Crystal Structure and Luminescence of 1,10-Phenanthroline-tris(4-methoxybenzoato)Europium

1,10 Phenanthroline tris(4 methoxybenzoate)europium, Eu( p MOBA) 3phen(where p MOBA= p methoxybenzoate and phen=1,10 phenanthroline) has been obtained in the ethanol solution. The crystal consists of binuclear molecules of the title compound. In the binuclear molecule each Eu 3+ ion is coordinated not only by four oxygen atoms from the bridging carboxylates, but also by two oxygen atoms of a bidentate carboxyl group and two nitrogen atoms of a phen chelating ligand, giving coordination number of eight. Eu O distances range from 0 2336(3) to 0 2483(3) nm. The average Eu N distance is 0 2624(4) nm. Luminescence data indicate that one Eu 3+ ion site is in low symmetry in the complex.

Synthesis and Crystal Structure of α-( N-Protected a mino)β-lactam Derivative of 1 ,5-Benzothiazepine

The crystal of the title compound C, C 30 H 30 N 2O 3S has been prepared by reaction of 1,5 benzothiazepine with N protected glycine and determined by X ray single crystal diffraction. Crystal data: M r =498.62, triclinic with P 1 space group, a=10.880(2), b=13.955(3), c=9.537(2), α=99.34(3)°, β=110.43(3)°, γ=88 56(3)°, V=1338.2(5) 3, F(000)=528, λ (Mo Kα)=0.71073, Z=2, D c =1 237g/cm 3, μ =0.154mm -1 . Final R=0.0453, wR =0.1256 for 3491 observed reflections 〔 I>2σ(I) 〕. Structure analysis reveals that the substituents at C(23) and C(7) in four membered ring are located on the same side. The conformation of seven membered ring is chair like.

Syntheses and Crystal Structures of Pyrazoline Derivants

Two pyrazoline derivants 1-(2-benzothiazole)-3-phenyl-5-(3-thiophene)-2- pyrazoline (BPTP) and 1-(2-benzothiazole)-3-(2-thiophene)-5-phenyl-2-pyrazoline (BTPP) have been synthe- sized and their crystal structures were determined by X-ray single-crystal diffraction. Crystal of BPTP belongs to triclinic, space group P1 with a = 9.4430(11), b = 9.9384(13), c = 9.9394(13) ?, α = 83.107(10), β = 79.947(10), γ = 70.221(7)o, V = 862.42(19) ?3, Z = 2, Dc = 1.392 g/cm3, μ(MoKα) = 0.316 mm-1, F(000) = 376, λ = 0.71070 ?, (?ρ)max = 0.348, (?ρ)min = –0.481 e/?3, the final R = 0.0407 and wR = 0.1055 for 2844 observed reflections with I > 2σ(I). Crystal of BTPP is of monoclinic, space group P21/c with a = 11.6158(17), b = 11.2796(18), c = 13.082(2) ?, α = 90, β = 91.087(4), γ = 90o, V = 1713.7(5) ?3, Z = 4, Dc = 1.401 g/cm3, μ(MoKα) = 0.318 mm-1, Mr = 361.07, F(000) = 752, λ = 0.71070 ?, (?ρ)max = 0.322, (?ρ)min = –0.330 e/?3, the final R = 0.0563 and wR = 0.1058 for 3434 observed reflections with I > 2σ(I).

Synthesis and Crystal Structure of ( Z)-4-( p- Bromophenylthio)-3-( p-nitrobenzoyloxy)-3-buten-2-one

A new enone (CH 3CO C( p NO 2C 6H 4COO)=CH S C 6H 4( p Br) 5, C 17 H 12 NBrO 5S, M r =422.25) was synthesized and its crystal structure was determined by X ray diffraction method. The crystal belongs to the monoclinic system, space group P2 1/c with a=6.4121(9), b=12.804(1), c=20.998(2) , β=94.884(9)°, V=1717.1(3) 3, Z=4, D c =1.633 g/cm 3, μ (Mo Kα )=2.542 mm -1 , F( 000)=848. Final R =0.0428 and wR =0.0916 for 3335 reflections with I>2σ(I) . The title compound exists as Z isomer with p bromothiophenolate and o nitrobenzoate groups cis arranged around asymmetrical centre. This observation suggests that the substitution of thiophenolate for bromine is a stereoselective step.

