Synthesis,Crystal and Molecular Structure of 2‐Pyridylethanolbis(saccharinato)mercury(II)

2‐Pyridylethanolbis(saccharinato)mercury(II), [Hg(sac)2(pyet)], where sac and pyet are the saccharinate anion and the 2‐pyridylethanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 10.4518(6), b = 11.3796(6) (5), c = 19.9945(12) Å, a = 102.758(3)° b = 98.146(3)°, g = 104.751(3)°, Z = 4, V = 2193.0(2) ų. The unit cell contains two crystallographically independent [Hg(sac)2(pyet)] units in which the mercury(II) ion is tetrahedrally coordinated by two nitrogen atoms of two sac ligands, and one nitrogen and one oxygen atoms of one neutral pyet ligands. The pyet acts as a bidentate N‐ and O‐donor ligand forming a six‐membered chelate ring, while sac behaves as a monodentate N‐donor ligand. The average bite angle of the pyet ligand is 75.8(5)°. The Hg‐N_sac bond distances are in the range 2.0874(18) and 2.1931(18) Å, whereas the Hg‐N_pyet and Hg‐O_pyet bond distances are 2.2452(19)‐2.3202(19) and 2.6036(17)‐2.5902(16) Å, respectively. The crystal exhibits two strong hydrogen bonds between the hydroxyl O atom of pyet and sulfonyl O atoms of sac and the C‐H…O type weak hydrogen bonds between H atoms of the aromatic rings of the pyet and the sulfonyl O atoms of the sac ligands. Furthermore, packing of the molecules in the solid‐state results in aromatic π‐π interactions associated with the aromatic rings of sac‐sac and py‐py.     

Synthesis,crystal and molecular structure of trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II)

Trans‐bis(2‐pyridinepropanol)bis(saccharinato)nickel(II), [Ni(sac)₂(pypr)₂], where sac and pypr are the saccharinate anion and the 2‐pyridinepropanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 8.1981(8), b = 9.9680(10), c = 10.4956(10) Å, α = 90.740(3)° β = 108.142(3)°, γ = 111.025(3)°, Z = 1, V = 1.537 ų. The structure of the nickel(II) complex consists of neutral molecules in which the nickel(II) ion sits on a center of symmetry and is octahedrally coordinated by two sac ligands, and two neutral pypr ligands. The pypr acts as a bidentate N‐ and O‐donor ligand forming a seven‐membered chelate ring, while sac behaves as a monodentate O‐donor ligand via the carbonyl O atom. The Ni‐N bond distance is 2.1016(15) Å, whereas the Ni‐O_pypr and Ni‐O_sac bond distances are 2.1280(12) and 2.0792(11) Å, respectively. The individual molecules are held together with a strong hydrogen bond between the hydroxyl O atom of pypr and N atom of sac and the C‐H…O type weak hydrogen bonds between some ring hydrogen atoms of pypr and sac, and the carbonyl and sulfonyl O atoms of sac in the neighbouring molecules. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis, crystal structure, and thermal properties of {[Cd2(L1)3(sac)4]⋅2CH2Cl2}∞: A coordination polymer with non-interpenetrating ladders containing cadmium in a rare, trigonal bipyramidal coordination environment (L1 = 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene, sac = saccharinate)

The new coordination polymer, {[Cd₂(L1)₃(sac)₄]?2CH₂Cl₂}_∞:, has been prepared from the reaction of 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene (L1) with [Cd(sac)₂(H₂O)₄].2H₂O(sac = saccharinate) in a methylene chloride/ethanol solvent mixture. The compound features a non-interpenetrating ladder motif constructed from Cd(L1)3 T-shaped units. The Cd atoms are coordinated to three nitrogen donor atoms from three L1 ligands and two nitrogen donor atoms from two saccharinate ligands in a rare, trigonal bipyramidal coordination environment. The compoundwas further characterized by IR spectroscopy and DTA/TGA. {[Cd₂(L1)₃(sac)₄]?2CH₂Cl₂}_∞: crystallizes in the triclinic space group P-1 with a = 10.8747(19)Å, b = 12.626(2)Å, c = 15.749(3)Å, α = 111.839(3)^°, β = 97.442(3)., and γ = 106.239(3)^°     

