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1.
The title hydride and its deuteride were successfully synthesized. The heavy atom structure and hydrogen positions were determined respectively by X-ray powder diffraction and time-of-flight neutron powder diffraction. They crystallize with a new monoclinic structure in space group I2 (No. 5); cell parameters: a = 12.575(1) A, b = 9.799(1) A, c = 7.9911(8) A, beta = 100.270(4) degrees (hydride), a = 12.552(1) A, b = 9.7826(8) A, c = 7.9816(7) A, beta = 100.286(4) degrees (deuteride), Z = 8. Sr(2)AlH(7) is the first example that consists of isolated [AlH(6)] units and infinite one-dimensional twisted chains of edge-sharing [HSr(4)] tetrahedra along the crystallographic c axis.  相似文献   

2.
Single-phase ternary deuteride Li(2)BeD(4) was synthesized by a high-pressure high-temperature technique from LiD and BeD(2). The crystal structure of Li(2)BeD(4) was solved from X-ray and neutron powder diffraction data. The compound crystallizes in the monoclinic space group P2(1)/c with lattice parameters a = 7.06228(9) A, b = 8.3378(1) A, c = 8.3465(1) A, beta =93.577(1) degrees, and Z = 8. Its structure contains isolated BeD(4) tetrahedra and Li atoms that are located in the structure interstices. Li(2)BeD(4) does not undergo any structural phase transitions at temperatures down to 8 K.  相似文献   

3.
The intermediate valence compound Ce 2Ni 2Mg absorbs irreversibly hydrogen when exposed under 1 MPa of H 2 pressure at room temperature. The resulting hydride Ce 2Ni 2MgH 7.7 is stable in air and crystallizes as the deuteride La 2Ni 2MgD 8 in a monoclinic structure (space group P2 1 /c) with the unit cell parameters a = 11.7620(2), b = 7.7687(2), and c = 11.8969(2) A and beta = 92.75 degrees . The H-insertion in Ce 2Ni 2Mg induces a structural transition from a tetragonal to a monoclinic symmetry with an unit cell volume expansion Delta V m/ V m approximately 24.9%. The investigation of the hydride by magnetization, electrical resistivity, and specific heat measurements indicates a change from an intermediate valence behavior to a non-magnetic strongly correlated electron system. This transition results from a change of the coupling constant J cf between 4f(Ce) and conduction electrons induced by the hydrogenation.  相似文献   

4.
Wang XY  Sevov SC 《Inorganic chemistry》2008,47(3):1037-1043
Three hybrid organic-inorganic coordination polymers with benzenepentacarboxylate (BPCA) linkers, [Co3(C6H(COO)5)(OH)(H2O)3] (1-Co), [Zn3(C6H(COO)5)(OH)(H2O)3] (2-Zn), and [Co5(C6H(COO)5)2(H2O)12].(H2O)12 (3-Co), were synthesized hydrothermally and were characterized structurally and magnetically. 1-Co and 2-Zn are isostructural [C2/c; Z=8; 1-Co, a=19.5350(6) A, b=10.4494(4) A, and c=13.2353(5) A, beta=97.2768(8) degrees; 2-Zn, a=19.5418(9) A, b=10.3220(10) A, and c=13.4660(10) A, beta=98.455(10) degrees] with three-dimensional structures that contain [M6] secondary building units bridged by BPCA ligands. A different cobalt-based compound, 3-Co, forms at lower pH and lower reaction temperature. Its structure [P21/c; Z=2; a=12.6162(2) A, b=11.3768(2) A, and c=15.3401(3) A, beta=91.539(1) degrees] is a more loosely packed framework with free (noncoordinated) carboxylic groups pointing at water-filled cavities in the framework. The magnetic phase diagram of 1-Co established through detailed magnetic measurements shows a metamagnetic transition below TN=3.8 K. The less-packed compound 3-Co, on the other hand, remains paramagnetic above 1.9 K. The three compounds are the first examples of coordination polymers with benzenepentacarboxylate linkers and fill the gap of coordination polymers involving benzenepolycarboxylate linkers of the general type C6H6-n(COOH)n, where n=2-6.  相似文献   

