Crystal and molecular structure of four copper(II) ethylenediaminedisuccinates, [Cu2(RR,SS-Edds)] · 6H2O, Ba2[Cu(RR,SS-Edds)](ClO4)2 · 8H2O, Ba[Cu(SS-HEdds)]ClO4 · 2H2O, and Ba3[Cu2(RR,SS-Edds)2](ClO4)2 · 6H2O

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.     

Zn(II) and Cd(II) Complexes Extended Structures Sustained by Hydrogen Bonding, π–π and C–H···π Interactions

Abstract  

Two new complexes [Zn(sal)₂(tpt)]·H₂O(1), [Cd(sal)₂(tpt)(H₂O)]·H₂O(2), have been obtained through ligands tpt and Hsal, where Hsal is salicylic acid and tpt is 2,4,6-tripyridyl-1,3,5-triazine, reacting with Zn(II) and Cd(II) salts. Their structures are fully characterized by IR spectroscopy, elemental analysis, single crystal X-ray diffraction. In complex 1, Zn(II) is coordinated by three N atoms and two O atom with a distorted square pyramidal coordination geometry. In 2, Each Cd(II) atom is seven-coordinated with a distorted pentagonal bipyramidal coordination geometry. The structural differences between two complexes show the influence of the coordinating orientation of metal ions. These two mononuclear complexes are further extended into three-dimensional structure via π–π, C–H···π and hydrogen bonding interactions. The solid state luminescent properties of complex 1, 2 are also reported.     

X-Ray Diffraction and Thermographic Study of Mesomorphic 4-Acylphenyl 4'-Nonyloxybenzoate CH3C(O)C6H4–OC(O)–C6H4–OC9H19

Crystallography Reports - The structure and thermal properties of mesomorphic phenyl benzoate CH3–C(O)–C6H4–OC(O)–C6H4–OC9H19 (I) were studied by differential scanning...     

Analysis of C–H···O Intermolecular Interactions in 4-Androstene-3,17-dione

Abstract  4-Androstene-3,17-dione was synthesized for its crystallographic analysis and to investigate the role of intra- and intermolecular interactions in steroids. It crystallizes in the orthorhombic space group P2₁2₁2₁ with unit cell parameters, a = 7.330(2) ?, b = 13.095(11) ?, c = 16.856(17) ?, V = 1,618(5) ?³ and Z = 4. The structure has been solved by direct methods using X-ray diffraction techniques and the refined final reliability index for the computed structure is 0.033 for 1,655 observed reflections. Two six-membered rings B and C exist in chair conformation while ring A occupies a sofa conformation. The five-membered ring D depicts envelope conformation. The C–H···O intermolecular hydrogen interaction results into a ring like configuration which makes the dimers. Index Abstract   Androgen is the generic term for any natural or synthetic compound, usually a steroid hormone, that stimulates or controls the development and maintenance of masculine characteristics in vertebrates by binding to androgen receptors [1]. Androgens have been used in breast cancer when excision or radiotherapy have failed to control the progress of local recurrent disease. They are also used in case where the primary tumour is inoperable or is unsuited for, or resistant to, radiotherapy. Androgens are also believed to be responsible for linear bone growth in both males and females, probably in conjunction with somatotrophin [2]. In continuation to our work on the single crystal growth of X-ray diffraction quality crystals and crystallographic analysis of steroidal molecules, [3-7] synthesis and crystallographic study 4-androstene-3,17-dione is reported in this paper.     

