCTURE OF A NOVEL TETRANUCLEAR SILVER CLUSTER COMPLEX Ag_4(α-C_(10)H_7CS_2)_4(Py)_4·2Py

The title compound has been synthesized by the reaction of α-dithionaphthoic acidwith AgNO_3 in an organic solvent. The single crystals were obtained by recrystallizingfrom pyridine. We obtained two kinds of crystal with different colours (A and B), usingdifferent ratios of silver nitrate and α-dithionaphthoic acid (1:2,1:4) in the reactions. The structures of the two kinds of crystal were determined by a single-crystal X-raydiffraction analysis. The crystal (A) belongs to monoclinic space group C_(2h)~5-P2_1/a withunit cell parameters: a = 22.822(4) A, b = 12.803 (4) A, c = 24.444 (7) A, β = 103.90 (2)°V = 6933.14 A~3, Z = 4. The crystal (B) belongs to monoclinic space group C_(2h)~6-C2/c witha = 29.150 (2) A, b = 12.799 (3) A, c = 24.413 (2) A, β = 130.56 (4)°, V = 6914.38 A~3,Z = 4. Both crystals (A) and (B) have the same molecular configuration, but they havedifferent symmetry. In crystal (B), the molecule possesses a C_2 symmetry. This paperreports the structure determination and parameters o     

CRYSTAL AND MOLECULAR STRUCTURE OF BINUCLEAR Ni(Ⅱ) COMPLEX--CNi(OC_6H_4CHNCH_2CH_2OH) (CH_3COO) (H_2O)_2

<正> The title complex crystallizes in the monoclinic space group P21/n,with a = 9. 509(2),b=17. 614(6),c=15. 013(3)A ,β=95. 21(1)°,V = 2504. lA3,Mr = 599.91,Z = 4, Dx= 1. 59g/cm3, μ= 15. 66cm-1F (000) = 1248. The structure was solved by direct method and the final R=0. 060. The crystal consists of discrete molecules with symmetric center at the center of the four-member ring consisting of two Ni atoms and two 0 atoms.     

PREPARATION AND CRYSTAL STRUCTURES OF Ln_2(S0_4)_3(H_2O)_4 (Ln=La COMPOUND Ⅰ;Nd,COMPOUND Ⅱ)

<正> The title crystal structures have been determined by X-ray diffraction. They crystallize in the monoclinic, space group P21/n, Z=4 with diaensions a= 12.388(1), b= 7.140(1), c= 14.302(1) A,β=90.65(1)° for compound Ⅰ, and a=12.987(2), b= 7.190(1), c=13.284(2) A,β=92.40(2)° for compound Ⅱ. The structures were solved by direct methods, and refined by full matrix least-squares to consistence factors R=0.026 for Ⅰ and R=0.031 for Ⅱ.     

Chemical Conversion of a Coumarin Derivative Containing Arylhydrazono: Crystal Structures and Fluorescence Properties

An arylhydrazono-containing coumarin derivative(1) can undergo chemical conversions in two modes. When in the presence of Cu~(2+), a Cu~(2+)-promoted cyclization reaction was observed in aqueous acetonitrile and gives compound 2, while a ring-opening reaction occurs to give compound 3 in the absence of Cu~(2+). Both 2 and 3 were characterized by single-crystal X-ray diffraction. Compound 2 crystallizes in monoclinic C2/c space group with a = 26.606(5), b = 5.8142(12), c = 26.906(5) ?, β = 103.41(3)°, Z = 8, F(000) = 1696, μ = 0.186 mm~(-1), R = 0.0487 and wR = 0.1129. Compound 3 crystallizes in monoclinic P21/n space group with a = 9.917(2), b = 13.644(3), c = 15.912(3) ?, β = 95.38(3)°, Z = 4, F(000) = 896, μ = 0.182 mm~(-1), R = 0.0769 and w R = 0.1617. The spectroscopic studies show that compound 2 exhibits strong fluorescence emission.     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF A NOVEL MOLYBDENUM-SULFUR CLUSTER COMPLEX, (NH_4)_4[Mo_3(NO)_4S_(13)]·3H_2O

