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1.
Fangfang Jian Kui Jiao Qingxiang Wang Huanxiang Wang 《Journal of chemical crystallography》2004,34(2):147-151
The mononuclear complex, Ni[N3-ImSP(OiPr)2]2[S2P(OiPr)2]2 (Im = imidazole; iPr = isopropyl), was unexpectedly obtained in a reaction of bis(O,O-diisopropyl-dithiophosphato) nickel(II) complex with imidazole ligand, and its structure was determined by X-ray crystallography. It crystallizes in the triclinic system, space group P
, with lattice parameters a = 12.437(3) Å, b = 13.181(3) Å, c = 8.4580(17) Å, = 93.16(3)°, = 101.93(3)°, = 65.26(3)°, and Z = 1. The Ni atom has almost perfect octahedral coordination geometry and is coordinated by two N atoms of imidazole from two O,O-diisopropylthiophosphoryl-1H-imidazole ligands in axial positions and four S atoms from two (O,O-diisopropyldithiophosphato) anions which act as bidentate ligands forming a four-membered chelate ring in the equatorial plane. The Ni—S bond distances are 2.469(1) and 2.507(1) Å, and the Ni—N bond distances are 2.097(2) Å. The IR spectra data are in agreement with the structural data. 相似文献
2.
三维孔道结构(H3 NCH2 CH2 NH3)2(H3 NCH2 CH2 NH2)[VⅢ(H2O)2(VⅣ O)8(OH)4(H(P,B)O4)4((P,B)O4)4(H2O)2]·3H2O的水热合成及晶体化学研究 --(2)晶体结构与晶体化学 总被引:3,自引:3,他引:0
在单晶X射线衍射实验的基础上,对孔道结构化合物V9P8-en的类质同象物V9(P,B)8-en的晶体结构和晶体化学进行了深入研究.结果表明,该化合物的晶体学数据为:P2(1)/n,a=1.43134(9)nm,b=1.01256(6)nm,c=1.83156(12)nm,β=90.280(2)°,V=2.6545(3)nm3,Z=2,R=0.0540,wR2=0.1551.结构中,沿着三个结晶轴方向发育复杂而规整的三维孔道,最大孔径达1.83nm(∥b轴),质子化乙二胺和水分子居于孔道中.硼部分替代四面体配位的磷,替代率为B8:P8=0.1838:7.8162;其中B与{P-OH}位P的替代量大于与[P-O]位P的替代量.相对于V9P8-en来说,V9(P,B)8-en的晶胞参数发生了变化,导致b轴增长(1.0150→1.0256nm)和c轴缩短(1.8374→1.8316nm),同时β角变小(90.39→90.278(2)°).二者的化学计量比也不同,体现在结构与孔容的关系、电荷平衡、满足亲水-疏水作用的结晶水的数量及有机模板分子的赋存状态等方面都有差异. 相似文献
3.
三维孔道结构(H3NCH2CH2NH3)2(H3NCH2CH2NH2)[VⅢ(H2O)2(VⅣO)8(OH)4(H(P,B)O4)4(P,B)O4)4(H2O)2]·3H2O的水热合成及晶体化学研究——(1)水热合成与产物表征 总被引:4,自引:4,他引:0
为了探讨化学成份对VPO体系孔道结构化合物结构稳定性的影响,根据酸碱平衡原理进行了合成实验设计;利用V2O5、H3PO4、H3BO3等简单的无机前驱物、乙二胺作结构导向剂,水热法合成了孔道结构钒硼磷酸盐化合物(H3NCH2CH2NH3)2(H3NCH2CH2NH2)[VⅢ(H2O)2(VⅣO)8(OH)4(H(P,B)O4)4((P,B)O4)4(H2O)2]·3H2O(简称V9(P,B)8-en).典型的反应起始物摩尔比为n(V2O5):n(H3BO3):n(H3PO4):n(en):n(H2O)=0.89:3.50:3.50:3.60:265(pH值为6.5),在175℃、自生压力条件下恒温晶化6.5d(最终pH值为5.9).通过电子探针、粉末X射线衍射、红外吸收光谱、原子占位度修正等方法,对产物的化学成份、物相及其结构等进行了实验研究.证实V9(P,B)8-en为V9P8-en的类质同象化合物,不同晶粒中B与P的含量有差别,B与P之比为O.1:7.9~2.54:5.46(原子比),但恒有V:(P+B)≈9:8.表明通过合理设计和控制合成条件,可在保持V9P8-en基本结构不变的前提下通过同晶取代引入新的化学成份,并由此探讨成份与结构稳定性的关系. 相似文献
4.