C–H···F Hydrogen-Bonded Assembly of Ni(II) and Cu(II) Complexes Generate 3D Supramolecular Frameworks

Abstract  Syntheses and X-ray structural characterizations of two new complexes [Ni(imi)₆](pfbz)₂ (1) and Cu(imi)₂(pfbz)₂ (2) (imi = imidazole, pfbz = pentafluorobenzoate) are reported. The first complex crystallizes in the triclinic space group P-1 with the crystal cell parameters a = 9.180(2) ?, b = 9.742(3) ?, c = 11.466(3) ?, α = 76.947(18)°, β = 80.629(18)°, γ = 78.043(19)°, V = 970.0(4) ?³ and Z = 1. The second complex crystallizes in the triclinic space group P-1 with the crystal cell parameters a = 7.3250(12) ?, b = 7.6685(10) ?, c = 10.888(4) ?, α = 92.80(2)°, β = 101.92(2)°, γ = 115.038(12)°, V = 535.7(2) ?³ and Z = 1. Examination of the structures shows that both complexes form three-dimensional hydrogen bonded networks in which C–H···F hydrogen bonds play significant roles. Index Abstract   C–H···F Hydrogen-Bonded Assembly of Ni(II) and Cu(II) Complexes Generate 3D Supramolecular Frameworks Chun-Hua Ge, Xiao-Yan Zhang, Fang Yu, Ya-Nan Guo, Xiang-Dong Zhang* and Qi-Tao Liu C–H···F interactions link simple complexes to form intricate three-dimensional supramolecular networks.      

Structural Study of Polymorphism in [La(Gly)3·2H2O](ClO4)3

Journal of Chemical Crystallography - The crystal structures of [La(Gly)3·2H2O](ClO4)3 were determined by X-ray diffraction analysis at temperatures 100 K and 300 K: space...     

Structure of a Cu(II)-containing peptide,diaquo-gly-l-tyr Cu(II) dihydrate, [Cu(C11N2O4H13)(H2O)2·2H2O

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.     

Production of Complex Hydrosulphates in the K3H(SO4)2–Rb3H(SO4)2 Series: Part I

Crystallography Reports - The phase equilibria in the K3H(SO4)2–Rb3H(SO4)2–H2O cross section have been investigated under isothermal conditions at 25°C. The concentration limits of...     

Crystal Structure of Potentially Mesomorphic 4-Nonyloxyphenyl-4'-Metacryloyloxy-Benzoate CH2=C(CH3)–COO–C6H4–COO–C6H4–O–С9Н19

Crystallography Reports - The crystal structure of 4,4'-substituted phenyl benzoate CH2=C(CH3)–COO–C6H4–COO–C6H4–O–С9Н19 has been investigated by...     

Crystal and molecular structure of 2,9-di-(methylnitronato)-3,5,10,12-tetramethyl-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) di-triethylammonium diperchlorate,C16H28N6O4Ni·2(C2H5)3NH·2ClO4

The crystal and molecular structure of 2,9-di-(methylnitronato)-3,5,10,12-tetramethyl-1,4,8,11-tetraazacyclotetradeca-4,11-dienenickel(II) di-triethylammonium diperchlorate (2c) has been determined of the basis of X-ray diffraction data. The crystals are monoclinic, space groupP2₁/c,Z=2; cell constants=11.478(3),b=15.177(3),c=11.431(3) Å,=99.34(2)°. The structure was refined (full matrix, least squares) with 3408 unique reflections givingR=0.0616. An octahedral configuration of the Ni(II) coordination sphere was found to consist of the macrocycle N₄ atoms occupying the equatorial plane of the octahedron with the O-atoms of the nitronato groups in the apical positions. The triethylammonium cations are hydrogen-bonded to the remaining O-atoms of the nitronato groups.     

Synthesis and crystal structure of [Cu(azpy)(H2O)4][Cu2(nta)2(azpy)]····6H2O: A two-dimensional network solid

The copper(II) complex [Cu(azpy)(H₂O)₄][Cu₂(nta)₂(azpy)]····6H₂O (nta = nitrilotriacetate, azpy = 4,4-azobispyridine) has been synthesized and structurally characterized. It crystallizes in the triclinic space group P , a = 8.6985(3) Å, b = 9.4776(3) Å, c = 14.6544(5) Å, = 71.5360(10)°, = 85.7600(10)°, = 88.1420(10)°, V = 1142.74(7) ų, Z = 1. The crystal structure consists of one-dimensional linear chain cations and dimeric anions. The copper centers in the anion possess distorted trigonal bipyramidal geometry, while Cu(2) has a distorted octahedral geometry in the cation. Coordinated water molecules in the one-dimensional chain form interionic hydrogen bonds with the oxygen atoms of the carboxylate of nta of the dimmer anion. These hydrogen bonds result in the formation of a two-dimensional network.     