5.
Tetraalkylammonium cations, (NR4)+ (R = C3H7, C4H9, and C5H11), have been used as templates to form a new family of [M(dca)3]- [M = Mn and Ni; dca = dicyanamide or N(CN)2(-)] salts. The tetrapropylammonium (TPrA) salts possess a perovskite-type anion structure. (TPrA)[Mn(dca)3] (1) crystallizes in the tetragonal space group P42(1)c, with a = 16.2945(8) A, c = 17.4321(8) A, and V = 4628.4(6) A(3) at T = 298 K. At room temperature, (TPrA)[Ni(dca)3] (2) crystallizes in the orthorhombic space group Pnna, with a = 17.171(2) A, b = 22.992(2) A, c = 22.750(2) A, and V = 8981(2) A3, but undergoes a first-order phase transition within the temperature range 150-220 K to the tetragonal space group P42(1)c, with a = 16.0985(7) A, c = 17.0287(8) A, and V = 4413.2(5) A3 at T = 160 K. At 110 K, 2 returns to the Pnna space group with a = 17.116(2) A, b = 22.800(3) A, c = 22.641(3) A, and V = 8835(3) A3. The tetrabutylammonium (TBA) salts possess a triple rutile structure. (TBA)[Mn(dca)3] (3) crystallizes in the orthorhombic space group P2(1)2(1)2, with a = 16.0107(6) A, b = 16.0114(6), c = 21.5577(8) A, and V = 5526.4(5) A3. (TBA)[Ni(dca)3] (4) also crystallizes in the orthorhombic space group P2(1)2(1)2, with a = 15.6842(5) A, b = 15.6841(6) A, c = 21.1551(8) A, and V = 5204.0(5) A3. The tetrapentylammonium (TPnA) salts crystallize with a LiSbO3 structure type, space group Pnna. Lattice parameters for (TPnA)[Mn(dca)3] (5) are a = 13.2236(6) A, b = 11.6300(6) A, c = 20.3176(9) A, and V = 3124.6(4) A3, and for (TPnA)[Ni(dca)3] (6), a = 12.9380(4) A, b = 11.6233(4) A, c = 19.8038(7) A, and V = 2978.1(2) A3. Long-range antiferromagnetic ordering has been observed in the manganese salts below 2.1 K, as indicated by alternating current susceptibility measurements. Magnetic susceptibility data for the nickel salts do not show evidence for long-range magnetic ordering but can be described using an S = 1 zero-field splitting model with the exchange Hamiltonian H = -J sigma(S(i)S(i+1)) + D sigma((S(i)z)2) + g mu(beta)B sigma(S(i)), giving absolute value(D)/kB values that range between 1.98(1) K and 3.20(2) K.  相似文献   

6.
We report the solvothermal synthesis and characterization of a series of layered lead phenylphosphonates. The crystals were suitable for single crystal X-ray diffraction data, and the two new structures we denote BING-6 [SUNY at Binghamton, Structure No. 6, Pb(PO(3)C(6)H(5)).0.25C(5)H(5)N, triclinic space group Ponemacr;, Z = 2, a = 7.0770(4) A, b = 9.3113(6) A, c = 14.6785(9) A, alpha = 80.456(1) degrees, beta = 78.023(1) degrees, gamma = 73.265(1)(o)] and BING-9 [Pb(PO(3)HC(6)H(5))(PO(3)HC(6)H(4)CH(3)), monoclinic space group C2/c, Z = 4, a = 32.663(8) A, b = 5.6220(13) A, c = 8.3307(19) A, beta = 101.419(4)(o)]. The third structure, a polytype of BING-9, was previously known only from powder X-ray diffraction methods and is denoted 3 [Pb(PO(3)HC(6)H(5))(2), monoclinic space group C2/c, Z = 4, a = 31.681(6) A, b = 5.5639(11) A, c = 8.2515(16) A, beta = 101.814(4)(o)]. All three structures possess Pb(II) and P centers connected by doubly and triply bridging oxygens. The phenyl groups cap and separate the charge-neutral layers. The phosphonates of BING-6 are nonprotonated, and the structure therefore has a Pb/P ratio of 1:1. Neutral, partially disordered pyridine solvent molecules also reside in the interlamellar space, increasing the layer to layer distance. BING-9 and 3 are polytypes and contain singly protonated phosphonates, for a Pb/P ratio of 1:2. Further characterization methods are discussed, including powder X-ray diffraction, in-situ variable temperature powder X-ray diffraction, thermogravimetric analysis, and scanning electron microscopy. Related work in the Ge, Sn, and Mn systems is also discussed. These low-dimensional materials may be useful intercalation compounds for ion-exchange or sensor applications.  相似文献   