A water soluble flavonoid sulfate, [Ni(H2O)6](C19H17O9S)2·2H2O was synthesized and its structure was determined by single-crystal X-ray diffraction analysis. The crystal of it belongs to triclinic crystal system, space group P–1. The results show that the title compound consists of [Ni(H2O)6]2+, C19H17O6SO3
− and H2O. Ni(II) is located on the symmetry center and octahedrally coordinated by six water molecules. A variety of hydrogen bonds among [Ni(H2O)6]2+, C19H17O6SO3
− and the lattice water molecules build a hydrophilic region. Aromatic π–π stacking interactions assemble isoflavone skeletons into a column and the columns form a hydrophobic region of the title compound. The sulfo-groups bridge the hydrophilic regions and the hydrophobic regions as well as the inorganic components and organic components. Hydrogen bonds, stacking interactions and the electrostatic interactions between cation [Ni(H2O)6]2+ and anion sulfonate C19H17O6SO3
− lead the moieties to a three-dimensional structure. 相似文献
5.
Indrani Dey B. P. Mukhopadhyay B. N. Das S. Chakraborty Asok Banerjee 《Journal of chemical crystallography》1993,23(1):65-68
The structure of the Cu(II) complex of gly-l-tyr [Cu(C11N2O4H13) (H2O)2]·2H2O has been solved by X-ray diffraction methods. The compound crystallizes in the orthorhombic space groupP212121 witha=11.970(2) Å,b=12.485(2) Å andc=10.418(3) Å, respectively, (MoK)=0.710 Å,D
c
=1.59 Mgm–3,D
m
=1.59 Mgm–3, finalR=0.04. The structure was solved by heavy atom (Cu) phased Fourier and refined by full-matrix least squares methods. The coordination geometry of the ligand around the Cu(II) ion has been established as a distorted tetragonal pyramid. The peptide molecule behaves as a tridentate ligand via its amino (N2), amido (N1) nitrogens and carboxyl (O2) oxygens. The peptide nitrogen is found to be deprotonated. 相似文献
6.
7.
The title compound has been synthesized, and characterized by means of X-ray, magnetic, and IR-spectroscopic measurements.The crystals of Cu(DPhP)2(H2O)2(DPhP=diphenylphosphate) are monoclinic, space groupI2/c witha=24.126(6),b=8.510(2),c=12.333(3) Å,=90.73(5)° andZ=4. The structure was solved by the heavy-atom technique, and refined by full-matrix least-squares calculations to a finalR of 0.040 for 1494 reflections.The complex is centrosymmetric, and the Cu atom at a center of symmetry is four-fold coordinated with two oxygen atoms from two phosphate groups and two water molecules. The coordination about the Cu atom is square-planar, with Cu-O and Cu-O(W) distances 1.926(3) and 1.912(3) Å, respectively.The O(2) phosphate oxygen is an acceptor of two H bonds; one of them is an intramolecular O(W)-H(2)O(2) of 2.714(4) Å, and the other is an intermolecularO(W)-H(1)O(2i) of 2.667(4) Å. Their presence is also deduced from the IR spectrum of this compound at 3250 and 3000 cm–1, respectively.The calculated magnetic moment value of 1.92 B.M. corresponds to that of the monomeric copper(II) complexes including those of some alkyl phosphates. 相似文献
8.
