THE CRYSTAL STRUCTURE OF A NOVEL TETRANUCLEAR SILVER CLUSTER COMPLEX Ag_4(α-C_(10)H_7CS_2)_4(Py)_4·2Py

The title compound has been synthesized by the reaction of α-dithionaphthoic acidwith AgNO_3 in an organic solvent. The single crystals were obtained by recrystallizingfrom pyridine. We obtained two kinds of crystal with different colours (A and B), usingdifferent ratios of silver nitrate and α-dithionaphthoic acid (1:2,1:4) in the reactions. The structures of the two kinds of crystal were determined by a single-crystal X-raydiffraction analysis. The crystal (A) belongs to monoclinic space group C_(2h)~5-P2_1/a withunit cell parameters: a = 22.822(4) A, b = 12.803 (4) A, c = 24.444 (7) A, β = 103.90 (2)°V = 6933.14 A~3, Z = 4. The crystal (B) belongs to monoclinic space group C_(2h)~6-C2/c witha = 29.150 (2) A, b = 12.799 (3) A, c = 24.413 (2) A, β = 130.56 (4)°, V = 6914.38 A~3,Z = 4. Both crystals (A) and (B) have the same molecular configuration, but they havedifferent symmetry. In crystal (B), the molecule possesses a C_2 symmetry. This paperreports the structure determination and parameters o     

CRYSTAL AND MOLECULAR STRUCTURE OF [Cu_2(α-C_(10)H_7-CH_2CO_2)_4(DMF)_2](DMF)_2· H_2O

<正> The title complex crystallizes in the triclinic system, space group P1, a =11. 912(4), b = 13. 626(2), c=10. 040(3)(?), a=95. 03(2) ,β= 114. 8 (3), γ = 73. 58(3)°, V = 1418.0(?)3, Z = 1, D,= 1. 37g/cm3, F(000) = 612, R = 0. 064 for 4860 independent reflections [I>3σ(I)]. Each Cu atom is coordinated by the oxygen atoms from the C10H7CH2COO groups and DMF in a square pyramid geometry.     

SYNTHESIS,CRYSTAL STRUCTURE AND MAGNETISM OF THE COMPLEX:GdFe(CN)_64H_2O

ＳＹＮＴＨＥＳＩＳ，ＣＲＹＳＴＡＬ　ＳＴＲＵＣＴＵＲＥ　ＡＮＤ　ＭＡＧＮＥＴＩＳＭ　ＯＦ　ＴＨＥ　ＣＯＭＰＬＥＸ：ＧｄＦｅ（ＣＮ）_６４Ｈ_２ＯＳＹＮＴＨＥＳＩＳ，ＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＡＮＤＭＡＧＮＥＴＩＳＭＯＦＴＨＥＣＯＭＰＬＥＸ：ＧｄＦ...     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF A NOVEL MOLYBDENUM-SULFUR CLUSTER COMPLEX, (NH_4)_4[Mo_3(NO)_4S_(13)]·3H_2O

The title compound has been synthesized, the crystal structure of which has been detorminedby the single-crystal X-ray diffraction method. The crystal belongs to triclinic space group C-P1 with the unit cell parameters: a =9.535(2)A, b = 9.740(2)A, c = 15.795(4)A, α = 89.85(2)°, β = 91.80(2)°, γ = 99.37(1)°,ν = 1446.6A~3, Ζ = 2. The structure is refined to R = 0.075, R_w = 0.074 for 1903 reflections. There are diverse bonding modes of molybdenum and sulfur in this eompound. The twosulfur atoms at the center bond to three molybdenum atoms from respective sides and formthe two apices of a trigonal bipyramid. Besides, there are S_2~(-2) ligands and a polysulfur chaincomposed of three sulfur atoms. The coordination number for the three molybdenum atomsis seven. Their coordination polyhedra are somewhat distorted pentagonal bipyramid. Eachof the three NO ligands coordinated to molybdenum gives a linear group of Mo-N-O, whilethe fourth NO ligund bonded with a polysulfur chain forms a bent group of S-N     

CRYSTAL STRUCTURE OF FIVE-COORDINATE ZIRCONOCENE COMPLEX (MeCp)_2ZrC1(α-C_(10)H_7COO)