7.
以六甲基二硅烷为原料,经氯代、格式反应和锂化反应制得双(环戊二烯基)配体(C5H5)2MeSiSiMe2R(3a^3c),将该配体分别与五羰基铁在对二甲苯中回流反应,合成了3种新型的硅基桥连双(环戊二烯基)四羰基二铁类配合物[η^5,η^5-C5H4MeSi(SiMe2R)C5H4]Fe2(CO)2(μ-CO)2[R=p-C6H4CH3(4a),R=p-C6H4OCH3(4b),R=CH2C6H5(4c)],其结构经1H NMR,13C NMR,IR和元素分析表征。并用X-射线单晶衍射法确定了配合物4b的分子结构。结果表明:4b(CCDC:1942618)属单斜晶系,Cc空间群,晶胞参数a=18.591(3)A,b=10.3080(10)A,c=14.136(2)A,α=90°,β=117.262(6)°,γ=90°,V=2408.1(6)A^3,Z=4,F(000)=1152,Dc=1.546 g·cm^-3,μ=1.338 mm^-1,R1=0.0351,wR2=0.0754。  相似文献   

8.
通过溶剂热技术,制得一种新型的Cd~(2+)配合物[Cd(L)_2(ba)_2]_2(1,L=4'-(4-甲基苯)-4,2':6',4″-三联吡啶,Hba=苯甲酸),其结构经IR,元素分析和单晶射线衍射表征。1属单斜晶系,空间群为P2_1/c,晶胞参数a=1.095 5(2)nm,b=1.404 1(3)nm,c=3.045 5(8)nm,β=103.37(3)°,V=4 557.6(18)3,D_c=1.459g·cm~(-3),Z=2,R_1=0.045 5,wR_2=0.094 0[I2σ(I)]。结构分析表明:1为零维双核结构,通过π…π堆积作用拓展为二维层状超分子。  相似文献   

9.
A series of novel uranium sulfates containing organic structure directing cations has been synthesized from amine sulfate precursors under hydrothermal conditions. The amine sulfates act as a soluble source of the protonated amines and sulfate ions at low temperature and provide a reaction pathway in which no amine decomposition is observed. The protonated amines act as both space fillers and hydrogen-bond donors in the three-dimensional structure. The factors governing the formation of the observed hydrogen-bonding networks were probed through the use of bond valence sums, which allow the quantification of residual negative charge and determination of the relative nucleophilicity of each oxide ligand. The hydrogen bonding in these new compounds is dependent upon two factors. First, the oxide ligands with the highest nucleophilicities are preferential acceptors with respect to their less nucleophilic counterparts. Second, geometric constraints that result from the formation of multiple hydrogen bonds from a single ammonium center can dictate the donation to oxides with smaller negative charges. Crystal data for [N4C6H12][SO4]2 x 2H2O, a = 7.2651(2) A, b = 7.3012(2) A, c = 8.3877(3) A, alpha = 90.260(1) degrees, beta = 100.323(1) degrees, gamma = 113.0294(15) degrees, triclinic, P-1 (No. 2), Z = 1; for [N4C6H22][UO2(H2O)(SO4)2]2 x 6H2O, a = 6.7318(1) A, b = 9.2975(1) A, c = 13.1457(3) A, alpha = 72.3395(6) degrees, beta = 89.1401(7) degrees, gamma = 70.0267(12) degrees, triclinic, P-1 (No. 2), Z = 1; for [N4C6H22][UO2(SO4)2)2, a = 9.3771(2) A, b = 12.9523(3) A, c = 18.9065(6) A, orthorhombic, Pbca (No. 61), Z = 4; for [N5C8H28]2[(UO2)5(H2O)5(SO4)10] x H2O, a = 7.76380(5) A, b = 14.16890(5) A, c = 56.46930(5) A, orthorhombic, Pbnm (No. 62), Z = 4.  相似文献   

