Na3La2(BO3)3的晶体结构

以Na2CO3-H3BO3-NaF为助熔剂,使用顶部籽晶法生长出Na3La2(BO3)3透明单晶.测定了Na3La2(BO3)3的晶体结构,该晶体属正交晶系,空间群:mm2(No.38),晶胞参数为a＝0.51580(10)nm,b=1.1350(2)nm,c=0.73230(15)nm,α＝β＝γ＝90°,V＝0.42871(15)nm3,密度:.053g/cm3.晶体结构中的硼氧基团是平面的BO3基团,BO3基团相互独立,且与Na(1)O6、Na(2)O8、Na(3)O6和La(1)O9配位多面体连结形成三维网络骨架结构.讨论了Na3La2(BO3)3的晶体结构与倍频效应的关系.     

Na3La9O3(BO3)8的晶体结构

以Na2CO3-H3BO3为助熔剂,用顶部籽晶法生长出Na3La9O3(BO3)8单晶.测定了Na3La9O3(BO3)8晶体结构,结果表明:该晶体属六方晶系,空间群:P62m,晶胞参数为a=b=0.89229(13)nm,c=O.87366(17)nm,α=β=90°,γ=120°,Z=1,V=0.60240(17)nm3,密度为5.066g/cm3.晶体结构中的硼氧基团是平面的BO3基团,BO3基团相互独立,通过与Na(1)O6、La(1)O9和La(2)O8的配位多面体连结形成层状结构,所有层平行于(001)面.描述了Na3La9O3(BO3)8晶体在非线性光学材料领域的应用前景.     

Na3La2(BO3)3晶体生长及光谱特性

本文以起始摩尔比为1:1的Na2CO3:H3BO3,并添加5;质量分数的NaF为助熔剂,用顶部籽晶法生长出φ35mm×5mm的透明Na3La2(BO3)3单晶.该晶体属正交晶系,空间群:Amm2,晶胞参数为a=0.51580(10)nm,b=1.1350(2)nm,c=0.73230(15)nm,α=β=γ=90°.测量了Na3La2(BO3)3晶体在室温下的透过光谱,紫外截止波长约为200nm.该晶体常温下稳定,不吸潮,但却易溶于稀酸.     

Ba7(BO3)3F5晶体结构及热分析

采用高温溶液法从BaCO3,BaF2及H3BO3混合体系中生长出了一种氟硼酸钡晶体,Ba7(BO3)3F5晶体属六方晶系,空间群为P63mc,晶胞参数:a=1.11562(15) nm,c=0.72415(14) nm,Z=2,V=0.7805(2) nm3.Ba7(BO3)3F5晶体结构是由Ba(1)O7F3基团,Ba(2)O4F3基团,Ba(3)O6F4基团和独立的BO3基团相互连接形成的三维空间网络结构.Ba7(BO3)3F5的热分析分析结果表明Ba7(BO3)3F5在1070℃同成份熔化.     

YBaNa(BO3)2晶体的助熔剂法生长与表征

采用助熔剂自发成核法,探索了生长YBaNa(BO3)2晶体的不同助熔剂体系,从中选出2Na2CO3-4H3BO3-BaCO3做助熔剂,生长了YBaNa(BO3)2晶体.采用X射线衍射(XRD),红外吸收光谱和透过光谱,差热失重分析对生长的晶体进行了表征.结果表明,晶体属于六方晶系,空间群为R3,晶胞参数为a=0.53382(2) nm,c=3.58303(19) nm.BO3-3基团存在于晶体结构中,晶体的紫外截止波长在208 nm左右,晶体在800℃时有明显的相变点.     

Nd3+:Na3La9O3(BO3)8晶体生长和光谱性能

采用顶部籽晶法生长Nd3+:Na3La9O3(BO3)8 晶体.在室温下测试了吸收光谱、发射光谱和荧光寿命.应用Judd-Ofelt理论评价了Nd3+:Na3La9O3(BO3)8晶体的光谱性能.812 nm处较宽的吸收峰适合AlGaAs LD泵浦的吸收.分别计算了Nd3+离子的唯象强度、谱线强度、辐射寿命、荧光分支比和荧光量子效率.     

