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

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Chinese Journal of Structural Chemistry 2001年第4期20卷 256-258页

作者：林洲斌王国富等 Fujian Institute of Research on the structure of matter Chinese Academy of Sciences

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 structure 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

Rapid growth of a large-scale(600 mm aperture) KDP crystal and its optical quality

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High Power Laser Science and Engineering 2014年第1期2卷 40-44页

作者： Guohui Li Guozong Zheng Yingkun Qi Peixiu Yin En Tang Fei Li Jing Xu Taiming Lei Xiuqin Lin Min Zhang Junye Lu Jinbo Ma Youping He Yuangen Yao Fujian Institute of Research on the structure of matter Chinese Academy of Sciences

Potassium dihydrogen phosphate(KDP) single crystals are the only nonlinear crystals currently used for electro-optic switches and frequency converters in inertial confinement fusion research, due to their large dimension and exclusive physical properties. Based on the traditional solution-growth process, large bulk KDP crystals, usually with sizes up to600 × 600 mm2 so as to make a frequency doubler for the facility requirement loading highly flux of power laser, can be grown in standard Holden-type crystallizers, without spontaneous nucleation and visible defects, one to two orders of magnitude faster than by conventional methods. Pure water and KDP raw material with a few ion impurities such as Fe,Cr, and Al(less than 0.1 ppm) were used. The rapid-growth method includes extreme conditions such as temperature range from 60 to 35℃ , overcooling up to 5℃ , growth rates exceeding 10 mm/day, and crystal size up to 600 mm. The optical parameters of KDP crystals were determined. The optical properties of crystals determined indicate that they are of favorable quality for application in the facility.

关键词： large-scale KDP crystals rapid growth optical quality

The Reaction of Octacarbonyldicobalt and Dipropargyl Malonate

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Chinese Journal of Structural Chemistry 2001年第2期20卷 104-107页

作者：张玉华劳文剑罗资琴殷元骐黄子祥吴锵金 Lanzhou Institute of Chemical Physics Chinese Academy of Sciences Lanzhou Petro-chemical College of technology Fujian Institute of Research on the structure of matter Chinese Academy of Sciences

The reaction of octacarbonyldicobalt and dipropargyl malonate afforded the two expected compounds [CH 2(CO 2CH 2C 2H\|μ) 2][Co 2(CO) 6] 2 1 and [HC 2CH 2O(O)C^CH 2CO 2CH 2C 2H\|μ][Co 2(CO) 6)] 2. Both 1 and 2 were characterized by elemental analysis, IR and NMR. The molecular structure of 1 was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with the following crystallographic parameters~: a=7.7492(15), b=12.925(3), c=14.366(3) , α=81.92(3), β=77.94(3), γ=89.48(3)°, V=1392.9(5)  3, Z= 2, M r=751.99, D c=1.793 g/cm 3, F(000)=740, μ(Mo-Kα)=24.13 cm -1 and final R=0.0880 for 5421 observations with I>2σ(I).

关键词： cobalt alkyne carbonyl crystal structure

Growth and Characteristics of Nd^(3+):GdAl_3(BO_3)_4 Crystal

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Chinese Journal of Structural Chemistry 2003年第2期22卷 169-173页

作者： TU Chao-Yang② ZHU Zhao-Jie LI Jian-Fu WU Bai-Chang (Fujian Institute of Research on the structure of matter, The Chinese Academy of sciences, Fuzhou, Fujian 350002, China) BRENIER Alain (Laboratoire de Physico-Chimie des Mat閞iaux Luminescents, Universit?Claude Bernard-Lyon1,UMR CNRS 5620, France) Fujian Institute of Research on the structure of matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China

Nd3+:GdAl3(BO3)4 (NGAB) crystal with the size of 30 mm was grown from the solvent system of K2O-Gd2O3-MoO3-B2O3 by combining accelerated seed rotation technology with medium seeded solution growth (MSSG) method, and its crystal structure has been determined by X-ray powder diffraction. It crystallizes in the trigonal system, space group R32 with a = 9.2734(2), c = 7.2438(1) ? V = 538 ?, Z = 3 and Dc = 4.379 g/cm3. The absorption and emission spectra of NGAB in the function of s and polarizations at room temperature have been measured. UV generation tuneable in 378～382 nm, green (531 nm) generation and blue generation tuneable in 436～443 nm as well as red (669 nm) generation by self-frequency changing were obtained with the output of 105, 119.5, 445 and 19 mJ/pulse, respectively, when the crystal was pumped by a dye laser.