(MeCp)_2ZrCl(&-C_(10)H_7COO)has five-coordinate bentzirconocene in which the-naphthoyloxyis a bidentate ligand(Zr-O 2.317(2),2.260(2)(?);Zr-Cl 2.521(1);Zr-C 2.480-2.550;Zr-cent-CH_3C_5H_4 2.217,2.23OA;Cl-Zr-O1 134.8(1)~O;Cl-Zr-O2 78.6(1)~O;O1-Zr-O2 56.3(1)~O).     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF NdBr_3(i-C_3H_7OH)_2(THF)_2

ＴＨＥ　ＳＹＮＴＨＥＳＩＳ　ＡＮＤ　ＣＲＹＳＴＡＬ　ＳＴＲＵＣＴＵＲＥ　ＯＦ　ＮｄＢｒ＿３（ｉ－Ｃ＿３Ｈ＿７ＯＨ）＿２（ＴＨＦ）＿２￥ＨｏｎｇＹｅＳＵＮ；ＣｈｕｎＨｕｉＨＵＡＮＧａｎｄＧｕａｎｇＸｉａｎＸＵ（ＲｅｓｅａｒｃｈＣｅｎｔｅｒｏｆＲａｒｅＥ...     

SYNTHESIS AND CRYSTAL STRUCTURE OF THE CLUSTER COMPOUND MoS_4Cu_2Ag（Ph_3P）_3Br．H_2O

ＳＹＮＴＨＥＳＩＳ ＡＮＤ ＣＲＹＳＴＡＬ ＳＴＲＵＣＴＵＲＥ ＯＦ ＴＨＥ ＣＬＵＳＴＥＲ ＣＯＭＰＯＵＮＤ ＭｏＳ_４Ｃｕ_２Ａｇ（Ｐｈ_３Ｐ）_３Ｂｒ．Ｈ_２Ｏ￥ＤｅＬｉａｎｇＬＯＮＧ；ＸｉｎＱｕａｎＸＩＮ（ＳｔａｌｅＫｅｙＬａｂｏｒａｔｏｒｙｏｆ?..     

SYNTHESIS AND CRYSTAL STRUCTURE OF A MOLYBDENUM-COPPER-SULFUR CLUSTER COMPLEX WITH DITHIOBENZOATE LIGAND [Bu_4N]_2[MoCu_2S_4(C_6H_5CS_2)_2]

<正> The title compound has been synthesized by the reaction of (Bu4N)2MoS4, CuCl and (C6H5CS2)(Bu4N) in DMF and recrystallized from DMF/ Et2O. The red black crystal belongs to the triclinic space group P1 with a = 12. 021 (6), b = 17.045(8), c=17. 136(7)(?) , α=110.05(3), β=108.64(4), γ=103.87 (4)°, V = 2873(3)(?)3, Dc=1. 321gcm-3, Z = 2. The structure was refined to R = 0. 065 for .4783 reflections. The anion of the title compound can be described as a MoS42- tetrahedron coordinated by two [Cu(C6H5CS2)] units with the three metal atoms lying on a line. The coordination number of each Cu atom is three.     

SYNTHESIS AND STRUCTURE OF A NOVEL INFINITE-LAYER COPPER(Ⅱ)COMPLEX BRIDGED BY OXAMIDE AND PYRIMIDINE

The complex polymer[Cu_2(oxap)(pyr)_2]_n(ClO_4)_(2n),where oxap~(2-)stands for N,N'-bis(2—aminopropyl)oxamide,have been synthesized.It crystallizes in monoclinic system,space group P2_1/C,with a=8.721(2),b=8.679(2),c=16.741(2),β=98.59(0),Z=4.Theleast-square refinement coverged at R=0.054,R_w=0.055 with 1869 unique reflections.Thewhole structure of the complcx consists of layers of two-dimensional network arrayingalong a-axis with perchlorate ions interspersed in the gap between layers.Inside the layer.trans-oxamide-bridged copper(Ⅱ)dimers connected by pyrimidine in an asymmetric fashionspread out along be plane to form an infinite two-dimensional network.     

CRYSTAL STRUCTURE OF A NOVEL TETRANUCLEAR MIXED-METAL CLUSTER Mo_2Fe_2Te_3(CO)_6(C_3H_3)_2

<正> Mr = 984. 63, orthorhombic Imm2, a = 14.562(3), b = 10.391(1), c = 7.139(4) A; V = 1080.2(1) A3, Z = 2, DC = 3.027 g.cm-3. Final R= 0.022 for 620 reflections with I > 20(Ⅰ). In the title compound, four metal atoms form a butterfly configuration, one ,μ-Te is bonded to these four metals and two μ3-Te cap two Fe-Mo-Mo faces. All these atoms as a whole give a bicapped trigonal bipyramidal structure.     

