Synthesis and Crystal Structure of a Binuclear Cobalt(Ⅱ)Carboxylate Complex Co2(O2CCMe3)4(C9H7N)2

Reaction of cobalt carbonate, pivalic acid and quinoline in a refluxing ethanol solvent yielded the dicobalt(Ⅱ) compound, Co2(O2CCMe3)4(C9H7N)2 (1) (C9H7N is quinoline), which has been characterised by elemental analysis, IR and X-ray diffraction method. Crystallographic data: monoclinic, P21/a, a=9.341(2), b=18.591(4), c=11.822(2)(), β=97.71(2), V=2034(1)()3, Z=2, Mr=918.19, Dc=1.27 g/cm-3, F(000)=820, μ(MoKα)=8.60 cm-1, T=293K, final R=0.049, Rw=0.060 for 2715 observed reflections with I>3.0 σ(I). The centrosymmetric molecule comprises a pair of cobalt(Ⅱ) atoms connected by four pivalate ligands in syn-syn bridging modes. Square pyramidal five-coordination of cobalt(Ⅱ) is further completed by a quimoline molecule. The CoⅡ-CoⅡ distance is 2.784(1)().     

SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [CrMo_3 (μ_3-O)_3(μ-O)(μ-O_2CCH_3)_5(O_2CCH_3)_3]Na2 · H_2O

<正> The title complex C CrMo3 (μ3-O )3 (μ-O) (μ-O2CCH3 )5 (O2CCH3)3]2Na2 · H2O (Mr=1814. 32) crystallizes in monoclinic, space group P21/ n with a=11.209(5), b=18. 05(1), c=14. 44(1) A , β= 98. 30(5)°. V=2890 (3) A3, Z=2, A = 2. 08 g/cm3, F(000) -1780, Final R = 0. 049, Rw = 0. 058 for 2622 independent reflectons with I>3σ(I). The complex anion contains two Mo3O4 cores which connect two chromium atoms through four μ3-O atoms and eight bridging CH3COO- groups. Each of the Cr atoms and the Mo atoms is coordinated by six oxygen atoms. The anions are linked by Na cations to form one-dimensional infinite chain structure.     

Synthesis, Characterization and Crystal Structure of [Co2Mo2(μ4-C2HPh)(μ-CO)4(CO)4(η5-C5H4C(O)Me)2]

The reaction of μ-alkyne-bridged dimolybdenum compound [Mo2(μ-C2HPh)(CO)4(η5-C5H4C(O)Me)2] 1 with Co2(CO)8 in refluxing toluene gave a new butterfly compound [Co2Mo2(μ4-C2HPh)(μ-CO)4(CO)4(η5-C5H4C(O)Me)2] 2 which was fully characterized by elemental analysis, IR, 1H NMR and X-ray single crystal diffraction techniques. 2 crystallized in monoclinic system, C30H20Co2Mo2O10, Mr=850.23, space group P21/a(#14), a=14.165(5), b=12.498(2), c=16.204(2)(A), β = 96.50(2)°, V = 2850(1)(A)3, Z = 4, Dc = 1.981 g cm-3, F(000)=1672, μ(MoKα)=20.41 cm-1, final R=0.030, Rw=0.039 for 4831 observable reflections with I>2σ(I). The structure contains a Co2Mo2 butterfly core, and each Mo-Co bond is spanned by an asymmetric semi-bridging carbonyl ligand.     

Synthesis and Crystal Structure of[Co3(CO)9(μ3-C)C(O)OCH2]2

The title compound [Co3(CO)9(μ3-C)C(O)OCH2]2 was synthesized by the reaction of [Cl3CC(O)OCH2]2 with Co2(CO)8 at 40～50 ℃. Crystal data: C24H4O22Co6, Mr=997.88, monoclinic, space group P21/n(#14), a=9.330(2), b=15.197(4), c=11.783(4), β=91.16(2)°, V=1670.4(7) 3, Z=2, Dc=1.984 g/cm3, μ(MoKα)=30.01 cm-1, F(000)=972.00, T=293K, final R=0.045, Rw=0.051 for 1936 observed reflections with I＞2σ(I). The structure contains two centrosymmetric dimeric molecules in a unit cell, each of which has two tetrahedral skeletons (CCo3) connected through a C(O)OCH3CH2OC(O) bridge.     

