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水、氯配位的Shiff碱单核及双核锰化合物的合成与结构表征

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化学学报 2002年第7期60卷 1242-1247页

作者：黄德光陈昌能朱红平刘秋田中国科学院福建物质结构研究所结构化学国家重点实验室福州350002

在水杨醛与二元胺形成的Schiff碱与Mn盐的反应体系中 ,分离出两个单核Mn化合物 ,(salen)Mn(H2 O)Cl(1)和 [(salpr)Mn(H2 O) 2 ]Cl (2 ) ,并测定了结构 .应用对苯二甲酸在碱性条件下拉接两个单核Mn的Schiff碱配位单元 ,生成 (salen) 2 Mn... 详细信息

在水杨醛与二元胺形成的Schiff碱与Mn盐的反应体系中 ,分离出两个单核Mn化合物 ,(salen)Mn(H2 O)Cl(1)和 [(salpr)Mn(H2 O) 2 ]Cl (2 ) ,并测定了结构 .应用对苯二甲酸在碱性条件下拉接两个单核Mn的Schiff碱配位单元 ,生成 (salen) 2 Mn2 [μ p C6H4 (COO) 2 ](H2 O) (CH3 OH) (3)并进行了结构表征 .讨论了这些化合物的红外及1HNMR谱。

关键词：合成结构表征锰配合物晶体结构 Schiff碱光系统Ⅱ 水氯配体

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

Synthesis and Crystal Structure of a 2D Cu Framework Constructed from Dinuclear Building Units

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Chinese Journal of Structural Chemistry 2014年第12期33卷 1807-1812页

作者：陈惠马成丙陈昌能 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences University of Chinese Academy of Sciences

A novel 2D Cu coordination polymer [Cu4(pca)4(H2O)2(DMSO)2·2DMSO·2H2O]n(2, H2 pca = pyrazole-3-carboxylic acid) has been prepared by dissolving a dinuclear Cu complex Cu2(py)3(pca)2(H2O)·(H2O)(1) in DMSO solution and structurally characterized by X-ray diffraction. The polymer crystallizes in space group P1 with a = 9.538(3), b = 9.714(3), c = 10.765(3) A, α = 86.492(6), β = 84.007(7), γ = 82.592(6)o, Mr = 1079.04, V = 982.4(5) A3, Z = 1, Dc = 1.824 g/cm3, μ = 2.425 mm-1 and F(000) = 548. The final refinement gave R = 0.0785 and w R = 0.1940 for 2787 reflections with I > 2σ(I). The structure of 2 consists of Cu4(pca)4(H2O)2(DMSO)2·2DMSO·2H2O units, which can be viewed as two dinuclear subunits of Cu2(pca)2(H2O)2 and Cu2(pca)2(DMSO)2 connected to each other alternately, with solvent DMSO and H2 O molecules around. The framework features a grid-like topology, with the walls of the grids composed of Cu4(pca)4 units, and the coordinated solvent molecules trapped in the grids.

关键词： copper coordination polymer crystal structure building block

Synthesis and Crystal Structure of Mn(phen)(CF_3COO)(H_2O)_3·NO_3

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Chinese Journal of Structural Chemistry 2004年第8期23卷 908-911页

作者：王文国陈昌能刘秋田 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China

The mononuclear manganese complex Mn(phen)(CF3COO)(H2O)3NO3 (C14H14- O8N3F3Mn) has been synthesized, where phen = 1,10-phenanthroline. The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 8.8550(3), b = 10.6529(3), c = 19.8763(2) ? ?= 97.762(2), V = 1857.78(8) 3, Z = 4, Mr = 464.22, Dc = 1.660 g/cm3, ?= 0.789 mm-1, F(000) = 940, T = 293(2) K, R = 0.0764 and wR = 0.2441 for 1995 observed reflections with I > 2s(I). In the crystal the manganese atom is six-coordinated by two chelated nitrogen atoms from phenanthroline, three oxygen atoms from water molecules and one oxygen atom from trifluoroacetate, completing an octahedral geometry.

关键词： manganese complex crystal structure trifluoroacetate

二核Fe/S化合物(Et_4N)_2[Fe_2S_2Br_4]的合成与结构

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化学学报 1999年第8期57卷 846-851页

作者：邓玉恒温庭斌朱红平陈昌能刘秋田首都师范大学化学系中国科学院福建物质结构研究所

标题化合物(Et_4N)_2[Fe_2S_2Br_4](1)在VS_4^(3-)/FeBr_2/imnt^(2-)/Et_4NCI的反应体系中获得,它属于单斜晶系,空间群P2_1/n,主要晶胞参数为:α=0.91193(2)nm,b=1.03874(3)nm,c=1.54360(1)nm,β=105.090(1)°,V=1.41177(5)nm^3,Z=2, ρ=1.778g/cm^3,μ=6.841cm^(-1),F(000)=748,结构精修结果为:R_1=0.0287,wR_2=0.0640.簇阴离子[Fe_2S_2Br_4]^(2-)含有一个菱形Fe_2S_2单元,铁的配位几何构型明显偏离了理想的T_d对称性,导致整个阴离子的对称性降低为D_(2h).同时观察到它的Fe-Br键呈现反常加长倾向.