Synthesis and structure of the three‐dimensional coordination polymer [Ag3hmt3(μ3 ‐btc)]·5H2O

A new coordination polymer, [Ag₃hmt₃(μ₃ ‐btc)]·5H₂O (1) (hmt = hexamethylenetetramine, btc=1,3,5‐benzenetricarboxlic), has been successfully synthesized. Crystal data: P2₁/a, a = 11.9906(2) Å, b = 17.3689(2) Å, c = 16.96100(10) Å, β = 101.9820(14)°, V = 3455.40(7) ų, Z = 4, Dc = 2.002 Mg/m³. In the hexagonal structure of Ag‐hmt unit, each Ag‐hmt unit comprises three Ag atoms and three hmt ligands. The μ₃ ‐btc ligands bridge adjacent two‐dimensional honeycomb‐like Ag‐hmt layers to form three‐dimensional networks. Structure analysis show that hydrogen bonds play a key role for the stable structure in the compounds. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal of Tetrakis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II) bis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II)

Abstract  A new complex [Cu(NCS)₄ (N-Eim)₄] [Cu(NCS)₂ (N-Eim)₂] (where N-Eim = N-ethylimidazole) has been synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the Triclinic space group P−1 with the parameters: a = 8.7707(18) ?, b = 10.712(2) ?, c = 13.511(3) ?, α = 104.73(3)°, β = 104.84(3)°, γ = 102.52(3)°, V = 1131.54(3) ?³, with Z = 1 formula units. In the structure, the copper atoms all assume an elongated octahedral geometry with two distinct coordination environments; one is coordinated by four N-ethyl-imidazole ligands and two axial SCN groups, and another by two SCN groups and two N-ethyl-imidazole ligands. The two units form one infinite 1D zigzag chain along the [1 0 1] plane by two thiocyanate ligands from the [Cu(NCS)₄ (N-Eim)₄] units. Index Abstract  The title compound, tetrakis(1-ethyl-1H-imidazole)diisothio cyanatocopper(II) bis(1-ethyl-1H-imidazole)diisothiocyanatocopper(II) has been synthesized and structurally characterized by single-crystal X-ray diffraction. In the structure, the copper atoms all assume an elongated octahedral geometry with two distinct coordination environments. The two units form one infinite 1D zigzag chain along the [1 0 1] plane by two thiocyanate ligands from the [Cu(NCS)₄ (N-Eim) 4] units.      

The Crystal and Molecular Structure of the Complex Diaquatetrakis(imidazole)copper(II) Terephthalate Crystal Structure Containing Cu(II) Him and TA

The title compound has been synthesized and its crystals structure determined at room temperature. MW = 536.01, monoclinic, space group C2/c, Z = 4, a = 22.193(5) Å, b = 8.038(2) Å, c = 15.699(4) Å, β = 119.64(2)°. The crystal structure consists of repeated [Cu(Him)₄(H₂O)₂] (Him = imidazole) cations and non-coordinated terephthalato dianions. The copper(II) ion displays an elongated octahedral coordination being linked to the four nitrogen atoms of the four imidazole ligands and to the two oxygen atoms of the two water molecules. The terephthalato dianions are hydrogen bonded to the four water molecules and four imidazole groups.     

The crystal and molecular structure of bis(tetramethylammonium) hexamolybdate(VI)

The crystal structure of the title compound, C₈H₂₄N₂Mo₆O₁₉ was determined by single crystal X‐ray diffraction technique. The crystals are trigonals, space group P‐3c1, with a = b = 10.0176(11) Å, c = 14.089(2) Å, γ = 120°, V = 1224.4(3) Å₃, Z = 2. The structure was solved by direct methods and refined by least‐squares methods to a Final R = 0.0316 for 1114 observed reflections with I > 2σ(I). In hexamolybdate anion, six MoO₆ distorted octahedra are fused together so that they all share a common vertex. O atoms are of three types: central, terminal and bridging, bonded to six, one and two Mo atoms, respectively. The crystallographic data of the structure was deposited with the Cambridge Data Center as No. CCDC 199679. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural analysis of bis{(N,N′–dimethylformamide) (μ‐formato)[μ‐bis(salicylidene)–1,3‐propanediaminato] nickel(II)} copper(II) and zinc(II) monohydrate hetero‐trinuclear complexes