CRYSTAL AND MOLECULAR STRUCTURE OF TETRANUCLEAR MOLYBDENUM CLUSTER Mo_4(μ_3-O)_2Cl_2(o-CH_3C_6H_4COO)_6

<正> Cluster compound [Mo4(μ3-O)2O4Cl2(o-CH3C6H4COO)6] has been prepared by the reaction of molybdenum pentachloride and o-methylbenzoic acid. It crystllizes in the orthorhombic space group Praia with cell parameters:Mr= 1361. 6,a=13. 792(4), b=17. 957(3),c= 20. 974(9) A ,V=5194(2) A3,Z= 4,Dc= 1. 74g/cm3,F(000) = 2704,μ(MoKa) = 11. 0/cm. The final R=0. 061 and Rw=0. 064 for 1441(I>3oooooooooo(I)) observed unique reflections. The tetranuclear complex molecule, where the molybdenum atoms are bridged by two μ3-O atoms and six bidentate o-methylbenzoato ligands,is located at crystallographic two-fold axis(x,-1/4,1/4) with one Mo-Mo bond of 2. 610A     

THE CRYSTAL STRUCTURE OF BIS(TETRAETHYLAMMONIUM)(μ-OXO)BIS[TRIPHENYL-THIOLATO-IRON(Ⅲ)],(Et_4N)_2[Fe_2O(SPh)_6]

<正> Fe_2OSsN_2C_(52)H_(70),Mr=1043.23,monoclinic, P21/a, a=18.121(3), b=15.249(3), c=20.369(4)A,β=102.49(8)°,V=5495(1)A3, Z=4, Dc=1.261g.cm-3,MoKα(λ =0.710691), μ=17.816mm-1, F(000)=2208. R=0.073 for 4374 observed reflections with I≥3.0σ(I). The structure of the anion contains a linear Fe-O-Fe unit, with mean Fe-O distance of 1.766(2)A. The coordination geometry about each iron atom is close to tetrahedral with the angles O-Fe-S and S-Fe-S being 115.3° and 103.1°, respectively.     

Synthesis and Crystal Structure of [{Cd(hmbdc)(H2O)3}·2H2O]n

A novel coordination polymer [{Cd(hmbdc)(H2O)3}·2H2O]n (hmbdc=5-hydroxy- isophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a=9.599(3), b=18.699(5), c=7.557(2) (A), β= 108.198(4)°, V=1288.6(6) (A)3, Z=4, Mr=382.60, Dc=1.972 g/cm3, F(000)=760, μ=1.740, the final R=0.0555 and wR=0.0995 for 1732 observed reflections with Ⅰ ＞ 2σ(Ⅰ). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.     

Reaction of Mo(CO)6 with Alkoxide: Synthesis and Structure of the Mo(0)-OR Complex [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2C6H5)3]

The reaction of molybdenum hexacarbonyl with C6H5CH2OC6H4ONa and Et4NBr in CH3CN at 60 ℃ afforded the di-nuclear Mo(0) compound [Et4N]3[Mo2(CO)6(μ-OC6H4OCH2- C6H5)3] 1. 1 crystallizes in monoclinic, space group P21/c with a=15.359(2), b=18.378(3), c=24.952(2)(A), β=102.268(4)°, V=6882.3(16) (A)3, Mr=1348.34, Z=4, Dc=1.301 g/cm3, F(000)=2832 and μ= 0.424 mm-1. The final R=0.0606 and wR=0.1552 for 9396 observed reflections (Ⅰ ＞ 2σ(Ⅰ)). 1 contains a [Mo2O3]3- core in triangular bi-pyramidal configuration and each Mo atom adopts a distorted octahedral geometry with three carbon atoms from carbonyls and three μ-O atoms from C6H5CH2OC6H4O- bridging ligands. The Mo…Mo distance is 3.30(8) (A), indicating no metalmetal bonding. A formation pathway via forming a di-molybdenum(0) di-bridging OR compound [Mo2(μ-OR)2(CO)8]2- has been figured out and the reaction of Mo(CO)6 with alkoxide has also been discussed.     

Crystal Structure of [CH_3CH(OH)COO]_2Fe(H_2O)_2·H_2O

<正> The title compound C6H16O9Fe, Mr = 288. 13, was synthesized and crystallized in monoclinic space group P21/c, a = 9. 409(4), b = 5. 812(4), c= 22. 122(7)(?) , β=90. 80(3)°. V = 1209. 6(?)3, Z = 4, Dc=1. 572g/cm3, F(000) = 592, μ = 12. 73cm-1, R = 0. 063, Rw= 0. 068 for 1191 observed reflections. The iron atom is surrounded by O(1 - 6) in a distorted octahedron.     