K.C. Kumara Swamy S. Kumaraswamy S. Raja K.S. Kumar 《Journal of chemical crystallography》2001,31(1):51-56
X-ray structures of the cyclic dithiophosphate salts [Et3NH]+[(OCH2CMe2CH2O)P(S)(S)]– (1) and [Et3NH]+[CH2{6-t-Bu-4-Me-C6H4O}2P(S)S]– (2) have been determined. Crystal data for 1: Tetragonal, P42/m, a = 13.416(7), b = 13.416(2), c = 9.153(2) Å, and Z = 4. Crystal data for 2 = Monoclinic, P21/c, a = 19.1112(17), b = 14.649(9), c = 22.7166(19) Å, = 102.883(7)°, and Z = 8. The six- and eight-membered rings in 1 and 2 have chair and boat-chair conformations respectively. Both of these compounds show weak N—H······S hydrogen bonds; interestingly, in 2 both two-center and three-center hydrogen bonds are observed in the solid state. 相似文献
9.
Wu Lei Qingli Hao Lude Lu Xujie Yang Xin Wang 《Journal of chemical crystallography》2004,34(6):387-391
A new adduct bis(pyridine)-bis(O,O-diisopropyl dithiophosphato-S,S)nickel(II), [Ni(i-Pr2dtp)2(py)2] (dtp = dithiophosphate, py = pyridine) has been obtained by re-crystallization from CH3COCH3. The crystal and molecular structure of the title complex has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group P21/c, with lattice parameters a = 6.4890(13) Å, b = 16.386(3) Å, c = 14.830(3) Å, = 99.74(3)°, V = 1554.1(5) Å3, and Z = 2. The crystal structure consists of discrete molecules of [Ni(i-Pr2dtp)2(py)2], which displays a slightly distorted octahedral geometry for the NiS4N2 chromophore. Two O,O-diisopropyl dithiophosphate ions act as bidentate ligands with their S atoms coordinated to Ni atom. Each forms a four-membered chelate ring in the equatorial plane. The N atoms from two pyridine ligands are axially coordinated to the Ni atom. The Ni
S bond distances are 2.4492(8) Å and 2.5711(9) Å, and the Ni
bond distances are 2.127(3) Å. Thermal analyses show that the thermal decomposition of this adduct is so unstable that loss of two pyridine ligands begins at about 65°C. Electronic and IR spectra data is in agreement with the structural data. 相似文献
10.
Four Cu(II) complexes with the RR,SS-Edds 4? and SS-HEdds 3? anions are synthesized, and their crystal structures are studied. In the compounds [Cu2(RR,SS-Edds)] · 6H2O (I) and Ba2[Cu(RR,SS-Edds)](ClO4)2 · 8H2O (II), the ligand forms hexacoordinate chelate [Cu(Edds)]2? complexes with the N atoms and O atoms of the propionate groups in the equatorial positions and the O atoms of the acetate groups in the axial vertices. In the compounds Ba[Cu(SS-HEdds)]ClO4 · 2H2O (III) and Ba3[Cu2(RR,SS-Edds)2](ClO4)2 · 6H2O (IV), one of the propionate arms, the protonated arm in III and the deprotonated arm in IV, does not enter into the coordination sphere of the Cu atom. An acetate arm moves to its position in the equatorial plane, and the free axial vertex is occupied by an O atom of the perchlorate ion. In I–IV, the lengths of the equatorial Cu-N and Cu-O bonds fall in the ranges 1.970–2.014 and 1.921–1.970 Å, respectively. The axial Cu-O bonds with the acetate groups and ClO 4 ? anions are elongated to 2.293–2.500 and 2.727–2.992 Å, respectively. In structure I, the second Cu atom acts as a counterion forming bonds with the O atoms of two water molecules and three O atoms of the Edds ligands. In II–IV, the Ba2+ cations are hydrated and bound to the O atoms of the anionic complexes and (except for one of the cations in IV) ClO 4 ? anions. The coordination number of the Ba cations is nine. The structural units in I–IV are connected into layers. In I, an extended system of hydrogen bonds links the layers into a framework. In II and III, the layers are linked only by weak hydrogen bonds, one bond per structural unit. In IV, ClO 4 ? anions are bound to the Ba and Cu atoms of neighboring layers, thus serving as bridges between the layers. 相似文献
11.