关键词： flux crystal growth Nd3+:GdAl3(BO3)4 crystal self-frequency changing laser

H_2O_2-Promoted Size Growth of Sulfated TiO_2 Nanocrystals

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Chinese Journal of Structural Chemistry 2008年第5期27卷 622-628页

作者：闫友军邱晓清王辉李莉萍李广社 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

Anatase nanoparticles modified by sulfate groups were synthesized using hydrothermal method. The particles were controlled to large sizes by simply adjusting the amount of H2O2, in which HOO^- ions replaced the surface sulfate groups and reduced the steric effect to promote the grain growth. The size-induced microstructural changes of the as-prepared nanoparticles were characterized using powder XRD, FT-IR, TG. and UV-vis analyses. The sulfate groups existed on anatase surface in unidentate and bidentate coordination forms. With the particle size reduction, bandgap energies of the as-prepared anatase nanoparticles decreased, and the desorption temperature of sulfate groups shifted towards lower temperatures.

关键词： hydrothermal synthesis nucleophilie substitution particle growth microstructure

Syntheses and Crystal structures of Two New Iron-sulfur Carbonyl Complexes: [Fe_2(SC_6H_4Cl)_2(CO)_6]·0.5(Et_2O) and [Fe_3(SC_6H_4NH_2)_6(CO)_6]·2(MeOH)

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Chinese Journal of Structural Chemistry 2006年第3期25卷 326-332页

作者：马成丙陈昌能刘秋田 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

Two new iron-sulfur carbonyl complexes, [Fe2（SC6H4Cl）2（CO）6]·0.5（Et2O） 1 and [Fe3（SC6H4NH2）6（CO）6]·2（MeOH） 2, have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Crystal data for 1： monoclinic, C2/c, a = 18.4439（8）, b = 11.0999（5）, c = 25.1830（10）A°, β = 97.0370（10）°, V = 5116.8（4） A°^3, Z = 8, C20H13Cl2Fe2O6.50S2, Mr = 604.02, Dc = 1.568 g/cm^3, μ = 1.540 mm^-1, F（000） = 2424, the final R = 0.0545 and wR = 0.1454 for 3443 observed reflections with I 〉 2σ（I）; 2： monoclinic, P21/n, a = 12.350, b = 26.3050（11）, c = 16.057A°, β = 97.891 （3）°, V = 5166.9（2）A°^3, Z = 4, C44H44Fe3N6O8S6, Mr = 1144.76, Dc = 1.472 g/cm^3, μ = 1.128 mm^-1, F（000） = 2352, the final R = 0.0442 and wR = 0.1197 for 7978 observed reflections with I 〉 2σ（I）. Complex 1 contains one iron dimer, in which two tricarbonyliron（Ⅰ） fragments are bridged together by two 4-chlorophenylthiolate ligands, whereas complex 2 contains a linear tri-iron cluster, in which two terminal tricarbonyliron（Ⅱ） fragments and the central Fe（Ⅱ） atom are linked together by six 4-aminophenylthiolate bridging ligands.

关键词： iron-sulfur carbonyl complex thiophenol synthesis crystal structure

Syntheses, Crystal structures and Magnetism of Two New Coordination Polymers [Ni(bix)_2Cl_2]_n and [Co(bix)Cl_2]_n

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Chinese Journal of Structural Chemistry 2007年第6期26卷 711-716页