CRYSTAL STRUCTURE OF (C_5H_9C_5H_4)_3Er_4(μ_2-Cl)_6(μ_3-Cl)(μ_4-O)-(THF)_3

<正> The crystal of (C5H9C5H4)Er4(μ2-Cl)6(μ3-Cl)(μ4-O)(THF)3 belongs to triclinic space group P1, with a = 11. 909(4), b = 15.343(5), c=15. 619 (4)(?), α=104. 18(2), β=98. 81(3), γ= 111. 06(2)°, V = 2486(1)(?)3, Z = 2, Dc = 2. 07g/cm3, λ(MoKα) = 0.71073(?), μ= 73. 4cm-1, F(000) = 1476, Mr=1549. 25. The structure was solved by Patterson and Fourier techniques and refined by block diagonel least-squares method to final R = 0. 078 and Rw = 0. 084 for 5594 reflections with I≥1. 5σ(I). The results revealed that the complex is composed of four Er atoms bridged by seven Cl and one oxygen atoms with three of the Er atoms bonded each to a cyclopentylcyclopentadienyl group, and one Er atom, bonded to three THF. The Er atoms constitute a pseudo-tetrahedron.     

Crystal Structure of [PrAl（CF3COO）2（CF3CHOO）（C2H5）2（C4H8O）2]2

[PrAl(CF3COO)2(CF3CHOO)(C2H5)2(C4H8O)2]2 Mr=1420.56, monoclinic, P21/n, a=10.651(6), b=24.276(9), c=11.110(5)(), β=107.650(4)°, V=2737.4(1)()3, Z=2, Dc=3.45 g/cm3, F(000)=2816, T=233K, MoKα radiation (λ=0.71069()), μ(MoKα)=38.017 cm-1, R=0.048 for 2847 observed reflections (I≥3σ(I)). It is isostructural with [LnAl(CF3COO)2(CF3CHOO)-R2(C4H8O)2]2 (Ln=Ho, R=Et; Ln=Nd, Y, R=iBu). Pr3+ is coordinated by eight oxygen atoms from five bridging ligands and two THF forming a distorted bicap-prism.     

CRYSTAL AND MOLECULAR STRUCTURE OF (μ-PhS) (μ-σ,π-CH_3CH = CH)Fe_2(CO)_6

<正> The crystal and molecular structure of (μ-PhS) (μ-σ, n-CH3CH = CH)-Fe2(CO)6 has been determined by X - ray diffraction technique. The complex has chemical formula of C15H10O6SFe2 and Mr=129. 99. The crystals are monoclinic,space group P21/c,with α=11. 789(2),b= 7. 159(1),c = 20. 890(4) A ;β = 100. 89(2);V = 1731. 32 A3;Z=4,Dc=1. 65g·cm-3;F(000) = 863. 86. The final R and Rw equal 0. 0315 and 0. 0405 respectively for 2527 observed unique reflections.     

A Three—dimensional Network Topology in [Mn（N3）2（4,4‘—bipy）]n,Generat

Compound [Mn(N3)2(4, 4'-bipy)]n having three-dimensional structure was obtained with crystallographic data: C10H8N8Mn (Mr=295.16), tetragonal, space group P412121(#99), a=8.220(2), c=16.918(5)(), V=1143.1(5)()3, Z=4, Dc=1.715 g/cm-3, μ=11.07 cm-1, F(000)=596, R=0.042, Rw=0.051, for 590 observable reflections. The special topology structure in the compound occurs from the helical chain consisting of the -Mn-N-N-N-Mn'-unit. The value of χmT decreases with the decreasing of temperature     

Synthesis, Crystal Structure, and Photoluminescent and Semiconductive Properties of [La(C6NO2H5)3-(H2O)2]2n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O)

A new heterometallic 4f-5d inorganic-organic metal-isonicotinic acid complex [La(C6NO2H5)3(H2O)2]2n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydro-thermal reaction and structurally characterized. Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell: α= 24.140(7), b = 20.884(7), c = 15.462(2) (A), β = 127.46(1)°,V = 6187(3) (A)3, C36H47Cl13Hg3La2N6O20, Mr = 2224.24, Dc = 2.388 g/cm3, Z = 4, T = 293(2) K, μ(MoKα) = 9.401 mm-1, F(000) = 4160 and R/wR = 0.0376/0.0636 for 4130 observed reflections (I > 2σ(I)) and 5617 unique reflections. Complex 1 is characteristic of a one-dimensional polycationic chain-like structure. Photoluminescent investigation reveals that the title complex displays interesting emissions in violet and orange regions. The luminescence spectra show stronger orange emission than violet emission. Optical absorption spectra of 1 reveal the presence of a wide optical bandgap of 3.41 eV.     