The two linear hetero‐trinuclear metallic complexes with Cu²⁺, Ni²⁺ and Zn²⁺ ions, [CuNi₂ {(CHO₂)(SALPD)[(CH₃)₂NCHO]}₂],(I) and [ZnNi₂{(CHO₂)(SALPD)[(CH₃)₂NCHO]}₂],(II), form crystals which belong to the monoclinic system, space group P2₁/c, with unit cell dimensions a=10.537(4), b=16.612(5), c=13.837(3) Å, β=111.09(5)°, V=2259.8(12) ų in (I) and a=10.525(4), b=16.658(5), c=13.826(3) Å, β=111.11(5) °, V=2261.4(8) ų in (II), respectively. The coordinations around the M (Ni²⁺, Cu²⁺, Zn²⁺) ions in the title complexes are distorted octahedrals. The stereochemistries of the bridge ligands, linking to the metal ions each other, are changed between Ni…M (Cu²⁺, Zn²⁺) distances. The Ni…M (Cu²⁺, Zn²⁺) distances are 3.0469(13) and 3.0645(14), respectively. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The crystal and molecular structure of bis(tetramethylammonium) pentachlorooxomolybdate(V)‐acetonitrile(1:1)

The crystal structure of the title compound, C₁₀H₂₇Cl₅MoN₃O was determined by single crystal X‐ray diffraction technique. The crystals are monoclinic, space group C 2/m, with a= 29.075(8) Å, b= 11.843(4) Å, c= 13.252(4) Å, β=117.049(7)°, V = 4064(2) ų, Z=8. The structure was solved by direct methods and refined by least‐squares methods to a final R = 0.0307 for 5095 observed reflections with I>2σ(I). In the pentachlorooxomolybdate anion, the planar chlorines are bent away from the axial oxygen ligand. The Mo‐O bond length is 1.6620(18) Å that indicates significant double bond character. The oxygen trans Mo‐Cl bond is significantly longer than all of the planar Mo‐Cl bonds. These differences can be attributed to a trans influence of the oxygen atom. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and structure of a new one‐dimensional cobalt complex with dicyanamide and 4‐picolyl choride bridges

The synthesis and structure of the 1D cobalt (II) complex, [Co( L )₂(dca)₂] ( 1 ) (dca = dicyanamide, C₂N₃^–, L = 4‐picolyl choride) is reported. Complex 1 crystallized in triclinic system, space group P ‐1, with cell dimensions of a = 7.291(2) Å, b = 7.481(2) Å, c = 9.007(3) Å, α =104.444(4)°, β = 96.971(4)°, γ =102.618(4)°, V = 456.1(2) ų, Z = 1, Dc = 1.624 Mg/m³. In complex 1 , Co (II) is 6‐coordinated by N atoms of four dca ligands and two L ligands. The centrosymmetric CoN6 chromophore is an axially elongated octahedron that has Co‐N distances ranging from 2.122(3) to 2.154(3) Å. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Rh(I) and Pd(II) complexes of methoxy functionalized heterocyclic carbene: Synthesis and characterization

A new methoxy functionalized 2‐(trichloromethyl)‐1,3‐diarylimidazolidin (6) was synthesized as the precursor for N‐heterocyclic carbene complexes of Pd(II) and Rh(I) by the condensation of N,N'‐bis(2,4‐dimethoxyphenyl)‐1,2‐diaminoethane with chloral. The structures of all compounds have been elucidated by a combination of multinuclear NMR spectroscopy, elemental analysis and in one instance, by single crystal X‐ray diffraction. Compound 8, C₂₇H₃₄N₂O₄ClRh, crystallizes in the triclinic space group P‐1 with cell dimensions a = 9.7642(12)Å, b = 11.1914(11)Å, c = 13.0102(14)Å, α = 104.034(9)°, β = 106.658(9)°, γ = 99.658(9)° with Z = 2. The molecular structure of 8 shows the geometry around the Rh metal to be a slightly distorted square planar. The crystal structure shows the formation of centrosymmetric dimers via intermolecular C‐H...Cl hydrogen bonds. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Copper, a chemical Janus: two copper(II) complexes with different ligand in one single crystal