The title compound has been synthesized, the crystal structure of which has been detorminedby the single-crystal X-ray diffraction method. The crystal belongs to triclinic space group C-P1 with the unit cell parameters: a =9.535(2)A, b = 9.740(2)A, c = 15.795(4)A, α = 89.85(2)°, β = 91.80(2)°, γ = 99.37(1)°,ν = 1446.6A~3, Ζ = 2. The structure is refined to R = 0.075, R_w = 0.074 for 1903 reflections. There are diverse bonding modes of molybdenum and sulfur in this eompound. The twosulfur atoms at the center bond to three molybdenum atoms from respective sides and formthe two apices of a trigonal bipyramid. Besides, there are S_2~(-2) ligands and a polysulfur chaincomposed of three sulfur atoms. The coordination number for the three molybdenum atomsis seven. Their coordination polyhedra are somewhat distorted pentagonal bipyramid. Eachof the three NO ligands coordinated to molybdenum gives a linear group of Mo-N-O, whilethe fourth NO ligund bonded with a polysulfur chain forms a bent group of S-N     

Hydrothermal Syntheses and Structural Characterizations of Two ML-Containing Polyoxomolybdates:[Cu~Ⅱ_2(HL)_3]_2[Mo_8O_(26)]·(H_2O)_4 and [Ni~Ⅱ(HL)_3]_2(Mo_8O_(26))·(H_2O)_3(HL=3-(2-Pyridyl)pyrazole)

Two new polyoxomolybdate compounds,namely CuII2(HL)3]2[Mo8O26]·(H2O)4(1) and [NiII(HL)3]2(Mo8O26)·(H2O)3(2)(HL = 3-(2-pyridyl)pyrazole),were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu(II) ions linked by three 3-(2-pyridyl)pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-(2-pyridyl)pyrazole ligands.Crystal data of 1:C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850(2),b = 18.510(4),c = 17.230(3) ,β = 100.57(3)°,V = 3401.6(12) 3,Z = 4,Dc = 2.324 g/cm3,F(000) = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775(Ⅰ 2σ(Ⅰ));Crystal data for 2:C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799(2),b = 14.7970(13),c = 23.141(2) ,β = 91.6180(10)°,V = 7119.0(11) 3,Z = 4,Dc = 2.077 g/cm3,F(000) = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696(Ⅰ 2σ(Ⅰ)).     

SYNTHESIS AND STRUCTURE OF Ni_2(PBu_3~n)_2(SC_7H_6S)_2

<正> The nickel(Ⅱ) complex Ni2(PBu3n)2(tdt)2(tdt = SC7H6S2-) containing dithiolato and phosphino ligands has been prepared and characterized by X-ray diffraction. The complex crystallizes in triclinic system, space group P1, with a = 14. 423(4), b = 15. 053(3), c=10. 648(3)(?), α=93.,95(2), β=100. 31(3), γ = 84. 16(2)°; V =2259.6 (?)3; Z = 2, Dc= 1. 22 gem-3, Mr = 830. 57; μ = 11. 076cm-1, F (000) = 888. In the complex, the Nickel atoms are linked by two bridging sulfur atoms from the two tdt ligands with the Ni-Ni distance of 2. 679 (?) . and each nickel atom is four coordinated by one phosphorus and three sulfur atoms with a square-planar geometry, the average length of Ni -S bond is 2. 193(?) and that of Ni-P bond 2.186(?).     