KCaZn2(BO3)2F的固相合成、晶体结构及表征

采用高温固相合成了一种新的类Sr2Be2B2O7族化合物KCaZn2(BO3)2F,利用粉末X射线衍射精修其晶体结构.该晶体同KCdZn2(BO3) 2F同构,为三方晶系,空间群为P31c,单胞参数为a=5.03096(5)A,c=15.3940(2)A,Z=2.晶体基本阴离子基元是平面三角形的BO3和四面体的ZnO3F基元,两个基元通过共顶的O原子相连,在ab平面形成二维的十二元环的(Zn3B3O6 F3)∞结构.(Zn3B3O6F3)∞结构通过F原子连接,形成(Zr6B6O12F3)∞双层单元,双层单元之内的两层BO3基元排列方式基本相反.(Zn6B6O12F3)∞双层单元与同它中心对称的另一个(Zn6B6O12F3)∞双层单元在c方向堆垛成三维的结构,K+和Ca2+分别位于(Zn6B6O12F3)∞双层单元的层内和层间空隙处.紫外可见漫反射光谱表明该晶体在400～2500 nm范围具有高的透过率,晶体的紫外截止波长为235 nm.     

Na3Sm2(BO3)3的晶体生长及热学和光谱性质

以Na2CO3-H3BO3为助溶剂,用顶部籽晶法生长了14mm×8mm×2mm的Na3Sm2(BO3)3晶体.差热分析(DTA)表明Na3Sm2(BO3)3非同成分熔融,熔点为1089.1℃.该晶体易溶于酸,在空气条件下能稳定存在,不易潮解.测量了室温下晶体在200～2500nm范围内的吸收光谱,并对跃迁能级进行了初步指认.     

一种新的非线性光学材料—Na3Sm2（BO3）3

本文采用固相反应法合成了一种新的硼酸盐化合物Na3Sm2(BO3)3,以Na2CO3-H3BO3为助熔剂,用悬挂铂丝法获得了3mm×2mm×0.5mm的透明单晶,X射线粉末衍射分析表明,该化合物属正交晶系,晶胞参数a=0.50585nm,b=1.10421nm,c=0.70316nm.红外光谱测量证实晶体结构中含有BO33-基团,粉末倍频效应测试表明该化合物具有非线性光学效应,粉末倍频信号强度接近KDP.     

双掺Er~(3+)/Yb~(3+)∶Sr_3La_2(BO_3)_4晶体的生长与光谱特性

采用提拉法生长了尺寸为20mm×30mm的Er3+/Yb3+∶Sr3La2(BO3)4晶体,研究了Er3+/Yb3+∶Sr3La2(BO3)4晶体的吸收光谱和荧光光谱。根据Judd-Ofelt理论分析并计算了辐射跃迁几率、辐射寿命、荧光分支比等光谱参数,获得的唯象参数为:Ω2=15.59×10-20cm2,Ω4=2.25×10-20cm2,Ω6=1.49×10-20cm2。在Er3+/Yb3+∶Sr3La2(BO3)4晶体中Er3+在1533nm处发射跃迁截面为7.88×10-21cm2,Er3+的4I13/2→4I15/2能级跃迁的荧光寿命和辐射寿命分别为0.728ms和4.24ms,结果表明Yb3+对Er3+有敏化作用,提高了对泵浦光的吸收能力,Er3+/Yb3+∶Sr3La2(BO3)4晶体可望作为1.55μm波段的一种有潜力的激光材料。     

Molecular structure of (tBu)3AlP(nPr)3

The crystal and molecular structure of (^tBu)₃AlP(ⁿPr)₃ has been determined. The Al(1)?P(1) bond distance [2.594(3) Å] is slightly longer than other aluminum-phosphine complexes; however, the geometry about aluminum is similar to that of the [AlCl(^tBu)₃]^? anion, suggesting that the geometry about the aluminum in tri-tert-butylaluminum complexes is defined by the size of thetert-butyl ligands and not as a consequence of the steric bulk of the Lewis base. Crystal data: Monoclinic,P2_t,a=8.932(2),b=16.832(3),c=9.328(2), Å, β=114.36(3)°,V=1277.6(6) ų,Z=4,R.=0.055,R _w =0.053.     

The structures of three trimethylarsine-boron trihalide adducts: (CH3)3AsBCl3, (CH3)3AsBBr3, and (CH3)3AsBI3

An X-ray structure analysis of three trimethylarsine-boron trihalide adducts has been undertaken. Crystals of (CH₃)₃AsBCl₃ and (CH₃)₃AsBBr₃ are monoclinic with space groupP2₁/m (No. 11) withZ=2 while those of (CH₃)₃AsBI₃ are orthorhombic with space groupPnma (No. 62) withZ=4. For (CH₃)₃AsBCl₃,a=6.497(3) Å,b=10.735(3) Å,c=7.070(2) Å,=111.8(3)°,V=458.4(3) ų,R=0.0343. For (CH₃)₃AsBBr₃,a=6.672(4) Å,b=11.135(7) Å,c=7.199(4) Å,=111.5(1)°,V=497.7(5) ų,R=0.0434. For (CH₃)₃ÅsBI₃,a=13.113(7) Å,b=11.733(5) Å,c=7.387(3) Å,V=1136.5(5) ų,R=0.0329. The As-B bond lengths are 2.065(6), 2.04(1), and 2.03(1) Å, respectively, for the chloride, bromide, and iodide. These and other structural parameters are discussed with reference to previous predictions based on vibrational spectra and previous structural studies on the trimethyl-phosphine and trimethylamine adducts.     

