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1.
I. V. Medrish A. V. Virovets E. V. Peresypkina L. B. Serezhkina 《Russian Journal of Inorganic Chemistry》2008,53(7):1034-1039
Single crystals of Cs4[(UO2)2(C2O4)(SO4)2(NCS)2] · 4H2O (I) and (NH4)4[(UO2)2(C2O4)(SO4)2(NCS)2] · 6H2O (II) have been synthesized and studied by X-ray diffraction. The crystals of both compounds are orthorhombic with the space group
Pbam, Z = 2, and unit cell parameters a = 12.0177(3) ?, b = 18.6182(5) ?, c = 6.7573(10) ?, R = 0.0376 (I); a = 11.6539(9) ?, b = 18.3791(13) ?, c = 6.7216(5) ?, R = 0.0179 (II). The main structural units of crystals I and II are [(UO2)2(C2O4)(SO4)2(NCS)2]4− chains belonging to the crystal-chemical group A2K02B22M21 (A = UO22+, K02 = C2O42−, B2 = SO42−, M1 = NCS−) of the uranyl complexes. The uranium-containing chains are joined into a three-dimensional framework due to a system of
electrostatic interactions with the cesium or ammonium ions in the structure of I. In the structure of II, this framework is additionally stabilized by hydrogen bonds involving the outer-sphere water molecules and ammonium ions.
Original Russian Text ? I.V. Medrish, A.V. Virovets, E.V. Peresypkina, L.B. Serezhkina, 2008, published in Zhurnal Neorganicheskoi
Khimii, 2008, Vol. 53, No. 7, pp. 1115–1120. 相似文献
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A new polymer azido-bridged copper(II) complex [Cu4(En)2(μ1,1-N3)4(μ1,1,1-N3)2(μ1,3-N3)2]
n
(I) (En = ethylenediamine) has been synthesized and crystallography characterized. Complex I shows one-dimensional coordination polymeric structure based on a tetranuclear cluster unit [Cu4(En)2(μ1,1-N3)4(μ1,1,1-N3)2(μ1,3-N3)2], in which the azido ions display three different bridging modes. 相似文献
5.
Oxo/hydoxo zirconium(IV) complex of the general formula [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9(μ2-OH)3]2 has been isolated, when Zr(OiPr)4 reacted with a 2-fold excess of 3,3-dimethylbutyric acid. Single crystal X-ray diffraction data, collected at 103 and 153 K, showed that the studied compound crystallizes in hexagonal system (P63/m (no. 176)). Structure consists of dimers composed of [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9] sub-units, linked by six μ2-OH bridges. Infrared spectroscopic studies proved the presence of hydroxo groups in the structure of studied clusters and formation of different types of oxo/hydroxo bridges. The application of variable temperature infrared spectroscopy and differential scanning calorimetry revealed that the structure of this complex undergoes the phase transitions at 143–183 and 203–293 K. Comparison of spectral and crystallographic data suggests that these phase transitions might be related to changes in the strength of Zr–O bonds of μ2-OH bridges linking complex sub-units, and change in symmetry of the crystal lattice (from hexagonal to trigonal). Analysis of thermogravimetric data showed that decomposition of [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9(μ2-OH)3]2 proceeds with complete conversion to ZrO2 (monoclinic form) between 603 and 803 K. 相似文献
6.
A. A. Rybinskaya E. A. Shusharina P. E. Plyusnin Yu. V. Shubin S. V. Korenev S. A. Gromilov 《Journal of Structural Chemistry》2011,52(4):816-819
A single crystal of [Pd(NH3)4]3[Ir(NO2)6]2·H2O double complex salt is studied by X-ray diffraction. Crystallographic characteristics are as follows: a = 21.0335(5) ?, b = 8.0592(2) ?, c = 21.3452(5) ?, β = 91.254(1)°, V = 3617.43(15) ?3, P21/c space group, Z = 4, d
x = 2.714 g/cm3. Single-layer pseudohexagonal packing of complex anions is determined along the [−1 0 1] direction in the structure. Complex
cations and crystallization water molecules are located between the mentioned layers. 相似文献
7.