Syntheses,Structures and Properties for Zn~Ⅱ Coordination Polymers Based on a Functional 4'-(3-Pyridyl)-3,2':6',3'-terpyridine Ligand

Two new Zn~Ⅱ coordination polymers,namely,[Zn L(o-bdc)]n(1) and [Zn L(mbdc)]_n·n H_2O(2)(L = 4?-(3-pyridyl)-3,2?:6?,3??-terpyridine,H_2(o-bdc) = benzene-1,2-dicarboxylic acid,H_2(m-bdc) = benzene-1,3-dicarboxylic acid),were synthesized by hydrothermal methods. The crystal structures have been determined by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic C2/c space group,with a = 28.016(2),b = 11.3815(11),c = 19.8071(17) ?,β = 133.961(2)°,V = 4546.2(7) ?3,Z = 8,Mr = 539.83,Dc = 1.577 Mg/m~3,μ = 1.127 mm-1,F(000) = 2208,the final R = 0.0426 and w R = 0.0986 for 2875 observed reflections with I 2σ(I) and displays a 1D coordination chain. While compound 2 crystallizes in monoclinic C2/c space group,with a = 15.6003(14),b = 11.9152(11),c = 26.633(3) ?,β = 94.320(2)°,V = 4936.5(8) ?~3,Z = 4,M_r = 1115.67,Dc = 1.496 Mg/m~3,μ = 1.043 mm~(-1),F(000) = 2272,the final R = 0.0499 and w R = 0.1342 for 2659 observed reflections with I 2σ(I) and shows a classical 3D cds topological network with point symbol of {65.8}. Furthermore,thermal stability and luminescent properties of 1 and 2 have also been investigated.     

CRYSTAL AND MOLECULAR STRUCTURE OF [K(C_(14)H_(20)O_5)_2]_2[Co(NCS)_4]

<正> The title complex (Mr= 1442.6) crystallizes in the monoclinic, space group PC, with a =14.515(7),b =15.773(5), c =16.287(11)51,β=95.13(5)°,Z=2,V=3713.8A3,Dc=1.29 g·cm-3. The structure was solved by Patterson method and the final R=0.068. The potassium atom in the cation lies between the two planes of the oxygen atoms from two benzo-15-crown-5 molecules.     

CRYSTAL STRUCTURE OF [(C_4H_9)_4N][O_2Mo~(VI)S_2Cu~Itu](tu=(NH_2)_2CS)

<正> Crystal and molecular structure of [(C4H9)4N][O2MoS2Cutu] (tu-thiourea) has been determined by X-ray diffraction technique. The crystal is monoclinic, space group P21/n, with a = 11.871(4), b=13.920(2), c= 15.814(11)A;β= 90.22(4)°,V=2613.2A3,Z = 4, DC= 1.459, Do = 1.46g/cm3. The final R and Rw are 0.049 and 0.056, respectively. The title complex has a rhombic planar MoCu(μ-S)2 core with Mo-Cu distance of 2.647A.The Ho atom is tetrahedrally coordinated by two 0 atoms and two u-S atoms. The Cu-S(tu) bond length of 2.191 A is significantly shorter than the Cu-S(bridge) in analogues.     

SYNTHESIS AND CRYSTAL STRUCTURE OF [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2

All attempts to prepare light lanthanide dicyclopeutadienyt chloride failed,due to the disproportionation reaction. The crystal complex of [(η~5-C_5H_5)_2NdCl.OC_4H_8]_2 was successfully prepared by the reaction of NdCl_3·2C_4H_8O with cyclopentadienyl sodium (molar ratio 1:1.8)in tetrahydrofuran at room temperatureThe composition of the title compound was determined by the methods of elemental analysis, infrared spectroscopy and photoelectron spectroscopy. The crystal structure of [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2 was determined from single crystal X-ray diffraction. Data were collected at-60℃ under dry nitrogen atmosphere.The complex crystallizes in the monoclinic space group P2_1/c,with Z=2. Lattice parameters are: a=8.201(3), b=21.589(6),c=8.596(3),β=109.10(3)°.The structure was solved by Patterson and Fourier techniques and refined by least-squares to a final conventional R=0.0636 for 1680 reflections. There are two Nd atoms in the dimeric unit which are bridged asymmetrically by the two chlori     

Syntheses,Crystal Structures,and Antimicrobial Activities of N′-(5-Hydroxy-2-nitrobenzylidene)-4-dimethylaminobenzohydrazide Methanol Solvate and 2-Fluoro-N′-(5-hydroxy-2-nitrobenzylidene)benzohydrazide

