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Growth and Characterization of γ-Nd^(3+): LaSc_3(BO_3)_4 Crystal

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Chinese Journal of struct.ral Chemistry 2001年第4期20卷 256-258页

作者：林洲斌王国富等 Fujian inst. res. struct. of matter Chinese Academy of Sciences Fuzhou Fujian 350002 China

A new laser crystal Nd0.05La0.95Sc3(BO3)4 up to 50mm(38mm(7 mm was grown by top-seeded solution growth method from a Li6B4O9 flux. The grown crystal was characterized by X-ray powder diffraction. Its crystal struct.re is monoclinic with space group Cc and the unit cell dimensions: a=12.066(5), b=9.864(2), c=7.740(3) ?,β= 105.48(5)(, V=887.8(6)?3, Z=4, Dc=3.81g/cm3, which belongs to low-temperature phase. The optical absorption of the crystal shows that NLSB has a strong absorption band at 807.7 nm, which is suitable for laser-diode pumping.

关键词： lanthanum scandium borate crystal flux method X-ray powder diffraction absorption spectrum

Synthesis and Crystal struct.re of [(NH_4)_6][Gd_2Mo_(36)O_(112)(H_2O)_(20)]·52H_2O

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Chinese Journal of struct.ral Chemistry 2001年第5期20卷 358-362页

作者：吴传德林祥等 State Key Lab. of struct. Chemistry Fujian Inst. Res. Struct. of Matter Chinese Academy of Sciences Fuzhou Fujian 350002 China

A novel compound [(NH_4)_6][Gd_2Mo_(36)O_(112)(H_2O)_(20)]·52H_2O (1) was obtained from the reaction of (NH_4)_6Mo7O24·4H_2O with GdCl3 at pH = 1.32. The X-ray struct.ral analysis reveals that 1 crystallizes in monoclinic system, space group C2/c, Mr = 6937.77, a = 42.313(1), b=12.924(1), c=26.404(1) ?, β= 127.07(1)o, V=15086.2(6) ? 3, Z = 4, Dc = 2.976g·cm－3, ( = 3.316 mm－1, F(000) = 12963, the final R = 0.0585 and wR = 0.1490 for 5431 observed reflections. It contains a usual struct.ral unit {Mo36}, which is linked to two eight-coordinated Gd3+ cations with the Gd-O distances from 2.31(5) to 2.46(5)

关键词： heteropolymolybdate polyoxoanion trans influence effect subunit

Synthesis and Crystal struct.re of 18-Tungstotetranickel(II) diphosphate Na_(10){(PW_9O_(34))_2Ni_4(H_2O)_2}·26H_2O

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Chinese Journal of struct.ral Chemistry 2001年第4期20卷 274-277页

作者：崔传鹏吴新涛等 State Key Lab. of struct. Chemistry Fujian Inst. Res. Struct. of Matter Chinese Academy of Sciences Fuzhou Fujian 350002 China

The struct.re of single crystal of the polyoxotungstate salt Na10{(PW9O34)2Ni4（H2O）2}·26H2O ( Na10Ni4O96P2W18H56, Mr=5371.96) has been determined by X-ray diffraction (MoK（）. Crystal data: P21/n, a=11.898（2）, b=16.629（4）, c=21.413（4） ?, ( = 100.59（1）o, V= 4164.5（1） ?3, Z=2, Dc = 4.284g/cm3, F（000） = 4704, ( =2.5847cm-1, final R = 0.0344, and wR= 0.0804 for 5830 independent reflections. Two B-(-PW9O349- units in the compound are linked via a set of four coplanar Ni2+ atoms, which also carry H2O ligands. The NiO6 octahedra in each centrosymmetric anion are all tetragonally elongated with their long axes parallel.

关键词： B-(-PW_9O_(34)9- units polyoxotungstate salts crystal struct.re

Synthesis,X-Ray struct.re and Characterization of a Triruthenium Cluster Complex Ru3Ⅲ（μ3-O）(μ-CH3COO)6（py）2Cl with Four Steps One-electron Redox Processes

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Chinese Chemical Letters 2003年第5期14卷 519-522页

作者： Jing Lin CHEN, Gang Qiang YIN, Zhong Ning CHEN* State Key Laboratory of struct.ral Chemistry, Fujian inst.tute of res.arch on the struct.re of matter, fuzhou 350002 Stt. Key Lab. of struct. Chemistry Fujian Inst. Res. Struct. of Matter Fuzhou 350002 China

The synthesis and crystal struct.re of oxo-centered carboxylate-bridge trinuclear ruthenium complex, Ru3O(CH3COO)6(py)2Cl (py = pyridine) (1), are reported herein. The complex 1 has been characterized by IR, cyclic voltammetry (CV), UV-Vis and X-ray crystal analysis. The complex 1 in 0.1 mol/L (n-C4H9)4NPF6-CH2Cl2 solution at room temperature shows four one- electron redox processes at E1/2 = -1.38, -1.20, -0.17 and 1.07 V vs. Ag/AgCl.