A chemical Janus, binuclear copper(II) complexes, {[Cu(TPA)Cl][Cu(BPA)Cl]}(ClO₄)₂ (TPA = Tris(2-pyridylmethyl) amine, BPA = bis-(2-pyridylmethyl)amine) containing two different ligands has been synthesized and characterized by X-ray single crystal analysis. Crystal data: triclinic, space group P1$sm, a = 12.529(3), b = 12.655(3), c = 13.458(3) Å, = 70.48(3), = 67.40(3), = 75.81(3)°, D _x = 1.648 mg m^–3, and Z = 2. The molecular structure shows that the binuclear copper complex consists of two positive cation and two perchlorate anions. The positive cations moieties have different ligands. Cu(1) is coordinated by four nitrogen atoms from TPA and one chloride atom, forming a square-pyramidal geometry, whereas the coordinate number of Cu(2) is four, three of which are from BPA, one from chloride. There are two weak bonds between the Cl(2a) ion and the Cu(2) ion (2.844 Å) and the distance of Cu(2)=O(13) is 2.750(9) Å.     

Synthesis,Crystal and Molecular Structure of Cd2(sacch)4(Im)4

The title compound has been synthesized and its crystal structure determined at room temperature. Cd₂(Sacch)₄(Im)₄ F.W. = 1225.83, monoclinic. Space group: C2/c, Z = 4, a = 20.065(3) Å, b = 11.164(4) Å, c = 20.697(6) Å, β = 94.69(5)°, The coordination polyhedron of Cd(II) correspond to a five-coordinate trigonal-bipyramid. In the title complex, two of the saccharin groups act as monodentate ligands. The other two act as bidentate ligands. The two Cd(II) ions are bridged by the two bidentate saccharin groups and the distance is 4.75 Å.     

Crystal structure investigation of [Mn(3-CH3C5H4N)2(N3)2(H2O)2]

The crystal structure of the title compound has been determined by single crystal X-ray diffraction methods. [Mn(3-CH₃C₅H₄N)₂(N₃)₂(H₂O)₂] crystallizes in the space group P 1 with a = 7.444(2) Å, b = 7.691(2) Å, c = 8.926(3) Å, α = 99.82(3)°, β = 108.80(2)°, γ = 114.99(2)° and Z = 1. Least squares refinement gave a R value of R_w = 0.046 for 1414 observed reflections. The manganese atom in the title complex is octahedrally coordinated by two oxygen atoms of the water molecules and four nitrogen atoms; two N-atoms are the end atoms of azide groups and the other two nitrogen atoms belong to the 3-methylpyridine molecules. The polyhedra are linked via hydrogen bonds between the water molecules and the azide groups.     

Crystal Structure of 1,2,3‐Tribromoindane,C9H7Br3

The title compound (C₉H₇Br₃) crystallizes in the triclinic space group with Z = 2; R = 0.043 for 1518 observed reflections [I = 2σ (I)]. The average Br‐C distance is 1.974 Å, Br‐C‐C angle is 110.0°. The five‐membered ring adopts a somewhat flattened structure. The atoms C1 and C3 have opposite configurations. The whole molecule has approximate (non‐crystallographic) C_s‐symmetry.     

Synthesis,crystal structure and vibrational characterization of bis‐μ‐peroxo‐hexacarbonatodicerate(IV) complexes of rubidium and cesium

The new compounds Rb₈[Ce(O₂)(CO₃)₃]₂ · 12 H₂O (1) and Cs₈[Ce(O₂)(CO₃)₃]₂ · 10 H₂O (2) were obtained from the reaction of hydrogen peroxide and Ce(III) in saturated alkali carbonate solutions. The crystal structures and the unit cell parameters of (1) triclinic, P‐1 with a = 8.973(2) Å, b = 10.815(2) Å, c = 11.130(3) Å, α = 66.992(2)°, β = 68.337(2)°, γ = 74.639(2)°, V_EZ = 914.7(4) ų, Z = 2, and (2) orthorhombic, Pbca, a = 19.3840(16) Å, b = 18.528(2) Å, c = 10.487(3) Å, V_EZ = 3766.4(13) ų, Z = 8, were determined. Both compounds contain the bis‐µ‐peroxo‐hexacarbonatodicerate(IV)‐ion, [(CO₃)₃Ce(O₂)₂Ce(CO₃)₃]^8‐. IR and Raman spectra were measured and discussed. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and Crystal Structure Analysis of One Dimensional Supramolecular [Cd (Glu) (Tu)2]n