Two new hydrazone compounds,N'-(5-hydroxy-2-nitrobenzylidene)-4-dimethyl-aminobenzohydrazide methanol solvate (1) and 2-fluoro-N'-(5-hydroxy-2-nitrobenzylidene)benzo-hydrazide (2),have been synthesized and characterized by elemental analysis,IR spectra,1H NMR,and single-crystal X-ray diffraction.Compound 1 crystallizes in the monoclinic space group P21/c with a=11.571(3),b=12.420(3),c=12.360(2) ?,β=97.495(2)°,V=1761.1(7) 3,Z=4,R=0.0735 and wR=0.1344.Compound 2 crystallizes in the triclinic space group P with a=7.551(3),b=8.254(3),c=11.365(2) ?,α=79.352(2),β=76.154(2),γ=71.624(2)°,V=648.2(4) 3,Z=2,R=0.0393 and wR=0.1008.The hydrazone molecules of the compounds display E configurations with respect to the C=N double bonds.In the crystal structure of 1,the hydrazone molecules are linked by methanol molecules through N-H…O,O-H…N and O-H…O hydrogen bonds,forming chains running along the c axis.In the crystal structure of 2,molecules are linked through N-H…O and O-H…O hydrogen bonds,forming ribbons running along the b axis.The preliminary antimicrobial activities were studied.     

Syntheses,Characterizations and Crystal Structures of (E)-2-Methyl-1,3-diphenylisothiouronium Iodide and 1,3-Dibenzyl-2-methylisothiouronium Iodide

Two thiouronium iodide salts,(E)-2-methyl-1,3-diphenylisothiouronium iodide(1) and 1,3-dibenzyl-2-methylisothiouronium iodide(2),were synthesized and characterized by single-crystal X-ray diffraction,1H NMR,IR,UV-vis and luminescence spectra.Single-crystal X-ray diffraction reveals that compound 1 crystallizes in monoclinic system,P21/n space group with a = 11.273(2),b = 10.318(2),c = 12.962(3) ?,β = 99.03(3)°,V = 1489.0(5) ?3 and Z = 4;compound 2 crystallizes in monoclinic system,C2/c space group with a = 11.706(2),b = 14.119(3),c = 20.930(4) ?,β = 103.84(3)°,V = 3358.8(12) ?3 and Z = 8.The thiouroniums of both compounds are Y-shaped planar structures to form a cross-conjugated system.The averaged bond lengths of C-N and C-S indicate the presence of "Y" aromaticity.The researches on UV-vis and luminescence spectra of compounds 1 and 2 indicate that they can form inclusion complex with β-CD in the aqueous solution.     

CRYSTAL STRUCTURES OF COPPER (Ⅱ) AND COBALT (Ⅲ) COM- PLEXES OF o-HYDROXYBENZYLGLYCINATE (HBG)

<正> The structures of two complexes C(CuOC6H4CH2NHCH2COO)2 (H2 O)]·H2P(1) and [Co(NH3)6[Co(OC6H4CH2NHCH2COO)2]2[C1]·10H2O (2) were determined by X-ray analyses. Compound (1) crystallizes in the orthorhombic space group P212121 with a=11. 357(1),b= 24. 304(2),c=7.317(4) A,Z= 4;While compound (2) in the monoclinic space group A2/a(C2/c) with a=23. 486(9) ,b=26. 605(6) ,c= 10. 542(1) A,γ= 128. 42(4)°,Z= 4. In compound (1),two Cu(Ⅱ) ions are bonded together by the phenolic oxygen atoms of two tridentate chelating ligands and each of them is separately coordinated by the carboxyl oxygen,amino nitrogen of each chelate ligand and by the fifth oxygen atom as well (from aqua or the carbonyl group in adjacent molecule). Thus the coordination of each Cu(Ⅱ) is a square pyramid with distances of 1. 93- 1. 97A to the four corner atoms and 2. 30 and 2. 32 A to the apex atoms. The whole molecule has an approximately planar configuratioir with the two pyramid apexes pointing towards one side. Compound (2) consists of     