Crystal Structure of RbYbI_3

The crystal structure of RbYBI 3 is determined by X ray powder diffraction method, and its crystal structure is refined by Rietveld technique Its crystal structure is orthorhombic system with a =1 0383(3) nm, b =0 4667(1) nm, c =1 7200(5) nm The space group is Pnma (62), Z =4, and all of the atoms occupy the 4 c positions of the Pnma space group Each Yb atom is coordinated by six I atoms to form a distorted octahedron The main feature of the crystal structure of RbYbI 3 is two chains along the b axis which are composed of the edge sharing octahedra

Synthesis and Crystal Structure of Quaternary Mixed Anion Complexes of Lanthanide Containing 1,10-Phenanthroline

A series of novel quaternary mixed anion complexes of lanthanide containing 1,10 phenanthroline(phen) were synthesized from the water/ethanol solution with slightly acidic solution and characterized by elemental analysis, IR and UV spectra, thermal analysis and single crystal X ray diffraction analysis. The crystal of [Ce(CH 3COO) 2(NO 3)(phen)] 2 belongs to monoclinic system, lattice type C centered, space group C 2/m, a =1 5444(6) nm, b =1 2273(5) nm, c =1 2776(5) nm, β =131 89(2)°, V =1 802(1) nm 3, Z =2, R =0 024, R w =0 032.

Synthesis and Crystal Structure of an Erbium Complex with Valine [Er_2(Val)_4(H_2O)_8](ClO_4)_6·4H_2O

The title complex was synthesized in aqueous solution, and its crystal structure was determined by X ray diffraction. The crystal is triclinic space group P 1 with a =1 00935(9) nm, b =1 20190(2) nm, c =1 28432(8) nm, α =95 013(9)°, β =102 814(5)°, γ =113 368(9)°, V =1 3676(3) nm 3, Z =1, D c=1 962 g/cm 3. The complex is a dimeric molecule with four bridging carboxyl groups from four valine molecules between two erbium ions. Each erbium ion is coordinated by four oxygen atoms from four carboxyl groups and four oxygen atoms of four water molecules with the coordination number 8, taking a square antiprism arrangement.

Synthesis and Crystal Structure of [Er(OH_2)_8](ClO_4)·3·5(1,4Diox.)·2H_2O

The title complex was synthesized in aqueous solution, and its crystal structure was determined by X ray diffraction. The crystal is monoclinic, space group P2 1/n with a =1 1243(3) nm, b =2 4853(2) nm, c =1 2962(1) nm, β =95 08(1)°, V =3 608(1) nm 3, Z =4, D c=1 757 g/cm 3. Each of the erbium ion is coordinated by eight water molecules. The complex is of polymeric structure with the octaaqua erbium complex species connected by 1,4 dioxane moieties through hydrogen bonds.

Crystal Structure and X-ray Powder Diffraction Data for Rare Earth Compound PrNiSn

The compound PrNiSn was studied by X ray powder diffraction technique. The crystal structure and the X ray diffraction data for this compound at room temperature were reported. The compound PrNiSn is orthorhombic with lattice parameters a =0.74569(3) nm, b =0.76851(5) nm, c =0.45676(8) nm, V =0.26176 nm 3, Z =4 and D x=8.076 g·cm -3 , space group Pna2 1(33). The figure of merit F N for the compound is F 30 =54 (0.0093, 60).