The sandwich-type [Na(UO2)2(H2O)4(BiW9O33)2]13− uranium (VI) has been synthesized by reacting the trivacant species of B-α-[BiW9O33]9− with
and investigated by IR and UV–Vis spectroscopy, and elemental analysis. The X-ray single crystal analysis was carried out
on Na13[Na(UO2)2(H2O)4(BiW9O33)2] · 33H2O (I) which crystallizes in the orthorhombic system, space group Pna21 with a = 33.8454(19) ?, b = 21.1484(12) ?, c = 13.2403(7) ?, α = 90°, β = 90°, γ = 90°, and Z = 4. The polyanion consists
of two lacunary B-α-[BiW9O33]9− groups which sandwich two uranyl cations and one sodium cation. The uranium atoms adopt distorted pentagonal–bipyramidal coordination,
achieved by two equatorial bonds to each BiW9O33 unit and one external water ligand. The coordination of each uranium atom is evident by the shift of νas(W–Ob–W) and νas(Bi–O) stretching vibrational bonds.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
8.
The title compound was synthesized by reaction of Cu(ClO4)2, picolinic acid and carbamide in C2H5OH/CH3CN solution, and characterized by single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a=14.0481(8), b=9.0130(5), c=18.626(1)?, V=2358.3(2)?3, Z=4, Dx=1.771g·cm-3, μ=1.235mm-1 and F(000)=1276. The final R factor is 0.0440 for 1434 observed reflections. The X-ray analysis revealed that the copper(Ⅱ) atom is coordinated by two picolinic ligands in the equatorial plane, while the two oxygen atoms of perchlorate occupy the axial positions of octahedron with lengthened Cu-O distances, resulting in a 4+2 elongated octahedral environment. In the compound, there also exist two protonated carbamide cations for charge balance. CCDC: 195354. 相似文献
9.
The compound [{Pt4(en)4(NHCOtBu)4}{Tl(18-crown-6)}2](PF6)6 has been synthesized by a simple one-pot multicomponent reaction. Its structure was determined by X-ray single crystal diffraction analysis. The cation of the compound consists of one linearly arranged [Pt4(en)4(NHCOtBu)4]4+ chain and two [Tl(18-crown-6)]+ ions located at the two ends of the platinum chain. The complex crystallizes in a triclinic P1 with a=1.060 5(1), b=1.252 3(1), c=2.015(2) nm, α=107.430(2)°, β=91.032(2)°, γ=101.910(2)°, V=2.489 6(4) nm3, Z=2, R1=0.074 4, wR2(I>2σ(I))=0.222 5, S=1.062. CCDC: 294083. 相似文献
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Van An Du Gregor N. Stipicic Maria Bendova Ulrich Schubert 《Monatshefte für Chemie / Chemical Monthly》2010,10(2):671-675
Abstract
Thermolysis of cis-Fe(CO)4(SiCl3)2 results in the formation of the novel compound Fe2(CO)6(μ2-SiCl2)3, which was characterized by single crystal X-ray diffraction. Density functional theory calculations were carried out to elucidate possible reaction steps leading to the formation of Fe2(CO)6(SiCl2)3, including CO dissociation and chlorine abstraction by a SiCl3 radical generated from homolytic Fe–Si bond cleavage involving a singlet–triplet intersystem crossing. 相似文献12.
A coordination polymer, {[Cu4(nip)4(4,4′-bipy)4(DMF)4]·CH3OH}n, have been synthesized by the layer method using 5-nitroisophthalic acid (H2nip), Cu(CH3COOH)2 and 4,4′-bipyridine(4,4′-bipy) with three solutions in a marrow tube and structurally characterized by X-ray single-crystal structure analysis. The results indicated that the nip ligand has a μ2 mono-atomic bridging-monodentate coordination mode and the structure is a two-dimensional network. CCDC: 623420. 相似文献
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利用微波技术合成了配合物[Gd2(Gly)6(H2O)4](ClO4)6(H2O)5, 进行了化学成分分析、红外表征和热重分析. 应用X衍射仪测定其晶体结构, 该晶体为一维链结构, 属三斜晶系, P 空间群, 晶胞参数: a=1.1569(17) nm, b=1.4138(2) nm, c=1.5642(2) nm, α=96.910(2)°, β=102.735(2)°, γ=105.512(2)°, V=2.3606(6) nm3, Z=2, Dc=2.144 g•cm-3. 采用精密溶解-反应量热计, 通过设计热化学循环, 计算出了该配合物的标准摩尔生成焓为 -(7960.73±3.23) kJ•mol-1. 相似文献
15.