CRYSTAL AND MOLECULAR STRUCTURE OF GUANIDINIUM BIS (o-AMINOPHENYLARSENIC) HEXAMOLYBDATE (CN_3H_6)_4[(o NH_2C_6H_4 As)_2Mo_6O_(24)]

<正> Guanidinium bis (o - aminophenylarsenic) hexamolybdate belongs to monoclinic space group P21/c,with a=10. 217(2),b= 18. 870(2),c= 10. 939(2)A,β = 102. 82(3)°,Z = 2,V=2056. 4A3,and Dc=2. 477 g·cm-3. Each molecule contains one [(o-NH2C6H4As)2Mo6O24]4- anion and four CN3H6+ cations. In the anion,six distorted MoO6 octahedra are connected with edges-sharing to form a six-membered Mo ring which is capped above and below by two o - aminophenylarsenic groups. There is half a molecule in an asymmetric unit. It is interesting that both phenyl planes are almost perpendicular to the plane of the Mo atoms. The structure of the anion is similar to that of [ (CH3 As)2Mo6O24]4-,[(n-C3H7As)2Mo6O24]4- or [(C6H5CH2As)2Mo6O24]4-. This is the first example of this type of compounds in which the As atom is directly connected to a substituted phenyl group.     

SYNTHESIS AND STRUCTURE OF A COBALT DIMER COMPLEX (Bt_4N)_2 [Co(SOC_6H_4 )(HOSC_6H_4)]_2

<正> The title compound was obtained by reaction of CoCl2.6H2O and mp2- (σ-C6H4SO2-) in MeCN,crystallized as Et4N+ salt in monoclinic system with space group P21/c, Mr=877.040. The cell parameters are:a =16.606(2), b=15.575(1),c=17.725(2)A,β=111.07(1)°,V=4277.8A3,Z=4,Dx= 1.36g/cm3.It is a dimer of [Co(mp)(Hmp)]- connected by two strong hydrogen bonds with a twist angle of about 36.94 .     

Synthesis, Characterization, Crystal Structure and Antibacterial Activities of a Nickel(Ⅱ) Complex with 2'-(2-Thienylidene)-hydroxybenzoylhydrazide

In the ethanol solvent, a nickel(II) complex Ni(C12H10N2O2S)2 upon reaction of 2'-(2-thienylidene)-hydroxybenzoylhydrazide with nickel acetate was synthesized, and its structure was characterized by IR, UV, elemental analysis and X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with a = 22.052(3), b = 5.9681(6), c = 18.522(2) , β = 110.679(4)°, V = 2280.6(4) 3, Z = 4, Mr = 551.27, μ = 1.606 mm-1, Dc = 1.075 g/cm3, F(000) = 1136 and Rint = 0.0556. The nickel(Ⅱ ) atom in the compound is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The biological activities have been measured, show- ing the compound exhibits better anti-bacterial activity than the ligand.     

Syntheses and Structures of Two Ruthenium(Ⅲ) Complexes [Ru(PPh_3)_2(S_2CNR_2)Cl_2]·CH_2Cl_2(R=Et and ~iPr)

Oxidation reaction of [Ru(PPh3)3Cl2] with tetraethylthiuram disulfide [Et2NCS2]2 or tetra-iso-propylthiuram disulfide [iPr2NCS2]2 afforded ruthenium(Ⅲ) complexes [Ru(PPh3)2(S2CNR2) Cl2]·CH2Cl2(R=Et 1,iPr 2) which were characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P with a = 11.5065(6),b = 12.1458(7),c = 18.0034(9) ,α = 109.380(4),β = 95.279(4),γ = 97.969(4)°,V = 2324.8(2) 3 and Z = 2.Complex 2 belongs to the monoclinic system,space group P21/n with a = 12.5752(3),b = 20.7562(5),c = 17.6821(3) ,β = 105.934(1)°,V = 4437.94(17) 3 and Z = 4.Both mononuclear complexes 1 and 2 have an octahedral configuration around the central ruthenium atom which is bonded to one chelated dithiocarbamate ligand,two PPh3 ligands in mutually trans and two chlorides in mutually cis positions.The average Ru-S,Ru-P and Ru-Cl bond lengths are 2.377(2),2.412(2) and 2.369(2)  for 1,and 2.376(2),2.414(1) and 2.383(2)  for 2,respectively.The electrochemical properties of these two complexes were studied in CH2Cl2 solution by cyclic voltammetry.     