Crystal and molecular structures of three trimethylamine-boron halide adducts: (CH3)3NBCl3, (CH3)3NBBr3, and (CH3)3NBI3

X-ray diffraction data from single crystals of the trimethylamine complexes of the three boron halides, BCl₃, BBr₃, and BI₃, lead to aP2₁/m monoclinic cell containing two molecules for each complex. The unit cell dimensions area = 6·68(1),b = 10·247(3),c = 6·502(6) Å, =116·2(1)° (chloro);a = 6·86(1),b = 10·612(4),c = 6·737(6) Å, = 115·8(1)° (bromo);a = 6·92(2),b = 10·86(1),c = 7·147(6) Å, = 93·9(1)° (iodo). The structures were solved by three-dimensional sharpened Patterson functions and show only the chloro and bromo compounds to be isomorphous. Refinement of 662,718 and 954 observed reflexions for the chloro, bromo and iodo complexes, respectively, using anisotropic thermal parameters yielded conventionalR factors of 0·045, 0·087 and 0·054.The molecules are shown to possess a B—N dative bond, a staggered conformation, and effective 3m (C _3v) symmetry. Average C—N bond lengths are 1·52(1) Å for all three complexes. Boronhalogen bond lengths average 1·864(4), 2·04(2) and 2·28(2) Å, while B—N bond distances are 1·609(6), 1·60(2) and 1·58(3) Å, respectively, for the chloro through iodo compounds. Bond angles are approximately tetrahedral with the C—N—C angle decreasing by several degrees in the Cl Br I series.Based in part on a dissertation submitted by Patty H. Clippard to the Rackham School of Graduate Studies of the University of Michigan, January 1969 in partial fulfillment of the requirements of the Ph.D. Degree.     

Synthesis, spectroscopy, and X-ray structures of fac-(CO)3(dppe)MnSC(S)H, fac-(CO)3(dppe)ReSC(S)H, fac-(CO)3(dppp)ReSC(S)H, and fac-(CO)3(dppb)ReSC(S)H

The monodentate dithioformato complexes, fac-(CO)₃(dppe)MnSC(S)H (1), fac- (CO)₃(dppe)ReSC(S)H (2), fac-(CO)₃(dppp)ReSC(S)H (3), and fac-(CO)₃ (dppb)ReSC(S)H (4), where dppe is 1,2-bis(diphenylphosphino)ethane, dppp is 1,3-bis(diphenylphosphino)propane, and dppb is 1,4-bis(diphenylphosphino)butane, were synthesized from the treatment of the corresponding hydrides, fac-(CO)₃ (P-P)MSC(S)H with CS₂. Compounds 1–4 crystallize in the monoclinic crystal system: for 1, space group = P2₁/c, a = 15.3139(3) Å, b = 9.7297(4) Å, c = 19.0991(6) Å, = 105.928(1), V = 2736.5 ų, Z = 4; for 2, space group = P2₁/c, a = 15.6395(8) Å, b = 9.8182(5) Å, c = 19.4153(11) Å, = 106.741(1), V = 2854.9(3) ų, Z = 4; for 3, space group = P2₁/n, a = 11.3570(10) Å, b = 19.465(2) Å, c = 15.5702(14) Å, = 104.776(2), V = 3328.3(5) ų, Z = 4; and for 4, space group = C2/c, a = 32.078(2) Å, b = 10.4741(6) Å, c = 19.0608(9) Å, = 94.315(2), V = 6386.1(6) ų, Z = 8.     

Crystal and molecular structure of OC(CoC5H5)3(CF3CCCF3)

The structure of the title compound has been confirmed by an X-ray diffraction analysis, and refined by full-matrix least squares. The crystals are mono-clinic:a=9.171(3),b=25.176(15)c=9.192(3) Å,=117.08(3)°,Z=4,D _x =1.976g cm^–3,=2.66mm^¯1, space groupP2₁/n (No. 14). The finalR value is 5.7%. Interatomic distances and bond angles are compared with those reported in related molecules.The preferred name of this compound according to the IUPAC rules is ₃-[11–2-bis(trifluoromethyl)vinylene]- ₃-carbonyl-tris (-cyclopentadienyl)-triangulo-tricobalt.     