10.
Flux conditions using liquid indium bypass the thermodynamically stable structure and yield new forms of the phases RENiGe2 (RE = Dy, Er, Yb, Lu). The compounds crystallize in the orthorhombic Immm space group and possess the YIrGe2 structure type. Lattice parameters for ErNiGe2, DyNiGe2, YbNiGe2, and LuNiGe2 are a = 4.114(1) A, b = 8.430(2) A, c = 15.741(5) A; a = 4.1784(9) A, b = 8.865(2) A, c = 15.745(3) A; a = 4.0935(6) A, b = 8.4277(13) A, c = 15.751(2) A, and a = 4.092(1) A, b = 8.418(3) A, c = 15.742(5) A, respectively. These phases represent a new structural arrangement (beta) of the compound type RENiGe2 as another set of compounds with identical stoichiometry are known to adopt the orthorhombic Cmcm CeNiSi2 type structure (alpha). In this paper we report the crystal and electronic band structure of four new members of the YIrGe2 structure type, as well as an investigation of the relative thermodynamic stabilities of the two forms.  相似文献   

11.
The synthesis, crystal structure, and physical characterization of the coordination compounds [Ni(en)2]4[Fe(CN)5NO]2[Fe(CN)6]x5H2O (1), [Ni(en)2][Fe(CN)5NO]x3H2O (2), [Mn(3-MeOsalen)(H2O)]2[Fe(CN)5NO] (3), and [Mn(5-Brsalen)]2[Fe(CN)5NO] (4) are presented. 1 crystallizes in the monoclinic space group P2(1)/n (a = 7.407(4) A, b = 28.963(6) A, c = 14.744(5) A, alpha = 90 degrees, beta = 103.26(4) degrees, gamma = 90 degrees, Z = 2). Its structure consists of branched linear chains formed by cis-[Ni(en)2]2+ cations and ferrocyanide and nitroprusside anions. The presence of two kinds of iron(II) sites has been demonstrated by M?ssbauer spectroscopy. 2 crystallizes in the monoclinic space group P2(1)/c (a = 11.076(3) A, b = 10.983(2) A, c = 17.018(5) A, alpha = 90 degrees, beta = 107.25(2) degrees, gamma = 90 degrees, Z = 4). Its structure consists of zigzag chains formed by an alternated array of cis-[Ni(en)2]2+ cations and nitroprusside anions. 3 crystallizes in the triclinic space group P1 (a = 8.896(5) A, b = 10.430(5) A, c = 12.699(5) A, alpha = 71.110(5) degrees, beta = 79.990(5) degrees, gamma = 89.470(5) degrees, Z = 1). Its structure comprises neutral trinuclear bimetallic complexes in which a central [Fe(CN)5NO]2- anion is linked to two [Mn(3-MeOsalen)]+ cations. 4 crystallizes in the tetragonal space group P4/ncc (a = 13.630(5) A, c = 21.420(8) A, Z = 4). Its structure shows an extended 2D neutral network formed by cyclic octameric [-Mn-NC-Fe-CN-]4 units. The magnetic properties of these compounds indicate the presence of quasi-isolated paramagnetic Ni2+ and Mn3+. Irradiated samples of the four compounds have been studied by differential scanning calorimetry to detect the existence of the long-lived metastable states of nitroprusside.  相似文献   