配合物Fe(pda)2(H2O)4和[FeCo(pda)4(H2O)4]n的合成与晶体结构 总被引:1,自引:0,他引:1
采用水热法合成了2个3-(3-吡啶基)丙烯酸的配合物:Fe(pda)2(H2O)4(1)和[FeCo(pda)4(H2O)4]n(2)(pda=3-(3-吡啶基)丙烯酸),用红外光谱、元素分析、热重-差热以及X-射线衍射单晶结构分析进行了表征.2个配合物都属于单斜晶系,配合物1的空间群为P21/n,配合物2的为P21/c.配合物1是一个pda配体中仅吡啶基氮原子参与配位、而羧基上的氧原子未参与配位的单核结构,通过大量的氢键作用形成三维超分子体系.2是pda配体桥联Fe和Co的异核二维层状配位聚合物;配体吡啶基上的氮原子和羧基上的氧原子都参与了配位,其中羧基采用单齿配位模式. 相似文献
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Crystal structure of a tetrahedral cluster complex [Zn2(NH3)6(μ-OH)][Zn(NH3)4]0.5[Re4Te4(CN)12]·5H2O
A cluster complex of the composition [Zn2(NH3)6(μ-OH)][Zn(NH3)4]0.5[Re4Te4(CN)12]·5H2O is obtained by the interaction of an aqueous solution of K4[Re4Te4(CN)12]·5H2O with an aqueous ammonia solution of ZnCl2. The compound crystallizes in the C2/m (12) monoclinic space group with unit cell parameters a = 23.233(2) ?, b = 14.5906(16) ?, c = 14.3825(15) ?, β = 125.169(1)°, V = 3985.5(7) ?3, Z = 4, d
x = 3.290 g/cm3. The structure is built from cluster [Re4Te4(CN)12]4− anions and complex [Zn2(NH3)6(μ-OH)]3+ and [Zn(NH3)4]2+ cations; the latter is disordered over two positions. 相似文献
18.
E. A. Gerasimova T. V. Utkina E. V. Peresypkina A. V. Virovets T. G. Cherkasova 《Russian Journal of Inorganic Chemistry》2009,54(5):692-697
New mixed-ligand coordination compounds[Cd(DMSO)5(NCS)][Cr(NH3)2(NCS)4] · 3DMSO (I) and [Mn(DMSO)4(H2O)2][Cr(NH3)2(NCS)4]2 · 6DMSO · 2H2O (II) have been synthesized and studied by IR spectroscopy and X-ray diffraction analysis. The crystals of compound I are monoclinic, a = 14.5275(7), b = 23.1692(11), c = 14.6969(6) ?, β = 97.057(2)°, V = 4909.4(4) ?3, space group P21/c, Z = 4, ρcalcd = 1.507 g/cm3, R = 0.0556. The crystals of compound II are triclinic, a = 11.7784(3), b = 12.1760(3), c = 13.1922(2) ?, α = 85.5420(10)°, β = 87.9000(10)°, γ = 70.3680(10)°, V = 1776.46(7) ?3, space group P
, Z = 1, ρcalcd = 1.444 g/cm3, R = 0.0350.
Original Russian Text ? E.A. Gerasimova, T.V. Utkina, E.V. Peresypkina, A.V. Virovets, T.G. Cherkasova, 2009, published in
Zhurnal Neorganicheskoi Khimii, 2009, Vol. 54, No. 5, pp. 751–755. 相似文献
19.
用液相反应-前驱物烧结法制备了Cr2(WO4)3和Cr2(MoO4)3粉体。298~1 073 K的原位粉末X射线衍射数据表明Cr2(WO4)3和Cr2(MoO4)3的晶胞体积随温度的升高而增大, 本征线热膨胀系数分别为(1.274±0.003)×10-6 K-1和(1.612±0.003)×10-6 K-1。用热膨胀仪研究了Cr2(WO4)3和Cr2(MoO4)3在静态空气中298~1 073 K范围内热膨胀行为,即开始表现为正热膨胀,随后在相转变点达到最大值,最后表现为负热膨胀,其负热膨胀系数分别为(-7.033±0.014)×10-6 K-1和(-9.282±0.019)×10-6 K-1。 相似文献
20.
W. -T. Chen S. -M. Ying Y. -P. Xu Q. -Y. Luo D. -S. Liu 《Journal of Structural Chemistry》2011,52(3):631-634
A novel bimetallic 4f-3d metal-isonicotinic acid inorganic-organic hybrid complex [Tb0.5(C6NO2H5)3(H2O)2]2n
·(H3O)4n
(ZnCl5)
n
(ZnCl4)2n
(1) is synthesized. It has a one-dimensional polycationic chain-like structure. Photoluminescent investigation reveals that
it displays interesting emissions in the violet, blue, green, and yellow regions. 相似文献