The complex of [Cd (C₅H₆O₄) (CH₄N₂S)₂]_n ( I ) has been synthesized and its X‐ray crystal structure determined at room temperature, M = 394.74, monoclinic, space group Pc (No. 7), with lattice parameters a = 7.683(3), b = 11.566, c = 16.00(1) Å, β = 100.32 (4)°, and Z = 4. There are two different Cd sites in this complex. Cd (1) coordinates to four oxygen atoms from Glutaric anion and two sulfide atoms from thiourea. Cd (2) coordinates to three oxygen and two sulfide atoms. The Cd atoms are linked by glutaric anion to form one‐dimensional chains. The adjacent chains are held together by hydrogen bonds to form a three dimensional network.     

Syntheses and crystal structures of two polymorphs of three‐dimensional silver (I) 5‐(3‐aminophenyl)tetrazolates

Two polymorphs of silver 5‐(3‐aminophenyl)tetrazolates – α‐ and β‐Ag(amphttz) have been obtained by the reaction of amphttzH with AgNO₃ in presence of ammonia either in ambient condition or under the hydrothermal condition, respectively (amphttzH = 5‐(3‐aminophenyl)tetrazole). Both of the two phases of Ag(amphttz) were characterized by elemental analyses, IR spectra and single‐crystal X‐ray diffraction. X‐ray analysis shows α‐, β‐phases crystallize in P ‐1 with a = 8.551 (2) Å, b = 8.720(2) Å, c = 11.173(2) Å, α = 98.15(3)°, β = 90.95(3)°, γ = 95.45(3)° and C 2/c with a = 13.542(3) Å, b = 10.135(2) Å, c = 12.610(3) Å, β = 113.58(3)°, respectively. The two polymorphs exhibit different 3D structures. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and structural characterization of the dinuclear bis(glutarato)bis(urea)copper(II)complex, dihydrate

The complex [Cu(OOC-(CH₂)₃-COO)(O=C(NH₂)₂]₂·2H₂O has been synthesized and characterized by X-ray crystallography. It crystallizes in the triclinic system P-1 with a = 8.003(2) ?, b = 8.611(2) ?, c = 8.620(2) ?, α = 96.14(3)°, β = 116.66(2)°, γ = 105.66(4)° and V = 492.9(3) ?³. The structure consists of discrete centrosymmetric binuclear units and water molecules. The Cu(II) ions adopt a square-pyramidal coordination with four oxygen atoms of four bridging carboxylate and one carbonyl oxygen of the monodentate urea ligand. There is a very strong interaction between the two copper centers in binuclear entities (CuCu: 2.6266(15) ?).     

Crystal and molecular structures of a samarium complex with the 3,5-Di-tert-butyl-1,2-quinone-1-(2-hydroxy-3,5-Di-tert-butylphenyl)imine ligand

X-ray structure analysis of Sm(C₂₈H₄₀NO₂)₃ is performed. The crystals are monoclinic, a = 13.490(2) Å, b = 27.955(5) Å, c = 23.000(6) Å, β = 105.30(2)°, Z = 4, space group P2₁/c, and R = 0.0332 for 9670 reflections. The coordination number of the Sm atom is nine (tricapped trigonal prism with the O atoms in the base and the N atoms at the caps). The approximate symmetry of the complex is D ₃. The mean C-O and C-N bond lengths (1.266 and 1.342 Å, respectively) correspond to the monoanion redox form of the ligands. In distinction to the earlier studied complexes ML ₂ with the same ligands, the six-membered rings in the ligands of this complex are essentially noncoplanar: the dihedral angles between them are 42.8°, 34.0°, and 41.1°.