THE CRYSTAL AND MOLECULAR STRUCTURE OF Cu_2(■-OCH_2COO)_4(DMF)_2

<正> INTRODUCTION. The complexes of some transition metals with plant growth regulators still have growth-regulating activity. For example the copper(Ⅱ) chelates of N-phenyl thalaminic acid derivatives are this type complexes. We have synthesized complex of Cu(Ⅱ) with β-naphthoxyacetic acid which has the action of stimulating plant growth. The crystal structure of Cu_2(β-C_(10)oH_7OCH_2COO)_4(DMF)_2 has been determined.     

CRYSTAL STRUCTURE OF TETRANUCLEAR MIXED METAL CLUSTER Fe_2Mo_2Te_2(CO)_7(C_5H_5)_2

<正> The title compound is orthorhombic, space group Pbn2 , with a=12.172(5), b=13.595(2), c=12.924(4), V=2138.5(2) ~3, z=4, Dx=2.749 g/cm~3. The octahedral-shaped black crystal was selected for data collection on a CAD-4 diffractometer, using graphite monochromator Moka radiation (λ=0.7107), ω-2θ     

SYNTHESIS AND STRUCTURE OF THE DINUCLEAR MANGANESE-SULFUR COMPLEX (Ph_4As)_2Mn_2(SC_3H_6S)_4

<正> (Ph4As)2[Mn2(SC3H8S)4] was obtained from the reaction of MnCl2-4H2O,Na2(1,2-pdt)(1,2-H2pdt=CH3CH(SH)CH2SH),and Ph4AsCl.C80H64As2Mn2S8, Mr =1301.41,orthorhombic,Pbca; a=10.854(2), b =22.562(6), c =24.545(6)A; V=6010.8A3;Z =4,Dc=1.44g/cm3. The centrosymmetic anion of title compound is a dimer of (Mn(pdt)2]- bridged by one sulfur atom each of the two bridging pdt2-, The atom Mo(Ⅲ) is in a distorted trigonal bipyramidal geometry.     

CRYSTAL AND MOLECULAR STRUCTURE OF TETRANUCLEAR MOLYBDENUM CLUSTER Mo_4(μ_3-O)_2Cl_2(o-CH_3C_6H_4COO)_6

<正> Cluster compound [Mo4(μ3-O)2O4Cl2(o-CH3C6H4COO)6] has been prepared by the reaction of molybdenum pentachloride and o-methylbenzoic acid. It crystllizes in the orthorhombic space group Praia with cell parameters:Mr= 1361. 6,a=13. 792(4), b=17. 957(3),c= 20. 974(9) A ,V=5194(2) A3,Z= 4,Dc= 1. 74g/cm3,F(000) = 2704,μ(MoKa) = 11. 0/cm. The final R=0. 061 and Rw=0. 064 for 1441(I>3oooooooooo(I)) observed unique reflections. The tetranuclear complex molecule, where the molybdenum atoms are bridged by two μ3-O atoms and six bidentate o-methylbenzoato ligands,is located at crystallographic two-fold axis(x,-1/4,1/4) with one Mo-Mo bond of 2. 610A     

SYNTHESIS AND CRYSTAL STRUCTURE OF [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2

All attempts to prepare light lanthanide dicyclopeutadienyt chloride failed,due to the disproportionation reaction. The crystal complex of [(η~5-C_5H_5)_2NdCl.OC_4H_8]_2 was successfully prepared by the reaction of NdCl_3·2C_4H_8O with cyclopentadienyl sodium (molar ratio 1:1.8)in tetrahydrofuran at room temperatureThe composition of the title compound was determined by the methods of elemental analysis, infrared spectroscopy and photoelectron spectroscopy. The crystal structure of [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2 was determined from single crystal X-ray diffraction. Data were collected at-60℃ under dry nitrogen atmosphere.The complex crystallizes in the monoclinic space group P2_1/c,with Z=2. Lattice parameters are: a=8.201(3), b=21.589(6),c=8.596(3),β=109.10(3)°.The structure was solved by Patterson and Fourier techniques and refined by least-squares to a final conventional R=0.0636 for 1680 reflections. There are two Nd atoms in the dimeric unit which are bridged asymmetrically by the two chlori     

SYNTHESIS AND STRUCTURE OF TETRANUCLEAR MOLYBDENUM CLUSTER COMPOUND[Mo_4S_4(μ-O_2CC_6H_5)_2(dtp)_4]