关键词： Crystal struct.re ruthenium carboxylate electrochemistry.

Syntheses and Crystal struct.res.of Two Trinuclear Iron(Ⅲ) Carboxylate Complexes: Fe 3 (μ 3 O)( μ O 2CEt) 6(H 2O) 3 Cl· 3H 2O and Fe 3 (μ 3 O)( μ O 2CEt) 6Py 3 Cl(Py=pyridine) ①

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Chinese Journal of struct.ral Chemistry 1999年第1期18卷 53-58页

作者： Cui Y. Wang Y.-M. Zheng Y. Zhou W.-B. He L.-J. Cai S.-H. Chen B. Zhang L.-N. Fujian inst. res. struct. of matter State Key Lab. of Struct. Chemistry Chinese Academy of Sciences Fuzhou Fujian 350002 China

Two new oxo centered trinuclear iron complexes Fe 3 (μ 3 O)( μ O 2CEt) 6(H 2O) 3 Cl·3H 2O 1 and Fe 3 (μ 3 O)( μ O 2CEt) 6Py 3 Cl 2 were prepared in non aqueous solvent and thei... 详细信息

Two new oxo centered trinuclear iron complexes Fe 3 (μ 3 O)( μ O 2CEt) 6(H 2O) 3 Cl·3H 2O 1 and Fe 3 (μ 3 O)( μ O 2CEt) 6Py 3 Cl 2 were prepared in non aqueous solvent and their crystal struct.res.have been determined. Crystal 1 is monoclinic, space group P2 1/n, a=9.909(3), b=24.467(8), c=14.542(7) , β=107.85(4)° V=3356(4)  3, Z=4, M r=765.52, D c =1.52 g/cm 3, μ= 14.28 cm -1 , F(000) =1588 and R=0.059, R w =0.071 for 3745 unique reflections with I>3σ(I) . Crystal 2 belongs to the monoclinic system with space group C2/c, a=13.750(3), b=18.439(4), c=16.696(3) , β=93.42(3)°, V=4226(3)  3, Z=4, M r=894.73, D c =1.41 g/cm 3, μ =11.4 cm -1, F (000)=2322 and R=0.058, R w =0 062 for 2272 unique reflections with I>3σ(I). The two struct.res.contain the same trimetal framework in which three iron(Ⅲ) atoms form a nearly equilateral triangle with a μ 3 oxygen atom in the centre.

关键词： syntheses crystal struct.res carboxylate complexes iron complexes

The Synthesis and struct.re of Adduct of a New Schiff Base Macrocycle with Two THF: THIONE_2B_4[36]ENE-O_6N_8·2THF

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Chinese Chemical Letters 1996年第10期7卷 884-885页

作者： Lin Z.G. Chen H.Y. Lin Y.J. Huang F.H. Department of Chemistry Fujian Teachers' University Fuzhou 350007 State Key Lab. of struct. Chemistry Fujian Inst. Res. Struct. of Matter Fuzhou 350002

New Schiff base Macrocyclic compound of 2,3: 11, 12:20, 21:29, 30-tetrabenzo-1,13,16,19,31,34-hexaoxa-5,6,8,9,23,24,26,27-octaaza-7,25-dithione-2,3:4,5:9,10:11,12:22, 23:27,28:29,30 cyclo-[36]ene (thione2B4[36] ene-O6N8) containing THF has been prepared. It crystallizes in the monoclinic, space group P21/n. with parameters a=9.829(5) b=24.23(1), c=10.181(9), β=92.93(5)°, Z=2, V=2422(3)3, Dc=1.25gcm-3. Data collection: Rigaku AFC-5R diffractometer,(MoKα, λ=0.71069), ω /2θ scans. θmax=25°, empirical absorption correction, 4658 measured reflections, 4387 independent, 1743 observed reflections [I≥3σ(I)]. The final R=0.056. RW=0.069,S=1 .54, (Δ/σ)max=0.01,Δρmax=0.36e-3.