Production of Complex Hydrosulphates in the K3H(SO4)2–Rb3H(SO4)2 Series: II. Phase Equilibria in the K2SO4–Rb2SO4–H2SO4–H2O System

Crystallography Reports - The phase equilibria in the K2SO4–Rb2SO4–H2SO4–H2O system have been investigated under isothermal conditions at 25°C. The concentration limits of...     

三维(C2H7N4S)+·(C7H5O4)——超分子氢键网格的构筑

利用脒基硫脲和3,5-二羟基苯甲酸制备出了一种新型的加合物(C2H7N4S)+·(C7H5O4)-,用X射线单晶衍射试验方法测定其晶体结构.结果表明,晶体属单斜晶系,P21/n空间群,其中a=0.72303(1)nm,b=1.42970(3) nm,c=1.07991(2)nm,β=91.591(2)°,Z=4,R1=0.0303, wR=0.0823(I>2σ(I)).在标题化合物的晶体结构中,3,5-二羟基苯甲酸通过羧基和羟基的O-H…O氢键头尾相连形成了沿b轴无限延伸的"Z"型链,脒基硫脲通过氢键的缔合和静电相互作用连接3,5-二羟基苯甲酸的"Z"型链构成了3D超分子氢键网络结构.     

C–H···π and C=O···π Intermolecular Interactions in Dibenzyl-3,6-dimethylpyrazine-2,5-dicarboxylate

Abstract A new pyrazine compound, has been synthesised and characterised by single-crystal X-ray diffraction: monoclinic, P2₁/c with a = 11.0707(3) ?, b = 5.23700(10) ?, c = 16.6997(5) ?, β = 103.5385(16)°, Mr = 376.40, V = 941.30(4) ?³, Z = 2. Each molecule possesses C _i symmetry with the two halves of the molecule related by an inversion centre. C–H···π and C=O···π interactions held the molecules together. Index Abstract C–H···π and C=O···π intermolecular interactions in dibenzyl-3,6-dimethylpyrazine-2,5-dicarboxylate Joana A. Silva, Ana C. Santos, Ana T. Marques, Manuela Ramos Silva, Ana Matos Beja, Abílio J. F. N. Sobrala In dibenzyl-3,6-dimethylpyrazine-2,5-dicarboxylate, each molecule possesses C _i symmetry. The molecules are assembled in chains via carbonyl···π interactions. Electronic supplementary material The online version of this article (doi: ) contains supplementary material, which is available to authorized users.     

Synthesis,crystal structure and spectral studies of the complex [Ni(C3H4N2)4(H2O)2]·(C6H4COSO2N)2

The title compound has been synthesized and its crystal structure determined at room temperature.M _r =731.39, triclinic, space groupP¯1,a=9.020(3),b=11.280(7),c=7.784(2)Å,=97.05(4),=97.08(2), =105.32(4)°, U=748(1)ų,Z=1,D _calc.=1.624 g/cm³. The finalR is 0.030 for 3095 independent observed reflections withI3(I). The crystal structure consists of repeated [Ni(im)₄(H₂O)₂]²⁺ cations and noncoordinated saccharin anions. In the complex cation [Ni(im)₄(H₂O)₂]²⁺, Ni² is bonded to four N atoms from four imidazole molecules and two O atoms from two water molecules forming an approximately square octahedral stereochemistry. The d-d transition spectrum of the title compound is also reported and is explained perfectly with the scaling radial theory which was proposed by us.     

Mesophase-Preceding Crystal Packing of 4,4'-Dialkyl-Substituted Salicylideneanilines; C10H21O–C6H3(OH)–CH=N–C6H4–С7Н13) Structure

Crystallography Reports - The crystal structure of 4,4'-substituted salicylideneaniline C10H21O–C6H3(OH)–CH=N–C6H4–C7H13 has been investigated by X-ray diffraction. A...     