The cluster compound[Mo_4S_4(μ-O_2CC_5H_5)_2(dtp)_4](dtp=S_2P(OEt)_2)wasobtained by the ligand substitution reaction of tetranuclear molybdenum cluster[Mo_4S_4(μ-dtp)_2(dtp)_4]in the mixed solvent of acetone,ethanol and water in thepresence of C_6H_5CO_2Na.It is monoclinic and crystallizes in space group C2/c,Mr=1495.09,a=12.175(5),b=22.01(1),c=20.875(9),β=99.04(4)°;V=5575(5);Z=4;Dc=1.78g/cm~3.Final R factor is 0.066.The result reveals that the[Mo_4S_4]clustercore and t-(dtp)~(-1)ligands are retained and only μ-bridged(dtp)~(-1)ligands aresubstituted by(C_6H_5CO_2)~(-1)in the substitution reaction,thus producing the newtitle cluster compound,the structure of which contains two species of bidentateligand.     

SYNTHESIS AND CRYSTAL STRUCTURE OF MgCl_2(CH_3COOC_2H_5)_2

The crystal of the title compound was prepared and its structure determined by X-ray diffraction method.1672 independent reflections were collected. The crystal is orthogonal with space group P2_12_12, and a=7.353(3),b=25.111(10), c=8.631(2), Z=8. The structure was solved by using Patterson method and modified with LSM program.The final R= 0.0795. The structural features of the title compound are:Mg(Ⅱ) is octahedral and ethyl acetate is located on trans-position.Mg atoms are connected by double chloro-bridge and form polychains.     

THE FORMATION AND CRYSTAL STRUCTURE OF (η~5-C_5H_5)_3Nd·OC_4H_8 AND (η~5-C_5H_5)_3Pr·OC_4H_8

Under suitable reactant ratios without sublimation or reerystallization, single crystals of(η~5-C_5,H_5)_3 Ln-OC_4H_8(In = La, Pr, Nd) could be prepared by the reaction of cyclopentadienylsodium with respective lanthanide trichlorides in THF. Using low temperature technique wehave collected the X-ray data of single crystals of the title compounds at -60℃ under N_2and determined crystal structures. (η~5-C_5H_5)_3 Pr·OC_4H_8, [(η_5-C_5H_5)_3 Nd·OC_4H_8] recrystallizesin the monoclinic space group P2_1/n[P2_1/n] with unit cell parameters a = 8.406(3) [8.364(3)],b = 24. 510(9) [24.467(9)], c = 8. 284(3) [8.254(3)] A, β= 101.60(3) [101.42 (3)], D_c = 1. 62 [1.65]gem~(-3) for z = 4 [4]. Least-square refinement has led to a final R value of 0.056 [0.063],R_W = 0.049 [0.062]. The THF molecule is coordinated to the Pr [Nd] atom at a Pr-O [Nd-O]bond length of 2.16(1) [2.54(1)], A. The Pr-C (Cp) [Nd-C(Cp)] bond distances average 2.80(2) [2.78(2)] A. The title compounds are isostructaral with (η~5-C_5H_5)_3     

SYNTHESIS AND CRYSTAL STRUCTURE OF Ta_3(Te_2)_6

<正> Ta3(Te2)6, Mr = 2074. 04, tetragonal, P4/ncc, a = 9. 204(1) A , c=20,401(8) A, V=1728. 3 A 3, Z = 4, Dc = 7. 97g/cm3, λ(MoKa) = 0. 71073 A . μ= 386, 3cm-1,F(000) = 3372, T= 296K , R= 0. 027, Rw = 0, 029 for 493 observed unique reflections. The structure is composed of infinite [TaTe4] chains along the e axis. In these chains, the Ta sequences distort in such a way that linear Ta, clusters are formed.     

SYNTHESIS， STRUCTURE AND PROPERTIES OF THE COMPLEX OF COPPER CHLORIDE WITH A STABLE RADICAL

ＳＹＮＴＨＥＳＩＳ，ＳＴＲＵＣＴＵＲＥＡＮＤＰＲＯＰＥＲＴＩＥＳＯＦＴＨＥＣＯＭＰＬＥＸＯＦＣＯＰＰＥＲＣＨＬＯＲＩＤＥＷＩＴＨＡＳＴＡＢＬＥＲＡＤＩＣＡＬ￥ＺｏｎｇＨｕｉＪＩＡＮＧ；ＢａｉＷａｎｇＳＵＮ；ＤａｉＺｈｅｎｇＬＩＡＯ；ＷｅｉＺＨＡＮＧ；...