Synthesis and Crystal Structure of 10-Phenyl-1,7-dithia-4-oxa-10-aza-12-crown-4

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Synthesis and Crystal Structure of〔( PPh_3)( CH_3 COS) _2 NiB_(10) H_(10)〕·0 .4( C_5 H_(12))

The title compound 〔(PPh 3)(CH 3COS) 2NiB 10 H 10 〕·0.4(C 5H 12 ) has been synthesized by the reaction of 〔NiCl 2(PPh 3) 2〕, closo 〔B 10 H 10 〕 2- and CH 3COSH in CH 2Cl 2 solution. It was recrystallized from n pentane/CH 2Cl 2 solution and its structure was determined by X ray diffraction analysis. The crystal is triclinic, space group P1, M r= 618.23, with a=10.049(1), b=12.638(2), c=14.077(2) , α=110.13(1), β=87.65(1), γ=96.01(1)°, V=1669.3(4) 3, D c =1.230 g/cm 3, Z=2, λ (Mo Kα )=0.71073 , μ =7.76 cm -1 , F (000)=642. The final refinement is converged with R =0.042 (5986 observed reflections with I≥2σ(I)), wR 2 =0.151. The cluster is a nido eleven vertex {NiB 10 } cage with the Ni atom in the open NiB 4 face. Cyclizations resulting in two five membered rings, Ni(7)-S(1)-C(1)-O(1)-B(2) and Ni(7)-S(2)-C(2)-O(2)-B(3), have occurred.

Crystal Structure of 2-〔(P,P-Diphenoxy)phosphono(p-methyl)benzyl〕-1,2-benzisoselenazol-3(2H)-one

The crystal structure of the title compound 2 (P, P Diphenoxy)phosphono( p methyl)benzyl 1, 2 benzisoselenazol 3 (2H) one, C 27 H 22 NO 4PSe, was determined by single crystal X ray diffraction. It crystallizes in the triclinic system, space group P1 (No. 2) with M r=534.41, a=9.761(2), b=10.304(2), c=13.396(3) , α=110.97(3), β=107.70(3). γ=90.02(3)°, V=1190(1) 3, Z=2, D x =1.492 g/cm 3 , λ=0.71073 , μ =1.6596 mm 1 and F(000)=544. The structure was solved by direct methods. The final R factor is 0.068 and R w is 0.074 for 2500 unique observed reflections I≥3σ(I) . The results presented herein indicate that the selenium containing bicyclic moiety is a coplanar structure and that two adjacent molecules are symmetrically linked to each other forming a dimer through the Se(1c)…O=P(1) bonding interaction with an intermolecular Se(1c)…O distance of 2.797 .

The Crystal Structure of Biphenyltetracarboxylic Dianhydride Isomers

Biphenyltetracarboxylic dianhydride (2,2',3,3' BPDA), C 16 H 6O 6, M r =294.21, monoclinic, P2 1/c, a=11.694(2), b=8.111(2), c=13 494(3) , β=103.47(3)°, V=1244.7(4) 3, Z=4, D c =1.570 g/cm 3 , F (000)=450, Mo Kα radiation( λ =0.71073), μ (Mo Kα )=0.092 mm -1 , R =0.0329 for 2180 observed reflections 〔 I>2σ(I) 〕. 3,3',4,4' Biphenyltetracarboxylic dianhydride (3,3',4,4' BPDA), C 16 H 6O 6, M r =294.21, monoclinic, P2 1/n, a=6.8720(14), b=5.1870(10), c=17.288(4), β=94.96(3)°, V= 613.9(2) 3, Z=2, D c =1 592 gcm -3 , F(000)=300 , μ (Mo Kα )=0.125mm -1 , R =0.0331 for 1079 observed reflections〔 I>2σ(I) 〕. The dianhydride isomers have different symmetry caused by alternating two anhydride group positions and the dihedral angle between the two phenyl rings are 62.9°for 2,2',3,3', BPDA and 0°for 3,3',4,4' BPDA respectively.