12.
雷晓武  岳呈阳 《结构化学》2012,31(3):389-395
A new intermetallic compound,YbCu6In6,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.YbCu6In6 crystallizes in tetragonal space group I4/mmm with a = 9.2283(5),c = 5.4015(4),V = 460.00(5) 3,Z = 2,Mr = 1243.20,Dc = 8.976 g/cm3,μ = 38.243 mm-1,F(000) = 1076,and the final R = 0.0258 and wR = 0.0602 for 173 observed reflections with I > 2σ(I).The structure of YbCu6In6 belongs to the ThMn12 type.It is isostructural with RECu6In6(RE = Y,Ce,Pr,Nd,Gd,Tb,Dy),containing one-dimensional(1D) [Cu10In6] cluster chain along the c axis,which is interconnected via sharing the Cu(1) atoms to form a three-dimensional(3D) [Cu6In6] framework with Yb atoms encapsulated in the 1D tunnels along the c axis.Band structure calculations based on Density Functional Theory(DFT) method indicate that YbCu6In6 is metallic.  相似文献   

13.
1 INTRODUCTION In the last decade, we have been interested in the synthesis of [PPh4][(h5-C5Me5)MS3] (M = Mo, W)[1, 2] , Whose organometallic trisulfido anions show high reactivity towards various transition metals[3~6] . We once reported that the reaction of [PPh4][(h5-C5Me5)WS3] with CuBr in CH3CN afforded a double incomplete-cubane cluster [PPh4]2[(h5-C5Me5)WS3(CuBr)3]2[3], while the analogous reaction of [PPh4][(h5-C5Me5)WS3] with CuBr in CHCl3 gave rise to a 揻our-…  相似文献   

14.
标题化合物C24H30O5是由邻甲氧基苯甲醛与5,5-二甲基-1,3-环己二酮在N,N-二甲基甲酰胺中反应而得。结构通过单晶X-射线衍射法确定,其晶体属于单斜晶系,空间群C2/c,a=33.942(6),b=7273(1),c=22667(4)A,β=128.989(9)°,Mr=398.50,V=4349(1)A3,Dc=1.2179·cm-3,Z=8,μ(MoKa)=840mm-1,F(000)=1712。晶体结构用直接法解出,经用全矩阵最小二乘法对原子参数进行修正,最后的偏离因子为R=0.043,Rw=0.052。在晶体结构中,存在一个分子间氢键。  相似文献   

15.
The first successful attempt to construct 3D supramolecular frameworks with high-nuclear 3d-4f heterometallic clusters as a node is reported. The self-assembly of Ln3+, Cu2+ and amino acid in solution leads to the formation of two polymers, 35-nuclear complex [Sm6Cu29] 1 with a primitive cubic net-like structure and 36-nuclear complex [Nd6Cu30] 2 with a face-centred cubic network type structure. Glycine and L-proline, respectively, were used as ligands. It should be noted that 2 has a chiral framework. X-ray structure analyses show that 1 crystallizes in the triclinic P1 space group (a=19.6451(8), b=20.4682(8), c=20.7046(8) A, alpha=89.453(1), beta=66.290(1), gamma=68.572(1) degrees, V=7003.0(5) A3 and Z=1) and 2 belongs to the cubic P2(1)3 space group (a=b=c=32.4341(3) A, V=34 119.7(5) A3 and Z=4). Both complexes utilize Ln6Cu24 octahedral clusters as nodes and trans-Cu(amino acid)2 groups as bridges. Electrical conductivity measurements reveal that both polymers behave as semiconductors.  相似文献   

16.
A rare micro6-oxo-centered Mn6 mixed-valent cluster (1) is prepared and used as a secondary building unit for the self-assembly of its azido-bridged polymeric analogue (2) in a systematic way with the retention of the Mn6 core of 1. Both complexes are characterized by X-ray single-crystal structure determination. The complex 1 was crystallized in a monoclinic system, space group P21, a=11.252(5) A, b=20.893(9) A, c=12.301(6) A, and beta=115.853(7) degrees, whereas the polymeric analogue 2 was crystallized in an orthorhombic system, space group P212121, a=13.1941(8) A, b=14.9897(9) A, and c=27.8746(14) A. Variable-temperature magnetic behavior showed the presence of strong antiferromagnetic interaction in both cases.  相似文献   