Crystal Structures,Luminescent Properties and Hirshfeld Surface Analyses of Zn(Ⅱ) and Cd(Ⅱ) Compounds Based on 1-(2-Carboxyl-phenyl)-3-(pyridin-2-yl)pyrazole

Two compounds,[Zn_2(Hcppp)_2(cppp)_2(H_2O)_2]·2 NO_3·6 H_2O(1) and [Cd(Hcppp)_2Cl_2]· 3H_2O(2)(Hcppp = 1-(2-carboxyl-phenyl)-3-(pyridin-2-yl)pyrazole),are synthesized and characterized by IR,TGA and X-ray single-crystal/powder diffraction.Compound 1 crystallizes in monoclinic system,space group P2_1/c with a = 9.894(2),b = 15.856(3),c = 20.430(4) ?,β = 101.70(3)°,V = 3138.5(11) ?~3,Z = 2,M_r = 1457.94,D_c = 1.543 g/cm~3,F(000) = 1504,R = 0.0278 and wR = 0.0749 for 6157 observed reflections(I 2σ(I)).Compound 2 crystallizes in triclinic system,space group P1 with a = 9.1424(4),b = 11.6427(5),c = 16.1345(7) ?,α = 102.6430(10)°,β = 95.4530(10)°,γ = 104.0060(10)°,V = 1605.94(12) ?~3,Z = 2,M_r = 767.88,D_c = 1.588 g/cm~3,F(000) = 776,R = 0.0307 and wR = 0.0764 for 6275 observed reflections(I 2σ(I)).Compound 1 exhibits a binuclear structure while compound 2 shows a mononuclear structure.In compound 1,two cppp-ligands display the μ_2-kN,N′:k O and two Hcppp ligands show the μ_1-kN,N′ coordination modes.However,two Hcppp ligands connect one Cd(Ⅱ) cation and exhibit the μ_1-kN,N′ binding mode in compound 2.The compounds are both studied using Hirshfeld surface analyses and 2D fingerprint plots.The luminescent properties are also discussed.     

CRYSTAL STRUCTURE INVESTIGATION OF VANADYL COMPLEXES OF TRIDENTATE LIGAND (Ⅰ)——THE CRYSTAL STRUCTURES OF BIS[(1-(2,4-PENTANE- DIONATO(NITROBENZOYL) HYDRAZONE)-2- ETHOXY)OXOVANADIUM] AND BIS-[(1-(2, 4-PENTANEDIONATO-(3-NITROBENZOYL) HYDRAZONE)-2- METHO

The title complexes were obtained by the reactions of bis(2,4-pentanedionato)oxovanadium VO(Acac)_2 and m-nitrophenylhydrazide m-NO_2PhCONHNH_2 in the media EtOH and MeOH respectively. The compound (Ⅰ) crystallizes in the space group PT with unit cell dimensions a=8.123(2), b=10.409(5), c=10.822(4), α=65.78(3)°, β=85.50(3)°,γ=89.04(3)°. The compound (Ⅱ) crystallizes in the space group P2_1/a with unit cell dimensions a=7.745(2), b=19.164(5), c=10.787(4), β=107.87(2)°. The resuhs of structural analyses show that the two compounds have the same characteristics: the tridentate ligand formed by condensation occupies three of the four equatorial positions of vanadium and the rest equatorial position is occupied by alkoxy group RO~-. As RO~-group also bridges the sixth coordinated position of each vanadium atom, it brings about the formation of the new type binuclear complexes of vanadium.