La0.5Sr0.5CoO3/Pb(Zr0.4Ti0.6)O3/La0.5Sr0.5CoO3铁电电容器的结构和性能研究

采用磁控溅射法和脉冲激光沉积法,在SrTiO3(001)衬底上制备了La0.5Sr0.5CoO3(70 nm)/Pb(Zr0.4Ti0.6)O3(70 nm)/La0.5Sr0.5CoO3(70 nm) (LSCO/PZT/LSCO)铁电电容器异质结.X射线衍射结果表明:LSCO和PZT薄膜均为外延结构.在5 V的外加电压下, LSCO/PZT/LSCO电容器具有较低的矫顽电压(0.49 V),较高的剩余极化强度(41.7 μC/cm2 )和较低的漏电流密度(1.97×10-5 A/cm2),LSCO/PZT/LSCO电容器的最大介电常数为1073.漏电流的分析表明:当外加电压小于0.6 V时,电容器满足欧姆导电机制;当外加电压大于0.6 V时,符合空间电荷限制电流(SCLC)导电机制.     

Synthesis and structure of two crystalline modifications of Bis(1,10-Phenanthroline)trinitratoeuropium(III) Eu(NO3)3(Phen)2

Two crystalline modifications (I and II) of the phenanthroline complex of europium nitrate with the same chemical composition, Eu(NO₃)₃(Phen)₂, are synthesized under different conditions by varying the solvents, temperatures, and crystallization rates. The crystal structures of these modifications are determined using X-ray diffraction. Crystalline modifications I and II differ in the unit cell parameters and the positions of the complexes in the unit cell. The geometric characteristics of the complexes in the structures of compounds I and II differ insignificantly. Crystals of compound I belong to the isostructural family Ln(NO₃)₃(Phen)₂ (Ln = La-Lu). Crystals of compound II (new phase) are studied for the first time. Crystals of I and II are monoclinic, space group C2/c, and Z = 4. The unit cell parameters are as follows: a = 11.1555(10) Å, b = 17.9698(10) Å, c = 13.0569(10) Å, β = 100.507(10)°, and V = 2572.1(3) ų for modification I and a = 9.5153(10) Å, b = 15.4546(10) Å, c = 17.1763(10) Å, β = 93.451(10)°, and V = 2521.3(3) ų for modification II. The difference between the molecular complexes in the structures of compounds I and II is revealed by the superposition method. Complexes II are arranged along the C ₂ axis and are statistically disordered with respect to this axis.     

Crystal structure of dinitratotris(pyridine)nickel(II), Ni(NC5H5)3(NO3)2

Ni(NC₅H₅)₃(NO₃)₂ crystallizes in the triclinic space group P¯1 witha=8.432(2),b=9.993(2),c=12.181(3)Å, =69.78(2),=83.16(2), =67.73(1), andD _c =1.57 g cm^–3 forZ=2. The Ni²⁺ ion is six-coordinate with one bidentate and one monodentate nitrato ligand.     

Electrical Conductivity of Phenoxazine-Iodine (2:3) and Phenothiazine-Iodine (2:3) Crystals

Abstract

Single crystals of phenoxazine-iodine (2 : 3) and phenothiazine-iodine (2 : 3) salts are found to be highly conducting ([sgrave] _R.T. = 5–20 ohm^?1 cm^?1). The observed deviation from the exponential temperature dependence of the conductivities is ascribed to the degenerate semiconducting phases or alternatively to the metallic phases with impurities. However, phenoxazine-iodine and phenothiazine-iodine are perfect semiconductors below 220° K with activation energies of 0.12 eV and 0.14 eV, respectively. The absorption features related with (phenoxazine)⁺ ₂ and (phenothiazine); cations are observed in the infrared spectra of the salts.     

Crystal structure ofcis-diaqua bis(2,2′-bipyridyl)chromium(III) nitrate, [Cr(bipy)2(H2O)2] (NO3)3

cis-Diaquabis(2,2-bipyridyl)chromium(III) nitrate crystallizes in the mono-clinic system, space groupP2₁/c, witha=16.102(6),b=10.792(5),c=15.076(6) Å,=112.90(5)°, andZ=4. The saltlike structure was determined from X-ray crystallography and refined toR=7.5% for 3342 observed reflections. The Cr atom is octahedrally surrounded by twocis water molecules and by two chelated 2,2-bypiridyl ligands forming two nearly orthogonal planes. Selected bond distances are: Cr-O, 2.00(1) and 1.98(1) Å, Cr-N, 2.04 Å (mean).