Hydrothermal Synthesis and Crystal Structure of a Keggin Polyoxometalate [Co^Ⅱ（2,2′-bipy）2（H2O）]2[SiW^Ⅵ12O40]·2H2O

A Keggin-type tungstosilicate compound [Co^Ⅱ（2,2′-bipy）2（H2O）]2[SiW^Ⅵ12O40]·2H2O 1 （bipy = bipyridine） was prepared by a hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 （C40H40Co2N8O44SiW12） crystallizes in the triclinic system, space group P1 with a = 10.4979（6）, b = 13.3946（7）, c = 13.5756（8）A, α= 70.0769（18）, β = 68.910（3）, γ = 74.186（4）°, V = 1649.84（16）A^3, Mr = 3688.95, Z = 1, Dc = 3.713 mg·m^-3, μ = 21.432 mm^-1, F（000） = 1644, S = 1.058, the final R = 0.0511 and wR =0.1023 for 6523 observed reflections （I 〉 2σ（I））. Compound 1 consists of two coordinated cation fragments [Co^Ⅱ（2,2′-bipy）2（H2O）]^2＋, one normal Keggin polyanion unit [SiW^Ⅵ12O40]^4- and two lattice water molecules. To be noted, each polyanion unit is linked to two cation fragments by its two surface terminal oxygen atoms and two cobalt atoms of two cation fragments forming an organic-inorganic hybrid unit in 1. Furthermore, the compound shows strong photoluminescence property in the solid state at room temperature.

Crystal Structure of cis-2-〔(P,P-Diethoxy)phosphono(m-nitro)benzyloxy〕-4-Phenyl-5,5-Dimethyl-1,3,2-Dioxaphosphorinane 2-Sulfide

The crystal structure of the title compound cis 2 (P, P Diethoxy)phosphono( m nitro)benzyloxy 4 Phenyl 5,5 Dimethyl 1,3,2 Dioxaphosphorinane 2 Sulfide, C 22 H 29 NO 8P 2S, was determined by single crystal X ray diffraction. It crystallizes in the monoclinic system, space group P2 1/c, with M r=529.49, a=9.888(2), b=20.831(4), c=12.797(3) , β=94.42(3)°, V=2628(1) 3, Z=4, D x =1.338 g/cm 3 , λ=0.71073 , μ =0.2796 mm 1 and F(000) =556. The structure was solved by direct methods. The final R factor is 0.052 and R w is 0.057 for 1793 unique observed reflections I≥3σ(I) . A cis configuration and a preferred chair conformation for the molecule have been established by X ray diffraction analysis. The results presented also give a good explanation to the correlation between the configurational assignments and the regularity in the chemical shifts of C 4-H and 31 P NMR.

Synthesis and Crystal Structure of ｛( P Ph_3)_2 Cl Ru( μ- Cl) Ru( P Ph_3) B_(10)H_7〔 O C H( C H_3)_2〕_3｝·0 .4( H_2O)

The title compound has been synthesized by the reaction of 〔RuCl 2(PPh 3) 3〕 and closo 〔B 10 H 10 〕 2- in (CH 3) 2CHOH solution. Crystals suitable for a single crystal X ray diffraction analysis were obtained from n pentane diffused to CH 2Cl 2 solution. The crystal {(PPh 3) 2ClRu( μ Cl)Ru(PPh 3)B 10 H 7〔OCH(CH 3) 2〕 3}·0.4(H 2O) is monoclinic , space group P2 1/n , M r= 1359.47, with a=19.434(4), b =14.340(4), c=25.865(9) , β= 95.48(3)°, V=7175(4) 3, D c =1.258 g/cm 3, Z=4, λ (Mo Kα )=0.71073, μ=6.03 cm -1 , F(000)=2784, R=0.0631, wR 2 = 0.1425, S =1.001. The title compound is a bimetallic species in which the second ruthenium center is bound to the cluster {(PPh 3)RuB 10 H 7〔OCH(CH 3) 2〕 3} via an Ru-Cl-Ru and two Ru-H-B-Ru bridges. The third isoproxy group replaces a hydrogen atom on B(10) of the cage, which indicates the activity of the cage.