关键词： ENE and Macrocycle New O6N8 Schiff struct.re Synthesis THIONE2B4 The Adduct THF

31~P NMR Studies on Quasi-Aromaticity of Mo_3S_3 Core and struct.re of {Mo_3(μ_3-S)_3[μ-SOP(OEt)_2][S_2P(OEt)_2]_3(CH3CN)}*CH_3CN

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Chinese Journal of struct.ral Chemistry 1998年第4期17卷 302-308页

作者： XIA Ji-Bo WU Ling WANG Quan-Ming CHEN Jiu-Tong WU Da-Xu YAO Yuan-Gen LU Jia-Xi(State Key Laboratory of struct.ral Chemistry, Fujian inst.tute of res.arch onthe struct.re of matter, the Chinese Academy of Sciences, fuzhou, 350002) State Key Lab. of struct. Chemistry Fujian Inst. Res. Struct. of Matter Fuzhou 350002 China

The title compound {Mo3 (μ3,-S) (μ-S)3 [μ-SOP (OEt )2] [S2P (OEt)2]3(CH3CN) }. CH3CN, C20H46,Mo3N2O9P4S11, Mr= 1222. 9, has been synthesized bythe reaction of [Mo3 (μ3,-S) (μ-S)3]4+ with Hdtp (hydrogen diethyldithiophosphate)and its struct.res.was dctermined by X-ray crystallography. The crystal data for the title compound: triclinic, P1, Z= 2, a= 13. 011 (8), b= 13. 411 (9), c= 14. 385 (5)A, a=76. 59(5), B=78. 09(5), Y=82. 20(3), V= 2382(2) A3, Dc= 1.705 g/cm3, μ (MoKa) = 1. 434 mm-1, F (000) = 1228. The struct.re was refined to R =0.080 for 5485 observed reflections. Quasi-aromaticity in the puckered-ring of Mo3S3was experimentally probed by 31p NMR spectroscopic measurements. The 31p chemicalshifts of ligand DTP’s (diethyldithiophosphate) were modulated by the substituent effect of the adjacent bridging aromatic carboxylate through the long-distance super-conjugation via the trinuclear Mo cluster core.

关键词： X-ray struct.re quasi-aromaticity 31p NMR molybdenum cluster

A New Advance in Preparation of Mo-S(O) Clusters

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Chinese Journal of struct.ral Chemistry 1996年第2期15卷 117-122页

作者： Yao Yuan-Gen Wu Ling Zhu Yong-Bao Lu Shao-Fang (Fujtan inst.tute of res.arch on the struct.re of matter,Academia Sinica,fuzhou,Fujian 350002,China) Fujian inst. res. struct. of matter Academia Sinica Fuzhou Fujian 350002 China

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ＡＮｅｗＡｄｖａｎｃｅｉｎＰｒｅｐａｒａｔｉｏｎｏｆＭｏ－Ｓ（Ｏ）Ｃｌｕｓｔｅｒｓ￥ＹａｏＹｕａｎ－Ｇｅｎ；ＷｕＬｉｎｇ；ＺｈｕＹｏｎｇ－Ｂａｏ；ＬｕＳｈａｏ－Ｆａｎｇ；（ＦｕｊｔａｎＩｎｓｔｉｔｕｔｅｏｆＲｅｓｅａｒｃｈｏｎｔｈｅＳｔｒｕｃｔｕｒｅ...

关键词： molybdenum cluster preparation electrolysis reduction gel chromatography

Crystal struct.re of 〔PdCl_4〕·〔C_4H_(10)NO〕_2 Compound

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Chinese Journal of struct.ral Chemistry 1997年第3期16卷 191-194页

作者： WU Ling YAO Yuan-Gen HUANG Xiao-Ying(Fujian inst.tute of res.arch on the struct.re of matter,the Chinese Academy of Sciences, fuzhou, 350002 China) Fujian inst. res. struct. of matter Chinese Academy of Sciences Fuzhou 350002 China

The crystal struct.re of the title compound was determined, Mr =424. 47, orthorhombic, Pbca, a= 20. 780(5), b= 8. 601 (3), c= 8. 285(3) A, V=1480. 8(5) A, Z=4, Dc= 1. 904 g/cm3, μ(MoKa) = 19. 59 cm-1, F(000)=*** final R =0. 038, Rw=0.063 for 1554 independent observed reflections (I> 3σ(I) ). The crystal contains an isolated [PdCl4]2- planar tetragon and two morpholiniumcations which are linked to the anion ed N -H...Cl hydrogen bonds with donor-acceptor distances of 3. 394 and 3. 399 A, res.ectively.

关键词： crystal struct.re Pd compound morpholinium