17.
The crystal structure of 1-[(1'-phenyl-5'-methyl-4'-pyrazolcarbonyl)]-3-methyl thio-5-amino-1H-yl-1,2,4-triazole (C14H14N6OS, Mr = 314.37) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic, space group P with a = 8.026(3), b = 8.651(4), c = 11.369(5) (A), α = 89.917(7), β= 89.084(7), γ = 68.470(6)°, V = 734.2(5) (A)3, Z = 2, Dc = 1.422 g/cm3, ( = 0.232 mm-1, F(000) = 328, R = 0.0376 and wR = 0.0890 for 2950 unique reflections. The crystal structure shows the presence of a dimmer with intermolecular N(4)-H(4)…N(3A) hydrogen bonds.  相似文献   

18.
刘扬  刘秀华 《结构化学》1990,9(2):87-89
<正> C11H13 N3 O5·t-Bu- N = CHC6H3(NO2)2,Mr = 267. 27, Monoclinic space group C2/c,a= 18. 546(3),b = 5. 729(1),c= 27. 479(5) A,β= 118. 42(1)°/,F = 2567. 6(9)A3,F(000) = 1120,Z=8,Dx=1. 38g/cm3. The structure of DNPBN is akin to that of PBN reported by us except for shorter N - O and C = N bonds.  相似文献   

19.
本文报道了(η~5-C_5H_4C_3H_7—i)_2Mo_2(CO)_6的合成及晶体结构。晶体属于三斜晶系,空间群P,晶胞参数a=7.548(2),b=8.662(1),c=8.888(1),a=91.11(1),β=106.43(1),γ=92.59(1)°,V=556.48,M_r=574.3,Z=1,D_x=1.714g/cm~3,μ(MoKα)=11.33cm~(-1),F(000)=286。最后偏离因子R=0.016。分子具有C_i对称性。分子中存在Mo—Mo单键,键长为3.222。异丙基的引入使得茂环与金属钼的键合加强。  相似文献   

20.
Six new zirconogermanates have been prepared under hydrothermal conditions using amines as bases. There are four new structure types (ASU-n) with a common motif of ZrGe(5). ASU-23 is a layered structure: ZrGe(3)O(8)(OH)F.[C(10)H(26)N(4)].H(2)O, space group P2(1)/n, a = 6.7957(8) A, b = 12.700(1) A, c = 24.293(3) A, beta = 97.936(2) degrees, V = 2076.4(4) A(3). ASU-24 is a pillared layered structure: Zr(3)Ge(6)O(18)(OH(2),F)(4)F(2).[C(6)H(18)N(2)].[C(6)H(17)N(2)](2).2H(2)O, space group P2(1)/n, a = 7.4249(3) A, b = 25.198(1) A, c = 11.3483(5) A, beta = 90.995(1) degrees, V = 2122.9(2) A(3). This material has the lowest framework density (FD) of any oxide material that we are aware of (FD = 8.48 metal atoms/nm(3)). Two other materials form three-dimensional open-frameworks, ASU-25: ZrGe(3)O(9).[C(3)H(12)N(2)], space group P112(1)/a, a = 13.1994(4) A, b = 7.6828(2) A, c = 11.2373(3) A, gamma = 91.233(3) degrees, V = 1139.29(5) A(3). The other is ASU-26: ZrGe(3)O(9).[C(2)H(10)N(2)], space group Pn, a = 13.7611(3) A, b = 7.7294(2) A, c = 11.2331(3) A, beta = 104.793(1) degrees, V = 1155.21(4) A(3). ASU-25 is related to the mineral umbite K(2)ZrSi(3)O(9).H(2)O. The germanium equivalent has been prepared through the inorganic route: K(2)ZrGe(3)O(9).H(2)O, space group P2(1)2(1)2(1), a = 13.6432(6) A, b = 7.4256(3) A, c = 10.3973(4) A, V = 1053.33(8) A(3). The structural relationships between ASU-25 and its inorganic counterpart are described. The thermal decomposition of the germanium umbite generated the cyclic trigermanate K(2)ZrGe(3)O(9), analogue of the mineral wadeite, crystallizing in the orthorhombic system, a = 7.076 A, b = 12.123 A, c = 10.451 A, V = 904.5 A(3).  相似文献   

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