Molecular and Crystal Structure of Cinnam ylidene Acetophenone

The title compound C 17 H 14 O, M r =234.30, is orthorhombic, space group Pbca with unit cell of a=16.410 (2), b=15.451(2), c=10.261(2); Z=8, D c =1.196 g/cm 3; V=2601(1) 3; λ (Mo Kα)=0.71069, μ (Mo Kα ) =0.73 cm -1 , F (000)=992, final R=0.048, R w =0.053 for 1121 observed reflections with I>3.00σ(I ). As the two phenyl planes and the C 4H 4CO group are non coplanar ,the molecular conjugated system was disturbed.

Synthesis and Crystal Structure ofα-Mo_4 X S_3( μ-dtp)_3(dtp)_3( X= 0 .6S + 0 .4O)

The title compound (Mo 4XS 15 P 6O 12 C 24 H 30 ), α Mo 4XS 3( μ dtp) 3(dtp) 3 (X=0.6S+0.4O; dtp= -S 2P〔OEt〕 2), isolated as a prismatic black crystal, was prepared from ethanolic solution of Mo(CO) 6, MoCl 5 and P 2S 5. It crystallizes in triclinic system, space group P1 with a=14.031(4), b=13.372(2), c=16.270(8), α=92.15(2), β = 72.91(3), γ = 95.20(2)°, V = 2905.4(2) 3, Z = 2, D c = 1.82 g/cm 3, M r=1598.93, F(000)=1564.8, λ =0.71069 (Mo Kα ), μ =1.584 mm -1 . The final R=0.058, R w =0.057 for 5016 observed reflections with I≥3.0σ(I ). The structure analysis reveals that the title compound has a 〔Mo 4XS 3〕 core, belonging to the cubane type tetranuclear molybdenum clusters family, with one of its four μ 3 caps being statistically occupied by S and O. Three dtp ligands chelated three μ X capped Mo atoms as terminal ligands, while another three dtp bridged these three Mo atoms and the fourth one, forming an α type cluster compound.

Synthesis and Crystal Structure of Binuclear Complex of Copper(Ⅱ)Chloroacetate with Acetamine

The title complex, Cu 2(O 2CCH 2Cl) 4 OC(NH 2)CH 3 2, crystallizes in space group P2 1/a with a=7.616(4), b=18.665(5), c=7.949(5) , β=106.29(5)°. V=1084(1) 3, Z=2, M r=619.19, D c =1.896 g/cm 3; μ =25.05 cm -1 and F(000)=620.00, R =0.045 and R w =0.054 for 1807 observable reflections. X ray crystal structure analysis revealed that two Cu atoms are bridged by four chloroacetate groups, and the acetamine ligands are bonded by O(carboxide) to the terminal Cu atoms of each dimeric unit. The coordination geometry of Cu atom is a distorted octahedral configuration. The distance between the two Cu atoms is 2.648(1) .

Chiral Phosphine Ligands Derived fro m Sugars .14 . Crystal Structure of Diphenyl( m ethyl4’,6’-O-benzylidene-3’-deoxy-α- D-altropyranoside-3-)phosphine Oxide

The crystal structure of the title compound, C 26 H 27 O 6P, has been determined by single crystal X ray diffraction analysis. The crystal is orthorhombic with space group P2 12 12 1, a=6.154(4), b=17.199(8), c=22.180(3) , V=2347.6 3, D c=1.32 g/cm 3, F(000)=984, μ=1.5 cm -1 , Z =4, and final R =0.075 and R w =0.080 for 1417 reflections (I≥3σ(I)) . The X ray diffraction analysis revealed that the structure of the title compound s similar to that of its parent phosphine and the pyranose and 4, 6 O benzylidene rings remain distorted chair conformations.