THE SYNTHESIS AND STRUCTURE OF Mo_3(μ_3-O)(μ-S)_3(μ-O_2CC_6H_5)_2(dtp)_2(Py)

<正> The title compound was prepared by reaction of Mo3(μ3-O) (μ-S)3-(dtp)4 (H2O) with C6H5COONa and pyridine. C27 H35 Mo3NO9P2S7, Mr = 1091.76, monoclinic, space group P21/c, a = 15. 057(5), b = 13. 052(5), c = 21. 662(6)(?), β=105.97(2)°, V = 4093(2) (?)3, Z = 4, Dc= 1. 77gcm-3, F(000) = 2176, μ(MoKα)=13.50cm-1, final R =0. 068 for 2835 observations. The molecular configuration is new and of approximate C, symmetry, and there are two C6H5COO bridging groups in the structure. The three Mo atoms form an isosceles triangle with three sides of 2. 567(3), 2. 576(3), and 2. 649(3)(?), where the two Mo-Mo bonds bridged by C6H5COO group are much shorter than that without. Something about the reactivity of Mo clusters is discussed.     

Synthesis and Characterization of Tetrametal Cluster [Co2(CO)6][μ-HC2CH2OCH2C2H-μ][Co2(CO)6]

The treatment of dipropargyl ether HC2CH2OCH2C2H with Co2(CO)8 resulted in the formation of a novel cluster [Co2(CO)6][μ-HC2CH2OCH2C2H-μ][Co2(CO)6]. The cluster was characterized by C/H analyses, IR and 1H NMR spectroscopy and X-ray crystal structure determination. It belongs to monoclinic system, space group P21/c with the following crystallographic parameters: a=18.149(2), b=7.0111(7), c=20.897(2)(A), β=115.318(7)°, V=2403.7(5)(A)3, Z=4, Mr=665.97, Dc=1.840 g·cm-3, F(000)=1304.00, μ(Mo-Kα)=27.76 cm-1 and R=0.030 for 2372 observed reflections.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A TUNGSTEN-COPPER-SULFUR CLUSTER [Et_4N]_2[WCU_3S_4(S_2CNEt_2)_3]

<正> [Et4N]2 [WCu3S4 (S2CNEt2)3], Mr = 1172. 01, orthorhombic, space group P212121 with a=12. 858(9),b=13. 204(5) ,c=29. 501(9) A ,V=5008. 7 A3, Z = 4, Dc = 1. 55gcm-3, μ(MoKa) = 40. 3cm-1. The final R and Rw are 0. 069 and 0. 075, respectively, for 3072 observed unique reflections. The anion contains a slightly distorted WS42~ tetrahedron coordinated by three CuS2 CNEt2 units,with four metal atoms lying in a plane.     

STRUCTURE OF TRISUBSTITUTED TUNGSTOSILICATE ANION [A-β-SiW_9Al_3(H_2O)_2O_36(μ_3-O2/2)]_2~14-

<正> Crystal of H14C[A-β-SiW9Al3(H2O)2O36(μ3-O2/2)]2 ·8H2O belongs to monoclinic system, space group P2/m. with a= 1 7. 525(6), b=14.348(3). c= 21. 669(8) A , β=113. 12(8)°, V = 5011 (3) A3,Z = 2. Dc = 3. 254 g. cm-3, A (MoKα) = 0. 70169 A , μ=223. 21 cm-1, F(000) = 4614, T = 298K. R=0. 066 for 3010 unique reflections [I≥5σ(I) ]. The crystal consists of water molecules, protons (or H3O+ ) and dimeric anions [A-β-SiW9Al3 (H2O)2O36(μ3-O2/2)D214.the half of which has a SiO1 tetrahedron in the center, a W3O13 group, two W2Al(H2O) O12 groups and a W2AlO13 group around the SiO4.     

CRYSTAL STRUCTURE OF Mo_3(μ_3-O) (μ-S_2)_ 3 [S_2P(OEt)_2]_3I

<正> Mr=1178.9, monoclinic, P21/n, a=16.570(2), b=12.370(1), c=20.007(2) A,β=99.97(1)°, V=4039.0A3, Z=4, Dx=1.938 Mgm-3, λ(MoKα)=0.7107A, μ(MoKα)=23.96 F(000)=2296, room temperature. Final R value=0.047 for 4387 unique observed reflections. It consists of neutral mono-oxo-capped trinuclear molybdenum cluster molecules with an average Mo-Mo bond length of 2.626(4)A and an average Mo-0 bond length of 2.036(2)8.     

CRYSTAL STRUCTURE OF (Et_4N)_2[Mo_6O(μ-O)_(12)O_5]

<正> Mr= 1140.4, tetragonal,P4/mnc,a=10.726(2), c=14.208(3)A, Z=2,Dc=2.316 g.cm-3,V=1634.5(9)A3,final R=0.050 for 1457 independent reflections. The anion [Mo6O19]2- has its No atoas in octahedral configuration with one oxygen atom situated in the center of the octahedron, twelve bridging oxygen atoms,and six terminal oxygen atoms. The average bond lengths of the three types of Mo-O bonds are 1.678 A (Mo=0), 1.919A [Mo-(μ-O)], and 2.310 A [Mo-(μs-O)], respectively.