关键词：晶体结构铁硫化合物铁硫蛋白活性中心模拟物

Activation of Nitromethane to Cyanide by a Mononuclear Cu(Ⅱ) Complex

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Chinese Journal of Structural Chemistry 2014年第11期33卷 1643-1648页

作者：吴楠楠陈昌能黄德光 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences University of Chinese Academy of Sciences

The tridentate ligand DPA-Me（2） was readily prepared from DPA（DPA = 2,2-dipicolylamine） in high yield. The mixture of 2 and Cu（ClO4）26H2O in methanol gave a five-coordinated mononuclear complex [（DPA-Me）Cu（Me CN）（ClO4）]（ClO4）（3）. Recrystallization of 3 in CH3NO2 led to an activation of CH3NO2 to CN- by the formation of product as a dinuclear cyanide bridged complex {[Cu（DPA-Me）]2（CN）（ClO4）3CH3NO2}n（4）. Both 3 and 4 were characterized by X-ray crystallography, IR spectroscopy and elemental analysis. The crystal of 4 was grown in space group P21/c with a = 17.74582（15）, b = 13.89877（11）, c = 14.92546（13） A, β = 91.4246（8）°, V = 3680.15（5） 3, Z = 4, Dc = 1.695 g/cm^3, F（000） = 1912, C28H33Cl3Cu2N8O14, Mr = 939.05, μ = 1.602 cm^-1, Cu Kα radiation（λ = 1.54184 ）, R = 0.0485 and w R = 0.1246 for 6414 observed reflections with I 〉 2σ（I）.

关键词： tridentate ligand,copper,activation,nitromethane,cyanide

六核簇合物[Mn4Ln2]的合成与晶体结构研究

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六核簇合物[Mn4Ln2]的合成与晶体结构研究

Synthesis and Crystal Structure of Mn(phen)(PhCOO)_2(H_2O)

中国化学会第九届全国无机化学学术会议

作者：孙磊陈昌能中国科学院福建物质结构研究所

近年来锰-稀土异金属簇合物作为分子基磁体由于其独特的性能引起了人们的广泛关注[1]。相比于传统的无机磁性材料,分子基材料具有体积小、耗能小、结构多样等优点[2]。最近,我们合成出一种新的锰-稀土异金属六核簇合物:[Mn4Pr2（O）2（... 详细信息

近年来锰-稀土异金属簇合物作为分子基磁体由于其独特的性能引起了人们的广泛关注[1]。相比于传统的无机磁性材料,分子基材料具有体积小、耗能小、结构多样等优点[2]。最近,我们合成出一种新的锰-稀土异金属六核簇合物:[Mn4Pr2（O）2（hmp）4（O2CPh）6（NO3）4]。该簇合物属于单斜晶系,P 1 21/c 1空间群。其晶体学数据为:a=14.8125A,b=13.8251A,c=19.4672A,α=90°,β=101.766°,γ=90°,V=3902.80A3,Z=2。通过化合价平衡以及价键和理论（BVS）[3]计算确定四个Mn原子的氧化态为+3价。根据配位化学的有关原理,d4（Mn3+）容易发生Jahn-Teller效应,使得正八面体发生畸变。在该簇合物中,每个MnⅢ都是六配位的,中心均为拉长的八面体配位方式,沿着Jahn-Teller伸长轴O1-Mn1-O12,O3-Mn2-O6,O1A-Mn1A-O12A和O3A-Mn2A-O6A拉长的四个键长（如图所示）,轴向位置的键长比水平面的键长长0.256-0.39A。两个Pr原子为九个氧原子配位。其磁性的研究还在进一步的进行中。

关键词：锰-镧异金属簇合物磁性

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Chinese Journal of Structural Chemistry 2003年第4期22卷 399-402页

作者：王文国陈峰陈昌能刘秋田 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China

The manganese benzoate complex Mn(phen)(PhCOO)2(H2O) (C26H20MnN2O5) has been synthesized, where phen = 1,10-phenanthroline. The molecular and crystal structures were determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with unit cell parameters: a = 10.7145(7), b = 21.218(1), c = 11.2743(7) ? ?= 117.7342(2), V = 2268.6(3) ?, Z = 4, Mr = 495.38, Dc = 1.450 g/cm3, ?= 0.623 mm-1, F(000) = 1020, T = 293(2) K, R = 0.0563 and wR = 0.1339 for 2468 observed reflections with I > 2s(I). In the crystal the manganese atom is five-coordinated by two chelated nitrogen atoms from phenanthroline, three oxygen atoms from two benzoates and one water molecule, completing a triangular bipyramid geometry. The complex exists in a dimer mode by intermolecular hydrogen-bonding interactions.

关键词：合成晶体结构 Mn(phen)(PhCOO)2(H2O) 锰配合物苯甲酸酯邻二氮杂菲

Synthesis and Crystal Structure of a New Three-dimensional Coordination Polymer:[Mn(2,3-pdc) (H_2O)]_n (2,3-pdc=Pyridine-2,3-dicarboxylate)

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Chinese Journal of Structural Chemistry 2008年第11期27卷 1370-1374页

作者：张春霞马成丙王梅陈昌能 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences Graduate School of the Chinese Academy of Sciences

A new three-dimensional coordination polymer [Mn（2,3-pdc）（H20）]n （2,3-pdc = pyridine-2,3-dicarboxylate） 1 has been hydrothermally synthesized and structurally characterized. The crystal belongs to the monoclinic system, space group P21/c with a = 6.4168（5）, b = 10.7939（9）, c = 11.1549（10） A, β = 94.733（4）°, V = 769.98（11） A3, Z = 4, Mr = 238.06, De = 2.054 g/cm3, μ（MoKa） = 1.707 mm-1, F（000） = 476, Rint = 0.0326; R = 0.0499 and wR = 0.1636 for 1564 observed reflections with I 〉 2σ（I）. X-ray diffraction analyses reveal that the title compound is a three-dimensional coordination polymer consisting of one MnⅡ center with a distorted octahedral environment arranged by four 2,3-pdc ligands and one water molecule.

关键词： manganese crystal structure pyridinedicarboxylate coordinated polymer