作者：周慧杜少武 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

The self-assembly reactions of M^ⅡCl2 （M = Ni, Co） with the flexible bix ligand [bix = 1,4-bis（imidazole-1-ylmethyl）benzene] yielded a 2D network [N^Ⅲ（bix）2Cl2]n 1 and a 1D chain [Co^Ⅱ（bix）Cl2]n 2. Their crystal structures have been determined by X-ray single-crystal diffraction analysis. Complex 1 characters a two-dimensional grid-type structure and crystallizes in monoclinic, space group P21/c with a = 7.7231（7）, b = 12.7787（9）, c = 13.9374（13）A, β = 105.419（4）°, C28H28Cl2N8Ni, Mr = 606.19, Ζ = 2, V = 1326.0（2）A^3, Dc = 1.518 g/cm^3, μ = 0.969 mm^-1, F（000） = 628, R = 0.0429 and wR = 0.0783 for 2503 observed reflections （Ⅰ〉 2σ（Ⅰ））. Compound 2 is a one-dimensional chain and crystallizes in orthorhombic, space group Pbca with a = 11.3696（6）, b = 10.2128（6）, c = 14.4943（9）（A）, C14H14Cl2CoN4, Mr = 368.12, Z = 4, V = 1683.01（17）A^3, Dc = 1.453 g/cm^3, μ = 1.334 mm^-1, F（000） = 748, R = 0.0317 and wR = 0.0800 for 1778 observed reflections （Ⅰ〉 2σ（Ⅰ））. Magnetic properties of the title complexes were also investigated.

关键词： bix magnetic property non-rigid ligand crystal structure

A New Luminescent Complex Cd(Ⅱ)-xanthene-9-carboxylate: [Cd(L)_2(H_2O)]_n

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Chinese Journal of Structural Chemistry 2013年第1期32卷 96-100页

作者：尚洁吴小园王飞杨文斌余荣民卢灿忠 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Graduate School of Chinese Academy of sciences Key Laboratory of Coal to Ethylene Glycol and Its Related technology Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences

A new luminescent Cd（Ⅱ） coordination polymer, [Cd（L）2（H2O）]n 1 （HL = xan-thene-9-carboxylic acid）, was synthesized hydrothermally and characterized by satisfactory elemental analysis, FT-IR spectra and single-crystal X-ray diffraction. The crystal is of orthorhombic system, space group P212121 with a = 6.4548（4）, b = 13.0876（12）, c = 27.466（2）, V = 2320.3（3）3, C28H20CdO7, Mr = 580.84, Z = 4, Dc = 1.663 g/cm3, F（000） = 1168, μ = 0.990 mm-1, Flack parameter = 0.00（2）, the final R = 0.0296 and wR = 0.0691 for 5301 observed reflections （I 2σ（I））. 1 features a one-dimensional （1D） carboxylate oxygen-bridged inorganic chain, which is further connected by intermolecular hydrogen bonds into a three-dimensional （3D） framework. Moreover, compound 1 exhibits strong photoluminescence in the solid state at room temperature.

关键词： cadmium hydrothermal synthesis supramolecular structure photoluminescence

Organic Carboxylate Ligand Tuned Topological Variations in Three Zn(Ⅱ)Coordination Polymers:Syntheses,Crystal structures and Photoluminescent Properties

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Chinese Journal of Structural Chemistry 2018年第9期37卷 1470-1478页

作者：柳长庆杨锦霞张鑫覃业燕姚元根 Key Laboratory of Coal to Ethylene Glycol and Its Related technology Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences University of Chinese Academy sciences

Three new Zn（Ⅱ） coordination polymers, namely [Zn2（suc）2（bib）2]n·nH2 O（1）, [Zn（glu）（bib）]n·4 nH2 O（2）, and [Zn（adp）（bib）]n（3）（bib = 1,4-bis（N-imidazolyl）butane, H2 suc = succinic acid, H2 glu = glutaric acid, H2 adp = adipic acid） have been hydrothermally synthesized and structurally characterized. Compound 1 features a 3D framework with 4-connected hxg-d topological network, compound 2 is comprised of 2D 44-sql-type sheets, and the adjacent 2D sheets are further packed into a 3D supramolecular architecture via intermolecular hydrogenbonding interactions, and compound 3 is a 3D framework with 4-fold interpenetrating dia topology. The structural comparison of these three compounds demonstrates that the topological variations can be well controlled by employing aliphatic dicarboxylate ligands with different spacer lengths. Moreover, the thermal stabilities and photoluminescent properties of them were also studied in detail.

关键词： zinc(Ⅱ) compound aliphatic dicarboxylate ligands hydrothermal reaction meso-helix hydrogen bond photoluminescence