The crystal structure of the bimetallic cyanide bridged complex [(DMF)4(H2O)3LuCo(CN)6]·H2O (1) was obtained by single-crystal X-ray diffraction. The central lutetium(III) ion is eight coordinate arranged in a square antiprism while the cobalt(III) ion is six coordinate, oriented octahedrally. Molecules in the crystal lattice are held together by a network of hydrogen bonding. Crystallization of 1 occurs in the centrosymmetric monoclinic space group P21/c (No. 14) with a = 13.875(2), b = 8.8352(9), c = 24.633(2) Å = 96.392(8)° and Z = 4. 相似文献
12.
[Mn(H2O)3(phen)(C4H4O4)]·2H2O was obtained by reaction of freshly prepared MnCO3, phen and succinic acid in CH3OH/H2O (1:1 v/v), and its crystal structure has been determined by single crystal X-ray diffraction methods. The title mixed ligand complex crystallizes in the triclinic space group
with cell dimensions a = 7.590(1) Å, b = 9.324(1) Å, c = 13.917(1) Å, = 85.64(1)°, = 74.56(1)°, = 77.10(1)°, and D
calc = 1.584 g/cm3 for Z = 2. The crystal structure consists of the [Mn(H2O)3(phen)(C4H4O4)] complex molecules and lattice H2O molecules. The Mn atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of three H2O molecules and one succinato ligand with d(Mn—N) = 2.271 and 2.299 Å, and d(Mn—O) = 2.133–2.239 Å. Through intermolecular hydrogen bondings, the complex molecules are interlinked to form 2D layers, which are assembled by – stacking interactions into 3D framework with tunnels occupied by the lattice H2O molecules. Thermal analyses showed that the title compound decomposes in two steps over the range 25–600°C upon heating in flowing Ar. 相似文献
13.
The synthesis and X-ray crystal structure of [Cu(C7H3NO4)(C6H7NO)], [Cu(dipic)(4-MeO-Py)], (dipic = pyridine-2,6-dicarboxylate, 4-MeO-Py = 4-methoxypyridine), is described. Molecules of [Cu(dipic)(4-MeO-Py)] are formed {via} coordination of the copper(II) cation to two nitrogen atoms, from the dipic and 4-MeO-Py ligands respectively, and to two oxygen atoms from the carboxylate groups of the dipic ligand. The molecules pack in a non-centrosymmetric manner, stacked eclipsed with respect to one another along the b-axis and aligned parallel in a head-to-tail motif. The title compound crystallizes in the orthorhombic space group, Pca2(1), with a = 27.339(3) Å, b = 3.7130(4) Å, c = 11.6859(12) Å, V = 1186.2(2) Å3, and Z = 4. The structure was solved by direct methods and refined by least-squares methods to a final R-factor of 0.0327 for 2648 independent reflections. 相似文献
14.
Ping Lin Xintao Wu Ling Chen Wenxin Du Yifan Zheng 《Journal of chemical crystallography》1999,29(5):581-586
The complex (Ph4P)2[Mo2S2O2(S2)(S4)] reacts with CuBr to give the dodecanuclear heterobimetallic Mo—Cu—S cage cluster: (Ph4P)2[{Mo2Cu2O2S2(S2)2}3(6-S)] (1), which crystallizes in the triclinic space group P1¯, a = 14.445(5), b = 15.396(5), c = 18.858(5) Å, = 103.12(3), = 101.93(2), = 113.92(3)°, and V = 3517(2) Å3 for Z = 2. The anion 1 can be described as a cage with S2– at the center binding to six Cu atoms; the cage has two big windows each composed of a puckered Cu3S6 9-membered ring. 相似文献
15.