一种双核铜配合物[Cu(II)2(Paba)2(4,4'-Bipy)(H2O)2]·(ClO4)2的合成、表征及晶体结构

在水和甲醇的溶剂中合成了标题配合物[Cu(II)2(Paba)2(4,4'-Bipy)(H2O)2]·(ClO4)2 [PabaH=2-(2-吡啶甲基亚氨基)苯磺酸],通过红外光谱、元素分析、X射线单晶衍射等手段对配合物进行了表征.结果表明,该配合物晶体属于单斜晶系,空间群为P2(1)/n. 晶体学参数: a=14.559(2) nm, b=0.95984(13) nm, c=1.6038(2) nm, α=γ=90°, β=115.694(2)°, V=2.0197(5) nm3, Z=2.     

Crystal structure of radical cation salt (BEDT-TTF)4(GaCl4)2 · C6H5CH3

A new radical cation salt based on bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF) with the tetrahedral anion GaCl ₄ ^? , namely, (BEDT-TTF)₄(GaCl₄)₂ · C₆H₅CH₃, has been synthesized. The crystal structure of this salt is determined by X-ray diffraction analysis [a = 31.757(2) Å, b = 6.8063(3) Å, c = 34.879(2) Å, β = 90.453(4)°, V = 7538.8(7) ų, space group I2/c, and Z = 4]. In the structure, the radical cation layers alternate with the anion layers along the c-axis. The anion layers consist of the GaCl ₄ ^? tetrahedra and solvent molecules. The packing of BEDT-TTF molecules in the radical cation layer differs from that in the structure of the known salt (BEDT-TTF)₂GaCl₄, even though both compounds exhibit semiconductor properties.     

Crystal structure of dibarium (Ethylenediaminetetraacetato)cuprate(II) diperchlorate hexahydrate, Ba2[Cu(Edta)](ClO4)2 ⋅ 6H2O

Compound Ba₂[Cu(Edta)](ClO₄)₂ ? 6H₂O is synthesized and its crystal structure is determined [R = 0.0500 for 4439 reflections with I > 2σ(I)]. The structure consists of the [Cu(Edta)]^2? anionic complexes, hydrated barium cations, Cl ₄ ^? anions, and molecules of crystallization water, which are interlinked into a framework. The hexadentate Edta ^4? ligand coordinates the Cu atom forming the polyhedron in a shape of a tetragonal bipyramid, which is asymmetrically stretched along the OR-Cu-OR, axis (Cu-O, 2.262 and 2.532 Å). The mean lengths of the equatorial Cu-N and Cu-O bonds are 2.011 and 1.952 Å, respectively. The anionic complex is bound to six Ba atoms. Two independent Ba atoms have different environments; their coordination numbers are nine and ten. The Ba-O distances lie in the range 2.669–3.136 Å. Layers of Ba atoms parallel to the x0z plane are distinguished in the structure.     

C–H...O,C–H...π and π–π stacking interactions in 3-(2,4-dimethylphenyloxymethyl)-3,4-dihydroisocoumarin

3-(2,4-Dimethylphenyloxymethyl)-3,4-dihydroisocoumarin (C₁₈H₁₈O₃) was prepared by the alkylation of o-lithio N-methyl benzamide with 2-(2,4-dimethylphenoxy)methyl oxirane, followed by alkaline hydrolysis. The compound crystallizes in the orthorhombic space group Pbca with unit cell parameters : a = 8.239(2) Å, b = 14.918(5) Å, c = 24.831(9) Å, Z = 8. The crystal structure was solved by direct methods and refined to R = 0.0514 for 1564 observed reflections. The heterocyclic ring adopts a distorted half-chair conformation. Molecules are connected by π–π interactions between phenyl rings of the isocoumarin nucleus forming dimers. Dimers are connected via C–H...O hydrogen bonds forming chains. Further intermolecular C–H...π hydrogen bonds link the dimer chains to form supramolecular structure.