Yue-Qing Zheng Jian-Li Lin Zu-Ping Kong Bao-Ya Chen 《Journal of chemical crystallography》2002,32(10):399-408
The complex [Ni(H2O)3(phen)(C4H2O4)] H2O (1), which was obtained by reaction of phenanthroline, Ni(NO3)2 6H2O, and maleic acid in CH3OH/H2O at pH = 7.05, crystallized in the monoclinic space group P21 (no. 4) with cell dimensions: a = 9.350(1) Å, b = 7.631(1) Å, c = 12.821(1) Å, = 106.25(1), and D
calc = 1.607 g/cm3 for Z = 2. The Ni atoms are each octahe drally coordinated by one chelating phen ligand, three H2O molecules and one monodentate maleato ligand to form [Ni(H2O)3(phen)(C4H2O4)] complex molecules with d(Ni–O) = 2.038–2.090 Å, d(Ni–N) = 2.066, 2.089 Å. The formed complex molecules are, via the intermolecular hydrogen bonds, assembled into columnar 1D chains. Interdigitation of the chelating phen ligands of the neighboring chains leads to 2D layers and the crystal H2O molecules are hydrogen bonded to the oxygen atoms of the maleate not coordinated to the Ni atom. However, reaction of NiCO3, phen, and maleic acid in CH3OH/H2O at pH = 6.33 afforded [Ni(H2O)2(phen)(C4H2O4)] 2H2O (2), which crystallized in the triclinic space group
(no. 2) with cell dimensions: a = 7.971(1) Å, b = 8.237(1) Å, c = 13.304(1) Å, = 81.005(6)°, = 87.877(8)°, = 78.322(8)°, and D
calc = 1.671 g/cm3 for Z = 2. The Ni atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of two H2O molecules and two bis–monodentate maleato ligands with d(Ni–O) = 2.041–2.120 Å and d(Ni–N) = 2.095 Å. The Ni atoms are bridged by the maleato ligands to generate 1D
1
[Ni(H2O)2(phen)(C4H2O4)2/2] chains along [100]. The supramolecular assemblies of the 1D chains via – stacking inter- actions result in thick 2D layers parallel to (001), between which the noncoordinating H2O molecules are sandwiched. The paramagnetic [Ni(H2O)2(phen)(C4H2O4)2/2] 2H2O (2) obeys the Curie–Weiss law m(T-) = 1.139cm3 mol–1 K with the Weiss constant = –0.95 K. 相似文献
16.
M. John Plater Mark R. St J. Foreman R. Alan Howie 《Journal of chemical crystallography》2000,30(7):445-447
The title compound exists as a 1D coordination polymer consisting of succinate anions, manganese cations and 2,2-bipyridyl molecules. Twelve water molecules are present in the unit cell and are part of a hydrogen bonding system. Some of these waters are binding to manganese cations while others are only participating in hydrogen bonding. The structure has a monoclinic space group P21/c with a = 8.2750(3) Å, b = 11.5104(3) Å and c = 16.9113(6) Å, = 95.2727(16); V = 1603.96(9) Å3 and Z = 4. 相似文献
17.
The crystal and molecular structures of the complex of [Ni{(iPrO)2dtp}2(py)2] and [Cd{(iPrO)2dtp}2(py)2] (dtp = dithiophosphate, py = pyridine) have been determined by X-ray crystallography. They are isomorphous. The crystal structures are very similar and consist of discrete molecules of [Ni{(iPrO)2dtp}2(py)2] and [Cd{(iPrO)2dtp}2(py)2], respectively. They both crystallize in the monoclinic system, space group P21/c, the former with lattice parameters a = 6.489(1) Å, b = 14.830(3) Å, c = 16.386(3) Å, = 99.74(3), and Z = 2; the latter with a = 6.461(3) Å, b = 14.583(4) Å, c = 17.433(4) Å, = 99.55(3)°, and Z = 2. They all display distorted octahedral geometry around the central metal atom. In the complexes, two O,O-diisopropyl dithiophosphate ions act as bidentate ligands with their S atoms coordinated to metal. Each forms a four-membered chelate ring in the equatorial plane. The N atoms from two pyridine ligands are axially coordinated to the metal atom. The Ni–S bond distances are 2.5137(10) and 2.5386(9) Å, and the Ni–N bond distances are 2.127(3) Å. The Cd–S(1) and Cd–S(2) bond distance are 2.694(1) and 2.704(1) Å, respectively, and the Cd–N bond distances are 2.399(3) Å. The IR spectra data is in agreement with the structural data. 相似文献
18.
Sp. Chidambaram G. Aravamudan V. Ganesh M. Seshasayee T. A. Sibanova B. V. Merinov V. I. Simonov 《Journal of chemical crystallography》1989,19(3):465-473
The synthesis and crystal structure ofbis(o-phenylenethiourea)selenium(II)-chloride dihydrate, Se(C7H6N2S)2Cl2·2H2O are reported. The compound crystallizes in the monoclinic space group, P21/n, with four molecules per unit cell, the dimensions of which area=10.243(3),b=13.341(4),c=14.273(4) Å,=93.00(3)°,U=1947.76 Å3. The structure was solved by direct methods and refined by full-matrix least-squares toR=0.039 andR
w
=0.040 for 3314 unique reflections. Selenium displays two strong coordinations arising from the two sulfurs, Se-S(1)=2.191(1), Se-S(2)=2.206(1) Å, and S(1)-Se-S(2)=101.0(1)°, and four secondary interactions involving three chlorines and one sulfur. The complex occurs as a dimer with two sets of very weakly interacting bridging pairs S(2), S(2)a; and Cl(2), Cl(2)a, where a denotes the inversion related atom. Lattice stabilization is ensured by the extensive network of hydrogen bonds involving chlorines, water oxygens, and nitrogens of phenylenethiourea ligands. 相似文献
19.
以乙醇为溶剂,在低温条件下合成出了两种手性硼磷酸盐化合物BaBPO5(1)(T=120℃,t=5d)和(H3O)Zn(H2O)2BP2O8·H2O (2)(T=80℃,t=5d).XRD单晶衍射仪测定了化合物的结构,结果表明:(1)属三方晶系,P3221空间群,a=b=7.1162(3)(A),c=6.9979(6),(A)=3,该晶体含有一维线性链状阴离子结构;(2)属六方晶系,P6122空间群,a=b =9.513(2)(A),c=15.906(8),(A)=6.该晶体具有三维骨架结构.实验结果表明使用乙醇作溶剂可以极大降低硼磷酸盐的合成温度,进而有助于获得手性硼磷酸盐化合物,这为手性硼磷酸盐的合成提供了一种新思路. 相似文献
20.
Can-Zhong Lu Jun-Ning Zhuang Li-Sheng Chi Yin-Gui Wang Jin-Shun Huang Hong-Hui Zhuang Qian-Er Zhang 《Journal of chemical crystallography》1999,29(9):1019-1022
The title compound, [Mo3(3-S)(-S2)3(S2CNEt2)3]I·S8, was obtained by solid state reaction of (NH4)2MoS4, Et2NCS2Na, and Et4NI at low heating temperature and crystallizes in space group P
with a = 13.572(3), b = 13.813(4), c = 13.239(3) Å, = 92.63(3), = 100.15(3), = 117.89(2)°, V = 2136(2) Å3, and D
calc. = 2.08 g/cm3 for Z = 2. The structure reveals that it consists of a trinuclear Mo cluster molecule, [Mo3S7(S2CNEt2)3]I, and one S8, which are connected to form a quasi-layer structure by the interaction between S8 and the S atoms of the cluster molecule. 相似文献